#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Asselberghs, I ' 'Bildstein, Benno' 'Fiorini, Celine' 'Kowallick, Ralph' 'Malaun, Michael' 'Marcaccio, Massimo' 'McCleverty, J.A.' 'McDonagh, A.M.' 'Nunzi, Jean-Michel' 'Paul, Rowena L.' 'Persoons, A.' 'Ward, Mike' _publ_contact_author ; Prof. J. A. McCleverty School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; _publ_contact_author_fax 0117 9290509 _publ_contact_author_email jon.mccleverty@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper 'Donor acceptor complexes incorporating ferrocenes...' by M. Malaun, et al, submitted to Dalton Transactions for publication. ; #======================================================== data_fcm _database_code_CSD 165091 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H53 B Cl Fe Mo N8 O' _chemical_formula_weight 859.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1843(10) _cell_length_b 13.8687(15) _cell_length_c 18.0066(19) _cell_angle_alpha 69.162(2) _cell_angle_beta 87.834(2) _cell_angle_gamma 71.966(2) _cell_volume 2031.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17786 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.1162 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7134 _reflns_number_gt 4329 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0535P)^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 7134 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1103 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _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 Mo1 Mo 0.30839(6) 0.16264(4) 0.13954(3) 0.02398(14) Uani 1 1 d . . . Fe2 Fe 0.87596(8) 0.28754(6) 0.51997(4) 0.0234(2) Uani 1 1 d . . . Cl1 Cl 0.10360(19) 0.21255(14) 0.22193(9) 0.0518(4) Uani 1 1 d . . . O1 O 0.3295(6) -0.0638(4) 0.2052(3) 0.0515(13) Uani 1 1 d . . . N100 N 0.3206(6) 0.0146(5) 0.1799(3) 0.0374(14) Uani 1 1 d . . . N1 N 0.3054(5) 0.3353(3) 0.0941(3) 0.0307(11) Uani 1 1 d . . . N2 N 0.2927(5) 0.3889(3) 0.0120(3) 0.0307(11) Uani 1 1 d . . . N3 N 0.1664(5) 0.2795(4) -0.0332(2) 0.0313(11) Uani 1 1 d . . . N4 N 0.1442(5) 0.2097(3) 0.0396(2) 0.0275(10) Uani 1 1 d . . . N5 N 0.4516(5) 0.2285(3) -0.0215(2) 0.0256(10) Uani 1 1 d . . . N6 N 0.4762(5) 0.1435(3) 0.0523(2) 0.0251(10) Uani 1 1 d . . . N31 N 0.4898(5) 0.1298(3) 0.2293(2) 0.0245(10) Uani 1 1 d . . . C3 C 0.0611(6) 0.2885(4) -0.0879(3) 0.0310(13) Uani 1 1 d . . . C4 C 0.0539(7) 0.3577(5) -0.1746(3) 0.0509(17) Uani 1 1 d . . . H4A H 0.0503 0.4311 -0.1794 0.076 Uiso 1 1 calc R . . H4B H -0.0384 0.3617 -0.2026 0.076 Uiso 1 1 calc R . . H4C H 0.1453 0.3255 -0.1982 0.076 Uiso 1 1 calc R . . C5 C -0.0269(6) 0.2234(5) -0.0513(3) 0.0366(14) Uani 1 1 d . . . H5 H -0.1075 0.2127 -0.0757 0.044 Uiso 1 1 calc R . . C6 C 0.0270(6) 0.1762(4) 0.0293(3) 0.0308(13) Uani 1 1 d . . . C7 C -0.0293(7) 0.1007(5) 0.0967(3) 0.0420(15) Uani 1 1 d . . . H7A H 0.0294 0.0253 0.1039 0.063 Uiso 1 1 calc R . . H7B H -0.1384 0.1133 0.0850 0.063 Uiso 1 1 calc R . . H7C H -0.0161 0.1137 0.1457 0.063 Uiso 1 1 calc R . . C13 C 0.5624(6) 0.1991(4) -0.0680(3) 0.0264(12) Uani 1 1 d . . . C14 C 0.5681(7) 0.2723(5) -0.1528(3) 0.0359(14) Uani 1 1 d . . . H14A H 0.4810 0.2787 -0.1861 0.054 Uiso 1 1 calc R . . H14B H 0.6644 0.2411 -0.1734 0.054 Uiso 1 1 calc R . . H14C H 0.5624 0.3445 -0.1539 0.054 Uiso 1 1 calc R . . C15 C 0.6575(6) 0.0973(4) -0.0254(3) 0.0303(13) Uani 1 1 d . . . H15 H 0.7454 0.0565 -0.0432 0.036 Uiso 1 1 calc R . . C16 C 0.6009(6) 0.0645(4) 0.0495(3) 0.0256(12) Uani 1 1 d . . . C17 C 0.6638(6) -0.0403(4) 0.1186(3) 0.0337(14) Uani 1 1 d . . . H17A H 0.6707 -0.0249 0.1672 0.051 Uiso 1 1 calc R . . H17B H 0.7663 -0.0801 0.1085 0.051 Uiso 1 1 calc R . . H17C H 0.5955 -0.0844 0.1252 0.051 Uiso 1 1 calc R . . C23 C 0.2786(7) 0.4951(5) -0.0052(4) 0.0427(16) Uani 1 1 d . . . C24 C 0.2594(9) 0.5763(5) -0.0884(4) 0.065(2) Uani 1 1 d . . . H24A H 0.3438 0.5499 -0.1184 0.098 Uiso 1 1 calc R . . H24B H 0.2607 0.6460 -0.0868 0.098 Uiso 1 1 calc R . . H24C H 0.1613 0.5864 -0.1145 0.098 Uiso 1 1 calc R . . C25 C 0.2836(8) 0.5104(5) 0.0659(4) 0.0514(18) Uani 1 1 d . . . H25 H 0.2772 0.5765 0.0726 0.062 Uiso 1 1 calc R . . C26 C 0.3001(7) 0.4097(5) 0.1264(4) 0.0381(15) Uani 1 1 d . . . C27 C 0.3112(8) 0.3849(5) 0.2152(4) 0.0536(18) Uani 1 1 d . . . H27A H 0.2531 0.3352 0.2414 0.080 Uiso 1 1 calc R . . H27B H 0.2686 0.4526 0.2255 0.080 Uiso 1 1 calc R . . H27C H 0.4192 0.3508 0.2362 0.080 Uiso 1 1 calc R . . C32 C 0.6066(6) 0.1710(4) 0.2139(3) 0.0265(12) Uani 1 1 d . . . H32 H 0.6175 0.2107 0.1599 0.032 Uiso 1 1 calc R . . C33 C 0.7121(6) 0.1592(4) 0.2718(3) 0.0295(13) Uani 1 1 d . . . H33 H 0.7926 0.1902 0.2574 0.035 Uiso 1 1 calc R . . C34 C 0.6994(6) 0.1011(4) 0.3524(3) 0.0259(12) Uani 1 1 d . . . C35 C 0.5827(6) 0.0538(4) 0.3667(3) 0.0307(13) Uani 1 1 d . . . H35 H 0.5720 0.0104 0.4196 0.037 Uiso 1 1 calc R . . C36 C 0.4829(6) 0.0685(4) 0.3060(3) 0.0311(13) Uani 1 1 d . . . H36 H 0.4056 0.0341 0.3184 0.037 Uiso 1 1 calc R . . C37 C 0.7912(6) 0.0933(4) 0.4194(3) 0.0278(12) Uani 1 1 d . . . H37 H 0.7860 0.0404 0.4695 0.033 Uiso 1 1 calc R . . C38 C 0.8818(6) 0.1521(4) 0.4183(3) 0.0250(12) Uani 1 1 d . . . H38 H 0.9002 0.1967 0.3673 0.030 