# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2^.^0.5H~2~O _database_code_depnum_ccdc_archive 'CCDC 928965' #TrackingRef 'ZhangZY.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H22 B Cl4 Cu3 Mo N6 S3, 2(C8 H20 N),0.5(H2 O)' _chemical_formula_sum 'C31 H63 B Cl4 Cu3 Mo N8 O0.50 S3' _chemical_formula_weight 1091.24 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'tetragonal ' _symmetry_space_group_name_H-M 'I 4' _symmetry_space_group_name_HALL 'I 4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 27.8478(9) _cell_length_b 27.8478(9) _cell_length_c 11.9710(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9283.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 2144 _cell_measurement_theta_min 3.1325 _cell_measurement_theta_max 29.3314 _exptl_crystal_description Prism _exptl_crystal_colour Dark-green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4472 _exptl_absorpt_coefficient_mu 2.019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82235 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_detector_area_resol_mean 10.4692 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10135 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.1408 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6354 _reflns_number_gt 4299 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. As the solvent molecule is likely to evaporate, the diffraction is weak in high angles. Thus the reflections at 2theta > 50 \% were omitted. The CH~2~-CH~3~ bond lengths of the ethyl groups in the Et~4~N^+^ cation (N8-C24-C31) were fixed to be the same, while the C atoms (C24~C31) were refined to have the same anisotropic displacement parameters. Atom C12 was refined to be approximate isotropic. During the solvated water molecule, the O atom of was refined isotropically, while the H atoms were not located. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 6354 _refine_ls_number_parameters 434 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.75400(4) 0.01748(4) 0.92765(9) 0.0256(3) Uani 1 1 d . . . S1 S 0.73204(14) -0.02444(13) 0.7686(3) 0.0381(9) Uani 1 1 d . . . S2 S 0.79214(13) 0.08435(12) 0.8607(3) 0.0313(8) Uani 1 1 d . . . S3 S 0.68318(14) 0.04647(13) 0.9973(3) 0.0368(9) Uani 1 1 d . . . Cu1 Cu 0.75550(7) 0.04945(6) 0.71536(13) 0.0387(5) Uani 1 1 d . . . Cu2 Cu 0.71587(6) 0.10531(6) 0.89340(13) 0.0388(5) Uani 1 1 d . . . Cu3 Cu 0.66791(7) 0.01731(7) 0.82699(16) 0.0450(5) Uani 1 1 d . . . Cl1 Cl 0.78486(17) 0.06539(16) 0.5480(3) 0.0597(12) Uani 1 1 d . . . Cl2 Cl 0.69620(14) 0.18169(12) 0.9224(3) 0.0483(9) Uani 1 1 d . . . Cl3 Cl 0.59322(17) -0.0019(2) 0.7920(4) 0.0793(16) Uani 1 1 d . . . Cl4 Cl 0.67510(15) 0.09472(14) 0.7008(3) 0.0504(10) Uani 1 1 d . . . B1 B 0.8230(6) -0.0486(6) 1.1142(12) 0.028(4) Uani 1 1 d . . . H1 H 0.847(5) -0.059(4) 1.159(11) 0.034 Uiso 1 1 d . . . N1 N 0.8288(4) -0.0209(4) 0.9109(9) 0.034(3) Uani 1 1 d . . . N2 N 0.8487(4) -0.0453(4) 0.9977(9) 0.032(3) Uani 1 1 d . . . N3 N 0.7873(4) 0.0365(4) 1.1009(9) 0.036(3) Uani 1 1 d . . . N4 N 0.8151(4) 0.0028(4) 1.1569(8) 0.032(3) Uani 1 1 d . . . N5 N 0.7383(4) -0.0533(4) 1.0295(9) 0.033(3) Uani 1 1 d . . . N6 N 0.7736(4) -0.0720(4) 1.0976(9) 0.034(3) Uani 1 1 d . . . N7 N 0.7812(4) -0.1739(4) 0.6995(10) 0.040(3) Uani 1 1 d . . . N8 N 0.6350(5) -0.0166(5) 1.4144(13) 0.067(4) Uani 1 1 d . . . C1 C 0.8612(5) -0.0247(5) 0.8272(11) 0.042(4) Uani 1 1 d . . . C2 C 0.9003(5) -0.0506(5) 0.8616(11) 0.041(4) Uani 1 1 d . . . H2 H 0.9279 -0.0577 0.8193 0.049 Uiso 1 1 calc R . . C3 C 0.8915(5) -0.0641(5) 0.9700(12) 0.044(4) Uani 1 1 d . . . C4 C 0.8566(5) -0.0021(5) 0.7134(11) 0.043(4) Uani 1 1 d . . . H4A H 0.8300 -0.0167 0.6737 0.065 Uiso 1 1 calc R . . H4B H 0.8860 -0.0072 0.6716 0.065 Uiso 1 1 calc R . . H4C H 0.8508 0.0320 0.7215 0.065 Uiso 1 1 calc R . . C5 C 0.9235(6) -0.0911(6) 1.0480(16) 0.064(5) Uani 1 1 d . . . H5A H 0.9377 -0.0689 1.1011 0.097 Uiso 1 1 calc R . . H5B H 0.9488 -0.1068 1.0058 0.097 Uiso 1 1 calc R . . H5C H 0.9049 -0.1150 1.0878 0.097 Uiso 1 1 calc R . . C6 C 0.7857(5) 0.0763(5) 1.1669(11) 0.035(4) Uani 1 1 d . . . C7 C 0.8116(5) 0.0675(5) 1.2613(11) 0.037(4) Uani 1 1 d . . . H7 H 0.8156 0.0887 1.3216 0.045 Uiso 1 1 calc R . . C8 C 0.8304(5) 0.0233(6) 1.2536(11) 0.040(4) Uani 1 1 d . . . C9 C 0.7595(6) 0.1209(5) 1.1414(12) 0.042(4) Uani 1 1 d . . . H9A H 0.7694 0.1328 1.0688 0.063 Uiso 1 1 calc R . . H9B H 0.7667 0.1448 1.1980 0.063 Uiso 1 1 calc R . . H9C H 0.7253 0.1145 1.1408 0.063 Uiso 1 1 calc R . . C10 C 0.8598(6) -0.0043(6) 1.3378(12) 0.061(5) Uani 1 1 d . . . H10A H 0.8567 0.0106 1.4106 0.091 Uiso 1 1 calc R . . H10B H 0.8933 -0.0041 1.3153 0.091 Uiso 1 1 calc R . . H10C H 0.8484 -0.0372 1.3414 0.091 Uiso 1 1 calc R . . C11 C 0.6995(5) -0.0798(5) 1.0457(12) 0.037(4) Uani 1 1 d . . . C12 C 0.7104(6) -0.1158(6) 1.1247(12) 0.045(4) Uani 1 1 d U . . H12 H 0.6896 -0.1399 1.1505 0.054 Uiso 1 1 calc R . . C13 C 0.7567(6) -0.1088(5) 1.1566(12) 0.042(4) Uani 1 1 d . . . C14 C 0.6530(5) -0.0724(5) 0.9858(14) 0.051(4) Uani 1 1 d . . . H14A H 0.6373 -0.0438 1.0145 0.076 Uiso 1 1 calc R . . H14B H 0.6324 -0.1000 0.9974 0.076 Uiso 1 1 calc R . . H14C H 0.6591 -0.0685 0.9065 0.076 Uiso 1 1 calc R . . C15 C 0.7850(6) -0.1384(6) 1.2361(13) 0.057(5) Uani 1 1 d . . . H15A H 0.8161 -0.1456 1.2037 0.086 Uiso 1 1 calc R . . H15B H 0.7680 -0.1680 1.2514 0.086 Uiso 1 1 calc R . . H15C H 0.7894 -0.1207 1.3052 0.086 Uiso 1 1 calc R . . C16 C 0.7775(7) -0.1397(7) 0.6024(17) 0.074(6) Uani 1 1 d . . . H16A H 0.7597 -0.1553 0.5419 0.089 Uiso 1 1 calc R . . H16B H 0.7591 -0.1115 0.6259 0.089 Uiso 1 1 calc R . . C17 C 0.8252(7) -0.1232(6) 0.5579(16) 0.075(6) Uani 1 1 d . . . H17A H 0.8214 -0.0925 0.5206 0.113 Uiso 1 1 calc R . . H17B H 0.8374 -0.1467 0.5051 0.113 Uiso 1 1 calc R . . H17C H 0.8478 -0.1198 0.6192 0.113 Uiso 1 1 calc R . . C18 C 0.8017(5) -0.1474(5) 0.8046(13) 0.041(4) Uani 1 1 d . . . H18A H 0.8359 -0.1415 0.7914 0.050 Uiso 1 1 calc R . . H18B H 0.7860 -0.1159 0.8088 0.050 Uiso 1 1 calc R . . C19 C 0.7971(6) -0.1696(6) 0.9110(14) 0.068(5) Uani 1 1 d . . . H19A H 0.7634 -0.1756 0.9265 0.102 Uiso 1 1 calc R . . H19B H 0.8102 -0.1486 0.9679 0.102 Uiso 1 1 calc R . . H19C H 0.8145 -0.1998 0.9110 0.102 Uiso 1 1 calc R . . C20 C 0.7300(6) -0.1914(8) 0.7288(16) 0.078(6) Uani 1 1 d . . . H20A H 0.7172 -0.2083 0.6636 0.093 Uiso 1 1 calc R . . H20B H 0.7327 -0.2148 0.7895 0.093 Uiso 1 1 calc R . . C21 C 0.6956(7) -0.1559(8) 0.7616(19) 0.098(8) Uani 1 1 d . . . H21A H 0.7122 -0.1277 0.7894 0.147 Uiso 1 1 calc R . . H21B H 0.6752 -0.1688 0.8200 0.147 Uiso 1 1 calc R . . H21C H 0.6761 -0.1471 0.6978 0.147 Uiso 1 1 calc R . . C22 C 0.8116(6) -0.2162(5) 0.6780(12) 0.046(4) Uani 1 1 d . . . H22A H 0.8105 -0.2369 0.7443 0.055 Uiso 1 1 calc R . . H22B H 0.8448 -0.2052 0.6693 0.055 Uiso 1 1 calc R . . C23 C 0.7985(6) -0.2469(6) 0.5757(14) 0.060(5) Uani 1 1 d . . . H23A H 0.7686 -0.2636 0.5896 0.090 Uiso 1 1 calc R . . H23B H 0.8238 -0.2701 0.5620 0.090 Uiso 1 1 calc R . . H23C H 0.7950 -0.2263 0.5109 0.090 Uiso 1 1 calc R . . C24 C 0.6862(9) -0.0048(10) 1.433(3) 0.138(4) Uiso 1 1 d D . . H24A H 0.6924 -0.0071 1.5136 0.165 Uiso 1 1 calc R . . H24B H 0.6911 0.0288 1.4116 0.165 Uiso 1 1 calc R . . C25 C 0.7230(9) -0.0343(10) 1.374(2) 0.138(4) Uiso 1 1 d D . . H25A H 0.7232 -0.0665 1.4056 0.207 Uiso 1 1 calc R . . H25B H 0.7543 -0.0198 1.3841 0.207 Uiso 1 1 calc R . . H25C H 0.7153 -0.0359 1.2955 0.207 Uiso 1 1 calc R . . C26 C 0.6272(10) -0.0693(10) 1.440(2) 0.138(4) Uiso 1 1 d D . . H26A H 0.5936 -0.0769 1.4228 0.165 Uiso 1 1 calc R . . H26B H 0.6471 -0.0879 1.3879 0.165 Uiso 1 1 calc R . . C27 C 0.6376(10) -0.0870(10) 1.556(2) 0.138(4) Uiso 1 1 d D . . H27A H 0.6703 -0.0788 1.5764 0.207 Uiso 1 1 calc R . . H27B H 0.6336 -0.1216 1.5588 0.207 Uiso 1 1 calc R . . H27C H 0.6156 -0.0721 1.6084 0.207 Uiso 1 1 calc R . . C28 C 0.6066(9) 0.0120(11) 1.497(3) 0.138(4) Uiso 1 1 d D . . H28A H 0.6132 0.0463 1.4860 0.165 Uiso 1 1 calc R . . H28B H 0.6172 0.0036 1.5730 0.165 Uiso 1 1 calc R . . C29 C 0.5535(9) 0.0036(10) 1.488(2) 0.138(4) Uiso 1 1 d D . . H29A H 0.5422 0.0152 1.4165 0.207 Uiso 1 1 calc R . . H29B H 0.5371 0.0207 1.5476 0.207 Uiso 1 1 calc R . . H29C H 0.5469 -0.0305 1.4945 0.207 Uiso 1 1 calc R . . C30 C 0.6168(11) -0.0128(9) 1.288(2) 0.138(4) Uiso 1 1 d D . . H30A H 0.6350 -0.0342 1.2388 0.165 Uiso 1 1 calc R . . H30B H 0.5825 -0.0206 1.2818 0.165 Uiso 1 1 calc R . . C31 C 0.6260(10) 0.0397(9) 1.258(2) 0.138(4) Uiso 1 1 d D . . H31A H 0.6419 0.0416 1.1864 0.207 Uiso 1 1 calc R . . H31B H 0.6463 0.0541 1.3151 0.207 Uiso 1 1 calc R . . H31C H 0.5957 0.0568 1.2551 0.207 Uiso 1 1 calc R . . O1 O 1.0000 0.0000 0.6509(12) 0.021(4) Uiso 1 4 d S . . O2 O 1.0000 0.0000 0.2956(13) 0.028(4) Uiso 1 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 Mo1 0.0298(6) 0.0280(6) 0.0192(5) 0.0006(6) 0.0027(5) -0.0019(6) S1 0.049(2) 0.034(2) 0.0310(18) -0.0039(17) -0.0020(17) -0.0001(19) S2 0.039(2) 0.0313(19) 0.0240(17) 0.0004(15) 0.0029(15) -0.0025(17) S3 0.040(2) 0.038(2) 0.0321(19) 0.0005(17) 0.0040(17) -0.0005(19) Cu1 0.0544(12) 0.0410(11) 0.0206(8) -0.0004(8) 0.0023(8) -0.0011(10) Cu2 0.0468(11) 0.0335(10) 0.0362(10) -0.0015(8) 0.0062(8) 0.0032(9) Cu3 0.0391(11) 0.0538(13) 0.0423(10) -0.0045(9) -0.0045(9) -0.0034(11) Cl1 0.087(3) 0.074(3) 0.0188(17) 0.004(2) 0.008(2) 0.005(3) Cl2 0.063(2) 0.0353(19) 0.046(2) -0.002(2) 0.010(2) 0.0124(18) Cl3 0.057(3) 0.105(4) 0.076(3) 0.013(3) -0.021(3) -0.023(3) Cl4 0.063(3) 0.049(2) 0.039(2) 0.0038(19) -0.010(2) 0.015(2) B1 0.034(9) 0.029(9) 0.022(8) 0.008(7) 0.000(7) -0.004(8) N1 0.033(6) 0.045(7) 0.025(6) 0.005(5) 0.015(5) 0.004(6) N2 0.039(7) 0.028(7) 0.029(6) 0.007(5) -0.006(5) -0.004(6) N3 0.039(7) 0.032(7) 0.036(7) -0.003(6) -0.010(6) 0.000(6) N4 0.043(7) 0.034(7) 0.020(6) 0.003(5) -0.009(5) 0.006(6) N5 0.045(8) 0.030(7) 0.025(6) 0.006(5) -0.007(6) -0.009(6) N6 0.037(7) 0.033(7) 0.030(6) 0.005(6) 0.010(6) -0.002(6) N7 0.035(7) 0.047(8) 0.037(7) -0.005(6) -0.016(6) 0.003(6) N8 0.071(10) 0.051(9) 0.080(11) -0.015(8) -0.006(9) 0.019(8) C1 0.051(10) 0.049(10) 0.026(7) -0.002(7) 0.002(7) 0.009(9) C2 0.043(9) 0.055(10) 0.025(8) -0.005(7) 0.017(7) 0.010(8) C3 0.037(9) 0.038(9) 0.057(10) -0.003(7) 0.006(7) 0.031(8) C4 0.039(9) 0.067(11) 0.024(7) 0.000(8) 0.011(7) 0.024(8) C5 0.062(12) 0.059(12) 0.073(12) 0.002(10) -0.003(10) 0.036(10) C6 0.041(9) 0.044(9) 0.021(7) -0.016(7) 0.002(6) 0.007(8) C7 0.054(10) 0.041(9) 0.018(7) -0.005(7) 0.001(7) 0.000(8) C8 0.035(9) 0.064(11) 0.022(7) -0.011(7) 0.005(6) 0.002(8) C9 0.067(11) 0.030(8) 0.029(7) 0.007(7) 0.010(7) 0.006(8) C10 0.058(11) 0.086(13) 0.038(9) 0.021(9) -0.031(8) -0.002(10) C11 0.034(9) 0.041(9) 0.037(8) 0.001(7) 0.013(7) -0.021(8) C12 0.050(8) 0.047(7) 0.038(7) 0.014(6) 0.011(6) -0.016(7) C13 0.059(11) 0.035(9) 0.032(8) -0.002(7) 0.009(8) 0.007(8) C14 0.047(10) 0.035(9) 0.069(11) 0.006(8) -0.007(8) -0.007(8) C15 0.070(12) 0.045(10) 0.056(11) 0.035(8) 0.018(9) 0.008(9) C16 0.080(15) 0.053(12) 0.090(15) 0.000(11) -0.046(12) 0.003(11) C17 0.097(16) 0.059(13) 0.070(12) 0.020(10) -0.017(12) -0.024(12) C18 0.032(8) 0.041(9) 0.051(10) -0.004(7) -0.016(7) 0.012(8) C19 0.079(13) 0.072(12) 0.052(11) -0.020(10) 0.000(10) 0.023(10) C20 0.045(11) 0.120(17) 0.068(13) -0.047(12) -0.013(9) -0.008(12) C21 0.065(14) 0.12(2) 0.109(18) -0.058(16) 0.002(12) 0.008(14) C22 0.054(11) 0.036(9) 0.049(10) -0.001(7) -0.008(8) -0.007(8) C23 0.077(13) 0.043(10) 0.061(11) -0.016(9) -0.014(9) 