# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ps235 _database_code_depnum_ccdc_archive 'CCDC 906406' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1'-(diphenylphosphino)ferrocenyl]methanol-borane (1/1) ; _chemical_formula_moiety 'C23 H24 B Fe O P' _chemical_formula_sum 'C23 H24 B Fe O P' _chemical_formula_weight 414.05 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4231(2) _cell_length_b 17.6047(2) _cell_length_c 34.0211(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.6903(6) _cell_angle_gamma 90.00 _cell_volume 7924.81(18) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17811 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.10 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 118977 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.12 _reflns_number_total 17472 _reflns_number_gt 11375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'PLATON (Spek, 2007)' _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^)+(0.0712P)^2^+3.5238P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom + difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17472 _refine_ls_number_parameters 967 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.00768(3) -0.03629(2) 0.202235(11) 0.02066(10) Uani 1 1 d . . . P1 P 0.91712(5) 0.14528(4) 0.19404(2) 0.01885(15) Uani 1 1 d . . . O1 O 1.23122(15) -0.02870(12) 0.31180(6) 0.0371(5) Uani 1 1 d . . . H91 H 1.2390 0.0090 0.3348 0.045 Uiso 1 1 d R . . B1 B 1.0018(2) 0.1817(2) 0.15817(10) 0.0288(7) Uani 1 1 d . . . H1B H 0.9966 0.2456 0.1564 0.035 Uiso 1 1 d R . . H2B H 0.9633 0.1596 0.1279 0.035 Uiso 1 1 d R . . H3B H 1.0841 0.1596 0.1673 0.035 Uiso 1 1 d R . . C101 C 0.89950(19) 0.04442(15) 0.19326(8) 0.0196(6) Uani 1 1 d . . . C102 C 0.8952(2) -0.00161(16) 0.15846(8) 0.0267(6) Uani 1 1 d . . . H102 H 0.9028 0.0155 0.1333 0.032 Uiso 1 1 calc R . . C103 C 0.8776(2) -0.07759(17) 0.16888(9) 0.0333(7) Uani 1 1 d . . . H103 H 0.8722 -0.1192 0.1518 0.040 Uiso 1 1 calc R . . C104 C 0.8697(2) -0.07939(16) 0.21010(10) 0.0310(7) Uani 1 1 d . . . H104 H 0.8576 -0.1223 0.2245 0.037 Uiso 1 1 calc R . . C105 C 0.88335(19) -0.00439(15) 0.22541(9) 0.0240(6) Uani 1 1 d . . . H105 H 0.8821 0.0105 0.2516 0.029 Uiso 1 1 calc R . . C106 C 1.1301(2) -0.03926(15) 0.24745(8) 0.0235(6) Uani 1 1 d . . . C107 C 1.14592(19) 0.01485(16) 0.21786(8) 0.0235(6) Uani 1 1 d . . . H107 H 1.1580 0.0665 0.2221 0.028 Uiso 1 1 calc R . . C108 C 1.1400(2) -0.02325(17) 0.18095(9) 0.0296(7) Uani 1 1 d . . . H108 H 1.1469 -0.0010 0.1568 0.036 Uiso 1 1 calc R . . C109 C 1.1219(2) -0.10081(17) 0.18720(9) 0.0300(7) Uani 1 1 d . . . H109 H 1.1154 -0.1386 0.1679 0.036 Uiso 1 1 calc R . . C110 C 1.1151(2) -0.11138(16) 0.22816(9) 0.0265(6) Uani 1 1 d . . . H110 H 1.1031 -0.1571 0.2402 0.032 Uiso 1 1 calc R . . C111 C 1.1299(2) -0.02208(17) 0.29038(8) 0.0278(6) Uani 1 1 d . . . H11A H 1.1048 0.0290 0.2931 0.033 Uiso 1 1 calc R . . H11C H 1.0859 -0.0574 0.3011 0.033 Uiso 1 1 calc R . . C112 C 0.95968(19) 0.17245(14) 0.24554(8) 0.0195(6) Uani 1 1 d . . . C113 C 1.0595(2) 0.19596(15) 0.25775(9) 0.0273(6) Uani 1 1 d . . . H113 H 1.1034 0.1987 0.2393 0.033 Uiso 1 1 calc R . . C114 C 1.0934(2) 0.21533(16) 0.29731(9) 0.0351(8) Uani 1 1 d . . . H114 H 1.1601 0.2304 0.3054 0.042 Uiso 1 1 calc R . . C115 C 1.0285(3) 0.21225(17) 0.32461(9) 0.0357(8) Uani 1 1 d . . . H115 H 1.0517 0.2246 0.3511 0.043 Uiso 1 1 calc R . . C116 C 0.9291(2) 0.19087(17) 0.31275(8) 0.0334(7) Uani 1 1 d . . . H116 H 0.8850 0.1898 0.3311 0.040 Uiso 1 1 calc R . . C117 C 0.8951(2) 0.17094(16) 0.27324(8) 0.0269(6) Uani 1 1 d . . . H117 H 0.8281 0.1564 0.2653 0.032 Uiso 1 1 calc R . . C118 C 0.78973(19) 0.18409(15) 0.18172(7) 0.0197(6) Uani 1 1 d . . . C119 C 0.7769(2) 0.26280(15) 0.18132(8) 0.0257(6) Uani 1 1 d . . . H119 H 0.8327 0.2943 0.1882 0.031 Uiso 1 1 calc R . . C120 C 0.6813(2) 0.29455(17) 0.17079(8) 0.0305(7) Uani 1 1 d . . . H120 H 0.6731 0.3470 0.1709 0.037 Uiso 1 1 calc R . . C121 C 0.5986(2) 0.24783(17) 0.16019(8) 0.0304(7) Uani 1 1 d . . . H121 H 0.5347 0.2689 0.1529 0.036 Uiso 1 1 calc R . . C122 C 0.6106(2) 0.16933(17) 0.16040(8) 0.0278(6) Uani 1 1 d . . . H122 H 0.5547 0.1380 0.1531 0.033 Uiso 1 1 calc R . . C123 C 0.7056(2) 0.13775(16) 0.17142(8) 0.0246(6) Uani 1 1 d . . . H123 H 0.7132 0.0852 0.1719 0.030 Uiso 1 1 calc R . . Fe2 Fe 0.23724(3) 1.11252(2) 0.048483(12) 0.02612(11) Uani 1 1 d . A . P2 P 0.32906(5) 0.93129(4) 0.05924(2) 0.02076(16) Uani 1 1 d . . . O2A O 0.0607(3) 1.1183(2) -0.07171(11) 0.0459(10) Uiso 0.60 1 d P A 1 H92A H 0.0189 1.0866 -0.0676 0.055 Uiso 0.60 1 d PR A 1 O2B O 0.1567(5) 1.1424(4) -0.0590(2) 0.0589(18) Uiso 0.40 1 d P B 2 H92B H 0.1481 1.1323 -0.0829 0.088 Uiso 0.40 1 calc PR B 2 B2 B 0.2396(2) 0.8954(2) 0.09384(10) 0.0289(8) Uani 1 1 d . . . H4B H 0.2502 0.8366 0.0942 0.035 Uiso 1 1 d R . . H5B H 0.2842 0.9236 0.1250 0.035 Uiso 1 1 d R . . H6B H 0.1553 0.9150 0.0827 0.035 Uiso 1 1 d R . . C201 C 0.3463(2) 1.03212(16) 0.05982(9) 0.0260(6) Uani 1 1 d . . . C202 C 0.3654(2) 1.08056(17) 0.02793(10) 0.0333(7) Uani 1 1 d . . . H202 H 0.3701 1.0654 0.0021 0.040 Uiso 1 1 calc R . . C203 C 0.3758(2) 1.15572(18) 0.04297(12) 0.0454(9) Uani 1 1 d . . . H203 H 0.3882 1.1986 0.0286 0.054 Uiso 1 1 calc R . . C204 C 0.3641(2) 1.15463(18) 0.08368(12) 0.0455(9) Uani 1 1 d . . . H204 H 0.3677 1.1966 0.1005 0.055 Uiso 1 1 calc R . . C205 C 0.3462(2) 1.07888(18) 0.09429(10) 0.0350(7) Uani 1 1 d . . . H205 H 0.3361 1.0623 0.1193 0.042 Uiso 1 1 calc R . . C206 C 0.1208(3) 1.11412(18) 0.00127(10) 0.0411(8) Uani 1 1 d . . . C207 C 0.1329(3) 1.18739(18) 0.02029(10) 0.0408(8) Uani 1 1 d . A . H207 H 0.1464 1.2328 0.0083 0.049 Uiso 1 1 calc R . . C208 C 0.1205(2) 1.17799(19) 0.06051(10) 0.0393(8) Uani 1 1 d . . . H208 H 0.1246 1.2163 0.0795 0.047 Uiso 1 1 calc R A . C209 C 0.1010(2) 1.1005(2) 0.06693(10) 0.0407(8) Uani 1 1 d . A . H209 H 0.0902 1.0790 0.0908 0.049 Uiso 1 1 calc R . . C210 C 0.1008(2) 1.06112(18) 0.03049(10) 0.0356(8) Uani 1 1 d . A . H210 H 0.0896 1.0094 0.0264 0.043 Uiso 1 1 calc R . . C21A C 0.1470(4) 1.0970(4) -0.04130(17) 0.0393(12) Uiso 0.60 1 d P A 1 H21A H 0.2062 1.1257 -0.0452 0.047 Uiso 0.60 1 calc PR A 1 H21B H 0.1616 1.0434 -0.0436 0.047 Uiso 0.60 1 calc PR A 1 C21B C 0.1009(7) 1.0927(5) -0.0398(3) 0.0393(12) Uiso 0.40 1 d P B 2 H21C H 0.1216 1.0406 -0.0431 0.047 Uiso 0.40 1 calc