data_Molybdomenite-M2 _audit_creation_method 'SHELXL-2019/2' _shelx_SHELXL_version_number '2019/2' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'O3 Pb Se' _chemical_formula_weight 334.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.160(4) _cell_length_b 8.074(4) _cell_length_c 8.763(4) _cell_angle_alpha 90 _cell_angle_beta 103.17(3) _cell_angle_gamma 90 _cell_volume 631.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 672 _cell_measurement_theta_min 6.83 _cell_measurement_theta_max 50.09 _exptl_crystal_description elongated _exptl_crystal_colour yellowish _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 7.034 _exptl_crystal_F_000 1120 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 64.791 _shelx_estimated_absorpt_T_min 0.112 _shelx_estimated_absorpt_T_max 0.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1 _exptl_absorpt_correction_T_max 0.3 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type Bruker-APEX2 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 1690 _diffrn_reflns_av_unetI/netI 0.1345 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.404 _diffrn_reflns_theta_max 28.256 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_point_group_measured_fraction_full 0.985 _reflns_number_total 1690 _reflns_number_gt 953 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 3-component twin. ; _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^)+(0.0648P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1690 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1338 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1597 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _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 Pb1 Pb 0.60362(12) 0.17570(15) 0.72648(13) 0.0276(3) Uani 1 1 d . . . . . Pb2 Pb 0.00440(12) 0.16536(14) 0.17288(12) 0.0256(3) Uani 1 1 d . . . . . Se1 Se 0.7966(3) 0.0079(3) 0.4486(3) 0.0216(6) Uani 1 1 d . . . . . Se2 Se 0.6817(3) 0.9000(3) 0.0527(3) 0.0224(6) Uani 1 1 d . . . . . O1 O 0.868(2) 0.180(2) 0.371(2) 0.025(4) Uani 1 1 d . . . . . O2 O 0.616(2) 0.054(3) 0.401(2) 0.031(5) Uani 1 1 d . . . . . O3 O 0.845(2) 0.058(3) 0.645(2) 0.026(4) Uani 1 1 d . . . . . O4 O 0.655(2) 0.851(3) 0.862(3) 0.042(6) Uani 1 1 d . . . . . O5 O 0.670(3) 0.111(2) 0.042(3) 0.040(5) Uani 1 1 d . . . . . O6 O 0.864(2) 0.873(3) 0.120(2) 0.037(5) Uani 1 1 d . . . . . 