# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2105 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H40 N4 P2 S4 Zn' _chemical_formula_weight 1024.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Zn' 'Zn' 0.2839 1.4301 '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' 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 17.5248(7) _cell_length_b 16.7568(7) _cell_length_c 18.3862(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.155(10) _cell_angle_gamma 90.00 _cell_volume 5068.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 75 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 25.02 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.662828 _exptl_absorpt_correction_T_max 0.928069 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 AXS SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32774 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.1448 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 28.28 _reflns_number_total 12030 _reflns_number_gt 4685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0227P)^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 12030 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1477 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 0.738 _refine_ls_restrained_S_all 0.738 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 Zn1 Zn 0.23781(2) 0.40888(2) 0.44227(2) 0.05531(12) Uani 1 1 d . . . S1 S 0.22457(5) 0.50975(4) 0.35062(5) 0.0555(2) Uani 1 1 d . . . S2 S 0.21793(5) 0.49426(5) 0.53317(5) 0.0623(2) Uani 1 1 d . . . S3 S 0.35837(5) 0.33559(5) 0.48328(5) 0.0607(2) Uani 1 1 d . . . S4 S 0.15828(5) 0.29712(5) 0.38824(5) 0.0648(3) Uani 1 1 d . . . P1 P 0.48101(5) 0.80912(4) 0.22042(5) 0.0460(2) Uani 1 1 d . . . P2 P 0.04599(5) -0.06482(5) 0.35735(5) 0.0490(2) Uani 1 1 d . . . N1 N 0.21565(18) 0.72683(16) 0.34697(17) 0.0862(10) Uani 1 1 d . . . N2 N 0.21530(19) 0.71023(16) 0.56011(18) 0.0858(10) Uani 1 1 d . . . N3 N 0.42706(17) 0.14331(16) 0.43638(18) 0.0862(10) Uani 1 1 d . . . N4 N 0.19650(17) 0.10830(16) 0.30817(18) 0.0778(9) Uani 1 1 d . . . C1 C 0.21637(16) 0.58885(17) 0.40903(18) 0.0497(8) Uani 1 1 d . . . C2 C 0.21440(16) 0.58245(16) 0.48229(18) 0.0498(8) Uani 1 1 d . . . C3 C 0.31932(19) 0.24967(16) 0.43243(17) 0.0490(8) Uani 1 1 d . . . C4 C 0.23890(19) 0.23422(16) 0.39262(18) 0.0503(8) Uani 1 1 d . . . C5 C 0.21514(19) 0.6663(2) 0.37502(19) 0.0575(9) Uani 1 1 d . . . C6 C 0.21390(19) 0.6546(2) 0.52489(19) 0.0597(9) Uani 1 1 d . . . C7 C 0.3781(2) 0.18966(19) 0.43296(19) 0.0601(9) Uani 1 1 d . . . C8 C 0.21641(19) 0.16353(19) 0.3465(2) 0.0570(9) Uani 1 1 d . . . C9 C 0.43712(18) 0.87537(15) 0.27185(18) 0.0452(7) Uani 1 1 d . . . C10 C 0.47113(18) 0.88232(17) 0.35170(19) 0.0604(9) Uani 1 1 d . . . H10A H 0.5189 0.8553 0.3783 0.073 Uiso 1 1 calc R . . C11 C 0.4343(2) 0.92930(19) 0.3919(2) 0.0753(10) Uani 1 1 d . . . H11A H 0.4566 0.9333 0.4456 0.090 Uiso 1 1 calc R . . C12 C 0.3637(2) 0.97045(19) 0.3513(2) 0.0752(11) Uani 1 1 d . . . H12A H 0.3390 1.0026 0.3780 0.090 Uiso 1 1 calc R . . C13 C 0.3302(2) 0.96438(19) 0.2728(2) 0.0705(10) Uani 1 1 d . . . H13A H 0.2831 0.9927 0.2464 0.085 Uiso 1 1 calc R . . C14 C 0.36569(18) 0.91632(17) 0.23191(19) 0.0606(9) Uani 1 1 d . . . H14A H 0.3421 0.9115 0.1784 0.073 Uiso 1 1 calc R . . C15 C 0.44492(17) 0.71098(15) 0.22722(16) 0.0452(7) Uani 1 1 d . . . C16 C 0.48559(18) 0.64470(17) 0.21443(17) 0.0604(9) Uani 1 1 d . . . H16A H 0.5324 0.6514 0.2022 0.073 Uiso 1 1 calc R . . C17 C 0.4577(2) 0.56899(18) 0.2196(2) 0.0744(11) Uani 1 1 d . . . H17A H 0.4859 0.5248 0.2116 0.089 Uiso 1 1 calc R . . C18 C 0.3878(2) 0.5589(2) 0.2368(2) 0.0748(11) Uani 1 1 d . . . H18A H 0.3683 0.5078 0.2395 0.090 Uiso 1 1 calc R . . C19 C 0.34682(19) 0.6236(2) 0.24976(18) 0.0640(9) Uani 1 1 d . . . H19A H 0.3000 0.6160 0.2619 0.077 Uiso 1 1 calc R . . C20 C 0.37418(18) 0.70029(17) 0.24505(16) 0.0529(8) Uani 1 1 d . . . H20A H 0.3459 0.7441 0.2536 0.063 Uiso 1 1 calc R . . C21 C 0.45251(15) 0.83967(17) 0.12172(17) 0.0453(7) Uani 1 1 d . . . C22 C 0.43575(16) 0.78321(18) 0.06338(19) 0.0563(8) Uani 1 1 d . . . H22A H 0.4366 0.7292 0.0754 0.068 Uiso 1 1 calc R . . C23 C 0.41774(18) 0.8067(2) -0.0127(2) 0.0697(10) Uani 1 1 d . . . H23A H 0.4069 0.7685 -0.0516 0.084 Uiso 1 1 calc R . . C24 C 0.41582(18) 0.8861(3) -0.0309(2) 0.0754(11) Uani 1 1 d . . . H24A H 0.4036 0.9016 -0.0822 0.091 Uiso 1 1 calc R . . C25 C 0.58946(16) 0.80666(15) 0.26235(17) 0.0455(7) Uani 1 1 d . . . C26 C 0.43189(18) 0.9427(2) 0.0262(2) 0.0681(10) Uani 1 1 d . . . H26A H 0.4300 0.9966 0.0135 0.082 Uiso 1 1 calc R . . C27 C 0.45091(17) 0.91982(18) 0.10248(19) 0.0583(9) Uani 1 1 d . . . H27A H 0.4627 0.9583 0.1412 0.070 Uiso 1 1 calc R . . C28 C 0.6277(2) 0.76679(17) 0.33232(19) 0.0612(9) Uani 1 1 d . . . H28A H 0.5965 0.7412 0.3571 0.073 Uiso 1 1 calc R . . C29 C 0.7110(2) 0.76509(19) 0.36477(19) 0.0698(10) Uani 1 1 d . . . H29A H 0.7360 0.7389 0.4116 0.084 Uiso 1 1 calc R . . C30 C 0.75740(19) 0.80221(19) 0.3279(2) 0.0699(10) Uani 1 1 d . . . H30A H 0.8138 0.8012 0.3499 0.084 Uiso 1 1 calc R . . C31 C 0.7211(2) 0.84076(18) 0.2588(2) 0.0631(9) Uani 1 1 d . . . H31A H 0.7531 0.8652 0.2341 0.076 Uiso 1 1 calc R . . C32 C 0.63789(19) 0.84367(15) 0.22561(17) 0.0508(8) Uani 1 1 d . . . H32A H 0.6138 0.8702 0.1788 0.061 Uiso 1 1 calc R . . C33 C 0.14365(18) -0.04620(19) 0.43094(17) 0.0502(8) Uani 1 1 d . . . C34 C 0.1981(2) -0.10868(19) 0.45480(19) 0.0673(9) Uani 1 1 d . . . H34A H 0.1824 -0.1601 0.4369 0.081 Uiso 1 1 calc R . . C35 C 0.2758(2) -0.0943(2) 0.5053(2) 0.0789(11) Uani 1 1 d . . . H35A H 0.3123 -0.1364 0.5215 0.095 Uiso 1 1 calc R . . C36 C 0.2996(2) -0.0200(3) 0.5314(2) 0.0874(13) Uani 1 1 d . . . H36A H 0.3527 -0.0111 0.5643 0.105 Uiso 1 1 calc R . . C37 C 0.2464(3) 0.0423(2) 0.5101(2) 0.0833(11) Uani 1 1 d . . . H37A H 0.2628 0.0932 0.5295 0.100 Uiso 1 1 calc R . . C38 C 0.1675(2) 0.0296(2) 0.45906(19) 0.0643(9) Uani 1 1 d . . . H38A H 0.1311 0.0719 0.4441 0.077 Uiso 1 1 calc R . . C39 C 0.00902(16) -0.15768(16) 0.38065(18) 0.0480(8) Uani 1 1 d . . . C40 C 0.00698(19) -0.17010(18) 0.45458(19) 0.0668(9) Uani 1 1 d . . . H40A H 0.0242 -0.1299 0.4915 0.080 Uiso 1 1 calc R . . C41 C -0.0203(2) -0.2414(2) 0.4737(2) 0.0786(11) Uani 1 1 d . . . H41A H -0.0222 -0.2489 0.5232 0.094 Uiso 1 1 calc R . . C42 C -0.0446(2) -0.3012(2) 0.4197(2) 0.0791(11) Uani 1 1 d . . . H42A H -0.0624 -0.3496 0.4328 0.095 Uiso 1 1 calc R . . C43 C -0.0427(2) -0.2901(2) 0.3471(2) 0.0813(11) Uani 1 1 d . . . H43A H -0.0586 -0.3311 0.3109 0.098 Uiso 1 1 calc R . . C44 C -0.01719(18) -0.2180(2) 0.32702(19) 0.0669(9) Uani 1 1 d . . . H44A H -0.0178 -0.2102 0.2768 0.080 Uiso 1 1 calc R . . C45 C 0.05606(17) -0.07169(16) 0.26374(17) 0.0471(8) Uani 1 1 d . . . C46 C 0.12400(17) -0.10561(17) 0.25502(18) 0.0612(9) Uani 1 1 d . . . H46A H 0.1665 -0.1231 0.2982 0.073 Uiso 1 1 calc R . . C47 C 0.1288(2) -0.1135(2) 0.1821(2) 0.0737(10) Uani 1 1 d . . . H47A H 0.1741 -0.1373 0.1761 0.088 Uiso 1 1 calc R . . C48 C 0.0672(2) -0.0865(2) 0.1187(2) 0.0717(10) Uani 1 1 d . . . H48A H 0.0716 -0.0908 0.0698 0.086 Uiso 1 1 calc R . . C49 C -0.0008(2) -0.0530(2) 0.1262(2) 0.0763(10) Uani 1 1 d . . . H49A H -0.0429 -0.0352 0.0827 0.092 Uiso 1 1 calc R . . C50 C -0.00663(18) -0.04584(18) 0.1989(2) 0.0652(9) Uani 1 1 d . . . H50A H -0.0530 -0.0235 0.2043 0.078 Uiso 1 1 calc R . . C51 C -0.00856(19) 0.08984(19) 0.32932(17) 0.0621(9) Uani 1 1 d . . . H51A H 0.0366 0.0975 0.3145 0.075 Uiso 1 1 calc R . . C52 C -0.02290(17) 0.01512(16) 0.35394(16) 0.0476(8) Uani 1 1 d . . . C53 C -0.0595(2) 0.15299(19) 0.32628(18) 0.0670(10) Uani 1 1 d . . . H53A H -0.0486 0.2032 0.3106 0.080 Uiso 1 1 calc R . . C54 C -0.1278(2) 0.1407(2) 0.34706(18) 0.0643(9) Uani 1 1 d . . . H54A H -0.1627 0.1830 0.3454 0.077 Uiso 1 1 calc R . . C55 C -0.14395(19) 0.0671(2) 0.36984(17) 0.0614(9) Uani 1 1 d . . . H55A H -0.1903 0.0593 0.3827 0.074 Uiso 1 1 calc R . . C56 C -0.09217(17) 0.00408(18) 0.37396(16) 0.0528(8) Uani 1 1 d . . . H56A H -0.1033 -0.0458 0.3901 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0616(3) 0.0540(2) 0.0548(3) -0.00169(19) 0.0257(2) -0.00212(19) S1 0.0707(6) 0.0543(5) 0.0463(5) -0.0051(4) 0.0263(5) -0.0070(4) S2 0.0779(6) 0.0636(6) 0.0542(6) -0.0016(4) 0.0341(5) -0.0014(5) S3 0.0565(5) 0.0601(5) 0.0618(6) -0.0048(4) 0.0158(5) -0.0042(4) S4 0.0523(6) 0.0612(5) 0.0826(7) -0.0059(5) 0.0256(5) -0.0037(4) P1 0.0505(5) 0.0434(5) 0.0462(5) 0.0018(4) 0.0194(4) -0.0010(4) P2 0.0483(5) 0.0573(5) 0.0436(5) -0.0001(4) 0.0185(4) 0.0055(4) N1 0.122(3) 0.061(2) 0.075(2) 0.0035(18) 0.034(2) 0.0093(19) N2 0.124(3) 0.071(2) 0.080(2) -0.0152(18) 0.057(2) 0.0020(19) N3 0.069(2) 0.068(2) 0.113(3) -0.0089(19) 0.022(2) 0.0094(17) N4 0.082(2) 0.061(2) 0.086(3) -0.0063(17) 0.0239(18) -0.0029(17) C1 0.0467(19) 0.0485(19) 0.055(2) -0.0008(17) 0.0187(16) 0.0005(15) C2 0.0449(19) 0.053(2) 0.056(2) -0.0049(17) 0.0228(17) 0.0019(15) C3 0.053(2) 0.049(2) 0.049(2) 0.0103(15) 0.0232(18) 0.0024(17) C4 0.059(2) 0.0462(19) 0.052(2) 0.0021(16) 0.0271(18) -0.0021(17) C5 0.066(2) 0.054(2) 0.053(2) -0.0025(18) 0.0211(18) 0.0071(19) C6 0.067(2) 0.064(2) 0.060(3) 0.0030(19) 0.037(2) 0.0059(19) C7 0.055(2) 0.056(2) 0.068(3) 0.0005(19) 0.019(2) -0.0088(19) C8 0.058(2) 0.049(2) 0.065(3) 0.0025(19) 0.0219(19) -0.0022(18) C9 0.050(2) 0.0388(17) 0.049(2) -0.0031(15) 0.0210(17) -0.0046(15) C10 0.066(2) 0.058(2) 0.056(2) 0.0012(18) 0.020(2) 0.0043(17) C11 0.100(3) 0.075(3) 0.056(3) -0.011(2) 0.033(2) 0.001(2) C12 0.087(3) 0.064(2) 0.088(3) -0.012(2) 0.048(3) 0.005(2) C13 0.065(2) 0.071(2) 0.078(3) -0.002(2) 0.028(2) 0.0079(19) C14 0.055(2) 0.064(2) 0.064(2) -0.0086(19) 0.0222(19) 0.0037(18) C15 0.050(2) 0.0406(18) 0.047(2) 0.0021(15) 0.0188(16) 0.0012(15) C16 0.067(2) 0.048(2) 0.070(2) 0.0025(18) 0.0289(19) 0.0060(18) C17 0.091(3) 0.041(2) 0.090(3) 0.0030(19) 0.029(2) 0.011(2) C18 0.090(3) 0.049(2) 0.072(3) 0.0092(19) 0.012(2) -0.019(2) C19 0.065(2) 0.065(2) 0.060(2) 0.0056(19) 0.0194(19) -0.016(2) C20 0.059(2) 0.046(2) 0.055(2) 0.0052(16) 0.0208(18) -0.0004(16) C21 0.0427(19) 0.0468(19) 0.047(2) 0.0033(16) 0.0163(16) 0.0006(15) C22 0.054(2) 0.059(2) 0.056(2) 0.0009(19) 0.0186(18) 0.0011(17) C23 0.064(2) 0.092(3) 0.050(3) -0.005(2) 0.0146(19) 0.003(2) C24 0.053(2) 0.120(3) 0.051(3) 0.025(3) 0.016(2) 0.013(2) C25 0.048(2) 0.0468(18) 0.046(2) 0.0033(15) 0.0212(17) 0.0003(15) C26 0.057(2) 0.078(3) 0.072(3) 0.028(2) 0.025(2) 0.0122(19) C27 0.062(2) 0.059(2) 0.056(2) 0.0104(18) 0.0231(18) 0.0031(17) C28 0.053(2) 0.075(2) 0.059(2) 0.0164(19) 0.0233(19) 0.0001(19) C29 0.057(2) 0.089(3) 0.058(2) 0.0206(19) 0.013(2) 0.007(2) C30 0.043(2) 0.086(3) 0.080(3) 0.008(2) 0.020(2) 0.0088(19) C31 0.059(2) 0.066(2) 0.074(3) 0.006(2) 0.035(2) 0.0001(19) C32 0.055(2) 0.0506(19) 0.051(2) 0.0013(16) 0.0234(18) 0.0028(17) C33 0.053(2) 0.058(2) 0.044(2) -0.0012(17) 0.0219(17) 0.0050(18) C34 0.066(3) 0.075(3) 0.057(2) -0.0056(19) 0.018(2) 0.013(2) C35 0.051(3) 0.113(3) 0.065(3) 0.008(2) 0.010(2) 0.019(2) C36 0.060(3) 0.135(4) 0.058(3) 0.011(3) 0.008(2) -0.019(3) C37 0.091(3) 0.094(3) 0.061(3) -0.006(2) 0.020(3) -0.035(3) C38 0.071(3) 0.068(2) 0.053(2) 0.0072(19) 0.019(2) -0.004(2) C39 0.0471(19) 0.0499(19) 0.044(2) -0.0016(16) 0.0113(16) 0.0052(15) C40 0.089(3) 0.062(2) 0.045(2) -0.0028(18) 0.0169(19) -0.0111(19) C41 0.100(3) 0.074(3) 0.053(3) 0.014(2) 0.014(2) -0.012(2) C42 0.081(3) 0.063(3) 0.088(3) 0.009(2) 0.023(2) -0.008(2) C43 0.103(3) 0.062(3) 0.079(3) -0.018(2) 0.032(3) -0.013(2) C44 0.076(3) 0.070(2) 0.059(3) -0.007(2) 0.030(2) -0.005(2) C45 0.0417(19) 0.058(2) 0.043(2) -0.0012(16) 0.0171(16) 0.0035(15) C46 0.052(2) 0.084(2) 0.048(2) -0.0017(18) 0.0177(17) 0.0132(18) C47 0.056(2) 0.103(3) 0.071(3) -0.016(2) 0.034(2) 0.004(2) C48 0.067(3) 0.109(3) 0.048(2) -0.015(2) 0.031(2) -0.021(2) C49 0.061(3) 0.119(3) 0.045(2) 0.005(2) 0.014(2) -0.004(2) C50 0.045(2) 0.097(3) 0.057(3) 0.003(2) 0.022(2) 0.0093(19) C51 0.061(2) 0.070(2) 0.063(2) 0.0111(19) 0.0312(19) 0.008(2) C52 0.051(2) 0.050(2) 0.044(2) 0.0043(15) 0.0196(16) 0.0050(16) C53 0.082(3) 0.058(2) 0.063(2) 0.0128(18) 0.027(2) 0.017(2) C54 0.067(2) 0.072(3) 0.052(2) 0.0025(19) 0.0182(19) 0.028(2) C55 0.056(2) 0.082(3) 0.051(2) -0.0027(19) 0.0237(18) 0.016(2) C56 0.054(2) 0.064(2) 0.044(2) 0.0029(16) 0.0221(17) 0.0006(18) _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 Zn1 S2 2.3158(8) . ? Zn1 S3 2.3329(9) . ? Zn1 S1 2.3410(8) . ? Zn1 S4 2.3414(9) . ? S1 C1 1.743(3) . ? S2 C2 1.739(3) . ? S3 C3 1.725(3) . ? S4 C4 1.742(3) . ? P1 C15 1.782(3) . ? P1 C21 1.783(3) . ? P1 C25 1.788(3) . ? P1 C9 1.794(3) . ? P2 C52 1.790(3) . ? P2 C45 1.793(3) . ? P2 C39 1.793(3) . ? P2 C33 1.806(3) . ? N1 C5 1.139(3) . ? N2 C6 1.130(3) . ? N3 C7 1.143(3) . ? N4 C8 1.143(3) . ? C1 C2 1.363(4) . ? C1 C5 1.438(4) . ? C2 C6 1.442(4) . ? C3 C4 1.370(4) . ? C3 C7 1.437(4) . ? C4 C8 1.431(4) . ? C9 C10 1.386(4) . ? C9 C14 1.394(4) . ? C10 C11 1.383(4) . ? C11 C12 1.388(4) . ? C12 C13 1.361(4) . ? C13 C14 1.387(4) . ? C15 C16 1.383(3) . ? C15 C20 1.399(3) . ? C16 C17 1.375(4) . ? C17 C18 1.376(4) . ? C18 C19 1.365(4) . ? C19 C20 1.385(3) . ? C21 C22 1.384(4) . ? C21 C27 1.387(3) . ? C22 C23 1.380(4) . ? C23 C24 1.370(4) . ? C24 C26 1.371(4) . ? C25 C32 1.399(3) . ? C25 C28 1.399(4) . ? C26 C27 1.379(4) . ? C28 C29 1.374(4) . ? C29 C30 1.373(4) . ? C30 C31 1.371(4) . ? C31 C32 1.374(4) . ? C33 C38 1.380(4) . ? C33 C34 1.382(4) . ? C34 C35 1.380(4) . ? C35 C36 1.349(4) . ? C36 C37 1.364(4) . ? C37 C38 1.395(4) . ? C39 C44 1.376(4) . ? C39 C40 1.388(4) . ? C40 C41 1.377(4) . ? C41 C42 1.372(4) . ? C42 C43 1.360(4) . ? C43 C44 1.381(4) . ? C45 C46 1.378(3) . ? C45 C50 1.383(4) . ? C46 C47 1.378(4) . ? C47 C48 1.364(4) . ? C48 C49 1.368(4) . ? C49 C50 1.379(4) . ? C51 C53 1.373(3) . ? C51 C52 1.384(3) . ? C52 C56 1.397(3) . ? C53 C54 