0.009(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 Mo1 S3 2.288(4) . ? Mo1 S2 2.289(4) . ? Mo1 S1 2.315(4) . ? Mo1 N3 2.332(11) . ? Mo1 N1 2.350(10) . ? Mo1 N5 2.358(11) . ? Mo1 Cu3 2.683(2) . ? Mo1 Cu1 2.693(2) . ? Mo1 Cu2 2.698(2) . ? S1 Cu3 2.242(4) . ? S1 Cu1 2.251(4) . ? S2 Cu2 2.237(4) . ? S2 Cu1 2.239(4) . ? S3 Cu3 2.235(4) . ? S3 Cu2 2.250(4) . ? Cu1 Cl1 2.209(4) . ? Cu1 Cl4 2.575(4) . ? Cu1 Cu2 2.860(2) . ? Cu1 Cu3 2.922(3) . ? Cu2 Cl2 2.224(4) . ? Cu2 Cl4 2.587(4) . ? Cu2 Cu3 2.902(3) . ? Cu3 Cl3 2.188(5) . ? Cu3 Cl4 2.640(4) . ? B1 N4 1.534(19) . ? B1 N6 1.54(2) . ? B1 N2 1.571(18) . ? B1 H1 0.92(13) . ? N1 C1 1.352(17) . ? N1 N2 1.360(14) . ? N2 C3 1.344(17) . ? N3 C6 1.361(17) . ? N3 N4 1.389(15) . ? N4 C8 1.360(16) . ? N5 C11 1.322(16) . ? N5 N6 1.379(14) . ? N6 C13 1.331(18) . ? N7 C22 1.472(18) . ? N7 C16 1.51(2) . ? N7 C20 1.55(2) . ? N7 C18 1.566(17) . ? N8 C24 1.48(3) . ? N8 C28 1.50(3) . ? N8 C26 1.51(3) . ? N8 C30 1.60(3) . ? C1 C2 1.37(2) . ? C1 C4 1.507(18) . ? C2 C3 1.372(19) . ? C2 H2 0.9400 . ? C3 C5 1.49(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.364(18) . ? C6 C9 1.473(19) . ? C7 C8 1.340(19) . ? C7 H7 0.9400 . ? C8 C10 1.509(19) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.41(2) . ? C11 C14 1.50(2) . ? C12 C13 1.36(2) . ? C12 H12 0.9400 . ? C13 C15 1.48(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.50(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.42(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 C21 1.43(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.54(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.49(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C27 1.51(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.50(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 C31 1.52(2) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? 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 S3 Mo1 S2 103.91(14) . . ? S3 Mo1 S1 104.46(14) . . ? S2 Mo1 S1 104.18(13) . . ? S3 Mo1 N3 86.5(3) . . ? S2 Mo1 N3 86.7(3) . . ? S1 Mo1 N3 161.9(3) . . ? S3 Mo1 N1 162.9(3) . . ? S2 Mo1 N1 85.9(3) . . ? S1 Mo1 N1 86.2(3) . . ? N3 Mo1 N1 80.0(4) . . ? S3 Mo1 N5 87.0(3) . . ? S2 Mo1 N5 161.3(3) . . ? S1 Mo1 N5 87.4(3) . . ? N3 Mo1 N5 78.7(4) . . ? N1 Mo1 N5 80.1(4) . . ? S3 Mo1 Cu3 52.71(10) . . ? S2 Mo1 Cu3 105.00(11) . . ? S1 Mo1 Cu3 52.69(11) . . ? N3 Mo1 Cu3 139.0(3) . . ? N1 Mo1 Cu3 138.8(3) . . ? N5 Mo1 Cu3 93.7(3) . . ? S3 Mo1 Cu1 103.92(11) . . ? S2 Mo1 Cu1 52.66(9) . . ? S1 Mo1 Cu1 52.76(10) . . ? N3 Mo1 Cu1 139.3(3) . . ? N1 Mo1 Cu1 93.2(3) . . ? N5 Mo1 Cu1 140.1(3) . . ? Cu3 Mo1 Cu1 65.83(6) . . ? S3 Mo1 Cu2 52.87(10) . . ? S2 Mo1 Cu2 52.53(10) . . ? S1 Mo1 Cu2 103.19(11) . . ? N3 Mo1 Cu2 94.9(3) . . ? N1 Mo1 Cu2 138.4(3) . . ? N5 Mo1 Cu2 139.8(3) . . ? Cu3 Mo1 Cu2 65.27(6) . . ? Cu1 Mo1 Cu2 64.08(6) . . ? Cu3 S1 Cu1 81.11(14) . . ? Cu3 S1 Mo1 72.12(12) . . ? Cu1 S1 Mo1 72.27(12) . . ? Cu2 S2 Cu1 79.43(13) . . ? Cu2 S2 Mo1 73.17(12) . . ? Cu1 S2 Mo1 72.99(12) . . ? Cu3 S3 Cu2 80.63(13) . . ? Cu3 S3 Mo1 72.75(12) . . ? Cu2 S3 Mo1 72.95(12) . . ? Cl1 Cu1 S2 116.67(17) . . ? Cl1 Cu1 S1 123.24(17) . . ? S2 Cu1 S1 107.99(14) . . ? Cl1 Cu1 Cl4 99.32(16) . . ? S2 Cu1 Cl4 103.67(14) . . ? S1 Cu1 Cl4 102.39(15) . . ? Cl1 Cu1 Mo1 158.12(15) . . ? S2 Cu1 Mo1 54.36(9) . . ? S1 Cu1 Mo1 54.97(10) . . ? Cl4 Cu1 Mo1 102.27(11) . . ? Cl1 Cu1 Cu2 135.18(15) . . ? S2 Cu1 Cu2 50.26(10) . . ? S1 Cu1 Cu2 100.02(11) . . ? Cl4 Cu1 Cu2 56.56(10) . . ? Mo1 Cu1 Cu2 58.04(5) . . ? Cl1 Cu1 Cu3 141.76(15) . . ? S2 Cu1 Cu3 99.09(11) . . ? S1 Cu1 Cu3 49.32(11) . . ? Cl4 Cu1 Cu3 57.00(10) . . ? Mo1 Cu1 Cu3 56.92(5) . . ? Cu2 Cu1 Cu3 60.24(6) . . ? Cl2 Cu2 S2 120.72(15) . . ? Cl2 Cu2 S3 120.71(15) . . ? S2 Cu2 S3 106.91(14) . . ? Cl2 Cu2 Cl4 98.05(15) . . ? S2 Cu2 Cl4 103.35(14) . . ? S3 Cu2 Cl4 103.43(15) . . ? Cl2 Cu2 Mo1 160.13(14) . . ? S2 Cu2 Mo1 54.29(10) . . ? S3 Cu2 Mo1 54.19(10) . . ? Cl4 Cu2 Mo1 101.82(11) . . ? Cl2 Cu2 Cu1 137.03(13) . . ? S2 Cu2 Cu1 50.31(10) . . ? S3 Cu2 Cu1 99.90(12) . . ? Cl4 Cu2 Cu1 56.16(10) . . ? Mo1 Cu2 Cu1 57.88(5) . . ? Cl2 Cu2 Cu3 137.49(13) . . ? S2 Cu2 Cu3 99.71(11) . . ? S3 Cu2 Cu3 49.47(11) . . ? Cl4 Cu2 Cu3 57.16(10) . . ? Mo1 Cu2 Cu3 57.12(6) . . ? Cu1 Cu2 Cu3 60.93(6) . . ? Cl3 Cu3 S3 116.36(19) . . ? Cl3 Cu3 S1 124.8(2) . . ? S3 Cu3 S1 108.72(16) . . ? Cl3 Cu3 Cl4 99.34(18) . . ? S3 Cu3 Cl4 102.18(15) . . ? S1 Cu3 Cl4 100.64(15) . . ? Cl3 Cu3 Mo1 159.34(16) . . ? S3 Cu3 Mo1 54.54(11) . . ? S1 Cu3 Mo1 55.19(10) . . ? Cl4 Cu3 Mo1 100.83(11) . . ? Cl3 Cu3 Cu2 134.13(17) . . ? S3 Cu3 Cu2 49.90(10) . . ? S1 Cu3 Cu2 99.01(12) . . ? Cl4 Cu3 Cu2 55.41(10) . . ? Mo1 Cu3 Cu2 57.61(6) . . ? Cl3 Cu3 Cu1 141.36(16) . . ? S3 Cu3 Cu1 98.46(12) . . ? S1 Cu3 Cu1 49.57(11) . . ? Cl4 Cu3 Cu1 54.88(10) . . ? Mo1 Cu3 Cu1 57.25(5) . . ? Cu2 Cu3 Cu1 58.83(6) . . ? Cu1 Cl4 Cu2 67.28(11) . . ? Cu1 Cl4 Cu3 68.12(11) . . ? Cu2 Cl4 Cu3 67.43(10) . . ? N4 B1 N6 108.1(12) . . ? N4 B1 N2 107.9(11) . . ? N6 B1 N2 108.5(11) . . ? N4 B1 H1 102(8) . . ? N6 B1 H1 127(8) . . ? N2 B1 H1 102(8) . . ? C1 N1 N2 104.7(10) . . ? C1 N1 Mo1 133.7(9) . . ? N2 N1 Mo1 121.6(8) . . ? C3 N2 N1 111.6(11) . . ? C3 N2 B1 127.0(11) . . ? N1 N2 B1 121.4(11) . . ? C6 N3 N4 106.8(11) . . ? C6 N3 Mo1 133.4(9) . . ? N4 N3 Mo1 119.8(8) . . ? C8 N4 N3 107.5(11) . . ? C8 N4 B1 129.1(12) . . ? N3 N4 B1 123.3(11) . . ? C11 N5 N6 106.5(11) . . ? C11 N5 Mo1 133.9(10) . . ? N6 N5 Mo1 119.3(8) . . ? C13 N6 N5 110.7(11) . . ? C13 N6 B1 125.2(12) . . ? N5 N6 B1 123.6(10) . . ? C22 N7 C16 114.2(13) . . ? C22 N7 C20 108.6(12) . . ? C16 N7 C20 108.1(13) . . ? C22 N7 C18 108.0(10) . . ? C16 N7 C18 110.2(11) . . ? C20 N7 C18 107.5(11) . . ? C24 N8 C28 106.8(17) . . ? C24 N8 C26 108.8(17) . . ? C28 N8 C26 107.9(19) . . ? C24 N8 C30 116(2) . . ? C28 N8 C30 115.2(18) . . ? C26 N8 C30 102.1(17) . . ? N1 C1 C2 110.4(12) . . ? N1 C1 C4 125.4(13) . . ? C2 C1 C4 124.1(13) . . ? C1 C2 C3 106.7(12) . . ? C1 C2 H2 126.7 . . ? C3 C2 H2 126.7 . . ? N2 C3 C2 106.5(12) . . ? N2 C3 C5 124.8(14) . . ? C2 C3 C5 128.5(14) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 108.5(13) . . ? N3 C6 C9 125.7(12) . . ? C7 C6 C9 125.8(13) . . ? C8 C7 C6 108.3(13) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? C7 C8 N4 108.8(12) . . ? C7 C8 C10 129.3(13) . . ? N4 C8 C10 121.6(14) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 108.7(13) . . ? N5 C11 C14 124.1(13) . . ? C12 C11 C14 127.3(13) . . ? C13 C12 C11 106.9(13) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? N6 C13 C12 107.2(13) . . ? N6 C13 C15 125.4(15) . . ? C12 C13 C15 127.3(14) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N7 113.9(14) . . ? C17 C16 H16A 108.8 . . ? N7 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? N7 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N7 118.8(13) . . ? C19 C18 H18A 107.6 . . ? N7 C18 H18A 107.6 . . ? C19 C18 H18B 107.6 . . ? N7 C18 H18B 107.6 . . ? H18A C18 H18B 107.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N7 117.6(17) . . ? C21 C20 H20A 107.9 . . ? N7 C20 H20A 107.9 . . ? C21 C20 H20B 107.9 . . ? N7 C20 H20B 107.9 . . ? H20A C20 H20B 107.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 C23 116.6(12) . . ? N7 C22 H22A 108.1 . . ? C23 C22 H22A 108.1 . . ? N7 C22 H22B 108.1 . . ? C23 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N8 C24 C25 118(2) . . ? N8 C24 H24A 107.8 . . ? C25 C24 H24A 107.8 . . ? N8 C24 H24B 107.8 . . ? C25 C24 H24B 107.8 . . ? H24A C24 H24B 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 N8 118(2) . . ? C27 C26 H26A 107.7 . . ? N8 C26 H26A 107.7 . . ? C27 C26 H26B 107.7 . . ? N8 C26 H26B 107.7 . . ? H26A C26 H26B 107.1 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C29 113(2) . . ? N8 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? N8 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 N8 103(2) . . ? C31 C30 H30A 111.1 . . ? N8 C30 H30A 111.1 . . ? C31 C30 H30B 111.1 . . ? N8 C30 H30B 111.1 . . ? H30A C30 H30B 109.1 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.225 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.130 data_3^.^CH~2~Cl~2~ _database_code_depnum_ccdc_archive 'CCDC 928966' #TrackingRef 'ZhangZY.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H22 B Br3 Cu3 Mo N6 S3, C8 H20 N, C H2 Cl2' _chemical_formula_sum 'C24 H44 B Br3 Cl2 Cu3 Mo N7 S3' _chemical_formula_weight 1134.84 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.394(2) _cell_length_b 10.638(2) _cell_length_c 18.519(4) _cell_angle_alpha 77.96(3) _cell_angle_beta 85.42(3) _cell_angle_gamma 80.26(3) _cell_volume 1971.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9559 _cell_measurement_theta_min 3.0212 _cell_measurement_theta_max 27.5398 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 5.269 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5873 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17659 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8787 _reflns_number_gt 6225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvated CH~2~Cl~2~ molecule was refined to be disordered over two positions by sharing the Cl1 and Cl2 atoms with occupations of 0.60/0.40 for C24/C24A. The ethyl groups of the Et~4~N^+^ cation (N7-C17-C24) were restrained to be approximately isotropic. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8787 _refine_ls_number_parameters 419 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.22122(3) 0.91029(3) 0.22847(2) 0.02208(10) Uani 1 1 d . . . S1 S 0.43081(10) 0.95758(10) 0.21495(7) 0.0306(3) Uani 1 1 d . . . S2 S 0.24023(11) 0.70761(10) 0.19641(7) 0.0303(2) Uani 1 1 d . . . S3 S 0.18122(10) 0.86590(10) 0.35519(6) 0.0282(2) Uani 1 1 d . . . Cu1 Cu 0.43731(5) 0.75226(5) 0.20610(3) 0.03206(14) Uani 1 1 d . . . Cu2 Cu 0.23814(5) 0.68159(5) 0.31694(3) 0.02957(14) Uani 1 1 d . . . Cu3 Cu 0.39006(5) 0.88039(5) 0.33218(3) 0.03044(14) Uani 1 1 d . . . Br1 Br 0.62717(5) 0.61937(6) 0.18743(3) 0.05688(17) Uani 1 1 d . . . Br2 Br 0.26390(5) 0.48889(4) 0.39849(3) 0.04240(14) Uani 1 1 d . . . Br3 Br 0.54224(5) 0.85982(5) 0.41737(3) 0.04226(14) Uani 1 1 d . . . B1 B 0.0087(5) 1.1480(5) 0.1320(3) 0.0305(11) Uani 1 1 d . . . H1 H -0.058(4) 1.219(4) 0.094(3) 0.037 Uiso 1 1 d . . . N1 N 0.2102(3) 0.9948(3) 0.1050(2) 0.0264(8) Uani 1 1 d . . . N2 N 0.1083(3) 1.0882(3) 0.0788(2) 0.0270(8) Uani 1 1 d . . . N3 N 0.0029(3) 0.9296(3) 0.2172(2) 0.0273(8) Uani 1 1 d . . . N4 N -0.0635(3) 1.0427(3) 0.1779(2) 0.0285(8) Uani 1 1 d . . . N5 N 0.1567(3) 1.1246(3) 0.2361(2) 0.0285(8) Uani 1 1 d . . . N6 N 0.0777(3) 1.2055(3) 0.1841(2) 0.0277(8) Uani 1 1 d . . . N7 N 0.2453(4) 0.7227(4) 0.6011(2) 0.0357(9) Uani 1 1 d . . . C1 C 0.2875(4) 0.9723(4) 0.0451(3) 0.0308(10) Uani 1 1 d . . . C2 C 0.2332(5) 1.0513(4) -0.0175(3) 0.0364(11) Uani 1 1 d . . . H2 H 0.2675 1.0558 -0.0663 0.044 Uiso 1 1 calc R . . C3 C 0.1201(4) 1.1220(4) 0.0049(3) 0.0326(10) Uani 1 1 d . . . C4 C 0.4081(4) 0.8759(5) 0.0449(3) 0.0425(12) Uani 1 1 d . . . H4A H 0.4709 0.8942 0.0758 0.064 Uiso 1 1 calc R . . H4B H 0.4449 0.8810 -0.0052 0.064 Uiso 1 1 calc R . . H4C H 0.3874 0.7892 0.0640 0.064 Uiso 1 1 calc R . . C5 C 0.0219(5) 1.2194(5) -0.0416(3) 0.0527(14) Uani 1 1 d . . . H5A H -0.0592 1.1848 -0.0392 0.079 Uiso 1 1 calc R . . H5B H 0.0557 1.2366 -0.0924 0.079 Uiso 1 1 calc R . . H5C H 0.0059 1.2997 -0.0230 0.079 Uiso 1 1 calc R . . C6 C -0.0905(4) 0.8579(4) 0.2490(3) 0.0300(10) Uani 1 1 d . . . C7 C -0.2114(4) 0.9263(4) 0.2300(3) 0.0344(11) Uani 1 1 d . . . H7 H -0.2922 