data_hydropascoite _audit_creation_method SHELXL-2013 _chemical_name_mineral 'hydropascoite' _chemical_compound_source 'Packrat mine, Colorado' _chemical_formula_sum 'H48 Ca3 O52 V10' _chemical_formula_weight 1510.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.08700(19) _cell_length_b 11.0708(2) _cell_length_c 21.8112(15) _cell_angle_alpha 94.112(7) _cell_angle_beta 96.053(7) _cell_angle_gamma 116.398(8) _cell_volume 2150.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.332 _exptl_crystal_F_000 1508 _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 2.566 _shelx_estimated_absorpt_T_min 0.731 _shelx_estimated_absorpt_T_max 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 36752 _diffrn_reflns_av_unetI/netI 0.0355 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.989 _diffrn_reflns_theta_max 27.443 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 9782 _reflns_number_gt 8187 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+12.1991P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9782 _refine_ls_number_parameters 730 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.16388(8) 0.49631(7) 0.00189(3) 0.01382(15) Uani 1 1 d . . . . . V2 V 0.85498(8) 0.24079(7) 0.94275(3) 0.01585(16) Uani 1 1 d . . . . . V3 V 0.92766(8) 0.32503(7) 0.08574(3) 0.01542(16) Uani 1 1 d . . . . . V4 V 0.21973(8) 0.58107(8) 0.14479(3) 0.01813(17) Uani 1 1 d . . . . . V5 V 0.91531(9) 0.58628(8) 0.14078(4) 0.01859(17) Uani 1 1 d . . . . . V6 V 0.10026(8) 0.44718(8) 0.46174(4) 0.01800(17) Uani 1 1 d . . . . . V7 V 0.84736(9) 0.24654(9) 0.53196(4) 0.02327(18) Uani 1 1 d . . . . . V8 V 0.13397(9) 0.47523(9) 0.60958(4) 0.02138(18) Uani 1 1 d . . . . . V9 V 0.80603(9) 0.22238(9) 0.38815(4) 0.02408(19) Uani 1 1 d . . . . . V10 V 0.38144(9) 0.67560(9) 0.54033(4) 0.02555(19) Uani 1 1 d . . . . . Ca1 Ca 0.71772(10) 0.92913(9) 0.03622(4) 0.0208(2) Uani 1 1 d . . . . . Ca2 Ca 0.52033(11) 0.72454(11) 0.30301(5) 0.0245(2) Uani 1 1 d . . . . . Ca3 Ca 0.21419(11) 0.11006(10) 0.27334(5) 0.0241(2) Uani 1 1 d . . . . . O1 O 0.0323(3) 0.5368(3) 0.06272(13) 0.0147(6) Uani 1 1 d . . . . . O2 O 0.0302(3) 0.3141(3) 0.01215(14) 0.0157(6) Uani 1 1 d . . . . . O3 O 0.2129(3) 0.6789(3) 0.98862(13) 0.0146(6) Uani 1 1 d . . . . . O4 O 0.8387(3) 0.3948(3) 0.13598(15) 0.0198(6) Uani 1 1 d . . . . . O5 O 0.2310(3) 0.4566(3) 0.93896(15) 0.0193(6) Uani 1 1 d . . . . . O6 O 0.9771(4) 0.2411(3) 0.88789(14) 0.0196(6) Uani 1 1 d . . . . . O7 O 0.1032(3) 0.3896(3) 0.13661(14) 0.0167(6) Uani 1 1 d . . . . . O8 O 0.7147(3) 0.2498(3) 0.88650(14) 0.0191(6) Uani 1 1 d . . . . . O9 O 0.0935(4) 0.6114(3) 0.18974(14) 0.0191(6) Uani 1 1 d . . . . . O10 O 0.2957(3) 0.5301(3) 0.06378(15) 0.0208(7) Uani 1 1 d . . . . . O11 O 0.8257(4) 0.6244(4) 0.18981(16) 0.0277(8) Uani 1 1 d . . . . . O12 O 0.7764(4) 0.0833(3) 0.95643(16) 0.0226(7) Uani 1 1 d . . . . . O13 O 0.3604(4) 0.6095(4) 0.19671(16) 0.0254(7) Uani 1 1 d . . . . . O14 O 0.8437(4) 0.1632(3) 0.09119(15) 0.0213(7) Uani 1 1 d . . . . . O15 O 0.1255(3) 0.5987(3) 0.53320(15) 0.0195(6) Uani 1 1 d . . . . . O16 O 0.0681(4) 0.3434(3) 0.53045(16) 0.0217(7) Uani 1 1 d . . . . . O17 O 0.0836(4) 0.5769(3) 0.41116(15) 0.0213(7) Uani 1 1 d . . . . . O18 O 0.0328(4) 0.3126(4) 0.40469(15) 0.0244(7) Uani 1 1 d . . . . . O19 O 0.2897(4) 0.5143(4) 0.47163(16) 0.0238(7) Uani 1 1 d . . . . . O20 O 0.6178(4) 0.2007(4) 0.39829(17) 0.0281(8) Uani 1 1 d . . . . . O21 O 0.1656(4) 0.6299(4) 0.65632(15) 0.0255(7) Uani 1 1 d . . . . . O22 O 0.8203(4) 0.1411(4) 0.45897(17) 0.0270(7) Uani 1 1 d . . . . . O23 O 0.3271(4) 0.5414(4) 0.59389(16) 0.0267(8) Uani 1 1 d . . . . . O24 O 0.6594(4) 0.2315(4) 0.52193(17) 0.0271(8) Uani 1 1 d . . . . . O25 O 0.8435(4) 0.1485(4) 0.58355(18) 0.0326(8) Uani 1 1 d . . . . . O26 O 0.7757(5) 0.1050(4) 0.33277(19) 0.0370(9) Uani 1 1 d . . . . . O27 O 0.5555(4) 0.7183(5) 0.5400(2) 0.0388(10) Uani 1 1 d . . . . . O28 O 0.1267(4) 0.3747(4) 0.66096(17) 0.0328(8) Uani 1 1 d . . . . . OW1 O 0.8392(5) 0.8522(5) 0.9676(2) 0.0362(9) Uani 1 1 d D . . . . H1A H 0.876(7) 0.870(7) 0.935(2) 0.043 Uiso 1 1 d D U . . . H1B H 0.866(8) 0.798(6) 0.981(3) 0.043 Uiso 1 1 d D U . . . OW2 O 0.9283(5) 0.9520(4) 0.10571(19) 0.0381(10) Uani 1 1 d D . . . . H2A H 0.941(8) 0.884(5) 0.109(3) 0.046 Uiso 1 1 d D U . . . H2B H 0.928(8) 0.978(6) 0.1420(17) 0.046 Uiso 1 1 d D U . . . OW3 O 0.5775(4) 0.9284(4) 0.1199(2) 0.0354(9) Uani 1 1 d D . . . . H3A H 0.545(7) 0.969(6) 0.097(3) 0.043 Uiso 1 1 d D U . . . H3B H 0.498(5) 0.865(5) 0.125(3) 0.043 Uiso 1 1 d D U . . . OW4 O 0.6108(5) 0.6978(5) 0.0573(3) 0.0618(16) Uani 1 1 d D . . . . H4A H 0.656(7) 0.657(7) 0.065(4) 0.074 Uiso 1 1 d D U . . . H4B H 0.523(4) 0.652(7) 0.059(4) 0.074 Uiso 1 1 d D U . . . OW5 O 0.4918(5) 0.8416(6) 0.9670(2) 0.0564(15) Uani 1 1 d D . . . . H5A H 0.408(5) 0.793(7) 0.972(3) 0.068 Uiso 1 1 d D U . . . H5B H 0.495(8) 0.860(8) 0.9319(19) 0.068 Uiso 1 1 d D U . . . OW6 O 0.5785(4) 0.5361(4) 0.25920(19) 0.0332(9) Uani 1 1 d D . . . . H6A H 0.491(4) 0.483(6) 0.266(3) 0.040 Uiso 1 1 d D U . . . H6B H 0.569(7) 0.518(7) 0.2217(14) 0.040 Uiso 1 1 d D U . . . OW7 O 0.4851(5) 0.5677(5) 0.38018(19) 0.0353(9) Uani 1 1 d D . . . . H7A H 0.549(6) 0.542(7) 0.388(3) 0.042 Uiso 1 1 d D U . . . H7B H 0.448(7) 0.563(7) 0.412(2) 0.042 Uiso 1 1 d D U . . . OW8 O 0.5461(5) 0.8688(4) 0.4006(2) 0.0403(10) Uani 1 1 d D . . . . H8A H 0.483(6) 0.841(6) 0.424(3) 0.048 Uiso 1 1 d D U . . . H8B H 0.597(7) 0.950(3) 0.414(3) 0.048 Uiso 1 1 d D U . . . OW9 O 0.6899(5) 0.8189(4) 0.21966(19) 0.0352(9) Uani 1 1 d D . . . . H9A H 0.718(8) 0.767(6) 0.203(3) 0.042 Uiso 1 1 d D U . . . H9B H 0.662(8) 0.849(6) 0.191(2) 0.042 Uiso 1 1 d D U . . . OW10 O 0.4822(5) 0.9072(5) 0.2639(2) 0.0399(10) Uani 1 1 d D . . . . H10A H 0.573(3) 0.960(6) 0.279(3) 0.048 Uiso 1 1 d D U . . . H10B H 0.438(6) 0.938(7) 0.284(3) 0.048 Uiso 1 1 d D U . . . OW11 O 0.2603(4) 0.6503(5) 0.31414(18) 0.0396(10) Uani 1 1 d D . . . . H11A H 0.218(7) 0.645(7) 0.3460(18) 0.047 Uiso 1 1 d D U . . . H11B H 0.198(6) 0.644(8) 0.287(2) 0.047 Uiso 1 1 d D U . . . OW12 O 0.7834(5) 0.8314(5) 0.3541(2) 0.0416(10) Uani 1 1 d D . . . . H12A H 0.744(8) 0.800(7) 0.384(2) 0.050 Uiso 1 1 d D U . . . H12B H 0.811(8) 0.782(6) 0.339(3) 0.050 Uiso 1 1 d D U . . . OW13 O 0.2768(6) -0.0092(5) 0.1938(2) 0.0467(11) Uani 1 1 d D . . . . H13A H 0.250(8) -0.087(3) 0.181(4) 0.056 Uiso 1 1 d D U . . . H13B H 0.352(6) 0.042(5) 0.183(4) 0.056 Uiso 1 1 d D U . . . OW14 O 0.3458(4) 0.0202(4) 0.34168(18) 0.0313(8) Uani 1 1 d D . . . . H14A H 0.295(6) -0.036(5) 0.362(2) 0.038 Uiso 1 1 d D U . . . H14B H 0.416(5) 0.080(5) 0.366(2) 0.038 Uiso 1 1 d D U . . . OW15 O 0.9635(4) 0.0765(4) 0.2299(2) 0.0337(9) Uani 1 1 d D . . . . H15A H 0.897(6) 0.015(4) 0.243(3) 0.040 Uiso 1 1 d D U . . . H15B H 0.957(7) 0.146(4) 0.238(3) 0.040 Uiso 1 1 d D U . . . OW16 O 0.2331(6) 0.2230(6) 0.1774(2) 0.0517(12) Uani 1 1 d D . . . . H16A H 0.199(9) 0.224(8) 0.211(2) 0.062 Uiso 1 1 d D U . . . H16B H 0.201(9) 0.266(8) 0.157(3) 0.062 Uiso 1 1 d D