# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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 #============================================================================== # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H37 B Br Cu2 N6 P S3 W' _chemical_formula_sum 'C33 H37 B Br Cu2 N6 P S3 W' _chemical_formula_weight 1046.49 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' Br Br -0.2901 2.4595 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.3258(9) _cell_length_b 11.3987(8) _cell_length_c 16.8771(11) _cell_angle_alpha 85.284(6) _cell_angle_beta 87.650(6) _cell_angle_gamma 60.504(8) _cell_volume 1890.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4146 _cell_measurement_theta_min 3.2710 _cell_measurement_theta_max 28.3990 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 5.449 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1149 _exptl_absorpt_correction_T_max 0.2917 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14392 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_unetI/netI 0.0656 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6646 _reflns_number_gt 5567 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0329P)^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 6646 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.020 _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 W1 W 0.33489(2) 0.36725(2) 0.197092(12) 0.02015(8) Uani 1 1 d . . . Cu1 Cu 0.45754(8) 0.10290(7) 0.20892(4) 0.03274(19) Uani 1 1 d . . . Cu2 Cu 0.56024(7) 0.25294(7) 0.28335(4) 0.02588(17) Uani 1 1 d . . . Br1 Br 0.54306(8) -0.12406(7) 0.22965(4) 0.04752(19) Uani 1 1 d . . . S1 S 0.24154(16) 0.23696(15) 0.22540(8) 0.0293(4) Uani 1 1 d . . . S2 S 0.36249(16) 0.41640(15) 0.31895(8) 0.0269(3) Uani 1 1 d . . . S3 S 0.55481(15) 0.21967(15) 0.15714(8) 0.0268(3) Uani 1 1 d . . . P1 P 0.73799(16) 0.15506(15) 0.36352(8) 0.0241(3) Uani 1 1 d . . . N1 N 0.1800(5) 0.5201(4) 0.0340(2) 0.0224(11) Uani 1 1 d . . . N2 N 0.2652(5) 0.3946(5) 0.0691(2) 0.0243(11) Uani 1 1 d . . . N3 N 0.0677(5) 0.6498(4) 0.1525(2) 0.0227(10) Uani 1 1 d . . . N4 N 0.1221(5) 0.5375(4) 0.2066(2) 0.0231(11) Uani 1 1 d . . . N5 N 0.2759(5) 0.6436(5) 0.0952(2) 0.0243(11) Uani 1 1 d . . . N6 N 0.3703(5) 0.5412(5) 0.1448(2) 0.0242(11) Uani 1 1 d . . . C1 C 0.0553(7) 0.6278(7) -0.0937(3) 0.0398(17) Uani 1 1 d . . . H1A H -0.0324 0.6754 -0.0694 0.060 Uiso 1 1 calc R . . H1B H 0.0466 0.5968 -0.1431 0.060 Uiso 1 1 calc R . . H1C H 0.0925 0.6873 -0.1033 0.060 Uiso 1 1 calc R . . C2 C 0.1477(6) 0.5090(6) -0.0393(3) 0.0285(14) Uani 1 1 d . . . C3 C 0.2126(6) 0.3734(6) -0.0519(3) 0.0319(15) Uani 1 1 d . . . H3 H 0.2077 0.3357 -0.0977 0.038 Uiso 1 1 calc R . . C4 C 0.2856(6) 0.3044(6) 0.0150(3) 0.0249(13) Uani 1 1 d . . . C5 C 0.3720(7) 0.1566(6) 0.0275(3) 0.0392(16) Uani 1 1 d . . . H5A H 0.4624 0.1355 0.0407 0.059 Uiso 1 1 calc R . . H5B H 0.3743 0.1152 -0.0202 0.059 Uiso 1 1 calc R . . H5C H 0.3357 0.1229 0.0702 0.059 Uiso 1 1 calc R . . C6 C -0.1355(7) 0.8769(6) 0.1330(4) 0.0382(16) Uani 1 1 d . . . H6A H -0.0938 0.9317 0.1380 0.057 Uiso 1 1 calc R . . H6B H -0.2255 0.9209 0.1548 0.057 Uiso 1 1 calc R . . H6C H -0.1401 0.8645 0.0778 0.057 Uiso 1 1 calc R . . C7 C -0.0533(6) 0.7426(6) 0.1770(3) 0.0266(13) Uani 1 1 d . . . C8 C -0.0818(6) 0.6914(6) 0.2469(3) 0.0290(14) Uani 1 1 d . . . H8 H -0.1602 0.7346 0.2771 0.035 Uiso 1 1 calc R . . C9 C 0.0254(6) 0.5658(6) 0.2641(3) 0.0295(14) Uani 1 1 d . . . C10 C 0.0362(7) 0.4713(7) 0.3337(3) 0.0410(17) Uani 1 1 d . . . H10A H 0.0110 0.4077 0.3178 0.061 Uiso 1 1 calc R . . H10B H -0.0235 0.5218 0.3752 0.061 Uiso 1 1 calc R . . H10C H 0.1279 0.4238 0.3529 0.061 Uiso 1 1 calc R . . C11 C 0.2340(7) 0.8608(6) 0.0218(4) 0.0428(17) Uani 1 1 d . . . H11A H 0.2144 0.8381 -0.0277 0.064 Uiso 1 1 calc R . . H11B H 0.2831 0.9093 0.0117 0.064 Uiso 1 1 calc R . . H11C H 0.1507 0.9163 0.0487 0.064 Uiso 1 1 calc R . . C12 C 0.3181(6) 0.7341(6) 0.0728(3) 0.0275(14) Uani 1 1 d . . . C13 C 0.4425(6) 0.6873(6) 0.1067(3) 0.0303(14) Uani 1 1 d . . . H13 H 0.4968 0.7276 0.1006 0.036 Uiso 1 1 calc R . . C14 C 0.4722(6) 0.5698(6) 0.1513(3) 0.0291(14) Uani 1 1 d . . . C15 C 0.5978(7) 0.4882(7) 0.1992(4) 0.0485(19) Uani 1 1 d . . . H15A H 0.5741 0.4728 0.2528 0.073 Uiso 1 1 calc R . . H15B H 0.6479 0.5359 0.1991 0.073 Uiso 1 1 calc R . . H15C H 0.6525 0.4030 0.1765 0.073 Uiso 1 1 calc R . . C16 C 0.7165(6) 0.0461(6) 0.4407(3) 0.0281(14) Uani 1 1 d . . . C17 C 0.6791(7) -0.0458(6) 0.4180(4) 0.0368(16) Uani 1 1 d . . . H17 H 0.6648 -0.0491 0.3645 0.044 Uiso 1 1 calc R . . C18 C 0.6630(7) -0.1323(7) 0.4742(4) 0.0452(18) Uani 1 1 d . . . H18 H 0.6395 -0.1942 0.4582 0.054 Uiso 1 1 calc R . . C19 C 0.6814(7) -0.1272(7) 0.5529(4) 0.0477(19) Uani 1 1 d . . . H19 H 0.6704 -0.1856 0.5904 0.057 Uiso 1 1 calc R . . C20 C 0.7165(7) -0.0350(7) 0.5772(4) 0.0460(18) Uani 1 1 d . . . H20 H 0.7291 -0.0318 0.6309 0.055 Uiso 1 1 calc R . . C21 C 0.7328(7) 0.0524(7) 0.5212(3) 0.0412(17) Uani 1 1 d . . . H21 H 0.7546 0.1153 0.5376 0.049 Uiso 1 1 calc R . . C22 C 0.7658(6) 0.2731(6) 0.4148(3) 0.0252(14) Uani 1 1 d . . . C23 C 0.8939(7) 0.2403(7) 0.4420(3) 0.0354(16) Uani 1 1 d . . . H23 H 0.9678 0.1557 0.4344 0.042 Uiso 1 1 calc R . . C24 C 0.9107(8) 0.3333(7) 0.4802(3) 0.0412(18) Uani 1 1 d . . . H24 H 0.9962 0.3108 0.4983 0.049 Uiso 1 1 calc R . . C25 C 0.8021(8) 0.4595(8) 0.4919(4) 0.048(2) Uani 1 1 d . . . H25 H 0.8146 0.5219 0.5173 0.058 Uiso 1 1 calc R . . C26 C 0.6772(8) 0.4920(8) 0.4662(4) 0.057(2) Uani 1 1 d . . . H26 H 0.6036 0.5762 0.4752 0.068 Uiso 1 1 calc R . . C27 C 0.6580(7) 0.4005(7) 0.4266(4) 0.0417(17) Uani 1 1 d . . . H27 H 0.5723 0.4249 0.4078 0.050 Uiso 1 1 calc R . . C28 C 0.9026(6) 0.0480(6) 0.3195(3) 0.0268(14) Uani 1 1 d . . . C29 C 0.9471(7) 0.1045(7) 0.2574(4) 0.0437(17) Uani 1 1 d . . . H29 H 0.8908 0.1935 0.2383 0.052 Uiso 1 1 calc R . . C30 C 1.0719(8) 0.0320(8) 0.2237(4) 0.0493(19) Uani 1 1 d . . . H30 H 1.0999 0.0712 0.1820 0.059 Uiso 1 1 calc R . . C31 C 1.1568(8) -0.1007(8) 0.2522(4) 0.0491(19) Uani 1 1 d . . . H31 H 1.2428 -0.1501 0.2305 0.059 Uiso 1 1 calc R . . C32 C 1.1129(7) -0.1586(7) 0.3126(4) 0.0469(18) Uani 1 1 d . . . H32 H 1.1689 -0.2479 0.3312 0.056 Uiso 1 1 calc R . . C33 C 0.9863(7) -0.0845(7) 0.3456(4) 0.0399(16) Uani 1 1 d . . . H33 H 0.9572 -0.1247 0.3861 0.048 Uiso 1 1 calc R . . B1 B 0.1432(7) 0.6484(7) 0.0756(4) 0.0229(14) Uani 1 1 d . . . HB1 H 0.080(5) 0.744(5) 0.036(3) 0.019(13) Uiso 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 W1 0.01702(15) 0.01970(14) 0.01911(12) 0.00183(8) -0.00381(9) -0.00567(12) Cu1 0.0306(5) 0.0247(4) 0.0380(4) -0.0018(3) -0.0072(3) -0.0094(4) Cu2 0.0217(4) 0.0273(4) 0.0242(4) 0.0012(3) -0.0076(3) -0.0085(4) Br1 0.0427(5) 0.0259(4) 0.0692(5) -0.0037(3) -0.0115(4) -0.0123(4) S1 0.0256(10) 0.0282(9) 0.0329(8) 0.0051(6) -0.0060(7) -0.0129(8) S2 0.0238(9) 0.0315(9) 0.0212(7) -0.0038(6) -0.0024(6) -0.0100(8) S3 0.0193(9) 0.0276(9) 0.0250(7) -0.0030(6) -0.0016(6) -0.0047(8) P1 0.0225(9) 0.0275(9) 0.0213(7) 0.0013(6) -0.0053(6) -0.0115(8) N1 0.019(3) 0.021(3) 0.018(2) 0.0055(18) -0.0047(19) -0.004(3) N2 0.022(3) 0.021(3) 0.024(2) 0.0001(19) -0.002(2) -0.006(3) N3 0.017(3) 0.013(3) 0.029(2) 0.0040(19) -0.007(2) -0.001(2) N4 0.017(3) 0.019(3) 0.024(2) 0.0008(19) -0.004(2) -0.002(2) N5 0.026(3) 0.020(3) 0.024(2) 0.0044(19) -0.006(2) -0.009(3) N6 0.022(3) 0.032(3) 0.021(2) 0.002(2) -0.001(2) -0.016(3) C1 0.035(4) 0.053(5) 0.022(3) 0.004(3) -0.008(3) -0.015(4) C2 0.019(4) 0.039(4) 0.021(3) 0.003(2) -0.005(2) -0.010(3) C3 0.033(4) 0.040(4) 0.024(3) -0.004(3) -0.005(3) -0.018(4) C4 0.024(4) 0.031(4) 0.020(3) -0.005(2) -0.003(2) -0.013(3) C5 0.051(5) 0.022(4) 0.035(3) -0.010(3) -0.012(3) -0.009(4) C6 0.024(4) 0.021(4) 0.057(4) -0.003(3) 0.000(3) -0.001(3) C7 0.018(4) 0.021(3) 0.035(3) -0.004(2) -0.006(3) -0.004(3) C8 0.017(4) 0.029(4) 0.032(3) -0.008(3) 0.002(3) -0.004(3) C9 0.024(4) 0.034(4) 0.026(3) -0.008(3) 0.004(3) -0.010(3) C10 0.030(4) 0.054(5) 0.024(3) 0.008(3) 0.000(3) -0.010(4) C11 0.045(5) 0.035(4) 0.046(4) 0.010(3) 0.006(3) -0.020(4) C12 0.034(4) 0.026(4) 0.024(3) 0.001(2) 0.005(3) -0.017(3) C13 0.026(4) 0.028(4) 0.041(3) -0.001(3) 0.003(3) -0.017(3) C14 0.023(4) 0.036(4) 0.030(3) -0.001(3) 0.004(3) -0.017(3) C15 0.030(5) 0.052(5) 0.070(5) 0.015(4) -0.020(4) -0.026(4) C16 0.017(4) 0.030(4) 0.031(3) 0.003(2) -0.002(3) -0.008(3) C17 0.035(4) 0.035(4) 0.039(3) 0.001(3) -0.007(3) -0.016(4) C18 0.033(5) 0.027(4) 0.075(5) 0.001(3) -0.006(4) -0.014(4) C19 0.043(5) 0.044(5) 0.051(4) 0.021(3) 0.000(3) -0.021(4) C20 0.045(5) 0.054(5) 0.034(4) 0.011(3) -0.006(3) -0.022(4) C21 0.047(5) 0.053(5) 0.026(3) 0.004(3) -0.004(3) -0.027(4) C22 0.033(4) 0.025(4) 0.017(3) 0.002(2) 0.001(3) -0.014(3) C23 0.036(4) 0.036(4) 0.034(3) 0.006(3) -0.014(3) -0.019(4) C24 0.041(5) 0.059(5) 0.036(4) 0.004(3) -0.010(3) -0.035(5) C25 0.063(6) 0.068(6) 0.034(4) -0.018(3) 0.004(4) -0.045(5) C26 0.052(6) 0.053(5) 0.065(5) -0.032(4) 0.005(4) -0.021(5) C27 0.037(5) 0.053(5) 0.043(4) -0.014(3) 0.003(3) -0.027(4) C28 0.025(4) 0.035(4) 0.023(3) -0.003(2) -0.004(2) -0.016(3) C29 0.043(5) 0.046(5) 0.043(4) -0.005(3) 0.003(3) -0.023(4) C30 0.044(5) 0.060(6) 0.042(4) -0.008(4) 0.015(4) -0.025(5) C31 0.032(5) 0.067(6) 0.052(4) -0.024(4) 0.008(3) -0.025(5) C32 0.033(5) 0.030(4) 0.058(4) -0.014(3) -0.001(4) 0.001(4) C33 0.031(4) 0.047(5) 0.034(3) 0.003(3) -0.007(3) -0.013(4) B1 0.013(4) 0.020(4) 0.029(3) 0.003(3) -0.006(3) -0.003(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 W1 S1 2.2225(13) . ? W1 N4 2.240(5) . ? W1 S2 2.2485(13) . ? W1 N2 2.275(4) . ? W1 N6 2.311(4) . ? W1 S3 2.3261(15) . ? W1 Cu1 2.6175(8) . ? W1 Cu2 2.6550(8) . ? Cu1 S1 2.1749(18) . ? Cu1 S3 2.2187(15) . ? Cu1 Br1 2.2726(10) . ? Cu1 Cu2 2.8789(9) . ? Cu2 S2 2.1938(17) . ? Cu2 S3 2.2026(15) . ? Cu2 P1 2.2117(17) . ? P1 C22 1.814(5) . ? P1 C16 1.818(5) . ? P1 C28 1.820(6) . ? N1 C2 1.337(7) . ? N1 N2 1.370(6) . ? N1 B1 1.534(8) . ? N2 C4 1.358(7) . ? N3 C7 1.328(7) . ? N3 N4 1.389(6) . ? N3 B1 1.522(7) . ? N4 C9 1.364(7) . ? N5 C12 1.358(6) . ? N5 N6 1.374(6) . ? N5 B1 1.526(8) . ? N6 C14 1.356(7) . ? C1 C2 1.500(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.377(8) . ? C3 C4 1.367(8) . ? C3 H3 0.9300 . ? C4 C5 1.475(8) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.493(8) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.371(7) . ? C8 C9 1.363(8) . ? C8 H8 0.9300 . ? C9 C10 1.494(7) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.497(8) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.368(8) . ? C13 C14 1.373(8) . ? C13 H13 0.9300 . ? C14 C15 1.486(9) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C21 1.392(8) . ? C16 C17 1.393(8) . ? C17 C18 1.383(8) . ? C17 H17 0.9300 . ? C18 C19 1.364(9) . ? C18 H18 0.9300 . ? C19 C20 1.387(9) . ? C19 H19 0.9300 . ? C20 C21 1.390(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.386(8) . ? C22 C23 1.395(8) . ? C23 C24 1.377(8) . ? C23 H23 0.9300 . ? C24 C25 1.380(10) . ? C24 H24 0.9300 . ? C25 C26 1.354(10) . ? C25 H25 0.9300 . ? C26 C27 1.390(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.375(9) . ? C28 C29 1.392(8) . ? C29 C30 1.365(9) . ? C29 H29 0.9300 . ? C30 C31 1.388(10) . ? C30 H30 0.9300 . ? C31 C32 1.376(9) . ? C31 H31 0.9300 . ? C32 C33 1.378(9) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? B1 HB1 1.14(5) . ? 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 S1 W1 N4 84.25(11) . . ? S1 W1 S2 101.69(5) . . ? N4 W1 S2 85.08(11) . . ? S1 W1 N2 88.76(11) . . ? N4 W1 N2 79.77(16) . . ? S2 W1 N2 160.65(12) . . ? S1 W1 N6 162.02(12) . . ? N4 W1 N6 81.74(16) . . ? S2 W1 N6 88.31(11) . . ? N2 W1 N6 77.71(15) . . ? S1 W1 S3 104.66(6) . . ? N4 W1 S3 165.66(11) . . ? S2 W1 S3 103.67(5) . . ? N2 W1 S3 89.09(12) . . ? N6 W1 S3 87.12(12) . . ? S1 W1 Cu1 52.64(5) . . ? N4 W1 Cu1 136.88(11) . . ? S2 W1 Cu1 102.81(4) . . ? N2 W1 Cu1 96.48(11) . . ? N6 W1 Cu1 139.93(12) . . ? S3 W1 Cu1 52.94(4) . . ? S1 W1 Cu2 104.70(4) . . ? N4 W1 Cu2 137.36(11) . . ? S2 W1 Cu2 52.36(4) . . ? N2 W1 Cu2 140.69(12) . . ? N6 W1 Cu2 93.25(12) . . ? S3 W1 Cu2 51.98(4) . . ? Cu1 W1 Cu2 66.19(2) . . ? S1 Cu1 S3 110.09(6) . . ? S1 Cu1 Br1 119.31(5) . . ? S3 Cu1 Br1 130.06(6) . . ? S1 Cu1 W1 54.31(4) . . ? S3 Cu1 W1 56.78(4) . . ? Br1 Cu1 W1 172.91(4) . . ? S1 Cu1 Cu2 99.03(5) . . ? S3 Cu1 Cu2 49.13(4) . . ? Br1 Cu1 Cu2 124.18(4) . . ? W1 Cu1 Cu2 57.53(2) . . ? S2 Cu2 S3 109.81(6) . . ? S2 Cu2 P1 122.68(6) . . ? S3 Cu2 P1 127.28(6) . . ? S2 Cu2 W1 54.25(4) . . ? S3 Cu2 W1 56.30(4) . . ? P1 Cu2 W1 175.17(5) . . ? S2 Cu2 Cu1 96.43(5) . . ? S3 Cu2 Cu1 49.62(4) . . ? P1 Cu2 Cu1 122.62(5) . . ? W1 Cu2 Cu1 56.28(2) . . ? Cu1 S1 W1 73.05(5) . . ? Cu2 S2 W1 73.39(5) . . ? Cu2 S3 Cu1 81.26(5) . . ? Cu2 S3 W1 71.73(5) . . ? Cu1 S3 W1 70.28(5) . . ? C22 P1 C16 106.1(2) . . ? C22 P1 C28 103.4(3) . . ? C16 P1 C28 104.8(3) . . ? C22 P1 Cu2 113.9(2) . . ? C16 P1 Cu2 110.31(19) . . ? C28 P1 Cu2 117.37(18) . . ? C2 N1 N2 110.0(4) . . ? C2 N1 B1 128.8(5) . . ? N2 N1 B1 121.0(4) . . ? C4 N2 N1 106.5(4) . . ? C4 N2 W1 132.1(4) . . ? N1 N2 W1 121.3(3) . . ? C7 N3 N4 110.4(4) . . ? C7 N3 B1 129.8(5) . . ? N4 N3 B1 119.7(5) . . ? C9 N4 N3 105.0(5) . . ? C9 N4 W1 132.1(4) . . ? N3 N4 W1 122.5(3) . . ? C12 N5 N6 109.9(5) . . ? C12 N5 B1 128.8(5) . . ? N6 N5 B1 121.2(4) . . ? C14 N6 N5 105.9(4) . . ? C14 N6 W1 133.5(4) . . ? N5 N6 W1 120.6(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 107.3(5) . . ? N1 C2 C1 123.5(5) . . ? C3 C2 C1 129.2(5) . . ? C4 C3 C2 107.5(5) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? N2 C4 C3 108.7(5) . . ? N2 C4 C5 125.1(5) . . ? C3 C4 C5 126.2(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 107.6(5) . . ? N3 C7 C6 123.2(5) . . ? C8 C7 C6 129.3(6) . . ? C9 C8 C7 107.7(5) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? N4 C9 C8 109.4(5) . . ? N4 C9 C10 124.6(6) . . ? C8 C9 C10 126.0(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 107.2(5) . . ? N5 C12 C11 122.7(5) . . ? C13 C12 C11 130.1(5) . . ? C12 C13 C14 107.3(5) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N6 C14 C13 109.7(5) . . ? N6 C14 C15 126.0(5) . . ? C13 C14 C15 124.3(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 118.7(5) . . ? C21 C16 P1 123.0(4) . . ? C17 C16 P1 118.3(4) . . ? C18 C17 C16 120.6(6) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 120.4(6) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.1(5) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 120.0(6) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C16 C21 C20 120.1(6) . . ? C16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C27 C22 C23 118.6(5) . . ? C27 C22 P1 119.6(5) . . ? C23 C22 P1 121.8(5) . . ? C24 C23 C22 119.9(6) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.8(6) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 119.7(6) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.6(8) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.4(6) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C33 C28 C29 118.4(6) . . ? C33 C28 P1 123.5(4) . . ? C29 C28 P1 118.1(5) . . ? C30 C29 C28 121.3(7) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 119.6(6) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 119.7(7) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.1(7) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C28 C33 C32 120.9(6) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? N3 B1 N5 109.1(4) . . ? N3 B1 N1 109.6(4) . . ? N5 B1 N1 107.2(5) . . ? N3 B1 HB1 110(3) . . ? N5 B1 HB1 109(2) . . ? N1 B1 HB1 112(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.188 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.140 _database_code_depnum_ccdc_archive 'CCDC 973424' ####################################################################### # # 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_3^.