# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2205 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Mark Thornton-Pett' _publ_contact_author_address ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_phone '+44 (0)113 2336423' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email marktp@chem.leeds.ac.uk _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_contact_letter ; The following set of data is for the cluster-compound included M/S B006329K ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Sterically Hindered Iminophosphorane Complexes of Vanadium, Iron, Cobalt and Nickel: A Synthetic, Structural and Catalytic Study ; loop_ _publ_author_name _publ_author_address 'Manfred Bochmann' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Sara Al-Benna' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mark Sarsfield' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; #================================================================= data_sab9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77.50 H71 Cl11 Co2 N4 P4' _chemical_formula_weight 1690.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5550(8) _cell_length_b 15.5053(7) _cell_length_c 18.2403(9) _cell_angle_alpha 89.686(3) _cell_angle_beta 68.223(2) _cell_angle_gamma 85.079(3) _cell_volume 3807.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37726 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 30.72 _exptl_crystal_description prism _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1730 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7255 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47456 _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.63 _reflns_number_total 14209 _reflns_number_gt 9685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0748P)^2^+21.0890P] 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 0.0056(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 14209 _refine_ls_number_parameters 911 _refine_ls_number_restraints 1126 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.2434 _refine_ls_wR_factor_gt 0.2222 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 1.064 _refine_ls_shift/su_mean 0.017 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 -0.00310(8) 0.72016(6) 0.07509(6) 0.0354(3) Uani 1 1 d . . . Cl1 Cl 0.00276(14) 0.79737(11) 0.17855(11) 0.0387(4) Uani 1 1 d . . . Cl2 Cl -0.00546(15) 0.57405(12) 0.08729(11) 0.0402(4) Uani 1 1 d . . . N1 N 0.1197(4) 0.7418(4) -0.0202(3) 0.0386(15) Uani 1 1 d D . . C11 C 0.2131(5) 0.7370(4) -0.0095(4) 0.0371(17) Uani 1 1 d D . . C12 C 0.2256(5) 0.6871(5) 0.0501(4) 0.0418(18) Uani 1 1 d D . . H12 H 0.1728 0.6558 0.0828 0.050 Uiso 1 1 calc R . . C13 C 0.3144(6) 0.6825(5) 0.0624(5) 0.048(2) Uani 1 1 d D . . H13 H 0.3211 0.6492 0.1043 0.058 Uiso 1 1 calc R . . C14 C 0.3932(6) 0.7257(5) 0.0146(5) 0.049(2) Uani 1 1 d D . . H14 H 0.4541 0.7220 0.0229 0.059 Uiso 1 1 calc R . . C15 C 0.3814(6) 0.7746(5) -0.0455(5) 0.046(2) Uani 1 1 d D . . H15 H 0.4348 0.8051 -0.0785 0.056 Uiso 1 1 calc R . . C16 C 0.2930(5) 0.7798(5) -0.0584(4) 0.0384(17) Uani 1 1 d D . . H16 H 0.2869 0.8125 -0.1008 0.046 Uiso 1 1 calc R . . P1 P 0.11931(15) 0.73847(12) -0.10809(11) 0.0349(4) Uani 1 1 d D . . C111 C 0.2108(5) 0.6583(4) -0.1706(4) 0.0367(17) Uani 1 1 d D . . C112 C 0.2014(6) 0.5717(5) -0.1464(5) 0.046(2) Uani 1 1 d D . . H112 H 0.1493 0.5586 -0.0990 0.056 Uiso 1 1 calc R . . C113 C 0.2689(6) 0.5055(5) -0.1924(5) 0.048(2) Uani 1 1 d D . . H113 H 0.2632 0.4473 -0.1760 0.057 Uiso 1 1 calc R . . C114 C 0.3441(6) 0.5245(5) -0.2618(5) 0.053(2) Uani 1 1 d D . . H114 H 0.3886 0.4790 -0.2936 0.064 Uiso 1 1 calc R . . C115 C 0.3551(7) 0.6087(5) -0.2853(5) 0.058(2) Uani 1 1 d D . . H115 H 0.4076 0.6211 -0.3327 0.069 Uiso 1 1 calc R . . C116 C 0.2888(5) 0.6763(5) -0.2394(4) 0.0453(19) Uani 1 1 d D . . H116 H 0.2973 0.7345 -0.2552 0.054 Uiso 1 1 calc R . . C121 C 0.1262(4) 0.8400(4) -0.1573(4) 0.0359(16) Uani 1 1 d D . . C122 C 0.1374(6) 0.8436(5) -0.2370(4) 0.0417(18) Uani 1 1 d D . . H122 H 0.1450 0.7916 -0.2668 0.050 Uiso 1 1 calc R . . C123 C 0.1373(6) 0.9228(4) -0.2720(4) 0.0421(18) Uani 1 1 d D . . H123 H 0.1433 0.9254 -0.3256 0.051 Uiso 1 1 calc R . . C124 C 0.1286(6) 0.9983(5) -0.2292(4) 0.048(2) Uani 1 1 d D . . H124 H 0.1309 1.0525 -0.2540 0.058 Uiso 1 1 calc R . . C125 C 0.1167(7) 0.9954(5) -0.1512(5) 0.054(2) Uani 1 1 d D . . H125 H 0.1087 1.0477 -0.1217 0.065 Uiso 1 1 calc R . . C126 C 0.1164(6) 0.9164(4) -0.1147(4) 0.047(2) Uani 1 1 d D . . H126 H 0.1094 0.9147 -0.0609 0.057 Uiso 1 1 calc R . . C1 C 0.0029(5) 0.6998(5) -0.1017(4) 0.0358(16) Uani 1 1 d . . . H1A H 0.0030 0.6397 -0.0832 0.043 Uiso 1 1 calc R . . H1B H 0.0043 0.6964 -0.1563 0.043 Uiso 1 1 calc R . . P2 P -0.11642(15) 0.75568(12) -0.04150(11) 0.0354(4) Uani 1 1 d D . . C211 C -0.1310(4) 0.8589(4) -0.0831(4) 0.0364(17) Uani 1 1 d D . . C212 C -0.1151(5) 0.8661(4) -0.1636(4) 0.0388(17) Uani 1 1 d D . . H212 H -0.0974 0.8159 -0.1973 0.047 Uiso 1 1 calc R . . C213 C -0.1253(6) 0.9470(5) -0.1934(5) 0.0452(19) Uani 1 1 d D . . H213 H -0.1128 0.9524 -0.2481 0.054 Uiso 1 1 calc R . . C214 C -0.1537(6) 1.0205(5) -0.1444(5) 0.049(2) Uani 1 1 d D . . H214 H -0.1620 1.0756 -0.1653 0.059 Uiso 1 1 calc R . . C215 C -0.1697(7) 1.0135(5) -0.0656(5) 0.052(2) Uani 1 1 d D . . H215 H -0.1883 1.0639 -0.0322 0.062 Uiso 1 1 calc R . . C216 C -0.1588(6) 0.9330(4) -0.0345(5) 0.047(2) Uani 1 1 d D . . H216 H -0.1703 0.9285 0.0201 0.057 Uiso 1 1 calc R . . C221 C -0.2027(5) 0.6847(4) -0.0514(3) 0.0360(16) Uani 1 1 d D . . C222 C -0.2672(5) 0.7068(5) -0.0904(4) 0.0437(19) Uani 1 1 d D . . H222 H -0.2664 0.7614 -0.1143 0.052 Uiso 1 1 calc R . . C223 C -0.3333(7) 0.6479(5) -0.0941(6) 0.056(2) Uani 1 1 d D . . H223 H -0.3771 0.6624 -0.1210 0.067 Uiso 1 1 calc R . . C224 C -0.3347(7) 0.5692(6) -0.0590(6) 0.062(3) Uani 1 1 d D . . H224 H -0.3797 0.5294 -0.0613 0.075 Uiso 1 1 calc R . . C225 C -0.2705(7) 0.5477(6) -0.0200(6) 0.061(3) Uani 1 1 d D . . H225 H -0.2719 0.4933 0.0045 0.073 Uiso 1 1 calc R . . C226 C -0.2048(6) 0.6047(5) -0.0168(5) 0.051(2) Uani 1 1 d D . . H226 H -0.1605 0.5892 0.0093 0.062 Uiso 1 1 calc R . . N2 N -0.1237(4) 0.7610(4) 0.0489(3) 0.0363(14) Uani 1 1 d D . . C21 C -0.2207(5) 0.7688(4) 0.1103(4) 0.0400(18) Uani 1 1 d D . . C22 C -0.3064(5) 0.8050(6) 0.0996(5) 0.052(2) Uani 1 1 d D . . H22 H -0.3008 0.8283 0.0500 0.063 Uiso 1 1 calc R . . C23 C -0.3993(6) 0.8073(7) 0.1602(5) 0.061(3) Uani 1 1 d D . . H23 H -0.4569 0.8297 0.1512 0.074 Uiso 1 1 calc R . . C24 C -0.4074(6) 0.7772(7) 0.2330(5) 0.066(3) Uani 1 1 d D . . H24 H -0.4707 0.7804 0.2747 0.079 Uiso 1 1 calc R . . C25 C -0.3249(6) 0.7425(6) 0.2459(5) 0.056(2) Uani 1 1 d D . . H25 H -0.3312 0.7210 0.2963 0.067 Uiso 1 1 calc R . . C26 C -0.2319(6) 0.7388(5) 0.1852(4) 0.046(2) Uani 1 1 d D . . H26 H -0.1750 0.7156 0.1948 0.055 Uiso 1 1 calc R . . Co2 Co -0.00621(8) 0.21774(7) 0.42746(6) 0.0374(3) Uani 1 1 d . . . Cl3 Cl -0.00265(15) 0.07164(12) 0.41467(11) 0.0426(5) Uani 1 1 d . . . Cl4 Cl -0.00340(15) 0.29659(12) 0.32107(11) 0.0411(5) Uani 1 1 d . . . N3 N 0.1132(4) 0.2440(4) 0.4529(3) 0.0371(14) Uani 1 1 d D . . C31 C 0.2084(5) 0.2416(4) 0.3881(4) 0.0376(17) Uani 1 1 d D . . C32 C 0.2850(5) 0.2871(5) 0.3939(5) 0.0463(19) Uani 1 1 d D . . H32 H 0.2743 0.3196 0.4408 0.056 Uiso 1 1 calc R . . C33 C 0.3758(6) 0.2848(6) 0.3319(5) 0.058(2) Uani 1 1 d D . . H33 H 0.4271 0.3156 0.3365 0.070 Uiso 1 1 calc R . . C34 C 0.3923(7) 0.2384(6) 0.2638(5) 0.059(2) Uani 1 1 d D . . H34 H 0.4547 0.2371 0.2213 0.071 Uiso 1 1 calc R . . C35 C 0.3171(6) 0.1931(6) 0.2573(4) 0.052(2) Uani 1 1 d D . . H35 H 0.3277 0.1608 0.2104 0.062 Uiso 1 1 calc R . . C36 C 0.2262(6) 0.1957(5) 0.3202(4) 0.046(2) Uani 1 1 d D . . H36 H 0.1751 0.1645 0.3156 0.055 Uiso 1 1 calc R . . P3 P 0.11161(15) 0.23613(12) 0.54100(11) 0.0354(4) Uani 1 1 d D . . C311 C 0.2080(5) 0.1566(4) 0.5442(3) 0.0352(16) Uani 1 1 d D . . C312 C 0.2020(6) 0.0713(4) 0.5219(4) 0.0437(19) Uani 1 1 d D . . H312 H 0.1483 0.0579 0.5077 0.052 Uiso 1 1 calc R . . C313 C 0.2743(6) 0.0071(5) 0.5208(5) 0.050(2) Uani 1 1 d D . . H313 H 0.2699 -0.0506 0.5060 0.059 Uiso 1 1 calc R . . C314 C 0.3527(6) 0.0260(5) 0.5410(5) 0.053(2) Uani 1 1 d D . . H314 H 0.4022 -0.0186 0.5400 0.064 Uiso 1 1 calc R . . C315 C 0.3595(6) 0.1098(5) 0.5628(6) 0.057(2) Uani 1 1 d D . . H315 H 0.4141 0.1227 0.5762 0.069 Uiso 1 1 calc R . . C316 C 0.2866(6) 0.1754(5) 0.5652(5) 0.048(2) Uani 1 1 d D . . H316 H 0.2907 0.2327 0.5812 0.058 Uiso 1 1 calc R . . C321 C 0.1163(4) 0.3364(4) 0.5880(4) 0.0373(17) Uani 1 1 d D . . C322 C 0.1305(6) 0.3380(5) 0.6598(4) 0.0430(19) Uani 1 1 d D . . H322 H 0.1393 0.2852 0.6841 0.052 Uiso 1 1 calc R . . C323 C 0.1318(6) 0.4163(5) 0.6957(5) 0.047(2) Uani 1 1 d D . . H323 H 0.1414 0.4176 0.7444 0.056 Uiso 1 1 calc R . . C324 C 0.1188(7) 0.4923(5) 0.6594(5) 0.051(2) Uani 1 1 d D . . H324 H 0.1214 0.5460 0.6831 0.062 Uiso 1 1 calc R . . C325 C 0.1023(7) 0.4921(5) 0.5906(5) 0.053(2) Uani 1 1 d D . . H325 H 0.0899 0.5454 0.5685 0.064 Uiso 1 1 calc R . . C326 C 0.1035(6) 0.4141(4) 0.5524(4) 0.0441(19) Uani 1 1 d D . . H326 H 0.0956 0.4138 0.5029 0.053 Uiso 1 1 calc R . . C3 C -0.0037(5) 0.1944(5) 0.6027(4) 0.0352(16) Uani 1 1 d . . . H3A H -0.0031 0.1909 0.6567 0.042 Uiso 1 1 calc R . . H3B H -0.0017 0.1342 0.5839 0.042 Uiso 1 1 calc R . . P4 P -0.12356(15) 0.24847(13) 0.61142(11) 0.0372(5) Uani 1 1 d D . . C411 C -0.2094(5) 0.1780(4) 0.6745(4) 0.0361(17) Uani 1 1 d D . . C412 C -0.2136(6) 0.0981(5) 0.6425(5) 0.0453(19) Uani 1 1 d D . . H412 H -0.1708 0.0821 0.5899 0.054 Uiso 1 1 calc R . . C413 C -0.2803(6) 0.0417(5) 0.6871(5) 0.050(2) Uani 1 1 d D . . H413 H -0.2848 -0.0121 0.6646 0.060 Uiso 1 1 calc R . . C414 C -0.3399(6) 0.0640(5) 0.7641(5) 0.049(2) Uani 1 1 d D . . H414 H -0.3853 0.0251 0.7948 0.059 Uiso 1 1 calc R . . C415 C -0.3343(6) 0.1417(5) 0.7967(5) 0.049(2) Uani 1 1 d D . . H415 H -0.3750 0.1558 0.8502 0.059 Uiso 1 1 calc R . . C416 C -0.2697(5) 0.2001(5) 0.7525(4) 0.0433(19) Uani 1 1 d D . . H416 H -0.2667 0.2543 0.7752 0.052 Uiso 1 1 calc R . . C421 C -0.1381(4) 0.3524(4) 0.6585(4) 0.0391(17) Uani 1 1 d D . . C422 C -0.1672(6) 0.4254(4) 0.6249(5) 0.0456(19) Uani 1 1 d D . . H422 H -0.1802 0.4194 0.5779 0.055 Uiso 1 1 calc R . . C423 C -0.1774(7) 0.5067(5) 0.6595(5) 0.052(2) Uani 1 1 d D . . H423 H -0.1963 0.5563 0.6359 0.062 Uiso 1 1 calc R . . C424 C -0.1602(7) 0.5155(5) 0.7279(5) 0.051(2) Uani 1 1 d D . . H424 H -0.1689 0.5714 0.7520 0.061 Uiso 1 1 calc R . . C425 C -0.1303(6) 0.4445(5) 0.7623(4) 0.0449(19) Uani 1 1 d D . . H425 H -0.1165 0.4517 0.8088 0.054 Uiso 1 1 calc R . . C426 C -0.1207(6) 0.3626(4) 0.7286(4) 0.0393(17) Uani 1 1 d D . . H426 H -0.1022 0.3134 0.7529 0.047 Uiso 1 1 calc R . . N4 N -0.1299(5) 0.2524(4) 0.5249(4) 0.0401(15) Uani 1 1 d D . . C41 C -0.2252(5) 0.2556(4) 0.5183(4) 0.0422(19) Uani 1 1 d D . . C42 C -0.2317(6) 0.2232(5) 0.4503(5) 0.048(2) Uani 1 1 d D . . H42 H -0.1725 0.2008 0.4088 0.057 Uiso 1 1 calc R . . C43 C -0.3217(6) 0.2222(6) 0.4402(5) 0.053(2) Uani 1 1 d D . . H43 H -0.3237 0.1987 0.3929 0.063 Uiso 1 1 calc R . . C44 C -0.4085(6) 0.2558(6) 0.4998(5) 0.060(3) Uani 1 1 d D . . H44 H -0.4703 0.2566 0.4932 0.072 Uiso 1 1 calc R . . C45 C -0.4044(6) 0.2879(6) 0.5685(5) 0.057(2) Uani 1 1 d D . . H45 H -0.4639 0.3098 0.6098 0.069 Uiso 1 1 calc R . . C46 C -0.3139(6) 0.2886(6) 0.5781(5) 0.054(2) Uani 1 1 d D . . H46 H -0.3123 0.3116 0.6257 0.065 Uiso 1 1 calc R . . C1AS C 0.3609(12) 0.5120(8) 0.5171(7) 0.059(4) Uani 0.50 1 d PDU A 1 H1AS H 0.2905 0.5349 0.5433 0.071 Uiso 0.50 1 calc PR A 1 H1AS H 0.4035 0.5548 0.5247 0.071 Uiso 0.50 1 calc PR A 1 C1BS C 0.4508(17) 0.4830(15) 0.4876(11) 0.136(9) Uani 0.50 1 d PDU A 2 H1BS H 0.5210 0.4595 0.4618 0.163 Uiso 0.50 1 calc PR A 2 H1BS H 0.4483 0.5401 0.5126 0.163 Uiso 0.50 1 calc PR A 2 Cl1S Cl 0.3893(3) 0.4916(3) 0.4168(3) 0.1193(13) Uani 1 1 d DU . . Cl2S Cl 0.3830(4) 0.4121(3) 0.5563(3) 0.1287(14) Uani 1 1 d DU . . C2AS C 0.4370(11) 0.4927(8) 0.2079(8) 0.068(4) Uani 0.50 1 d PDU B 1 H2AS H 0.3731 0.4825 0.2034 0.082 Uiso 0.50 1 calc PR B 1 H2AS H 0.4363 0.4692 0.2586 0.082 Uiso 0.50 1 calc PR B 1 C2BS C 0.5361(14) 0.5497(8) 0.1293(11) 0.092(6) Uani 0.50 1 d PDU B 2 H2BS H 0.6017 0.5645 0.1275 0.110 Uiso 0.50 1 calc PR B 2 H2BS H 0.5276 0.5714 0.0809 0.110 Uiso 0.50 1 calc PR B 2 Cl3S Cl 0.4468(4) 0.6002(3) 0.2087(3) 0.151(2) Uani 1 1 d DU . . Cl4S Cl 0.5347(2) 0.43686(19) 0.1298(2) 0.0814(9) Uani 1 1 d DU . . C3S C 0.6088(9) 0.0088(9) 0.2599(6) 0.099(4) Uani 1 1 d DU . . H3SA H 0.6134 -0.0552 0.2617 0.118 Uiso 1 1 calc R . . H3SB H 0.6697 0.0284 0.2641 0.118 Uiso 1 1 calc R . . Cl5S Cl 0.6027(3) 0.0402(2) 0.1700(2) 0.1065(12) Uani 1 1 d DU . . Cl6S Cl 0.5068(4) 0.0510(5) 0.3392(3) 0.195(3) Uani 1 1 d DU . . C4S C 0.4442(11) -0.0286(9) 0.0072(15) 0.090(7) Uani 0.50 1 d PDU . . H4S1 H 0.4142 -0.0369 -0.0326 0.108 Uiso 0.50 1 calc PR . . H4S2 H 0.4048 -0.0580 0.0555 0.108 Uiso 0.50 1 calc PR . . Cl7S Cl 0.4342(3) 0.0795(2) 0.0290(2) 0.1056(11) Uani 1 1 d DU . . 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 0.0419(6) 0.0370(6) 0.0314(5) 0.0048(4) -0.0177(5) -0.0059(4) Cl1 0.0520(11) 0.0353(9) 0.0343(10) 0.0017(7) -0.0220(8) -0.0068(8) Cl2 0.0492(11) 0.0357(9) 0.0403(10) 0.0027(8) -0.0210(9) -0.0077(8) N1 0.046(4) 0.045(4) 0.028(3) 0.006(3) -0.016(3) -0.009(3) C11 0.041(4) 0.037(4) 0.039(4) -0.002(3) -0.022(4) -0.002(3) C12 0.044(5) 0.051(5) 0.035(4) 0.001(3) -0.020(4) -0.008(4) C13 0.051(5) 0.054(5) 0.045(5) 0.003(4) -0.025(4) 0.000(4) C14 0.045(5) 0.058(5) 0.048(5) -0.007(4) -0.022(4) 0.000(4) C15 0.042(5) 0.053(5) 0.046(5) 0.001(4) -0.015(4) -0.015(4) C16 0.041(4) 0.043(4) 0.035(4) -0.002(3) -0.017(3) -0.010(3) P1 0.0433(11) 0.0356(10) 0.0301(10) 0.0037(8) -0.0178(9) -0.0083(8) C111 0.040(4) 0.035(4) 0.042(4) 0.002(3) -0.022(4) -0.005(3) C112 0.052(5) 0.052(5) 0.041(5) -0.001(4) -0.022(4) -0.011(4) C113 0.051(5) 0.043(5) 0.059(6) -0.006(4) -0.032(4) -0.004(4) C114 0.045(5) 0.055(5) 0.061(6) -0.009(4) -0.023(4) 0.003(4) C115 0.056(6) 0.065(6) 0.047(5) 0.001(4) -0.015(4) 0.001(5) C116 0.046(5) 0.046(5) 0.046(5) 0.004(4) -0.020(4) -0.002(4) C121 0.044(4) 0.032(4) 0.037(4) 0.004(3) -0.019(3) -0.009(3) C122 0.057(5) 0.040(4) 0.030(4) 0.004(3) -0.018(4) -0.009(4) C123 0.041(4) 0.044(4) 0.043(5) 0.002(4) -0.019(4) -0.002(3) C124 0.052(5) 0.054(5) 0.043(5) 0.008(4) -0.022(4) -0.006(4) C125 0.079(6) 0.032(4) 0.066(6) 0.002(4) -0.044(5) -0.005(4) C126 0.066(6) 0.049(5) 0.036(4) -0.002(4) -0.029(4) -0.004(4) C1 0.041(4) 0.038(4) 0.033(4) 0.005(3) -0.019(3) -0.005(3) P2 0.0425(11) 0.0361(10) 0.0331(10) 0.0034(8) -0.0200(9) -0.0055(8) C211 0.042(4) 0.032(4) 0.040(4) 0.003(3) -0.020(3) -0.008(3) C212 0.044(4) 0.039(4) 0.036(4) 0.000(3) -0.019(4) -0.001(3) C213 0.054(5) 0.051(5) 0.039(4) 0.010(4) -0.025(4) -0.014(4) C214 0.053(5) 0.038(4) 0.062(6) 0.013(4) -0.028(4) -0.007(4) C215 0.068(6) 0.035(4) 0.060(6) -0.010(4) -0.032(5) -0.001(4) C216 0.057(5) 0.047(5) 0.044(5) -0.001(4) -0.028(4) 0.005(4) C221 0.044(4) 0.036(4) 0.031(4) 0.000(3) -0.017(3) -0.005(3) C222 0.046(5) 0.050(5) 0.043(5) 0.006(4) -0.025(4) -0.008(4) C223 0.060(6) 0.060(6) 0.070(6) 0.008(5) -0.047(5) -0.015(4) C224 0.068(6) 0.059(6) 0.078(7) 0.018(5) -0.044(6) -0.031(5) C225 0.068(6) 0.057(6) 0.073(7) 0.024(5) -0.040(5) -0.020(5) C226 0.060(6) 0.050(5) 0.057(6) 0.010(4) -0.036(5) -0.007(4) N2 0.040(4) 0.041(3) 0.030(3) 0.002(3) -0.015(3) -0.003(3) C21 0.038(4) 0.048(4) 0.034(4) 0.003(3) -0.013(3) -0.007(3) C22 0.041(5) 0.074(6) 0.042(5) 0.009(4) -0.017(4) 0.000(4) C23 0.039(5) 0.088(7) 0.052(6) 0.007(5) -0.014(4) 0.008(5) C24 0.041(5) 0.092(8) 0.058(6) 0.005(5) -0.011(5) -0.007(5) C25 0.054(5) 0.075(6) 0.039(5) 0.012(4) -0.015(4) -0.015(5) C26 0.048(5) 0.055(5) 0.037(4) 0.005(4) -0.018(4) -0.004(4) Co2 0.0485(6) 0.0380(6) 0.0306(6) 0.0029(4) -0.0194(5) -0.0079(5) Cl3 0.0576(12) 0.0356(10) 0.0393(10) 0.0059(8) -0.0223(9) -0.0092(8) Cl4 0.0609(12) 0.0346(9) 0.0339(10) 0.0044(7) -0.0246(9) -0.0054(8) N3 0.047(4) 0.036(3) 0.028(3) 0.002(3) -0.013(3) -0.009(3) C31 0.046(4) 0.036(4) 0.029(4) 0.013(3) -0.012(3) -0.002(3) C32 0.052(5) 0.042(4) 0.044(5) -0.001(4) -0.016(4) -0.006(4) C33 0.055(6) 0.055(5) 0.058(6) 0.003(5) -0.012(5) -0.012(4) C34 0.057(6) 0.059(6) 0.051(6) 0.006(4) -0.010(5) 0.009(5) C35 0.062(6) 0.061(5) 0.032(4) 0.003(4) -0.020(4) 0.002(4) C36 0.058(5) 0.048(5) 0.034(4) 0.003(4) -0.020(4) -0.006(4) P3 0.0452(11) 0.0343(10) 0.0316(10) 0.0041(8) -0.0191(9) -0.0082(8) C311 0.036(4) 0.039(4) 0.032(4) 0.007(3) -0.014(3) -0.008(3) C312 0.051(5) 0.043(4) 0.041(5) 0.004(4) -0.020(4) -0.013(4) C313 0.060(6) 0.034(4) 0.057(5) 0.000(4) -0.026(4) -0.001(4) C314 0.053(5) 0.045(5) 0.068(6) 0.008(4) -0.031(5) 0.002(4) C315 0.049(5) 0.057(6) 0.078(7) 0.008(5) -0.037(5) -0.007(4) C316 0.051(5) 0.039(4) 0.059(5) 0.001(4) -0.025(4) -0.007(4) C321 0.042(4) 0.039(4) 0.037(4) 0.002(3) -0.019(3) -0.010(3) C322 0.057(5) 0.043(4) 0.040(4) 0.003(4) -0.029(4) -0.009(4) C323 0.057(5) 0.047(5) 0.040(5) 0.000(4) -0.023(4) -0.005(4) C324 0.070(6) 0.039(4) 0.048(5) -0.005(4) -0.025(5) -0.012(4) C325 0.082(7) 0.036(4) 0.044(5) 0.004(4) -0.024(5) -0.007(4) C326 0.066(6) 0.036(4) 0.031(4) 0.006(3) -0.019(4) -0.007(4) C3 0.046(4) 0.031(4) 0.033(4) 0.004(3) -0.020(3) -0.005(3) P4 0.0459(12) 0.0383(10) 0.0313(10) 0.0045(8) -0.0184(9) -0.0071(9) C411 0.041(4) 0.036(4) 0.036(4) 0.006(3) -0.019(3) -0.008(3) C412 0.051(5) 0.045(5) 0.042(5) 0.003(4) -0.018(4) -0.010(4) C413 0.053(5) 0.045(5) 0.055(5) -0.001(4) -0.023(4) -0.001(4) C414 0.046(5) 0.053(5) 0.052(5) 0.012(4) -0.020(4) -0.011(4) C415 0.049(5) 0.058(5) 0.042(5) 0.010(4) -0.017(4) -0.014(4) C416 0.046(5) 0.041(4) 0.051(5) -0.001(4) -0.026(4) -0.005(4) C421 0.043(4) 0.036(4) 0.043(4) 