#------------------------------------------------------------------------------ #$Date: 2021-11-06 22:14:29 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270462 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243740.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_7243740 loop_ _publ_author_name 'Chang, Shenzhen' 'Chen, Yanhong' 'An, Haiyan' 'Zhu, Qingshan' 'Luo, Huiyun' 'Huang, Yaohui' _publ_section_title ; Polyoxometalate-based supramolecular porous frameworks with dual-active centers towards highly efficient synthesis of functionalized p-benzoquinones ; _journal_issue 21 _journal_name_full 'Green Chemistry' _journal_page_first 8591 _journal_page_last 8603 _journal_paper_doi 10.1039/D1GC03061B _journal_volume 23 _journal_year 2021 _chemical_formula_sum 'C18 H67 Cu3 K3 N24 O76 Si W12' _chemical_formula_weight 4378.16 _chemical_name_systematic SiWCu _space_group_crystal_system trigonal _space_group_IT_number 147 _space_group_name_Hall '-P 3' _space_group_name_H-M_alt 'P -3' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-06-15 deposited with the CCDC. 2021-09-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 1 _cell_length_a 15.570(3) _cell_length_b 15.570(3) _cell_length_c 10.337(3) _cell_measurement_reflns_used 2548 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 24.992 _cell_measurement_theta_min 2.483 _cell_volume 2170.2(9) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_unetI/netI 0.0341 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 11390 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 24.992 _diffrn_reflns_theta_max 24.992 _diffrn_reflns_theta_min 2.483 _exptl_absorpt_coefficient_mu 16.836 _exptl_absorpt_correction_T_max 0.021 _exptl_absorpt_correction_T_min 0.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 3.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1997 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.230 _refine_diff_density_max 2.126 _refine_diff_density_min -2.791 _refine_diff_density_rms 0.367 _refine_ls_extinction_coef 0.0038(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 233 _refine_ls_number_reflns 2548 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0445 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+41.4034P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1258 _refine_ls_wR_factor_ref 0.1284 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2353 _reflns_number_total 2548 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1gc03061b2.cif _cod_data_source_block SiWCu _cod_depositor_comments 'Adding full bibliography for 7243739--7243740.cif.' _cod_original_cell_volume 2170.3(11) _cod_database_code 7243740 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_min 0.102 _shelx_estimated_absorpt_t_max 0.113 _shelx_res_file ; TITL mo_21APR11ANHY0407_2_H_0m_a.res in P-3 Q.res created by SHELXL-2018/3 at 13:28:36 on 21-Apr-2021 CELL 0.71073 15.5699 15.5699 10.3375 90.000 90.000 120.000 ZERR 1 0.0032 0.0032 0.0029 0.000 0.000 0.000 LATT 1 SYMM -y, x-y, z SYMM -x+y, -x, z SFAC C H N O SI W K Cu UNIT 18 67 24 76 1 12 3 3 TEMP 22.750 SIZE 0.230 0.240 0.250 L.S. 12 BOND $H ACTA CONF HTAB FMAP 2 PLAN 5 OMIT -3 50 Shel 999 0.84 ISOR 0.01 O7 O9 O10 ISOR 0.01 N2 N4 isor 0.01 o1w omit -2 4 0 omit -1 2 0 omit 0 2 2 omit 2 3 1 omit 0 2 0 omit -2 2 2 exyz k1 cu1 eadp k1 cu1 WGHT 0.070100 41.403400 EXTI 0.003759 FVAR 0.19618 W1 6 0.945876 0.850863 0.219829 11.00000 0.02967 0.03261 = 0.01840 -0.00424 -0.00144 0.01577 W2 6 1.041155 0.797125 0.499335 11.00000 0.04631 0.02908 = 0.04352 0.00869 0.01324 0.02721 PART 1 O3 4 0.839540 0.791518 0.340602 10.50000 0.01711 0.04278 = 0.01257 0.00975 0.00510 0.01433 PART 2 O3A 4 0.820520 0.743896 0.300445 10.50000 0.04819 0.02930 = 0.02123 -0.00576 -0.00158 0.01384 PART 3 O4 4 1.008133 0.779390 0.301274 10.50000 0.05563 0.03016 = 0.02409 -0.00734 -0.00013 0.03185 PART 4 O4A 4 1.020659 0.824279 0.338762 10.50000 0.03035 0.03944 = 0.01799 0.00062 0.00460 0.02835 PART 0 O5 4 0.919790 0.777413 0.091132 11.00000 0.05224 0.06710 = 0.07061 -0.05261 -0.02136 0.03372 O6 4 1.071808 0.960494 0.174683 11.00000 0.02560 0.02805 = 0.11683 -0.00103 -0.00498 0.01257 PART 5 O7 4 0.894723 0.709700 0.516225 10.50000 0.03523 0.02042 = 0.02987 -0.00201 -0.00455 0.01579 PART 6 O7A 4 0.912583 0.757224 0.548197 10.50000 0.04302 0.01752 = 0.02323 0.00081 -0.00040 0.01911 PART 0 O8 4 1.059750 0.699375 0.500181 11.00000 0.10466 0.06147 = 0.04376 0.00483 0.00276 0.06765 O9 4 0.002259 0.399367 1.145169 11.00000 0.08734 0.07385 = 0.10794 0.00057 -0.03150 0.04751 O10 4 0.115388 0.457034 1.022720 11.00000 0.13749 0.07896 = 0.07991 -0.00014 -0.01246 0.06476 O1W 4 0.568987 0.423153 1.214378 11.00000 0.19714 0.18626 = 0.18887 0.00641 -0.01013 0.09045 OW1 4 0.666667 0.333333 1.065857 10.33333 0.12860 OW2 4 1.018019 0.509349 0.556794 11.00000 0.11399 OW3 4 0.787662 0.564455 1.253277 11.00000 0.23200 N1 3 0.235176 0.413387 1.177221 11.00000 0.06078 0.04862 = 0.06513 0.01121 0.02449 0.02180 N2 3 0.286383 0.402907 1.083138 11.00000 0.09788 0.09911 = 0.10700 -0.01823 0.03400 0.03552 part 7 N3 3 0.396413 0.457844 1.135275 10.50000 0.04324 0.05870 = 0.05790 -0.01197 -0.01955 0.02014 part 8 N3A 3 0.369538 0.481544 1.076218 10.50000 0.01787 0.04348 = 0.05410 -0.02151 -0.00223 -0.00384 part 0 N4 3 0.375525 0.521226 1.203632 11.00000 0.09700 0.10623 = 0.11658 -0.03026 0.01421 0.04434 C1 1 0.078950 0.410627 1.114674 11.00000 0.11422 0.04021 = 0.05050 -0.00657 -0.01976 0.04317 C2 1 0.127284 0.363166 