data_bur _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common 'chiyokoite' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C1.08 H32.56 Al0.36 As0.28 B0.64 Ca3 O24.64 Si0.64' _chemical_formula_weight 615.86 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' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' _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, x, z+1/2' 'y, -x+y, z+1/2' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' _cell_length_a 11.0119(5) _cell_length_b 11.0119(5) _cell_length_c 10.5252(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1105.31(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7416 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 31.75 _exptl_crystal_description 'prismatic crystal' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_F_000 644 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.005 _exptl_crystal_size_min 0.005 _exptl_absorpt_coefficient_mu 1.319 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'STOE StadiVari' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11111 _diffrn_reflns_av_unetI/netI 0.0912 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.136 _diffrn_reflns_theta_max 28.269 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.948 _diffrn_reflns_point_group_measured_fraction_full 0.951 _reflns_number_total 1747 _reflns_number_gt 1093 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.807 _reflns_Friedel_fraction_max 0.893 _reflns_Friedel_fraction_full 0.901 _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. 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-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion 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^)+(0.0386P)^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_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.6(2) _chemical_absolute_configuration ? _refine_ls_number_reflns 1747 _refine_ls_number_parameters 110 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.960 _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 Ca Ca 0.19968(10) 0.00008(10) 0.2521(6) 0.0140(2) Uani 1 1 d . . . . . Si Si 0.000000 0.000000 0.0002(12) 0.0087(4) Uani 0.64 3 d S T P . . Al Al 0.000000 0.000000 0.0002(12) 0.0087(4) Uani 0.36 3 d S T P . . B B 0.333333 0.666667 0.0035(10) 0.0118(15) Uani 0.64 3 d S T P . . As1 As 0.333333 0.666667 0.0035(10) 0.0118(15) Uani 0.18 3 d S T P . . C1 C 0.333333 0.666667 0.0035(10) 0.0118(15) Uani 0.18 3 d S T P . . C2 C 0.333333 0.666667 0.5049(19) 0.023(3) Uani 0.9 3 d S T P . . As2 As 0.333333 0.666667 0.5049(19) 0.023(3) Uani 0.1 3 d DS T P . . O1 O 0.4067(5) 0.2556(5) 0.2455(14) 0.0306(12) Uani 1 1 d . . . . . O2 O 0.2558(5) 0.4070(4) 0.2567(14) 0.0321(13) Uani 1 1 d . . . . . O3 O 0.0027(11) 0.3435(11) 0.0806(11) 0.035(3) Uani 1 1 d . . . . . O4 O 0.9974(9) 0.3389(10) 0.4311(9) 0.024(2) Uani 1 1 d . . . . . O5 O 0.1311(10) 0.1295(10) 0.1082(7) 0.014(2) Uani 1 1 d . . . . . O6 O 0.9980(7) 0.1314(12) 0.8969(7) 0.016(2) Uani 1 1 d . . . . . OB1A O 0.8130(11) 0.4309(13) 0.4561(16) 0.027(3) Uani 0.5 1 d . . P . . OB1B O 0.666667 0.333333 0.646(2) 0.006(4) Uiso 0.32 3 d S . P . . OB2A O 0.8067(15) 0.3797(17) 0.547(2) 0.035(4) Uani 0.5 1 d . . P . . OB2B O 0.666667 0.333333 0.358(2) 0.007(4) Uani 0.32 3 d S T P . . OC O 0.4679(6) 0.7338(7) 0.5026(12) 0.0397(15) Uani 0.9 1 d . . P . . OAS O 0.439(5) 0.839(3) 0.451(5) 0.004(11) Uiso 0.1 1 d D . P . . 