U . . . OW17 O 0.4886(4) 0.2601(4) 0.28010(19) 0.0328(8) Uani 1 1 d D . . . . H17A H 0.537(7) 0.271(6) 0.3142(18) 0.039 Uiso 1 1 d D U . . . H17B H 0.505(7) 0.335(4) 0.272(3) 0.039 Uiso 1 1 d D U . . . OW18 O 0.0897(6) 0.0880(5) 0.3687(2) 0.0488(12) Uani 1 1 d D . . . . H18A H 0.045(8) 0.013(4) 0.348(3) 0.059 Uiso 1 1 d D U . . . H18B H 0.091(9) 0.071(7) 0.4051(15) 0.059 Uiso 1 1 d D U . . . OW19 O 0.0484(6) -0.1383(5) 0.2747(2) 0.0532(13) Uani 1 1 d D . . . . H19A H 0.088(8) -0.096(7) 0.248(3) 0.064 Uiso 1 1 d D U . . . H19B H -0.032(5) -0.200(6) 0.258(3) 0.064 Uiso 1 1 d D U . . . OW20 O 0.2418(6) 0.3299(5) 0.3079(3) 0.0539(13) Uani 1 1 d D . . . . H20A H 0.316(5) 0.401(5) 0.322(4) 0.065 Uiso 1 1 d D U . . . H20B H 0.176(6) 0.346(7) 0.294(4) 0.065 Uiso 1 1 d D U . . . OW21 O 0.9818(6) 0.3319(5) 0.2525(2) 0.0433(11) Uani 1 1 d D . . . . H21A H 0.996(8) 0.379(7) 0.225(2) 0.052 Uiso 1 1 d D U . . . H21B H 0.940(8) 0.359(7) 0.275(3) 0.052 Uiso 1 1 d D U . . . OW22 O 0.4798(8) 0.4093(8) 0.1278(3) 0.0739(17) Uani 1 1 d D . . . . H22A H 0.450(11) 0.426(10) 0.093(2) 0.089 Uiso 1 1 d D U . . . H22B H 0.511(11) 0.355(9) 0.116(4) 0.089 Uiso 1 1 d D U . . . OW23 O 0.5982(6) 0.1749(6) 0.1691(3) 0.0617(15) Uani 1 1 d D . . . . H23A H 0.657(8) 0.170(10) 0.199(3) 0.074 Uiso 1 1 d D U . . . H23B H 0.537(7) 0.183(9) 0.190(3) 0.074 Uiso 1 1 d D U . . . OW24 O 0.1645(11) 0.1424(12) 0.5121(4) 0.134(4) Uani 1 1 d D . . . . H24A H 0.192(14) 0.126(14) 0.481(4) 0.161 Uiso 1 1 d D U . . . H24B H 0.084(9) 0.081(11) 0.513(7) 0.161 Uiso 1 1 d D U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0122(3) 0.0138(3) 0.0151(3) 0.0021(3) 0.0029(3) 0.0055(3) V2 0.0174(4) 0.0117(3) 0.0159(3) 0.0008(3) 0.0022(3) 0.0046(3) V3 0.0164(3) 0.0128(3) 0.0151(3) 0.0025(3) 0.0024(3) 0.0048(3) V4 0.0163(4) 0.0182(4) 0.0163(4) 0.0016(3) -0.0008(3) 0.0055(3) V5 0.0211(4) 0.0189(4) 0.0164(4) 0.0011(3) 0.0063(3) 0.0091(3) V6 0.0170(4) 0.0199(4) 0.0184(4) 0.0030(3) 0.0058(3) 0.0090(3) V7 0.0233(4) 0.0211(4) 0.0237(4) 0.0082(3) 0.0065(3) 0.0072(3) V8 0.0214(4) 0.0244(4) 0.0194(4) 0.0053(3) 0.0023(3) 0.0112(3) V9 0.0218(4) 0.0225(4) 0.0245(4) -0.0013(3) 0.0045(3) 0.0075(3) V10 0.0170(4) 0.0313(5) 0.0255(4) 0.0003(3) 0.0042(3) 0.0087(3) Ca1 0.0189(4) 0.0173(4) 0.0246(5) 0.0043(4) 0.0045(3) 0.0064(4) Ca2 0.0237(5) 0.0283(5) 0.0237(5) 0.0063(4) 0.0055(4) 0.0131(4) Ca3 0.0223(5) 0.0239(5) 0.0250(5) 0.0007(4) 0.0022(4) 0.0101(4) O1 0.0145(14) 0.0137(14) 0.0149(14) 0.0028(11) 0.0039(11) 0.0051(12) O2 0.0136(14) 0.0132(14) 0.0200(15) 0.0023(12) 0.0032(11) 0.0058(12) O3 0.0130(14) 0.0145(14) 0.0144(14) 0.0019(11) 0.0035(11) 0.0042(12) O4 0.0173(15) 0.0197(16) 0.0206(16) 0.0040(13) 0.0063(12) 0.0059(13) O5 0.0161(15) 0.0212(16) 0.0217(16) 0.0036(13) 0.0059(12) 0.0087(13) O6 0.0241(16) 0.0170(16) 0.0173(15) 0.0006(12) 0.0040(12) 0.0089(13) O7 0.0189(15) 0.0160(15) 0.0154(14) 0.0026(12) 0.0040(11) 0.0078(12) O8 0.0160(15) 0.0164(15) 0.0190(15) 0.0011(12) 0.0006(12) 0.0028(12) O9 0.0206(16) 0.0194(16) 0.0160(15) 0.0022(12) 0.0024(12) 0.0081(13) O10 0.0148(15) 0.0212(16) 0.0246(17) 0.0004(13) -0.0001(12) 0.0077(13) O11 0.0292(18) 0.0303(19) 0.0232(17) -0.0011(14) 0.0095(14) 0.0127(16) O12 0.0255(17) 0.0131(15) 0.0252(17) 0.0033(13) 0.0035(13) 0.0053(13) O13 0.0209(16) 0.0293(19) 0.0233(17) -0.0019(14) -0.0038(13) 0.0115(15) O14 0.0228(16) 0.0165(16) 0.0239(17) 0.0058(13) 0.0059(13) 0.0074(13) O15 0.0170(15) 0.0209(16) 0.0211(16) 0.0041(13) 0.0049(12) 0.0085(13) O16 0.0220(16) 0.0213(16) 0.0255(17) 0.0075(13) 0.0059(13) 0.0120(14) O17 0.0219(16) 0.0252(17) 0.0181(15) 0.0045(13) 0.0049(12) 0.0113(14) O18 0.0262(17) 0.0258(18) 0.0213(16) 0.0000(14) 0.0066(13) 0.0118(15) O19 0.0178(16) 0.0299(18) 0.0248(17) 0.0021(14) 0.0058(13) 0.0116(14) O20 0.0221(17) 0.0305(19) 0.0271(18) -0.0018(15) 0.0041(14) 0.0087(15) O21 0.0247(17) 0.0301(19) 0.0198(16) 0.0024(14) 0.0045(13) 0.0107(15) O22 0.0291(18) 0.0198(17) 0.0307(19) 0.0041(14) 0.0069(14) 0.0093(15) O23 0.0222(17) 0.038(2) 0.0230(17) 0.0056(15) 0.0040(13) 0.0161(16) O24 0.0217(17) 0.0287(19) 0.0279(18) 0.0066(15) 0.0098(14) 0.0071(15) O25 0.039(2) 0.0260(19) 0.031(2) 0.0149(16) 0.0119(16) 0.0104(16) O26 0.036(2) 0.035(2) 0.034(2) -0.0092(17) 0.0061(17) 0.0127(18) O27 0.0202(18) 0.050(3) 0.042(2) 0.0020(19) 0.0060(16) 0.0123(18) O28 0.036(2) 0.040(2) 0.0268(19) 0.0141(16) 0.0043(15) 0.0203(18) OW1 0.046(2) 0.043(2) 0.038(2) 0.0133(19) 0.0164(18) 0.033(2) OW2 0.049(2) 0.036(2) 0.037(2) -0.0087(18) -0.0089(19) 0.032(2) OW3 0.0247(19) 0.034(2) 0.040(2) 0.0039(17) 0.0138(16) 0.0049(16) OW4 0.031(2) 0.029(2) 0.135(5) 0.034(3) 0.030(3) 0.016(2) OW5 0.019(2) 0.081(4) 0.046(3) 0.033(3) 0.0001(18) 0.000(2) OW6 0.031(2) 0.036(2) 0.035(2) 0.0100(17) 0.0131(16) 0.0148(17) OW7 0.042(2) 0.047(2) 0.034(2) 0.0175(19) 0.0174(18) 0.031(2) OW8 0.043(2) 0.032(2) 0.038(2) 0.0007(18) 0.0195(19) 0.0075(19) OW9 0.038(2) 0.036(2) 0.034(2) 0.0095(18) 0.0090(17) 0.0176(18) OW10 0.047(3) 0.041(2) 0.042(2) 0.0117(19) 0.010(2) 0.028(2) OW11 0.027(2) 0.064(3) 0.0239(19) 0.005(2) 0.0069(15) 0.016(2) OW12 0.032(2) 0.048(3) 0.045(3) -0.002(2) 0.0042(18) 0.020(2) OW13 0.053(3) 0.049(3) 0.037(2) -0.013(2) 0.005(2) 0.025(2) OW14 0.0255(19) 0.027(2) 0.033(2) 0.0092(16) -0.0004(15) 0.0055(15) OW15 0.0236(19) 0.035(2) 0.039(2) 0.0054(18) 0.0046(16) 0.0107(17) OW16 0.060(3) 0.065(3) 0.050(3) 0.033(3) 0.019(2) 0.040(3) OW17 0.030(2) 0.028(2) 0.035(2) 0.0088(16) -0.0021(16) 0.0102(17) OW18 0.068(3) 0.056(3) 0.038(2) 0.005(2) 0.016(2) 0.041(3) OW19 0.049(3) 0.030(2) 0.058(3) 0.001(2) -0.001(2) 0.001(2) OW20 0.039(3) 0.032(2) 0.086(4) -0.009(2) 0.006(3) 0.015(2) OW21 0.059(3) 0.055(3) 0.032(2) 0.019(2) 0.025(2) 0.034(2) OW22 0.078(4) 0.089(5) 0.069(4) 0.032(4) 0.026(3) 0.045(4) OW23 0.055(3) 0.045(3) 0.079(4) 0.000(3) 0.037(3) 0.013(3) OW24 0.168(8) 0.266(12) 0.108(6) 0.133(7) 0.098(6) 0.190(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O10 1.684(3) . ? V1 O5 1.706(3) 1_554 ? V1 O3 1.908(3) 1_554 ? V1 O2 1.910(3) . ? V1 O1 2.131(3) . ? V1 O1 2.174(3) 2_565 ? V1 V5 3.0947(10) 2_665 ? V1 V4 3.1067(10) . ? V2 O12 1.629(3) . ? V2 O6 1.805(3) . ? V2 O8 1.815(3) . ? V2 O2 2.014(3) 1_656 ? V2 O3 2.016(3) 2_667 ? V2 O1 2.225(3) 2_666 ? V2 V3 3.1027(10) 1_556 ? V2 V4 3.1082(11) 2_666 ? V3 O14 1.626(3) . ? V3 O7 1.795(3) 1_655 ? V3 O4 1.818(3) . ? V3 O3 2.023(3) 2_666 ? V3 O2 2.023(3) 1_655 ? V3 O1 2.224(3) 1_655 ? V3 V4 3.1022(11) 1_655 ? V3 V2 3.1028(10) 1_554 ? V3 V5 3.1107(11) . ? V4 O13 1.615(3) . ? V4 O9 1.815(3) . ? V4 O8 1.894(3) 2_666 ? V4 O7 1.895(3) . ? V4 O10 2.134(3) . ? V4 O1 2.314(3) . ? V4 V5 3.0890(11) 1_455 ? V4 V3 3.1022(11) 1_455 ? V4 V2 3.1082(11) 2_666 ? V5 O11 1.617(3) . ? V5 O9 1.886(3) 1_655 ? V5 O4 1.897(3) . ? V5 O6 1.921(3) 2_766 ? V5 O5 2.036(3) 2_666 ? V5 O1 2.335(3) 1_655 ? V5 V4 3.0890(11) 1_655 ? V5 V1 3.0946(10) 2_665 ? V6 O19 1.696(3) . ? V6 O18 1.699(3) . ? V6 O16 1.921(3) . ? V6 O17 1.926(3) . ? V6 O15 2.114(3) . ? V6 O15 2.119(3) 2_566 ? V6 V10 3.0582(12) . ? V6 V9 3.0713(12) 1_455 ? V7 O25 1.610(4) . ? V7 