1.188594 11.00000 0.04592 0.04052 = 0.06068 0.01553 0.00345 0.01676 AFIX 23 H2A 2 0.110208 0.360588 1.279302 11.00000 -1.20000 H2B 2 0.099970 0.295408 1.158666 11.00000 -1.20000 AFIX 0 C3 1 0.294288 0.490242 1.248078 11.00000 0.03505 0.07531 = 0.05692 -0.03012 0.01001 0.01067 AFIX 43 H3A 2 0.276793 0.515536 1.318391 11.00000 -1.20000 AFIX 0 O2 4 0.959552 0.887466 0.442053 11.00000 0.08104 0.07816 = 0.07657 -0.00083 -0.00769 0.03858 O1 4 1.000000 1.000000 0.345370 10.33333 0.07126 0.07126 = 0.08425 0.00000 0.00000 0.03563 SI1 5 1.000000 1.000000 0.500000 10.16667 0.01677 0.01677 = 0.01656 0.00000 0.00000 0.00838 K1 7 0.519245 0.480731 1.051098 10.50000 0.05812 0.06299 = 0.08970 -0.01276 -0.00593 0.02657 CU1 8 0.519245 0.480731 1.051098 10.50000 0.05812 0.06299 = 0.08970 -0.01276 -0.00593 0.02657 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_21APR11ANHY0407_2_H_0m_a.res in P-3 REM wR2 = 0.128411, GooF = S = 1.07519, Restrained GooF = 1.08405 for all data REM R1 = 0.044497 for 2353 Fo > 4sig(Fo) and 0.047542 for all 2548 data REM 233 parameters refined using 36 restraints END WGHT 0.0698 41.4187 REM Instructions for potential hydrogen bonds EQIV $8 -x+1, -y+1, -z+2 HTAB C2 O7_$8 HTAB C2 O7A_$8 EQIV $12 -y+1, x-y, z+1 HTAB C2 O6_$12 REM Highest difference peak 2.126, deepest hole -2.791, 1-sigma level 0.367 Q1 1 0.1701 0.4880 1.0206 11.00000 0.05 2.13 Q2 1 0.2019 0.5287 1.4873 11.00000 0.05 1.62 Q3 1 0.9013 0.5697 1.2589 11.00000 0.05 1.57 Q4 1 1.0000 0.5000 0.5000 10.50000 0.05 1.56 Q5 1 0.6794 0.4862 1.3191 11.00000 0.05 1.46 ; _shelx_res_checksum 86322 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -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 W1 W 0.94588(3) 0.85086(3) 0.21983(4) 0.0268(2) Uani 1 1 d . . . . . W2 W 1.04116(4) 0.79713(4) 0.49934(5) 0.0359(2) Uani 1 1 d . . . . . O3 O 0.8395(12) 0.7915(15) 0.3406(16) 0.024(4) Uani 0.5 1 d . . P A 1 O3A O 0.8205(16) 0.7439(15) 0.3004(18) 0.035(5) Uani 0.5 1 d . . P A 2 O4 O 1.0081(15) 0.7794(15) 0.3013(18) 0.032(4) Uani 0.5 1 d . . P A 3 O4A O 1.0207(13) 0.8243(15) 0.3388(16) 0.024(4) Uani 0.5 1 d . . P A 4 O5 O 0.9198(8) 0.7774(9) 0.0911(11) 0.062(3) Uani 1 1 d . . . . . O6 O 1.0718(7) 0.9605(7) 0.1747(13) 0.057(3) Uani 1 1 d . . . . . O7 O 0.8947(13) 0.7097(14) 0.5162(17) 0.028(4) Uani 0.5 1 d . U P A 5 O7A O 0.9126(14) 0.7572(14) 0.5482(16) 0.026(4) Uani 0.5 1 d . . P A 6 O8 O 1.0597(10) 0.6994(8) 0.5002(10) 0.058(3) Uani 1 1 d . . . . . O9 O 0.0023(12) 0.3994(11) 1.1452(16) 0.087(4) Uani 1 1 d . U . . . O10 O 0.1154(14) 0.4570(12) 1.0227(15) 0.094(4) Uani 1 1 d . U . . . O1W O 0.569(2) 0.423(2) 1.214(3) 0.193(12) Uani 1 1 d . U . . . OW1 O 0.666667 0.333333 1.066(4) 0.129(12) Uiso 1 3 d S . P . . OW2 O 1.0180(15) 0.5093(15) 