#------------------------------------------------------------------------------ #$Date: 2018-08-09 14:59:48 +0300 (Thu, 09 Aug 2018) $ #$Revision: 209502 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/00/40/1004005.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_1004005 loop_ _publ_author_name 'Jin, Song' 'Zhou, Ran' 'Scheuer, Ellen M.' 'Adamchuk, Jennifer' 'Rayburn, Lori L.' 'DiSalvo, Francis J.' _publ_section_title ; Synthesis, Characterization, and Ligand Exchange Studies of W~6~S~8~L~6~ Cluster Compounds ; _journal_issue 12 _journal_name_full 'Inorganic Chemistry' _journal_page_first 2666 _journal_page_last 2674 _journal_paper_doi 10.1021/ic001314q _journal_volume 40 _journal_year 2001 _chemical_formula_moiety 'W6 S8 (C5H9N)6' _chemical_formula_sum 'C54 H78 N6 S8 W6' _chemical_formula_weight 2170.80 _chemical_melting_point ? _chemical_name_common 'Tungsten Sulfide cluster' _chemical_name_systematic ; octakis(\m~3~-sulfido)-hexakis(tert-butylisocyanide)-hexa-tungsten tetrakis(benzene) solvate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 111.5324(11) _cell_angle_beta 110.3392(11) _cell_angle_gamma 93.1387(11) _cell_formula_units_Z 1 _cell_length_a 12.1751(6) _cell_length_b 12.5456(6) _cell_length_c 12.7678(6) _cell_measurement_reflns_used ? _cell_measurement_temperature 173(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 1663.41(14) _computing_cell_refinement 'Bruker SAINT Plus' _computing_data_collection 'BRUKER SMART' _computing_data_reduction SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 18014 _diffrn_reflns_theta_full 26.39 _diffrn_reflns_theta_max 26.39 _diffrn_reflns_theta_min 2.81 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 10.619 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.3644 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ? _exptl_crystal_colour RED _exptl_crystal_density_diffrn 2.167 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description ROD _exptl_crystal_F_000 1016 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 2.277 _refine_diff_density_min -2.039 _refine_diff_density_rms 0.256 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 274 _refine_ls_number_reflns 6799 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.993 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0412 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.0910 _reflns_number_gt 4978 _reflns_number_total 6799 