PR B 2 H21D H 0.0294 1.0973 -0.0504 0.047 Uiso 0.40 1 calc PR B 2 C212 C 0.2913(2) 0.90412(15) 0.00751(8) 0.0221(6) Uani 1 1 d . . . C213 C 0.1932(2) 0.87887(15) -0.00596(8) 0.0249(6) Uani 1 1 d . . . H213 H 0.1470 0.8758 0.0115 0.030 Uiso 1 1 calc R . . C214 C 0.1644(2) 0.85815(16) -0.04590(8) 0.0283(7) Uani 1 1 d . . . H214 H 0.0990 0.8413 -0.0550 0.034 Uiso 1 1 calc R . . C215 C 0.2325(2) 0.86263(16) -0.07173(8) 0.0305(7) Uani 1 1 d . . . H215 H 0.2125 0.8496 -0.0984 0.037 Uiso 1 1 calc R . . C216 C 0.3306(2) 0.88635(16) -0.05837(8) 0.0294(7) Uani 1 1 d . . . H216 H 0.3768 0.8882 -0.0759 0.035 Uiso 1 1 calc R . . C217 C 0.3600(2) 0.90721(16) -0.01901(8) 0.0266(6) Uani 1 1 d . . . H217 H 0.4259 0.9234 -0.0101 0.032 Uiso 1 1 calc R . . C218 C 0.4557(2) 0.89157(15) 0.07239(8) 0.0225(6) Uani 1 1 d . . . C219 C 0.5401(2) 0.93703(16) 0.08328(8) 0.0257(6) Uani 1 1 d . . . H219 H 0.5329 0.9895 0.0839 0.031 Uiso 1 1 calc R . . C220 C 0.6355(2) 0.90473(18) 0.09335(9) 0.0315(7) Uani 1 1 d . . . H220 H 0.6917 0.9356 0.1010 0.038 Uiso 1 1 calc R . . C221 C 0.6468(2) 0.82677(18) 0.09202(9) 0.0341(7) Uani 1 1 d . . . H221 H 0.7106 0.8051 0.0986 0.041 Uiso 1 1 calc R . . C222 C 0.5626(2) 0.78085(18) 0.08090(9) 0.0350(7) Uani 1 1 d . . . H222 H 0.5703 0.7284 0.0797 0.042 Uiso 1 1 calc R . . C223 C 0.4672(2) 0.81276(16) 0.07151(8) 0.0281(6) Uani 1 1 d . . . H223 H 0.4109 0.7817 0.0646 0.034 Uiso 1 1 calc R . . Fe3 Fe 0.49341(3) 0.18823(2) 0.297418(11) 0.01992(10) Uani 1 1 d . C . P3 P 0.58546(5) 0.00755(4) 0.31280(2) 0.01784(15) Uani 1 1 d . . . O3A O 0.4025(3) 0.2087(2) 0.19086(13) 0.0370(10) Uiso 0.50 1 d P C 1 H93A H 0.3908 0.1965 0.1673 0.055 Uiso 0.50 1 calc PR C 1 O3B O 0.2994(4) 0.1813(3) 0.18068(14) 0.0510(13) Uiso 0.50 1 d P D 2 H93B H 0.2921 0.2275 0.1811 0.077 Uiso 0.50 1 calc PR D 2 B3 B 0.5111(2) -0.02260(19) 0.35358(9) 0.0263(7) Uani 1 1 d . . . H7B H 0.5105 -0.0822 0.3543 0.032 Uiso 1 1 d R . . H8B H 0.5596 -0.0005 0.3814 0.032 Uiso 1 1 d R . . H9B H 0.4394 0.0032 0.3487 0.032 Uiso 1 1 d R . . C301 C 0.60326(19) 0.10766(15) 0.30937(8) 0.0205(6) Uani 1 1 d . . . C302 C 0.6161(2) 0.15117(16) 0.27490(9) 0.0267(6) Uani 1 1 d . . . H302 H 0.6155 0.1320 0.2494 0.032 Uiso 1 1 calc R . . C304 C 0.6255(2) 0.23402(17) 0.32781(9) 0.0326(7) Uani 1 1 d . . . H304 H 0.6327 0.2783 0.3429 0.039 Uiso 1 1 calc R . . C303 C 0.6300(2) 0.22876(16) 0.28655(10) 0.0311(7) Uani 1 1 d . . . H303 H 0.6402 0.2690 0.2700 0.037 Uiso 1 1 calc R . . C305 C 0.6082(2) 0.15961(16) 0.34217(9) 0.0271(6) Uani 1 1 d . . . H305 H 0.6014 0.1471 0.3681 0.033 Uiso 1 1 calc R . . C306 C 0.3680(2) 0.18477(17) 0.25328(9) 0.0345(7) Uani 1 1 d . . . C307 C 0.3848(2) 0.26002(16) 0.26904(9) 0.0311(7) Uani 1 1 d . C . H307 H 0.3960 0.3031 0.2546 0.037 Uiso 1 1 calc R . . C308 C 0.3814(2) 0.25742(17) 0.31037(9) 0.0306(7) Uani 1 1 d . . . H308 H 0.3896 0.2986 0.3277 0.037 Uiso 1 1 calc R C . C309 C 0.3632(2) 0.18109(17) 0.32080(10) 0.0321(7) Uani 1 1 d . C . H309 H 0.3579 0.1634 0.3461 0.039 Uiso 1 1 calc R . . C310 C 0.3544(2) 0.13684(16) 0.28571(9) 0.0290(7) Uani 1 1 d . C . H310 H 0.3419 0.0849 0.2841 0.035 Uiso 1 1 calc R . . C31A C 0.3456(5) 0.1615(4) 0.21298(19) 0.0311(10) Uiso 0.50 1 d P C 1 H31A H 0.2739 0.1670 0.2030 0.037 Uiso 0.50 1 calc PR C 1 H31B H 0.3640 0.1087 0.2105 0.037 Uiso 0.50 1 calc PR C 1 C31B C 0.3849(5) 0.1599(4) 0.20955(19) 0.0311(10) Uiso 0.50 1 d P D 2 H31C H 0.4452 0.1842 0.2033 0.037 Uiso 0.50 1 calc PR D 2 H31D H 0.3945 0.1054 0.2088 0.037 Uiso 0.50 1 calc PR D 2 C312 C 0.53703(19) -0.02319(14) 0.26254(8) 0.0194(5) Uani 1 1 d . . . C313 C 0.4371(2) -0.04724(15) 0.25201(8) 0.0235(6) Uani 1 1 d . . . H313 H 0.3952 -0.0492 0.2711 0.028 Uiso 1 1 calc R . . C314 C 0.4006(2) -0.06820(15) 0.21294(9) 0.0299(7) Uani 1 1 d . . . H314 H 0.3339 -0.0840 0.2058 0.036 Uiso 1 1 calc R . . C315 C 0.4636(2) -0.06563(16) 0.18446(8) 0.0319(7) Uani 1 1 d . . . H315 H 0.4384 -0.0793 0.1583 0.038 Uiso 1 1 calc R . . C316 C 0.5632(2) -0.04291(16) 0.19468(8) 0.0309(7) Uani 1 1 d . . . H316 H 0.6052 -0.0416 0.1755 0.037 Uiso 1 1 calc R . . C317 C 0.6000(2) -0.02207(15) 0.23380(8) 0.0233(6) Uani 1 1 d . . . H317 H 0.6671 -0.0073 0.2409 0.028 Uiso 1 1 calc R . . C318 C 0.7112(2) -0.03389(15) 0.32235(7) 0.0203(6) Uani 1 1 d . . . C319 C 0.7983(2) 0.01018(16) 0.32816(8) 0.0226(6) Uani 1 1 d . . . H319 H 0.7932 0.0629 0.3272 0.027 Uiso 1 1 calc R . . C320 C 0.8927(2) -0.02371(17) 0.33543(8) 0.0292(7) Uani 1 1 d . . . H320 H 0.9507 0.0061 0.3396 0.035 Uiso 1 1 calc R . . C321 C 0.9002(2) -0.10229(17) 0.33650(8) 0.0294(7) Uani 1 1 d . . . H321 H 0.9636 -0.1251 0.3412 0.035 Uiso 1 1 calc R . . C322 C 0.8145(2) -0.14684(17) 0.33068(9) 0.0308(7) Uani 1 1 d . . . H322 H 0.8202 -0.1995 0.3315 0.037 Uiso 1 1 calc R . . C323 C 0.7198(2) -0.11300(15) 0.32358(8) 0.0259(6) Uani 1 1 d . . . H323 H 0.6619 -0.1430 0.3197 0.031 Uiso 1 1 calc R . . Fe4 Fe 0.74979(3) 0.38575(2) 0.048284(11) 0.02008(10) Uani 1 1 d . . . P4 P 0.84006(5) 0.56741(4) 0.06124(2) 0.02004(16) Uani 1 1 d . . . O4 O 0.51737(14) 0.39948(12) -0.05865(6) 0.0325(5) Uani 1 1 d . . . H94 H 0.5044 0.4284 -0.0853 0.039 Uiso 1 1 d R . . B4 B 0.7697(3) 0.59907(19) 0.10337(9) 0.0270(7) Uani 1 1 d . . . H10B H 0.8234 0.5822 0.1302 0.032 Uiso 1 1 d R . . H11B H 0.6923 0.5720 0.0982 0.032 Uiso 1 1 d R . . H12B H 0.7680 0.6631 0.1021 0.032 Uiso 1 1 d R . . C401 C 0.8581(2) 0.46713(15) 0.05872(8) 0.0220(6) Uani 1 1 d . . . C402 C 0.87106(19) 0.42227(15) 0.02448(8) 0.0230(6) Uani 1 1 d . . . H402 H 0.8698 0.4403 -0.0013 0.028 Uiso 1 1 calc R . . C403 C 0.8861(2) 0.34589(17) 0.03706(9) 0.0285(7) Uani 1 1 d . . . H403 H 0.8964 0.3051 0.0209 0.034 Uiso 1 1 calc R . . C404 C 0.8828(2) 0.34197(17) 0.07872(9) 0.0294(7) Uani 1 1 d . . . H404 H 0.8908 0.2983 0.0943 0.035 Uiso 1 1 calc R . . C405 C 0.8651(2) 0.41622(16) 0.09212(8) 0.0260(6) Uani 1 1 d . . . H405 H 0.8591 0.4297 0.1180 0.031 Uiso 1 1 calc R . . C406 C 0.62333(19) 0.38766(15) 0.00460(8) 0.0218(6) Uani 1 1 d . . . C407 C 0.6409(2) 0.31294(15) 0.02099(8) 0.0234(6) Uani 1 1 d . . . H407 H 0.6517 0.2694 0.0068 0.028 Uiso 1 1 calc R . . C408 C 0.6391(2) 0.31677(16) 0.06274(8) 0.0266(6) Uani 1 1 d . . . H408 H 0.6485 0.2763 0.0805 0.032 Uiso 1 1 calc R . . C409 C 0.6203(2) 0.39323(16) 0.07233(8) 0.0265(6) Uani 1 1 d . . . H409 H 0.6156 0.4117 0.0976 0.032 Uiso 1 1 calc R . . C410 