#------------------------------------------------------------------------------ #$Date: 2021-02-26 02:50:01 +0200 (Fri, 26 Feb 2021) $ #$Revision: 262244 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/02/3000281.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3000281 loop_ _publ_author_name 'Koichi Momma' 'Takuji Ikeda' 'Toshiro Nagase' 'Takahiro Kuribayashi' 'Chibune Honma' 'Katsumi Nishikubo' 'Naoki Takahashi' 'Masayuki Takada' 'Yoshitaka Matsushita' 'Ritsuro Miyawaki' 'Satoshi Matsubara' _publ_section_title ; Bosoite, a new silica clathrate mineral from Chiba Prefecture, Japan ; _journal_name_full 'Mineralogical Magazine' _journal_page_first 941 _journal_volume 84 _journal_year 2020 _chemical_formula_sum 'C17 H68 O68 Si34' _chemical_formula_weight 2315.77 _space_group_crystal_system hexagonal _space_group_IT_number 191 _space_group_name_Hall '-P 6 2' _space_group_name_H-M_alt 'P 6/m m m' _atom_sites_solution_hydrogens . _audit_creation_method SHELXL-2018/1 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 1 _cell_length_a 13.9020(3) _cell_length_b 13.9020(3) _cell_length_c 11.2802(2) _cell_measurement_reflns_used 22203 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 68.2 _cell_measurement_theta_min 3.6 _cell_volume 1888.00(7) _computing_cell_refinement 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku VariMax with RAPID' _diffrn_measurement_method '\w scan' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_unetI/netI 0.0115 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 22203 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.687 _diffrn_reflns_theta_max 68.193 _diffrn_reflns_theta_min 3.671 _diffrn_source 'rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 6.527 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_type numerical _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.037 _exptl_crystal_description block _exptl_crystal_F_000 1190 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.550 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.082 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 739 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.168 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0426 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+2.6529P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1200 _refine_ls_wR_factor_ref 0.1208 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 705 _reflns_number_total 739 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file Bosoite_non_split_model_COD.cif _cod_data_source_block shelx _cod_depositor_comments 'Releasing structure 3000281 into public domain as published material.' _cod_original_cell_volume 1887.99(8) _cod_database_code 3000281 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 x-y,x,z 3 -y,x-y,z 4 -x,-y,z 5 -x+y,-x,z 6 y,-x+y,z 7 -x+y,y,z 8 y,x,z 9 x,x-y,z 10 x-y,-y,z 11 -y,-x,z 12 -x,-x+y,z 13 -x,-y,-z 14 -x+y,-x,-z 15 y,-x+y,-z 16 x,y,-z 17 x-y,x,-z 18 -y,x-y,-z 19 x-y,-y,-z 20 -y,-x,-z 21 -x,-x+y,-z 22 -x+y,y,-z 23 y,x,-z 24 x,x-y,-z 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 Si1 Si 0.41870(9) 0.20935(4) 0.22527(9) 0.0300(4) Uani 1 2 d S T P . . Si2 Si 0.38736(8) 0.38736(8) 0.36254(9) 0.0305(4) Uani 1 2 d S T P . . Si3 Si 0.26279(12) 0.13140(6) 0.000000 0.0296(4) Uani 1 4 d S T P . . Si4 Si 0.666667 0.333333 0.13850(15) 0.0318(5) Uani 1 6 d S T P . . O1 O 0.3946(3) 0.2885(2) 0.3036(3) 0.0786(10) Uani 1 1 d . . . . . O2 O 0.5438(3) 0.27189(15) 0.1844(4) 0.0836(14) Uani 1 2 d S T P . . O3 O 0.3394(3) 0.16968(17) 0.1142(3) 0.0724(12) Uani 1 2 d S T P . . O4 O 0.3616(4) 0.000000 0.500000 0.0611(15) Uani 1 4 d S T P . . O5 O 0.1850(4) 0.000000 0.000000 0.0651(15) Uani 1 4 d S T P . . O6 O 0.500000 0.000000 0.3425(5) 0.0725(18) Uani 1 4 d S T P . . O7 O 0.666667 0.333333 0.000000 0.102(4) Uani 1 12 d S T P . . C1 C 0.333333 0.666667 0.500000 0.127(9) Uani 1 12 d S T P . . C2 C 0.500000 0.000000 0.000000 0.137(8) Uani 1 8 d S T P . . C3A C 0.000000 0.000000 0.265(9) 0.28(7) Uiso 0.73(14) 12 d S . . . . C3B C -0.044(3) 0.044(3) 0.571(6) 0.279(12) Uiso 0.30(3) 2 d S . . . . C3C C 0.000000 0.112(6) 0.315(6) 0.279(12) Uiso 0.33(3) 2 d S . . . . C3D C 0.000000 0.000000 0.06(2) 0.279(12) Uiso 0.21(6) 12 d S . . . . C3E C 0.177(8) 0.088(4) 0.500000 0.279(12) Uiso 0.50(6) 4 d S . . . . 