Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date ' 2007' _audit_creation_method SHELX-97' _audit_update_record ; ? ; #============================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 222 _publ_contact_author_name 'F. Gordon A. Stone' _publ_contact_author_address ; Chemistry and Biochemistry Baylor University One Bear Place # 97348 Waco TX 76706 UNITED STATES OF AMERICA ; _publ_contact_author_email Gordon_Stone@baylor.edu _publ_contact_author_fax '+1 254 710 2403' _publ_contact_author_phone '+1 254 710 4427' _publ_requested_journal ; Dalton Transactions ; _publ_contact_letter ; This CIF is submitted as supplementary data for the following manuscript, submitted to Dalton Transactions: Synthesis and Reactivity of Fluorinated Ferracarborane Anions With thanks, Professor F. G. A. Stone Jan 18th, 2007 ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Reactivity of Fluorinated Ferracarborane Anions ; loop_ _publ_author_name F.G.A.Stone A.Franken B.Hodson T.D.McGrath #============================================================================= _publ_section_exptl_refinement ; Diffracted intensities for 3, 4, 5, 6 and 10 were collected at 110(2) K on a Bruker-Nonius X8 APEX CCD area-detector diffractometer using Mo-K\a X-radiation. Several sets of narrow data 'frames' were collected at different values of \q, for various initial values of \f and\w, and using 0.5\% increments of \f or \w. The data frames were integrated using SAINT (Bruker, 2003); the substantial redundancy in data allowed an empirical absorption correction (SADABS: Bruker, 2003) to be applied, based on multiple measurements of equivalent reflections. The structures were solved using conventional direct methods and refined by full- matrix least-squares on all F2 data using SHELXTL (Bruker 2001). All non-hydrogen atoms were assigned anisotropic displacement parameters. The locations of the cage carbon atoms were verified by examination of the appropriate internuclear distances and the magnitudes of their isotropic thermal displacement parameters. Hydrogen atoms were included in calculated positions and set riding on their parent atoms. All hydrogen atoms were assigned calculated isotropic thermal parameters [U~iso~(H) = 1.2 x U~iso~(parent), or U~iso~(H) = 1.5 x U~iso~(parent) for methyl hydrogens]. ; _publ_section_references ; Bruker (2001). SHELXTL-PC. Version 6.12. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. Bruker (2003).APEX 2. Version 2.1-0. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. Sheldrick, G.M. (1990). SHELXS97. Program for crystal structure solution. University of G\\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 634918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H35 B7 F3 Fe2 N O6 P2' _chemical_formula_weight 968.03 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.942(3) _cell_length_b 8.7935(13) _cell_length_c 27.143(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.138(8) _cell_angle_gamma 90.00 _cell_volume 4271.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3500 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.54 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8614 _exptl_absorpt_correction_T_max 0.9278 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X-8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27045 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.24 _reflns_number_total 7959 _reflns_number_gt 5408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _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^)+(0.0320P)^2^+1.3420P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7959 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Fe6 Fe 0.18168(3) 0.78723(5) 0.289965(18) 0.02097(14) Uani 1 1 d . . . Fe10 Fe 0.27520(3) 0.56743(5) 0.305929(19) 0.02267(14) Uani 1 1 d . . . P1 P 0.32975(5) 0.14132(9) 0.58312(3) 0.0156(2) Uani 1 1 d . . . P2 P 0.16252(5) 0.10798(9) 0.54872(3) 0.0163(2) Uani 1 1 d . . . N1 N 0.24362(14) 0.1793(3) 0.56614(10) 0.0172(6) Uani 1 1 d . . . C1 C 0.29962(19) 1.0003(4) 0.37038(13) 0.0325(10) Uani 1 1 d . . . H1 H 0.3081 1.1163 0.3884 0.039 Uiso 1 1 calc R . . B3 B 0.2628(2) 0.9710(4) 0.30946(15) 0.0226(10) Uani 1 1 d . . . H3 H 0.2465 1.0668 0.2808 0.027 Uiso 1 1 calc R . . B4 B 0.3555(2) 0.9109(5) 0.34842(15) 0.0284(11) Uani 1 1 d . . . H4 H 0.4107 0.9602 0.3501 0.034 Uiso 1 1 calc R . . B2 B 0.2279(2) 0.8971(5) 0.36526(15) 0.0295(11) Uani 1 1 d . . . H2 H 0.1836 0.9330 0.3818 0.035 Uiso 1 1 calc R . . B5 B 0.3236(2) 0.8433(5) 0.39925(16) 0.0348(12) Uani 1 1 d . . . H5 H 0.3536 0.8385 0.4423 0.042 Uiso 1 1 calc R . . B7 B 0.3010(2) 0.7944(4) 0.29181(15) 0.0205(9) Uani 1 1 d . . . B8 B 0.3483(2) 0.7064(5) 0.35831(15) 0.0259(10) Uani 1 1 d . . . B9 B 0.2542(2) 0.6965(5) 0.36645(16) 0.0299(11) Uani 1 1 d . . . F7 F 0.32424(10) 0.8138(2) 0.24885(7) 0.0268(5) Uani 1 1 d . . . F8 F 0.41846(10) 0.6471(2) 0.38518(7) 0.0327(5) Uani 1 1 d . . . F9 F 0.22891(12) 0.6117(2) 0.40069(8) 0.0438(6) Uani 1 1 d . . . C62 C 0.16127(19) 0.7874(4) 0.22088(14) 0.0287(9) Uani 1 1 d . . . C61 C 0.11841(19) 0.9383(4) 0.28589(13) 0.0260(9) Uani 1 1 d . . . C63 C 0.1172(2) 0.6459(4) 0.29538(15) 0.0364(10) Uani 1 1 d . . . C103 C 0.25434(19) 0.5305(4) 0.23795(15) 0.0298(10) Uani 1 1 d . . . C101 C 0.3542(2) 0.4487(4) 0.32038(13) 0.0320(10) Uani 1 1 d . . . C102 C 0.2229(2) 0.4147(5) 0.3192(2) 0.0523(13) Uani 1 1 d . . . O61 O 0.07747(14) 1.0371(3) 0.28330(10) 0.0376(7) Uani 1 1 d . . . O62 O 0.14859(15) 0.7980(3) 0.17711(9) 0.0440(8) Uani 1 1 d . . . O63 O 0.07420(15) 0.5600(3) 0.29972(13) 0.0593(9) Uani 1 1 d . . . O103 O 0.24506(15) 0.5065(3) 0.19512(10) 0.0471(8) Uani 1 1 d . . . O101 O 0.40457(15) 0.3675(3) 0.32844(10) 0.0505(8) Uani 1 1 d . . . O102 O 0.1930(2) 0.3119(3) 0.32976(18) 0.1028(16) Uani 1 1 d . . . C111 C 0.36905(17) 0.2106(3) 0.53552(11) 0.0150(7) Uani 1 1 d . . . C116 C 0.43787(17) 0.1577(4) 0.53434(12) 0.0191(8) Uani 1 1 d . . . H116 H 0.4638 0.0818 0.5584 0.023 Uiso 1 1 calc R . . C112 C 0.33169(18) 0.3209(3) 0.49944(12) 0.0194(8) Uani 1 1 d . . . H112 H 0.2847 0.3583 0.4997 0.023 Uiso 1 1 calc R . . C113 C 0.36233(19) 0.3761(4) 0.46346(12) 0.0237(9) Uani 1 1 d . . . H113 H 0.3362 0.4504 0.4388 0.028 Uiso 1 1 calc R . . C115 C 0.46842(18) 0.2143(4) 0.49881(12) 0.0230(8) Uani 1 1 d . . . H115 H 0.5156 0.1783 0.4986 0.028 Uiso 1 1 calc R . . C114 C 0.43064(19) 0.3239(4) 0.46328(12) 0.0246(9) Uani 1 1 d . . . H114 H 0.4520 0.3630 0.4387 0.030 Uiso 1 1 calc R . . C122 C 0.33700(18) 0.2867(4) 0.67464(12) 0.0216(8) Uani 1 1 d . . . H122 H 0.2842 0.2753 0.6631 0.026 Uiso 1 1 calc R . . C121 C 0.37735(17) 0.2342(3) 0.64404(12) 0.0143(7) Uani 1 1 d . . . C124 C 0.44939(19) 0.3723(4) 0.73893(13) 0.0276(9) Uani 1 1 d . . . H124 H 0.4741 0.4205 0.7713 0.033 Uiso 1 1 calc R . . C126 C 0.45405(18) 0.2506(4) 0.66141(12) 0.0239(8) Uani 1 1 d . . . H126 H 0.4822 0.2145 0.6406 0.029 Uiso 1 1 calc R . . C123 C 0.37305(19) 0.3559(4) 0.72212(13) 0.0255(9) Uani 1 1 d . . . H123 H 0.3450 0.3919 0.7430 0.031 Uiso 1 1 calc R . . C125 C 0.49017(19) 0.3189(4) 0.70879(13) 0.0282(9) Uani 1 1 d . . . H125 H 0.5430 0.3291 0.7206 0.034 Uiso 1 1 calc R . . C131 C 0.35519(17) -0.0561(3) 0.59118(12) 0.0166(7) Uani 1 1 d . . . C134 C 0.3966(2) -0.3604(4) 0.60108(16) 0.0354(10) Uani 1 1 d . . . H134 H 0.4122 -0.4637 0.6045 0.042 Uiso 1 1 calc R . . C132 C 0.34873(18) -0.1429(4) 0.54731(13) 0.0237(8) Uani 1 1 d . . . H132 H 0.3299 -0.0981 0.5137 0.028 Uiso 1 1 calc R . . C136 C 0.38083(17) -0.1236(4) 0.64008(13) 0.0234(8) Uani 1 1 d . . . H136 H 0.3846 -0.0655 0.6703 0.028 Uiso 1 1 calc R . . C133 C 0.36971(19) -0.2950(4) 0.55223(15) 0.0314(9) Uani 1 1 d . . . H133 H 0.3655 -0.3539 0.5221 0.038 Uiso 1 1 calc R . . C135 C 0.4010(2) -0.2768(4) 0.64483(15) 0.0344(10) Uani 1 1 d . . . H135 H 0.4177 -0.3234 0.6782 0.041 Uiso 1 1 calc R . . C211 C 0.10618(17) 0.2061(3) 0.49078(12) 0.0178(8) Uani 1 1 d . . . C212 C 0.13134(18) 0.2173(4) 0.44840(12) 0.0230(8) Uani 1 1 d . . . H212 H 0.1768 0.1694 0.4495 0.028 Uiso 1 1 calc R . . C216 C 0.03964(17) 0.2776(3) 0.48911(13) 0.0209(8) Uani 1 1 d . . . H216 H 0.0218 0.2702 0.5179 0.025 Uiso 1 1 calc R . . C213 C 0.0909(2) 0.2974(4) 0.40467(13) 0.0308(9) Uani 1 1 d . . . H213 H 0.1080 0.3033 0.3755 0.037 Uiso 1 1 calc R . . C215 C -0.00034(18) 0.3594(4) 0.44509(13) 0.0260(9) Uani 1 1 d . . . H215 H -0.0455 0.4088 0.4439 0.031 Uiso 1 1 calc R . . C214 C 0.02512(19) 0.3693(4) 0.40322(14) 0.0294(9) Uani 1 1 d . . . H214 H -0.0024 0.4256 0.3732 0.035 Uiso 1 1 calc R . . C221 C 0.11902(17) 0.1374(4) 0.59736(11) 0.0164(8) Uani 1 1 d . . . C226 C 0.07324(18) 0.0276(4) 0.60836(12) 0.0222(8) Uani 1 1 d . . . H226 H 0.0625 -0.0638 0.5887 0.027 Uiso 1 1 calc R . . C223 C 0.10243(19) 0.2950(4) 0.66523(13) 0.0254(9) Uani 1 1 d . . . H223 H 0.1120 0.3870 0.6847 0.031 Uiso 1 1 calc R . . C222 C 0.13224(18) 0.2729(4) 0.62585(12) 0.0199(8) Uani 1 1 d . . . H222 H 0.1619 0.3502 0.6180 0.024 Uiso 1 1 calc R . . C224 C 0.05859(19) 0.1836(4) 0.67656(13) 0.0278(9) Uani 1 1 d . . . H224 H 0.0389 0.1982 0.7042 0.033 Uiso 1 1 calc R . . C225 C 0.04348(19) 0.0514(4) 0.64773(13) 0.0294(9) Uani 1 1 d . . . H225 H 0.0123 -0.0239 0.6550 0.035 Uiso 1 1 calc R . . C231 C 0.15989(17) -0.0921(4) 0.53519(13) 0.0203(8) Uani 1 1 d . . . C236 C 0.19291(18) -0.1917(4) 0.57599(15) 0.0291(9) Uani 1 1 d . . . H236 H 0.2117 -0.1547 0.6107 0.035 Uiso 1 1 calc R . . C235 C 0.1985(2) -0.3458(4) 0.56601(19) 0.0421(11) Uani 1 1 d . . . H235 H 0.2213 -0.4139 0.5939 0.051 Uiso 1 1 calc R . . C232 C 0.13182(19) -0.1478(4) 0.48434(14) 0.0296(9) Uani 1 1 d . . . H232 H 0.1086 -0.0806 0.4563 0.036 Uiso 1 1 calc R . . C234 C 0.1710(2) -0.3992(5) 0.5154(2) 0.0484(13) Uani 1 1 d . . . H234 H 0.1749 -0.5043 0.5087 0.058 Uiso 1 1 calc R . . C233 C 0.1378(2) -0.3022(5) 0.47476(18) 0.0422(11) Uani 1 1 d . . . H233 H 0.1191 -0.3403 0.4401 0.051 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 Fe6 0.0166(3) 0.0218(3) 0.0251(3) 0.0029(2) 0.0075(2) 0.0028(2) Fe10 0.0193(3) 0.0220(3) 0.0294(3) 0.0040(2) 0.0116(2) 0.0037(2) P1 0.0154(4) 0.0145(5) 0.0178(4) 0.0003(3) 0.0068(4) 0.0006(4) P2 0.0148(4) 0.0168(5) 0.0187(4) -0.0024(4) 0.0073(4) -0.0004(4) N1 0.0151(14) 0.0159(15) 0.0221(14) 0.0001(11) 0.0081(12) -0.0008(11) C1 0.029(2) 0.037(2) 0.031(2) -0.0112(17) 0.0092(18) 0.0037(18) B3 0.018(2) 0.022(2) 0.028(2) -0.0001(17) 0.0092(18) 0.0008(17) B4 0.021(2) 0.033(3) 0.032(2) -0.008(2) 0.0079(19) -0.0014(19) B2 0.025(2) 0.040(3) 0.024(2) 0.002(2) 0.0100(19) 0.012(2) B5 0.028(2) 0.055(3) 0.021(2) -0.007(2) 0.007(2) 0.010(2) B7 0.017(2) 0.021(2) 0.024(2) -0.0012(17) 0.0084(17) 0.0011(17) B8 0.022(2) 0.037(3) 0.021(2) 0.0030(19) 0.0102(18) 0.0107(19) B9 0.030(2) 0.041(3) 0.023(2) 0.013(2) 0.0138(19) 0.014(2) F7 0.0291(11) 0.0305(12) 0.0268(11) 0.0034(9) 0.0174(9) 0.0013(9) F8 0.0216(11) 0.0444(13) 0.0299(11) 0.0050(10) 0.0055(9) 0.0106(9) F9 0.0471(14) 0.0561(15) 0.0424(13) 0.0275(11) 0.0342(12) 0.0237(12) C62 0.022(2) 0.022(2) 0.036(2) -0.0046(17) -0.0001(17) 0.0107(16) C61 0.0197(19) 0.033(2) 0.0280(19) 0.0049(17) 0.0121(16) -0.0019(18) C63 0.026(2) 0.029(2) 0.052(3) 0.0088(19) 0.0104(19) 0.0067(19) C103 0.024(2) 0.020(2) 0.037(2) -0.0039(17) -0.0012(18) 0.0043(16) C101 0.037(2) 0.040(2) 0.0195(18) 0.0001(17) 0.0099(17) 0.008(2) C102 0.058(3) 0.023(2) 0.105(4) 0.003(2) 0.065(3) 0.011(2) O61 0.0305(15) 0.0390(17) 0.0484(17) 0.0100(13) 0.0197(13) 0.0180(13) O62 0.0521(19) 0.0464(18) 0.0235(14) -0.0028(13) -0.0012(13) 0.0222(14) O63 0.0319(17) 0.0449(19) 0.098(3) 0.0163(17) 0.0179(17) -0.0089(15) O103 0.0524(19) 0.0396(17) 0.0331(16) -0.0120(13) -0.0081(14) 0.0162(13) O101 0.0464(18) 0.060(2) 0.0370(16) -0.0051(14) 0.0026(14) 0.0332(16) O102 0.123(3) 0.0234(19) 0.229(5) 0.004(2) 0.149(4) -0.001(2) C111 0.0177(17) 0.0142(17) 0.0152(16) -0.0015(13) 0.0082(14) -0.0008(14) C116 0.0173(18) 0.0211(19) 0.0194(17) 0.0025(14) 0.0068(15) 0.0021(15) C112 0.0155(18) 0.0206(19) 0.0212(17) 0.0000(14) 0.0047(15) 0.0024(14) C113 0.031(2) 0.022(2) 0.0171(17) 0.0041(15) 0.0065(16) 0.0016(16) C115 0.0195(18) 0.030(2) 0.0231(18) -0.0022(16) 0.0112(16) 0.0011(16) C114 0.030(2) 0.029(2) 0.0181(17) 0.0024(15) 0.0122(16) -0.0039(17) C122 0.0139(17) 0.023(2) 0.0284(19) -0.0008(16) 0.0075(15) -0.0011(15) C121 0.0147(17) 0.0135(17) 0.0179(16) 0.0019(13) 0.0095(14) 0.0022(14) C124 0.029(2) 0.029(2) 0.0221(18) -0.0033(16) 0.0038(17) -0.0023(17) C126 0.0212(19) 0.034(2) 0.0196(17) 0.0000(15) 0.0106(15) 0.0021(16) C123 0.027(2) 0.028(2) 0.0255(19) -0.0049(16) 0.0147(17) 0.0014(16) C125 0.0148(18) 0.041(2) 0.0256(19) -0.0028(17) 0.0029(16) -0.0036(16) C131 0.0139(17) 0.0144(18) 0.0239(17) -0.0015(14) 0.0097(14) -0.0004(14) C134 0.031(2) 0.015(2) 0.062(3) 0.0048(19) 0.017(2) 0.0027(17) C132 0.025(2) 0.019(2) 0.0316(19) -0.0030(16) 0.0145(16) -0.0006(15) C136 0.0218(19) 0.0182(19) 0.0279(19) 0.0034(15) 0.0051(16) -0.0017(15) C133 0.033(2) 0.020(2) 0.048(2) -0.0063(18) 0.0235(19) 0.0005(17) C135 0.034(2) 0.021(2) 0.042(2) 0.0092(18) 0.0048(19) -0.0017(17) C211 0.0144(17) 0.0195(19) 0.0201(17) -0.0053(14) 0.0064(14) -0.0062(14) C212 0.0189(18) 0.030(2) 0.0240(18) -0.0015(16) 0.0116(16) -0.0021(16) C216 0.0190(18) 0.0190(19) 0.0260(18) -0.0038(15) 0.0090(15) -0.0037(15) C213 0.029(2) 0.046(2) 0.0192(18) -0.0018(17) 0.0101(17) -0.0105(19) C215 0.0153(18) 0.027(2) 0.033(2) -0.0016(16) 0.0044(16) -0.0012(15) C214 0.022(2) 0.032(2) 0.027(2) 0.0036(17) -0.0023(17) -0.0031(17) C221 0.0151(17) 0.0195(19) 0.0160(16) 0.0013(14) 0.0069(14) 0.0009(14) C226 0.025(2) 0.0209(19) 0.0209(18) -0.0020(15) 0.0086(16) -0.0028(16) C223 0.033(2) 0.020(2) 0.0260(19) -0.0044(15) 0.0126(17) 0.0029(17) C222 0.0199(18) 0.0178(19) 0.0242(18) 0.0016(15) 0.0100(15) -0.0007(15) C224 0.030(2) 0.038(2) 0.0238(19) -0.0038(17) 0.0195(17) 0.0020(18) C225 0.030(2) 0.030(2) 0.033(2) -0.0022(17) 0.0169(18) -0.0077(17) C231 0.0165(17) 0.0159(18) 0.0335(19) -0.0068(15) 0.0151(15) -0.0040(14) C236 0.023(2) 0.023(2) 0.046(2) 0.0034(17) 0.0187(18) -0.0037(16) C235 0.030(2) 0.018(2) 0.093(4) 0.009(2) 0.040(2) 0.0008(18) C232 0.029(2) 0.028(2) 0.041(2) -0.0161(17) 0.0234(18) -0.0097(17) C234 0.045(3) 0.018(2) 0.108(4) -0.023(3) 0.059(3) -0.012(2) C233 0.042(3) 0.037(3) 0.067(3) -0.028(2) 0.045(2) -0.017(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 Fe6 C61 1.768(4) . ? Fe6 C63 1.781(4) . ? Fe6 C62 1.786(4) . ? Fe6 B2 2.169(4) . ? Fe6 B3 2.173(4) . ? Fe6 B9 2.228(4) . ? Fe6 B7 2.246(4) . ? Fe6 Fe10 2.5609(7) . ? Fe10 C101 1.761(4) . ? Fe10 C102 1.775(5) . ? Fe10 C103 1.786(4) . ? Fe10 B8 2.036(4) . ? Fe10 B7 2.120(4) . ? Fe10 B9 2.139(4) . ? P1 N1 1.579(3) . ? P1 C131 1.796(3) . ? P1 C111 1.796(3) . ? P1 C121 1.799(3) . ? P2 N1 1.581(3) . ? P2 C221 1.789(3) . ? P2 C231 1.794(3) . ? P2 C211 1.805(3) . ? C1 B5 1.579(6) . ? C1 B4 1.583(5) . ? C1 B3 1.591(5) . ? C1 B2 1.601(6) . ? C1 H1 1.1200 . ? B3 B4 1.805(5) . ? B3 B7 1.842(5) . ? B3 B2 1.952(6) . ? B3 H3 1.1200 . ? B4 B5 1.780(6) . ? B4 B8 1.829(6) . ? B4 B7 1.853(5) . ? B4 H4 1.1200 . ? B2 B5 1.806(5) . ? B2 B9 1.830(6) . ? B2 H2 1.1200 . ? B5 B8 1.802(6) . ? B5 B9 1.849(6) . ? B5 H5 1.1200 . ? B7 F7 1.385(4) . ? B7 B8 1.897(5) . ? B8 F8 1.390(4) . ? B8 B9 1.870(6) . ? B9 F9 1.393(5) . ? C62 O62 1.136(4) . ? C61 O61 1.151(4) . ? C63 O63 1.146(4) . ? C103 O103 1.137(4) . ? C101 O101 1.153(4) . ? C102 O102 1.151(5) . ? C111 C116 1.394(4) . ? C111 C112 1.395(4) . ? C116 C115 1.370(4) . ? C116 H116 0.9500 . ? C112 C113 1.378(4) . ? C112 H112 0.9500 . ? C113 C114 1.375(5) . ? C113 H113 0.9500 . ? C115 C114 1.385(4) . ? C115 H115 0.9500 . ? C114 H114 0.9500 . ? C122 C121 1.380(4) . ? C122 C123 1.386(4) . ? C122 H122 0.9500 . ? C121 C126 1.380(4) . ? C124 C123 1.374(5) . ? C124 C125 1.379(5) . ? C124 H124 0.9500 . ? C126 C125 1.381(4) . ? C126 H126 0.9500 . ? C123 H123 0.9500 . ? C125 H125 0.9500 . ? C131 C132 1.386(4) . ? C131 C136 1.388(4) . ? C134 C135 1.376(5) . ? C134 C133 1.380(5) . ? C134 H134 0.9500 . ? C132 C133 1.389(4) . ? C132 H132 0.9500 . ? C136 C135 1.394(4) . ? C136 H136 0.9500 . ? C133 H133 0.9500 . ? C135 H135 0.9500 . ? C211 C212 1.385(5) . ? C211 C216 1.396(4) . ? C212 C213 1.377(4) . ? C212 H212 0.9500 . ? C216 C215 1.388(4) . ? C216 H216 0.9500 . ? C213 C214 1.386(5) . ? C213 H213 0.9500 . ? C215 C214 1.375(5) . ? C215 H215 0.9500 . ? C214 H214 0.9500 . ? C221 C226 1.394(4) . ? C221 C222 1.398(4) . ? C226 C225 1.378(5) . ? C226 H226 0.9500 . ? C223 C222 1.377(5) . ? C223 C224 1.383(5) . ? C223 H223 0.9500 . ? C222 H222 0.9500 . ? C224 C225 1.378(5) . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C231 C236 1.390(4) . ? C231 C232 1.395(4) . ? C236 C235 1.393(5) . ? C236 H236 0.9500 . ? C235 C234 1.381(6) . ? C235 H235 0.9500 . ? C232 C233 1.394(5) . ? C232 H232 0.9500 . ? C234 C233 1.373(6) . ? C234 H234 0.9500 . ? C233 H233 0.9500 . ? 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 C61 Fe6 C63 93.47(16) . . ? C61 Fe6 C62 91.42(15) . . ? C63 Fe6 C62 99.72(17) . . ? C61 Fe6 B2 77.31(15) . . ? C63 Fe6 B2 108.00(18) . . ? C62 Fe6 B2 150.50(17) . . ? C61 Fe6 B3 82.38(15) . . ? C63 Fe6 B3 161.42(17) . . ? C62 Fe6 B3 98.48(16) . . ? B2 Fe6 B3 53.43(16) . . ? C61 Fe6 B9 121.70(16) . . ? C63 Fe6 B9 84.44(17) . . ? C62 Fe6 B9 146.48(16) . . ? B2 Fe6 B9 49.18(15) . . ? B3 Fe6 B9 82.45(16) . . ? C61 Fe6 B7 129.57(15) . . ? C63 Fe6 B7 136.87(15) . . ? C62 Fe6 B7 83.87(15) . . ? B2 Fe6 B7 82.74(15) . . ? B3 Fe6 B7 49.23(14) . . ? B9 Fe6 B7 71.38(15) . . ? C61 Fe6 Fe10 174.10(12) . . ? C63 Fe6 Fe10 85.08(12) . . ? C62 Fe6 Fe10 94.46(11) . . ? B2 Fe6 Fe10 97.67(11) . . ? B3 Fe6 Fe10 97.19(10) . . ? B9 Fe6 Fe10 52.50(11) . . ? B7 Fe6 Fe10 51.83(10) . . ? C101 Fe10 C102 89.81(19) . . ? C101 Fe10 C103 90.36(16) . . ? C102 Fe10 C103 97.1(2) . . ? C101 Fe10 B8 82.31(16) . . ? C102 Fe10 B8 127.6(2) . . ? C103 Fe10 B8 134.45(17) . . ? C101 Fe10 B7 111.65(17) . . ? C102 Fe10 B7 157.90(17) . . ? C103 Fe10 B7 88.30(15) . . ? B8 Fe10 B7 54.29(15) . . ? C101 Fe10 B9 120.16(15) . . ? C102 Fe10 B9 89.35(19) . . ? C103 Fe10 B9 148.91(15) . . ? B8 Fe10 B9 53.15(17) . . ? B7 Fe10 B9 75.59(16) . . ? C101 Fe10 Fe6 167.35(13) . . ? C102 Fe10 Fe6 101.77(13) . . ? C103 Fe10 Fe6 93.21(11) . . ? B8 Fe10 Fe6 86.54(11) . . ? B7 Fe10 Fe6 56.40(11) . . ? B9 Fe10 Fe6 55.72(10) . . ? N1 P1 C131 116.76(14) . . ? N1 P1 C111 110.54(14) . . ? C131 P1 C111 104.93(15) . . ? N1 P1 C121 109.32(15) . . ? C131 P1 C121 107.06(14) . . ? C111 P1 C121 107.82(14) . . ? N1 P2 C221 111.07(14) . . ? N1 P2 C231 114.13(14) . . ? C221 P2 C231 107.70(16) . . ? N1 P2 C211 108.06(14) . . ? C221 P2 C211 106.86(15) . . ? C231 P2 C211 108.75(15) . . ? P1 N1 P2 144.42(17) . . ? B5 C1 B4 68.5(3) . . ? B5 C1 B3 109.3(3) . . ? B4 C1 B3 69.3(2) . . ? B5 C1 B2 69.2(3) . . ? B4 C1 B2 109.8(3) . . ? B3 C1 B2 75.4(3) . . ? B5 C1 H1 127.1 . . ? B4 C1 H1 126.8 . . ? B3 C1 H1 123.5 . . ? B2 C1 H1 123.4 . . ? C1 B3 B4 55.1(2) . . ? C1 B3 B7 109.4(3) . . ? B4 B3 B7 61.1(2) . . ? C1 B3 B2 52.5(2) . . ? B4 B3 B2 87.7(3) . . ? B7 B3 B2 100.5(3) . . ? C1 B3 Fe6 114.0(3) . . ? B4 B3 Fe6 113.5(2) . . ? B7 B3 Fe6 67.43(17) . . ? B2 B3 Fe6 63.18(17) . . ? C1 B3 H3 121.9 . . ? B4 B3 H3 128.5 . . ? B7 B3 H3 119.7 . . ? B2 B3 H3 134.7 . . ? Fe6 B3 H3 112.2 . . ? C1 B4 B5 55.6(2) . . ? C1 B4 B3 55.5(2) . . ? B5 B4 B3 92.3(3) . . ? C1 B4 B8 110.0(3) . . ? B5 B4 B8 59.9(2) . . ? B3 B4 B8 105.6(3) . . ? C1 B4 B7 109.1(3) . . ? B5 B4 B7 102.7(3) . . ? B3 B4 B7 60.4(2) . . ? B8 B4 B7 62.0(2) . . ? C1 B4 H4 121.6 . . ? B5 B4 H4 130.3 . . ? B3 B4 H4 128.8 . . ? B8 B4 H4 119.1 . . ? B7 B4 H4 120.5 . . ? C1 B2 B5 54.8(2) . . ? C1 B2 B9 109.1(3) . . ? B5 B2 B9 61.1(2) . . ? C1 B2 B3 52.1(2) . . ? B5 B2 B3 86.9(3) . . ? B9 B2 B3 100.1(3) . . ? C1 B2 Fe6 113.8(3) . . ? B5 B2 Fe6 113.1(3) . . ? B9 B2 Fe6 67.08(19) . . ? B3 B2 Fe6 63.39(17) . . ? C1 B2 H2 122.2 . . ? B5 B2 H2 128.8 . . ? B9 B2 H2 119.9 . . ? B3 B2 H2 135.0 . . ? Fe6 B2 H2 112.3 . . ? C1 B5 B4 55.8(2) . . ? C1 B5 B8 111.6(3) . . ? B4 B5 B8 61.4(2) . . ? C1 B5 B2 56.0(2) . . ? B4 B5 B2 93.2(3) . . ? B8 B5 B2 106.3(3) . . ? C1 B5 B9 109.2(3) . . ? B4 B5 B9 103.2(3) . . ? B8 B5 B9 61.6(2) . . ? B2 B5 B9 60.1(2) . . ? C1 B5 H5 121.0 . . ? B4 B5 H5 129.5 . . ? B8 B5 H5 118.2 . . ? B2 B5 H5 128.6 . . ? B9 B5 H5 120.9 . . ? F7 B7 B3 112.0(3) . . ? F7 B7 B4 112.7(3) . . ? B3 B7 B4 58.5(2) . . ? F7 B7 B8 132.1(3) . . ? B3 B7 B8 101.5(3) . . ? B4 B7 B8 58.4(2) . . ? F7 B7 Fe10 115.1(2) . . ? B3 B7 Fe10 127.8(3) . . ? B4 B7 Fe10 118.0(2) . . ? B8 B7 Fe10 60.60(17) . . ? F7 B7 Fe6 125.4(2) . . ? B3 B7 Fe6 63.34(17) . . ? B4 B7 Fe6 108.5(2) . . ? B8 B7 Fe6 99.7(2) . . ? Fe10 B7 Fe6 71.77(13) . . ? F8 B8 B5 108.9(3) . . ? F8 B8 B4 110.0(3) . . ? B5 B8 B4 58.7(2) . . ? F8 B8 B9 134.8(3) . . ? B5 B8 B9 60.4(2) . . ? B4 B8 B9 100.5(3) . . ? F8 B8 B7 136.4(3) . . ? B5 B8 B7 100.2(3) . . ? B4 B8 B7 59.6(2) . . ? B9 B8 B7 87.7(2) . . ? F8 B8 Fe10 117.1(3) . . ? B5 B8 Fe10 125.2(3) . . ? B4 B8 Fe10 123.6(2) . . ? B9 B8 Fe10 66.26(19) . . ? B7 B8 Fe10 65.12(16) . . ? F9 B9 B2 112.2(3) . . ? F9 B9 B5 113.5(3) . . ? B2 B9 B5 58.8(2) . . ? F9 B9 B8 130.8(3) . . ? B2 B9 B8 102.5(3) . . ? B5 B9 B8 58.0(2) . . ? F9 B9 Fe10 114.8(3) . . ? B2 B9 Fe10 128.0(3) . . ? B5 B9 Fe10 117.3(3) . . ? B8 B9 Fe10 60.59(18) . . ? F9 B9 Fe6 124.9(3) . . ? B2 B9 Fe6 63.74(17) . . ? B5 B9 Fe6 108.8(2) . . ? B8 B9 Fe6 101.2(2) . . ? Fe10 B9 Fe6 71.78(13) . . ? O62 C62 Fe6 175.3(3) . . ? O61 C61 Fe6 179.7(4) . . ? O63 C63 Fe6 176.9(4) . . ? O103 C103 Fe10 176.3(3) . . ? O101 C101 Fe10 177.6(3) . . ? O102 C102 Fe10 175.8(5) . . ? C116 C111 C112 118.6(3) . . ? C116 C111 P1 121.0(2) . . ? C112 C111 P1 120.4(3) . . ? C115 C116 C111 120.6(3) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C113 C112 C111 120.5(3) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C114 C113 C112 120.0(3) . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C116 C115 C114 120.1(3) . . ? C116 C115 H115 119.9 . . ? C114 C115 H115 119.9 . . ? C113 C114 C115 120.2(3) . . ? C113 C114 H114 119.9 . . ? C115 C114 H114 119.9 . . ? C121 C122 C123 120.4(3) . . ? C121 C122 H122 119.8 . . ? C123 C122 H122 119.8 . . ? C122 C121 C126 119.2(3) . . ? C122 C121 P1 119.7(2) . . ? C126 C121 P1 121.0(3) . . ? C123 C124 C125 120.0(3) . . ? C123 C124 H124 120.0 . . ? C125 C124 H124 120.0 . . ? C121 C126 C125 120.6(3) . . ? C121 C126 H126 119.7 . . ? C125 C126 H126 119.7 . . ? C124 C123 C122 119.9(3) . . ? C124 C123 H123 120.0 . . ? C122 C123 H123 120.0 . . ? C124 C125 C126 119.9(3) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? C132 C131 C136 119.4(3) . . ? C132 C131 P1 118.9(2) . . ? C136 C131 P1 121.7(3) . . ? C135 C134 C133 120.3(3) . . ? C135 C134 H134 119.8 . . ? C133 C134 H134 119.8 . . ? C131 C132 C133 120.4(3) . . ? C131 C132 H132 119.8 . . ? C133 C132 H132 119.8 . . ? C131 C136 C135 120.1(3) . . ? C131 C136 H136 120.0 . . ? C135 C136 H136 120.0 . . ? C134 C133 C132 119.8(4) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C134 C135 C136 119.9(3) . . ? C134 C135 H135 120.0 . . ? C136 C135 H135 120.0 . . ? C212 C211 C216 119.6(3) . . ? C212 C211 P2 119.4(2) . . ? C216 C211 P2 120.9(3) . . ? C213 C212 C211 120.4(3) . . ? C213 C212 H212 119.8 . . ? C211 C212 H212 119.8 . . ? C215 C216 C211 119.6(3) . . ? C215 C216 H216 120.2 . . ? C211 C216 H216 120.2 . . ? C212 C213 C214 119.9(4) . . ? C212 C213 H213 120.0 . . ? C214 C213 H213 120.0 . . ? C214 C215 C216 120.3(3) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C215 C214 C213 120.2(3) . . ? C215 C214 H214 119.9 . . ? C213 C214 H214 119.9 . . ? C226 C221 C222 118.9(3) . . ? C226 C221 P2 121.8(3) . . ? C222 C221 P2 119.3(3) . . ? C225 C226 C221 120.2(3) . . ? C225 C226 H226 119.9 . . ? C221 C226 H226 119.9 . . ? C222 C223 C224 120.1(3) . . ? C222 C223 H223 119.9 . . ? C224 C223 H223 119.9 . . ? C223 C222 C221 120.3(3) . . ? C223 C222 H222 119.8 . . ? C221 C222 H222 119.8 . . ? C225 C224 C223 120.0(4) . . ? C225 C224 H224 120.0 . . ? C223 C224 H224 120.0 . . ? C226 C225 C224 120.4(3) . . ? C226 C225 H225 119.8 . . ? C224 C225 H225 119.8 . . ? C236 C231 C232 119.5(3) . . ? C236 C231 P2 118.7(3) . . ? C232 C231 P2 121.5(3) . . ? C231 C236 C235 120.1(4) . . ? C231 C236 H236 120.0 . . ? C235 C236 H236 120.0 . . ? C234 C235 C236 119.7(4) . . ? C234 C235 H235 120.1 . . ? C236 C235 H235 120.1 . . ? C233 C232 C231 119.9(4) . . ? C233 C232 H232 120.0 . . ? C231 C232 H232 120.0 . . ? C233 C234 C235 120.8(4) . . ? C233 C234 H234 119.6 . . ? C235 C234 H234 119.6 . . ? C234 C233 C232 119.9(4) . . ? C234 C233 H233 120.0 . . ? C232 C233 H233 120.0 . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.443 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.083 #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 634919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H35 B7 F3 Fe2 N O6 P2' _chemical_formula_weight 968.03 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.6161(9) _cell_length_b 13.4715(8) _cell_length_c 20.3842(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.618(3) _cell_angle_gamma 90.00 _cell_volume 4372.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2148 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 21.26 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8722 _exptl_absorpt_correction_T_max 0.9447 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X-8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24762 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.1301 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7982 _reflns_number_gt 4517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7982 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1515 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2279 _refine_ls_wR_factor_gt 0.1929 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe6 Fe 0.28673(6) 0.27101(7) 0.15836(5) 0.0237(3) Uani 1 1 d . . . Fe7 Fe 0.14983(6) 0.24993(8) 0.19891(5) 0.0340(3) Uani 1 1 d . . . P2 P 0.22033(10) 0.65616(13) 0.48057(8) 0.0196(4) Uani 1 1 d . . . P1 P 0.29147(10) 0.82893(13) 0.42378(8) 0.0204(4) Uani 1 1 d . . . C1 C 0.3050(5) 0.3405(7) 0.3138(5) 0.057(2) Uani 1 1 d . . . H1 H 0.3445 0.3335 0.3683 0.068 Uiso 1 1 calc R . . B3 B 0.2806(6) 0.2460(8) 0.2677(5) 0.052(3) Uani 1 1 d . . . H3 H 0.3009 0.1698 0.2875 0.063 Uiso 1 1 calc R . . B2 B 0.3432(6) 0.3633(7) 0.2482(5) 0.049(3) Uani 1 1 d . . . H2 H 0.4111 0.3783 0.2538 0.059 Uiso 1 1 calc R . . B5 B 0.2669(6) 0.4409(7) 0.2726(5) 0.048(3) Uani 1 1 d . . . H5 H 0.2771 0.5160 0.2971 0.057 Uiso 1 1 calc R . . B4 B 0.2061(5) 0.3386(7) 0.2905(4) 0.035(2) Uani 1 1 d . . . H4 H 0.1693 0.3350 0.3287 0.042 Uiso 1 1 calc R . . B8 B 0.1669(6) 0.4117(7) 0.2117(5) 0.039(2) Uani 1 1 d . . . B10 B 0.1804(7) 0.3621(8) 0.1373(5) 0.049(3) Uani 1 1 d . . . B9 B 0.2631(6) 0.4245(7) 0.1861(5) 0.045(3) Uani 1 1 d . . . F8 F 0.1012(3) 0.4767(3) 0.2022(2) 0.0537(13) Uani 1 1 d . . . F9 F 0.2861(3) 0.5087(4) 0.1541(3) 0.0655(15) Uani 1 1 d . . . F10 F 0.1314(3) 0.3964(4) 0.0746(2) 0.0620(14) Uani 1 1 d . . . C63 C 0.2278(5) 0.2253(6) 0.0762(4) 0.0364(19) Uani 1 1 d . . . C62 C 0.3619(5) 0.3236(5) 0.1219(4) 0.0332(18) Uani 1 1 d . . . C61 C 0.3461(6) 0.1597(6) 0.1854(4) 0.047(2) Uani 1 1 d . . . C73 C 0.0774(5) 0.2318(7) 0.1159(4) 0.049(2) Uani 1 1 d . . . C72 C 0.0641(5) 0.2593(5) 0.2345(4) 0.0332(18) Uani 1 1 d . . . C71 C 0.1724(5) 0.1199(7) 0.2187(4) 0.042(2) Uani 1 1 d . . . O63 O 0.1933(3) 0.1970(4) 0.0227(3) 0.0514(15) Uani 1 1 d . . . O62 O 0.4068(3) 0.3578(4) 0.0956(3) 0.0534(16) Uani 1 1 d . . . O61 O 0.3862(5) 0.0910(5) 0.2017(3) 0.089(3) Uani 1 1 d . . . O72 O 0.0072(3) 0.2663(4) 0.2553(3) 0.0411(14) Uani 1 1 d . . . O71 O 0.1861(4) 0.0371(5) 0.2292(3) 0.0616(18) Uani 1 1 d . . . O73 O 0.0288(4) 0.2159(5) 0.0642(3) 0.071(2) Uani 1 1 d . . . N1 N 0.2326(3) 0.7388(4) 0.4282(2) 0.0239(13) Uani 1 1 d . . . C112 C 0.3440(4) 0.7127(5) 0.3334(3) 0.0289(17) Uani 1 1 d . . . H112 H 0.3217 0.6590 0.3529 0.035 Uiso 1 1 calc R . . C116 C 0.3665(4) 0.8873(5) 0.3234(3) 0.0271(16) Uani 1 1 d . . . H116 H 0.3590 0.9539 0.3358 0.033 Uiso 1 1 calc R . . C111 C 0.3356(4) 0.8079(5) 0.3542(3) 0.0203(15) Uani 1 1 d . . . C115 C 0.4079(4) 0.8673(5) 0.2747(3) 0.0310(18) Uani 1 1 d . . . H115 H 0.4303 0.9206 0.2549 0.037 Uiso 1 1 calc R . . C114 C 0.4171(4) 0.7719(5) 0.2549(3) 0.0296(17) Uani 1 1 d . . . H114 H 0.4454 0.7592 0.2213 0.036 Uiso 1 1 calc R . . C113 C 0.3848(5) 0.6940(6) 0.2839(4) 0.039(2) Uani 1 1 d . . . H113 H 0.3905 0.6278 0.2699 0.047 Uiso 1 1 calc R . . C121 C 0.2316(4) 0.9424(5) 0.4100(3) 0.0228(16) Uani 1 1 d . . . C126 C 0.1452(4) 0.9390(6) 0.3829(3) 0.0288(17) Uani 1 1 d . . . H126 H 0.1178 0.8772 0.3699 0.035 Uiso 1 1 calc R . . C125 C 0.0982(5) 1.0263(6) 0.3748(4) 0.038(2) Uani 1 1 d . . . H125 H 0.0388 1.0235 0.3567 0.045 Uiso 1 1 calc R . . C124 C 0.1374(5) 1.1165(6) 0.3928(4) 0.041(2) Uani 1 1 d . . . H124 H 0.1050 1.1756 0.3877 0.049 Uiso 1 1 calc R . . C122 C 0.2709(4) 1.0338(5) 0.4273(3) 0.0285(17) Uani 1 1 d . . . H122 H 0.3303 1.0365 0.4455 0.034 Uiso 1 1 calc R . . C123 C 0.2250(5) 1.1210(6) 0.4185(4) 0.039(2) Uani 1 1 d . . . H123 H 0.2525 1.1831 0.4298 0.047 Uiso 1 1 calc R . . C132 C 0.4601(4) 0.8180(5) 0.4985(3) 0.0246(16) Uani 1 1 d . . . H132 H 0.4695 0.7914 0.4581 0.029 Uiso 1 1 calc R . . C131 C 0.3795(4) 0.8479(5) 0.4988(3) 0.0209(15) Uani 1 1 d . . . C134 C 0.5119(4) 0.8667(5) 0.6167(3) 0.0314(18) Uani 1 1 d . . . H134 H 0.5572 0.8728 0.6573 0.038 Uiso 1 1 calc R . . C136 C 0.3660(4) 0.8878(5) 0.5579(3) 0.0248(16) Uani 1 1 d . . . H136 H 0.3114 0.9088 0.5577 0.030 Uiso 1 1 calc R . . C133 C 0.5265(4) 0.8278(5) 0.5581(3) 0.0277(17) Uani 1 1 d . . . H133 H 0.5815 0.8079 0.5586 0.033 Uiso 1 1 calc R . . C135 C 0.4321(4) 0.8968(5) 0.6167(3) 0.0289(17) Uani 1 1 d . . . H135 H 0.4229 0.9235 0.6571 0.035 Uiso 1 1 calc R . . C216 C 0.1012(4) 0.5059(5) 0.4670(3) 0.0237(16) Uani 1 1 d . . . H216 H 0.1221 0.4986 0.5153 0.028 Uiso 1 1 calc R . . C215 C 0.0368(4) 0.4450(5) 0.4304(4) 0.0344(18) Uani 1 1 d . . . H215 H 0.0149 0.3949 0.4533 0.041 Uiso 1 1 calc R . . C211 C 0.1360(4) 0.5779(5) 0.4341(3) 0.0195(15) Uani 1 1 d . . . C212 C 0.1030(4) 0.5890(5) 0.3631(3) 0.0240(16) Uani 1 1 d . . . H212 H 0.1264 0.6369 0.3396 0.029 Uiso 1 1 calc R . . C213 C 0.0365(4) 0.5306(5) 0.3271(4) 0.0336(18) Uani 1 1 d . . . H213 H 0.0126 0.5406 0.2793 0.040 Uiso 1 1 calc R . . C214 C 0.0045(4) 0.4575(5) 0.3606(4) 0.0289(17) Uani 1 1 d . . . H214 H -0.0397 0.4158 0.3353 0.035 Uiso 1 1 calc R . . C222 C 0.1486(4) 0.7979(5) 