1.391(4) . ? C54 C55 1.364(4) . ? C55 C56 1.377(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 Zn1 S3 115.89(3) . . ? S2 Zn1 S1 94.08(3) . . ? S3 Zn1 S1 117.83(3) . . ? S2 Zn1 S4 125.78(3) . . ? S3 Zn1 S4 93.24(3) . . ? S1 Zn1 S4 112.03(3) . . ? C1 S1 Zn1 96.57(11) . . ? C2 S2 Zn1 97.07(10) . . ? C3 S3 Zn1 96.79(11) . . ? C4 S4 Zn1 96.29(11) . . ? C15 P1 C21 110.77(14) . . ? C15 P1 C25 107.38(13) . . ? C21 P1 C25 109.19(12) . . ? C15 P1 C9 107.89(12) . . ? C21 P1 C9 109.76(14) . . ? C25 P1 C9 111.84(13) . . ? C52 P2 C45 107.62(14) . . ? C52 P2 C39 111.28(13) . . ? C45 P2 C39 109.68(14) . . ? C52 P2 C33 110.52(14) . . ? C45 P2 C33 110.42(13) . . ? C39 P2 C33 107.34(14) . . ? C2 C1 C5 119.9(3) . . ? C2 C1 S1 125.8(2) . . ? C5 C1 S1 114.3(2) . . ? C1 C2 C6 118.5(3) . . ? C1 C2 S2 126.2(2) . . ? C6 C2 S2 115.2(2) . . ? C4 C3 C7 118.3(3) . . ? C4 C3 S3 126.2(2) . . ? C7 C3 S3 115.5(2) . . ? C3 C4 C8 119.7(3) . . ? C3 C4 S4 125.4(2) . . ? C8 C4 S4 114.8(2) . . ? N1 C5 C1 177.9(3) . . ? N2 C6 C2 177.9(4) . . ? N3 C7 C3 177.0(4) . . ? N4 C8 C4 177.9(4) . . ? C10 C9 C14 119.8(3) . . ? C10 C9 P1 120.3(2) . . ? C14 C9 P1 119.8(2) . . ? C11 C10 C9 120.3(3) . . ? C10 C11 C12 119.2(3) . . ? C13 C12 C11 120.9(3) . . ? C12 C13 C14 120.5(3) . . ? C13 C14 C9 119.3(3) . . ? C16 C15 C20 119.2(3) . . ? C16 C15 P1 120.9(2) . . ? C20 C15 P1 120.0(2) . . ? C17 C16 C15 120.8(3) . . ? C16 C17 C18 119.7(3) . . ? C19 C18 C17 120.4(3) . . ? C18 C19 C20 120.8(3) . . ? C19 C20 C15 119.2(3) . . ? C22 C21 C27 119.0(3) . . ? C22 C21 P1 120.2(2) . . ? C27 C21 P1 120.8(2) . . ? C23 C22 C21 120.2(3) . . ? C24 C23 C22 120.2(3) . . ? C23 C24 C26 120.2(3) . . ? C32 C25 C28 118.5(3) . . ? C32 C25 P1 120.9(2) . . ? C28 C25 P1 120.6(2) . . ? C24 C26 C27 120.0(3) . . ? C26 C27 C21 120.4(3) . . ? C29 C28 C25 120.7(3) . . ? C28 C29 C30 119.8(3) . . ? C31 C30 C29 120.4(3) . . ? C30 C31 C32 120.8(3) . . ? C31 C32 C25 119.8(3) . . ? C38 C33 C34 119.4(3) . . ? C38 C33 P2 121.7(3) . . ? C34 C33 P2 118.6(3) . . ? C35 C34 C33 119.6(3) . . ? C36 C35 C34 120.9(4) . . ? C35 C36 C37 120.5(4) . . ? C36 C37 C38 119.8(4) . . ? C33 C38 C37 119.6(3) . . ? C44 C39 C40 118.5(3) . . ? C44 C39 P2 121.7(2) . . ? C40 C39 P2 119.8(2) . . ? C41 C40 C39 120.6(3) . . ? C42 C41 C40 119.8(3) . . ? C43 C42 C41 120.3(3) . . ? C42 C43 C44 120.1(3) . . ? C39 C44 C43 120.6(3) . . ? C46 C45 C50 119.4(3) . . ? C46 C45 P2 120.9(2) . . ? C50 C45 P2 119.7(2) . . ? C45 C46 C47 119.8(3) . . ? C48 C47 C46 120.3(3) . . ? C47 C48 C49 120.6(3) . . ? C48 C49 C50 119.5(3) . . ? C49 C50 C45 120.4(3) . . ? C53 C51 C52 121.4(3) . . ? C51 C52 C56 118.6(3) . . ? C51 C52 P2 119.5(2) . . ? C56 C52 P2 121.9(2) . . ? C51 C53 C54 118.9(3) . . ? C55 C54 C53 120.5(3) . . ? C54 C55 C56 120.5(3) . . ? C55 C56 C52 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.407 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.044 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H40 Cu N4 P2 S4' _chemical_formula_weight 1022.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.148(2) _cell_length_b 15.318(3) _cell_length_c 14.587(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.92(3) _cell_angle_gamma 90.00 _cell_volume 2472.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 20.66 _exptl_crystal_description cubes _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.62 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 4347 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1437 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4347 _reflns_number_gt 2188 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0117P)^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 4347 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1262 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _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 Cu1 Cu 0.0000 0.0000 0.0000 0.05738(19) Uani 1 2 d S . . S1 S 0.10391(8) -0.00051(7) -0.12587(6) 0.0703(3) Uani 1 1 d . . . S2 S 0.13398(9) 0.09877(7) 0.06818(7) 0.0757(3) Uani 1 1 d . . . P1 P 0.50305(7) 0.05611(6) -0.29106(6) 0.0451(2) Uani 1 1 d . . . N1 N 0.0772(3) -0.0950(3) -0.3613(2) 0.0941(12) Uani 1 1 d . . . N2 N 0.1959(3) 0.2216(2) 0.2870(2) 0.0856(11) Uani 1 1 d . . . C1 C 0.0175(3) -0.0715(2) -0.1979(2) 0.0564(9) Uani 1 1 d . . . C2 C 0.0512(3) -0.0853(3) -0.2887(3) 0.0661(11) Uani 1 1 d . . . C3 C 0.0819(3) 0.1127(2) 0.1740(2) 0.0538(9) Uani 1 1 d . . . C4 C 0.1465(3) 0.1728(3) 0.2372(3) 0.0623(10) Uani 1 1 d . . . C5 C 0.4970(3) 0.0945(2) -0.1751(2) 0.0471(8) Uani 1 1 d . . . C6 C 0.4064(3) 0.1497(3) -0.1560(2) 0.0712(11) Uani 1 1 d . . . H6A H 0.3504 0.1700 -0.2036 0.085 Uiso 1 1 calc R . . C7 C 0.3985(4) 0.1752(3) -0.0654(3) 0.0857(13) Uani 1 1 d . . . H7A H 0.3369 0.2124 -0.0523 0.103 Uiso 1 1 calc R . . C8 C 0.4801(4) 0.1460(3) 0.0032(3) 0.0748(12) Uani 1 1 d . . . H8A H 0.4741 0.1631 0.0636 0.090 Uiso 1 1 calc R . . C9 C 0.5709(4) 0.0920(3) -0.0145(3) 0.0725(11) Uani 1 1 d . . . H9A H 0.6282 0.0739 0.0333 0.087 Uiso 1 1 calc R . . C10 C 0.5783(3) 0.0642(2) -0.1033(2) 0.0609(10) Uani 1 1 d . . . H10A H 0.6382 0.0249 -0.1149 0.073 Uiso 1 1 calc R . . C11 C 0.4765(3) -0.0591(2) -0.2925(2) 0.0437(8) Uani 1 1 d . . . C12 C 0.5404(3) -0.1158(2) -0.3421(2) 0.0626(10) Uani 1 1 d . . . H12A H 0.6032 -0.0950 -0.3727 0.075 Uiso 1 1 calc R . . C13 C 0.5111(3) -0.2027(3) -0.3463(3) 0.0764(11) Uani 1 1 d . . . H13A H 0.5541 -0.2407 -0.3799 0.092 Uiso 1 1 calc R . . C14 C 0.4191(3) -0.2340(3) -0.3016(3) 0.0739(11) Uani 1 1 d . . . H14A H 0.3992 -0.2929 -0.3055 0.089 Uiso 1 1 calc R . . C15 C 0.3561(3) -0.1791(3) -0.2510(3) 0.0683(11) Uani 1 1 d . . . H15A H 0.2942 -0.2009 -0.2202 0.082 Uiso 1 1 calc R . . C16 C 0.3843(3) -0.0918(3) -0.2457(2) 0.0595(9) Uani 1 1 d . . . H16A H 0.3419 -0.0545 -0.2109 0.071 Uiso 1 1 calc R . . C17 C 0.3858(3) 0.1085(2) -0.3668(2) 0.0470(8) Uani 1 1 d . . . C18 C 0.2853(3) 0.0631(3) -0.4043(2) 0.0646(10) Uani 1 1 d . . . H18A H 0.2756 0.0049 -0.3885 0.078 Uiso 1 1 calc R . . C19 C 0.1991(3) 0.1037(3) -0.4652(3) 0.0805(12) Uani 1 1 d . . . H19A H 0.1321 0.0724 -0.4914 0.097 Uiso 1 1 calc R . . C20 C 0.2108(4) 0.1893(3) -0.4875(3) 0.0786(13) Uani 1 1 d . . . H20A H 0.1519 0.2163 -0.5286 0.094 Uiso 1 1 calc R . . C21 C 0.3100(4) 0.2360(3) -0.4493(3) 0.0787(12) Uani 1 1 d . . . H21A H 0.3181 0.2946 -0.4639 0.094 Uiso 1 1 calc R . . C22 C 0.3969(3) 0.1953(3) -0.3893(2) 0.0662(10) Uani 1 1 d . . . H22A H 0.4641 0.2266 -0.3636 0.079 Uiso 1 1 calc R . . C23 C 0.6444(3) 0.08068(19) -0.3325(2) 0.0464(8) Uani 1 1 d . . . C24 C 0.6447(3) 0.1025(3) -0.4238(2) 0.0673(10) Uani 1 1 d . . . H24A H 0.5724 0.1033 -0.4629 0.081 Uiso 1 1 calc R . . C25 C 0.7516(4) 0.1232(3) -0.4584(3) 0.0862(13) Uani 1 1 d . . . H25A H 0.7507 0.1381 -0.5203 0.103 Uiso 1 1 calc R . . C26 C 0.8567(4) 0.1218(3) -0.4023(3) 0.0776(12) Uani 1 1 d . . . H26A H 0.9282 0.1364 -0.4256 0.093 Uiso 1 1 calc R . . C27 C 0.8595(3) 0.0994(3) -0.3121(3) 0.0764(12) Uani 1 1 d . . . H27A H 0.9328 0.0975 -0.2742 0.092 Uiso 1 1 calc R . . C28 C 0.7533(3) 0.0793(2) -0.2765(3) 0.0716(12) Uani 1 1 d . . . H28A H 0.7553 0.0647 -0.2144 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0548(4) 0.0644(4) 0.0548(4) 0.0052(4) 0.0141(3) 0.0094(3) S1 0.0610(6) 0.0911(8) 0.0618(6) -0.0087(6) 0.0194(5) -0.0138(6) S2 0.0732(6) 0.0915(8) 0.0677(7) -0.0060(6) 0.0304(5) -0.0155(6) P1 0.0395(5) 0.0518(6) 0.0448(5) 0.0007(5) 0.0083(4) -0.0002(4) N1 0.080(2) 0.135(3) 0.073(2) -0.021(2) 0.032(2) -0.024(2) N2 0.086(3) 0.092(3) 0.079(3) -0.008(2) 0.012(2) -0.018(2) C1 0.052(2) 0.062(3) 0.057(2) 0.0036(19) 0.0140(18) 0.0047(18) C2 0.049(2) 0.081(3) 0.070(3) -0.005(2) 0.014(2) -0.0120(19) C3 0.055(2) 0.053(2) 0.055(2) 0.0033(19) 0.0135(18) 0.0054(18) C4 0.056(2) 0.067(3) 0.067(3) 0.011(2) 0.017(2) 0.003(2) C5 0.0423(18) 0.051(2) 0.048(2) 0.0012(17) 0.0082(16) -0.0037(17) C6 0.073(3) 0.087(3) 0.053(2) -0.008(2) 0.0065(19) 0.021(2) C7 0.096(3) 0.091(4) 0.074(3) -0.014(3) 0.025(3) 0.023(3) C8 0.101(3) 0.072(3) 0.053(2) -0.010(2) 0.016(2) -0.019(3) C9 0.071(3) 0.092(3) 0.053(3) 0.003(2) -0.001(2) -0.016(2) C10 0.057(2) 0.070(3) 0.057(2) -0.003(2) 0.0109(19) 0.0013(19) C11 0.0401(18) 0.049(2) 0.0414(19) 0.0040(17) 0.0035(15) -0.0028(16) C12 0.053(2) 0.056(3) 0.081(3) 0.001(2) 0.0172(19) 0.0017(19) C13 0.074(3) 0.059(3) 0.098(3) -0.011(2) 0.017(2) 0.004(2) C14 0.069(3) 0.057(3) 0.093(3) 0.011(2) -0.004(2) -0.006(2) C15 0.066(2) 0.066(3) 0.073(3) 0.012(2) 0.008(2) -0.019(2) C16 0.060(2) 0.067(3) 0.052(2) 0.0004(19) 0.0078(18) -0.009(2) C17 0.046(2) 0.052(2) 0.045(2) -0.0004(17) 0.0092(16) 0.0077(18) C18 0.047(2) 0.071(3) 0.075(3) 0.013(2) 0.0028(19) 0.003(2) C19 0.051(2) 0.104(4) 0.083(3) 0.002(3) -0.005(2) 0.016(3) C20 0.077(3) 0.100(4) 0.057(3) 0.000(3) 0.003(2) 0.047(3) C21 0.101(3) 0.067(3) 0.069(3) 0.007(2) 0.012(3) 0.034(3) C22 0.069(2) 0.057(3) 0.071(3) -0.001(2) 0.002(2) 0.006(2) C23 0.0416(19) 0.045(2) 0.054(2) -0.0007(17) 0.0137(16) -0.0012(15) C24 0.055(2) 0.091(3) 0.057(2) 0.002(2) 0.0125(18) -0.013(2) C25 0.080(3) 0.112(4) 0.072(3) 0.008(3) 0.033(3) -0.014(3) C26 0.057(3) 0.073(3) 0.111(4) 0.006(3) 0.038(3) -0.004(2) C27 0.043(2) 0.085(3) 0.101(3) 0.006(3) 0.009(2) 0.007(2) C28 0.049(2) 0.096(3) 0.071(3) 0.020(2) 0.012(2) 0.006(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 Cu1 S2 2.2695(11) . ? Cu1 S2 2.2695(11) 3 ? Cu1 S1 2.2860(10) 3 ? Cu1 S1 2.2860(10) . ? S1 C1 1.724(4) . ? S2 C3 1.726(3) . ? P1 C11 1.789(3) . ? P1 C23 1.794(3) . ? P1 C17 1.796(3) . ? P1 C5 1.800(3) . ? N1 C2 1.141(4) . ? N2 C4 1.137(4) . ? C1 C3 1.357(4) 3 ? C1 C2 1.435(5) . ? C3 C1 1.357(4) 3 ? C3 C4 1.434(5) . ? C5 C6 1.371(4) . ? C5 C10 1.380(4) . ? C6 C7 1.391(5) . ? C7 C8 1.345(5) . ? C8 C9 1.356(5) . ? C9 C10 1.374(4) . ? C11 C12 1.382(4) . ? C11 C16 1.394(4) . ? C12 C13 1.370(5) . ? C13 C14 1.367(5) . ? C14 C15 1.366(5) . ? C15 C16 1.374(5) . ? C17 C18 1.375(4) . ? C17 C22 1.378(4) . ? C18 C19 1.376(5) . ? C19 C20 1.361(5) . ? C20 C21 1.377(5) . ? C21 C22 1.374(5) . ? C23 C24 1.374(4) . ? C23 C28 1.379(4) . ? C24 C25 1.385(5) . ? C25 C26 1.346(5) . ? C26 C27 1.357(5) . ? C27 C28 1.384(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 S2 Cu1 S2 180.0 . 3 ? S2 Cu1 S1 90.92(4) . 3 ? S2 Cu1 S1 89.08(4) 3 3 ? S2 Cu1 S1 89.07(4) . . ? S2 Cu1 S1 90.92(4) 3 . ? S1 Cu1 S1 180.000(1) 3 . ? C1 S1 Cu1 101.06(11) . . ? C3 S2 Cu1 101.53(13) . . ? C11 P1 C23 110.71(14) . . ? C11 P1 C17 109.06(15) . . ? C23 P1 C17 107.62(15) . . ? C11 P1 C5 107.96(15) . . ? C23 P1 C5 112.44(15) . . ? C17 P1 C5 109.00(15) . . ? C3 C1 C2 118.8(3) 3 . ? C3 C1 S1 123.4(3) 3 . ? C2 C1 S1 117.8(3) . . ? N1 C2 C1 178.9(5) . . ? C1 C3 C4 119.7(3) 3 . ? C1 C3 S2 123.1(3) 3 . ? C4 C3 S2 117.2(3) . . ? N2 C4 C3 178.6(4) . . ? C6 C5 C10 119.0(3) . . ? C6 C5 P1 120.2(3) . . ? C10 C5 P1 120.6(3) . . ? C5 C6 C7 119.9(4) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 121.0(4) . . ? C8 C9 C10 119.9(4) . . ? C9 C10 C5 120.2(4) . . ? C12 C11 C16 119.2(3) . . ? C12 C11 P1 122.1(2) . . ? C16 C11 P1 118.6(3) . . ? C13 C12 C11 119.9(3) . . ? C14 C13 C12 120.5(4) . . ? C15 C14 C13 120.4(4) . . ? C14 C15 C16 120.0(3) . . ? C15 C16 C11 119.9(3) . . ? C18 C17 C22 119.1(3) . . ? C18 C17 P1 121.1(3) . . ? C22 C17 P1 119.8(3) . . ? C17 C18 C19 120.0(4) . . ? C20 C19 C18 120.7(4) . . ? C19 C20 C21 119.9(4) . . ? C22 C21 C20 119.5(4) . . ? C21 C22 C17 120.9(4) . . ? C24 C23 C28 118.2(3) . . ? C24 C23 P1 118.9(3) . . ? C28 C23 P1 122.9(3) . . ? C23 C24 C25 120.8(4) . . ? C26 C25 C24 119.9(4) . . ? C25 C26 C27 120.6(4) . . ? C26 C27 C28 120.0(4) . . ? C23 C28 C27 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.256 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.044 #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H40 N4 Ni P2 S4' _chemical_formula_weight 1017.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclininc _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.223(2) _cell_length_b 15.164(3) _cell_length_c 14.670(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.90(3) _cell_angle_gamma 90.00 _cell_volume 2483.