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; Updating space group information. Antanas Vaitkus, 2018-08-09 The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to 'empirical' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 1004005 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.94651(3) -0.07588(3) 0.32710(3) 0.01353(10) Uani 1 1 d . . . W2 W 0.93918(3) 0.13211(3) 0.48498(3) 0.01379(10) Uani 1 1 d . . . W3 W 1.14927(3) 0.06580(3) 0.51048(3) 0.01356(10) Uani 1 1 d . . . S1 S 1.0333(2) 0.1112(2) 0.3388(2) 0.0223(5) Uani 1 1 d . . . S2 S 0.7592(2) -0.0095(2) 0.3189(2) 0.0204(5) Uani 1 1 d . . . S3 S 0.8709(2) -0.2495(2) 0.3460(2) 0.0215(5) Uani 1 1 d . . . S4 S 1.1421(2) -0.1293(2) 0.3651(2) 0.0214(5) Uani 1 1 d . . . C11 C 0.8772(8) -0.1627(8) 0.1308(9) 0.021(2) Uani 1 1 d . . . N1 N 0.8319(7) -0.2104(7) 0.0244(7) 0.0249(19) Uani 1 1 d . . . C12 C 0.7663(9) -0.2639(9) -0.1071(9) 0.027(2) Uani 1 1 d . . . C13 C 0.8428(11) -0.2244(12) -0.1648(11) 0.053(4) Uani 1 1 d . . . H13A H 0.9168 -0.2543 -0.1474 0.079 Uiso 1 1 calc R . . H13B H 0.8627 -0.1386 -0.1302 0.079 Uiso 1 1 calc R . . H13C H 0.7979 -0.2551 -0.2537 0.079 Uiso 1 1 calc R . . C14 C 0.7422(10) -0.3950(9) -0.1485(10) 0.039(3) Uani 1 1 d . . . H14A H 0.6930 -0.4169 -0.1101 0.059 Uiso 1 1 calc R . . H14B H 0.8184 -0.4203 -0.1244 0.059 Uiso 1 1 calc R . . H14C H 0.6997 -0.4330 -0.2379 0.059 Uiso 1 1 calc R . . C15 C 0.6515(10) -0.2193(10) -0.1347(10) 0.046(3) Uani 1 1 d . . . H15A H 0.6027 -0.2453 -0.0981 0.069 Uiso 1 1 calc R . . H15B H 0.6069 -0.2502 -0.2236 0.069 Uiso 1 1 calc R . . H15C H 0.6703 -0.1335 -0.1001 0.069 Uiso 1 1 calc R . . C21 C 0.8689(8) 0.2779(8) 0.4548(8) 0.020(2) Uani 1 1 d . . . N2 N 0.8318(7) 0.3516(7) 0.4294(8) 0.027(2) Uani 1 1 d . . . C22 C 0.7892(8) 0.4351(9) 0.3792(9) 0.026(2) Uani 1 1 d . . . C23 C 0.8077(10) 0.5507(9) 0.4846(10) 0.035(3) Uani 1 1 d . . . H23A H 0.8936 0.5814 0.5344 0.053 Uiso 1 1 calc R . . H23B H 0.7677 0.5390 0.5353 0.053 Uiso 1 1 calc R . . H23C H 0.7738 0.6067 0.4523 0.053 Uiso 1 1 calc R . . C24 C 0.8564(10) 0.4444(10) 0.3028(11) 0.038(3) Uani 1 1 d . . . H24A H 0.9416 0.4767 0.3555 0.056 Uiso 1 1 calc R . . H24B H 0.8245 0.4961 0.2631 0.056 Uiso 1 1 calc R . . H24C H 0.8470 0.3664 0.2401 0.056 Uiso 1 1 calc R . . C25 C 0.6564(9) 0.3859(10) 0.2995(10) 0.037(3) Uani 1 1 d . . . H25A H 0.6462 0.3109 0.2321 0.056 Uiso 1 1 calc R . . H25B H 0.6225 0.4412 0.2661 0.056 Uiso 1 1 calc R . . H25C H 0.6151 0.3739 0.3492 0.056 Uiso 1 1 calc R . . C31 C 1.3189(8) 0.1460(8) 0.5240(8) 0.022(2) Uani 1 1 d . . . N3 N 1.4077(6) 0.1902(7) 0.5336(8) 0.0241(19) Uani 1 1 d . . . C32 C 1.5213(8) 0.2496(8) 0.5475(9) 0.024(2) Uani 1 1 d . . . C33 C 1.5592(9) 0.1671(9) 0.4538(10) 0.035(3) Uani 1 1 d . . . H33A H 1.5722 0.0974 0.4701 0.053 Uiso 1 1 calc R . . H33B H 1.6337 0.2061 0.4582 0.053 Uiso 1 1 calc R . . H33C H 1.4964 0.1440 0.3718 0.053 Uiso 1 1 calc R . . C34 C 1.6099(9) 0.2811(11) 0.6743(11) 0.043(3) Uani 1 1 d . . . H34A H 1.6236 0.2095 0.6866 0.065 Uiso 1 1 calc R . . H34B H 1.5791 0.3292 0.7333 0.065 Uiso 1 1 calc R . . H34C H 1.6856 0.3254 0.6867 0.065 Uiso 1 1 calc R . . C35 C 1.5009(10) 0.3594(10) 0.5278(10) 0.039(3) Uani 1 1 d . . . H35A H 1.4759 0.4108 0.5904 0.058 Uiso 1 1 calc R . . H35B H 1.4381 0.3387 0.4463 0.058 Uiso 1 1 calc R . . H35C H 1.5753 0.4001 0.5338 0.058 Uiso 1 1 calc R . . C1S C 1.8102(16) 0.0920(15) 0.9315(17) 0.089(5) Uiso 1 1 d . . . H1SA H 1.8802 0.0828 0.9148 0.107 Uiso 1 1 calc R . . C2S C 1.8089(17) 0.1075(15) 1.0384(17) 0.091(6) Uiso 1 1 d . . . H2SA H 1.8843 0.1208 1.1026 0.110 Uiso 1 1 calc R . . C3S C 1.7168(14) 0.1068(13) 1.0659(15) 0.076(5) Uiso 1 1 d . . . H3SA H 1.7242 0.1120 1.1442 0.091 Uiso 1 1 calc R . . C4S C 1.5963(14) 0.0975(13) 0.9699(14) 0.068(4) Uiso 1 1 d . . . H4SA H 1.5249 0.0972 0.9844 0.082 Uiso 1 1 calc R . . C5S C 1.5981(11) 0.0894(10) 0.8589(11) 0.044(3) Uiso 1 1 d . . . H5SA H 1.5269 0.0836 0.7933 0.053 Uiso 1 1 calc R . . C6S C 1.7057(13) 0.0900(12) 0.8473(14) 0.064(4) Uiso 1 1 d . . . H6SA H 1.7065 0.0889 0.7728 0.077 Uiso 1 1 calc R . . C7S C 1.0614(9) -0.3865(10) 0.0724(10) 0.035(3) Uiso 1 1 d . . . H7SA H 1.1040 -0.3078 0.1227 0.052 Uiso 1 1 calc R . . C8S C 0.9914(9) -0.4408(10) 0.1094(10) 0.036(3) Uiso 1 1 d . . . H8SA H 0.9854 -0.3996 0.1855 0.043 Uiso 1 1 calc R . . C9S C 0.9299(10) -0.5544(10) 0.0373(10) 0.036(3) Uiso 1 1 d . . . H9SA H 0.8815 -0.5919 0.0635 0.053 Uiso 1 1 calc R . . C10S C 0.5506(11) -0.3837(11) 0.0717(11) 0.047(3) Uiso 1 1 d . . . H10A H 0.5854 -0.3028 0.1209 0.071 Uiso 1 1 calc R . . C11S C 0.6228(11) -0.4650(10) 0.0601(11) 0.043(3) Uiso 1 1 d . . . H11A H 0.7074 -0.4406 0.1022 0.051 Uiso 1 1 calc R . . C12S C 0.5722(10) -0.5794(11) -0.0114(11) 0.043(3) Uiso 1 1 d . . . H12A H 0.6218 -0.6352 -0.0203 0.064 Uiso 1 1 calc R . . 