O24 1.815(4) . ? V7 O22 1.825(4) . ? V7 O16 2.002(3) 1_655 ? V7 O17 2.026(3) 2_666 ? V7 O15 2.246(3) 2_666 ? V7 V8 3.0788(12) 1_655 ? V7 V9 3.0965(12) . ? V8 O28 1.620(4) . ? V8 O21 1.808(4) . ? V8 O23 1.832(4) . ? V8 O17 1.995(3) 2_566 ? V8 O16 2.021(4) . ? V8 O15 2.247(3) . ? V8 V7 3.0788(12) 1_455 ? V9 O26 1.608(4) . ? V9 O20 1.844(4) . ? V9 O22 1.866(4) . ? V9 O21 1.888(4) 2_666 ? V9 O18 2.025(4) 1_655 ? V9 O15 2.322(3) 2_666 ? V9 V6 3.0713(12) 1_655 ? V9 V10 3.0908(12) 2_666 ? V10 O27 1.603(4) . ? V10 O20 1.842(4) 2_666 ? V10 O23 1.879(4) . ? V10 O24 1.879(4) 2_666 ? V10 O19 2.036(4) . ? V10 O15 2.314(3) . ? V10 V9 3.0908(12) 2_666 ? Ca1 OW5 2.348(4) 1_554 ? Ca1 OW1 2.366(4) 1_554 ? Ca1 OW2 2.379(4) . ? Ca1 OW4 2.398(4) . ? Ca1 OW3 2.423(4) . ? Ca1 O12 2.457(3) 1_564 ? Ca1 O14 2.464(3) 1_565 ? Ca1 H3A 2.47(7) . ? Ca2 OW10 2.415(4) . ? Ca2 OW11 2.421(4) . ? Ca2 OW7 2.443(4) . ? Ca2 OW12 2.466(5) . ? Ca2 OW8 2.486(4) . ? Ca2 OW6 2.555(4) . ? Ca2 O13 2.561(3) . ? Ca2 OW9 2.581(4) . ? Ca2 H6A 2.62(7) . ? Ca2 H10A 2.52(7) . ? Ca2 H12A 2.49(8) . ? Ca2 H12B 2.72(7) . ? Ca3 OW20 2.379(5) . ? Ca3 OW13 2.407(4) . ? Ca3 OW14 2.438(4) . ? Ca3 OW15 2.457(4) 1_455 ? Ca3 OW16 2.496(5) . ? Ca3 OW17 2.497(4) . ? Ca3 OW19 2.508(5) . ? Ca3 OW18 2.513(5) . ? Ca3 H13B 2.78(6) . ? Ca3 H16A 1.97(6) . ? Ca3 H18A 2.43(7) . ? Ca3 H19A 2.06(7) . ? O1 V1 2.174(3) 2_565 ? O1 V3 2.224(3) 1_455 ? O1 V2 2.225(3) 2_666 ? O1 V5 2.335(3) 1_455 ? O2 V2 2.014(3) 1_454 ? O2 V3 2.023(3) 1_455 ? O3 V1 1.908(3) 1_556 ? O3 V2 2.016(3) 2_667 ? O3 V3 2.023(3) 2_666 ? O5 V1 1.706(3) 1_556 ? O5 V5 2.036(3) 2_666 ? O6 V5 1.921(3) 2_766 ? O7 V3 1.795(3) 1_455 ? O8 V4 1.894(3) 2_666 ? O9 V5 1.886(3) 1_455 ? O12 Ca1 2.457(3) 1_546 ? O14 Ca1 2.464(3) 1_545 ? O15 V6 2.119(3) 2_566 ? O15 V7 2.246(3) 2_666 ? O15 V9 2.322(3) 2_666 ? O16 V7 2.002(3) 1_455 ? O17 V8 1.995(3) 2_566 ? O17 V7 2.026(3) 2_666 ? O18 V9 2.026(4) 1_455 ? O20 V10 1.842(4) 2_666 ? O21 V9 1.888(4) 2_666 ? O24 V10 1.879(4) 2_666 ? OW1 Ca1 2.366(4) 1_556 ? OW1 H1A 0.84(3) . ? OW1 H1B 0.81(3) . ? OW2 H2A 0.83(3) . ? OW2 H2B 0.82(3) . ? OW3 H3A 0.83(3) . ? OW3 H3B 0.82(3) . ? OW4 H4A 0.79(3) . ? OW4 H4B 0.81(3) . ? OW5 Ca1 2.348(4) 1_556 ? OW5 H5A 0.80(3) . ? OW5 H5B 0.80(3) . ? OW6 H6A 0.85(3) . ? OW6 H6B 0.81(3) . ? OW7 H7A 0.82(3) . ? OW7 H7B 0.82(3) . ? OW8 H8A 0.82(3) . ? OW8 H8B 0.82(3) . ? OW9 H9A 0.82(3) . ? OW9 H9B 0.81(3) . ? OW10 H10A 0.85(3) . ? OW10 H10B 0.81(3) . ? OW11 H11A 0.84(3) . ? OW11 H11B 0.79(3) . ? OW12 H12A 0.81(3) . ? OW12 H12B 0.79(3) . ? OW13 H13A 0.80(3) . ? OW13 H13B 0.80(3) . ? OW14 H14A 0.81(3) . ? OW14 H14B 0.82(3) . ? OW15 Ca3 2.457(4) 1_655 ? OW15 H15A 0.81(3) . ? OW15 H15B 0.81(3) . ? OW16 H16A 0.84(3) . ? OW16 H16B 0.82(3) . ? OW17 H17A 0.81(3) . ? OW17 H17B 0.81(3) . ? OW18 H18A 0.82(3) . ? OW18 H18B 0.83(3) . ? OW19 H19A 0.80(3) . ? OW19 H19B 0.82(3) . ? OW20 H20A 0.82(3) . ? OW20 H20B 0.80(3) . ? OW21 H21A 0.81(3) . ? OW21 H21B 0.81(3) . ? OW22 H22A 0.84(3) . ? OW22 H22B 0.83(3) . ? OW23 H23A 0.86(3) . ? OW23 H23B 0.83(3) . ? OW24 H24A 0.81(3) . ? OW24 H24B 0.80(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 V1 O5 106.03(16) . 1_554 ? O10 V1 O3 98.46(15) . 1_554 ? O5 V1 O3 96.83(14) 1_554 1_554 ? O10 V1 O2 98.56(15) . . ? O5 V1 O2 96.91(15) 1_554 . ? O3 V1 O2 154.21(13) 1_554 . ? O10 V1 O1 88.84(14) . . ? O5 V1 O1 165.13(14) 1_554 . ? O3 V1 O1 80.54(12) 1_554 . ? O2 V1 O1 80.59(12) . . ? O10 V1 O1 167.26(14) . 2_565 ? O5 V1 O1 86.71(13) 1_554 2_565 ? O3 V1 O1 79.49(12) 1_554 2_565 ? O2 V1 O1 79.64(12) . 2_565 ? O1 V1 O1 78.42(12) . 2_565 ? O10 V1 V5 143.86(12) . 2_665 ? O5 V1 V5 37.82(11) 1_554 2_665 ? O3 V1 V5 88.58(9) 1_554 2_665 ? O2 V1 V5 89.01(10) . 2_665 ? O1 V1 V5 127.30(9) . 2_665 ? O1 V1 V5 48.88(8) 2_565 2_665 ? O10 V1 V4 40.70(11) . . ? O5 V1 V4 146.74(11) 1_554 . ? O3 V1 V4 90.16(9) 1_554 . ? O2 V1 V4 90.21(10) . . ? O1 V1 V4 48.14(8) . . ? O1 V1 V4 126.56(8) 2_565 . ? V5 V1 V4 175.43(3) 2_665 . ? O12 V2 O6 103.20(16) . . ? O12 V2 O8 103.57(16) . . ? O6 V2 O8 95.91(15) . . ? O12 V2 O2 98.15(15) . 1_656 ? O6 V2 O2 89.73(14) . 1_656 ? O8 V2 O2 155.61(14) . 1_656 ? O12 V2 O3 98.12(15) . 2_667 ? O6 V2 O3 155.91(14) . 2_667 ? O8 V2 O3 89.81(14) . 2_667 ? O2 V2 O3 76.14(12) 1_656 2_667 ? O12 V2 O1 172.62(15) . 2_666 ? O6 V2 O1 81.80(13) . 2_666 ? O8 V2 O1 81.06(13) . 2_666 ? O2 V2 O1 76.28(12) 1_656 2_666 ? O3 V2 O1 75.98(12) 2_667 2_666 ? O12 V2 V3 87.41(12) . 1_556 ? O6 V2 V3 129.62(11) . 1_556 ? O8 V2 V3 129.70(11) . 1_556 ? O2 V2 V3 39.89(9) 1_656 1_556 ? O3 V2 V3 39.89(9) 2_667 1_556 ? O1 V2 V3 85.21(8) 2_666 1_556 ? O12 V2 V4 137.24(13) . 2_666 ? O6 V2 V4 83.79(11) . 2_666 ? O8 V2 V4 33.87(10) . 2_666 ? O2 V2 V4 124.28(9) 1_656 2_666 ? O3 V2 V4 88.17(9) 2_667 2_666 ? O1 V2 V4 48.00(8) 2_666 2_666 ? V3 V2 V4 120.65(3) 1_556 2_666 ? O14 V3 O7 104.99(16) . 1_655 ? O14 V3 O4 103.19(16) . . ? O7 V3 O4 96.35(14) 1_655 . ? O14 V3 O3 96.90(15) . 2_666 ? O7 V3 O3 155.33(13) 1_655 2_666 ? O4 V3 O3 89.47(14) . 2_666 ? O14 V3 O2 97.55(15) . 1_655 ? O7 V3 O2 89.99(13) 1_655 1_655 ? O4 V3 O2 155.87(14) . 1_655 ? O3 V3 O2 75.79(12) 2_666 1_655 ? O14 V3 O1 171.25(15) . 1_655 ? O7 V3 O1 81.13(13) 1_655 1_655 ? O4 V3 O1 82.03(13) . 1_655 ? O3 V3 O1 75.95(12) 2_666 1_655 ? O2 V3 O1 75.97(12) 1_655 1_655 ? O14 V3 V4 138.65(12) . 1_655 ? O7 V3 V4 33.82(10) 1_655 1_655 ? O4 V3 V4 84.27(10) . 1_655 ? O3 V3 V4 124.06(9) 2_666 1_655 ? O2 V3 V4 88.29(9) 1_655 1_655 ? O1 V3 V4 48.11(8) 1_655 1_655 ? O14 V3 V2 86.32(12) . 1_554 ? O7 V3 V2 129.66(10) 1_655 1_554 ? O4 V3 V2 129.20(11) . 1_554 ? O3 V3 V2 39.74(9) 2_666 1_554 ? O2 V3 V2 39.68(9) 1_655 1_554 ? O1 V3 V2 84.96(8) 1_655 1_554 ? V4 V3 V2 120.51(3) 1_655 1_554 ? O14 V3 V5 137.12(12) . . ? O7 V3 V5 85.47(10) 1_655 . ? O4 V3 V5 33.94(10) . . ? O3 V3 V5 86.15(9) 2_666 . ? O2 V3 V5 124.35(9) 1_655 . ? O1 V3 V5 48.50(8) 1_655 . ? V4 V3 V5 59.63(2) 1_655 . ? V2 V3 V5 119.01(3) 1_554 . ? O13 V4 O9 103.19(16) . . ? O13 V4 O8 101.93(17) . 2_666 ? O9 V4 O8 93.25(15) . 2_666 ? O13 V4 O7 103.09(17) . . ? O9 V4 O7 92.73(14) . . ? O8 V4 O7 152.18(14) 2_666 . ? O13 V4 O10 99.75(16) . . ? O9 V4 O10 157.06(14) . . ? O8 V4 O10 81.88(14) 2_666 . ? O7 V4 O10 82.08(13) . . ? O13 V4 O1 174.01(15) . . ? O9 V4 O1 82.79(12) . . ? O8 V4 O1 77.11(12) 2_666 . ? O7 V4 O1 76.73(12) . . ? O10 V4 O1 74.26(11) . . ? O13 V4 V5 137.32(13) . 1_455 ? O9 V4 V5 34.13(10) . 1_455 ? O8 V4 V5 85.32(10) 2_666 1_455 ? O7 V4 V5 84.53(10) . 1_455 ? O10 V4 V5 122.93(9) . 1_455 ? O1 V4 V5 48.66(7) . 1_455 ? O13 V4 V3 134.76(14) . 1_455 ? O9 V4 V3 82.52(10) . 1_455 ? O8 V4 V3 122.75(10) 2_666 1_455 ? O7 V4 V3 31.81(9) . 1_455 ? O10 V4 V3 81.42(9) . 1_455 ? O1 V4 V3 45.66(7) . 1_455 ? V5 V4 V3 60.32(2) 1_455 1_455 ? O13 V4 V1 130.73(13) . . ? O9 V4 V1 126.08(10) . . ? O8 V4 V1 77.32(10) 2_666 . ? O7 V4 V1 77.21(9) . . ? O10 V4 V1 30.98(9) . . ? O1 V4 V1 43.29(7) . . ? V5 V4 V1 91.95(3) 1_455 . ? V3 V4 V1 61.29(2) 1_455 . ? O13 V4 V2 134.05(14) . 2_666 ? O9 V4 V2 82.78(11) . 2_666 ? O8 V4 V2 32.27(9) 2_666 2_666 ? O7 V4 V2 122.31(10) . 