0.006(3) -0.020(4) -0.009(3) C422 0.053(5) 0.044(5) 0.042(5) 0.011(4) -0.020(4) -0.004(4) C423 0.068(6) 0.033(4) 0.047(5) 0.008(4) -0.014(4) 0.001(4) C424 0.061(6) 0.043(5) 0.047(5) -0.004(4) -0.018(4) -0.007(4) C425 0.053(5) 0.050(5) 0.036(4) 0.002(4) -0.020(4) -0.012(4) C426 0.046(5) 0.039(4) 0.035(4) 0.006(3) -0.017(4) -0.008(3) N4 0.045(4) 0.047(4) 0.030(3) 0.006(3) -0.016(3) -0.005(3) C41 0.048(5) 0.045(4) 0.040(4) 0.013(4) -0.024(4) -0.008(4) C42 0.046(5) 0.052(5) 0.048(5) 0.003(4) -0.018(4) -0.011(4) C43 0.052(5) 0.065(6) 0.054(5) 0.011(4) -0.033(5) -0.014(4) C44 0.053(6) 0.071(6) 0.073(7) 0.021(5) -0.040(5) -0.017(5) C45 0.050(5) 0.072(6) 0.050(5) 0.015(5) -0.019(4) -0.002(5) C46 0.055(6) 0.070(6) 0.047(5) 0.017(4) -0.029(4) -0.012(5) C1AS 0.033(9) 0.038(8) 0.066(8) -0.021(7) 0.023(8) 0.013(7) C1BS 0.31(3) 0.058(15) 0.049(14) 0.019(10) -0.076(16) 0.005(16) Cl1S 0.123(3) 0.113(3) 0.132(3) -0.041(2) -0.062(3) 0.009(2) Cl2S 0.136(4) 0.108(3) 0.149(4) 0.016(3) -0.060(3) -0.015(3) C2AS 0.051(10) 0.131(10) 0.026(8) 0.011(9) -0.015(7) -0.025(10) C2BS 0.090(15) 0.092(9) 0.119(17) 0.016(13) -0.065(11) -0.029(12) Cl3S 0.249(6) 0.106(3) 0.121(3) -0.044(2) -0.117(4) 0.087(3) Cl4S 0.0723(17) 0.0792(18) 0.107(2) -0.0305(16) -0.0515(17) 0.0042(14) C3S 0.103(9) 0.089(9) 0.112(8) 0.005(7) -0.050(7) -0.006(7) Cl5S 0.108(3) 0.095(2) 0.107(3) 0.044(2) -0.025(2) -0.031(2) Cl6S 0.119(3) 0.358(9) 0.096(3) 0.015(4) -0.050(3) 0.089(5) C4S 0.079(16) 0.112(11) 0.082(17) 0.020(13) -0.026(13) -0.039(14) Cl7S 0.103(3) 0.110(3) 0.130(3) 0.005(2) -0.073(2) -0.012(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 Co1 N1 2.030(6) . ? Co1 N2 2.034(6) . ? Co1 Cl1 2.272(2) . ? Co1 Cl2 2.277(2) . ? N1 C11 1.439(8) . ? N1 P1 1.606(6) . ? C11 C12 1.388(8) . ? C11 C16 1.395(8) . ? C12 C13 1.388(9) . ? C13 C14 1.382(9) . ? C14 C15 1.384(9) . ? C15 C16 1.388(9) . ? P1 C111 1.796(7) . ? P1 C121 1.800(6) . ? P1 C1 1.808(7) . ? C111 C116 1.391(9) . ? C111 C112 1.412(8) . ? C112 C113 1.396(9) . ? C113 C114 1.381(9) . ? C114 C115 1.375(9) . ? C115 C116 1.403(9) . ? C121 C126 1.388(8) . ? C121 C122 1.402(8) . ? C122 C123 1.382(8) . ? C123 C124 1.380(9) . ? C124 C125 1.369(9) . ? C125 C126 1.390(9) . ? C1 P2 1.819(8) . ? P2 N2 1.615(6) . ? P2 C221 1.797(7) . ? P2 C211 1.798(6) . ? C211 C216 1.391(8) . ? C211 C212 1.404(8) . ? C212 C213 1.383(8) . ? C213 C214 1.386(9) . ? C214 C215 1.374(9) . ? C215 C216 1.388(9) . ? C221 C226 1.386(8) . ? C221 C222 1.393(8) . ? C222 C223 1.401(9) . ? C223 C224 1.374(9) . ? C224 C225 1.388(9) . ? C225 C226 1.373(9) . ? N2 C21 1.437(8) . ? C21 C26 1.395(8) . ? C21 C22 1.403(9) . ? C22 C23 1.391(9) . ? C23 C24 1.371(10) . ? C24 C25 1.374(10) . ? C25 C26 1.392(9) . ? Co2 N3 2.030(6) . ? Co2 N4 2.039(6) . ? Co2 Cl3 2.273(2) . ? Co2 Cl4 2.277(2) . ? N3 C31 1.447(8) . ? N3 P3 1.603(6) . ? C31 C36 1.358(9) . ? C31 C32 1.406(9) . ? C32 C33 1.382(9) . ? C33 C34 1.370(10) . ? C34 C35 1.390(10) . ? C35 C36 1.390(9) . ? P3 C321 1.799(7) . ? P3 C311 1.804(6) . ? P3 C3 1.811(8) . ? C311 C316 1.387(8) . ? C311 C312 1.405(8) . ? C312 C313 1.379(9) . ? C313 C314 1.376(9) . ? C314 C315 1.382(9) . ? C315 C316 1.394(9) . ? C321 C326 1.397(8) . ? C321 C322 1.399(8) . ? C322 C323 1.387(9) . ? C323 C324 1.381(9) . ? C324 C325 1.364(9) . ? C325 C326 1.395(9) . ? C3 P4 1.821(7) . ? P4 N4 1.616(6) . ? P4 C421 1.788(7) . ? P4 C411 1.798(6) . ? C411 C412 1.389(8) . ? C411 C416 1.394(8) . ? C412 C413 1.385(9) . ? C413 C414 1.377(9) . ? C414 C415 1.370(9) . ? C415 C416 1.389(9) . ? C421 C422 1.393(8) . ? C421 C426 1.406(8) . ? C422 C423 1.385(9) . ? C423 C424 1.369(9) . ? C424 C425 1.381(9) . ? C425 C426 1.388(9) . ? N4 C41 1.432(8) . ? C41 C42 1.379(9) . ? C41 C46 1.402(9) . ? C42 C43 1.390(9) . ? C43 C44 1.386(10) . ? C44 C45 1.374(10) . ? C45 C46 1.393(9) . ? C1AS Cl1S 1.743(12) . ? C1AS Cl2S 1.757(11) . ? C1BS Cl2S 1.733(14) . ? C1BS Cl1S 1.821(14) . ? C2AS Cl3S 1.684(13) . ? C2AS Cl4S 1.761(12) . ? C2BS Cl3S 1.685(14) . ? C2BS Cl4S 1.751(13) . ? C3S Cl6S 1.724(10) . ? C3S Cl5S 1.740(10) . ? C4S Cl7S 1.705(13) . ? C4S Cl7S 1.758(13) 2_655 ? Cl7S C4S 1.758(13) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N2 107.5(2) . . ? N1 Co1 Cl1 107.04(18) . . ? N2 Co1 Cl1 111.71(18) . . ? N1 Co1 Cl2 107.17(19) . . ? N2 Co1 Cl2 105.96(18) . . ? Cl1 Co1 Cl2 117.07(8) . . ? C11 N1 P1 119.3(5) . . ? C11 N1 Co1 117.4(4) . . ? P1 N1 Co1 121.2(3) . . ? C12 C11 C16 118.5(6) . . ? C12 C11 N1 119.6(6) . . ? C16 C11 N1 121.9(6) . . ? C11 C12 C13 120.6(7) . . ? C14 C13 C12 121.0(7) . . ? C13 C14 C15 118.5(7) . . ? C14 C15 C16 121.1(7) . . ? C15 C16 C11 120.3(7) . . ? N1 P1 C111 112.4(3) . . ? N1 P1 C121 116.4(3) . . ? C111 P1 C121 110.3(3) . . ? N1 P1 C1 107.5(3) . . ? C111 P1 C1 103.4(3) . . ? C121 P1 C1 105.6(3) . . ? C116 C111 C112 119.3(6) . . ? C116 C111 P1 124.4(5) . . ? C112 C111 P1 116.3(5) . . ? C113 C112 C111 119.8(7) . . ? C114 C113 C112 120.1(7) . . ? C115 C114 C113 120.7(8) . . ? C114 C115 C116 120.1(8) . . ? C111 C116 C115 120.0(7) . . ? C126 C121 C122 119.4(6) . . ? C126 C121 P1 119.3(5) . . ? C122 C121 P1 121.3(5) . . ? C123 C122 C121 119.9(7) . . ? C122 C123 C124 120.1(7) . . ? C125 C124 C123 120.4(7) . . ? C124 C125 C126 120.4(7) . . ? C121 C126 C125 119.8(7) . . ? P1 C1 P2 122.1(4) . . ? N2 P2 C221 110.7(3) . . ? N2 P2 C211 114.4(3) . . ? C221 P2 C211 110.6(3) . . ? N2 P2 C1 108.8(3) . . ? C221 P2 C1 102.3(3) . . ? C211 P2 C1 109.2(3) . . ? C216 C211 C212 119.5(6) . . ? C216 C211 P2 119.2(5) . . ? C212 C211 P2 121.3(5) . . ? C213 C212 C211 119.3(6) . . ? C212 C213 C214 120.9(7) . . ? C215 C214 C213 119.9(7) . . ? C214 C215 C216 120.3(7) . . ? C215 C216 C211 120.2(7) . . ? C226 C221 C222 119.5(6) . . ? C226 C221 P2 117.0(5) . . ? C222 C221 P2 123.5(5) . . ? C221 C222 C223 119.6(7) . . ? C224 C223 C222 120.0(7) . . ? C223 C224 C225 120.2(7) . . ? C226 C225 C224 120.2(7) . . ? C225 C226 C221 120.6(7) . . ? C21 N2 P2 118.0(5) . . ? C21 N2 Co1 119.7(4) . . ? P2 N2 Co1 119.5(3) . . ? C26 C21 C22 117.4(6) . . ? C26 C21 N2 119.0(6) . . ? C22 C21 N2 123.6(6) . . ? C23 C22 C21 121.2(7) . . ? C24 C23 C22 119.8(8) . . ? C23 C24 C25 120.5(8) . . ? C24 C25 C26 119.9(8) . . ? C25 C26 C21 121.2(7) . . ? N3 Co2 N4 107.2(2) . . ? N3 Co2 Cl3 107.97(18) . . ? N4 Co2 Cl3 105.07(19) . . ? N3 Co2 Cl4 107.54(17) . . ? N4 Co2 Cl4 111.77(18) . . ? Cl3 Co2 Cl4 116.82(8) . . ? C31 N3 P3 118.5(5) . . ? C31 N3 Co2 117.6(4) . . ? P3 N3 Co2 120.9(3) . . ? C36 C31 C32 118.2(7) . . ? C36 C31 N3 121.2(6) . . ? C32 C31 N3 120.6(6) . . ? C33 C32 C31 120.5(7) . . ? C34 C33 C32 120.5(8) . . ? C33 C34 C35 119.6(8) . . ? C34 C35 C36 119.3(8) . . ? C31 C36 C35 121.9(7) . . ? N3 P3 C321 115.3(3) . . ? N3 P3 C311 110.8(3) . . ? C321 P3 C311 110.7(3) . . ? N3 P3 C3 108.6(3) . . ? C321 P3 C3 105.7(3) . . ? C311 P3 C3 105.1(3) . . ? C316 C311 C312 119.5(6) . . ? C316 C311 P3 124.2(5) . . ? C312 C311 P3 116.3(5) . . ? C313 C312 C311 119.9(7) . . ? C314 C313 C312 120.5(7) . . ? C313 C314 C315 120.1(7) . . ? C314 C315 C316 120.3(7) . . ? C311 C316 C315 119.7(7) . . ? C326 C321 C322 119.8(6) . . ? C326 C321 P3 118.7(5) . . ? C322 C321 P3 121.4(5) . . ? C323 C322 C321 120.3(7) . . ? C324 C323 C322 118.9(7) . . ? C325 C324 C323 121.6(7) . . ? C324 C325 C326 120.4(7) . . ? C325 C326 C321 118.9(7) . . ? P3 C3 P4 121.4(4) . . ? N4 P4 C421 113.9(3) . . ? N4 P4 C411 111.5(3) . . ? C421 P4 C411 110.9(3) . . ? N4 P4 C3 108.9(3) . . ? C421 P4 C3 108.6(3) . . ? C411 P4 C3 102.5(3) . . ? C412 C411 C416 119.9(6) . . ? C412 C411 P4 117.1(5) . . ? C416 C411 P4 123.0(5) . . ? C413 C412 C411 120.1(7) . . ? C414 C413 C412 119.8(7) . . ? C415 C414 C413 120.4(7) . . ? C414 C415 C416 120.8(7) . . ? C415 C416 C411 119.0(7) . . ? C422 C421 C426 118.8(6) . . ? C422 C421 P4 119.4(5) . . ? C426 C421 P4 121.8(5) . . ? C423 C422 C421 120.5(7) . . ? C424 C423 C422 120.0(7) . . ? C423 C424 C425 121.0(7) . . ? C424 C425 C426 119.5(7) . . ? C425 C426 C421 120.2(6) . . ? C41 N4 P4 119.1(5) . . ? C41 N4 Co2 118.8(5) . . ? P4 N4 Co2 119.7(3) . . ? C42 C41 C46 117.3(7) . . ? C42 C41 N4 119.0(6) . . ? C46 C41 N4 123.8(6) . . ? C41 C42 C43 122.4(7) . . ? C44 C43 C42 119.5(8) . . ? C45 C44 C43 119.5(8) . . ? C44 C45 C46 120.7(8) . . ? C45 C46 C41 120.7(8) . . ? Cl1S C1AS Cl2S 106.0(7) . . ? Cl2S C1BS Cl1S 103.7(9) . . ? C1AS Cl1S C1BS 41.3(9) . . ? C1BS Cl2S C1AS 42.3(10) . . ? Cl3S C2AS Cl4S 112.8(8) . . ? Cl3S C2BS Cl4S 113.3(10) . . ? C2AS Cl3S C2BS 68.4(7) . . ? C2BS Cl4S C2AS 65.2(7) . . ? Cl6S C3S Cl5S 112.3(7) . . ? Cl7S C4S Cl7S 115.5(10) . 2_655 ? C4S Cl7S C4S 64.5(10) . 