0.5568(17) 0.114(6) Uiso 1 1 d . . . . . OW3 O 0.788(3) 0.564(3) 1.253(4) 0.232(15) Uiso 1 1 d . . . . . N1 N 0.2352(11) 0.4134(10) 1.1772(14) 0.061(4) Uani 1 1 d . . . . . N2 N 0.2864(17) 0.4029(16) 1.083(2) 0.107(6) Uani 1 1 d . U . . . N3 N 0.396(2) 0.458(2) 1.135(3) 0.056(7) Uani 0.5 1 d . . P B 7 N3A N 0.3695(16) 0.4815(19) 1.076(3) 0.047(6) Uani 0.5 1 d . . P B 8 N4 N 0.3755(17) 0.5212(17) 1.204(2) 0.109(7) Uani 1 1 d . U . . . C1 C 0.0789(19) 0.4106(12) 1.1147(17) 0.066(5) Uani 1 1 d . . . . . C2 C 0.1273(11) 0.3632(11) 1.1886(16) 0.051(4) Uani 1 1 d . . . . . H2A H 0.110208 0.360588 1.279302 0.061 Uiso 1 1 calc R U . . . H2B H 0.099970 0.295408 1.158666 0.061 Uiso 1 1 calc R U . . . C3 C 0.2943(11) 0.4902(13) 1.2481(16) 0.063(5) Uani 1 1 d . . . . . H3A H 0.276793 0.515536 1.318391 0.076 Uiso 1 1 calc R U . . . O2 O 0.9596(11) 0.8875(11) 0.4421(14) 0.079(4) Uani 1 1 d . . . . . O1 O 1.000000 1.000000 0.345(2) 0.076(6) Uani 1 3 d S T P A . Si1 Si 1.000000 1.000000 0.500000 0.0167(13) Uani 1 6 d S T P . . K1 K 0.5192(2) 0.4807(2) 1.0511(3) 0.0719(8) Uani 0.5 1 d . . P B . Cu1 Cu 0.5192(2) 0.4807(2) 1.0511(3) 0.0719(8) Uani 0.5 1 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 W1 0.0297(3) 0.0326(3) 0.0184(3) -0.00424(16) -0.00144(16) 0.0158(2) W2 0.0463(4) 0.0291(3) 0.0435(4) 0.0087(2) 0.0132(2) 0.0272(3) O3 0.017(8) 0.043(11) 0.013(8) 0.010(8) 0.005(6) 0.014(8) O3A 0.048(12) 0.029(10) 0.021(9) -0.006(8) -0.002(8) 0.014(10) O4 0.056(12) 0.030(10) 0.024(9) -0.007(8) 0.000(8) 0.032(10) O4A 0.030(9) 0.039(11) 0.018(8) 0.001(8) 0.005(7) 0.028(9) O5 0.052(6) 0.067(7) 0.071(7) -0.053(6) -0.021(5) 0.034(6) O6 0.026(5) 0.028(5) 0.117(10) -0.001(5) -0.005(5) 0.013(4) O7 0.035(8) 0.020(7) 0.030(7) -0.002(6) -0.005(6) 0.016(6) O7A 0.043(10) 0.018(9) 0.023(8) 0.001(7) 0.000(7) 0.019(8) O8 0.105(9) 0.061(7) 0.044(5) 0.005(5) 0.003(6) 0.068(7) O9 0.087(8) 0.074(7) 0.108(8) 0.001(6) -0.032(7) 0.048(6) O10 0.137(9) 0.079(7) 0.080(7) 0.000(6) -0.012(7) 0.065(7) O1W 0.197(15) 0.186(14) 0.189(15) 0.006(9) -0.010(9) 0.090(10) N1 0.061(8) 0.049(8) 0.065(8) 0.011(7) 0.024(7) 0.022(7) N2 0.098(10) 0.099(10) 0.107(10) -0.018(8) 0.034(8) 0.036(7) N3 0.043(15) 0.059(18) 0.058(17) -0.012(14) -0.020(13) 0.020(14) N3A 0.018(11) 0.043(14) 0.054(15) -0.022(12) -0.002(10) -0.004(10) N4 0.097(10) 0.106(10) 0.117(10) -0.030(8) 0.014(8) 0.044(8) C1 0.114(17) 0.040(9) 0.051(9) -0.007(7) -0.020(10) 0.043(10) C2 0.046(8) 0.041(8) 0.061(9) 0.016(7) 0.003(7) 0.017(7) C3 0.035(8) 0.075(11) 0.057(9) -0.030(8) 0.010(7) 0.011(8) O2 0.081(9) 0.078(9) 0.077(9) -0.001(7) -0.008(7) 0.039(8) O1 0.071(9) 0.071(9) 0.084(15) 0.000 0.000 0.036(4) Si1 0.017(2) 0.017(2) 0.017(3) 0.000 0.000 0.0084(10) K1 0.0581(16) 0.0630(17) 0.090(2) -0.0128(15) -0.0059(14) 0.0266(14) Cu1 0.0581(16) 0.0630(17) 0.090(2) -0.0128(15) -0.0059(14) 0.0266(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 _geom_angle_publ_flag O5 W1 O4A 109.7(7) . . ? O5 W1 O6 102.1(6) . 