^MeCN^.^Et~2~O #============================================================================== # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C41 H44 B Cu2 N7 P2 S4 W), C4 H10 O, C2 H3 N' _chemical_formula_sum 'C88 H101 B2 Cu4 N15 O P4 S8 W2' _chemical_formula_weight 2408.68 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' Cu Cu 0.3201 1.2651 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.3725(6) _cell_length_b 15.9248(8) _cell_length_c 16.9548(8) _cell_angle_alpha 77.783(4) _cell_angle_beta 79.692(4) _cell_angle_gamma 79.364(4) _cell_volume 2661.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7068 _cell_measurement_theta_min 3.0060 _cell_measurement_theta_max 26.9580 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 3.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65419 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23736 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_unetI/netI 0.0725 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9360 _reflns_number_gt 7533 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 solvent MeCN was refined to have rigid bond restrains and similar Uij, with the C46-C47 and C46\\tbN8 bond distances fixed to be 1.51 and 1.14 \%A, respectively ; _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^)+(0.0753P)^2^+8.6586P] 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 9360 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1071 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _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 W1 W 0.19853(3) 0.17959(2) 0.264319(18) 0.02750(12) Uani 1 1 d . . . Cu1 Cu 0.36973(9) 0.28323(6) 0.15561(6) 0.0314(2) Uani 1 1 d . . . Cu2 Cu 0.15022(9) 0.35133(6) 0.25003(6) 0.0301(2) Uani 1 1 d . . . S1 S 0.41803(19) 0.15441(13) 0.24247(13) 0.0345(5) Uani 1 1 d . . . S2 S 0.15843(18) 0.25700(13) 0.36452(12) 0.0307(4) Uani 1 1 d . . . S3 S 0.14737(19) 0.28067(13) 0.15038(12) 0.0312(4) Uani 1 1 d . . . S4 S 0.5764(3) 0.26884(18) -0.11443(16) 0.0666(8) Uani 1 1 d . . . P1 P 0.43449(19) 0.40387(13) 0.18552(12) 0.0282(4) Uani 1 1 d . . . P2 P 0.16121(19) 0.49082(13) 0.23482(12) 0.0288(4) Uani 1 1 d . . . N1 N 0.1366(6) -0.0013(4) 0.2331(4) 0.0317(12) Uani 1 1 d U . . N2 N 0.1998(6) 0.0705(4) 0.1960(4) 0.0358(13) Uani 1 1 d U . . N3 N 0.1276(6) 0.0009(4) 0.3791(4) 0.0316(12) Uani 1 1 d U . . N4 N 0.2093(6) 0.0635(4) 0.3677(4) 0.0319(12) Uani 1 1 d U . . N5 N -0.0568(6) 0.0804(4) 0.3036(4) 0.0296(12) Uani 1 1 d U . . N6 N -0.0218(6) 0.1619(4) 0.2945(4) 0.0299(12) Uani 1 1 d U . . N7 N 0.4688(7) 0.2805(5) 0.0458(4) 0.0435(16) Uani 1 1 d U . . N8 N 0.844(2) -0.0444(13) 0.0945(14) 0.103(7) Uani 0.50 1 d PDU . . C1 C 0.1089(10) -0.1444(6) 0.2069(6) 0.053(2) Uani 1 1 d U . . H1A H 0.1166 -0.1691 0.2635 0.079 Uiso 1 1 calc R . . H1B H 0.1585 -0.1845 0.1726 0.079 Uiso 1 1 calc R . . H1C H 0.0163 -0.1339 0.1994 0.079 Uiso 1 1 calc R . . C2 C 0.1632(8) -0.0604(5) 0.1838(5) 0.0363(15) Uani 1 1 d U . . C3 C 0.2445(9) -0.0276(5) 0.1147(5) 0.0413(17) Uani 1 1 d U . . H3 H 0.2793 -0.0551 0.0699 0.050 Uiso 1 1 calc R . . C4 C 0.2651(9) 0.0518(6) 0.1232(5) 0.0428(17) Uani 1 1 d U . . C5 C 0.3453(11) 0.1118(7) 0.0624(6) 0.064(3) Uani 1 1 d U . . H5A H 0.4122 0.1266 0.0881 0.096 Uiso 1 1 calc R . . H5B H 0.2876 0.1643 0.0423 0.096 Uiso 1 1 calc R . . H5C H 0.3880 0.0833 0.0172 0.096 Uiso 1 1 calc R . . C6 C 0.0784(9) -0.1339(5) 0.4773(5) 0.042(2) Uani 1 1 d U . . H6A H 0.1012 -0.1630 0.5305 0.063 Uiso 1 1 calc R . . H6B H 0.1042 -0.1741 0.4395 0.063 Uiso 1 1 calc R . . H6C H -0.0164 -0.1145 0.4818 0.063 Uiso 1 1 calc R . . C7 C 0.1496(8) -0.0576(5) 0.4470(5) 0.0327(15) Uani 1 1 d U . . C8 C 0.2434(8) -0.0334(5) 0.4806(5) 0.0360(16) Uani 1 1 d U . . H8 H 0.2777 -0.0624 0.5285 0.043 Uiso 1 1 calc R . . C9 C 0.2787(7) 0.0424(5) 0.4305(5) 0.0318(15) Uani 1 1 d U . . C10 C 0.3771(8) 0.0939(6) 0.4450(5) 0.044(2) Uani 1 1 d U . . H10A H 0.4575 0.0860 0.4064 0.066 Uiso 1 1 calc R . . H10B H 0.3976 0.0741 0.5001 0.066 Uiso 1 1 calc R . . H10C H 0.3395 0.1551 0.4378 0.066 Uiso 1 1 calc R . . C11 C -0.2567(8) 0.0114(6) 0.3141(5) 0.040(2) Uani 1 1 d U . . H11A H -0.3496 0.0311 0.3087 0.060 Uiso 1 1 calc R . . H11B H -0.2495 -0.0258 0.3668 0.060 Uiso 1 1 calc R . . H11C H -0.2153 -0.0209 0.2713 0.060 Uiso 1 1 calc R . . C12 C -0.1898(7) 0.0870(5) 0.3069(5) 0.0317(14) Uani 1 1 d U . . C13 C -0.2414(8) 0.1732(5) 0.3022(5) 0.0326(15) Uani 1 1 d U . . H13 H -0.3313 0.1975 0.3035 0.039 Uiso 1 1 calc R . . C14 C -0.1361(7) 0.2178(5) 0.2951(5) 0.0299(15) Uani 1 1 d U . . C15 C -0.1478(8) 0.3134(5) 0.2925(5) 0.0377(19) Uani 1 1 d U . . H15A H -0.1034 0.3231 0.3348 0.057 Uiso 1 1 calc R . . H15B H -0.2407 0.3383 0.3014 0.057 Uiso 1 1 calc R . . H15C H -0.1068 0.3407 0.2396 0.057 Uiso 1 1 calc R . . C16 C 0.5877(8) 0.4273(6) 0.1199(5) 0.0349(14) Uani 1 1 d U . . C17 C 0.6919(8) 0.3560(6) 0.1170(5) 0.0453(16) Uani 1 1 d U . . H17 H 0.6783 0.3001 0.1453 0.054 Uiso 1 1 calc R . . C18 C 0.8138(9) 0.3696(7) 0.0719(5) 0.0484(18) Uani 1 1 d U . . H18 H 0.8836 0.3228 0.0703 0.058 Uiso 1 1 calc R . . C19 C 0.8340(9) 0.4509(7) 0.0295(5) 0.0481(18) Uani 1 1 d U . . H19 H 0.9176 0.4594 -0.0004 0.058 Uiso 1 1 calc R . . C20 C 0.7316(9) 0.5204(7) 0.0307(6) 0.0497(18) Uani 1 1 d U . . H20 H 0.7449 0.5757 0.0007 0.060 Uiso 1 1 calc R . . C21 C 0.6094(8) 0.5081(6) 0.0764(5) 0.0401(15) Uani 1 1 d U . . H21 H 0.5405 0.5555 0.0777 0.048 Uiso 1 1 calc R . . C22 C 0.4741(8) 0.4034(6) 0.2863(5) 0.0381(14) Uani 1 1 d U . . C23 C 0.5182(8) 0.4728(6) 0.3050(5) 0.0398(14) Uani 1 1 d U . . H23 H 0.5298 0.5224 0.2647 0.048 Uiso 1 1 calc R . . C24 C 0.5448(9) 0.4696(7) 0.3815(6) 0.0492(18) Uani 1 1 d U . . H24 H 0.5737 0.5174 0.3935 0.059 Uiso 1 1 calc R . . C25 C 0.5301(9) 0.3977(7) 0.4411(6) 0.0494(18) Uani 1 1 d U . . H25 H 0.5495 0.3965 0.4934 0.059 Uiso 1 1 calc R . . C26 C 0.4877(9) 0.3278(7) 0.4249(6) 0.0472(18) Uani 1 1 d U . . H26 H 0.4772 0.2787 0.4660 0.057 Uiso 1 1 calc R . . C27 C 0.4598(8) 0.3298(6) 0.3468(5) 0.0404(16) Uani 1 1 d U . . H27 H 0.4314 0.2817 0.3350 0.048 Uiso 1 1 calc R . . C28 C 0.0323(8) 0.5705(6) 0.1890(5) 0.0386(15) Uani 1 1 d U . . C29 C 0.0588(9) 0.6479(6) 0.1392(5) 0.0451(16) Uani 1 1 d U . . H29 H 0.1462 0.6601 0.1262 0.054 Uiso 1 1 calc R . . C30 C -0.0437(9) 0.7076(7) 0.1083(6) 0.0535(19) Uani 1 1 d U . . H30 H -0.0258 0.7602 0.0742 0.064 Uiso 1 1 calc R . . C31 C -0.1706(10) 0.6900(7) 0.1275(6) 0.0551(19) Uani 1 1 d U . . H31 H -0.2395 0.7300 0.1053 0.066 Uiso 1 1 calc R . . C32 C -0.1987(10) 0.6149(7) 0.1787(6) 0.0547(19) Uani 1 1 d U . . H32 H -0.2870 0.6048 0.1937 0.066 Uiso 1 1 calc R . . C33 C -0.0971(9) 0.5539(6) 0.2084(6) 0.0467(17) Uani 1 1 d U . . H33 H -0.1159 0.5011 0.2416 0.056 Uiso 1 1 calc R . . C34 C 0.1750(8) 0.5328(6) 0.3247(5) 0.0413(14) Uani 1 1 d U . . C35 C 0.2064(9) 0.6161(6) 0.3155(6) 0.0473(15) Uani 1 1 d U . . H35 H 0.2229 0.6498 0.2632 0.057 Uiso 1 1 calc R . . C36 C 0.2134(10) 0.6490(7) 0.3840(6) 0.0559(19) Uani 1 1 d U . . H36 H 0.2333 0.7054 0.3784 0.067 Uiso 1 1 calc R . . C37 C 0.1904(10) 0.5973(7) 0.4613(6) 0.0551(19) Uani 1 1 d U . . H37 H 0.1941 0.6193 0.5080 0.066 Uiso 1 1 calc R . . C38 C 0.1631(10) 0.5165(7) 0.4690(6) 0.0572(19) Uani 1 1 d U . . H38 H 0.1495 0.4819 0.5212 0.069 Uiso 1 1 calc R . . C39 C 0.1550(9) 0.4839(7) 0.4012(6) 0.0484(17) Uani 1 1 d U . . H39 H 0.1353 0.4273 0.4077 0.058 Uiso 1 1 calc R . . C40 C 0.3168(8) 0.5058(5) 0.1661(5) 0.0360(14) Uani 1 1 d U . . H40A H 0.3529 0.5544 0.1765 0.043 Uiso 1 1 calc R . . H40B H 0.3011 0.5185 0.1091 0.043 Uiso 1 1 calc R . . C41 C 0.5146(9) 0.2753(6) -0.0194(6) 0.0419(19) Uani 1 1 d U . . C42 C 0.1629(19) 0.2676(15) 0.5971(14) 0.066(6) Uani 0.50 1 d PU . . H42A H 0.2058 0.2777 0.5409 0.100 Uiso 0.50 1 calc PR . . H42B H 0.0884 0.3133 0.6047 0.100 Uiso 0.50 1 calc PR . . H42C H 0.1317 0.2118 0.6096 0.100 Uiso 0.50 1 calc PR . . C43 C 0.250(3) 0.268(2) 0.6468(15) 0.085(6) Uani 0.50 1 d PU . . H43A H 0.2077 0.2533 0.7035 0.102 Uiso 0.50 1 calc PR . . H43B H 0.2729 0.3261 0.6382 0.102 Uiso 0.50 1 calc PR . . C44 C 0.456(3) 0.207(2) 0.6898(16) 0.090(6) Uani 0.50 1 d PU . . H44A H 0.4904 0.2626 0.6767 0.108 Uiso 0.50 1 calc PR . . H44B H 0.4078 0.2017 0.7455 0.108 Uiso 0.50 1 calc PR . . C45 C 0.555(2) 0.1443(18) 0.6873(16) 0.082(7) Uani 0.50 1 d PU . . H45A H 0.5356 0.0955 0.7303 0.123 Uiso 0.50 1 calc PR . . H45B H 0.6342 0.1639 0.6949 0.123 Uiso 0.50 1 calc PR . . H45C H 0.5690 0.1263 0.6348 0.123 Uiso 0.50 1 calc PR . . C46 C 0.832(2) 0.0283(13) 0.0930(12) 0.059(5) Uani 0.50 1 d PDU . . C47 C 0.883(3) 0.1144(13) 0.0789(15) 0.082(7) Uani 0.50 1 d PDU . . H47A H 0.8882 0.1286 0.1309 0.123 Uiso 0.50 1 calc PR . . H47B H 0.8220 0.1596 0.0503 0.123 Uiso 0.50 1 calc PR . . H47C H 0.9697 0.1103 0.0463 0.123 Uiso 0.50 1 calc PR . . B1 B 0.0459(9) -0.0014(6) 0.3139(5) 0.0293(19) Uani 1 1 d . . . H1 H -0.0061 -0.0547 0.3381 0.035 Uiso 1 1 d R . . O1 O 0.3654(12) 0.2091(10) 0.6348(8) 0.059(4) 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 W1 0.02703(18) 0.01943(19) 0.03451(19) -0.00126(13) -0.00216(12) -0.00615(12) Cu1 0.0307(5) 0.0258(5) 0.0350(5) -0.0037(4) 0.0011(4) -0.0054(4) Cu2 0.0311(5) 0.0210(5) 0.0373(5) -0.0031(4) -0.0032(4) -0.0058(4) S1 0.0274(10) 0.0243(11) 0.0462(12) 0.0012(9) -0.0003(8) -0.0033(8) S2 0.0287(10) 0.0268(11) 0.0352(10) -0.0033(8) -0.0037(8) -0.0043(8) S3 0.0320(10) 0.0253(11) 0.0360(11) -0.0014(8) -0.0046(8) -0.0087(8) S4 0.093(2) 0.0487(17) 0.0523(15) -0.0208(13) 0.0302(14) -0.0229(15) P1 0.0262(10) 0.0227(11) 0.0356(11) -0.0034(8) -0.0040(8) -0.0059(8) P2 0.0303(10) 0.0212(11) 0.0346(11) -0.0052(8) -0.0029(8) -0.0047(8) N1 0.035(2) 0.022(2) 0.037(2) -0.003(2) -0.004(2) -0.006(2) N2 0.038(3) 0.025(3) 0.043(3) -0.006(2) -0.002(2) -0.007(2) N3 0.034(2) 0.022(2) 0.036(2) 0.001(2) -0.003(2) -0.007(2) N4 0.034(3) 0.024(3) 0.035(3) 0.002(2) -0.005(2) -0.005(2) N5 0.032(2) 0.022(2) 0.035(2) -0.002(2) -0.007(2) -0.006(2) N6 0.030(2) 0.022(3) 0.039(3) -0.006(2) -0.004(2) -0.007(2) N7 0.044(3) 0.039(4) 0.046(4) -0.012(3) 0.011(3) -0.017(3) N8 0.111(10) 0.112(10) 0.085(9) -0.009(8) -0.036(8) -0.008(8) C1 0.056(6) 0.030(5) 0.073(6) -0.016(5) 0.000(5) -0.009(4) C2 0.043(3) 0.026(3) 0.040(3) -0.007(3) -0.005(3) -0.006(3) C3 0.052(4) 0.027(3) 0.044(4) -0.014(3) 0.003(3) -0.007(3) C4 0.051(4) 0.028(3) 0.048(4) -0.009(3) 0.004(3) -0.011(3) C5 0.086(7) 0.049(6) 0.054(6) -0.015(5) 0.024(5) -0.031(5) C6 0.051(5) 0.022(4) 0.047(5) 0.004(4) 0.005(4) -0.010(4) C7 0.035(3) 0.022(3) 0.036(3) 0.001(3) 0.000(3) -0.003(3) C8 0.040(3) 0.027(3) 0.038(3) 0.003(3) -0.009(3) -0.004(3) C9 0.033(3) 0.027(3) 0.033(3) 0.000(3) -0.006(3) -0.006(3) C10 0.037(5) 0.044(5) 0.047(5) 0.007(4) -0.012(4) -0.007(4) C11 0.034(4) 0.034(5) 0.053(5) -0.008(4) -0.005(4) -0.011(4) C12 0.029(3) 0.026(3) 0.037(3) 0.000(3) -0.002(2) -0.006(3) C13 0.029(3) 0.025(3) 0.042(3) -0.002(3) -0.006(3) -0.005(3) C14 0.027(3) 0.022(3) 0.037(3) 0.001(3) -0.005(3) -0.003(3) C15 0.032(4) 0.023(4) 0.056(5) -0.002(4) -0.009(4) -0.004(3) C16 0.032(3) 0.040(3) 0.036(3) -0.012(2) -0.002(2) -0.010(2) C17 0.037(3) 0.048(3) 0.048(3) -0.006(3) 0.001(3) -0.009(3) C18 0.036(3) 0.058(4) 0.049(4) -0.011(3) -0.001(3) -0.006(3) C19 0.039(3) 0.061(4) 0.046(3) -0.013(3) 0.004(3) -0.019(3) C20 0.048(4) 0.053(4) 0.048(4) -0.008(3) 0.004(3) -0.019(3) C21 0.037(3) 0.042(3) 0.042(3) -0.010(3) 0.001(3) -0.011(3) C22 0.032(3) 0.042(3) 0.043(3) -0.014(2) -0.005(2) -0.006(2) C23 0.038(3) 0.044(3) 0.043(3) -0.015(2) -0.011(2) -0.008(2) C24 0.049(4) 0.053(4) 0.053(4) -0.022(3) -0.011(3) -0.007(3) C25 0.045(3) 0.061(4) 0.045(3) -0.016(3) -0.011(3) -0.004(3) C26 0.041(3) 0.054(4) 0.046(3) -0.009(3) -0.008(3) -0.004(3) C27 0.034(3) 0.048(3) 0.041(3) -0.011(3) -0.008(3) -0.005(3) C28 0.037(3) 0.033(3) 0.049(3) -0.011(3) -0.009(3) -0.006(3) C29 0.041(3) 0.039(3) 0.052(3) -0.006(3) -0.007(3) -0.003(3) C30 0.050(4) 0.042(4) 0.061(4) 0.001(3) -0.009(3) -0.001(3) C31 0.049(4) 0.049(4) 0.063(4) -0.002(3) -0.017(3) 0.002(3) C32 0.044(4) 0.049(4) 0.068(4) -0.004(3) -0.011(3) -0.004(3) C33 0.042(3) 0.039(3) 0.060(4) -0.007(3) -0.010(3) -0.010(3) C34 0.041(3) 0.042(3) 0.046(3) -0.017(2) -0.009(2) -0.006(2) C35 0.050(3) 0.043(3) 0.053(3) -0.017(3) -0.010(3) -0.005(3) C36 0.059(4) 0.054(4) 0.061(4) -0.025(3) -0.010(3) -0.009(3) C37 0.055(4) 0.059(4) 0.056(4) -0.028(3) -0.010(3) -0.002(3) C38 0.060(4) 0.059(4) 0.053(4) -0.017(3) -0.005(3) -0.005(4) C39 0.049(3) 0.049(3) 0.049(3) -0.016(3) -0.004(3) -0.008(3) C40 0.033(3) 0.036(3) 0.042(3) -0.012(3) -0.002(2) -0.008(3) C41 0.045(4) 0.029(4) 0.052(4) -0.013(4) 0.007(4) -0.013(3) C42 0.041(11) 0.067(14) 0.087(14) -0.011(12) -0.010(10) -0.003(10) C43 0.087(12) 0.110(14) 0.071(11) -0.048(10) -0.023(9) 0.001(11) C44 0.092(12) 0.115(14) 0.076(11) -0.044(11) -0.030(10) 0.002(11) C45 0.053(12) 0.111(18) 0.094(15) -0.065(14) -0.026(11) 0.020(12) C46 0.087(9) 0.053(8) 0.044(7) -0.013(7) -0.030(7) -0.004(7) C47 0.104(10) 0.069(10) 0.063(9) -0.006(7) -0.005(7) -0.001(8) B1 0.034(5) 0.025(5) 0.026(4) -0.002(4) 0.000(3) -0.005(4) O1 0.041(7) 0.081(11) 0.057(8) -0.006(7) -0.032(6) 0.001(7) _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 W1 S1 2.2149(19) . ? W1 S2 2.241(2) . ? W1 N4 2.264(6) . ? W1 N2 2.280(7) . ? W1 N6 2.307(6) . ? W1 S3 2.311(2) . ? W1 Cu2 2.6546(10) . ? W1 Cu1 2.8103(10) . ? Cu1 N7 1.964(7) . ? Cu1 S1 2.288(2) . ? Cu1 P1 2.326(2) . ? Cu1 S3 2.332(2) . ? Cu1 Cu2 2.7281(12) . ? Cu2 S2 2.193(2) . ? Cu2 P2 2.203(2) . ? Cu2 S3 2.226(2) . ? S4 C41 1.642(9) . ? P1 C16 1.821(8) . ? P1 C22 1.825(8) . ? P1 C40 1.849(8) . ? P2 C28 1.825(9) . ? P2 C34 1.826(8) . ? P2 C40 1.836(8) . ? N1 C2 1.347(10) . ? N1 N2 1.400(9) . ? N1 B1 1.517(10) . ? N2 C4 1.360(10) . ? N3 C7 1.344(10) . ? N3 N4 1.386(9) . ? N3 B1 1.518(11) . ? N4 C9 1.341(10) . ? N5 C12 1.356(10) . ? N5 N6 1.382(9) . ? N5 B1 1.523(10) . ? N6 C14 1.345(9) . ? N7 C41 1.136(10) . ? N8 C46 1.138(15) . ? C1 C2 1.495(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.380(12) . ? C3 C4 1.362(12) . ? C3 H3 0.9400 . ? C4 C5 1.496(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.489(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.360(11) . ? C8 C9 1.390(11) . ? C8 H8 0.9400 . ? C9 C10 1.503(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.471(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.369(11) . ? C13 C14 1.383(10) . ? C13 H13 0.9400 . ? C14 C15 1.497(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C21 1.377(12) . ? C16 C17 1.418(12) . ? C17 C18 1.384(12) . ? C17 H17 0.9400 . ? C18 C19 1.374(13) . ? C18 H18 0.9400 . ? C19 C20 1.387(13) . ? C19 H19 0.9400 . ? C20 C21 1.386(11) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 C23 1.386(12) . ? C22 C27 1.395(12) . ? C23 C24 1.362(12) . ? C23 H23 0.9400 . ? C24 C25 1.369(14) . ? C24 H24 0.9400 . ? C25 C26 1.365(13) . ? C25 H25 0.9400 . ? C26 C27 1.399(12) . ? C26 H26 0.9400 . ? C27 H27 0.9400 . ? C28 C29 1.382(12) . ? C28 C33 1.384(12) . ? C29 C30 1.387(12) . ? C29 H29 0.9400 . ? C30 C31 1.365(13) . ? C30 H30 0.9400 . ? C31 C32 1.366(14) . ? C31 H31 0.9400 . ? C32 C33 1.384(13) . ? C32 H32 0.9400 . ? C33 H33 0.9400 . ? C34 C39 1.366(13) . ? C34 C35 1.395(13) . ? C35 C36 1.388(13) . ? C35 H35 0.9400 . ? C36 C37 1.399(14) . ? C36 H36 0.9400 . ? C37 C38 1.343(14) . ? C37 H37 0.9400 . ? C38 C39 1.379(13) . ? C38 H38 0.9400 . ? C39 H39 0.9400 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C42 C43 1.34(3) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 O1 1.39(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.30(3) . ? C44 O1 1.43(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 C47 1.513(15) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? B1 H1 1.0593 . ? 