C 0.6102(2) 0.43683(16) 0.03676(8) 0.0243(6) Uani 1 1 d . . . H410 H 0.5971 0.4887 0.0347 0.029 Uiso 1 1 calc R . . C411 C 0.6189(2) 0.41021(17) -0.03803(8) 0.0277(6) Uani 1 1 d . . . H41A H 0.6384 0.4630 -0.0396 0.033 Uiso 1 1 calc R . . H41B H 0.6652 0.3793 -0.0502 0.033 Uiso 1 1 calc R . . C412 C 0.7841(2) 0.59764(15) 0.01134(8) 0.0217(6) Uani 1 1 d . . . C413 C 0.6839(2) 0.62062(15) 0.00357(9) 0.0257(6) Uani 1 1 d . . . H413 H 0.6462 0.6231 0.0241 0.031 Uiso 1 1 calc R . . C414 C 0.6400(2) 0.64000(16) -0.03507(9) 0.0329(7) Uani 1 1 d . . . H414 H 0.5728 0.6553 -0.0403 0.039 Uiso 1 1 calc R . . C415 C 0.6953(2) 0.63667(16) -0.06560(9) 0.0354(8) Uani 1 1 d . . . H415 H 0.6651 0.6488 -0.0915 0.042 Uiso 1 1 calc R . . C416 C 0.7966(2) 0.61511(17) -0.05785(9) 0.0340(7) Uani 1 1 d . . . H416 H 0.8342 0.6135 -0.0784 0.041 Uiso 1 1 calc R . . C417 C 0.8408(2) 0.59611(16) -0.01959(8) 0.0265(6) Uani 1 1 d . . . H417 H 0.9085 0.5822 -0.0143 0.032 Uiso 1 1 calc R . . C418 C 0.9662(2) 0.60785(15) 0.06843(8) 0.0215(6) Uani 1 1 d . . . C419 C 0.9757(2) 0.68690(16) 0.06821(8) 0.0266(6) Uani 1 1 d . . . H419 H 0.9183 0.7173 0.0635 0.032 Uiso 1 1 calc R . . C420 C 1.0709(2) 0.72005(17) 0.07511(9) 0.0314(7) Uani 1 1 d . . . H420 H 1.0772 0.7726 0.0748 0.038 Uiso 1 1 calc R . . C421 C 1.1570(2) 0.67454(17) 0.08246(8) 0.0295(7) Uani 1 1 d . . . H421 H 1.2208 0.6968 0.0870 0.035 Uiso 1 1 calc R . . C422 C 1.1477(2) 0.59660(17) 0.08307(8) 0.0274(6) Uani 1 1 d . . . H422 H 1.2052 0.5663 0.0882 0.033 Uiso 1 1 calc R . . C423 C 1.0526(2) 0.56315(16) 0.07606(8) 0.0231(6) Uani 1 1 d . . . H423 H 1.0468 0.5105 0.0765 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0198(2) 0.0195(2) 0.0218(2) -0.00104(16) 0.00111(16) 0.00238(16) P1 0.0175(3) 0.0197(3) 0.0189(3) 0.0007(3) 0.0017(3) 0.0004(3) O1 0.0331(12) 0.0435(13) 0.0308(12) -0.0079(10) -0.0060(10) 0.0061(10) B1 0.0256(17) 0.0335(19) 0.0289(18) 0.0072(15) 0.0090(14) -0.0003(14) C101 0.0161(13) 0.0197(13) 0.0220(14) -0.0010(11) 0.0004(11) 0.0027(10) C102 0.0257(15) 0.0282(15) 0.0232(15) -0.0068(12) -0.0047(12) 0.0045(12) C103 0.0261(16) 0.0262(16) 0.0427(19) -0.0097(14) -0.0083(14) 0.0011(13) C104 0.0213(15) 0.0216(15) 0.050(2) 0.0010(14) 0.0056(14) -0.0020(12) C105 0.0172(13) 0.0251(14) 0.0301(15) 0.0018(12) 0.0050(12) -0.0002(11) C106 0.0186(14) 0.0259(15) 0.0251(14) -0.0007(12) 0.0014(11) 0.0035(11) C107 0.0159(13) 0.0257(14) 0.0289(15) 0.0027(12) 0.0039(11) 0.0005(11) C108 0.0256(15) 0.0372(17) 0.0278(15) 0.0049(13) 0.0093(13) 0.0071(13) C109 0.0274(16) 0.0289(16) 0.0334(17) -0.0047(13) 0.0036(13) 0.0082(13) C110 0.0246(15) 0.0225(15) 0.0312(16) 0.0003(12) 0.0015(12) 0.0048(12) C111 0.0264(15) 0.0316(16) 0.0243(15) -0.0024(12) 0.0015(12) 0.0053(12) C112 0.0207(13) 0.0161(13) 0.0201(13) -0.0001(10) -0.0009(11) 0.0006(10) C113 0.0231(15) 0.0236(14) 0.0340(16) -0.0023(12) 0.0007(13) 0.0023(12) C114 0.0287(16) 0.0280(16) 0.0420(19) -0.0055(14) -0.0125(15) 0.0006(13) C115 0.053(2) 0.0279(16) 0.0210(15) -0.0023(13) -0.0094(15) -0.0018(15) C116 0.050(2) 0.0297(16) 0.0213(15) 0.0018(13) 0.0075(14) -0.0063(15) C117 0.0297(16) 0.0259(15) 0.0244(15) -0.0013(12) 0.0026(13) -0.0059(12) C118 0.0210(14) 0.0232(14) 0.0145(13) -0.0003(11) 0.0019(11) 0.0027(11) C119 0.0278(15) 0.0218(14) 0.0260(15) 0.0003(12) -0.0001(12) -0.0015(12) C120 0.0335(17) 0.0253(15) 0.0312(16) 0.0016(13) 0.0009(13) 0.0092(13) C121 0.0256(15) 0.0390(17) 0.0262(15) 0.0049(13) 0.0030(12) 0.0127(14) C122 0.0224(15) 0.0331(16) 0.0269(15) 0.0003(13) 0.0013(12) 0.0014(12) C123 0.0252(15) 0.0244(15) 0.0237(14) 0.0014(12) 0.0027(12) 0.0000(12) Fe2 0.0248(2) 0.0232(2) 0.0299(2) -0.00253(17) 0.00336(18) 0.00260(17) P2 0.0195(4) 0.0220(4) 0.0203(4) -0.0022(3) 0.0020(3) -0.0018(3) B2 0.0266(18) 0.0345(19) 0.0260(17) 0.0022(14) 0.0052(14) -0.0080(15) C201 0.0212(14) 0.0235(15) 0.0323(16) -0.0035(12) 0.0022(12) -0.0008(12) C202 0.0260(16) 0.0249(15) 0.052(2) 0.0007(14) 0.0169(15) 0.0010(13) C203 0.0327(19) 0.0236(16) 0.082(3) 0.0009(18) 0.0162(19) -0.0057(14) C204 0.0322(18) 0.0272(17) 0.072(3) -0.0192(17) -0.0067(17) 0.0008(14) C205 0.0271(16) 0.0362(18) 0.0374(18) -0.0115(14) -0.0065(14) 0.0052(14) C206 0.045(2) 0.0349(18) 0.0375(19) -0.0005(15) -0.0102(16) 0.0080(15) C207 0.048(2) 0.0263(17) 0.045(2) 0.0039(15) -0.0025(16) 0.0100(15) C208 0.0313(17) 0.043(2) 0.043(2) -0.0069(16) 0.0073(15) 0.0150(15) C209 0.0281(17) 0.051(2) 0.044(2) 0.0064(17) 0.0102(15) 0.0090(15) C210 0.0225(16) 0.0325(17) 0.048(2) 0.0027(15) -0.0045(14) 0.0009(13) C212 0.0250(15) 0.0188(13) 0.0219(14) -0.0013(11) 0.0024(12) -0.0005(11) C213 0.0210(14) 0.0257(15) 0.0277(15) -0.0018(12) 0.0033(12) 0.0002(12) C214 0.0229(15) 0.0297(16) 0.0296(16) -0.0040(13) -0.0036(12) 0.0011(12) C215 0.0386(18) 0.0305(16) 0.0207(14) -0.0033(12) -0.0002(13) 0.0023(13) C216 0.0376(18) 0.0296(16) 0.0217(15) -0.0012(12) 0.0071(13) -0.0031(13) C217 0.0257(15) 0.0262(15) 0.0282(15) -0.0005(12) 0.0053(12) -0.0041(12) C218 0.0250(15) 0.0246(14) 0.0177(13) 0.0003(11) 0.0030(11) -0.0004(12) C219 0.0272(15) 0.0256(15) 0.0247(15) 0.0000(12) 0.0057(12) -0.0010(12) C220 0.0254(16) 0.0372(17) 0.0317(16) 0.0004(14) 0.0040(13) -0.0017(13) C221 0.0274(16) 0.0410(18) 0.0334(17) 0.0038(14) 0.0039(13) 0.0102(14) C222 0.0418(19) 0.0285(17) 0.0339(17) -0.0001(13) 0.0040(15) 0.0064(14) C223 0.0271(16) 0.0270(15) 0.0289(16) -0.0027(12) 0.0012(13) -0.0017(12) Fe3 0.0214(2) 0.01812(19) 0.0204(2) 0.00071(15) 0.00378(16) 0.00127(16) P3 0.0178(3) 0.0183(3) 0.0173(3) -0.0004(3) 0.0026(3) 0.0000(3) B3 0.0279(17) 0.0267(17) 0.0260(17) 0.0038(14) 0.0098(14) 0.0025(14) C301 0.0186(13) 0.0195(13) 0.0232(14) -0.0040(11) 0.0026(11) 0.0005(11) C302 0.0248(15) 0.0244(15) 0.0333(16) 0.0001(12) 0.0122(13) 0.0005(12) C304 0.0283(16) 0.0242(15) 0.0416(18) -0.0060(14) -0.0046(14) -0.0022(13) C303 0.0248(15) 0.0228(15) 0.0481(19) 0.0045(14) 0.0131(14) -0.0024(12) C305 0.0273(15) 0.0244(15) 0.0269(15) -0.0034(12) -0.0038(12) 0.0025(12) C306 0.0375(18) 0.0289(16) 0.0316(17) 0.0020(13) -0.0095(14) 0.0045(13) C307 0.0345(17) 0.0213(15) 0.0364(17) 0.0062(13) 0.0031(14) 0.0036(13) C308 0.0293(16) 0.0249(15) 0.0390(17) -0.0034(13) 0.0097(14) 0.0086(13) C309 0.0266(16) 0.0311(16) 0.0420(18) 0.0031(14) 0.0153(14) 0.0048(13) C310 0.0217(15) 0.0232(15) 0.0411(18) 0.0040(13) 0.0021(13) 0.0024(12) C312 0.0214(14) 0.0162(13) 0.0198(13) 