3_675 ? O4A W1 O6 148.1(7) . 3_675 ? O5 W1 O3 109.6(8) . . ? O6 W1 O3 84.2(6) 3_675 . ? O5 W1 O6 102.0(6) . . ? O4A W1 O6 83.3(7) . . ? O6 W1 O6 88.3(6) 3_675 . ? O3 W1 O6 148.4(8) . . ? O5 W1 O4 88.5(7) . . ? O6 W1 O4 169.1(7) 3_675 . ? O6 W1 O4 91.9(7) . . ? O5 W1 O3A 87.7(7) . . ? O6 W1 O3A 93.4(7) 3_675 . ? O6 W1 O3A 169.6(7) . . ? O5 W1 O2 155.2(6) . . ? O4A W1 O2 54.7(7) . . ? O6 W1 O2 95.8(5) 3_675 . ? O3 W1 O2 55.1(7) . . ? O6 W1 O2 95.4(5) . . ? O4 W1 O2 73.3(6) . . ? O3A W1 O2 74.2(7) . . ? O5 W1 O1 159.6(7) . . ? O4A W1 O1 84.4(7) . . ? O6 W1 O1 64.3(5) 3_675 . ? O3 W1 O1 85.1(8) . . ? O6 W1 O1 64.0(5) . . ? O4 W1 O1 106.1(7) . . ? O3A W1 O1 107.6(7) . . ? O2 W1 O1 45.2(6) . . ? O8 W2 O3 109.1(8) . 6_656 ? O8 W2 O4A 110.6(7) . . ? O8 W2 O7A 110.0(7) . . ? O8 W2 O7A 111.2(7) . 6_656 ? O3 W2 O7A 92.1(7) 6_656 6_656 ? O8 W2 O7 93.1(7) . 6_656 ? O3 W2 O7 87.5(7) 6_656 6_656 ? O4A W2 O7 90.6(8) . 6_656 ? O7A W2 O7 153.9(9) . 6_656 ? O7A W2 O7 21.5(5) 6_656 6_656 ? O8 W2 O7 92.1(7) . . ? O7 W2 O7 174.8(10) 6_656 . ? O8 W2 O4 91.6(6) . . ? O8 W2 O3A 90.1(7) . 6_656 ? O3 W2 O3A 20.2(7) 6_656 6_656 ? O4A W2 O3A 158.3(9) . 6_656 ? O7A W2 O3A 86.3(8) . 6_656 ? O7A W2 O3A 92.9(8) 6_656 6_656 ? O7 W2 O3A 81.4(8) 6_656 6_656 ? O7 W2 O3A 98.2(8) . 6_656 ? O4 W2 O3A 178.0(8) . 6_656 ? O8 W2 O2 155.9(5) . . ? O3 W2 O2 87.9(8) 6_656 . ? O4A W2 O2 54.5(7) . . ? O7A W2 O2 57.3(6) . . ? O7A W2 O2 84.2(7) 6_656 . ? O7 W2 O2 104.9(7) 6_656 . ? O7 W2 O2 70.2(6) . . ? O4 W2 O2 70.6(6) . . ? O3A W2 O2 108.0(6) 6_656 . ? O8 W2 O2 156.1(6) . 6_656 ? O3 W2 O2 55.1(7) 6_656 6_656 ? O2 W2 O2 47.9(6) . 6_656 ? W2 O3 W1 149.9(10) 5_566 . ? W1 O3A W2 118.0(10) . 5_566 ? W1 O4 W2 119.7(9) . . ? W2 O4A W1 150.2(10) . . ? W1 O6 W1 137.4(7) 2_765 . ? W2 O7 W2 124.5(10) 5_566 . ? W2 O7A W2 144.5(9) . 5_566 ? C1 O9 K1 114.4(14) . 3_565 ? C1 O9 K1 81.0(12) . 6_557 ? K1 O9 K1 33.9(3) 3_565 6_557 ? C1 O10 K1 112.7(17) . 6_557 ? C1 O10 K1 78.4(15) . 3_565 ? K1 O10 K1 34.3(3) 6_557 3_565 ? C3 N1 N2 109.5(15) . . ? C3 N1 C2 122.6(14) . . ? N2 N1 C2 126.7(17) . . ? N3A N2 N1 108(2) . . ? N1 N2 N3 103.9(19) . . ? N3A N2 K1 31.5(13) . 4_667 ? N1 N2 K1 139.6(14) . 4_667 ? N3 N2 K1 48.1(13) . 4_667 ? N3A N2 K1 38.0(16) . . ? N1 N2 K1 131.9(15) . . ? N3 N2 K1 28.0(12) . . ? K1 N2 K1 27.3(2) 4_667 . ? N4 N3 N2 89(2) . . ? N4 N3 K1 131(2) . . ? N2 N3 K1 129.9(19) . . ? N4 N3 K1 115(2) . 4_667 ? N2 N3 K1 100.5(17) . 4_667 ? K1 N3 K1 40.3(6) . 4_667 ? N2 N3A N4 100(2) . . ? N2 N3A K1 129.4(18) . 4_667 ? N4 N3A K1 127.7(16) . 