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 S1 W1 S2 102.13(7) . . ? S1 W1 N4 86.99(17) . . ? S2 W1 N4 84.14(17) . . ? S1 W1 N2 87.89(17) . . ? S2 W1 N2 160.46(17) . . ? N4 W1 N2 79.6(2) . . ? S1 W1 N6 163.15(17) . . ? S2 W1 N6 86.98(16) . . ? N4 W1 N6 79.8(2) . . ? N2 W1 N6 79.5(2) . . ? S1 W1 S3 102.83(7) . . ? S2 W1 S3 104.13(7) . . ? N4 W1 S3 165.27(17) . . ? N2 W1 S3 89.67(18) . . ? N6 W1 S3 88.38(17) . . ? S1 W1 Cu2 101.98(6) . . ? S2 W1 Cu2 52.40(5) . . ? N4 W1 Cu2 136.52(16) . . ? N2 W1 Cu2 142.28(17) . . ? N6 W1 Cu2 94.81(16) . . ? S3 W1 Cu2 52.73(5) . . ? S1 W1 Cu1 52.55(6) . . ? S2 W1 Cu1 97.01(5) . . ? N4 W1 Cu1 139.02(16) . . ? N2 W1 Cu1 102.37(16) . . ? N6 W1 Cu1 141.16(16) . . ? S3 W1 Cu1 53.09(5) . . ? Cu2 W1 Cu1 59.81(3) . . ? N7 Cu1 S1 111.3(2) . . ? N7 Cu1 P1 101.0(2) . . ? S1 Cu1 P1 116.01(8) . . ? N7 Cu1 S3 108.1(2) . . ? S1 Cu1 S3 99.96(8) . . ? P1 Cu1 S3 120.54(8) . . ? N7 Cu1 Cu2 147.8(2) . . ? S1 Cu1 Cu2 97.91(6) . . ? P1 Cu1 Cu2 76.83(6) . . ? S3 Cu1 Cu2 51.48(5) . . ? N7 Cu1 W1 135.3(2) . . ? S1 Cu1 W1 50.23(5) . . ? P1 Cu1 W1 123.74(6) . . ? S3 Cu1 W1 52.41(5) . . ? Cu2 Cu1 W1 57.26(3) . . ? S2 Cu2 P2 125.34(8) . . ? S2 Cu2 S3 108.66(8) . . ? P2 Cu2 S3 125.79(8) . . ? S2 Cu2 W1 54.06(6) . . ? P2 Cu2 W1 166.52(7) . . ? S3 Cu2 W1 55.69(5) . . ? S2 Cu2 Cu1 100.62(6) . . ? P2 Cu2 Cu1 106.00(6) . . ? S3 Cu2 Cu1 55.04(6) . . ? W1 Cu2 Cu1 62.93(3) . . ? W1 S1 Cu1 77.22(7) . . ? Cu2 S2 W1 73.54(6) . . ? Cu2 S3 W1 71.59(6) . . ? Cu2 S3 Cu1 73.48(7) . . ? W1 S3 Cu1 74.50(6) . . ? C16 P1 C22 101.9(4) . . ? C16 P1 C40 104.4(4) . . ? C22 P1 C40 103.1(4) . . ? C16 P1 Cu1 109.7(3) . . ? C22 P1 Cu1 121.3(3) . . ? C40 P1 Cu1 114.6(3) . . ? C28 P2 C34 102.9(4) . . ? C28 P2 C40 106.1(4) . . ? C34 P2 C40 104.9(4) . . ? C28 P2 Cu2 119.1(3) . . ? C34 P2 Cu2 117.9(3) . . ? C40 P2 Cu2 104.6(3) . . ? C2 N1 N2 109.6(6) . . ? C2 N1 B1 129.7(7) . . ? N2 N1 B1 120.6(6) . . ? C4 N2 N1 105.4(6) . . ? C4 N2 W1 133.1(6) . . ? N1 N2 W1 121.0(5) . . ? C7 N3 N4 109.2(6) . . ? C7 N3 B1 129.5(7) . . ? N4 N3 B1 120.7(6) . . ? C9 N4 N3 106.4(6) . . ? C9 N4 W1 131.7(5) . . ? N3 N4 W1 121.7(5) . . ? C12 N5 N6 110.0(6) . . ? C12 N5 B1 128.6(7) . . ? N6 N5 B1 121.2(6) . . ? C14 N6 N5 105.8(6) . . ? C14 N6 W1 133.5(5) . . ? N5 N6 W1 120.0(4) . . ? C41 N7 Cu1 172.4(7) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 107.5(7) . . ? N1 C2 C1 122.0(7) . . ? C3 C2 C1 130.5(8) . . ? C4 C3 C2 107.5(7) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? N2 C4 C3 110.0(7) . . ? N2 C4 C5 123.8(8) . . ? C3 C4 C5 126.2(8) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 108.3(7) . . ? N3 C7 C6 123.4(8) . . ? C8 C7 C6 128.3(8) . . ? C7 C8 C9 106.8(7) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N4 C9 C8 109.3(7) . . ? N4 C9 C10 125.1(7) . . ? C8 C9 C10 125.6(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 107.2(7) . . ? N5 C12 C11 122.8(7) . . ? C13 C12 C11 130.0(7) . . ? C12 C13 C14 107.0(7) . . ? C12 C13 H13 126.5 . . ? C14 C13 H13 126.5 . . ? N6 C14 C13 109.9(7) . . ? N6 C14 C15 124.8(7) . . ? C13 C14 C15 125.2(7) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 119.3(7) . . ? C21 C16 P1 124.9(6) . . ? C17 C16 P1 115.8(6) . . ? C18 C17 C16 119.2(9) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 120.8(9) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 120.2(8) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.8(9) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C16 C21 C20 120.8(9) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C23 C22 C27 118.7(8) . . ? C23 C22 P1 122.7(7) . . ? C27 C22 P1 118.5(6) . . ? C24 C23 C22 120.4(9) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 121.0(9) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 120.4(9) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 119.5(9) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C22 C27 C26 120.0(9) . . ? C22 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C33 119.4(8) . . ? C29 C28 P2 122.3(7) . . ? C33 C28 P2 118.2(7) . . ? C28 C29 C30 119.9(9) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 119.9(9) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.7(9) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C31 C32 C33 120.0(9) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.0(9) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C39 C34 C35 119.2(8) . . ? C39 C34 P2 121.1(7) . . ? C35 C34 P2 119.7(7) . . ? C36 C35 C34 119.8(9) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 119.3(10) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 120.2(9) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.6(10) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C34 C39 C38 120.9(9) . . ? C34 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? P2 C40 P1 107.6(4) . . ? P2 C40 H40A 110.2 . . ? P1 C40 H40A 110.2 . . ? P2 C40 H40B 110.2 . . ? P1 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? N7 C41 S4 178.3(9) . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C42 C43 O1 113(2) . . ? C42 C43 H43A 108.9 . . ? O1 C43 H43A 108.9 . . ? C42 C43 H43B 108.9 . . ? O1 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C45 C44 O1 114(2) . . ? C45 C44 H44A 108.8 . . ? O1 C44 H44A 108.8 . . ? C45 C44 H44B 108.8 . . ? O1 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N8 C46 C47 154(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N1 B1 N3 108.8(6) . . ? N1 B1 N5 107.1(6) . . ? N3 B1 N5 109.8(6) . . ? N1 B1 H1 118.7 . . ? N3 B1 H1 104.8 . . ? N5 B1 H1 107.4 . . ? C43 O1 C44 113.2(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.260 _refine_diff_density_min -1.563 _refine_diff_density_rms 0.172 _database_code_depnum_ccdc_archive 'CCDC 973425' ####################################################################### # # 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_4^.^1.25MeCN #============================================================================== # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H48 B Cu2 N6 P2 S5 W, F6 P, 1.25(C2 H3 N)' _chemical_formula_sum 'C44.50 H51.75 B Cu2 F6 N7.25 P3 S5 W' _chemical_formula_weight 1377.13 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmc2(1) _symmetry_space_group_name_Hall 'C 2c -2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 16.1727(5) _cell_length_b 20.7446(5) _cell_length_c 16.2709(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5458.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5726 _cell_measurement_theta_min 3.8800 _cell_measurement_theta_max 28.4280 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2742 _exptl_absorpt_coefficient_mu 3.213 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5005 _exptl_absorpt_correction_T_max 0.6274 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Atlas, Gemini' _diffrn_detector_area_resol_mean 10.4692 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 10580 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_unetI/netI 0.0406 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4490 _reflns_number_gt 4255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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 H atoms of a methyl group (C(4)) was refined to be disordered over two sites by rotating along the C(4)-C(5) bond with equal occupancies. The residue electron density was assumed to be MeCN, but stable refinement of the solvent molecule could not be achieved. Since the disorder model did not give satisfactory results, the solvent contribution to the scattering factors has been taken into account with PLATON/SQUEEZE. A total of 112 electrons were found in each unit cell, corresponding to approximate 5 MeCN molecules per unit cell. The PF~6~ group was constrined to have the same displacement parameters ; _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^)+(0.0517P)^2^+19.8977P] 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 -0.008(9) _refine_ls_number_reflns 4490 _refine_ls_number_parameters 305 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 W1 W 0.5000 0.103725(15) 0.24679(2) 0.02774(11) Uani 1 2 d S . . Cu1 Cu 0.41341(6) 0.20772(4) 0.27849(5) 0.0346(2) Uani 1 1 d . . . S1 S 0.5000 0.16459(12) 0.36840(15) 0.0337(6) Uani 1 2 d S . . S2 S 0.39343(12) 0.14257(9) 0.17478(12) 0.0358(4) Uani 1 1 d . . . S3 S 0.35280(13) 0.30180(9) 0.29042(12) 0.0384(5) Uani 1 1 d . . . P1 P 0.33104(12) 0.32272(10) 0.17231(12) 0.0339(4) Uani 1 1 d . . . N1 N 0.5000 -0.0405(4) 0.1765(6) 0.0324(19) Uani 1 2 d S . . N2 N 0.5000 0.0252(4) 0.1530(5) 0.0318(19) Uani 1 2 d S . . N3 N 0.4108(4) 0.0348(3) 0.3101(4) 0.0331(14) Uani 1 1 d . . . N4 N 0.5763(4) -0.0311(3) 0.3073(4) 0.0312(14) Uani 1 1 d . . . C1 C 0.6441(6) -0.1331(4) 0.3532(6) 0.051(2) Uani 1 1 d . . . H1A H 0.6948 -0.1448 0.3813 0.077 Uiso 1 1 calc R . . H1B H 0.6437 -0.1524 0.2988 0.077 Uiso 1 1 calc R . . H1C H 0.5971 -0.1488 0.3843 0.077 Uiso 1 1 calc R . . C2 C 0.6391(4) -0.0614(4) 0.3456(5) 0.0349(16) Uani 1 1 d . . . C3 C 0.6933(5) -0.0147(4) 0.3734(5) 0.046(2) Uani 1 1 d . . . H3 H 0.7428 -0.0218 0.4024 0.056 Uiso 1 1 calc R . . C4 C 0.5000 -0.1503(5) 0.1130(8) 0.059(4) Uani 1 2 d S . . H4A H 0.5000 -0.1638 0.1701 0.088 Uiso 0.50 2 calc SPR . . H4B H 0.5490 -0.1669 0.0859 0.088 Uiso 0.25 1 calc PR . . H4C H 0.4510 -0.1669 0.0859 0.088 Uiso 0.25 1 calc PR . . H4D H 0.5000 -0.1680 0.0578 0.088 Uiso 0.50 2 calc SPR . . H4E H 0.4510 -0.1648 0.1420 0.088 Uiso 0.25 1 calc PR . . H4F H 0.5490 -0.1648 0.1420 0.088 Uiso 0.25 1 calc PR . . C5 C 0.5000 -0.0770(5) 0.1085(7) 0.040(3) Uani 1 2 d S . . C6 C 0.5000 -0.0382(5) 0.0413(6) 0.041(3) Uani 1 2 d S . . H6 H 0.5000 -0.0510 -0.0141 0.049 Uiso 1 2 calc SR . . C7 C 0.5000 0.0233(6) 0.0711(6) 0.042(3) Uani 1 2 d S . . C8 C 0.5000 0.0851(6) 0.0177(8) 0.054(3) Uani 1 2 d S . . H8A H 0.4436 0.0999 0.0102 0.080 Uiso 0.50 1 calc PR . . H8B H 0.5244 0.0757 -0.0354 0.080 Uiso 0.50 1 calc PR . . H8C H 0.5320 0.1184 0.0450 0.080 Uiso 0.50 1 calc PR . . C9 C 0.3385(5) 0.0433(4) 0.3509(5) 0.0376(18) Uani 1 1 d . . . C10 C 0.2985(6) 0.1075(4) 0.3668(6) 0.057(3) Uani 1 1 d . . . H10A H 0.2457 0.1010 0.3938 0.085 Uiso 1 1 calc R . . H10B H 0.2899 0.1297 0.3150 0.085 Uiso 1 1 calc R . . H10C H 0.3341 0.1333 0.4018 0.085 Uiso 1 1 calc R . . C11 C 0.3038(5) 0.4068(4) 0.1661(5) 0.043(2) Uani 1 1 d . . . C12 C 0.3510(6) 0.4511(4) 0.2092(6) 0.056(2) Uani 1 1 d . . . H12 H 0.3923 0.4366 0.2453 0.068 Uiso 1 1 calc R . . C13 C 0.3379(7) 0.5161(4) 0.1995(7) 0.067(3) Uani 1 1 d . . . H13 H 0.3724 0.5460 0.2261 0.080 Uiso 1 1 calc R . . C14 C 0.2728(7) 0.5372(5) 0.1498(8) 0.075(3) Uani 1 1 d . . . H14 H 0.2627 0.5815 0.1429 0.090 Uiso 1 1 calc R . . C15 C 0.2235(7) 0.4922(5) 0.1108(7) 0.063(3) Uani 1 1 d . . . H15 H 0.1787 0.5059 0.0785 0.076 Uiso 1 1 calc R . . C16 C 0.2393(6) 0.4288(4) 0.1189(6) 0.052(2) Uani 1 1 d . . . H16 H 0.2054 0.3988 0.0916 0.063 Uiso 1 1 calc R . . C17 C 0.2516(5) 0.2736(3) 0.1267(5) 0.0371(17) Uani 1 1 d . . . C18 C 0.2476(6) 0.2671(5) 0.0428(5) 0.058(2) Uani 1 1 d . . . H18 H 0.2855 0.2893 0.0093 0.069 Uiso 1 1 calc R . . C19 C 0.1877(7) 0.2277(6) 0.0070(7) 0.076(3) Uani 1 1 d . . . H19 H 0.1866 0.2219 -0.0503 0.091 Uiso 1 1 calc R . . C20 C 0.1306(7) 0.1976(5) 0.0556(8) 0.077(3) Uani 1 1 d . . . H20 H 0.0901 0.1707 0.0325 0.093 Uiso 1 1 calc R . . C21 C 0.1338(6) 0.2079(4) 0.1412(7) 0.061(3) Uani 1 1 d . . . H21 H 0.0921 0.1905 0.1746 0.073 Uiso 1 1 calc R . . C22 C 0.1945(5) 0.2418(3) 0.1760(5) 0.0403(18) Uani 1 1 d . . . H22 H 0.1986 0.2441 0.2336 0.048 Uiso 1 1 calc R . . C23 C 0.4222(4) 0.3113(4) 0.1091(4) 0.0374(17) Uani 1 1 d . . . H23A H 0.4313 0.2651 0.1010 0.045 Uiso 1 1 calc R . . H23B H 0.4125 0.3307 0.0551 0.045 Uiso 1 1 calc R . . C24 C 0.5000 0.3410(5) 0.1467(7) 0.037(2) Uani 1 2 d S . . H24A H 0.5000 0.3338 0.2062 0.045 Uiso 1 2 calc SR . . H24B H 0.5000 0.3876 0.1370 0.045 Uiso 1 2 calc SR . . P2 P 0.0000 0.1867(2) 0.3656(3) 0.0854(9) Uani 1 2 d S . . F1 F 0.0000 0.1355(5) 0.4354(5) 0.0854(9) Uani 1 2 d S . . F2 F 0.0000 0.2379(5) 0.2960(5) 0.0854(9) Uani 1 2 d S . . F3 F 0.0000 0.1321(5) 0.2976(5) 0.0854(9) Uani 1 2 d S . . F4 F 0.0000 0.2411(5) 0.4337(5) 0.0854(9) Uani 1 2 d S . . F5 F 0.1000(5) 0.1895(3) 0.3645(4) 0.0854(9) Uani 1 1 d . . . B1 B 0.5000 -0.0588(6) 0.2667(7) 0.032(3) Uani 1 2 d S . . HB1 H 0.5000 -0.106(5) 0.272(6) 0.038 Uiso 1 2 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 W1 0.0386(2) 0.02011(18) 0.02454(18) 0.00090(18) 0.000 0.000 Cu1 0.0467(5) 0.0269(4) 0.0302(4) 0.0011(3) 0.0010(4) 0.0053(4) S1 0.0484(15) 0.0275(13) 0.0250(13) 0.0042(10) 0.000 0.000 S2 0.0447(11) 0.0293(9) 0.0333(9) -0.0013(7) -0.0057(8) 0.0038(8) S3 0.0571(13) 0.0309(10) 0.0272(10) -0.0019(8) 0.0016(9) 0.0118(9) P1 0.0405(11) 0.0300(10) 0.0312(10) 0.0024(8) -0.0004(8) 0.0070(9) N1 0.048(5) 0.009(4) 0.040(5) 0.006(3) 0.000 0.000 N2 0.051(5) 0.013(4) 0.032(5) 0.004(3) 0.000 0.000 N3 0.039(3) 0.028(3) 0.033(3) 0.005(3) 0.004(3) -0.001(3) N4 0.040(4) 0.019(3) 0.035(3) 0.002(2) 0.000(3) 0.004(3) C1 0.057(6) 0.033(4) 0.064(6) 0.000(4) 0.004(4) 0.015(4) C2 0.032(4) 0.034(4) 0.039(4) 0.005(3) 0.003(3) 0.003(3) C3 0.042(5) 0.049(5) 0.048(5) 0.006(4) -0.013(4) 0.018(4) C4 0.102(11) 0.031(6) 0.043(7) -0.007(5) 0.000 0.000 C5 0.055(7) 0.032(6) 0.032(6) -0.008(5) 0.000 0.000 C6 0.061(7) 0.039(6) 0.022(6) -0.009(5) 0.000 0.000 C7 0.053(7) 0.045(7) 0.027(6) -0.001(5) 0.000 0.000 C8 0.081(9) 0.035(6) 0.045(7) 0.006(5) 0.000 0.000 C9 0.040(4) 0.034(4) 0.039(4) 0.000(3) 0.005(3) 0.008(3) C10 0.053(6) 0.047(5) 0.071(6) 0.000(4) 0.032(5) 0.006(4) C11 0.049(5) 0.029(4) 0.051(5) 0.006(4) 0.007(4) 0.018(4) C12 0.055(5) 0.046(5) 0.068(6) -0.014(4) -0.014(4) 0.017(4) C13 0.071(7) 0.038(5) 0.091(8) -0.009(5) -0.005(6) 0.004(5) C14 0.072(7) 0.037(5) 0.116(10) 0.017(6) 0.027(7) 0.016(5) C15 0.062(6) 0.045(6) 0.082(7) 0.021(5) 0.001(5) 0.018(5) C16 0.047(5) 0.048(5) 0.062(6) 0.002(4) -0.009(4) 0.010(4) C17 0.038(4) 0.027(4) 0.047(4) -0.003(3) -0.005(3) 0.011(3) C18 0.069(6) 0.065(6) 0.040(5) 0.003(5) -0.009(4) -0.013(5) C19 0.071(7) 0.104(9) 0.053(6) -0.018(6) -0.017(5) -0.013(7) C20 0.070(7) 0.066(7) 0.096(9) -0.039(6) -0.013(6) 0.000(6) C21 0.063(6) 0.033(5) 0.086(7) -0.021(5) 0.006(5) -0.013(4) C22 0.047(5) 0.029(4) 0.045(4) -0.008(3) 0.002(4) 0.004(4) C23 0.041(4) 0.039(4) 0.032(4) 0.004(3) -0.004(3) 0.004(4) C24 0.048(6) 0.021(5) 0.042(6) -0.002(4) 0.000 0.000 P2 0.120(2) 0.0766(19) 0.0592(15) -0.0008(14) 0.000 0.000 F1 0.120(2) 0.0766(19) 0.0592(15) -0.0008(14) 0.000 0.000 F2 0.120(2) 0.0766(19) 0.0592(15) -0.0008(14) 0.000 0.000 F3 0.120(2) 0.0766(19) 0.0592(15) -0.0008(14) 0.000 0.000 F4 0.120(2) 0.0766(19) 0.0592(15) -0.0008(14) 0.000 0.000 F5 0.120(2) 0.0766(19) 0.0592(15) -0.0008(14) 0.000 0.000 B1 0.038(6) 0.022(5) 0.035(8) -0.001(4) 0.000 0.000 _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 W1 N2 2.232(8) . ? W1 S2 2.2346(19) . ? W1 S2 2.2346(19) 4_655 ? W1 N3 2.278(6) . ? W1 N3 2.278(6) 4_655 ? W1 S1 2.347(3) . ? W1 Cu1 2.6232(9) . ? W1 Cu1 2.6232(9) 4_655 ? Cu1 S2 2.186(2) . ? Cu1 S3 2.193(2) . ? Cu1 S1 2.214(2) . ? Cu1 Cu1 2.8009(19) 4_655 ? S1 Cu1 2.214(2) 4_655 ? S3 P1 2.001(3) . ? P1 C17 1.800(8) . ? P1 C11 1.801(7) . ? P1 C23 1.813(7) . ? N1 C5 1.341(14) . ? N1 N2 1.417(11) . ? N1 B1 1.515(15) . ? N2 C7 1.334(13) . ? N3 C9 1.355(9) . ? N3 N4 1.383(8) 4_655 ? N4 C2 1.348(9) . ? N4 N3 1.383(8) 4_655 ? N4 B1 1.513(9) . ? C1 C2 1.496(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.383(12) . ? C3 C9 1.359(12) 4_655 ? C3 H3 0.9400 . ? C4 C5 1.522(16) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C4 H4E 0.9700 . ? C4 H4F 0.9700 . ? C5 C6 1.358(16) . ? C6 C7 1.365(16) . ? C6 H6 0.9400 . ? C7 C8 1.547(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C3 1.359(12) 4_655 ? C9 C10 1.504(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C16 1.373(12) . ? C11 C12 1.385(12) . ? C12 C13 1.374(12) . ? C12 H12 0.9400 . ? C13 C14 1.398(15) . ? C13 H13 0.9400 . ? C14 C15 1.382(16) . ? C14 H14 0.9400 . ? C15 C16 1.347(13) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 C18 1.374(12) . ? C17 C22 1.390(11) . ? C18 C19 1.395(14) . ? C18 H18 0.9400 . ? C19 C20 1.367(16) . ? C19 H19 0.9400 . ? C20 C21 1.410(16) . ? C20 H20 0.9400 . ? C21 C22 1.332(12) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? C23 C24 1.528(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C23 1.528(9) 4_655 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? P2 F2 1.552(10) . ? P2 F1 1.555(10) . ? P2 F3 1.583(10) . ? P2 F4 1.582(10) . ? P2 F5 1.619(8) . ? P2 F5 1.619(8) 4 ? B1 N4 1.513(9) 4_655 ? B1 HB1 0.98(10) . ? 