Uiso 1 1 calc R . . C51 C 0.9556(6) 0.1556(4) 0.4867(3) 0.0234(12) Uani 1 1 d . . . C52 C 0.9143(6) 0.1230(4) 0.5687(3) 0.0238(12) Uani 1 1 d . . . C53 C 0.8017(6) 0.0658(4) 0.6038(3) 0.0296(13) Uani 1 1 d . . . H53A H 0.8449 -0.0110 0.6103 0.044 Uiso 1 1 calc R . . H53B H 0.7070 0.0991 0.5684 0.044 Uiso 1 1 calc R . . H53C H 0.7789 0.0716 0.6560 0.044 Uiso 1 1 calc R . . C54 C 1.0073(6) 0.1529(4) 0.6118(3) 0.0245(12) Uani 1 1 d . . . C55 C 1.0108(6) 0.1283(4) 0.7017(3) 0.0331(14) Uani 1 1 d . . . H55A H 0.9074 0.1328 0.7192 0.050 Uiso 1 1 calc R . . H55B H 1.0461 0.1814 0.7137 0.050 Uiso 1 1 calc R . . H55C H 1.0813 0.0549 0.7297 0.050 Uiso 1 1 calc R . . C56 C 1.1035(6) 0.2044(4) 0.5597(3) 0.0264(12) Uani 1 1 d . . . C57 C 1.2227(6) 0.2440(5) 0.5837(3) 0.0382(14) Uani 1 1 d . . . H57A H 1.3211 0.1853 0.5988 0.057 Uiso 1 1 calc R . . H57B H 1.1903 0.2665 0.6291 0.057 Uiso 1 1 calc R . . H57C H 1.2341 0.3061 0.5387 0.057 Uiso 1 1 calc R . . C58 C 1.0725(6) 0.2063(4) 0.4823(3) 0.0270(12) Uani 1 1 d . . . C59 C 1.1564(6) 0.2482(5) 0.4101(3) 0.0367(14) Uani 1 1 d . . . H59A H 1.1903 0.3067 0.4141 0.055 Uiso 1 1 calc R . . H59B H 1.0873 0.2762 0.3617 0.055 Uiso 1 1 calc R . . H59C H 1.2460 0.1888 0.4077 0.055 Uiso 1 1 calc R . . C61 C 0.7559(7) 0.4282(4) 0.4282(3) 0.0343(14) Uani 1 1 d . . . C62 C 0.7770(8) 0.4582(5) 0.3402(3) 0.0541(19) Uani 1 1 d . . . H62A H 0.7503 0.4075 0.3209 0.081 Uiso 1 1 calc R . . H62B H 0.8843 0.4541 0.3312 0.081 Uiso 1 1 calc R . . H62C H 0.7099 0.5324 0.3112 0.081 Uiso 1 1 calc R . . C63 C 0.6528(6) 0.3762(4) 0.4709(3) 0.0299(13) Uani 1 1 d . . . C64 C 0.5405(7) 0.3403(5) 0.4376(4) 0.0461(16) Uani 1 1 d . . . H64A H 0.4381 0.3941 0.4292 0.069 Uiso 1 1 calc R . . H64B H 0.5375 0.2697 0.4751 0.069 Uiso 1 1 calc R . . H64C H 0.5725 0.3336 0.3866 0.069 Uiso 1 1 calc R . . C65 C 0.6688(6) 0.3660(4) 0.5522(3) 0.0317(13) Uani 1 1 d . . . C66 C 0.5735(7) 0.3209(5) 0.6176(4) 0.0500(17) Uani 1 1 d . . . H66A H 0.4815 0.3795 0.6186 0.075 Uiso 1 1 calc R . . H66B H 0.6342 0.2891 0.6690 0.075 Uiso 1 1 calc R . . H66C H 0.5430 0.2646 0.6075 0.075 Uiso 1 1 calc R . . C67 C 0.7813(7) 0.4128(4) 0.5599(3) 0.0337(14) Uani 1 1 d . . . C68 C 0.8340(8) 0.4214(5) 0.6346(4) 0.0554(19) Uani 1 1 d . . . H68A H 0.9442 0.4123 0.6349 0.083 Uiso 1 1 calc R . . H68B H 0.8151 0.3645 0.6812 0.083 Uiso 1 1 calc R . . H68C H 0.7772 0.4929 0.6365 0.083 Uiso 1 1 calc R . . C69 C 0.8349(7) 0.4500(4) 0.4833(4) 0.0394(15) Uani 1 1 d . . . H69 H 0.9153 0.4870 0.4700 0.047 Uiso 1 1 calc R . . B1 B 0.3029(7) 0.3252(5) -0.0432(4) 0.0308(15) Uani 1 1 d . . . H1 H 0.3003 0.3741 -0.0998 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0277(3) 0.0321(3) 0.0117(2) -0.0045(2) 0.00180(19) -0.0131(2) Fe2 0.0264(5) 0.0262(4) 0.0158(4) -0.0041(3) 0.0006(3) -0.0100(4) Cl1 0.0563(11) 0.0610(10) 0.0363(9) -0.0120(8) -0.0019(8) -0.0220(9) O1 0.058(3) 0.072(3) 0.041(3) -0.035(3) 0.011(2) -0.026(3) N100 0.031(3) 0.083(4) 0.011(3) -0.026(3) 0.008(2) -0.025(3) N1 0.034(3) 0.031(3) 0.022(3) -0.006(2) -0.003(2) -0.008(2) N2 0.033(3) 0.029(3) 0.023(3) -0.004(2) 0.002(2) -0.007(2) N3 0.032(3) 0.040(3) 0.014(2) 0.000(2) -0.002(2) -0.011(2) N4 0.030(3) 0.035(3) 0.014(2) -0.003(2) 0.007(2) -0.013(2) N5 0.028(3) 0.034(3) 0.011(2) -0.003(2) 0.0024(19) -0.012(2) N6 0.029(3) 0.027(2) 0.016(2) -0.0010(19) -0.0011(19) -0.012(2) N31 0.028(3) 0.030(2) 0.017(2) -0.005(2) 0.004(2) -0.014(2) C3 0.027(3) 0.042(3) 0.017(3) -0.007(3) -0.005(2) -0.004(3) C4 0.050(4) 0.076(5) 0.019(3) -0.003(3) -0.006(3) -0.025(4) C5 0.032(3) 0.052(4) 0.023(3) -0.011(3) -0.004(3) -0.012(3) C6 0.027(3) 0.041(3) 0.027(3) -0.014(3) 0.002(3) -0.013(3) C7 0.043(4) 0.061(4) 0.026(3) -0.008(3) 0.004(3) -0.031(3) C13 0.030(3) 0.038(3) 0.019(3) -0.012(3) 0.008(2) -0.020(3) C14 0.044(4) 0.050(4) 0.016(3) -0.010(3) 0.009(3) -0.022(3) C15 0.030(3) 0.039(3) 0.028(3) -0.017(3) 0.005(3) -0.013(3) C16 0.025(3) 0.036(3) 0.019(3) -0.009(2) 0.002(2) -0.015(3) C17 0.036(3) 0.035(3) 0.030(3) -0.011(3) 0.004(3) -0.013(3) C23 0.053(4) 0.029(3) 0.031(4) 0.000(3) 0.004(3) -0.006(3) C24 0.098(6) 0.033(4) 0.044(4) 0.009(3) 0.011(4) -0.022(4) C25 0.073(5) 0.033(4) 0.050(4) -0.016(3) 0.014(4) -0.019(3) C26 0.045(4) 0.031(3) 0.038(4) -0.019(3) 0.004(3) -0.006(3) C27 0.075(5) 0.050(4) 0.041(4) -0.026(4) 0.005(4) -0.015(4) C32 0.028(3) 0.033(3) 0.017(3) -0.005(2) 0.004(2) -0.011(3) C33 0.031(3) 0.037(3) 0.025(3) -0.011(3) 0.006(3) -0.017(3) C34 0.031(3) 0.024(3) 0.019(3) -0.006(2) 0.000(2) -0.006(2) C35 0.043(4) 0.036(3) 0.018(3) -0.010(3) 0.003(3) -0.020(3) C36 0.036(3) 0.040(3) 0.023(3) -0.009(3) 0.006(3) -0.022(3) C37 0.030(3) 0.033(3) 0.018(3) -0.006(2) 0.005(2) -0.010(3) C38 0.027(3) 0.025(3) 0.017(3) -0.004(2) -0.002(2) -0.004(2) C51 0.023(3) 0.032(3) 0.016(3) -0.006(2) 0.001(2) -0.011(2) C52 0.025(3) 0.027(3) 0.018(3) -0.006(2) 0.000(2) -0.010(2) C53 0.037(3) 0.034(3) 0.019(3) -0.005(2) 0.006(3) -0.019(3) C54 0.027(3) 0.032(3) 0.011(3) -0.002(2) -0.006(2) -0.009(2) C55 0.036(3) 0.038(3) 0.018(3) -0.005(3) -0.004(3) -0.007(3) C56 0.028(3) 0.027(3) 0.024(3) -0.008(2) -0.001(2) -0.010(2) C57 0.032(3) 0.047(4) 0.033(3) -0.009(3) -0.003(3) -0.015(3) C58 0.029(3) 0.029(3) 