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 67 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 22.49 _exptl_crystal_description parallelepipeds _exptl_crystal_colour brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 4364 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4364 _reflns_number_gt 2600 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0575P)^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 4364 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 Ni1 Ni 1.0000 1.0000 1.0000 0.05760(19) Uani 1 2 d S . . P1 P 0.50544(6) 0.93676(5) 0.71169(5) 0.0504(2) Uani 1 1 d . . . S1 S 0.86490(8) 1.08739(7) 0.93270(6) 0.0722(3) Uani 1 1 d . . . S2 S 0.90277(7) 1.00634(6) 1.12106(6) 0.0697(3) Uani 1 1 d . . . N1 N 0.7918(3) 1.2039(3) 0.7120(2) 0.0976(11) Uani 1 1 d . . . N2 N 0.9238(3) 0.9219(2) 1.3608(2) 0.0931(11) Uani 1 1 d . . . C1 C 0.9119(3) 1.1009(2) 0.8250(2) 0.0586(8) Uani 1 1 d . . . C2 C 0.8440(3) 1.1571(3) 0.7621(3) 0.0712(10) Uani 1 1 d . . . C3 C 0.9875(3) 0.9396(2) 1.1981(2) 0.0600(8) Uani 1 1 d . . . C4 C 0.9521(3) 0.9291(2) 1.2886(2) 0.0681(9) Uani 1 1 d . . . C7 C 0.4063(4) 0.8114(3) 0.9353(3) 0.0900(12) Uani 1 1 d . . . H7A H 0.3478 0.7714 0.9487 0.108 Uiso 1 1 calc R . . C5 C 0.4989(3) 0.8984(2) 0.8267(2) 0.0536(8) Uani 1 1 d . . . C6 C 0.4157(3) 0.8357(3) 0.8451(2) 0.0745(10) Uani 1 1 d . . . H6A H 0.3664 0.8101 0.7976 0.089 Uiso 1 1 calc R . . C8 C 0.4825(4) 0.8459(3) 1.0040(3) 0.0819(11) Uani 1 1 d . . . H8A H 0.4774 0.8279 1.0641 0.098 Uiso 1 1 calc R . . C9 C 0.5662(4) 0.9066(3) 0.9858(2) 0.0774(11) Uani 1 1 d . . . H9A H 0.6181 0.9296 1.0333 0.093 Uiso 1 1 calc R . . C10 C 0.5743(3) 0.9338(2) 0.8980(2) 0.0631(9) Uani 1 1 d . . . H10A H 0.6305 0.9762 0.8860 0.076 Uiso 1 1 calc R . . C11 C 0.4704(2) 1.0526(2) 0.71006(18) 0.0495(7) Uani 1 1 d . . . C12 C 0.5287(3) 1.1115(2) 0.6591(2) 0.0680(9) Uani 1 1 d . . . H12A H 0.5913 1.0928 0.6269 0.082 Uiso 1 1 calc R . . C13 C 0.4937(3) 1.1984(2) 0.6559(3) 0.0842(11) Uani 1 1 d . . . H13A H 0.5330 1.2381 0.6211 0.101 Uiso 1 1 calc R . . C14 C 0.4023(3) 1.2274(2) 0.7029(3) 0.0764(10) Uani 1 1 d . . . H14A H 0.3792 1.2863 0.6994 0.092 Uiso 1 1 calc R . . C15 C 0.3446(3) 1.1692(2) 0.7555(2) 0.0681(9) Uani 1 1 d . . . H15A H 0.2835 1.1889 0.7887 0.082 Uiso 1 1 calc R . . C16 C 0.3777(3) 1.0823(2) 0.7589(2) 0.0593(8) Uani 1 1 d . . . H16A H 0.3382 1.0428 0.7938 0.071 Uiso 1 1 calc R . . C17 C 0.3953(3) 0.8800(2) 0.6351(2) 0.0553(8) Uani 1 1 d . . . C18 C 0.2915(3) 0.9207(3) 0.6006(2) 0.0713(9) Uani 1 1 d . . . H18A H 0.2743 0.9775 0.6195 0.086 Uiso 1 1 calc R . . C19 C 0.2123(3) 0.8772(3) 0.5377(3) 0.0848(11) Uani 1 1 d . . . H19A H 0.1426 0.9053 0.5130 0.102 Uiso 1 1 calc R . . C20 C 0.2360(4) 0.7936(3) 0.5117(3) 0.0881(13) Uani 1 1 d . . . H20A H 0.1823 0.7647 0.4694 0.106 Uiso 1 1 calc R . . C21 C 0.3382(4) 0.7515(3) 0.5475(3) 0.0861(12) Uani 1 1 d . . . H21A H 0.3529 0.6937 0.5306 0.103 Uiso 1 1 calc R . . C22 C 0.4190(3) 0.7949(2) 0.6084(2) 0.0713(9) Uani 1 1 d . . . H22A H 0.4896 0.7670 0.6315 0.086 Uiso 1 1 calc R . . C23 C 0.6487(3) 0.9169(2) 0.6713(2) 0.0547(8) Uani 1 1 d . . . C24 C 0.7514(3) 0.9063(2) 0.7297(3) 0.0731(10) Uani 1 1 d . . . H24A H 0.7492 0.9098 0.7928 0.088 Uiso 1 1 calc R . . C25 C 0.8592(3) 0.8900(3) 0.6928(3) 0.0857(12) Uani 1 1 d . . . H25A H 0.9295 0.8833 0.7316 0.103 Uiso 1 1 calc R . . C26 C 0.8621(4) 0.8838(3) 0.6005(4) 0.0923(13) Uani 1 1 d . . . H26A H 0.9343 0.8719 0.5771 0.111 Uiso 1 1 calc R . . C27 C 0.7621(4) 0.8945(3) 0.5427(3) 0.0977(13) Uani 1 1 d . . . H27A H 0.7654 0.8906 0.4798 0.117 Uiso 1 1 calc R . . C28 C 0.6540(3) 0.9114(2) 0.5775(2) 0.0779(10) Uani 1 1 d . . . H28A H 0.5848 0.9190 0.5377 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0479(3) 0.0701(4) 0.0568(4) -0.0050(3) 0.0150(2) -0.0067(3) P1 0.0428(4) 0.0621(5) 0.0475(4) 0.0001(4) 0.0100(3) 0.0018(4) S1 0.0559(5) 0.0974(7) 0.0665(6) 0.0024(5) 0.0216(4) 0.0084(5) S2 0.0594(5) 0.0898(7) 0.0629(5) 0.0023(5) 0.0205(4) 0.0090(5) N1 0.089(2) 0.124(3) 0.080(2) 0.006(2) 0.0071(19) 0.019(2) N2 0.084(2) 0.126(3) 0.074(2) 0.007(2) 0.0294(18) 0.010(2) C1 0.0532(18) 0.067(2) 0.0559(19) 0.0004(16) 0.0076(15) -0.0041(16) C2 0.056(2) 0.091(3) 0.067(2) -0.007(2) 0.0126(18) -0.0015(19) C3 0.0513(18) 0.071(2) 0.060(2) -0.0019(17) 0.0165(15) -0.0076(16) C4 0.0562(19) 0.083(2) 0.067(2) 0.005(2) 0.0165(17) 0.0033(17) C7 0.091(3) 0.110(3) 0.071(3) 0.024(2) 0.023(2) -0.012(2) C5 0.0495(16) 0.064(2) 0.0488(18) 0.0002(15) 0.0118(14) 0.0068(15) C6 0.072(2) 0.091(3) 0.061(2) 0.009(2) 0.0099(17) -0.014(2) C8 0.103(3) 0.091(3) 0.053(2) 0.017(2) 0.017(2) 0.022(2) C9 0.092(3) 0.080(3) 0.058(2) -0.006(2) -0.0016(19) 0.023(2) C10 0.069(2) 0.069(2) 0.0520(19) -0.0025(17) 0.0095(16) 0.0023(17) C11 0.0433(15) 0.061(2) 0.0448(16) -0.0013(15) 0.0059(13) -0.0001(14) C12 0.0593(19) 0.071(2) 0.077(2) -0.0039(19) 0.0202(17) 0.0006(18) C13 0.083(3) 0.065(3) 0.108(3) 0.005(2) 0.023(2) -0.003(2) C14 0.071(2) 0.060(2) 0.096(3) -0.007(2) -0.001(2) 0.0062(18) C15 0.062(2) 0.077(2) 0.066(2) -0.0110(19) 0.0082(16) 0.0141(19) C16 0.0563(18) 0.069(2) 0.0545(19) -0.0011(16) 0.0143(15) 0.0016(16) C17 0.0530(18) 0.067(2) 0.0466(17) 0.0013(15) 0.0106(14) -0.0045(16) C18 0.0512(19) 0.090(3) 0.072(2) -0.005(2) 0.0032(16) -0.0045(18) C19 0.059(2) 0.116(4) 0.078(3) 0.002(3) -0.0037(19) -0.017(2) C20 0.096(3) 0.107(4) 0.062(2) 0.005(2) 0.008(2) -0.049(3) C21 0.119(4) 0.074(3) 0.067(2) -0.007(2) 0.016(2) -0.029(3) C22 0.078(2) 0.065(2) 0.070(2) -0.0006(19) 0.0042(19) -0.0050(19) C23 0.0477(16) 0.060(2) 0.0584(19) 0.0001(16) 0.0172(14) 0.0029(14) C24 0.0519(18) 0.088(3) 0.080(3) -0.011(2) 0.0118(17) 0.0002(18) C25 0.0429(19) 0.091(3) 0.124(4) -0.013(3) 0.010(2) 0.0012(18) C26 0.069(3) 0.082(3) 0.135(4) -0.005(3) 0.054(3) 0.004(2) C27 0.091(3) 0.115(3) 0.095(3) 0.008(3) 0.051(3) 0.025(3) C28 0.070(2) 0.099(3) 0.068(2) 0.005(2) 0.0229(18) 0.015(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 Ni1 S1 2.1731(10) 3_777 ? Ni1 S1 2.1731(10) . ? Ni1 S2 2.1799(10) . ? Ni1 S2 2.1800(10) 3_777 ? P1 C5 1.794(3) . ? P1 C23 1.795(3) . ? P1 C11 1.800(3) . ? P1 C17 1.801(3) . ? S1 C1 1.728(3) . ? S2 C3 1.729(3) . ? N1 C2 1.139(4) . ? N2 C4 1.142(4) . ? C1 C3 1.358(4) 3_777 ? C1 C2 1.420(5) . ? C3 C1 1.358(4) 3_777 ? C3 C4 1.433(4) . ? C7 C8 1.357(5) . ? C7 C6 1.389(5) . ? C5 C6 1.378(4) . ? C5 C10 1.384(4) . ? C8 C9 1.361(5) . ? C9 C10 1.364(4) . ? C11 C12 1.373(4) . ? C11 C16 1.397(4) . ? C12 C13 1.373(5) . ? C13 C14 1.366(5) . ? C14 C15 1.377(5) . ? C15 C16 1.368(4) . ? C17 C18 1.370(4) . ? C17 C22 1.383(4) . ? C18 C19 1.382(5) . ? C19 C20 1.358(6) . ? C20 C21 1.370(6) . ? C21 C22 1.373(5) . ? C23 C24 1.373(4) . ? C23 C28 1.386(4) . ? C24 C25 1.397(5) . ? C25 C26 1.360(6) . ? C26 C27 1.345(6) . ? C27 C28 1.388(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 Ni1 S1 180.00(3) 3_777 . ? S1 Ni1 S2 92.35(4) 3_777 . ? S1 Ni1 S2 87.65(4) . . ? S1 Ni1 S2 87.65(4) 3_777 3_777 ? S1 Ni1 S2 92.35(4) . 3_777 ? S2 Ni1 S2 180.00(5) . 3_777 ? C5 P1 C23 112.38(14) . . ? C5 P1 C11 107.41(14) . . ? C23 P1 C11 111.17(14) . . ? C5 P1 C17 109.86(14) . . ? C23 P1 C17 107.12(15) . . ? C11 P1 C17 108.87(14) . . ? C1 S1 Ni1 102.90(12) . . ? C3 S2 Ni1 102.67(10) . . ? C3 C1 C2 120.9(3) 3_777 . ? C3 C1 S1 121.0(3) 3_777 . ? C2 C1 S1 118.1(2) . . ? N1 C2 C1 178.2(4) . . ? C1 C3 C4 119.9(3) 3_777 . ? C1 C3 S2 121.1(2) 3_777 . ? C4 C3 S2 119.0(2) . . ? N2 C4 C3 179.1(4) . . ? C8 C7 C6 120.1(4) . . ? C6 C5 C10 119.6(3) . . ? C6 C5 P1 120.1(3) . . ? C10 C5 P1 120.3(2) . . ? C5 C6 C7 119.3(3) . . ? C7 C8 C9 120.6(4) . . ? C8 C9 C10 120.3(4) . . ? C9 C10 C5 120.0(3) . . ? C12 C11 C16 119.4(3) . . ? C12 C11 P1 121.8(2) . . ? C16 C11 P1 118.7(2) . . ? C13 C12 C11 119.5(3) . . ? C14 C13 C12 121.2(4) . . ? C13 C14 C15 119.8(3) . . ? C16 C15 C14 119.7(3) . . ? C15 C16 C11 120.3(3) . . ? C18 C17 C22 119.8(3) . . ? C18 C17 P1 121.2(3) . . ? C22 C17 P1 118.9(3) . . ? C17 C18 C19 119.7(4) . . ? C20 C19 C18 120.1(4) . . ? C19 C20 C21 120.6(4) . . ? C20 C21 C22 119.8(4) . . ? C21 C22 C17 119.9(4) . . ? C24 C23 C28 119.6(3) . . ? C24 C23 P1 122.4(2) . . ? C28 C23 P1 118.0(2) . . ? C23 C24 C25 118.9(4) . . ? C26 C25 C24 120.5(4) . . ? C27 C26 C25 121.0(3) . . ? C26 C27 C28 119.7(4) . . ? C23 C28 C27 120.3(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.301 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.056 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H20 N4 Ni P S4' _chemical_formula_weight 678.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Ni' 'Ni' 0.3393 1.1124 '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' 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 8.242(2) _cell_length_b 16.083(3) _cell_length_c 24.806(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.24(3) _cell_angle_gamma 90.00 _cell_volume 3172.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description cubes _exptl_crystal_colour black _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5584 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5584 _reflns_number_gt 2714 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0168P)^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 5584 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1142 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 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 Ni1 Ni 0.0000 0.5000 0.5000 0.05023(15) Uani 1 2 d S . . Ni2 Ni -0.5000 1.0000 0.0000 0.06986(18) Uani 1 2 d S . . P1 P -0.23298(9) 0.50991(4) 0.17336(3) 0.0491(2) Uani 1 1 d . . . S1 S 0.07426(10) 0.50615(5) 0.42312(3) 0.0579(2) Uani 1 1 d . . . S2 S 0.00029(10) 0.63315(4) 0.49990(4) 0.0582(2) Uani 1 1 d . . . S3 S -0.50911(11) 0.86663(6) 0.00320(4) 0.0762(3) Uani 1 1 d . . . S4 S -0.43286(11) 0.99898(6) -0.07781(4) 0.0794(3) Uani 1 1 d . . . N1 N 0.1888(4) 0.36577(18) 0.31974(13) 0.0816(9) Uani 1 1 d . . . N2 N -0.0953(4) 0.81279(17) 0.57788(13) 0.0858(9) Uani 1 1 d . . . N3 N -0.4242(4) 0.6791(2) -0.07004(15) 0.1011(11) Uani 1 1 d . . . N4 N -0.3295(4) 0.8535(2) -0.17960(15) 0.1077(12) Uani 1 1 d . . . C1 C 0.0975(3) 0.40310(17) 0.40817(12) 0.0507(7) Uani 1 1 d . . . C2 C 0.1501(4) 0.38299(19) 0.35920(15) 0.0592(8) Uani 1 1 d . . . C3 C -0.0658(3) 0.65725(17) 0.55794(12) 0.0499(7) Uani 1 1 d . . . C4 C -0.0842(4) 0.7438(2) 0.56955(14) 0.0611(8) Uani 1 1 d . . . C5 C -0.4183(4) 0.8949(2) -0.09093(14) 0.0718(10) Uani 1 1 d . . . C7 C -0.4358(4) 0.7493(3) -0.06411(15) 0.0774(11) Uani 1 1 d . . . C8 C -0.3674(4) 0.8716(2) -0.14012(16) 0.0788(11) Uani 1 1 d . . . C9 C -0.3197(4) 0.44937(16) 0.21956(13) 0.0505(7) Uani 1 1 d . . . C10 C -0.4699(4) 0.40680(19) 0.19746(14) 0.0700(9) Uani 1 1 d . . . H10A H -0.5241 0.4112 0.1596 0.084 Uiso 1 1 calc R . . C11 C -0.5379(4) 0.3580(2) 0.23190(17) 0.0814(11) Uani 1 1 d . . . H11A H -0.6376 0.3292 0.2173 0.098 Uiso 1 1 calc R . . C12 C -0.4581(5) 0.3524(2) 0.28725(18) 0.0883(12) Uani 1 1 d . . . H12A H -0.5036 0.3193 0.3103 0.106 Uiso 1 1 calc R . . C13 C -0.3122(5) 0.3948(3) 0.30946(15) 0.0872(12) Uani 1 1 d . . . H13A H -0.2597 0.3904 0.3474 0.105 Uiso 1 1 calc R . . C14 C -0.2421(4) 0.4440(2) 0.27590(14) 0.0669(9) Uani 1 1 d . . . H14A H -0.1435 0.4734 0.2912 0.080 Uiso 1 1 calc R . . C15 C -0.4026(3) 0.56931(16) 0.13105(12) 0.0502(7) Uani 1 1 d . . . C16 C -0.5088(4) 0.6111(2) 0.15705(14) 0.0714(9) Uani 1 1 d . . . H16A H -0.4879 0.6096 0.1957 0.086 Uiso 1 1 calc R . . C17 C -0.6452(4) 0.6549(2) 0.12557(17) 0.0866(12) Uani 1 1 d . . . H17A H -0.7161 0.6829 0.1431 0.104 Uiso 1 1 calc R . . C18 C -0.6759(5) 0.6570(2) 0.06895(17) 0.0906(12) Uani 1 1 d . . . H18A H -0.7678 0.6866 0.0479 0.109 Uiso 1 1 calc R . . C19 C -0.5732(5) 0.6163(2) 0.04297(15) 0.0829(11) Uani 1 1 d . . . H19A H -0.5954 0.6183 0.0043 0.099 Uiso 1 1 calc R . . C20 C -0.4355(4) 0.57158(19) 0.07367(13) 0.0640(8) Uani 1 1 d . . . H20A H -0.3662 0.5435 0.0557 0.077 Uiso 1 1 calc R . . C21 C -0.1410(3) 0.44300(17) 0.13162(12) 0.0495(7) Uani 1 1 d . . . C22 C -0.1648(4) 0.35814(18) 0.13104(13) 0.0630(9) Uani 1 1 d . . . H22A H -0.2337 0.3348 0.1512 0.076 Uiso 1 1 calc R . . C23 C -0.0860(4) 0.3076(2) 0.10037(15) 0.0813(11) Uani 1 1 d . . . H23A H -0.1031 0.2504 0.0996 0.098 Uiso 1 1 calc R . . C24 C 0.0162(4) 0.3418(2) 0.07148(15) 0.0791(11) Uani 1 1 d . . . H24A H 0.0698 0.3077 0.0512 0.095 Uiso 1 1 calc R . . C25 C 0.0412(4) 0.4257(2) 0.07179(15) 0.0829(11) Uani 1 1 d . . . H25A H 0.1114 0.4484 0.0518 0.099 Uiso 1 1 calc R . . C26 C -0.0374(4) 0.47676(19) 0.10166(14) 0.0719(10) Uani 1 1 d . . . H26A H -0.0208 0.5340 0.1017 0.086 Uiso 1 1 calc R . . C27 C -0.0653(3) 0.57406(17) 0.21215(11) 0.0512(7) Uani 1 1 d . . . C28 C 0.0873(4) 0.53682(19) 0.23727(13) 0.0666(9) Uani 1 1 d . . . H28A H 0.1005 0.4799 0.2336 0.080 Uiso 1 1 calc R . . C29 C 0.2186(4) 0.5834(2) 0.26745(15) 0.0812(11) Uani 1 1 d . . . H29A H 0.3206 0.5580 0.2844 0.097 Uiso 1 1 calc R . . C30 C 0.2006(5) 0.6671(2) 0.27277(16) 0.0919(12) Uani 1 1 d . . . H30A H 0.2903 0.6987 0.2932 0.110 Uiso 1 1 calc R . . C31 C 0.0505(5) 0.7043(2) 0.24806(15) 0.0886(12) Uani 1 1 d . . . H31A H 0.0392 0.7614 0.2517 0.106 Uiso 1 1 calc R . . C32 C -0.0843(4) 0.65878(18) 0.21793(13) 0.0673(9) Uani 1 1 d . . . H32A H -0.1864 0.6845 0.2017 0.081 Uiso 1 1 calc R . . C44 C -0.4515(4) 0.8368(2) -0.05557(14) 0.0686(9) 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 Ni1 0.0537(3) 0.0412(3) 0.0557(3) 0.0023(3) 0.0142(2) 0.0018(3) Ni2 0.0569(3) 0.0954(5) 0.0567(4) -0.0013(4) 0.0141(3) 0.0135(4) P1 0.0524(4) 0.0460(4) 0.0496(4) -0.0019(4) 0.0146(3) 0.0016(4) S1 0.0689(5) 0.0474(4) 0.0594(5) 0.0044(4) 0.0205(4) 0.0003(4) S2 0.0694(5) 0.0430(4) 0.0661(5) 0.0033(4) 0.0247(4) 0.0001(4) S3 0.0659(5) 0.0963(7) 0.0677(6) -0.0033(6) 0.0200(4) 0.0059(5) S4 0.0765(6) 0.1036(7) 0.0606(5) 0.0020(6) 0.0223(5) 0.0135(6) N1 0.086(2) 0.082(2) 0.087(2) -0.0058(18) 0.0400(19) -0.0007(16) N2 0.095(2) 0.0566(17) 0.113(3) -0.0118(18) 0.0399(19) 0.0036(16) N3 0.097(2) 0.109(3) 0.100(3) -0.034(2) 0.031(2) -0.008(2) N4 0.112(3) 0.129(3) 0.092(3) -0.026(2) 0.045(2) -0.007(2) C1 0.0426(17) 0.0510(17) 0.055(2) -0.0011(16) 0.0072(15) 0.0011(14) C2 0.055(2) 0.053(2) 0.071(2) -0.0001(18) 0.0185(18) -0.0029(16) C3 0.0432(17) 0.0452(16) 0.059(2) -0.0012(15) 0.0101(15) 0.0020(14) C4 0.060(2) 0.0550(19) 0.071(2) -0.0033(18) 0.0207(17) 0.0011(17) C5 0.052(2) 0.105(3) 0.055(2) -0.014(2) 0.0063(17) 0.005(2) C7 0.051(2) 0.112(3) 0.068(2) -0.021(3) 0.0130(18) -0.005(2) C8 0.064(2) 0.105(3) 0.069(3) -0.011(2) 0.018(2) -0.002(2) C9 0.0550(19) 0.0456(17) 0.055(2) -0.0027(15) 0.0210(16) 0.0008(14) C10 0.074(2) 0.073(2) 0.067(2) -0.0079(19) 0.0256(19) -0.0155(19) C11 0.072(3) 0.076(2) 0.104(3) -0.001(2) 0.036(2) -0.019(2) C12 0.081(3) 0.094(3) 0.103(3) 0.033(3) 0.049(3) 0.015(2) C13 0.072(3) 0.124(3) 0.068(3) 0.031(2) 0.024(2) 0.016(2) C14 0.056(2) 0.081(2) 0.065(2) 0.0087(19) 0.0195(18) 0.0023(17) C15 0.0510(18) 0.0465(16) 0.0517(19) -0.0038(15) 0.0113(15) 0.0002(14) C16 0.074(2) 0.078(2) 0.061(2) -0.0108(19) 0.0138(18) 0.017(2) C17 0.079(3) 0.092(3) 0.086(3) -0.012(2) 0.015(2) 0.033(2) C18 0.087(3) 0.099(3) 0.078(3) 0.008(2) 0.007(2) 0.032(2) C19 0.087(3) 0.099(3) 0.058(2) 0.015(2) 0.011(2) 0.013(2) C20 0.065(2) 0.067(2) 0.060(2) 0.0056(18) 0.0179(17) 0.0100(18) C21 0.0515(18) 0.0422(18) 0.056(2) -0.0052(14) 0.0171(15) 0.0026(14) C22 0.062(2) 0.055(2) 0.076(2) -0.0060(17) 0.0260(18) -0.0037(16) C23 0.095(3) 0.051(2) 0.106(3) -0.024(2) 0.038(2) -0.0022(19) C24 0.082(3) 0.075(3) 0.086(3) -0.019(2) 0.031(2) 0.015(2) C25 0.088(3) 0.083(3) 0.095(3) 0.000(2) 0.055(2) 0.005(2) C26 0.085(2) 0.056(2) 0.088(3) 0.0020(18) 0.045(2) 0.0044(18) C27 0.0547(19) 0.0480(17) 0.0503(18) 0.0006(15) 0.0128(15) -0.0009(15) C28 0.061(2) 0.0534(17) 0.078(2) -0.0022(18) 0.0066(19) 0.0001(17) C29 0.059(2) 0.080(3) 0.093(3) 0.001(2) -0.002(2) -0.004(2) C30 0.089(3) 0.075(3) 0.096(3) -0.014(2) -0.004(2) -0.025(2) C31 0.095(3) 0.055(2) 0.097(3) -0.014(2) -0.008(2) -0.001(2) C32 0.066(2) 0.058(2) 0.069(2) -0.0081(17) 0.0019(18) 0.0034(17) C44 0.0475(19) 0.098(3) 0.059(2) -0.014(2) 0.0112(17) 0.0020(19) _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 Ni1 S2 2.1416(8) . ? Ni1 S2 2.1416(8) 3_566 ? Ni1 S1 2.1529(9) 3_566 ? Ni1 S1 2.1529(9) . ? Ni2 S4 2.1431(10) 3_475 ? Ni2 S4 2.1432(10) . ? Ni2 S3 2.1485(11) . ? Ni2 S3 2.1485(11) 3_475 ? P1 C9 1.790(3) . ? P1 C27 1.789(3) . ? P1 C15 1.788(3) . ? P1 C21 1.794(3) . ? S1 C1 1.720(3) . ? S2 C3 1.712(3) . ? S3 C44 1.716(3) . ? S4 C5 1.715(4) . ? N1 C2 1.141(4) . ? N2 C4 1.136(3) . ? N3 C7 1.145(4) . ? N4 C8 1.142(4) . ? C1 C3 1.354(4) 3_566 ? C1 C2 1.430(4) . ? C3 C1 1.354(4) 3_566 ? C3 C4 1.438(4) . ? C5 C44 1.358(4) . ? C5 C8 1.440(5) . ? C7 C44 1.435(5) . ? C9 C14 1.378(4) . ? C9 C10 1.395(4) . ? C10 C11 1.382(4) . ? C11 C12 1.361(5) . ? C12 C13 1.366(5) . ? C13 C14 1.381(4) . ? C15 C20 1.378(4) . ? C15 C16 1.389(4) . ? C16 C17 1.382(4) . ? C17 C18 1.360(5) . ? C18 C19 1.359(4) . ? C19 C20 1.389(4) . ? C21 C22 1.379(3) . ? C21 C26 1.382(4) . ? C22 C23 1.386(4) . ? C23 C24 1.357(4) . ? C24 C25 1.364(4) . ? C25 C26 1.377(4) . ? C27 C28 1.385(4) . ? C27 C32 1.383(4) . ? C28 C29 1.367(4) . ? C29 C30 1.364(4) . ? C30 C31 1.366(4) . ? C31 C32 1.375(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 S2 Ni1 S2 179.998(1) . 