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 Pb1 0.0331(6) 0.0277(6) 0.0242(6) 0.0009(5) 0.0109(5) -0.0012(5) Pb2 0.0379(7) 0.0233(6) 0.0182(6) 0.0009(5) 0.0121(5) 0.0002(5) Se1 0.0287(14) 0.0199(13) 0.0167(13) 0.0004(12) 0.0061(10) -0.0011(11) Se2 0.0303(15) 0.0186(13) 0.0187(14) 0.0014(12) 0.0062(11) 0.0005(11) O1 0.041(11) 0.020(10) 0.024(10) -0.005(9) 0.027(9) -0.012(8) O2 0.024(11) 0.028(11) 0.039(13) 0.003(9) 0.006(9) -0.009(8) O3 0.031(11) 0.038(12) 0.012(10) -0.002(9) 0.009(8) -0.008(9) O4 0.034(12) 0.056(16) 0.031(13) -0.018(11) -0.003(10) 0.017(10) O5 0.069(16) 0.014(10) 0.040(14) -0.006(10) 0.021(12) 0.000(10) O6 0.048(13) 0.044(14) 0.023(12) -0.005(10) 0.015(10) -0.007(10) _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 Pb1 O5 2.53(2) 4_566 ? Pb1 O3 2.648(19) . ? Pb1 O2 2.66(2) 4_566 ? Pb1 O4 2.72(2) 2_646 ? Pb1 O1 2.73(2) 4_566 ? Pb1 O5 2.74(2) 1_556 ? Pb1 O2 2.775(19) 3_656 ? Pb1 O4 2.87(2) 1_545 ? Pb1 O2 3.04(2) . ? Pb2 O1 2.364(17) 1_455 ? Pb2 O6 2.56(2) 2_645 ? Pb2 O3 2.59(2) 3_656 ? Pb2 O3 2.652(19) 4_465 ? Pb2 O6 2.68(2) 1_445 ? Pb2 O1 2.930(19) 4_465 ? Pb2 O5 3.05(2) 1_455 ? Pb2 O6 3.09(2) 3_665 ? Pb2 O4 3.21(2) 3_666 ? Se1 O2 1.653(19) . ? Se1 O3 1.721(18) . ? Se1 O1 1.740(17) . ? Se2 O6 1.65(2) . ? Se2 O4 1.68(2) 1_554 ? Se2 O5 1.71(2) 1_565 ? 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 O5 Pb1 O3 74.6(6) 4_566 . ? O5 Pb1 O2 79.8(7) 4_566 4_566 ? O3 Pb1 O2 121.5(6) . 4_566 ? O5 Pb1 O4 77.5(7) 4_566 2_646 ? O3 Pb1 O4 146.8(6) . 2_646 ? O2 Pb1 O4 69.8(6) 4_566 2_646 ? O5 Pb1 O1 71.9(6) 4_566 4_566 ? O3 Pb1 O1 64.7(5) . 4_566 ? O2 Pb1 O1 57.6(5) 4_566 4_566 ? O4 Pb1 O1 122.4(6) 2_646 4_566 ? O5 Pb1 O5 138.1(7) 4_566 1_556 ? O3 Pb1 O5 101.4(6) . 1_556 ? O2 Pb1 O5 66.8(6) 4_566 1_556 ? O4 Pb1 O5 111.4(7) 2_646 1_556 ? O1 Pb1 O5 69.0(6) 4_566 1_556 ? O5 Pb1 O2 117.0(7) 4_566 3_656 ? O3 Pb1 O2 102.9(6) . 3_656 ? O2 Pb1 O2 135.5(2) 4_566 3_656 ? O4 Pb1 O2 74.2(6) 2_646 3_656 ? O1 Pb1 O2 163.3(6) 4_566 3_656 ? O5 Pb1 O2 104.7(6) 1_556 3_656 ? O5 Pb1 O4 147.7(7) 4_566 1_545 ? O3 Pb1 O4 73.5(6) . 