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 Ca 0.0136(5) 0.0179(5) 0.0118(4) 0.0005(16) 0.0007(15) 0.0089(4) Si 0.0102(6) 0.0102(6) 0.0055(11) 0.000 0.000 0.0051(3) Al 0.0102(6) 0.0102(6) 0.0055(11) 0.000 0.000 0.0051(3) B 0.012(2) 0.012(2) 0.011(3) 0.000 0.000 0.0060(12) As1 0.012(2) 0.012(2) 0.011(3) 0.000 0.000 0.0060(12) C1 0.012(2) 0.012(2) 0.011(3) 0.000 0.000 0.0060(12) C2 0.016(4) 0.016(4) 0.038(6) 0.000 0.000 0.0079(19) As2 0.016(4) 0.016(4) 0.038(6) 0.000 0.000 0.0079(19) O1 0.024(2) 0.030(2) 0.033(3) -0.007(5) -0.004(5) 0.0102(17) O2 0.029(2) 0.025(2) 0.040(3) 0.015(6) 0.008(6) 0.0118(18) O3 0.034(6) 0.034(6) 0.040(7) 0.010(5) -0.009(5) 0.020(5) O4 0.017(4) 0.019(4) 0.028(5) -0.013(4) -0.007(4) 0.003(3) O5 0.006(4) 0.014(4) 0.017(5) 0.010(3) 0.004(3) 0.001(4) O6 0.013(5) 0.024(5) 0.013(4) 0.005(4) -0.006(3) 0.010(4) OB1A 0.022(6) 0.023(5) 0.035(8) -0.005(6) -0.003(5) 0.010(4) OB2A 0.020(6) 0.035(8) 0.037(9) -0.005(7) -0.007(6) 0.005(6) OB2B 0.008(6) 0.008(6) 0.004(10) 0.000 0.000 0.004(3) OC 0.024(3) 0.038(4) 0.051(4) -0.008(3) -0.001(3) 0.012(3) _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 Ca O3 2.393(12) 5 ? Ca O4 2.438(11) 5_665 ? Ca O5 2.444(8) . ? Ca O6 2.450(8) 6_654 ? Ca O5 2.469(8) 5 ? Ca O6 2.479(9) 3_564 ? Ca O1 2.589(5) . ? Ca O2 2.593(5) 5 ? Ca Si 3.413(10) 2 ? Ca Si 3.445(10) . ? Ca Ca 3.8078(16) 5 ? Si O6 1.819(13) 4_544 ? Si O6 1.819(13) 5_664 ? Si O6 1.819(13) 1_454 ? Si O5 1.831(13) 5 ? Si O5 1.831(13) 4 ? Si O5 1.831(13) . ? B OB2A 1.437(16) 6_664 ? B OB2A 1.437(16) 2_554 ? B OB2A 1.437(16) 3_564 ? B OB1B 1.50(2) 2_554 ? B OB1A 1.506(13) 2_554 ? B OB1A 1.506(13) 6_664 ? B OB1A 1.506(13) 3_564 ? B OB2B 1.53(2) 2_554 ? B O2 3.683(14) 5_565 ? B O2 3.683(14) 4_665 ? B O2 3.683(14) . ? B O3 3.691(11) 5_565 ? B O3 3.691(11) . ? B O3 3.691(11) 4_665 ? B O4 3.691(10) 6_664 ? B O4 3.691(10) 2_554 ? C2 OC 1.283(6) . ? C2 OC 1.283(6) 4_665 ? C2 OC 1.283(6) 5_565 ? C2 OAS 1.751(14) . ? C2 OAS 1.751(14) 4_665 ? C2 OAS 1.751(14) 5_565 ? C2 O1 3.591(19) 3_565 ? C2 O1 3.591(19) 6_665 ? C2 O1 3.591(19) 2 ? C2 O2 3.65(2) . ? C2 O2 3.65(2) 5_565 ? C2 O2 3.65(2) 4_665 ? C2 OB2B 3.72(3) 2 ? C2 O3 3.731(11) 3 ? C2 O3 3.732(11) 2_665 ? C2 O3 3.732(11) 6_565 ? O1 OC 2.881(16) 6_664 ? O1 OC 4.071(12) 2_654 ? O2 OC 2.908(16) 5_565 ? O2 OC 4.086(13) . ? O3 OC 2.764(12) 3_454 ? O3 OC 3.918(12) 2_554 ? O4 OC 2.747(10) 5_665 ? O4 OC 3.923(11) 4_765 ? O5 OC 4.044(11) 6_664 ? O6 OC 4.025(12) 3 ? OB1A OB2A 1.099(17) . ? OB1A OB2B 1.754(18) . ? OB1B OB2A 1.71(2) . ? OB1B OB2A 1.71(2) 5_665 ? OB1B OB2A 1.71(2) 4_655 ? OB1B OC 3.97(2) 3 ? OB1B OC 3.97(2) 2_655 ? OB1B OC 3.97(2) 6_665 ? OB2B OC 3.96(2) 3_554 ? OB2B OC 3.96(2) 6_664 ? OB2B OC 3.96(2) 2_654 ? OC OAS 1.45(4) . ? OC OAS 1.75(4) 5_565 ? OC OC 2.223(10) 5_565 ? OC OC 2.223(10) 4_665 ? OC OAS 2.983(19) 4_665 ? 