0.8985 0.2453 0.041 Uiso 1 1 calc R . . C8 C -0.1932(4) 1.0419(4) 0.1851(3) 0.0302(10) Uani 1 1 d . . . C9 C -0.0647(5) 0.7247(5) 0.2964(3) 0.0451(14) Uani 1 1 d . . . H9A H -0.0044 0.6680 0.2701 0.068 Uiso 1 1 calc R . . H9B H -0.1461 0.6902 0.3081 0.068 Uiso 1 1 calc R . . H9C H -0.0270 0.7296 0.3418 0.068 Uiso 1 1 calc R . . C10 C -0.2897(4) 1.1531(5) 0.1476(3) 0.0415(12) Uani 1 1 d . . . H10A H -0.2777 1.2326 0.1623 0.062 Uiso 1 1 calc R . . H10B H -0.3778 1.1358 0.1619 0.062 Uiso 1 1 calc R . . H10C H -0.2758 1.1629 0.0945 0.062 Uiso 1 1 calc R . . C11 C 0.1923(4) 1.2021(4) 0.2788(3) 0.0318(10) Uani 1 1 d . . . C12 C 0.1360(4) 1.3298(4) 0.2525(3) 0.0365(12) Uani 1 1 d . . . H12 H 0.1450 1.4028 0.2717 0.044 Uiso 1 1 calc R . . C13 C 0.0646(4) 1.3298(4) 0.1930(3) 0.0334(11) Uani 1 1 d . . . C14 C 0.2707(5) 1.1577(5) 0.3444(3) 0.0468(14) Uani 1 1 d . . . H14A H 0.2263 1.0990 0.3814 0.070 Uiso 1 1 calc R . . H14B H 0.2823 1.2321 0.3645 0.070 Uiso 1 1 calc R . . H14C H 0.3555 1.1127 0.3308 0.070 Uiso 1 1 calc R . . C15 C -0.0149(6) 1.4407(5) 0.1455(3) 0.0545(15) Uani 1 1 d . . . H15A H 0.0107 1.4404 0.0940 0.082 Uiso 1 1 calc R . . H15B H -0.0007 1.5217 0.1574 0.082 Uiso 1 1 calc R . . H15C H -0.1067 1.4325 0.1540 0.082 Uiso 1 1 calc R . . C16 C 0.1102(5) 0.6835(6) 0.6098(3) 0.0534(15) Uani 1 1 d . . . H16A H 0.0538 0.7390 0.6395 0.064 Uiso 1 1 calc R . . H16B H 0.1170 0.5937 0.6376 0.064 Uiso 1 1 calc R . . C17 C 0.0444(6) 0.6926(6) 0.5380(4) 0.0649(17) Uani 1 1 d U . . H17A H 0.0331 0.7819 0.5110 0.097 Uiso 1 1 calc R . . H17B H -0.0403 0.6644 0.5490 0.097 Uiso 1 1 calc R . . H17C H 0.0985 0.6371 0.5083 0.097 Uiso 1 1 calc R . . C18 C 0.2421(5) 0.8616(5) 0.5598(3) 0.0420(12) Uani 1 1 d U . . H18A H 0.3309 0.8826 0.5563 0.050 Uiso 1 1 calc R . . H18B H 0.2161 0.8673 0.5094 0.050 Uiso 1 1 calc R . . C19 C 0.1525(6) 0.9625(6) 0.5932(4) 0.0671(17) Uani 1 1 d U . . H19A H 0.0632 0.9463 0.5941 0.101 Uiso 1 1 calc R . . H19B H 0.1593 1.0481 0.5638 0.101 Uiso 1 1 calc R . . H19C H 0.1769 0.9582 0.6432 0.101 Uiso 1 1 calc R . . C20 C 0.3384(4) 0.6363(4) 0.5576(3) 0.0364(11) Uani 1 1 d U . . H20A H 0.3062 0.6500 0.5078 0.044 Uiso 1 1 calc R . . H20B H 0.4238 0.6656 0.5524 0.044 Uiso 1 1 calc R . . C21 C 0.3581(6) 0.4926(5) 0.5893(4) 0.0593(15) Uani 1 1 d U . . H21A H 0.3946 0.4766 0.6376 0.089 Uiso 1 1 calc R . . H21B H 0.4176 0.4472 0.5567 0.089 Uiso 1 1 calc R . . H21C H 0.2748 0.4614 0.5941 0.089 Uiso 1 1 calc R . . C22 C 0.2913(5) 0.7068(6) 0.6790(3) 0.0524(14) Uani 1 1 d U . . H22A H 0.2285 0.7624 0.7057 0.063 Uiso 1 1 calc R . . H22B H 0.2905 0.6165 0.7045 0.063 Uiso 1 1 calc R . . C23 C 0.4256(6) 0.7399(6) 0.6831(4) 0.0696(18) Uani 1 1 d U . . H23A H 0.4897 0.6816 0.6598 0.104 Uiso 1 1 calc R . . H23B H 0.4454 0.7302 0.7345 0.104 Uiso 1 1 calc R . . H23C H 0.4281 0.8290 0.6577 0.104 Uiso 1 1 calc R . . C24 C 0.3870(13) 1.4353(12) 0.0945(9) 0.091(4) Uani 0.60 1 d PU A 1 H24A H 0.4794 1.4449 0.0864 0.109 Uiso 0.60 1 calc PR A 1 H24B H 0.3546 1.4587 0.1419 0.109 Uiso 0.60 1 calc PR A 1 C24A C 0.355(2) 1.3983(19) 0.0182(14) 0.131(10) Uani 0.40 1 d P A 2 H24C H 0.4444 1.4043 -0.0009 0.157 Uiso 0.40 1 calc PR A 2 H24D H 0.3142 1.3623 -0.0175 0.157 Uiso 0.40 1 calc PR A 2 Cl1 Cl 0.2818(3) 1.5461(3) 0.01138(18) 0.1409(11) Uani 1 1 d . . . Cl2 Cl 0.3665(2) 1.2861(2) 0.09284(15) 0.1087(8) 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 Mo1 0.01899(17) 0.02007(17) 0.0265(2) -0.00414(14) -0.00139(15) -0.00165(13) S1 0.0213(5) 0.0312(6) 0.0384(7) -0.0040(5) -0.0019(5) -0.0045(4) S2 0.0345(6) 0.0258(5) 0.0317(6) -0.0093(5) -0.0038(5) -0.0028(4) S3 0.0296(5) 0.0269(5) 0.0283(6) -0.0077(4) 0.0004(5) -0.0031(4) Cu1 0.0269(3) 0.0312(3) 0.0352(3) -0.0075(2) -0.0008(2) 0.0044(2) Cu2 0.0358(3) 0.0231(3) 0.0295(3) -0.0039(2) -0.0027(2) -0.0046(2) Cu3 0.0273(3) 0.0310(3) 0.0342(3) -0.0082(2) -0.0057(2) -0.0035(2) Br1 0.0456(3) 0.0592(4) 0.0514(4) -0.0075(3) 0.0023(3) 0.0259(3) Br2 0.0653(3) 0.0236(2) 0.0377(3) -0.00348(19) -0.0062(2) -0.0066(2) Br3 0.0394(3) 0.0459(3) 0.0433(3) -0.0074(2) -0.0143(2) -0.0078(2) B1 0.027(2) 0.026(2) 0.034(3) -0.001(2) 0.002(2) 0.0015(19) N1 0.0236(17) 0.0262(18) 0.026(2) 0.0001(15) -0.0001(15) -0.0007(14) N2 0.0265(18) 0.0254(18) 0.026(2) -0.0015(15) -0.0019(16) 0.0015(14) N3 0.0208(17) 0.0240(17) 0.035(2) -0.0002(15) -0.0023(16) -0.0029(14) N4 0.0222(17) 0.0291(19) 0.032(2) -0.0032(16) -0.0026(16) -0.0003(14) N5 0.0255(17) 0.0219(17) 0.039(2) -0.0095(16) -0.0010(17) -0.0032(14) N6 0.0258(18) 0.0228(18) 0.032(2) -0.0039(15) 0.0010(16) 0.0009(14) N7 0.034(2) 0.040(2) 0.031(2) -0.0089(18) 0.0024(18) -0.0033(17) C1 0.030(2) 0.036(2) 0.026(2) -0.0084(19) 0.0009(19) -0.0007(18) C2 0.045(3) 0.039(3) 0.024(2) -0.007(2) 0.001(2) -0.002(2) C3 0.039(2) 0.027(2) 0.028(3) 0.0013(19) -0.003(2) -0.0024(19) C4 0.036(3) 0.049(3) 0.034(3) -0.005(2) 0.005(2) 0.009(2) C5 0.062(3) 0.053(3) 0.033(3) 0.003(3) -0.010(3) 0.010(3) C6 0.022(2) 0.039(2) 0.031(3) -0.006(2) 0.0003(19) -0.0140(18) C7 0.021(2) 0.045(3) 0.038(3) -0.006(2) 0.000(2) -0.0106(19) C8 0.023(2) 0.040(2) 0.028(2) -0.008(2) -0.0029(19) -0.0024(18) C9 0.036(3) 0.039(3) 0.056(4) 0.010(2) -0.008(2) -0.016(2) C10 0.026(2) 0.049(3) 0.046(3) -0.008(2) -0.005(2) 0.003(2) C11 0.028(2) 0.026(2) 0.045(3) -0.013(2) 0.002(2) -0.0060(17) C12 0.039(3) 0.021(2) 0.049(3) -0.014(2) 0.010(2) -0.0025(18) C13 0.033(2) 0.023(2) 0.042(3) -0.006(2) 0.011(2) -0.0025(18) C14 0.047(3) 0.033(3) 0.066(4) -0.020(3) -0.024(3) -0.002(2) C15 0.069(4) 0.029(3) 0.057(4) -0.002(2) -0.001(3) 0.007(2) C16 0.049(3) 0.060(3) 0.050(4) -0.006(3) 0.017(3) -0.018(3) C17 0.0641(18) 0.0658(18) 0.0652(19) -0.0127(10) -0.0033(10) -0.0115(10) C18 0.0424(14) 0.0411(14) 0.0425(15) -0.0084(9) -0.0011(9) -0.0067(9) C19 0.0676(19) 0.0663(19) 0.0671(19) -0.0149(10) -0.0030(10) -0.0077(10) C20 0.0368(13) 0.0360(13) 0.0358(14) -0.0073(9) 0.0002(9) -0.0045(9) C21 0.0602(17) 0.0583(17) 0.0588(18) -0.0119(10) -0.0022(10) -0.0079(10) C22 0.0525(16) 0.0534(16) 0.0505(16) -0.0111(10) -0.0010(10) -0.0054(10) C23 0.069(2) 0.070(2) 0.069(2) -0.0153(10) -0.0040(10) -0.0091(10) C24 0.091(4) 0.091(4) 0.091(4) -0.0183(12) -0.0035(10) -0.0152(12) C24A 0.15(2) 0.081(15) 0.11(2) 0.028(13) -0.013(16) 0.072(14) Cl1 0.152(2) 0.0977(17) 0.134(2) 0.0110(16) 0.0181(19) 0.0365(16) Cl2 0.0946(14) 0.0870(14) 0.125(2) -0.0116(13) 0.0302(14) 0.0128(11) _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 Mo1 N3 2.266(3) . ? Mo1 N1 2.281(4) . ? Mo1 N5 2.295(3) . ? Mo1 S1 2.3005(12) . ? Mo1 S3 2.3131(13) . ? Mo1 S2 2.3263(12) . ? Mo1 Cu2 2.6215(11) . ? Mo1 Cu1 2.6280(10) . ? Mo1 Cu3 2.6390(10) . ? S1 Cu3 2.1894(15) . ? S1 Cu1 2.2135(13) . ? S2 Cu2 2.1899(14) . ? S2 Cu1 2.2085(13) . ? S3 Cu2 2.1945(13) . ? S3 Cu3 2.2034(12) . ? Cu1 Br1 2.2723(10) . ? Cu1 Cu2 2.8753(12) . ? Cu1 Cu3 2.9101(11) . ? Cu2 Br2 2.2676(10) . ? Cu2 Cu3 2.9148(10) . ? Cu3 Br3 2.2752(10) . ? B1 N2 1.525(6) . ? B1 N6 1.525(7) . ? B1 N4 1.525(6) . ? B1 H1 1.11(5) . ? N1 C1 1.354(5) . ? N1 N2 1.367(5) . ? N2 C3 1.341(6) . ? N3 C6 1.358(5) . ? N3 N4 1.374(5) . ? N4 C8 1.345(5) . ? N5 C11 1.366(6) . ? N5 N6 1.373(5) . ? N6 C13 1.349(5) . ? N7 C18 1.512(6) . ? N7 C16 1.518(6) . ? N7 C20 1.521(6) . ? N7 C22 1.522(7) . ? C1 C2 1.381(6) . ? C1 C4 1.480(6) . ? C2 C3 1.368(6) . ? C2 H2 0.9400 . ? C3 C5 1.506(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.373(6) . ? C6 C9 1.497(6) . ? C7 C8 1.367(6) . ? C7 H7 0.9400 . ? C8 C10 1.501(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.387(6) . ? C11 C14 1.467(7) . ? C12 C13 1.376(7) . ? C12 H12 0.9400 . ? C13 C15 1.484(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.522(9) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.499(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 C21 1.504(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.507(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 Cl2 1.644(13) . ? C24 Cl1 2.008(14) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24A Cl1 1.610(18) . ? C24A Cl2 1.63(2) . ? C24A H24C 0.9800 . ? C24A H24D 0.9800 . ? 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 N3 Mo1 N1 80.52(13) . . ? N3 Mo1 N5 79.43(12) . . ? N1 Mo1 N5 82.12(13) . . ? N3 Mo1 S1 160.98(9) . . ? N1 Mo1 S1 85.46(9) . . ? N5 Mo1 S1 86.00(9) . . ? N3 Mo1 S3 87.53(10) . . ? N1 Mo1 S3 164.28(9) . . ? N5 Mo1 S3 85.70(11) . . ? S1 Mo1 S3 103.61(5) . . ? N3 Mo1 S2 87.39(10) . . ? N1 Mo1 S2 86.17(10) . . ? N5 Mo1 S2 163.61(10) . . ? S1 Mo1 S2 104.51(5) . . ? S3 Mo1 S2 103.56(5) . . ? N3 Mo1 Cu2 94.10(9) . . ? N1 Mo1 Cu2 138.25(9) . . ? N5 Mo1 Cu2 137.94(10) . . ? S1 Mo1 Cu2 104.91(4) . . ? S3 Mo1 Cu2 52.36(4) . . ? S2 Mo1 Cu2 52.13(3) . . ? N3 Mo1 Cu1 139.65(9) . . ? N1 Mo1 Cu1 91.23(9) . . ? N5 Mo1 Cu1 138.80(9) . . ? S1 Mo1 Cu1 52.87(3) . . ? S3 Mo1 Cu1 104.49(5) . . ? S2 Mo1 Cu1 52.52(4) . . ? Cu2 Mo1 Cu1 66.42(3) . . ? N3 Mo1 Cu3 139.49(10) . . ? N1 Mo1 Cu3 137.42(9) . . ? N5 Mo1 Cu3 90.91(10) . . ? S1 Mo1 Cu3 52.07(4) . . ? S3 Mo1 Cu3 52.34(3) . . ? S2 Mo1 Cu3 105.46(4) . . ? Cu2 Mo1 Cu3 67.30(3) . . ? Cu1 Mo1 Cu3 67.08(3) . . ? Cu3 S1 Cu1 82.74(5) . . ? Cu3 S1 Mo1 71.95(5) . . ? Cu1 S1 Mo1 71.18(4) . . ? Cu2 S2 Cu1 81.64(5) . . ? Cu2 S2 Mo1 70.89(5) . . ? Cu1 S2 Mo1 70.78(4) . . ? Cu2 S3 Cu3 83.02(5) . . ? Cu2 S3 Mo1 71.06(5) . . ? Cu3 S3 Mo1 71.46(5) . . ? S2 Cu1 S1 111.66(5) . . ? S2 Cu1 Br1 124.77(4) . . ? S1 Cu1 Br1 122.61(4) . . ? S2 Cu1 Mo1 56.71(3) . . ? S1 Cu1 Mo1 55.95(4) . . ? Br1 Cu1 Mo1 178.52(3) . . ? S2 Cu1 Cu2 48.90(4) . . ? S1 Cu1 Cu2 99.50(5) . . ? Br1 Cu1 Cu2 124.05(4) . . ? Mo1 Cu1 Cu2 56.68(3) . . ? S2 Cu1 Cu3 100.32(4) . . ? S1 Cu1 Cu3 48.27(4) . . ? Br1 Cu1 Cu3 122.33(4) . . ? Mo1 Cu1 Cu3 56.64(3) . . ? Cu2 Cu1 Cu3 60.50(3) . . ? S2 Cu2 S3 112.47(5) . . ? S2 Cu2 Br2 126.17(4) . . ? S3 Cu2 Br2 120.90(4) . . ? S2 Cu2 Mo1 56.98(4) . . ? S3 Cu2 Mo1 56.58(4) . . ? Br2 Cu2 Mo1 175.55(3) . . ? S2 Cu2 Cu1 49.46(4) . . ? S3 Cu2 Cu1 100.11(4) . . ? Br2 Cu2 Cu1 121.95(4) . . ? Mo1 Cu2 Cu1 56.90(3) . . ? S2 Cu2 Cu3 100.64(4) . . ? S3 Cu2 Cu3 48.62(3) . . ? Br2 Cu2 Cu3 118.91(3) . . ? Mo1 Cu2 Cu3 56.64(3) . . ? Cu1 Cu2 Cu3 60.34(3) . . ? S1 Cu3 S3 111.27(6) . . ? S1 Cu3 Br3 121.22(4) . . ? S3 Cu3 Br3 126.45(5) . . ? S1 Cu3 Mo1 55.98(4) . . ? S3 Cu3 Mo1 56.20(4) . . ? Br3 Cu3 Mo1 177.18(3) . . ? S1 Cu3 Cu1 48.98(4) . . ? S3 Cu3 Cu1 98.86(5) . . ? Br3 Cu3 Cu1 122.60(3) . . ? Mo1 Cu3 Cu1 56.28(3) . . ? S1 Cu3 Cu2 98.92(5) . . ? S3 Cu3 Cu2 48.36(4) . . ? Br3 Cu3 Cu2 126.08(3) . . ? Mo1 Cu3 Cu2 56.06(3) . . ? Cu1 Cu3 Cu2 59.16(3) . . ? N2 B1 N6 110.1(4) . . ? N2 B1 N4 109.4(4) . . ? N6 B1 N4 108.6(4) . . ? N2 B1 H1 102(2) . . ? N6 B1 H1 115(2) . . ? N4 B1 H1 111(2) . . ? C1 N1 N2 106.2(3) . . ? C1 N1 Mo1 133.5(3) . . ? N2 N1 Mo1 120.4(3) . . ? C3 N2 N1 110.4(3) . . ? C3 N2 B1 128.8(4) . . ? N1 N2 B1 120.5(4) . . ? C6 N3 N4 105.4(3) . . ? C6 N3 Mo1 134.4(3) . . ? N4 N3 Mo1 119.7(2) . . ? C8 N4 N3 110.8(3) . . ? C8 N4 B1 127.8(4) . . ? N3 N4 B1 121.3(3) . . ? C11 N5 N6 106.1(3) . . ? C11 N5 Mo1 133.4(3) . . ? N6 N5 Mo1 120.0(3) . . ? C13 N6 N5 110.6(4) . . ? C13 N6 B1 129.3(4) . . ? N5 N6 B1 119.8(3) . . ? C18 N7 C16 111.4(4) . . ? C18 N7 C20 107.3(3) . . ? C16 N7 C20 110.7(4) . . ? C18 N7 C22 110.6(4) . . ? C16 N7 C22 106.3(4) . . ? C20 N7 C22 110.6(4) . . ? N1 C1 C2 108.9(4) . . ? N1 C1 C4 126.5(4) . . ? C2 C1 C4 124.5(4) . . ? C3 C2 C1 107.1(4) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? N2 C3 C2 107.4(4) . . ? N2 C3 C5 124.0(4) . . ? C2 C3 C5 128.7(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 109.3(4) . . ? N3 C6 C9 125.0(4) . . ? C7 C6 C9 125.7(4) . . ? C8 C7 C6 107.8(4) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? N4 C8 C7 106.7(4) . . ? N4 C8 C10 122.3(4) . . ? C7 C8 C10 130.9(4) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 108.8(4) . . ? N5 C11 C14 125.9(4) . . ? C12 C11 C14 125.2(4) . . ? C13 C12 C11 107.4(4) . . ? C13 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? N6 C13 C12 107.2(4) . . ? N6 C13 C15 123.7(5) . . ? C12 C13 C15 129.1(4) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 C17 115.4(4) . . ? N7 C16 H16A 108.4 . . ? C17 C16 H16A 108.4 . . ? N7 C16 H16B 108.4 . . ? C17 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N7 115.6(4) . . ? C19 C18 H18A 108.4 . . ? N7 C18 H18A 108.4 . . ? C19 C18 H18B 108.4 . . ? N7 C18 H18B 108.4 . . ? H18A C18 H18B 107.