3_566 ? S2 Ni1 S1 92.73(3) . 3_566 ? S2 Ni1 S1 87.27(3) 3_566 3_566 ? S2 Ni1 S1 87.27(3) . . ? S2 Ni1 S1 92.73(3) 3_566 . ? S1 Ni1 S1 180.0 3_566 . ? S4 Ni2 S4 179.999(1) 3_475 . ? S4 Ni2 S3 87.40(4) 3_475 . ? S4 Ni2 S3 92.60(4) . . ? S4 Ni2 S3 92.60(4) 3_475 3_475 ? S4 Ni2 S3 87.40(4) . 3_475 ? S3 Ni2 S3 180.0 . 3_475 ? C9 P1 C27 110.56(14) . . ? C9 P1 C15 106.51(14) . . ? C27 P1 C15 112.44(13) . . ? C9 P1 C21 110.10(13) . . ? C27 P1 C21 105.83(13) . . ? C15 P1 C21 111.45(14) . . ? C1 S1 Ni1 102.73(11) . . ? C3 S2 Ni1 102.98(10) . . ? C44 S3 Ni2 103.16(14) . . ? C5 S4 Ni2 103.05(13) . . ? C3 C1 C2 121.1(3) 3_566 . ? C3 C1 S1 120.4(2) 3_566 . ? C2 C1 S1 118.5(2) . . ? N1 C2 C1 178.4(4) . . ? C1 C3 C4 121.5(3) 3_566 . ? C1 C3 S2 121.1(2) 3_566 . ? C4 C3 S2 117.5(2) . . ? N2 C4 C3 178.0(4) . . ? C44 C5 C8 121.4(3) . . ? C44 C5 S4 120.9(3) . . ? C8 C5 S4 117.7(3) . . ? N3 C7 C44 178.7(5) . . ? N4 C8 C5 178.9(4) . . ? C14 C9 C10 119.7(3) . . ? C14 C9 P1 121.8(2) . . ? C10 C9 P1 118.5(2) . . ? C11 C10 C9 119.9(3) . . ? C12 C11 C10 119.6(3) . . ? C11 C12 C13 121.0(4) . . ? C12 C13 C14 120.4(4) . . ? C9 C14 C13 119.4(3) . . ? C20 C15 C16 119.3(3) . . ? C20 C15 P1 122.1(2) . . ? C16 C15 P1 118.5(2) . . ? C17 C16 C15 120.2(3) . . ? C18 C17 C16 119.9(3) . . ? C17 C18 C19 120.5(4) . . ? C18 C19 C20 120.7(3) . . ? C15 C20 C19 119.4(3) . . ? C22 C21 C26 119.3(3) . . ? C22 C21 P1 121.3(2) . . ? C26 C21 P1 119.3(2) . . ? C21 C22 C23 120.0(3) . . ? C24 C23 C22 119.9(3) . . ? C23 C24 C25 120.7(3) . . ? C24 C25 C26 120.1(3) . . ? C25 C26 C21 120.0(3) . . ? C28 C27 C32 119.5(3) . . ? C28 C27 P1 118.3(2) . . ? C32 C27 P1 122.1(2) . . ? C29 C28 C27 120.3(3) . . ? C30 C29 C28 120.2(3) . . ? C29 C30 C31 119.8(3) . . ? C30 C31 C32 121.2(3) . . ? C31 C32 C27 118.9(3) . . ? C5 C44 C7 122.6(3) . . ? C5 C44 S3 120.2(3) . . ? C7 C44 S3 117.1(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.153 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.047 #===END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H40 Co2 N8 P2 S8' _chemical_formula_weight 1357.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Co' 'Co' 0.3494 0.9721 '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)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.1391(14) _cell_length_b 16.085(3) _cell_length_c 26.993(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.83(3) _cell_angle_gamma 90.00 _cell_volume 3099.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 93 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 24.98 _exptl_crystal_description rhombohedrons _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.848246 _exptl_absorpt_correction_T_max 0.968657 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 AXS SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_reflns_number 15063 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.1154 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 23.99 _reflns_number_total 4864 _reflns_number_gt 2429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0154P)^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 4864 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 0.774 _refine_ls_restrained_S_all 0.774 _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 Co1 Co 0.86981(7) 0.91832(3) 0.50138(2) 0.04712(17) Uani 1 1 d . . . P1 P 0.97428(15) 1.38197(7) 0.33718(4) 0.0504(3) Uani 1 1 d . . . S1 S 0.80209(14) 1.05161(6) 0.49909(4) 0.0510(3) Uani 1 1 d . . . S2 S 0.81937(15) 0.91498(7) 0.58089(4) 0.0570(3) Uani 1 1 d . . . S3 S 0.80349(14) 0.91313(7) 0.42232(4) 0.0539(3) Uani 1 1 d . . . S4 S 0.89698(15) 0.78252(6) 0.50505(4) 0.0554(3) Uani 1 1 d . . . N1 N 0.6249(5) 1.2243(2) 0.57792(16) 0.0854(14) Uani 1 1 d . . . N2 N 0.6108(6) 1.0284(3) 0.68248(16) 0.0912(15) Uani 1 1 d . . . N3 N 0.7824(6) 0.7604(3) 0.31851(16) 0.0864(14) Uani 1 1 d . . . N4 N 0.8435(5) 0.5944(2) 0.42693(16) 0.0829(14) Uani 1 1 d . . . C1 C 0.7257(5) 1.0731(3) 0.55841(16) 0.0482(11) Uani 1 1 d . . . C2 C 0.7315(5) 1.0122(3) 0.59338(17) 0.0477(12) Uani 1 1 d . . . C3 C 0.8248(5) 0.8079(3) 0.40886(18) 0.0497(12) Uani 1 1 d . . . C4 C 0.8621(5) 0.7516(3) 0.44510(16) 0.0464(11) Uani 1 1 d . . . C5 C 0.6685(6) 1.1571(3) 0.56969(17) 0.0587(14) Uani 1 1 d . . . C6 C 0.6640(6) 1.0238(3) 0.6427(2) 0.0611(14) Uani 1 1 d . . . C7 C 0.7999(6) 0.7817(3) 0.3588(2) 0.0613(14) Uani 1 1 d . . . C8 C 0.8559(6) 0.6641(3) 0.43468(16) 0.0544(13) Uani 1 1 d . . . C9 C 1.1155(5) 1.3136(2) 0.30027(17) 0.0462(11) Uani 1 1 d . . . C10 C 1.0903(6) 1.3069(3) 0.25008(18) 0.0604(13) Uani 1 1 d . . . H10A H 1.0014 1.3396 0.2338 0.072 Uiso 1 1 calc R . . C11 C 1.1982(7) 1.2512(3) 0.22375(18) 0.0766(15) Uani 1 1 d . . . H11A H 1.1831 1.2470 0.1896 0.092 Uiso 1 1 calc R . . C12 C 1.3269(7) 1.2022(3) 0.2478(2) 0.0807(17) Uani 1 1 d . . . H12A H 1.3965 1.1641 0.2298 0.097 Uiso 1 1 calc R . . C13 C 1.3550(6) 1.2084(3) 0.2982(2) 0.0742(16) Uani 1 1 d . . . H13A H 1.4431 1.1750 0.3143 0.089 Uiso 1 1 calc R . . C14 C 1.2502(6) 1.2650(3) 0.32438(17) 0.0679(14) Uani 1 1 d . . . H14A H 1.2696 1.2707 0.3583 0.081 Uiso 1 1 calc R . . C15 C 0.8205(5) 1.4423(3) 0.29907(15) 0.0467(11) Uani 1 1 d . . . C16 C 0.6873(6) 1.4009(3) 0.26995(17) 0.0620(13) Uani 1 1 d . . . H16A H 0.6812 1.3432 0.2712 0.074 Uiso 1 1 calc R . . C17 C 0.5656(6) 1.4430(3) 0.23961(18) 0.0719(15) Uani 1 1 d . . . H17A H 0.4774 1.4144 0.2205 0.086 Uiso 1 1 calc R . . C18 C 0.5748(6) 1.5292(3) 0.23758(18) 0.0748(15) Uani 1 1 d . . . H18A H 0.4944 1.5582 0.2164 0.090 Uiso 1 1 calc R . . C19 C 0.7017(7) 1.5718(3) 0.26662(18) 0.0724(14) Uani 1 1 d . . . H19A H 0.7048 1.6296 0.2655 0.087 Uiso 1 1 calc R . . C20 C 0.8252(6) 1.5292(3) 0.29753(16) 0.0605(13) Uani 1 1 d . . . H20A H 0.9109 1.5583 0.3172 0.073 Uiso 1 1 calc R . . C21 C 0.8289(5) 1.3206(3) 0.37613(15) 0.0492(12) Uani 1 1 d . . . C22 C 0.8221(5) 1.2341(3) 0.37258(16) 0.0560(12) Uani 1 1 d . . . H22A H 0.8989 1.2066 0.3504 0.067 Uiso 1 1 calc R . . C23 C 0.7016(7) 1.1891(3) 0.40194(19) 0.0667(14) Uani 1 1 d . . . H23A H 0.6970 1.1315 0.3991 0.080 Uiso 1 1 calc R . . C24 C 0.5885(6) 1.2289(4) 0.43526(19) 0.0714(16) Uani 1 1 d . . . H24A H 0.5097 1.1984 0.4555 0.086 Uiso 1 1 calc R . . C25 C 0.5927(6) 1.3145(3) 0.43846(18) 0.0738(15) Uani 1 1 d . . . H25A H 0.5150 1.3415 0.4607 0.089 Uiso 1 1 calc R . . C26 C 0.7108(6) 1.3608(3) 0.40912(17) 0.0638(13) Uani 1 1 d . . . H26A H 0.7114 1.4185 0.4114 0.077 Uiso 1 1 calc R . . C27 C 1.1292(5) 1.4456(2) 0.37375(18) 0.0478(11) Uani 1 1 d . . . C28 C 1.1337(5) 1.4427(3) 0.42485(18) 0.0579(13) Uani 1 1 d . . . H28A H 1.0565 1.4058 0.4415 0.069 Uiso 1 1 calc R . . C29 C 1.2538(7) 1.4949(3) 0.45145(18) 0.0720(15) Uani 1 1 d . . . H29A H 1.2586 1.4923 0.4859 0.086 Uiso 1 1 calc R . . C30 C 1.3648(6) 1.5499(3) 0.4267(2) 0.0804(17) Uani 1 1 d . . . H30A H 1.4412 1.5863 0.4446 0.097 Uiso 1 1 calc R . . C31 C 1.3650(6) 1.5523(3) 0.3760(2) 0.0786(16) Uani 1 1 d . . . H31A H 1.4439 1.5888 0.3597 0.094 Uiso 1 1 calc R . . C32 C 1.2481(6) 1.5004(3) 0.34915(17) 0.0635(13) Uani 1 1 d . . . H32A H 1.2484 1.5019 0.3147 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0487(3) 0.0385(3) 0.0541(4) -0.0005(3) 0.0009(3) -0.0028(3) P1 0.0521(7) 0.0460(7) 0.0533(9) 0.0013(6) 0.0019(6) -0.0017(6) S1 0.0526(7) 0.0408(7) 0.0594(9) 0.0021(6) -0.0019(6) 0.0009(6) S2 0.0684(7) 0.0461(7) 0.0566(8) -0.0002(7) 0.0059(6) 0.0024(6) S3 0.0599(7) 0.0435(7) 0.0581(8) 0.0017(7) -0.0076(6) -0.0042(6) S4 0.0707(8) 0.0399(7) 0.0555(9) 0.0002(6) 0.0005(6) -0.0027(6) N1 0.079(3) 0.053(3) 0.124(4) -0.018(3) 0.017(3) 0.006(2) N2 0.109(4) 0.085(3) 0.080(4) -0.015(3) 0.029(3) -0.007(3) N3 0.119(3) 0.077(3) 0.063(3) -0.010(3) -0.015(3) 0.007(3) N4 0.089(3) 0.055(3) 0.104(4) -0.015(3) -0.009(3) 0.008(3) C1 0.039(2) 0.038(3) 0.068(4) -0.008(3) 0.007(2) -0.003(2) C2 0.039(3) 0.051(3) 0.053(3) -0.011(3) 0.006(2) -0.005(2) C3 0.040(3) 0.052(3) 0.056(4) -0.016(3) -0.005(2) -0.003(2) C4 0.043(3) 0.040(3) 0.056(3) -0.010(3) 0.003(2) 0.000(2) C5 0.048(3) 0.051(3) 0.077(4) -0.006(3) 0.014(3) -0.008(3) C6 0.054(3) 0.056(3) 0.073(4) -0.011(3) 0.005(3) -0.001(2) C7 0.071(3) 0.052(3) 0.061(4) -0.002(3) -0.008(3) -0.001(3) C8 0.049(3) 0.055(3) 0.059(3) -0.006(3) -0.005(2) 0.002(3) C9 0.046(3) 0.041(3) 0.051(3) -0.001(2) 0.008(3) -0.004(2) C10 0.066(3) 0.061(3) 0.054(4) -0.003(3) 0.005(3) 0.007(3) C11 0.093(4) 0.076(4) 0.061(4) -0.017(3) 0.010(3) 0.004(3) C12 0.071(4) 0.072(4) 0.099(5) -0.019(4) 0.013(4) 0.006(3) C13 0.052(3) 0.066(4) 0.104(5) -0.003(4) -0.004(3) 0.012(3) C14 0.068(3) 0.078(4) 0.057(4) -0.002(3) -0.009(3) 0.007(3) C15 0.051(3) 0.037(3) 0.053(3) 0.003(2) 0.005(2) -0.001(2) C16 0.064(3) 0.046(3) 0.076(4) -0.003(3) -0.009(3) 0.004(3) C17 0.068(3) 0.055(4) 0.091(4) -0.004(3) -0.023(3) 0.000(3) C18 0.073(4) 0.068(4) 0.083(4) 0.012(3) -0.012(3) 0.016(3) C19 0.096(4) 0.047(3) 0.074(4) 0.004(3) -0.006(3) 0.004(3) C20 0.069(3) 0.050(3) 0.062(4) 0.007(3) -0.004(3) -0.001(3) C21 0.049(3) 0.055(3) 0.044(3) 0.004(3) 0.001(2) 0.001(2) C22 0.051(3) 0.057(3) 0.060(4) 0.003(3) -0.005(2) -0.003(3) C23 0.067(3) 0.060(3) 0.073(4) 0.022(3) -0.016(3) -0.020(3) C24 0.047(3) 0.096(5) 0.071(4) 0.026(4) 0.003(3) -0.010(3) C25 0.057(3) 0.094(4) 0.071(4) 0.009(4) 0.010(3) 0.005(3) C26 0.064(3) 0.061(3) 0.066(4) 0.012(3) 0.012(3) 0.003(3) C27 0.046(3) 0.042(3) 0.056(3) 0.001(2) 0.007(3) -0.004(2) C28 0.054(3) 0.059(3) 0.060(4) 0.003(3) -0.001(3) 0.000(2) C29 0.075(4) 0.082(4) 0.059(4) -0.012(3) -0.020(3) 0.001(3) C30 0.063(3) 0.072(4) 0.106(5) -0.015(4) -0.016(4) -0.011(3) C31 0.071(4) 0.079(4) 0.086(5) -0.005(4) 0.004(3) -0.020(3) C32 0.059(3) 0.071(4) 0.060(3) -0.009(3) 0.002(3) -0.010(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 Co1 S3 2.1809(13) . ? Co1 S2 2.1820(13) . ? Co1 S4 2.1949(12) . ? Co1 S1 2.1986(12) . ? Co1 S1 2.3919(12) 3_776 ? P1 C15 1.781(4) . ? P1 C21 1.785(4) . ? P1 C27 1.793(4) . ? P1 C9 1.802(4) . ? S1 C1 1.734(4) . ? S1 Co1 2.3919(12) 3_776 ? S2 C2 1.721(4) . ? S3 C3 1.738(4) . ? S4 C4 1.708(4) . ? N1 C5 1.148(5) . ? N2 C6 1.146(5) . ? N3 C7 1.145(5) . ? N4 C8 1.144(5) . ? C1 C2 1.361(5) . ? C1 C5 1.444(5) . ? C2 C6 1.435(6) . ? C3 C4 1.357(5) . ? C3 C7 1.424(6) . ? C4 C8 1.435(5) . ? C9 C10 1.368(5) . ? C9 C14 1.394(5) . ? C10 C11 1.385(5) . ? C11 C12 1.367(6) . ? C12 C13 1.376(6) . ? C13 C14 1.380(5) . ? C15 C16 1.394(5) . ? C15 C20 1.399(5) . ? C16 C17 1.366(5) . ? C17 C18 1.388(5) . ? C18 C19 1.373(6) . ? C19 C20 1.387(5) . ? C21 C26 1.394(5) . ? C21 C22 1.395(5) . ? C22 C23 1.383(5) . ? C23 C24 1.375(6) . ? C24 C25 1.380(6) . ? C25 C26 1.382(5) . ? C27 C28 1.380(5) . ? C27 C32 1.398(5) . ? C28 C29 1.392(5) . ? C29 C30 1.368(6) . ? C30 C31 1.369(6) . ? C31 C32 1.379(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 S3 Co1 S2 157.66(4) . . ? S3 Co1 S4 91.37(5) . . ? S2 Co1 S4 86.95(5) . . ? S3 Co1 S1 88.01(5) . . ? S2 Co1 S1 90.70(5) . . ? S4 Co1 S1 172.29(5) . . ? S3 Co1 S1 101.61(5) . 3_776 ? S2 Co1 S1 100.71(5) . 3_776 ? S4 Co1 S1 96.64(4) . 3_776 ? S1 Co1 S1 91.01(4) . 3_776 ? C15 P1 C21 106.41(18) . . ? C15 P1 C27 112.2(2) . . ? C21 P1 C27 110.5(2) . . ? C15 P1 C9 111.0(2) . . ? C21 P1 C9 108.8(2) . . ? C27 P1 C9 107.90(19) . . ? C1 S1 Co1 103.94(15) . . ? C1 S1 Co1 106.60(13) . 3_776 ? Co1 S1 Co1 88.99(4) . 3_776 ? C2 S2 Co1 103.66(16) . . ? C3 S3 Co1 102.91(17) . . ? C4 S4 Co1 103.63(15) . . ? C2 C1 C5 122.2(4) . . ? C2 C1 S1 119.3(3) . . ? C5 C1 S1 118.4(3) . . ? C1 C2 C6 122.9(4) . . ? C1 C2 S2 121.7(3) . . ? C6 C2 S2 115.4(3) . . ? C4 C3 C7 120.4(4) . . ? C4 C3 S3 121.1(4) . . ? C7 C3 S3 118.5(4) . . ? C3 C4 C8 120.5(4) . . ? C3 C4 S4 120.8(3) . . ? C8 C4 S4 118.4(3) . . ? N1 C5 C1 178.7(5) . . ? N2 C6 C2 176.2(5) . . ? N3 C7 C3 179.1(5) . . ? N4 C8 C4 177.2(5) . . ? C10 C9 C14 119.9(4) . . ? C10 C9 P1 121.9(4) . . ? C14 C9 P1 118.2(4) . . ? C9 C10 C11 119.5(5) . . ? C12 C11 C10 120.3(5) . . ? C11 C12 C13 121.0(5) . . ? C12 C13 C14 118.8(5) . . ? C13 C14 C9 120.5(5) . . ? C16 C15 C20 118.5(4) . . ? C16 C15 P1 118.4(3) . . ? C20 C15 P1 123.1(4) . . ? C17 C16 C15 121.6(4) . . ? C16 C17 C18 119.3(4) . . ? C19 C18 C17 120.5(5) . . ? C18 C19 C20 120.3(4) . . ? C19 C20 C15 119.8(4) . . ? C26 C21 C22 119.0(4) . . ? C26 C21 P1 118.8(4) . . ? C22 C21 P1 122.0(4) . . ? C23 C22 C21 120.2(4) . . ? C24 C23 C22 120.5(5) . . ? C23 C24 C25 119.5(5) . . ? C24 C25 C26 120.9(5) . . ? C25 C26 C21 119.8(4) . . ? C28 C27 C32 119.4(4) . . ? C28 C27 P1 122.4(3) . . ? C32 C27 P1 118.2(4) . . ? C27 C28 C29 120.0(4) . . ? C30 C29 C28 119.7(5) . . ? C29 C30 C31 120.9(5) . . ? C30 C31 C32 120.0(5) . . ? C31 C32 C27 119.9(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.327 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.052 #===END data_alpha-8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H40 Fe N6 P2 S6' _chemical_formula_weight 1155.