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 N2 W1 S2 84.52(13) . . ? N2 W1 S2 84.52(13) . 4_655 ? S2 W1 S2 100.95(10) . 4_655 ? N2 W1 N3 81.4(2) . . ? S2 W1 N3 88.55(16) . . ? S2 W1 N3 162.22(16) 4_655 . ? N2 W1 N3 81.4(2) . 4_655 ? S2 W1 N3 162.21(16) . 4_655 ? S2 W1 N3 88.56(16) 4_655 4_655 ? N3 W1 N3 78.6(3) . 4_655 ? N2 W1 S1 165.7(2) . . ? S2 W1 S1 104.36(6) . . ? S2 W1 S1 104.36(6) 4_655 . ? N3 W1 S1 87.51(16) . . ? N3 W1 S1 87.52(16) 4_655 . ? N2 W1 Cu1 137.26(12) . . ? S2 W1 Cu1 52.75(5) . . ? S2 W1 Cu1 102.61(5) 4_655 . ? N3 W1 Cu1 95.12(15) . . ? N3 W1 Cu1 139.97(16) 4_655 . ? S1 W1 Cu1 52.55(5) . . ? N2 W1 Cu1 137.26(12) . 4_655 ? S2 W1 Cu1 102.61(5) . 4_655 ? S2 W1 Cu1 52.75(5) 4_655 4_655 ? N3 W1 Cu1 139.97(16) . 4_655 ? N3 W1 Cu1 95.12(15) 4_655 4_655 ? S1 W1 Cu1 52.55(5) . 4_655 ? Cu1 W1 Cu1 64.54(4) . 4_655 ? S2 Cu1 S3 123.54(8) . . ? S2 Cu1 S1 110.72(9) . . ? S3 Cu1 S1 125.73(9) . . ? S2 Cu1 W1 54.46(5) . . ? S3 Cu1 W1 171.15(7) . . ? S1 Cu1 W1 57.31(7) . . ? S2 Cu1 Cu1 98.50(6) . 4_655 ? S3 Cu1 Cu1 116.55(6) . 4_655 ? S1 Cu1 Cu1 50.76(5) . 4_655 ? W1 Cu1 Cu1 57.73(2) . 4_655 ? Cu1 S1 Cu1 78.47(9) . 4_655 ? Cu1 S1 W1 70.15(7) . . ? Cu1 S1 W1 70.15(7) 4_655 . ? Cu1 S2 W1 72.79(6) . . ? P1 S3 Cu1 100.76(9) . . ? C17 P1 C11 110.5(4) . . ? C17 P1 C23 105.8(4) . . ? C11 P1 C23 107.1(4) . . ? C17 P1 S3 113.5(3) . . ? C11 P1 S3 107.8(3) . . ? C23 P1 S3 111.9(3) . . ? C5 N1 N2 108.7(8) . . ? C5 N1 B1 131.1(8) . . ? N2 N1 B1 120.1(8) . . ? C7 N2 N1 104.0(8) . . ? C7 N2 W1 134.8(7) . . ? N1 N2 W1 121.2(6) . . ? C9 N3 N4 106.0(6) . 4_655 ? C9 N3 W1 133.3(5) . . ? N4 N3 W1 120.6(4) 4_655 . ? C2 N4 N3 109.4(6) . 4_655 ? C2 N4 B1 129.7(6) . . ? N3 N4 B1 120.9(6) 4_655 . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N4 C2 C3 107.6(6) . . ? N4 C2 C1 122.9(7) . . ? C3 C2 C1 129.4(7) . . ? C9 C3 C2 106.9(7) 4_655 . ? C9 C3 H3 126.5 4_655 . ? C2 C3 H3 126.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 C4 H4D 109.5 . . ? H4A C4 H4D 141.1 . . ? H4B C4 H4D 56.3 . . ? H4C C4 H4D 56.3 . . ? C5 C4 H4E 109.5 . . ? H4A C4 H4E 56.3 . . ? H4B C4 H4E 141.1 . . ? H4C C4 H4E 56.3 . . ? H4D C4 H4E 109.5 . . ? C5 C4 H4F 109.5 . . ? H4A C4 H4F 56.3 . . ? H4B C4 H4F 56.3 . . ? H4C C4 H4F 141.1 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? N1 C5 C6 109.2(9) . . ? N1 C5 C4 121.6(10) . . ? C6 C5 C4 129.2(10) . . ? C5 C6 C7 105.6(9) . . ? C5 C6 H6 127.2 . . ? C7 C6 H6 127.2 . . ? N2 C7 C6 112.5(10) . . ? N2 C7 C8 122.4(10) . . ? C6 C7 C8 125.1(10) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C3 110.1(7) . 4_655 ? N3 C9 C10 124.8(7) . . ? C3 C9 C10 125.1(7) 4_655 . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 118.7(7) . . ? C16 C11 P1 122.6(7) . . ? C12 C11 P1 118.6(6) . . ? C13 C12 C11 120.6(9) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 119.3(10) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 119.2(9) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 120.4(10) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 121.6(10) . . ? C15 C16 H16 119.2 . . ? C11 C16 H16 119.2 . . ? C18 C17 C22 119.7(8) . . ? C18 C17 P1 119.9(7) . . ? C22 C17 P1 120.4(6) . . ? C17 C18 C19 120.3(9) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 119.6(10) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 118.6(10) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C22 C21 C20 121.8(10) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C17 119.6(9) . . ? C21 C22 H22 120.2 . . ? C17 C22 H22 120.2 . . ? C24 C23 P1 113.0(5) . . ? C24 C23 H23A 109.0 . . ? P1 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? P1 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 C23 110.8(8) . 4_655 ? C23 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 4_655 . ? C23 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 4_655 . ? H24A C24 H24B 108.1 . . ? F2 P2 F1 179.9(6) . . ? F2 P2 F3 88.9(5) . . ? F1 P2 F3 91.2(5) . . ? F2 P2 F4 91.3(5) . . ? F1 P2 F4 88.6(5) . . ? F3 P2 F4 179.8(6) . . ? F2 P2 F5 88.1(3) . . ? F1 P2 F5 91.9(3) . . ? F3 P2 F5 91.0(3) . . ? F4 P2 F5 89.0(3) . . ? F2 P2 F5 88.1(3) . 4 ? F1 P2 F5 91.9(3) . 4 ? F3 P2 F5 91.0(3) . 4 ? F4 P2 F5 89.0(3) . 4 ? F5 P2 F5 175.7(6) . 4 ? N4 B1 N4 109.2(8) . 4_655 ? N4 B1 N1 109.1(6) . . ? N4 B1 N1 109.1(6) 4_655 . ? N4 B1 HB1 110(3) . . ? N4 B1 HB1 110(3) 4_655 . ? N1 B1 HB1 110(6) . . ? 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 0.000 0.031 -0.038 162 28 ' ' 2 0.000 -0.031 0.462 162 28 ' ' 3 0.500 0.469 0.462 162 28 ' ' 4 0.500 0.531 0.962 162 28 ' ' _platon_squeeze_details ; The solvated MeCN molecules were squeezed ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.359 _refine_diff_density_min -1.274 _refine_diff_density_rms 0.110 _database_code_depnum_ccdc_archive 'CCDC 973426' ####################################################################### # # 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_5^.^3MeCN #============================================================================== # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H50 B Cu2 N8 P2 S3 W, F6 P, 3(C2 H3 N)' _chemical_formula_sum 'C52 H59 B Cu2 F6 N11 P3 S3 W' _chemical_formula_weight 1462.93 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 12.9289(5) _cell_length_b 14.5593(5) _cell_length_c 16.3703(6) _cell_angle_alpha 89.5230(10) _cell_angle_beta 89.6630(10) _cell_angle_gamma 71.5480(10) _cell_volume 2922.94(19) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9843 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.63 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 2.939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5641 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction' _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 'Bruker ApexII' _diffrn_measurement_method 'phi and omega scans' _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 82609 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_unetI/netI 0.0197 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10297 _reflns_number_gt 9725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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 the C---C and C\\tbN bond distances of the solvent MeCN molecules were fixed to be 1.42 and 1.12 ?, respectively. ; _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^)+(0.0216P)^2^+5.3136P] 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 10297 _refine_ls_number_parameters 721 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0517 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.033 _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 W1 W 0.389310(8) 0.744075(7) 0.203660(6) 0.01154(4) Uani 1 1 d . . . P1 P 0.55640(5) 0.73351(5) 0.47068(4) 0.01386(14) Uani 1 1 d . . . P2 P 0.68218(5) 0.87680(5) 0.25361(4) 0.01374(14) Uani 1 1 d . . . P3 P -0.00517(8) 0.70991(6) 0.72346(5) 0.0347(2) Uani 1 1 d . . . S2 S 0.39642(5) 0.88964(5) 0.16306(4) 0.01623(13) Uani 1 1 d . . . S3 S 0.56789(5) 0.65973(5) 0.24132(4) 0.01490(13) Uani 1 1 d . . . S1 S 0.30112(5) 0.78067(5) 0.32290(4) 0.01740(14) Uani 1 1 d . . . F1 F -0.0364(2) 0.68520(17) 0.81309(14) 0.0605(6) Uani 1 1 d . . . F2 F 0.1150(2) 0.6910(2) 0.7565(2) 0.0859(9) Uani 1 1 d . . . F3 F 0.0253(2) 0.59833(15) 0.70116(14) 0.0643(7) Uani 1 1 d . . . F4 F 0.0304(3) 0.7322(2) 0.63622(18) 0.1202(15) Uani 1 1 d . . . F5 F -0.1251(2) 0.7264(2) 0.6937(2) 0.0989(12) Uani 1 1 d . . . F6 F -0.0403(3) 0.82048(17) 0.74671(18) 0.0808(9) Uani 1 1 d . . . N1 N 0.35176(18) 0.60222(16) 0.20381(13) 0.0155(5) Uani 1 1 d . . . N2 N 0.28868(17) 0.58273(16) 0.14277(13) 0.0150(5) Uani 1 1 d . . . N3 N 0.20026(17) 0.74420(16) 0.07930(13) 0.0145(5) Uani 1 1 d . . . N4 N 0.22313(17) 0.79287(15) 0.14516(13) 0.0146(5) Uani 1 1 d . . . N5 N 0.38160(18) 0.64263(15) 0.02975(13) 0.0146(5) Uani 1 1 d . . . N6 N 0.43909(17) 0.69075(15) 0.07342(13) 0.0144(4) Uani 1 1 d . . . N7 N 0.57285(18) 0.90460(15) 0.40381(13) 0.0166(5) Uani 1 1 d . . . N8 N 0.40381(19) 0.92793(16) 0.45864(13) 0.0180(5) Uani 1 1 d . . . N9 N 1.0801(4) 0.0340(4) 0.5999(2) 0.0947(17) Uani 1 1 d D . . N10 N 0.1089(3) 0.3426(3) 0.9523(3) 0.0755(13) Uani 1 1 d D . . N11 N 0.6307(4) 0.8192(4) 0.8348(3) 0.0801(15) Uani 1 1 d D . . C1 C 0.0642(2) 0.7671(2) -0.03244(19) 0.0286(7) Uani 1 1 d . . . H1A H 0.0301 0.7186 -0.0181 0.043 Uiso 1 1 calc R . . H1B H 0.1236 0.7398 -0.0705 0.043 Uiso 1 1 calc R . . H1C H 0.0107 0.8224 -0.0576 0.043 Uiso 1 1 calc R . . C2 C 0.1076(2) 0.7988(2) 0.04277(17) 0.0201(6) Uani 1 1 d . . . C3 C 0.0689(2) 0.8833(2) 0.08619(18) 0.0218(6) Uani 1 1 d . . . H3 H 0.0055 0.9351 0.0747 0.026 Uiso 1 1 calc R . . C4 C 0.1408(2) 0.8780(2) 0.15004(17) 0.0190(6) Uani 1 1 d . . . C5 C 0.1277(2) 0.9509(2) 0.21534(19) 0.0265(7) Uani 1 1 d . . . H5A H 0.1974 0.9603 0.2258 0.040 Uiso 1 1 calc R . . H5B H 0.1017 0.9283 0.2649 0.040 Uiso 1 1 calc R . . H5C H 0.0754 1.0118 0.1981 0.040 Uiso 1 1 calc R . . C6 C 0.1877(3) 0.4672(2) 0.1103(2) 0.0279(7) Uani 1 1 d . . . H6A H 0.2279 0.4401 0.0612 0.042 Uiso 1 1 calc R . . H6B H 0.1224 0.5193 0.0954 0.042 Uiso 1 1 calc R . . H6C H 0.1675 0.4172 0.1395 0.042 Uiso 1 1 calc R . . C7 C 0.2574(2) 0.50585(19) 0.16361(17) 0.0181(6) Uani 1 1 d . . . C8 C 0.3009(2) 0.4738(2) 0.23908(17) 0.0204(6) Uani 1 1 d . . . H8 H 0.2927 0.4210 0.2689 0.024 Uiso 1 1 calc R . . C9 C 0.3589(2) 0.53436(19) 0.26260(16) 0.0187(6) Uani 1 1 d . . . C10 C 0.4221(3) 0.5248(2) 0.34002(18) 0.0301(7) Uani 1 1 d . . . H10A H 0.3920 0.5826 0.3726 0.045 Uiso 1 1 calc R . . H10B H 0.4978 0.5168 0.3273 0.045 Uiso 1 1 calc R . . H10C H 0.4176 0.4688 0.3705 0.045 Uiso 1 1 calc R . . C11 C 0.3852(3) 0.5634(2) -0.10610(17) 0.0255(6) Uani 1 1 d . . . H11A H 0.3143 0.6039 -0.1249 0.038 Uiso 1 1 calc R . . H11B H 0.3784 0.5047 -0.0815 0.038 Uiso 1 1 calc R . . H11C H 0.4352 0.5467 -0.1521 0.038 Uiso 1 1 calc R . . C12 C 0.4278(2) 0.61701(19) -0.04428(16) 0.0173(6) Uani 1 1 d . . . C13 C 0.5171(2) 0.6489(2) -0.04908(16) 0.0194(6) Uani 1 1 d . . . H13 H 0.5654 0.6413 -0.0935 0.023 Uiso 1 1 calc R . . C14 C 0.5221(2) 0.69420(19) 0.02408(16) 0.0168(6) Uani 1 1 d . . . C15 C 0.6071(2) 0.7397(2) 0.04475(18) 0.0240(6) Uani 1 1 d . . . H15A H 0.6431 0.7115 0.0950 0.036 Uiso 1 1 calc R . . H15B H 0.5731 0.8088 0.0517 0.036 Uiso 1 1 calc R . . H15C H 0.6604 0.7283 0.0009 0.036 Uiso 1 1 calc R . . C16 C 0.7778(2) 1.0178(2) 0.20795(19) 0.0238(6) Uani 1 1 d . . . H16 H 0.8210 0.9995 0.2550 0.029 Uiso 1 1 calc R . . C17 C 0.7890(3) 1.0910(2) 0.1576(2) 0.0320(7) Uani 1 1 d . . . H17 H 0.8406 1.1220 0.1702 0.038 Uiso 1 1 calc R . . C18 C 0.7250(3) 1.1185(2) 0.0894(2) 0.0378(8) Uani 1 1 d . . . H18 H 0.7331 1.1683 0.0555 0.045 Uiso 1 1 calc R . . C19 C 0.6493(3) 1.0738(3) 0.0703(2) 0.0416(9) Uani 1 1 d . . . H19 H 0.6055 1.0932 0.0236 0.050 Uiso 1 1 calc R . . C20 C 0.6374(3) 0.9998(2) 0.11996(19) 0.0299(7) Uani 1 1 d . . . H20 H 0.5856 0.9692 0.1070 0.036 Uiso 1 1 calc R . . C21 C 0.7021(2) 0.97131(19) 0.18857(16) 0.0186(6) Uani 1 1 d . . . C22 C 0.8149(2) 0.78522(19) 0.26663(16) 0.0160(5) Uani 1 1 d . . . C23 C 0.9094(2) 0.7878(2) 0.22772(19) 0.0270(7) Uani 1 1 d . . . H23 H 0.9074 0.8392 0.1920 0.032 Uiso 1 1 calc R . . C24 C 1.0071(3) 0.7147(2) 0.2414(2) 0.0349(8) Uani 1 1 d . . . H24 H 1.0711 0.7174 0.2153 0.042 Uiso 1 1 calc R . . C25 C 1.0114(2) 0.6382(2) 0.2929(2) 0.0313(7) Uani 1 1 d . . . H25 H 1.0780 0.5892 0.3021 0.038 Uiso 1 1 calc R . . C26 C 0.9173(2) 0.6342(2) 0.33084(19) 0.0291(7) Uani 1 1 d . . . H26 H 0.9195 0.5819 0.3657 0.035 Uiso 1 1 calc R . . C27 C 0.8197(2) 0.7069(2) 0.31770(17) 0.0224(6) Uani 1 1 d . . . H27 H 0.7559 0.7035 0.3435 0.027 Uiso 1 1 calc R . . C28 C 0.6791(2) 0.63084(19) 0.48980(16) 0.0164(5) Uani 1 1 d . . . C29 C 0.6945(2) 0.5455(2) 0.44748(19) 0.0252(6) Uani 1 1 d . . . H29 H 0.6413 0.5408 0.4103 0.030 Uiso 1 1 calc R . . C30 C 0.7879(3) 0.4669(2) 0.4595(2) 0.0342(8) Uani 1 1 d . . . H30 H 0.7979 0.4094 0.4302 0.041 Uiso 1 1 calc R . . C31 C 0.8658(3) 0.4732(2) 0.5141(2) 0.0326(7) Uani 1 1 d . . . H31 H 0.9288 0.4198 0.5223 0.039 Uiso 1 1 calc R . . C32 C 0.8516(2) 0.5573(2) 0.55675(19) 0.0283(7) Uani 1 1 d . . . H32 H 0.9048 0.5613 0.5942 0.034 Uiso 1 1 calc R . . C33 C 0.7592(2) 0.6361(2) 0.54459(17) 0.0223(6) Uani 1 1 d . . . H33 H 0.7503 0.6936 0.5735 0.027 Uiso 1 1 calc R . . C34 C 0.4761(2) 0.73978(19) 0.56323(16) 0.0172(6) Uani 1 1 d . . . C35 C 0.5142(2) 0.7534(2) 0.64017(17) 0.0236(6) Uani 1 1 d . . . H35 H 0.5827 0.7623 0.6453 0.028 Uiso 1 1 calc R . . C36 C 0.4515(3) 0.7538(2) 0.70921(18) 0.0307(7) Uani 1 1 d . . . H36 H 0.4776 0.7631 0.7610 0.037 Uiso 1 1 calc R . . C37 C 0.3511(3) 0.7407(2) 0.7021(2) 0.0344(8) Uani 1 1 d . . . H37 H 0.3095 0.7395 0.7491 0.041 Uiso 1 1 calc R . . C38 C 0.3116(3) 0.7292(3) 0.6263(2) 0.0366(8) Uani 1 1 d . . . H38 H 0.2422 0.7218 0.6215 0.044 Uiso 1 1 calc R . . C39 C 0.3737(3) 0.7285(2) 0.55716(18) 0.0277(7) Uani 1 1 d . . . H39 H 0.3465 0.7203 0.5056 0.033 Uiso 1 1 calc R . . C40 C 0.4624(2) 0.95337(18) 0.40010(16) 0.0155(5) Uani 1 1 d . . . B1 B 0.2710(2) 0.6396(2) 0.06212(18) 0.0163(6) Uani 1 1 d . . . H1D H 0.2371 0.6057 0.0179 0.020 Uiso 1 1 d R . . C41 C 0.4146(2) 1.02165(19) 0.33895(16) 0.0191(6) Uani 1 1 d . . . H41 H 0.4574 1.0378 0.2981 0.023 Uiso 1 1 calc R . . C42 C 0.3031(2) 1.0641(2) 0.34083(18) 0.0252(6) Uani 1 1 d . . . H42 H 0.2686 1.1101 0.3008 0.030 Uiso 1 1 calc R . . C43 C 0.2416(2) 1.0390(2) 0.40178(19) 0.0277(7) Uani 1 1 d . . . H43 H 0.1655 1.0679 0.4042 0.033 Uiso 1 1 calc R . . C44 C 0.2953(2) 0.9707(2) 0.45824(18) 0.0234(6) Uani 1 1 d . . . H44 H 0.2538 0.9529 0.4990 0.028 Uiso 1 1 calc R . . C45 C 0.6115(2) 0.83759(19) 0.47181(16) 0.0169(5) Uani 1 1 d . . . H45A H 0.5904 0.8728 0.5232 0.020 Uiso 1 1 calc R . . H45B H 0.6914 0.8126 0.4699 0.020 Uiso 1 1 calc R . . C46 C 0.6503(2) 0.93612(19) 0.35608(16) 0.0175(6) Uani 1 1 d . . . H46A H 0.7182 0.9224 0.3871 0.021 Uiso 1 1 calc R . . H46B H 0.6211 1.0064 0.3481 0.021 Uiso 1 1 calc R . . C47 C 0.1323(4) 0.4784(3) 0.8609(3) 0.0558(11) Uani 1 1 d D . . H47A H 0.2071 0.4599 0.8416 0.084 Uiso 1 1 calc R . . H47B H 0.1161 0.5379 0.8918 0.084 Uiso 1 1 calc R . . H47C H 0.0835 0.4885 0.8146 0.084 Uiso 1 1 calc R . . C48 C 0.1178(3) 0.4028(3) 0.9124(2) 0.0382(8) Uani 1 1 d D . . C49 C 0.9386(5) 0.1773(4) 0.5317(4) 0.095(2) Uani 1 1 d D . . H49A H 0.8721 0.1949 0.5640 0.143 Uiso 1 1 calc R . . H49B H 0.9239 0.1578 0.4777 0.143 Uiso 1 1 calc R . . H49C H 0.9650 0.2325 0.5271 0.143 Uiso 1 1 calc R . . C50 C 1.0188(4) 0.0993(4) 0.5704(3) 0.0589(12) Uani 1 1 d D . . C51 C 0.7743(3) 0.8611(4) 0.9132(3) 0.0707(16) Uani 1 1 d D . . H51A H 0.8253 0.8022 0.9353 0.106 Uiso 1 1 calc R . . H51B H 0.7403 0.9040 0.9575 0.106 Uiso 1 1 calc R . . H51C H 0.8129 0.8930 0.8777 0.106 Uiso 1 1 calc R . . C52 C 0.6879(4) 0.8364(3) 0.8649(3) 0.0571(12) Uani 1 1 d D . . Cu1 Cu 0.47618(3) 0.72624(2) 0.352261(18) 0.01540(7) Uani 1 1 d . . . Cu2 Cu 0.55284(3) 0.81455(2) 0.221183(19) 0.01557(7) 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 W1 0.01161(6) 0.01312(6) 0.01001(6) 0.00008(4) -0.00096(4) -0.00406(4) P1 0.0159(3) 0.0143(3) 0.0113(3) 0.0011(3) -0.0026(3) -0.0047(3) P2 0.0136(3) 0.0145(3) 0.0137(3) 0.0022(3) -0.0007(3) -0.0053(3) P3 0.0398(5) 0.0266(4) 0.0316(5) -0.0035(4) 0.0041(4) -0.0017(4) S2 0.0166(3) 