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 0.01222(18) 0.0150(2) 0.01235(19) 0.00511(15) 0.00424(14) 0.00334(14) W2 0.01264(18) 0.0134(2) 0.01627(19) 0.00730(15) 0.00524(15) 0.00485(14) W3 0.00963(18) 0.0156(2) 0.01595(19) 0.00708(15) 0.00502(14) 0.00223(14) S1 0.0257(13) 0.0233(13) 0.0206(13) 0.0123(11) 0.0094(10) 0.0015(10) S2 0.0157(12) 0.0249(13) 0.0188(12) 0.0105(11) 0.0032(10) 0.0052(10) S3 0.0235(13) 0.0124(12) 0.0224(13) 0.0042(10) 0.0057(10) -0.0008(10) S4 0.0204(12) 0.0249(14) 0.0206(13) 0.0066(11) 0.0123(10) 0.0089(10) C11 0.024(5) 0.020(5) 0.019(5) 0.008(4) 0.008(4) 0.008(4) N1 0.022(4) 0.024(5) 0.022(5) 0.004(4) 0.007(4) 0.009(4) C12 0.026(5) 0.027(6) 0.014(5) -0.004(4) 0.006(4) 0.000(4) C13 0.054(8) 0.059(9) 0.028(7) 0.009(6) 0.008(6) 0.001(7) C14 0.044(7) 0.031(7) 0.023(6) -0.002(5) 0.005(5) 0.000(5) C15 0.041(7) 0.042(8) 0.030(7) 0.006(6) -0.004(5) 0.006(6) C21 0.022(5) 0.013(5) 0.022(5) 0.007(4) 0.007(4) -0.002(4) N2 0.020(4) 0.022(5) 0.045(6) 0.021(4) 0.012(4) 0.007(4) C22 0.021(5) 0.032(6) 0.035(6) 0.023(5) 0.012(5) 0.008(4) C23 0.038(6) 0.025(6) 0.053(7) 0.020(6) 0.023(6) 0.019(5) C24 0.038(6) 0.038(7) 0.047(7) 0.021(6) 0.025(6) 0.010(5) C25 0.033(6) 0.042(7) 0.039(7) 0.022(6) 0.011(5) 0.012(5) C31 0.023(5) 0.029(6) 0.018(5) 0.015(4) 0.006(4) 0.004(4) N3 0.007(4) 0.029(5) 0.036(5) 0.014(4) 0.008(4) 0.000(3) C32 0.011(5) 0.023(5) 0.035(6) 0.013(5) 0.005(4) -0.002(4) C33 0.028(6) 0.033(7) 0.043(7) 0.014(6) 0.012(5) 0.011(5) C34 0.028(6) 0.051(8) 0.046(7) 0.023(6) 0.007(5) 0.002(6) C35 0.039(7) 0.048(8) 0.032(6) 0.018(6) 0.015(5) 0.010(6) 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' S S 0.1246 0.1234 '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' 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 C11 W1 S4 96.4(2) . . ? C11 W1 S3 92.7(3) . . ? S4 W1 S3 89.65(8) . . ? C11 W1 S1 95.1(3) . . ? S4 W1 S1 89.37(8) . . ? S3 W1 S1 172.16(8) . . ? C11 W1 S2 91.2(2) . . ? S4 W1 S2 172.32(8) . . ? S3 W1 S2 89.69(8) . . ? S1 W1 S2 90.25(8) . . ? C11 W1 W2 133.9(3) . . ? S4 W1 W2 116.80(6) . . ? S3 W1 W2 116.91(6) . . ? S1 W1 W2 56.98(6) . . ? S2 W1 W2 57.01(6) . . ? C11 W1 W3 132.4(2) . 2_756 ? S4 W1 W3 116.77(6) . 2_756 ? S3 W1 W3 56.92(6) . 2_756 ? S1 W1 W3 116.95(6) . 2_756 ? S2 W1 W3 56.88(6) . 2_756 ? W2 W1 W3 60.040(14) . 2_756 ? C11 W1 W3 137.6(3) . . ? S4 W1 W3 56.77(6) . . ? S3 W1 W3 116.67(6) . . ? S1 W1 W3 56.68(6) . . ? S2 W1 W3 117.04(6) . . ? W2 W1 W3 60.082(13) . . ? W3 W1 W3 89.953(15) 2_756 . ? C11 W1 W2 135.9(3) . 