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.401(5) _cell_length_b 15.487(4) _cell_length_c 17.965(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5676(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 48.96 _exptl_crystal_description cubes _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 5.077 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5378 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.3064 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 70.06 _reflns_number_total 5378 _reflns_number_gt 1439 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0008P)^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 5378 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2490 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 0.745 _refine_ls_restrained_S_all 0.745 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.006 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 Fe1 Fe 1.0000 1.66983(6) -0.2500 0.0687(3) Uani 1 2 d S . . S1 S 1.05221(5) 1.68187(7) -0.36085(6) 0.0775(4) Uani 1 1 d . . . S2 S 0.94352(6) 1.56433(7) -0.30884(7) 0.0855(4) Uani 1 1 d . . . S3 S 0.92732(5) 1.76754(7) -0.29676(6) 0.0744(3) Uani 1 1 d . . . N1 N 1.1716(2) 1.8163(3) -0.4628(2) 0.1082(15) Uani 1 1 d . . . N2 N 0.7960(2) 1.9196(3) -0.2374(3) 0.1331(18) Uani 1 1 d . . . N3 N 0.9319(3) 1.3294(3) -0.3337(3) 0.175(2) Uani 1 1 d . . . P1 P 0.86426(5) 1.83049(7) -0.59756(6) 0.0641(3) Uani 1 1 d . . . C1 C 1.10658(19) 1.7661(2) -0.3478(3) 0.0645(12) Uani 1 1 d . . . C2 C 1.1431(2) 1.7949(3) -0.4115(3) 0.0759(14) Uani 1 1 d . . . C3 C 0.88303(19) 1.8015(3) -0.2204(2) 0.0632(12) Uani 1 1 d . . . C4 C 0.8340(2) 1.8672(3) -0.2307(3) 0.0850(15) Uani 1 1 d . . . C5 C 0.9770(2) 1.4694(3) -0.2757(2) 0.0842(17) Uani 1 1 d . . . C6 C 0.9517(3) 1.3908(4) -0.3078(3) 0.117(2) Uani 1 1 d . . . C13 C 0.8778(2) 1.7176(3) -0.5832(3) 0.0661(12) Uani 1 1 d . . . C14 C 0.9120(2) 1.6885(3) -0.5224(3) 0.1079(17) Uani 1 1 d . . . H14A H 0.9281 1.7278 -0.4879 0.129 Uiso 1 1 calc R . . C15 C 0.9229(3) 1.6005(4) -0.5119(3) 0.124(2) Uani 1 1 d . . . H15A H 0.9467 1.5814 -0.4710 0.149 Uiso 1 1 calc R . . C16 C 0.8989(3) 1.5436(3) -0.5613(3) 0.1070(19) Uani 1 1 d . . . H16A H 0.9065 1.4849 -0.5546 0.128 Uiso 1 1 calc R . . C17 C 0.8642(3) 1.5709(3) -0.6201(3) 0.1026(17) Uani 1 1 d . . . H17A H 0.8467 1.5308 -0.6531 0.123 Uiso 1 1 calc R . . C18 C 0.8540(2) 1.6587(3) -0.6323(3) 0.0859(14) Uani 1 1 d . . . H18A H 0.8310 1.6770 -0.6741 0.103 Uiso 1 1 calc R . . C19 C 0.81683(19) 1.8733(3) -0.5224(2) 0.0615(11) Uani 1 1 d . . . C20 C 0.7846(3) 1.8219(3) -0.4724(3) 0.1070(17) Uani 1 1 d . . . H20A H 0.7902 1.7623 -0.4737 0.128 Uiso 1 1 calc R . . C21 C 0.7442(3) 1.8585(4) -0.4205(3) 0.133(2) Uani 1 1 d . . . H21A H 0.7223 1.8231 -0.3869 0.159 Uiso 1 1 calc R . . C22 C 0.7353(3) 1.9450(4) -0.4169(3) 0.1028(18) Uani 1 1 d . . . H22A H 0.7080 1.9689 -0.3809 0.123 Uiso 1 1 calc R . . C23 C 0.7671(3) 1.9967(3) -0.4669(3) 0.0965(16) Uani 1 1 d . . . H23A H 0.7611 2.0562 -0.4653 0.116 Uiso 1 1 calc R . . C24 C 0.8071(2) 1.9616(3) -0.5189(3) 0.0818(14) Uani 1 1 d . . . H24A H 0.8284 1.9974 -0.5527 0.098 Uiso 1 1 calc R . . C25 C 0.9396(2) 1.8898(3) -0.6060(2) 0.0619(11) Uani 1 1 d . . . C26 C 0.9390(2) 1.9658(3) -0.6450(3) 0.1100(18) Uani 1 1 d . . . H26A H 0.9013 1.9828 -0.6702 0.132 Uiso 1 1 calc R . . C27 C 0.9944(3) 2.0172(3) -0.6468(3) 0.1155(19) Uani 1 1 d . . . H27A H 0.9933 2.0691 -0.6728 0.139 Uiso 1 1 calc R . . C28 C 1.0494(2) 1.9939(4) -0.6121(3) 0.0948(15) Uani 1 1 d . . . H28A H 1.0866 2.0286 -0.6142 0.114 Uiso 1 1 calc R . . C29 C 1.0500(3) 1.9192(4) -0.5740(3) 0.122(2) Uani 1 1 d . . . H29A H 1.0879 1.9027 -0.5491 0.147 Uiso 1 1 calc R . . C30 C 0.9949(3) 1.8660(3) -0.5710(3) 0.1095(17) Uani 1 1 d . . . H30A H 0.9965 1.8142 -0.5449 0.131 Uiso 1 1 calc R . . C31 C 0.8181(2) 1.8440(2) -0.6816(2) 0.0589(11) Uani 1 1 d . . . C32 C 0.7520(2) 1.8631(2) -0.6783(3) 0.0660(12) Uani 1 1 d . . . H32A H 0.7316 1.8720 -0.6327 0.079 Uiso 1 1 calc R . . C33 C 0.7169(2) 1.8687(3) -0.7430(3) 0.0790(14) Uani 1 1 d . . . H33A H 0.6725 1.8824 -0.7412 0.095 Uiso 1 1 calc R . . C34 C 0.7455(3) 1.8546(3) -0.8090(3) 0.0857(16) Uani 1 1 d . . . H34A H 0.7207 1.8581 -0.8523 0.103 Uiso 1 1 calc R . . C35 C 0.8114(3) 1.8349(3) -0.8137(3) 0.0927(16) Uani 1 1 d . . . H35A H 0.8310 1.8249 -0.8596 0.111 Uiso 1 1 calc R . . C36 C 0.8477(2) 1.8303(3) -0.7491(3) 0.0795(13) Uani 1 1 d . . . H36A H 0.8922 1.8179 -0.7513 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0637(6) 0.0596(6) 0.0829(7) 0.000 0.0129(5) 0.000 S1 0.0763(7) 0.0743(8) 0.0819(8) -0.0109(7) 0.0127(7) -0.0150(7) S2 0.0765(8) 0.0704(8) 0.1097(10) -0.0056(7) 0.0167(7) -0.0151(7) S3 0.0797(8) 0.0640(7) 0.0795(8) 0.0080(6) 0.0055(7) -0.0017(7) N1 0.117(4) 0.094(3) 0.114(4) 0.023(3) 0.024(3) -0.007(3) N2 0.153(4) 0.100(4) 0.146(4) -0.012(3) -0.030(3) 0.062(3) N3 0.200(5) 0.085(4) 0.240(6) -0.038(4) 0.026(4) -0.049(4) P1 0.0700(8) 0.0529(7) 0.0695(8) -0.0002(7) -0.0064(7) -0.0034(7) C1 0.066(3) 0.051(3) 0.077(3) 0.006(3) 0.003(3) 0.000(2) C2 0.079(4) 0.057(3) 0.092(4) 0.008(3) -0.004(3) -0.002(3) C3 0.060(3) 0.051(3) 0.079(3) -0.005(2) 0.000(3) -0.006(2) C4 0.094(4) 0.059(3) 0.102(4) -0.009(3) -0.010(3) 0.010(3) C5 0.080(4) 0.063(3) 0.109(5) -0.003(3) 0.037(3) -0.010(2) C6 0.113(5) 0.077(4) 0.160(6) -0.021(4) 0.053(4) -0.026(4) C13 0.073(3) 0.058(3) 0.067(3) 0.005(3) -0.012(3) -0.003(2) C14 0.153(5) 0.062(3) 0.109(4) 0.004(3) -0.041(4) 0.001(3) C15 0.167(6) 0.080(4) 0.125(5) 0.021(4) -0.041(4) 0.014(4) C16 0.146(5) 0.055(3) 0.120(5) 0.022(4) 0.009(4) 0.011(3) C17 0.141(5) 0.062(4) 0.105(5) -0.012(3) 0.003(4) -0.014(4) C18 0.108(4) 0.058(3) 0.092(4) 0.006(3) -0.003(3) -0.008(3) C19 0.072(3) 0.052(3) 0.060(3) -0.004(2) -0.002(3) -0.002(2) C20 0.158(5) 0.066(3) 0.098(4) 0.009(3) 0.043(4) -0.001(4) C21 0.202(6) 0.087(5) 0.109(5) 0.007(4) 0.072(5) -0.005(4) C22 0.132(5) 0.081(4) 0.095(4) -0.019(4) 0.039(4) -0.004(4) C23 0.130(4) 0.062(3) 0.098(4) -0.006(3) 0.031(4) -0.015(3) C24 0.100(4) 0.065(3) 0.080(4) -0.006(3) 0.022(3) -0.015(3) C25 0.061(3) 0.060(3) 0.065(3) 0.001(2) -0.009(2) -0.002(2) C26 0.072(4) 0.099(4) 0.159(5) 0.045(4) -0.031(4) -0.021(3) C27 0.092(4) 0.099(4) 0.155(5) 0.049(4) -0.027(4) -0.018(4) C28 0.062(3) 0.099(4) 0.123(5) 0.006(3) -0.001(3) -0.009(4) C29 0.081(4) 0.137(5) 0.149(5) 0.048(4) -0.038(4) -0.010(4) C30 0.080(4) 0.102(4) 0.147(5) 0.046(4) -0.036(4) -0.018(4) C31 0.069(3) 0.044(3) 0.063(3) -0.004(2) -0.003(3) -0.007(2) C32 0.068(3) 0.058(3) 0.072(3) -0.004(2) -0.006(3) -0.006(3) C33 0.072(3) 0.066(3) 0.099(4) 0.011(3) -0.013(4) -0.018(3) C34 0.111(5) 0.061(3) 0.085(4) 0.021(3) -0.035(4) -0.016(3) C35 0.124(5) 0.092(4) 0.063(4) -0.002(3) -0.005(4) -0.006(4) C36 0.076(3) 0.094(3) 0.068(3) 0.004(4) -0.006(4) 0.002(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 Fe1 S2 2.2615(13) . ? Fe1 S2 2.2615(14) 3_754 ? Fe1 S1 2.2659(12) 3_754 ? Fe1 S1 2.2660(12) . ? Fe1 S3 2.2790(13) . ? Fe1 S3 2.2791(12) 3_754 ? S1 C1 1.729(4) . ? S2 C5 1.727(4) . ? S3 C3 1.724(4) . ? N1 C2 1.139(5) . ? N2 C4 1.128(5) . ? N3 C6 1.134(5) . ? P1 C19 1.789(4) . ? P1 C13 1.789(4) . ? P1 C25 1.796(4) . ? P1 C31 1.792(4) . ? C1 C3 1.358(5) 3_754 ? C1 C2 1.437(6) . ? C3 C1 1.358(5) 3_754 ? C3 C4 1.440(6) . ? C5 C5 1.318(8) 3_754 ? C5 C6 1.442(6) . ? C13 C18 1.359(5) . ? C13 C14 1.372(5) . ? C14 C15 1.393(5) . ? C15 C16 1.342(6) . ? C16 C17 1.341(6) . ? C17 C18 1.392(5) . ? C19 C20 1.368(5) . ? C19 C24 1.384(5) . ? C20 C21 1.368(6) . ? C21 C22 1.353(6) . ? C22 C23 1.368(5) . ? C23 C24 1.353(5) . ? C25 C30 1.344(5) . ? C25 C26 1.370(5) . ? C26 C27 1.383(6) . ? C27 C28 1.334(6) . ? C28 C29 1.344(6) . ? C29 C30 1.395(6) . ? C31 C36 1.370(5) . ? C31 C32 1.383(5) . ? C32 C33 1.367(5) . ? C33 C34 1.339(5) . ? C34 C35 1.382(6) . ? C35 C36 1.377(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 S2 Fe1 S2 87.49(7) . 3_754 ? S2 Fe1 S1 103.34(5) . 3_754 ? S2 Fe1 S1 83.59(4) 3_754 3_754 ? S2 Fe1 S1 83.58(4) . . ? S2 Fe1 S1 103.34(5) 3_754 . ? S1 Fe1 S1 170.56(7) 3_754 . ? S2 Fe1 S3 88.62(4) . . ? S2 Fe1 S3 169.57(4) 3_754 . ? S1 Fe1 S3 87.90(4) 3_754 . ? S1 Fe1 S3 85.83(4) . . ? S2 Fe1 S3 169.56(4) . 3_754 ? S2 Fe1 S3 88.62(4) 3_754 3_754 ? S1 Fe1 S3 85.83(4) 3_754 3_754 ? S1 Fe1 S3 87.90(4) . 3_754 ? S3 Fe1 S3 96.79(6) . 3_754 ? C1 S1 Fe1 104.13(17) . . ? C5 S2 Fe1 104.64(15) . . ? C3 S3 Fe1 104.50(17) . . ? C19 P1 C13 109.7(2) . . ? C19 P1 C25 109.67(18) . . ? C13 P1 C25 112.3(2) . . ? C19 P1 C31 108.0(2) . . ? C13 P1 C31 108.5(2) . . ? C25 P1 C31 108.6(2) . . ? C3 C1 C2 120.8(4) 3_754 . ? C3 C1 S1 121.8(4) 3_754 . ? C2 C1 S1 117.3(4) . . ? N1 C2 C1 178.6(6) . . ? C1 C3 C4 120.6(4) 3_754 . ? C1 C3 S3 120.8(4) 3_754 . ? C4 C3 S3 118.5(4) . . ? N2 C4 C3 178.5(6) . . ? C5 C5 C6 122.4(3) 3_754 . ? C5 C5 S2 121.56(14) 3_754 . ? C6 C5 S2 116.1(3) . . ? N3 C6 C5 179.3(7) . . ? C18 C13 C14 118.5(4) . . ? C18 C13 P1 120.5(4) . . ? C14 C13 P1 121.0(4) . . ? C13 C14 C15 120.7(5) . . ? C16 C15 C14 119.6(5) . . ? C15 C16 C17 120.4(5) . . ? C16 C17 C18 120.7(5) . . ? C13 C18 C17 120.0(5) . . ? C20 C19 C24 118.4(4) . . ? C20 C19 P1 122.7(4) . . ? C24 C19 P1 118.6(4) . . ? C19 C20 C21 119.8(5) . . ? C22 C21 C20 121.5(5) . . ? C21 C22 C23 119.1(5) . . ? C24 C23 C22 120.3(5) . . ? C23 C24 C19 121.0(4) . . ? C30 C25 C26 118.9(4) . . ? C30 C25 P1 122.6(4) . . ? C26 C25 P1 118.4(4) . . ? C25 C26 C27 120.0(5) . . ? C28 C27 C26 121.4(5) . . ? C27 C28 C29 118.5(5) . . ? C28 C29 C30 121.5(5) . . ? C25 C30 C29 119.8(5) . . ? C36 C31 C32 120.0(4) . . ? C36 C31 P1 119.8(4) . . ? C32 C31 P1 120.1(4) . . ? C33 C32 C31 119.2(4) . . ? C34 C33 C32 120.9(5) . . ? C33 C34 C35 121.0(5) . . ? C34 C35 C36 118.8(5) . . ? C31 C36 C35 120.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 70.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.190 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.040 #===END data_beta-8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H40 Fe N6 P2 S6' _chemical_formula_weight 1155.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.978(6) _cell_length_b 13.402(3) _cell_length_c 19.882(4) _cell_angle_alpha 90.00 _cell_angle_beta 130.09(3) _cell_angle_gamma 90.00 _cell_volume 5703(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.00 _exptl_crystal_description black _exptl_crystal_colour diamonds _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 5.053 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7823 _exptl_absorpt_correction_T_max 0.8415 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_standards_decay_% ? _diffrn_reflns_number 5405 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.1296 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 69.97 _reflns_number_total 5405 _reflns_number_gt 2466 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5405 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1327 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 0.716 _refine_ls_restrained_S_all 0.716 _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 Fe1 Fe 1.0000 0.20326(6) 0.7500 0.0542(2) Uani 1 2 d S . . P1 P 0.67044(4) 0.82320(7) 0.20845(6) 0.0524(2) Uani 1 1 d . . . S1 S 1.00876(5) 0.19076(8) 0.64490(6) 0.0692(3) Uani 1 1 d . . . S2 S 1.08196(5) 0.09819(7) 0.83367(6) 0.0643(3) Uani 1 1 d . . . S3 S 0.92816(4) 0.32548(8) 0.66805(6) 0.0673(3) Uani 1 1 d . . . N1 N 1.1142(2) 0.1081(4) 0.6074(3) 0.1230(17) Uani 1 1 d . . . N2 N 1.2131(2) -0.0060(3) 0.8544(3) 0.1196(17) Uani 1 1 d . . . N3 N 0.9084(3) 0.5979(3) 0.6396(3) 0.132(2) Uani 1 1 d . . . C1 C 1.07781(19) 0.1262(3) 0.6960(3) 0.0652(10) Uani 1 1 d . . . C2 C 1.10928(17) 0.0884(3) 0.7772(3) 0.0631(10) Uani 1 1 d . . . C3 C 1.0985(2) 0.1154(4) 0.6468(3) 0.0861(14) Uani 1 1 d . . . C4 C 1.1675(2) 0.0362(3) 0.8206(3) 0.0836(13) Uani 1 1 d . . . C5 C 0.96913(17) 0.4351(3) 0.7140(2) 0.0567(9) Uani 1 1 d . . . C6 C 0.9360(2) 0.5260(3) 0.6738(3) 0.0808(13) Uani 1 1 d . . . C7 C 0.61317(18) 0.7372(3) 0.1860(2) 0.0602(9) Uani 1 1 d . . . C8 C 0.5987(2) 0.7357(4) 0.2407(3) 0.0847(13) Uani 1 1 d . . . H8A H 0.6207 0.7760 0.2905 0.102 Uiso 1 1 calc R . . C9 C 0.5522(3) 0.6752(5) 0.2219(4) 0.1134(19) Uani 1 1 d . . . H9A H 0.5438 0.6730 0.2602 0.136 Uiso 1 1 calc R . . C10 C 0.5174(3) 0.6172(4) 0.1467(5) 0.115(2) Uani 1 1 d . . . H10A H 0.4844 0.5785 0.1327 0.138 Uiso 1 1 calc R . . C11 C 0.5322(2) 0.6178(4) 0.0941(4) 0.1007(16) Uani 1 1 d . . . H11A H 0.5096 0.5776 0.0442 0.121 Uiso 1 1 calc R . . C12 C 0.5802(2) 0.6768(3) 0.1125(3) 0.0791(12) Uani 1 1 d . . . H12A H 0.5900 0.6756 0.0758 0.095 Uiso 1 1 calc R . . C13 C 0.72711(17) 0.8420(3) 0.3247(2) 0.0547(9) Uani 1 1 d . . . C14 C 0.74966(19) 0.9357(3) 0.3592(2) 0.0746(12) Uani 1 1 d . . . H14A H 0.7343 0.9910 0.3224 0.090 Uiso 1 1 calc R . . C15 C 0.7955(2) 0.9470(4) 0.4495(3) 0.0953(16) Uani 1 1 d . . . H15A H 0.8108 1.0103 0.4731 0.114 Uiso 1 1 calc R . . C16 C 0.8180(2) 0.8673(4) 0.5035(3) 0.0883(15) Uani 1 1 d . . . H16A H 0.8487 0.8762 0.5639 0.106 Uiso 1 1 calc R . . C17 C 0.7961(2) 0.7731(4) 0.4702(2) 0.0784(13) Uani 1 1 d . . . H17A H 0.8120 0.7184 0.5078 0.094 Uiso 1 1 calc R . . C18 C 0.75048(19) 0.7599(3) 0.3808(2) 0.0677(11) Uani 