2_666 ? O10 V4 V2 81.26(9) . 2_666 ? O1 V4 V2 45.59(7) . 2_666 ? V5 V4 V2 60.68(3) 1_455 2_666 ? V3 V4 V2 91.06(3) 1_455 2_666 ? V1 V4 V2 61.18(2) . 2_666 ? O11 V5 O9 104.12(17) . 1_655 ? O11 V5 O4 104.60(17) . . ? O9 V5 O4 90.48(14) 1_655 . ? O11 V5 O6 100.90(17) . 2_766 ? O9 V5 O6 89.75(14) 1_655 2_766 ? O4 V5 O6 153.63(14) . 2_766 ? O11 V5 O5 99.62(16) . 2_666 ? O9 V5 O5 156.22(13) 1_655 2_666 ? O4 V5 O5 84.82(14) . 2_666 ? O6 V5 O5 84.42(14) 2_766 2_666 ? O11 V5 O1 174.58(16) . 1_655 ? O9 V5 O1 80.77(12) 1_655 1_655 ? O4 V5 O1 77.44(12) . 1_655 ? O6 V5 O1 76.57(12) 2_766 1_655 ? O5 V5 O1 75.45(12) 2_666 1_655 ? O11 V5 V4 136.78(14) . 1_655 ? O9 V5 V4 32.69(10) 1_655 1_655 ? O4 V5 V4 83.44(10) . 1_655 ? O6 V5 V4 82.60(10) 2_766 1_655 ? O5 V5 V4 123.54(9) 2_666 1_655 ? O1 V5 V4 48.08(7) 1_655 1_655 ? O11 V5 V1 130.51(14) . 2_665 ? O9 V5 V1 125.30(10) 1_655 2_665 ? O4 V5 V1 79.47(10) . 2_665 ? O6 V5 V1 78.94(10) 2_766 2_665 ? O5 V5 V1 30.92(9) 2_666 2_665 ? O1 V5 V1 44.53(7) 1_655 2_665 ? V4 V5 V1 92.62(3) 1_655 2_665 ? O11 V5 V3 136.89(14) . . ? O9 V5 V3 81.26(10) 1_655 . ? O4 V5 V3 32.34(10) . . ? O6 V5 V3 122.05(10) 2_766 . ? O5 V5 V3 82.39(9) 2_666 . ? O1 V5 V3 45.49(7) 1_655 . ? V4 V5 V3 60.05(3) 1_655 . ? V1 V5 V3 61.99(2) 2_665 . ? O19 V6 O18 106.74(17) . . ? O19 V6 O16 97.47(16) . . ? O18 V6 O16 96.56(16) . . ? O19 V6 O17 96.93(16) . . ? O18 V6 O17 97.38(16) . . ? O16 V6 O17 156.14(14) . . ? O19 V6 O15 87.90(15) . . ? O18 V6 O15 165.35(15) . . ? O16 V6 O15 80.65(14) . . ? O17 V6 O15 80.98(13) . . ? O19 V6 O15 166.16(15) . 2_566 ? O18 V6 O15 87.09(15) . 2_566 ? O16 V6 O15 80.41(13) . 2_566 ? O17 V6 O15 81.06(13) . 2_566 ? O15 V6 O15 78.26(13) . 2_566 ? O19 V6 V10 38.80(12) . . ? O18 V6 V10 145.54(12) . . ? O16 V6 V10 89.63(11) . . ? O17 V6 V10 89.76(10) . . ? O15 V6 V10 49.10(9) . . ? O15 V6 V10 127.36(9) 2_566 . ? O19 V6 V9 144.80(12) . 1_455 ? O18 V6 V9 38.06(12) . 1_455 ? O16 V6 V9 89.12(11) . 1_455 ? O17 V6 V9 90.00(10) . 1_455 ? O15 V6 V9 127.30(9) . 1_455 ? O15 V6 V9 49.04(9) 2_566 1_455 ? V10 V6 V9 176.36(3) . 1_455 ? O25 V7 O24 103.63(19) . . ? O25 V7 O22 103.18(19) . . ? O24 V7 O22 95.30(17) . . ? O25 V7 O16 99.79(18) . 1_655 ? O24 V7 O16 153.88(16) . 1_655 ? O22 V7 O16 90.45(15) . 1_655 ? O25 V7 O17 99.20(18) . 2_666 ? O24 V7 O17 88.59(15) . 2_666 ? O22 V7 O17 155.65(15) . 2_666 ? O16 V7 O17 76.31(14) 1_655 2_666 ? O25 V7 O15 173.75(18) . 2_666 ? O24 V7 O15 80.08(14) . 2_666 ? O22 V7 O15 81.30(14) . 2_666 ? O16 V7 O15 75.64(13) 1_655 2_666 ? O17 V7 O15 75.70(13) 2_666 2_666 ? O25 V7 V8 89.13(15) . 1_655 ? O24 V7 V8 128.25(12) . 1_655 ? O22 V7 V8 130.74(12) . 1_655 ? O16 V7 V8 40.29(10) 1_655 1_655 ? O17 V7 V8 39.66(9) 2_666 1_655 ? O15 V7 V8 84.63(9) 2_666 1_655 ? O25 V7 V9 136.46(15) . . ? O24 V7 V9 84.01(12) . . ? O22 V7 V9 33.40(11) . . ? O16 V7 V9 86.97(10) 1_655 . ? O17 V7 V9 124.03(10) 2_666 . ? O15 V7 V9 48.35(8) 2_666 . ? V8 V7 V9 119.86(3) 1_655 . ? O28 V8 O21 103.01(19) . . ? O28 V8 O23 103.09(19) . . ? O21 V8 O23 94.66(17) . . ? O28 V8 O17 99.67(17) . 2_566 ? O21 V8 O17 90.77(15) . 2_566 ? O23 V8 O17 154.72(15) . 2_566 ? O28 V8 O16 100.44(18) . . ? O21 V8 O16 154.92(15) . . ? O23 V8 O16 88.55(15) . . ? O17 V8 O16 76.57(14) 2_566 . ? O28 V8 O15 174.77(17) . . ? O21 V8 O15 80.71(14) . . ? O23 V8 O15 80.08(14) . . ? O17 V8 O15 76.46(13) 2_566 . ? O16 V8 O15 75.35(13) . . ? O28 V8 V7 89.82(15) . 1_455 ? O21 V8 V7 131.15(12) . 1_455 ? O23 V8 V7 128.39(12) . 1_455 ? O17 V8 V7 40.40(10) 2_566 1_455 ? O16 V8 V7 39.84(10) . 1_455 ? O15 V8 V7 84.96(9) . 1_455 ? O26 V9 O20 104.42(19) . . ? O26 V9 O22 102.4(2) . . ? O20 V9 O22 91.89(17) . . ? O26 V9 O21 101.3(2) . 2_666 ? O20 V9 O21 89.72(17) . 2_666 ? O22 V9 O21 154.98(16) . 2_666 ? O26 V9 O18 99.78(18) . 1_655 ? O20 V9 O18 155.76(15) . 1_655 ? O22 V9 O18 84.32(15) . 1_655 ? O21 V9 O18 84.03(15) 2_666 1_655 ? O26 V9 O15 174.34(17) . 2_666 ? O20 V9 O15 81.09(14) . 2_666 ? O22 V9 O15 78.43(14) . 2_666 ? O21 V9 O15 77.16(13) 2_666 2_666 ? O18 V9 O15 74.69(12) 1_655 2_666 ? O26 V9 V6 130.89(15) . 1_655 ? O20 V9 V6 124.64(12) . 1_655 ? O22 V9 V6 79.79(11) . 1_655 ? O21 V9 V6 78.79(11) 2_666 1_655 ? O18 V9 V6 31.13(10) 1_655 1_655 ? O15 V9 V6 43.56(8) 2_666 1_655 ? O26 V9 V10 137.43(15) . 2_666 ? O20 V9 V10 33.01(11) . 2_666 ? O22 V9 V10 84.51(12) . 2_666 ? O21 V9 V10 83.32(11) 2_666 2_666 ? O18 V9 V10 122.77(10) 1_655 2_666 ? O15 V9 V10 48.08(8) 2_666 2_666 ? V6 V9 V10 91.65(3) 1_655 2_666 ? O26 V9 V7 134.93(17) . . ? O20 V9 V7 82.19(12) . . ? O22 V9 V7 32.55(11) . . ? O21 V9 V7 123.46(11) 2_666 . ? O18 V9 V7 81.83(10) 1_655 . ? O15 V9 V7 46.30(8) 2_666 . ? V6 V9 V7 61.90(3) 1_655 . ? V10 V9 V7 60.62(3) 2_666 . ? O27 V10 O20 104.0(2) . 2_666 ? O27 V10 O23 102.6(2) . . ? O20 V10 O23 90.53(17) 2_666 . ? O27 V10 O24 102.4(2) . 2_666 ? O20 V10 O24 91.17(17) 2_666 2_666 ? O23 V10 O24 153.79(16) . 2_666 ? O27 V10 O19 99.58(18) . . ? O20 V10 O19 156.46(15) 2_666 . ? O23 V10 O19 84.29(15) . . ? O24 V10 O19 83.78(15) 2_666 . ? O27 V10 O15 174.70(18) . . ? O20 V10 O15 81.33(14) 2_666 . ? O23 V10 O15 77.39(13) . . ? O24 V10 O15 77.03(14) 2_666 . ? O19 V10 O15 75.13(12) . . ? O27 V10 V6 131.05(16) . . ? O20 V10 V6 125.00(12) 2_666 . ? O23 V10 V6 78.98(11) . . ? O24 V10 V6 78.67(11) 2_666 . ? O19 V10 V6 31.47(9) . . ? O15 V10 V6 43.66(8) . . ? O27 V10 V9 137.00(16) . 2_666 ? O20 V10 V9 33.05(11) 2_666 2_666 ? O23 V10 V9 84.06(11) . 2_666 ? O24 V10 V9 83.21(11) 2_666 2_666 ? O19 V10 V9 123.42(10) . 2_666 ? O15 V10 V9 48.29(8) . 2_666 ? V6 V10 V9 91.95(3) . 2_666 ? OW5 Ca1 OW1 94.16(19) 1_554 1_554 ? OW5 Ca1 OW2 163.91(19) 1_554 . ? OW1 Ca1 OW2 79.31(15) 1_554 . ? OW5 Ca1 OW4 81.0(2) 1_554 . ? OW1 Ca1 OW4 83.11(18) 1_554 . ? OW2 Ca1 OW4 83.60(18) . . ? OW5 Ca1 OW3 88.03(17) 1_554 . ? OW1 Ca1 OW3 158.61(16) 1_554 . ? OW2 Ca1 OW3 92.85(15) . . ? OW4 Ca1 OW3 76.22(18) . . ? OW5 Ca1 O12 76.47(14) 1_554 1_564 ? OW1 Ca1 O12 74.36(13) 1_554 1_564 ? OW2 Ca1 O12 115.16(15) . 1_564 ? OW4 Ca1 O12 146.6(2) . 1_564 ? OW3 Ca1 O12 126.64(14) . 1_564 ? OW5 Ca1 O14 123.47(19) 1_554 1_565 ? OW1 Ca1 O14 120.70(14) 1_554 1_565 ? OW2 Ca1 O14 72.03(13) . 1_565 ? OW4 Ca1 O14 140.5(2) . 1_565 ? OW3 Ca1 O14 74.47(13) . 