2_756 ? S4 W1 W2 56.85(6) . 2_756 ? S3 W1 W2 56.79(6) . 2_756 ? S1 W1 W2 116.56(6) . 2_756 ? S2 W1 W2 116.80(6) . 2_756 ? W2 W1 W2 90.057(16) . 2_756 ? W3 W1 W2 59.968(14) 2_756 2_756 ? W3 W1 W2 59.922(14) . 2_756 ? C21 W2 S3 96.2(2) . 2_756 ? C21 W2 S4 97.7(3) . 2_756 ? S3 W2 S4 89.32(8) 2_756 2_756 ? C21 W2 S1 90.6(3) . . ? S3 W2 S1 89.66(8) 2_756 . ? S4 W2 S1 171.73(8) 2_756 . ? C21 W2 S2 91.9(2) . . ? S3 W2 S2 171.98(8) 2_756 . ? S4 W2 S2 89.78(8) 2_756 . ? S1 W2 S2 90.09(8) . . ? C21 W2 W1 131.0(2) . . ? S3 W2 W1 116.77(6) 2_756 . ? S4 W2 W1 116.63(6) 2_756 . ? S1 W2 W1 56.87(6) . . ? S2 W2 W1 56.87(6) . . ? C21 W2 W3 135.9(2) . 2_756 ? S3 W2 W3 116.45(6) 2_756 2_756 ? S4 W2 W3 56.68(6) 2_756 2_756 ? S1 W2 W3 116.82(6) . 2_756 ? S2 W2 W3 56.83(6) . 2_756 ? W1 W2 W3 60.020(14) . 2_756 ? C21 W2 W3 133.9(2) . . ? S3 W2 W3 56.82(6) 2_756 . ? S4 W2 W3 116.38(6) 2_756 . ? S1 W2 W3 56.62(6) . . ? S2 W2 W3 116.82(6) . . ? W1 W2 W3 60.003(13) . . ? W3 W2 W3 89.896(15) 2_756 . ? C21 W2 W1 139.0(2) . 2_756 ? S3 W2 W1 56.58(6) 2_756 2_756 ? S4 W2 W1 56.55(6) 2_756 2_756 ? S1 W2 W1 116.46(6) . 2_756 ? S2 W2 W1 116.69(6) . 2_756 ? W1 W2 W1 89.943(16) . 2_756 ? W3 W2 W1 59.909(14) 2_756 2_756 ? W3 W2 W1 59.882(13) . 2_756 ? C31 W3 S4 95.5(3) . . ? C31 W3 S1 93.0(3) . . ? S4 W3 S1 89.51(8) . . ? C31 W3 S3 92.6(3) . 2_756 ? S4 W3 S3 171.95(8) . 2_756 ? S1 W3 S3 89.88(8) . 2_756 ? C31 W3 S2 94.4(3) . 2_756 ? S4 W3 S2 90.04(8) . 2_756 ? S1 W3 S2 172.67(8) . 2_756 ? S3 W3 S2 89.54(8) 2_756 2_756 ? C31 W3 W1 134.4(2) . 2_756 ? S4 W3 W1 116.81(6) . 2_756 ? S1 W3 W1 117.09(6) . 2_756 ? S3 W3 W1 56.68(6) 2_756 2_756 ? S2 W3 W1 56.88(6) 2_756 2_756 ? C31 W3 W1 135.5(2) . . ? S4 W3 W1 56.72(6) . . ? S1 W3 W1 56.95(6) . . ? S3 W3 W1 116.65(6) 2_756 . ? S2 W3 W1 117.10(6) 2_756 . ? W1 W3 W1 90.048(15) 2_756 . ? C31 W3 W2 136.5(3) . 2_756 ? S4 W3 W2 56.93(6) . 2_756 ? S1 W3 W2 117.08(6) . 2_756 ? S3 W3 W2 116.56(6) 2_756 2_756 ? S2 W3 W2 56.98(6) 2_756 2_756 ? W1 W3 W2 59.939(13) 2_756 2_756 ? W1 W3 W2 60.171(14) . 2_756 ? C31 W3 W2 133.4(3) . . ? S4 W3 W2 116.59(6) . . ? S1 W3 W2 56.99(6) . . ? S3 W3 W2 56.80(6) 2_756 . ? S2 W3 W2 116.99(6) 2_756 . ? W1 W3 W2 60.151(14) 2_756 . ? W1 W3 W2 59.915(13) . . ? W2 W3 W2 90.105(15) 2_756 . ? W3 S1 W1 66.37(7) . . ? W3 S1 W2 66.39(6) . . ? W1 S1 W2 66.15(6) . . ? W3 S2 W1 66.24(6) 2_756 . ? W3 S2 W2 66.19(6) 2_756 . ? W1 S2 W2 66.11(6) . . ? W1 S3 W2 66.62(6) . 