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N7 116.5(4) . . ? C21 C20 H20A 108.2 . . ? N7 C20 H20A 108.2 . . ? C21 C20 H20B 108.2 . . ? N7 C20 H20B 108.2 . . ? H20A C20 H20B 107.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 N7 115.1(5) . . ? C23 C22 H22A 108.5 . . ? N7 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? N7 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl2 C24 Cl1 104.2(8) . . ? Cl2 C24 H24A 110.9 . . ? Cl1 C24 H24A 110.9 . . ? Cl2 C24 H24B 110.9 . . ? Cl1 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? Cl1 C24A Cl2 126.6(17) . . ? Cl1 C24A H24C 105.7 . . ? Cl2 C24A H24C 105.7 . . ? Cl1 C24A H24D 105.7 . . ? Cl2 C24A H24D 105.7 . . ? H24C C24A H24D 106.1 . . ? C24A Cl1 C24 51.8(10) . . ? C24A Cl2 C24 59.4(11) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.060 _refine_diff_density_min -1.394 _refine_diff_density_rms 0.145 data_4^.^0.5CH~2~Cl~2~ _database_code_depnum_ccdc_archive 'CCDC 928967' #TrackingRef 'ZhangZY.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H22 B Cu3 I3 Mo N6 S3, C8 H20 N, 0.5(C H2 Cl2)' _chemical_formula_sum 'C23.50 H43 B Cl Cu3 I3 Mo N7 S3' _chemical_formula_weight 1233.35 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.485(2) _cell_length_b 10.901(2) _cell_length_c 18.762(4) _cell_angle_alpha 77.98(3) _cell_angle_beta 85.53(3) _cell_angle_gamma 80.75(3) _cell_volume 2068.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9436 _cell_measurement_theta_min 3.0374 _cell_measurement_theta_max 27.5982 _exptl_crystal_description Block _exptl_crystal_colour Dark-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1182 _exptl_absorpt_coefficient_mu 4.298 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5698 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16356 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7222 _reflns_number_gt 5061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. As the solvent molecule is likely to evaporate, the diffraction is weak in high angles. Thus the reflections at 2theta > 50 \% were omitted. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1391P)^2^+3.5052P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7222 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2376 _refine_ls_wR_factor_gt 0.2168 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.22051(9) 0.91732(9) 0.22294(6) 0.0276(3) Uani 1 1 d . . . S1 S 0.2345(3) 0.7197(3) 0.19223(18) 0.0359(7) Uani 1 1 d . . . S2 S 0.1817(3) 0.8747(3) 0.34910(18) 0.0350(7) Uani 1 1 d . . . S3 S 0.4313(3) 0.9593(3) 0.20891(19) 0.0371(7) Uani 1 1 d . . . Cu1 Cu 0.23428(15) 0.69406(14) 0.31164(9) 0.0374(4) Uani 1 1 d . . . Cu2 Cu 0.38971(14) 0.88378(15) 0.32522(9) 0.0374(4) Uani 1 1 d . . . Cu3 Cu 0.43198(14) 0.75991(14) 0.20062(9) 0.0383(4) Uani 1 1 d . . . I1 I 0.26765(11) 0.49041(9) 0.39724(6) 0.0565(3) Uani 1 1 d . . . I2 I 0.55170(9) 0.85297(9) 0.41691(5) 0.0478(3) Uani 1 1 d . . . I3 I 0.63152(9) 0.61665(10) 0.18015(6) 0.0596(3) Uani 1 1 d . . . B1 B 0.0118(13) 1.1508(12) 0.1265(8) 0.033(3) Uani 1 1 d . . . H1 H -0.053(12) 1.235(12) 0.082(7) 0.039 Uiso 1 1 d . . . N1 N 0.0008(9) 0.9408(9) 0.2132(6) 0.033(2) Uani 1 1 d . . . N2 N -0.0596(8) 1.0468(9) 0.1735(6) 0.032(2) Uani 1 1 d . . . N3 N 0.1611(9) 1.1266(9) 0.2294(6) 0.033(2) Uani 1 1 d . . . N4 N 0.0797(9) 1.2064(9) 0.1783(6) 0.035(2) Uani 1 1 d . . . N5 N 0.2105(9) 0.9989(10) 0.1006(5) 0.036(2) Uani 1 1 d . . . N6 N 0.1100(9) 1.0918(9) 0.0749(6) 0.035(2) Uani 1 1 d . . . N7 N -0.2281(11) 1.2673(10) 0.3965(6) 0.045(3) Uani 1 1 d . . . C1 C -0.0901(11) 0.8677(13) 0.2455(8) 0.040(3) Uani 1 1 d . . . C2 C -0.2116(11) 0.9362(14) 0.2257(7) 0.044(3) Uani 1 1 d . . . H2 H -0.2928 0.9107 0.2400 0.052 Uiso 1 1 calc R . . C3 C -0.1888(12) 1.0437(13) 0.1827(7) 0.040(3) Uani 1 1 d . . . C4 C -0.0669(13) 0.7392(12) 0.2923(8) 0.048(4) Uani 1 1 d . . . H4A H -0.0182 0.6804 0.2643 0.072 Uiso 1 1 calc R . . H4B H -0.1491 0.7113 0.3096 0.072 Uiso 1 1 calc R . . H4C H -0.0181 0.7419 0.3337 0.072 Uiso 1 1 calc R . . C5 C -0.2862(11) 1.1541(14) 0.1443(8) 0.045(3) Uani 1 1 d . . . H5A H -0.3734 1.1402 0.1613 0.068 Uiso 1 1 calc R . . H5B H -0.2768 1.1589 0.0920 0.068 Uiso 1 1 calc R . . H5C H -0.2696 1.2330 0.1555 0.068 Uiso 1 1 calc R . . C6 C 0.2021(12) 1.2003(11) 0.2716(8) 0.039(3) Uani 1 1 d . . . C7 C 0.1429(13) 1.3274(13) 0.2437(8) 0.047(3) Uani 1 1 d . . . H7 H 0.1537 1.3997 0.2613 0.056 Uiso 1 1 calc R . . C8 C 0.0695(12) 1.3263(12) 0.1883(8) 0.043(3) Uani 1 1 d . . . C9 C 0.2863(16) 1.1592(15) 0.3327(10) 0.066(5) Uani 1 1 d . . . H9A H 0.2490 1.0970 0.3696 0.099 Uiso 1 1 calc R . . H9B H 0.2956 1.2316 0.3534 0.099 Uiso 1 1 calc R . . H9C H 0.3706 1.1217 0.3159 0.099 Uiso 1 1 calc R . . C10 C -0.0076(16) 1.4374(13) 0.1401(10) 0.065(5) Uani 1 1 d . . . H10A H 0.0214 1.4393 0.0896 0.097 Uiso 1 1 calc R . . H10B H 0.0049 1.5156 0.1538 0.097 Uiso 1 1 calc R . . H10C H -0.0986 1.4287 0.1461 0.097 Uiso 1 1 calc R . . C11 C 0.2849(12) 0.9754(12) 0.0421(7) 0.039(3) Uani 1 1 d . . . C12 C 0.2297(13) 1.0569(13) -0.0200(8) 0.044(3) Uani 1 1 d . . . H12 H 0.2622 1.0612 -0.0685 0.053 Uiso 1 1 calc R . . C13 C 0.1249(12) 1.1258(12) 0.0016(7) 0.039(3) Uani 1 1 d . . . C14 C 0.4044(12) 0.8797(13) 0.0405(8) 0.045(3) Uani 1 1 d . . . H14A H 0.4668 0.8944 0.0722 0.067 Uiso 1 1 calc R . . H14B H 0.4414 0.8879 -0.0090 0.067 Uiso 1 1 calc R . . H14C H 0.3823 0.7951 0.0572 0.067 Uiso 1 1 calc R . . C15 C 0.0278(16) 1.2239(15) -0.0449(9) 0.064(5) Uani 1 1 d . . . H15A H 0.0539 1.2295 -0.0961 0.096 Uiso 1 1 calc R . . H15B H 0.0254 1.3059 -0.0321 0.096 Uiso 1 1 calc R . . H15C H -0.0574 1.1984 -0.0361 0.096 Uiso 1 1 calc R . . C16 C -0.3246(16) 1.3552(14) 0.4385(9) 0.059(4) Uani 1 1 d . . . H16A H -0.4103 1.3290 0.4409 0.071 Uiso 1 1 calc R . . H16B H -0.2972 1.3417 0.4886 0.071 Uiso 1 1 calc R . . C17 C -0.337(2) 1.4952(16) 0.4061(11) 0.079(6) Uani 1 1 d . . . H17A H -0.2583 1.5265 0.4126 0.118 Uiso 1 1 calc R . . H17B H -0.4095 1.5401 0.4305 0.118 Uiso 1 1 calc R . . H17C H -0.3522 1.5091 0.3545 0.118 Uiso 1 1 calc R . . C18 C -0.2707(19) 1.2853(18) 0.3199(9) 0.070(5) Uani 1 1 d . . . H18A H -0.2662 1.3733 0.2955 0.084 Uiso 1 1 calc R . . H18B H -0.2090 1.2307 0.2938 0.084 Uiso 1 1 calc R . . C19 C -0.4030(17) 1.258(2) 0.3128(10) 0.079(6) Uani 1 1 d . . . H19A H -0.4014 1.1666 0.3204 0.118 Uiso 1 1 calc R . . H19B H -0.4321 1.2969 0.2643 0.118 Uiso 1 1 calc R . . H19C H -0.4617 1.2913 0.3489 0.118 Uiso 1 1 calc R . . C20 C -0.2299(16) 1.1317(15) 0.4379(9) 0.060(4) Uani 1 1 d . . . H20A H -0.2074 1.1265 0.4883 0.073 Uiso 1 1 calc R . . H20B H -0.3184 1.1126 0.4394 0.073 Uiso 1 1 calc R . . C21 C -0.1402(19) 1.0309(17) 0.4070(12) 0.084(6) Uani 1 1 d . . . H21A H -0.1495 1.0449 0.3547 0.126 Uiso 1 1 calc R . . H21B H -0.1619 0.9480 0.4298 0.126 Uiso 1 1 calc R . . H21C H -0.0516 1.0350 0.4166 0.126 Uiso 1 1 calc R . . C22 C -0.0965(17) 1.3048(19) 0.3912(10) 0.078(6) Uani 1 1 d . . . H22A H -0.1027 1.3942 0.3669 0.094 Uiso 1 1 calc R . . H22B H -0.0406 1.2550 0.3599 0.094 Uiso 1 1 calc R . . C23 C -0.0292(18) 1.287(2) 0.4652(11) 0.092(7) Uani 1 1 d . . . H23A H -0.0740 1.3484 0.4930 0.139 Uiso 1 1 calc R . . H23B H 0.0602 1.3011 0.4554 0.139 Uiso 1 1 calc R . . H23C H -0.0322 1.2022 0.4929 0.139 Uiso 1 1 calc R . . C24 C 0.382(4) 1.439(4) 0.0888(18) 0.089(15) Uani 0.50 1 d P . . H24A H 0.4733 1.4510 0.0803 0.107 Uiso 0.50 1 calc PR . . H24B H 0.3533 1.4564 0.1371 0.107 Uiso 0.50 1 calc PR . . Cl1 Cl 0.3688(7) 1.2898(6) 0.0867(4) 0.054(2) Uani 0.50 1 d P . . Cl2 Cl 0.2838(8) 1.5517(7) 0.0180(4) 0.060(2) Uani 0.50 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 Mo1 0.0212(5) 0.0258(5) 0.0349(6) -0.0059(4) -0.0013(4) -0.0008(4) S1 0.0358(16) 0.0327(16) 0.0394(19) -0.0113(14) -0.0010(13) -0.0012(13) S2 0.0313(16) 0.0365(17) 0.0370(18) -0.0101(14) 0.0042(13) -0.0031(13) S3 0.0246(15) 0.0382(17) 0.048(2) -0.0066(15) 0.0005(13) -0.0051(13) Cu1 0.0405(9) 0.0309(8) 0.0397(10) -0.0047(7) -0.0025(7) -0.0049(7) Cu2 0.0293(8) 0.0417(9) 0.0423(10) -0.0115(7) -0.0041(7) -0.0037(7) Cu3 0.0308(8) 0.0379(9) 0.0437(10) -0.0105(7) -0.0001(7) 0.0041(7) I1 0.0869(8) 0.0329(5) 0.0490(6) -0.0052(4) -0.0082(5) -0.0079(5) I2 0.0411(5) 0.0551(6) 0.0478(6) -0.0083(4) -0.0101(4) -0.0074(4) I3 0.0464(6) 0.0624(7) 0.0583(7) -0.0099(5) 0.0016(5) 0.0224(5) B1 0.031(7) 0.020(6) 0.045(9) -0.008(6) 0.000(6) 0.001(6) N1 0.025(5) 0.033(6) 0.040(6) -0.010(5) 0.003(4) -0.002(4) N2 0.015(4) 0.029(5) 0.049(7) -0.008(5) 0.001(4) 0.008(4) N3 0.022(5) 0.021(5) 0.049(7) -0.005(5) 0.002(4) 0.008(4) N4 0.025(5) 0.031(6) 0.042(7) -0.001(5) 0.007(4) 0.007(4) N5 0.030(5) 0.053(7) 0.020(6) -0.003(5) -0.001(4) -0.001(5) N6 0.024(5) 0.031(5) 0.042(7) 0.002(5) -0.007(4) 0.008(4) N7 0.053(7) 0.037(6) 0.045(7) -0.013(5) 0.010(5) -0.009(5) C1 0.020(6) 0.048(8) 0.048(9) -0.006(7) 0.010(5) -0.003(5) C2 0.019(6) 0.068(10) 0.044(8) -0.007(7) -0.008(5) -0.008(6) C3 0.033(7) 0.051(8) 0.036(8) -0.012(6) -0.003(5) -0.008(6) C4 0.038(7) 0.038(7) 0.064(10) 0.008(7) -0.018(7) -0.008(6) C5 0.018(6) 0.060(9) 0.054(9) -0.014(7) 0.002(6) 0.005(6) C6 0.029(6) 0.026(6) 0.068(10) -0.024(6) 0.000(6) -0.005(5) C7 0.042(8) 0.042(8) 0.060(10) -0.019(7) 0.000(7) -0.003(6) C8 0.033(7) 0.028(7) 0.059(10) -0.002(6) 0.004(6) 0.012(5) C9 0.065(10) 0.052(9) 0.096(14) -0.044(9) -0.035(9) 0.000(8) C10 0.066(10) 0.021(7) 0.097(14) 0.001(8) -0.013(9) 0.012(7) C11 0.045(8) 0.037(7) 0.032(8) -0.001(6) -0.006(6) -0.004(6) C12 0.046(8) 0.052(8) 0.030(7) 0.001(6) 0.003(6) -0.005(7) C13 0.031(7) 0.041(7) 0.038(8) -0.003(6) 0.010(5) 0.003(6) C14 0.036(7) 0.045(8) 0.048(9) -0.008(7) -0.005(6) 0.009(6) C15 0.070(11) 0.057(10) 0.053(10) 0.006(8) -0.021(8) 0.010(8) C16 0.067(10) 0.050(9) 0.055(10) -0.012(8) 0.017(8) -0.005(8) C17 0.096(15) 0.048(10) 0.090(15) -0.019(10) -0.017(11) 0.007(9) C18 0.096(14) 0.076(12) 0.036(9) -0.020(8) 0.010(9) -0.001(10) C19 0.064(12) 0.107(16) 0.061(12) -0.020(11) -0.007(9) 0.005(11) C20 0.065(10) 0.053(9) 0.070(12) -0.020(8) -0.012(8) -0.013(8) C21 0.086(14) 0.055(11) 0.118(18) -0.044(11) -0.018(12) 0.013(10) C22 0.071(12) 0.091(14) 0.082(14) -0.017(11) 0.019(10) -0.053(11) C23 0.064(11) 0.133(19) 0.103(17) -0.041(14) 0.005(11) -0.063(13) C24 0.12(3) 0.12(3) 0.06(2) -0.06(2) 0.07(2) -0.11(3) Cl1 0.048(4) 0.031(3) 0.073(5) -0.012(3) 0.031(4) 0.012(3) Cl2 0.064(5) 0.040(4) 0.057(5) 0.001(3) 0.006(4) 0.030(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 Mo1 N5 2.287(10) . ? Mo1 N3 2.293(9) . ? Mo1 N1 2.294(9) . ? Mo1 S3 2.313(3) . ? Mo1 S1 2.323(3) . ? Mo1 S2 2.332(3) . ? Mo1 Cu1 2.637(2) . ? Mo1 Cu3 2.640(2) . ? Mo1 Cu2 2.6445(19) . ? S1 Cu1 2.199(4) . ? S1 Cu3 2.208(3) . ? S2 Cu1 2.200(4) . ? S2 Cu2 2.206(3) . ? S3 Cu2 2.202(4) . ? S3 Cu3 2.211(4) . ? Cu1 I1 2.4461(19) . ? Cu1 Cu3 2.887(2) . ? Cu1 Cu2 2.892(2) . ? Cu2 I2 2.4471(18) . ? Cu2 Cu3 2.906(2) . ? Cu3 I3 2.4571(19) . ? B1 N6 1.518(18) . ? B1 N4 1.520(18) . ? B1 N2 1.543(16) . ? B1 H1 1.25(12) . ? N1 N2 1.330(13) . ? N1 C1 1.364(15) . ? N2 C3 1.357(15) . ? N3 C6 1.373(15) . ? N3 N4 1.395(13) . ? N4 C8 1.345(17) . ? N5 C11 1.340(17) . ? N5 N6 1.380(13) . ? N6 C13 1.351(16) . ? N7 C22 1.491(18) . ? N7 C18 1.504(19) . ? N7 C20 1.522(19) . ? N7 C16 1.562(18) . ? C1 C2 1.404(17) . ? C1 C4 1.486(18) . ? C2 C3 1.321(19) . ? C2 H2 0.9400 . ? C3 C5 1.539(18) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.432(19) . ? C6 C9 1.45(2) . ? C7 C8 1.34(2) . ? C7 H7 0.9400 . ? C8 C10 1.511(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.412(18) . ? C11 C14 1.499(18) . ? C12 C13 1.314(18) . ? C12 H12 0.9400 . ? C13 C15 1.530(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.51(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.49(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 C21 1.51(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.57(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 Cl1 1.66(3) . ? C24 Cl2 1.86(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? 