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 O3 Ca O4 99.61(19) 5 5_665 ? O3 Ca O5 86.1(4) 5 . ? O4 Ca O5 148.8(3) 5_665 . ? O3 Ca O6 148.5(4) 5 6_654 ? O4 Ca O6 84.3(3) 5_665 6_654 ? O5 Ca O6 106.73(19) . 6_654 ? O3 Ca O5 85.9(4) 5 5 ? O4 Ca O5 149.7(3) 5_665 5 ? O5 Ca O5 60.8(5) . 5 ? O6 Ca O5 76.31(12) 6_654 5 ? O3 Ca O6 149.6(4) 5 3_564 ? O4 Ca O6 84.3(3) 5_665 3_564 ? O5 Ca O6 76.23(13) . 3_564 ? O6 Ca O6 61.6(5) 6_654 3_564 ? O5 Ca O6 105.91(18) 5 3_564 ? O3 Ca O1 76.6(4) 5 . ? O4 Ca O1 78.3(3) 5_665 . ? O5 Ca O1 73.2(3) . . ? O6 Ca O1 134.3(4) 6_654 . ? O5 Ca O1 131.7(4) 5 . ? O6 Ca O1 74.7(3) 3_564 . ? O3 Ca O2 77.4(3) 5 5 ? O4 Ca O2 77.3(3) 5_665 5 ? O5 Ca O2 133.6(4) . 5 ? O6 Ca O2 73.0(3) 6_654 5 ? O5 Ca O2 74.8(3) 5 5 ? O6 Ca O2 132.4(4) 3_564 5 ? O1 Ca O2 140.56(14) . 5 ? O3 Ca Si 178.9(3) 5 2 ? O4 Ca Si 79.5(3) 5_665 2 ? O5 Ca Si 95.0(2) . 2 ? O6 Ca Si 30.9(3) 6_654 2 ? O5 Ca Si 94.6(2) 5 2 ? O6 Ca Si 31.1(3) 3_564 2 ? O1 Ca Si 103.8(3) . 2 ? O2 Ca Si 101.7(3) 5 2 ? O3 Ca Si 80.7(4) 5 . ? O4 Ca Si 179.4(2) 5_665 . ? O5 Ca Si 30.6(2) . . ? O6 Ca Si 95.7(2) 6_654 . ? O5 Ca Si 30.8(2) 5 . ? O6 Ca Si 95.2(2) 3_564 . ? O1 Ca Si 101.2(3) . . ? O2 Ca Si 103.3(3) 5 . ? Si Ca Si 100.24(2) 2 . ? O3 Ca Ca 124.2(3) 5 5 ? O4 Ca Ca 123.7(2) 5_665 5 ? O5 Ca Ca 74.5(2) . 5 ? O6 Ca Ca 39.7(2) 6_654 5 ? O5 Ca Ca 38.9(2) 5 5 ? O6 Ca Ca 74.8(3) 3_564 5 ? O1 Ca Ca 139.70(11) . 5 ? O2 Ca Ca 79.73(10) 5 5 ? Si Ca Ca 56.09(11) 2 5 ? Si Ca Ca 56.45(11) . 5 ? O6 Si O6 87.9(6) 4_544 5_664 ? O6 Si O6 87.9(6) 4_544 1_454 ? O6 Si O6 87.9(6) 5_664 1_454 ? O6 Si O5 92.5(3) 4_544 5 ? O6 Si O5 94.0(3) 5_664 5 ? O6 Si O5 178.0(8) 1_454 5 ? O6 Si O5 94.0(3) 4_544 4 ? O6 Si O5 178.0(8) 5_664 4 ? O6 Si O5 92.5(3) 1_454 4 ? O5 Si O5 85.5(6) 5 4 ? O6 Si O5 178.0(7) 4_544 . ? O6 Si O5 92.5(3) 5_664 . ? O6 Si O5 94.0(3) 1_454 . ? O5 Si O5 85.5(6) 5 . ? O5 Si O5 85.5(6) 4 . ? O6 Si Ca 44.8(3) 4_544 6_554 ? O6 Si Ca 93.4(5) 5_664 6_554 ? O6 Si Ca 43.8(3) 1_454 6_554 ? O5 Si Ca 136.3(3) 5 6_554 ? O5 Si Ca 88.3(3) 4 6_554 ? O5 Si Ca 137.1(3) . 6_554 ? O6 Si Ca 93.4(5) 4_544 2_554 ? O6 Si Ca 43.8(3) 5_664 2_554 ? O6 Si Ca 44.8(3) 1_454 2_554 ? O5 Si Ca 137.1(3) 5 2_554 ? O5 Si Ca 136.3(3) 4 2_554 ? O5 Si Ca 88.3(3) . 2_554 ? Ca Si Ca 67.8(2) 6_554 2_554 ? O6 Si Ca 43.8(3) 4_544 3_554 ? O6 Si Ca 44.8(3) 5_664 3_554 ? O6 Si Ca 93.4(5) 1_454 3_554 ? O5 Si Ca 88.3(3) 5 3_554 ? O5 Si Ca 137.1(3) 4 3_554 ? O5 Si Ca 136.3(3) . 3_554 ? Ca Si Ca 67.8(2) 6_554 3_554 ? Ca Si Ca 67.8(2) 2_554 3_554 ? O6 Si Ca 87.1(4) 4_544 5 ? O6 Si Ca 136.2(3) 5_664 5 ? O6 Si Ca 135.3(3) 1_454 5 ? O5 Si Ca 42.9(3) 5 5 ? O5 Si Ca 43.7(3) 4 5 ? O5 Si Ca 91.3(5) . 