1 1 d . . . H18A H 0.7353 0.6963 0.3579 0.081 Uiso 1 1 calc R . . C19 C 0.63089(16) 0.9383(3) 0.1530(2) 0.0552(9) Uani 1 1 d . . . C20 C 0.64952(19) 0.9970(3) 0.1166(3) 0.0716(11) Uani 1 1 d . . . H20A H 0.6834 0.9776 0.1211 0.086 Uiso 1 1 calc R . . C21 C 0.6178(2) 1.0850(3) 0.0732(3) 0.0800(13) Uani 1 1 d . . . H21A H 0.6297 1.1239 0.0473 0.096 Uiso 1 1 calc R . . C22 C 0.5690(2) 1.1135(3) 0.0690(3) 0.0822(13) Uani 1 1 d . . . H22A H 0.5476 1.1721 0.0398 0.099 Uiso 1 1 calc R . . C23 C 0.5511(2) 1.0576(3) 0.1070(3) 0.0812(13) Uani 1 1 d . . . H23A H 0.5188 1.0791 0.1055 0.097 Uiso 1 1 calc R . . C24 C 0.58130(19) 0.9693(3) 0.1473(2) 0.0667(10) Uani 1 1 d . . . H24A H 0.5681 0.9297 0.1711 0.080 Uiso 1 1 calc R . . C25 C 0.70824(16) 0.7760(3) 0.1688(2) 0.0524(8) Uani 1 1 d . . . C26 C 0.67713(17) 0.7723(3) 0.0795(2) 0.0638(10) Uani 1 1 d . . . H26A H 0.6364 0.7960 0.0392 0.077 Uiso 1 1 calc R . . C27 C 0.70697(19) 0.7329(3) 0.0507(2) 0.0680(11) Uani 1 1 d . . . H27A H 0.6862 0.7304 -0.0092 0.082 Uiso 1 1 calc R . . C28 C 0.76681(18) 0.6978(3) 0.1096(2) 0.0644(10) Uani 1 1 d . . . H28A H 0.7865 0.6717 0.0897 0.077 Uiso 1 1 calc R . . C29 C 0.79769(18) 0.7009(3) 0.1977(2) 0.0619(10) Uani 1 1 d . . . H29A H 0.8382 0.6763 0.2375 0.074 Uiso 1 1 calc R . . C30 C 0.76926(16) 0.7401(3) 0.2278(2) 0.0553(9) Uani 1 1 d . . . H30A H 0.7908 0.7427 0.2879 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0470(4) 0.0480(5) 0.0509(4) 0.000 0.0239(4) 0.000 P1 0.0513(5) 0.0530(5) 0.0481(5) 0.0001(4) 0.0298(4) -0.0002(4) S1 0.0610(6) 0.0808(7) 0.0576(5) 0.0086(5) 0.0346(5) 0.0003(5) S2 0.0618(6) 0.0578(6) 0.0605(5) 0.0096(4) 0.0336(5) 0.0134(5) S3 0.0458(5) 0.0613(6) 0.0621(5) 0.0002(4) 0.0198(4) 0.0046(4) N1 0.099(3) 0.174(5) 0.123(4) -0.034(4) 0.084(3) -0.026(3) N2 0.094(3) 0.096(3) 0.178(5) 0.033(3) 0.092(3) 0.032(3) N3 0.171(5) 0.079(3) 0.098(3) 0.014(3) 0.065(3) 0.052(3) C1 0.062(2) 0.056(2) 0.079(3) -0.010(2) 0.046(2) -0.0101(19) C2 0.055(2) 0.047(2) 0.079(3) -0.0034(18) 0.039(2) -0.0024(18) C3 0.073(3) 0.104(4) 0.096(3) -0.023(3) 0.061(3) -0.017(3) C4 0.080(3) 0.063(3) 0.113(4) 0.005(3) 0.065(3) 0.002(2) C5 0.069(2) 0.051(2) 0.0550(19) 0.0027(15) 0.0423(18) 0.0101(18) C6 0.108(4) 0.061(3) 0.061(2) 0.002(2) 0.049(2) 0.018(3) C7 0.059(2) 0.057(2) 0.064(2) 0.0047(17) 0.039(2) 0.0005(18) C8 0.078(3) 0.098(4) 0.098(3) -0.008(3) 0.066(3) -0.014(3) C9 0.091(4) 0.135(5) 0.137(5) 0.020(4) 0.084(4) -0.007(4) C10 0.072(3) 0.093(4) 0.166(6) 0.029(4) 0.069(4) -0.004(3) C11 0.082(3) 0.072(3) 0.111(4) -0.014(3) 0.045(3) -0.023(3) C12 0.079(3) 0.073(3) 0.076(3) -0.004(2) 0.045(2) -0.011(2) C13 0.060(2) 0.052(2) 0.0516(19) 0.0027(16) 0.0357(17) 0.0048(17) C14 0.076(3) 0.062(2) 0.057(2) -0.0111(19) 0.030(2) 0.000(2) C15 0.105(4) 0.084(3) 0.062(3) -0.018(2) 0.038(3) 0.001(3) C16 0.082(3) 0.112(4) 0.049(2) -0.008(2) 0.032(2) 0.012(3) C17 0.084(3) 0.098(4) 0.053(2) 0.014(2) 0.044(2) 0.020(3) C18 0.079(3) 0.065(3) 0.065(2) 0.0010(19) 0.049(2) 0.004(2) C19 0.051(2) 0.055(2) 0.0479(18) -0.0016(15) 0.0262(16) -0.0006(17) C20 0.066(2) 0.066(3) 0.077(3) 0.009(2) 0.043(2) 0.000(2) C21 0.091(3) 0.067(3) 0.077(3) 0.008(2) 0.052(3) -0.006(3) C22 0.083(3) 0.061(3) 0.064(3) 0.002(2) 0.030(2) 0.009(2) C23 0.075(3) 0.071(3) 0.083(3) 0.003(2) 0.044(3) 0.015(2) C24 0.063(2) 0.067(3) 0.065(2) 0.0027(19) 0.039(2) 0.008(2) C25 0.0495(19) 0.056(2) 0.0462(17) -0.0027(15) 0.0284(16) -0.0051(17) C26 0.050(2) 0.079(3) 0.0507(19) 0.0061(18) 0.0273(17) 0.008(2) C27 0.070(3) 0.084(3) 0.0472(19) 0.0018(19) 0.036(2) 0.004(2) C28 0.065(2) 0.070(3) 0.067(2) -0.0012(19) 0.046(2) -0.003(2) C29 0.055(2) 0.069(3) 0.061(2) 0.0062(18) 0.0372(18) 0.0040(19) C30 0.055(2) 0.058(2) 0.0473(18) -0.0001(16) 0.0305(17) -0.0015(17) _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 Fe1 S2 2.2571(13) 2_756 ? Fe1 S2 2.2572(13) . ? Fe1 S1 2.2614(11) 2_756 ? Fe1 S1 2.2615(11) . ? Fe1 S3 2.2715(13) . ? Fe1 S3 2.2715(13) 2_756 ? P1 C7 1.782(4) . ? P1 C13 1.789(4) . ? P1 C25 1.792(4) . ? P1 C19 1.802(4) . ? S1 C1 1.728(4) . ? S2 C2 1.723(4) . ? S3 C5 1.720(4) . ? N1 C3 1.123(5) . ? N2 C4 1.138(6) . ? N3 C6 1.144(5) . ? C1 C2 1.345(5) . ? C1 C3 1.427(6) . ? C2 C4 1.441(6) . ? C5 C5 1.360(7) 2_756 ? C5 C6 1.425(5) . ? C7 C12 1.380(5) . ? C7 C8 1.384(6) . ? C8 C9 1.365(6) . ? C9 C10 1.383(8) . ? C10 C11 1.350(7) . ? C11 C12 1.390(6) . ? C13 C14 1.374(5) . ? C13 C18 1.394(5) . ? C14 C15 1.387(5) . ? C15 C16 1.349(6) . ? C16 C17 1.373(6) . ? C17 C18 1.377(5) . ? C19 C20 1.379(5) . ? C19 C24 1.381(5) . ? C20 C21 1.393(5) . ? C21 C22 1.368(6) . ? C22 C23 1.368(6) . ? C23 C24 1.372(5) . ? C25 C26 1.387(4) . ? C25 C30 1.394(5) . ? C26 C27 1.386(5) . ? C27 C28 1.368(5) . ? C28 C29 1.366(5) . ? C29 C30 1.371(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 S2 Fe1 S2 102.81(7) 2_756 . ? S2 Fe1 S1 88.37(5) 2_756 2_756 ? S2 Fe1 S1 86.33(5) . 2_756 ? S2 Fe1 S1 86.33(5) 2_756 . ? S2 Fe1 S1 88.37(5) . . ? S1 Fe1 S1 171.51(7) 2_756 . ? S2 Fe1 S3 84.92(5) 2_756 . ? S2 Fe1 S3 171.17(5) . . ? S1 Fe1 S3 98.27(5) 2_756 . ? S1 Fe1 S3 87.88(5) . . ? S2 Fe1 S3 171.17(5) 2_756 2_756 ? S2 Fe1 S3 84.92(5) . 2_756 ? S1 Fe1 S3 87.89(5) 2_756 2_756 ? S1 Fe1 S3 98.26(5) . 2_756 ? S3 Fe1 S3 87.70(7) . 2_756 ? C7 P1 C13 108.67(18) . . ? C7 P1 C25 110.60(17) . . ? C13 P1 C25 109.56(16) . . ? C7 P1 C19 107.57(18) . . ? C13 P1 C19 110.72(16) . . ? C25 P1 C19 109.70(17) . . ? C1 S1 Fe1 103.87(14) . . ? C2 S2 Fe1 103.51(13) . . ? C5 S3 Fe1 104.82(12) . . ? C2 C1 C3 122.9(4) . . ? C2 C1 S1 120.9(3) . . ? C3 C1 S1 116.2(3) . . ? C1 C2 C4 121.0(4) . . ? C1 C2 S2 122.1(3) . . ? C4 C2 S2 116.8(3) . . ? N1 C3 C1 179.0(7) . . ? N2 C4 C2 179.2(7) . . ? C5 C5 C6 121.2(2) 2_756 . ? C5 C5 S3 121.30(12) 2_756 . ? C6 C5 S3 117.5(3) . . ? N3 C6 C5 178.3(4) . . ? C12 C7 C8 119.3(4) . . ? C12 C7 P1 121.6(3) . . ? C8 C7 P1 118.9(3) . . ? C9 C8 C7 120.2(5) . . ? C8 C9 C10 120.9(6) . . ? C11 C10 C9 118.7(5) . . ? C10 C11 C12 121.7(5) . . ? C7 C12 C11 119.1(5) . . ? C14 C13 C18 119.6(3) . . ? C14 C13 P1 120.9(3) . . ? C18 C13 P1 119.4(3) . . ? C13 C14 C15 119.4(4) . . ? C16 C15 C14 120.8(4) . . ? C15 C16 C17 120.6(4) . . ? C16 C17 C18 119.7(4) . . ? C17 C18 C13 119.9(4) . . ? C20 C19 C24 119.0(4) . . ? C20 C19 P1 121.2(3) . . ? C24 C19 P1 119.8(3) . . ? C19 C20 C21 120.3(4) . . ? C22 C21 C20 119.1(4) . . ? C23 C22 C21 121.3(4) . . ? C22 C23 C24 119.2(4) . . ? C23 C24 C19 121.1(4) . . ? C26 C25 C30 118.9(3) . . ? C26 C25 P1 120.9(3) . . ? C30 C25 P1 120.1(3) . . ? C27 C26 C25 119.7(3) . . ? C28 C27 C26 120.5(3) . . ? C29 C28 C27 120.2(4) . . ? C28 C29 C30 120.4(4) . . ? C29 C30 C25 120.4(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 69.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.238 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.043 #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86.25 H64.50 Cr N6 O0.75 P3 S6' _chemical_formula_weight 1534.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Cr' 'Cr' 0.3209 0.6236 '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' 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 24.5937(9) _cell_length_b 14.7251(6) _cell_length_c 25.2038(10) _cell_angle_alpha 90.00 _cell_angle_beta 117.822(10) _cell_angle_gamma 90.00 _cell_volume 8072.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 116 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 24.98 _exptl_crystal_description plates _exptl_crystal_colour brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3180 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.855886 _exptl_absorpt_correction_T_max 0.968679 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 AXS SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56320 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 22.50 _reflns_number_total 10555 _reflns_number_gt 5665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0540P)^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 10555 _refine_ls_number_parameters 937 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.565 _refine_ls_shift/su_mean 0.041 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 Cr1 Cr 0.24340(3) 0.42263(4) 0.63907(3) 0.0522(2) Uani 1 1 d . . . P1 P 0.02896(5) 0.68405(7) 0.73577(5) 0.0556(3) Uani 1 1 d . . . P2 P 0.49738(6) 0.25706(9) 0.93596(6) 0.0693(4) Uani 1 1 d . . . P3 P 0.20274(6) 0.85930(8) 0.56058(6) 0.0679(4) Uani 1 1 d . . . S1 S 0.32702(5) 0.52787(7) 0.68177(5) 0.0616(3) Uani 1 1 d . . . S2 S 0.21717(5) 0.47076(7) 0.71527(5) 0.0613(3) Uani 1 1 d . . . S3 S 0.16733(5) 0.52284(7) 0.56854(5) 0.0582(3) Uani 1 1 d . . . S4 S 0.27153(5) 0.39213(7) 0.56158(5) 0.0604(3) Uani 1 1 d . . . S5 S 0.31352(5) 0.30862(7) 0.70116(5) 0.0643(3) Uani 1 1 d . . . S6 S 0.16464(5) 0.31036(7) 0.60965(5) 0.0591(3) Uani 1 1 d . . . N1 N 0.4156(2) 0.6609(3) 0.8201(2) 0.1036(16) Uani 1 1 d . . . N2 N 0.2822(2) 0.5942(3) 0.8578(2) 0.1028(15) Uani 1 1 d . . . N3 N 0.0904(2) 0.5830(3) 0.4079(2) 0.1017(16) Uani 1 1 d . . . N4 N 0.2206(2) 0.4298(3) 0.4015(2) 0.1041(16) Uani 1 1 d . . . N5 N 0.3143(2) 0.0812(3) 0.7620(2) 0.1206(19) Uani 1 1 d . . . N6 N 0.1375(2) 0.0777(3) 0.6432(2) 0.1000(15) Uani 1 1 d . . . C1 C 0.3264(2) 0.5577(3) 0.74822(18) 0.0552(12) Uani 1 1 d . . . C2 C 0.2813(2) 0.5344(3) 0.76186(19) 0.0560(12) Uani 1 1 d . . . C3 C 0.17146(19) 0.5029(3) 0.50321(19) 0.0537(11) Uani 1 1 d . . . C4 C 0.21502(19) 0.4492(3) 0.50031(18) 0.0528(11) Uani 1 1 d . . . C5 C 0.2644(2) 0.2191(3) 0.69344(19) 0.0587(12) Uani 1 1 d . . . C6 C 0.2034(2) 0.2195(3) 0.65537(19) 0.0565(12) Uani 1 1 d . . . C7 C 0.3761(2) 0.6145(3) 0.7886(2) 0.0717(14) Uani 1 1 d . . . C8 C 0.2833(2) 0.5668(3) 0.8158(2) 0.0702(14) Uani 1 1 d . . . C9 C 0.1269(2) 0.5471(3) 0.4494(2) 0.0635(13) Uani 1 1 d . . . C10 C 0.2177(2) 0.4383(3) 0.4449(2) 0.0677(14) Uani 1 1 d . . . C11 C 0.2920(2) 0.1416(3) 0.7313(2) 0.0753(15) Uani 1 1 d . . . C12 C 0.1674(2) 0.1401(3) 0.6498(2) 0.0723(14) Uani 1 1 d . . . C13 C 0.08141(19) 0.7759(3) 0.7509(2) 0.0561(12) Uani 1 1 d . . . C14 C 0.0785(2) 0.8277(3) 0.7038(2) 0.0713(13) Uani 1 1 d . . . H14A H 0.0526 0.8105 0.6645 0.086 Uiso 1 1 calc R . . C15 C 0.1140(3) 0.9049(3) 0.7153(3) 0.0877(16) Uani 1 1 d . . . H15A H 0.1119 0.9398 0.6836 0.105 Uiso 1 1 calc R . . C16 C 0.1522(3) 0.9300(3) 0.7729(3) 0.0862(16) Uani 1 1 d . . . H16A H 0.1758 0.9824 0.7804 0.103 Uiso 1 1 calc R . . C17 C 0.1562(2) 0.8786(4) 0.8201(3) 0.0867(16) Uani 1 1 d . . . H17A H 0.1829 0.8955 0.8594 0.104 Uiso 1 1 calc R . . C18 C 0.1203(2) 0.8016(3) 0.8088(2) 0.0724(14) Uani 1 1 d . . . H18A H 0.1224 0.7670 0.8406 0.087 Uiso 1 1 calc R . . C19 C 0.0065(2) 0.6460(3) 0.66137(19) 0.0554(11) Uani 1 1 d . . . C20 C -0.0449(2) 0.6825(3) 0.6128(2) 0.0682(13) Uani 1 1 d . . . H20A H -0.0710 0.7210 0.6194 0.082 Uiso 1 1 calc R . . C21 C -0.0572(2) 0.6619(4) 0.5553(2) 0.0849(16) Uani 1 1 d . . . H21A H -0.0918 0.6864 0.5232 0.102 Uiso 1 1 calc R . . C22 C -0.0191(3) 0.6058(4) 0.5448(3) 0.0985(19) Uani 1 1 d . . . H22A H -0.0273 0.5933 0.5056 0.118 Uiso 1 1 calc R . . C23 C 0.0312(3) 0.5679(4) 0.5918(3) 0.0961(18) Uani 1 1 d . . . H23A H 0.0567 0.5288 0.5846 0.115 Uiso 1 1 calc R . . C24 C 0.0440(2) 0.5881(3) 0.6501(2) 0.0726(14) Uani 1 1 d . . . H24A H 0.0781 0.5624 0.6820 0.087 Uiso 1 1 calc R . . C25 C 0.0656(2) 0.5957(3) 0.78968(19) 0.0582(12) Uani 1 1 d . . . C26 C 0.1250(2) 0.5692(3) 0.8060(2) 0.0753(14) Uani 1 1 d . . . H26A H 0.1471 0.5998 0.7899 0.090 Uiso 1 1 calc R . . C27 C 0.1525(3) 0.4991(4) 0.8450(3) 0.0936(17) Uani 1 1 d . . . H27A H 0.1926 0.4822 0.8550 0.112 Uiso 1 1 calc R . . C28 C 0.1207(3) 0.4540(4) 0.8692(2) 0.1005(19) Uani 1 1 d . . . H28A H 0.1391 0.4062 0.8958 0.121 Uiso 1 1 calc R . . C29 C 0.0622(3) 0.4789(4) 0.8546(3) 0.109(2) Uani 1 1 d . . . H29A H 0.0408 0.4480 0.8712 0.131 Uiso 1 1 calc R . . C30 C 0.0340(2) 0.5503(3) 0.8149(2) 0.0845(15) Uani 1 1 d . . . H30A H -0.0060 0.5674 0.8054 0.101 Uiso 1 1 calc R . . C31 C -0.0367(2) 0.7232(3) 0.74170(18) 0.0551(12) Uani 1 1 d . . . C32 C -0.0335(2) 0.8006(3) 0.77423(19) 0.0683(13) Uani 1 1 d . . . H32A H 0.0026 0.8345 0.7919 0.082 Uiso 1 1 calc R . . C33 C -0.0842(3) 0.8273(3) 0.7803(2) 0.0777(15) Uani 1 1 d . . . H33A H -0.0817 0.8786 0.8028 0.093 Uiso 1 1 calc R . . C34 C -0.1375(2) 0.7796(4) 0.7540(2) 0.0768(15) Uani 1 1 d . . . H34A H -0.1714 0.7991 0.7579 0.092 Uiso 1 1 calc R . . C35 C -0.1413(2) 0.7025(3) 0.7216(2) 0.0775(14) Uani 1 1 d . . . H35A H -0.1778 0.6696 0.7039 0.093 Uiso 1 1 calc R . . C36 C -0.0912(2) 0.6739(3) 0.7152(2) 0.0676(13) Uani 1 1 d . . . H36A H -0.0939 0.6218 0.6933 0.081 Uiso 1 1 calc R . . C37 C 0.5013(3) 0.2198(3) 0.8707(2) 0.0770(15) Uani 1 1 d . . . C38 C 0.5513(3) 0.2428(4) 0.8632(3) 0.1049(19) Uani 1 1 d . . . H38A H 0.5813 0.2812 0.8905 0.126 Uiso 1 1 calc R . . C39 C 0.5569(3) 0.2092(6) 0.8151(4) 0.140(3) Uani 1 1 d . . . H39A H 0.5911 0.2242 0.8103 0.168 Uiso 1 1 calc R . . C40 C 0.5123(4) 0.1538(6) 0.7742(4) 0.153(3) Uani 1 1 d . . . H40A H 0.5160 0.1321 0.7413 0.183 Uiso 1 1 calc R . . C41 C 0.4625(4) 0.1305(5) 0.7815(3) 0.147(3) Uani 1 1 d . . . H41A H 0.4324 0.0927 0.7537 0.177 Uiso 1 1 calc R . . C42 C 0.4568(3) 0.1627(4) 0.8301(3) 0.1061(19) Uani 1 1 d . . . H42A H 0.4232 0.1461 0.8354 0.127 Uiso 1 1 calc R . . C43 C 0.5400(2) 0.1801(3) 0.9964(2) 0.0700(13) Uani 1 1 d . . . C44 C 0.5548(2) 0.0945(4) 0.9842(3) 0.0868(16) Uani 1 1 d . . . H44A H 0.5438 0.0775 0.9450 0.104 Uiso 1 1 calc R . . C45 C 0.5860(3) 0.0348(4) 1.0308(4) 0.106(2) Uani 1 1 d . . . H45A H 0.5960 -0.0228 1.0230 0.128 Uiso 1 1 calc R . . C46 C 0.6021(3) 0.0595(5) 1.0878(3) 0.114(2) Uani 1 1 d . . . H46A H 0.6234 0.0186 1.1188 0.137 Uiso 1 1 calc R . . C47 C 0.5878(3) 0.1428(5) 1.1008(3) 0.110(2) Uani 1 1 d . . . H47A H 0.5987 0.1583 1.1403 0.132 Uiso 1 1 calc R . . C48 C 0.5571(2) 0.2040(4) 1.0552(3) 0.0925(17) Uani 1 1 d . . . H48A H 0.5478 