0.5443(4) 0.0296(17) Uani 1 1 d . . . H222 H 0.1351 0.8309 0.5013 0.036 Uiso 1 1 calc R . . C226 C 0.2113(4) 0.6598(5) 0.6162(3) 0.0255(16) Uani 1 1 d . . . H226 H 0.2406 0.5984 0.6232 0.031 Uiso 1 1 calc R . . C225 C 0.1866(4) 0.7032(6) 0.6694(4) 0.0327(18) Uani 1 1 d . . . H225 H 0.1991 0.6707 0.7125 0.039 Uiso 1 1 calc R . . C221 C 0.1931(4) 0.7068(5) 0.5527(3) 0.0229(15) Uani 1 1 d . . . C224 C 0.1447(5) 0.7911(6) 0.6606(4) 0.037(2) Uani 1 1 d . . . H224 H 0.1289 0.8199 0.6976 0.045 Uiso 1 1 calc R . . C223 C 0.1249(4) 0.8391(5) 0.5977(4) 0.0346(19) Uani 1 1 d . . . H223 H 0.0951 0.9001 0.5915 0.042 Uiso 1 1 calc R . . C231 C 0.3105(4) 0.5765(5) 0.5139(3) 0.0217(16) Uani 1 1 d . . . C236 C 0.3149(4) 0.4828(5) 0.4856(3) 0.0264(17) Uani 1 1 d . . . H236 H 0.2690 0.4587 0.4497 0.032 Uiso 1 1 calc R . . C232 C 0.3803(4) 0.6101(6) 0.5666(3) 0.0296(17) Uani 1 1 d . . . H232 H 0.3785 0.6738 0.5861 0.036 Uiso 1 1 calc R . . C233 C 0.4508(4) 0.5524(6) 0.5902(3) 0.0313(18) Uani 1 1 d . . . H233 H 0.4973 0.5763 0.6256 0.038 Uiso 1 1 calc R . . C234 C 0.4537(4) 0.4597(6) 0.5624(4) 0.0342(19) Uani 1 1 d . . . H234 H 0.5021 0.4193 0.5792 0.041 Uiso 1 1 calc R . . C235 C 0.3865(5) 0.4250(6) 0.5100(4) 0.039(2) Uani 1 1 d . . . H235 H 0.3894 0.3613 0.4908 0.047 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 Fe6 0.0259(6) 0.0240(6) 0.0242(5) 0.0002(4) 0.0119(5) 0.0017(4) Fe7 0.0275(6) 0.0373(8) 0.0412(7) 0.0007(5) 0.0162(5) 0.0063(5) P2 0.0196(9) 0.0200(10) 0.0197(9) -0.0002(8) 0.0064(8) -0.0031(8) P1 0.0217(10) 0.0193(11) 0.0213(9) -0.0007(8) 0.0078(8) -0.0048(8) C1 0.055(6) 0.057(7) 0.057(6) 0.004(5) 0.016(5) 0.012(5) B3 0.047(6) 0.055(7) 0.066(7) -0.029(6) 0.035(6) -0.012(5) B2 0.043(6) 0.053(7) 0.057(6) -0.019(5) 0.021(5) -0.012(5) B5 0.048(6) 0.036(6) 0.069(7) -0.027(5) 0.034(6) -0.022(5) B4 0.034(5) 0.046(6) 0.028(5) -0.010(4) 0.015(4) -0.010(4) B8 0.040(6) 0.037(6) 0.046(6) 0.006(5) 0.022(5) 0.005(5) B10 0.063(7) 0.051(7) 0.036(6) 0.011(5) 0.018(5) 0.014(6) B9 0.060(7) 0.031(6) 0.054(6) 0.008(5) 0.033(5) 0.001(5) F8 0.058(3) 0.043(3) 0.072(3) 0.011(2) 0.037(3) 0.013(2) F9 0.075(4) 0.049(3) 0.084(4) 0.007(3) 0.043(3) 0.002(3) F10 0.094(4) 0.054(3) 0.040(3) 0.010(2) 0.022(3) 0.028(3) C63 0.035(5) 0.048(5) 0.031(4) -0.008(4) 0.016(4) -0.010(4) C62 0.033(4) 0.030(5) 0.043(5) -0.004(4) 0.019(4) 0.002(4) C61 0.078(6) 0.034(5) 0.040(5) 0.005(4) 0.035(5) 0.018(5) C73 0.027(5) 0.084(7) 0.033(5) 0.000(5) 0.003(4) -0.003(5) C72 0.042(5) 0.025(5) 0.032(4) 0.001(3) 0.010(4) -0.004(4) C71 0.029(4) 0.040(6) 0.058(5) -0.007(4) 0.012(4) 0.001(4) O63 0.052(4) 0.063(4) 0.041(3) -0.017(3) 0.016(3) -0.015(3) O62 0.047(4) 0.063(4) 0.062(4) 0.010(3) 0.034(3) 0.003(3) O61 0.143(7) 0.071(5) 0.080(5) 0.037(4) 0.076(5) 0.077(5) O72 0.030(3) 0.042(4) 0.056(3) -0.011(3) 0.020(3) -0.001(2) O71 0.051(4) 0.034(4) 0.101(5) 0.001(4) 0.023(4) 0.011(3) O73 0.044(4) 0.118(6) 0.044(4) -0.009(4) 0.004(3) -0.011(4) N1 0.027(3) 0.027(4) 0.017(3) 0.003(3) 0.003(2) -0.007(3) C112 0.040(4) 0.021(4) 0.027(4) -0.001(3) 0.012(3) -0.004(3) C116 0.025(4) 0.025(4) 0.032(4) -0.006(3) 0.010(3) -0.001(3) C111 0.021(4) 0.021(4) 0.017(3) -0.004(3) 0.004(3) -0.004(3) C115 0.035(4) 0.031(5) 0.030(4) 0.000(3) 0.014(4) -0.005(4) C114 0.033(4) 0.031(5) 0.029(4) -0.004(3) 0.016(3) -0.002(3) C113 0.059(5) 0.029(5) 0.038(4) -0.008(4) 0.024(4) -0.003(4) C121 0.021(4) 0.024(4) 0.026(4) -0.001(3) 0.010(3) 0.002(3) C126 0.025(4) 0.032(5) 0.029(4) 0.004(3) 0.008(3) -0.008(4) C125 0.029(4) 0.048(6) 0.036(5) 0.008(4) 0.010(4) 0.007(4) C124 0.043(5) 0.034(5) 0.047(5) 0.009(4) 0.014(4) 0.018(4) C122 0.026(4) 0.027(5) 0.036(4) 0.001(3) 0.013(3) 0.001(3) C123 0.040(5) 0.029(5) 0.051(5) 0.002(4) 0.016(4) 0.006(4) C132 0.022(4) 0.019(4) 0.030(4) 0.001(3) 0.003(3) -0.004(3) C131 0.022(4) 0.018(4) 0.023(4) 0.002(3) 0.007(3) -0.004(3) C134 0.035(4) 0.025(4) 0.027(4) 0.005(3) -0.004(3) -0.009(4) C136 0.024(4) 0.026(4) 0.026(4) 0.002(3) 0.011(3) -0.002(3) C133 0.029(4) 0.022(4) 0.032(4) 0.002(3) 0.008(3) 0.003(3) C135 0.036(4) 0.025(4) 0.024(4) -0.003(3) 0.006(3) -0.001(3) C216 0.021(4) 0.026(4) 0.024(4) 0.002(3) 0.007(3) 0.000(3) C215 0.021(4) 0.026(5) 0.054(5) 0.002(4) 0.008(4) -0.009(3) C211 0.021(4) 0.015(4) 0.025(4) 0.005(3) 0.010(3) 0.006(3) C212 0.017(4) 0.029(4) 0.025(4) -0.005(3) 0.004(3) -0.007(3) C213 0.026(4) 0.046(5) 0.029(4) -0.002(4) 0.008(3) -0.001(4) C214 0.020(4) 0.024(4) 0.040(5) -0.012(4) 0.005(3) -0.007(3) C222 0.032(4) 0.028(5) 0.032(4) 0.006(3) 0.014(3) -0.003(4) C226 0.023(4) 0.025(4) 0.028(4) 0.001(3) 0.007(3) -0.002(3) C225 0.041(5) 0.032(5) 0.028(4) -0.005(3) 0.015(4) -0.018(4) C221 0.026(4) 0.019(4) 0.021(4) 0.000(3) 0.002(3) -0.005(3) C224 0.048(5) 0.032(5) 0.043(5) -0.005(4) 0.031(4) -0.004(4) C223 0.038(5) 0.028(5) 0.043(5) 0.002(4) 0.021(4) 0.001(4) C231 0.019(4) 0.030(4) 0.018(3) 0.005(3) 0.009(3) -0.004(3) C236 0.023(4) 0.030(5) 0.026(4) -0.005(3) 0.006(3) 0.003(3) C232 0.028(4) 0.031(5) 0.030(4) 0.002(3) 0.008(3) -0.004(4) C233 0.023(4) 0.044(5) 0.023(4) 0.007(4) 0.000(3) -0.002(4) C234 0.023(4) 0.051(6) 0.031(4) 0.009(4) 0.012(4) 0.010(4) C235 0.045(5) 0.035(5) 0.043(5) -0.005(4) 0.020(4) 0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe6 C62 1.774(7) . ? Fe6 C63 1.790(8) . ? Fe6 C61 1.793(9) . ? Fe6 B10 2.092(10) . ? Fe6 B2 2.190(9) . ? Fe6 B9 2.208(9) . ? Fe6 B3 2.284(10) . ? Fe6 Fe7 2.6484(13) . ? Fe7 C72 1.779(8) . ? Fe7 C73 1.790(9) . ? Fe7 C71 1.812(10) . ? Fe7 B10 2.118(10) . ? Fe7 B4 2.188(8) . ? Fe7 B8 2.204(10) . ? Fe7 B3 2.224(11) . ? P2 N1 1.595(5) . ? P2 C221 1.793(6) . ? P2 C211 1.793(7) . ? P2 C231 1.810(7) . ? P1 N1 1.578(5) . ? P1 C111 1.795(6) . ? P1 C121 1.801(7) . ? P1 C131 1.807(7) . ? C1 B3 1.566(12) . ? C1 B4 1.576(12) . ? C1 B5 1.623(13) . ? C1 B2 1.665(12) . ? C1 H1 1.1200 . ? B3 B4 1.906(12) . ? B3 B2 1.993(14) . ? B3 H3 1.1200 . ? B2 B9 1.757(14) . ? B2 B5 1.819(13) . ? B2 H2 1.1200 . ? B5 B9 1.759(13) . ? B5 B8 1.809(14) . ? B5 B4 1.806(12) . ? B5 H5 1.1200 . ? B4 B8 1.837(12) . ? B4 H4 1.1200 . ? B8 F8 1.369(9) . ? B8 B10 1.731(13) . ? B8 B9 1.826(12) . ? B10 F10 1.382(10) . ? B10 B9 1.675(15) . ? B9 F9 1.414(9) . ? C63 O63 1.143(8) . ? C62 O62 1.133(8) . ? C61 O61 1.133(9) . ? C73 O73 1.149(9) . ? C72 O72 1.146(8) . ? C71 O71 1.147(9) . ? C112 C111 1.371(9) . ? C112 C113 1.390(9) . ? C112 H112 0.9500 . ? C116 C115 1.385(8) . ? C116 C111 1.410(9) . ? C116 H116 0.9500 . ? C115 C114 1.369(9) . ? C115 H115 0.9500 . ? C114 C113 1.386(9) . ? C114 H114 0.9500 . ? C113 H113 0.9500 . ? C121 C126 1.384(9) . ? C121 C122 1.391(9) . ? C126 C125 1.395(10) . ? C126 H126 0.9500 . ? C125 C124 1.377(10) . ? C125 H125 0.9500 . ? C124 C123 1.400(10) . ? C124 H124 0.9500 . ? C122 C123 1.384(9) . ? C122 H122 0.9500 . ? C123 H123 0.9500 . ? C132 C133 1.394(9) . ? C132 C131 1.401(9) . ? C132 H132 0.9500 . ? C131 C136 1.395(8) . ? C134 C135 1.388(9) . ? C134 C133 1.387(9) . ? C134 H134 0.9500 . ? C136 C135 1.380(9) . ? C136 H136 0.9500 . ? C133 H133 0.9500 . ? C135 H135 0.9500 . ? C216 C215 1.385(9) . ? C216 C211 1.395(8) . ? C216 H216 0.9500 . ? C215 C214 1.381(10) . ? C215 H215 0.9500 . ? C211 C212 1.401(8) . ? C212 C213 1.384(9) . ? C212 H212 0.9500 . ? C213 C214 1.388(9) . ? C213 H213 0.9500 . ? C214 H214 0.9500 . ? C222 C223 1.375(9) . ? C222 C221 1.417(9) . ? C222 H222 0.9500 . ? C226 C225 1.392(9) . ? C226 C221 1.394(9) . ? C226 H226 0.9500 . ? C225 C224 1.360(10) . ? C225 H225 0.9500 . ? C224 C223 1.389(10) . ? C224 H224 0.9500 . ? C223 H223 0.9500 . ? C231 C236 1.399(9) . ? C231 C232 1.411(9) . ? C236 C235 1.389(9) . ? C236 H236 0.9500 . ? C232 C233 1.373(9) . ? C232 H232 0.9500 . ? C233 C234 1.379(10) . ? C233 H233 0.9500 . ? C234 C235 1.387(10) . ? C234 H234 0.9500 . ? C235 H235 0.9500 . ? 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 C62 Fe6 C63 90.4(3) . . ? C62 Fe6 C61 94.1(3) . . ? C63 Fe6 C61 96.1(4) . . ? C62 Fe6 B10 109.5(4) . . ? C63 Fe6 B10 78.8(4) . . ? C61 Fe6 B10 155.7(4) . . ? C62 Fe6 B2 86.5(3) . . ? C63 Fe6 B2 165.1(4) . . ? C61 Fe6 B2 98.7(4) . . ? B10 Fe6 B2 88.5(4) . . ? C62 Fe6 B9 86.1(3) . . ? C63 Fe6 B9 118.2(4) . . ? C61 Fe6 B9 145.8(4) . . ? B10 Fe6 B9 45.8(4) . . ? B2 Fe6 B9 47.1(4) . . ? C62 Fe6 B3 134.5(3) . . ? C63 Fe6 B3 134.2(3) . . ? C61 Fe6 B3 75.6(3) . . ? B10 Fe6 B3 90.9(4) . . ? B2 Fe6 B3 52.8(3) . . ? B9 Fe6 B3 80.1(3) . . ? C62 Fe6 Fe7 160.8(2) . . ? C63 Fe6 Fe7 88.1(2) . . ? C61 Fe6 Fe7 105.1(3) . . ? B10 Fe6 Fe7 51.4(3) . . ? B2 Fe6 Fe7 90.0(2) . . ? B9 Fe6 Fe7 77.8(2) . . ? B3 Fe6 Fe7 53.0(2) . . ? C72 Fe7 C73 89.7(3) . . ? C72 Fe7 C71 96.7(3) . . ? C73 Fe7 C71 96.8(4) . . ? C72 Fe7 B10 123.2(3) . . ? C73 Fe7 B10 75.4(4) . . ? C71 Fe7 B10 138.8(3) . . ? C72 Fe7 B4 79.0(3) . . ? C73 Fe7 B4 152.7(4) . . ? C71 Fe7 B4 109.0(4) . . ? B10 Fe7 B4 90.0(4) . . ? C72 Fe7 B8 88.4(3) . . ? C73 Fe7 B8 106.0(4) . . ? C71 Fe7 B8 156.6(4) . . ? B10 Fe7 B8 47.2(3) . . ? B4 Fe7 B8 49.5(3) . . ? C72 Fe7 B3 119.8(3) . . ? C73 Fe7 B3 149.7(3) . . ? C71 Fe7 B3 74.6(4) . . ? B10 Fe7 B3 91.9(4) . . ? B4 Fe7 B3 51.2(3) . . ? B8 Fe7 B3 83.1(4) . . ? C72 Fe7 Fe6 168.3(2) . . ? C73 Fe7 Fe6 97.2(2) . . ? C71 Fe7 Fe6 91.8(2) . . ? B10 Fe7 Fe6 50.6(3) . . ? B4 Fe7 Fe6 90.7(2) . . ? B8 Fe7 Fe6 80.7(2) . . ? B3 Fe7 Fe6 55.1(2) . . ? N1 P2 C221 113.2(3) . . ? N1 P2 C211 106.7(3) . . ? C221 P2 C211 108.3(3) . . ? N1 P2 C231 114.5(3) . . ? C221 P2 C231 107.1(3) . . ? C211 P2 C231 106.7(3) . . ? N1 P1 C111 108.9(3) . . ? N1 P1 C121 109.8(3) . . ? C111 P1 C121 110.0(3) . . ? N1 P1 C131 115.2(3) . . ? C111 P1 C131 106.0(3) . . ? C121 P1 C131 106.8(3) . . ? B3 C1 B4 74.7(6) . . ? B3 C1 B5 111.7(8) . . ? B4 C1 B5 68.7(6) . . ? B3 C1 B2 76.1(6) . . ? B4 C1 B2 111.4(7) . . ? B5 C1 B2 67.2(6) . . ? B3 C1 H1 120.3 . . ? B4 C1 H1 124.2 . . ? B5 C1 H1 127.9 . . ? B2 C1 H1 124.3 . . ? C1 B3 B4 52.9(5) . . ? C1 B3 B2 54.2(5) . . ? B4 B3 B2 86.7(6) . . ? C1 B3 Fe7 113.5(6) . . ? B4 B3 Fe7 63.4(4) . . ? B2 B3 Fe7 109.1(6) . . ? C1 B3 Fe6 113.0(6) . . ? B4 B3 Fe6 110.8(6) . . ? B2 B3 Fe6 61.1(4) . . ? Fe7 B3 Fe6 71.9(3) . . ? C1 B3 H3 121.9 . . ? B4 B3 H3 131.4 . . ? B2 B3 H3 132.7 . . ? Fe7 B3 H3 112.9 . . ? Fe6 B3 H3 113.3 . . ? C1 B2 B9 106.3(7) . . ? C1 B2 B5 55.3(5) . . ? B9 B2 B5 58.9(5) . . ? C1 B2 B3 49.7(5) . . ? B9 B2 B3 100.6(6) . . ? B5 B2 B3 87.5(6) . . ? C1 B2 Fe6 113.4(6) . . ? B9 B2 Fe6 67.0(5) . . ? B5 B2 Fe6 112.9(6) . . ? B3 B2 Fe6 66.0(4) . . ? C1 B2 H2 123.8 . . ? B9 B2 H2 121.4 . . ? B5 B2 H2 129.0 . . ? B3 B2 H2 133.8 . . ? Fe6 B2 H2 111.5 . . ? C1 B5 B9 108.1(7) . . ? C1 B5 B8 108.7(7) . . ? B9 B5 B8 61.6(5) . . ? C1 B5 B4 54.4(5) . . ? B9 B5 B4 104.2(6) . . ? B8 B5 B4 61.1(5) . . ? C1 B5 B2 57.5(5) . . ? B9 B5 B2 58.8(5) . . ? B8 B5 B2 105.3(6) . . ? B4 B5 B2 95.2(6) . . ? C1 B5 H5 122.3 . . ? B9 B5 H5 121.1 . . ? B8 B5 H5 119.7 . . ? B4 B5 H5 128.5 . . ? B2 B5 H5 127.7 . . ? C1 B4 B5 56.9(5) . . ? C1 B4 B8 109.5(6) . . ? B5 B4 B8 59.5(5) . . ? C1 B4 B3 52.4(5) . . ? B5 B4 B3 90.6(5) . . ? B8 B4 B3 103.3(6) . . ? C1 B4 Fe7 114.9(5) . . ? B5 B4 Fe7 111.8(5) . . ? B8 B4 Fe7 65.7(4) . . ? B3 B4 Fe7 65.4(4) . . ? C1 B4 H4 121.4 . . ? B5 B4 H4 128.4 . . ? B8 B4 H4 120.2 . . ? B3 B4 H4 131.6 . . ? Fe7 B4 H4 112.6 . . ? F8 B8 B10 114.8(7) . . ? F8 B8 B5 119.8(7) . . ? B10 B8 B5 111.2(6) . . ? F8 B8 B9 128.8(7) . . ? B10 B8 B9 56.1(5) . . ? B5 B8 B9 57.9(5) . . ? F8 B8 B4 122.5(6) . . ? B10 B8 B4 117.2(7) . . ? B5 B8 B4 59.4(5) . . ? B9 B8 B4 100.4(6) . . ? F8 B8 Fe7 123.0(6) . . ? B10 B8 Fe7 63.8(5) . . ? B5 B8 Fe7 111.0(5) . . ? B9 B8 Fe7 98.8(5) . . ? B4 B8 Fe7 64.8(4) . . ? F10 B10 B9 123.2(8) . . ? F10 B10 B8 119.4(7) . . ? B9 B10 B8 64.8(6) . . ? F10 B10 Fe6 128.7(6) . . ? B9 B10 Fe6 70.8(5) . . ? B8 B10 Fe6 111.1(6) . . ? F10 B10 Fe7 127.5(7) . . ? B9 B10 Fe7 107.5(6) . . ? B8 B10 Fe7 69.0(4) . . ? Fe6 B10 Fe7 78.0(3) . . ? F9 B9 B10 114.4(7) . . ? F9 B9 B2 117.3(7) . . ? B10 B9 B2 121.1(7) . . ? F9 B9 B5 115.1(7) . . ? B10 B9 B5 116.5(6) . . ? B2 B9 B5 62.3(5) . . ? F9 B9 B8 125.5(7) . . ? B10 B9 B8 59.1(5) . . ? B2 B9 B8 107.1(6) . . ? B5 B9 B8 60.6(5) . . ? F9 B9 Fe6 122.8(5) . . ? B10 B9 Fe6 63.5(5) . . ? B2 B9 Fe6 65.9(4) . . ? B5 B9 Fe6 114.6(6) . . ? B8 B9 Fe6 102.7(5) . . ? O63 C63 Fe6 176.9(6) . . ? O62 C62 Fe6 176.5(7) . . ? O61 C61 Fe6 177.2(8) . . ? O73 C73 Fe7 176.1(8) . . ? O72 C72 Fe7 177.7(7) . . ? O71 C71 Fe7 178.0(8) . . ? P1 N1 P2 140.8(4) . . ? C111 C112 C113 120.5(6) . . ? C111 C112 H112 119.8 . . ? C113 C112 H112 119.8 . . ? C115 C116 C111 119.4(6) . . ? C115 C116 H116 120.3 . . ? C111 C116 H116 120.3 . . ? C112 C111 C116 119.3(5) . . ? C112 C111 P1 119.5(5) . . ? C116 C111 P1 121.0(5) . . ? C114 C115 C116 120.9(6) . . ? C114 C115 H115 119.5 . . ? C116 C115 H115 119.5 . . ? C115 C114 C113 119.7(6) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C114 C113 C112 120.1(7) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C126 C121 C122 119.2(6) . . ? C126 C121 P1 119.8(5) . . ? C122 C121 P1 120.9(5) . . ? C121 C126 C125 120.1(7) . . ? C121 C126 H126 120.0 . . ? C125 C126 H126 120.0 . . ? C124 C125 C126 120.4(7) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C124 C123 120.0(7) . . ? C125 C124 H124 120.0 . . ? C123 C124 H124 120.0 . . ? C123 C122 C121 121.1(7) . . ? C123 C122 H122 119.4 . . ? C121 C122 H122 119.4 . . ? C122 C123 C124 119.2(7) . . ? C122 C123 H123 120.4 . . ? C124 C123 H123 120.4 . . ? C133 C132 C131 119.2(6) . . ? C133 C132 H132 120.4 . . ? C131 C132 H132 120.4 . . ? C136 C131 C132 120.3(6) . . ? C136 C131 P1 119.6(5) . . ? C132 C131 P1 120.0(5) . . ? C135 C134 C133 120.9(7) . . ? C135 C134 H134 119.5 . . ? C133 C134 H134 119.5 . . ? C135 C136 C131 120.0(6) . . ? C135 C136 H136 120.0 . . ? C131 C136 H136 120.0 . . ? C134 C133 C132 119.8(6) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C136 C135 C134 119.8(6) . . ? C136 C135 H135 120.1 . . ? C134 C135 H135 120.1 . . ? C215 C216 C211 121.0(6) . . ? C215 C216 H216 119.5 . . ? C211 C216 H216 119.5 . . ? C214 C215 C216 119.7(6) . . ? C214 C215 H215 120.1 . . ? C216 C215 H215 120.1 . . ? C216 C211 C212 118.6(6) . . ? C216 C211 P2 121.5(5) . . ? C212 C211 P2 119.9(5) . . ? C213 C212 C211 120.3(6) . . ? C213 C212 H212 119.9 . . ? C211 C212 H212 119.9 . . ? C212 C213 C214 120.2(6) . . ? C212 C213 H213 119.9 . . ? C214 C213 H213 119.9 . . ? C215 C214 C213 120.2(6) . . ? C215 C214 H214 119.9 . . ? C213 C214 H214 119.9 . . ? C223 C222 C221 120.7(6) . . ? C223 C222 H222 119.7 . . ? C221 C222 H222 119.7 . . ? C225 C226 C221 119.8(7) . . ? C225 C226 H226 120.1 . . ? C221 C226 H226 120.1 . . ? C224 C225 C226 121.1(7) . . ? C224 C225 H225 119.4 . . ? C226 C225 H225 119.4 . . ? C226 C221 C222 118.3(6) . . ? C226 C221 P2 123.3(5) . . ? C222 C221 P2 118.4(5) . . ? C225 C224 C223 120.3(7) . . ? C225 C224 H224 119.9 . . ? C223 C224 H224 119.9 . . ? C222 C223 C224 119.8(7) . . ? C222 C223 H223 120.1 . . ? C224 C223 H223 120.1 . . ? C236 C231 C232 118.4(6) . . ? C236 C231 P2 121.0(5) . . ? C232 C231 P2 120.5(5) . . ? C235 C236 C231 119.9(6) . . ? C235 C236 H236 120.1 . . ? C231 C236 H236 120.1 . . ? C233 C232 C231 121.2(7) . . ? C233 C232 H232 119.4 . . ? C231 C232 H232 119.4 . . ? C232 C233 C234 119.7(7) . . ? C232 C233 H233 120.1 . . ? C234 C233 H233 120.1 . . ? C233 C234 C235 120.4(7) . . ? C233 C234 H234 119.8 . . ? C235 C234 H234 119.8 . . ? C236 C235 C234 120.4(7) . . ? C236 C235 H235 119.8 . . ? C234 C235 H235 119.8 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.692 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.119 #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 634920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H34 B7 F4 Fe2 N O6 P2' _chemical_formula_weight 986.02 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' P P 0.1023 0.0942 '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' F F 0.0171 0.0103 '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 11.074(5) _cell_length_b 12.705(5) _cell_length_c 16.503(7) _cell_angle_alpha 89.392(12) _cell_angle_beta 75.878(12) _cell_angle_gamma 84.497(12) _cell_volume 2241.