5 ? Ca Si Ca 112.541(19) 6_554 5 ? Ca Si Ca 179.6(3) 2_554 5 ? Ca Si Ca 112.541(19) 3_554 5 ? O6 Si Ca 135.3(3) 4_544 . ? O6 Si Ca 87.1(4) 5_664 . ? O6 Si Ca 136.2(3) 1_454 . ? O5 Si Ca 43.7(3) 5 . ? O5 Si Ca 91.3(5) 4 . ? O5 Si Ca 42.9(3) . . ? Ca Si Ca 179.6(3) 6_554 . ? Ca Si Ca 112.541(19) 2_554 . ? Ca Si Ca 112.540(19) 3_554 . ? Ca Si Ca 67.1(2) 5 . ? O6 Si Ca 136.2(3) 4_544 4 ? O6 Si Ca 135.3(3) 5_664 4 ? O6 Si Ca 87.1(4) 1_454 4 ? O5 Si Ca 91.3(5) 5 4 ? O5 Si Ca 42.9(3) 4 4 ? O5 Si Ca 43.7(3) . 4 ? Ca Si Ca 112.541(19) 6_554 4 ? Ca Si Ca 112.541(19) 2_554 4 ? Ca Si Ca 179.6(3) 3_554 4 ? Ca Si Ca 67.1(2) 5 4 ? Ca Si Ca 67.1(2) . 4 ? OB2A B OB2A 110.2(9) 6_664 2_554 ? OB2A B OB2A 110.2(9) 6_664 3_564 ? OB2A B OB2A 110.2(9) 2_554 3_564 ? OB2A B OB1B 71.2(9) 6_664 2_554 ? OB2A B OB1B 71.2(9) 2_554 2_554 ? OB2A B OB1B 71.2(9) 3_564 2_554 ? OB2A B OB1A 103.4(7) 6_664 2_554 ? OB2A B OB1A 43.8(7) 2_554 2_554 ? OB2A B OB1A 144.1(7) 3_564 2_554 ? OB1B B OB1A 109.3(8) 2_554 2_554 ? OB2A B OB1A 43.8(7) 6_664 6_664 ? OB2A B OB1A 144.1(7) 2_554 6_664 ? OB2A B OB1A 103.4(7) 3_564 6_664 ? OB1B B OB1A 109.3(8) 2_554 6_664 ? OB1A B OB1A 109.6(8) 2_554 6_664 ? OB2A B OB1A 144.1(7) 6_664 3_564 ? OB2A B OB1A 103.4(7) 2_554 3_564 ? OB2A B OB1A 43.8(7) 3_564 3_564 ? OB1B B OB1A 109.3(8) 2_554 3_564 ? OB1A B OB1A 109.6(8) 2_554 3_564 ? OB1A B OB1A 109.6(8) 6_664 3_564 ? OB2A B OB2B 108.8(9) 6_664 2_554 ? OB2A B OB2B 108.8(9) 2_554 2_554 ? OB2A B OB2B 108.8(9) 3_564 2_554 ? OB1B B OB2B 180.0 2_554 2_554 ? OB1A B OB2B 70.7(8) 2_554 2_554 ? OB1A B OB2B 70.7(8) 6_664 2_554 ? OB1A B OB2B 70.6(8) 3_564 2_554 ? OB2A B O2 40.3(8) 6_664 5_565 ? OB2A B O2 72.6(8) 2_554 5_565 ? OB2A B O2 111.3(10) 3_564 5_565 ? OB1B B O2 43.6(2) 2_554 5_565 ? OB1A B O2 86.3(6) 2_554 5_565 ? OB1A B O2 83.8(7) 6_664 5_565 ? OB1A B O2 152.9(9) 3_564 5_565 ? OB2B B O2 136.4(2) 2_554 5_565 ? OB2A B O2 111.3(10) 6_664 4_665 ? OB2A B O2 40.3(8) 2_554 4_665 ? OB2A B O2 72.6(8) 3_564 4_665 ? OB1B B O2 43.6(2) 2_554 4_665 ? OB1A B O2 83.8(7) 2_554 4_665 ? OB1A B O2 152.9(9) 6_664 4_665 ? OB1A B O2 86.3(6) 3_564 4_665 ? OB2B B O2 136.4(2) 2_554 4_665 ? O2 B O2 73.4(4) 5_565 4_665 ? OB2A B O2 72.6(8) 6_664 . ? OB2A B O2 111.3(10) 2_554 . ? OB2A B O2 40.3(8) 3_564 . ? OB1B B O2 43.6(2) 2_554 . ? OB1A B O2 152.9(9) 2_554 . ? OB1A B O2 86.3(6) 6_664 . ? OB1A B O2 83.8(7) 3_564 . ? OB2B B O2 136.4(2) 2_554 . ? O2 B O2 73.4(4) 5_565 . ? O2 B O2 73.4(3) 4_665 . ? OB2A B O3 76.7(7) 6_664 5_565 ? OB2A B O3 38.8(7) 2_554 5_565 ? OB2A B O3 142.8(10) 3_564 5_565 ? OB1B B O3 77.3(3) 2_554 5_565 ? OB1A B O3 36.6(6) 2_554 5_565 ? OB1A B O3 105.3(5) 6_664 5_565 ? OB1A B O3 139.2(5) 3_564 5_565 ? OB2B B O3 102.7(3) 2_554 5_565 ? O2 B O3 50.1(2) 5_565 5_565 ? O2 B O3 71.1(3) 4_665 5_565 ? O2 B O3 119.3(4) . 