0.2615 1.0640 0.111 Uiso 1 1 calc R . . C49 C 0.5302(2) 0.3676(3) 0.9545(2) 0.0710(14) Uani 1 1 d . . . C50 C 0.4956(2) 0.4431(4) 0.9254(2) 0.0983(18) Uani 1 1 d . . . H50A H 0.4543 0.4367 0.8980 0.118 Uiso 1 1 calc R . . C51 C 0.5229(3) 0.5291(4) 0.9371(3) 0.112(2) Uani 1 1 d . . . H51A H 0.4995 0.5796 0.9172 0.134 Uiso 1 1 calc R . . C52 C 0.5823(3) 0.5394(4) 0.9767(3) 0.108(2) Uani 1 1 d . . . H52A H 0.6003 0.5966 0.9831 0.129 Uiso 1 1 calc R . . C53 C 0.6162(3) 0.4673(5) 1.0074(3) 0.109(2) Uani 1 1 d . . . H53A H 0.6568 0.4758 1.0363 0.131 Uiso 1 1 calc R . . C54 C 0.5911(3) 0.3802(4) 0.9962(2) 0.0946(17) Uani 1 1 d . . . H54A H 0.6152 0.3307 1.0167 0.114 Uiso 1 1 calc R . . C55 C 0.4190(2) 0.2599(3) 0.9210(2) 0.0652(13) Uani 1 1 d . . . C56 C 0.4022(2) 0.2254(3) 0.9621(2) 0.0734(14) Uani 1 1 d . . . H56A H 0.4316 0.1984 0.9972 0.088 Uiso 1 1 calc R . . C57 C 0.3416(3) 0.2308(3) 0.9513(3) 0.0843(16) Uani 1 1 d . . . H57A H 0.3303 0.2064 0.9787 0.101 Uiso 1 1 calc R . . C58 C 0.2983(3) 0.2721(4) 0.9001(3) 0.0946(18) Uani 1 1 d . . . H58A H 0.2578 0.2769 0.8934 0.113 Uiso 1 1 calc R . . C59 C 0.3148(3) 0.3061(4) 0.8591(3) 0.0913(17) Uani 1 1 d . . . H59A H 0.2854 0.3339 0.8244 0.110 Uiso 1 1 calc R . . C60 C 0.3741(2) 0.2996(3) 0.8688(2) 0.0755(14) Uani 1 1 d . . . H60A H 0.3846 0.3220 0.8403 0.091 Uiso 1 1 calc R . . C61 C 0.2266(3) 0.9719(3) 0.5561(2) 0.0832(16) Uani 1 1 d . . . C62 C 0.1889(3) 1.0441(4) 0.5341(3) 0.116(2) Uani 1 1 d . . . H62A H 0.1467 1.0353 0.5178 0.139 Uiso 1 1 calc R . . C63 C 0.2114(5) 1.1323(6) 0.5350(4) 0.146(4) Uani 1 1 d . . . H63A H 0.1849 1.1814 0.5191 0.176 Uiso 1 1 calc R . . C64 C 0.2722(6) 1.1422(6) 0.5595(5) 0.165(5) Uani 1 1 d . . . H64A H 0.2874 1.2003 0.5603 0.198 Uiso 1 1 calc R . . C65 C 0.3141(4) 1.0727(5) 0.5839(4) 0.157(3) Uani 1 1 d . . . H65A H 0.3562 1.0830 0.6014 0.188 Uiso 1 1 calc R . . C66 C 0.2898(4) 0.9859(4) 0.5810(3) 0.120(2) Uani 1 1 d . . . H66A H 0.3163 0.9366 0.5959 0.144 Uiso 1 1 calc R . . C67 C 0.1218(2) 0.8486(3) 0.5198(2) 0.0762(14) Uani 1 1 d . . . C68 C 0.0851(3) 0.8924(4) 0.5398(3) 0.1049(19) Uani 1 1 d . . . H68A H 0.1027 0.9320 0.5722 0.126 Uiso 1 1 calc R . . C69 C 0.0224(4) 0.8777(5) 0.5120(4) 0.132(3) Uani 1 1 d . . . H69A H -0.0020 0.9066 0.5261 0.159 Uiso 1 1 calc R . . C70 C -0.0042(3) 0.8199(6) 0.4631(4) 0.140(3) Uani 1 1 d . . . H70A H -0.0466 0.8111 0.4436 0.169 Uiso 1 1 calc R . . C71 C 0.0320(4) 0.7759(5) 0.4439(3) 0.131(3) Uani 1 1 d . . . H71A H 0.0141 0.7363 0.4115 0.157 Uiso 1 1 calc R . . C72 C 0.0949(3) 0.7893(4) 0.4715(3) 0.0977(18) Uani 1 1 d . . . H72A H 0.1191 0.7587 0.4579 0.117 Uiso 1 1 calc R . . C73 C 0.2227(2) 0.8304(3) 0.63572(19) 0.0589(12) Uani 1 1 d . . . C74 C 0.1978(2) 0.7530(3) 0.6467(2) 0.0697(13) Uani 1 1 d . . . H74A H 0.1713 0.7168 0.6148 0.084 Uiso 1 1 calc R . . C75 C 0.2121(2) 0.7291(3) 0.7046(3) 0.0788(15) Uani 1 1 d . . . H75A H 0.1957 0.6766 0.7119 0.095 Uiso 1 1 calc R . . C76 C 0.2509(3) 0.7834(4) 0.7515(3) 0.0937(17) Uani 1 1 d . . . H76A H 0.2612 0.7668 0.7907 0.112 Uiso 1 1 calc R . . C77 C 0.2744(2) 0.8610(4) 0.7412(3) 0.0953(18) Uani 1 1 d . . . H77A H 0.2997 0.8980 0.7731 0.114 Uiso 1 1 calc R . . C78 C 0.2609(2) 0.8848(3) 0.6840(3) 0.0810(15) Uani 1 1 d . . . H78A H 0.2774 0.9377 0.6772 0.097 Uiso 1 1 calc R . . C79 C 0.2391(2) 0.7857(3) 0.5310(2) 0.0611(12) Uani 1 1 d . . . C80 C 0.2382(2) 0.8084(3) 0.4769(2) 0.0800(15) Uani 1 1 d . . . H80A H 0.2204 0.8628 0.4580 0.096 Uiso 1 1 calc R . . C81 C 0.2635(2) 0.7512(4) 0.4509(2) 0.0846(16) Uani 1 1 d . . . H81A H 0.2620 0.7664 0.4144 0.102 Uiso 1 1 calc R . . C82 C 0.2910(2) 0.6715(3) 0.4792(2) 0.0761(14) Uani 1 1 d . . . H82A H 0.3080 0.6327 0.4618 0.091 Uiso 1 1 calc R . . C83 C 0.29330(19) 0.6493(3) 0.5327(2) 0.0693(13) Uani 1 1 d . . . H83A H 0.3123 0.5956 0.5518 0.083 Uiso 1 1 calc R . . C84 C 0.2676(2) 0.7059(3) 0.5588(2) 0.0620(12) Uani 1 1 d . . . H84A H 0.2696 0.6901 0.5954 0.074 Uiso 1 1 calc R . . O1 O 0.4376(8) 1.4106(8) 0.5985(6) 0.333(7) Uani 0.75 1 d PDU . . C85 C 0.4365(6) 1.2738(10) 0.6268(5) 0.251(7) Uani 0.75 1 d PDU . . H85A H 0.4153 1.2738 0.5837 0.377 Uiso 0.75 1 calc PR . . H85B H 0.4103 1.2486 0.6417 0.377 Uiso 0.75 1 calc PR . . H85C H 0.4732 1.2379 0.6406 0.377 Uiso 0.75 1 calc PR . . C86 C 0.4542(16) 1.3745(12) 0.6503(7) 0.54(2) Uani 0.75 1 d PDU . . C87 C 0.4944(12) 1.4001(9) 0.7182(7) 0.500(19) Uani 0.75 1 d PDU . . H87A H 0.5021 1.4643 0.7217 0.750 Uiso 0.75 1 calc PR . . H87B H 0.5328 1.3681 0.7341 0.750 Uiso 0.75 1 calc PR . . H87C H 0.4730 1.3836 0.7403 0.750 Uiso 0.75 1 calc PR . . 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 Cr1 0.0620(5) 0.0427(4) 0.0504(5) 0.0010(3) 0.0252(4) -0.0041(3) P1 0.0643(8) 0.0525(7) 0.0534(8) -0.0013(6) 0.0303(7) 0.0013(6) P2 0.0612(9) 0.0679(9) 0.0682(9) 0.0025(7) 0.0212(7) 0.0059(7) P3 0.0868(10) 0.0436(7) 0.0665(9) 0.0005(6) 0.0300(8) 0.0005(7) S1 0.0704(8) 0.0550(7) 0.0637(8) -0.0037(6) 0.0349(7) -0.0120(6) S2 0.0705(8) 0.0620(8) 0.0576(8) -0.0033(6) 0.0351(7) -0.0112(6) S3 0.0693(8) 0.0514(7) 0.0609(8) 0.0042(6) 0.0363(7) 0.0066(6) S4 0.0720(8) 0.0539(7) 0.0560(8) 0.0060(6) 0.0306(7) 0.0140(6) S5 0.0634(8) 0.0528(7) 0.0627(8) 0.0058(6) 0.0177(6) -0.0055(6) S6 0.0617(8) 0.0508(7) 0.0543(7) 0.0045(6) 0.0181(6) -0.0059(6) N1 0.083(3) 0.116(4) 0.097(4) -0.034(3) 0.030(3) -0.030(3) N2 0.123(4) 0.120(4) 0.069(3) -0.017(3) 0.047(3) 0.004(3) N3 0.097(4) 0.127(4) 0.076(3) 0.042(3) 0.037(3) 0.039(3) N4 0.146(4) 0.106(4) 0.067(3) 0.013(3) 0.055(3) 0.056(3) N5 0.121(4) 0.065(3) 0.111(4) 0.029(3) 0.001(3) -0.009(3) N6 0.110(4) 0.075(3) 0.102(4) 0.005(3) 0.039(3) -0.033(3) C1 0.060(3) 0.046(3) 0.050(3) 0.002(2) 0.018(3) -0.001(2) C2 0.070(3) 0.051(3) 0.046(3) 0.001(2) 0.027(3) 0.006(2) C3 0.059(3) 0.045(3) 0.056(3) 0.007(2) 0.025(3) 0.003(2) C4 0.065(3) 0.045(3) 0.048(3) -0.001(2) 0.026(3) -0.005(2) C5 0.082(4) 0.043(3) 0.045(3) 0.004(2) 0.024(3) -0.004(3) C6 0.071(3) 0.044(3) 0.048(3) -0.003(2) 0.023(3) -0.015(2) C7 0.069(4) 0.077(4) 0.068(4) -0.007(3) 0.031(3) 0.000(3) C8 0.074(3) 0.075(4) 0.059(4) 0.001(3) 0.029(3) 0.005(3) C9 0.068(4) 0.063(3) 0.069(4) 0.008(3) 0.039(3) 0.008(3) C10 0.079(4) 0.062(3) 0.060(4) 0.008(3) 0.030(3) 0.020(3) C11 0.086(4) 0.053(3) 0.066(4) 0.003(3) 0.018(3) -0.012(3) C12 0.080(4) 0.065(4) 0.057(3) 0.004(3) 0.020(3) -0.009(3) C13 0.062(3) 0.054(3) 0.055(3) -0.005(3) 0.030(3) -0.001(2) C14 0.082(4) 0.063(3) 0.068(4) 0.006(3) 0.034(3) -0.002(3) C15 0.111(5) 0.068(4) 0.095(5) 0.014(3) 0.058(4) -0.004(3) C16 0.100(5) 0.048(3) 0.121(5) -0.009(4) 0.060(4) -0.007(3) C17 0.095(4) 0.075(4) 0.088(4) -0.017(3) 0.041(3) -0.016(3) C18 0.087(4) 0.063(3) 0.074(4) -0.003(3) 0.043(3) -0.014(3) C19 0.058(3) 0.056(3) 0.056(3) -0.007(2) 0.030(3) -0.002(2) C20 0.073(4) 0.074(3) 0.056(3) -0.004(3) 0.029(3) 0.007(3) C21 0.090(4) 0.102(4) 0.059(4) -0.001(3) 0.031(3) -0.004(3) C22 0.104(5) 0.136(6) 0.063(4) -0.031(4) 0.046(4) -0.033(4) C23 0.083(4) 0.117(5) 0.101(5) -0.052(4) 0.053(4) -0.009(4) C24 0.067(3) 0.080(4) 0.072(4) -0.020(3) 0.034(3) -0.002(3) C25 0.061(3) 0.058(3) 0.053(3) -0.001(2) 0.025(3) -0.005(3) C26 0.077(4) 0.070(3) 0.077(4) 0.015(3) 0.035(3) 0.002(3) C27 0.085(4) 0.082(4) 0.099(5) 0.019(3) 0.030(4) 0.014(3) C28 0.107(5) 0.085(4) 0.078(4) 0.025(3) 0.017(4) 0.010(4) C29 0.109(5) 0.104(5) 0.105(5) 0.043(4) 0.042(4) -0.003(4) C30 0.072(4) 0.090(4) 0.085(4) 0.013(3) 0.031(3) 0.004(3) C31 0.060(3) 0.057(3) 0.049(3) 0.000(2) 0.026(3) 0.001(2) C32 0.078(4) 0.065(3) 0.071(3) -0.009(3) 0.043(3) -0.004(3) C33 0.103(4) 0.069(4) 0.076(4) -0.011(3) 0.054(4) 0.013(3) C34 0.078(4) 0.085(4) 0.082(4) 0.009(3) 0.049(3) 0.018(3) C35 0.079(4) 0.077(4) 0.087(4) 0.002(3) 0.047(3) -0.001(3) C36 0.072(4) 0.065(3) 0.076(3) -0.008(3) 0.042(3) 0.007(3) C37 0.061(4) 0.086(4) 0.076(4) -0.001(3) 0.025(3) 0.012(3) C38 0.099(5) 0.123(5) 0.105(5) -0.014(4) 0.057(4) 0.006(4) C39 0.117(6) 0.190(8) 0.140(7) -0.009(6) 0.083(6) 0.010(6) C40 0.140(8) 0.221(9) 0.117(7) -0.035(6) 0.077(6) 0.025(7) C41 0.115(6) 0.199(8) 0.122(7) -0.056(6) 0.051(5) 0.004(6) C42 0.091(5) 0.138(5) 0.094(5) -0.034(4) 0.046(4) -0.006(4) C43 0.058(3) 0.064(4) 0.069(4) 0.005(3) 0.014(3) 0.001(3) C44 0.077(4) 0.061(4) 0.097(4) 0.006(3) 0.020(3) -0.004(3) C45 0.103(5) 0.061(4) 0.129(6) 0.002(4) 0.032(5) -0.004(3) C46 0.103(5) 0.080(5) 0.120(6) 0.038(4) 0.020(5) 0.001(4) C47 0.104(5) 0.113(5) 0.079(4) 0.023(4) 0.013(4) 0.005(4) C48 0.091(4) 0.085(4) 0.075(4) 0.006(4) 0.017(3) 0.014(3) C49 0.059(3) 0.060(3) 0.077(4) 0.006(3) 0.018(3) 0.005(3) C50 0.078(4) 0.082(4) 0.106(5) 0.012(4) 0.018(3) 0.002(4) C51 0.107(5) 0.072(4) 0.131(6) 0.019(4) 0.034(5) 0.012(4) C52 0.119(6) 0.074(4) 0.121(6) -0.003(4) 0.048(5) -0.018(4) C53 0.094(5) 0.103(5) 0.098(5) 0.006(4) 0.017(4) -0.016(4) C54 0.076(4) 0.077(4) 0.104(5) 0.012(3) 0.019(4) 0.000(3) C55 0.063(3) 0.060(3) 0.060(3) -0.001(3) 0.018(3) 0.000(3) C56 0.066(4) 0.062(3) 0.078(4) 0.002(3) 0.021(3) -0.004(3) C57 0.085(4) 0.078(4) 0.088(4) 0.005(3) 0.040(4) -0.015(3) C58 0.066(4) 0.094(4) 0.115(6) -0.005(4) 0.035(4) -0.006(3) C59 0.064(4) 0.100(4) 0.082(4) 0.006(3) 0.011(3) -0.003(3) C60 0.060(4) 0.088(4) 0.071(4) 0.007(3) 0.024(3) -0.001(3) C61 0.124(5) 0.048(3) 0.089(4) -0.008(3) 0.060(4) -0.007(4) C62 0.210(7) 0.056(4) 0.108(5) 0.017(3) 0.096(5) 0.026(5) C63 0.290(12) 0.066(6) 0.151(7) 0.013(5) 0.160(9) 0.030(7) C64 0.327(15) 0.061(5) 0.212(11) -0.016(6) 0.214(12) -0.020(9) C65 0.232(9) 0.091(5) 0.226(9) -0.047(6) 0.173(8) -0.061(6) C66 0.172(7) 0.052(4) 0.162(6) -0.020(4) 0.100(6) -0.032(4) C67 0.080(4) 0.061(3) 0.068(4) 0.001(3) 0.018(3) 0.009(3) C68 0.086(5) 0.099(5) 0.106(5) -0.012(4) 0.024(4) 0.012(4) C69 0.093(6) 0.120(6) 0.160(7) -0.005(5) 0.038(5) 0.025(5) C70 0.077(5) 0.142(7) 0.143(8) 0.025(6) 0.002(5) 0.010(5) C71 0.099(6) 0.136(6) 0.112(6) -0.017(4) 0.011(5) -0.007(5) C72 0.085(5) 0.101(4) 0.083(4) -0.007(4) 0.019(4) 0.000(4) C73 0.063(3) 0.044(3) 0.059(3) -0.003(2) 0.019(3) -0.002(2) C74 0.078(4) 0.056(3) 0.074(4) -0.001(3) 0.034(3) 0.004(3) C75 0.087(4) 0.059(3) 0.098(5) 0.016(3) 0.049(4) 0.012(3) C76 0.117(5) 0.084(4) 0.077(4) 0.016(4) 0.042(4) 0.032(4) C77 0.105(5) 0.072(4) 0.077(5) -0.001(3) 0.016(4) -0.004(3) C78 0.089(4) 0.065(3) 0.069(4) 0.008(3) 0.021(3) -0.003(3) C79 0.078(3) 0.045(3) 0.056(3) 0.005(2) 0.028(3) -0.003(2) C80 0.111(4) 0.052(3) 0.071(4) 0.003(3) 0.039(3) -0.002(3) C81 0.111(4) 0.080(4) 0.077(4) -0.006(3) 0.055(4) -0.017(3) C82 0.085(4) 0.065(4) 0.087(4) -0.010(3) 0.046(3) -0.006(3) C83 0.062(3) 0.060(3) 0.082(4) 0.007(3) 0.031(3) 0.003(3) C84 0.066(3) 0.059(3) 0.064(3) 0.002(3) 0.033(3) -0.007(3) O1 0.358(18) 0.266(12) 0.370(15) 0.007(11) 0.165(14) -0.100(12) C85 0.174(12) 0.333(19) 0.194(12) 0.094(12) 0.042(10) 0.016(13) C86 0.25(2) 0.36(3) 0.87(5) 0.11(4) 0.15(3) 0.02(2) C87 0.67(4) 0.095(10) 0.50(3) 0.095(14) 0.08(3) 0.013(17) _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 Cr1 S6 2.3863(12) . ? Cr1 S5 2.3921(12) . ? Cr1 S1 2.3923(13) . ? Cr1 S3 2.3944(13) . ? Cr1 S4 2.3989(13) . ? Cr1 S2 2.4009(13) . ? P1 C19 1.780(4) . ? P1 C13 1.784(4) . ? P1 C31 1.786(4) . ? P1 C25 1.791(4) . ? P2 C49 1.779(5) . ? P2 C37 1.778(5) . ? P2 C55 1.784(5) . ? P2 C43 1.793(5) . ? P3 C67 1.771(5) . ? P3 C73 1.772(4) . ? P3 C61 1.781(5) . ? P3 C79 1.777(5) . ? S1 C1 1.738(4) . ? S2 C2 1.736(4) . ? S3 C3 1.722(4) . ? S4 C4 1.737(4) . ? S5 C5 1.737(4) . ? S6 C6 1.732(4) . ? N1 C7 1.150(5) . ? N2 C8 1.145(5) . ? N3 C9 1.143(5) . ? N4 C10 1.136(5) . ? N5 C11 1.137(5) . ? N6 C12 1.138(5) . ? C1 C2 1.351(5) . ? C1 C7 1.437(6) . ? C2 C8 1.420(6) . ? C3 C4 1.361(5) . ? C3 C9 1.441(6) . ? C4 C10 1.437(6) . ? C5 C6 1.351(5) . ? C5 C11 1.438(6) . ? C6 C12 1.435(6) . ? C13 C18 1.373(5) . ? C13 C14 1.383(5) . ? C14 C15 1.379(6) . ? C15 C16 1.362(7) . ? C16 C17 1.374(6) . ? C17 C18 1.384(6) . ? C19 C24 1.379(5) . ? C19 C20 1.393(5) . ? C20 C21 1.368(6) . ? C21 C22 1.366(7) . ? C22 C23 1.370(7) . ? C23 C24 1.385(6) . ? C25 C26 1.378(6) . ? C25 C30 1.385(6) . ? C26 C27 1.366(6) . ? C27 C28 1.370(7) . ? C28 C29 1.358(7) . ? C29 C30 1.393(6) . ? C31 C32 1.385(5) . ? C31 C36 1.390(5) . ? C32 C33 1.383(6) . ? C33 C34 1.355(6) . ? C34 C35 1.376(6) . ? C35 C36 1.381(6) . ? C37 C38 1.372(7) . ? C37 C42 1.380(6) . ? C38 C39 1.375(8) . ? C39 C40 1.370(9) . ? C40 C41 1.365(9) . ? C41 C42 1.380(8) . ? C43 C44 1.386(6) . ? C43 C48 1.384(6) . ? C44 C45 1.378(7) . ? C45 C46 1.348(8) . ? C46 C47 1.358(7) . ? C47 C48 1.376(6) . ? C49 C50 1.384(6) . ? C49 C54 1.383(6) . ? C50 C51 1.398(7) . ? C51 C52 1.340(7) . ? C52 C53 1.347(7) . ? C53 C54 1.394(7) . ? C55 C56 1.378(6) . ? C55 C60 1.391(6) . ? C56 C57 1.387(6) . ? C57 C58 1.373(6) . ? C58 C59 1.370(7) . ? C59 C60 1.365(6) . ? C61 C62 1.347(7) . ? C61 C66 1.393(7) . ? C62 C63 1.407(9) . ? C63 C64 1.334(11) . ? C64 C65 1.376(11) . ? C65 C66 1.398(7) . ? C67 C68 1.382(7) . ? C67 C72 1.389(6) . ? C68 C69 1.381(8) . ? C69 C70 1.385(8) . ? C70 C71 1.361(9) . ? C71 C72 1.383(7) . ? C73 C74 1.382(5) . ? C73 C78 1.392(6) . ? C74 C75 1.378(6) . ? C75 C76 1.377(6) . ? C76 C77 1.359(7) . ? C77 C78 1.365(6) . ? C79 C84 1.380(5) . ? C79 C80 1.394(6) . ? C80 C81 1.381(6) . ? C81 C82 1.376(6) . ? C82 C83 1.363(6) . ? C83 C84 1.384(5) . ? O1 C86 1.288(12) . ? C85 C86 1.581(11) . ? C86 C87 1.571(11) . ? 