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1312 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.77 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8968 _exptl_absorpt_correction_T_max 0.9264 _exptl_absorpt_process_details 'SADABS (Bruker, 2003) ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X-8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32717 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.34 _reflns_number_total 8941 _reflns_number_gt 5887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _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^)+(0.0913P)^2^+0.8710P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8941 _refine_ls_number_parameters 611 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1765 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 C1 C 0.7324(4) 0.6573(4) 0.1494(3) 0.0392(12) Uani 1 1 d . . . H1 H 0.8036 0.6075 0.1077 0.047 Uiso 1 1 calc R A 1 B2 B 0.6593(5) 0.6225(4) 0.2419(3) 0.0301(11) Uani 0.327(10) 1 d P B 1 F2 F 0.6839(9) 0.5213(8) 0.2682(6) 0.062(4) Uani 0.327(10) 1 d P B 1 B20 B 0.6593(5) 0.6225(4) 0.2419(3) 0.0301(11) Uani 0.673(10) 1 d P B 2 H2 H 0.6801 0.5436 0.2690 0.036 Uiso 0.673(10) 1 calc PR B 2 B3 B 0.7586(5) 0.7440(4) 0.2101(4) 0.0368(13) Uani 0.074(7) 1 d P B 1 F3 F 0.879(5) 0.759(4) 0.209(3) 0.078(5) Uani 0.074(7) 1 d P B 1 B30 B 0.7586(5) 0.7440(4) 0.2101(4) 0.0368(13) Uani 0.926(7) 1 d P B 2 H3 H 0.8556 0.7590 0.2127 0.044 Uiso 0.926(7) 1 calc PR B 2 B4 B 0.6872(5) 0.7757(4) 0.1269(4) 0.0371(13) Uani 0.249(10) 1 d P B 1 F4 F 0.7467(12) 0.8052(12) 0.0485(9) 0.069(6) Uani 0.249(10) 1 d P B 1 B40 B 0.6872(5) 0.7757(4) 0.1269(4) 0.0371(13) Uani 0.751(10) 1 d P B 2 H4 H 0.7288 0.8140 0.0665 0.044 Uiso 0.751(10) 1 calc PR B 2 B5 B 0.5833(5) 0.6520(4) 0.1583(3) 0.0354(12) Uani 0.330(10) 1 d P B 1 F5 F 0.5416(12) 0.5768(8) 0.1139(6) 0.078(5) Uani 0.330(10) 1 d P B 1 B50 B 0.5833(5) 0.6520(4) 0.1583(3) 0.0354(12) Uani 0.670(10) 1 d P B 2 H5 H 0.5452 0.5951 0.1219 0.042 Uiso 0.670(10) 1 calc PR B 2 Fe6 Fe 0.62424(5) 0.74828(5) 0.33519(4) 0.02624(18) Uani 1 1 d . . . B7 B 0.6396(5) 0.8498(4) 0.2222(3) 0.0322(12) Uani 1 1 d . B . F7 F 0.6709(2) 0.95414(19) 0.22432(17) 0.0399(7) Uani 1 1 d . . . Fe8 Fe 0.48225(5) 0.81229(5) 0.16855(4) 0.02800(18) Uani 1 1 d . . . B9 B 0.5025(4) 0.6844(4) 0.2608(3) 0.0278(11) Uani 1 1 d . B . F9 F 0.4003(2) 0.6279(2) 0.30089(16) 0.0369(6) Uani 1 1 d . . . B10 B 0.4849(4) 0.8253(4) 0.2906(3) 0.0251(10) Uani 1 1 d . B . F10 F 0.3904(2) 0.8895(2) 0.34251(15) 0.0349(6) Uani 1 1 d . . . C61 C 0.7745(4) 0.7075(3) 0.3564(3) 0.0343(11) Uani 1 1 d . B . O61 O 0.8692(3) 0.6811(3) 0.3724(2) 0.0467(9) Uani 1 1 d . . . C62 C 0.5413(4) 0.6672(4) 0.4151(3) 0.0339(10) Uani 1 1 d . B . O62 O 0.4873(3) 0.6118(3) 0.4635(2) 0.0501(10) Uani 1 1 d . . . C63 C 0.6020(4) 0.8684(4) 0.3943(3) 0.0354(11) Uani 1 1 d . B . O63 O 0.5896(3) 0.9459(3) 0.4318(2) 0.0494(9) Uani 1 1 d . . . C81 C 0.3168(4) 0.8091(4) 0.2094(3) 0.0354(11) Uani 1 1 d . B . O81 O 0.2113(3) 0.8086(3) 0.2397(2) 0.0469(9) Uani 1 1 d . . . C82 C 0.4732(4) 0.9507(4) 0.1472(3) 0.0362(11) Uani 1 1 d . B . O82 O 0.4688(3) 1.0399(3) 0.1352(2) 0.0478(9) Uani 1 1 d . . . C83 C 0.4871(4) 0.7734(4) 0.0621(3) 0.0378(11) Uani 1 1 d . B . O83 O 0.4906(3) 0.7492(3) -0.0050(2) 0.0507(9) Uani 1 1 d . . . P1 P -0.00725(9) 0.14420(8) 0.22338(6) 0.0210(2) Uani 1 1 d . . . N1 N 0.1028(3) 0.2139(3) 0.2278(2) 0.0239(8) Uani 1 1 d . . . C111 C 0.0574(3) 0.0415(3) 0.1458(2) 0.0219(8) Uani 1 1 d . . . C112 C -0.0170(4) -0.0349(3) 0.1308(3) 0.0257(9) Uani 1 1 d . . . H112 H -0.1009 -0.0348 0.1628 0.031 Uiso 1 1 calc R . . C113 C 0.0318(4) -0.1113(3) 0.0690(3) 0.0284(10) Uani 1 1 d . . . H113 H -0.0182 -0.1642 0.0592 0.034 Uiso 1 1 calc R . . C114 C 0.1544(4) -0.1103(3) 0.0213(3) 0.0282(10) Uani 1 1 d . . . H114 H 0.1873 -0.1626 -0.0211 0.034 Uiso 1 1 calc R . . C115 C 0.2288(4) -0.0338(3) 0.0351(3) 0.0319(10) Uani 1 1 d . . . H115 H 0.3123 -0.0337 0.0024 0.038 Uiso 1 1 calc R . . C116 C 0.1802(4) 0.0432(3) 0.0974(3) 0.0262(9) Uani 1 1 d . . . H116 H 0.2301 0.0964 0.1069 0.031 Uiso 1 1 calc R . . C121 C -0.1331(4) 0.2195(3) 0.1900(2) 0.0227(9) Uani 1 1 d . . . C122 C -0.1049(4) 0.3084(3) 0.1410(3) 0.0308(10) Uani 1 1 d . . . H122 H -0.0220 0.3287 0.1269 0.037 Uiso 1 1 calc R . . C123 C -0.1995(5) 0.3673(3) 0.1129(3) 0.0379(11) Uani 1 1 d . . . H123 H -0.1810 0.4284 0.0803 0.046 Uiso 1 1 calc R . . C124 C -0.3199(5) 0.3373(4) 0.1322(3) 0.0364(11) Uani 1 1 d . . . H124 H -0.3836 0.3784 0.1131 0.044 Uiso 1 1 calc R . . C125 C -0.3481(4) 0.2485(4) 0.1788(3) 0.0327(10) Uani 1 1 d . . . H125 H -0.4308 0.2279 0.1910 0.039 Uiso 1 1 calc R . . C126 C -0.2565(4) 0.1894(3) 0.2078(2) 0.0262(9) Uani 1 1 d . . . H126 H -0.2764 0.1281 0.2399 0.031 Uiso 1 1 calc R . . C131 C -0.0744(4) 0.0823(3) 0.3212(2) 0.0244(9) Uani 1 1 d . . . C132 C -0.0259(4) -0.0190(4) 0.3386(3) 0.0334(10) Uani 1 1 d . . . H132 H 0.0346 -0.0588 0.2964 0.040 Uiso 1 1 calc R . . C133 C -0.0661(5) -0.0613(4) 0.4173(3) 0.0427(12) Uani 1 1 d . . . H133 H -0.0328 -0.1298 0.4292 0.051 Uiso 1 1 calc R . . C134 C -0.1550(5) -0.0033(5) 0.4786(3) 0.0461(13) Uani 1 1 d . . . H134 H -0.1821 -0.0325 0.5325 0.055 Uiso 1 1 calc R . . C135 C -0.2044(4) 0.0960(4) 0.4622(3) 0.0400(12) Uani 1 1 d . . . H135 H -0.2657 0.1347 0.5046 0.048 Uiso 1 1 calc R . . C136 C -0.1644(4) 0.1396(4) 0.3838(3) 0.0304(10) Uani 1 1 d . . . H136 H -0.1981 0.2082 0.3726 0.036 Uiso 1 1 calc R . . P2 P 0.12860(9) 0.31355(8) 0.27567(6) 0.0203(2) Uani 1 1 d . . . C211 C 0.1598(4) 0.4231(3) 0.2058(2) 0.0226(9) Uani 1 1 d . . . C212 C 0.2491(4) 0.4038(4) 0.1299(3) 0.0359(11) Uani 1 1 d . . . H212 H 0.2875 0.3341 0.1159 0.043 Uiso 1 1 calc R . . C213 C 0.2818(5) 0.4854(4) 0.0752(3) 0.0446(13) Uani 1 1 d . . . H213 H 0.3449 0.4726 0.0248 0.053 Uiso 1 1 calc R . . C214 C 0.2212(5) 0.5862(4) 0.0947(3) 0.0416(12) Uani 1 1 d . . . H214 H 0.2427 0.6422 0.0570 0.050 Uiso 1 1 calc R . . C215 C 0.1305(4) 0.6059(4) 0.1679(3) 0.0370(11) Uani 1 1 d . . . H215 H 0.0882 0.6748 0.1796 0.044 Uiso 1 1 calc R . . C216 C 0.1006(4) 0.5252(3) 0.2250(3) 0.0307(10) Uani 1 1 d . . . H216 H 0.0404 0.5394 0.2765 0.037 Uiso 1 1 calc R . . C221 C 0.0042(3) 0.3576(3) 0.3656(2) 0.0214(8) Uani 1 1 d . . . C222 C -0.1120(4) 0.4027(3) 0.3542(3) 0.0248(9) Uani 1 1 d . . . H222 H -0.1230 0.4148 0.2994 0.030 Uiso 1 1 calc R . . C223 C -0.2108(4) 0.4294(3) 0.4236(3) 0.0295(10) Uani 1 1 d . . . H223 H -0.2891 0.4596 0.4160 0.035 Uiso 1 1 calc R . . C224 C -0.1946(4) 0.4119(4) 0.5034(3) 0.0334(11) Uani 1 1 d . . . H224 H -0.2621 0.4305 0.5504 0.040 Uiso 1 1 calc R . . C225 C -0.0806(4) 0.3674(4) 0.5156(3) 0.0335(10) Uani 1 1 d . . . H225 H -0.0705 0.3550 0.5706 0.040 Uiso 1 1 calc R . . C226 C 0.0187(4) 0.3412(3) 0.4466(3) 0.0290(10) Uani 1 1 d . . . H226 H 0.0969 0.3119 0.4548 0.035 Uiso 1 1 calc R . . C231 C 0.2689(3) 0.2824(3) 0.3125(2) 0.0222(9) Uani 1 1 d . . . C232 C 0.3369(4) 0.3633(3) 0.3298(3) 0.0276(9) Uani 1 1 d . . . H232 H 0.3133 0.4346 0.3179 0.033 Uiso 1 1 calc R . . C233 C 0.4387(4) 0.3398(4) 0.3643(3) 0.0348(11) Uani 1 1 d . . . H233 H 0.4853 0.3946 0.3755 0.042 Uiso 1 1 calc R . . C234 C 0.4718(4) 0.2354(4) 0.3822(3) 0.0363(11) Uani 1 1 d . . . H234 H 0.5401 0.2192 0.4071 0.044 Uiso 1 1 calc R . . C235 C 0.4065(4) 0.1547(4) 0.3643(3) 0.0341(11) Uani 1 1 d . . . H235 H 0.4307 0.0837 0.3763 0.041 Uiso 1 1 calc R . . C236 C 0.3051(4) 0.1775(3) 0.3285(3) 0.0285(10) Uani 1 1 d . . . H236 H 0.2611 0.1221 0.3152 0.034 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 C1 0.036(3) 0.037(3) 0.035(3) -0.001(2) 0.004(2) 0.011(2) B2 0.031(3) 0.025(3) 0.029(3) -0.002(2) 0.000(2) 0.004(2) F2 0.065(7) 0.056(7) 0.063(7) -0.012(5) -0.013(5) 0.008(5) B20 0.031(3) 0.025(3) 0.029(3) -0.002(2) 0.000(2) 0.004(2) B3 0.023(3) 0.042(3) 0.041(3) 0.006(3) 0.000(2) 0.004(2) F3 0.112(10) 0.054(7) 0.057(7) -0.022(5) -0.015(6) 0.027(6) B30 0.023(3) 0.042(3) 0.041(3) 0.006(3) 0.000(2) 0.004(2) B4 0.023(3) 0.042(3) 0.042(3) 0.010(3) 0.000(2) 0.001(2) F4 0.049(9) 0.088(11) 0.064(10) 0.012(8) -0.003(6) -0.006(7) B40 0.023(3) 0.042(3) 0.042(3) 0.010(3) 0.000(2) 0.001(2) B5 0.038(3) 0.035(3) 0.030(3) -0.004(2) -0.008(2) 0.008(2) F5 0.112(10) 0.054(7) 0.057(7) -0.022(5) -0.015(6) 0.027(6) B50 0.038(3) 0.035(3) 0.030(3) -0.004(2) -0.008(2) 0.008(2) Fe6 0.0189(3) 0.0286(4) 0.0303(4) -0.0021(3) -0.0049(2) -0.0005(2) B7 0.023(2) 0.032(3) 0.040(3) 0.002(2) -0.005(2) -0.005(2) F7 0.0277(14) 0.0340(15) 0.0593(18) 0.0071(13) -0.0107(12) -0.0104(11) Fe8 0.0214(3) 0.0310(4) 0.0294(4) -0.0028(3) -0.0037(2) 0.0024(2) B9 0.026(2) 0.031(3) 0.030(3) 0.000(2) -0.010(2) -0.008(2) F9 0.0309(14) 0.0413(15) 0.0402(15) 0.0039(12) -0.0078(11) -0.0147(11) B10 0.017(2) 0.030(3) 0.025(3) -0.007(2) 0.0016(18) -0.0008(18) F10 0.0213(12) 0.0429(15) 0.0376(15) -0.0117(12) -0.0041(10) 0.0051(10) C61 0.034(3) 0.023(2) 0.048(3) -0.005(2) -0.013(2) 0.0002(18) O61 0.0329(19) 0.044(2) 0.068(3) -0.0036(18) -0.0246(17) 0.0040(15) C62 0.030(2) 0.042(3) 0.033(3) -0.003(2) -0.014(2) -0.006(2) O62 0.041(2) 0.079(3) 0.035(2) 0.0148(19) -0.0109(16) -0.0272(19) C63 0.025(2) 0.041(3) 0.042(3) -0.004(2) -0.013(2) 0.0052(19) O63 0.046(2) 0.045(2) 0.064(2) -0.0216(19) -0.0300(18) 0.0114(16) C81 0.029(3) 0.037(3) 0.042(3) -0.013(2) -0.012(2) 0.0025(19) O81 0.0257(18) 0.051(2) 0.062(2) -0.0125(18) -0.0081(16) -0.0009(15) C82 0.024(2) 0.040(3) 0.043(3) 0.004(2) -0.006(2) -0.001(2) O82 0.038(2) 0.036(2) 0.071(3) 0.0118(19) -0.0174(18) -0.0023(15) C83 0.027(2) 0.039(3) 0.045(3) -0.006(2) -0.008(2) 0.0090(19) O83 0.051(2) 0.066(3) 0.033(2) -0.0109(18) -0.0133(16) 0.0145(18) P1 0.0181(5) 0.0229(5) 0.0200(6) -0.0015(4) -0.0005(4) -0.0021(4) N1 0.0202(17) 0.0253(18) 0.0248(19) -0.0031(15) -0.0016(14) -0.0054(13) C111 0.020(2) 0.025(2) 0.018(2) -0.0016(17) -0.0035(15) 0.0024(16) C112 0.022(2) 0.027(2) 0.027(2) -0.0047(18) -0.0041(17) -0.0020(16) C113 0.031(2) 0.024(2) 0.031(2) -0.0031(19) -0.0077(18) -0.0022(17) C114 0.032(2) 0.026(2) 0.024(2) -0.0092(18) -0.0043(18) 0.0055(17) C115 0.024(2) 0.038(3) 0.029(2) 0.001(2) 0.0002(18) 0.0035(18) C116 0.022(2) 0.027(2) 0.026(2) 0.0011(18) -0.0008(17) -0.0032(17) C121 0.028(2) 0.021(2) 0.018(2) -0.0036(17) -0.0045(16) 0.0010(16) C122 0.041(3) 0.033(2) 0.024(2) 0.0025(19) -0.0153(19) -0.011(2) C123 0.059(3) 0.020(2) 0.039(3) 0.005(2) -0.021(2) -0.003(2) C124 0.045(3) 0.032(3) 0.033(3) -0.009(2) -0.016(2) 0.011(2) C125 0.022(2) 0.044(3) 0.031(3) -0.006(2) -0.0059(18) 0.0059(19) C126 0.023(2) 0.031(2) 0.020(2) -0.0079(18) 0.0016(16) 0.0004(17) C131 0.021(2) 0.029(2) 0.023(2) 0.0020(18) -0.0038(16) -0.0041(16) C132 0.035(3) 0.035(3) 0.032(3) 0.005(2) -0.011(2) -0.0045(19) C133 0.045(3) 0.042(3) 0.046(3) 0.018(2) -0.019(2) -0.011(2) C134 0.044(3) 0.073(4) 0.027(3) 0.016(3) -0.011(2) -0.028(3) C135 0.033(3) 0.054(3) 0.030(3) -0.002(2) 0.000(2) -0.014(2) C136 0.026(2) 0.036(2) 0.028(2) -0.002(2) -0.0001(18) -0.0105(18) P2 0.0169(5) 0.0229(6) 0.0193(5) -0.0020(4) -0.0013(4) -0.0007(4) C211 0.023(2) 0.021(2) 0.024(2) 0.0026(17) -0.0065(16) -0.0017(16) C212 0.041(3) 0.032(3) 0.030(3) -0.001(2) 0.000(2) -0.003(2) C213 0.059(3) 0.041(3) 0.026(3) 0.004(2) 0.007(2) -0.006(2) C214 0.054(3) 0.043(3) 0.031(3) 0.015(2) -0.014(2) -0.018(2) C215 0.037(3) 0.027(2) 0.048(3) 0.005(2) -0.012(2) -0.0073(19) C216 0.024(2) 0.031(2) 0.035(3) -0.002(2) -0.0016(18) -0.0043(18) C221 0.0181(19) 0.024(2) 0.020(2) -0.0007(17) -0.0015(15) -0.0010(15) C222 0.022(2) 0.028(2) 0.025(2) 0.0010(18) -0.0067(16) -0.0028(16) C223 0.019(2) 0.031(2) 0.034(3) 0.001(2) 0.0006(17) 0.0027(17) C224 0.022(2) 0.041(3) 0.032(3) -0.009(2) 0.0037(18) -0.0028(18) C225 0.026(2) 0.052(3) 0.021(2) 0.000(2) -0.0032(17) -0.003(2) C226 0.020(2) 0.037(3) 0.028(2) -0.005(2) -0.0053(17) 0.0029(17) C231 0.0175(19) 0.029(2) 0.018(2) -0.0012(17) -0.0019(15) 0.0022(16) C232 0.024(2) 0.031(2) 0.027(2) -0.0031(19) -0.0041(17) 0.0002(17) C233 0.023(2) 0.051(3) 0.030(3) -0.004(2) -0.0053(18) -0.002(2) C234 0.021(2) 0.058(3) 0.026(2) -0.001(2) -0.0029(18) 0.007(2) C235 0.032(2) 0.037(3) 0.029(3) 0.005(2) -0.0060(19) 0.010(2) C236 0.022(2) 0.033(2) 0.028(2) 0.0002(19) -0.0009(17) 0.0019(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 B3 1.590(7) . ? C1 B4 1.608(7) . ? C1 B2 1.622(7) . ? C1 B5 1.629(7) . ? C1 H1 1.0699 . ? B2 F2 1.377(11) . ? B2 B9 1.791(7) . ? B2 B5 1.801(8) . ? B2 B3 1.973(7) . ? B2 Fe6 2.172(5) . ? B3 F3 1.36(6) . ? B3 B7 1.767(7) . ? B3 B4 1.769(8) . ? B3 Fe6 2.228(5) . ? B4 F4 1.368(14) . ? B4 B7 1.780(8) . ? B4 B5 2.024(8) . ? B4 Fe8 2.210(5) . ? B5 F5 1.389(12) . ? B5 B9 1.742(7) . ? B5 Fe8 2.215(5) . ? Fe6 C63 1.784(5) . ? Fe6 C62 1.790(5) . ? Fe6 C61 1.810(5) . ? Fe6 B10 2.032(5) . ? Fe6 B7 2.237(6) . ? Fe6 B9 2.241(5) . ? B7 F7 1.405(5) . ? B7 B10 1.859(7) . ? B7 Fe8 2.229(5) . ? Fe8 C82 1.788(5) . ? Fe8 C81 1.795(5) . ? Fe8 C83 1.817(5) . ? Fe8 B10 2.030(5) . ? Fe8 B9 2.249(5) . ? B9 F9 1.419(5) . ? B9 B10 1.841(7) . ? B10 F10 1.381(5) . ? C61 O61 1.160(5) . ? C62 O62 1.152(5) . ? C63 O63 1.148(5) . ? C81 O81 1.154(5) . ? C82 O82 1.147(5) . ? C83 O83 1.143(5) . ? P1 N1 1.590(3) . ? P1 C111 1.807(4) . ? P1 C121 1.808(4) . ? P1 C131 1.811(4) . ? N1 P2 1.584(3) . ? C111 C112 1.393(5) . ? C111 C116 1.401(5) . ? C112 C113 1.387(5) . ? C112 H112 0.9500 . ? C113 C114 1.394(6) . ? C113 H113 0.9500 . ? C114 C115 1.388(6) . ? C114 H114 0.9500 . ? C115 C116 1.398(6) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.398(6) . ? C121 C126 1.415(6) . ? C122 C123 1.397(6) . ? C122 H122 0.9500 . ? C123 C124 1.382(7) . ? C123 H123 0.9500 . ? C124 C125 1.376(6) . ? C124 H124 0.9500 . ? C125 C126 1.382(6) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C131 C132 1.401(6) . ? C131 C136 1.402(6) . ? C132 C133 1.386(6) . ? C132 H132 0.9500 . ? C133 C134 1.387(7) . ? C133 H133 0.9500 . ? C134 C135 1.378(7) . ? C134 H134 0.9500 . ? C135 C136 1.388(6) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? P2 C211 1.802(4) . ? P2 C231 1.810(4) . ? P2 C221 1.813(4) . ? C211 C216 1.400(6) . ? C211 C212 1.400(6) . ? C212 C213 1.383(6) . ? C212 H212 0.9500 . ? C213 C214 1.390(7) . ? C213 H213 0.9500 . ? C214 C215 1.378(7) . ? C214 H214 0.9500 . ? C215 C216 1.393(6) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C226 1.396(6) . ? C221 C222 1.412(5) . ? C222 C223 1.396(6) . ? C222 H222 0.9500 . ? C223 C224 1.385(6) . ? C223 H223 0.9500 . ? C224 C225 1.393(6) . ? C224 H224 0.9500 . ? C225 C226 1.394(6) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C231 C236 1.396(6) . ? C231 C232 1.403(6) . ? C232 C233 1.389(6) . ? C232 H232 0.9500 . ? C233 C234 1.391(7) . ? C233 H233 0.9500 . ? C234 C235 1.383(7) . ? C234 H234 0.9500 . ? C235 C236 1.397(6) . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? 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 B3 C1 B4 67.2(3) . . ? B3 C1 B2 75.8(3) . . ? B4 C1 B2 112.7(4) . . ? B3 C1 B5 112.1(4) . . ? B4 C1 B5 77.4(3) . . ? B2 C1 B5 67.3(3) . . ? B3 C1 H1 124.4 . . ? B4 C1 H1 123.2 . . ? B2 C1 H1 124.0 . . ? B5 C1 H1 123.5 . . ? F2 B2 C1 119.2(5) . . ? F2 B2 B9 121.2(6) . . ? C1 B2 B9 107.0(4) . . ? F2 B2 B5 123.2(6) . . ? C1 B2 B5 56.5(3) . . ? B9 B2 B5 58.0(3) . . ? F2 B2 B3 134.7(6) . . ? C1 B2 B3 51.4(3) . . ? B9 B2 B3 101.9(3) . . ? B5 B2 B3 89.9(3) . . ? F2 B2 Fe6 117.0(5) . . ? C1 B2 Fe6 113.8(3) . . ? B9 B2 Fe6 68.1(2) . . ? B5 B2 Fe6 113.2(3) . . ? B3 B2 Fe6 64.8(2) . . ? F3 B3 C1 119.1(18) . . ? F3 B3 B7 122.1(19) . . ? C1 B3 B7 108.8(4) . . ? F3 B3 B4 124(2) . . ? C1 B3 B4 56.9(3) . . ? B7 B3 B4 60.5(3) . . ? F3 B3 B2 133(2) . . ? C1 B3 B2 52.8(3) . . ? B7 B3 B2 101.4(3) . . ? B4 B3 B2 91.7(3) . . ? F3 B3 Fe6 117(2) . . ? C1 B3 Fe6 112.4(3) . . ? B7 B3 Fe6 67.0(2) . . ? B4 B3 Fe6 113.8(3) . . ? B2 B3 Fe6 61.9(2) . . ? F4 B4 C1 113.2(7) . . ? F4 B4 B3 126.0(7) . . ? C1 B4 B3 56.0(3) . . ? F4 B4 B7 130.3(8) . . ? C1 B4 B7 107.4(4) . . ? B3 B4 B7 59.7(3) . . ? F4 B4 B5 127.6(7) . . ? C1 B4 B5 51.7(3) . . ? B3 B4 B5 89.2(3) . . ? B7 B4 B5 99.8(3) . . ? F4 B4 Fe8 118.4(6) . . ? C1 B4 Fe8 112.5(3) . . ? B3 B4 Fe8 113.2(3) . . ? B7 B4 Fe8 66.9(2) . . ? B5 B4 Fe8 62.9(2) . . ? F5 B5 C1 120.5(6) . . ? F5 B5 B9 119.9(6) . . ? C1 B5 B9 109.1(4) . . ? F5 B5 B2 124.6(6) . . ? C1 B5 B2 56.2(3) . . ? B9 B5 B2 60.7(3) . . ? F5 B5 B4 134.8(6) . . ? C1 B5 B4 50.8(3) . . ? B9 B5 B4 102.1(3) . . ? B2 B5 B4 89.1(3) . . ? F5 B5 Fe8 116.6(5) . . ? C1 B5 Fe8 111.4(3) . . ? B9 B5 Fe8 68.0(2) . . ? B2 B5 Fe8 113.4(3) . . ? B4 B5 Fe8 62.6(2) . . ? C63 Fe6 C62 98.2(2) . . ? C63 Fe6 C61 94.03(19) . . ? C62 Fe6 C61 93.6(2) . . ? C63 Fe6 B10 80.78(19) . . ? C62 Fe6 B10 102.8(2) . . ? C61 Fe6 B10 163.3(2) . . ? C63 Fe6 B2 168.6(2) . . ? C62 Fe6 B2 92.6(2) . . ? C61 Fe6 B2 88.98(19) . . ? B10 Fe6 B2 93.24(19) . . ? C63 Fe6 B3 116.9(2) . . ? C62 Fe6 B3 143.6(2) . . ? C61 Fe6 B3 75.7(2) . . ? B10 Fe6 B3 92.44(19) . . ? B2 Fe6 B3 53.3(2) . . ? C63 Fe6 B7 86.6(2) . . ? C62 Fe6 B7 152.82(19) . . ? C61 Fe6 B7 112.8(2) . . ? B10 Fe6 B7 51.34(18) . . ? B2 Fe6 B7 82.1(2) . . ? B3 Fe6 B7 46.62(19) . . ? C63 Fe6 B9 129.78(19) . . ? C62 Fe6 B9 82.79(19) . . ? C61 Fe6 B9 136.16(19) . . ? B10 Fe6 B9 50.76(19) . . ? B2 Fe6 B9 47.87(19) . . ? B3 Fe6 B9 81.8(2) . . ? B7 Fe6 B9 73.87(18) . . ? F7 B7 B3 119.4(4) . . ? F7 B7 B4 119.6(4) . . ? B3 B7 B4 59.8(3) . . ? F7 B7 B10 114.9(4) . . ? B3 B7 B10 116.2(4) . . ? B4 B7 B10 116.0(3) . . ? F7 B7 Fe8 120.9(3) . . ? B3 B7 Fe8 112.4(3) . . ? B4 B7 Fe8 65.8(2) . . ? B10 B7 Fe8 58.7(2) . . ? F7 B7 Fe6 120.3(3) . . ? B3 B7 Fe6 66.4(2) . . ? B4 B7 Fe6 112.9(3) . . ? B10 B7 Fe6 58.6(2) . . ? Fe8 B7 Fe6 104.8(2) . . ? C82 Fe8 C81 95.0(2) . . ? C82 Fe8 C83 94.1(2) . . ? C81 Fe8 C83 96.8(2) . . ? C82 Fe8 B10 96.9(2) . . ? C81 Fe8 B10 84.13(19) . . ? C83 Fe8 B10 168.8(2) . . ? C82 Fe8 B4 98.8(2) . . ? C81 Fe8 B4 166.1(2) . . ? C83 Fe8 B4 83.1(2) . . ? B10 Fe8 B4 93.3(2) . . ? C82 Fe8 B5 152.5(2) . . ? C81 Fe8 B5 111.9(2) . . ? C83 Fe8 B5 77.7(2) . . ? B10 Fe8 B5 91.6(2) . . ? B4 Fe8 B5 54.4(2) . . ? C82 Fe8 B7 83.0(2) . . ? C81 Fe8 B7 134.6(2) . . ? C83 Fe8 B7 128.6(2) . . ? B10 Fe8 B7 51.50(18) . . ? B4 Fe8 B7 47.3(2) . . ? B5 Fe8 B7 82.0(2) . . ? C82 Fe8 B9 147.4(2) . . ? C81 Fe8 B9 85.6(2) . . ? C83 Fe8 B9 118.2(2) . . ? B10 Fe8 B9 50.66(19) . . ? B4 Fe8 B9 82.30(19) . . ? B5 Fe8 B9 45.95(19) . . ? B7 Fe8 B9 73.89(18) . . ? F9 B9 B5 119.9(4) . . ? F9 B9 B2 120.2(4) . . ? B5 B9 B2 61.3(3) . . ? F9 B9 B10 114.4(4) . . ? B5 B9 B10 116.4(4) . . ? B2 B9 B10 114.6(3) . . ? F9 B9 Fe6 120.3(3) . . ? B5 B9 Fe6 112.5(3) . . ? B2 B9 Fe6 64.0(2) . . ? B10 B9 Fe6 58.7(2) . . ? F9 B9 Fe8 121.6(3) . . ? B5 B9 Fe8 66.0(2) . . ? B2 B9 Fe8 112.2(3) . . ? B10 B9 Fe8 58.5(2) . . ? Fe6 B9 Fe8 103.99(19) . . ? F10 B10 B9 133.3(4) . . ? F10 B10 B7 133.3(4) . . ? B9 B10 B7 93.3(3) . . ? F10 B10 Fe8 118.2(3) . . ? B9 B10 Fe8 70.8(2) . . ? B7 B10 Fe8 69.8(2) . . ? F10 B10 Fe6 120.6(3) . . ? B9 B10 Fe6 70.5(2) . . ? B7 B10 Fe6 70.0(2) . . ? Fe8 B10 Fe6 121.1(2) . . ? O61 C61 Fe6 178.1(4) . . ? O62 C62 Fe6 176.6(4) . . ? O63 C63 Fe6 179.0(4) . . ? O81 C81 Fe8 176.4(4) . . ? O82 C82 Fe8 178.1(4) . . ? O83 C83 Fe8 179.7(5) . . ? N1 P1 C111 107.17(17) . . ? N1 P1 C121 112.29(18) . . ? C111 P1 C121 107.21(18) . . ? N1 P1 C131 113.77(18) . . ? C111 P1 C131 108.39(19) . . ? C121 P1 C131 107.74(19) . . ? P2 N1 P1 140.6(2) . . ? C112 C111 C116 120.3(4) . . ? C112 C111 P1 120.1(3) . . ? C116 C111 P1 119.5(3) . . ? C113 C112 C111 119.8(4) . . ? C113 C112 H112 120.1 . . ? C111 C112 H112 120.1 . . ? C112 C113 C114 119.9(4) . . ? C112 C113 H113 120.1 . . ? C114 C113 H113 120.1 . . ? C115 C114 C113 120.8(4) . . ? C115 C114 H114 119.6 . . ? C113 C114 H114 119.6 . . ? C114 C115 C116 119.5(4) . . ? C114 C115 H115 120.2 . . ? C116 C115 H115 120.2 . . ? C115 C116 C111 119.6(4) . . ? C115 C116 H116 120.2 . . ? C111 C116 H116 120.2 . . ? C122 C121 C126 118.9(4) . . ? C122 C121 P1 118.1(3) . . ? C126 C121 P1 122.9(3) . . ? C123 C122 C121 119.5(4) . . ? C123 C122 H122 120.2 . . ? C121 C122 H122 120.2 . . ? C124 C123 C122 120.5(4) . . ? C124 C123 H123 119.7 . . ? C122 C123 H123 119.7 . . ? C125 C124 C123 120.5(4) . . ? C125 C124 H124 119.7 . . ? C123 C124 H124 119.7 . . ? C124 C125 C126 120.1(4) . . ? C124 C125 H125 120.0 . . ? C126 C125 H125 120.0 . . ? C125 C126 C121 120.4(4) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? C132 C131 C136 119.3(4) . . ? C132 C131 P1 119.9(3) . . ? C136 C131 P1 120.4(3) . . ? C133 C132 C131 120.0(4) . . ? C133 C132 H132 120.0 . . ? C131 C132 H132 120.0 . . ? C132 C133 C134 119.9(5) . . ? C132 C133 H133 120.0 . . ? C134 C133 H133 120.0 . . ? C135 C134 C133 120.8(4) . . ? C135 C134 H134 119.6 . . ? C133 C134 H134 119.6 . . ? C134 C135 C136 119.9(5) . . ? C134 C135 H135 120.0 . . ? C136 C135 H135 120.0 . . ? C135 C136 C131 120.0(4) . . ? C135 C136 H136 120.0 . . ? C131 C136 H136 120.0 . . ? N1 P2 C211 110.75(18) . . ? N1 P2 C231 109.27(18) . . ? C211 P2 C231 105.87(18) . . ? N1 P2 C221 114.69(17) . . ? C211 P2 C221 108.67(18) . . ? C231 P2 C221 107.17(18) . . ? C216 C211 C212 119.5(4) . . ? C216 C211 P2 122.9(3) . . ? C212 C211 P2 117.6(3) . . ? C213 C212 C211 120.6(4) . . ? C213 C212 H212 119.7 . . ? C211 C212 H212 119.7 . . ? C212 C213 C214 119.2(4) . . ? C212 C213 H213 120.4 . . ? C214 C213 H213 120.4 . . ? C215 C214 C213 121.0(4) . . ? C215 C214 H214 119.5 . . ? C213 C214 H214 119.5 . . ? C214 C215 C216 120.2(4) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C215 C216 C211 119.5(4) . . ? C215 C216 H216 120.3 . . ? C211 C216 H216 120.3 . . ? C226 C221 C222 119.2(3) . . ? C226 C221 P2 120.8(3) . . ? C222 C221 P2 119.8(3) . . ? C223 C222 C221 119.8(4) . . ? C223 C222 H222 120.1 . . ? C221 C222 H222 120.1 . . ? C224 C223 C222 120.0(4) . . ? C224 C223 H223 120.0 . . ? C222 C223 H223 120.0 . . ? C223 C224 C225 120.8(4) . . ? C223 C224 H224 119.6 . . ? C225 C224 H224 119.6 . . ? C224 C225 C226 119.5(4) . . ? C224 C225 H225 120.3 . . ? C226 C225 H225 120.3 . . ? C225 C226 C221 120.7(4) . . ? C225 C226 H226 119.7 . . ? C221 C226 H226 119.7 . . ? C236 C231 C232 119.8(4) . . ? C236 C231 P2 119.6(3) . . ? C232 C231 P2 120.5(3) . . ? C233 C232 C231 120.3(4) . . ? C233 C232 H232 119.8 . . ? C231 C232 H232 119.8 . . ? C232 C233 C234 119.4(4) . . ? C232 C233 H233 120.3 . . ? C234 C233 H233 120.3 . . ? C235 C234 C233 120.8(4) . . ? C235 C234 H234 119.6 . . ? C233 C234 H234 119.6 . . ? C234 C235 C236 120.2(4) . . ? C234 C235 H235 119.9 . . ? C236 C235 H235 119.9 . . ? C231 C236 C235 119.5(4) . . ? C231 C236 H236 120.2 . . ? C235 C236 H236 120.2 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.661 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.112 #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 634921' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H33 B7 F3 Fe N O3 P2' _chemical_formula_weight 826.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.3552(13) _cell_length_b 10.4426(7) _cell_length_c 22.5348(15) _cell_angle_alpha 90.00 _cell_angle_beta 95.363(4) _cell_angle_gamma 90.00 _cell_volume 4066.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2182 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 20.55 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.186 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.105 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23088 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.09 _reflns_number_total 7340 _reflns_number_gt 4338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _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^)+(0.0470P)^2^+2.0675P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7340 _refine_ls_number_parameters 528 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.72667(4) 0.26287(6) 0.04194(3) 0.0234(2) Uani 1 1 d . . . P2 P 0.40030(7) 0.39083(10) 0.24089(5) 0.0169(3) Uani 1 1 d . . . P1 P 0.49983(7) 0.61203(10) 0.27464(5) 0.0173(3) Uani 1 1 d . . . N1 N 0.4371(2) 0.5289(3) 0.23637(15) 0.0172(9) Uani 1 1 d . . . C211 C 0.4119(2) 0.3050(4) 0.17364(18) 0.0153(10) Uani 1 1 d . . . C216 C 0.4649(3) 0.3466(4) 0.1356(2) 0.0238(11) Uani 1 1 d . . . H216 H 0.4943 0.4218 0.1448 0.029 Uiso 1 1 calc R . . C215 C 0.4750(3) 0.2787(4) 0.0841(2) 0.0297(12) Uani 1 1 d . . . H215 H 0.5111 0.3081 0.0580 0.036 Uiso 1 1 calc R . . C213 C 0.3800(3) 0.1269(4) 0.1086(2) 0.0254(12) Uani 1 1 d . . . H213 H 0.3512 0.0510 0.0993 0.030 Uiso 1 1 calc R . . C212 C 0.3684(3) 0.1941(4) 0.1599(2) 0.0233(11) Uani 1 1 d . . . H212 H 0.3315 0.1655 0.1855 0.028 Uiso 1 1 calc R . . C214 C 0.4329(3) 0.1688(4) 0.0706(2) 0.0307(13) Uani 1 1 d . . . H214 H 0.4402 0.1221 0.0353 0.037 Uiso 1 1 calc R . . C112 C 0.3818(3) 0.6681(4) 0.3444(2) 0.0217(11) Uani 1 1 d . . . H112 H 0.3500 0.6215 0.3154 0.026 Uiso 1 1 calc R . . C115 C 0.4734(3) 0.8075(4) 0.4287(2) 0.0278(12) Uani 1 1 d . . . H115 H 0.5043 0.8564 0.4574 0.033 Uiso 1 1 calc R . . C116 C 0.5067(3) 0.7533(4) 0.38111(19) 0.0214(11) Uani 1 1 d . . . H116 H 0.5604 0.7638 0.3776 0.026 Uiso 1 1 calc R . . C111 C 0.4607(3) 0.6827(4) 0.33807(19) 0.0183(10) Uani 1 1 d . . . C114 C 0.3952(3) 0.7907(4) 0.4345(2) 0.0264(12) Uani 1 1 d . . . H114 H 0.3728 0.8274 0.4674 0.032 Uiso 1 1 calc R . . C113 C 0.3500(3) 0.7211(4) 0.3926(2) 0.0272(12) Uani 1 1 d . . . H113 H 0.2965 0.7094 0.3969 0.033 Uiso 1 1 calc R . . C126 C 0.5995(3) 0.4813(4) 0.3593(2) 0.0226(11) Uani 1 1 d . . . H126 H 0.5675 0.5092 0.3887 0.027 Uiso 1 1 calc R . . C125 C 0.6615(3) 0.3986(4) 0.3743(2) 0.0287(12) Uani 1 1 d . . . H125 H 0.6713 0.3690 0.4142 0.034 Uiso 1 1 calc R . . C122 C 0.6331(3) 0.4825(4) 0.2577(2) 0.0267(12) Uani 1 1 d . . . H122 H 0.6236 0.5116 0.2178 0.032 Uiso 1 1 calc R . . C121 C 0.5855(3) 0.5222(4) 0.3006(2) 0.0207(11) Uani 1 1 d . . . C123 C 0.6946(3) 0.4004(4) 0.2734(2) 0.0305(13) Uani 1 1 d . . . H123 H 0.7269 0.3724 0.2441 0.037 Uiso 1 1 calc R . . C124 C 0.7086(3) 0.3597(4) 0.3317(2) 0.0336(13) Uani 1 1 d . . . H124 H 0.7510 0.3043 0.3426 0.040 Uiso 1 1 calc R . . C222 C 0.2567(2) 0.4839(4) 0.20325(19) 0.0189(11) Uani 1 1 d . . . H222 H 0.2839 0.5298 0.1753 0.023 Uiso 1 1 calc R . . C221 C 0.2971(2) 0.4037(4) 0.24544(19) 0.0178(10) Uani 1 1 d . . . C223 C 0.1773(3) 0.4959(4) 0.2024(2) 0.0266(12) Uani 1 1 d . . . H223 H 0.1496 0.5485 0.1734 0.032 Uiso 1 1 calc R . . C226 C 0.2569(3) 0.3366(4) 0.2853(2) 0.0212(11) Uani 1 1 d . . . H226 H 0.2838 0.2796 0.3128 0.025 Uiso 1 1 calc R . . C224 C 0.1386(3) 0.4316(4) 0.2437(2) 0.0259(12) Uani 1 1 d . . . H224 H 0.0842 0.4419 0.2436 0.031 Uiso 1 1 calc R . . C225 C 0.1778(3) 0.3515(4) 0.2854(2) 0.0278(12) Uani 1 1 d . . . H225 H 0.1506 0.3075 0.3139 0.033 Uiso 1 1 calc R . . C231 C 0.4430(2) 0.2952(4) 0.30221(19) 0.0159(10) Uani 1 1 d . . . C232 C 0.4272(3) 0.3216(4) 0.36069(19) 0.0212(11) Uani 1 1 d . . . H232 H 0.3917 0.3877 0.3681 0.025 Uiso 1 1 calc R . . C235 C 0.5322(3) 0.1312(4) 0.3395(2) 0.0275(12) Uani 1 1 d . . . H235 H 0.5689 0.0668 0.3324 0.033 Uiso 1 1 calc R . . C236 C 0.4956(3) 0.1996(4) 0.2920(2) 0.0221(11) Uani 1 1 d . . . H236 H 0.5066 0.1809 0.2524 0.027 Uiso 1 1 calc R . . C233 C 0.4629(3) 0.2521(4) 0.4078(2) 0.0268(11) Uani 1 1 d . . . H233 H 0.4516 0.2697 0.4474 0.032 Uiso 1 1 calc R . . C234 C 0.5152(3) 0.1565(4) 0.3967(2) 0.0264(12) Uani 1 1 d . . . H234 H 0.5396 0.1082 0.4289 0.032 Uiso 1 1 calc R . . C132 C 0.5812(3) 0.8309(4) 0.2480(2) 0.0233(11) Uani 1 1 d . . . H132 H 0.6027 0.8282 0.2883 0.028 Uiso 1 1 calc R . . C131 C 0.5294(2) 0.7360(4) 0.22615(19) 0.0175(10) Uani 1 1 d . . . C136 C 0.5005(3) 0.7387(4) 0.1667(2) 0.0247(11) Uani 1 1 d . . . H136 H 0.4661 0.6736 0.1511 0.030 Uiso 1 1 calc R . . C133 C 0.6012(3) 0.9291(4) 0.2110(2) 0.0284(12) Uani 1 1 d . . . H133 H 0.6357 0.9942 0.2264 0.034 Uiso 1 1 calc R . . C135 C 0.5220(3) 0.8371(5) 0.1300(2) 0.0354(14) Uani 1 1 d . . . H135 H 0.5024 0.8383 0.0892 0.042 Uiso 1 1 calc R . . C134 C 0.5714(3) 0.9330(4) 0.1522(2) 0.0326(13) Uani 1 1 d . . . H134 H 0.5848 1.0010 0.1271 0.039 Uiso 1 1 calc R . . C1 C 0.6558(3) 0.5437(4) 0.0178(2) 0.0332(13) Uani 1 1 d . . . H1 H 0.6093 0.6183 0.0161 0.040 Uiso 1 1 calc R . . C72 C 0.7976(3) 0.1615(5) 0.0161(2) 0.0337(13) Uani 1 1 d . . . C71 C 0.6478(3) 0.1622(4) 0.0178(2) 0.0290(12) Uani 1 1 d . . . C73 C 0.7330(3) 0.2115(4) 0.1179(2) 0.0308(13) Uani 1 1 d . . . O71 O 0.5956(2) 0.0970(3) 0.00272(16) 0.0434(10) Uani 1 1 d . . . O73 O 0.7355(2) 0.1793(3) 0.16687(16) 0.0434(10) Uani 1 1 d . . . O72 O 0.8443(2) 0.0976(3) -0.00231(17) 0.0502(11) Uani 1 1 d . . . B6 B 0.7703(4) 0.4255(5) 0.0850(3) 0.0316(15) Uani 1 1 d . . . B3 B 0.6734(4) 0.4522(6) 0.0746(3) 0.0333(15) Uani 1 1 d . . . B5 B 0.7130(3) 0.5187(5) -0.0326(3) 0.0303(15) Uani 1 1 d . . . H5 H 0.7178 0.5827 -0.0720 0.036 Uiso 1 1 calc R . . B2 B 0.7422(4) 0.5617(5) 0.0485(2) 0.0338(16) Uani 1 1 d . . . H2 H 0.7667 0.6554 0.0655 0.041 Uiso 1 1 calc R . . B4 B 0.6410(4) 0.4081(5) -0.0136(3) 0.0309(15) Uani 1 1 d . . . B9 B 0.7927(3) 0.4241(5) 0.0114(3) 0.0301(14) Uani 1 1 d . . . B8 B 0.7241(4) 0.3565(5) -0.0404(3) 0.0327(15) Uani 1 1 d . . . F9 F 0.87087(17) 0.4312(3) -0.00015(14) 0.0515(9) Uani 1 1 d . . . F6 F 0.8177(2) 0.4291(3) 0.13620(15) 0.0197(8) Uani 0.619(3) 1 d P . . F4 F 0.5686(2) 0.3755(4) -0.03753(18) 0.0360(16) Uani 0.623(6) 1 d P . . F8 F 0.7318(4) 0.2997(5) -0.0925(3) 0.0197(8) Uani 0.381(3) 1 d P . . F3 F 0.6346(5) 0.4626(7) 0.1192(4) 0.050(3) Uani 0.377(6) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0265(4) 0.0219(3) 0.0219(4) -0.0003(3) 0.0028(3) -0.0021(3) P2 0.0167(7) 0.0162(5) 0.0181(7) -0.0003(5) 0.0029(5) 0.0013(5) P1 0.0160(7) 0.0169(5) 0.0192(7) -0.0002(5) 0.0027(5) 0.0003(5) N1 0.017(2) 0.0167(17) 0.018(2) -0.0013(16) -0.0005(17) 0.0035(16) C211 0.013(2) 0.016(2) 0.017(3) 0.0015(19) 0.000(2) -0.0003(19) C216 0.028(3) 0.020(2) 0.024(3) -0.002(2) 0.009(2) -0.002(2) C215 