5_565 ? OB2A B O3 38.8(7) 6_664 . ? OB2A B O3 142.8(10) 2_554 . ? OB2A B O3 76.7(7) 3_564 . ? OB1B B O3 77.3(3) 2_554 . ? OB1A B O3 139.2(5) 2_554 . ? OB1A B O3 36.6(6) 6_664 . ? OB1A B O3 105.3(5) 3_564 . ? OB2B B O3 102.7(3) 2_554 . ? O2 B O3 71.1(3) 5_565 . ? O2 B O3 119.3(4) 4_665 . ? O2 B O3 50.1(2) . . ? O3 B O3 115.3(2) 5_565 . ? OB2A B O3 142.8(10) 6_664 4_665 ? OB2A B O3 76.7(7) 2_554 4_665 ? OB2A B O3 38.8(7) 3_564 4_665 ? OB1B B O3 77.3(3) 2_554 4_665 ? OB1A B O3 105.3(5) 2_554 4_665 ? OB1A B O3 139.2(5) 6_664 4_665 ? OB1A B O3 36.6(6) 3_564 4_665 ? OB2B B O3 102.7(3) 2_554 4_665 ? O2 B O3 119.3(4) 5_565 4_665 ? O2 B O3 50.1(2) 4_665 4_665 ? O2 B O3 71.1(3) . 4_665 ? O3 B O3 115.3(2) 5_565 4_665 ? O3 B O3 115.3(2) . 4_665 ? OB2A B O4 35.5(8) 6_664 6_664 ? OB2A B O4 104.9(7) 2_554 6_664 ? OB2A B O4 139.1(7) 3_564 6_664 ? OB1B B O4 101.9(3) 2_554 6_664 ? OB1A B O4 76.7(5) 2_554 6_664 ? OB1A B O4 39.2(5) 6_664 6_664 ? OB1A B O4 143.1(8) 3_564 6_664 ? OB2B B O4 78.1(3) 2_554 6_664 ? O2 B O4 60.4(2) 5_565 6_664 ? O2 B O4 130.5(3) 4_665 6_664 ? O2 B O4 107.0(2) . 6_664 ? O3 B O4 66.22(14) 5_565 6_664 ? O3 B O4 62.61(15) . 6_664 ? O3 B O4 177.9(2) 4_665 6_664 ? OB2A B O4 139.1(7) 6_664 2_554 ? OB2A B O4 35.5(8) 2_554 2_554 ? OB2A B O4 104.9(7) 3_564 2_554 ? OB1B B O4 101.9(3) 2_554 2_554 ? OB1A B O4 39.2(5) 2_554 2_554 ? OB1A B O4 143.1(8) 6_664 2_554 ? OB1A B O4 76.7(5) 3_564 2_554 ? OB2B B O4 78.1(3) 2_554 2_554 ? O2 B O4 107.0(2) 5_565 2_554 ? O2 B O4 60.4(2) 4_665 2_554 ? O2 B O4 130.5(3) . 2_554 ? O3 B O4 62.61(15) 5_565 2_554 ? O3 B O4 177.9(2) . 2_554 ? O3 B O4 66.22(14) 4_665 2_554 ? O4 B O4 115.85(17) 6_664 2_554 ? OC C2 OC 119.97(8) . 4_665 ? OC C2 OC 119.96(8) . 5_565 ? OC C2 OC 119.96(8) 4_665 5_565 ? OC C2 OAS 54.6(18) . . ? OC C2 OAS 68.3(18) 4_665 . ? OC C2 OAS 159(3) 5_565 . ? OC C2 OAS 159(3) . 4_665 ? OC C2 OAS 54.6(18) 4_665 4_665 ? OC C2 OAS 68.3(18) 5_565 4_665 ? OAS C2 OAS 110(2) . 4_665 ? OC C2 OAS 68.3(18) . 5_565 ? OC C2 OAS 159(3) 4_665 5_565 ? OC C2 OAS 54.6(18) 5_565 5_565 ? OAS C2 OAS 110(2) . 5_565 ? OAS C2 OAS 110(2) 4_665 5_565 ? OC C2 O1 102.7(9) . 3_565 ? OC C2 O1 47.4(9) 4_665 3_565 ? OC C2 O1 119.8(11) 5_565 3_565 ? OAS C2 O1 80.8(19) . 3_565 ? OAS C2 O1 87.3(19) 4_665 3_565 ? OAS C2 O1 154(2) 5_565 3_565 ? OC C2 O1 47.4(9) . 6_665 ? OC C2 O1 119.8(11) 4_665 6_665 ? OC C2 O1 102.7(9) 5_565 6_665 ? OAS C2 O1 87.3(19) . 6_665 ? OAS C2 O1 154(2) 4_665 6_665 ? OAS C2 O1 80.8(19) 5_565 6_665 ? O1 C2 O1 75.7(5) 3_565 6_665 ? OC C2 O1 119.8(11) . 2 ? OC C2 O1 102.7(9) 4_665 2 ? OC C2 O1 47.4(9) 5_565 2 ? OAS C2 O1 154(2) . 2 ? OAS C2 O1 80.8(19) 4_665 2 ? OAS C2 O1 87.3(19) 5_565 2 ? O1 C2 O1 75.7(5) 3_565 2 ? O1 C2 O1 75.7(5) 6_665 2 ? OC C2 O2 100.9(9) . . ? OC C2 O2 117.6(11) 4_665 . ? OC C2 O2 46.2(9) 5_565 . ? OAS C2 O2 113(2) . . ? OAS C2 O2 70.0(19) 4_665 . ? OAS C2 O2 42.1(19) 5_565 . ? O1 C2 O2 156.36(11) 3_565 . ? O1 C2 O2 122.61(15) 6_665 . ? O1 C2 O2 93.5(2) 2 . ? OC C2 O2 117.6(11) . 5_565 ? OC C2 O2 46.2(9) 4_665 5_565 ? OC C2 O2 100.9(9) 5_565 5_565 ? OAS C2 O2 70.0(19) . 5_565 ? OAS C2 O2 42.1(19) 4_665 5_565 ? OAS C2 O2 113(2) 5_565 5_565 ? O1 C2 O2 93.5(2) 3_565 5_565 ? O1 C2 O2 156.36(11) 6_665 5_565 ? O1 C2 O2 122.61(15) 2 5_565 ? O2 C2 O2 74.3(5) . 