0.0149(3) 0.0171(3) 0.0026(2) -0.0032(3) -0.0049(3) S3 0.0136(3) 0.0154(3) 0.0143(3) 0.0004(2) -0.0017(2) -0.0027(3) S1 0.0161(3) 0.0222(3) 0.0129(3) -0.0015(3) 0.0015(3) -0.0047(3) F1 0.0767(17) 0.0550(14) 0.0457(13) 0.0011(11) 0.0151(12) -0.0151(13) F2 0.0466(15) 0.098(2) 0.121(3) 0.0003(19) -0.0042(16) -0.0348(15) F3 0.0877(18) 0.0328(12) 0.0544(14) -0.0109(10) -0.0252(13) 0.0070(12) F4 0.175(4) 0.085(2) 0.0582(18) 0.0259(16) 0.054(2) 0.017(2) F5 0.0619(18) 0.0741(19) 0.133(3) -0.0343(19) -0.0530(18) 0.0197(15) F6 0.120(2) 0.0292(12) 0.090(2) -0.0089(13) 0.0162(18) -0.0186(14) N1 0.0190(12) 0.0171(11) 0.0117(11) -0.0002(9) -0.0012(9) -0.0075(9) N2 0.0155(11) 0.0172(11) 0.0141(11) 0.0001(9) -0.0009(9) -0.0075(9) N3 0.0130(11) 0.0197(11) 0.0127(11) 0.0025(9) -0.0030(9) -0.0076(9) N4 0.0127(11) 0.0161(11) 0.0157(11) 0.0004(9) -0.0014(9) -0.0054(9) N5 0.0166(11) 0.0163(11) 0.0121(11) -0.0002(9) -0.0017(9) -0.0069(9) N6 0.0152(11) 0.0170(11) 0.0111(11) -0.0005(9) -0.0006(9) -0.0052(9) N7 0.0169(12) 0.0147(11) 0.0171(11) 0.0031(9) 0.0010(9) -0.0035(9) N8 0.0218(12) 0.0173(11) 0.0159(11) -0.0030(9) 0.0018(9) -0.0074(10) N9 0.065(3) 0.131(4) 0.046(2) 0.014(3) 0.009(2) 0.027(3) N10 0.068(3) 0.102(3) 0.077(3) 0.043(3) -0.029(2) -0.056(3) N11 0.078(3) 0.125(4) 0.061(3) 0.039(3) -0.009(2) -0.068(3) C1 0.0232(16) 0.0375(18) 0.0273(16) 0.0074(13) -0.0127(13) -0.0129(14) C2 0.0150(14) 0.0269(15) 0.0202(14) 0.0076(12) -0.0020(11) -0.0093(12) C3 0.0124(13) 0.0234(15) 0.0273(16) 0.0080(12) -0.0022(11) -0.0025(12) C4 0.0137(13) 0.0201(14) 0.0226(14) 0.0031(11) 0.0021(11) -0.0045(11) C5 0.0215(15) 0.0217(15) 0.0310(17) -0.0034(13) 0.0002(13) 0.0009(12) C6 0.0278(16) 0.0262(16) 0.0354(18) 0.0029(13) -0.0063(13) -0.0166(13) C7 0.0170(14) 0.0156(13) 0.0219(14) -0.0009(11) 0.0030(11) -0.0055(11) C8 0.0244(15) 0.0160(13) 0.0224(15) 0.0038(11) 0.0027(12) -0.0090(12) C9 0.0226(15) 0.0168(13) 0.0164(14) 0.0023(11) 0.0007(11) -0.0056(11) C10 0.049(2) 0.0250(16) 0.0208(15) 0.0103(12) -0.0112(14) -0.0178(15) C11 0.0323(17) 0.0283(16) 0.0169(14) -0.0065(12) 0.0010(12) -0.0110(13) C12 0.0213(14) 0.0163(13) 0.0127(13) 0.0006(10) 0.0005(11) -0.0036(11) C13 0.0206(14) 0.0218(14) 0.0135(13) 0.0002(11) 0.0049(11) -0.0035(12) C14 0.0140(13) 0.0181(13) 0.0172(13) 0.0028(11) 0.0018(11) -0.0035(11) C15 0.0187(15) 0.0344(17) 0.0217(15) -0.0029(12) 0.0062(12) -0.0126(13) C16 0.0225(15) 0.0214(15) 0.0283(16) 0.0025(12) 0.0020(12) -0.0083(12) C17 0.0278(17) 0.0228(16) 0.047(2) 0.0021(14) 0.0106(15) -0.0099(13) C18 0.039(2) 0.0261(17) 0.046(2) 0.0143(15) 0.0153(16) -0.0078(15) C19 0.048(2) 0.042(2) 0.0314(19) 0.0216(16) -0.0071(16) -0.0107(17) C20 0.0335(18) 0.0312(17) 0.0271(16) 0.0096(13) -0.0061(13) -0.0133(14) C21 0.0197(14) 0.0169(13) 0.0181(14) 0.0041(11) 0.0038(11) -0.0042(11) C22 0.0159(13) 0.0177(13) 0.0145(13) -0.0017(10) -0.0002(10) -0.0053(11) C23 0.0220(16) 0.0242(15) 0.0322(17) 0.0072(13) 0.0085(13) -0.0039(13) C24 0.0188(16) 0.0341(18) 0.048(2) 0.0074(15) 0.0123(14) -0.0040(14) C25 0.0182(15) 0.0283(17) 0.0391(19) 0.0052(14) 0.0014(13) 0.0043(13) C26 0.0247(16) 0.0260(16) 0.0318(17) 0.0122(13) 0.0001(13) -0.0017(13) C27 0.0175(14) 0.0255(15) 0.0234(15) 0.0059(12) 0.0023(12) -0.0058(12) C28 0.0174(14) 0.0172(13) 0.0143(13) 0.0039(10) -0.0018(11) -0.0050(11) C29 0.0251(16) 0.0212(15) 0.0294(16) 0.0000(12) -0.0072(13) -0.0074(13) C30 0.0331(18) 0.0181(15) 0.047(2) -0.0036(14) -0.0054(15) -0.0011(13) C31 0.0237(16) 0.0242(16) 0.043(2) 0.0061(14) -0.0047(14) 0.0020(13) C32 0.0227(16) 0.0319(17) 0.0282(16) 0.0054(13) -0.0090(13) -0.0056(13) C33 0.0250(15) 0.0207(14) 0.0198(14) 0.0003(11) -0.0048(12) -0.0050(12) C34 0.0221(14) 0.0139(13) 0.0154(13) 0.0008(10) 0.0006(11) -0.0054(11) C35 0.0274(16) 0.0254(15) 0.0186(14) -0.0008(12) -0.0013(12) -0.0094(13) C36 0.046(2) 0.0327(17) 0.0140(14) -0.0021(12) 0.0018(13) -0.0125(15) C37 0.046(2) 0.0347(18) 0.0271(17) -0.0044(14) 0.0161(15) -0.0188(16) C38 0.0353(19) 0.047(2) 0.0348(19) -0.0075(16) 0.0104(15) -0.0240(17) C39 0.0296(17) 0.0370(18) 0.0215(15) -0.0039(13) 0.0021(13) -0.0177(14) C40 0.0190(14) 0.0131(13) 0.0144(13) -0.0044(10) 0.0005(11) -0.0049(11) B1 0.0180(15) 0.0206(15) 0.0123(14) 0.0004(12) -0.0017(12) -0.0089(13) C41 0.0257(15) 0.0167(13) 0.0141(13) -0.0013(11) 0.0014(11) -0.0057(12) C42 0.0304(17) 0.0178(14) 0.0219(15) -0.0037(12) -0.0065(13) 0.0004(12) C43 0.0181(15) 0.0285(16) 0.0327(17) -0.0086(13) -0.0018(13) -0.0016(13) C44 0.0226(15) 0.0255(15) 0.0237(15) -0.0072(12) 0.0048(12) -0.0097(13) C45 0.0190(14) 0.0165(13) 0.0154(13) 0.0016(10) -0.0041(11) -0.0056(11) C46 0.0190(14) 0.0171(13) 0.0176(14) 0.0001(11) 0.0012(11) -0.0075(11) C47 0.058(3) 0.055(3) 0.059(3) 0.017(2) -0.018(2) -0.025(2) C48 0.0258(18) 0.049(2) 0.042(2) 0.0032(17) -0.0131(15) -0.0158(16) C49 0.085(4) 0.098(4) 0.082(4) 0.035(3) 0.026(3) -0.001(3) C50 0.046(3) 0.086(3) 0.044(2) -0.005(2) 0.016(2) -0.020(3) C51 0.0221(19) 0.084(3) 0.104(4) 0.065(3) -0.019(2) -0.016(2) C52 0.051(3) 0.069(3) 0.044(3) 0.035(2) 0.012(2) -0.008(2) Cu1 0.01776(17) 0.01749(16) 0.01099(15) 0.00059(12) -0.00291(12) -0.00560(13) Cu2 0.01468(16) 0.01746(16) 0.01597(16) 0.00147(13) -0.00255(13) -0.00707(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 W1 S1 2.2363(6) . ? W1 S2 2.2452(6) . ? W1 N4 2.255(2) . ? W1 N1 2.266(2) . ? W1 N6 2.293(2) . ? W1 S3 2.3298(6) . ? W1 Cu2 2.6440(3) . ? W1 Cu1 2.6615(3) . ? P1 C34 1.818(3) . ? P1 C28 1.829(3) . ? P1 C45 1.868(3) . ? P1 Cu1 2.2229(7) . ? P2 C21 1.814(3) . ? P2 C22 1.822(3) . ? P2 C46 1.876(3) . ? P2 Cu2 2.2085(7) . ? P3 F4 1.561(3) . ? P3 F5 1.572(3) . ? P3 F6 1.577(2) . ? P3 F2 1.587(3) . ? P3 F1 1.588(2) . ? P3 F3 1.591(2) . ? S2 Cu2 2.1901(7) . ? S3 Cu1 2.2180(7) . ? S3 Cu2 2.2222(7) . ? S1 Cu1 2.2030(7) . ? N1 C9 1.356(3) . ? N1 N2 1.380(3) . ? N2 C7 1.346(3) . ? N2 B1 1.532(4) . ? N3 C2 1.350(3) . ? N3 N4 1.379(3) . ? N3 B1 1.536(4) . ? N4 C4 1.357(3) . ? N5 C12 1.350(3) . ? N5 N6 1.378(3) . ? N5 B1 1.536(4) . ? N6 C14 1.353(3) . ? N7 C40 1.381(3) . ? N7 C46 1.449(3) . ? N7 C45 1.456(3) . ? N8 C40 1.338(3) . ? N8 C44 1.342(4) . ? N9 C50 1.133(6) . ? N10 C48 1.123(5) . ? N11 C52 0.988(5) . ? C1 C2 1.491(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.375(4) . ? C3 C4 1.388(4) . ? C3 H3 0.9400 . ? C4 C5 1.484(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.493(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.376(4) . ? C8 C9 1.385(4) . ? C8 H8 0.9400 . ? C9 C10 1.493(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.493(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.375(4) . ? C13 C14 1.384(4) . ? C13 H13 0.9400 . ? C14 C15 1.493(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.386(4) . ? C16 C21 1.393(4) . ? C16 H16 0.9400 . ? C17 C18 1.373(5) . ? C17 H17 0.9400 . ? C18 C19 1.376(5) . ? C18 H18 0.9400 . ? C19 C20 1.391(4) . ? C19 H19 0.9400 . ? C20 C21 1.385(4) . ? C20 H20 0.9400 . ? C22 C23 1.386(4) . ? C22 C27 1.394(4) . ? C23 C24 1.388(4) . ? C23 H23 0.9400 . ? C24 C25 1.378(5) . ? C24 H24 0.9400 . ? C25 C26 1.382(4) . ? C25 H25 0.9400 . ? C26 C27 1.383(4) . ? C26 H26 0.9400 . ? C27 H27 0.9400 . ? C28 C29 1.385(4) . ? C28 C33 1.395(4) . ? C29 C30 1.390(4) . ? C29 H29 0.9400 . ? C30 C31 1.375(5) . ? C30 H30 0.9400 . ? C31 C32 1.376(5) . ? C31 H31 0.9400 . ? C32 C33 1.384(4) . ? C32 H32 0.9400 . ? C33 H33 0.9400 . ? C34 C39 1.388(4) . ? C34 C35 1.393(4) . ? C35 C36 1.385(4) . ? C35 H35 0.9400 . ? C36 C37 1.377(5) . ? C36 H36 0.9400 . ? C37 C38 1.377(5) . ? C37 H37 0.9400 . ? C38 C39 1.382(4) . ? C38 H38 0.9400 . ? C39 H39 0.9400 . ? C40 C41 1.405(4) . ? B1 H1D 1.0516 . ? C41 C42 1.377(4) . ? C41 H41 0.9400 . ? C42 C43 1.389(4) . ? C42 H42 0.9400 . ? C43 C44 1.371(4) . ? C43 H43 0.9400 . ? C44 H44 0.9400 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.440(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C49 C50 1.419(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C51 C52 1.507(7) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? Cu1 Cu2 2.8241(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 W1 S2 101.32(2) . . ? S1 W1 N4 86.26(6) . . ? S2 W1 N4 84.20(6) . . ? S1 W1 N1 89.07(6) . . ? S2 W1 N1 160.48(6) . . ? N4 W1 N1 79.99(8) . . ? S1 W1 N6 163.67(6) . . ? S2 W1 N6 87.74(6) . . ? N4 W1 N6 81.13(8) . . ? N1 W1 N6 78.60(8) . . ? S1 W1 S3 103.84(2) . . ? S2 W1 S3 104.14(2) . . ? N4 W1 S3 165.08(6) . . ? N1 W1 S3 89.09(6) . . ? N6 W1 S3 86.79(6) . . ? S1 W1 Cu2 102.480(19) . . ? S2 W1 Cu2 52.454(18) . . ? N4 W1 Cu2 136.61(5) . . ? N1 W1 Cu2 141.52(6) . . ? N6 W1 Cu2 93.82(5) . . ? S3 W1 Cu2 52.613(17) . . ? S1 W1 Cu1 52.592(19) . . ? S2 W1 Cu1 102.338(18) . . ? N4 W1 Cu1 138.85(5) . . ? N1 W1 Cu1 97.11(5) . . ? N6 W1 Cu1 139.02(5) . . ? S3 W1 Cu1 52.251(17) . . ? Cu2 W1 Cu1 64.320(10) . . ? C34 P1 C28 103.54(12) . . ? C34 P1 C45 107.59(12) . . ? C28 P1 C45 101.83(12) . . ? C34 P1 Cu1 117.48(9) . . ? C28 P1 Cu1 113.98(9) . . ? C45 P1 Cu1 111.02(8) . . ? C21 P2 C22 107.20(12) . . ? C21 P2 C46 103.53(12) . . ? C22 P2 C46 104.55(12) . . ? C21 P2 Cu2 118.38(10) . . ? C22 P2 Cu2 112.87(9) . . ? C46 P2 Cu2 109.09(9) . . ? F4 P3 F5 91.3(2) . . ? F4 P3 F6 91.27(17) . . ? F5 P3 F6 88.34(17) . . ? F4 P3 F2 90.8(2) . . ? F5 P3 F2 177.7(2) . . ? F6 P3 F2 92.38(18) . . ? F4 P3 F1 177.7(2) . . ? F5 P3 F1 90.85(18) . . ? F6 P3 F1 89.48(14) . . ? F2 P3 F1 87.01(16) . . ? F4 P3 F3 90.18(17) . . ? F5 P3 F3 89.71(15) . . ? F6 P3 F3 177.59(17) . . ? F2 P3 F3 89.52(15) . . ? F1 P3 F3 89.14(14) . . ? Cu2 S2 W1 73.17(2) . . ? Cu1 S3 Cu2 78.99(2) . . ? Cu1 S3 W1 71.59(2) . . ? Cu2 S3 W1 70.97(2) . . ? Cu1 S1 W1 73.67(2) . . ? C9 N1 N2 105.8(2) . . ? C9 N1 W1 132.35(18) . . ? N2 N1 W1 120.26(15) . . ? C7 N2 N1 110.2(2) . . ? C7 N2 B1 128.8(2) . . ? N1 N2 B1 120.8(2) . . ? C2 N3 N4 110.0(2) . . ? C2 N3 B1 129.8(2) . . ? N4 N3 B1 120.0(2) . . ? C4 N4 N3 106.5(2) . . ? C4 N4 W1 130.94(18) . . ? N3 N4 W1 120.85(15) . . ? C12 N5 N6 110.5(2) . . ? C12 N5 B1 129.2(2) . . ? N6 N5 B1 119.5(2) . . ? C14 N6 N5 105.6(2) . . ? C14 N6 W1 132.81(17) . . ? N5 N6 W1 121.55(15) . . ? C40 N7 C46 121.3(2) . . ? C40 N7 C45 117.3(2) . . ? C46 N7 C45 119.5(2) . . ? C40 N8 C44 117.8(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C2 C3 107.4(2) . . ? N3 C2 C1 122.5(3) . . ? C3 C2 C1 130.1(3) . . ? C2 C3 C4 107.3(2) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? N4 C4 C3 108.8(2) . . ? N4 C4 C5 125.2(2) . . ? C3 C4 C5 125.9(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 107.7(2) . . ? N2 C7 C6 123.0(2) . . ? C8 C7 C6 129.3(3) . . ? C7 C8 C9 106.7(2) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N1 C9 C8 109.6(2) . . ? N1 C9 C10 125.2(2) . . ? C8 C9 C10 125.1(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 107.3(2) . . ? N5 C12 C11 123.6(2) . . ? C13 C12 C11 129.1(3) . . ? C12 C13 C14 106.8(2) . . ? C12 C13 H13 126.6 . . ? C14 C13 H13 126.6 . . ? N6 C14 C13 109.8(2) . . ? N6 C14 C15 125.6(2) . . ? C13 C14 C15 124.6(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.7(3) . . ? C17 C16 H16 120.1 . . ? C21 C16 H16 120.1 . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 120.0(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C16 119.8(3) . . ? C20 C21 P2 118.7(2) . . ? C16 C21 P2 121.4(2) . . ? C23 C22 C27 118.7(3) . . ? C23 C22 P2 124.2(2) . . ? C27 C22 P2 117.1(2) . . ? C22 C23 C24 120.1(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.5(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 120.1(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C22 120.8(3) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? C29 C28 C33 118.6(3) . . ? C29 C28 P1 119.2(2) . . ? C33 C28 P1 122.2(2) . . ? C28 C29 C30 120.6(3) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 120.0(3) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 120.1(3) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.6(3) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? C39 C34 C35 118.7(3) . . ? C39 C34 P1 118.7(2) . . ? C35 C34 P1 122.6(2) . . ? C36 C35 C34 120.4(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 120.0(3) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.2(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C34 120.6(3) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? N8 C40 N7 114.1(2) . . ? N8 C40 C41 122.6(2) . . ? N7 C40 C41 123.2(2) . . ? N2 B1 N3 108.4(2) . . ? N2 B1 N5 109.0(2) . . ? N3 B1 N5 107.6(2) . . ? N2 B1 H1D 110.8 . . ? N3 B1 H1D 113.0 . . ? N5 B1 H1D 107.9 . . ? C42 C41 C40 117.8(3) . . ? C42 C41 H41 121.1 . . ? C40 C41 H41 121.1 . . ? C41 C42 C43 120.1(3) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 117.9(3) . . ? C44 C43 H43 121.0 . . ? C42 C43 H43 121.0 . . ? N8 C44 C43 123.8(3) . . ? N8 C44 H44 118.1 . . ? C43 C44 H44 118.1 . . ? N7 C45 P1 113.00(18) . . ? N7 C45 H45A 109.0 . . ? P1 C45 H45A 109.0 . . ? N7 C45 H45B 109.0 . . ? P1 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? N7 C46 P2 113.87(18) . . ? N7 C46 H46A 108.8 . . ? P2 C46 H46A 108.8 . . ? N7 C46 H46B 108.8 . . ? P2 C46 H46B 108.8 . . ? H46A C46 H46B 107.7 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N10 C48 C47 178.4(5) . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N9 C50 C49 176.5(6) . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N11 C52 C51 178.3(5) . . ? S1 Cu1 S3 108.79(3) . . ? S1 Cu1 P1 128.19(3) . . ? S3 Cu1 P1 123.02(3) . . ? S1 Cu1 W1 53.738(18) . . ? S3 Cu1 W1 56.158(18) . . ? P1 Cu1 W1 170.27(2) . . ? S1 Cu1 Cu2 97.94(2) . . ? S3 Cu1 Cu2 50.569(19) . . ? P1 Cu1 Cu2 113.70(2) . . ? W1 Cu1 Cu2 57.539(9) . . ? S2 Cu2 P2 127.07(3) . . ? S2 Cu2 S3 109.76(3) . . ? P2 Cu2 S3 123.15(3) . . ? S2 Cu2 W1 54.372(18) . . ? P2 Cu2 W1 172.08(2) . . ? S3 Cu2 W1 56.413(18) . . ? S2 Cu2 Cu1 98.87(2) . . ? P2 Cu2 Cu1 114.84(2) . . ? S3 Cu2 Cu1 50.438(19) . . ? W1 Cu2 Cu1 58.141(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.700 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 973427' ####################################################################### # # 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_6^.^Et~2~O #============================================================================== # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H96 B2 Cu4 N14 P4 S6 W2, 2(F6 P), C4 H10 O' _chemical_formula_sum 'C88 H106 B2 Cu4 F12 N14 O P6 S6 W2' _chemical_formula_weight 2625.53 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' W W -0.8490 6.8722 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0992(3) _cell_length_b 18.1283(4) _cell_length_c 22.0485(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.890(2) _cell_angle_gamma 90.00 _cell_volume 5235.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14067 _cell_measurement_theta_min 3.4270 _cell_measurement_theta_max 28.8740 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 3.