4_667 ? N2 N3A K1 123(2) . . ? N4 N3A K1 104.6(18) . . ? K1 N3A K1 38.7(5) 4_667 . ? C3 N4 N3 119(2) . . ? C3 N4 N3A 110(2) . . ? C3 N4 K1 148.4(17) . . ? N3 N4 K1 29.2(14) . . ? N3A N4 K1 48.3(13) . . ? C3 N4 K1 141.0(16) . 4_667 ? N3 N4 K1 41.0(15) . 4_667 ? N3A N4 K1 30.8(10) . 4_667 ? K1 N4 K1 27.8(2) . 4_667 ? O10 C1 O9 118(2) . . ? O10 C1 C2 121(2) . . ? O9 C1 C2 121.2(18) . . ? O10 C1 K1 76.2(13) . 3_565 ? O9 C1 K1 42.0(10) . 3_565 ? C2 C1 K1 162.2(15) . 3_565 ? O10 C1 K1 44.0(12) . 6_557 ? O9 C1 K1 73.9(12) . 6_557 ? C2 C1 K1 164.8(16) . 6_557 ? K1 C1 K1 32.2(3) 3_565 6_557 ? N1 C2 C1 114.9(15) . . ? N1 C2 H2A 108.5 . . ? C1 C2 H2A 108.5 . . ? N1 C2 H2B 108.5 . . ? C1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N4 C3 N1 105.8(16) . . ? N4 C3 H3A 127.1 . . ? N1 C3 H3A 127.1 . . ? Si1 O2 W1 123.5(8) . . ? Si1 O2 W2 120.1(7) . . ? W1 O2 W2 96.3(5) . . ? Si1 O2 W2 119.6(8) . 5_566 ? W1 O2 W2 96.4(5) . 5_566 ? W2 O2 W2 94.5(5) . 5_566 ? Si1 O1 W1 122.5(5) . . ? Si1 O1 W1 122.5(5) . 3_675 ? W1 O1 W1 93.8(7) . 3_675 ? Si1 O1 W1 122.5(5) . 2_765 ? W1 O1 W1 93.8(7) . 2_765 ? W1 O1 W1 93.8(7) 3_675 2_765 ? O1 Si1 O1 180.0 . 4_776 ? O1 Si1 O2 111.3(5) . 4_776 ? O1 Si1 O2 68.7(5) 4_776 4_776 ? O1 Si1 O2 111.3(5) . 5_566 ? O1 Si1 O2 68.7(5) 4_776 5_566 ? O2 Si1 O2 107.6(5) 4_776 5_566 ? O1 Si1 O2 68.7(5) . 2_765 ? O1 Si1 O2 111.3(5) 4_776 2_765 ? O2 Si1 O2 72.4(5) 4_776 2_765 ? O2 Si1 O2 180.0 5_566 2_765 ? O1 Si1 O2 111.3(5) . 6_656 ? O1 Si1 O2 68.7(5) 4_776 6_656 ? O2 Si1 O2 107.6(5) 4_776 6_656 ? O2 Si1 O2 107.6(5) 5_566 6_656 ? O2 Si1 O2 72.4(5) 2_765 6_656 ? O1 Si1 O2 68.7(5) . 3_675 ? O1 Si1 O2 111.3(5) 4_776 3_675 ? O2 Si1 O2 72.4(5) 4_776 3_675 ? O2 Si1 O2 72.4(5) 5_566 3_675 ? O2 Si1 O2 107.6(5) 2_765 3_675 ? O2 Si1 O2 180.0 6_656 3_675 ? O1 Si1 O2 68.7(5) . . ? O1 Si1 O2 111.3(5) 4_776 . ? O2 Si1 O2 180.0 4_776 . ? O2 Si1 O2 72.4(5) 5_566 . ? O2 Si1 O2 107.6(5) 2_765 . ? O2 Si1 O2 72.4(5) 6_656 . ? O2 Si1 O2 107.6(5) 3_675 . ? K1 K1 O9 99.1(6) 4_667 2_665 ? K1 K1 N3 80.5(10) 4_667 . ? O9 K1 N3 93.2(9) 2_665 . ? K1 K1 N3A 83.0(10) 4_667 4_667 ? O9 K1 N3A 89.8(8) 2_665 4_667 ? K1 K1 O10 95.2(6) 4_667 5_557 ? O9 K1 O10 164.9(7) 2_665 5_557 ? K1 K1 O1W 175.8(9) 4_667 . ? O9 K1 O1W 80.0(10) 2_665 . ? N3 K1 O1W 95.4(13) . . ? N3A K1 O1W 101.0(13) 4_667 . ? O10 K1 O1W 86.1(10) 5_557 . ? K1 K1 N3 59.1(8) 4_667 4_667 ? O9 K1 N3 93.2(9) 2_665 4_667 ? O10 K1 N3 89.8(9) 5_557 4_667 ? O1W K1 N3 124.9(12) . 4_667 ? K1 K1 N3A 58.3(8) 4_667 . ? O9 K1 N3A 95.9(7) 2_665 . ? N3A K1 N3A 141.3(5) 4_667 . ? O10 K1 N3A 95.8(8) 5_557 . ? O1W K1 N3A 117.7(12) . . ? K1 K1 O10 50.5(4) 4_667 2_665 ? O9 K1 O10 48.8(6) 2_665 2_665 ? O10 K1 O10 145.7(3) 5_557 2_665 ? O1W K1 O10 128.1(9) . 