0.039(3) 0.022(2) 0.030(3) 0.000(2) 0.013(3) -0.007(2) C213 0.028(3) 0.018(2) 0.030(3) -0.003(2) 0.001(2) -0.004(2) C212 0.024(3) 0.024(2) 0.022(3) -0.002(2) 0.005(2) 0.000(2) C214 0.044(3) 0.025(2) 0.024(3) -0.008(2) 0.009(3) 0.000(2) C112 0.020(3) 0.020(2) 0.025(3) 0.000(2) 0.003(2) 0.003(2) C115 0.038(3) 0.023(2) 0.022(3) -0.007(2) -0.003(3) -0.002(2) C116 0.020(3) 0.024(2) 0.019(3) -0.001(2) 0.001(2) 0.004(2) C111 0.024(3) 0.018(2) 0.013(2) 0.0036(19) 0.002(2) 0.002(2) C114 0.031(3) 0.027(2) 0.022(3) -0.006(2) 0.008(2) 0.007(2) C113 0.021(3) 0.030(3) 0.032(3) -0.004(2) 0.010(2) 0.006(2) C126 0.020(3) 0.019(2) 0.028(3) 0.000(2) 0.002(2) -0.001(2) C125 0.024(3) 0.027(3) 0.034(3) 0.007(2) -0.003(2) 0.005(2) C122 0.027(3) 0.025(2) 0.027(3) -0.008(2) 0.002(2) 0.001(2) C121 0.016(3) 0.021(2) 0.024(3) -0.001(2) -0.001(2) 0.003(2) C123 0.021(3) 0.032(3) 0.040(3) -0.018(3) 0.005(2) 0.005(2) C124 0.025(3) 0.028(3) 0.048(4) -0.001(3) -0.001(3) 0.010(2) C222 0.017(3) 0.016(2) 0.024(3) -0.001(2) 0.001(2) -0.0025(19) C221 0.014(2) 0.016(2) 0.023(3) -0.006(2) 0.001(2) -0.0014(19) C223 0.025(3) 0.020(2) 0.032(3) -0.005(2) -0.005(2) 0.004(2) C226 0.020(3) 0.018(2) 0.026(3) 0.005(2) 0.007(2) -0.001(2) C224 0.013(3) 0.023(2) 0.042(3) -0.006(2) 0.002(2) 0.000(2) C225 0.022(3) 0.025(2) 0.039(3) 0.001(2) 0.015(2) -0.002(2) C231 0.013(2) 0.016(2) 0.019(3) -0.0028(19) 0.000(2) -0.0037(19) C232 0.019(3) 0.021(2) 0.023(3) -0.001(2) 0.003(2) 0.000(2) C235 0.025(3) 0.021(2) 0.037(3) -0.003(2) -0.001(2) 0.004(2) C236 0.022(3) 0.021(2) 0.023(3) -0.006(2) 0.003(2) 0.001(2) C233 0.031(3) 0.033(3) 0.016(3) 0.002(2) 0.003(2) 0.001(2) C234 0.029(3) 0.025(2) 0.025(3) 0.005(2) -0.002(2) -0.001(2) C132 0.021(3) 0.030(3) 0.019(3) -0.003(2) 0.002(2) -0.004(2) C131 0.015(2) 0.017(2) 0.021(3) -0.003(2) 0.004(2) 0.0033(19) C136 0.016(3) 0.030(3) 0.028(3) -0.002(2) 0.004(2) -0.003(2) C133 0.025(3) 0.022(2) 0.039(3) -0.003(2) 0.008(3) -0.004(2) C135 0.031(3) 0.044(3) 0.030(3) 0.011(3) -0.001(3) -0.007(3) C134 0.028(3) 0.031(3) 0.039(3) 0.013(2) 0.002(3) -0.004(2) C1 0.034(3) 0.032(3) 0.033(3) 0.003(2) 0.002(3) 0.004(2) C72 0.041(4) 0.026(3) 0.034(3) 0.011(2) 0.005(3) -0.006(3) C71 0.036(3) 0.026(3) 0.026(3) -0.006(2) 0.007(3) 0.003(2) C73 0.035(3) 0.024(3) 0.034(3) 0.000(2) 0.005(3) -0.003(2) O71 0.044(2) 0.0322(19) 0.053(3) -0.0088(18) -0.004(2) -0.0068(19) O73 0.071(3) 0.0304(19) 0.029(2) 0.0014(17) 0.008(2) 0.0016(19) O72 0.052(3) 0.038(2) 0.065(3) 0.008(2) 0.029(2) 0.015(2) B6 0.040(4) 0.025(3) 0.030(4) 0.002(3) 0.000(3) -0.011(3) B3 0.038(4) 0.047(4) 0.015(3) -0.009(3) 0.005(3) 0.000(3) B5 0.032(4) 0.030(3) 0.028(3) 0.006(3) 0.001(3) -0.003(3) B2 0.049(4) 0.026(3) 0.025(3) -0.004(3) -0.007(3) 0.002(3) B4 0.041(4) 0.027(3) 0.026(3) 0.004(3) 0.006(3) -0.008(3) B9 0.017(3) 0.031(3) 0.043(4) 0.005(3) 0.004(3) -0.004(3) B8 0.035(4) 0.031(3) 0.033(4) 0.003(3) 0.006(3) -0.004(3) F9 0.037(2) 0.0435(17) 0.076(2) 0.0108(17) 0.0108(17) -0.0040(15) F6 0.023(2) 0.0206(17) 0.0133(18) 0.0043(15) -0.0105(16) -0.0086(15) F4 0.032(3) 0.041(3) 0.033(3) 0.005(2) -0.007(2) -0.015(2) F8 0.023(2) 0.0206(17) 0.0133(18) 0.0043(15) -0.0105(16) -0.0086(15) F3 0.051(6) 0.046(5) 0.054(6) 0.002(4) 0.007(5) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C72 1.764(6) . ? Fe1 C71 1.771(5) . ? Fe1 C73 1.787(5) . ? Fe1 B6 2.065(5) . ? Fe1 B8 2.094(6) . ? Fe1 B9 2.185(6) . ? Fe1 B3 2.330(6) . ? Fe1 B4 2.393(6) . ? P2 N1 1.584(3) . ? P2 C211 1.788(4) . ? P2 C231 1.807(4) . ? P2 C221 1.808(4) . ? P1 N1 1.584(3) . ? P1 C111 1.798(5) . ? P1 C131 1.799(4) . ? P1 C121 1.808(4) . ? C211 C216 1.384(6) . ? C211 C212 1.401(6) . ? C216 C215 1.384(6) . ? C216 H216 0.9500 . ? C215 C214 1.379(6) . ? C215 H215 0.9500 . ? C213 C212 1.382(6) . ? C213 C214 1.385(6) . ? C213 H213 0.9500 . ? C212 H212 0.9500 . ? C214 H214 0.9500 . ? C112 C113 1.379(6) . ? C112 C111 1.398(6) . ? C112 H112 0.9500 . ? C115 C116 1.385(6) . ? C115 C114 1.387(6) . ? C115 H115 0.9500 . ? C116 C111 1.406(6) . ? C116 H116 0.9500 . ? C114 C113 1.377(6) . ? C114 H114 0.9500 . ? C113 H113 0.9500 . ? C126 C121 1.388(6) . ? C126 C125 1.396(6) . ? C126 H126 0.9500 . ? C125 C124 1.379(7) . ? C125 H125 0.9500 . ? C122 C123 1.389(6) . ? C122 C121 1.392(6) . ? C122 H122 0.9500 . ? C123 C124 1.382(6) . ? C123 H123 0.9500 . ? C124 H124 0.9500 . ? C222 C223 1.382(6) . ? C222 C221 1.405(5) . ? C222 H222 0.9500 . ? C221 C226 1.379(6) . ? C223 C224 1.373(6) . ? C223 H223 0.9500 . ? C226 C225 1.382(6) . ? C226 H226 0.9500 . ? C224 C225 1.389(6) . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C231 C236 1.386(6) . ? C231 C232 1.399(6) . ? C232 C233 1.383(6) . ? C232 H232 0.9500 . ? C235 C234 1.375(6) . ? C235 C236 1.391(6) . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? C233 C234 1.388(6) . ? C233 H233 0.9500 . ? C234 H234 0.9500 . ? C132 C133 1.385(6) . ? C132 C131 1.396(6) . ? C132 H132 0.9500 . ? C131 C136 1.385(6) . ? C136 C135 1.391(6) . ? C136 H136 0.9500 . ? C133 C134 1.378(6) . ? C133 H133 0.9500 . ? C135 C134 1.381(6) . ? C135 H135 0.9500 . ? C134 H134 0.9500 . ? C1 B4 1.592(7) . ? C1 B5 1.599(8) . ? C1 B2 1.602(8) . ? C1 B3 1.603(7) . ? C1 H1 1.1200 . ? C72 O72 1.156(6) . ? C71 O71 1.158(5) . ? C73 O73 1.151(5) . ? B6 F6 1.353(6) . ? B6 B2 1.692(7) . ? B6 B3 1.699(9) . ? B6 B9 1.740(8) . ? B3 F3 1.267(10) . ? B3 B2 1.792(9) . ? B3 B4 2.065(8) . ? B5 B8 1.716(8) . ? B5 B4 1.783(8) . ? B5 B9 1.902(8) . ? B5 B2 1.904(8) . ? B5 H5 1.1200 . ? B2 B9 1.916(8) . ? B2 H2 1.1200 . ? B4 F4 1.365(7) . ? B4 B8 1.702(9) . ? B9 F9 1.406(6) . ? B9 B8 1.737(8) . ? B8 F8 1.333(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C72 Fe1 C71 94.9(2) . . ? C72 Fe1 C73 98.8(2) . . ? C71 Fe1 C73 95.3(2) . . ? C72 Fe1 B6 114.3(2) . . ? C71 Fe1 B6 150.7(2) . . ? C73 Fe1 B6 79.0(2) . . ? C72 Fe1 B8 86.9(2) . . ? C71 Fe1 B8 93.0(2) . . ? C73 Fe1 B8 169.4(2) . . ? B6 Fe1 B8 90.5(2) . . ? C72 Fe1 B9 87.4(2) . . ? C71 Fe1 B9 140.7(2) . . ? C73 Fe1 B9 123.1(2) . . ? B6 Fe1 B9 48.2(2) . . ? B8 Fe1 B9 47.9(2) . . ? C72 Fe1 B3 157.4(2) . . ? C71 Fe1 B3 106.4(2) . . ? C73 Fe1 B3 86.7(2) . . ? B6 Fe1 B3 45.0(2) . . ? B8 Fe1 B3 84.7(2) . . ? B9 Fe1 B3 71.4(2) . . ? C72 Fe1 B4 128.8(2) . . ? C71 Fe1 B4 77.9(2) . . ? C73 Fe1 B4 132.1(2) . . ? B6 Fe1 B4 84.7(2) . . ? B8 Fe1 B4 44.0(2) . . ? B9 Fe1 B4 70.4(2) . . ? B3 Fe1 B4 51.84(19) . . ? N1 P2 C211 108.87(19) . . ? N1 P2 C231 114.41(18) . . ? C211 P2 C231 107.49(19) . . ? N1 P2 C221 110.06(19) . . ? C211 P2 C221 106.02(19) . . ? C231 P2 C221 109.6(2) . . ? N1 P1 C111 111.5(2) . . ? N1 P1 C131 106.51(18) . . ? C111 P1 C131 109.73(19) . . ? N1 P1 C121 113.23(18) . . ? C111 P1 C121 108.4(2) . . ? C131 P1 C121 107.3(2) . . ? P2 N1 P1 136.4(2) . . ? C216 C211 C212 119.8(4) . . ? C216 C211 P2 120.1(3) . . ? C212 C211 P2 120.1(4) . . ? C211 C216 C215 120.2(4) . . ? C211 C216 H216 119.9 . . ? C215 C216 H216 119.9 . . ? C214 C215 C216 120.3(5) . . ? C214 C215 H215 119.8 . . ? C216 C215 H215 119.8 . . ? C212 C213 C214 120.9(4) . . ? C212 C213 H213 119.6 . . ? C214 C213 H213 119.6 . . ? C213 C212 C211 119.2(5) . . ? C213 C212 H212 120.4 . . ? C211 C212 H212 120.4 . . ? C215 C214 C213 119.6(4) . . ? C215 C214 H214 120.2 . . ? C213 C214 H214 120.2 . . ? C113 C112 C111 120.3(4) . . ? C113 C112 H112 119.8 . . ? C111 C112 H112 119.8 . . ? C116 C115 C114 120.2(4) . . ? C116 C115 H115 119.9 . . ? C114 C115 H115 119.9 . . ? C115 C116 C111 119.8(4) . . ? C115 C116 H116 120.1 . . ? C111 C116 H116 120.1 . . ? C112 C111 C116 119.0(4) . . ? C112 C111 P1 118.9(3) . . ? C116 C111 P1 122.1(4) . . ? C113 C114 C115 120.2(5) . . ? C113 C114 H114 119.9 . . ? C115 C114 H114 119.9 . . ? C114 C113 C112 120.4(5) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C121 C126 C125 119.0(5) . . ? C121 C126 H126 120.5 . . ? C125 C126 H126 120.5 . . ? C124 C125 C126 120.4(4) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C123 C122 C121 120.0(4) . . ? C123 C122 H122 120.0 . . ? C121 C122 H122 120.0 . . ? C126 C121 C122 120.4(4) . . ? C126 C121 P1 122.3(4) . . ? C122 C121 P1 116.9(3) . . ? C124 C123 C122 119.6(5) . . ? C124 C123 H123 120.2 . . ? C122 C123 H123 120.2 . . ? C125 C124 C123 120.6(4) . . ? C125 C124 H124 119.7 . . ? C123 C124 H124 119.7 . . ? C223 C222 C221 119.8(4) . . ? C223 C222 H222 120.1 . . ? C221 C222 H222 120.1 . . ? C226 C221 C222 119.5(4) . . ? C226 C221 P2 124.3(3) . . ? C222 C221 P2 116.2(3) . . ? C224 C223 C222 119.9(4) . . ? C224 C223 H223 120.1 . . ? C222 C223 H223 120.1 . . ? C221 C226 C225 120.5(4) . . ? C221 C226 H226 119.7 . . ? C225 C226 H226 119.7 . . ? C223 C224 C225 120.8(4) . . ? C223 C224 H224 119.6 . . ? C225 C224 H224 119.6 . . ? C226 C225 C224 119.4(5) . . ? C226 C225 H225 120.3 . . ? C224 C225 H225 120.3 . . ? C236 C231 C232 119.3(4) . . ? C236 C231 P2 120.0(3) . . ? C232 C231 P2 120.6(3) . . ? C233 C232 C231 120.4(4) . . ? C233 C232 H232 119.8 . . ? C231 C232 H232 119.8 . . ? C234 C235 C236 120.1(4) . . ? C234 C235 H235 120.0 . . ? C236 C235 H235 120.0 . . ? C231 C236 C235 120.2(4) . . ? C231 C236 H236 119.9 . . ? C235 C236 H236 119.9 . . ? C232 C233 C234 119.6(4) . . ? C232 C233 H233 120.2 . . ? C234 C233 H233 120.2 . . ? C235 C234 C233 120.5(4) . . ? C235 C234 H234 119.7 . . ? C233 C234 H234 119.7 . . ? C133 C132 C131 120.2(4) . . ? C133 C132 H132 119.9 . . ? C131 C132 H132 119.9 . . ? C136 C131 C132 119.3(4) . . ? C136 C131 P1 120.3(3) . . ? C132 C131 P1 120.5(3) . . ? C131 C136 C135 119.8(4) . . ? C131 C136 H136 120.1 . . ? C135 C136 H136 120.1 . . ? C134 C133 C132 120.5(4) . . ? C134 C133 H133 119.7 . . ? C132 C133 H133 119.7 . . ? C134 C135 C136 120.8(4) . . ? C134 C135 H135 119.6 . . ? C136 C135 H135 119.6 . . ? C133 C134 C135 119.4(4) . . ? C133 C134 H134 120.3 . . ? C135 C134 H134 120.3 . . ? B4 C1 B5 67.9(4) . . ? B4 C1 B2 113.7(4) . . ? B5 C1 B2 73.0(4) . . ? B4 C1 B3 80.5(4) . . ? B5 C1 B3 112.7(4) . . ? B2 C1 B3 68.0(4) . . ? B4 C1 H1 121.2 . . ? B5 C1 H1 125.6 . . ? B2 C1 H1 125.1 . . ? B3 C1 H1 121.6 . . ? O72 C72 Fe1 177.9(5) . . ? O71 C71 Fe1 179.0(5) . . ? O73 C73 Fe1 178.6(5) . . ? F6 B6 B2 121.1(4) . . ? F6 B6 B3 128.9(5) . . ? B2 B6 B3 63.8(4) . . ? F6 B6 B9 129.9(5) . . ? B2 B6 B9 67.9(3) . . ? B3 B6 B9 100.2(4) . . ? F6 B6 Fe1 126.2(4) . . ? B2 B6 Fe1 112.7(3) . . ? B3 B6 Fe1 75.8(3) . . ? B9 B6 Fe1 69.5(3) . . ? F3 B3 C1 120.4(6) . . ? F3 B3 B6 119.9(6) . . ? C1 B3 B6 108.7(5) . . ? F3 B3 B2 128.8(6) . . ? C1 B3 B2 56.0(3) . . ? B6 B3 B2 57.9(3) . . ? F3 B3 B4 131.7(6) . . ? C1 B3 B4 49.5(3) . . ? B6 B3 B4 105.9(4) . . ? B2 B3 B4 87.5(4) . . ? F3 B3 Fe1 125.4(5) . . ? C1 B3 Fe1 107.8(4) . . ? B6 B3 Fe1 59.2(3) . . ? B2 B3 Fe1 98.2(4) . . ? B4 B3 Fe1 65.6(2) . . ? C1 B5 B8 108.4(4) . . ? C1 B5 B4 55.8(3) . . ? B8 B5 B4 58.2(3) . . ? C1 B5 B9 100.6(4) . . ? B8 B5 B9 57.1(3) . . ? B4 B5 B9 91.7(4) . . ? C1 B5 B2 53.6(3) . . ? B8 B5 B2 108.0(4) . . ? B4 B5 B2 92.9(4) . . ? B9 B5 B2 60.4(3) . . ? C1 B5 H5 124.2 . . ? B8 B5 H5 119.4 . . ? B4 B5 H5 133.0 . . ? B9 B5 H5 128.3 . . ? B2 B5 H5 126.0 . . ? C1 B2 B6 109.1(4) . . ? C1 B2 B3 56.1(3) . . ? B6 B2 B3 58.3(3) . . ? C1 B2 B5 53.4(3) . . ? B6 B2 B5 107.9(4) . . ? B3 B2 B5 92.3(4) . . ? C1 B2 B9 99.9(4) . . ? B6 B2 B9 57.2(3) . . ? B3 B2 B9 90.6(4) . . ? B5 B2 B9 59.7(3) . . ? C1 B2 H2 124.1 . . ? B6 B2 H2 119.0 . . ? B3 B2 H2 133.5 . . ? B5 B2 H2 126.4 . . ? B9 B2 H2 129.1 . . ? F4 B4 C1 120.1(5) . . ? F4 B4 B8 124.1(5) . . ? C1 B4 B8 109.4(4) . . ? F4 B4 B5 135.0(4) . . ? C1 B4 B5 56.2(3) . . ? B8 B4 B5 58.9(3) . . ? F4 B4 B3 126.5(5) . . ? C1 B4 B3 50.0(3) . . ? B8 B4 B3 104.4(4) . . ? B5 B4 B3 87.3(4) . . ? F4 B4 Fe1 123.6(4) . . ? C1 B4 Fe1 105.4(3) . . ? B8 B4 Fe1 58.6(3) . . ? B5 B4 Fe1 97.0(3) . . ? B3 B4 Fe1 62.5(2) . . ? F9 B9 B8 120.6(5) . . ? F9 B9 B6 118.8(4) . . ? B8 B9 B6 116.3(4) . . ? F9 B9 B5 122.9(4) . . ? B8 B9 B5 56.1(3) . . ? B6 B9 B5 106.0(4) . . ? F9 B9 B2 122.0(4) . . ? B8 B9 B2 106.6(4) . . ? B6 B9 B2 54.9(3) . . ? B5 B9 B2 59.8(3) . . ? F9 B9 Fe1 130.0(4) . . ? B8 B9 Fe1 63.3(3) . . ? B6 B9 Fe1 62.3(3) . . ? B5 B9 Fe1 100.8(3) . . ? B2 B9 Fe1 99.5(3) . . ? F8 B8 B4 127.7(5) . . ? F8 B8 B5 123.3(5) . . ? B4 B8 B5 62.9(3) . . ? F8 B8 B9 130.8(6) . . ? B4 B8 B9 100.5(4) . . ? B5 B8 B9 66.8(3) . . ? F8 B8 Fe1 125.3(4) . . ? B4 B8 Fe1 77.4(3) . . ? B5 B8 Fe1 111.3(4) . . ? B9 B8 Fe1 68.8(3) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.704 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.087 #============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 634922' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H5 B7 F3 Fe2 N O6' _chemical_formula_weight 431.48 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7205(4) _cell_length_b 30.2753(13) _cell_length_c 13.3901(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.357(2) _cell_angle_gamma 90.00 _cell_volume 3018.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5082 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.21 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6610 _exptl_absorpt_correction_T_max 0.8236 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X-8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49068 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6900 _reflns_number_gt 5725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _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^)+(0.0300P)^2^+1.2791P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6900 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe6 Fe 0.97237(4) 0.182410(10) 0.22345(2) 0.01272(8) Uani 1 1 d . . . Fe6A Fe 0.84532(4) 0.406059(10) 0.28088(2) 0.01235(8) Uani 1 1 d . . . Fe1A Fe 0.66691(4) 0.476869(10) 0.27552(2) 0.01255(8) Uani 1 1 d . . . Fe10 Fe 0.86595(4) 0.155766(10) 0.37734(2) 0.01283(8) Uani 1 1 d . . . C103 C 0.8027(3) 0.18557(8) 0.48288(18) 0.0188(5) Uani 1 1 d . . . N101 N 1.0836(3) 0.14502(7) 0.43326(15) 0.0199(4) Uani 1 1 d . . . O103 O 0.7631(3) 0.20320(6) 0.54708(13) 0.0284(4) Uani 1 1 d . . . O101 O 1.2323(2) 0.13716(7) 0.47440(14) 0.0316(5) Uani 1 1 d . . . O61 O 1.0846(2) 0.21093(6) 0.04108(13) 0.0249(4) Uani 1 1 d . . . C61 C 1.0426(3) 0.20022(8) 0.11248(19) 0.0183(5) Uani 1 1 d . . . C1 C 0.5751(3) 0.20518(7) 0.08920(17) 0.0168(5) Uani 1 1 d . . . H1 H 0.4907 0.2180 0.0134 0.020 Uiso 1 1 calc R . . F7 F 0.82162(17) 0.25446(4) 0.35452(10) 0.0174(3) Uani 1 1 d . . . F8 F 0.48007(17) 0.16335(4) 0.33728(10) 0.0181(3) Uani 1 1 d . . . B5 B 0.5323(4) 0.16272(9) 0.1483(2) 0.0154(5) Uani 1 1 d . . . H5 H 0.4094 0.1420 0.1174 0.019 Uiso 1 1 calc R . . B3 B 0.7567(4) 0.22852(9) 0.1544(2) 0.0158(5) Uani 1 1 d . . . H3 H 0.8061 0.2602 0.1289 0.019 Uiso 1 1 calc R . . B4 B 0.5567(4) 0.21853(8) 0.2003(2) 0.0159(5) Uani 1 1 d . . . H4 H 0.4529 0.2426 0.2110 0.019 Uiso 1 1 calc R . . B2 B 0.7314(3) 0.16929(8) 0.0994(2) 0.0152(5) Uani 1 1 d . . . H2 H 0.7609 0.1538 0.0297 0.018 Uiso 1 1 calc R . . B7 B 0.7843(3) 0.21756(8) 0.29210(19) 0.0139(5) Uani 1 1 d . . . B8 B 0.6094(3) 0.17160(8) 0.2866(2) 0.0145(5) Uani 1 1 d . . . B7A B 0.5768(4) 0.41758(9) 0.1816(2) 0.0157(5) Uani 1 1 d . . . F7A F 0.53333(18) 0.42567(4) 0.07716(10) 0.0203(3) Uani 1 1 d . . . F8A F 0.30063(17) 0.45845(4) 0.27989(10) 0.0194(3) Uani 1 1 d . . . B8A B 0.4550(4) 0.43541(8) 0.2830(2) 0.0148(5) Uani 1 1 d . . . C1A C 0.5182(3) 0.34495(7) 