0.024(3) -0.008(2) 0.003(2) -0.012(2) C59 0.039(4) 0.050(4) 0.028(3) -0.013(3) 0.013(3) -0.026(3) C61 0.039(3) 0.034(3) 0.020(3) -0.002(3) -0.003(3) -0.007(3) C62 0.065(5) 0.048(4) 0.021(3) 0.006(3) 0.011(3) -0.001(3) C63 0.026(3) 0.034(3) 0.025(3) -0.009(3) 0.000(2) -0.005(3) C64 0.036(4) 0.053(4) 0.053(4) -0.025(4) -0.009(3) -0.010(3) C65 0.031(3) 0.029(3) 0.028(3) -0.007(3) 0.006(3) -0.004(3) C66 0.045(4) 0.061(4) 0.042(4) -0.018(3) 0.019(3) -0.018(3) C67 0.048(4) 0.026(3) 0.022(3) -0.007(2) -0.008(3) -0.004(3) C68 0.070(5) 0.049(4) 0.046(4) -0.026(4) -0.015(4) -0.004(4) C69 0.037(4) 0.031(3) 0.049(4) -0.010(3) -0.003(3) -0.013(3) B1 0.044(4) 0.031(3) 0.012(3) 0.001(3) 0.008(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N100 1.886(6) . ? Mo1 N4 2.168(4) . ? Mo1 N6 2.185(4) . ? Mo1 N31 2.193(4) . ? Mo1 N1 2.229(4) . ? Mo1 Cl1 2.4353(18) . ? Fe2 C69 2.022(5) . ? Fe2 C51 2.041(5) . ? Fe2 C58 2.044(5) . ? Fe2 C67 2.049(5) . ? Fe2 C52 2.050(5) . ? Fe2 C65 2.056(5) . ? Fe2 C54 2.058(5) . ? Fe2 C56 2.060(5) . ? Fe2 C61 2.065(5) . ? Fe2 C63 2.073(5) . ? O1 N100 0.996(6) . ? N1 C26 1.342(6) . ? N1 N2 1.389(6) . ? N2 C23 1.358(7) . ? N2 B1 1.532(7) . ? N3 C3 1.354(6) . ? N3 N4 1.377(5) . ? N3 B1 1.549(8) . ? N4 C6 1.340(6) . ? N5 C13 1.350(6) . ? N5 N6 1.396(5) . ? N5 B1 1.533(7) . ? N6 C16 1.331(6) . ? N31 C32 1.342(6) . ? N31 C36 1.351(6) . ? C3 C5 1.374(7) . ? C3 C4 1.505(7) . ? C5 C6 1.400(7) . ? C6 C7 1.490(7) . ? C13 C15 1.364(7) . ? C13 C14 1.513(7) . ? C15 C16 1.396(7) . ? C16 C17 1.497(7) . ? C23 C25 1.374(8) . ? C23 C24 1.497(8) . ? C25 C26 1.400(8) . ? C26 C27 1.511(8) . ? C32 C33 1.382(7) . ? C33 C34 1.409(7) . ? C34 C35 1.392(7) . ? C34 C37 1.451(7) . ? C35 C36 1.370(7) . ? C37 C38 1.329(7) . ? C38 C51 1.450(6) . ? C51 C58 1.441(7) . ? C51 C52 1.456(7) . ? C52 C54 1.416(7) . ? C52 C53 1.483(7) . ? C54 C56 1.422(7) . ? C54 C55 1.530(6) . ? C56 C58 1.423(7) . ? C56 C57 1.504(7) . ? C58 C59 1.512(7) . ? C61 C63 1.407(7) . ? C61 C69 1.416(7) . ? C61 C62 1.511(7) . ? C63 C65 1.427(7) . ? C63 C64 1.500(7) . ? C65 C67 1.414(8) . ? C65 C66 1.510(8) . ? C67 C69 1.417(8) . ? C67 C68 1.503(7) . ? 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 N100 Mo1 N4 95.68(18) . . ? N100 Mo1 N6 94.17(18) . . ? N4 Mo1 N6 83.28(15) . . ? N100 Mo1 N31 90.29(18) . . ? N4 Mo1 N31 172.19(16) . . ? N6 Mo1 N31 91.29(15) . . ? N100 Mo1 N1 177.3(2) . . ? N4 Mo1 N1 86.68(16) . . ? N6 Mo1 N1 84.75(15) . . ? N31 Mo1 N1 87.24(15) . . ? N100 Mo1 Cl1 93.54(16) . . ? N4 Mo1 Cl1 91.51(11) . . ? N6 Mo1 Cl1 171.09(11) . . ? N31 Mo1 Cl1 93.14(11) . . ? N1 Mo1 Cl1 87.74(12) . . ? C69 Fe2 C51 144.1(2) . . ? C69 Fe2 C58 114.2(2) . . ? C51 Fe2 C58 41.32(19) . . ? C69 Fe2 C67 40.7(2) . . ? C51 Fe2 C67 174.4(2) . . ? C58 Fe2 C67 143.7(2) . . ? C69 Fe2 C52 174.1(2) . . ? C51 Fe2 C52 41.70(19) . . ? C58 Fe2 C52 69.6(2) . . ? C67 Fe2 C52 133.6(2) . . ? C69 Fe2 C65 67.6(2) . . ? C51 Fe2 C65 134.8(2) . . ? C58 Fe2 C65 175.5(2) . . ? C67 Fe2 C65 40.3(2) . . ? C52 Fe2 C65 109.0(2) . . ? C69 Fe2 C54 135.8(2) . . ? C51 Fe2 C54 68.47(19) . . ? C58 Fe2 C54 68.2(2) . . ? C67 Fe2 C54 109.8(2) . . ? C52 Fe2 C54 40.30(19) . . ? C65 Fe2 C54 113.7(2) . . ? C69 Fe2 C56 110.9(2) . . ? C51 Fe2 C56 68.85(19) . . ? C58 Fe2 C56 40.56(19) . . ? C67 Fe2 C56 113.6(2) . . ? C52 Fe2 C56 68.7(2) . . ? C65 Fe2 C56 143.4(2) . . ? C54 Fe2 C56 40.39(19) . . ? C69 Fe2 C61 40.5(2) . . ? C51 Fe2 C61 113.5(2) . . ? C58 Fe2 C61 110.6(2) . . ? C67 Fe2 C61 68.6(2) . . ? C52 Fe2 C61 143.6(2) . . ? C65 Fe2 C61 67.8(2) . . ? C54 Fe2 C61 175.8(2) . . ? C56 Fe2 C61 136.2(2) . . ? C69 Fe2 C63 67.2(2) . . ? C51 Fe2 C63 110.0(2) . . ? C58 Fe2 C63 135.7(2) . . ? C67 Fe2 C63 68.0(2) . . ? C52 Fe2 C63 113.6(2) . . ? C65 Fe2 C63 40.4(2) . . ? C54 Fe2 C63 143.8(2) . . ? C56 Fe2 C63 175.4(2) . . ? C61 Fe2 C63 39.8(2) . . ? O1 N100 Mo1 175.8(6) . . ? C26 N1 N2 106.3(4) . . ? C26 N1 Mo1 135.9(4) . . ? N2 N1 Mo1 117.5(3) . . ? C23 N2 N1 109.7(4) . . ? C23 N2 B1 130.4(5) . . ? N1 N2 B1 119.8(4) . . ? C3 N3 N4 108.0(4) . . ? C3 N3 B1 130.7(4) . . ? N4 N3 B1 121.1(4) . . ? C6 N4 N3 108.1(4) . . ? C6 N4 Mo1 133.3(4) . . ? N3 N4 Mo1 118.2(3) . . ? C13 N5 N6 108.5(4) . . ? C13 N5 B1 129.9(4) . . ? N6 N5 B1 120.6(4) . . ? C16 N6 N5 107.2(4) . . ? C16 N6 Mo1 135.2(3) . . ? N5 N6 Mo1 117.5(3) . . ? C32 N31 C36 116.6(4) . . ? C32 N31 Mo1 124.0(3) . . ? C36 N31 Mo1 119.4(3) . . ? N3 C3 C5 109.2(5) . . ? N3 C3 C4 122.1(5) . . ? C5 C3 C4 128.7(5) . . ? C3 C5 C6 105.7(5) . . ? N4 C6 C5 108.9(5) . . ? N4 C6 C7 122.3(5) . . ? C5 C6 C7 128.8(5) . . ? N5 C13 C15 108.3(5) . . ? N5 C13 C14 122.3(5) . . ? C15 C13 C14 129.5(5) . . ? C13 C15 C16 106.9(5) . . ? N6 C16 C15 109.1(5) . . ? N6 C16 C17 122.6(4) . . ? C15 C16 C17 128.3(5) . . ? N2 C23 C25 107.6(5) . . ? N2 C23 C24 123.4(6) . . ? C25 C23 C24 129.0(6) . . ? C23 C25 C26 106.6(5) . . ? N1 C26 C25 109.7(5) . . ? N1 C26 C27 123.6(5) . . ? C25 C26 C27 126.7(5) . . ? N31 C32 C33 123.9(5) . . ? C32 C33 C34 119.6(5) . . ? C35 C34 C33 115.5(5) . . ? C35 C34 C37 119.4(5) . . ? C33 C34 C37 125.0(5) . . ? C36 C35 C34 121.5(5) . . ? N31 C36 C35 122.7(5) . . ? C38 C37 C34 127.1(5) . . ? C37 C38 C51 126.9(5) . . ? C58 C51 C38 