2_756 ? W1 S3 W3 66.41(6) . 2_756 ? W2 S3 W3 66.38(6) 2_756 2_756 ? W1 S4 W3 66.51(6) . . ? W1 S4 W2 66.60(6) . 2_756 ? W3 S4 W2 66.39(6) . 2_756 ? N1 C11 W1 175.3(8) . . ? C11 N1 C12 174.5(9) . . ? N1 C12 C14 108.2(9) . . ? N1 C12 C15 107.3(8) . . ? C14 C12 C15 111.6(9) . . ? N1 C12 C13 107.8(8) . . ? C14 C12 C13 111.8(9) . . ? C15 C12 C13 109.8(10) . . ? N2 C21 W2 174.4(9) . . ? C21 N2 C22 170.3(11) . . ? N2 C22 C24 108.4(8) . . ? N2 C22 C23 108.2(9) . . ? C24 C22 C23 112.5(9) . . ? N2 C22 C25 106.4(8) . . ? C24 C22 C25 110.5(9) . . ? C23 C22 C25 110.6(8) . . ? N3 C31 W3 178.3(9) . . ? C31 N3 C32 178.6(10) . . ? N3 C32 C34 108.5(9) . . ? N3 C32 C33 107.5(8) . . ? C34 C32 C33 111.6(9) . . ? N3 C32 C35 107.5(8) . . ? C34 C32 C35 109.7(9) . . ? C33 C32 C35 111.9(9) . . ? C2S C1S C6S 115.2(18) . . ? C3S C2S C1S 127(2) . . ? C2S C3S C4S 118.3(17) . . ? C5S C4S C3S 114.9(14) . . ? C6S C5S C4S 117.9(13) . . ? C1S C6S C5S 126.0(16) . . ? C8S C7S C9S 119.9(11) . 2_745 ? C7S C8S C9S 120.4(11) . . ? C7S C9S C8S 119.7(11) 2_745 . ? C12S C10S C11S 119.6(12) 2_645 . ? C12S C11S C10S 119.5(12) . . ? C11S C12S C10S 120.8(12) . 2_645 ? 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 C11 2.146(9) . ? W1 S4 2.443(2) . ? W1 S3 2.443(2) . ? W1 S1 2.452(2) . ? W1 S2 2.452(2) . ? W1 W2 2.6776(5) . ? W1 W3 2.6798(5) 2_756 ? W1 W3 2.6799(5) . ? W1 W2 2.6870(5) 2_756 ? W2 C21 2.165(10) . ? W2 S3 2.449(2) 2_756 ? W2 S4 2.451(2) 2_756 ? W2 S1 2.455(2) . ? W2 S2 2.456(2) . ? W2 W3 2.6803(5) 2_756 ? W2 W3 2.6821(5) . ? W2 W1 2.6870(5) 2_756 ? W3 C31 2.169(9) . ? W3 S4 2.444(2) . ? W3 S1 2.444(3) . ? W3 S3 2.450(2) 2_756 ? W3 S2 2.452(2) 2_756 ? W3 W1 2.6798(5) 2_756 ? W3 W2 2.6803(5) 2_756 ? S2 W3 2.452(2) 2_756 ? S3 W2 2.449(2) 2_756 ? S3 W3 2.450(2) 2_756 ? S4 W2 2.451(2) 2_756 ? C11 N1 1.163(11) . ? N1 C12 1.446(12) . ? C12 C14 1.507(14) . ? C12 C15 1.510(15) . ? C12 C13 1.533(15) . ? C21 N2 1.153(12) . ? N2 C22 1.448(12) . ? C22 C24 1.504(14) . ? C22 C23 1.512(14) . ? C22 C25 1.522(13) . ? C31 N3 1.133(11) . ? N3 C32 1.455(11) . ? C32 C34 1.488(14) . ? C32 C33 1.497(14) . ? C32 C35 1.507(14) . ? C1S C2S 1.31(2) . ? C1S C6S 1.34(2) . ? C2S C3S 1.29(2) . ? C3S C4S 1.51(2) . ? C4S C5S 1.391(19) . ? C5S C6S 1.369(17) . ? C7S C8S 1.366(15) . ? C7S C9S 1.368(15) 2_745 ? C8S C9S 1.371(15) . ? C9S C7S 1.368(15) 2_745 ? C10S C12S 1.381(16) 2_645 ? C10S C11S 1.383(16) . ? C11S C12S 1.350(15) . ? C12S C10S 1.381(16) 2_645 ?