2_665 ? K1 K1 O9 46.9(4) 4_667 5_557 ? O9 K1 O9 146.1(3) 2_665 5_557 ? O10 K1 O9 48.5(6) 5_557 5_557 ? O1W K1 O9 133.8(9) . 5_557 ? O10 K1 O9 97.3(5) 2_665 5_557 ? K1 K1 C1 75.9(5) 4_667 2_665 ? O9 K1 C1 23.6(6) 2_665 2_665 ? O10 K1 C1 171.1(7) 5_557 2_665 ? O1W K1 C1 102.8(10) . 2_665 ? O10 K1 C1 25.4(5) 2_665 2_665 ? O9 K1 C1 122.7(5) 5_557 2_665 ? K1 K1 C1 71.8(6) 4_667 5_557 ? O9 K1 C1 170.1(7) 2_665 5_557 ? O10 K1 C1 23.3(7) 5_557 5_557 ? O1W K1 C1 109.3(10) . 5_557 ? O10 K1 C1 122.4(6) 2_665 5_557 ? O9 K1 C1 25.2(5) 5_557 5_557 ? C1 K1 C1 147.8(3) 2_665 5_557 ? 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 W1 O5 1.667(9) . ? W1 O4A 1.876(16) . ? W1 O6 1.879(9) 3_675 ? W1 O3 1.904(15) . ? W1 O6 1.905(10) . ? W1 O4 1.991(18) . ? W1 O3A 2.01(2) . ? W1 O2 2.351(14) . ? W1 O1 2.414(13) . ? W2 O8 1.685(9) . ? W2 O3 1.765(15) 6_656 ? W2 O4A 1.781(16) . ? W2 O7A 1.845(17) . ? W2 O7A 1.854(17) 6_656 ? W2 O7 1.987(18) 6_656 ? W2 O7 1.995(18) . ? W2 O4 2.095(19) . ? W2 O3A 2.126(19) 6_656 ? W2 O2 2.394(15) . ? W2 O2 2.403(15) 6_656 ? O9 C1 1.16(3) . ? O9 K1 1.939(14) 3_565 ? O9 K1 2.620(15) 6_557 ? O10 C1 1.16(2) . ? O10 K1 2.028(16) 6_557 ? O10 K1 2.617(18) 3_565 ? O1W K1 2.22(3) . ? OW2 OW2 1.27(3) 4_766 ? N1 C3 1.31(2) . ? N1 N2 1.32(2) . ? N1 C2 1.46(2) . ? N2 N3A 1.26(3) . ? N2 N3 1.58(4) . ? N2 K1 2.98(2) 4_667 ? N2 K1 3.21(2) . ? N3 N4 1.38(4) . ? N3 K1 1.96(3) . ? N3 K1 2.26(3) 4_667 ? N3A N4 1.44(3) . ? N3A K1 2.01(2) 4_667 ? N3A K1 2.35(3) . ? N4 C3 1.20(2) . ? N4 K1 3.05(2) . ? N4 K1 3.11(2) 4_667 ? C1 C2 1.50(2) . ? C1 K1 2.64(2) 3_565 ? C1 K1 2.694(17) 6_557 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9300 . ? O2 Si1 1.650(15) . ? O1 Si1 1.60(2) . ? K1 K1 1.482(7) 4_667 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 W2 O4A W1 131(2) . . . . ? O2 W2 O4A W1 -28(2) . . . . ? O2 W2 O4A W1 -66(3) 6_656 . . . ? O5 W1 O4A W2 -130(2) . . . . ? O6 W1 O4A W2 54(3) 3_675 . . . ? O6 W1 O4A W2 130(3) . . . . ? O2 W1 O4A W2 28(2) . . . . ? O1 W1 O4A W2 65(3) . . . . ? O8 W2 O7A W2 -125.5(18) . . . 5_566 ? O7A W2 O7A W2 55.4(18) 6_656 . . 5_566 ? O2 W2 O7A W2 31.6(16) . . . 5_566 ? O2 W2 O7A W2 74.3(19) 6_656 . . 5_566 ? C3 N1 N2 N3A -14(3) . . . . ? C2 N1 N2 N3A 154(2) . . . . ? C3 N1 N2 N3 23(2) . . . . ? C2 N1 N2 N3 -169.4(18) . . . . ? C3 N1 N2 K1 -17(3) . . . 4_667 ? C2 N1 N2 K1 150.9(17) . . . 4_667 ? C3 N1 N2 K1 21(3) . . . . ? C2 N1 N2 K1 -171.1(12) . . . . ? N1 N2 N3 N4 -30(2) . . . . ? K1 N2 N3 N4 116(2) 4_667 . . . ? K1 N2 N3 N4 147(4) . . . . ? N1 N2 N3 K1 -177(2) . . . . ? K1 N2 N3 K1 -31.2(16) 4_667 . . . ? N1 N2 N3 K1 -146.2(16) . . . 4_667 ? K1 N2 N3 K1 31.2(16) . . . 4_667 ? N1 N2 N3A N4 21(3) . . . . ? K1 N2 N3A N4 -163(5) 4_667 . . . ? K1 N2 N3A N4 -115(3) . . . . ? N1 N2 N3A K1 -176(2) . . . 