2_655 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.432 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.107 #===END data_mb52 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H57 Br Cl2 N2 Ni P2' _chemical_formula_weight 957.44 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' 'Br' 'Br' -0.2901 2.4595 '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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.00350(10) _cell_length_b 21.2311(2) _cell_length_c 18.15510(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.9940(5) _cell_angle_gamma 90.00 _cell_volume 4767.08(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 77375 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.460 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5532 _exptl_absorpt_correction_T_max 0.8329 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77373 _diffrn_reflns_av_R_equivalents 0.0106 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9352 _reflns_number_gt 8606 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0302P)^2^+3.8638P] 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 9352 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Ni1 Ni 0.197063(16) 0.732614(9) 0.571705(11) 0.01605(6) Uani 1 1 d . . . Br1 Br 0.181477(15) 0.689984(9) 0.685320(10) 0.02746(6) Uani 1 1 d . . . N1 N 0.07722(11) 0.79044(7) 0.54764(8) 0.0191(3) Uani 1 1 d . . . C11 C -0.02728(14) 0.79173(8) 0.55834(10) 0.0216(3) Uani 1 1 d . . . C12 C -0.11039(15) 0.75361(9) 0.51157(12) 0.0302(4) Uani 1 1 d . . . C13 C -0.21399(17) 0.75988(11) 0.51827(15) 0.0424(5) Uani 1 1 d . . . H13 H -0.2714 0.7355 0.4857 0.051 Uiso 1 1 calc R . . C14 C -0.23516(18) 0.80055(11) 0.57084(16) 0.0446(6) Uani 1 1 d . . . H14 H -0.3068 0.8052 0.5730 0.054 Uiso 1 1 calc R . . C15 C -0.15147(17) 0.83448(10) 0.62034(13) 0.0353(5) Uani 1 1 d . . . H15 H -0.1657 0.8612 0.6581 0.042 Uiso 1 1 calc R . . C16 C -0.04596(15) 0.83031(8) 0.61603(11) 0.0256(4) Uani 1 1 d . . . C121 C -0.09071(16) 0.70325(10) 0.45826(13) 0.0369(5) Uani 1 1 d . . . H121 H -0.0149 0.7082 0.4568 0.044 Uiso 1 1 calc R . . C122 C -0.0998(2) 0.63806(11) 0.49236(15) 0.0497(6) Uani 1 1 d . . . H12A H -0.0482 0.6351 0.5446 0.075 Uiso 1 1 calc R . . H12B H -0.0837 0.6054 0.4594 0.075 Uiso 1 1 calc R . . H12C H -0.1734 0.6321 0.4949 0.075 Uiso 1 1 calc R . . C123 C -0.16608(19) 0.70866(11) 0.37533(14) 0.0451(5) Uani 1 1 d . . . H12D H -0.2407 0.7008 0.3745 0.068 Uiso 1 1 calc R . . H12E H -0.1453 0.6776 0.3426 0.068 Uiso 1 1 calc R . . H12F H -0.1607 0.7511 0.3556 0.068 Uiso 1 1 calc R . . C161 C 0.04438(16) 0.86520(9) 0.67438(11) 0.0284(4) Uani 1 1 d . . . H161 H 0.1140 0.8512 0.6670 0.034 Uiso 1 1 calc R . . C162 C 0.0492(2) 0.84846(12) 0.75757(12) 0.0442(5) Uani 1 1 d . . . H16A H -0.0132 0.8669 0.7691 0.066 Uiso 1 1 calc R . . H16B H 0.1160 0.8652 0.7937 0.066 Uiso 1 1 calc R . . H16C H 0.0478 0.8026 0.7630 0.066 Uiso 1 1 calc R . . C163 C 0.03616(19) 0.93658(10) 0.66231(14) 0.0400(5) Uani 1 1 d . . . H16D H 0.0357 0.9466 0.6095 0.060 Uiso 1 1 calc R . . H16E H 0.0983 0.9570 0.6995 0.060 Uiso 1 1 calc R . . H16F H -0.0308 0.9519 0.6702 0.060 Uiso 1 1 calc R . . P2 P 0.11866(3) 0.825364(19) 0.48353(2) 0.01638(9) Uani 1 1 d . . . C211 C 0.01707(13) 0.84600(8) 0.39421(10) 0.0201(3) Uani 1 1 d . . . C212 C 0.03033(15) 0.83014(10) 0.32350(11) 0.0285(4) Uani 1 1 d . . . H212 H 0.0920 0.8067 0.3222 0.034 Uiso 1 1 calc R . . C213 C -0.04598(16) 0.84827(11) 0.25458(11) 0.0375(5) Uani 1 1 d . . . H213 H -0.0372 0.8366 0.2064 0.045 Uiso 1 1 calc R . . C214 C -0.13485(16) 0.88338(11) 0.25644(12) 0.0357(5) Uani 1 1 d . . . H214 H -0.1869 0.8961 0.2094 0.043 Uiso 1 1 calc R . . C215 C -0.14803(15) 0.90003(9) 0.32676(12) 0.0305(4) Uani 1 1 d . . . H215 H -0.2088 0.9245 0.3277 0.037 Uiso 1 1 calc R . . C216 C -0.07352(14) 0.88133(8) 0.39562(11) 0.0251(4) Uani 1 1 d . . . H216 H -0.0836 0.8923 0.4436 0.030 Uiso 1 1 calc R . . C221 C 0.18864(13) 0.89852(8) 0.51733(10) 0.0195(3) Uani 1 1 d . . . C222 C 0.25778(14) 0.90262(8) 0.59313(10) 0.0237(4) Uani 1 1 d . . . H222 H 0.2681 0.8670 0.6263 0.028 Uiso 1 1 calc R . . C223 C 0.31158(16) 0.95855(9) 0.62035(12) 0.0309(4) Uani 1 1 d . . . H223 H 0.3589 0.9611 0.6719 0.037 Uiso 1 1 calc R . . C224 C 0.29609(16) 1.01065(9) 0.57214(13) 0.0340(4) Uani 1 1 d . . . H224 H 0.3335 1.0487 0.5906 0.041 Uiso 1 1 calc R . . C225 C 0.22662(16) 1.00745(9) 0.49748(13) 0.0333(4) Uani 1 1 d . . . H225 H 0.2153 1.0435 0.4650 0.040 Uiso 1 1 calc R . . C226 C 0.17315(15) 0.95161(8) 0.46965(11) 0.0256(4) Uani 1 1 d . . . H226 H 0.1259 0.9495 0.4180 0.031 Uiso 1 1 calc R . . C3 C 0.20267(13) 0.76466(8) 0.46897(9) 0.0169(3) Uani 1 1 d . . . H3 H 0.1650(16) 0.7342(10) 0.4348(12) 0.022(5) Uiso 1 1 d . . . P4 P 0.33984(3) 0.744661(19) 0.50523(2) 0.01557(9) Uani 1 1 d . . . C411 C 0.42157(13) 0.81450(7) 0.53293(10) 0.0186(3) Uani 1 1 d . . . C412 C 0.48181(14) 0.82731(9) 0.60881(10) 0.0245(4) Uani 1 1 d . . . H412 H 0.4780 0.7999 0.6492 0.029 Uiso 1 1 calc R . . C413 C 0.54782(15) 0.88023(9) 0.62587(12) 0.0308(4) Uani 1 1 d . . . H413 H 0.5900 0.8886 0.6778 0.037 Uiso 1 1 calc R . . C414 C 0.55221(16) 0.92069(9) 0.56745(13) 0.0323(4) Uani 1 1 d . . . H414 H 0.5980 0.9566 0.5792 0.039 Uiso 1 1 calc R . . C415 C 0.49035(17) 0.90916(9) 0.49189(12) 0.0327(4) Uani 1 1 d . . . H415 H 0.4924 0.9376 0.4520 0.039 Uiso 1 1 calc R . . C416 C 0.42529(15) 0.85610(8) 0.47416(11) 0.0265(4) Uani 1 1 d . . . H416 H 0.3833 0.8480 0.4221 0.032 Uiso 1 1 calc R . . C421 C 0.39093(14) 0.70880(8) 0.43314(10) 0.0195(3) Uani 1 1 d . . . C422 C 0.33322(15) 0.71156(8) 0.35468(10) 0.0246(4) Uani 1 1 d . . . H422 H 0.2653 0.7324 0.3380 0.029 Uiso 1 1 calc R . . C423 C 0.37496(18) 0.68370(9) 0.30047(11) 0.0320(4) Uani 1 1 d . . . H423 H 0.3358 0.6858 0.2469 0.038 Uiso 1 1 calc R . . C424 C 0.47354(18) 0.65304(9) 0.32486(12) 0.0335(5) Uani 1 1 d . . . H424 H 0.5014 0.6335 0.2879 0.040 Uiso 1 1 calc R . . C425 C 0.53190(16) 0.65061(9) 0.40286(12) 0.0312(4) Uani 1 1 d . . . H425 H 0.6000 0.6299 0.4191 0.037 Uiso 1 1 calc R . . C426 C 0.49114(15) 0.67839(8) 0.45737(11) 0.0248(4) Uani 1 1 d . . . H426 H 0.5312 0.6767 0.5108 0.030 Uiso 1 1 calc R . . N5 N 0.33715(11) 0.69846(6) 0.57463(8) 0.0183(3) Uani 1 1 d . . . C51 C 0.38686(14) 0.63846(8) 0.59772(10) 0.0203(3) Uani 1 1 d . . . C52 C 0.46906(15) 0.63303(8) 0.66926(11) 0.0248(4) Uani 1 1 d . . . C53 C 0.52154(17) 0.57522(9) 0.68968(12) 0.0344(4) Uani 1 1 d . . . H53 H 0.5784 0.5716 0.7372 0.041 Uiso 1 1 calc R . . C54 C 0.49229(19) 0.52335(10) 0.64220(13) 0.0413(5) Uani 1 1 d . . . H54 H 0.5301 0.4847 0.6562 0.050 Uiso 1 1 calc R . . C55 C 0.40766(18) 0.52791(9) 0.57419(12) 0.0365(5) Uani 1 1 d . . . H55 H 0.3863 0.4916 0.5426 0.044 Uiso 1 1 calc R . . C56 C 0.35261(15) 0.58450(8) 0.55058(11) 0.0251(4) Uani 1 1 d . . . C521 C 0.50332(16) 0.68770(9) 0.72495(11) 0.0297(4) Uani 1 1 d . . . H521 H 0.4488 0.7221 0.7065 0.036 Uiso 1 1 calc R . . C522 C 0.5053(3) 0.66972(12) 0.80703(13) 0.0582(8) Uani 1 1 d . . . H52A H 0.4339 0.6542 0.8059 0.087 Uiso 1 1 calc R . . H52B H 0.5240 0.7068 0.8407 0.087 Uiso 1 1 calc R . . H52C H 0.5594 0.6367 0.8270 0.087 Uiso 1 1 calc R . . C523 C 0.61324(18) 0.71331(12) 0.72418(18) 0.0550(7) Uani 1 1 d . . . H52D H 0.6698 0.6825 0.7482 0.082 Uiso 1 1 calc R . . H52E H 0.6285 0.7529 0.7533 0.082 Uiso 1 1 calc R . . H52F H 0.6117 0.7209 0.6706 0.082 Uiso 1 1 calc R . . C561 C 0.25474(16) 0.58447(9) 0.47794(11) 0.0282(4) Uani 1 1 d . . . H561 H 0.2404 0.6291 0.4602 0.034 Uiso 1 1 calc R . . C562 C 0.15564(19) 0.56069(14) 0.49751(14) 0.0507(6) Uani 1 1 d . . . H56A H 0.1684 0.5174 0.5170 0.076 Uiso 1 1 calc R . . H56B H 0.0926 0.5616 0.4508 0.076 Uiso 1 1 calc R . . H56C H 0.1422 0.5878 0.5372 0.076 Uiso 1 1 calc R . . C563 C 0.2727(2) 0.54674(12) 0.41155(13) 0.0480(6) Uani 1 1 d . . . H56D H 0.3376 0.5622 0.4008 0.072 Uiso 1 1 calc R . . H56E H 0.2099 0.5517 0.3652 0.072 Uiso 1 1 calc R . . H56F H 0.2819 0.5021 0.4259 0.072 Uiso 1 1 calc R . . C1S C 0.2524(3) 0.53060(11) 0.71430(14) 0.0519(6) Uani 1 1 d . . . H1SA H 0.3179 0.5479 0.7048 0.062 Uiso 1 1 calc R . . H1SB H 0.1889 0.5536 0.6808 0.062 Uiso 1 1 calc R . . Cl1S Cl 0.26103(7) 0.54238(3) 0.81130(3) 0.06004(18) Uani 1 1 d . . . Cl2S Cl 0.24010(7) 0.44998(3) 0.68972(4) 0.0692(2) 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 0.01767(11) 0.01518(10) 0.01721(11) 0.00197(8) 0.00817(8) 0.00185(8) Br1 0.03486(11) 0.02881(10) 0.02403(10) 0.00798(7) 0.01689(8) 0.00488(7) N1 0.0184(7) 0.0190(7) 0.0223(7) 0.0036(6) 0.0098(6) 0.0024(5) C11 0.0191(8) 0.0211(8) 0.0275(9) 0.0043(7) 0.0112(7) 0.0027(7) C12 0.0228(9) 0.0282(10) 0.0422(11) -0.0033(8) 0.0137(8) -0.0022(8) C13 0.0223(10) 0.0414(12) 0.0658(15) -0.0114(11) 0.0168(10) -0.0070(9) C14 0.0271(11) 0.0449(13) 0.0718(16) -0.0041(12) 0.0296(11) -0.0001(9) C15 0.0335(11) 0.0336(11) 0.0479(12) -0.0016(9) 0.0259(10) 0.0044(9) C16 0.0276(9) 0.0225(9) 0.0316(10) 0.0040(7) 0.0161(8) 0.0033(7) C121 0.0238(10) 0.0369(11) 0.0502(13) -0.0169(10) 0.0118(9) -0.0072(8) C122 0.0455(13) 0.0375(12) 0.0565(15) -0.0114(11) 0.0015(11) 0.0038(10) C123 0.0450(13) 0.0430(13) 0.0478(13) -0.0085(11) 0.0153(11) -0.0143(10) C161 0.0314(10) 0.0279(10) 