124.5(5) . . ? C58 C51 C52 107.5(4) . . ? C38 C51 C52 127.6(5) . . ? C58 C51 Fe2 69.5(3) . . ? C38 C51 Fe2 120.4(3) . . ? C52 C51 Fe2 69.5(3) . . ? C54 C52 C51 106.8(4) . . ? C54 C52 C53 124.9(4) . . ? C51 C52 C53 128.3(4) . . ? C54 C52 Fe2 70.1(3) . . ? C51 C52 Fe2 68.8(3) . . ? C53 C52 Fe2 127.7(4) . . ? C52 C54 C56 109.7(4) . . ? C52 C54 C55 125.4(5) . . ? C56 C54 C55 124.8(5) . . ? C52 C54 Fe2 69.5(3) . . ? C56 C54 Fe2 69.9(3) . . ? C55 C54 Fe2 129.6(4) . . ? C54 C56 C58 107.9(4) . . ? C54 C56 C57 125.7(5) . . ? C58 C56 C57 126.3(5) . . ? C54 C56 Fe2 69.7(3) . . ? C58 C56 Fe2 69.1(3) . . ? C57 C56 Fe2 129.1(4) . . ? C56 C58 C51 108.1(4) . . ? C56 C58 C59 125.1(5) . . ? C51 C58 C59 126.7(5) . . ? C56 C58 Fe2 70.3(3) . . ? C51 C58 Fe2 69.2(3) . . ? C59 C58 Fe2 129.0(4) . . ? C63 C61 C69 106.9(5) . . ? C63 C61 C62 127.2(5) . . ? C69 C61 C62 125.9(6) . . ? C63 C61 Fe2 70.4(3) . . ? C69 C61 Fe2 68.1(3) . . ? C62 C61 Fe2 127.5(4) . . ? C61 C63 C65 108.4(5) . . ? C61 C63 C64 126.6(5) . . ? C65 C63 C64 124.9(5) . . ? C61 C63 Fe2 69.8(3) . . ? C65 C63 Fe2 69.1(3) . . ? C64 C63 Fe2 128.4(4) . . ? C67 C65 C63 108.4(5) . . ? C67 C65 C66 125.5(5) . . ? C63 C65 C66 125.9(5) . . ? C67 C65 Fe2 69.6(3) . . ? C63 C65 Fe2 70.4(3) . . ? C66 C65 Fe2 129.2(4) . . ? C65 C67 C69 106.6(5) . . ? C65 C67 C68 126.7(6) . . ? C69 C67 C68 126.7(6) . . ? C65 C67 Fe2 70.1(3) . . ? C69 C67 Fe2 68.6(3) . . ? C68 C67 Fe2 126.1(4) . . ? C61 C69 C67 109.8(5) . . ? C61 C69 Fe2 71.4(3) . . ? C67 C69 Fe2 70.6(3) . . ? N2 B1 N5 110.2(5) . . ? N2 B1 N3 109.8(4) . . ? N5 B1 N3 107.7(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.611 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.098 #=END data_tpstarm _database_code_CSD 165092 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H73 B2 Cl4 Fe2 Mo2 N16 O2' _chemical_formula_weight 1445.28 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3036(14) _cell_length_b 12.1739(16) _cell_length_c 23.272(3) _cell_angle_alpha 89.163(3) _cell_angle_beta 87.426(3) _cell_angle_gamma 76.802(3) _cell_volume 3114.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1478 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32882 _diffrn_reflns_av_R_equivalents 0.1219 _diffrn_reflns_av_sigmaI/netI 0.2073 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.54 _reflns_number_total 14154 _reflns_number_gt 6257 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0813P)^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 14154 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1976 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2042 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.52467(7) 0.24073(6) 0.24892(3) 0.0289(2) Uani 1 1 d . . . Mo2 Mo 0.93670(7) 0.58488(7) 0.30272(3) 0.0316(2) Uani 1 1 d . . . Fe1 Fe 0.39370(11) 0.53109(11) 0.11968(5) 0.0353(3) Uani 1 1 d . . . Fe2 Fe 0.91177(11) 0.29238(11) 0.42968(5) 0.0361(3) Uani 1 1 d . . . Cl1 Cl 0.6938(2) 0.33272(19) 0.23733(10) 0.0379(5) Uani 1 1 d . . . Cl2 Cl 1.1452(2) 0.4780(2) 0.31274(10) 0.0406(6) Uani 1 1 d . . . Cl10 Cl 0.2249(4) 0.7040(3) 0.97652(15) 0.0981(13) Uani 1 1 d . . . Cl11 Cl 0.0505(7) 0.8742(4) 0.9249(3) 0.214(4) Uani 1 1 d . . . O1 O 0.5896(6) 0.1239(5) 0.1368(3) 0.0480(18) Uani 1 1 d . . . O2 O 0.9382(6) 0.7051(6) 0.4128(3) 0.0537(19) Uani 1 1 d . . . N1 N 0.3955(6) 0.3594(6) 0.2195(3) 0.0306(17) Uani 1 1 d . . . H102 H 0.3544 0.3997 0.2481 0.037 Uiso 1 1 calc R . . N2 N 0.5631(6) 0.1689(6) 0.1825(3) 0.0337(18) Uani 1 1 d . . . N3 N 0.3994(6) 0.1404(6) 0.2786(3) 0.0318(17) Uani 1 1 d . . . N4 N 0.3933(6) 0.1070(6) 0.3355(3) 0.0290(17) Uani 1 1 d . . . N5 N 0.6469(6) 0.1102(6) 0.3003(3) 0.0308(17) Uani 1 1 d . . . N6 N 0.6113(6) 0.0906(6) 0.3561(3) 0.0307(17) Uani 1 1 d . . . N7 N 0.4747(6) 0.3311(6) 0.3327(3) 0.0320(17) Uani 1 1 d . . . N8 N 0.4580(6) 0.2704(6) 0.3814(3) 0.0289(16) Uani 1 1 d . . . N9 N 0.8536(6) 0.4715(6) 0.3328(3) 0.0311(17) Uani 1 1 d . . . H101 H 0.8308 0.4335 0.3051 0.037 Uiso 1 1 calc R . . N10 N 0.9365(7) 0.6550(6) 0.3682(3) 0.040(2) Uani 1 1 d . . . N11 N 0.9393(7) 0.5016(6) 0.2168(3) 0.0344(18) Uani 1 1 d . . . N12 N 0.9037(6) 0.5692(6) 0.1702(3) 0.0347(18) Uani 1 1 d . . . N13 N 0.7700(6) 0.6970(6) 0.2750(3) 0.0328(17) Uani 1 1 d . . . N14 N 0.7622(7) 0.7323(6) 0.2193(3) 0.0357(18) Uani 1 1 d . . . N15 N 1.0129(7) 0.7122(6) 0.2529(3) 0.0351(18) Uani 1 1 d . . . N16 N 0.9794(7) 0.7369(6) 0.1976(3) 0.0368(18) Uani 1 1 d . . . C1 C 0.3481(7) 0.4002(7) 0.1670(3) 0.028(2) Uani 1 1 d . . . C2 C 0.2455(8) 0.4932(8) 0.1614(4) 0.039(2) Uani 1 1 d . . . H2 H 0.1988 0.5366 0.1917 0.047 Uiso 1 1 calc R . . C3 C 0.2275(9) 0.5076(8) 0.1005(4) 0.045(3) Uani 1 1 d . . . H3 H 0.1637 0.5614 0.0837 0.054 Uiso 1 1 calc R . . C4 C 0.3193(9) 0.4293(8) 0.0695(4) 0.043(2) Uani 1 1 d . . . H4 H 0.3276 0.4209 0.0289 0.052 Uiso 1 1 calc R . . C5 C 0.3975(8) 0.3649(8) 0.1112(4) 0.037(2) Uani 1 1 d . . . H5 H 0.4695 0.3087 0.1028 0.045 Uiso 1 1 calc R . . C6 C 0.5374(8) 0.5791(8) 0.1560(5) 0.046(3) Uani 1 1 d . . . H6 H 0.5842 0.5426 0.1866 0.055 Uiso 1 1 calc R . . C7 C 0.4315(9) 0.6670(8) 0.1623(5) 0.050(3) Uani 1 1 d . . . H7 H 0.3935 0.6991 0.1974 0.060 Uiso 1 1 calc R . . C8 C 0.3927(9) 