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 Si1 0.0330(6) 0.0292(5) 0.0290(6) -0.0010(2) -0.0019(4) 0.0165(3) Si2 0.0336(5) 0.0336(5) 0.0247(6) -0.0045(3) -0.0045(3) 0.0171(5) Si3 0.0312(8) 0.0296(6) 0.0286(7) 0.000 0.000 0.0156(4) Si4 0.0334(6) 0.0334(6) 0.0287(9) 0.000 0.000 0.0167(3) O1 0.107(2) 0.0688(18) 0.0800(18) -0.0271(15) 0.0040(17) 0.0594(18) O2 0.034(2) 0.091(3) 0.107(3) 0.0100(11) 0.020(2) 0.0171(10) O3 0.068(2) 0.091(2) 0.050(2) -0.0147(10) -0.029(2) 0.0338(12) O4 0.068(2) 0.098(4) 0.028(2) 0.000 0.000 0.049(2) O5 0.065(3) 0.029(2) 0.089(4) 0.000 0.000 0.0146(12) O6 0.056(2) 0.132(5) 0.055(3) 0.000 0.000 0.066(3) O7 0.139(7) 0.139(7) 0.029(4) 0.000 0.000 0.070(4) C1 0.161(14) 0.161(14) 0.058(10) 0.000 0.000 0.081(7) C2 0.161(16) 0.110(15) 0.124(15) 0.000 0.000 0.055(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' 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 O1 Si1 O1 107.5(2) . 9 O1 Si1 O2 109.95(15) . . O1 Si1 O2 109.95(15) 9 . O1 Si1 O3 109.56(15) . . O1 Si1 O3 109.56(15) 9 . O2 Si1 O3 110.3(2) . . O1 Si2 O1 108.4(2) . 8 O1 Si2 O6 109.90(16) . 2 O1 Si2 O6 109.90(16) 8 2 O1 Si2 O4 108.68(15) . 2 O1 Si2 O4 108.68(15) 8 2 O6 Si2 O4 111.2(3) 2 2 O3 Si3 O3 108.8(3) 16 . O3 Si3 O5 110.04(13) 16 . O3 Si3 O5 110.04(13) . . O3 Si3 O5 110.04(13) 16 2 O3 Si3 O5 110.04(13) . 2 O5 Si3 O5 107.8(4) . 2 O7 Si4 O2 109.29(18) . . O7 Si4 O2 109.29(18) . 3_655 O2 Si4 O2 109.65(18) . 3_655 O7 Si4 O2 109.29(18) . 5_665 O2 Si4 O2 109.65(18) . 5_665 O2 Si4 O2 109.65(18) 3_655 5_665 Si1 O1 Si2 167.7(2) . . Si4 O2 Si1 177.7(4) . . Si1 O3 Si3 178.3(3) . . Si2 O4 Si2 154.0(4) 15_556 6 Si3 O5 Si3 167.8(4) 15 . Si2 O6 Si2 163.6(4) 3_655 6 Si4 O7 Si4 180.0 . 14_665 C3C C3A C3C 141(9) 6 3 C3C C3A C3C 56.2(18) 6 5 C3C C3A C3C 109(5) 3 5 C3C C3A C3C 109(5) 6 2 C3C C3A C3C 56.2(18) 3 2 C3C C3A C3C 141(9) 5 2 C3C C3A C3C 109(5) 6 4 C3C C3A C3C 56.2(18) 3 4 C3C C3A C3C 56.2(18) 5 4 C3C C3A C3C 109(5) 2 4 C3C C3A C3C 56.2(18) 6 . C3C C3A C3C 109(5) 3 . C3C C3A C3C 109(5) 5 . C3C C3A C3C 56.2(18) 2 . C3C C3A C3C 141(9) 4 . C3B C3B C3B 120.001(16) 6 2 C3B C3B C3E 113.6(12) 6 3 C3B C3B C3E 113.6(12) 2 3 C3B C3B C3C 69.8(16) 6 16_556 C3B C3B C3C 122(3) 2 16_556 C3E C3B C3C 111(4) 3 16_556 C3B C3B C3C 122(3) 6 17_556 C3B C3B C3C 69.8(16) 2 17_556 C3E C3B C3C 111(4) 3 17_556 C3C C3B C3C 61(3) 16_556 17_556 C3B C3B C3B 89.998(17) 6 16_556 C3B C3B C3B 89.998(6) 2 16_556 C3E C3B C3B 53(4) 3 16_556 C3C C3B C3B 147(3) 16_556 16_556 C3C C3B C3B 147(3) 17_556 16_556 C3B C3C C3B 40(3) 15_556 16_556 C3B C3C C3C 95(3) 15_556 2 C3B C3C C3C 59.6(17) 16_556 2 C3B C3C C3C 59.6(17) 15_556 6 C3B C3C C3C 95(3) 16_556 6 C3C C3C C3C 119.998(10) 2 6 C3B C3C C3A 84(6) 15_556 . C3B C3C C3A 84(6) 16_556 . C3C C3C C3A 61.9(9) 2 . C3C C3C C3A 61.9(9) 6 . C3B C3E C3B 74(7) 14_556 5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 O1 1.573(2) . Si1 O1 1.573(2) 9 Si1 O2 1.575(4) . Si1 O3 1.575(3) . Si2 O1 1.574(2) . Si2 O1 1.574(2) 8 Si2 O6 1.5821(13) 2 Si2 O4 1.5914(15) 2 Si3 O3 1.584(3) 16 Si3 O3 1.584(3) . Si3 O5 1.5909(10) . Si3 O5 1.5909(10) 2 Si4 O7 1.5623(17) . Si4 O2 1.568(4) . Si4 O2 1.568(4) 3_655 Si4 O2 1.568(4) 5_665 C3A C3C 1.65(7) 6 C3A C3C 1.65(7) 3 C3A C3C 1.65(7) 5 C3A C3C 1.65(7) 2 C3A C3C 1.65(7) 4 C3A C3C 1.65(7) . C3B C3B 1.06(8) 6 C3B C3B 1.06(8) 2 C3B C3E 1.33(6) 3 C3B C3C 1.54(6) 16_556 C3B C3C 1.54(6) 17_556 C3B C3B 1.60(13) 16_556 C3C C3C 1.55(8) 2 C3C C3C 1.55(8) 6 C3D C3D 1.5(5) 13