0.0301(10) -0.0017(8) 0.0155(8) 0.0044(8) C162 0.0546(14) 0.0478(13) 0.0317(11) 0.0029(10) 0.0157(10) 0.0099(11) C163 0.0470(13) 0.0288(11) 0.0455(12) -0.0028(9) 0.0162(10) -0.0012(9) P2 0.0162(2) 0.01576(19) 0.0178(2) 0.00143(15) 0.00622(16) 0.00139(15) C211 0.0187(8) 0.0191(8) 0.0220(8) 0.0031(6) 0.0058(7) -0.0005(6) C212 0.0229(9) 0.0390(11) 0.0242(9) 0.0029(8) 0.0080(7) 0.0055(8) C213 0.0308(11) 0.0592(14) 0.0223(9) 0.0058(9) 0.0080(8) 0.0082(10) C214 0.0245(10) 0.0489(13) 0.0287(10) 0.0100(9) 0.0010(8) 0.0050(9) C215 0.0193(9) 0.0323(10) 0.0366(10) 0.0029(8) 0.0040(8) 0.0056(8) C216 0.0229(9) 0.0249(9) 0.0274(9) -0.0003(7) 0.0076(7) 0.0028(7) C221 0.0180(8) 0.0185(8) 0.0246(8) -0.0009(7) 0.0103(7) 0.0012(6) C222 0.0231(9) 0.0242(9) 0.0258(9) -0.0018(7) 0.0105(7) 0.0007(7) C223 0.0286(10) 0.0337(10) 0.0320(10) -0.0121(8) 0.0119(8) -0.0049(8) C224 0.0335(11) 0.0236(9) 0.0513(12) -0.0135(9) 0.0227(10) -0.0090(8) C225 0.0353(11) 0.0183(9) 0.0512(12) 0.0030(8) 0.0208(10) -0.0017(8) C226 0.0248(9) 0.0216(9) 0.0318(9) 0.0031(7) 0.0109(8) -0.0003(7) C3 0.0169(8) 0.0163(8) 0.0177(8) -0.0007(6) 0.0057(6) 0.0007(6) P4 0.0168(2) 0.01511(19) 0.01617(19) 0.00037(15) 0.00717(16) 0.00107(15) C411 0.0172(8) 0.0166(8) 0.0242(8) -0.0016(6) 0.0098(7) 0.0010(6) C412 0.0235(9) 0.0260(9) 0.0244(9) 0.0000(7) 0.0081(7) -0.0009(7) C413 0.0255(10) 0.0336(10) 0.0322(10) -0.0091(8) 0.0072(8) -0.0062(8) C414 0.0280(10) 0.0233(9) 0.0500(12) -0.0086(9) 0.0183(9) -0.0080(8) C415 0.0405(11) 0.0213(9) 0.0426(11) 0.0036(8) 0.0219(9) -0.0043(8) C416 0.0328(10) 0.0225(9) 0.0260(9) 0.0019(7) 0.0115(8) -0.0015(7) C421 0.0231(8) 0.0162(8) 0.0228(8) -0.0019(6) 0.0123(7) -0.0019(6) C422 0.0279(9) 0.0239(9) 0.0236(9) -0.0026(7) 0.0104(7) -0.0017(7) C423 0.0461(12) 0.0306(10) 0.0234(9) -0.0076(8) 0.0165(9) -0.0072(9) C424 0.0501(12) 0.0243(9) 0.0377(11) -0.0081(8) 0.0305(10) -0.0029(9) C425 0.0329(10) 0.0239(9) 0.0448(11) -0.0010(8) 0.0239(9) 0.0040(8) C426 0.0268(9) 0.0228(9) 0.0279(9) 0.0003(7) 0.0133(8) 0.0020(7) N5 0.0208(7) 0.0163(7) 0.0196(7) 0.0032(5) 0.0088(6) 0.0032(5) C51 0.0227(8) 0.0180(8) 0.0239(8) 0.0044(7) 0.0125(7) 0.0059(7) C52 0.0258(9) 0.0230(9) 0.0271(9) 0.0047(7) 0.0102(7) 0.0056(7) C53 0.0359(11) 0.0283(10) 0.0352(10) 0.0075(8) 0.0055(9) 0.0129(8) C54 0.0497(13) 0.0251(10) 0.0473(12) 0.0071(9) 0.0123(10) 0.0186(9) C55 0.0512(13) 0.0189(9) 0.0404(11) -0.0005(8) 0.0156(10) 0.0078(9) C56 0.0316(10) 0.0188(8) 0.0278(9) 0.0020(7) 0.0135(8) 0.0032(7) C521 0.0321(10) 0.0263(10) 0.0257(9) 0.0034(7) 0.0014(8) 0.0079(8) C522 0.104(2) 0.0388(13) 0.0248(11) 0.0058(9) 0.0095(13) 0.0247(14) C523 0.0261(11) 0.0380(13) 0.0856(19) -0.0052(13) -0.0050(12) 0.0054(10) C561 0.0375(11) 0.0191(9) 0.0280(9) -0.0010(7) 0.0099(8) -0.0004(8) C562 0.0401(13) 0.0677(17) 0.0432(13) -0.0006(12) 0.0110(10) -0.0109(12) C563 0.0657(16) 0.0438(13) 0.0338(11) -0.0107(10) 0.0147(11) 0.0042(11) C1S 0.091(2) 0.0304(11) 0.0377(12) -0.0003(9) 0.0248(13) -0.0072(12) Cl1S 0.0959(5) 0.0514(4) 0.0317(3) 0.0069(2) 0.0181(3) 0.0129(3) Cl2S 0.1091(6) 0.0331(3) 0.0507(4) -0.0031(3) 0.0032(4) -0.0110(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 Ni1 N1 1.9251(14) . ? Ni1 N5 1.9461(14) . ? Ni1 C3 2.0077(16) . ? Ni1 Br1 2.3180(3) . ? Ni1 P4 2.5206(4) . ? Ni1 P2 2.5439(4) . ? N1 C11 1.431(2) . ? N1 P2 1.6070(14) . ? C11 C12 1.406(3) . ? C11 C16 1.409(3) . ? C12 C13 1.396(3) . ? C12 C121 1.516(3) . ? C13 C14 1.376(3) . ? C14 C15 1.381(3) . ? C15 C16 1.401(3) . ? C16 C161 1.511(3) . ? C121 C123 1.526(3) . ? C121 C122 1.536(3) . ? C161 C163 1.530(3) . ? C161 C162 1.534(3) . ? P2 C3 1.7614(16) . ? P2 C211 1.8009(17) . ? P2 C221 1.8088(17) . ? C211 C212 1.388(2) . ? C211 C216 1.404(2) . ? C212 C213 1.390(3) . ? C213 C214 1.384(3) . ? C214 C215 1.385(3) . ? C215 C216 1.382(3) . ? C221 C222 1.395(2) . ? C221 C226 1.397(2) . ? C222 C223 1.389(3) . ? C223 C224 1.386(3) . ? C224 C225 1.379(3) . ? C225 C226 1.388(3) . ? C3 P4 1.7522(17) . ? C3 H3 0.92(2) . ? P4 N5 1.6057(14) . ? P4 C411 1.8030(17) . ? P4 C421 1.8087(16) . ? C411 C412 1.385(2) . ? C411 C416 1.397(2) . ? C412 C413 1.390(3) . ? C413 C414 1.380(3) . ? C414 C415 1.381(3) . ? C415 C416 1.386(3) . ? C421 C422 1.391(2) . ? C421 C426 1.398(2) . ? C422 C423 1.394(3) . ? C423 C424 1.383(3) . ? C424 C425 1.386(3) . ? C425 C426 1.390(3) . ? N5 C51 1.431(2) . ? C51 C52 1.409(3) . ? C51 C56 1.417(2) . ? C52 C53 1.397(3) . ? C52 C521 1.513(3) . ? C53 C54 1.378(3) . ? C54 C55 1.380(3) . ? C55 C56 1.397(3) . ? C56 C561 1.524(3) . ? C521 C522 1.531(3) . ? C521 C523 1.533(3) . ? C561 C563 1.524(3) . ? C561 C562 1.525(3) . ? C1S Cl1S 1.748(2) . ? C1S Cl2S 1.764(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N5 158.30(6) . . ? N1 Ni1 C3 80.34(6) . . ? N5 Ni1 C3 81.33(6) . . ? N1 Ni1 Br1 99.42(4) . . ? N5 Ni1 Br1 99.71(4) . . ? C3 Ni1 Br1 175.72(5) . . ? N1 Ni1 P4 119.41(4) . . ? N5 Ni1 P4 39.57(4) . . ? C3 Ni1 P4 43.72(5) . . ? Br1 Ni1 P4 138.201(14) . . ? N1 Ni1 P2 39.16(4) . . ? N5 Ni1 P2 119.70(4) . . ? C3 Ni1 P2 43.58(5) . . ? Br1 Ni1 P2 137.222(13) . . ? P4 Ni1 P2 80.296(14) . . ? C11 N1 P2 129.37(12) . . ? C11 N1 Ni1 135.84(11) . . ? P2 N1 Ni1 91.69(6) . . ? C12 C11 C16 120.46(16) . . ? C12 C11 N1 119.47(16) . . ? C16 C11 N1 120.07(16) . . ? C13 C12 C11 118.35(18) . . ? C13 C12 C121 118.74(18) . . ? C11 C12 C121 122.79(16) . . ? C14 C13 C12 121.7(2) . . ? C13 C14 C15 119.50(19) . . ? C14 C15 C16 121.28(19) . . ? C15 C16 C11 118.36(18) . . ? C15 C16 C161 119.52(17) . . ? C11 C16 C161 122.09(16) . . ? C12 C121 C123 113.15(18) . . ? C12 C121 C122 109.20(19) . . ? C123 C121 C122 111.07(18) . . ? C16 C161 C163 112.36(17) . . ? C16 C161 C162 111.29(17) . . ? C163 C161 C162 110.49(17) . . ? N1 P2 C3 97.66(7) . . ? N1 P2 C211 116.59(8) . . ? C3 P2 C211 111.05(8) . . ? N1 P2 C221 113.37(8) . . ? C3 P2 C221 114.14(8) . . ? C211 P2 C221 104.41(8) . . ? N1 P2 Ni1 49.15(5) . . ? C3 P2 Ni1 51.79(5) . . ? C211 P2 Ni1 142.64(6) . . ? C221 P2 Ni1 112.92(6) . . ? C212 C211 C216 119.41(16) . . ? C212 C211 P2 120.50(13) . . ? C216 C211 P2 119.99(13) . . ? C211 C212 C213 120.48(18) . . ? C214 C213 C212 119.77(19) . . ? C213 C214 C215 120.12(18) . . ? C216 C215 C214 120.56(18) . . ? C215 C216 C211 119.65(17) . . ? C222 C221 C226 119.11(16) . . ? C222 C221 P2 119.45(13) . . ? C226 C221 P2 121.42(14) . . ? C223 C222 C221 120.31(17) . . ? C224 C223 C222 119.90(18) . . ? C225 C224 C223 120.31(18) . . ? C224 C225 C226 120.15(18) . . ? C225 C226 C221 120.21(18) . . ? P4 C3 P2 136.68(10) . . ? P4 C3 Ni1 83.90(7) . . ? P2 C3 Ni1 84.63(7) . . ? P4 C3 H3 110.5(12) . . ? P2 C3 H3 112.8(12) . . ? Ni1 C3 H3 102.9(12) . . ? N5 P4 C3 100.16(7) . . ? N5 P4 C411 115.93(8) . . ? C3 P4 C411 110.45(8) . . ? N5 P4 C421 114.37(7) . . ? C3 P4 C421 112.89(8) . . ? C411 P4 C421 103.39(8) . . ? N5 P4 Ni1 50.54(5) . . ? C3 P4 Ni1 52.37(5) . . ? C411 P4 Ni1 114.06(5) . . ? C421 P4 Ni1 142.49(6) . . ? C412 C411 C416 119.54(16) . . ? C412 C411 P4 122.85(13) . . ? C416 C411 P4 117.60(13) . . ? C411 C412 C413 120.07(17) . . ? C414 C413 C412 120.10(18) . . ? C413 C414 C415 120.23(17) . . ? C414 C415 C416 120.09(18) . . ? C415 C416 C411 119.94(18) . . ? C422 C421 C426 119.83(16) . . ? C422 C421 P4 121.38(13) . . ? C426 C421 P4 118.79(13) . . ? C421 C422 C423 120.03(18) . . ? C424 C423 C422 119.89(18) . . ? C423 C424 C425 120.37(17) . . ? C424 C425 C426 120.19(18) . . ? C425 C426 C421 119.68(18) . . ? C51 N5 P4 131.01(11) . . ? C51 N5 Ni1 132.36(11) . . ? P4 N5 Ni1 89.89(6) . . ? C52 C51 C56 119.87(15) . . ? C52 C51 N5 119.22(15) . . ? C56 C51 N5 120.89(15) . . ? C53 C52 C51 119.06(17) . . ? C53 C52 C521 118.53(17) . . ? C51 C52 C521 122.41(15) . . ? C54 C53 C52 121.22(19) . . ? C53 C54 C55 119.56(18) . . ? C54 C55 C56 121.75(19) . . ? C55 C56 C51 118.33(17) . . ? C55 C56 C561 118.50(17) . . ? C51 C56 C561 123.07(16) . . ? C52 C521 C522 111.84(17) . . ? C52 C521 C523 110.42(18) . . ? C522 C521 C523 111.2(2) . . ? C56 C561 C563 113.20(17) . . ? C56 C561 C562 109.78(16) . . ? C563 C561 C562 110.91(19) . . ? Cl1S C1S Cl2S 111.50(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.710 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.051 #===END data_ms425 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H43 Br2 Cl2 Fe N3 P2 Si2' _chemical_formula_weight 922.42 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4409(2) _cell_length_b 20.1425(5) _cell_length_c 22.0698(5) _cell_angle_alpha 79.8090(13) _cell_angle_beta 79.5410(14) _cell_angle_gamma 88.6500(15) _cell_volume 4061.87(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 66136 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 28.33 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 2.