0.6979(8) 0.1048(4) 0.047(3) Uani 1 1 d . . . H8 H 0.3246 0.7563 0.0958 0.056 Uiso 1 1 calc R . . C9 C 0.4729(9) 0.6272(9) 0.0630(5) 0.053(3) Uani 1 1 d . . . H9 H 0.4672 0.6289 0.0223 0.064 Uiso 1 1 calc R . . C10 C 0.5629(9) 0.5539(9) 0.0963(5) 0.052(3) Uani 1 1 d . . . H10 H 0.6289 0.4976 0.0810 0.062 Uiso 1 1 calc R . . C11 C 0.3156(8) 0.0391(8) 0.3423(4) 0.036(2) Uani 1 1 d . . . C12 C 0.2664(8) 0.0311(7) 0.2902(4) 0.032(2) Uani 1 1 d . . . H12 H 0.2071 -0.0102 0.2825 0.038 Uiso 1 1 calc R . . C13 C 0.3191(8) 0.0941(7) 0.2509(4) 0.032(2) Uani 1 1 d . . . C14 C 0.2936(8) -0.0134(7) 0.3986(4) 0.040(2) Uani 1 1 d . . . H14A H 0.3708 -0.0581 0.4122 0.060 Uiso 1 1 calc R . . H14B H 0.2370 -0.0624 0.3941 0.060 Uiso 1 1 calc R . . H14C H 0.2587 0.0458 0.4266 0.060 Uiso 1 1 calc R . . C15 C 0.3000(8) 0.1105(8) 0.1892(4) 0.040(2) Uani 1 1 d . . . H15A H 0.2690 0.1909 0.1812 0.060 Uiso 1 1 calc R . . H15B H 0.2409 0.0682 0.1777 0.060 Uiso 1 1 calc R . . H15C H 0.3773 0.0833 0.1676 0.060 Uiso 1 1 calc R . . C16 C 0.7582(8) 0.0420(7) 0.2905(4) 0.035(2) Uani 1 1 d . . . C17 C 0.7924(9) -0.0199(7) 0.3407(4) 0.040(2) Uani 1 1 d . . . H17 H 0.8666 -0.0737 0.3458 0.048 Uiso 1 1 calc R . . C18 C 0.6996(8) 0.0113(7) 0.3811(4) 0.034(2) Uani 1 1 d . . . C19 C 0.8244(8) 0.0391(8) 0.2335(4) 0.045(3) Uani 1 1 d . . . H19A H 0.7787 0.0112 0.2043 0.068 Uiso 1 1 calc R . . H19B H 0.9053 -0.0112 0.2356 0.068 Uiso 1 1 calc R . . H19C H 0.8327 0.1153 0.2230 0.068 Uiso 1 1 calc R . . C20 C 0.6915(8) -0.0234(8) 0.4427(4) 0.044(3) Uani 1 1 d . . . H20A H 0.6959 0.0399 0.4674 0.067 Uiso 1 1 calc R . . H20B H 0.7592 -0.0875 0.4503 0.067 Uiso 1 1 calc R . . H20C H 0.6143 -0.0454 0.4507 0.067 Uiso 1 1 calc R . . C21 C 0.4542(7) 0.4399(7) 0.3503(4) 0.033(2) Uani 1 1 d . . . C22 C 0.4265(7) 0.4475(8) 0.4077(3) 0.033(2) Uani 1 1 d . . . H22 H 0.4087 0.5145 0.4300 0.039 Uiso 1 1 calc R . . C23 C 0.4290(7) 0.3397(9) 0.4276(3) 0.036(2) Uani 1 1 d . . . C24 C 0.4650(8) 0.5380(8) 0.3086(3) 0.038(2) Uani 1 1 d . . . H24A H 0.5493 0.5274 0.2937 0.056 Uiso 1 1 calc R . . H24B H 0.4411 0.6098 0.3293 0.056 Uiso 1 1 calc R . . H24C H 0.4115 0.5388 0.2766 0.056 Uiso 1 1 calc R . . C25 C 0.4039(9) 0.3013(8) 0.4865(4) 0.044(2) Uani 1 1 d . . . H25A H 0.3451 0.2534 0.4854 0.066 Uiso 1 1 calc R . . H25B H 0.3703 0.3669 0.5109 0.066 Uiso 1 1 calc R . . H25C H 0.4796 0.2580 0.5022 0.066 Uiso 1 1 calc R . . C26 C 0.8209(7) 0.4350(8) 0.3870(4) 0.035(2) Uani 1 1 d . . . C27 C 0.8640(9) 0.4632(8) 0.4405(4) 0.043(3) Uani 1 1 d . . . H27 H 0.9203 0.5144 0.4461 0.052 Uiso 1 1 calc R . . C28 C 0.8071(10) 0.4064(9) 0.4850(4) 0.055(3) Uani 1 1 d . . . H28 H 0.8192 0.4104 0.5272 0.066 Uiso 1 1 calc R . . C29 C 0.7354(9) 0.3417(10) 0.4598(5) 0.061(3) Uani 1 1 d . . . H29 H 0.6873 0.2929 0.4807 0.073 Uiso 1 1 calc R . . C30 C 0.7448(8) 0.3568(9) 0.3984(4) 0.048(3) Uani 1 1 d . . . H30 H 0.7040 0.3209 0.3690 0.058 Uiso 1 1 calc R . . C31 C 1.0800(9) 0.2326(8) 0.3912(4) 0.047(3) Uani 1 1 d . . . H31 H 1.1219 0.2718 0.3613 0.056 Uiso 1 1 calc R . . C32 C 1.0026(9) 0.1580(8) 0.3815(4) 0.047(3) Uani 1 1 d . . . H32 H 0.9788 0.1376 0.3429 0.056 Uiso 1 1 calc R . . C33 C 0.9636(9) 0.1188(8) 0.4342(4) 0.047(3) Uani 1 1 d . . . H33 H 0.9084 0.0657 0.4400 0.057 Uiso 1 1 calc R . . C34 C 1.0172(9) 0.1679(8) 0.4777(4) 0.042(3) Uani 1 1 d . . . H34 H 1.0067 0.1558 0.5201 0.051 Uiso 1 1 calc R . . C35 C 1.0892(8) 0.2368(8) 0.4510(5) 0.046(3) Uani 1 1 d . . . H35 H 1.1378 0.2819 0.4714 0.055 Uiso 1 1 calc R . . C36 C 0.9764(8) 0.3956(7) 0.1966(4) 0.032(2) Uani 1 1 d . . . C37 C 0.9669(8) 0.3947(8) 0.1385(4) 0.044(3) Uani 1 1 d . . . H37 H 0.9876 0.3305 0.1142 0.053 Uiso 1 1 calc R . . C38 C 0.9205(8) 0.5071(8) 0.1213(4) 0.032(2) Uani 1 1 d . . . C39 C 1.0214(8) 0.2950(8) 0.2362(4) 0.045(3) Uani 1 1 d . . . H39A H 1.1020 0.2973 0.2493 0.068 Uiso 1 1 calc R . . H39B H 1.0267 0.2248 0.2152 0.068 Uiso 1 1 calc R . . H39C H 0.9645 0.2984 0.2695 0.068 Uiso 1 1 calc R . . C40 C 0.8931(9) 0.5552(9) 0.0626(4) 0.053(3) Uani 1 1 d . . . H40A H 0.8100 0.6018 0.0631 0.080 Uiso 1 1 calc R . . H40B H 0.9009 0.4937 0.0350 0.080 Uiso 1 1 calc R . . H40C H 0.9506 0.6017 0.0513 0.080 Uiso 1 1 calc R . . C41 C 0.6676(8) 0.7460(7) 0.3036(4) 0.037(2) Uani 1 1 d . . . C42 C 0.5895(8) 0.8121(8) 0.2660(4) 0.040(2) Uani 1 1 d . . . H42 H 0.5100 0.8559 0.2748 0.048 Uiso 1 1 calc R . . C43 C 0.6515(9) 0.8012(7) 0.2129(4) 0.040(2) Uani 1 1 d . . . C44 C 0.6455(9) 0.7238(9) 0.3655(4) 0.051(3) Uani 1 1 d . . . H44A H 0.6427 0.6445 0.3709 0.076 Uiso 1 1 calc R . . H44B H 0.5678 0.7721 0.3789 0.076 Uiso 1 1 calc R . . H44C H 0.7113 0.7402 0.3875 0.076 Uiso 1 1 calc R . . C45 C 0.6103(9) 0.8560(8) 0.1555(4) 0.047(3) Uani 1 1 d . . . H45A H 0.6670 0.9013 0.1415 0.070 Uiso 1 1 calc R . . H45B H 0.5286 0.9046 0.1609 0.070 Uiso 1 1 calc R . . H45C H 0.6088 0.7971 0.1275 0.070 Uiso 1 1 calc R . . C46 C 1.1058(9) 0.7627(8) 0.2614(4) 0.042(2) Uani 1 1 d . . . C47 C 1.1311(9) 0.8157(8) 0.2123(4) 0.044(3) Uani 1 1 d . . . H47 H 1.1940 0.8555 0.2070 0.053 Uiso 1 1 calc R . . C48 C 1.0513(9) 0.8029(8) 0.1713(4) 0.045(3) Uani 1 1 d . . . C49 C 1.1654(10) 0.7573(9) 0.3174(4) 0.053(3) Uani 1 1 d . . . H49A H 1.1117 0.8075 0.3450 0.080 Uiso 1 1 calc R . . H49B H 1.2423 0.7812 0.3119 0.080 Uiso 1 1 calc R . . H49C H 1.1814 0.6798 0.3321 0.080 Uiso 1 1 calc R . . C50 C 1.0334(10) 0.8431(9) 0.1119(4) 0.052(3) Uani 1 1 d . . . H50A H 1.0913 0.8896 0.1013 0.078 Uiso 1 1 calc R . . H50B H 0.9502 0.8881 0.1086 0.078 Uiso 1 1 calc R . . H50C H 1.0468 0.7782 0.0860 0.078 Uiso 1 1 calc R . . C600 C 0.736(3) 0.8442(18) 0.9837(10) 0.189(12) Uani 1 1 d . . . C601 C 0.666(3) 1.006(3) 0.9833(12) 0.278(19) Uani 1 1 d . . . C602 C 0.568(4) 0.970(6) 0.9910(13) 0.408(16) Uani 1 1 d . . . C999 C 0.1930(14) 0.7913(14) 0.9172(6) 0.103(5) Uani 1 1 d . . . B1 B 0.4799(10) 0.1419(9) 0.3784(5) 0.036(3) Uani 1 1 d . . . H100 H 0.4658 0.1109 0.4175 0.043 Uiso 1 1 calc R . . B2 B 0.8693(10) 0.6960(9) 0.1754(4) 0.037(3) Uani 1 1 d . . . H200 H 0.8470 0.7308 0.1371 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0238(4) 0.0324(4) 0.0288(4) 0.0005(3) -0.0030(3) -0.0024(3) Mo2 0.0249(4) 0.0371(5) 0.0314(4) -0.0041(4) -0.0034(3) -0.0033(4) Fe1 0.0260(7) 0.0413(8) 0.0374(8) 0.0086(6) -0.0030(6) -0.0056(6) Fe2 0.0231(7) 0.0454(8) 0.0361(7) 0.0022(6) -0.0048(6) 0.0003(6) Cl1 0.0256(12) 0.0435(14) 0.0444(13) 0.0014(11) -0.0022(10) -0.0075(10) Cl2 0.0257(12) 0.0461(14) 0.0478(14) 0.0038(11) -0.0041(10) -0.0032(10) Cl10 0.106(3) 0.102(3) 0.072(2) -0.015(2) -0.024(2) 0.010(2) Cl11 0.261(8) 0.061(3) 0.298(8) -0.027(4) -0.155(6) 0.035(4) O1 0.050(5) 0.050(4) 0.037(4) -0.011(3) 0.003(3) 0.003(3) O2 0.056(5) 0.066(5) 0.044(4) -0.020(4) -0.005(3) -0.023(4) N1 0.028(4) 0.034(4) 0.029(4) -0.002(3) -0.006(3) -0.006(3) N2 0.028(4) 0.037(4) 0.033(4) 0.002(4) 0.000(3) -0.001(3) N3 0.020(4) 0.036(4) 0.037(4) -0.006(3) -0.001(3) -0.001(3) N4 0.025(4) 0.032(4) 0.028(4) 0.005(3) -0.002(3) -0.003(3) N5 0.027(4) 0.032(4) 0.032(4) 0.002(3) -0.001(3) -0.002(3) N6 0.029(4) 0.026(4) 0.036(4) 0.008(3) -0.009(3) -0.002(3) N7 0.022(4) 0.041(5) 0.035(4) 0.004(4) -0.008(3) -0.011(3) N8 0.024(4) 0.037(4) 0.026(4) 0.004(3) -0.004(3) -0.007(3) N9 0.023(4) 0.031(4) 0.035(4) 0.001(3) -0.004(3) 0.002(3) N10 0.033(5) 0.049(5) 0.034(4) -0.009(4) 0.006(4) -0.002(4) N11 0.034(4) 0.042(5) 0.027(4) 0.003(4) -0.011(3) -0.005(4) N12 0.025(4) 0.040(5) 0.040(4) -0.005(4) 0.004(3) -0.009(3) N13 0.028(4) 0.034(4) 0.034(4) -0.009(3) -0.001(3) -0.002(3) N14 0.028(4) 0.044(5) 0.029(4) 0.008(4) -0.008(3) 0.003(4) N15 0.033(5) 0.031(4) 0.041(5) -0.005(4) -0.002(4) -0.006(4) N16 0.030(4) 0.041(5) 0.040(5) -0.001(4) -0.002(4) -0.009(4) C1 0.022(5) 0.032(5) 0.028(5) 0.006(4) -0.007(4) -0.001(4) C2 0.025(5) 0.045(6) 0.046(6) 0.009(5) -0.009(4) -0.003(4) C3 0.033(6) 0.054(6) 0.051(6) 0.026(5) -0.011(5) -0.014(5) C4 0.046(6) 0.061(7) 0.024(5) 0.008(5) -0.008(4) -0.015(5) C5 0.030(5) 0.040(5) 0.040(5) 0.005(4) -0.001(4) -0.004(4) C6 0.027(5) 0.052(6) 0.064(7) 0.011(5) -0.010(5) -0.021(5) C7 0.042(6) 0.046(6) 0.064(7) 0.006(5) -0.015(5) -0.011(5) C8 0.036(6) 0.042(6) 0.060(7) 0.015(5) -0.007(5) -0.006(5) C9 0.042(6) 0.063(7) 0.053(6) 0.030(6) 0.001(5) -0.011(6) C10 0.036(6) 0.047(6) 0.074(8) 0.006(6) 0.012(5) -0.013(5) C11 0.030(5) 0.037(5) 0.040(5) 0.001(4) -0.003(4) -0.005(4) C12 0.021(5) 0.027(5) 0.047(6) -0.003(4) -0.005(4) -0.004(4) C13 0.022(5) 0.039(5) 0.035(5) -0.001(4) -0.007(4) -0.006(4) C14 0.038(6) 0.036(5) 0.043(6) -0.003(4) 0.001(4) -0.004(4) C15 0.032(5) 0.043(6) 0.044(6) -0.005(5) -0.010(4) -0.003(4) C16 0.021(5) 0.034(5) 0.045(6) -0.006(4) -0.003(4) 0.005(4) C17 0.035(6) 0.028(5) 0.052(6) 0.002(5) -0.011(5) 0.001(4) C18 0.025(5) 0.025(5) 0.050(6) -0.001(4) -0.007(4) -0.004(4) C19 0.026(5) 0.044(6) 0.060(7) 0.000(5) -0.002(5) 0.004(4) C20 0.034(6) 0.049(6) 0.044(6) 0.012(5) -0.009(4) 0.002(5) C21 0.015(4) 0.029(5) 0.053(6) -0.007(4) -0.005(4) 0.000(4) C22 0.022(5) 0.047(6) 0.027(5) -0.004(4) -0.001(4) -0.004(4) C23 0.019(5) 0.065(7) 0.021(5) -0.007(5) -0.002(4) -0.001(4) C24 0.039(6) 0.051(6) 0.027(5) -0.010(4) 0.008(4) -0.021(5) C25 0.038(6) 0.060(7) 0.032(5) -0.007(5) -0.004(4) -0.005(5) C26 0.016(5) 0.046(6) 0.034(5) -0.001(4) 0.001(4) 0.011(4) C27 0.041(6) 0.042(6) 0.035(5) -0.001(5) -0.005(4) 0.014(5) C28 0.041(7) 0.069(8) 0.038(6) 0.014(6) 0.003(5) 0.020(6) C29 0.017(5) 0.090(9) 0.068(8) 0.039(7) -0.001(5) 0.001(6) C30 0.026(5) 0.064(7) 0.053(6) 0.004(6) -0.014(5) -0.007(5) C31 0.033(6) 0.044(6) 0.055(7) 0.000(5) 0.007(5) 0.006(5) C32 0.040(6) 0.052(7) 0.042(6) -0.004(5) -0.014(5) 0.004(5) C33 0.044(6) 0.045(6) 0.054(6) 0.010(5) -0.008(5) -0.011(5) C34 0.045(6) 0.046(6) 0.026(5) -0.003(4) -0.010(4) 0.010(5) C35 0.025(5) 0.040(6) 0.068(7) -0.004(5) -0.007(5) 0.002(4) C36 0.022(5) 0.037(5) 0.036(5) -0.014(4) 0.003(4) -0.001(4) C37 0.030(6) 0.050(6) 0.056(6) -0.025(5) 0.007(5) -0.015(5) C38 0.027(5) 0.040(6) 0.034(5) -0.011(4) -0.003(4) -0.018(4) C39 0.019(5) 0.049(6) 0.061(6) -0.030(5) -0.002(4) 0.008(4) C40 0.044(7) 0.070(8) 0.046(6) -0.016(6) -0.001(5) -0.013(6) C41 0.032(5) 0.035(5) 0.046(6) -0.012(4) 0.004(4) -0.011(4) C42 0.027(5) 0.040(6) 0.047(6) 0.006(5) 0.002(4) 0.002(4) C43 0.039(6) 0.030(5) 0.049(6) 0.002(5) -0.011(5) -0.005(4) C44 0.031(6) 0.069(7) 0.048(6) -0.026(5) 0.005(5) 0.001(5) C45 0.038(6) 0.045(6) 0.058(7) 