1_565 ? O12 Ca1 O14 72.94(11) 1_564 1_565 ? OW5 Ca1 H3A 75.9(14) 1_554 . ? OW1 Ca1 H3A 168.5(15) 1_554 . ? OW2 Ca1 H3A 108.7(12) . . ? OW4 Ca1 H3A 89.6(11) . . ? OW3 Ca1 H3A 19.5(7) . . ? O12 Ca1 H3A 108.2(7) 1_564 . ? O14 Ca1 H3A 70.3(15) 1_565 . ? OW10 Ca2 OW11 79.69(17) . . ? OW10 Ca2 OW7 149.80(15) . . ? OW11 Ca2 OW7 78.13(15) . . ? OW10 Ca2 OW12 105.27(16) . . ? OW11 Ca2 OW12 147.37(15) . . ? OW7 Ca2 OW12 83.50(16) . . ? OW10 Ca2 OW8 77.96(16) . . ? OW11 Ca2 OW8 78.89(15) . . ? OW7 Ca2 OW8 77.86(15) . . ? OW12 Ca2 OW8 70.97(15) . . ? OW10 Ca2 OW6 136.66(15) . . ? OW11 Ca2 OW6 114.59(15) . . ? OW7 Ca2 OW6 72.08(14) . . ? OW12 Ca2 OW6 84.33(14) . . ? OW8 Ca2 OW6 142.91(16) . . ? OW10 Ca2 O13 78.11(14) . . ? OW11 Ca2 O13 71.90(13) . . ? OW7 Ca2 O13 113.55(14) . . ? OW12 Ca2 O13 140.67(14) . . ? OW8 Ca2 O13 144.94(15) . . ? OW6 Ca2 O13 69.36(13) . . ? OW10 Ca2 OW9 70.78(15) . . ? OW11 Ca2 OW9 137.62(14) . . ? OW7 Ca2 OW9 138.46(14) . . ? OW12 Ca2 OW9 71.75(15) . . ? OW8 Ca2 OW9 121.78(14) . . ? OW6 Ca2 OW9 72.70(13) . . ? O13 Ca2 OW9 72.75(13) . . ? OW10 Ca2 H6A 141.0(13) . . ? OW11 Ca2 H6A 96.1(8) . . ? OW7 Ca2 H6A 62.1(12) . . ? OW12 Ca2 H6A 98.8(11) . . ? OW8 Ca2 H6A 139.7(12) . . ? OW6 Ca2 H6A 18.9(7) . . ? O13 Ca2 H6A 64.0(13) . . ? OW9 Ca2 H6A 88.8(8) . . ? OW10 Ca2 H10A 19.8(8) . . ? OW11 Ca2 H10A 96.3(9) . . ? OW7 Ca2 H10A 148.6(15) . . ? OW12 Ca2 H10A 85.5(8) . . ? OW8 Ca2 H10A 70.7(15) . . ? OW6 Ca2 H10A 135.8(14) . . ? O13 Ca2 H10A 93.3(12) . . ? OW9 Ca2 H10A 63.3(14) . . ? H6A Ca2 H10A 149.0(18) . . ? OW10 Ca2 H12A 114.6(15) . . ? OW11 Ca2 H12A 129.9(8) . . ? OW7 Ca2 H12A 67.0(11) . . ? OW12 Ca2 H12A 18.9(7) . . ? OW8 Ca2 H12A 60.0(13) . . ? OW6 Ca2 H12A 88.1(15) . . ? O13 Ca2 H12A 154.9(12) . . ? OW9 Ca2 H12A 90.6(7) . . ? H6A Ca2 H12A 98(2) . . ? H10A Ca2 H12A 95.7(17) . . ? OW10 Ca2 H12B 115.3(13) . . ? OW11 Ca2 H12B 156.5(13) . . ? OW7 Ca2 H12B 80.9(14) . . ? OW12 Ca2 H12B 16.5(9) . . ? OW8 Ca2 H12B 86.5(9) . . ? OW6 Ca2 H12B 67.9(10) . . ? O13 Ca2 H12B 127.1(10) . . ? OW9 Ca2 H12B 65.8(13) . . ? H6A Ca2 H12B 83.2(14) . . ? H10A Ca2 H12B 96.1(15) . . ? H12A Ca2 H12B 28.6(9) . . ? OW20 Ca3 OW13 141.7(2) . . ? OW20 Ca3 OW14 116.60(18) . . ? OW13 Ca3 OW14 82.30(16) . . ? OW20 Ca3 OW15 81.41(16) . 1_455 ? OW13 Ca3 OW15 103.48(16) . 1_455 ? OW14 Ca3 OW15 143.17(14) . 1_455 ? OW20 Ca3 OW16 75.4(2) . . ? OW13 Ca3 OW16 70.63(18) . . ? OW14 Ca3 OW16 141.85(15) . . ? OW15 Ca3 OW16 71.34(16) 1_455 . ? OW20 Ca3 OW17 76.53(16) . . ? OW13 Ca3 OW17 78.73(16) . . ? OW14 Ca3 OW17 72.19(13) . . ? OW15 Ca3 OW17 144.58(14) 1_455 . ? OW16 Ca3 OW17 76.44(16) . . ? OW20 Ca3 OW19 142.1(2) . . ? OW13 Ca3 OW19 73.98(19) . . ? OW14 Ca3 OW19 70.93(16) . . ? OW15 Ca3 OW19 75.80(17) 1_455 . ? OW16 Ca3 OW19 123.34(19) . . ? OW17 Ca3 OW19 136.35(17) . . ? OW20 Ca3 OW18 73.44(19) . . ? OW13 Ca3 OW18 144.89(18) . . ? OW14 Ca3 OW18 77.31(15) . . ? OW15 Ca3 OW18 78.01(16) 1_455 . ? OW16 Ca3 OW18 138.85(17) . . ? OW17 Ca3 OW18 120.46(16) . . ? OW19 Ca3 OW18 72.48(18) . . ? OW20 Ca3 H13B 127.4(10) . . ? OW13 Ca3 H13B 15.7(9) . . ? OW14 Ca3 H13B 84.0(17) . . ? OW15 Ca3 H13B 111.3(16) 1_455 . ? OW16 Ca3 H13B 62.8(16) . . ? OW17 Ca3 H13B 64.2(11) . . ? OW19 Ca3 H13B 89.4(9) . . ? OW18 Ca3 H13B 157.3(14) . . ? OW20 Ca3 H16A 61.5(19) . . ? OW13 Ca3 H16A 86.9(15) . . ? OW14 Ca3 H16A 155(2) . . ? OW15 Ca3 H16A 62(2) 1_455 . ? OW16 Ca3 H16A 16.8(14) . . ? OW17 Ca3 H16A 83(2) . . ? OW19 Ca3 H16A 128(3) . . ? OW18 Ca3 H16A 122.2(14) . . ? H13B Ca3 H16A 80(2) . . ? OW20 Ca3 H18A 90.2(11) . . ? OW13 Ca3 H18A 127.7(10) . . ? OW14 Ca3 H18A 76.6(19) . . ? OW15 Ca3 H18A 71.2(18) 1_455 . ? OW16 Ca3 H18A 141.4(19) . . ? OW17 Ca3 H18A 135.4(13) . . ? OW19 Ca3 H18A 54.0(9) . . ? OW18 Ca3 H18A 19.0(7) . . ? H13B Ca3 H18A 142.4(15) . . ? H16A Ca3 H18A 127(3) . . ? OW20 Ca3 H19A 152(2) . . ? OW13 Ca3 H19A 59.2(17) . . ? OW14 Ca3 H19A 78(2) . . ? OW15 Ca3 H19A 74(2) 1_455 . ? OW16 Ca3 H19A 108.0(14) . . ? OW17 Ca3 H19A 131(2) . . ? OW19 Ca3 H19A 16.8(13) . . ? OW18 Ca3 H19A 88.6(14) . . ? H13B Ca3 H19A 74.9(19) . . ? H16A Ca3 H19A 115(3) . . ? H18A Ca3 H19A 69.8(16) . . ? V1 O1 V1 101.58(12) . 2_565 ? V1 O1 V3 93.22(12) . 1_455 ? V1 O1 V3 93.21(11) 2_565 1_455 ? V1 O1 V2 93.09(11) . 2_666 ? V1 O1 V2 92.90(12) 2_565 2_666 ? V3 O1 V2 170.17(15) 1_455 2_666 ? V1 O1 V4 88.58(11) . . ? V1 O1 V4 169.84(15) 2_565 . ? V3 O1 V4 86.23(11) 1_455 . ? V2 O1 V4 86.41(10) 2_666 . ? V1 O1 V5 171.83(15) . 1_455 ? V1 O1 V5 86.59(11) 2_565 1_455 ? V3 O1 V5 86.02(10) 1_455 1_455 ? V2 O1 V5 86.66(11) 2_666 1_455 ? V4 O1 V5 83.26(10) . 1_455 ? V1 O2 V2 108.66(15) . 1_454 ? V1 O2 V3 107.12(14) . 1_455 ? V2 O2 V3 100.43(13) 1_454 1_455 ? V1 O3 V2 107.36(14) 1_556 2_667 ? V1 O3 V3 108.74(14) 1_556 2_666 ? V2 O3 V3 100.37(13) 2_667 2_666 ? V3 O4 V5 113.72(16) . . ? V1 O5 V5 111.26(16) 1_556 2_666 ? V2 O6 V5 114.28(17) . 2_766 ? V3 O7 V4 114.37(16) 1_455 . ? V2 O8 V4 113.86(16) . 2_666 ? V4 O9 V5 113.18(16) . 1_455 ? V1 O10 V4 108.32(16) . . ? V2 O12 Ca1 146.11(19) . 1_546 ? V4 O13 Ca2 150.3(2) . . ? V3 O14 Ca1 147.14(19) . 1_545 ? V6 O15 V6 101.74(13) . 2_566 ? V6 O15 V7 93.66(12) . 2_666 ? V6 O15 V7 93.17(12) 2_566 2_666 ? V6 O15 V8 93.75(13) . . ? V6 O15 V8 92.54(12) 2_566 . ? V7 O15 V8 169.54(16) 2_666 . ? V6 O15 V10 87.24(11) . . ? V6 O15 V10 171.02(17) 2_566 . ? V7 O15 V10 86.42(11) 2_666 . ? V8 O15 V10 86.57(11) . . ? V6 O15 V9 170.85(16) . 2_666 ? V6 O15 V9 87.40(12) 2_566 2_666 ? V7 O15 V9 85.34(11) 2_666 2_666 ? V8 O15 V9 86.17(11) . 2_666 ? V10 O15 V9 83.63(11) . 2_666 ? V6 O16 V7 107.91(16) . 1_455 ? V6 O16 V8 107.76(16) . . ? V7 O16 V8 99.87(15) 1_455 . ? V6 O17 V8 107.18(16) . 2_566 ? V6 O17 V7 107.18(15) . 2_666 ? V8 O17 V7 99.94(15) 2_566 2_666 ? V6 O18 V9 110.82(17) . 1_455 ? V6 O19 V10 109.73(17) . . ? V10 O20 V9 113.94(19) 2_666 . ? V8 O21 V9 115.21(18) . 2_666 ? V7 O22 V9 114.05(19) . . ? V8 O23 V10 114.87(18) . . ? V7 O24 V10 115.38(18) . 2_666 ? Ca1 OW1 H1A 141(4) 1_556 . ? Ca1 OW1 H1B 115(4) 1_556 . ? H1A OW1 H1B 104(4) . . ? Ca1 OW2 H2A 118(5) . . ? Ca1 OW2 H2B 113(5) . . ? H2A OW2 H2B 103(4) . . ? Ca1 OW3 H3A 83(5) . . ? Ca1 OW3 H3B 126(5) . . ? H3A OW3 H3B 100(4) . . ? Ca1 OW4 H4A 126(6) . . ? Ca1 OW4 H4B 124(6) . . ? H4A OW4 H4B 110(5) . . ? Ca1 OW5 H5A 130(5) 1_556 . ? Ca1 OW5 H5B 118(5) 1_556 . ? H5A OW5 H5B 112(5) . . ? Ca2 OW6 H6A 85(5) . . ? Ca2 OW6 H6B 119(5) . . ? H6A OW6 H6B 101(4) . . ? Ca2 OW7 H7A 119(4) . . ? Ca2 OW7 H7B 130(5) . . ? H7A OW7 H7B 104(4) . . ? Ca2 OW8 H8A 121(4) . . ? Ca2 OW8 H8B 134(5) . . ? H8A OW8 H8B 104(4) . . ? Ca2 OW9 H9A 115(5) . . ? Ca2 OW9 H9B 120(5) . . ? H9A OW9 H9B 105(4) . . ? Ca2 OW10 H10A 87(5) . . ? Ca2 OW10 H10B 117(6) . . ? H10A OW10 H10B 102(4) . . ? Ca2 OW11 H11A 131(4) . . ? Ca2 OW11 H11B 123(5) . . ? H11A OW11 H11B 103(4) . . ? Ca2 OW12 H12A 82(6) . . ? Ca2 OW12 H12B 100(6) . . ? H12A OW12 H12B 109(5) . . ? Ca3 OW13 H13A 135(5) . . ? Ca3 OW13 H13B 110(5) . . ? H13A OW13 H13B 114(5) . . ? Ca3 OW14 H14A 116(5) . . ? Ca3 OW14 H14B 113(5) . . ? H14A OW14 H14B 107(4) . . ? Ca3 OW15 H15A 113(5) 1_655 . ? Ca3 OW15 H15B 110(5) 1_655 . ? H15A OW15 H15B 109(4) . . ? Ca3 OW16 H16A 43(5) . . ? Ca3 OW16 H16B 145(5) . . ? H16A OW16 H16B 103(4) . . ? Ca3 OW17 H17A 114(5) . . ? Ca3 OW17 H17B 111(5) . . ? H17A OW17 H17B 107(4) . . ? Ca3 OW18 H18A 74(5) . . ? Ca3 OW18 H18B 146(6) . . ? H18A OW18 H18B 104(4) . . ? Ca3 OW19 H19A 48(6) . . ? Ca3 OW19 H19B 141(6) . . ? H19A OW19 H19B 106(5) . . ? Ca3 OW20 H20A 131(5) . . ? Ca3 OW20 H20B 115(5) . . ? H20A OW20 H20B 110(5) . . ? H21A OW21 H21B 104(4) . . ? H22A OW22 H22B 101(4) . . ? H23A OW23 H23B 98(4) . . ? H24A OW24 H24B 108(5) . . ? _refine_diff_density_max 2.375 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.162 _shelxl_version_number 2013-4 _shelx_res_file ; TITL TR-PR-01 numerical and empirial absorption corrections CELL 