5_565 ? OC C2 O2 46.2(9) . 4_665 ? OC C2 O2 100.9(9) 4_665 4_665 ? OC C2 O2 117.6(11) 5_565 4_665 ? OAS C2 O2 42.1(19) . 4_665 ? OAS C2 O2 113(2) 4_665 4_665 ? OAS C2 O2 70.0(19) 5_565 4_665 ? O1 C2 O2 122.61(15) 3_565 4_665 ? O1 C2 O2 93.5(2) 6_665 4_665 ? O1 C2 O2 156.36(11) 2 4_665 ? O2 C2 O2 74.3(5) . 4_665 ? O2 C2 O2 74.3(5) 5_565 4_665 ? OC C2 OB2B 91.1(11) . 2 ? OC C2 OB2B 91.1(11) 4_665 2 ? OC C2 OB2B 91.1(11) 5_565 2 ? OAS C2 OB2B 109(2) . 2 ? OAS C2 OB2B 109(2) 4_665 2 ? OAS C2 OB2B 109(2) 5_565 2 ? O1 C2 OB2B 45.1(3) 3_565 2 ? O1 C2 OB2B 45.1(3) 6_665 2 ? O1 C2 OB2B 45.1(3) 2 2 ? O2 C2 OB2B 135.8(3) . 2 ? O2 C2 OB2B 135.8(3) 5_565 2 ? O2 C2 OB2B 135.8(3) 4_665 2 ? OC C2 O3 88.7(4) . 3 ? OC C2 O3 149.7(6) 4_665 3 ? OC C2 O3 34.1(4) 5_565 3 ? OAS C2 O3 142.0(18) . 3 ? OAS C2 O3 102.3(18) 4_665 3 ? OAS C2 O3 37.6(19) 5_565 3 ? O1 C2 O3 121.1(6) 3_565 3 ? O1 C2 O3 71.0(3) 6_665 3 ? O1 C2 O3 49.9(2) 2 3 ? O2 C2 O3 60.4(2) . 3 ? O2 C2 O3 131.5(5) 5_565 3 ? O2 C2 O3 106.8(3) 4_665 3 ? OB2B C2 O3 77.7(4) 2 3 ? OC C2 O3 34.1(4) . 2_665 ? OC C2 O3 88.7(4) 4_665 2_665 ? OC C2 O3 149.7(6) 5_565 2_665 ? OAS C2 O3 37.6(19) . 2_665 ? OAS C2 O3 142.0(18) 4_665 2_665 ? OAS C2 O3 102.3(18) 5_565 2_665 ? O1 C2 O3 71.0(3) 3_565 2_665 ? O1 C2 O3 49.9(2) 6_665 2_665 ? O1 C2 O3 121.1(6) 2 2_665 ? O2 C2 O3 131.5(5) . 2_665 ? O2 C2 O3 106.8(3) 5_565 2_665 ? O2 C2 O3 60.4(2) 4_665 2_665 ? OB2B C2 O3 77.7(4) 2 2_665 ? O3 C2 O3 115.6(3) 3 2_665 ? OC C2 O3 149.7(6) . 6_565 ? OC C2 O3 34.1(4) 4_665 6_565 ? OC C2 O3 88.7(4) 5_565 6_565 ? OAS C2 O3 102.3(18) . 6_565 ? OAS C2 O3 37.6(19) 4_665 6_565 ? OAS C2 O3 142.0(18) 5_565 6_565 ? O1 C2 O3 49.9(2) 3_565 6_565 ? O1 C2 O3 121.1(6) 6_665 6_565 ? O1 C2 O3 71.0(3) 2 6_565 ? O2 C2 O3 106.8(3) . 6_565 ? O2 C2 O3 60.4(2) 5_565 6_565 ? O2 C2 O3 131.5(5) 4_665 6_565 ? OB2B C2 O3 77.7(4) 2 6_565 ? O3 C2 O3 115.6(3) 3 6_565 ? O3 C2 O3 115.6(3) 2_665 6_565 ? Ca O1 OC 102.2(4) . 6_664 ? Ca O1 C2 116.2(4) . 2_654 ? OC O1 C2 19.1(3) 6_664 2_654 ? Ca O1 B 112.9(4) . 2_655 ? OC O1 B 109.9(2) 6_664 2_655 ? C2 O1 B 91.71(17) 2_654 2_655 ? Ca O1 OC 133.4(4) . 2_654 ? OC O1 OC 31.81(19) 6_664 2_654 ? C2 O1 OC 17.91(11) 2_654 2_654 ? B O1 OC 88.1(2) 2_655 2_654 ? Ca O2 OC 101.6(4) 4 5_565 ? Ca O2 C2 115.4(4) 4 . ? OC O2 C2 18.6(3) 5_565 . ? Ca O2 B 113.5(4) 4 . ? OC O2 B 109.7(2) 5_565 . ? C2 O2 B 92.14(16) . . ? Ca O2 OC 132.7(4) 4 . ? OC O2 OC 31.72(19) 5_565 . ? C2 O2 OC 17.97(12) . . ? B O2 OC 88.1(2) . . ? Ca O3 OC 111.3(4) 4 3_454 ? Ca O3 B 119.0(4) 4 . ? OC O3 B 128.3(4) 3_454 . ? Ca O3 C2 117.2(5) 4 2_554 ? OC O3 C2 15.1(2) 3_454 2_554 ? B O3 C2 117.9(3) . 2_554 ? Ca O3 OC 128.9(4) 4 2_554 ? OC O3 OC 33.5(2) 3_454 2_554 ? B O3 OC 99.8(3) . 2_554 ? C2 O3 OC 19.12(10) 2_554 2_554 ? Ca O4 OC 110.6(4) 4_655 5_665 ? Ca O4 B 118.1(3) 4_655 2_655 ? OC O4 B 128.8(4) 5_665 2_655 ? Ca O4 C2 116.8(4) 4_655 1_655 ? OC O4 C2 14.65(17) 5_665 1_655 ? B O4 C2 117.7(3) 2_655 1_655 ? Ca O4 OC 127.3(4) 4_655 4_765 ? OC O4 OC 33.4(2) 5_665 4_765 ? B O4 OC 99.8(3) 2_655 4_765 ? C2 O4 OC 19.10(10) 1_655 4_765 ? Si O5 Ca 106.5(4) . . ? Si O5 Ca 105.5(4) . 