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6205 _exptl_absorpt_correction_T_max 0.9491 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66136 _diffrn_reflns_av_R_equivalents 0.0962 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15808 _reflns_number_gt 11398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0583P)^2^+20.2429P] 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 0.0016(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15808 _refine_ls_number_parameters 878 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1738 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.005 _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_1 Fe 1.41622(9) -0.23961(5) 0.20344(4) 0.0292(2) Uani 1 1 d . . . Br1_1 Br 1.52945(8) -0.26626(4) 0.29719(3) 0.03907(19) Uani 1 1 d . . . Br2_1 Br 1.52745(8) -0.23425(4) 0.09296(3) 0.04005(19) Uani 1 1 d . . . N1_1 N 1.3363(6) -0.3497(3) 0.2163(3) 0.0322(12) Uani 1 1 d . . . Si1_1 Si 1.4460(2) -0.41952(10) 0.23133(10) 0.0386(4) Uani 1 1 d . . . C11_1 C 1.3976(9) -0.4938(4) 0.1984(4) 0.0473(19) Uani 1 1 d . . . H11A_1 H 1.2941 -0.5031 0.2112 0.071 Uiso 1 1 calc R . . H11B_1 H 1.4516 -0.5333 0.2141 0.071 Uiso 1 1 calc R . . H11C_1 H 1.4220 -0.4837 0.1526 0.071 Uiso 1 1 calc R . . C12_1 C 1.4409(10) -0.4511(4) 0.3166(4) 0.056(2) Uani 1 1 d . . . H12A_1 H 1.4697 -0.4147 0.3361 0.085 Uiso 1 1 calc R . . H12B_1 H 1.5073 -0.4889 0.3218 0.085 Uiso 1 1 calc R . . H12C_1 H 1.3429 -0.4662 0.3365 0.085 Uiso 1 1 calc R . . C13_1 C 1.6329(8) -0.3967(4) 0.1939(4) 0.050(2) Uani 1 1 d . . . H13A_1 H 1.6399 -0.3874 0.1483 0.075 Uiso 1 1 calc R . . H13B_1 H 1.6966 -0.4341 0.2054 0.075 Uiso 1 1 calc R . . H13C_1 H 1.6619 -0.3564 0.2079 0.075 Uiso 1 1 calc R . . P1_1 P 1.17194(17) -0.35165(8) 0.21492(8) 0.0277(3) Uani 1 1 d . . . C111_1 C 1.1236(7) -0.3545(3) 0.1395(3) 0.0298(14) Uani 1 1 d . . . C112_1 C 0.9863(8) -0.3374(4) 0.1275(3) 0.0398(16) Uani 1 1 d . . . H112_1 H 0.9161 -0.3229 0.1589 0.048 Uiso 1 1 calc R . . C113_1 C 0.9512(9) -0.3416(4) 0.0695(4) 0.0458(19) Uani 1 1 d . . . H113_1 H 0.8580 -0.3292 0.0611 0.055 Uiso 1 1 calc R . . C114_1 C 1.0531(10) -0.3637(4) 0.0244(4) 0.050(2) Uani 1 1 d . . . H114_1 H 1.0289 -0.3673 -0.0148 0.060 Uiso 1 1 calc R . . C115_1 C 1.1887(9) -0.3805(4) 0.0354(3) 0.0470(19) Uani 1 1 d . . . H115_1 H 1.2578 -0.3958 0.0040 0.056 Uiso 1 1 calc R . . C116_1 C 1.2250(8) -0.3751(3) 0.0928(3) 0.0370(16) Uani 1 1 d . . . H116_1 H 1.3198 -0.3857 0.1001 0.044 Uiso 1 1 calc R . . C121_1 C 1.0681(7) -0.4169(3) 0.2702(3) 0.0275(13) Uani 1 1 d . . . C122_1 C 0.9916(8) -0.4673(4) 0.2523(3) 0.0375(16) Uani 1 1 d . . . H122_1 H 0.9900 -0.4668 0.2093 0.045 Uiso 1 1 calc R . . C123_1 C 0.9192(8) -0.5173(4) 0.2974(4) 0.0448(18) Uani 1 1 d . . . H123_1 H 0.8674 -0.5512 0.2854 0.054 Uiso 1 1 calc R . . C124_1 C 0.9217(8) -0.5182(4) 0.3594(4) 0.0430(17) Uani 1 1 d . . . H124_1 H 0.8715 -0.5530 0.3900 0.052 Uiso 1 1 calc R . . C125_1 C 0.9962(8) -0.4693(4) 0.3785(3) 0.0408(17) Uani 1 1 d . . . H125_1 H 0.9968 -0.4703 0.4216 0.049 Uiso 1 1 calc R . . C126_1 C 1.0698(7) -0.4189(3) 0.3334(3) 0.0325(14) Uani 1 1 d . . . H126_1 H 1.1218 -0.3854 0.3459 0.039 Uiso 1 1 calc R . . N2_1 N 1.4265(5) -0.1278(3) 0.2058(3) 0.0298(12) Uani 1 1 d . . . Si2_1 Si 1.5843(2) -0.08439(10) 0.20470(9) 0.0339(4) Uani 1 1 d . . . C21_1 C 1.7345(7) -0.1245(4) 0.1589(4) 0.0464(19) Uani 1 1 d . . . H21A_1 H 1.7421 -0.1717 0.1787 0.070 Uiso 1 1 calc R . . H21B_1 H 1.8245 -0.1005 0.1574 0.070 Uiso 1 1 calc R . . H21C_1 H 1.7166 -0.1225 0.1162 0.070 Uiso 1 1 calc R . . C22_1 C 1.6196(8) -0.0808(4) 0.2846(3) 0.0384(16) Uani 1 1 d . . . H22A_1 H 1.5560 -0.0475 0.3029 0.058 Uiso 1 1 calc R . . H22B_1 H 1.7202 -0.0677 0.2818 0.058 Uiso 1 1 calc R . . H22C_1 H 1.6010 -0.1252 0.3112 0.058 Uiso 1 1 calc R . . C23_1 C 1.5822(8) 0.0061(4) 0.1650(4) 0.0481(19) Uani 1 1 d . . . H23A_1 H 1.5560 0.0083 0.1238 0.072 Uiso 1 1 calc R . . H23B_1 H 1.6780 0.0263 0.1602 0.072 Uiso 1 1 calc R . . H23C_1 H 1.5116 0.0310 0.1905 0.072 Uiso 1 1 calc R . . P2_1 P 1.27394(17) -0.09398(8) 0.21591(8) 0.0262(3) Uani 1 1 d . . . C211_1 C 1.2243(7) -0.0449(3) 0.1458(3) 0.0301(14) Uani 1 1 d . . . C212_1 C 1.0918(8) -0.0110(3) 0.1455(3) 0.0362(15) Uani 1 1 d . . . H212_1 H 1.0263 -0.0110 0.1836 0.043 Uiso 1 1 calc R . . C213_1 C 1.0571(8) 0.0219(4) 0.0901(4) 0.0427(18) Uani 1 1 d . . . H213_1 H 0.9674 0.0441 0.0899 0.051 Uiso 1 1 calc R . . C214_1 C 1.1534(9) 0.0225(4) 0.0344(4) 0.0448(18) Uani 1 1 d . . . H214_1 H 1.1296 0.0459 -0.0037 0.054 Uiso 1 1 calc R . . C215_1 C 1.2824(9) -0.0104(4) 0.0337(3) 0.0447(18) Uani 1 1 d . . . H215_1 H 1.3474 -0.0096 -0.0047 0.054 Uiso 1 1 calc R . . C216_1 C 1.3183(8) -0.0450(4) 0.0894(3) 0.0382(16) Uani 1 1 d . . . H216_1 H 1.4067 -0.0687 0.0888 0.046 Uiso 1 1 calc R . . C221_1 C 1.2394(7) -0.0454(3) 0.2786(3) 0.0302(14) Uani 1 1 d . . . C222_1 C 1.2552(7) -0.0778(4) 0.3378(3) 0.0363(15) Uani 1 1 d . . . H222_1 H 1.2792 -0.1243 0.3443 0.044 Uiso 1 1 calc R . . C223_1 C 1.2364(8) -0.0436(4) 0.3875(3) 0.0413(17) Uani 1 1 d . . . H223_1 H 1.2484 -0.0665 0.4277 0.050 Uiso 1 1 calc R . . C224_1 C 1.2004(9) 0.0234(4) 0.3792(4) 0.0479(19) Uani 1 1 d . . . H224_1 H 1.1863 0.0468 0.4136 0.058 Uiso 1 1 calc R . . C225_1 C 1.1846(9) 0.0568(4) 0.3201(4) 0.051(2) Uani 1 1 d . . . H225_1 H 1.1604 0.1032 0.3143 0.061 Uiso 1 1 calc R . . C226_1 C 1.2037(8) 0.0232(4) 0.2693(3) 0.0383(16) Uani 1 1 d . . . H226_1 H 1.1927 0.0463 0.2291 0.046 Uiso 1 1 calc R . . C1_1 C 1.0918(6) -0.2737(3) 0.2364(3) 0.0256(13) Uani 1 1 d . . . C2_1 C 0.9493(6) -0.2676(3) 0.2635(3) 0.0278(13) Uani 1 1 d . . . H2_1 H 0.8847 -0.3048 0.2711 0.033 Uiso 1 1 calc R . . C3_1 C 0.9021(7) -0.2058(3) 0.2795(3) 0.0325(14) Uani 1 1 d . . . H3_1 H 0.8051 -0.2005 0.2989 0.039 Uiso 1 1 calc R . . C4_1 C 0.9981(7) -0.1527(3) 0.2669(3) 0.0317(14) Uani 1 1 d . . . H4_1 H 0.9673 -0.1101 0.2771 0.038 Uiso 1 1 calc R . . C5_1 C 1.1403(6) -0.1613(3) 0.2390(3) 0.0257(13) Uani 1 1 d . . . N6_1 N 1.1874(5) -0.2214(3) 0.2247(2) 0.0256(11) Uani 1 1 d . . . Fe1_2 Fe 0.88382(9) 0.24027(4) 0.37781(4) 0.0273(2) Uani 1 1 d . . . Br1_2 Br 0.85517(8) 0.11946(3) 0.41726(4) 0.0443(2) Uani 1 1 d . . . Br2_2 Br 0.69662(7) 0.32770(3) 0.36733(3) 0.03592(18) Uani 1 1 d . . . N1_2 N 0.8878(6) 0.2290(3) 0.2738(3) 0.0412(14) Uani 1 1 d . . . Si1_2 Si 0.7593(2) 0.17649(12) 0.25719(11) 0.0485(5) Uani 1 1 d . . . C11_2 C 0.8441(10) 0.0953(5) 0.2445(6) 0.071(3) Uani 1 1 d . . . H11A_2 H 0.9139 0.1022 0.2052 0.106 Uiso 1 1 calc R . . H11B_2 H 0.7698 0.0631 0.2423 0.106 Uiso 1 1 calc R . . H11C_2 H 0.8935 0.0775 0.2793 0.106 Uiso 1 1 calc R . . C12_2 C 0.5977(9) 0.1617(5) 0.3184(5) 0.062(2) Uani 1 1 d . . . H12A_2 H 0.6235 0.1359 0.3568 0.092 Uiso 1 1 calc R . . H12B_2 H 0.5264 0.1362 0.3044 0.092 Uiso 1 1 calc R . . H12C_2 H 0.5568 0.2051 0.3267 0.092 Uiso 1 1 calc R . . C13_2 C 0.6726(11) 0.2090(5) 0.1892(4) 0.068(3) Uani 1 1 d . . . H13A_2 H 0.6076 0.2459 0.1989 0.102 Uiso 1 1 calc R . . H13B_2 H 0.6175 0.1726 0.1798 0.102 Uiso 1 1 calc R . . H13C_2 H 0.7467 0.2258 0.1528 0.102 Uiso 1 1 calc R . . P1_2 P 1.01359(17) 0.26797(9) 0.22758(8) 0.0279(3) Uani 1 1 d . . . C111_2 C 1.1216(7) 0.2285(3) 0.1666(3) 0.0279(13) Uani 1 1 d . . . C112_2 C 1.0813(7) 0.2326(4) 0.1087(3) 0.0350(15) Uani 1 1 d . . . H112_2 H 0.9968 0.2566 0.1008 0.042 Uiso 1 1 calc R . . C113_2 C 1.1603(8) 0.2027(4) 0.0625(3) 0.0398(17) Uani 1 1 d . . . H113_2 H 1.1308 0.2065 0.0231 0.048 Uiso 1 1 calc R . . C114_2 C 1.2832(8) 0.1669(4) 0.0731(3) 0.0430(18) Uani 1 1 d . . . H114_2 H 1.3396 0.1470 0.0409 0.052 Uiso 1 1 calc R . . C115_2 C 1.3222(8) 0.1606(4) 0.1306(4) 0.0435(17) Uani 1 1 d . . . H115_2 H 1.4052 0.1352 0.1384 0.052 Uiso 1 1 calc R . . C116_2 C 1.2429(8) 0.1906(3) 0.1781(3) 0.0369(15) Uani 1 1 d . . . H116_2 H 1.2709 0.1853 0.2179 0.044 Uiso 1 1 calc R . . C121_2 C 0.9687(7) 0.3481(3) 0.1840(3) 0.0316(14) Uani 1 1 d . . . C122_2 C 0.8267(8) 0.3693(4) 0.1927(4) 0.0433(17) Uani 1 1 d . . . H122_2 H 0.7563 0.3429 0.2231 0.052 Uiso 1 1 calc R . . C123_2 C 0.7861(9) 0.4287(4) 0.1576(4) 0.054(2) Uani 1 1 d . . . H123_2 H 0.6881 0.4420 0.1632 0.065 Uiso 1 1 calc R . . C124_2 C 0.8885(9) 0.4680(4) 0.1149(4) 0.0473(19) Uani 1 1 d . . . H124_2 H 0.8614 0.5087 0.0910 0.057 Uiso 1 1 calc R . . C125_2 C 1.0298(9) 0.4484(4) 0.1069(4) 0.0427(17) Uani 1 1 d . . . H125_2 H 1.1006 0.4759 0.0779 0.051 Uiso 1 1 calc R . . C126_2 C 1.0690(8) 0.3896(4) 0.1403(4) 0.0420(17) Uani 1 1 d . . . H126_2 H 1.1671 0.3765 0.1337 0.050 Uiso 1 1 calc R . . N2_2 N 0.9487(5) 0.2663(3) 0.4632(2) 0.0259(11) Uani 1 1 d . . . Si2_2 Si 0.82069(18) 0.27968(9) 0.52724(8) 0.0261(4) Uani 1 1 d . . . C21_2 C 0.8936(7) 0.2561(4) 0.6017(3) 0.0367(15) Uani 1 1 d . . . H21A_2 H 0.9286 0.2096 0.6053 0.055 Uiso 1 1 calc R . . H21B_2 H 0.8172 0.2597 0.6375 0.055 Uiso 1 1 calc R . . H21C_2 H 0.9732 0.2866 0.6013 0.055 Uiso 1 1 calc R . . C22_2 C 0.6581(7) 0.2277(3) 0.5326(3) 0.0352(15) Uani 1 1 d . . . H22A_2 H 0.6119 0.2437 0.4964 0.053 Uiso 1 1 calc R . . H22B_2 H 0.5907 0.2314 0.5712 0.053 Uiso 1 1 calc R . . H22C_2 H 0.6859 0.1805 0.5329 0.053 Uiso 1 1 calc R . . C23_2 C 0.7708(8) 0.3709(3) 0.5213(3) 0.0377(16) Uani 1 1 d . . . H23A_2 H 0.8585 0.3985 0.5136 0.057 Uiso 1 1 calc R . . H23B_2 H 0.7099 0.3780 0.5606 0.057 Uiso 1 1 calc R . . H23C_2 H 0.7181 0.3838 0.4867 0.057 Uiso 1 1 calc R . . P2_2 P 1.11695(16) 0.26498(8) 0.45734(7) 0.0237(3) Uani 1 1 d . . . C211_2 C 1.2020(6) 0.3271(3) 0.4891(3) 0.0258(13) Uani 1 1 d . . . C212_2 C 1.1959(7) 0.3951(3) 0.4606(3) 0.0325(14) Uani 1 1 d . . . H212_2 H 1.1450 0.4071 0.4269 0.039 Uiso 1 1 calc R . . C213_2 C 1.2638(8) 0.4450(3) 0.4815(3) 0.0376(16) Uani 1 1 d . . . H213_2 H 1.2609 0.4907 0.4616 0.045 Uiso 1 1 calc R . . C214_2 C 1.3360(8) 0.4277(4) 0.5316(4) 0.0422(17) Uani 1 1 d . . . H214_2 H 1.3826 0.4616 0.5460 0.051 Uiso 1 1 calc R . . C215_2 C 1.3400(8) 0.3615(4) 0.5603(3) 0.0402(17) Uani 1 1 d . . . H215_2 H 1.3888 0.3500 0.5947 0.048 Uiso 1 1 calc R . . C216_2 C 1.2741(7) 0.3112(3) 0.5397(3) 0.0329(14) Uani 1 1 d . . . H216_2 H 1.2778 0.2657 0.5601 0.039 Uiso 1 1 calc R . . C221_2 C 1.1952(7) 0.1847(3) 0.4853(3) 0.0282(13) Uani 1 1 d . . . C222_2 C 1.3427(7) 0.1733(3) 0.4722(3) 0.0340(15) Uani 1 1 d . . . H222_2 H 1.4050 0.2076 0.4467 0.041 Uiso 1 1 calc R . . C223_2 C 1.3993(8) 0.1124(4) 0.4962(4) 0.0424(17) Uani 1 1 d . . . H223_2 H 1.5003 0.1054 0.4881 0.051 Uiso 1 1 calc R . . C224_2 C 1.3088(8) 0.0620(4) 0.5318(4) 0.0438(17) Uani 1 1 d . . . H224_2 H 1.3474 0.0200 0.5480 0.053 Uiso 1 1 calc R . . C225_2 C 1.1618(8) 0.0723(4) 0.5441(4) 0.0400(16) Uani 1 1 d . . . H225_2 H 1.1001 0.0372 0.5688 0.048 Uiso 1 1 calc R . . C226_2 C 1.1038(7) 0.1330(3) 0.5208(3) 0.0332(14) Uani 1 1 d . . . H226_2 H 1.0025 0.1395 0.5288 0.040 Uiso 1 1 calc R . . C1_2 C 1.1455(6) 0.2878(3) 0.2738(3) 0.0254(12) Uani 1 1 d . . . C2_2 C 1.2819(7) 0.3140(4) 0.2472(3) 0.0347(15) Uani 1 1 d . . . H2_2 H 1.3110 0.3239 0.2031 0.042 Uiso 1 1 calc R . . C3_2 C 1.3751(7) 0.3256(3) 0.2864(3) 0.0322(14) Uani 1 1 d . . . H3_2 H 1.4691 0.3433 0.2693 0.039 Uiso 1 1 calc R . . C4_2 C 1.3298(7) 0.3110(3) 0.3503(3) 0.0300(14) Uani 1 1 d . . . H4_2 H 1.3919 0.3183 0.3779 0.036 Uiso 1 1 calc R . . C5_2 C 1.1917(6) 0.2854(3) 0.3735(3) 0.0251(12) Uani 1 1 d . . . N6_2 N 1.1006(5) 0.2739(2) 0.3358(2) 0.0227(10) Uani 1 1 d . . . C1S_3 C 2.2010(10) -0.1926(5) 0.0330(5) 0.063(2) Uani 1 1 d . . . H1SA_3 H 2.2795 -0.1869 0.0559 0.076 Uiso 1 1 calc R . . H1SB_3 H 2.1895 -0.2415 0.0337 0.076 Uiso 1 1 calc R . . Cl1_3 Cl 2.2501(4) -0.15240(18) -0.04381(13) 0.0947(10) Uani 1 1 d . . . Cl2_3 Cl 2.0411(2) -0.16213(10) 0.07160(10) 0.0533(5) Uani 1 1 d . . . C2S_3 C 1.5892(13) -0.3458(5) -0.0246(5) 0.086(4) Uani 1 1 d . . . H2SA_3 H 1.5293 -0.3203 0.0050 0.103 Uiso 1 1 calc R . . H2SB_3 H 1.6831 -0.3221 -0.0394 0.103 Uiso 1 1 calc R . . Cl3_3 Cl 1.5065(4) -0.3469(3) -0.08677(15) 0.1294(16) Uani 1 1 d . . . Cl4_3 Cl 1.6169(4) -0.4266(2) 0.01417(16) 0.1089(12) 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 Fe1_1 0.0224(4) 0.0373(5) 0.0282(5) -0.0068(4) -0.0041(4) 0.0007(4) Br1_1 0.0386(4) 0.0399(4) 0.0387(4) 0.0005(3) -0.0140(3) -0.0029(3) Br2_1 0.0443(4) 0.0441(4) 0.0303(4) -0.0097(3) 0.0010(3) -0.0044(3) N1_1 0.030(3) 0.026(3) 0.041(3) -0.009(2) -0.006(2) -0.001(2) Si1_1 0.0333(10) 0.0335(10) 0.0474(12) -0.0059(9) -0.0047(8) 0.0031(8) C11_1 0.048(4) 0.026(4) 0.068(5) -0.015(4) -0.007(4) 0.003(3) C12_1 0.054(5) 0.049(5) 0.061(5) 0.003(4) -0.010(4) 0.009(4) C13_1 0.035(4) 0.044(4) 0.068(5) -0.009(4) -0.001(4) 0.008(3) P1_1 0.0279(8) 0.0252(8) 0.0312(8) -0.0062(7) -0.0071(6) -0.0018(6) C111_1 0.038(4) 0.024(3) 0.029(3) -0.001(3) -0.011(3) -0.006(3) C112_1 0.043(4) 0.042(4) 0.037(4) -0.002(3) -0.015(3) -0.004(3) C113_1 0.048(4) 0.050(5) 0.044(4) -0.002(4) -0.026(4) -0.015(4) C114_1 0.075(6) 0.044(5) 0.032(4) -0.005(3) -0.012(4) -0.017(4) C115_1 0.059(5) 0.046(5) 0.033(4) -0.006(3) -0.002(3) -0.009(4) C116_1 0.046(4) 0.030(4) 0.031(3) -0.004(3) 0.002(3) -0.008(3) C121_1 0.029(3) 0.023(3) 0.031(3) -0.005(3) -0.006(3) -0.003(2) C122_1 0.042(4) 0.037(4) 0.037(4) -0.011(3) -0.011(3) -0.006(3) C123_1 0.053(5) 0.032(4) 0.049(4) -0.006(3) -0.007(4) -0.018(3) C124_1 0.047(4) 0.033(4) 0.043(4) 0.008(3) -0.006(3) -0.013(3) C125_1 0.053(5) 0.040(4) 0.029(3) -0.002(3) -0.008(3) -0.003(3) C126_1 0.036(4) 0.026(3) 0.038(4) -0.010(3) -0.006(3) -0.004(3) N2_1 0.020(3) 0.032(3) 0.038(3) -0.006(2) -0.007(2) 0.000(2) Si2_1 0.0278(9) 0.0322(10) 0.0421(11) -0.0055(8) -0.0079(8) -0.0044(7) C21_1 0.028(4) 0.059(5) 0.054(5) -0.016(4) -0.004(3) -0.006(3) C22_1 0.037(4) 0.037(4) 0.045(4) -0.011(3) -0.013(3) -0.001(3) C23_1 0.041(4) 0.042(4) 0.060(5) -0.001(4) -0.014(4) -0.018(3) P2_1 0.0251(8) 0.0241(8) 0.0300(8) -0.0042(6) -0.0067(6) -0.0022(6) C211_1 0.030(3) 0.030(3) 0.032(3) -0.004(3) -0.011(3) -0.006(3) C212_1 0.038(4) 0.030(4) 0.044(4) -0.007(3) -0.015(3) 0.000(3) C213_1 0.042(4) 0.032(4) 0.059(5) -0.003(3) -0.027(4) 0.000(3) C214_1 0.061(5) 0.035(4) 0.042(4) 0.004(3) -0.026(4) -0.011(3) C215_1 0.051(5) 0.053(5) 0.028(4) 0.001(3) -0.009(3) -0.014(4) C216_1 0.043(4) 0.039(4) 0.033(4) -0.003(3) -0.010(3) -0.005(3) C221_1 0.027(3) 0.026(3) 0.039(4) -0.010(3) -0.007(3) -0.002(2) C222_1 0.037(4) 0.033(4) 0.038(4) -0.002(3) -0.008(3) -0.011(3) C223_1 0.049(4) 0.041(4) 0.032(4) -0.006(3) -0.003(3) -0.006(3) C224_1 0.058(5) 0.051(5) 0.037(4) -0.017(4) -0.006(3) -0.005(4) C225_1 0.069(6) 0.037(4) 0.050(5) -0.018(4) -0.011(4) 0.007(4) C226_1 0.044(4) 0.034(4) 0.038(4) -0.009(3) -0.009(3) -0.001(3) C1_1 0.025(3) 0.026(3) 0.028(3) -0.004(2) -0.011(2) -0.005(2) C2_1 0.022(3) 0.026(3) 0.034(3) -0.003(3) -0.006(2) -0.003(2) C3_1 0.018(3) 0.036(4) 0.041(4) -0.004(3) -0.003(3) -0.002(3) C4_1 0.025(3) 0.029(3) 0.040(4) -0.001(3) -0.009(3) 0.005(3) C5_1 0.024(3) 0.023(3) 0.031(3) -0.004(2) -0.009(2) 0.001(2) N6_1 0.021(3) 0.028(3) 0.028(3) -0.005(2) -0.005(2) -0.003(2) Fe1_2 0.0207(4) 0.0254(5) 0.0357(5) -0.0052(4) -0.0047(4) -0.0022(3) Br1_2 0.0513(5) 0.0249(4) 0.0559(5) -0.0102(3) -0.0036(3) -0.0052(3) Br2_2 0.0252(3) 0.0340(4) 0.0492(4) -0.0045(3) -0.0110(3) 0.0003(3) N1_2 0.034(3) 0.047(4) 0.044(3) -0.010(3) -0.007(3) -0.005(3) Si1_2 0.0398(12) 0.0535(13) 0.0576(14) -0.0221(11) -0.0106(10) -0.0043(10) C11_2 0.052(5) 0.061(6) 0.111(8) -0.046(6) -0.014(5) -0.003(4) C12_2 0.039(5) 0.065(6) 0.089(7) -0.028(5) -0.022(4) 0.003(4) C13_2 0.092(7) 0.089(7) 0.042(5) -0.033(5) -0.045(5) 0.029(6) P1_2 0.0254(8) 0.0324(9) 0.0272(8) -0.0078(7) -0.0062(6) 0.0014(6) C111_2 0.033(3) 0.021(3) 0.030(3) -0.001(2) -0.007(3) 0.003(2) C112_2 0.034(4) 0.039(4) 0.033(4) -0.011(3) -0.007(3) 0.000(3) C113_2 0.047(4) 0.042(4) 0.031(4) -0.012(3) -0.004(3) -0.009(3) C114_2 0.051(5) 0.039(4) 0.037(4) -0.016(3) 0.007(3) -0.010(3) C115_2 0.039(4) 0.035(4) 0.056(5) -0.011(3) -0.005(3) 0.009(3) C116_2 0.045(4) 0.033(4) 0.034(4) -0.008(3) -0.009(3) 0.005(3) C121_2 0.035(4) 0.037(4) 0.027(3) -0.012(3) -0.013(3) 0.004(3) C122_2 0.031(4) 0.045(4) 0.055(5) -0.009(4) -0.012(3) 0.005(3) C123_2 0.041(4) 0.052(5) 0.074(6) -0.009(4) -0.023(4) 0.014(4) C124_2 0.066(5) 0.033(4) 0.049(5) -0.010(3) -0.025(4) 0.003(4) C125_2 0.054(5) 0.032(4) 0.044(4) -0.007(3) -0.011(3) 0.002(3) C126_2 0.044(4) 0.037(4) 0.046(4) -0.004(3) -0.014(3) -0.002(3) N2_2 0.027(3) 0.026(3) 0.024(3) -0.003(2) -0.005(2) 0.001(2) Si2_2 0.0237(8) 0.0275(9) 0.0278(9) -0.0075(7) -0.0037(7) -0.0020(7) C21_2 0.036(4) 0.042(4) 0.033(4) -0.008(3) -0.006(3) -0.002(3) C22_2 0.035(4) 0.031(4) 0.039(4) -0.008(3) -0.003(3) -0.007(3) C23_2 0.042(4) 0.031(4) 0.041(4) -0.015(3) -0.002(3) 0.002(3) P2_2 0.0225(8) 0.0246(8) 0.0253(8) -0.0046(6) -0.0074(6) -0.0011(6) C211_2 0.024(3) 0.030(3) 0.026(3) -0.007(3) -0.006(2) -0.002(2) C212_2 0.041(4) 0.026(3) 0.032(3) -0.006(3) -0.011(3) 0.004(3) C213_2 0.044(4) 0.025(3) 0.045(4) -0.007(3) -0.013(3) 0.000(3) C214_2 0.039(4) 0.043(4) 0.051(4) -0.019(4) -0.013(3) -0.012(3) C215_2 0.042(4) 0.046(4) 0.040(4) -0.014(3) -0.018(3) -0.003(3) C216_2 0.033(4) 0.030(3) 0.035(4) -0.002(3) -0.011(3) -0.001(3) C221_2 0.027(3) 0.027(3) 0.033(3) -0.003(3) -0.012(3) -0.001(2) C222_2 0.033(4) 0.022(3) 0.048(4) -0.002(3) -0.013(3) 0.000(3) C223_2 0.034(4) 0.038(4) 0.060(5) -0.014(4) -0.016(3) 0.008(3) C224_2 0.049(4) 0.030(4) 0.054(5) -0.001(3) -0.018(4) 0.000(3) C225_2 0.038(4) 0.029(4) 0.050(4) -0.001(3) -0.006(3) -0.004(3) C226_2 0.033(4) 0.032(4) 0.034(3) -0.003(3) -0.005(3) -0.001(3) C1_2 0.025(3) 0.026(3) 0.026(3) -0.005(2) -0.007(2) 0.005(2) C2_2 0.028(3) 0.048(4) 0.027(3) -0.004(3) -0.005(3) 0.000(3) C3_2 0.018(3) 0.042(4) 0.035(4) -0.005(3) -0.002(3) -0.004(3) C4_2 0.024(3) 0.032(3) 0.035(3) -0.005(3) -0.008(3) 0.003(3) C5_2 0.022(3) 0.024(3) 0.032(3) -0.008(3) -0.009(2) 0.005(2) N6_2 0.020(2) 0.026(3) 0.023(2) -0.005(2) -0.0050(19) -0.0015(19) C1S_3 0.049(5) 0.050(5) 0.087(7) -0.004(5) -0.012(5) -0.002(4) Cl1_3 0.105(2) 0.120(3) 0.0543(15) -0.0164(15) -0.0016(14) 0.0280(19) Cl2_3 