1_545 ? O2 Pb1 O4 122.1(6) 4_566 1_545 ? O4 Pb1 O4 130.1(5) 2_646 1_545 ? O1 Pb1 O4 98.8(6) 4_566 1_545 ? O5 Pb1 O4 55.3(6) 1_556 1_545 ? O2 Pb1 O4 66.0(6) 3_656 1_545 ? O5 Pb1 O2 63.7(6) 4_566 . ? O3 Pb1 O2 54.4(5) . . ? O2 Pb1 O2 143.2(5) 4_566 . ? O4 Pb1 O2 96.8(6) 2_646 . ? O1 Pb1 O2 110.8(5) 4_566 . ? O5 Pb1 O2 146.6(6) 1_556 . ? O2 Pb1 O2 65.4(6) 3_656 . ? O4 Pb1 O2 93.0(6) 1_545 . ? O1 Pb2 O6 71.8(7) 1_455 2_645 ? O1 Pb2 O3 83.0(6) 1_455 3_656 ? O6 Pb2 O3 85.4(6) 2_645 3_656 ? O1 Pb2 O3 69.7(6) 1_455 4_465 ? O6 Pb2 O3 71.1(6) 2_645 4_465 ? O3 Pb2 O3 148.2(3) 3_656 4_465 ? O1 Pb2 O6 81.8(6) 1_455 1_445 ? O6 Pb2 O6 146.1(4) 2_645 1_445 ? O3 Pb2 O6 70.3(6) 3_656 1_445 ? O3 Pb2 O6 119.5(6) 4_465 1_445 ? O1 Pb2 O1 117.0(7) 1_455 4_465 ? O6 Pb2 O1 113.3(6) 2_645 4_465 ? O3 Pb2 O1 155.5(5) 3_656 4_465 ? O3 Pb2 O1 56.3(5) 4_465 4_465 ? O6 Pb2 O1 97.4(6) 1_445 4_465 ? O1 Pb2 O5 68.4(6) 1_455 1_455 ? O6 Pb2 O5 129.3(6) 2_645 1_455 ? O3 Pb2 O5 118.8(6) 3_656 1_455 ? O3 Pb2 O5 66.5(6) 4_465 1_455 ? O6 Pb2 O5 53.4(6) 1_445 1_455 ? O1 Pb2 O5 62.4(6) 4_465 1_455 ? O1 Pb2 O6 171.1(6) 1_455 3_665 ? O6 Pb2 O6 116.3(7) 2_645 3_665 ? O3 Pb2 O6 100.8(6) 3_656 3_665 ? O3 Pb2 O6 108.6(6) 4_465 3_665 ? O6 Pb2 O6 91.8(6) 1_445 3_665 ? O1 Pb2 O6 57.4(5) 4_465 3_665 ? O5 Pb2 O6 102.8(6) 1_455 3_665 ? O1 Pb2 O4 139.5(6) 1_455 3_666 ? O6 Pb2 O4 77.4(6) 2_645 3_666 ? O3 Pb2 O4 68.6(6) 3_656 3_666 ? O3 Pb2 O4 123.7(6) 4_465 3_666 ? O6 Pb2 O4 112.9(6) 1_445 3_666 ? O1 Pb2 O4 99.0(5) 4_465 3_666 ? O5 Pb2 O4 151.0(5) 1_455 3_666 ? O6 Pb2 O4 49.0(6) 3_665 3_666 ? O2 Se1 O3 102.2(10) . . ? O2 Se1 O1 99.7(10) . . ? O3 Se1 O1 99.6(9) . . ? O2 Se1 Pb1 48.5(7) . 4_565 ? O3 Se1 Pb1 111.8(7) . 4_565 ? O1 Se1 Pb1 51.5(7) . 4_565 ? O2 Se1 Pb2 110.5(7) . 4_666 ? O3 Se1 Pb2 45.1(6) . 4_666 ? O1 Se1 Pb2 54.7(7) . 4_666 ? Pb1 Se1 Pb2 84.47(7) 4_565 4_666 ? O2 Se1 Pb1 57.7(7) . . ? O3 Se1 Pb1 44.5(6) . . ? O1 Se1 Pb1 104.4(6) . . ? Pb1 Se1 Pb1 80.47(7) 4_565 . ? Pb2 Se1 Pb1 68.29(6) 4_666 . ? O2 Se1 Pb2 129.9(7) . 2_645 ? O3 Se1 Pb2 116.3(7) . 2_645 ? O1 Se1 Pb2 103.8(6) . 