0.29622(18) 0.0181(5) Uani 1 1 d . . . H1A H 0.4717 0.3102 0.3020 0.022 Uiso 1 1 calc R . . C62A C 0.9177(3) 0.42850(8) 0.17218(18) 0.0181(5) Uani 1 1 d . . . B3A B 0.6299(3) 0.36017(9) 0.2172(2) 0.0164(5) Uani 1 1 d . . . H3A H 0.6626 0.3367 0.1601 0.020 Uiso 1 1 calc R . . B2A B 0.7048(4) 0.36413(9) 0.3653(2) 0.0171(5) Uani 1 1 d . . . H2A H 0.7979 0.3439 0.4267 0.020 Uiso 1 1 calc R . . B4A B 0.4105(4) 0.38206(9) 0.2223(2) 0.0182(6) Uani 1 1 d . . . H4A H 0.2741 0.3759 0.1689 0.022 Uiso 1 1 calc R . . B9A B 0.6784(3) 0.42322(8) 0.38602(19) 0.0137(5) Uani 1 1 d . . . F9A F 0.74185(18) 0.43658(4) 0.48636(10) 0.0203(3) Uani 1 1 d . . . N10A N 0.8630(3) 0.50313(6) 0.28326(17) 0.0221(5) Uani 1 1 d . . . O10A O 0.9951(2) 0.52246(6) 0.28981(17) 0.0341(5) Uani 1 1 d . . . O62A O 0.9582(2) 0.44168(6) 0.10276(14) 0.0273(4) Uani 1 1 d . . . O63A O 1.1199(2) 0.44220(6) 0.45813(14) 0.0304(4) Uani 1 1 d . . . C63A C 1.0191(3) 0.42860(8) 0.38760(19) 0.0192(5) Uani 1 1 d . . . C62 C 1.1389(3) 0.21653(7) 0.31174(18) 0.0169(5) Uani 1 1 d . . . O62 O 1.2380(2) 0.23853(6) 0.36762(14) 0.0246(4) Uani 1 1 d . . . O102 O 0.6920(2) 0.07197(6) 0.41660(13) 0.0256(4) Uani 1 1 d . . . C102 C 0.7596(3) 0.10359(8) 0.40243(17) 0.0179(5) Uani 1 1 d . . . C11A C 0.5878(3) 0.51036(7) 0.36949(18) 0.0167(5) Uani 1 1 d . . . B5A B 0.4810(4) 0.38578(9) 0.3617(2) 0.0184(6) Uani 1 1 d . . . H5A H 0.4018 0.3826 0.4204 0.022 Uiso 1 1 calc R . . C12A C 0.5148(3) 0.50467(8) 0.16496(19) 0.0207(5) Uani 1 1 d . . . O11A O 0.5366(2) 0.53151(6) 0.42504(13) 0.0236(4) Uani 1 1 d . . . O12A O 0.4175(3) 0.52240(6) 0.09879(15) 0.0347(5) Uani 1 1 d . . . O61A O 1.0502(2) 0.32478(6) 0.27993(16) 0.0305(4) Uani 1 1 d . . . C61A C 0.9708(3) 0.35629(8) 0.28018(19) 0.0202(5) Uani 1 1 d . . . C63 C 1.1027(3) 0.13169(8) 0.23167(18) 0.0174(5) Uani 1 1 d . . . O63 O 1.1779(2) 0.09936(6) 0.23540(14) 0.0255(4) Uani 1 1 d . . . B9 B 0.7503(3) 0.13679(8) 0.2159(2) 0.0143(5) Uani 1 1 d . . . F9 F 0.75570(17) 0.09190(4) 0.20108(10) 0.0177(3) 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 Fe6 0.01298(17) 0.00975(16) 0.01594(16) -0.00060(12) 0.00471(13) -0.00057(12) Fe6A 0.01188(16) 0.01089(16) 0.01463(16) -0.00046(12) 0.00411(13) 0.00056(12) Fe1A 0.01351(17) 0.00932(16) 0.01530(16) -0.00007(12) 0.00463(13) -0.00007(12) Fe10 0.01336(17) 0.01084(16) 0.01357(16) 0.00085(12) 0.00233(13) 0.00067(12) C103 0.0218(13) 0.0145(12) 0.0173(12) 0.0038(9) 0.0001(10) 0.0007(9) N101 0.0195(11) 0.0226(11) 0.0176(10) 0.0060(8) 0.0051(9) 0.0010(8) O103 0.0422(12) 0.0246(10) 0.0191(9) -0.0029(8) 0.0091(8) 0.0083(8) O101 0.0177(10) 0.0480(12) 0.0277(10) 0.0169(9) 0.0034(8) 0.0051(8) O61 0.0283(10) 0.0250(10) 0.0260(10) 0.0022(8) 0.0150(8) -0.0030(8) C61 0.0167(12) 0.0136(11) 0.0244(13) -0.0038(10) 0.0053(10) 0.0002(9) C1 0.0186(12) 0.0157(12) 0.0156(11) 0.0005(9) 0.0038(10) 0.0003(9) F7 0.0213(7) 0.0109(6) 0.0191(7) -0.0035(5) 0.0036(6) -0.0005(5) F8 0.0147(7) 0.0216(7) 0.0194(7) 0.0028(5) 0.0071(6) 0.0011(5) B5 0.0147(13) 0.0156(13) 0.0166(13) -0.0019(10) 0.0052(10) -0.0007(10) B3 0.0180(13) 0.0141(13) 0.0150(12) -0.0010(10) 0.0038(10) 0.0015(10) B4 0.0157(13) 0.0134(13) 0.0170(13) -0.0010(10) 0.0018(10) 0.0020(10) B2 0.0150(13) 0.0140(13) 0.0169(13) -0.0019(10) 0.0046(10) -0.0024(10) B7 0.0135(13) 0.0117(12) 0.0160(12) 0.0002(10) 0.0031(10) -0.0003(10) B8 0.0127(12) 0.0125(12) 0.0169(13) -0.0014(10) 0.0018(10) 0.0008(10) B7A 0.0152(13) 0.0151(13) 0.0164(12) -0.0016(10) 0.0033(10) -0.0003(10) F7A 0.0237(7) 0.0217(7) 0.0133(6) -0.0009(5) 0.0011(6) 0.0014(6) F8A 0.0138(7) 0.0159(7) 0.0292(8) -0.0009(6) 0.0067(6) 0.0021(5) B8A 0.0146(13) 0.0125(12) 0.0172(12) 0.0009(10) 0.0040(10) 0.0001(10) C1A 0.0179(12) 0.0122(11) 0.0254(13) 0.0002(9) 0.0079(10) -0.0022(9) C62A 0.0155(12) 0.0173(12) 0.0212(12) -0.0032(10) 0.0046(10) -0.0010(9) B3A 0.0152(13) 0.0140(13) 0.0193(13) -0.0023(10) 0.0032(11) -0.0003(10) B2A 0.0208(14) 0.0138(13) 0.0187(13) 0.0019(10) 0.0088(11) 0.0021(10) B4A 0.0172(14) 0.0131(13) 0.0249(14) -0.0029(11) 0.0066(11) -0.0035(10) B9A 0.0142(13) 0.0125(12) 0.0148(12) -0.0002(10) 0.0046(10) 0.0010(10) F9A 0.0248(8) 0.0216(7) 0.0140(6) -0.0018(5) 0.0043(6) 0.0038(6) N10A 0.0215(11) 0.0099(10) 0.0374(13) 0.0011(9) 0.0122(10) 0.0031(8) O10A 0.0202(10) 0.0162(9) 0.0688(15) 0.0013(9) 0.0170(10) -0.0035(7) O62A 0.0260(10) 0.0349(11) 0.0240(10) 0.0028(8) 0.0118(8) -0.0038(8) O63A 0.0201(9) 0.0407(12) 0.0259(10) -0.0055(8) -0.0018(8) -0.0026(8) C63A 0.0175(12) 0.0173(12) 0.0238(13) 0.0004(10) 0.0075(10) 0.0031(10) C62 0.0173(12) 0.0136(11) 0.0219(12) 0.0014(9) 0.0087(10) 0.0039(9) O62 0.0199(9) 0.0205(9) 0.0309(10) -0.0067(8) 0.0022(8) -0.0037(7) O102 0.0284(10) 0.0189(9) 0.0278(10) 0.0032(7) 0.0045(8) -0.0056(8) C102 0.0186(12) 0.0189(13) 0.0144(11) -0.0019(9) 0.0012(9) 0.0022(10) C11A 0.0153(12) 0.0122(11) 0.0214(12) 0.0013(9) 0.0027(10) -0.0017(9) B5A 0.0195(14) 0.0127(13) 0.0251(14) 0.0021(11) 0.0099(12) 0.0012(10) C12A 0.0268(14) 0.0133(12) 0.0227(13) 0.0025(10) 0.0079(11) 0.0004(10) O11A 0.0258(10) 0.0197(9) 0.0280(10) -0.0053(7) 0.0120(8) -0.0002(7) O12A 0.0412(12) 0.0306(11) 0.0293(10) 0.0134(9) 0.0038(9) 0.0067(9) O61A 0.0243(10) 0.0157(9) 0.0546(13) 0.0009(8) 0.0156(9) 0.0044(8) C61A 0.0160(12) 0.0187(13) 0.0275(13) 0.0023(10) 0.0082(10) -0.0027(10) C63 0.0166(12) 0.0173(12) 0.0199(12) 0.0002(9) 0.0075(10) -0.0031(10) O63 0.0224(9) 0.0158(9) 0.0389(11) -0.0020(8) 0.0094(8) 0.0040(7) B9 0.0148(13) 0.0133(12) 0.0164(12) -0.0029(10) 0.0066(10) -0.0012(10) F9 0.0212(7) 0.0096(6) 0.0232(7) -0.0033(5) 0.0077(6) -0.0024(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 Fe6 C61 1.794(3) . ? Fe6 C62 1.820(2) . ? Fe6 C63 1.823(2) . ? Fe6 B2 2.178(3) . ? Fe6 B3 2.182(3) . ? Fe6 B9 2.183(3) . ? Fe6 B7 2.189(3) . ? Fe6 Fe10 2.5434(5) . ? Fe6A C61A 1.793(2) . ? Fe6A C63A 1.815(2) . ? Fe6A C62A 1.823(3) . ? Fe6A B3A 2.162(3) . ? Fe6A B2A 2.171(3) . ? Fe6A B7A 2.174(3) . ? Fe6A B9A 2.208(3) . ? Fe6A Fe1A 2.5389(4) . ? Fe1A N10A 1.689(2) . ? Fe1A C12A 1.832(2) . ? Fe1A C11A 1.842(2) . ? Fe1A B8A 2.085(3) . ? Fe1A B9A 2.183(3) . ? Fe1A B7A 2.197(3) . ? Fe10 N101 1.680(2) . ? Fe10 C103 1.848(3) . ? Fe10 C102 1.852(2) . ? Fe10 B8 2.086(3) . ? Fe10 B9 2.185(3) . ? Fe10 B7 2.195(2) . ? C103 O103 1.121(3) . ? N101 O101 1.159(2) . ? O61 C61 1.135(3) . ? C1 B4 1.584(3) . ? C1 B5 1.589(3) . ? C1 B2 1.602(3) . ? C1 B3 1.606(3) . ? F7 B7 1.379(3) . ? F8 B8 1.370(3) . ? B5 B8 1.810(4) . ? B5 B4 1.818(4) . ? B5 B2 1.834(4) . ? B5 B9 1.861(4) . ? B3 B7 1.829(4) . ? B3 B4 1.831(4) . ? B3 B2 1.929(4) . ? B4 B8 1.809(4) . ? B4 B7 1.859(3) . ? B2 B9 1.818(4) . ? B7 B8 1.927(4) . ? B8 B9 1.933(4) . ? B7A F7A 1.371(3) . ? B7A B3A 1.820(4) . ? B7A B4A 1.863(4) . ? B7A B8A 1.922(4) . ? F8A B8A 1.372(3) . ? B8A B4A 1.800(4) . ? B8A B5A 1.816(4) . ? B8A B9A 1.938(4) . ? C1A B4A 1.581(3) . ? C1A B5A 1.585(4) . ? C1A B3A 1.599(4) . ? C1A B2A 1.600(3) . ? C62A O62A 1.129(3) . ? B3A B4A 1.837(4) . ? B3A B2A 1.916(4) . ? B2A B9A 1.830(4) . ? B2A B5A 1.837(4) . ? B4A B5A 1.805(4) . ? B9A F9A 1.364(3) . ? B9A B5A 1.858(4) . ? N10A O10A 1.159(3) . ? O63A C63A 1.130(3) . ? C62 O62 1.134(3) . ? O102 C102 1.130(3) . ? C11A O11A 1.129(3) . ? C12A O12A 1.134(3) . ? O61A C61A 1.135(3) . ? C63 O63 1.132(3) . ? B9 F9 1.376(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C61 Fe6 C62 92.92(10) . . ? C61 Fe6 C63 91.15(10) . . ? C62 Fe6 C63 98.93(10) . . ? C61 Fe6 B2 78.90(10) . . ? C62 Fe6 B2 155.91(10) . . ? C63 Fe6 B2 103.81(10) . . ? C61 Fe6 B3 79.71(10) . . ? C62 Fe6 B3 103.92(10) . . ? C63 Fe6 B3 155.72(10) . . ? B2 Fe6 B3 52.53(10) . . ? C61 Fe6 B9 123.91(10) . . ? C62 Fe6 B9 143.13(10) . . ? C63 Fe6 B9 83.34(10) . . ? B2 Fe6 B9 49.28(10) . . ? B3 Fe6 B9 83.29(10) . . ? C61 Fe6 B7 125.53(10) . . ? C62 Fe6 B7 83.36(10) . . ? C63 Fe6 B7 143.22(10) . . ? B2 Fe6 B7 83.19(10) . . ? B3 Fe6 B7 49.46(9) . . ? B9 Fe6 B7 74.14(9) . . ? C61 Fe6 Fe10 178.35(8) . . ? C62 Fe6 Fe10 88.74(8) . . ? C63 Fe6 Fe10 88.59(7) . . ? B2 Fe6 Fe10 99.57(7) . . ? B3 Fe6 Fe10 99.90(7) . . ? B9 Fe6 Fe10 54.44(7) . . ? B7 Fe6 Fe10 54.66(7) . . ? C61A Fe6A C63A 91.84(11) . . ? C61A Fe6A C62A 91.64(11) . . ? C63A Fe6A C62A 99.76(11) . . ? C61A Fe6A B3A 79.53(10) . . ? C63A Fe6A B3A 152.08(11) . . ? C62A Fe6A B3A 106.93(10) . . ? C61A Fe6A B2A 81.76(10) . . ? C63A Fe6A B2A 100.22(11) . . ? C62A Fe6A B2A 159.13(10) . . ? B3A Fe6A B2A 52.48(10) . . ? C61A Fe6A B7A 124.11(10) . . ? C63A Fe6A B7A 143.88(10) . . ? C62A Fe6A B7A 84.04(10) . . ? B3A Fe6A B7A 49.64(10) . . ? B2A Fe6A B7A 83.39(10) . . ? C61A Fe6A B9A 127.50(10) . . ? C63A Fe6A B9A 81.04(10) . . ? C62A Fe6A B9A 140.86(10) . . ? B3A Fe6A B9A 83.37(10) . . ? B2A Fe6A B9A 49.40(10) . . ? B7A Fe6A B9A 74.28(10) . . ? C61A Fe6A Fe1A 178.09(8) . . ? C63A Fe6A Fe1A 89.27(7) . . ? C62A Fe6A Fe1A 86.64(7) . . ? B3A Fe6A Fe1A 100.17(7) . . ? B2A Fe6A Fe1A 99.57(7) . . ? B7A Fe6A Fe1A 54.90(7) . . ? B9A Fe6A Fe1A 54.23(7) . . ? N10A Fe1A C12A 101.86(10) . . ? N10A Fe1A C11A 98.79(10) . . ? C12A Fe1A C11A 92.39(10) . . ? N10A Fe1A B8A 169.23(10) . . ? C12A Fe1A B8A 88.41(10) . . ? C11A Fe1A B8A 83.83(10) . . ? N10A Fe1A B9A 115.70(10) . . ? C12A Fe1A B9A 142.34(10) . . ? C11A Fe1A B9A 84.72(10) . . ? B8A Fe1A B9A 53.94(10) . . ? N10A Fe1A B7A 124.25(10) . . ? C12A Fe1A B7A 82.80(10) . . ? C11A Fe1A B7A 136.82(10) . . ? B8A Fe1A B7A 53.27(10) . . ? B9A Fe1A B7A 74.33(10) . . ? N10A Fe1A Fe6A 85.69(7) . . ? C12A Fe1A Fe6A 129.60(8) . . ? C11A Fe1A Fe6A 136.15(7) . . ? B8A Fe1A Fe6A 85.24(7) . . ? B9A Fe1A Fe6A 55.12(7) . . ? B7A Fe1A Fe6A 54.08(7) . . ? N101 Fe10 C103 100.92(10) . . ? N101 Fe10 C102 101.14(10) . . ? C103 Fe10 C102 93.33(10) . . ? N101 Fe10 B8 170.72(10) . . ? C103 Fe10 B8 86.01(10) . . ? C102 Fe10 B8 84.46(10) . . ? N101 Fe10 B9 119.23(10) . . ? C103 Fe10 B9 139.72(10) . . ? C102 Fe10 B9 82.55(10) . . ? B8 Fe10 B9 53.73(10) . . ? N101 Fe10 B7 120.81(10) . . ? C103 Fe10 B7 83.33(10) . . ? C102 Fe10 B7 137.85(10) . . ? B8 Fe10 B7 53.42(10) . . ? B9 Fe10 B7 73.98(9) . . ? N101 Fe10 Fe6 85.58(7) . . ? C103 Fe10 Fe6 132.24(7) . . ? C102 Fe10 Fe6 132.18(7) . . ? B8 Fe10 Fe6 85.19(8) . . ? B9 Fe10 Fe6 54.36(7) . . ? B7 Fe10 Fe6 54.43(7) . . ? O103 C103 Fe10 179.2(2) . . ? O101 N101 Fe10 177.95(19) . . ? O61 C61 Fe6 178.6(2) . . ? B4 C1 B5 69.92(16) . . ? B4 C1 B2 110.26(19) . . ? B5 C1 B2 70.16(16) . . ? B4 C1 B3 70.08(16) . . ? B5 C1 B3 110.61(19) . . ? B2 C1 B3 73.93(16) . . ? C1 B5 B8 109.51(18) . . ? C1 B5 B4 54.90(14) . . ? B8 B5 B4 59.82(14) . . ? C1 B5 B2 55.24(14) . . ? B8 B5 B2 105.64(17) . . ? B4 B5 B2 91.39(17) . . ? C1 B5 B9 107.63(18) . . ? B8 B5 B9 63.52(14) . . ? B4 B5 B9 102.53(17) . . ? B2 B5 B9 58.94(14) . . ? C1 B3 B7 108.70(19) . . ? C1 B3 B4 54.40(14) . . ? B7 B3 B4 61.05(14) . . ? C1 B3 B2 52.95(13) . . ? B7 B3 B2 100.93(17) . . ? B4 B3 B2 88.03(16) . . ? C1 B3 Fe6 114.02(16) . . ? B7 B3 Fe6 65.47(11) . . ? B4 B3 Fe6 111.66(15) . . ? B2 B3 Fe6 63.62(11) . . ? C1 B4 B8 109.80(18) . . ? C1 B4 B5 55.19(14) . . ? B8 B4 B5 59.86(14) . . ? C1 B4 B3 55.52(14) . . ? B8 B4 B3 106.08(17) . . ? B5 B4 B3 92.08(17) . . ? C1 B4 B7 108.21(19) . . ? B8 B4 B7 63.36(14) . . ? B5 B4 B7 102.86(17) . . ? B3 B4 B7 59.40(14) . . ? C1 B2 B9 109.11(19) . . ? C1 B2 B5 54.59(14) . . ? B9 B2 B5 61.25(14) . . ? C1 B2 B3 53.12(14) . . ? B9 B2 B3 101.42(17) . . ? B5 B2 B3 88.50(16) . . ? C1 B2 Fe6 114.40(16) . . ? B9 B2 Fe6 65.53(11) . . ? B5 B2 Fe6 112.02(15) . . ? B3 B2 Fe6 63.86(11) . . ? F7 B7 B3 114.45(18) . . ? F7 B7 B4 113.40(18) . . ? B3 B7 B4 59.54(14) . . ? F7 B7 B8 129.8(2) . . ? B3 B7 B8 101.49(16) . . ? B4 B7 B8 57.05(13) . . ? F7 B7 Fe6 126.37(17) . . ? B3 B7 Fe6 65.07(12) . . ? B4 B7 Fe6 110.24(14) . . ? B8 B7 Fe6 99.73(13) . . ? F7 B7 Fe10 112.95(15) . . ? B3 B7 Fe10 128.28(16) . . ? B4 B7 Fe10 116.63(14) . . ? B8 B7 Fe10 60.40(10) . . ? Fe6 B7 Fe10 70.91(8) . . ? F8 B8 B4 112.91(19) . . ? F8 B8 B5 113.21(18) . . ? B4 B8 B5 60.32(14) . . ? F8 B8 B7 135.07(19) . . ? B4 B8 B7 59.59(14) . . ? B5 B8 B7 100.57(17) . . ? F8 B8 B9 136.16(19) . . ? B4 B8 B9 100.12(17) . . ? B5 B8 B9 59.52(14) . . ? B7 B8 B9 86.15(15) . . ? F8 B8 Fe10 111.96(16) . . ? B4 B8 Fe10 124.80(16) . . ? B5 B8 Fe10 124.48(16) . . ? B7 B8 Fe10 66.19(11) . . ? B9 B8 Fe10 65.75(11) . . ? F7A B7A B3A 114.55(19) . . ? F7A B7A B4A 113.58(19) . . ? B3A B7A B4A 59.81(14) . . ? F7A B7A B8A 129.56(19) . . ? B3A B7A B8A 101.62(17) . . ? B4A B7A B8A 56.76(14) . . ? F7A B7A Fe6A 126.05(18) . . ? B3A B7A Fe6A 64.81(11) . . ? B4A B7A Fe6A 110.36(15) . . ? B8A B7A Fe6A 100.29(14) . . ? F7A B7A Fe1A 113.12(16) . . ? B3A B7A Fe1A 127.95(15) . . ? B4A B7A Fe1A 116.27(15) . . ? B8A B7A Fe1A 60.40(11) . . ? Fe6A B7A Fe1A 71.02(8) . . ? F8A B8A B4A 112.47(19) . . ? F8A B8A B5A 113.56(19) . . ? B4A B8A B5A 59.89(15) . . ? F8A B8A B7A 134.83(19) . . ? B4A B8A B7A 59.97(14) . . ? B5A B8A B7A 100.27(17) . . ? F8A B8A B9A 136.1(2) . . ? B4A B8A B9A 100.27(17) . . ? B5A B8A B9A 59.22(14) . . ? B7A B8A B9A 86.55(15) . . ? F8A B8A Fe1A 112.26(16) . . ? B4A B8A Fe1A 125.23(17) . . ? B5A B8A Fe1A 123.94(16) . . ? B7A B8A Fe1A 66.33(12) . . ? B9A B8A Fe1A 65.61(11) . . ? B4A C1A B5A 69.52(17) . . ? B4A C1A B3A 70.56(17) . . ? B5A C1A B3A 110.47(19) . . ? B4A C1A B2A 110.35(19) . . ? B5A C1A B2A 70.41(17) . . ? B3A C1A B2A 73.57(16) . . ? O62A C62A Fe6A 177.8(2) . . ? C1A B3A B7A 108.97(19) . . ? C1A B3A B4A 54.25(14) . . ? B7A B3A B4A 61.26(14) . . ? C1A B3A B2A 53.24(14) . . ? B7A B3A B2A 101.34(17) . . ? B4A B3A B2A 88.16(17) . . ? C1A B3A Fe6A 114.68(16) . . ? B7A B3A Fe6A 65.55(12) . . ? B4A B3A Fe6A 111.99(15) . . ? B2A B3A Fe6A 64.02(11) . . ? C1A B2A B9A 108.86(19) . . ? C1A B2A B5A 54.41(14) . . ? B9A B2A B5A 60.89(14) . . ? C1A B2A B3A 53.19(14) . . ? B9A B2A B3A 101.73(17) . . ? B5A B2A B3A 88.38(16) . . ? C1A B2A Fe6A 114.14(16) . . ? B9A B2A Fe6A 66.33(12) . . ? B5A B2A Fe6A 111.98(15) . . ? B3A B2A Fe6A 63.50(11) . . ? C1A B4A B8A 110.42(19) . . ? C1A B4A B5A 55.36(15) . . ? B8A B4A B5A 60.49(14) . . ? C1A B4A B3A 55.19(15) . . ? B8A B4A B3A 105.82(18) . . ? B5A B4A B3A 91.84(17) . . ? C1A B4A B7A 107.72(19) . . ? B8A B4A B7A 63.27(15) . . ? B5A B4A B7A 102.94(17) . . ? B3A B4A B7A 58.93(14) . . ? F9A B9A B2A 114.47(18) . . ? F9A B9A B5A 114.67(19) . . ? B2A B9A B5A 59.73(14) . . ? F9A B9A B8A 131.66(19) . . ? B2A B9A B8A 101.06(16) . . ? B5A B9A B8A 57.12(13) . . ? F9A B9A Fe1A 112.74(16) . . ? B2A B9A Fe1A 127.63(16) . . ? B5A B9A Fe1A 116.81(15) . . ? B8A B9A Fe1A 60.46(10) . . ? F9A B9A Fe6A 125.45(16) . . ? B2A B9A Fe6A 64.27(12) . . ? B5A B9A Fe6A 109.58(15) . . ? B8A B9A Fe6A 98.66(13) . . ? Fe1A B9A Fe6A 70.65(8) . . ? O10A N10A Fe1A 177.57(19) . . ? O63A C63A Fe6A 175.4(2) . . ? O62 C62 Fe6 177.7(2) . . ? O102 C102 Fe10 178.8(2) . . ? O11A C11A Fe1A 178.2(2) . . ? C1A B5A B4A 55.12(15) . . ? C1A B5A B8A 109.4(2) . . ? B4A B5A B8A 59.62(14) . . ? C1A B5A B2A 55.18(15) . . ? B4A B5A B2A 91.62(18) . . ? B8A B5A B2A 105.59(18) . . ? C1A B5A B9A 108.19(19) . . ? B4A B5A B9A 103.18(18) . . ? B8A B5A B9A 63.66(14) . . ? B2A B5A B9A 59.38(14) . . ? O12A C12A Fe1A 177.6(2) . . ? O61A C61A Fe6A 179.9(3) . . ? O63 C63 Fe6 177.5(2) . . ? F9 B9 B2 114.15(18) . . ? F9 B9 B5 113.88(18) . . ? B2 B9 B5 59.81(14) . . ? F9 B9 B8 130.71(19) . . ? B2 B9 B8 101.41(17) . . ? B5 B9 B8 56.96(13) . . ? F9 B9 Fe6 125.30(17) . . ? B2 B9 Fe6 65.20(11) . . ? B5 B9 Fe6 110.71(15) . . ? B8 B9 Fe6 99.75(13) . . ? F9 B9 Fe10 112.49(16) . . ? B2 B9 Fe10 128.72(15) . . ? B5 B9 Fe10 116.79(15) . . ? B8 B9 Fe10 60.51(10) . . ? Fe6 B9 Fe10 71.20(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.488 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.084 #============================================================================== data_10 _database_code_depnum_ccdc_archive 'CCDC 634923' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H29 B7 F3 Fe2 N2 O4 P' _chemical_formula_weight 576.74 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 9.9020(13) _cell_length_b 11.1053(14) _cell_length_c 13.2738(16) _cell_angle_alpha 76.602(8) _cell_angle_beta 77.069(8) _cell_angle_gamma 63.929(7) _cell_volume 1263.