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63130 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Atlas, Gemini' _diffrn_detector_area_resol_mean 10.4692 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 31589 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_unetI/netI 0.0564 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9220 _reflns_number_gt 7376 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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 solvent Et~2~O molecule was refined to have rigid bond restrains and similar Uij, while the C---C and C---O bond lengths were fixed to be 1.50 and 1.45 \%A, respectively. The PF~6~ anion was constrined to be a rigid octahedron with same displacement parameters. ; _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^)+(0.0574P)^2^+6.9929P] 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 9220 _refine_ls_number_parameters 623 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.002 _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 W1 W 0.268812(17) 0.936613(13) 0.157555(11) 0.02396(10) Uani 1 1 d . . . Cu1 Cu 0.46635(5) 0.91056(4) 0.14683(4) 0.0306(2) Uani 1 1 d . . . Cu2 Cu 0.31288(6) 0.84850(4) 0.06480(4) 0.0333(2) Uani 1 1 d . . . S1 S 0.39822(12) 1.01882(9) 0.16066(8) 0.0303(4) Uani 1 1 d . . . S2 S 0.21468(12) 0.94633(10) 0.06123(8) 0.0334(4) Uani 1 1 d . . . S3 S 0.35094(12) 0.82299(9) 0.16060(7) 0.0305(4) Uani 1 1 d . . . P1 P 0.61842(11) 0.87237(9) 0.11877(8) 0.0269(4) Uani 1 1 d . . . P2 P 0.37277(12) 0.79319(9) -0.01731(8) 0.0287(4) Uani 1 1 d . . . N1 N 0.1898(4) 0.9536(3) 0.2948(2) 0.0295(12) Uani 1 1 d . . . N2 N 0.2742(4) 0.9366(3) 0.2616(2) 0.0300(12) Uani 1 1 d . . . N3 N 0.1006(4) 1.0363(3) 0.2221(2) 0.0291(12) Uani 1 1 d . . . N4 N 0.1684(4) 1.0351(3) 0.1750(2) 0.0284(12) Uani 1 1 d . . . N5 N 0.0584(4) 0.9032(3) 0.2241(2) 0.0286(12) Uani 1 1 d . . . N6 N 0.1217(4) 0.8776(3) 0.1794(2) 0.0301(12) Uani 1 1 d . . . N7 N 0.5105(4) 0.8973(3) 0.0141(2) 0.0277(12) Uani 1 1 d . . . C1 C 0.1375(6) 0.9719(5) 0.4021(3) 0.056(2) Uani 1 1 d . . . H1A H 0.1130 1.0220 0.3969 0.084 Uiso 1 1 calc R . . H1B H 0.1698 0.9668 0.4417 0.084 Uiso 1 1 calc R . . H1C H 0.0805 0.9379 0.3987 0.084 Uiso 1 1 calc R . . C2 C 0.2135(5) 0.9548(4) 0.3540(3) 0.0354(16) Uani 1 1 d . . . C3 C 0.3147(5) 0.9377(4) 0.3605(3) 0.0388(17) Uani 1 1 d . . . H3 H 0.3521 0.9340 0.3971 0.047 Uiso 1 1 calc R . . C4 C 0.3513(5) 0.9271(4) 0.3027(3) 0.0325(15) Uani 1 1 d . . . C5 C 0.4572(5) 0.9049(5) 0.2889(3) 0.0467(19) Uani 1 1 d . . . H5A H 0.4564 0.8577 0.2682 0.070 Uiso 1 1 calc R . . H5B H 0.4966 0.9008 0.3263 0.070 Uiso 1 1 calc R . . H5C H 0.4880 0.9418 0.2630 0.070 Uiso 1 1 calc R . . C6 C -0.0242(6) 1.1207(4) 0.2708(4) 0.050(2) Uani 1 1 d . . . H6A H -0.0754 1.0821 0.2718 0.075 Uiso 1 1 calc R . . H6B H -0.0567 1.1673 0.2605 0.075 Uiso 1 1 calc R . . H6C H 0.0091 1.1247 0.3102 0.075 Uiso 1 1 calc R . . C7 C 0.0541(5) 1.1023(4) 0.2236(3) 0.0354(16) Uani 1 1 d . . . C8 C 0.0909(5) 1.1435(4) 0.1776(3) 0.0365(16) Uani 1 1 d . . . H8 H 0.0714 1.1921 0.1678 0.044 Uiso 1 1 calc R . . C9 C 0.1619(5) 1.1017(4) 0.1478(3) 0.0332(15) Uani 1 1 d . . . C10 C 0.2204(5) 1.1247(4) 0.0937(3) 0.0443(18) Uani 1 1 d . . . H10A H 0.2923 1.1142 0.1005 0.066 Uiso 1 1 calc R . . H10B H 0.2112 1.1772 0.0870 0.066 Uiso 1 1 calc R . . H10C H 0.1959 1.0977 0.0584 0.066 Uiso 1 1 calc R . . C11 C -0.1109(5) 0.8749(5) 0.2690(4) 0.049(2) Uani 1 1 d . . . H11A H -0.0839 0.8767 0.3102 0.074 Uiso 1 1 calc R . . H11B H -0.1606 0.8353 0.2656 0.074 Uiso 1 1 calc R . . H11C H -0.1436 0.9215 0.2592 0.074 Uiso 1 1 calc R . . C12 C -0.0264(5) 0.8613(4) 0.2265(3) 0.0350(16) Uani 1 1 d . . . C13 C -0.0179(5) 0.8071(4) 0.1830(3) 0.0386(17) Uani 1 1 d . . . H13 H -0.0654 0.7696 0.1744 0.046 Uiso 1 1 calc R . . C14 C 0.0733(5) 0.8185(4) 0.1549(3) 0.0359(16) Uani 1 1 d . . . C15 C 0.1139(6) 0.7715(4) 0.1051(4) 0.054(2) Uani 1 1 d . . . H15A H 0.1243 0.8015 0.0693 0.081 Uiso 1 1 calc R . . H15B H 0.0653 0.7326 0.0956 0.081 Uiso 1 1 calc R . . H15C H 0.1783 0.7498 0.1180 0.081 Uiso 1 1 calc R . . C16 C 0.6568(4) 0.7857(4) 0.1538(3) 0.0300(14) Uani 1 1 d . . . C17 C 0.6486(6) 0.7804(5) 0.2154(4) 0.059(2) Uani 1 1 d . . . H17 H 0.6273 0.8215 0.2379 0.071 Uiso 1 1 calc R . . C18 C 0.6720(7) 0.7138(6) 0.2452(5) 0.077(3) Uani 1 1 d . . . H18 H 0.6660 0.7101 0.2875 0.093 Uiso 1 1 calc R . . C19 C 0.7039(6) 0.6539(5) 0.2120(4) 0.059(2) Uani 1 1 d . . . H19 H 0.7180 0.6087 0.2312 0.071 Uiso 1 1 calc R . . C20 C 0.7146(7) 0.6611(5) 0.1512(5) 0.065(3) Uani 1 1 d . . . H20 H 0.7388 0.6207 0.1289 0.079 Uiso 1 1 calc R . . C21 C 0.6913(6) 0.7253(4) 0.1215(4) 0.052(2) Uani 1 1 d . . . H21 H 0.6988 0.7284 0.0793 0.063 Uiso 1 1 calc R . . C22 C 0.7324(5) 0.9301(4) 0.1177(3) 0.0341(16) Uani 1 1 d . . . C23 C 0.7305(6) 1.0002(4) 0.1416(4) 0.0484(19) Uani 1 1 d . . . H23 H 0.6718 1.0174 0.1611 0.058 Uiso 1 1 calc R . . C24 C 0.8167(7) 1.0459(5) 0.1367(4) 0.063(2) Uani 1 1 d . . . H24 H 0.8166 1.0934 0.1538 0.076 Uiso 1 1 calc R . . C25 C 0.9005(6) 1.0209(5) 0.1069(4) 0.061(2) Uani 1 1 d . . . H25 H 0.9570 1.0522 0.1022 0.073 Uiso 1 1 calc R . . C26 C 0.9035(6) 0.9511(5) 0.0839(4) 0.059(2) Uani 1 1 d . . . H26 H 0.9624 0.9340 0.0647 0.070 Uiso 1 1 calc R . . C27 C 0.8192(5) 0.9056(4) 0.0890(3) 0.0410(17) Uani 1 1 d . . . H27 H 0.8210 0.8577 0.0729 0.049 Uiso 1 1 calc R . . C28 C 0.4461(5) 0.7084(4) -0.0070(3) 0.0374(17) Uani 1 1 d . . . C29 C 0.4330(7) 0.6666(5) 0.0445(5) 0.066(3) Uani 1 1 d . . . H29 H 0.3845 0.6806 0.0733 0.079 Uiso 1 1 calc R . . C30 C 0.4923(9) 0.6035(6) 0.0537(6) 0.093(4) Uani 1 1 d . . . H30 H 0.4853 0.5751 0.0891 0.111 Uiso 1 1 calc R . . C31 C 0.5605(8) 0.5835(5) 0.0106(7) 0.090(4) Uani 1 1 d . . . H31 H 0.5994 0.5404 0.0160 0.108 Uiso 1 1 calc R . . C32 C 0.5731(7) 0.6245(5) -0.0396(5) 0.068(3) Uani 1 1 d . . . H32 H 0.6216 0.6102 -0.0683 0.081 Uiso 1 1 calc R . . C33 C 0.5162(6) 0.6865(5) -0.0492(4) 0.057(2) Uani 1 1 d . . . H33 H 0.5249 0.7144 -0.0847 0.068 Uiso 1 1 calc R . . C34 C 0.2963(5) 0.7752(4) -0.0850(3) 0.0346(15) Uani 1 1 d . . . C35 C 0.3368(6) 0.7809(5) -0.1426(3) 0.049(2) Uani 1 1 d . . . H35 H 0.4042 0.7973 -0.1475 0.059 Uiso 1 1 calc R . . C36 C 0.2770(7) 0.7623(5) -0.1927(4) 0.066(3) Uani 1 1 d . . . H36 H 0.3033 0.7674 -0.2319 0.079 Uiso 1 1 calc R . . C37 C 0.1807(7) 0.7367(4) -0.1852(4) 0.060(3) Uani 1 1 d . . . H37 H 0.1416 0.7222 -0.2193 0.072 Uiso 1 1 calc R . . C38 C 0.1402(6) 0.7320(5) -0.1291(5) 0.061(2) Uani 1 1 d . . . H38 H 0.0727 0.7155 -0.1245 0.073 Uiso 1 1 calc R . . C39 C 0.1979(5) 0.7511(4) -0.0788(4) 0.0475(19) Uani 1 1 d . . . H39 H 0.1695 0.7477 -0.0400 0.057 Uiso 1 1 calc R . . C40 C 0.4651(5) 0.8636(4) -0.0406(3) 0.0307(15) Uani 1 1 d . . . H40A H 0.5186 0.8410 -0.0650 0.037 Uiso 1 1 calc R . . H40B H 0.4307 0.9014 -0.0653 0.037 Uiso 1 1 calc R . . C41 C 0.5926(5) 0.8503(4) 0.0388(3) 0.0302(14) Uani 1 1 d . . . H41A H 0.6548 0.8578 0.0153 0.036 Uiso 1 1 calc R . . H41B H 0.5728 0.7984 0.0351 0.036 Uiso 1 1 calc R . . C42 C 0.5455(4) 0.9735(3) 0.0031(3) 0.0258(13) Uani 1 1 d . . . H42A H 0.5854 0.9749 -0.0341 0.031 Uiso 1 1 calc R . . H42B H 0.5898 0.9895 0.0368 0.031 Uiso 1 1 calc R . . O1 O 0.2833(13) 0.5771(10) 0.1454(6) 0.102(5) Uani 0.50 1 d PDU . . C43 C 0.1571(18) 0.5605(10) 0.0736(8) 0.088(6) Uani 0.50 1 d PDU . . H43A H 0.1148 0.5231 0.0543 0.133 Uiso 0.50 1 calc PR . . H43B H 0.1993 0.5840 0.0435 0.133 Uiso 0.50 1 calc PR . . H43C H 0.1139 0.5971 0.0924 0.133 Uiso 0.50 1 calc PR . . C44 C 0.2220(13) 0.5263(11) 0.1197(9) 0.091(5) Uani 0.50 1 d PDU . . H44A H 0.1796 0.5035 0.1507 0.109 Uiso 0.50 1 calc PR . . H44B H 0.2634 0.4876 0.1012 0.109 Uiso 0.50 1 calc PR . . C45 C 0.3329(16) 0.5587(14) 0.1966(10) 0.118(8) Uani 0.50 1 d PDU . . H45A H 0.3564 0.5076 0.1930 0.141 Uiso 0.50 1 calc PR . . H45B H 0.2845 0.5604 0.2301 0.141 Uiso 0.50 1 calc PR . . C46 C 0.4211(16) 0.6053(13) 0.2127(10) 0.101(7) Uani 0.50 1 d PDU . . H46A H 0.4539 0.5864 0.2492 0.151 Uiso 0.50 1 calc PR . . H46B H 0.3982 0.6554 0.2196 0.151 Uiso 0.50 1 calc PR . . H46C H 0.4693 0.6048 0.1797 0.151 Uiso 0.50 1 calc PR . . B1 B 0.0876(6) 0.9693(4) 0.2632(4) 0.0317(17) Uani 1 1 d . . . H1B1 H 0.035(5) 0.976(4) 0.295(3) 0.038 Uiso 1 1 d . . . P3 P -0.1087(2) 0.81918(16) 0.48638(13) 0.0803(6) Uani 1 1 d D . . F1 F -0.0033(5) 0.8613(5) 0.4882(4) 0.0803(6) Uani 0.697(5) 1 d PD A 1 F2 F -0.1090(6) 0.8083(5) 0.4155(3) 0.0803(6) Uani 0.697(5) 1 d PD A 1 F3 F -0.0462(6) 0.7444(4) 0.4772(4) 0.0803(6) Uani 0.697(5) 1 d PD A 1 F4 F -0.0948(6) 0.8281(5) 0.5581(3) 0.0803(6) Uani 0.697(5) 1 d PD A 1 F5 F -0.1716(6) 0.8933(4) 0.4924(4) 0.0803(6) Uani 0.697(5) 1 d PD A 1 F6 F -0.2127(5) 0.7739(4) 0.4888(4) 0.0803(6) Uani 0.697(5) 1 d PD A 1 F1A F 0.0140(6) 0.8176(12) 0.4854(9) 0.0803(6) Uani 0.303(5) 1 d PD A 2 F2A F -0.1469(13) 0.8419(11) 0.4205(5) 0.0803(6) Uani 0.303(5) 1 d PD A 2 F3A F -0.0811(14) 0.7368(6) 0.5058(9) 0.0803(6) Uani 0.303(5) 1 d PD A 2 F4A F -0.1064(14) 0.7889(11) 0.5546(5) 0.0803(6) Uani 0.303(5) 1 d PD A 2 F5A F -0.0731(14) 0.8979(6) 0.4625(8) 0.0803(6) Uani 0.303(5) 1 d PD A 2 F6A F -0.2002(11) 0.8695(10) 0.5115(9) 0.0803(6) Uani 0.303(5) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02769(15) 0.02323(16) 0.02090(16) 0.00105(10) -0.00102(10) 0.00040(10) Cu1 0.0289(4) 0.0321(5) 0.0308(5) 0.0020(4) -0.0008(3) 0.0041(3) Cu2 0.0400(4) 0.0347(5) 0.0251(4) -0.0035(4) -0.0015(3) 0.0017(3) S1 0.0330(8) 0.0271(9) 0.0309(9) -0.0012(7) -0.0001(7) -0.0020(6) S2 0.0366(9) 0.0377(10) 0.0256(9) 0.0026(7) -0.0056(7) 0.0019(7) S3 0.0384(9) 0.0269(9) 0.0261(9) 0.0015(7) -0.0008(7) 0.0027(7) P1 0.0276(8) 0.0257(9) 0.0275(9) 0.0014(7) -0.0048(7) 0.0025(6) P2 0.0323(9) 0.0269(9) 0.0268(9) -0.0032(7) -0.0041(7) -0.0024(7) N1 0.035(3) 0.027(3) 0.026(3) 0.001(2) 0.002(2) -0.005(2) N2 0.039(3) 0.027(3) 0.024(3) 0.003(2) 0.001(2) 0.004(2) N3 0.027(3) 0.027(3) 0.034(3) -0.006(2) 0.003(2) 0.001(2) N4 0.027(3) 0.027(3) 0.032(3) 0.003(2) 0.001(2) 0.002(2) N5 0.025(3) 0.030(3) 0.031(3) 0.005(2) 0.001(2) -0.004(2) N6 0.032(3) 0.025(3) 0.032(3) 0.002(2) -0.003(2) -0.004(2) N7 0.034(3) 0.022(3) 0.027(3) 0.003(2) -0.007(2) -0.002(2) C1 0.070(5) 0.071(6) 0.027(4) -0.009(4) 0.006(4) -0.005(4) C2 0.051(4) 0.032(4) 0.023(4) -0.005(3) 0.004(3) -0.004(3) C3 0.050(4) 0.039(4) 0.027(4) 0.001(3) -0.006(3) -0.005(3) C4 0.042(4) 0.034(4) 0.022(4) 0.001(3) -0.009(3) -0.002(3) C5 0.044(4) 0.065(5) 0.031(4) 0.005(4) -0.011(3) 0.006(4) C6 0.052(4) 0.043(5) 0.055(5) -0.006(4) 0.010(4) 0.018(4) C7 0.034(3) 0.029(4) 0.044(4) -0.006(3) -0.004(3) 0.003(3) C8 0.031(3) 0.023(4) 0.055(5) 0.003(3) -0.009(3) 0.006(3) C9 0.032(3) 0.024(4) 0.043(4) 0.008(3) -0.012(3) -0.002(3) C10 0.048(4) 0.037(4) 0.048(5) 0.014(4) 0.007(3) 0.008(3) C11 0.030(4) 0.061(5) 0.057(5) -0.003(4) 0.010(3) -0.010(3) C12 0.032(4) 0.036(4) 0.036(4) 0.009(3) -0.005(3) -0.002(3) C13 0.032(4) 0.037(4) 0.047(5) 0.009(4) -0.007(3) -0.008(3) C14 0.036(4) 0.031(4) 0.040(4) -0.002(3) -0.011(3) -0.005(3) C15 0.057(5) 0.048(5) 0.056(5) -0.026(4) 0.005(4) -0.020(4) C16 0.027(3) 0.028(4) 0.034(4) 0.008(3) -0.006(3) -0.002(3) C17 0.075(6) 0.064(6) 0.040(5) 0.008(4) -0.002(4) 0.028(5) C18 0.092(7) 0.084(8) 0.056(6) 0.040(6) -0.002(5) 0.030(6) C19 0.059(5) 0.049(5) 0.070(7) 0.034(5) -0.008(4) 0.014(4) C20 0.081(6) 0.040(5) 0.075(7) 0.002(5) -0.008(5) 0.020(4) C21 0.076(5) 0.042(5) 0.040(5) 0.010(4) 0.003(4) 0.025(4) C22 0.037(4) 0.032(4) 0.033(4) 0.007(3) -0.013(3) -0.001(3) C23 0.048(4) 0.039(5) 0.058(5) -0.007(4) -0.018(4) 0.000(3) C24 0.072(6) 0.038(5) 0.078(7) -0.003(5) -0.028(5) -0.015(4) C25 0.047(5) 0.060(6) 0.075(6) 0.015(5) -0.021(4) -0.024(4) C26 0.042(4) 0.068(6) 0.065(6) 0.002(5) -0.013(4) -0.011(4) C27 0.033(4) 0.041(4) 0.048(5) 0.009(4) -0.007(3) -0.003(3) C28 0.036(4) 0.022(4) 0.054(5) -0.002(3) -0.013(3) -0.004(3) C29 0.067(6) 0.040(5) 0.092(7) 0.020(5) 0.009(5) 0.002(4) C30 0.099(8) 0.053(6) 0.126(11) 0.046(7) 0.015(7) 0.016(6) C31 0.073(7) 0.034(5) 0.162(13) 0.006(7) -0.023(7) 0.019(5) C32 0.068(6) 0.049(6) 0.085(8) -0.024(6) -0.015(5) 0.014(5) C33 0.056(5) 0.049(5) 0.065(6) -0.014(4) -0.012(4) 0.011(4) C34 0.039(4) 0.027(4) 0.038(4) -0.007(3) -0.013(3) 0.002(3) C35 0.049(4) 0.059(5) 0.039(5) -0.018(4) -0.008(3) 0.005(4) C36 0.089(7) 0.074(7) 0.034(5) -0.025(5) -0.021(4) 0.021(5) C37 0.072(6) 0.037(5) 0.069(7) -0.018(4) -0.051(5) 0.008(4) C38 0.055(5) 0.050(6) 0.075(7) 0.002(5) -0.032(5) -0.012(4) C39 0.043(4) 0.049(5) 0.050(5) -0.001(4) -0.014(3) -0.004(3) C40 0.039(4) 0.031(4) 0.022(3) 0.001(3) -0.005(3) -0.002(3) C41 0.033(3) 0.024(3) 0.033(4) 0.002(3) -0.002(3) 0.000(3) C42 0.029(3) 0.023(3) 0.025(3) 0.002(3) -0.006(3) -0.004(2) O1 0.136(12) 0.107(12) 0.062(9) 0.019(8) 0.017(7) -0.005(8) C43 0.161(18) 0.061(13) 0.044(11) -0.034(9) 0.023(9) -0.036(11) C44 0.082(12) 0.081(14) 0.112(14) 0.018(10) 0.075(8) -0.010(8) C45 0.098(15) 0.15(2) 0.110(15) 0.089(14) 0.024(10) 0.029(11) C46 0.119(16) 0.13(2) 0.057(13) 0.022(13) -0.001(10) 0.051(12) B1 0.035(4) 0.027(4) 0.033(4) 0.000(3) 0.009(3) -0.001(3) P3 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F1 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F2 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F3 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F4 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F5 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F6 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F1A 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F2A 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F3A 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F4A 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F5A 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(10) F6A 0.0819(13) 0.0767(15) 0.0827(14) -0.0079(12) 0.0116(11) -0.0016(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 W1 S2 2.2355(17) . ? W1 N4 2.255(5) . ? W1 S1 2.2572(16) . ? W1 N6 2.263(5) . ? W1 N2 2.295(5) . ? W1 S3 2.3243(16) . ? W1 Cu1 2.6446(7) . ? W1 Cu2 2.6653(8) . ? Cu1 S1 2.1793(18) . ? Cu1 P1 2.2065(17) . ? Cu1 S3 2.2163(18) . ? Cu1 Cu2 2.9096(11) . ? Cu2 S2 2.1915(18) . ? Cu2 S3 2.2116(18) . ? Cu2 P2 2.2231(18) . ? P1 C16 1.818(6) . ? P1 C22 1.824(7) . ? P1 C41 1.835(7) . ? P2 C34 1.814(7) . ? P2 C28 1.825(7) . ? P2 C40 1.838(6) . ? N1 C2 1.338(8) . ? N1 N2 1.371(7) . ? N1 B1 1.526(9) . ? N2 C4 1.357(8) . ? N3 C7 1.343(8) . ? N3 N4 1.376(7) . ? N3 B1 1.526(9) . ? N4 C9 1.351(8) . ? N5 C12 1.347(8) . ? N5 N6 1.378(7) . ? N5 B1 1.521(10) . ? N6 C14 1.352(8) . ? N7 C40 1.469(8) . ? N7 C41 1.470(8) . ? N7 C42 1.477(8) . ? C1 C2 1.497(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.366(10) . ? C3 C4 1.382(9) . ? C3 H3 0.9400 . ? C4 C5 1.480(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.509(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.356(10) . ? C8 C9 1.374(9) . ? C8 H8 0.9400 . ? C9 C10 1.487(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.483(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.378(10) . ? C13 C14 1.371(9) . ? C13 H13 0.9400 . ? C14 C15 1.495(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.369(10) . ? C16 C21 1.385(10) . ? C17 C18 1.407(12) . ? C17 H17 0.9400 . ? C18 C19 1.378(13) . ? C18 H18 0.9400 . ? C19 C20 1.354(12) . ? C19 H19 0.9400 . ? C20 C21 1.368(11) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 C23 1.376(10) . ? C22 C27 1.382(10) . ? C23 C24 1.406(11) . ? C23 H23 0.9400 . ? C24 C25 1.365(12) . ? C24 H24 0.9400 . ? C25 C26 1.364(12) . ? C25 H25 0.9400 . ? C26 C27 1.384(10) . ? C26 H26 0.9400 . ? C27 H27 0.9400 . ? C28 C33 1.375(10) . ? C28 C29 1.378(11) . ? C29 C30 1.397(13) . ? C29 H29 0.9400 . ? C30 C31 1.364(15) . ? C30 H30 0.9400 . ? C31 C32 1.345(15) . ? C31 H31 0.9400 . ? C32 C33 1.365(12) . ? C32 H32 0.9400 . ? C33 H33 0.9400 . ? C34 C39 1.371(10) . ? C34 C35 1.386(10) . ? C35 C36 1.386(11) . ? C35 H35 0.9400 . ? C36 C37 1.357(12) . ? C36 H36 0.9400 . ? C37 C38 1.357(13) . ? C37 H37 0.9400 . ? C38 C39 1.376(11) . ? C38 H38 0.9400 . ? C39 H39 0.9400 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C42 1.535(11) 3_675 ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? O1 C45 1.336(12) . ? O1 C44 1.342(12) . ? C43 C44 1.453(13) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.470(13) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? B1 H1B1 0.99(6) . ? P3 F2 1.575(6) . ? P3 F1 1.577(6) . ? P3 F5 1.583(6) . ? P3 F2A 1.584(8) . ? P3 F6 1.593(6) . ? P3 F3A 1.593(7) . ? P3 F5A 1.594(8) . ? P3 F3 1.597(6) . ? P3 F4 1.598(6) . ? P3 F4A 1.602(8) . ? P3 F1A 1.608(7) . ? P3 F6A 1.612(7) . ? F2A F5A 1.67(2) . ? F3A F4A 1.47(3) . ? 