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 N5 Mo1 N3 82.0(4) . . ? N5 Mo1 N1 81.1(4) . . ? N3 Mo1 N1 78.7(3) . . ? N5 Mo1 S3 85.4(3) . . ? N3 Mo1 S3 86.5(2) . . ? N1 Mo1 S3 161.1(3) . . ? N5 Mo1 S1 86.2(3) . . ? N3 Mo1 S1 163.5(3) . . ? N1 Mo1 S1 88.1(3) . . ? S3 Mo1 S1 104.05(12) . . ? N5 Mo1 S2 164.6(3) . . ? N3 Mo1 S2 86.0(3) . . ? N1 Mo1 S2 87.1(3) . . ? S3 Mo1 S2 103.56(12) . . ? S1 Mo1 S2 103.37(12) . . ? N5 Mo1 Cu1 138.4(3) . . ? N3 Mo1 Cu1 138.0(3) . . ? N1 Mo1 Cu1 94.5(3) . . ? S3 Mo1 Cu1 104.36(10) . . ? S1 Mo1 Cu1 52.18(9) . . ? S2 Mo1 Cu1 52.13(9) . . ? N5 Mo1 Cu3 91.0(3) . . ? N3 Mo1 Cu3 138.9(2) . . ? N1 Mo1 Cu3 140.3(3) . . ? S3 Mo1 Cu3 52.52(9) . . ? S1 Mo1 Cu3 52.36(9) . . ? S2 Mo1 Cu3 104.42(10) . . ? Cu1 Mo1 Cu3 66.34(6) . . ? N5 Mo1 Cu2 137.5(2) . . ? N3 Mo1 Cu2 91.8(3) . . ? N1 Mo1 Cu2 139.0(3) . . ? S3 Mo1 Cu2 52.23(10) . . ? S1 Mo1 Cu2 104.67(10) . . ? S2 Mo1 Cu2 52.18(8) . . ? Cu1 Mo1 Cu2 66.41(6) . . ? Cu3 Mo1 Cu2 66.73(6) . . ? Cu1 S1 Cu3 81.84(12) . . ? Cu1 S1 Mo1 71.27(11) . . ? Cu3 S1 Mo1 71.21(10) . . ? Cu1 S2 Cu2 82.05(12) . . ? Cu1 S2 Mo1 71.08(11) . . ? Cu2 S2 Mo1 71.23(11) . . ? Cu2 S3 Cu3 82.38(13) . . ? Cu2 S3 Mo1 71.65(10) . . ? Cu3 S3 Mo1 71.36(10) . . ? S1 Cu1 S2 112.23(13) . . ? S1 Cu1 I1 125.64(11) . . ? S2 Cu1 I1 121.90(11) . . ? S1 Cu1 Mo1 56.56(9) . . ? S2 Cu1 Mo1 56.79(9) . . ? I1 Cu1 Mo1 174.38(8) . . ? S1 Cu1 Cu3 49.21(9) . . ? S2 Cu1 Cu3 100.41(10) . . ? I1 Cu1 Cu3 119.78(8) . . ? Mo1 Cu1 Cu3 56.88(5) . . ? S1 Cu1 Cu2 100.41(10) . . ? S2 Cu1 Cu2 49.07(9) . . ? I1 Cu1 Cu2 117.73(7) . . ? Mo1 Cu1 Cu2 56.93(5) . . ? Cu3 Cu1 Cu2 60.38(6) . . ? S3 Cu2 S2 111.73(13) . . ? S3 Cu2 I2 122.19(10) . . ? S2 Cu2 I2 125.18(11) . . ? S3 Cu2 Mo1 56.12(9) . . ? S2 Cu2 Mo1 56.60(9) . . ? I2 Cu2 Mo1 178.21(8) . . ? S3 Cu2 Cu1 99.54(10) . . ? S2 Cu2 Cu1 48.89(9) . . ? I2 Cu2 Cu1 124.06(7) . . ? Mo1 Cu2 Cu1 56.66(5) . . ? S3 Cu2 Cu3 48.93(10) . . ? S2 Cu2 Cu3 99.68(11) . . ? I2 Cu2 Cu3 122.09(7) . . ? Mo1 Cu2 Cu3 56.55(5) . . ? Cu1 Cu2 Cu3 59.72(6) . . ? S1 Cu3 S3 111.60(13) . . ? S1 Cu3 I3 124.75(11) . . ? S3 Cu3 I3 122.71(11) . . ? S1 Cu3 Mo1 56.42(9) . . ? S3 Cu3 Mo1 56.13(9) . . ? I3 Cu3 Mo1 178.83(8) . . ? S1 Cu3 Cu1 48.94(10) . . ? S3 Cu3 Cu1 99.49(11) . . ? I3 Cu3 Cu1 123.89(7) . . ? Mo1 Cu3 Cu1 56.78(5) . . ? S1 Cu3 Cu2 99.77(11) . . ? S3 Cu3 Cu2 48.69(10) . . ? I3 Cu3 Cu2 122.55(7) . . ? Mo1 Cu3 Cu2 56.71(5) . . ? Cu1 Cu3 Cu2 59.90(6) . . ? N6 B1 N4 110.3(10) . . ? N6 B1 N2 109.2(10) . . ? N4 B1 N2 107.2(11) . . ? N6 B1 H1 100(6) . . ? N4 B1 H1 112(6) . . ? N2 B1 H1 117(6) . . ? N2 N1 C1 108.3(9) . . ? N2 N1 Mo1 119.3(7) . . ? C1 N1 Mo1 132.2(8) . . ? N1 N2 C3 108.0(10) . . ? N1 N2 B1 123.4(9) . . ? C3 N2 B1 128.6(10) . . ? C6 N3 N4 107.6(9) . . ? C6 N3 Mo1 131.9(8) . . ? N4 N3 Mo1 120.1(8) . . ? C8 N4 N3 109.4(10) . . ? C8 N4 B1 130.5(10) . . ? N3 N4 B1 120.0(9) . . ? C11 N5 N6 106.6(10) . . ? C11 N5 Mo1 133.6(8) . . ? N6 N5 Mo1 119.8(8) . . ? C13 N6 N5 109.3(10) . . ? C13 N6 B1 128.9(10) . . ? N5 N6 B1 121.4(10) . . ? C22 N7 C18 107.0(12) . . ? C22 N7 C20 112.2(13) . . ? C18 N7 C20 111.6(12) . . ? C22 N7 C16 110.0(12) . . ? C18 N7 C16 108.9(12) . . ? C20 N7 C16 107.1(11) . . ? N1 C1 C2 107.2(11) . . ? N1 C1 C4 127.2(11) . . ? C2 C1 C4 125.7(11) . . ? C3 C2 C1 106.1(11) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? C2 C3 N2 110.3(12) . . ? C2 C3 C5 128.8(12) . . ? N2 C3 C5 120.9(11) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 105.7(11) . . ? N3 C6 C9 127.7(11) . . ? C7 C6 C9 126.5(12) . . ? C8 C7 C6 108.7(12) . . ? C8 C7 H7 125.7 . . ? C6 C7 H7 125.7 . . ? C7 C8 N4 108.6(11) . . ? C7 C8 C10 128.3(13) . . ? N4 C8 C10 123.0(13) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 107.6(12) . . ? N5 C11 C14 127.6(12) . . ? C12 C11 C14 124.7(13) . . ? C13 C12 C11 108.1(13) . . ? C13 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? C12 C13 N6 108.4(11) . . ? C12 C13 C15 128.5(13) . . ? N6 C13 C15 123.1(12) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N7 115.6(14) . . ? C17 C16 H16A 108.4 . . ? N7 C16 H16A 108.4 . . ? C17 C16 H16B 108.4 . . ? N7 C16 H16B 108.4 . . ? H16A C16 H16B 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N7 115.8(14) . . ? C19 C18 H18A 108.3 . . ? N7 C18 H18A 108.3 . . ? C19 C18 H18B 108.3 . . ? N7 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N7 115.7(15) . . ? C21 C20 H20A 108.4 . . ? N7 C20 H20A 108.4 . . ? C21 C20 H20B 108.4 . . ? N7 C20 H20B 108.4 . . ? H20A C20 H20B 107.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 C23 116.1(14) . . ? N7 C22 H22A 108.3 . . ? C23 C22 H22A 108.3 . . ? N7 C22 H22B 108.3 . . ? C23 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl1 C24 Cl2 110.8(19) . . ? Cl1 C24 H24A 109.5 . . ? Cl2 C24 H24A 109.5 . . ? Cl1 C24 H24B 109.5 . . ? Cl2 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.931 _refine_diff_density_min -1.567 _refine_diff_density_rms 0.253 data_5^.^CH~2~Cl~2~ _database_code_depnum_ccdc_archive 'CCDC 928968' #TrackingRef 'ZhangZY.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H22 B Cu I Mo N6 O S2, C8 H20 N, C H2 Cl2' _chemical_formula_sum 'C24 H44 B Cl2 Cu I Mo N7 O S2' _chemical_formula_weight 878.87 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_HALL 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.811(4) _cell_length_b 17.312(4) _cell_length_c 10.749(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3500.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 16685 _cell_measurement_theta_min 3.0216 _cell_measurement_theta_max 27.6139 _exptl_crystal_description Needle _exptl_crystal_colour Green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 2.149 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7041 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18815 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7050 _reflns_number_gt 5756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 7050 _refine_ls_number_parameters 370 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.18889(3) 0.61041(3) 0.26723(5) 0.02784(12) Uani 1 1 d . . . S1 S 0.15183(10) 0.73051(11) 0.31775(17) 0.0383(4) Uani 1 1 d . . . S2 S 0.17588(10) 0.54076(11) 0.44425(16) 0.0382(4) Uani 1 1 d . . . Cu1 Cu 0.12589(5) 0.65283(5) 0.46971(8) 0.0402(2) Uani 1 1 d . . . I1 I 0.05444(3) 0.69158(3) 0.65040(5) 0.05473(16) Uani 1 1 d . . . O1 O 0.1206(2) 0.5770(3) 0.1785(4) 0.0351(11) Uani 1 1 d . . . B1 B 0.3537(4) 0.5952(4) 0.1286(7) 0.0330(17) Uani 1 1 d . . . H1 H 0.408(4) 0.585(4) 0.085(6) 0.040 Uiso 1 1 d . . . N1 N 0.2535(3) 0.5097(3) 0.1953(5) 0.0305(12) Uani 1 1 d . . . N2 N 0.3189(2) 0.5162(3) 0.1427(6) 0.0310(12) Uani 1 1 d . . . N3 N 0.2366(3) 0.6604(3) 0.0889(5) 0.0284(11) Uani 1 1 d . . . N4 N 0.3056(3) 0.6489(3) 0.0532(5) 0.0294(12) Uani 1 1 d . . . N5 N 0.3059(3) 0.6432(3) 0.3325(5) 0.0322(13) Uani 1 1 d . . . N6 N 0.3643(2) 0.6293(3) 0.2575(5) 0.0298(11) Uani 1 1 d . . . N7 N -0.1233(3) 0.5754(3) 0.2889(5) 0.0372(13) Uani 1 1 d . . . C1 C 0.2363(4) 0.4341(4) 0.1915(6) 0.0362(16) Uani 1 1 d . . . C2 C 0.2925(4) 0.3933(4) 0.1374(8) 0.0455(19) Uani 1 1 d . . . H2 H 0.2945 0.3397 0.1235 0.055 Uiso 1 1 calc R . . C3 C 0.3440(4) 0.4462(4) 0.1083(7) 0.0402(17) Uani 1 1 d . . . C4 C 0.1678(4) 0.4011(4) 0.2370(7) 0.0430(19) Uani 1 1 d . . . H4A H 0.1711 0.3914 0.3257 0.064 Uiso 1 1 calc R . . H4B H 0.1582 0.3530 0.1939 0.064 Uiso 1 1 calc R . . H4C H 0.1296 0.4374 0.2210 0.064 Uiso 1 1 calc R . . C5 C 0.4135(4) 0.4347(5) 0.0472(10) 0.061(2) Uani 1 1 d . . . H5A H 0.4119 0.4556 -0.0364 0.091 Uiso 1 1 calc R . . H5B H 0.4241 0.3799 0.0434 0.091 Uiso 1 1 calc R . . H5C H 0.4502 0.4609 0.0945 0.091 Uiso 1 1 calc R . . C6 C 0.2057(3) 0.7040(4) 0.0015(6) 0.0297(14) Uani 1 1 d . . . C7 C 0.2565(3) 0.7209(4) -0.0898(6) 0.0343(15) Uani 1 1 d . . . H7 H 0.2497 0.7514 -0.1612 0.041 Uiso 1 1 calc R . . C8 C 0.3177(3) 0.6845(4) -0.0550(7) 0.0343(16) Uani 1 1 d . . . C9 C 0.1301(4) 0.7274(5) 0.0027(7) 0.0440(19) Uani 1 1 d . . . H9A H 0.1012 0.6847 0.0320 0.066 Uiso 1 1 calc R . . H9B H 0.1155 0.7415 -0.0808 0.066 Uiso 1 1 calc R . . H9C H 0.1240 0.7713 0.0577 0.066 Uiso 1 1 calc R . . C10 C 0.3897(4) 0.6829(5) -0.1186(8) 0.052(2) Uani 1 1 d . . . H10A H 0.4268 0.6893 -0.0569 0.078 Uiso 1 1 calc R . . H10B H 0.3923 0.7246 -0.1787 0.078 Uiso 1 1 calc R . . H10C H 0.3958 0.6339 -0.1609 0.078 Uiso 1 1 calc R . . C11 C 0.3322(4) 0.6716(4) 0.4391(7) 0.0363(16) Uani 1 1 d . . . C12 C 0.4054(4) 0.6775(4) 0.4323(7) 0.0434(19) Uani 1 1 d . . . H12 H 0.4359 0.6965 0.4946 0.052 Uiso 1 1 calc R . . C13 C 0.4252(3) 0.6503(4) 0.3171(7) 0.0344(16) Uani 1 1 d . . . C14 C 0.2877(4) 0.6936(5) 0.5492(7) 0.050(2) Uani 1 1 d . . . H14A H 0.2551 0.7346 0.5257 0.074 Uiso 1 1 calc R . . H14B H 0.3182 0.7116 0.6159 0.074 Uiso 1 1 calc R . . H14C H 0.2608 0.6491 0.5772 0.074 Uiso 1 1 calc R . . C15 C 0.4967(3) 0.6402(4) 0.2595(9) 0.0484(18) Uani 1 1 d . . . H15A H 0.5071 0.5855 0.2516 0.073 Uiso 1 1 calc R . . H15B H 0.5324 0.6645 0.3117 0.073 Uiso 1 1 calc R . . H15C H 0.4971 0.6640 0.1778 0.073 Uiso 1 1 calc R . . C16 C -0.1627(4) 0.5009(4) 0.2747(8) 0.0460(17) Uani 1 1 d . . . H16A H -0.1861 0.5011 0.1933 0.055 Uiso 1 1 calc R . . H16B H -0.1278 0.4588 0.2741 0.055 Uiso 1 1 calc R . . C17 C -0.2175(5) 0.4827(5) 0.3711(9) 0.072(3) Uani 1 1 d . . . H17A H -0.2399 0.4337 0.3515 0.108 Uiso 1 1 calc R . . H17B H -0.2531 0.5232 0.3722 0.108 Uiso 1 1 calc R . . H17C H -0.1950 0.4794 0.4521 0.108 Uiso 1 1 calc R . . C18 C -0.0723(4) 0.5813(4) 0.1829(8) 0.052(2) Uani 1 1 d . . . H18A H -0.0985 0.5735 0.1050 0.062 Uiso 1 1 calc R . . H18B H -0.0374 0.5395 0.1900 0.062 Uiso 1 1 calc R . . C19 C -0.0333(4) 0.6569(6) 0.1757(11) 0.081(3) Uani 1 1 d . . . H19A H -0.0027 0.6570 0.1031 0.121 Uiso 1 1 calc R . . H19B H -0.0048 0.6637 0.2501 0.121 Uiso 1 1 calc R . . H19C H -0.0674 0.6988 0.1692 0.121 Uiso 1 1 calc R . . C20 C -0.1767(4) 0.6418(4) 0.2849(9) 0.052(2) Uani 1 1 d . . . H20A H -0.2123 0.6337 0.3502 0.062 Uiso 1 1 calc R . . H20B H -0.1517 0.6901 0.3038 0.062 Uiso 1 1 calc R . . C21 C -0.2144(5) 0.6508(5) 0.1627(11) 0.072(3) Uani 1 1 d . . . H21A H -0.2469 0.6941 0.1673 0.108 Uiso 1 1 calc R . . H21B H -0.2408 0.6040 0.1444 0.108 Uiso 1 