0.012(5) -0.014(5) -0.009(5) C46 0.036(6) 0.029(5) 0.059(7) -0.002(5) -0.004(5) -0.002(4) C47 0.033(6) 0.035(6) 0.063(7) -0.018(5) 0.010(5) -0.006(5) C48 0.033(6) 0.055(7) 0.044(6) -0.007(5) 0.007(5) -0.003(5) C49 0.050(7) 0.050(7) 0.066(7) -0.008(6) -0.010(6) -0.022(6) C50 0.058(7) 0.059(7) 0.041(6) 0.007(5) -0.001(5) -0.017(6) C600 0.27(4) 0.112(17) 0.16(2) -0.007(15) -0.03(2) 0.007(18) C601 0.28(4) 0.39(5) 0.21(3) -0.18(3) 0.01(3) -0.17(4) C602 0.47(5) 0.86(6) 0.08(2) 0.13(3) -0.09(3) -0.529 C999 0.096(12) 0.137(14) 0.089(11) 0.027(10) 0.002(9) -0.059(11) B1 0.038(7) 0.036(6) 0.035(6) -0.003(5) -0.006(5) -0.006(5) B2 0.033(6) 0.049(7) 0.030(6) -0.005(5) -0.007(5) -0.012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 1.775(7) . ? Mo1 N1 1.946(7) . ? Mo1 N3 2.157(7) . ? Mo1 N5 2.225(7) . ? Mo1 N7 2.238(7) . ? Mo1 Cl1 2.430(2) . ? Mo2 N10 1.758(8) . ? Mo2 N9 1.945(7) . ? Mo2 N13 2.177(7) . ? Mo2 N15 2.226(7) . ? Mo2 N11 2.252(7) . ? Mo2 Cl2 2.438(2) . ? Fe1 C5 2.027(9) . ? Fe1 C3 2.034(10) . ? Fe1 C2 2.039(9) . ? Fe1 C10 2.043(10) . ? Fe1 C4 2.053(10) . ? Fe1 C8 2.053(9) . ? Fe1 C9 2.059(9) . ? Fe1 C6 2.065(9) . ? Fe1 C1 2.072(8) . ? Fe1 C7 2.077(10) . ? Fe2 C30 2.034(9) . ? Fe2 C28 2.038(10) . ? Fe2 C29 2.042(10) . ? Fe2 C27 2.042(9) . ? Fe2 C32 2.043(10) . ? Fe2 C31 2.045(9) . ? Fe2 C35 2.045(9) . ? Fe2 C34 2.053(9) . ? Fe2 C33 2.062(10) . ? Fe2 C26 2.070(8) . ? Cl10 C999 1.731(14) . ? Cl11 C999 1.697(17) . ? O1 N2 1.198(8) . ? O2 N10 1.213(9) . ? N1 C1 1.395(9) . ? N3 C13 1.360(10) . ? N3 N4 1.383(9) . ? N4 C11 1.340(11) . ? N4 B1 1.558(12) . ? N5 C16 1.352(10) . ? N5 N6 1.376(9) . ? N6 C18 1.365(10) . ? N6 B1 1.544(12) . ? N7 C21 1.358(10) . ? N7 N8 1.373(8) . ? N8 C23 1.359(10) . ? N8 B1 1.528(12) . ? N9 C26 1.394(10) . ? N11 C36 1.347(10) . ? N11 N12 1.369(9) . ? N12 C38 1.358(10) . ? N12 B2 1.508(13) . ? N13 C41 1.329(11) . ? N13 N14 1.360(9) . ? N14 C43 1.350(11) . ? N14 B2 1.537(12) . ? N15 C46 1.354(11) . ? N15 N16 1.369(9) . ? N16 C48 1.385(12) . ? N16 B2 1.552(12) . ? C1 C5 1.424(11) . ? C1 C2 1.433(11) . ? C2 C3 1.445(12) . ? C3 C4 1.416(13) . ? C4 C5 1.442(12) . ? C6 C7 1.416(13) . ? C6 C10 1.430(14) . ? C7 C8 1.445(13) . ? C8 C9 1.450(14) . ? C9 C10 1.438(13) . ? C11 C12 1.370(12) . ? C11 C14 1.483(11) . ? C12 C13 1.385(11) . ? C13 C15 1.465(11) . ? C16 C17 1.402(12) . ? C16 C19 1.491(12) . ? C17 C18 1.367(12) . ? C18 C20 1.492(12) . ? C21 C22 1.360(11) . ? C21 C24 1.549(11) . ? C22 C23 1.380(12) . ? C23 C25 1.479(11) . ? C26 C27 1.431(12) . ? C26 C30 1.435(13) . ? C27 C28 1.445(13) . ? C28 C29 1.403(15) . ? C29 C30 1.441(13) . ? C31 C35 1.402(13) . ? C31 C32 1.424(14) . ? C32 C33 1.400(12) . ? C33 C34 1.410(13) . ? C34 C35 1.415(13) . ? C36 C37 1.361(12) . ? C36 C39 1.527(12) . ? C37 C38 1.409(12) . ? C38 C40 1.494(12) . ? C41 C42 1.385(12) . ? C41 C44 1.481(12) . ? C42 C43 1.385(12) . ? C43 C45 1.527(12) . ? C46 C47 1.356(12) . ? C46 C49 1.487(13) . ? C47 C48 1.376(13) . ? C48 C50 1.468(12) . ? C600 C601 1.95(4) . ? C601 C602 1.28(4) . ? C602 C602 1.60(11) 2_677 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mo1 N1 95.7(3) . . ? N2 Mo1 N3 94.8(3) . . ? N1 Mo1 N3 92.8(3) . . ? N2 Mo1 N5 95.0(3) . . ? N1 Mo1 N5 167.4(3) . . ? N3 Mo1 N5 79.6(3) . . ? N2 Mo1 N7 179.5(3) . . ? N1 Mo1 N7 84.1(3) . . ? N3 Mo1 N7 84.8(3) . . ? N5 Mo1 N7 85.2(2) . . ? N2 Mo1 Cl1 92.1(2) . . ? N1 Mo1 Cl1 99.6(2) . . ? N3 Mo1 Cl1 165.09(19) . . ? N5 Mo1 Cl1 86.71(19) . . ? N7 Mo1 Cl1 88.28(19) . . ? N10 Mo2 N9 96.3(3) . . ? N10 Mo2 N13 94.3(3) . . ? N9 Mo2 N13 93.6(3) . . ? N10 Mo2 N15 92.9(3) . . ? N9 Mo2 N15 168.9(3) . . ? N13 Mo2 N15 79.6(3) . . ? N10 Mo2 N11 177.5(3) . . ? N9 Mo2 N11 86.1(3) . . ? N13 Mo2 N11 84.9(3) . . ? N15 Mo2 N11 84.6(3) . . ? N10 Mo2 Cl2 92.2(3) . . ? N9 Mo2 Cl2 98.2(2) . . ? N13 Mo2 Cl2 165.8(2) . . ? N15 Mo2 Cl2 87.51(19) . . ? N11 Mo2 Cl2 88.02(19) . . ? C5 Fe1 C3 68.9(4) . . ? C5 Fe1 C2 69.8(4) . . ? C3 Fe1 C2 41.5(3) . . ? C5 Fe1 C10 107.6(4) . . ? C3 Fe1 C10 151.9(4) . . ? C2 Fe1 C10 165.7(4) . . ? C5 Fe1 C4 41.4(3) . . ? C3 Fe1 C4 40.6(4) . . ? C2 Fe1 C4 69.7(4) . . ? C10 Fe1 C4 118.3(4) . . ? C5 Fe1 C8 164.7(4) . . ? C3 Fe1 C8 107.6(4) . . ? C2 Fe1 C8 118.1(4) . . ? C10 Fe1 C8 68.0(4) . . ? C4 Fe1 C8 126.5(4) . . ? C5 Fe1 C9 125.9(4) . . ? C3 Fe1 C9 116.9(4) . . ? C2 Fe1 C9 151.8(4) . . ? C10 Fe1 C9 41.1(4) . . ? C4 Fe1 C9 105.5(4) . . ? C8 Fe1 C9 41.3(4) . . ? C5 Fe1 C6 119.5(4) . . ? C3 Fe1 C6 165.4(4) . . ? C2 Fe1 C6 127.3(4) . . ? C10 Fe1 C6 40.7(4) . . ? C4 Fe1 C6 153.4(4) . . ? C8 Fe1 C6 67.5(4) . . ? C9 Fe1 C6 69.1(4) . . ? C5 Fe1 C1 40.7(3) . . ? C3 Fe1 C1 68.1(3) . . ? C2 Fe1 C1 40.8(3) . . ? C10 Fe1 C1 128.4(4) . . ? C4 Fe1 C1 68.4(3) . . ? C8 Fe1 C1 153.3(4) . . ? C9 Fe1 C1 164.9(4) . . ? C6 Fe1 C1 109.7(4) . . ? C5 Fe1 C7 152.8(4) . . ? C3 Fe1 C7 127.4(4) . . ? C2 Fe1 C7 106.9(4) . . ? C10 Fe1 C7 68.6(4) . . ? C4 Fe1 C7 164.8(4) . . ? C8 Fe1 C7 40.9(4) . . ? C9 Fe1 C7 70.1(4) . . ? C6 Fe1 C7 40.0(4) . . ? C1 Fe1 C7 119.4(4) . . ? C30 Fe2 C28 68.7(4) . . ? C30 Fe2 C29 41.4(4) . . ? C28 Fe2 C29 40.2(4) . . ? C30 Fe2 C27 69.6(4) . . ? C28 Fe2 C27 41.5(4) . . ? C29 Fe2 C27 69.4(5) . . ? C30 Fe2 C32 110.4(4) . . ? C28 Fe2 C32 