4 ? Ca O5 Ca 101.6(4) . 4 ? Si O5 OC 114.1(4) . 6_664 ? Ca O5 OC 77.8(2) . 6_664 ? Ca O5 OC 138.9(4) 4 6_664 ? Si O6 Ca 105.2(5) 1_656 6_655 ? Si O6 Ca 104.1(5) 1_656 2_655 ? Ca O6 Ca 101.2(4) 6_655 2_655 ? Si O6 OC 115.2(4) 1_656 3 ? Ca O6 OC 78.3(3) 6_655 3 ? Ca O6 OC 139.5(4) 2_655 3 ? OB2A OB1A B 64.8(11) . 2_655 ? OB2A OB1A OB2B 113.3(13) . . ? B OB1A OB2B 55.3(8) 2_655 . ? B OB1B OB2A 52.7(9) 2_655 . ? B OB1B OB2A 52.7(9) 2_655 5_665 ? OB2A OB1B OB2A 87.1(12) . 5_665 ? B OB1B OB2A 52.7(9) 2_655 4_655 ? OB2A OB1B OB2A 87.1(13) . 4_655 ? OB2A OB1B OB2A 87.1(12) 5_665 4_655 ? B OB1B C2 180.0 2_655 2_655 ? OB2A OB1B C2 127.3(9) . 2_655 ? OB2A OB1B C2 127.3(9) 5_665 2_655 ? OB2A OB1B C2 127.3(9) 4_655 2_655 ? B OB1B OC 161.13(14) 2_655 3 ? OB2A OB1B OC 113.9(8) . 3 ? OB2A OB1B OC 119.3(8) 5_665 3 ? OB2A OB1B OC 145.7(9) 4_655 3 ? C2 OB1B OC 18.87(14) 2_655 3 ? B OB1B OC 161.13(15) 2_655 2_655 ? OB2A OB1B OC 119.3(8) . 2_655 ? OB2A OB1B OC 145.7(9) 5_665 2_655 ? OB2A OB1B OC 113.9(8) 4_655 2_655 ? C2 OB1B OC 18.87(14) 2_655 2_655 ? OC OB1B OC 32.5(2) 3 2_655 ? B OB1B OC 161.13(14) 2_655 6_665 ? OB2A OB1B OC 145.7(9) . 6_665 ? OB2A OB1B OC 113.9(8) 5_665 6_665 ? OB2A OB1B OC 119.3(8) 4_655 6_665 ? C2 OB1B OC 18.87(14) 2_655 6_665 ? OC OB1B OC 32.5(2) 3 6_665 ? OC OB1B OC 32.5(2) 2_655 6_665 ? OB1A OB2A B 71.4(12) . 2_655 ? OB1A OB2A OB1B 119.9(15) . . ? B OB2A OB1B 56.1(9) 2_655 . ? B OB2B OB1A 54.1(8) 2_655 5_665 ? B OB2B OB1A 54.1(8) 2_655 . ? OB1A OB2B OB1A 89.1(11) 5_665 . ? B OB2B OB1A 54.1(8) 2_655 4_655 ? OB1A OB2B OB1A 89.1(11) 5_665 4_655 ? OB1A OB2B OB1A 89.1(11) . 4_655 ? B OB2B C2 180.0 2_655 2_654 ? OB1A OB2B C2 125.9(8) 5_665 2_654 ? OB1A OB2B C2 125.9(8) . 2_654 ? OB1A OB2B C2 125.9(8) 4_655 2_654 ? B OB2B OC 161.08(14) 2_655 3_554 ? OB1A OB2B OC 112.5(7) 5_665 3_554 ? OB1A OB2B OC 118.0(7) . 3_554 ? OB1A OB2B OC 144.4(9) 4_655 3_554 ? C2 OB2B OC 18.92(14) 2_654 3_554 ? B OB2B OC 161.08(14) 2_655 6_664 ? OB1A OB2B OC 118.0(7) 5_665 6_664 ? OB1A OB2B OC 144.4(9) . 6_664 ? OB1A OB2B OC 112.5(7) 4_655 6_664 ? C2 OB2B OC 18.92(14) 2_654 6_664 ? OC OB2B OC 32.6(2) 3_554 6_664 ? B OB2B OC 161.08(14) 2_655 2_654 ? OB1A OB2B OC 144.4(9) 5_665 2_654 ? OB1A OB2B OC 112.5(7) . 2_654 ? OB1A OB2B OC 118.0(7) 4_655 2_654 ? C2 OB2B OC 18.92(14) 2_654 2_654 ? OC OB2B OC 32.6(2) 3_554 2_654 ? OC OB2B OC 32.6(2) 6_664 2_654 ? C2 OC OAS 79.3(16) . . ? C2 OC OAS 68.7(14) . 5_565 ? OAS OC OAS 127(4) . 5_565 ? C2 OC OC 30.02(4) . 5_565 ? OAS OC OC 106.7(16) . 5_565 ? OAS OC OC 40.7(14) 5_565 5_565 ? C2 OC OC 30.02(4) . 4_665 ? OAS OC OC 51.7(16) . 4_665 ? OAS OC OC 96.7(14) 5_565 4_665 ? OC OC OC 60.001(3) 5_565 4_665 ? C2 OC O4 132.6(6) . 4_655 ? OAS OC O4 131(2) . 4_655 ? OAS OC O4 63.9(14) 5_565 4_655 ? OC OC O4 103.7(4) 5_565 4_655 ? OC OC O4 157.8(3) 4_665 4_655 ? C2 OC O3 130.8(6) . 