1 calc R . . H21C H -0.1798 0.6600 0.0974 0.108 Uiso 1 1 calc R . . C22 C -0.0871(5) 0.5803(7) 0.4126(9) 0.077(3) Uani 1 1 d . . . H22A H -0.1234 0.5791 0.4780 0.092 Uiso 1 1 calc R . . H22B H -0.0625 0.6300 0.4183 0.092 Uiso 1 1 calc R . . C23 C -0.0338(6) 0.5159(8) 0.4370(12) 0.111(5) Uani 1 1 d . . . H23A H -0.0133 0.5224 0.5191 0.167 Uiso 1 1 calc R . . H23B H 0.0037 0.5179 0.3750 0.167 Uiso 1 1 calc R . . H23C H -0.0576 0.4663 0.4323 0.167 Uiso 1 1 calc R . . C24 C 0.6401(5) 0.5339(6) -0.0364(9) 0.067(3) Uani 1 1 d . . . H24A H 0.6554 0.4888 -0.0845 0.080 Uiso 1 1 calc R . . H24B H 0.6764 0.5740 -0.0456 0.080 Uiso 1 1 calc R . . Cl1 Cl 0.63332(14) 0.50834(18) 0.1198(3) 0.0874(9) Uani 1 1 d . . . Cl2 Cl 0.55955(13) 0.56795(17) -0.0964(3) 0.0837(8) 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 Mo1 0.0264(2) 0.0327(3) 0.0244(3) 0.0013(3) -0.0005(2) 0.0018(2) S1 0.0409(10) 0.0394(10) 0.0346(9) -0.0013(8) -0.0001(8) 0.0115(8) S2 0.0425(10) 0.0429(10) 0.0293(9) 0.0087(8) 0.0041(7) 0.0053(8) Cu1 0.0379(5) 0.0522(5) 0.0305(4) -0.0012(4) 0.0031(4) 0.0098(4) I1 0.0589(3) 0.0714(4) 0.0339(2) -0.0020(3) 0.0073(3) 0.0222(3) O1 0.034(2) 0.044(3) 0.028(3) 0.005(2) -0.0017(19) -0.001(2) B1 0.034(4) 0.039(4) 0.026(4) -0.002(3) -0.001(3) 0.001(3) N1 0.028(3) 0.029(3) 0.035(3) 0.002(2) 0.001(2) -0.001(2) N2 0.030(3) 0.033(3) 0.031(3) 0.003(3) 0.003(3) -0.002(2) N3 0.027(3) 0.035(3) 0.023(3) 0.001(2) 0.001(2) -0.003(2) N4 0.028(3) 0.032(3) 0.028(3) 0.007(3) 0.001(2) -0.005(2) N5 0.034(3) 0.033(3) 0.030(3) -0.007(3) -0.006(2) 0.008(2) N6 0.022(2) 0.035(3) 0.032(3) -0.002(3) -0.002(2) -0.0011(19) N7 0.041(3) 0.034(3) 0.037(4) -0.006(3) 0.000(3) 0.001(2) C1 0.039(4) 0.031(3) 0.039(4) -0.003(3) -0.003(3) -0.006(3) C2 0.058(4) 0.019(3) 0.060(5) -0.006(4) 0.006(4) -0.003(3) C3 0.042(4) 0.033(4) 0.046(5) -0.006(3) 0.002(3) 0.004(3) C4 0.044(4) 0.036(4) 0.049(5) 0.003(4) 0.003(3) -0.013(3) C5 0.058(5) 0.038(5) 0.086(7) 0.000(5) 0.026(5) 0.012(4) C6 0.031(3) 0.033(4) 0.025(3) 0.003(3) -0.006(3) 0.002(3) C7 0.038(4) 0.040(4) 0.025(3) 0.012(3) -0.001(3) -0.007(3) C8 0.032(4) 0.033(4) 0.038(4) 0.008(3) -0.002(3) -0.006(3) C9 0.047(4) 0.054(5) 0.031(4) 0.013(4) 0.002(3) 0.012(4) C10 0.055(5) 0.064(6) 0.036(4) 0.013(4) 0.005(4) -0.002(4) C11 0.031(4) 0.044(4) 0.034(4) 0.000(3) -0.007(3) 0.004(3) C12 0.045(4) 0.040(4) 0.046(5) -0.005(4) -0.018(4) -0.003(3) C13 0.023(3) 0.037(4) 0.043(4) 0.006(3) -0.010(3) -0.002(3) C14 0.053(5) 0.059(5) 0.037(4) -0.024(4) -0.010(4) 0.014(4) C15 0.024(3) 0.057(4) 0.064(5) 0.006(5) -0.008(4) -0.011(3) C16 0.063(5) 0.038(4) 0.037(4) -0.005(4) 0.004(4) -0.004(3) C17 0.099(8) 0.064(6) 0.053(6) 0.013(5) 0.007(6) -0.023(5) C18 0.049(5) 0.044(4) 0.062(6) 0.000(4) 0.016(4) 0.007(4) C19 0.046(5) 0.089(7) 0.107(9) 0.019(7) 0.025(6) -0.011(5) C20 0.053(5) 0.030(3) 0.072(7) -0.002(4) 0.018(4) 0.004(3) C21 0.057(5) 0.062(6) 0.098(8) 0.026(6) -0.001(6) 0.018(4) C22 0.074(7) 0.102(8) 0.054(6) 0.007(6) -0.029(5) -0.007(6) C23 0.090(9) 0.135(11) 0.109(10) 0.048(9) -0.052(8) -0.030(8) C24 0.056(5) 0.073(6) 0.071(6) -0.009(6) 0.012(5) 0.006(5) Cl1 0.0784(18) 0.111(2) 0.073(2) -0.0190(16) 0.0087(14) 0.0114(15) Cl2 0.0601(15) 0.0902(19) 0.101(2) -0.0033(17) -0.0012(14) 0.0089(13) _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 Mo1 O1 1.702(4) . ? Mo1 S1 2.2592(19) . ? Mo1 N1 2.262(5) . ? Mo1 S2 2.2659(18) . ? Mo1 N3 2.286(5) . ? Mo1 N5 2.378(5) . ? Mo1 Cu1 2.5847(11) . ? S1 Cu1 2.171(2) . ? S2 Cu1 2.173(2) . ? Cu1 I1 2.4553(10) . ? B1 N6 1.520(9) . ? B1 N2 1.523(9) . ? B1 N4 1.529(9) . ? B1 H1 1.13(7) . ? N1 C1 1.348(8) . ? N1 N2 1.360(7) . ? N2 C3 1.351(8) . ? N3 C6 1.338(8) . ? N3 N4 1.369(7) . ? N4 C8 1.336(8) . ? N5 C11 1.341(8) . ? N5 N6 1.384(7) . ? N6 C13 1.362(8) . ? N7 C18 1.493(9) . ? N7 C22 1.495(10) . ? N7 C16 1.496(8) . ? N7 C20 1.528(9) . ? C1 C2 1.398(10) . ? C1 C4 1.492(9) . ? C2 C3 1.370(9) . ? C2 H2 0.9400 . ? C3 C5 1.477(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.400(9) . ? C6 C9 1.480(9) . ? C7 C8 1.366(9) . ? C7 H7 0.9400 . ? C8 C10 1.516(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.383(10) . ? C11 C14 1.499(10) . ? C12 C13 1.377(11) . ? C12 H12 0.9400 . ? C13 C15 1.491(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.495(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.503(11) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 C21 1.500(14) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.523(15) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 Cl1 1.740(10) . ? C24 Cl2 1.749(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? 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 O1 Mo1 S1 102.41(16) . . ? O1 Mo1 N1 87.2(2) . . ? S1 Mo1 N1 163.26(14) . . ? O1 Mo1 S2 102.02(16) . . ? S1 Mo1 S2 104.75(7) . . ? N1 Mo1 S2 86.25(14) . . ? O1 Mo1 N3 87.43(19) . . ? S1 Mo1 N3 88.51(14) . . ? N1 Mo1 N3 78.17(19) . . ? S2 Mo1 N3 161.41(14) . . ? O1 Mo1 N5 160.9(2) . . ? S1 Mo1 N5 89.71(14) . . ? N1 Mo1 N5 77.75(18) . . ? S2 Mo1 N5 88.80(15) . . ? N3 Mo1 N5 78.12(18) . . ? O1 Mo1 Cu1 102.86(15) . . ? S1 Mo1 Cu1 52.74(5) . . ? N1 Mo1 Cu1 138.86(14) . . ? S2 Mo1 Cu1 52.74(5) . . ? N3 Mo1 Cu1 141.08(13) . . ? N5 Mo1 Cu1 96.19(13) . . ? Cu1 S1 Mo1 71.35(6) . . ? Cu1 S2 Mo1 71.18(6) . . ? S1 Cu1 S2 111.16(8) . . ? S1 Cu1 I1 123.29(6) . . ? S2 Cu1 I1 125.47(6) . . ? S1 Cu1 Mo1 55.91(5) . . ? S2 Cu1 Mo1 56.08(5) . . ? I1 Cu1 Mo1 174.09(4) . . ? N6 B1 N2 108.3(6) . . ? N6 B1 N4 108.9(5) . . ? N2 B1 N4 110.2(5) . . ? N6 B1 H1 109(3) . . ? N2 B1 H1 107(3) . . ? N4 B1 H1 113(3) . . ? C1 N1 N2 106.5(5) . . ? C1 N1 Mo1 129.1(4) . . ? N2 N1 Mo1 124.4(4) . . ? C3 N2 N1 110.8(5) . . ? C3 N2 B1 128.9(6) . . ? N1 N2 B1 120.3(5) . . ? C6 N3 N4 107.3(5) . . ? C6 N3 Mo1 129.2(4) . . ? N4 N3 Mo1 123.5(4) . . ? C8 N4 N3 109.8(5) . . ? C8 N4 B1 129.9(6) . . ? N3 N4 B1 120.1(5) . . ? C11 N5 N6 105.6(5) . . ? C11 N5 Mo1 132.9(4) . . ? N6 N5 Mo1 121.4(4) . . ? C13 N6 N5 110.3(6) . . ? C13 N6 B1 130.0(6) . . ? N5 N6 B1 119.7(5) . . ? C18 N7 C22 112.5(6) . . ? C18 N7 C16 107.4(6) . . ? C22 N7 C16 111.4(6) . . ? C18 N7 C20 110.5(6) . . ? C22 N7 C20 106.4(6) . . ? C16 N7 C20 108.7(5) . . ? N1 C1 C2 108.8(6) . . ? N1 C1 C4 124.7(6) . . ? C2 C1 C4 126.6(6) . . ? C3 C2 C1 107.0(6) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? N2 C3 C2 106.8(6) . . ? N2 C3 C5 123.5(6) . . ? C2 C3 C5 129.6(7) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 108.3(5) . . ? N3 C6 C9 124.4(6) . . ? C7 C6 C9 127.2(6) . . ? C8 C7 C6 106.7(6) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? N4 C8 C7 107.9(6) . . ? N4 C8 C10 122.5(6) . . ? C7 C8 C10 129.6(6) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 110.5(6) . . ? N5 C11 C14 124.1(6) . . ? C12 C11 C14 125.4(7) . . ? C13 C12 C11 106.9(6) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? N6 C13 C12 106.7(6) . . ? N6 C13 C15 122.2(7) . . ? C12 C13 C15 131.1(7) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N7 116.9(6) . . ? C17 C16 H16A 108.1 . . ? N7 C16 H16A 108.1 . . ? C17 C16 H16B 108.1 . . ? N7 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 114.3(7) . . ? N7 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? N7 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N7 114.4(7) . . ? C21 C20 H20A 108.7 . . ? N7 C20 H20A 108.7 . . ? C21 C20 H20B 108.7 . . ? N7 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 C23 114.3(9) . . ? N7 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N7 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl1 C24 Cl2 112.2(5) . . ? Cl1 C24 H24A 109.2 . . ? Cl2 C24 H24A 109.2 . . ? Cl1 C24 H24B 109.2 . . ? Cl2 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.660 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.116 data_6 _database_code_depnum_ccdc_archive 'CCDC 928969' #TrackingRef 'ZhangZY.cif' #============================================================================== # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H22 B Cu Mo N7 O S2, C8 H20 N' _chemical_formula_sum 'C24 H42 B Cu Mo N8 O S2' _chemical_formula_weight 693.07 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6883(17) _cell_length_b 10.542(2) _cell_length_c 19.244(4) _cell_angle_alpha 81.38(3) _cell_angle_beta 85.90(3) _cell_angle_gamma 66.92(3) _cell_volume 1603.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7869 _cell_measurement_theta_min 3.1686 _cell_measurement_theta_max 27.4894 _exptl_crystal_description Block _exptl_crystal_colour Dark-red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 1.215 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5755 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12327 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5600 _reflns_number_gt 4101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Besides, several most disagreeable reflections were omitted. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5600 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.62722(6) 0.10206(5) 0.25950(2) 0.02502(17) Uani 1 1 d . . . S1 S 0.44206(19) 0.30940(15) 0.28959(7) 0.0347(4) Uani 1 1 d . . . S2 S 0.56652(18) 0.10113(15) 0.14646(7) 0.0336(4) Uani 1 1 d . . . Cu1 Cu 0.42158(8) 0.30666(7) 0.17781(4) 0.0323(2) Uani 1 1 d . . . O1 O 0.8062(4) 0.1305(4) 0.2483(2) 0.0366(10) Uani 1 1 d . . . B1 B 0.6493(8) -0.1887(7) 0.3754(3) 0.0329(15) Uani 1 1 d . . . H1 H 0.665(7) -0.293(6) 0.414(3) 0.039 Uiso 1 1 d . . . N1 N 0.7938(5) -0.1306(5) 0.2635(2) 0.0303(11) Uani 1 1 d . . . N2 N 0.7825(6) -0.2294(5) 0.3161(2) 0.0309(11) Uani 1 1 d . . . N3 N 0.6932(5) 0.0357(5) 0.3747(2) 0.0310(11) Uani 1 1 d . . . N4 N 0.6819(6) -0.0818(5) 0.4128(2) 0.0317(11) Uani 1 1 d . . . N5 N 0.4320(5) -0.0007(5) 0.2987(2) 0.0291(10) Uani 1 1 d . . . N6 N 0.4753(5) -0.1221(4) 0.3444(2) 0.0276(10) Uani 1 1 d . . . N7 N 0.2083(7) 0.5580(6) 0.0809(3) 0.0483(14) Uani 1 1 d . . . N8 N 0.6338(6) -0.3241(5) 0.1001(2) 0.0341(11) Uani 1 1 d . . . C1 C 0.9309(6) -0.1916(6) 0.2253(3) 0.0335(14) Uani 1 1 d . . . C2 C 1.0070(7) -0.3308(6) 0.2524(3) 0.0413(15) Uani 1 1 d . . . H2 H 1.1037 -0.3976 0.2349 0.050 Uiso 1 1 calc R . . C3 C 0.9122(7) -0.3515(6) 0.3102(3) 0.0389(15) Uani 1 1 d . . . C4 C 0.9907(7) -0.1166(6) 0.1642(3) 0.0415(15) Uani 1 1 d . . . H4A H 0.8953 -0.0425 0.1406 0.062 Uiso 1 1 calc R . . H4B H 1.0523 -0.1813 0.1315 0.062 Uiso 1 1 calc R . . H4C H 1.0631 -0.0773 0.1807 0.062 Uiso 1 1 calc R . . C5 C 0.9373(10) -0.4827(7) 0.3588(4) 0.069(2) Uani 1 1 d . . . H5A H 0.9470 -0.4682 0.4066 0.104 Uiso 1 1 calc R . . H5B H 1.0386 -0.5567 0.3453 0.104 Uiso 1 1 calc R . . H5C H 0.8424 -0.5083 0.3559 0.104 Uiso 1 1 calc R . . C6 C 0.7525(7) 0.0944(7) 0.4173(3) 0.0385(15) Uani 1 1 d . . . C7 C 0.7773(8) 0.0149(7) 0.4829(3) 0.0440(16) Uani 1 1 d . . . H7 H 0.8183 0.0324 0.5228 0.053 Uiso 1 1 calc R . . C8 C 0.7312(7) -0.0935(6) 0.4787(3) 0.0373(14) Uani 1 1 d . . . C9 C 0.7862(9) 0.2217(7) 0.3941(3) 0.0537(18) Uani 1 1 d . . . H9A H 0.8363 0.2172 0.3474 0.081 Uiso 1 1 calc R . . H9B H 0.8623 0.2284 0.4266 0.081 Uiso 1 1 calc R . . H9C H 0.6820 0.3027 0.3932 0.081 Uiso 1 1 calc R . . C10 C 0.7294(9) -0.2076(8) 0.5349(3) 0.0558(19) Uani 1 1 d . . . H10A H 0.6183 -0.2095 0.5388 0.084 Uiso 1 1 calc R . . H10B H 0.7589 -0.1912 0.5794 0.084 Uiso 1 1 calc R . . H10C H 0.8096 -0.2961 0.5230 0.084 Uiso 1 1 calc R . . C11 C 0.2697(7) 0.0352(6) 0.2839(3) 0.0330(13) Uani 1 1 d . . . C12 C 0.2107(7) -0.0608(6) 0.3196(3) 0.0363(14) Uani 1 1 d . . . H12 H 0.1020 -0.0591 0.3182 0.044 Uiso 1 1 calc R . . C13 C 