2_645 ? Pb1 Se1 Pb2 129.13(9) 4_565 2_645 ? Pb2 Se1 Pb2 119.19(8) 4_666 2_645 ? Pb1 Se1 Pb2 148.38(9) . 2_645 ? O2 Se1 Pb2 113.7(7) . 1_655 ? O3 Se1 Pb2 121.9(6) . 1_655 ? O1 Se1 Pb2 32.8(6) . 1_655 ? Pb1 Se1 Pb2 69.12(6) 4_565 1_655 ? Pb2 Se1 Pb2 79.22(6) 4_666 1_655 ? Pb1 Se1 Pb2 137.24(9) . 1_655 ? Pb2 Se1 Pb2 72.25(6) 2_645 1_655 ? O2 Se1 Pb2 124.9(7) . 3_656 ? O3 Se1 Pb2 39.4(7) . 3_656 ? O1 Se1 Pb2 120.1(7) . 3_656 ? Pb1 Se1 Pb2 151.22(9) 4_565 3_656 ? Pb2 Se1 Pb2 72.06(6) 4_666 3_656 ? Pb1 Se1 Pb2 75.57(7) . 3_656 ? Pb2 Se1 Pb2 78.14(6) 2_645 3_656 ? Pb2 Se1 Pb2 120.42(8) 1_655 3_656 ? O2 Se1 Pb1 36.3(7) . 3_656 ? O3 Se1 Pb1 118.8(6) . 3_656 ? O1 Se1 Pb1 123.4(7) . 3_656 ? Pb1 Se1 Pb1 75.29(6) 4_565 3_656 ? Pb2 Se1 Pb1 145.80(8) 4_666 3_656 ? Pb1 Se1 Pb1 81.21(7) . 3_656 ? Pb2 Se1 Pb1 94.87(7) 2_645 3_656 ? Pb2 Se1 Pb1 117.17(8) 1_655 3_656 ? Pb2 Se1 Pb1 115.81(8) 3_656 3_656 ? O6 Se2 O4 103.4(10) . 1_554 ? O6 Se2 O5 101.3(11) . 1_565 ? O4 Se2 O5 100.7(11) 1_554 1_565 ? O6 Se2 Pb1 111.7(7) . 1_564 ? O4 Se2 Pb1 52.5(8) 1_554 1_564 ? O5 Se2 Pb1 48.2(7) 1_565 1_564 ? O6 Se2 Pb2 43.9(8) . 1_665 ? O4 Se2 Pb2 110.7(8) 1_554 1_665 ? O5 Se2 Pb2 57.4(8) 1_565 1_665 ? Pb1 Se2 Pb2 82.22(7) 1_564 1_665 ? O6 Se2 Pb1 133.6(8) . 2_655 ? O4 Se2 Pb1 45.0(8) 1_554 2_655 ? O5 Se2 Pb1 115.7(8) 1_565 2_655 ? Pb1 Se2 Pb1 77.82(6) 1_564 2_655 ? Pb2 Se2 Pb1 155.36(9) 1_665 2_655 ? O6 Se2 Pb1 125.2(7) . 3_666 ? O4 Se2 Pb1 122.0(8) 1_554 3_666 ? O5 Se2 Pb1 98.9(8) 1_565 3_666 ? Pb1 Se2 Pb1 119.60(8) 1_564 3_666 ? Pb2 Se2 Pb1 125.74(8) 1_665 3_666 ? Pb1 Se2 Pb1 77.33(6) 2_655 3_666 ? O6 Se2 Pb2 32.2(7) . 2_655 ? O4 Se2 Pb2 115.4(7) 1_554 2_655 ? O5 Se2 Pb2 124.1(8) 1_565 2_655 ? Pb1 Se2 Pb2 143.33(9) 1_564 2_655 ? Pb2 Se2 Pb2 70.15(6) 1_665 2_655 ? Pb1 Se2 Pb2 120.11(8) 2_655 2_655 ? Pb1 Se2 Pb2 96.38(8) 3_666 2_655 ? O6 Se2 Pb2 50.1(7) . 3_665 ? O4 Se2 Pb2 54.4(7) 1_554 3_665 ? O5 Se2 Pb2 98.7(7) 1_565 3_665 ? Pb1 Se2 Pb2 73.31(6) 1_564 3_665 ? Pb2 Se2 Pb2 64.94(6) 1_665 3_665 ? Pb1 Se2 Pb2 95.29(7) 2_655 3_665 ? Pb1 Se2 Pb2 162.45(8) 3_666 3_665 ? Pb2 Se2 Pb2 73.34(6) 2_655 3_665 ? O6 Se2 Pb1 103.7(8) . 