0.0016(10) 0.0014(11) 0.0027(10) C313 0.0203(14) 0.0205(14) 0.0296(15) -0.0004(12) 0.0038(12) -0.0001(11) C314 0.0263(16) 0.0214(15) 0.0373(17) -0.0001(13) -0.0077(13) -0.0020(12) C315 0.0439(19) 0.0258(15) 0.0211(15) -0.0059(12) -0.0085(13) 0.0028(14) C316 0.0412(18) 0.0298(16) 0.0216(15) -0.0043(12) 0.0049(13) -0.0060(14) C317 0.0228(14) 0.0248(14) 0.0221(14) -0.0017(11) 0.0034(11) -0.0024(11) C318 0.0224(14) 0.0219(14) 0.0163(13) -0.0001(11) 0.0027(11) 0.0020(11) C319 0.0232(14) 0.0225(14) 0.0217(14) -0.0007(11) 0.0026(11) -0.0006(11) C320 0.0207(15) 0.0364(17) 0.0301(16) -0.0008(13) 0.0034(12) -0.0032(13) C321 0.0227(15) 0.0331(16) 0.0311(16) -0.0011(13) 0.0010(13) 0.0100(13) C322 0.0307(17) 0.0240(15) 0.0363(17) 0.0004(13) 0.0012(14) 0.0061(13) C323 0.0258(15) 0.0213(14) 0.0293(15) -0.0028(12) 0.0008(12) 0.0009(12) Fe4 0.0208(2) 0.0198(2) 0.0194(2) -0.00077(15) 0.00258(16) -0.00059(16) P4 0.0197(4) 0.0217(4) 0.0187(3) -0.0006(3) 0.0030(3) -0.0011(3) O4 0.0249(11) 0.0408(12) 0.0292(11) 0.0053(9) -0.0031(9) -0.0044(9) B4 0.0307(18) 0.0275(17) 0.0243(17) -0.0036(14) 0.0090(14) -0.0012(14) C401 0.0188(14) 0.0226(14) 0.0239(14) 0.0007(11) 0.0016(11) 0.0008(11) C402 0.0196(14) 0.0246(14) 0.0255(14) -0.0027(12) 0.0056(12) -0.0016(11) C403 0.0213(15) 0.0278(15) 0.0350(17) -0.0061(13) 0.0011(13) 0.0017(12) C404 0.0254(15) 0.0266(15) 0.0329(16) 0.0020(13) -0.0047(13) 0.0026(12) C405 0.0271(15) 0.0277(15) 0.0206(14) -0.0010(12) -0.0030(12) -0.0011(12) C406 0.0168(13) 0.0240(14) 0.0242(14) -0.0012(11) 0.0017(11) -0.0013(11) C407 0.0232(14) 0.0190(14) 0.0269(15) -0.0026(11) 0.0015(12) -0.0023(11) C408 0.0259(15) 0.0274(15) 0.0269(15) 0.0038(12) 0.0057(12) -0.0047(12) C409 0.0230(15) 0.0324(16) 0.0244(15) -0.0031(12) 0.0048(12) -0.0023(12) C410 0.0194(14) 0.0225(14) 0.0301(15) -0.0023(12) 0.0020(12) 0.0007(11) C411 0.0256(15) 0.0312(16) 0.0257(15) 0.0012(12) 0.0027(12) -0.0041(12) C412 0.0236(14) 0.0191(13) 0.0207(14) 0.0012(11) -0.0011(11) -0.0014(11) C413 0.0218(14) 0.0200(14) 0.0348(16) 0.0021(12) 0.0033(12) -0.0014(11) C414 0.0263(16) 0.0231(15) 0.0440(19) 0.0044(13) -0.0091(14) -0.0001(12) C415 0.048(2) 0.0262(16) 0.0270(16) 0.0017(13) -0.0087(15) -0.0009(14) C416 0.049(2) 0.0291(16) 0.0231(15) 0.0020(13) 0.0042(14) 0.0043(14) C417 0.0275(15) 0.0267(15) 0.0252(15) 0.0023(12) 0.0045(12) 0.0032(12) C418 0.0204(14) 0.0259(14) 0.0177(13) 0.0010(11) 0.0022(11) -0.0021(11) C419 0.0242(15) 0.0281(15) 0.0267(15) 0.0007(12) 0.0018(12) -0.0011(12) C420 0.0349(17) 0.0253(16) 0.0328(16) 0.0000(13) 0.0021(14) -0.0049(13) C421 0.0201(15) 0.0366(17) 0.0312(16) 0.0004(13) 0.0022(12) -0.0071(13) C422 0.0199(14) 0.0361(17) 0.0258(15) 0.0013(13) 0.0027(12) 0.0011(12) C423 0.0248(15) 0.0235(14) 0.0214(14) 0.0004(11) 0.0048(12) -0.0032(12) _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 C101 2.018(3) . ? Fe1 C102 2.028(3) . ? Fe1 C109 2.041(3) . ? Fe1 C108 2.041(3) . ? Fe1 C105 2.041(3) . ? Fe1 C110 2.044(3) . ? Fe1 C103 2.049(3) . ? Fe1 C107 2.050(3) . ? Fe1 C106 2.054(3) . ? Fe1 C104 2.061(3) . ? P1 C101 1.791(3) . ? P1 C112 1.813(3) . ? P1 C118 1.823(3) . ? P1 B1 1.913(3) . ? O1 C111 1.436(3) . ? O1 H91 1.0181 . ? B1 H1B 1.1291 . ? B1 H2B 1.1394 . ? B1 H3B 1.1626 . ? C101 C102 1.428(4) . ? C101 C105 1.436(4) . ? C102 C103 1.414(4) . ? C102 H102 0.9300 . ? C103 C104 1.425(4) . ? C103 H103 0.9300 . ? C104 C105 1.420(4) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? C106 C107 1.428(4) . ? C106 C110 1.428(4) . ? C106 C111 1.492(4) . ? C107 C108 1.414(4) . ? C107 H107 0.9300 . ? C108 C109 1.409(4) . ? C108 H108 0.9300 . ? C109 C110 1.424(4) . ? C109 H109 0.9300 . ? C110 H110 0.9300 . ? C111 H11A 0.9700 . ? C111 H11C 0.9700 . ? C112 C117 1.384(4) . ? C112 C113 1.397(4) . ? C113 C114 1.389(4) . ? C113 H113 0.9300 . ? C114 C115 1.378(4) . ? C114 H114 0.9300 . ? C115 C116 1.379(4) . ? C115 H115 0.9300 . ? C116 C117 1.390(4) . ? C116 H116 0.9300 . ? C117 H117 0.9300 . ? C118 C123 1.389(4) . ? C118 C119 1.396(4) . ? C119 C120 1.390(4) . ? C119 H119 0.9300 . ? C120 C121 1.379(4) . ? C120 H120 0.9300 . ? C121 C122 1.391(4) . ? C121 H121 0.9300 . ? C122 C123 1.384(4) . ? C122 H122 0.9300 . ? C123 H123 0.9300 . ? Fe2 C201 2.026(3) . ? Fe2 C205 2.038(3) . ? Fe2 C208 2.041(3) . ? Fe2 C207 2.041(3) . ? Fe2 C210 2.042(3) . ? Fe2 C202 2.042(3) . ? Fe2 C209 2.042(3) . ? Fe2 C206 2.044(3) . ? Fe2 C203 2.047(3) . ? Fe2 C204 2.049(3) . ? P2 C201 1.790(3) . ? P2 C212 1.812(3) . ? P2 C218 1.823(3) . ? P2 B2 1.924(3) . ? O2A C21A 1.465(7) . ? O2A H92A 0.8195 . ? O2B C21B 1.385(10) . ? O2B H92B 0.8200 . ? B2 H4B 1.0443 . ? B2 H5B 1.2299 . ? B2 H6B 1.1827 . ? C201 C205 1.433(4) . ? C201 C202 1.437(4) . ? C202 C203 1.417(4) . ? C202 H202 0.9300 . ? C203 C204 1.420(5) . ? C203 H203 0.9300 . ? C204 C205 1.413(5) . ? C204 H204 0.9300 . ? C205 H205 0.9300 . ? C206 C210 1.421(4) . ? C206 C21B 1.428(9) . ? C206 C207 1.440(4) . ? C206 C21A 1.576(7) . ? C207 C208 1.415(4) . ? C207 H207 0.9300 . ? C208 C209 1.414(5) . ? C208 H208 0.9300 . ? C209 C210 1.420(5) . ? C209 H209 0.9300 . ? C210 H210 0.9300 . ? C21A H21A 0.9700 . ? C21A H21B 0.9700 . ? C21B H21C 0.9700 . ? C21B H21D 0.9700 . ? C212 C213 1.393(4) . ? C212 C217 1.395(4) . ? C213 C214 1.397(4) . ? C213 H213 0.9300 . ? C214 C215 1.372(4) . ? C214 H214 0.9300 . ? C215 C216 1.384(4) . ? C215 H215 0.9300 . ? C216 C217 1.380(4) . ? C216 H216 0.9300 . ? C217 H217 0.9300 . ? C218 C219 1.386(4) . ? C218 C223 1.397(4) . ? C219 C220 1.391(4) . ? C219 H219 0.9300 . ? C220 C221 1.382(4) . ? C220 H220 0.9300 . ? C221 C222 1.389(4) . ? C221 H221 0.9300 . ? C222 C223 1.385(4) . ? C222 H222 0.9300 . ? C223 H223 0.9300 . ? Fe3 C301 2.037(3) . ? Fe3 C302 2.037(3) . ? Fe3 C305 2.039(3) . ? Fe3 C308 2.040(3) . ? Fe3 C309 2.043(3) . ? Fe3 C307 2.045(3) . ? Fe3 C310 2.051(3) . ? Fe3 C303 2.058(3) . ? Fe3 C306 2.059(3) . ? Fe3 C304 2.061(3) . ? P3 C301 1.785(3) . ? P3 C312 1.807(3) . ? P3 C318 1.818(3) . ? P3 B3 1.915(3) . ? O3A C31A 1.425(7) . ? O3A H93A 0.8200 . ? O3B C31B 1.429(8) . ? O3B H93B 0.8200 . ? B3 H7B 1.0505 . ? B3 H8B 1.1238 . ? B3 H9B 1.0522 . ? C301 C302 1.435(4) . ? C301 C305 1.436(4) . ? C302 C303 1.426(4) . ? C302 H302 0.9300 . ? C304 C303 1.418(4) . ? C304 C305 1.431(4) . ? C304 H304 0.9300 . ? C303 H303 0.9300 . ? C305 H305 0.9300 . ? C306 C31A 1.414(7) . ? C306 C310 1.425(4) . ? C306 C307 1.433(4) . ? C306 