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8005 _exptl_absorpt_correction_T_max 0.9148 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X-8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14315 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.47 _reflns_number_total 4726 _reflns_number_gt 3143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _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^)+(0.0608P)^2^+0.5091P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4726 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe10 Fe 0.60047(7) 0.30337(6) 0.20556(4) 0.0216(2) Uani 1 1 d . . . Fe6 Fe 0.84263(7) 0.09478(6) 0.17533(5) 0.02202(19) Uani 1 1 d . . . P1 P 0.34157(13) 0.37044(12) 0.25881(9) 0.0235(3) Uani 1 1 d . . . C1 C 0.8750(5) 0.0046(4) 0.4177(3) 0.0261(11) Uani 1 1 d . . . H1 H 0.9439 -0.0744 0.4772 0.031 Uiso 1 1 calc R . . B4 B 0.6960(6) 0.0710(5) 0.4281(4) 0.0246(12) Uani 1 1 d . . . H4 H 0.6232 0.0442 0.4993 0.029 Uiso 1 1 calc R . . B2 B 0.9485(7) 0.0683(5) 0.3114(4) 0.0277(13) Uani 1 1 d . . . H2 H 1.0736 0.0405 0.2929 0.033 Uiso 1 1 calc R . . B5 B 0.8127(6) 0.1631(5) 0.4112(4) 0.0245(12) Uani 1 1 d . . . H5 H 0.8322 0.2099 0.4697 0.029 Uiso 1 1 calc R . . B3 B 0.8224(6) -0.0307(5) 0.3273(4) 0.0249(12) Uani 1 1 d . . . H3 H 0.8473 -0.1374 0.3204 0.030 Uiso 1 1 calc R . . B7 B 0.6417(6) 0.1061(5) 0.2952(4) 0.0225(12) Uani 1 1 d . . . B8 B 0.6332(6) 0.2465(5) 0.3600(4) 0.0249(12) Uani 1 1 d . . . B9 B 0.8143(6) 0.2407(5) 0.2711(4) 0.0263(13) Uani 1 1 d . . . F8 F 0.5303(3) 0.3398(2) 0.42385(17) 0.0260(6) Uani 1 1 d . . . F7 F 0.5391(3) 0.0546(2) 0.29058(18) 0.0258(6) Uani 1 1 d . . . F9 F 0.8793(3) 0.3332(2) 0.24408(19) 0.0301(6) Uani 1 1 d . . . C61 C 1.0162(6) -0.0481(5) 0.1547(3) 0.0292(11) Uani 1 1 d . . . C63 C 0.7500(5) 0.0481(4) 0.0980(3) 0.0257(11) Uani 1 1 d . . . C62 C 0.8987(5) 0.2097(5) 0.0753(4) 0.0291(11) Uani 1 1 d . . . O61 O 1.1288(4) -0.1407(3) 0.1410(2) 0.0381(9) Uani 1 1 d . . . O62 O 0.9379(4) 0.2827(4) 0.0123(3) 0.0408(9) Uani 1 1 d . . . O63 O 0.6941(4) 0.0158(3) 0.0491(2) 0.0351(8) Uani 1 1 d . . . C101 C 0.5885(5) 0.4745(5) 0.2152(3) 0.0253(11) Uani 1 1 d . . . C102 C 0.6173(6) 0.6923(5) 0.2287(3) 0.0296(12) Uani 1 1 d . . . C103 C 0.7694(6) 0.6791(6) 0.1635(4) 0.0515(16) Uani 1 1 d . . . H10A H 0.7624 0.6882 0.0894 0.077 Uiso 1 1 calc R . . H10B H 0.8481 0.5901 0.1855 0.077 Uiso 1 1 calc R . . H10C H 0.7955 0.7505 0.1736 0.077 Uiso 1 1 calc R . . C105 C 0.4900(6) 0.8188(5) 0.1885(5) 0.0553(17) Uani 1 1 d . . . H10D H 0.4920 0.8213 0.1139 0.083 Uiso 1 1 calc R . . H10E H 0.5018 0.8983 0.1983 0.083 Uiso 1 1 calc R . . H10F H 0.3929 0.8197 0.2270 0.083 Uiso 1 1 calc R . . C104 C 0.6235(9) 0.6813(7) 0.3430(4) 0.067(2) Uani 1 1 d . . . H10G H 0.7096 0.5979 0.3647 0.101 Uiso 1 1 calc R . . H10H H 0.5291 0.6791 0.3843 0.101 Uiso 1 1 calc R . . H10I H 0.6360 0.7598 0.3543 0.101 Uiso 1 1 calc R . . N101 N 0.5919(4) 0.5740(4) 0.2191(3) 0.0217(8) Uani 1 1 d . . . N102 N 0.5816(4) 0.3280(4) 0.0803(3) 0.0260(9) Uani 1 1 d . . . O102 O 0.5668(4) 0.3462(3) -0.0088(2) 0.0353(9) Uani 1 1 d . . . C113 C 0.2702(5) 0.2902(5) 0.3836(3) 0.0279(11) Uani 1 1 d . . . H11A H 0.3149 0.1911 0.3834 0.033 Uiso 1 1 calc R . . H11B H 0.3069 0.3059 0.4408 0.033 Uiso 1 1 calc R . . C111 C 0.2476(5) 0.3531(5) 0.1620(4) 0.0311(12) Uani 1 1 d . . . H11C H 0.1364 0.3957 0.1833 0.037 Uiso 1 1 calc R . . H11D H 0.2710 0.4046 0.0939 0.037 Uiso 1 1 calc R . . C115 C 0.2370(5) 0.5526(5) 0.2636(4) 0.0305(11) Uani 1 1 d . . . H11E H 0.2768 0.6019 0.2008 0.037 Uiso 1 1 calc R . . H11F H 0.1293 0.5777 0.2588 0.037 Uiso 1 1 calc R . . C114 C 0.0974(5) 0.3399(5) 0.4078(4) 0.0362(13) Uani 1 1 d . . . H11G H 0.0704 0.2912 0.4753 0.054 Uiso 1 1 calc R . . H11H H 0.0594 0.3229 0.3528 0.054 Uiso 1 1 calc R . . H11I H 0.0516 0.4374 0.4110 0.054 Uiso 1 1 calc R . . C116 C 0.2428(6) 0.6029(5) 0.3601(4) 0.0372(13) Uani 1 1 d . . . H11J H 0.1839 0.7013 0.3539 0.056 Uiso 1 1 calc R . . H11K H 0.3485 0.5813 0.3652 0.056 Uiso 1 1 calc R . . H11L H 0.1997 0.5582 0.4231 0.056 Uiso 1 1 calc R . . C112 C 0.2908(6) 0.2079(5) 0.1459(4) 0.0341(12) Uani 1 1 d . . . H11M H 0.2358 0.2096 0.0924 0.051 Uiso 1 1 calc R . . H11N H 0.2640 0.1564 0.2118 0.051 Uiso 1 1 calc R . . H11O H 0.4003 0.1646 0.1233 0.051 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 Fe10 0.0313(4) 0.0185(4) 0.0130(3) -0.0031(2) -0.0058(3) -0.0067(3) Fe6 0.0294(4) 0.0181(4) 0.0171(3) -0.0043(3) -0.0048(3) -0.0070(3) P1 0.0298(7) 0.0226(7) 0.0172(6) -0.0039(5) -0.0042(5) -0.0091(5) C1 0.040(3) 0.020(3) 0.022(2) 0.0014(19) -0.017(2) -0.012(2) B4 0.036(3) 0.025(3) 0.016(2) -0.003(2) -0.009(2) -0.013(3) B2 0.037(3) 0.025(3) 0.024(3) -0.004(2) -0.010(2) -0.013(3) B5 0.030(3) 0.024(3) 0.023(3) -0.007(2) -0.008(2) -0.010(2) B3 0.035(3) 0.022(3) 0.019(3) -0.003(2) -0.010(2) -0.010(2) B7 0.032(3) 0.019(3) 0.014(2) -0.002(2) -0.007(2) -0.006(2) B8 0.036(3) 0.018(3) 0.020(3) -0.004(2) -0.009(2) -0.007(2) B9 0.035(3) 0.022(3) 0.022(3) -0.004(2) -0.011(2) -0.008(3) F8 0.0342(15) 0.0258(15) 0.0162(12) -0.0073(11) -0.0053(11) -0.0077(12) F7 0.0336(14) 0.0253(15) 0.0214(13) -0.0050(11) -0.0069(11) -0.0125(12) F9 0.0418(16) 0.0244(15) 0.0311(15) -0.0028(12) -0.0102(13) -0.0180(13) C61 0.042(3) 0.029(3) 0.018(2) -0.003(2) -0.005(2) -0.016(3) C63 0.032(3) 0.019(3) 0.020(2) -0.0047(19) 0.000(2) -0.007(2) C62 0.039(3) 0.029(3) 0.022(2) -0.007(2) -0.009(2) -0.013(2) O61 0.037(2) 0.030(2) 0.0316(19) -0.0070(16) -0.0033(16) 0.0004(18) O62 0.054(2) 0.041(2) 0.0313(19) -0.0007(17) -0.0018(18) -0.028(2) O63 0.047(2) 0.039(2) 0.0274(18) -0.0121(16) -0.0068(16) -0.0207(18) C101 0.026(3) 0.032(3) 0.011(2) -0.003(2) -0.0052(19) -0.006(2) C102 0.046(3) 0.025(3) 0.024(2) -0.003(2) -0.008(2) -0.019(2) C103 0.055(4) 0.046(4) 0.057(4) -0.008(3) 0.008(3) -0.031(3) C105 0.054(4) 0.024(3) 0.091(5) -0.009(3) -0.021(3) -0.014(3) C104 0.135(6) 0.083(5) 0.022(3) -0.009(3) -0.008(3) -0.079(5) N101 0.034(2) 0.022(2) 0.0144(18) -0.0057(16) -0.0031(16) -0.0146(19) N102 0.035(2) 0.021(2) 0.0178(19) -0.0058(16) -0.0060(17) -0.0059(18) O102 0.048(2) 0.037(2) 0.0143(16) -0.0062(14) -0.0095(15) -0.0077(17) C113 0.037(3) 0.031(3) 0.017(2) -0.005(2) -0.005(2) -0.013(2) C111 0.030(3) 0.036(3) 0.026(3) -0.002(2) -0.008(2) -0.012(2) C115 0.028(3) 0.027(3) 0.032(3) -0.007(2) -0.004(2) -0.007(2) C114 0.038(3) 0.039(3) 0.031(3) -0.005(2) 0.001(2) -0.019(3) C116 0.041(3) 0.034(3) 0.030(3) -0.012(2) 0.004(2) -0.010(3) C112 0.039(3) 0.040(3) 0.030(3) -0.011(2) -0.011(2) -0.016(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 Fe10 N102 1.661(4) . ? Fe10 C101 1.884(5) . ? Fe10 B8 2.056(5) . ? Fe10 B7 2.146(5) . ? Fe10 B9 2.230(5) . ? Fe10 P1 2.3197(14) . ? Fe10 Fe6 2.5288(9) . ? Fe6 C61 1.772(5) . ? Fe6 C62 1.791(5) . ? Fe6 C63 1.803(5) . ? Fe6 B9 2.171(5) . ? Fe6 B2 2.186(5) . ? Fe6 B3 2.194(5) . ? Fe6 B7 2.228(5) . ? P1 C115 1.832(5) . ? P1 C111 1.834(5) . ? P1 C113 1.839(4) . ? C1 B5 1.576(7) . ? C1 B4 1.578(7) . ? C1 B3 1.595(6) . ? C1 B2 1.597(7) . ? C1 H1 1.1200 . ? B4 B5 1.801(8) . ? B4 B3 1.828(7) . ? B4 B8 1.836(7) . ? B4 B7 1.864(7) . ? B4 H4 1.1200 . ? B2 B5 1.810(7) . ? B2 B9 1.823(7) . ? B2 B3 1.948(8) . ? B2 H2 1.1200 . ? B5 B8 1.811(7) . ? B5 B9 1.859(7) . ? B5 H5 1.1200 . ? B3 B7 1.829(7) . ? B3 H3 1.1200 . ? B7 F7 1.385(6) . ? B7 B8 1.911(7) . ? B8 F8 1.387(5) . ? B8 B9 1.897(8) . ? B9 F9 1.381(6) . ? C61 O61 1.150(5) . ? C63 O63 1.139(5) . ? C62 O62 1.150(5) . ? C101 N101 1.133(6) . ? C102 N101 1.479(6) . ? C102 C105 1.498(7) . ? C102 C104 1.507(6) . ? C102 C103 1.523(7) . ? C103 H10A 0.9800 . ? C103 H10B 0.9800 . ? C103 H10C 0.9800 . ? C105 H10D 0.9800 . ? C105 H10E 0.9800 . ? C105 H10F 0.9800 . ? C104 H10G 0.9800 . ? C104 H10H 0.9800 . ? C104 H10I 0.9800 . ? N102 O102 1.183(4) . ? C113 C114 1.531(6) . ? C113 H11A 0.9900 . ? C113 H11B 0.9900 . ? C111 C112 1.530(6) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C115 C116 1.533(6) . ? C115 H11E 0.9900 . ? C115 H11F 0.9900 . ? C114 H11G 0.9800 . ? C114 H11H 0.9800 . ? C114 H11I 0.9800 . ? C116 H11J 0.9800 . ? C116 H11K 0.9800 . ? C116 H11L 0.9800 . ? C112 H11M 0.9800 . ? C112 H11N 0.9800 . ? C112 H11O 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N102 Fe10 C101 99.69(18) . . ? N102 Fe10 B8 172.55(19) . . ? C101 Fe10 B8 87.53(19) . . ? N102 Fe10 B7 118.64(18) . . ? C101 Fe10 B7 141.51(18) . . ? B8 Fe10 B7 54.05(19) . . ? N102 Fe10 B9 126.87(19) . . ? C101 Fe10 B9 79.83(19) . . ? B8 Fe10 B9 52.4(2) . . ? B7 Fe10 B9 74.6(2) . . ? N102 Fe10 P1 92.67(14) . . ? C101 Fe10 P1 91.69(14) . . ? B8 Fe10 P1 88.91(16) . . ? B7 Fe10 P1 90.07(15) . . ? B9 Fe10 P1 140.34(14) . . ? N102 Fe10 Fe6 89.24(12) . . ? C101 Fe10 Fe6 125.70(14) . . ? B8 Fe10 Fe6 85.02(14) . . ? B7 Fe10 Fe6 56.21(14) . . ? B9 Fe10 Fe6 53.85(13) . . ? P1 Fe10 Fe6 141.65(5) . . ? C61 Fe6 C62 94.8(2) . . ? C61 Fe6 C63 92.8(2) . . ? C62 Fe6 C63 98.0(2) . . ? C61 Fe6 B9 122.1(2) . . ? C62 Fe6 B9 81.4(2) . . ? C63 Fe6 B9 145.1(2) . . ? C61 Fe6 B2 78.0(2) . . ? C62 Fe6 B2 106.9(2) . . ? C63 Fe6 B2 154.0(2) . . ? B9 Fe6 B2 49.47(19) . . ? C61 Fe6 B3 82.1(2) . . ? C62 Fe6 B3 159.7(2) . . ? C63 Fe6 B3 102.2(2) . . ? B9 Fe6 B3 83.3(2) . . ? B2 Fe6 B3 52.8(2) . . ? C61 Fe6 B7 128.0(2) . . ? C62 Fe6 B7 137.1(2) . . ? C63 Fe6 B7 83.75(19) . . ? B9 Fe6 B7 74.1(2) . . ? B2 Fe6 B7 83.2(2) . . ? B3 Fe6 B7 48.85(18) . . ? C61 Fe6 Fe10 177.85(16) . . ? C62 Fe6 Fe10 83.91(15) . . ? C63 Fe6 Fe10 89.15(14) . . ? B9 Fe6 Fe10 56.02(14) . . ? B2 Fe6 Fe10 100.69(14) . . ? B3 Fe6 Fe10 98.51(14) . . ? B7 Fe6 Fe10 53.17(13) . . ? C115 P1 C111 99.7(2) . . ? C115 P1 C113 104.1(2) . . ? C111 P1 C113 104.2(2) . . ? C115 P1 Fe10 114.01(17) . . ? C111 P1 Fe10 111.85(15) . . ? C113 P1 Fe10 120.55(15) . . ? B5 C1 B4 69.6(3) . . ? B5 C1 B3 110.2(4) . . ? B4 C1 B3 70.4(3) . . ? B5 C1 B2 69.6(3) . . ? B4 C1 B2 111.3(4) . . ? B3 C1 B2 75.2(3) . . ? B5 C1 H1 126.5 . . ? B4 C1 H1 125.6 . . ? B3 C1 H1 123.2 . . ? B2 C1 H1 123.1 . . ? C1 B4 B5 55.1(3) . . ? C1 B4 B3 55.2(3) . . ? B5 B4 B3 91.5(4) . . ? C1 B4 B8 109.0(4) . . ? B5 B4 B8 59.7(3) . . ? B3 B4 B8 104.2(3) . . ? C1 B4 B7 108.1(4) . . ? B5 B4 B7 102.7(4) . . ? B3 B4 B7 59.4(3) . . ? B8 B4 B7 62.2(3) . . ? C1 B4 H4 122.2 . . ? B5 B4 H4 130.3 . . ? B3 B4 H4 129.7 . . ? B8 B4 H4 119.7 . . ? B7 B4 H4 120.8 . . ? C1 B2 B5 54.7(3) . . ? C1 B2 B9 109.2(4) . . ? B5 B2 B9 61.6(3) . . ? C1 B2 B3 52.3(3) . . ? B5 B2 B3 87.5(3) . . ? B9 B2 B3 100.6(4) . . ? C1 B2 Fe6 113.8(3) . . ? B5 B2 Fe6 111.5(3) . . ? B9 B2 Fe6 64.9(2) . . ? B3 B2 Fe6 63.8(2) . . ? C1 B2 H2 121.9 . . ? B5 B2 H2 128.9 . . ? B9 B2 H2 120.3 . . ? B3 B2 H2 134.0 . . ? Fe6 B2 H2 113.5 . . ? C1 B5 B4 55.2(3) . . ? C1 B5 B2 55.8(3) . . ? B4 B5 B2 93.1(3) . . ? C1 B5 B8 110.3(4) . . ? B4 B5 B8 61.1(3) . . ? B2 B5 B8 105.8(3) . . ? C1 B5 B9 108.4(4) . . ? B4 B5 B9 103.7(3) . . ? B2 B5 B9 59.6(3) . . ? B8 B5 B9 62.2(3) . . ? C1 B5 H5 121.9 . . ? B4 B5 H5 129.4 . . ? B2 B5 H5 128.9 . . ? B8 B5 H5 118.6 . . ? B9 B5 H5 120.7 . . ? C1 B3 B4 54.4(3) . . ? C1 B3 B7 109.1(4) . . ? B4 B3 B7 61.3(3) . . ? C1 B3 B2 52.4(3) . . ? B4 B3 B2 87.8(3) . . ? B7 B3 B2 101.7(4) . . ? C1 B3 Fe6 113.4(3) . . ? B4 B3 Fe6 112.2(3) . . ? B7 B3 Fe6 66.6(2) . . ? B2 B3 Fe6 63.4(2) . . ? C1 B3 H3 122.4 . . ? B4 B3 H3 129.0 . . ? B7 B3 H3 119.5 . . ? B2 B3 H3 133.7 . . ? Fe6 B3 H3 113.0 . . ? F7 B7 B3 110.9(4) . . ? F7 B7 B4 113.5(4) . . ? B3 B7 B4 59.4(3) . . ? F7 B7 B8 134.8(4) . . ? B3 B7 B8 101.3(3) . . ? B4 B7 B8 58.2(3) . . ? F7 B7 Fe10 114.6(3) . . ? B3 B7 Fe10 128.6(3) . . ? B4 B7 Fe10 118.1(3) . . ? B8 B7 Fe10 60.6(2) . . ? F7 B7 Fe6 124.5(3) . . ? B3 B7 Fe6 64.6(2) . . ? B4 B7 Fe6 109.3(3) . . ? B8 B7 Fe6 97.4(3) . . ? Fe10 B7 Fe6 70.61(16) . . ? F8 B8 B5 108.8(4) . . ? F8 B8 B4 112.8(4) . . ? B5 B8 B4 59.2(3) . . ? F8 B8 B9 131.3(4) . . ? B5 B8 B9 60.1(3) . . ? B4 B8 B9 100.9(3) . . ? F8 B8 B7 138.8(4) . . ? B5 B8 B7 100.6(3) . . ? B4 B8 B7 59.6(3) . . ? B9 B8 B7 88.3(3) . . ? F8 B8 Fe10 113.7(3) . . ? B5 B8 Fe10 127.3(3) . . ? B4 B8 Fe10 124.3(3) . . ? B9 B8 Fe10 68.6(2) . . ? B7 B8 Fe10 65.4(2) . . ? F9 B9 B2 113.1(4) . . ? F9 B9 B5 113.6(4) . . ? B2 B9 B5 58.9(3) . . ? F9 B9 B8 130.8(4) . . ? B2 B9 B8 101.8(4) . . ? B5 B9 B8 57.6(3) . . ? F9 B9 Fe6 125.3(3) . . ? B2 B9 Fe6 65.7(2) . . ? B5 B9 Fe6 110.2(3) . . ? B8 B9 Fe6 99.8(3) . . ? F9 B9 Fe10 115.3(3) . . ? B2 B9 Fe10 127.3(3) . . ? B5 B9 Fe10 115.6(3) . . ? B8 B9 Fe10 59.1(2) . . ? Fe6 B9 Fe10 70.13(16) . . ? O61 C61 Fe6 179.8(4) . . ? O63 C63 Fe6 178.5(4) . . ? O62 C62 Fe6 178.2(4) . . ? N101 C101 Fe10 175.2(4) . . ? N101 C102 C105 108.5(4) . . ? N101 C102 C104 106.1(4) . . ? C105 C102 C104 112.9(5) . . ? N101 C102 C103 106.9(4) . . ? C105 C102 C103 111.3(4) . . ? C104 C102 C103 110.8(5) . . ? C102 C103 H10A 109.5 . . ? C102 C103 H10B 109.5 . . ? H10A C103 H10B 109.5 . . ? C102 C103 H10C 109.5 . . ? H10A C103 H10C 109.5 . . ? H10B C103 H10C 109.5 . . ? C102 C105 H10D 109.5 . . ? C102 C105 H10E 109.5 . . ? H10D C105 H10E 109.5 . . ? C102 C105 H10F 109.5 . . ? H10D C105 H10F 109.5 . . ? H10E C105 H10F 109.5 . . ? C102 C104 H10G 109.5 . . ? C102 C104 H10H 109.5 . . ? H10G C104 H10H 109.5 . . ? C102 C104 H10I 109.5 . . ? H10G C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? C101 N101 C102 172.1(4) . . ? O102 N102 Fe10 179.4(4) . . ? C114 C113 P1 115.4(3) . . ? C114 C113 H11A 108.4 . . ? P1 C113 H11A 108.4 . . ? C114 C113 H11B 108.4 . . ? P1 C113 H11B 108.4 . . ? H11A C113 H11B 107.5 . . ? C112 C111 P1 115.8(3) . . ? C112 C111 H11C 108.3 . . ? P1 C111 H11C 108.3 . . ? C112 C111 H11D 108.3 . . ? P1 C111 H11D 108.3 . . ? H11C C111 H11D 107.4 . . ? C116 C115 P1 116.7(3) . . ? C116 C115 H11E 108.1 . . ? P1 C115 H11E 108.1 . . ? C116 C115 H11F 108.1 . . ? P1 C115 H11F 108.1 . . ? H11E C115 H11F 107.3 . . ? C113 C114 H11G 109.5 . . ? C113 C114 H11H 109.5 . . ? H11G C114 H11H 109.5 . . ? C113 C114 H11I 109.5 . . ? H11G C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? C115 C116 H11J 109.5 . . ? C115 C116 H11K 109.5 . . ? H11J C116 H11K 109.5 . . ? C115 C116 H11L 109.5 . . ? H11J C116 H11L 109.5 . . ? H11K C116 H11L 109.5 . . ? C111 C112 H11M 109.5 . . ? C111 C112 H11N 109.5 . . ? H11M C112 H11N 109.5 . . ? C111 C112 H11O 109.5 . . ? H11M C112 H11O 109.5 . . ? H11N C112 H11O 109.5 . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 1.269 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.102 #===END