4_575 ? O4 Se2 Pb1 126.8(8) 1_554 4_575 ? O5 Se2 Pb1 29.2(7) 1_565 4_575 ? Pb1 Se2 Pb1 75.06(6) 1_564 4_575 ? Pb2 Se2 Pb1 64.74(6) 1_665 4_575 ? Pb1 Se2 Pb1 122.41(8) 2_655 4_575 ? Pb1 Se2 Pb1 73.79(6) 3_666 4_575 ? Pb2 Se2 Pb1 111.82(8) 2_655 4_575 ? Pb2 Se2 Pb1 122.98(7) 3_665 4_575 ? Se1 O1 Pb2 123.6(9) . 1_655 ? Se1 O1 Pb1 98.5(8) . 4_565 ? Pb2 O1 Pb1 104.0(7) 1_655 4_565 ? Se1 O1 Pb2 96.3(8) . 4_666 ? Pb2 O1 Pb2 119.8(7) 1_655 4_666 ? Pb1 O1 Pb2 112.9(6) 4_565 4_666 ? Se1 O2 Pb1 103.7(8) . 4_565 ? Se1 O2 Pb1 123.0(10) . 3_656 ? Pb1 O2 Pb1 112.6(7) 4_565 3_656 ? Se1 O2 Pb1 95.0(8) . . ? Pb1 O2 Pb1 105.5(7) 4_565 . ? Pb1 O2 Pb1 114.6(6) 3_656 . ? Se1 O3 Pb2 115.6(10) . 3_656 ? Se1 O3 Pb1 108.4(8) . . ? Pb2 O3 Pb1 116.3(7) 3_656 . ? Se1 O3 Pb2 107.5(8) . 4_666 ? Pb2 O3 Pb2 108.8(6) 3_656 4_666 ? Pb1 O3 Pb2 98.5(7) . 4_666 ? Se2 O4 Pb1 109.0(11) 1_556 2_656 ? Se2 O4 Pb1 99.7(9) 1_556 1_565 ? Pb1 O4 Pb1 107.9(7) 2_656 1_565 ? Se2 O4 Pb2 100.3(8) 1_556 3_666 ? Pb1 O4 Pb2 139.1(8) 2_656 3_666 ? Pb1 O4 Pb2 94.0(7) 1_565 3_666 ? Se2 O5 Pb1 131.6(11) 1_545 4_565 ? Se2 O5 Pb1 104.1(9) 1_545 1_554 ? Pb1 O5 Pb1 118.9(8) 4_565 1_554 ? Se2 O5 Pb2 94.5(9) 1_545 1_655 ? Pb1 O5 Pb2 91.6(6) 4_565 1_655 ? Pb1 O5 Pb2 109.0(7) 1_554 1_655 ? Se2 O6 Pb2 127.8(11) . 2_655 ? Se2 O6 Pb2 110.8(10) . 1_665 ? Pb2 O6 Pb2 108.9(8) 2_655 1_665 ? Se2 O6 Pb2 105.7(9) . 3_665 ? Pb2 O6 Pb2 108.1(7) 2_655 3_665 ? Pb2 O6 Pb2 88.2(6) 1_665 3_665 ? _refine_diff_density_max 3.219 _refine_diff_density_min -2.970 _refine_diff_density_rms 0.756 _shelx_res_file ; TITL twin5 in P2(1)/c twin5.res created by SHELXL-2019/2 at 02:02:05 on 06-May-2023 CELL 0.71073 9.1597 8.0741 8.7631 90.000 103.169 90.000 ZERR 8.000 0.0039 0.0035 0.0038 0.000 0.031 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC O SE PB UNIT 24 8 8 L.S. 10 BOND FMAP 2 PLAN 20 CONN 9 2.4 PB1 CONN 9 2.4 PB2 ACTA SIZE 0.06 0.04 0.03 OMIT 1 0 0 OMIT 6 4 4 OMIT 1 2 9 OMIT -8 1 1 WGHT 0.064800 BASF 0.14790 0.08705 FVAR 0.18055 PB1 3 0.603618 0.175703 0.726479 11.00000 0.03307 0.02770 = 0.02415 0.00087 0.01092 -0.00120 PB2 3 0.004403 0.165363 0.172881 11.00000 0.03789 0.02327 = 0.01823 0.00091 0.01207 0.00020 SE1 2 0.796623 0.007862 0.448572 11.00000 0.02872 0.01987 = 0.01670 0.00043 0.00611 -0.00108 SE2 2 0.681705 