0.0548(12) 0.0465(11) 0.0607(12) -0.0139(9) -0.0116(10) 0.0017(9) C2S_3 0.100(8) 0.063(6) 0.086(8) -0.036(6) 0.033(6) -0.039(6) Cl3_3 0.079(2) 0.217(5) 0.0591(17) 0.035(2) 0.0166(15) 0.013(2) Cl4_3 0.087(2) 0.148(3) 0.084(2) -0.008(2) -0.0120(17) 0.033(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 Fe1_1 N6_1 2.163(5) . ? Fe1_1 N2_1 2.267(5) . ? Fe1_1 N1_1 2.312(5) . ? Fe1_1 Br2_1 2.4583(11) . ? Fe1_1 Br1_1 2.4687(11) . ? N1_1 P1_1 1.559(6) . ? N1_1 Si1_1 1.747(6) . ? Si1_1 C13_1 1.840(8) . ? Si1_1 C12_1 1.868(9) . ? Si1_1 C11_1 1.874(7) . ? P1_1 C121_1 1.799(6) . ? P1_1 C111_1 1.815(6) . ? P1_1 C1_1 1.826(6) . ? C111_1 C116_1 1.388(9) . ? C111_1 C112_1 1.393(10) . ? C112_1 C113_1 1.395(10) . ? C113_1 C114_1 1.379(12) . ? C114_1 C115_1 1.369(12) . ? C115_1 C116_1 1.393(10) . ? C121_1 C126_1 1.391(9) . ? C121_1 C122_1 1.409(9) . ? C122_1 C123_1 1.381(10) . ? C123_1 C124_1 1.370(11) . ? C124_1 C125_1 1.388(10) . ? C125_1 C126_1 1.389(9) . ? N2_1 P2_1 1.574(5) . ? N2_1 Si2_1 1.740(5) . ? Si2_1 C21_1 1.843(8) . ? Si2_1 C22_1 1.867(7) . ? Si2_1 C23_1 1.879(8) . ? P2_1 C221_1 1.811(6) . ? P2_1 C211_1 1.813(7) . ? P2_1 C5_1 1.815(6) . ? C211_1 C216_1 1.392(9) . ? C211_1 C212_1 1.412(9) . ? C212_1 C213_1 1.374(10) . ? C213_1 C214_1 1.388(11) . ? C214_1 C215_1 1.371(12) . ? C215_1 C216_1 1.397(10) . ? C221_1 C222_1 1.386(10) . ? C221_1 C226_1 1.402(9) . ? C222_1 C223_1 1.379(10) . ? C223_1 C224_1 1.372(11) . ? C224_1 C225_1 1.390(11) . ? C225_1 C226_1 1.392(10) . ? C1_1 N6_1 1.362(7) . ? C1_1 C2_1 1.382(8) . ? C2_1 C3_1 1.394(9) . ? C3_1 C4_1 1.376(9) . ? C4_1 C5_1 1.391(9) . ? C5_1 N6_1 1.351(8) . ? Fe1_2 N6_2 2.159(5) . ? Fe1_2 N2_2 2.233(5) . ? Fe1_2 N1_2 2.340(6) . ? Fe1_2 Br1_2 2.4388(11) . ? Fe1_2 Br2_2 2.4771(11) . ? N1_2 P1_2 1.546(6) . ? N1_2 Si1_2 1.755(6) . ? Si1_2 C12_2 1.837(10) . ? Si1_2 C11_2 1.848(9) . ? Si1_2 C13_2 1.851(8) . ? P1_2 C121_2 1.810(7) . ? P1_2 C111_2 1.823(6) . ? P1_2 C1_2 1.838(6) . ? C111_2 C112_2 1.388(9) . ? C111_2 C116_2 1.399(9) . ? C112_2 C113_2 1.370(9) . ? C113_2 C114_2 1.385(11) . ? C114_2 C115_2 1.369(11) . ? C115_2 C116_2 1.394(10) . ? C121_2 C122_2 1.387(10) . ? C121_2 C126_2 1.395(10) . ? C122_2 C123_2 1.392(11) . ? C123_2 C124_2 1.375(12) . ? C124_2 C125_2 1.371(11) . ? C125_2 C126_2 1.360(10) . ? N2_2 P2_2 1.570(5) . ? N2_2 Si2_2 1.740(5) . ? Si2_2 C22_2 1.853(6) . ? Si2_2 C23_2 1.873(7) . ? Si2_2 C21_2 1.876(7) . ? P2_2 C211_2 1.806(6) . ? P2_2 C221_2 1.815(7) . ? P2_2 C5_2 1.833(6) . ? C211_2 C216_2 1.398(9) . ? C211_2 C212_2 1.408(9) . ? C212_2 C213_2 1.390(9) . ? C213_2 C214_2 1.391(10) . ? C214_2 C215_2 1.374(11) . ? C215_2 C216_2 1.382(9) . ? C221_2 C222_2 1.393(9) . ? C221_2 C226_2 1.397(9) . ? C222_2 C223_2 1.383(10) . ? C223_2 C224_2 1.375(11) . ? C224_2 C225_2 1.383(10) . ? C225_2 C226_2 1.381(10) . ? C1_2 N6_2 1.339(8) . ? C1_2 C2_2 1.388(9) . ? C2_2 C3_2 1.391(9) . ? C3_2 C4_2 1.377(9) . ? C4_2 C5_2 1.387(8) . ? C5_2 N6_2 1.351(7) . ? C1S_3 Cl1_3 1.729(10) . ? C1S_3 Cl2_3 1.748(9) . ? C2S_3 Cl3_3 1.701(13) . ? C2S_3 Cl4_3 1.737(13) . ? 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 N6_1 Fe1_1 N2_1 81.73(18) . . ? N6_1 Fe1_1 N1_1 81.77(19) . . ? N2_1 Fe1_1 N1_1 162.84(19) . . ? N6_1 Fe1_1 Br2_1 117.72(14) . . ? N2_1 Fe1_1 Br2_1 97.51(14) . . ? N1_1 Fe1_1 Br2_1 94.32(14) . . ? N6_1 Fe1_1 Br1_1 113.51(14) . . ? N2_1 Fe1_1 Br1_1 90.80(14) . . ? N1_1 Fe1_1 Br1_1 91.45(15) . . ? Br2_1 Fe1_1 Br1_1 128.75(4) . . ? P1_1 N1_1 Si1_1 126.1(3) . . ? P1_1 N1_1 Fe1_1 110.5(3) . . ? Si1_1 N1_1 Fe1_1 123.1(3) . . ? N1_1 Si1_1 C13_1 108.9(3) . . ? N1_1 Si1_1 C12_1 113.5(3) . . ? C13_1 Si1_1 C12_1 108.8(4) . . ? N1_1 Si1_1 C11_1 113.3(3) . . ? C13_1 Si1_1 C11_1 106.3(4) . . ? C12_1 Si1_1 C11_1 105.8(4) . . ? N1_1 P1_1 C121_1 116.4(3) . . ? N1_1 P1_1 C111_1 116.1(3) . . ? C121_1 P1_1 C111_1 106.4(3) . . ? N1_1 P1_1 C1_1 108.4(3) . . ? C121_1 P1_1 C1_1 103.7(3) . . ? C111_1 P1_1 C1_1 104.4(3) . . ? C116_1 C111_1 C112_1 119.0(6) . . ? C116_1 C111_1 P1_1 119.3(5) . . ? C112_1 C111_1 P1_1 121.7(5) . . ? C111_1 C112_1 C113_1 120.4(7) . . ? C114_1 C113_1 C112_1 119.4(8) . . ? C115_1 C114_1 C113_1 121.0(7) . . ? C114_1 C115_1 C116_1 119.8(7) . . ? C111_1 C116_1 C115_1 120.4(7) . . ? C126_1 C121_1 C122_1 119.1(6) . . ? C126_1 C121_1 P1_1 117.6(4) . . ? C122_1 C121_1 P1_1 123.2(5) . . ? C123_1 C122_1 C121_1 119.8(6) . . ? C124_1 C123_1 C122_1 120.2(6) . . ? C123_1 C124_1 C125_1 121.3(6) . . ? C124_1 C125_1 C126_1 118.9(6) . . ? C125_1 C126_1 C121_1 120.7(6) . . ? P2_1 N2_1 Si2_1 122.3(3) . . ? P2_1 N2_1 Fe1_1 113.4(3) . . ? Si2_1 N2_1 Fe1_1 124.0(3) . . ? N2_1 Si2_1 C21_1 108.2(3) . . ? N2_1 Si2_1 C22_1 113.1(3) . . ? C21_1 Si2_1 C22_1 111.2(4) . . ? N2_1 Si2_1 C23_1 112.8(3) . . ? C21_1 Si2_1 C23_1 106.4(4) . . ? C22_1 Si2_1 C23_1 104.9(4) . . ? N2_1 P2_1 C221_1 115.7(3) . . ? N2_1 P2_1 C211_1 114.8(3) . . ? C221_1 P2_1 C211_1 109.4(3) . . ? N2_1 P2_1 C5_1 107.5(3) . . ? C221_1 P2_1 C5_1 104.4(3) . . ? C211_1 P2_1 C5_1 103.7(3) . . ? C216_1 C211_1 C212_1 119.1(6) . . ? C216_1 C211_1 P2_1 117.6(5) . . ? C212_1 C211_1 P2_1 123.2(5) . . ? C213_1 C212_1 C211_1 120.2(7) . . ? C212_1 C213_1 C214_1 120.0(7) . . ? C215_1 C214_1 C213_1 120.7(7) . . ? C214_1 C215_1 C216_1 120.1(7) . . ? C211_1 C216_1 C215_1 119.9(7) . . ? C222_1 C221_1 C226_1 119.3(6) . . ? C222_1 C221_1 P2_1 117.4(5) . . ? C226_1 C221_1 P2_1 123.2(5) . . ? C223_1 C222_1 C221_1 120.9(7) . . ? C224_1 C223_1 C222_1 120.4(7) . . ? C223_1 C224_1 C225_1 119.5(7) . . ? C224_1 C225_1 C226_1 121.0(7) . . ? C225_1 C226_1 C221_1 118.9(7) . . ? N6_1 C1_1 C2_1 122.1(6) . . ? N6_1 C1_1 P1_1 113.6(4) . . ? C2_1 C1_1 P1_1 124.3(4) . . ? C1_1 C2_1 C3_1 118.9(5) . . ? C4_1 C3_1 C2_1 119.0(6) . . ? C3_1 C4_1 C5_1 120.0(6) . . ? N6_1 C5_1 C4_1 121.3(5) . . ? N6_1 C5_1 P2_1 114.6(4) . . ? C4_1 C5_1 P2_1 124.0(5) . . ? C5_1 N6_1 C1_1 118.8(5) . . ? C5_1 N6_1 Fe1_1 119.7(4) . . ? C1_1 N6_1 Fe1_1 120.2(4) . . ? N6_2 Fe1_2 N2_2 82.45(18) . . ? N6_2 Fe1_2 N1_2 79.25(19) . . ? N2_2 Fe1_2 N1_2 161.57(19) . . ? N6_2 Fe1_2 Br1_2 115.38(14) . . ? N2_2 Fe1_2 Br1_2 95.97(13) . . ? N1_2 Fe1_2 Br1_2 93.85(16) . . ? N6_2 Fe1_2 Br2_2 115.00(14) . . ? N2_2 Fe1_2 Br2_2 96.80(14) . . ? N1_2 Fe1_2 Br2_2 88.98(16) . . ? Br1_2 Fe1_2 Br2_2 129.17(4) . . ? P1_2 N1_2 Si1_2 127.8(4) . . ? P1_2 N1_2 Fe1_2 113.1(3) . . ? Si1_2 N1_2 Fe1_2 119.0(3) . . ? N1_2 Si1_2 C12_2 113.6(4) . . ? N1_2 Si1_2 C11_2 109.0(4) . . ? C12_2 Si1_2 C11_2 110.0(5) . . ? N1_2 Si1_2 C13_2 117.0(4) . . ? C12_2 Si1_2 C13_2 99.1(5) . . ? C11_2 Si1_2 C13_2 107.6(5) . . ? N1_2 P1_2 C121_2 116.1(3) . . ? N1_2 P1_2 C111_2 120.6(3) . . ? C121_2 P1_2 C111_2 102.2(3) . . ? N1_2 P1_2 C1_2 107.3(3) . . ? C121_2 P1_2 C1_2 105.6(3) . . ? C111_2 P1_2 C1_2 103.6(3) . . ? C112_2 C111_2 C116_2 118.3(6) . . ? C112_2 C111_2 P1_2 120.7(5) . . ? C116_2 C111_2 P1_2 120.9(5) . . ? C113_2 C112_2 C111_2 121.5(7) . . ? C112_2 C113_2 C114_2 120.2(7) . . ? C115_2 C114_2 C113_2 119.1(7) . . ? C114_2 C115_2 C116_2 121.4(7) . . ? C115_2 C116_2 C111_2 119.3(7) . . ? C122_2 C121_2 C126_2 117.4(7) . . ? C122_2 C121_2 P1_2 119.0(6) . . ? C126_2 C121_2 P1_2 123.5(5) . . ? C121_2 C122_2 C123_2 120.9(7) . . ? C124_2 C123_2 C122_2 119.7(8) . . ? C125_2 C124_2 C123_2 119.9(8) . . ? C126_2 C125_2 C124_2 120.3(8) . . ? C125_2 C126_2 C121_2 121.7(7) . . ? P2_2 N2_2 Si2_2 127.8(3) . . ? P2_2 N2_2 Fe1_2 110.7(3) . . ? Si2_2 N2_2 Fe1_2 121.3(3) . . ? N2_2 Si2_2 C22_2 109.6(3) . . ? N2_2 Si2_2 C23_2 111.3(3) . . ? C22_2 Si2_2 C23_2 109.9(3) . . ? N2_2 Si2_2 C21_2 110.7(3) . . ? C22_2 Si2_2 C21_2 108.9(3) . . ? C23_2 Si2_2 C21_2 106.3(3) . . ? N2_2 P2_2 C211_2 118.4(3) . . ? N2_2 P2_2 C221_2 116.5(3) . . ? C211_2 P2_2 C221_2 105.7(3) . . ? N2_2 P2_2 C5_2 106.4(3) . . ? C211_2 P2_2 C5_2 102.6(3) . . ? C221_2 P2_2 C5_2 105.7(3) . . ? C216_2 C211_2 C212_2 118.5(6) . . ? C216_2 C211_2 P2_2 123.7(5) . . ? C212_2 C211_2 P2_2 117.8(5) . . ? C213_2 C212_2 C211_2 120.4(6) . . ? C212_2 C213_2 C214_2 119.8(6) . . ? C215_2 C214_2 C213_2 120.0(6) . . ? C214_2 C215_2 C216_2 120.9(7) . . ? C215_2 C216_2 C211_2 120.3(6) . . ? C222_2 C221_2 C226_2 119.3(6) . . ? C222_2 C221_2 P2_2 122.0(5) . . ? C226_2 C221_2 P2_2 118.7(5) . . ? C223_2 C222_2 C221_2 120.5(6) . . ? C224_2 C223_2 C222_2 119.8(7) . . ? C223_2 C224_2 C225_2 120.2(7) . . ? C226_2 C225_2 C224_2 120.7(7) . . ? C225_2 C226_2 C221_2 119.4(6) . . ? N6_2 C1_2 C2_2 122.1(5) . . ? N6_2 C1_2 P1_2 114.5(4) . . ? C2_2 C1_2 P1_2 123.4(5) . . ? C1_2 C2_2 C3_2 118.9(6) . . ? C4_2 C3_2 C2_2 119.3(6) . . ? C3_2 C4_2 C5_2 118.7(6) . . ? N6_2 C5_2 C4_2 122.4(6) . . ? N6_2 C5_2 P2_2 114.4(4) . . ? C4_2 C5_2 P2_2 123.2(5) . . ? C1_2 N6_2 C5_2 118.6(5) . . ? C1_2 N6_2 Fe1_2 122.6(4) . . ? C5_2 N6_2 Fe1_2 118.6(4) . . ? Cl1_3 C1S_3 Cl2_3 113.3(5) . . ? Cl3_3 C2S_3 Cl4_3 112.0(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.353 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.128