4_667 ? K1 N2 N3A K1 47.7(18) . . . 4_667 ? N1 N2 N3A K1 136.1(19) . . . . ? K1 N2 N3A K1 -47.7(18) 4_667 . . . ? N2 N3 N4 C3 34(3) . . . . ? K1 N3 N4 C3 -179(2) . . . . ? K1 N3 N4 C3 135(2) 4_667 . . . ? N2 N3 N4 K1 -146(4) . . . . ? K1 N3 N4 K1 -45.2(19) 4_667 . . . ? N2 N3 N4 K1 -101(2) . . . 4_667 ? K1 N3 N4 K1 45.2(19) . . . 4_667 ? N2 N3A N4 C3 -24(3) . . . . ? K1 N3A N4 C3 173(2) 4_667 . . . ? K1 N3A N4 C3 -152(2) . . . . ? N2 N3A N4 K1 128(3) . . . . ? K1 N3A N4 K1 -35.1(16) 4_667 . . . ? N2 N3A N4 K1 163(4) . . . 4_667 ? K1 N3A N4 K1 35.1(16) . . . 4_667 ? K1 O10 C1 O9 6(2) 6_557 . . . ? K1 O10 C1 O9 7.0(16) 3_565 . . . ? K1 O10 C1 C2 -176.5(12) 6_557 . . . ? K1 O10 C1 C2 -175.5(16) 3_565 . . . ? K1 O10 C1 K1 -1.0(8) 6_557 . . 3_565 ? K1 O10 C1 K1 1.0(8) 3_565 . . 6_557 ? K1 O9 C1 O10 -10(2) 3_565 . . . ? K1 O9 C1 O10 -4.4(17) 6_557 . . . ? K1 O9 C1 C2 172.3(12) 3_565 . . . ? K1 O9 C1 C2 178.1(16) 6_557 . . . ? K1 O9 C1 K1 5.9(9) 6_557 . . 3_565 ? K1 O9 C1 K1 -5.9(9) 3_565 . . 6_557 ? C3 N1 C2 C1 83(2) . . . . ? N2 N1 C2 C1 -83(2) . . . . ? O10 C1 C2 N1 27(2) . . . . ? O9 C1 C2 N1 -155.5(18) . . . . ? K1 C1 C2 N1 -138(4) 3_565 . . . ? K1 C1 C2 N1 18(5) 6_557 . . . ? N3 N4 C3 N1 -25(3) . . . . ? N3A N4 C3 N1 16(3) . . . . ? K1 N4 C3 N1 -25(4) . . . . ? K1 N4 C3 N1 22(4) 4_667 . . . ? N2 N1 C3 N4 -3(3) . . . . ? C2 N1 C3 N4 -171.0(19) . . . . ? W1 O1 Si1 O2 -179.8(5) . . . 4_776 ? W1 O1 Si1 O2 -59.8(5) 3_675 . . 4_776 ? W1 O1 Si1 O2 60.2(5) 2_765 . . 4_776 ? W1 O1 Si1 O2 -59.8(5) . . . 5_566 ? W1 O1 Si1 O2 60.2(5) 3_675 . . 5_566 ? W1 O1 Si1 O2 -179.8(5) 2_765 . . 5_566 ? W1 O1 Si1 O2 120.2(5) . . . 2_765 ? W1 O1 Si1 O2 -119.8(5) 3_675 . . 2_765 ? W1 O1 Si1 O2 0.2(5) 2_765 . . 2_765 ? W1 O1 Si1 O2 60.2(5) . . . 6_656 ? W1 O1 Si1 O2 -179.8(5) 3_675 . . 6_656 ? W1 O1 Si1 O2 -59.8(5) 2_765 . . 6_656 ? W1 O1 Si1 O2 -119.8(5) . . . 3_675 ? W1 O1 Si1 O2 0.2(5) 3_675 . . 3_675 ? W1 O1 Si1 O2 120.2(5) 2_765 . . 3_675 ? W1 O1 Si1 O2 0.2(5) . . . . ? W1 O1 Si1 O2 120.2(5) 3_675 . . . ? W1 O1 Si1 O2 -119.8(5) 2_765 . . . ? W1 O2 Si1 O1 -0.2(6) . . . . ? W2 O2 Si1 O1 122.2(8) . . . . ? W2 O2 Si1 O1 -122.2(8) 5_566 . . . ? W1 O2 Si1 O1 179.8(6) . . . 4_776 ? W2 O2 Si1 O1 -57.8(8) . . . 4_776 ? W2 O2 Si1 O1 57.8(8) 5_566 . . 4_776 ? W1 O2 Si1 O2 121.9(8) . . . 5_566 ? W2 O2 Si1 O2 -115.7(13) . . . 5_566 ? W2 O2 Si1 O2 0.0(6) 5_566 . . 5_566 ? W1 O2 Si1 O2 -58.1(8) . . . 2_765 ? W2 O2 Si1 O2 64.3(13) . . . 2_765 ? W2 O2 Si1 O2 -180.0(6) 5_566 . . 2_765 ? W1 O2 Si1 O2 -122.4(8) . . . 6_656 ? W2 O2 Si1 O2 0.0(6) . . . 6_656 ? W2 O2 Si1 O2 115.7(13) 5_566 . . 6_656 ? W1 O2 Si1 O2 57.6(8) . . . 3_675 ? W2 O2 Si1 O2 -180.0(6) . . . 3_675 ? W2 O2 Si1 O2 -64.3(13) 5_566 . . 3_675 ?