0.899971 0.052706 11.00000 0.03030 0.01857 = 0.01870 0.00141 0.00623 0.00050 O1 1 0.868208 0.180351 0.371405 11.00000 0.04120 0.01972 = 0.02435 -0.00469 0.02716 -0.01161 O2 1 0.616029 0.053502 0.401347 11.00000 0.02395 0.02837 = 0.03934 0.00346 0.00630 -0.00866 O3 1 0.844571 0.057810 0.644563 11.00000 0.03118 0.03791 = 0.01223 -0.00223 0.00891 -0.00789 O4 1 0.654965 0.851012 0.861733 11.00000 0.03374 0.05591 = 0.03070 -0.01759 -0.00347 0.01660 O5 1 0.670066 0.110706 0.041734 11.00000 0.06906 0.01376 = 0.03996 -0.00554 0.02130 0.00026 O6 1 0.863555 0.873356 0.120006 11.00000 0.04821 0.04383 = 0.02327 -0.00461 0.01502 -0.00675 HKLF 5 REM twin5 in P2(1)/c REM wR2 = 0.1597, GooF = S = 1.005, Restrained GooF = 1.005 for all data REM R1 = 0.0635 for 953 Fo > 4sig(Fo) and 0.1338 for all 1690 data REM 93 parameters refined using 0 restraints END WGHT 0.0648 0.0000 REM Highest difference peak 3.219, deepest hole -2.970, 1-sigma level 0.756 Q1 1 0.5534 0.2539 0.6803 11.00000 0.05 3.22 Q2 1 0.0838 0.2260 0.1850 11.00000 0.05 3.16 Q3 1 0.0442 0.0605 0.2416 11.00000 0.05 3.10 Q4 1 -0.0396 0.0852 0.1294 11.00000 0.05 2.89 Q5 1 -0.0451 0.2471 0.1128 11.00000 0.05 2.67 Q6 1 0.5595 0.0988 0.6688 11.00000 0.05 2.66 Q7 1 0.8667 0.1261 0.4318 11.00000 0.05 2.55 Q8 1 0.7223 0.1516 0.7498 11.00000 0.05 2.42 Q9 1 0.7371 0.1139 0.4955 11.00000 0.05 2.30 Q10 1 0.6702 0.2416 0.7535 11.00000 0.05 2.30 Q11 1 0.7677 0.8286 0.9609 11.00000 0.05 2.29 Q12 1 0.9321 0.1763 0.2889 11.00000 0.05 2.29 Q13 1 -0.0644 0.0507 -0.0059 11.00000 0.05 2.29 Q14 1 0.1719 0.1720 0.1587 11.00000 0.05 2.27 Q15 1 0.5642 0.8903 0.0328 11.00000 0.05 2.25 Q16 1 0.5887 0.8997 0.8743 11.00000 0.05 2.19 Q17 1 -0.0913 0.2012 0.1393 11.00000 0.05 2.17 Q18 1 0.5067 0.7716 0.0842 11.00000 0.05 2.16 Q19 1 0.0881 0.1831 0.2992 11.00000 0.05 2.16 Q20 1 0.8241 0.0046 0.7147 11.00000 0.05 2.13 ; _shelx_res_checksum 41279 _shelx_hkl_file ; 1 0 0 -3.7978 1.93072 1 2 0 0 497.912 31.8947 1 3 0 0 2937.58 183.336 1 4 0 0 49.1136 8.14219 1 5 0 0 3276.44 205.248 1 6 0 0 380.994 23.1874 1 7 0 0 320.413 36.1366 1 8 1 0 235.799 34.8605 -3 8 0 0 235.799 34.8605 1 9 1 0 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