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 S2 W1 N4 85.57(14) . . ? S2 W1 S1 101.76(6) . . ? N4 W1 S1 84.93(13) . . ? S2 W1 N6 88.92(14) . . ? N4 W1 N6 80.63(18) . . ? S1 W1 N6 161.33(14) . . ? S2 W1 N2 162.64(14) . . ? N4 W1 N2 80.69(18) . . ? S1 W1 N2 87.61(14) . . ? N6 W1 N2 78.46(19) . . ? S2 W1 S3 103.71(6) . . ? N4 W1 S3 165.46(13) . . ? S1 W1 S3 103.72(6) . . ? N6 W1 S3 88.28(14) . . ? N2 W1 S3 87.94(13) . . ? S2 W1 Cu1 103.03(5) . . ? N4 W1 Cu1 136.96(13) . . ? S1 W1 Cu1 52.06(4) . . ? N6 W1 Cu1 140.56(13) . . ? N2 W1 Cu1 94.27(13) . . ? S3 W1 Cu1 52.50(4) . . ? S2 W1 Cu2 52.23(5) . . ? N4 W1 Cu2 137.71(14) . . ? S1 W1 Cu2 104.32(4) . . ? N6 W1 Cu2 94.33(14) . . ? N2 W1 Cu2 139.78(13) . . ? S3 W1 Cu2 52.08(4) . . ? Cu1 W1 Cu2 66.45(3) . . ? S1 Cu1 P1 134.05(7) . . ? S1 Cu1 S3 110.13(6) . . ? P1 Cu1 S3 115.74(7) . . ? S1 Cu1 W1 54.78(4) . . ? P1 Cu1 W1 165.93(6) . . ? S3 Cu1 W1 56.30(4) . . ? S1 Cu1 Cu2 98.90(5) . . ? P1 Cu1 Cu2 108.81(5) . . ? S3 Cu1 Cu2 48.85(5) . . ? W1 Cu1 Cu2 57.12(2) . . ? S2 Cu2 S3 109.08(7) . . ? S2 Cu2 P2 123.38(7) . . ? S3 Cu2 P2 127.32(7) . . ? S2 Cu2 W1 53.74(5) . . ? S3 Cu2 W1 56.00(5) . . ? P2 Cu2 W1 168.10(6) . . ? S2 Cu2 Cu1 96.25(5) . . ? S3 Cu2 Cu1 48.99(5) . . ? P2 Cu2 Cu1 115.56(5) . . ? W1 Cu2 Cu1 56.43(2) . . ? Cu1 S1 W1 73.16(5) . . ? Cu2 S2 W1 74.03(6) . . ? Cu2 S3 Cu1 82.16(6) . . ? Cu2 S3 W1 71.93(5) . . ? Cu1 S3 W1 71.20(5) . . ? C16 P1 C22 106.3(3) . . ? C16 P1 C41 105.4(3) . . ? C22 P1 C41 104.6(3) . . ? C16 P1 Cu1 113.4(2) . . ? C22 P1 Cu1 124.5(2) . . ? C41 P1 Cu1 100.6(2) . . ? C34 P2 C28 103.5(3) . . ? C34 P2 C40 104.6(3) . . ? C28 P2 C40 105.8(3) . . ? C34 P2 Cu2 123.7(2) . . ? C28 P2 Cu2 118.1(3) . . ? C40 P2 Cu2 99.0(2) . . ? C2 N1 N2 110.3(5) . . ? C2 N1 B1 129.2(5) . . ? N2 N1 B1 120.5(5) . . ? C4 N2 N1 105.7(5) . . ? C4 N2 W1 132.7(4) . . ? N1 N2 W1 121.4(4) . . ? C7 N3 N4 109.3(5) . . ? C7 N3 B1 129.7(5) . . ? N4 N3 B1 121.0(5) . . ? C9 N4 N3 106.5(5) . . ? C9 N4 W1 131.7(4) . . ? N3 N4 W1 121.7(4) . . ? C12 N5 N6 110.1(5) . . ? C12 N5 B1 128.5(5) . . ? N6 N5 B1 121.4(5) . . ? C14 N6 N5 105.7(5) . . ? C14 N6 W1 133.1(4) . . ? N5 N6 W1 121.1(4) . . ? C40 N7 C41 110.3(5) . . ? C40 N7 C42 112.1(5) . . ? C41 N7 C42 112.1(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.0(6) . . ? N1 C2 C1 123.2(6) . . ? C3 C2 C1 128.8(7) . . ? C2 C3 C4 106.6(6) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? N2 C4 C3 109.4(6) . . ? N2 C4 C5 125.9(6) . . ? C3 C4 C5 124.6(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 107.8(6) . . ? N3 C7 C6 121.9(6) . . ? C8 C7 C6 130.3(6) . . ? C7 C8 C9 107.7(6) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? N4 C9 C8 108.6(6) . . ? N4 C9 C10 125.2(6) . . ? C8 C9 C10 126.1(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 107.4(6) . . ? N5 C12 C11 123.7(6) . . ? C13 C12 C11 128.9(6) . . ? C14 C13 C12 106.7(6) . . ? C14 C13 H13 126.6 . . ? C12 C13 H13 126.6 . . ? N6 C14 C13 110.1(6) . . ? N6 C14 C15 125.2(6) . . ? C13 C14 C15 124.7(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.1(7) . . ? C17 C16 P1 117.2(6) . . ? C21 C16 P1 123.8(5) . . ? C16 C17 C18 120.3(8) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 119.6(9) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 119.2(8) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 121.9(8) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C16 119.9(8) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? C23 C22 C27 119.5(7) . . ? C23 C22 P1 120.3(5) . . ? C27 C22 P1 120.1(5) . . ? C22 C23 C24 119.7(8) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 119.6(8) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 121.0(7) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 119.7(8) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C22 C27 C26 120.6(8) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C33 C28 C29 119.5(7) . . ? C33 C28 P2 120.9(6) . . ? C29 C28 P2 119.5(6) . . ? C28 C29 C30 119.6(9) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C31 C30 C29 119.0(10) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C32 C31 C30 121.2(9) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C33 120.6(10) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 120.1(9) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? C39 C34 C35 119.3(7) . . ? C39 C34 P2 118.9(6) . . ? C35 C34 P2 121.7(5) . . ? C34 C35 C36 119.5(8) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 120.1(9) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 120.6(8) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C39 120.1(8) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C34 C39 C38 120.3(8) . . ? C34 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? N7 C40 P2 108.6(4) . . ? N7 C40 H40A 110.0 . . ? P2 C40 H40A 110.0 . . ? N7 C40 H40B 110.0 . . ? P2 C40 H40B 110.0 . . ? H40A C40 H40B 108.3 . . ? N7 C41 P1 110.6(4) . . ? N7 C41 H41A 109.5 . . ? P1 C41 H41A 109.5 . . ? N7 C41 H41B 109.5 . . ? P1 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? N7 C42 C42 110.9(6) . 3_675 ? N7 C42 H42A 109.5 . . ? C42 C42 H42A 109.5 3_675 . ? N7 C42 H42B 109.5 . . ? C42 C42 H42B 109.5 3_675 . ? H42A C42 H42B 108.0 . . ? C45 O1 C44 118(2) . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O1 C44 C43 110.1(17) . . ? O1 C44 H44A 109.6 . . ? C43 C44 H44A 109.6 . . ? O1 C44 H44B 109.6 . . ? C43 C44 H44B 109.6 . . ? H44A C44 H44B 108.2 . . ? O1 C45 C46 115.4(18) . . ? O1 C45 H45A 108.4 . . ? C46 C45 H45A 108.4 . . ? O1 C45 H45B 108.4 . . ? C46 C45 H45B 108.4 . . ? H45A C45 H45B 107.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N5 B1 N1 108.8(5) . . ? N5 B1 N3 108.7(6) . . ? N1 B1 N3 108.3(5) . . ? N5 B1 H1B1 109(4) . . ? N1 B1 H1B1 108(4) . . ? N3 B1 H1B1 113(4) . . ? F2 P3 F1 94.3(5) . . ? F2 P3 F5 101.3(5) . . ? F1 P3 F5 92.5(5) . . ? F2 P3 F2A 29.1(6) . . ? F1 P3 F2A 99.3(8) . . ? F5 P3 F2A 72.5(8) . . ? F2 P3 F6 88.9(4) . . ? F1 P3 F6 176.0(5) . . ? F5 P3 F6 89.3(4) . . ? F2A P3 F6 84.6(8) . . ? F2 P3 F3A 98.4(8) . . ? F1 P3 F3A 104.6(8) . . ? F5 P3 F3A 152.8(8) . . ? F2A P3 F3A 123.9(11) . . ? F6 P3 F3A 72.5(7) . . ? F2 P3 F5A 77.3(8) . . ? F1 P3 F5A 46.8(7) . . ? F5 P3 F5A 54.7(7) . . ? F2A P3 F5A 63.5(10) . . ? F6 P3 F5A 136.7(8) . . ? F3A P3 F5A 149.5(10) . . ? F2 P3 F3 76.2(5) . . ? F1 P3 F3 87.9(4) . . ? F5 P3 F3 177.5(5) . . ? F2A P3 F3 105.0(8) . . ? F6 P3 F3 90.4(4) . . ? F3A P3 F3 28.9(6) . . ? F5A P3 F3 124.4(7) . . ? F2 P3 F4 173.5(5) . . ? F1 P3 F4 80.7(5) . . ? F5 P3 F4 83.2(5) . . ? F2A P3 F4 155.7(8) . . ? F6 P3 F4 95.9(4) . . ? F3A P3 F4 78.9(8) . . ? F5A P3 F4 101.9(8) . . ? F3 P3 F4 99.3(5) . . ? F2 P3 F4A 152.8(8) . . ? F1 P3 F4A 97.9(8) . . ? F5 P3 F4A 102.4(8) . . ? F2A P3 F4A 162.2(10) . . ? F6 P3 F4A 78.2(8) . . ? F3A P3 F4A 54.9(10) . . ? F5A P3 F4A 128.0(11) . . ? F3 P3 F4A 80.0(8) . . ? F4 P3 F4A 26.4(7) . . ? F2 P3 F1A 88.4(8) . . ? F1 P3 F1A 30.1(7) . . ? F5 P3 F1A 122.6(9) . . ? F2A P3 F1A 107.2(10) . . ? F6 P3 F1A 147.9(8) . . ? F3A P3 F1A 76.3(10) . . ? F5A P3 F1A 73.4(10) . . ? F3 P3 F1A 57.9(8) . . ? F4 P3 F1A 85.2(8) . . ? F4A P3 F1A 90.1(10) . . ? F2 P3 F6A 114.9(9) . . ? F1 P3 F6A 111.9(8) . . ? F5 P3 F6A 25.8(7) . . ? F2A P3 F6A 86.6(10) . . ? F6 P3 F6A 68.8(8) . . ? F3A P3 F6A 127.2(11) . . ? F5A P3 F6A 80.2(10) . . ? F3 P3 F6A 155.4(9) . . ? F4 P3 F6A 71.1(8) . . ? F4A P3 F6A 82.8(10) . . ? F1A P3 F6A 139.8(11) . . ? P3 F2A F5A 58.5(6) . . ? F4A F3A P3 62.8(6) . . ? F3A F4A P3 62.2(6) . . ? P3 F5A F2A 58.0(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.950 _refine_diff_density_min -1.513 _refine_diff_density_rms 0.143 _database_code_depnum_ccdc_archive 'CCDC 973428' ####################################################################### # # 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_7^.^1.25MeCN #============================================================================== # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H96 B2 Cu4 N14 P4 S6 W2, 2(P F6), 1.25(C2 H3 N)' _chemical_formula_sum 'C90.50 H99.75 B2 Cu4 F12 N15.25 P6 S6 W2' _chemical_formula_weight 2650.77 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.9136(7) _cell_length_b 13.6447(8) _cell_length_c 14.9557(9) _cell_angle_alpha 83.530(2) _cell_angle_beta 86.989(2) _cell_angle_gamma 81.579(2) _cell_volume 2588.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9362 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.33 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1318 _exptl_absorpt_coefficient_mu 3.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5531 _exptl_absorpt_correction_T_max 0.9059 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction' _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 'Bruker ApexII' _diffrn_measurement_method 'phi and omega scans' _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 126275 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0230 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9096 _reflns_number_gt 8370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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 residue electron density was assumed to be MeCN, but stable refinement of the solvent molecule could not be achieved. Since the disorder model did not give satisfactory results, the solvent contribution to the scattering factors has been taken into account with PLATON/SQUEEZE. During each unit cell, there were four voids with 1 electron and one void with 27 electrons, which corresponds to approximate 1.25 MeCN molecules. The PF~6~ anion was constrined to be a rigid octahedron, the atoms of it were refined to have rigid bond restrains and similar Uij. ; _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^)+(0.0312P)^2^+2.7472P] 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 9096 _refine_ls_number_parameters 668 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _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 W1 W 0.098112(10) 0.775691(9) 0.696193(8) 0.01843(5) Uani 1 1 d . . . Cu1 Cu -0.01028(3) 0.80429(3) 0.84841(3) 0.02219(9) Uani 1 1 d . . . Cu2 Cu -0.09407(3) 0.72893(3) 0.70487(3) 0.02328(9) Uani 1 1 d . . . S1 S 0.15153(6) 0.73112(6) 0.83687(5) 0.02289(17) Uani 1 1 d . . . S2 S 0.04661(6) 0.63532(6) 0.66087(6) 0.02409(18) Uani 1 1 d . . . S3 S -0.05945(6) 0.88065(6) 0.71556(6) 0.02347(18) Uani 1 1 d . . . P1 P -0.11883(6) 0.80118(6) 0.96709(6) 0.02046(18) Uani 1 1 d . . . P2 P -0.23566(6) 0.65726(6) 0.73360(6) 0.02152(18) Uani 1 1 d . . . B1 B 0.2890(3) 0.8570(3) 0.5535(3) 0.0263(8) Uani 1 1 d . . . HB1 H 0.348(3) 0.883(3) 0.507(2) 0.032 Uiso 1 1 d . . . N1 N 0.2590(2) 0.92826(19) 0.62514(18) 0.0249(6) Uani 1 1 d . . . N2 N 0.1839(2) 0.91015(19) 0.69169(17) 0.0219(6) Uani 1 1 d . . . N3 N 0.3256(2) 0.75164(19) 0.59837(17) 0.0223(6) Uani 1 1 d . . . N4 N 0.2580(2) 0.70317(19) 0.65565(17) 0.0222(6) Uani 1 1 d . . . N5 N 0.1899(2) 0.85378(19) 0.50194(18) 0.0253(6) Uani 1 1 d . . . N6 N 0.0986(2) 0.8335(2) 0.54731(18) 0.0261(6) Uani 1 1 d . . . N7 N -0.1477(2) 0.63330(19) 0.89770(17) 0.0209(6) Uani 1 1 d . . . C1 C 0.3779(3) 1.0539(3) 0.5754(3) 0.0474(11) Uani 1 1 d . . . H1A H 0.4404 1.0062 0.5765 0.071 Uiso 1 1 calc R . . H1B H 0.3927 1.1146 0.5955 0.071 Uiso 1 1 calc R . . H1C H 0.3534 1.0671 0.5151 0.071 Uiso 1 1 calc R . . C2 C 0.2956(3) 1.0132(2) 0.6362(2) 0.0304(8) Uani 1 1 d . . . C3 C 0.2449(3) 1.0506(2) 0.7098(2) 0.0295(8) Uani 1 1 d . . . H3 H 0.2547 1.1089 0.7330 0.035 Uiso 1 1 calc R . . C4 C 0.1762(2) 0.9858(2) 0.7437(2) 0.0239(7) Uani 1 1 d . . . C5 C 0.1067(3) 0.9964(3) 0.8250(2) 0.0308(8) Uani 1 1 d . . . H5A H 0.0349 1.0067 0.8080 0.046 Uiso 1 1 calc R . . H5B H 0.1207 1.0524 0.8536 0.046 Uiso 1 1 calc R . . H5C H 0.1194 0.9370 0.8661 0.046 Uiso 1 1 calc R . . C6 C 0.5068(3) 0.7215(3) 0.5305(3) 0.0372(9) Uani 1 1 d . . . H6A H 0.4845 0.7454 0.4707 0.056 Uiso 1 1 calc R . . H6B H 0.5607 0.6653 0.5279 0.056 Uiso 1 1 calc R . . H6C H 0.5335 0.7735 0.5565 0.056 Uiso 1 1 calc R . . C7 C 0.4160(2) 0.6908(3) 0.5869(2) 0.0255(7) Uani 1 1 d . . . C8 C 0.4071(3) 0.6015(3) 0.6365(2) 0.0279(8) Uani 1 1 d . . . H8 H 0.4576 0.5452 0.6405 0.034 Uiso 1 1 calc R . . C9 C 0.3095(3) 0.6106(2) 0.6792(2) 0.0261(7) Uani 1 1 d . . . C10 C 0.2672(3) 0.5306(3) 0.7406(3) 0.0360(9) Uani 1 1 d . . . H10A H 0.2212 0.5602 0.7857 0.054 Uiso 1 1 calc R . . H10B H 0.3241 0.4871 0.7690 0.054 Uiso 1 1 calc R . . H10C H 0.2293 0.4931 0.7064 0.054 Uiso 1 1 calc R . . C11 C 0.2561(3) 0.9035(3) 0.3463(3) 0.0446(10) Uani 1 1 d . . . H11A H 0.2802 0.9632 0.3601 0.067 Uiso 1 1 calc R . . H11B H 0.2286 0.9141 0.2871 0.067 Uiso 1 1 calc R . . H11C H 0.3135 0.8501 0.3486 0.067 Uiso 1 1 calc R . . C12 C 0.1723(3) 0.8773(2) 0.4135(2) 0.0307(8) Uani 1 1 d . . . C13 C 0.0691(3) 0.8714(3) 0.4016(2) 0.0368(9) Uani 1 1 d . . . H13 H 0.0353 0.8830 0.3472 0.044 Uiso 1 1 calc R . . C14 C 0.0244(3) 0.8450(3) 0.4846(2) 0.0314(8) Uani 1 1 d . . . C15 C -0.0884(3) 0.8335(4) 0.5031(3) 0.0520(12) Uani 1 1 d . . . H15A H -0.0935 0.7690 0.5346 0.078 Uiso 1 1 calc R . . H15B H -0.1234 0.8400 0.4471 0.078 Uiso 1 1 calc R . . H15C H -0.1209 0.8841 0.5392 0.078 Uiso 1 1 calc R . . C16 C -0.2095(3) 0.9141(2) 0.9801(2) 0.0234(7) Uani 1 1 d . . . C17 C -0.1880(3) 1.0032(3) 0.9351(3) 0.0350(9) Uani 1 1 d . . . H17 H -0.1259 1.0054 0.9009 0.042 Uiso 1 1 calc R . . C18 C -0.2579(3) 1.0890(3) 0.9405(3) 0.0462(10) Uani 1 1 d . . . H18 H -0.2431 1.1487 0.9095 0.055 Uiso 1 1 calc R . . C19 C -0.3492(3) 1.0867(3) 0.9915(3) 0.0433(10) Uani 1 1 d . . . H19 H -0.3958 1.1449 0.9957 0.052 Uiso 1 1 calc R . . C20 C -0.3715(3) 0.9988(3) 1.0360(3) 0.0385(9) Uani 1 1 d . . . H20 H -0.4334 0.9975 1.0705 0.046 Uiso 1 1 calc R . . C21 C -0.3028(3) 0.9117(3) 1.0301(2) 0.0319(8) Uani 1 1 d . . . H21 H -0.3191 0.8519 1.0596 0.038 Uiso 1 1 calc R . . C22 C -0.0642(3) 0.7571(2) 1.0768(2) 0.0231(7) Uani 1 1 d . . . C23 C 0.0437(3) 0.7438(3) 1.0845(2) 0.0328(8) Uani 1 1 d . . . H23 H 0.0867 0.7588 1.0346 0.039 Uiso 1 1 calc R . . C24 C 0.0873(3) 0.7082(3) 1.1667(3) 0.0429(10) Uani 1 1 d . . . H24 H 0.1597 0.6998 1.1716 0.052 Uiso 1 1 calc R . . C25 C 0.0248(3) 0.6851(3) 1.2408(3) 0.0422(10) Uani 1 1 d . . . H25 H 0.0547 0.6608 1.2956 0.051 Uiso 1 1 calc R . . C26 C -0.0828(3) 0.6981(3) 1.2338(2) 0.0383(9) Uani 1 1 d . . . H26 H -0.1253 0.6824 1.2839 0.046 Uiso 1 1 calc R . . C27 C -0.1276(3) 0.7345(3) 1.1522(2) 0.0295(8) Uani 1 1 d . . . H27 H -0.2000 0.7438 1.1479 0.035 Uiso 1 1 calc R . . C28 C -0.3594(3) 0.7368(2) 0.7489(2) 0.0259(7) Uani 1 1 d . . . C29 C -0.3612(3) 0.8388(3) 0.7360(3) 0.0414(10) Uani 1 1 d . . . H29 H -0.3005 0.8652 0.7165 0.050 Uiso 1 1 calc R . . C30 C -0.4529(4) 0.9022(3) 0.7520(3) 0.0571(12) Uani 1 1 d . . . H30 H -0.4535 0.9708 0.7434 0.068 Uiso 1 1 calc R . . C31 C -0.5419(3) 0.8637(4) 0.7804(3) 0.0513(12) Uani 1 1 d . . . H31 H -0.6034 0.9063 0.7910 0.062 Uiso 1 1 calc R . . C32 C -0.5413(3) 0.7624(4) 0.7934(3) 0.0472(11) Uani 1 1 d . . . H32 H -0.6025 0.7366 0.8126 0.057 Uiso 1 1 calc R . . C33 C -0.4505(3) 0.6991(3) 0.7782(3) 0.0357(9) Uani 1 1 d . . . H33 H -0.4504 0.6305 0.7877 0.043 Uiso 1 1 calc R . . C34 C -0.2530(2) 0.5624(2) 0.6618(2) 0.0253(7) Uani 1 1 d . . . C35 C -0.3040(3) 0.4817(3) 0.6904(3) 0.0340(8) Uani 1 1 d . . . H35 H -0.3386 0.4781 0.7465 0.041 Uiso 1 1 calc R . . C36 C -0.3039(3) 0.4058(3) 0.6357(3) 0.0427(10) Uani 1 1 d . . . H36 H -0.3391 0.3521 0.6551 0.051 Uiso 1 1 calc R . . C37 C -0.2529(3) 0.4098(3) 0.5546(3) 0.0485(11) Uani 1 1 d . . . H37 H -0.2512 0.3578 0.5192 0.058 Uiso 1 1 calc R . . C38 C -0.2037(4) 0.4901(4) 0.5243(3) 0.0602(13) Uani 1 1 d . . . H38 H -0.1702 0.4931 0.4677 0.072 Uiso 1 1 calc R . . C39 C -0.2036(3) 0.5665(3) 0.5772(3) 0.0454(10) Uani 1 1 d . . . H39 H -0.1703 0.6210 0.5561 0.055 Uiso 1 1 calc R . . C40 C -0.2106(3) 0.5833(2) 0.8427(2) 0.0248(7) Uani 1 1 d . . . H40A H -0.2766 0.5744 0.8744 0.030 Uiso 1 1 calc R . . H40B H -0.1736 0.5179 0.8331 0.030 Uiso 1 1 calc R . . C41 C -0.2075(2) 0.7136(2) 0.9435(2) 0.0227(7) Uani 1 1 d . . . H41A H -0.2390 0.6864 0.9994 0.027 Uiso 1 1 calc R . . H41B H -0.2632 0.7483 0.9059 0.027 Uiso 1 1 calc R . . C42 C -0.0745(2) 