C31B 1.603(7) . ? C307 C308 1.416(4) . ? C307 H307 0.9300 . ? C308 C309 1.422(4) . ? C308 H308 0.9300 . ? C309 C310 1.414(4) . ? C309 H309 0.9300 . ? C310 H310 0.9300 . ? C31A H31A 0.9700 . ? C31A H31B 0.9700 . ? C31B H31C 0.9700 . ? C31B H31D 0.9700 . ? C312 C313 1.394(4) . ? C312 C317 1.396(4) . ? C313 C314 1.387(4) . ? C313 H313 0.9300 . ? C314 C315 1.389(4) . ? C314 H314 0.9300 . ? C315 C316 1.384(4) . ? C315 H315 0.9300 . ? C316 C317 1.389(4) . ? C316 H316 0.9300 . ? C317 H317 0.9300 . ? C318 C319 1.389(4) . ? C318 C323 1.397(4) . ? C319 C320 1.384(4) . ? C319 H319 0.9300 . ? C320 C321 1.387(4) . ? C320 H320 0.9300 . ? C321 C322 1.379(4) . ? C321 H321 0.9300 . ? C322 C323 1.389(4) . ? C322 H322 0.9300 . ? C323 H323 0.9300 . ? Fe4 C401 2.029(3) . ? Fe4 C405 2.033(3) . ? Fe4 C402 2.040(3) . ? Fe4 C408 2.042(3) . ? Fe4 C409 2.045(3) . ? Fe4 C407 2.045(3) . ? Fe4 C403 2.055(3) . ? Fe4 C410 2.056(3) . ? Fe4 C404 2.057(3) . ? Fe4 C406 2.060(3) . ? P4 C401 1.786(3) . ? P4 C418 1.815(3) . ? P4 C412 1.816(3) . ? P4 B4 1.927(3) . ? O4 C411 1.436(3) . ? O4 H94 1.0295 . ? B4 H10B 1.1046 . ? B4 H11B 1.1291 . ? B4 H12B 1.1274 . ? C401 C405 1.438(4) . ? C401 C402 1.442(4) . ? C402 C403 1.415(4) . ? C402 H402 0.9300 . ? C403 C404 1.427(4) . ? C403 H403 0.9300 . ? C404 C405 1.417(4) . ? C404 H404 0.9300 . ? C405 H405 0.9300 . ? C406 C410 1.429(4) . ? C406 C407 1.433(4) . ? C406 C411 1.495(4) . ? C407 C408 1.426(4) . ? C407 H407 0.9300 . ? C408 C409 1.417(4) . ? C408 H408 0.9300 . ? C409 C410 1.420(4) . ? C409 H409 0.9300 . ? C410 H410 0.9300 . ? C411 H41A 0.9700 . ? C411 H41B 0.9700 . ? C412 C413 1.387(4) . ? C412 C417 1.398(4) . ? C413 C414 1.389(4) . ? C413 H413 0.9300 . ? C414 C415 1.376(4) . ? C414 H414 0.9300 . ? C415 C416 1.393(4) . ? C415 H415 0.9300 . ? C416 C417 1.378(4) . ? C416 H416 0.9300 . ? C417 H417 0.9300 . ? C418 C423 1.390(4) . ? C418 C419 1.398(4) . ? C419 C420 1.388(4) . ? C419 H419 0.9300 . ? C420 C421 1.394(4) . ? C420 H420 0.9300 . ? C421 C422 1.378(4) . ? C421 H421 0.9300 . ? C422 C423 1.389(4) . ? C422 H422 0.9300 . ? C423 H423 0.9300 . ? 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 C101 Fe1 C102 41.33(10) . . ? C101 Fe1 C109 154.91(11) . . ? C102 Fe1 C109 118.75(12) . . ? C101 Fe1 C108 120.95(11) . . ? C102 Fe1 C108 106.88(12) . . ? C109 Fe1 C108 40.40(11) . . ? C101 Fe1 C105 41.43(10) . . ? C102 Fe1 C105 69.20(11) . . ? C109 Fe1 C105 161.34(12) . . ? C108 Fe1 C105 157.41(12) . . ? C101 Fe1 C110 163.41(11) . . ? C102 Fe1 C110 153.59(11) . . ? C109 Fe1 C110 40.80(11) . . ? C108 Fe1 C110 68.45(12) . . ? C105 Fe1 C110 125.09(11) . . ? C101 Fe1 C103 69.00(11) . . ? C102 Fe1 C103 40.58(11) . . ? C109 Fe1 C103 105.64(12) . . ? C108 Fe1 C103 123.70(13) . . ? C105 Fe1 C103 68.63(12) . . ? C110 Fe1 C103 118.89(12) . . ? C101 Fe1 C107 109.08(11) . . ? C102 Fe1 C107 125.97(11) . . ? C109 Fe1 C107 67.93(11) . . ? C108 Fe1 C107 40.44(11) . . ? C105 Fe1 C107 122.83(11) . . ? C110 Fe1 C107 68.29(11) . . ? C103 Fe1 C107 161.62(12) . . ? C101 Fe1 C106 126.59(10) . . ? C102 Fe1 C106 163.84(11) . . ? C109 Fe1 C106 68.50(11) . . ? C108 Fe1 C106 68.54(11) . . ? C105 Fe1 C106 108.72(11) . . ? C110 Fe1 C106 40.78(10) . . ? C103 Fe1 C106 154.90(12) . . ? C107 Fe1 C106 40.71(10) . . ? C101 Fe1 C104 68.85(11) . . ? C102 Fe1 C104 68.41(12) . . ? C109 Fe1 C104 123.86(12) . . ? C108 Fe1 C104 160.51(12) . . ? C105 Fe1 C104 40.50(11) . . ? C110 Fe1 C104 106.88(12) . . ? C103 Fe1 C104 40.57(12) . . ? C107 Fe1 C104 157.24(12) . . ? C106 Fe1 C104 121.12(12) . . ? C101 P1 C112 107.18(12) . . ? C101 P1 C118 104.58(12) . . ? C112 P1 C118 104.72(12) . . ? C101 P1 B1 114.43(14) . . ? C112 P1 B1 113.80(14) . . ? C118 P1 B1 111.29(13) . . ? C111 O1 H91 107.6 . . ? P1 B1 H1B 109.2 . . ? P1 B1 H2B 103.5 . . ? H1B B1 H2B 106.1 . . ? P1 B1 H3B 111.0 . . ? H1B B1 H3B 113.2 . . ? H2B B1 H3B 113.2 . . ? C102 C101 C105 107.6(2) . . ? C102 C101 P1 124.2(2) . . ? C105 C101 P1 128.2(2) . . ? C102 C101 Fe1 69.72(15) . . ? C105 C101 Fe1 70.15(15) . . ? P1 C101 Fe1 127.30(14) . . ? C103 C102 C101 108.3(3) . . ? C103 C102 Fe1 70.50(16) . . ? C101 C102 Fe1 68.95(15) . . ? C103 C102 H102 125.8 . . ? C101 C102 H102 125.8 . . ? Fe1 C102 H102 126.3 . . ? C102 C103 C104 108.1(3) . . ? C102 C103 Fe1 68.92(16) . . ? C104 C103 Fe1 70.16(16) . . ? C102 C103 H103 125.9 . . ? C104 C103 H103 125.9 . . ? Fe1 C103 H103 126.6 . . ? C105 C104 C103 108.3(3) . . ? C105 C104 Fe1 69.00(16) . . ? C103 C104 Fe1 69.27(16) . . ? C105 C104 H104 125.9 . . ? C103 C104 H104 125.9 . . ? Fe1 C104 H104 127.4 . . ? C104 C105 C101 107.7(3) . . ? C104 C105 Fe1 70.49(16) . . ? C101 C105 Fe1 68.42(15) . . ? C104 C105 H105 126.2 . . ? C101 C105 H105 126.2 . . ? Fe1 C105 H105 126.5 . . ? C107 C106 C110 107.2(2) . . ? C107 C106 C111 125.5(3) . . ? C110 C106 C111 127.4(3) . . ? C107 C106 Fe1 69.52(15) . . ? C110 C106 Fe1 69.23(15) . . ? C111 C106 Fe1 126.48(19) . . ? C108 C107 C106 108.5(2) . . ? C108 C107 Fe1 69.42(16) . . ? C106 C107 Fe1 69.77(15) . . ? C108 C107 H107 125.8 . . ? C106 C107 H107 125.8 . . ? Fe1 C107 H107 126.6 . . ? C109 C108 C107 108.1(3) . . ? C109 C108 Fe1 69.80(17) . . ? C107 C108 Fe1 70.14(16) . . ? C109 C108 H108 125.9 . . ? C107 C108 H108 125.9 . . ? Fe1 C108 H108 125.7 . . ? C108 C109 C110 108.4(3) . . ? C108 C109 Fe1 69.81(16) . . ? C110 C109 Fe1 69.72(16) . . ? C108 C109 H109 125.8 . . ? C110 C109 H109 125.8 . . ? Fe1 C109 H109 126.2 . . ? C109 C110 C106 107.8(3) . . ? C109 C110 Fe1 69.48(16) . . ? C106 C110 Fe1 69.98(15) . . ? C109 C110 H110 126.1 . . ? C106 C110 H110 126.1 . . ? Fe1 C110 H110 126.0 . . ? O1 C111 C106 108.8(2) . . ? O1 C111 H11A 109.9 . . ? C106 C111 H11A 109.9 . . ? O1 C111 H11C 109.9 . . ? C106 C111 H11C 109.9 . . ? H11A C111 H11C 108.3 . . ? C117 C112 C113 118.9(2) . . ? C117 C112 P1 121.4(2) . . ? C113 C112 P1 119.7(2) . . ? C114 C113 C112 120.2(3) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C115 C114 C113 120.2(3) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C114 C115 C116 120.3(3) . . ? C114 C115 H115 119.9 . . ? C116 C115 H115 119.9 . . ? C115 C116 C117 119.7(3) . . ? C115 C116 H116 120.1 . . ? C117 C116 H116 120.1 . . ? C112 C117 C116 120.8(3) . . ? C112 C117 H117 119.6 . . ? C116 C117 H117 119.6 . . ? C123 C118 C119 119.1(2) . . ? C123 C118 P1 121.9(2) . . ? C119 C118 P1 118.9(2) . . ? C120 C119 C118 120.6(3) . . ? C120 