169.9(4) . . ? C29 Fe2 C32 132.6(5) . . ? C27 Fe2 C32 148.4(4) . . ? C30 Fe2 C31 133.1(4) . . ? C28 Fe2 C31 146.9(5) . . ? C29 Fe2 C31 172.6(5) . . ? C27 Fe2 C31 114.9(4) . . ? C32 Fe2 C31 40.8(4) . . ? C30 Fe2 C35 171.9(4) . . ? C28 Fe2 C35 115.1(4) . . ? C29 Fe2 C35 145.9(4) . . ? C27 Fe2 C35 108.2(4) . . ? C32 Fe2 C35 67.1(4) . . ? C31 Fe2 C35 40.1(4) . . ? C30 Fe2 C34 146.7(4) . . ? C28 Fe2 C34 107.8(4) . . ? C29 Fe2 C34 114.2(4) . . ? C27 Fe2 C34 130.9(4) . . ? C32 Fe2 C34 67.0(4) . . ? C31 Fe2 C34 68.1(4) . . ? C35 Fe2 C34 40.4(4) . . ? C30 Fe2 C33 115.9(4) . . ? C28 Fe2 C33 130.7(4) . . ? C29 Fe2 C33 108.5(5) . . ? C27 Fe2 C33 169.9(4) . . ? C32 Fe2 C33 39.9(4) . . ? C31 Fe2 C33 68.4(4) . . ? C35 Fe2 C33 67.6(4) . . ? C34 Fe2 C33 40.1(4) . . ? C30 Fe2 C26 40.9(4) . . ? C28 Fe2 C26 68.3(4) . . ? C29 Fe2 C26 68.8(4) . . ? C27 Fe2 C26 40.7(3) . . ? C32 Fe2 C26 118.1(4) . . ? C31 Fe2 C26 110.2(4) . . ? C35 Fe2 C26 132.6(4) . . ? C34 Fe2 C26 170.7(4) . . ? C33 Fe2 C26 148.7(4) . . ? C1 N1 Mo1 139.3(6) . . ? O1 N2 Mo1 177.7(7) . . ? C13 N3 N4 106.3(7) . . ? C13 N3 Mo1 132.5(6) . . ? N4 N3 Mo1 121.2(5) . . ? C11 N4 N3 109.9(7) . . ? C11 N4 B1 130.8(7) . . ? N3 N4 B1 119.0(7) . . ? C16 N5 N6 106.6(7) . . ? C16 N5 Mo1 134.6(6) . . ? N6 N5 Mo1 118.7(5) . . ? C18 N6 N5 110.2(7) . . ? C18 N6 B1 129.2(7) . . ? N5 N6 B1 119.9(7) . . ? C21 N7 N8 105.2(7) . . ? C21 N7 Mo1 135.6(6) . . ? N8 N7 Mo1 119.3(5) . . ? C23 N8 N7 110.5(7) . . ? C23 N8 B1 129.6(7) . . ? N7 N8 B1 119.8(7) . . ? C26 N9 Mo2 136.3(6) . . ? O2 N10 Mo2 178.3(7) . . ? C36 N11 N12 106.4(7) . . ? C36 N11 Mo2 135.4(6) . . ? N12 N11 Mo2 118.0(5) . . ? C38 N12 N11 110.4(7) . . ? C38 N12 B2 127.6(8) . . ? N11 N12 B2 121.3(7) . . ? C41 N13 N14 108.5(7) . . ? C41 N13 Mo2 131.9(6) . . ? N14 N13 Mo2 119.5(5) . . ? C43 N14 N13 108.4(7) . . ? C43 N14 B2 130.1(8) . . ? N13 N14 B2 121.4(7) . . ? C46 N15 N16 106.4(7) . . ? C46 N15 Mo2 133.3(6) . . ? N16 N15 Mo2 119.3(5) . . ? N15 N16 C48 110.1(8) . . ? N15 N16 B2 119.0(7) . . ? C48 N16 B2 130.8(8) . . ? N1 C1 C5 126.8(8) . . ? N1 C1 C2 124.0(8) . . ? C5 C1 C2 109.0(7) . . ? N1 C1 Fe1 125.7(6) . . ? C5 C1 Fe1 68.0(5) . . ? C2 C1 Fe1 68.4(5) . . ? C1 C2 C3 106.0(8) . . ? C1 C2 Fe1 70.8(5) . . ? C3 C2 Fe1 69.0(5) . . ? C4 C3 C2 109.7(8) . . ? C4 C3 Fe1 70.4(6) . . ? C2 C3 Fe1 69.4(5) . . ? C3 C4 C5 107.1(8) . . ? C3 C4 Fe1 69.0(6) . . ? C5 C4 Fe1 68.3(5) . . ? C1 C5 C4 108.0(8) . . ? C1 C5 Fe1 71.4(5) . . ? C4 C5 Fe1 70.3(5) . . ? C7 C6 C10 109.3(9) . . ? C7 C6 Fe1 70.5(6) . . ? C10 C6 Fe1 68.8(6) . . ? C6 C7 C8 106.2(10) . . ? C6 C7 Fe1 69.6(6) . . ? C8 C7 Fe1 68.6(6) . . ? C7 C8 C9 110.2(9) . . ? C7 C8 Fe1 70.4(5) . . ? C9 C8 Fe1 69.6(5) . . ? C10 C9 C8 105.0(9) . . ? C10 C9 Fe1 68.9(5) . . ? C8 C9 Fe1 69.1(5) . . ? C6 C10 C9 109.3(9) . . ? C6 C10 Fe1 70.5(5) . . ? C9 C10 Fe1 70.1(6) . . ? N4 C11 C12 107.7(8) . . ? N4 C11 C14 122.2(8) . . ? C12 C11 C14 130.1(9) . . ? C11 C12 C13 107.5(8) . . ? N3 C13 C12 108.5(7) . . ? N3 C13 C15 122.4(8) . . ? C12 C13 C15 129.0(8) . . ? N5 C16 C17 108.7(8) . . ? N5 C16 C19 121.5(8) . . ? C17 C16 C19 129.8(8) . . ? C18 C17 C16 107.6(8) . . ? N6 C18 C17 106.9(8) . . ? N6 C18 C20 123.2(8) . . ? C17 C18 C20 129.8(8) . . ? N7 C21 C22 110.6(8) . . ? N7 C21 C24 122.5(8) . . ? C22 C21 C24 126.9(8) . . ? C21 C22 C23 107.1(8) . . ? N8 C23 C22 106.7(7) . . ? N8 C23 C25 124.2(9) . . ? C22 C23 C25 129.2(8) . . ? N9 C26 C27 125.7(9) . . ? N9 C26 C30 125.8(8) . . ? C27 C26 C30 108.4(8) . . ? N9 C26 Fe2 125.8(6) . . ? C27 C26 Fe2 68.6(5) . . ? C30 C26 Fe2 68.2(5) . . ? C26 C27 C28 106.6(10) . . ? C26 C27 Fe2 70.7(5) . . ? C28 C27 Fe2 69.1(6) . . ? C29 C28 C27 109.4(9) . . ? C29 C28 Fe2 70.0(6) . . ? C27 C28 Fe2 69.4(5) . . ? C28 C29 C30 107.8(9) . . ? C28 C29 Fe2 69.7(6) . . ? C30 C29 Fe2 69.0(5) . . ? C26 C30 C29 107.6(9) . . ? C26 C30 Fe2 70.9(5) . . ? C29 C30 Fe2 69.6(5) . . ? C35 C31 C32 106.3(9) . . ? C35 C31 Fe2 70.0(5) . . ? C32 C31 Fe2 69.6(6) . . ? C33 C32 C31 109.6(9) . . ? C33 C32 Fe2 70.8(6) . . ? C31 C32 Fe2 69.7(5) . . ? C32 C33 C34 107.2(9) . . ? C32 C33 Fe2 69.3(6) . . ? C34 C33 Fe2 69.6(5) . . ? C33 C34 C35 108.0(8) . . ? C33 C34 Fe2 70.3(5) . . ? C35 C34 Fe2 69.5(5) . . ? C31 C35 C34 109.0(9) . . ? C31 C35 Fe2 69.9(6) . . ? C34 C35 Fe2 70.1(5) . . ? N11 C36 C37 110.4(8) . . ? N11 C36 C39 122.0(7) . . ? C37 C36 C39 127.6(8) . . ? C36 C37 C38 106.9(8) . . ? N12 C38 C37 105.9(8) . . ? N12 C38 C40 124.2(8) . . ? C37 C38 C40 129.9(8) . . ? N13 C41 C42 109.2(8) . . ? N13 C41 C44 122.3(8) . . ? C42 C41 C44 128.4(8) . . ? C41 C42 C43 105.7(8) . . ? N14 C43 C42 108.1(8) . . ? N14 C43 C45 122.9(8) . . ? C42 C43 C45 128.9(9) . . ? N15 C46 C47 109.3(9) . . ? N15 C46 C49 122.5(9) . . ? C47 C46 C49 128.2(10) . . ? C46 C47 C48 109.2(9) . . ? C47 C48 N16 104.9(8) . . ? C47 C48 C50 133.6(10) . . ? N16 C48 C50 121.5(9) . . ? C602 C601 C600 80(4) . . ? C601 C602 C602 133(8) . 2_677 ? Cl11 C999 Cl10 110.1(8) . . ? N8 B1 N6 110.3(8) . . ? N8 B1 N4 110.4(7) . . ? N6 B1 N4 107.0(7) . . ? N12 B2 N14 110.5(8) . . ? N12 B2 N16 108.7(8) . . ? N14 B2 N16 107.9(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.792 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.132 #=END