0.71075 10.08700 11.07080 21.81120 94.11240 96.05260 116.39800 ZERR 2 0.00019 0.00022 0.00153 0.00660 0.00680 0.00820 LATT 1 SFAC CA H O V UNIT 6 96 104 20 L.S. 12 omit -2 -2 2 omit 1 -4 3 omit 0 3 3 omit -1 -1 8 omit -1 -1 1 omit 2 -1 2 omit 0 -2 7 omit -4 7 6 omit 1 -1 6 omit 4 3 2 omit 0 -1 8 omit 6 0 4 omit 1 -3 4 omit -2 -6 5 omit 0 3 10 omit 4 -1 7 omit 1 1 13 omit -3 1 7 omit 3 -1 2 omit 6 -2 2 omit -2 3 5 DFIX 0.82 0.03 OW1 H1a OW1 H1b OW2 H2a OW2 H2b OW3 H3a OW3 H3b DFIX 0.82 0.03 OW4 H4a OW4 H4b OW5 H5a OW5 H5b OW6 H6a OW6 H6b DFIX 0.82 0.03 OW7 H7a OW7 H7b OW8 H8a OW8 H8b OW9 H9a OW9 H9b DFIX 0.82 0.03 OW10 H10a OW10 H10b OW11 H11a OW11 H11b DFIX 0.82 0.03 OW12 H12a OW12 H12b OW13 H13a OW13 H13b DFIX 0.82 0.03 OW14 H14a OW14 H14b OW15 H15a OW15 H15b DFIX 0.82 0.03 OW16 H16a OW16 H16b OW17 H17a OW17 H17b DFIX 0.82 0.03 OW18 H18a OW18 H18b OW19 H19a OW19 H19b DFIX 0.82 0.03 OW20 H20a OW20 H20b OW21 H21a OW21 H21b DFIX 0.82 0.03 OW22 H22a OW22 H22b OW23 H23a OW23 H23b DFIX 0.82 0.03 OW24 H24a OW24 H24b DFIX 1.30 0.03 H1a H1b H2a H2b H3a H3b H4a H4b H5a H5b DFIX 1.30 0.03 H6a H6b H7a H7b H8a H8b H9a H9b H10a H10b DFIX 1.30 0.03 H11a H11b H12a H12b H13a H13b H14a H14b H15a H15b DFIX 1.30 0.03 H16a H16b H17a H17b H18a H18b H19a H19b H20a H20b DFIX 1.30 0.03 H21a H21b H22a H22b H23a H23b H24a H24b FMAP 2 PLAN 50 HTAB BOND $H ACTA SIZE 0.130 0.090 0.030 WGHT 0.062600 12.199100 FVAR 0.34970 V1 4 0.163879 0.496315 0.001893 11.00000 0.01225 0.01385 = 0.01508 0.00212 0.00285 0.00552 V2 4 0.854982 0.240793 0.942749 11.00000 0.01744 0.01169 = 0.01592 0.00083 0.00224 0.00463 V3 4 0.927657 0.325028 0.085743 11.00000 0.01638 0.01280 = 0.01514 0.00246 0.00244 0.00485 V4 4 0.219727 0.581067 0.144788 11.00000 0.01630 0.01816 = 0.01631 0.00155 -0.00084 0.00547 V5 4 0.915306 0.586285 0.140782 11.00000 0.02105 0.01888 = 0.01643 0.00107 0.00626 0.00909 V6 4 0.100264 0.447185 0.461739 11.00000 0.01704 0.01994 = 0.01843 0.00302 0.00578 0.00896 V7 4 0.847360 0.246537 0.531962 11.00000 0.02327 0.02108 = 0.02369 0.00821 0.00651 0.00717 V8 4 0.133972 0.475232 0.609579 11.00000 0.02138 0.02440 = 0.01943 0.00534 0.00232 0.01121 V9 4 0.806032 0.222385 0.388155 11.00000 0.02179 0.02250 = 0.02451 -0.00135 0.00448 0.00752 V10 4 0.381438 0.675600 0.540333 11.00000 0.01703 0.03125 = 0.02547 0.00031 0.00421 0.00873 CA1 1 0.717717 0.929127 0.036222 11.00000 0.01890 0.01731 = 0.02465 0.00427 0.00450 0.00643 CA2 1 0.520330 0.724539 0.303011 11.00000 0.02369 0.02831 = 0.02371 0.00628 0.00554 0.01312 CA3 1 0.214193 0.110060 0.273344 11.00000 0.02228 0.02392 = 0.02503 0.00073 0.00224 0.01013 O1 3 0.032251 0.536829 0.062724 11.00000 0.01452 0.01366 = 0.01490 0.00275 0.00391 0.00506 O2 3 0.030172 0.314084 0.012148 11.00000 0.01360 0.01320 = 0.02004 0.00227 0.00318 0.00577 O3 3 0.212875 0.678899 0.988621 11.00000 0.01304 0.01451 = 0.01437 0.00188 0.00351 0.00421 O4 3 0.838700 0.394754 0.135978 11.00000 0.01727 0.01970 = 0.02057 0.00403 0.00627 0.00588 O5 3 0.231037 0.456589 0.938958 11.00000 0.01613 0.02119 = 0.02169 0.00364 0.00590 0.00875 O6 3 0.977105 0.241101 0.887891 11.00000 0.02406 0.01698 = 0.01727 0.00058 0.00396 0.00892 O7 3 0.103173 0.389604 0.136607 11.00000 0.01893 0.01597 = 0.01541 0.00259 0.00401 0.00778 O8 3 0.714734 0.249782 0.886501 11.00000 0.01603 0.01643 = 0.01896 0.00111 0.00060 0.00279 O9 3 0.093477 0.611450 0.189741 11.00000 0.02062 0.01940 = 0.01602 0.00216 0.00245 0.00809 O10 3 0.295713 0.530087 0.063784 11.00000 0.01485 0.02118 = 0.02461 0.00037 -0.00007 0.00773 O11 3 0.825746 0.624432 0.189807 11.00000 0.02922 0.03034 = 0.02319 -0.00110 0.00954 0.01271 O12 3 0.776403 0.083262 0.956431 11.00000 0.02547 0.01314 = 0.02518 0.00329 0.00347 0.00525 O13 3 0.360395 0.609539 0.196706 11.00000 0.02093 0.02930 = 0.02332 -0.00191 -0.00378 0.01153 O14 3 0.843725 0.163169 0.091187 11.00000 0.02284 0.01650 = 0.02395 0.00579 0.00591 0.00736 O15 3 0.125500 0.598676 0.533200 11.00000 0.01701 0.02092 = 0.02108 0.00410 0.00495 0.00850 O16 3 0.068143 0.343433 0.530449 11.00000 0.02197 0.02135 = 0.02547 0.00747 0.00592 0.01204 O17 3 0.083569 0.576905 0.411161 11.00000 0.02190 0.02523 = 0.01809 0.00447 0.00492 0.01129 O18 3 0.032798 0.312607 0.404692 11.00000 0.02616 0.02585 = 0.02127 0.00001 0.00657 0.01181 O19 3 0.289662 0.514305 0.471628 11.00000 0.01777 0.02989 = 0.02481 0.00209 0.00577 0.01155 O20 3 0.617814 0.200677 0.398285 11.00000 0.02208 0.03052 = 0.02711 -0.00176 0.00406 0.00869 O21 3 0.165609 0.629930 0.656321 11.00000 0.02470 0.03005 = 0.01980 0.00243 0.00452 0.01074 O22 3 0.820325 0.141138 0.458974 11.00000 0.02909 0.01977 = 0.03073 0.00409 0.00691 0.00930 O23 3 0.327096 0.541402 0.593888 11.00000 0.02222 0.03809 = 0.02298 0.00564 0.00399 0.01614 O24 3 0.659441 0.231469 0.521934 11.00000 0.02169 0.02870 = 0.02794 0.00661 0.00981 0.00713 O25 3 0.843525 0.148489 0.583550 11.00000 0.03889 0.02602 = 0.03129 0.01492 0.01187 0.01039 O26 3 0.775697 0.104959 0.332770 11.00000 0.03607 0.03466 = 0.03424 -0.00915 0.00614 0.01274 O27 3 0.555479 0.718297 0.539991 11.00000 0.02017 0.04985 = 0.04188 0.00198 0.00599 0.01227 O28 3 0.126744 0.374716 0.660958 11.00000 0.03595 0.04036 = 0.02681 0.01413 0.00434 0.02028 OW1 3 0.839217 0.852206 0.967592 11.00000 0.04567 0.04333 = 0.03761 0.01334 0.01639 0.03280 H1A 2 0.876242 0.869582 0.934873 11.00000 -1.20000 H1B 2 0.865765 0.798198 0.980556 11.00000 -1.20000 OW2 3 0.928319 0.952015 0.105713 11.00000 0.04913 0.03643 = 0.03684 -0.00866 -0.00892 0.03204 H2A 2 0.940780 0.883781 0.108861 11.00000 -1.20000 H2B 2 0.927696 0.978272 0.141958 11.00000 -1.20000 OW3 3 0.577510 0.928361 0.119932 11.00000 0.02467 0.03394 = 0.04000 0.00390 0.01375 0.00487 H3A 2 0.545096 0.969442 0.097322 11.00000 -1.20000 H3B 2 0.498341 0.865102 0.125181 11.00000 -1.20000 OW4 3 0.610799 0.697850 0.057297 11.00000 0.03146 0.02868 = 0.13522 0.03378 0.02967 0.01572 H4A 2 0.656059 0.656686 0.065481 11.00000 -1.20000 H4B 2 0.522740 0.651509 0.058816 11.00000 -1.20000 OW5 3 0.491770 0.841594 0.966987 11.00000 0.01936 0.08105 = 0.04610 0.03300 0.00013 0.00044 H5A 2 0.408233 0.793144 0.972173 11.00000 -1.20000 H5B 2 0.495426 0.859704 0.931943 11.00000 -1.20000 OW6 3 0.578537 0.536145 0.259199 11.00000 0.03065 0.03622 = 0.03510 0.01000 0.01305 0.01477 H6A 2 0.491201 0.482576 0.265984 11.00000 -1.20000 H6B 2 0.569405 0.518145 0.221742 11.00000 -1.20000 OW7 3 0.485118 0.567717 0.380176 11.00000 0.04187 0.04742 = 0.03358 0.01753 0.01743 0.03100 H7A 2 0.549292 0.541837 0.388298 11.00000 -1.20000 H7B 2 0.447626 0.562883 0.411850 11.00000 -1.20000 OW8 3 0.546105 0.868803 0.400630 11.00000 0.04256 0.03189 = 0.03819 0.00067 0.01950 0.00749 H8A 2 0.483465 0.841109 0.424127 11.00000 -1.20000 H8B 2 0.597323 0.949684 0.414221 11.00000 -1.20000 OW9 3 0.689908 0.818902 0.219658 11.00000 0.03777 0.03617 = 0.03404 0.00949 0.00896 0.01760 H9A 2 0.718172 0.766699 0.203390 11.00000 -1.20000 H9B 2 0.662159 0.848712 0.191031 11.00000 -1.20000 OW10 3 0.482185 0.907176 0.263932 11.00000 0.04730 0.04094 = 0.04213 0.01168 