2_665 ? OAS OC O3 67.2(19) . 2_665 ? OAS OC O3 160.2(14) 5_565 2_665 ? OC OC O3 156.4(4) 5_565 2_665 ? OC OC O3 103.0(4) 4_665 2_665 ? O4 OC O3 96.5(2) 4_655 2_665 ? C2 OC O1 113.5(12) . 6_665 ? OAS OC O1 126(2) . 6_665 ? OAS OC O1 104.9(19) 5_565 6_665 ? OC OC O1 105.1(3) 5_565 6_665 ? OC OC O1 117.3(2) 4_665 6_665 ? O4 OC O1 80.1(3) 4_655 6_665 ? O3 OC O1 66.4(3) 2_665 6_665 ? C2 OC O2 115.3(12) . 4_665 ? OAS OC O2 64(2) . 4_665 ? OAS OC O2 92.7(19) 5_565 4_665 ? OC OC O2 117.0(2) 5_565 4_665 ? OC OC O2 104.8(2) 4_665 4_665 ? O4 OC O2 67.5(3) 4_655 4_665 ? O3 OC O2 81.8(4) 2_665 4_665 ? O1 OC O2 131.3(3) 6_665 4_665 ? C2 OC OAS 12.4(15) . 4_665 ? OAS OC OAS 71.2(12) . 4_665 ? OAS OC OAS 69.0(10) 5_565 4_665 ? OC OC OAS 35.6(10) 5_565 4_665 ? OC OC OAS 27.8(11) 4_665 4_665 ? O4 OC OAS 131.1(11) 4_655 4_665 ? O3 OC OAS 130.7(11) 2_665 4_665 ? O1 OC OAS 125.7(12) 6_665 4_665 ? O2 OC OAS 103.0(12) 4_665 4_665 ? C2 OC O3 72.2(4) . 3 ? OAS OC O3 149.7(17) . 3 ? OAS OC O3 30.7(19) 5_565 3 ? OC OC O3 43.4(3) 5_565 3 ? OC OC O3 101.7(3) 4_665 3 ? O4 OC O3 67.7(3) 4_655 3 ? O3 OC O3 141.2(4) 2_665 3 ? O1 OC O3 75.8(3) 6_665 3 ? O2 OC O3 119.7(3) 4_665 3 ? OAS OC O3 79.0(11) 4_665 3 ? C2 OC O4 72.3(4) . 5_675 ? OAS OC O4 13(2) . 5_675 ? OAS OC O4 129.9(17) 5_565 5_675 ? OC OC O4 101.5(3) 5_565 5_675 ? OC OC O4 42.9(3) 4_665 5_675 ? O4 OC O4 142.7(4) 4_655 5_675 ? O3 OC O4 67.5(2) 2_665 5_675 ? O1 OC O4 118.9(3) 6_665 5_675 ? O2 OC O4 76.7(3) 4_665 5_675 ? OAS OC O4 66.2(11) 4_665 5_675 ? O3 OC O4 144.5(3) 3 5_675 ? C2 OC OB2B 70.0(11) . 2 ? OAS OC OB2B 107(2) . 2 ? OAS OC OB2B 100.1(18) 5_565 2 ? OC OC OB2B 73.69(12) 5_565 2 ? OC OC OB2B 73.69(12) 4_665 2 ? O4 OC OB2B 118.5(4) 4_655 2 ? O3 OC OB2B 86.1(4) 2_665 2 ? O1 OC OB2B 45.2(2) 6_665 2 ? O2 OC OB2B 167.2(3) 4_665 2 ? OAS OC OB2B 81.7(11) 4_665 2 ? O3 OC OB2B 72.8(2) 3 2 ? O4 OC OB2B 94.7(2) 5_675 2 ? C2 OC OB1B 72.2(11) . 2_554 ? OAS OC OB1B 65(2) . 2_554 ? OAS OC OB1B 65.4(19) 5_565 2_554 ? OC OC OB1B 73.73(12) 5_565 2_554 ? OC OC OB1B 73.73(12) 4_665 2_554 ? O4 OC OB1B 87.6(3) 4_655 2_554 ? O3 OC OB1B 119.6(4) 2_665 2_554 ? O1 OC OB1B 167.0(3) 6_665 2_554 ? O2 OC OB1B 44.8(2) 4_665 2_554 ? OAS OC OB1B 60.6(11) 4_665 2_554 ? O3 OC OB1B 95.8(2) 3 2_554 ? O4 OC OB1B 73.7(2) 5_675 2_554 ? OB2B OC OB1B 142.2(2) 2 2_554 ? C2 OC O6 161.7(11) . 2_554 ? OAS OC O6 85.2(16) . 2_554 ? OAS OC O6 114.8(14) 5_565 2_554 ? OC OC O6 155.1(3) 5_565 2_554 ? OC OC O6 136.8(4) 4_665 2_554 ? O4 OC O6 54.0(3) 4_655 2_554 ? O3 OC O6 48.4(3) 2_665 2_554 ? O1 OC O6 83.6(2) 6_665 2_554 ? O2 OC O6 48.0(2) 4_665 2_554 ? OAS OC O6 149.6(12) 4_665 2_554 ? O3 OC O6 120.6(3) 3 2_554 ? O4 OC O6 94.1(3) 5_675 2_554 ? OB2B OC O6 124.6(3) 2 2_554 ? OB1B OC O6 92.5(3) 2_554 2_554 ? OC OAS OC 87.6(11) . 4_665 ? OC OAS C2 46.1(5) . . ? OC OAS C2 43.1(6) 4_665 . ? OC OAS OC 45.6(7) . 5_565 ? OC OAS OC 47.7(5) 4_665 5_565 ? C2 OAS OC 9.0(11) . 5_565 ? _refine_diff_density_max 0.619 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.112