C119 H119 119.7 . . ? C118 C119 H119 119.7 . . ? C121 C120 C119 119.6(3) . . ? C121 C120 H120 120.2 . . ? C119 C120 H120 120.2 . . ? C120 C121 C122 120.3(3) . . ? C120 C121 H121 119.9 . . ? C122 C121 H121 119.9 . . ? C123 C122 C121 120.0(3) . . ? C123 C122 H122 120.0 . . ? C121 C122 H122 120.0 . . ? C122 C123 C118 120.4(3) . . ? C122 C123 H123 119.8 . . ? C118 C123 H123 119.8 . . ? C201 Fe2 C205 41.29(11) . . ? C201 Fe2 C208 155.60(13) . . ? C205 Fe2 C208 119.17(13) . . ? C201 Fe2 C207 163.17(13) . . ? C205 Fe2 C207 153.46(13) . . ? C208 Fe2 C207 40.58(13) . . ? C201 Fe2 C210 109.27(12) . . ? C205 Fe2 C210 126.34(13) . . ? C208 Fe2 C210 68.32(13) . . ? C207 Fe2 C210 68.63(13) . . ? C201 Fe2 C202 41.36(12) . . ? C205 Fe2 C202 69.15(13) . . ? C208 Fe2 C202 160.65(13) . . ? C207 Fe2 C202 124.61(14) . . ? C210 Fe2 C202 122.67(13) . . ? C201 Fe2 C209 121.63(13) . . ? C205 Fe2 C209 107.43(14) . . ? C208 Fe2 C209 40.52(13) . . ? C207 Fe2 C209 68.44(14) . . ? C210 Fe2 C209 40.69(13) . . ? C202 Fe2 C209 157.86(13) . . ? C201 Fe2 C206 126.26(12) . . ? C205 Fe2 C206 163.84(13) . . ? C208 Fe2 C206 68.82(13) . . ? C207 Fe2 C206 41.28(12) . . ? C210 Fe2 C206 40.72(13) . . ? C202 Fe2 C206 108.14(14) . . ? C209 Fe2 C206 68.73(14) . . ? C201 Fe2 C203 68.81(12) . . ? C205 Fe2 C203 68.39(14) . . ? C208 Fe2 C203 123.27(14) . . ? C207 Fe2 C203 106.22(14) . . ? C210 Fe2 C203 156.92(15) . . ? C202 Fe2 C203 40.55(12) . . ? C209 Fe2 C203 160.29(14) . . ? C206 Fe2 C203 120.61(15) . . ? C201 Fe2 C204 68.82(12) . . ? C205 Fe2 C204 40.45(13) . . ? C208 Fe2 C204 105.62(14) . . ? C207 Fe2 C204 118.56(13) . . ? C210 Fe2 C204 161.97(15) . . ? C202 Fe2 C204 68.56(14) . . ? C209 Fe2 C204 123.88(15) . . ? C206 Fe2 C204 154.78(14) . . ? C203 Fe2 C204 40.57(14) . . ? C201 P2 C212 106.67(13) . . ? C201 P2 C218 105.34(13) . . ? C212 P2 C218 103.54(12) . . ? C201 P2 B2 114.31(15) . . ? C212 P2 B2 113.95(14) . . ? C218 P2 B2 112.10(14) . . ? C21A O2A H92A 100.8 . . ? C21B O2B H92B 109.5 . . ? P2 B2 H4B 103.5 . . ? P2 B2 H5B 97.5 . . ? H4B B2 H5B 110.2 . . ? P2 B2 H6B 111.6 . . ? H4B B2 H6B 114.5 . . ? H5B B2 H6B 117.4 . . ? C205 C201 C202 107.6(3) . . ? C205 C201 P2 124.1(2) . . ? C202 C201 P2 128.3(2) . . ? C205 C201 Fe2 69.79(16) . . ? C202 C201 Fe2 69.91(16) . . ? P2 C201 Fe2 127.10(15) . . ? C203 C202 C201 107.5(3) . . ? C203 C202 Fe2 69.93(18) . . ? C201 C202 Fe2 68.73(16) . . ? C203 C202 H202 126.2 . . ? C201 C202 H202 126.2 . . ? Fe2 C202 H202 126.7 . . ? C202 C203 C204 108.6(3) . . ? C202 C203 Fe2 69.52(17) . . ? C204 C203 Fe2 69.78(19) . . ? C202 C203 H203 125.7 . . ? C204 C203 H203 125.7 . . ? Fe2 C203 H203 126.6 . . ? C205 C204 C203 108.3(3) . . ? C205 C204 Fe2 69.34(17) . . ? C203 C204 Fe2 69.65(19) . . ? C205 C204 H204 125.9 . . ? C203 C204 H204 125.9 . . ? Fe2 C204 H204 126.7 . . ? C204 C205 C201 108.0(3) . . ? C204 C205 Fe2 70.20(19) . . ? C201 C205 Fe2 68.92(17) . . ? C204 C205 H205 126.0 . . ? C201 C205 H205 126.0 . . ? Fe2 C205 H205 126.5 . . ? C210 C206 C21B 119.0(5) . . ? C210 C206 C207 107.1(3) . . ? C21B C206 C207 131.6(5) . . ? C210 C206 C21A 127.9(4) . . ? C207 C206 C21A 124.0(4) . . ? C210 C206 Fe2 69.56(17) . . ? C21B C206 Fe2 139.3(4) . . ? C207 C206 Fe2 69.26(18) . . ? C21A C206 Fe2 117.4(3) . . ? C208 C207 C206 107.9(3) . . ? C208 C207 Fe2 69.70(18) . . ? C206 C207 Fe2 69.46(17) . . ? C208 C207 H207 126.1 . . ? C206 C207 H207 126.1 . . ? Fe2 C207 H207 126.4 . . ? C209 C208 C207 108.5(3) . . ? C209 C208 Fe2 69.79(18) . . ? C207 C208 Fe2 69.72(18) . . ? C209 C208 H208 125.7 . . ? C207 C208 H208 125.7 . . ? Fe2 C208 H208 126.3 . . ? C208 C209 C210 108.0(3) . . ? C208 C209 Fe2 69.69(19) . . ? C210 C209 Fe2 69.64(18) . . ? C208 C209 H209 126.0 . . ? C210 C209 H209 126.0 . . ? Fe2 C209 H209 126.2 . . ? C209 C210 C206 108.5(3) . . ? C209 C210 Fe2 69.67(18) . . ? C206 C210 Fe2 69.72(18) . . ? C209 C210 H210 125.7 . . ? C206 C210 H210 125.7 . . ? Fe2 C210 H210 126.5 . . ? O2A C21A C206 109.2(4) . . ? O2A C21A H21A 109.8 . . ? C206 C21A H21A 109.8 . . ? O2A C21A H21B 109.8 . . ? C206 C21A H21B 109.8 . . ? H21A C21A H21B 108.3 . . ? O2B C21B C206 105.5(7) . . ? O2B C21B H92A 99.5 . . ? C206 C21B H92A 135.6 . . ? O2B C21B H21C 110.6 . . ? C206 C21B H21C 110.6 . . ? H92A C21B H21C 93.5 . . ? O2B C21B H21D 110.6 . . ? C206 C21B H21D 110.6 . . ? H21C C21B H21D 108.8 . . ? C213 C212 C217 119.4(3) . . ? C213 C212 P2 119.9(2) . . ? C217 C212 P2 120.7(2) . . ? C212 C213 C214 119.6(3) . . ? C212 C213 H213 120.2 . . ? C214 C213 H213 120.2 . . ? C215 C214 C213 120.2(3) . . ? C215 C214 H214 119.9 . . ? C213 C214 H214 119.9 . . ? C214 C215 C216 120.4(3) . . ? C214 C215 H215 119.8 . . ? C216 C215 H215 119.8 . . ? C217 C216 C215 120.0(3) . . ? C217 C216 H216 120.0 . . ? C215 C216 H216 120.0 . . ? C216 C217 C212 120.3(3) . . ? C216 C217 H217 119.8 . . ? C212 C217 H217 119.8 . . ? C219 C218 C223 119.4(3) . . ? C219 C218 P2 122.1(2) . . ? C223 C218 P2 118.5(2) . . ? C218 C219 C220 120.5(3) . . ? C218 C219 H219 119.7 . . ? C220 C219 H219 119.7 . . ? C221 C220 C219 119.9(3) . . ? C221 C220 H220 120.0 . . ? C219 C220 H220 120.0 . . ? C220 C221 C222 119.9(3) . . ? C220 C221 H221 120.1 . . ? C222 C221 H221 120.1 . . ? C223 C222 C221 120.3(3) . . ? C223 C222 H222 119.8 . . ? C221 C222 H222 119.8 . . ? C222 C223 C218 120.0(3) . . ? C222 C223 H223 120.0 . . ? C218 C223 H223 120.0 . . ? C301 Fe3 C302 41.25(11) . . ? C301 Fe3 C305 41.25(10) . . ? C302 Fe3 C305 69.17(12) . . ? C301 Fe3 C308 155.18(11) . . ? C302 Fe3 C308 160.81(12) . . ? C305 Fe3 C308 118.56(12) . . ? C301 Fe3 C309 121.17(11) . . ? C302 Fe3 C309 157.79(12) . . ? C305 Fe3 C309 106.43(12) . . ? C308 Fe3 C309 40.75(11) . . ? C301 Fe3 C307 163.59(11) . . ? C302 Fe3 C307 125.28(12) . . ? C305 Fe3 C307 153.45(12) . . ? C308 Fe3 C307 40.55(11) . . ? C309 Fe3 C307 68.48(12) . . ? C301 Fe3 C310 109.62(11) . . ? C302 Fe3 C310 123.52(12) . . ? C305 Fe3 C310 125.76(12) . . ? C308 Fe3 C310 68.04(12) . . ? C309 Fe3 C310 40.40(12) . . ? C307 Fe3 C310 68.18(12) . . ? C301 Fe3 C303 68.92(11) . . ? C302 Fe3 C303 40.74(11) . . ? C305 Fe3 C303 68.62(12) . . ? C308 Fe3 C303 122.90(12) . . ? C309 Fe3 C303 159.71(12) . . ? C307 Fe3 C303 106.66(12) . . ? C310 Fe3 C303 157.93(12) . . ? C301 Fe3 C306 126.89(11) . . ? C302 Fe3 C306 109.24(13) . . ? C305 Fe3 C306 163.64(12) . . ? C308 Fe3 C306 68.51(12) . . ? C309 Fe3 