0.00985 0.02792 H10A 2 0.573484 0.959892 0.279178 11.00000 -1.20000 H10B 2 0.438056 0.937866 0.283846 11.00000 -1.20000 OW11 3 0.260277 0.650272 0.314139 11.00000 0.02663 0.06398 = 0.02393 0.00461 0.00689 0.01649 H11A 2 0.218374 0.645485 0.346002 11.00000 -1.20000 H11B 2 0.198439 0.644231 0.286790 11.00000 -1.20000 OW12 3 0.783402 0.831406 0.354140 11.00000 0.03234 0.04803 = 0.04475 -0.00163 0.00419 0.02008 H12A 2 0.744282 0.800059 0.383960 11.00000 -1.20000 H12B 2 0.810702 0.782043 0.338516 11.00000 -1.20000 OW13 3 0.276788 -0.009226 0.193834 11.00000 0.05275 0.04901 = 0.03693 -0.01342 0.00466 0.02512 H13A 2 0.250419 -0.087386 0.181418 11.00000 -1.20000 H13B 2 0.352384 0.042260 0.182648 11.00000 -1.20000 OW14 3 0.345758 0.020161 0.341684 11.00000 0.02545 0.02744 = 0.03330 0.00919 -0.00036 0.00548 H14A 2 0.295238 -0.036144 0.362094 11.00000 -1.20000 H14B 2 0.416453 0.079702 0.365701 11.00000 -1.20000 OW15 3 0.963543 0.076462 0.229931 11.00000 0.02361 0.03522 = 0.03913 0.00536 0.00457 0.01072 H15A 2 0.896502 0.015420 0.242863 11.00000 -1.20000 H15B 2 0.956832 0.145654 0.237585 11.00000 -1.20000 OW16 3 0.233100 0.222967 0.177361 11.00000 0.05998 0.06471 = 0.05043 0.03297 0.01914 0.04012 H16A 2 0.199142 0.224181 0.210620 11.00000 -1.20000 H16B 2 0.200991 0.265738 0.156547 11.00000 -1.20000 OW17 3 0.488625 0.260105 0.280103 11.00000 0.03040 0.02845 = 0.03475 0.00876 -0.00211 0.01017 H17A 2 0.536799 0.270575 0.314204 11.00000 -1.20000 H17B 2 0.504806 0.335116 0.271813 11.00000 -1.20000 OW18 3 0.089669 0.088021 0.368722 11.00000 0.06822 0.05591 = 0.03808 0.00531 0.01595 0.04073 H18A 2 0.045134 0.013198 0.347564 11.00000 -1.20000 H18B 2 0.090871 0.070881 0.405051 11.00000 -1.20000 OW19 3 0.048387 -0.138266 0.274701 11.00000 0.04919 0.03006 = 0.05760 0.00061 -0.00124 0.00082 H19A 2 0.087647 -0.096077 0.247750 11.00000 -1.20000 H19B 2 -0.032081 -0.200324 0.257690 11.00000 -1.20000 OW20 3 0.241775 0.329915 0.307923 11.00000 0.03921 0.03162 = 0.08588 -0.00905 0.00552 0.01500 H20A 2 0.316160 0.401363 0.321910 11.00000 -1.20000 H20B 2 0.175811 0.345582 0.293963 11.00000 -1.20000 OW21 3 0.981840 0.331887 0.252543 11.00000 0.05869 0.05543 = 0.03175 0.01870 0.02484 0.03436 H21A 2 0.996488 0.379478 0.224700 11.00000 -1.20000 H21B 2 0.939617 0.359133 0.275151 11.00000 -1.20000 OW22 3 0.479771 0.409341 0.127803 11.00000 0.07776 0.08949 = 0.06945 0.03205 0.02580 0.04510 H22A 2 0.450105 0.425710 0.093262 11.00000 -1.20000 H22B 2 0.510934 0.354553 0.116034 11.00000 -1.20000 OW23 3 0.598231 0.174894 0.169110 11.00000 0.05461 0.04525 = 0.07906 0.00032 0.03728 0.01270 H23A 2 0.656529 0.169734 0.199275 11.00000 -1.20000 H23B 2 0.537012 0.183133 0.189744 11.00000 -1.20000 OW24 3 0.164454 0.142382 0.512137 11.00000 0.16770 0.26635 = 0.10796 0.13293 0.09766 0.19022 H24A 2 0.192425 0.125902 0.480703 11.00000 -1.20000 H24B 2 0.084177 0.081235 0.513291 11.00000 -1.20000 HKLF 4 REM TR-PR-01 numerical and empirial absorption corrections REM R1 = 0.0488 for 8187 Fo > 4sig(Fo) and 0.0583 for all 9782 data REM 730 parameters refined using 72 restraints END WGHT 0.0626 12.2166 REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+2, -z+1 HTAB OW1 OW2_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB OW1 OW16_$2 HTAB OW1 O2_$2 EQIV $3 -x+2, -y+1, -z+1 HTAB OW2 O6_$3 EQIV $4 x, y+1, z HTAB OW2 OW15_$4 HTAB OW3 O8_$2 HTAB OW4 O5_$2 HTAB OW4 O10 HTAB OW5 O3 HTAB OW5 OW23_$2 HTAB OW6 OW22 HTAB OW7 O23_$2 HTAB OW7 O19 HTAB OW8 O24_$2 HTAB OW8 O22_$4 HTAB OW9 O11 HTAB OW9 OW3 HTAB OW10 OW14_$4 HTAB OW11 O17 HTAB OW11 O9 EQIV $5 -x+1, -y, -z+1 HTAB OW13 O6_$5 HTAB OW13 O8_$5 HTAB OW14 O25_$5 HTAB OW14 O20 EQIV $6 x, y-1, z HTAB OW15 OW9_$6 HTAB OW15 OW21 HTAB OW16 O7 HTAB OW17 O20 HTAB OW17 O23_$2 HTAB OW17 OW6 HTAB OW18 OW24 EQIV $7 x-1, y-1, z HTAB OW19 O11_$7 HTAB OW20 OW7 EQIV $8 x-1, y, z HTAB OW20 OW21_$8 HTAB OW21 O4 EQIV $9 x+1, y, z HTAB OW21 O7_$9 HTAB OW21 O9_$9 HTAB OW21 O21_$2 HTAB OW22 O10 HTAB OW23 OW13 HTAB OW23 OW17 HTAB OW24 O27_$2 HTAB OW24 OW18 REM Highest difference peak 2.375, deepest hole -1.095, 1-sigma level 0.162 Q1 1 0.2734 0.2714 0.5417 11.00000 0.05 2.37 Q2 1 0.0374 0.0500 0.4348 11.00000 0.05 1.91 Q3 1 0.7180 0.0603 0.4373 11.00000 0.05 1.88 Q4 1 -0.0527 0.2235 0.3502 11.00000 0.05 1.86 Q5 1 0.0242 0.3154 0.4900 11.00000 0.05 1.81 Q6 1 0.6574 0.9663 0.2965 11.00000 0.05 1.65 Q7 1 -0.0403 -0.0364 0.2961 11.00000 0.05 1.59 Q8 1 0.1041 0.1444 0.5763 11.00000 0.05 1.46 Q9 1 0.3937 0.5131 0.5229 11.00000 0.05 1.20 Q10 1 0.1658 0.6281 0.3954 11.00000 0.05 1.17 Q11 1 0.1667 0.4771 0.2666 11.00000 0.05 1.04 Q12 1 0.3081 0.5592 0.0333 11.00000 0.05 1.02 Q13 1 0.3893 0.6587 0.1781 11.00000 0.05 1.00 Q14 1 0.2178 0.5783 0.6358 11.00000 0.05 0.97 Q15 1 0.3927 0.3849 0.1269 11.00000 0.05 0.93 Q16 1 0.6930 0.7074 0.0180 11.00000 0.05 0.84 Q17 1 0.7168 0.3470 0.2217 11.00000 0.05 0.84 Q18 1 0.5742 1.0001 0.3975 11.00000 0.05 0.82 Q19 1 0.7995 0.1697 0.3075 11.00000 0.05 0.79 Q20 1 0.3588 0.5976 0.3500 11.00000 0.05 0.79 Q21 1 0.9583 0.3023 0.5388 11.00000 0.05 0.79 Q22 1 0.7084 0.0680 0.1672 11.00000 0.05 0.79 Q23 1 0.9642 0.8248 0.1679 11.00000 0.05 0.77 Q24 1 0.4380 0.2816 0.2158 11.00000 0.05 0.73 Q25 1 0.6643 0.8753 0.4535 11.00000 0.05 0.70 Q26 1 0.0137 0.2921 -0.0124 11.00000 0.05 0.68 Q27 1 0.5846 0.7903 0.3248 11.00000 0.05 0.68 Q28 1 0.1091 0.4147 0.6412 11.00000 0.05 0.66 Q29 1 0.1027 0.2372 0.4200 11.00000 0.05 0.66 Q30 1 0.8422 0.2499 0.4392 11.00000 0.05 0.66 Q31 1 0.3243 0.2734 0.1590 11.00000 0.05 0.65 Q32 1 0.6809 0.1617 0.3449 11.00000 0.05 0.63 Q33 1 0.7925 -0.0655 0.2456 11.00000 0.05 0.62 Q34 1 0.4112 0.0870 0.1669 11.00000 0.05 0.60 Q35 1 0.4741 0.1734 0.3133 11.00000 0.05 0.60 Q36 1 0.5810 1.0014 0.1435 11.00000 0.05 0.59 Q37 1 0.3478 0.2918 0.2592 11.00000 0.05 0.59 Q38 1 0.6539 0.6390 0.3917 11.00000 0.05 0.53 Q39 1 0.9090 0.2061 0.5720 11.00000 0.05 0.53 Q40 1 0.9018 0.2416 0.8912 11.00000 0.05 0.53 Q41 1 0.2044 0.4840 0.4694 11.00000 0.05 0.53 Q42 1 1.0358 0.3983 0.3397 11.00000 0.05 0.52 Q43 1 0.2636 0.2785 0.4653 11.00000 0.05 0.51 Q44 1 0.4656 0.7992 0.1615 11.00000 0.05 0.51 Q45 1 0.2159 0.5837 0.1112 11.00000 0.05 0.51 Q46 1 -0.0582 0.2676 0.4070 11.00000 0.05 0.49 Q47 1 0.2809 -0.1549 0.3673 11.00000 0.05 0.49 Q48 1 0.6605 0.6977 0.2406 11.00000 0.05 0.48 Q49 1 0.3866 0.8573 0.2568 11.00000 0.05 0.48 Q50 1 0.8304 0.1961 0.9675 11.00000 0.05 0.48 ; _shelx_res_checksum 77319 _shelx_hkl_file ; 0 1 2 136.72 3.64 1 -1 2 3666.81 90.35 -1 1 -2 3498.06 87.34 1 -1 2 3645.17 90.83 -1 1 -2 3698.06 91.48 -1 0 -2 236.54 4.48 1 0 2 250.67 4.54 1 0 2 241.78 4.53 -1 0 -2 240.13 4.66 -1 0 -2 241.04 4.49 1 0 2 235.96 3.99 0 -1 3 1313.33 28.26 0 -1 3 1560.69 25.62 0 1 -3 1348.12 28.88 1 0 -3 2668.25 62.19 1 0 -3 2560.59 63.57 1 0 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337.16 12.23 4 4 -2 325.37 13.73 -4 -4 2 307.30 12.95 -3 -5 1 384.69 15.75 3 5 -1 389.58 20.82 -3 -5 1 365.36 18.63 3 5 -1 396.04 14.87 -4 -1 13 236.00 10.71 4 1 -13 241.06 10.69 4 1 -13 252.37 11.35 4 