0.5648(2) 0.9515(2) 0.0200(7) Uani 1 1 d . . . C43 C -0.0949(3) 0.5337(2) 1.0412(2) 0.0240(7) Uani 1 1 d . . . H43 H -0.1589 0.5561 1.0688 0.029 Uiso 1 1 calc R . . C44 C -0.0206(3) 0.4698(2) 1.0896(2) 0.0239(7) Uani 1 1 d . . . H44 H -0.0341 0.4498 1.1501 0.029 Uiso 1 1 calc R . . P3 P 0.46896(10) 0.26056(9) 0.78045(9) 0.0582(3) Uani 1 1 d DU . . F1 F 0.3910(11) 0.3065(13) 0.8539(9) 0.058(5) Uani 0.264(19) 1 d PDU A 1 F2 F 0.479(4) 0.3658(13) 0.729(3) 0.112(8) Uani 0.264(19) 1 d PDU A 1 F3 F 0.5804(13) 0.262(3) 0.817(2) 0.111(8) Uani 0.264(19) 1 d PDU A 1 F4 F 0.460(4) 0.1466(10) 0.795(2) 0.111(8) Uani 0.264(19) 1 d PDU A 1 F5 F 0.518(2) 0.216(2) 0.6927(12) 0.115(8) Uani 0.264(19) 1 d PDU A 1 F6 F 0.3670(11) 0.270(2) 0.7239(15) 0.109(7) Uani 0.264(19) 1 d PDU A 1 F1A F 0.4332(13) 0.2753(9) 0.8820(6) 0.155(4) Uani 0.736(19) 1 d PDU A 2 F2A F 0.4779(11) 0.3750(4) 0.7637(8) 0.094(3) Uani 0.736(19) 1 d PDU A 2 F3A F 0.5843(6) 0.2434(9) 0.8151(7) 0.090(2) Uani 0.736(19) 1 d PDU A 2 F4A F 0.4618(11) 0.1479(3) 0.8092(8) 0.093(3) Uani 0.736(19) 1 d PDU A 2 F5A F 0.5141(6) 0.2430(8) 0.6841(4) 0.084(2) Uani 0.736(19) 1 d PDU A 2 F6A F 0.3528(4) 0.2759(6) 0.7498(8) 0.135(4) Uani 0.736(19) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01952(7) 0.01712(7) 0.01856(7) -0.00104(5) 0.00063(5) -0.00347(5) Cu1 0.0228(2) 0.0216(2) 0.0216(2) -0.00370(16) 0.00293(16) -0.00174(16) Cu2 0.0212(2) 0.0227(2) 0.0270(2) -0.00405(17) -0.00079(17) -0.00560(16) S1 0.0216(4) 0.0252(4) 0.0210(4) -0.0013(3) -0.0012(3) -0.0011(3) S2 0.0266(4) 0.0211(4) 0.0256(4) -0.0063(3) 0.0024(3) -0.0050(3) S3 0.0220(4) 0.0187(4) 0.0287(4) -0.0006(3) -0.0024(3) -0.0006(3) P1 0.0216(4) 0.0179(4) 0.0215(4) -0.0035(3) 0.0009(3) -0.0011(3) P2 0.0198(4) 0.0220(4) 0.0237(4) -0.0056(3) -0.0016(3) -0.0034(3) B1 0.029(2) 0.023(2) 0.026(2) -0.0001(16) 0.0081(17) -0.0059(17) N1 0.0296(15) 0.0203(14) 0.0260(15) -0.0041(12) 0.0065(12) -0.0085(12) N2 0.0225(14) 0.0226(14) 0.0208(14) -0.0007(11) 0.0024(11) -0.0067(11) N3 0.0208(14) 0.0253(15) 0.0217(14) -0.0056(12) 0.0028(11) -0.0056(12) N4 0.0229(14) 0.0202(14) 0.0229(14) -0.0028(11) 0.0051(11) -0.0025(11) N5 0.0324(16) 0.0208(14) 0.0217(15) -0.0002(11) 0.0047(12) -0.0039(12) N6 0.0328(16) 0.0259(15) 0.0202(14) 0.0007(12) -0.0010(12) -0.0082(13) N7 0.0222(14) 0.0190(14) 0.0216(14) -0.0043(11) -0.0035(11) -0.0003(11) C1 0.056(3) 0.037(2) 0.054(3) -0.0089(19) 0.022(2) -0.027(2) C2 0.0313(19) 0.0227(18) 0.038(2) -0.0009(15) 0.0013(16) -0.0089(15) C3 0.0331(19) 0.0214(17) 0.036(2) -0.0093(15) 0.0007(16) -0.0077(15) C4 0.0245(17) 0.0184(16) 0.0299(18) -0.0054(14) -0.0032(14) -0.0036(14) C5 0.035(2) 0.0264(18) 0.034(2) -0.0124(16) 0.0062(16) -0.0095(15) C6 0.0238(19) 0.049(2) 0.036(2) -0.0002(18) 0.0051(16) -0.0035(17) C7 0.0214(17) 0.0327(19) 0.0237(18) -0.0078(15) 0.0007(14) -0.0046(15) C8 0.0241(18) 0.0281(19) 0.0301(19) -0.0063(15) 0.0001(15) 0.0034(14) C9 0.0270(18) 0.0235(18) 0.0279(18) -0.0055(14) -0.0017(15) -0.0019(14) C10 0.033(2) 0.0247(19) 0.045(2) 0.0064(17) 0.0059(17) 0.0026(16) C11 0.048(2) 0.048(2) 0.029(2) 0.0085(18) 0.0112(18) 0.008(2) C12 0.048(2) 0.0197(17) 0.0214(18) 0.0014(14) 0.0021(16) 0.0023(16) C13 0.053(2) 0.034(2) 0.0211(19) 0.0040(16) -0.0085(17) -0.0026(18) C14 0.042(2) 0.0298(19) 0.0234(19) 0.0061(15) -0.0120(16) -0.0106(16) C15 0.050(3) 0.074(3) 0.035(2) 0.013(2) -0.020(2) -0.026(2) C16 0.0286(18) 0.0185(16) 0.0227(17) -0.0042(13) -0.0023(14) 0.0006(14) C17 0.036(2) 0.029(2) 0.038(2) -0.0018(16) 0.0075(17) -0.0025(16) C18 0.054(3) 0.025(2) 0.054(3) 0.0054(18) 0.005(2) 0.0020(18) C19 0.043(2) 0.028(2) 0.054(3) -0.0047(18) 0.002(2) 0.0119(17) C20 0.0283(19) 0.038(2) 0.047(2) -0.0085(18) 0.0041(17) 0.0044(17) C21 0.0315(19) 0.0266(19) 0.036(2) -0.0022(16) 0.0040(16) -0.0024(15) C22 0.0271(18) 0.0177(16) 0.0254(18) -0.0071(14) -0.0006(14) -0.0031(14) C23 0.0307(19) 0.037(2) 0.031(2) -0.0022(16) -0.0021(16) -0.0069(16) C24 0.031(2) 0.056(3) 0.042(2) -0.001(2) -0.0141(18) -0.0053(19) C25 0.050(2) 0.045(2) 0.033(2) -0.0033(18) -0.0158(19) -0.0044(19) C26 0.051(2) 0.038(2) 0.026(2) -0.0030(16) 0.0005(17) -0.0062(18) C27 0.0322(19) 0.0297(19) 0.0268(19) -0.0060(15) -0.0002(15) -0.0026(15) C28 0.0240(17) 0.0299(19) 0.0237(18) -0.0094(14) -0.0054(14) 0.0030(14) C29 0.034(2) 0.032(2) 0.056(3) -0.0036(19) 0.0014(19) 0.0007(17) C30 0.049(3) 0.038(2) 0.080(3) -0.012(2) -0.002(2) 0.013(2) C31 0.035(2) 0.063(3) 0.051(3) -0.023(2) -0.010(2) 0.024(2) C32 0.0211(19) 0.076(3) 0.046(2) -0.021(2) -0.0023(17) 0.001(2) C33 0.0255(19) 0.042(2) 0.041(2) -0.0119(18) -0.0019(16) -0.0039(16) C34 0.0202(16) 0.0282(18) 0.0288(18) -0.0097(15) -0.0050(14) -0.0017(14) C35 0.0307(19) 0.037(2) 0.037(2) -0.0104(17) 0.0025(16) -0.0100(17) C36 0.042(2) 0.037(2) 0.054(3) -0.016(2) -0.004(2) -0.0157(19) C37 0.055(3) 0.046(3) 0.052(3) -0.028(2) -0.008(2) -0.012(2) C38 0.076(3) 0.072(3) 0.041(3) -0.032(2) 0.016(2) -0.029(3) C39 0.059(3) 0.048(2) 0.036(2) -0.0180(19) 0.012(2) -0.026(2) C40 0.0253(17) 0.0216(17) 0.0283(18) -0.0044(14) -0.0057(14) -0.0032(14) C41 0.0253(17) 0.0200(16) 0.0222(17) -0.0037(13) -0.0023(14) 0.0000(14) C42 0.0231(16) 0.0133(15) 0.0243(17) -0.0023(13) -0.0038(13) -0.0033(13) C43 0.0227(17) 0.0199(16) 0.0283(18) -0.0023(14) 0.0027(14) -0.0002(14) C44 0.0291(18) 0.0220(17) 0.0202(17) -0.0002(13) 0.0010(14) -0.0050(14) P3 0.0578(7) 0.0417(7) 0.0673(8) 0.0057(6) 0.0257(6) 0.0004(6) F1 0.056(8) 0.052(8) 0.064(7) -0.009(6) 0.021(6) -0.011(5) F2 0.073(11) 0.081(9) 0.154(19) 0.057(10) 0.058(13) 0.001(10) F3 0.076(8) 0.111(19) 0.144(17) 0.020(13) -0.011(9) -0.031(11) F4 0.21(2) 0.053(7) 0.085(12) -0.049(7) 0.000(12) -0.050(9) F5 0.093(12) 0.143(15) 0.077(10) -0.013(9) 0.033(8) 0.074(12) F6 0.054(8) 0.158(15) 0.125(12) -0.093(12) 0.001(8) 0.012(9) F1A 0.257(10) 0.097(6) 0.127(5) -0.061(5) 0.141(6) -0.092(7) F2A 0.048(3) 0.040(2) 0.178(9) 0.026(3) 0.038(6) 0.003(2) F3A 0.121(4) 0.067(4) 0.077(4) -0.003(3) -0.055(4) 0.020(3) F4A 0.144(6) 0.040(3) 0.086(5) 0.012(3) 0.029(5) -0.005(3) F5A 0.072(4) 0.144(6) 0.043(3) 0.004(3) 0.003(2) -0.048(5) F6A 0.031(2) 0.074(4) 0.285(10) 0.023(6) 0.036(4) -0.004(2) _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 W1 S1 2.2391(8) . ? W1 N4 2.239(3) . ? W1 S2 2.2423(8) . ? W1 N2 2.271(3) . ? W1 N6 2.277(3) . ? W1 S3 2.3351(8) . ? W1 Cu2 2.6446(4) . ? W1 Cu1 2.6457(4) . ? Cu1 S1 2.1870(9) . ? Cu1 P1 2.2036(9) . ? Cu1 S3 2.2155(9) . ? Cu1 Cu2 2.8114(6) . ? Cu2 S2 2.1792(9) . ? Cu2 P2 2.1979(9) . ? Cu2 S3 2.2055(9) . ? P1 C16 1.816(3) . ? P1 C22 1.824(3) . ? P1 C41 1.844(3) . ? P2 C28 1.815(3) . ? P2 C34 1.817(3) . ? P2 C40 1.838(3) . ? B1 N1 1.524(5) . ? B1 N3 1.535(5) . ? B1 N5 1.537(5) . ? B1 HB1 1.08(4) . ? N1 C2 1.344(4) . ? N1 N2 1.380(4) . ? N2 C4 1.350(4) . ? N3 C7 1.345(4) . ? N3 N4 1.377(4) . ? N4 C9 1.356(4) . ? N5 C12 1.349(4) . ? N5 N6 1.377(4) . ? N6 C14 1.356(4) . ? N7 C42 1.438(4) . ? N7 C41 1.461(4) . ? N7 C40 1.469(4) . ? C1 C2 1.490(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.362(5) . ? C3 C4 1.381(5) . ? C3 H3 0.9300 . ? C4 C5 1.481(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.491(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.369(5) . ? C8 C9 1.379(5) . ? C8 H8 0.9300 . ? C9 C10 1.492(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.492(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.369(5) . ? C13 C14 1.375(5) . ? C13 H13 0.9300 . ? C14 C15 1.496(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.380(5) . ? C16 C21 1.386(5) . ? C17 C18 1.377(5) . ? C17 H17 0.9300 . ? C18 C19 1.372(6) . ? C18 H18 0.9300 . ? C19 C20 1.366(5) . ? C19 H19 0.9300 . ? C20 C21 1.383(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.388(5) . ? C22 C27 1.391(5) . ? C23 C24 1.387(5) . ? C23 H23 0.9300 . ? C24 C25 1.371(6) . ? C24 H24 0.9300 . ? C25 C26 1.383(6) . ? C25 H25 0.9300 . ? C26 C27 1.387(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.380(5) . ? C28 C33 1.383(5) . ? C29 C30 1.387(6) . ? C29 H29 0.9300 . ? C30 C31 1.361(7) . ? C30 H30 0.9300 . ? C31 C32 1.373(6) . ? C31 H31 0.9300 . ? C32 C33 1.376(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.380(5) . ? C34 C39 1.385(5) . ? C35 C36 1.390(5) . ? C35 H35 0.9300 . ? C36 C37 1.348(6) . ? C36 H36 0.9300 . ? C37 C38 1.367(6) . ? C37 H37 0.9300 . ? C38 C39 1.379(6) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.384(4) . ? C42 C44 1.388(4) 2_567 ? C43 C44 1.375(5) . ? C43 H43 0.9300 . ? C44 C42 1.388(4) 2_567 ? C44 H44 0.9300 . ? P3 F5A 1.556(4) . ? P3 F4A 1.564(4) . ? P3 F4 1.566(7) . ? P3 F2 1.568(7) . ? P3 F3 1.568(7) . ? P3 F6A 1.569(5) . ? P3 F1 1.571(7) . ? P3 F5 1.573(7) . ? P3 F2A 1.574(4) . ? P3 F3A 1.579(5) . ? P3 F6 1.584(7) . ? P3 F1A 1.591(5) . ? 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 S1 W1 N4 84.51(7) . . ? S1 W1 S2 102.07(3) . . ? N4 W1 S2 84.13(7) . . ? S1 W1 N2 88.28(7) . . ? N4 W1 N2 81.56(9) . . ? S2 W1 N2 161.45(7) . . ? S1 W1 N6 161.03(7) . . ? N4 W1 N6 81.28(10) . . ? S2 W1 N6 88.95(7) . . ? N2 W1 N6 77.29(9) . . ? S1 W1 S3 103.65(3) . . ? N4 W1 S3 167.22(7) . . ? S2 W1 S3 103.40(3) . . ? N2 W1 S3 88.78(7) . . ? N6 W1 S3 88.46(7) . . ? S1 W1 Cu2 102.92(2) . . ? N4 W1 Cu2 136.31(7) . . ? S2 W1 Cu2 52.18(2) . . ? N2 W1 Cu2 140.75(7) . . ? N6 W1 Cu2 96.03(7) . . ? S3 W1 Cu2 52.13(2) . . ? S1 W1 Cu1 52.39(2) . . ? N4 W1 Cu1 136.88(7) . . ? S2 W1 Cu1 101.87(2) . . ? N2 W1 Cu1 96.65(6) . . ? N6 W1 Cu1 140.71(7) . . ? S3 W1 Cu1 52.37(2) . . ? Cu2 W1 Cu1 64.203(12) . . ? S1 Cu1 P1 128.38(3) . . ? S1 Cu1 S3 109.55(3) . . ? P1 Cu1 S3 121.98(3) . . ? S1 Cu1 W1 54.20(2) . . ? P1 Cu1 W1 167.14(3) . . ? S3 Cu1 W1 56.59(2) . . ? S1 Cu1 Cu2 99.21(3) . . ? P1 Cu1 Cu2 110.51(3) . . ? S3 Cu1 Cu2 50.35(2) . . ? W1 Cu1 Cu2 57.879(12) . . ? S2 Cu2 P2 116.79(3) . . ? S2 Cu2 S3 110.04(3) . . ? P2 Cu2 S3 133.13(3) . . ? S2 Cu2 W1 54.37(2) . . ? P2 Cu2 W1 165.60(3) . . ? S3 Cu2 W1 56.69(2) . . ? S2 Cu2 Cu1 98.52(3) . . ? P2 Cu2 Cu1 117.57(3) . . ? S3 Cu2 Cu1 50.67(2) . . ? W1 Cu2 Cu1 57.918(11) . . ? Cu1 S1 W1 73.41(3) . . ? Cu2 S2 W1 73.46(3) . . ? Cu2 S3 Cu1 78.98(3) . . ? Cu2 S3 W1 71.18(3) . . ? Cu1 S3 W1 71.04(3) . . ? C16 P1 C22 107.47(14) . . ? C16 P1 C41 102.02(15) . . ? C22 P1 C41 107.25(15) . . ? C16 P1 Cu1 116.68(11) . . ? C22 P1 Cu1 117.98(11) . . ? C41 P1 Cu1 103.74(11) . . ? C28 P2 C34 109.52(15) . . ? C28 P2 C40 105.87(15) . . ? C34 P2 C40 102.12(15) . . ? C28 P2 Cu2 117.91(12) . . ? C34 P2 Cu2 115.93(11) . . ? C40 P2 Cu2 103.48(11) . . ? N1 B1 N3 110.0(3) . . ? N1 B1 N5 107.4(3) . . ? N3 B1 N5 108.2(3) . . ? N1 B1 HB1 110.8(19) . . ? N3 B1 HB1 111.2(19) . . ? N5 B1 HB1 109.2(19) . . ? C2 N1 N2 109.6(3) . . ? C2 N1 B1 129.5(3) . . ? N2 N1 B1 120.9(3) . . ? C4 N2 N1 106.2(2) . . ? C4 N2 W1 132.5(2) . . ? N1 N2 W1 121.25(19) . . ? C7 N3 N4 109.9(3) . . ? C7 N3 B1 130.1(3) . . ? N4 N3 B1 119.9(3) . . ? C9 N4 N3 106.2(2) . . ? C9 N4 W1 131.0(2) . . ? N3 N4 W1 122.79(19) . . ? C12 N5 N6 109.7(3) . . ? C12 N5 B1 129.4(3) . . ? N6 N5 B1 120.7(3) . . ? C14 N6 N5 106.4(3) . . ? C14 N6 W1 132.4(2) . . ? N5 N6 W1 120.8(2) . . ? C42 N7 C41 115.9(2) . . ? C42 N7 C40 113.0(2) . . ? C41 N7 C40 114.4(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 107.9(3) . . ? N1 C2 C1 123.1(3) . . ? C3 C2 C1 129.0(3) . . ? C2 C3 C4 107.2(3) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N2 C4 C3 109.1(3) . . ? N2 C4 C5 125.3(3) . . ? C3 C4 C5 125.5(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 107.6(3) . . ? N3 C7 C6 123.4(3) . . ? C8 C7 C6 129.0(3) . . ? C7 C8 C9 107.2(3) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N4 C9 C8 109.1(3) . . ? N4 C9 C10 125.7(3) . . ? C8 C9 C10 125.2(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 107.4(3) . . ? N5 C12 C11 122.6(3) . . ? C13 C12 C11 130.0(3) . . ? C12 C13 C14 107.6(3) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? N6 C14 C13 108.9(3) . . ? N6 C14 C15 125.6(3) . . ? C13 C14 C15 125.5(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.2(3) . . ? C17 C16 P1 119.3(3) . . ? C21 C16 P1 121.4(2) . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.1(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.5(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C16 119.7(3) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? C23 C22 C27 119.3(3) . . ? C23 C22 P1 118.9(3) . . ? C27 C22 P1 121.8(3) . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.6(4) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.8(4) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C27 120.3(4) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 120.0(3) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? C29 C28 C33 118.8(3) . . ? C29 C28 P2 118.7(3) . . ? C33 C28 P2 122.4(3) . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 120.1(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 120.4(4) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C35 C34 C39 118.5(3) . . ? C35 C34 P2 123.3(3) . . ? C39 C34 P2 117.8(3) . . ? C34 C35 C36 120.4(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 120.2(4) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.3(4) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C39 120.4(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 120.2(4) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? N7 C40 P2 110.5(2) . . ? N7 C40 H40A 109.6 . . ? P2 C40 H40A 109.6 . . ? N7 C40 H40B 109.6 . . ? P2 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? N7 C41 P1 109.0(2) . . ? N7 C41 H41A 109.9 . . ? P1 C41 H41A 109.9 . . ? N7 C41 H41B 109.9 . . ? P1 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? C43 C42 C44 119.8(3) . 2_567 ? C43 C42 N7 122.9(3) . . ? C44 C42 N7 117.4(3) 2_567 . ? C44 C43 C42 120.1(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C42 120.2(3) . 2_567 ? C43 C44 H44 119.9 . . ? C42 C44 H44 119.9 2_567 . ? F5A P3 F4A 94.1(7) . . ? F5A P3 F4 86.8(13) . . ? F4A P3 F4 8.2(16) . . ? F5A P3 F2 73.2(14) . . ? F4A P3 F2 166.8(17) . . ? F4 P3 F2 159(2) . . ? F5A P3 F3 92.5(14) . . ? F4A P3 F3 97.7(15) . . ? F4 P3 F3 102(2) . . ? F2 P3 F3 87(2) . . ? F5A P3 F6A 92.7(5) . . ? F4A P3 F6A 89.7(6) . . ? F4 P3 F6A 86.2(18) . . ? F2 P3 F6A 87.3(19) . . ? F3 P3 F6A 170.7(15) . . ? F5A P3 F1 157.1(7) . . ? F4A P3 F1 98.6(8) . . ? F4 P3 F1 104.2(17) . . ? F2 P3 F1 92.3(13) . . ? F3 P3 F1 104.5(15) . . ? F6A P3 F1 68.6(7) . . ? F5A P3 F5 13.7(14) . . ? F4A P3 F5 80.7(13) . . ? F4 P3 F5 73.7(19) . . ? F2 P3 F5 86.8(15) . . ? F3 P3 F5 91.5(18) . . ? F6A P3 F5 95.4(11) . . ? F1 P3 F5 164.0(12) . . ? F5A P3 F2A 91.9(4) . . ? F4A P3 F2A 173.2(7) . . ? F4 P3 F2A 178.6(13) . . ? F2 P3 F2A 19.9(18) . . ? F3 P3 F2A 78.8(16) . . ? F6A P3 F2A 93.3(6) . . ? F1 P3 F2A 76.8(8) . . ? F5 P3 F2A 105.1(13) . . ? F5A P3 F3A 89.2(5) . . ? F4A P3 F3A 89.1(7) . . ? F4 P3 F3A 92.8(18) . . ? F2 P3 F3A 94(2) . . ? F3 P3 F3A 9.5(19) . . ? F6A P3 F3A 177.7(6) . . ? F1 P3 F3A 109.8(8) . . ? F5 P3 F3A 86.2(11) . . ? F2A P3 F3A 87.8(6) . . ? F5A P3 F6 77.0(9) . . ? F4A P3 F6 90.4(13) . . ? F4 P3 F6 85(2) . . ? F2 P3 F6 83(2) . . ? F3 P3 F6 167.3(17) . . ? F6A P3 F6 15.7(10) . . ? F1 P3 F6 83.9(9) . . ? F5 P3 F6 80.1(13) . . ? F2A P3 F6 94.1(13) . . ? F3A P3 F6 166.2(9) . . ? F5A P3 F1A 174.9(7) . . ? F4A P3 F1A 85.0(6) . . ? F4 P3 F1A 92.6(13) . . ? F2 P3 F1A 108.0(14) . . ? F3 P3 F1A 82.6(15) . . ? F6A P3 F1A 92.4(6) . . ? F1 P3 F1A 27.7(7) . . ? F5 P3 F1A 163.7(11) . . ? F2A P3 F1A 88.8(4) . . ? F3A P3 F1A 85.7(7) . . ? F6 P3 F1A 108.0(9) . . ? 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 0.016 0.396 0.549 10 1 ' ' 2 0.500 0.500 0.000 166 27 ' ' 3 0.262 0.274 0.573 11 1 ' ' 4 0.737 0.726 0.427 11 1 ' ' 5 0.983 0.604 0.451 10 1 ' ' _platon_squeeze_details ; The solvent MeCN molecule were squeezed ; _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.651 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.085 #===END _database_code_depnum_ccdc_archive 'CCDC 973429'