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 S6 Cr1 S5 87.13(4) . . ? S6 Cr1 S1 172.42(5) . . ? S5 Cr1 S1 87.39(4) . . ? S6 Cr1 S3 87.51(4) . . ? S5 Cr1 S3 173.27(5) . . ? S1 Cr1 S3 98.31(4) . . ? S6 Cr1 S4 96.78(4) . . ? S5 Cr1 S4 90.42(4) . . ? S1 Cr1 S4 88.49(4) . . ? S3 Cr1 S4 86.18(4) . . ? S6 Cr1 S2 88.32(4) . . ? S5 Cr1 S2 93.71(5) . . ? S1 Cr1 S2 86.81(4) . . ? S3 Cr1 S2 90.19(4) . . ? S4 Cr1 S2 173.59(5) . . ? C19 P1 C13 107.5(2) . . ? C19 P1 C31 110.0(2) . . ? C13 P1 C31 109.3(2) . . ? C19 P1 C25 111.7(2) . . ? C13 P1 C25 109.4(2) . . ? C31 P1 C25 109.0(2) . . ? C49 P2 C37 108.2(3) . . ? C49 P2 C55 110.3(2) . . ? C37 P2 C55 109.4(3) . . ? C49 P2 C43 110.0(2) . . ? C37 P2 C43 109.2(2) . . ? C55 P2 C43 109.9(2) . . ? C67 P3 C73 105.9(2) . . ? C67 P3 C61 111.2(3) . . ? C73 P3 C61 110.9(2) . . ? C67 P3 C79 110.6(2) . . ? C73 P3 C79 111.1(2) . . ? C61 P3 C79 107.2(2) . . ? C1 S1 Cr1 101.86(16) . . ? C2 S2 Cr1 101.65(16) . . ? C3 S3 Cr1 103.32(15) . . ? C4 S4 Cr1 102.61(16) . . ? C5 S5 Cr1 102.00(16) . . ? C6 S6 Cr1 102.30(16) . . ? C2 C1 C7 119.7(4) . . ? C2 C1 S1 123.9(3) . . ? C7 C1 S1 116.3(3) . . ? C1 C2 C8 119.6(4) . . ? C1 C2 S2 124.1(4) . . ? C8 C2 S2 116.3(4) . . ? C4 C3 C9 119.0(4) . . ? C4 C3 S3 123.4(3) . . ? C9 C3 S3 117.7(3) . . ? C3 C4 C10 120.7(4) . . ? C3 C4 S4 123.8(3) . . ? C10 C4 S4 115.5(3) . . ? C6 C5 C11 120.0(4) . . ? C6 C5 S5 124.0(3) . . ? C11 C5 S5 116.0(3) . . ? C5 C6 C12 119.7(4) . . ? C5 C6 S6 124.1(3) . . ? C12 C6 S6 116.2(3) . . ? N1 C7 C1 178.9(6) . . ? N2 C8 C2 176.9(5) . . ? N3 C9 C3 177.5(5) . . ? N4 C10 C4 179.1(6) . . ? N5 C11 C5 179.0(6) . . ? N6 C12 C6 177.5(5) . . ? C18 C13 C14 119.4(4) . . ? C18 C13 P1 120.7(4) . . ? C14 C13 P1 119.5(4) . . ? C15 C14 C13 120.0(5) . . ? C16 C15 C14 120.1(5) . . ? C15 C16 C17 120.5(5) . . ? C16 C17 C18 119.5(5) . . ? C13 C18 C17 120.3(5) . . ? C24 C19 C20 118.5(4) . . ? C24 C19 P1 120.2(4) . . ? C20 C19 P1 120.9(4) . . ? C21 C20 C19 120.5(5) . . ? C20 C21 C22 120.4(5) . . ? C23 C22 C21 120.2(5) . . ? C22 C23 C24 119.8(5) . . ? C19 C24 C23 120.6(5) . . ? C26 C25 C30 118.1(4) . . ? C26 C25 P1 121.3(4) . . ? C30 C25 P1 120.6(4) . . ? C27 C26 C25 121.9(5) . . ? C26 C27 C28 119.5(5) . . ? C29 C28 C27 120.1(5) . . ? C28 C29 C30 120.5(6) . . ? C25 C30 C29 119.8(5) . . ? C32 C31 C36 119.4(4) . . ? C32 C31 P1 120.7(4) . . ? C36 C31 P1 119.9(3) . . ? C33 C32 C31 119.6(4) . . ? C34 C33 C32 121.0(5) . . ? C33 C34 C35 120.0(5) . . ? C34 C35 C36 120.2(5) . . ? C35 C36 C31 119.8(4) . . ? C38 C37 C42 119.9(5) . . ? C38 C37 P2 119.4(5) . . ? C42 C37 P2 120.6(5) . . ? C39 C38 C37 120.0(6) . . ? C38 C39 C40 120.2(7) . . ? C41 C40 C39 120.1(8) . . ? C40 C41 C42 120.2(7) . . ? C37 C42 C41 119.7(6) . . ? C44 C43 C48 119.3(5) . . ? C44 C43 P2 119.7(4) . . ? C48 C43 P2 121.0(4) . . ? C45 C44 C43 119.3(5) . . ? C46 C45 C44 120.4(6) . . ? C45 C46 C47 121.3(6) . . ? C46 C47 C48 119.6(6) . . ? C47 C48 C43 120.1(5) . . ? C50 C49 C54 118.3(5) . . ? C50 C49 P2 120.3(4) . . ? C54 C49 P2 121.3(4) . . ? C49 C50 C51 120.0(5) . . ? C52 C51 C50 120.6(6) . . ? C51 C52 C53 120.4(6) . . ? C52 C53 C54 120.8(6) . . ? C49 C54 C53 119.8(5) . . ? C56 C55 C60 118.9(5) . . ? C56 C55 P2 120.4(4) . . ? C60 C55 P2 120.8(4) . . ? C55 C56 C57 120.1(5) . . ? C58 C57 C56 120.1(5) . . ? C59 C58 C57 119.8(5) . . ? C60 C59 C58 120.5(5) . . ? C59 C60 C55 120.5(5) . . ? C62 C61 C66 118.5(6) . . ? C62 C61 P3 125.2(5) . . ? C66 C61 P3 116.1(4) . . ? C61 C62 C63 122.1(7) . . ? C64 C63 C62 117.1(10) . . ? C63 C64 C65 124.7(11) . . ? C64 C65 C66 116.4(9) . . ? C65 C66 C61 121.1(7) . . ? C68 C67 C72 119.3(5) . . ? C68 C67 P3 119.7(5) . . ? C72 C67 P3 120.7(5) . . ? C69 C68 C67 120.4(6) . . ? C68 C69 C70 120.0(7) . . ? C71 C70 C69 119.6(7) . . ? C70 C71 C72 121.2(7) . . ? C67 C72 C71 119.6(6) . . ? C74 C73 C78 118.8(4) . . ? C74 C73 P3 119.0(4) . . ? C78 C73 P3 122.2(4) . . ? C75 C74 C73 120.3(5) . . ? C74 C75 C76 119.6(5) . . ? C77 C76 C75 120.6(5) . . ? C76 C77 C78 120.2(5) . . ? C77 C78 C73 120.5(5) . . ? C84 C79 C80 118.3(4) . . ? C84 C79 P3 122.8(4) . . ? C80 C79 P3 118.9(4) . . ? C81 C80 C79 120.8(5) . . ? C82 C81 C80 119.7(5) . . ? C83 C82 C81 120.1(5) . . ? C82 C83 C84 120.5(5) . . ? C83 C84 C79 120.5(4) . . ? O1 C86 C87 138(2) . . ? O1 C86 C85 96.0(12) . . ? C87 C86 C85 123.8(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.384 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.043 #===END data_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H40 Cr N6 P2 S6' _chemical_formula_weight 1151.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.290(5) _cell_length_b 15.548(4) _cell_length_c 17.986(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5674(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 24.96 _exptl_crystal_description cubes _exptl_crystal_colour black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_type SADBAS _exptl_absorpt_correction_T_min 0.421591 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 AXS SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_reflns_number 38090 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.1510 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3720 _reflns_number_gt 1863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0644P)^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 3720 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1859 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 0.840 _refine_ls_restrained_S_all 0.840 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 Cr1 Cr 1.0000 1.66490(8) -0.2500 0.0818(5) Uani 1 2 d S . . S1 S 1.05414(8) 1.68193(10) -0.36360(11) 0.0884(6) Uani 1 1 d . . . S2 S 0.94315(9) 1.55570(11) -0.31089(11) 0.0967(6) Uani 1 1 d . . . S3 S 0.92418(8) 1.76682(10) -0.29774(11) 0.0863(6) Uani 1 1 d . . . N1 N 1.1732(3) 1.8199(4) -0.4634(4) 0.115(2) Uani 1 1 d . . . N2 N 0.7939(4) 1.9180(4) -0.2371(4) 0.136(3) Uani 1 1 d . . . N3 N 0.9365(4) 1.3215(5) -0.3362(6) 0.182(4) Uani 1 1 d . . . P1 P 0.86508(8) 1.83203(9) -0.59810(10) 0.0737(5) Uani 1 1 d . . . C1 C 1.1090(3) 1.7656(3) -0.3488(4) 0.0735(17) Uani 1 1 d . . . C2 C 1.1447(3) 1.7952(4) -0.4130(5) 0.088(2) Uani 1 1 d . . . C3 C 0.8806(3) 1.7987(4) -0.2184(4) 0.0761(18) Uani 1 1 d . . . C4 C 0.8318(4) 1.8663(4) -0.2307(4) 0.095(2) Uani 1 1 d . . . C5 C 0.9780(3) 1.4628(4) -0.2773(4) 0.089(2) Uani 1 1 d . . . C6 C 0.9546(4) 1.3837(5) -0.3106(6) 0.132(3) Uani 1 1 d . . . C13 C 0.8786(3) 1.7199(4) -0.5851(4) 0.0809(18) Uani 1 1 d . . . C14 C 0.9146(4) 1.6906(4) -0.5230(5) 0.115(3) Uani 1 1 d . . . H14A H 0.9315 1.7297 -0.4888 0.138 Uiso 1 1 calc R . . C15 C 0.9245(4) 1.6028(5) -0.5131(5) 0.123(3) Uani 1 1 d . . . H15A H 0.9480 1.5830 -0.4721 0.148 Uiso 1 1 calc R . . C16 C 0.9003(5) 1.5466(5) -0.5627(6) 0.121(3) Uani 1 1 d . . . H16A H 0.9079 1.4881 -0.5562 0.145 Uiso 1 1 calc R . . C17 C 0.8644(4) 1.5741(4) -0.6228(5) 0.111(3) Uani 1 1 d . . . H17A H 0.8471 1.5345 -0.6563 0.133 Uiso 1 1 calc R . . C18 C 0.8543(3) 1.6607(4) -0.6330(4) 0.090(2) Uani 1 1 d . . . H18A H 0.8300 1.6791 -0.6738 0.108 Uiso 1 1 calc R . . C19 C 0.8170(3) 1.8732(4) -0.5231(4) 0.0748(17) Uani 1 1 d . . . C20 C 0.7854(4) 1.8217(5) -0.4728(5) 0.115(3) Uani 1 1 d . . . H20A H 0.7923 1.7625 -0.4737 0.138 Uiso 1 1 calc R . . C21 C 0.7434(5) 1.8573(5) -0.4209(5) 0.141(3) Uani 1 1 d . . . H21A H 0.7207 1.8214 -0.3884 0.169 Uiso 1 1 calc R . . C22 C 0.7347(4) 1.9426(5) -0.4164(5) 0.118(3) Uani 1 1 d . . . H22A H 0.7083 1.9659 -0.3792 0.141 Uiso 1 1 calc R . . C23 C 0.7643(4) 1.9940(4) -0.4663(4) 0.098(2) Uani 1 1 d . . . H23A H 0.7563 2.0529 -0.4651 0.118 Uiso 1 1 calc R . . C24 C 0.8063(3) 1.9611(4) -0.5192(4) 0.094(2) Uani 1 1 d . . . H24A H 0.8275 1.9978 -0.5523 0.113 Uiso 1 1 calc R . . C25 C 0.9390(3) 1.8936(4) -0.6058(4) 0.0724(17) Uani 1 1 d . . . C26 C 0.9385(3) 1.9687(5) -0.6444(5) 0.112(3) Uani 1 1 d . . . H26A H 0.9006 1.9849 -0.6699 0.134 Uiso 1 1 calc R . . C27 C 0.9932(4) 2.0213(5) -0.6466(5) 0.117(3) Uani 1 1 d . . . H27A H 0.9915 2.0730 -0.6725 0.140 Uiso 1 1 calc R . . C28 C 1.0490(4) 1.9983(5) -0.6117(5) 0.103(2) Uani 1 1 d . . . H28A H 1.0860 2.0336 -0.6135 0.124 Uiso 1 1 calc R . . C29 C 1.0507(4) 1.9245(6) -0.5745(5) 0.124(3) Uani 1 1 d . . . H29A H 1.0893 1.9087 -0.5502 0.148 Uiso 1 1 calc R . . C30 C 0.9973(4) 1.8712(5) -0.5710(5) 0.111(3) Uani 1 1 d . . . H30A H 1.0001 1.8195 -0.5452 0.134 Uiso 1 1 calc R . . C31 C 0.8183(3) 1.8451(3) -0.6816(4) 0.0675(17) Uani 1 1 d . . . C32 C 0.7529(3) 1.8641(4) -0.6783(4) 0.0810(19) Uani 1 1 d . . . H32A H 0.7328 1.8729 -0.6324 0.097 Uiso 1 1 calc R . . C33 C 0.7160(4) 1.8705(4) -0.7426(6) 0.091(2) Uani 1 1 d . . . H33A H 0.6714 1.8841 -0.7403 0.109 Uiso 1 1 calc R . . C34 C 0.7464(5) 1.8566(4) -0.8110(5) 0.097(2) Uani 1 1 d . . . H34A H 0.7220 1.8603 -0.8546 0.117 Uiso 1 1 calc R . . C35 C 0.8112(5) 1.8376(5) -0.8141(4) 0.101(2) Uani 1 1 d . . . H35A H 0.8308 1.8277 -0.8600 0.121 Uiso 1 1 calc R . . C36 C 0.8489(3) 1.8327(4) -0.7501(5) 0.090(2) Uani 1 1 d . . . H36A H 0.8938 1.8213 -0.7528 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0788(10) 0.0616(9) 0.1052(13) 0.000 0.0100(8) 0.000 S1 0.0819(12) 0.0744(11) 0.1089(15) -0.0110(9) 0.0130(10) -0.0102(9) S2 0.0872(12) 0.0742(12) 0.1286(17) -0.0034(10) 0.0136(11) -0.0176(9) S3 0.0882(12) 0.0637(10) 0.1072(15) 0.0089(9) 0.0050(10) -0.0027(9) N1 0.120(5) 0.100(5) 0.126(6) 0.032(4) 0.025(4) -0.007(4) N2 0.155(7) 0.092(5) 0.160(7) 0.004(4) -0.013(5) 0.048(5) N3 0.177(8) 0.096(6) 0.272(11) -0.044(6) 0.065(7) -0.045(5) P1 0.0748(11) 0.0557(10) 0.0906(13) 0.0006(8) -0.0047(10) -0.0035(8) C1 0.070(4) 0.050(4) 0.100(6) 0.003(4) -0.001(4) 0.004(3) C2 0.080(5) 0.059(4) 0.124(7) 0.023(4) 0.006(5) 0.006(4) C3 0.067(4) 0.048(4) 0.113(6) -0.011(4) -0.001(4) -0.009(3) C4 0.103(6) 0.059(4) 0.123(6) -0.006(4) -0.023(5) 0.004(4) C5 0.087(6) 0.065(4) 0.116(7) -0.007(4) 0.037(4) -0.008(3) C6 0.137(7) 0.071(5) 0.187(10) -0.020(6) 0.044(6) -0.017(5) C13 0.088(5) 0.057(4) 0.098(5) 0.003(4) -0.002(4) -0.003(3) C14 0.152(7) 0.065(5) 0.128(7) 0.006(4) -0.038(6) 0.000(4) C15 0.167(8) 0.075(5) 0.129(8) 0.018(5) -0.028(6) 0.013(5) C16 0.153(8) 0.062(5) 0.147(9) 0.018(6) 0.013(7) 0.025(5) C17 0.130(7) 0.057(5) 0.146(8) -0.013(5) 0.018(6) -0.005(4) C18 0.103(5) 0.061(4) 0.105(6) -0.006(4) 0.000(4) -0.009(4) C19 0.081(4) 0.062(4) 0.082(5) 0.006(3) -0.003(4) -0.006(3) C20 0.162(8) 0.073(5) 0.110(6) 0.000(5) 0.030(6) 0.004(5) C21 0.214(10) 0.079(6) 0.129(8) 0.003(5) 0.069(7) -0.003(6) C22 0.153(7) 0.081(5) 0.120(7) -0.012(5) 0.048(6) -0.009(5) C23 0.117(6) 0.062(4) 0.115(6) -0.021(4) 0.020(5) -0.001(4) C24 0.114(6) 0.068(5) 0.101(6) -0.001(4) 0.007(5) -0.011(4) C25 0.071(4) 0.059(4) 0.087(5) 0.005(3) -0.010(3) 0.005(3) C26 0.072(5) 0.092(5) 0.170(8) 0.048(5) -0.024(5) -0.020(4) C27 0.077(5) 0.096(5) 0.178(8) 0.034(6) -0.006(5) -0.011(5) C28 0.071(5) 0.099(6) 0.139(7) 0.009(5) 0.006(5) -0.009(4) C29 0.068(5) 0.129(7) 0.174(9) 0.039(6) -0.024(5) -0.012(5) C30 0.092(6) 0.097(5) 0.144(7) 0.030(5) -0.009(5) -0.007(5) C31 0.067(4) 0.050(3) 0.086(5) 0.001(3) 0.002(4) -0.006(3) C32 0.079(5) 0.059(4) 0.105(6) 0.006(3) -0.007(4) -0.003(3) C33 0.081(5) 0.063(4) 0.129(7) 0.008(4) -0.019(6) -0.018(4) C34 0.113(7) 0.070(5) 0.108(7) 0.016(4) -0.031(6) -0.019(5) C35 0.117(7) 0.104(6) 0.081(6) 0.004(4) 0.001(5) -0.012(5) C36 0.093(5) 0.075(5) 0.103(6) 0.000(4) -0.010(5) -0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 S2 2.327(2) . ? Cr1 S2 2.327(2) 3_754 ? Cr1 S1 2.3348(19) . ? Cr1 S1 2.3349(19) 3_754 ? Cr1 S3 2.3695(19) . ? Cr1 S3 2.3696(19) 3_754 ? S1 C1 1.732(6) . ? S2 C5 1.718(6) . ? S3 C3 1.750(7) . ? N1 C2 1.141(8) . ? N2 C4 1.118(8) . ? N3 C6 1.133(9) . ? P1 C13 1.781(6) . ? P1 C25 1.785(6) . ? P1 C19 1.784(7) . ? P1 C31 1.789(6) . ? C1 C3 1.331(8) 3_754 ? C1 C2 1.440(10) . ? C3 C1 1.331(8) 3_754 ? C3 C4 1.461(10) . ? C5 C5 1.328(13) 3_754 ? C5 C6 1.447(10) . ? C13 C18 1.354(8) . ? C13 C14 1.409(9) . ? C14 C15 1.391(9) . ? C15 C16 1.342(11) . ? C16 C17 1.371(10) . ? C17 C18 1.375(8) . ? C19 C20 1.367(9) . ? C19 C24 1.385(8) . ? C20 C21 1.381(10) . ? C21 C22 1.340(9) . ? C22 C23 1.344(9) . ? C23 C24 1.376(9) . ? C25 C26 1.358(8) . ? C25 C30 1.382(8) . ? C26 C27 1.380(8) . ? C27 C28 1.342(9) . ? C28 C29 1.329(9) . ? C29 C30 1.366(9) . ? C31 C32 1.362(8) . ? C31 C36 1.393(9) . ? C32 C33 1.381(9) . ? C33 C34 1.393(9) . ? C34 C35 1.347(10) . ? C35 C36 1.384(9) . ? 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 Cr1 S2 86.26(11) . 3_754 ? S2 Cr1 S1 84.50(6) . . ? S2 Cr1 S1 105.15(7) 3_754 . ? S2 Cr1 S1 105.15(7) . 3_754 ? S2 Cr1 S1 84.50(7) 3_754 3_754 ? S1 Cr1 S1 166.98(10) . 3_754 ? S2 Cr1 S3 89.75(7) . . ? S2 Cr1 S3 168.66(6) 3_754 . ? S1 Cr1 S3 84.98(7) . . ? S1 Cr1 S3 86.32(7) 3_754 . ? S2 Cr1 S3 168.67(6) . 3_754 ? S2 Cr1 S3 89.75(7) 3_754 3_754 ? S1 Cr1 S3 86.32(7) . 3_754 ? S1 Cr1 S3 84.98(7) 3_754 3_754 ? S3 Cr1 S3 96.06(9) . 3_754 ? C1 S1 Cr1 104.6(3) . . ? C5 S2 Cr1 104.1(2) . . ? C3 S3 Cr1 102.8(2) . . ? C13 P1 C25 113.9(3) . . ? C13 P1 C19 109.7(3) . . ? C25 P1 C19 109.0(3) . . ? C13 P1 C31 107.7(3) . . ? C25 P1 C31 108.7(3) . . ? C19 P1 C31 107.7(3) . . ? C3 C1 C2 121.7(6) 3_754 . ? C3 C1 S1 122.2(6) 3_754 . ? C2 C1 S1 116.1(5) . . ? N1 C2 C1 178.9(8) . . ? C1 C3 C4 121.6(6) 3_754 . ? C1 C3 S3 123.4(5) 3_754 . ? C4 C3 S3 115.0(6) . . ? N2 C4 C3 177.2(9) . . ? C5 C5 C6 121.8(5) 3_754 . ? C5 C5 S2 122.5(2) 3_754 . ? C6 C5 S2 115.7(6) . . ? N3 C6 C5 179.4(13) . . ? C18 C13 C14 118.3(6) . . ? C18 C13 P1 121.7(6) . . ? C14 C13 P1 120.0(5) . . ? C15 C14 C13 119.5(7) . . ? C16 C15 C14 120.1(8) . . ? C15 C16 C17 121.0(7) . . ? C18 C17 C16 119.4(8) . . ? C13 C18 C17 121.7(7) . . ? C20 C19 C24 118.2(6) . . ? C20 C19 P1 123.1(5) . . ? C24 C19 P1 118.5(5) . . ? C19 C20 C21 120.1(7) . . ? C22 C21 C20 121.3(8) . . ? C21 C22 C23 119.3(7) . . ? C22 C23 C24 121.1(7) . . ? C23 C24 C19 119.9(6) . . ? C26 C25 C30 117.1(6) . . ? C26 C25 P1 119.6(5) . . ? C30 C25 P1 123.3(5) . . ? C25 C26 C27 121.2(7) . . ? C28 C27 C26 120.5(7) . . ? C29 C28 C27 119.1(7) . . ? C28 C29 C30 121.8(7) . . ? C29 C30 C25 120.3(7) . . ? C32 C31 C36 120.2(6) . . ? C32 C31 P1 120.4(6) . . ? C36 C31 P1 119.4(5) . . ? C31 C32 C33 120.5(7) . . ? C32 C33 C34 119.2(7) . . ? C35 C34 C33 120.2(7) . . ? C34 C35 C36 121.1(8) . . ? C35 C36 C31 118.7(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.327 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.057 #===END