1 -13 234.62 10.40 -4 -1 13 250.15 11.12 -1 -6 -4 95.37 6.96 1 6 4 79.27 11.77 1 6 4 95.53 7.62 -1 -6 -4 54.68 10.96 -1 6 -11 74.05 5.67 1 -6 11 61.70 2.44 1 -6 11 60.39 6.75 1 -6 11 72.33 5.72 2 0 14 96.82 5.09 2 0 14 100.21 7.02 2 0 14 100.69 5.66 -2 0 -14 97.45 7.10 -2 0 -14 90.98 9.83 0 -4 14 270.48 17.39 0 4 -14 266.23 16.79 0 -4 14 253.18 12.13 -3 -4 10 1737.75 51.57 3 4 -10 1716.23 53.54 -3 -4 10 1746.89 68.80 -3 -4 10 1756.15 57.94 3 4 -10 1709.18 57.68 3 4 -10 1791.64 67.57 -7 2 5 143.60 11.39 -7 2 5 158.96 9.00 7 -2 -5 131.16 8.70 -7 2 5 139.63 4.65 7 -2 -5 133.13 7.88 4 4 -4 841.61 30.38 -4 -4 4 872.56 34.66 4 4 -4 916.77 31.53 -4 -4 4 841.84 30.87 -7 2 -1 429.24 8.52 -7 2 -1 422.95 17.06 -7 2 -1 434.38 17.06 7 -2 1 443.03 17.56 7 -2 1 412.31 21.53 -7 2 -1 432.08 8.72 -4 1 14 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598.67 21.64 3 -1 -15 563.64 17.06 3 -8 0 750.81 23.32 3 -8 0 793.38 32.45 3 5 -5 1630.35 56.94 3 5 -5 1590.02 54.59 -3 -5 5 1649.17 53.52 -3 -5 5 1570.53 62.67 2 -2 -15 9.22 6.27 2 -2 -15 10.14 3.03 -2 2 15 8.03 2.61 -2 2 15 10.52 6.07 -7 4 -3 735.16 25.41 7 -4 3 707.59 28.51 7 -4 3 713.16 31.61 -7 4 -3 686.60 31.51 -3 -5 0 792.12 32.47 -3 -5 0 712.68 24.10 3 5 0 724.10 26.56 3 5 0 729.62 24.21 -6 1 -6 86.07 6.73 -6 1 -6 71.68 9.36 -6 1 -6 72.54 3.60 6 -1 6 71.78 6.12 6 -1 6 63.89 6.66 -3 0 15 1407.57 48.64 -3 0 15 1345.04 44.02 3 0 -15 1360.38 38.90 3 0 -15 1372.97 47.75 -1 7 -8 365.87 10.89 1 -7 8 386.58 13.86 1 -7 8 369.58 15.51 1 -7 8 368.24 10.50 -6 5 -7 7208.66 266.32 6 -5 7 7105.66 266.37 6 -5 7 7241.04 321.59 6 -5 7 7292.04 307.01 4 -4 12 41.63 3.29 -4 4 -12 42.76 5.85 4 -4 12 55.63 5.88 4 -4 12 41.95 3.89 7 -5 2 451.28 17.44 7 -5 2 456.42 20.59 -4 2 14 1009.53 34.36 -4 2 14 1069.65 29.95 4 -2 -14 1027.34 34.63 -1 3 -15 3.43 3.68 1 -3 15 10.12 3.71 -4 6 -10 304.75 10.27 4 -6 10 338.84 10.86 4 -6 10 312.66 7.83 5 0 -12 474.86 19.60 5 0 -12 460.97 20.32 5 0 -12 499.60 17.10 -5 0 12 490.89 20.82 -5 0 12 486.34 17.47 -1 3 14 60.47 2.18 -1 3 14 69.12 6.44 -1 3 14 59.06 2.22 1 -3 -14 77.32 5.40 1 -3 -14 73.33 6.66 4 -8 1 496.97 22.50 4 -8 1 491.15 14.78 4 -8 1 500.28 14.41 4 4 -5 676.77 24.36 -4 -4 5 658.87 23.06 -4 -4 5 681.12 22.62 4 4 -5 638.75 23.02 -4 -4 5 640.66 23.98 6 -7 -2 184.09 7.68 6 -7 -2 200.12 6.44 3 -8 3 1390.20 42.05 3 -8 3 1369.66 44.83 4 2 -12 903.71 26.73 4 2 -12 921.23 30.92 4 2 -12 908.79 29.98 -4 -2 12 877.83 29.40 -4 -2 12 870.35 30.90 -4 -2 12 873.94 25.51 3 -6 11 98.36 4.10 3 -6 11 104.93 2.81 5 -7 6 158.20 8.80 5 -7 6 165.13 7.61 -7 4 6 71.64 3.57 -7 4 6 60.50 5.16 7 -4 -6 67.02 3.53 7 -4 -6 73.03 6.72 7 -4 -6 70.65 7.27 2 -5 13 606.19 20.33 -2 5 -13 587.43 20.44 4 -8 0 17.30 6.06 4 -8 0 13.57 2.56 -2 4 -14 449.10 16.55 2 -4 14 454.04 16.50 -7 3 -3 28.46 1.22 -7 3 -3 28.30 1.04 -7 3 -3 30.99 7.41 -7 3 -3 39.84 5.17 7 -3 3 29.35 5.29 7 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21.57 3 -8 -1 660.42 29.41 0 -7 -2 956.54 35.08 0 -7 -2 950.21 30.09 0 -7 -2 1266.48 39.49 0 7 2 961.09 36.67 -1 2 15 150.33 6.32 1 -2 -15 155.35 7.24 1 -2 -15 171.76 13.37 -1 2 15 156.61 13.75 -1 2 15 159.98 6.43 2 2 -15 854.55 29.69 2 2 -15 780.89 20.50 -2 -2 15 857.71 30.00 -2 -2 15 829.14 33.23 -2 -5 10 1012.82 37.59 -2 -5 10 999.00 28.01 2 5 -10 1085.85 41.87 -2 -5 10 1069.30 34.80 2 5 -10 1023.23 30.52 2 6 -2 316.98 13.86 -2 -6 2 314.76 16.88 -2 -6 2 312.79 16.80 2 6 -2 297.12 12.82 2 6 -3 1078.93 37.21 2 6 -3 1083.67 36.80 -2 -6 3 1092.60 35.99 -2 -6 3 1054.67 36.03 -2 -6 3 1063.80 35.06 4 0 -14 22.98 3.20 4 0 -14 24.62 4.32 -4 0 14 27.63 4.48 4 0 -14 18.01 3.66 -4 0 14 21.78 3.78 4 2 8 1694.37 57.94 -4 -2 -8 1673.68 53.60 -4 -2 -8 1684.76 57.98 4 2 8 1639.75 57.60 -4 -2 -8 1690.40 58.66 4 2 8 1676.27 55.23 5 2 4 354.75 14.49 5 2 4 367.57 15.85 -5 -2 -4 371.77 14.58 -5 -2 -4 381.46 12.76 -5 -2 -4 378.22 15.87 -5 -1 11 92.96 9.51 -5 -1 11 111.97 6.18 5 1 -11 97.85 9.46 5 1 -11 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132.17 15.02 7 -10 -11 58.56 11.16 7 -10 -11 58.52 7.38 -2 -5 -17 376.21 22.48 -2 -5 -17 366.65 29.84 2 5 17 386.63 21.97 2 5 17 325.91 14.30 2 5 17 379.27 22.62 8 -11 -5 77.18 6.38 8 -11 -5 73.36 6.26 8 -11 -5 79.67 12.32 -10 3 12 72.53 9.80 10 -3 -12 77.49 16.67 10 -3 -12 69.99 5.72 -10 3 12 72.33 6.51 10 -3 -12 82.61 9.23 5 -3 20 432.35 16.81 5 -3 20 486.19 32.61 5 -3 20 508.03 29.52 -5 3 -20 520.37 23.29 -5 3 -20 424.78 17.07 -10 2 11 129.37 17.56 -10 2 11 100.90 10.98 10 -2 -11 88.75 12.54 10 -2 -11 105.73 11.39 -3 5 21 33.10 9.12 3 -5 -21 36.95 7.56 3 -5 -21 31.92 8.79 8 -8 13 -3.62 6.09 -8 8 -13 -1.44 3.47 8 -8 13 -1.23 2.18 8 -8 13 -3.91 4.53 7 5 -4 157.17 15.49 -7 -5 4 179.52 15.17 -7 -5 4 149.23 22.48 7 5 -4 174.51 15.63 6 -12 -1 1.58 5.48 6 -12 -1 -7.11 5.16 6 -12 -1 4.11 5.38 -3 -9 4 23.55 11.14 -3 -9 4 28.68 7.56 3 9 -4 24.68 8.07 3 9 -4 14.74 8.33 -1 4 -23 140.14 14.25 1 -4 23 143.47 13.19 1 -4 23 141.12 14.23 -4 -8 8 141.50 21.02 4 8 -8 141.50 13.65 4 8 -8 136.38 14.45 -4 -8 8 148.45 11.48 0 7 16 126.26 13.30 0 7 16 120.27 13.87 0 -7 -16 105.38 13.72 0 -7 -16 133.42 13.54 7 -2 -20 176.65 13.33 7 -2 -20 164.27 12.20 -7 2 20 166.72 11.30 -7 2 20 166.25 19.84 -2 -9 -5 103.29 8.92 2 9 5 109.66 10.57 -2 -9 -5 114.31 13.89 2 9 5 139.99 20.83 -11 5 5 42.78 9.04 11 -5 -5 38.80 12.97 11 -5 -5 54.86 15.31 3 9 -3 24.25 7.51 -3 -9 3 12.91 7.19 -3 -9 3 16.16 7.12 3 9 -3 26.98 7.98 4 -12 5 65.99 9.08 4 -12 5 67.89 12.27 -10 1 9 55.78 10.58 10 -1 -9 62.80 10.87 -10 1 9 63.34 10.73 -10 1 9 67.20 6.22 10 -1 -9 57.31 10.36 -5 -7 -1 211.75 17.28 -5 -7 -1 173.41 14.60 5 7 1 216.70 15.45 5 7 1 195.95 18.49 4 -12 -1 27.45 5.34 4 -12 -1 28.98 8.27 7 -2 16 1.06 3.68 7 -2 16 2.81 5.83 -7 2 -16 14.14 7.24 7 -2 16 4.12 4.09 -7 2 -16 1.72 3.83 -7 -5 5 585.00 29.72 -7 -5 5 567.88 31.40 7 5 -5 601.97 31.94 7 5 -5 541.40 30.87 -4 5 21 18.83 7.84 4 -5 -21 26.37 7.75 4 -5 -21 21.68 7.07 5 -12 -2 22.71 4.91 5 -12 -2 25.69 12.58 6 0 -21 86.15 10.02 -6 0 21 76.38 8.92 -6 0 21 78.32 10.49 6 0 -21 55.32 7.24 -7 -5 3 330.38 21.58 7 5 -3 330.00 22.51 -7 -5 3 315.47 28.99 7 5 -3 322.28 30.26 6 3 12 29.35 7.94 -6 -3 -12 27.66 7.79 6 3 12 28.37 6.85 -6 -3 -12 8.90 9.37 -6 -3 -12 11.33 6.06 -5 -6 14 21.72 7.69 5 6 -14 17.49 9.98 5 6 -14 25.03 8.91 -5 -6 14 38.83 8.54 -5 -6 14 19.80 5.28 1 3 21 0.65 2.48 -1 -3 -21 1.54 4.29 -1 -3 -21 6.60 5.73 1 3 21 6.88 5.72 11 -6 0 26.56 8.12 11 -6 0 36.24 7.91 -11 6 0 24.01 8.61 9 -10 6 2.36 10.20 9 -10 6 9.58 5.12 7 -7 16 308.34 14.58 7 -7 16 273.15 14.40 -7 7 -16 318.06 14.55 7 -7 16 369.66 23.53 5 -3 -22 135.21 15.88 -5 3 22 132.02 12.61 5 -3 -22 150.96 12.85 -5 3 22 94.39 9.41 5 -3 -22 134.42 10.12 -11 5 0 66.50 11.51 11 -5 0 76.69 10.93 11 -5 0 64.64 16.68 3 9 -5 13.44 7.39 -3 -9 5 17.47 6.32 -3 -9 5 17.22 10.58 3 9 -5 10.02 7.22 8 0 11 20.75 12.60 -8 0 -11 21.20 7.78 8 0 11 19.49 7.57 -8 0 -11 35.48 8.30 -8 0 -11 29.25 12.12 9 -2 10 1083.97 50.65 -9 2 -10 1023.60 48.32 -9 2 -10 891.32 31.73 -9 2 -10 958.00 46.39 9 -2 10 1020.56 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