C306 68.55(13) . . ? C307 Fe3 C306 40.87(11) . . ? C310 Fe3 C306 40.57(12) . . ? C303 Fe3 C306 121.52(13) . . ? C301 Fe3 C304 68.85(11) . . ? C302 Fe3 C304 68.40(12) . . ? C305 Fe3 C304 40.84(11) . . ? C308 Fe3 C304 105.16(12) . . ? C309 Fe3 C304 123.32(13) . . ? C307 Fe3 C304 118.69(12) . . ? C310 Fe3 C304 161.39(12) . . ? C303 Fe3 C304 40.27(12) . . ? C306 Fe3 C304 154.98(12) . . ? C301 P3 C312 105.35(12) . . ? C301 P3 C318 106.11(12) . . ? C312 P3 C318 102.96(12) . . ? C301 P3 B3 114.37(14) . . ? C312 P3 B3 117.02(14) . . ? C318 P3 B3 109.93(13) . . ? C31A O3A H93A 109.5 . . ? C31B O3B H93B 109.5 . . ? P3 B3 H7B 107.6 . . ? P3 B3 H8B 102.5 . . ? H7B B3 H8B 109.3 . . ? P3 B3 H9B 110.0 . . ? H7B B3 H9B 115.0 . . ? H8B B3 H9B 111.6 . . ? C302 C301 C305 107.4(2) . . ? C302 C301 P3 128.0(2) . . ? C305 C301 P3 124.6(2) . . ? C302 C301 Fe3 69.39(15) . . ? C305 C301 Fe3 69.45(15) . . ? P3 C301 Fe3 126.88(14) . . ? C303 C302 C301 108.2(3) . . ? C303 C302 Fe3 70.41(16) . . ? C301 C302 Fe3 69.36(15) . . ? C303 C302 H302 125.9 . . ? C301 C302 H302 125.9 . . ? Fe3 C302 H302 125.9 . . ? C303 C304 C305 108.3(3) . . ? C303 C304 Fe3 69.76(16) . . ? C305 C304 Fe3 68.75(16) . . ? C303 C304 H304 125.8 . . ? C305 C304 H304 125.8 . . ? Fe3 C304 H304 127.2 . . ? C304 C303 C302 108.2(3) . . ? C304 C303 Fe3 69.97(16) . . ? C302 C303 Fe3 68.85(16) . . ? C304 C303 H303 125.9 . . ? C302 C303 H303 125.9 . . ? Fe3 C303 H303 126.9 . . ? C304 C305 C301 107.9(3) . . ? C304 C305 Fe3 70.41(16) . . ? C301 C305 Fe3 69.31(15) . . ? C304 C305 H305 126.1 . . ? C301 C305 H305 126.1 . . ? Fe3 C305 H305 125.8 . . ? C31A C306 C310 123.1(4) . . ? C31A C306 C307 128.7(4) . . ? C310 C306 C307 106.9(3) . . ? C310 C306 C31B 127.8(3) . . ? C307 C306 C31B 124.2(4) . . ? C31A C306 Fe3 136.9(3) . . ? C310 C306 Fe3 69.41(16) . . ? C307 C306 Fe3 69.02(17) . . ? C31B C306 Fe3 117.3(3) . . ? C308 C307 C306 108.2(3) . . ? C308 C307 Fe3 69.56(16) . . ? C306 C307 Fe3 70.11(16) . . ? C308 C307 H307 125.9 . . ? C306 C307 H307 125.9 . . ? Fe3 C307 H307 126.0 . . ? C307 C308 C309 108.3(3) . . ? C307 C308 Fe3 69.89(16) . . ? C309 C308 Fe3 69.73(16) . . ? C307 C308 H308 125.8 . . ? C309 C308 H308 125.8 . . ? Fe3 C308 H308 126.1 . . ? C310 C309 C308 107.7(3) . . ? C310 C309 Fe3 70.11(16) . . ? C308 C309 Fe3 69.52(16) . . ? C310 C309 H309 126.2 . . ? C308 C309 H309 126.2 . . ? Fe3 C309 H309 125.8 . . ? C309 C310 C306 108.9(3) . . ? C309 C310 Fe3 69.49(17) . . ? C306 C310 Fe3 70.02(17) . . ? C309 C310 H310 125.5 . . ? C306 C310 H310 125.5 . . ? Fe3 C310 H310 126.5 . . ? C306 C31A O3A 107.3(5) . . ? C306 C31A H31A 110.2 . . ? O3A C31A H31A 110.2 . . ? C306 C31A H31B 110.2 . . ? O3A C31A H31B 110.2 . . ? H31A C31A H31B 108.5 . . ? O3B C31B C306 110.1(5) . . ? O3B C31B H31C 109.6 . . ? C306 C31B H31C 109.6 . . ? O3B C31B H31D 109.6 . . ? C306 C31B H31D 109.6 . . ? H31C C31B H31D 108.2 . . ? C313 C312 C317 119.6(2) . . ? C313 C312 P3 120.7(2) . . ? C317 C312 P3 119.7(2) . . ? C314 C313 C312 119.8(3) . . ? C314 C313 H313 120.1 . . ? C312 C313 H313 120.1 . . ? C313 C314 C315 120.1(3) . . ? C313 C314 H314 120.0 . . ? C315 C314 H314 120.0 . . ? C316 C315 C314 120.7(3) . . ? C316 C315 H315 119.7 . . ? C314 C315 H315 119.7 . . ? C315 C316 C317 119.3(3) . . ? C315 C316 H316 120.3 . . ? C317 C316 H316 120.3 . . ? C316 C317 C312 120.6(3) . . ? C316 C317 H317 119.7 . . ? C312 C317 H317 119.7 . . ? C319 C318 C323 119.3(3) . . ? C319 C318 P3 122.4(2) . . ? C323 C318 P3 118.3(2) . . ? C320 C319 C318 120.5(3) . . ? C320 C319 H319 119.8 . . ? C318 C319 H319 119.8 . . ? C319 C320 C321 119.7(3) . . ? C319 C320 H320 120.1 . . ? C321 C320 H320 120.1 . . ? C322 C321 C320 120.5(3) . . ? C322 C321 H321 119.7 . . ? C320 C321 H321 119.7 . . ? C321 C322 C323 119.9(3) . . ? C321 C322 H322 120.0 . . ? C323 C322 H322 120.0 . . ? C322 C323 C318 120.1(3) . . ? C322 C323 H323 120.0 . . ? C318 C323 H323 120.0 . . ? C401 Fe4 C405 41.46(11) . . ? C401 Fe4 C402 41.49(10) . . ? C405 Fe4 C402 69.38(11) . . ? C401 Fe4 C408 155.03(11) . . ? C405 Fe4 C408 118.39(11) . . ? C402 Fe4 C408 160.82(11) . . ? C401 Fe4 C409 121.08(11) . . ? C405 Fe4 C409 106.44(11) . . ? C402 Fe4 C409 157.91(11) . . ? C408 Fe4 C409 40.58(11) . . ? C401 Fe4 C407 163.30(11) . . ? C405 Fe4 C407 153.66(11) . . ? C402 Fe4 C407 125.04(11) . . ? C408 Fe4 C407 40.84(11) . . ? C409 Fe4 C407 68.40(11) . . ? C401 Fe4 C403 68.87(11) . . ? C405 Fe4 C403 68.55(11) . . ? C402 Fe4 C403 40.44(11) . . ? C408 Fe4 C403 123.27(12) . . ? C409 Fe4 C403 159.94(12) . . ? C407 Fe4 C403 106.99(11) . . ? C401 Fe4 C410 109.13(11) . . ? C405 Fe4 C410 125.58(11) . . ? C402 Fe4 C410 123.30(11) . . ? C408 Fe4 C410 68.23(11) . . ? C409 Fe4 C410 40.51(11) . . ? C407 Fe4 C410 68.21(11) . . ? C403 Fe4 C410 157.76(12) . . ? C401 Fe4 C404 68.96(11) . . ? C405 Fe4 C404 40.55(11) . . ? C402 Fe4 C404 68.59(11) . . ? C408 Fe4 C404 105.14(12) . . ? C409 Fe4 C404 123.13(12) . . ? C407 Fe4 C404 119.14(11) . . ? C403 Fe4 C404 40.62(11) . . ? C410 Fe4 C404 161.07(11) . . ? C401 Fe4 C406 126.42(11) . . ? C405 Fe4 C406 163.45(11) . . ? C402 Fe4 C406 108.91(11) . . ? C408 Fe4 C406 68.82(11) . . ? C409 Fe4 C406 68.61(11) . . ? C407 Fe4 C406 40.85(10) . . ? C403 Fe4 C406 121.53(11) . . ? C410 Fe4 C406 40.64(10) . . ? C404 Fe4 C406 155.43(11) . . ? C401 P4 C418 105.28(13) . . ? C401 P4 C412 106.43(12) . . ? C418 P4 C412 103.92(12) . . ? C401 P4 B4 114.14(14) . . ? C418 P4 B4 110.44(13) . . ? C412 P4 B4 115.66(14) . . ? C411 O4 H94 111.8 . . ? P4 B4 H10B 101.7 . . ? P4 B4 H11B 108.3 . . ? H10B B4 H11B 118.1 . . ? P4 B4 H12B 105.6 . . ? H10B B4 H12B 107.9 . . ? H11B B4 H12B 113.9 . . ? C405 C401 C402 107.2(2) . . ? C405 C401 P4 124.7(2) . . ? C402 C401 P4 128.0(2) . . ? C405 C401 Fe4 69.39(15) . . ? C402 C401 Fe4 69.66(15) . . ? P4 C401 Fe4 127.40(14) . . ? C403 C402 C401 107.9(2) . . ? C403 C402 Fe4 70.33(16) . . ? C401 C402 Fe4 68.85(15) . . ? C403 C402 H402 126.1 . . ? C401 C402 H402 126.1 . . ? Fe4 C402 H402 126.3 . . ? C402 C403 C404 108.6(3) . . ? C402 C403 Fe4 69.24(16) . . ? C404 C403 Fe4 69.78(16) . . ? C402 C403 H403 125.7 . . ? C404 C403 H403 125.7 . . ? Fe4 C403 H403 126.9 . . ? C405 C404 C403 108.0(3) . . ? C405 C404 Fe4 68.80(16) . . ? C403 C404 Fe4 69.60(16) . . ? C405 C404 H404 126.0 . . ? C403 C404 H404 126.0 . . ? Fe4 C404 H404 127.2 . . ? C404 C405 C401 108.2(2) . . ? C404 C405 