0.3438(7) -0.1602(6) 0.3581(3) 0.0345(13) Uani 1 1 d . . . C14 C 0.1705(7) 0.1607(7) 0.2367(4) 0.0498(18) Uani 1 1 d . . . H14A H 0.1571 0.2430 0.2573 0.075 Uiso 1 1 calc R . . H14B H 0.0613 0.1597 0.2301 0.075 Uiso 1 1 calc R . . H14C H 0.2278 0.1619 0.1916 0.075 Uiso 1 1 calc R . . C15 C 0.3524(9) -0.2901(7) 0.4044(3) 0.0520(18) Uani 1 1 d . . . H15A H 0.4215 -0.3706 0.3820 0.078 Uiso 1 1 calc R . . H15B H 0.2406 -0.2895 0.4123 0.078 Uiso 1 1 calc R . . H15C H 0.4007 -0.2945 0.4491 0.078 Uiso 1 1 calc R . . C16 C 0.2830(7) 0.4649(6) 0.1165(3) 0.0304(13) Uani 1 1 d . . . C17 C 0.7024(8) -0.4805(6) 0.0968(3) 0.0423(15) Uani 1 1 d . . . H17A H 0.6123 -0.5137 0.1103 0.051 Uiso 1 1 calc R . . H17B H 0.7341 -0.4962 0.0480 0.051 Uiso 1 1 calc R . . C18 C 0.8516(9) -0.5677(8) 0.1428(4) 0.065(2) Uani 1 1 d . . . H18A H 0.9468 -0.5448 0.1261 0.098 Uiso 1 1 calc R . . H18B H 0.8787 -0.6655 0.1408 0.098 Uiso 1 1 calc R . . H18C H 0.8250 -0.5485 0.1909 0.098 Uiso 1 1 calc R . . C19 C 0.4798(7) -0.2623(7) 0.0535(3) 0.0436(16) Uani 1 1 d . . . H19A H 0.5163 -0.2786 0.0051 0.052 Uiso 1 1 calc R . . H19B H 0.4067 -0.3126 0.0686 0.052 Uiso 1 1 calc R . . C20 C 0.3789(9) -0.1092(7) 0.0536(4) 0.063(2) Uani 1 1 d . . . H20A H 0.3397 -0.0915 0.1010 0.095 Uiso 1 1 calc R . . H20B H 0.2838 -0.0799 0.0230 0.095 Uiso 1 1 calc R . . H20C H 0.4483 -0.0575 0.0368 0.095 Uiso 1 1 calc R . . C21 C 0.5886(8) -0.2913(7) 0.1740(3) 0.0455(16) Uani 1 1 d . . . H21A H 0.5401 -0.1900 0.1730 0.055 Uiso 1 1 calc R . . H21B H 0.6914 -0.3275 0.2014 0.055 Uiso 1 1 calc R . . C22 C 0.4670(9) -0.3497(7) 0.2115(3) 0.0554(19) Uani 1 1 d . . . H22A H 0.3672 -0.3193 0.1836 0.083 Uiso 1 1 calc R . . H22B H 0.4371 -0.3168 0.2569 0.083 Uiso 1 1 calc R . . H22C H 0.5188 -0.4505 0.2180 0.083 Uiso 1 1 calc R . . C23 C 0.7609(8) -0.2632(7) 0.0743(3) 0.0435(15) Uani 1 1 d . . . H23A H 0.8585 -0.3079 0.1049 0.052 Uiso 1 1 calc R . . H23B H 0.7129 -0.1642 0.0798 0.052 Uiso 1 1 calc R . . C24 C 0.8209(9) -0.2767(8) -0.0009(3) 0.0545(18) Uani 1 1 d . . . H24A H 0.8641 -0.3738 -0.0079 0.082 Uiso 1 1 calc R . . H24B H 0.9087 -0.2411 -0.0107 0.082 Uiso 1 1 calc R . . H24C H 0.7283 -0.2237 -0.0323 0.082 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 Mo1 0.0251(3) 0.0239(3) 0.0272(3) 0.00015(19) -0.00228(19) -0.0115(2) S1 0.0408(8) 0.0276(8) 0.0333(8) -0.0026(6) -0.0027(6) -0.0107(6) S2 0.0388(8) 0.0298(8) 0.0302(7) -0.0038(6) -0.0054(6) -0.0105(6) Cu1 0.0342(4) 0.0265(4) 0.0348(4) 0.0026(3) -0.0059(3) -0.0116(3) O1 0.0268(19) 0.041(2) 0.044(2) 0.0000(18) -0.0035(18) -0.0165(18) B1 0.038(4) 0.027(3) 0.032(4) 0.000(3) -0.003(3) -0.011(3) N1 0.027(2) 0.027(3) 0.037(3) -0.002(2) -0.001(2) -0.011(2) N2 0.034(2) 0.025(3) 0.031(2) 0.003(2) -0.003(2) -0.010(2) N3 0.030(2) 0.034(3) 0.029(2) -0.004(2) -0.001(2) -0.013(2) N4 0.036(3) 0.031(3) 0.024(2) 0.005(2) -0.003(2) -0.011(2) N5 0.024(2) 0.029(3) 0.037(3) 0.001(2) -0.002(2) -0.015(2) N6 0.032(2) 0.026(2) 0.024(2) 0.0027(19) 0.000(2) -0.013(2) N7 0.050(3) 0.044(3) 0.052(3) -0.012(3) -0.004(3) -0.017(3) N8 0.039(3) 0.029(3) 0.038(3) 0.000(2) -0.004(2) -0.019(2) C1 0.022(3) 0.038(3) 0.043(3) -0.012(3) 0.001(3) -0.012(3) C2 0.031(3) 0.033(3) 0.051(4) -0.010(3) 0.001(3) -0.001(3) C3 0.040(3) 0.025(3) 0.043(4) -0.001(3) -0.005(3) -0.004(3) C4 0.031(3) 0.043(4) 0.048(4) -0.010(3) 0.006(3) -0.011(3) C5 0.071(5) 0.035(4) 0.076(5) 0.004(4) 0.011(4) 0.000(4) C6 0.035(3) 0.050(4) 0.035(3) -0.008(3) -0.006(3) -0.018(3) C7 0.049(4) 0.051(4) 0.029(3) -0.006(3) -0.012(3) -0.014(3) C8 0.035(3) 0.043(4) 0.028(3) -0.002(3) -0.001(3) -0.009(3) C9 0.076(5) 0.051(4) 0.049(4) -0.009(3) -0.013(4) -0.038(4) C10 0.070(5) 0.060(5) 0.032(3) 0.009(3) -0.009(3) -0.024(4) C11 0.029(3) 0.036(3) 0.039(3) -0.008(3) 0.003(3) -0.018(3) C12 0.032(3) 0.041(4) 0.042(3) -0.009(3) 0.006(3) -0.021(3) C13 0.047(3) 0.034(3) 0.031(3) -0.007(2) 0.007(3) -0.024(3) C14 0.026(3) 0.045(4) 0.074(5) 0.014(3) -0.013(3) -0.014(3) C15 0.066(5) 0.050(4) 0.048(4) 0.004(3) 0.005(3) -0.036(4) C16 0.035(3) 0.029(3) 0.031(3) -0.008(3) 0.000(3) -0.016(3) C17 0.049(4) 0.029(3) 0.047(4) -0.005(3) -0.005(3) -0.012(3) C18 0.056(4) 0.047(4) 0.081(5) 0.001(4) -0.013(4) -0.009(4) C19 0.039(3) 0.049(4) 0.045(4) 0.002(3) -0.010(3) -0.021(3) C20 0.053(4) 0.056(5) 0.070(5) 0.016(4) -0.003(4) -0.017(4) C21 0.057(4) 0.046(4) 0.041(4) -0.007(3) -0.004(3) -0.027(3) C22 0.074(5) 0.054(4) 0.047(4) -0.013(3) 0.015(4) -0.035(4) C23 0.044(4) 0.040(4) 0.053(4) -0.003(3) -0.002(3) -0.024(3) C24 0.057(4) 0.054(5) 0.054(4) -0.003(3) 0.009(3) -0.027(4) _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 Mo1 O1 1.689(4) . ? Mo1 N3 2.266(4) . ? Mo1 S2 2.2770(15) . ? Mo1 S1 2.2783(17) . ? Mo1 N1 2.301(4) . ? Mo1 N5 2.374(5) . ? Mo1 Cu1 2.5844(14) . ? S1 Cu1 2.1766(16) . ? S2 Cu1 2.1882(17) . ? Cu1 C16 1.914(6) . ? B1 N6 1.518(8) . ? B1 N4 1.546(8) . ? B1 N2 1.547(8) . ? B1 H1 1.19(6) . ? N1 C1 1.337(7) . ? N1 N2 1.367(6) . ? N2 C3 1.352(7) . ? N3 C6 1.335(7) . ? N3 N4 1.377(7) . ? N4 C8 1.341(7) . ? N5 C11 1.349(7) . ? N5 N6 1.372(6) . ? N6 C13 1.350(7) . ? N7 C16 1.103(7) . ? N8 C21 1.503(8) . ? N8 C23 1.503(8) . ? N8 C19 1.527(7) . ? N8 C17 1.528(7) . ? C1 C2 1.386(8) . ? C1 C4 1.496(8) . ? C2 C3 1.379(9) . ? C2 H2 0.9400 . ? C3 C5 1.496(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.386(8) . ? C6 C9 1.482(9) . ? C7 C8 1.365(9) . ? C7 H7 0.9400 . ? C8 C10 1.497(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.382(8) . ? C11 C14 1.475(8) . ? C12 C13 1.386(8) . ? C12 H12 0.9400 . ? C13 C15 1.497(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C17 C18 1.515(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.505(9) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 C22 1.511(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.511(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? 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 O1 Mo1 N3 86.89(18) . . ? O1 Mo1 S2 101.33(14) . . ? N3 Mo1 S2 162.60(13) . . ? O1 Mo1 S1 101.74(14) . . ? N3 Mo1 S1 87.78(13) . . ? S2 Mo1 S1 105.24(6) . . ? O1 Mo1 N1 86.43(18) . . ? N3 Mo1 N1 76.96(16) . . ? S2 Mo1 N1 88.17(12) . . ? S1 Mo1 N1 162.35(12) . . ? O1 Mo1 N5 161.69(16) . . ? N3 Mo1 N5 79.25(16) . . ? S2 Mo1 N5 89.15(12) . . ? S1 Mo1 N5 89.73(12) . . ? N1 Mo1 N5 78.86(16) . . ? O1 Mo1 Cu1 102.94(13) . . ? N3 Mo1 Cu1 140.35(12) . . ? S2 Mo1 Cu1 53.04(5) . . ? S1 Mo1 Cu1 52.73(4) . . ? N1 Mo1 Cu1 141.06(11) . . ? N5 Mo1 Cu1 95.37(10) . . ? Cu1 S1 Mo1 70.88(6) . . ? Cu1 S2 Mo1 70.70(6) . . ? C16 Cu1 S1 122.99(17) . . ? C16 Cu1 S2 124.88(17) . . ? S1 Cu1 S2 112.06(7) . . ? C16 Cu1 Mo1 175.21(17) . . ? S1 Cu1 Mo1 56.40(5) . . ? S2 Cu1 Mo1 56.26(4) . . ? N6 B1 N4 109.2(5) . . ? N6 B1 N2 110.1(5) . . ? N4 B1 N2 107.4(5) . . ? N6 B1 H1 111(3) . . ? N4 B1 H1 112(3) . . ? N2 B1 H1 107(3) . . ? C1 N1 N2 107.3(4) . . ? C1 N1 Mo1 128.8(4) . . ? N2 N1 Mo1 123.0(3) . . ? C3 N2 N1 109.2(5) . . ? C3 N2 B1 129.8(5) . . ? N1 N2 B1 120.5(4) . . ? C6 N3 N4 107.5(4) . . ? C6 N3 Mo1 129.3(4) . . ? N4 N3 Mo1 123.2(3) . . ? C8 N4 N3 109.0(5) . . ? C8 N4 B1 129.6(5) . . ? N3 N4 B1 120.4(4) . . ? C11 N5 N6 105.5(4) . . ? C11 N5 Mo1 132.5(4) . . ? N6 N5 Mo1 122.0(3) . . ? C13 N6 N5 110.9(4) . . ? C13 N6 B1 129.2(5) . . ? N5 N6 B1 119.7(5) . . ? C21 N8 C23 106.2(5) . . ? C21 N8 C19 111.1(5) . . ? C23 N8 C19 111.1(5) . . ? C21 N8 C17 111.7(5) . . ? C23 N8 C17 111.5(5) . . ? C19 N8 C17 105.3(4) . . ? N1 C1 C2 109.5(5) . . ? N1 C1 C4 123.8(5) . . ? C2 C1 C4 126.7(5) . . ? C3 C2 C1 106.2(5) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? N2 C3 C2 107.8(5) . . ? N2 C3 C5 123.5(6) . . ? C2 C3 C5 128.7(6) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 108.4(6) . . ? N3 C6 C9 123.1(5) . . ? C7 C6 C9 128.5(6) . . ? C8 C7 C6 107.2(5) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? N4 C8 C7 107.9(5) . . ? N4 C8 C10 123.0(6) . . ? C7 C8 C10 129.1(6) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 110.4(5) . . ? N5 C11 C14 124.2(5) . . ? C12 C11 C14 125.4(5) . . ? C11 C12 C13 106.3(5) . . ? C11 C12 H12 126.8 . . ? C13 C12 H12 126.8 . . ? N6 C13 C12 106.9(5) . . ? N6 C13 C15 123.7(6) . . ? C12 C13 C15 129.4(6) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 Cu1 177.2(6) . . ? C18 C17 N8 115.7(5) . . ? C18 C17 H17A 108.4 . . ? N8 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? N8 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N8 115.5(5) . . ? C20 C19 H19A 108.4 . . ? N8 C19 H19A 108.4 . . ? C20 C19 H19B 108.4 . . ? N8 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N8 C21 C22 115.0(5) . . ? N8 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N8 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N8 C23 C24 116.4(5) . . ? N8 C23 H23A 108.2 . . ? C24 C23 H23A 108.2 . . ? N8 C23 H23B 108.2 . . ? C24 C23 H23B 108.2 . . ? H23A C23 H23B 107.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.737 _refine_diff_density_min -0.956 _refine_diff_density_rms 0.126 data_7^.^MeCN _database_code_depnum_ccdc_archive 'CCDC 928970' #TrackingRef 'ZhangZY.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H88 B4 Cu12 Mo4 N24 S16, C2 H3 N' _chemical_formula_sum 'C62 H91 B4 Cu12 Mo4 N25 S16' _chemical_formula_weight 2889.04 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' B B 0.0013 0.0007 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a c d' _symmetry_space_group_name_HALL '-I 4bd 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/4, x+3/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+1/4, -x+1/4, z+3/4' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-x+1/2, y, -z' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+3/4, x+5/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+3/4, -x+3/4, z+5/4' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-x+1, y+1/2, -z+1/2' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'y-1/4, -x-3/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-1/4, x-1/4, -z-3/4' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'x-1/2, -y, z' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y+1/4, -x-1/4, -z+1/4' 'x, y+1/2, -z' '-y+1/4, x+1/4, -z-1/4' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'x, -y+1/2, z+1/2' 'y+1/4, x+1/4, z+1/4' _cell_length_a 26.175(12) _cell_length_b 26.175(12) _cell_length_c 32.823(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22488(16) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 51771 _cell_measurement_theta_min 3.1053 _cell_measurement_theta_max 27.5554 _exptl_crystal_description Block _exptl_crystal_colour Dark-brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11440 _exptl_absorpt_coefficient_mu 2.987 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6115 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 86824 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4952 _reflns_number_gt 4823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. As the solvent molecule is likely to evaporate, the diffraction is weak in high angles. Thus the reflections at 2theta > 50 \% were omitted. The solvated MeCN molecule was refined to be disordered over two sites by sharing the C17 atom with equal occupations. The C-CH~3~ and the C\\tbN bond lengths were fixed to be 1.46(0.02) and 1.12(0.02) \%A, respectively. The C and N atoms in the disordered MeCN molecule were refined isotropically, while the H atoms of the disordered MeCN molecule were not located. A void of 756(53) \%A^3^ (3.1% of the cell volume, calcd. by the PLATON/SQUEEZE) were found existing in each cell, whereas nothing were found based on the residual peaks by the SHELXL program. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1515P)^2^+17.3000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4952 _refine_ls_number_parameters 290 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2614 _refine_ls_wR_factor_gt 0.2584 _refine_ls_goodness_of_fit_ref 1.444 _refine_ls_restrained_S_all 1.443 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.12238(3) 0.16799(3) 0.29006(2) 0.0314(3) Uani 1 1 d . . . S1 S 0.05688(8) 0.20972(8) 0.25653(6) 0.0371(5) Uani 1 1 d . . . S2 S 0.15461(8) 0.22986(8) 0.33348(6) 0.0370(5) Uani 1 1 d . . . S3 S 0.08014(8) 0.11262(8) 0.33394(6) 0.0368(5) Uani 1 1 d . . . S4 S 0.05838(8) 0.33756(7) 0.31678(6) 0.0332(5) Uani 1 1 d . . . Cu1 Cu 0.08399(4) 0.25916(4) 0.30631(3) 0.0358(3) Uani 1 1 d . . . Cu2 Cu 0.10078(4) 0.18172(4) 0.36819(3) 0.0359(3) Uani 1 1 d . . . Cu3 Cu 0.02390(4) 0.16555(4) 0.30710(3) 0.0355(3) Uani 1 1 d . . . B1 B 0.2094(4) 0.1097(4) 0.2303(3) 0.044(2) Uani 1 1 d . . . H1 H 0.230(4) 0.086(4) 0.210(3) 0.053 Uiso 1 1 d . . . N1 N 0.1744(3) 0.1983(3) 0.2401(2) 0.0407(17) Uani 1 1 d . . . N2 N 0.2027(3) 0.1654(3) 0.2173(2) 0.0391(17) Uani 1 1 d . . . N3 N 0.1978(3) 0.1237(3) 0.3050(2) 0.0404(16) Uani 1 1 d . . . N4 N 0.2281(3) 0.1083(3) 0.2737(2) 0.0417(16) Uani 1 1 d . . . N5 N 0.1141(3) 0.1041(3) 0.2432(2) 0.0426(17) Uani 1 1 d . . . N6 N 0.1572(3) 0.0825(3) 0.2261(2) 0.0432(18) Uani 1 1 d . . . C1 C 0.1827(3) 0.2448(3) 0.2229(3) 0.043(2) Uani 1 1 d . . . C2 C 0.2134(4) 0.2400(4) 0.1901(3) 0.051(2) Uani 1 1 d . . . H2 H 0.2237 0.2666 0.1727 0.062 Uiso 1 1 calc R . . C3 C 0.2266(3) 0.1910(4) 0.1869(3) 0.045(2) Uani 1 1 d . . . C4 C 0.1602(5) 0.2931(4) 0.2394(3) 0.057(3) Uani 1 1 d . . . H4A H 0.1748 0.3221 0.2252 0.085 Uiso 1 1 calc R . . H4B H 0.1676 0.2957 0.2682 0.085 Uiso 1 1 calc R . . H4C H 0.1235 0.2927 0.2353 0.085 Uiso 1 1 calc R . . C5 C 0.2599(5) 0.1654(4) 0.1560(3) 0.063(3) Uani 1 1 d . . . H5A H 0.2407 0.1386 0.1424 0.095 Uiso 1 1 calc R . . H5B H 0.2894 0.1506 0.1695 0.095 Uiso 1 1 calc R . . H5C H 0.2712 0.1903 0.1360 0.095 Uiso 1 1 calc R . . C6 C 0.2240(3) 0.1165(4) 0.3392(3) 0.048(2) Uani 1 1 d . . . C7 C 0.2709(4) 0.0955(4) 0.3294(4) 0.059(3) Uani 1 1 d . . . H7 H 0.2964 0.0855 0.3480 0.071 Uiso 1 1 calc R . . C8 C 0.2735(4) 0.0919(4) 0.2883(4) 0.053(2) Uani 1 1 d . . . C9 C 0.2047(5) 0.1243(5) 0.3815(3) 0.065(3) Uani 1 1 d . . . H9A H 0.1706 0.1101 0.3838 0.098 Uiso 1 1 calc R . . H9B H 0.2037 0.1605 0.3875 0.098 Uiso 1 1 calc R . . H9C H 0.2272 0.1072 0.4006 0.098 Uiso 1 1 calc R . . C10 C 0.3150(4) 0.0717(5) 0.2604(4) 0.067(3) Uani 1 1 d . . . H10A H 0.3276 0.0992 0.2433 0.101 Uiso 1 1 calc R . . H10B H 0.3012 0.0447 0.2434 0.101 Uiso 1 1 calc R . . H10C H 0.3429 0.0583 0.2767 0.101 Uiso 1 1 calc R . . C11 C 0.0745(4) 0.0741(4) 0.2302(3) 0.047(2) Uani 1 1 d . . . C12 C 0.0929(4) 0.0344(4) 0.2058(3) 0.051(2) Uani 1 1 d . . . H12 H 0.0736 0.0085 0.1932 0.061 Uiso 1 1 calc R . . C13 C 0.1449(4) 0.0407(3) 0.2038(3) 0.045(2) Uani 1 1 d . . . C14 C 0.0199(4) 0.0823(4) 0.2406(4) 0.063(3) Uani 1 1 d . . . H14A H 0.0142 0.0735 0.2690 0.094 Uiso 1 1 calc R . . H14B H -0.0014 0.0610 0.2234 0.094 Uiso 1 1 calc R . . H14C H 0.0111 0.1179 0.2363 0.094 Uiso 1 1 calc R . . C15 C 0.1850(5) 0.0097(4) 0.1826(4) 0.062(3) Uani 1 1 d . . . H15A H 0.2039 0.0315 0.1640 0.092 Uiso 1 1 calc R . . H15B H 0.1688 -0.0177 0.1674 0.092 Uiso 1 1 calc R . . H15C H 0.2082 -0.0046 0.2025 0.092 Uiso 1 1 calc R . . C17 C 0.1025(18) 0.1475(18) 0.1250 0.122(18) Uiso 0.50 2 d SPD . . N7 N 0.007(2) 0.160(4) 0.140(3) 0.22(5) Uiso 0.25 1 d PD . . C16 C 0.048(3) 0.161(4) 0.129(4) 0.21(6) Uiso 0.25 1 d PD . . 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 Mo1 0.0348(5) 0.0307(4) 0.0288(5) -0.0018(3) 0.0054(3) 0.0009(3) S1 0.0424(12) 0.0357(11) 0.0333(11) 0.0010(8) 0.0024(8) 0.0003(8) S2 0.0386(11) 0.0381(11) 0.0342(11) -0.0016(8) 0.0038(8) -0.0013(8) S3 0.0434(12) 0.0315(11) 0.0354(11) 0.0039(9) 0.0032(8) 0.0011(8) S4 0.0369(11) 0.0319(10) 0.0307(10) -0.0030(8) -0.0020(8) 0.0005(7) Cu1 0.0403(6) 0.0329(6) 0.0343(6) -0.0025(4) 0.0036(4) 0.0009(4) Cu2 0.0399(6) 0.0372(6) 0.0307(6) -0.0017(4) 0.0051(4) -0.0010(4) Cu3 0.0370(6) 0.0357(6) 0.0338(6) 0.0007(4) 0.0040(4) -0.0010(4) B1 0.047(6) 0.050(6) 0.035(5) -0.007(4) 0.006(4) 0.007(5) N1 0.055(5) 0.036(4) 0.031(3) -0.006(3) 0.013(3) 0.001(3) N2 0.041(4) 0.038(4) 0.038(4) -0.005(3) 0.010(3) -0.001(3) N3 0.044(4) 0.036(4) 0.042(4) 0.000(3) -0.002(3) 0.008(3) N4 0.040(4) 0.041(4) 0.043(4) 0.000(3) 0.007(3) 0.003(3) N5 0.049(4) 0.045(4) 0.034(4) -0.007(3) 0.006(3) -0.002(3) N6 0.057(5) 0.034(4) 0.039(4) 0.000(3) 0.006(3) 0.001(3) C1 0.038(5) 0.046(5) 0.047(5) 0.005(4) 0.016(4) -0.004(4) C2 0.049(6) 0.060(6) 0.046(5) 0.011(5) 0.021(4) -0.001(4) C3 0.045(5) 0.044(5) 0.046(5) -0.003(4) 0.020(4) -0.002(4) C4 0.085(8) 0.034(5) 0.052(6) 0.008(4) 0.026(5) 0.000(5) C5 0.079(8) 0.059(6) 0.052(6) -0.008(5) 0.032(6) -0.011(5) C6 0.034(5) 0.053(6) 0.056(6) -0.005(5) 0.004(4) 0.000(4) C7 0.049(6) 0.058(6) 0.071(7) 0.004(5) -0.011(5) 0.006(5) C8 0.044(5) 0.037(5) 0.077(7) 0.008(5) 0.003(5) 0.008(4) C9 0.081(8) 0.082(8) 0.033(5) 0.003(5) -0.012(5) 0.019(6) C10 0.054(6) 0.057(7) 0.091(9) -0.016(6) -0.005(6) 0.008(5) C11 0.060(6) 0.049(5) 0.032(4) -0.017(4) 0.003(4) 0.000(4) C12 0.055(6) 0.055(6) 0.043(5) -0.005(5) -0.002(4) -0.009(5) C13 0.071(6) 0.026(4) 0.037(4) -0.001(3) 0.001(4) 0.006(4) C14 0.047(6) 0.065(7) 0.076(7) -0.033(6) -0.001(5) -0.010(5) C15 0.078(8) 0.042(6) 0.064(6) -0.010(5) -0.006(6) 0.017(5) _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 Mo1 N1 2.276(7) . ? Mo1 N5 2.282(7) . ? Mo1 S1 2.312(2) . ? Mo1 S2 2.316(2) . ? Mo1 S3 2.323(2) . ? Mo1 N3 2.342(7) . ? Mo1 Cu3 2.6386(17) . ? Mo1 Cu1 2.6439(17) . ? Mo1 Cu2 2.6505(15) . ? S1 Cu3 2.199(2) . ? S1 Cu1 2.202(2) . ? S2 Cu1 2.191(2) . ? S2 Cu2 2.207(2) . ? S3 Cu2 2.197(3) . ? S3 Cu3 2.205(2) . ? S4 Cu2 2.178(2) 28_556 ? S4 Cu3 2.178(3) 11_454 ? S4 Cu1 2.186(2) . ? Cu1 Cu2 2.9029(17) . ? Cu1 Cu3 2.912(2) . ? Cu2 S4 2.178(2) 18_566 ? Cu2 Cu3 2.8719(17) . ? Cu3 S4 2.178(3) 11_454 ? B1 N4 1.506(12) . ? B1 N2 1.527(13) . ? B1 N6 1.546(14) . ? B1 H1 1.05(10) . ? N1 C1 1.356(11) . ? N1 N2 1.362(9) . ? N2 C3 1.354(11) . ? N3 C6 1.330(12) . ? N3 N4 1.358(10) . ? N4 C8 1.351(12) . ? N5 C11 1.369(12) . ? N5 N6 1.381(11) . ? N6 C13 1.356(12) . ? C1 C2 1.349(12) . ? C1 C4 1.496(13) . ? C2 C3 1.332(14) . ? C2 H2 0.9400 . ? C3 C5 1.497(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.383(14) . ? C6 C9 1.489(14) . ? C7 C8 1.356(16) . ? C7 H7 0.9400 . ? C8 C10 1.516(15) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.398(14) . ? C11 C14 1.486(14) . ? C12 C13 1.373(14) . ? C12 H12 0.9400 . ? C13 C15 1.498(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C17 C16 1.47(2) 8 ? C17 C16 1.47(2) . ? N7 C16 1.13(2) . ? C16 C16 1.52(18) 8 ? 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 N1 Mo1 N5 80.1(3) . . ? N1 Mo1 S1 86.3(2) . . ? N5 Mo1 S1 87.4(2) . . ? N1 Mo1 S2 88.92(19) . . ? N5 Mo1 S2 164.1(2) . . ? S1 Mo1 S2 103.45(8) . . ? N1 Mo1 S3 161.75(19) . . ? N5 Mo1 S3 85.1(2) . . ? S1 Mo1 S3 103.70(8) . . ? S2 Mo1 S3 103.18(8) . . ? N1 Mo1 N3 79.6(3) . . ? N5 Mo1 N3 81.8(3) . . ? S1 Mo1 N3 163.54(19) . . ? S2 Mo1 N3 84.88(19) . . ? S3 Mo1 N3 87.85(19) . . ? N1 Mo1 Cu3 138.27(19) . . ? N5 Mo1 Cu3 91.85(19) . . ? S1 Mo1 Cu3 52.25(6) . . ? S2 Mo1 Cu3 104.02(6) . . ? S3 Mo1 Cu3 52.30(6) . . ? N3 Mo1 Cu3 140.11(18) . . ? N1 Mo1 Cu1 93.32(18) . . ? N5 Mo1 Cu1 139.6(2) . . ? S1 Mo1 Cu1 52.24(6) . . ? S2 Mo1 Cu1 51.91(6) . . ? S3 Mo1 Cu1 104.89(6) . . ? N3 Mo1 Cu1 136.51(18) . . ? Cu3 Mo1 Cu1 66.90(3) . . ? N1 Mo1 Cu2 141.05(18) . . ? N5 Mo1 Cu2 136.94(19) . . ? S1 Mo1 Cu2 103.78(6) . . ? S2 Mo1 Cu2 52.24(6) . . ? S3 Mo1 Cu2 51.92(6) . . ? N3 Mo1 Cu2 92.56(18) . . ? Cu3 Mo1 Cu2 65.77(4) . . ? Cu1 Mo1 Cu2 66.50(3) . . ? Cu3 S1 Cu1 82.84(9) . . ? Cu3 S1 Mo1 71.55(7) . . ? Cu1 S1 Mo1 71.67(7) . . ? Cu1 S2 Cu2 82.60(8) . . ? Cu1 S2 Mo1 71.77(7) . . ? Cu2 S2 Mo1 71.69(7) . . ? Cu2 S3 Cu3 81.45(8) . . ? Cu2 S3 Mo1 71.74(8) . . ? Cu3 S3 Mo1 71.22(7) . . ? Cu2 S4 Cu3 105.46(9) 28_556 11_454 ? Cu2 S4 Cu1 105.47(9) 28_556 . ? Cu3 S4 Cu1 104.19(9) 11_454 . ? S4 Cu1 S2 121.56(9) . . ? S4 Cu1 S1 124.73(9) . . ? S2 Cu1 S1 111.60(9) . . ? S4 Cu1 Mo1 174.66(7) . . ? S2 Cu1 Mo1 56.32(6) . . ? S1 Cu1 Mo1 56.09(6) . . ? S4 Cu1 Cu2 126.30(7) . . ? S2 Cu1 Cu2 48.94(6) . . ? S1 Cu1 Cu2 99.06(7) . . ? Mo1 Cu1 Cu2 56.86(4) . . ? S4 Cu1 Cu3 128.53(7) . . ? S2 Cu1 Cu3 99.06(7) . . ? S1 Cu1 Cu3 48.54(6) . . ? Mo1 Cu1 Cu3 56.46(3) . . ? Cu2 Cu1 Cu3 59.20(4) . . ? S4 Cu2 S3 124.08(9) 18_566 . ? S4 Cu2 S2 122.64(9) 18_566 . ? S3 Cu2 S2 111.28(9) . . ? S4 Cu2 Mo1 176.66(7) 18_566 . ? S3 Cu2 Mo1 56.35(6) . . ? S2 Cu2 Mo1 56.07(6) . . ? S4 Cu2 Cu3 126.19(7) 18_566 . ? S3 Cu2 Cu3 49.40(6) . . ? S2 Cu2 Cu3 99.85(7) . . ? Mo1 Cu2 Cu3 56.91(4) . . ? S4 Cu2 Cu1 125.34(8) 18_566 . ? S3 Cu2 Cu1 100.35(7) . . ? S2 Cu2 Cu1 48.46(6) . . ? Mo1 Cu2 Cu1 56.64(4) . . ? Cu3 Cu2 Cu1 60.55(4) . . ? S4 Cu3 S1 121.18(9) 11_454 . ? S4 Cu3 S3 125.32(9) 11_454 . ? S1 Cu3 S3 111.70(9) . . ? S4 Cu3 Mo1 176.08(7) 11_454 . ? S1 Cu3 Mo1 56.21(6) . . ? S3 Cu3 Mo1 56.48(6) . . ? S4 Cu3 Cu2 126.61(7) 11_454 . ? S1 Cu3 Cu2 100.05(8) . . ? S3 Cu3 Cu2 49.16(6) . . ? Mo1 Cu3 Cu2 57.31(4) . . ? S4 Cu3 Cu1 124.52(7) 11_454 . ? S1 Cu3 Cu1 48.62(6) . . ? S3 Cu3 Cu1 99.89(7) . . ? Mo1 Cu3 Cu1 56.64(3) . . ? Cu2 Cu3 Cu1 60.25(4) . . ? N4 B1 N2 109.0(8) . . ? N4 B1 N6 111.0(8) . . ? N2 B1 N6 108.3(8) . . ? N4 B1 H1 114(6) . . ? N2 B1 H1 117(6) . . ? N6 B1 H1 97(6) . . ? C1 N1 N2 104.6(7) . . ? C1 N1 Mo1 135.0(6) . . ? N2 N1 Mo1 120.0(5) . . ? C3 N2 N1 109.9(7) . . ? C3 N2 B1 128.8(7) . . ? N1 N2 B1 120.8(7) . . ? C6 N3 N4 107.3(7) . . ? C6 N3 Mo1 132.9(6) . . ? N4 N3 Mo1 118.6(5) . . ? C8 N4 N3 109.7(8) . . ? C8 N4 B1 129.0(8) . . ? N3 N4 B1 121.3(7) . . ? C11 N5 N6 104.9(7) . . ? C11 N5 Mo1 134.7(6) . . ? N6 N5 Mo1 119.7(6) . . ? C13 N6 N5 110.9(8) . . ? C13 N6 B1 129.0(8) . . ? N5 N6 B1 119.8(7) . . ? C2 C1 N1 110.1(8) . . ? C2 C1 C4 126.9(9) . . ? N1 C1 C4 123.0(7) . . ? C3 C2 C1 107.8(8) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? C2 C3 N2 107.4(7) . . ? C2 C3 C5 129.6(9) . . ? N2 C3 C5 123.0(8) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 108.5(9) . . ? N3 C6 C9 126.3(9) . . ? C7 C6 C9 124.9(10) . . ? C8 C7 C6 107.7(9) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? N4 C8 C7 106.7(9) . . ? N4 C8 C10 121.8(10) . . ? C7 C8 C10 131.4(10) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C12 110.2(9) . . ? N5 C11 C14 125.0(8) . . ? C12 C11 C14 124.9(9) . . ? C13 C12 C11 106.2(9) . . ? C13 C12 H12 126.9 . . ? C11 C12 H12 126.9 . . ? N6 C13 C12 107.9(8) . . ? N6 C13 C15 121.5(9) . . ? C12 C13 C15 130.6(9) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C16 C17 C16 62(8) 8 . ? N7 C16 C17 159(8) . . ? N7 C16 C16 138(10) . 8 ? C17 C16 C16 59(4) . 8 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.000 0.196 756 53 ' ' 2 0.750 0.000 0.212 756 53 ' ' 3 0.500 0.250 0.125 23 5 ' ' 4 0.000 0.250 0.375 23 5 ' ' 5 0.500 0.250 0.625 23 5 ' ' 6 0.000 0.250 0.875 23 5 ' ' 7 0.250 0.500 0.053 756 53 ' ' 8 0.750 0.500 0.445 756 53 ' ' 9 0.000 0.750 0.125 23 5 ' ' 10 0.500 0.750 0.375 23 5 ' ' 11 0.000 0.750 0.625 23 5 ' ' 12 0.500 0.750 0.875 23 5 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.659 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.140 #===END