Fe4 70.65(16) . . ? C401 C405 Fe4 69.15(15) . . ? C404 C405 H405 125.9 . . ? C401 C405 H405 125.9 . . ? Fe4 C405 H405 125.9 . . ? C410 C406 C407 106.9(2) . . ? C410 C406 C411 126.3(3) . . ? C407 C406 C411 126.8(2) . . ? C410 C406 Fe4 69.54(15) . . ? C407 C406 Fe4 69.04(15) . . ? C411 C406 Fe4 126.70(19) . . ? C408 C407 C406 108.4(2) . . ? C408 C407 Fe4 69.45(15) . . ? C406 C407 Fe4 70.11(15) . . ? C408 C407 H407 125.8 . . ? C406 C407 H407 125.8 . . ? Fe4 C407 H407 126.2 . . ? C409 C408 C407 107.9(2) . . ? C409 C408 Fe4 69.84(16) . . ? C407 C408 Fe4 69.70(15) . . ? C409 C408 H408 126.0 . . ? C407 C408 H408 126.0 . . ? Fe4 C408 H408 126.0 . . ? C408 C409 C410 108.2(2) . . ? C408 C409 Fe4 69.59(16) . . ? C410 C409 Fe4 70.14(16) . . ? C408 C409 H409 125.9 . . ? C410 C409 H409 125.9 . . ? Fe4 C409 H409 126.0 . . ? C409 C410 C406 108.6(2) . . ? C409 C410 Fe4 69.34(16) . . ? C406 C410 Fe4 69.82(15) . . ? C409 C410 H410 125.7 . . ? C406 C410 H410 125.7 . . ? Fe4 C410 H410 126.7 . . ? O4 C411 C406 108.6(2) . . ? O4 C411 H41A 110.0 . . ? C406 C411 H41A 110.0 . . ? O4 C411 H41B 110.0 . . ? C406 C411 H41B 110.0 . . ? H41A C411 H41B 108.4 . . ? C413 C412 C417 119.7(3) . . ? C413 C412 P4 119.9(2) . . ? C417 C412 P4 120.4(2) . . ? C412 C413 C414 119.7(3) . . ? C412 C413 H413 120.2 . . ? C414 C413 H413 120.2 . . ? C415 C414 C413 120.5(3) . . ? C415 C414 H414 119.8 . . ? C413 C414 H414 119.8 . . ? C414 C415 C416 120.1(3) . . ? C414 C415 H415 119.9 . . ? C416 C415 H415 119.9 . . ? C417 C416 C415 119.8(3) . . ? C417 C416 H416 120.1 . . ? C415 C416 H416 120.1 . . ? C416 C417 C412 120.3(3) . . ? C416 C417 H417 119.9 . . ? C412 C417 H417 119.9 . . ? C423 C418 C419 119.4(3) . . ? C423 C418 P4 122.3(2) . . ? C419 C418 P4 118.3(2) . . ? C420 C419 C418 120.0(3) . . ? C420 C419 H419 120.0 . . ? C418 C419 H419 120.0 . . ? C419 C420 C421 120.0(3) . . ? C419 C420 H420 120.0 . . ? C421 C420 H420 120.0 . . ? C422 C421 C420 120.0(3) . . ? C422 C421 H421 120.0 . . ? C420 C421 H421 120.0 . . ? C421 C422 C423 120.2(3) . . ? C421 C422 H422 119.9 . . ? C423 C422 H422 119.9 . . ? C422 C423 C418 120.4(3) . . ? C422 C423 H423 119.8 . . ? C418 C423 H423 119.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.711 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.083 data_ps256 _database_code_depnum_ccdc_archive 'CCDC 906407' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(Sp)-2-(diphenylphosphino)ferrocenyl]methanol--borane (1/1) ; _chemical_formula_moiety 'C23 H24 B Fe O P' _chemical_formula_sum 'C23 H24 B Fe O P' _chemical_formula_weight 414.05 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.7423(2) _cell_length_b 9.3366(3) _cell_length_c 24.9336(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2035.16(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2333 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description bar _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 19003 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 26.01 _reflns_number_total 4010 _reflns_number_gt 3619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'PLATON (Spek, 2007)' _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^)+(0.0267P)^2^+1.0791P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom + difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(16) _chemical_absolute_configuration rmad _refine_ls_number_reflns 4010 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Fe Fe 0.96161(4) 0.63010(4) 0.904768(15) 0.02688(10) Uani 1 1 d . . . P P 0.86795(8) 0.27344(7) 0.87398(3) 0.02445(16) Uani 1 1 d . . . O O 0.4963(2) 0.4586(2) 0.89328(8) 0.0426(5) Uani 1 1 d . . . H91 H 0.5051 0.3635 0.9051 0.051 Uiso 1 1 d R . . B B 0.7742(4) 0.1937(4) 0.93739(13) 0.0342(8) Uani 1 1 d . . . H1B H 0.7936 0.0811 0.9286 0.041 Uiso 1 1 d R . . H2B H 0.8500 0.2448 0.9675 0.041 Uiso 1 1 d R . . H3B H 0.6557 0.2403 0.9437 0.041 Uiso 1 1 d R . . C1 C 0.7487(3) 0.5617(3) 0.88355(11) 0.0283(6) Uani 1 1 d . . . C2 C 0.8648(3) 0.4634(3) 0.86479(10) 0.0248(5) Uani 1 1 d . . . C3 C 0.9652(4) 0.5431(3) 0.83016(10) 0.0309(6) Uani 1 1 d . . . H3 H 1.0502 0.5068 0.8124 0.037 Uiso 1 1 calc R . . C4 C 0.9128(3) 0.6856(3) 0.82782(11) 0.0345(7) Uani 1 1 d . . . H4 H 0.9575 0.7596 0.8084 0.041 Uiso 1 1 calc R . . C5 C 0.7796(3) 0.6967(3) 0.86039(11) 0.0328(7) Uani 1 1 d . . . H5 H 0.7222 0.7794 0.8656 0.039 Uiso 1 1 calc R . . C6 C 0.9663(4) 0.6585(4) 0.98587(11) 0.0439(8) Uani 1 1 d . . . H6 H 0.8858 0.6416 1.0094 0.053 Uiso 1 1 calc R . . C7 C 1.0768(4) 0.5586(4) 0.97085(12) 0.0431(8) Uani 1 1 d . . . H7 H 1.0826 0.4640 0.9823 0.052 Uiso 1 1 calc R . . C8 C 1.1772(3) 0.6265(5) 0.93534(13) 0.0527(9) Uani 1 1 d . . . H8 H 1.2622 0.5849 0.9192 0.063 Uiso 1 1 calc R . . C9 C 1.1283(5) 0.7673(4) 0.92831(14) 0.0592(10) Uani 1 1 d . . . H9 H 1.1747 0.8357 0.9066 0.071 Uiso 1 1 calc R . . C10 C 0.9960(4) 0.7881(4) 0.95982(14) 0.0544(10) Uani 1 1 d . . . H10 H 0.9393 0.8720 0.9627 0.065 Uiso 1 1 calc R . . C11 C 0.6187(3) 0.5302(3) 0.92089(11) 0.0335(6) Uani 1 1 d . . . H11A H 0.6547 0.4703 0.9501 0.040 Uiso 1 1 calc R . . H11B H 0.5811 0.6190 0.9361 0.040 Uiso 1 1 calc R . . C12 C 0.7767(3) 0.2052(3) 0.81331(11) 0.0267(6) Uani 1 1 d . . . C13 C 0.7139(3) 0.2925(3) 0.77452(12) 0.0372(7) Uani 1 1 d . . . H13 H 0.7180 0.3915 0.7784 0.045 Uiso 1 1 calc R . . C14 C 0.6448(4) 0.2330(4) 0.72970(13) 0.0465(8) Uani 1 1 d . . . H14 H 0.6053 0.2924 0.7032 0.056 Uiso 1 1 calc R . . C15 C 0.6342(3) 0.0864(4) 0.72422(12) 0.0430(8) Uani 1 1 d . . . H15 H 0.5855 0.0469 0.6945 0.052 Uiso 1 1 calc R . . C16 C 0.6960(3) -0.0005(3) 0.76283(13) 0.0399(8) Uani 1 1 d . . . H16 H 0.6897 -0.0994 0.7591 0.048 Uiso 1 1 calc R . . C17 C 0.7674(3) 0.0573(3) 0.80716(12) 0.0336(7) Uani 1 1 d . . . H17 H 0.8095 -0.0028 0.8330 0.040 Uiso 1 1 calc R . . C18 C 1.0655(3) 0.2151(3) 0.86816(11) 0.0272(6) Uani 1 1 d . . . C19 C 1.1331(3) 0.1897(3) 0.81857(12) 0.0349(7) Uani 1 1 d . . . H19 H 1.0774 0.2056 0.7874 0.042 Uiso 1 1 calc R . . C20 C 1.2831(3) 0.1406(4) 0.81506(12) 0.0406(7) Uani 1 1 d . . . H20 H 1.3273 0.1235 0.7817 0.049 Uiso 1 1 calc R . . C21 C 1.3658(3) 0.1177(3) 0.86138(13) 0.0415(7) Uani 1 1 d . . . H21 H 1.4662 0.0851 0.8592 0.050 Uiso 1 1 calc R . . C22 C 1.3010(3) 0.1424(3) 0.91092(13) 0.0407(7) Uani 1 1 d . . . H22 H 1.3576 0.1264 0.9419 0.049 Uiso 1 1 calc R . . C23 C 1.1505(3) 0.1915(3) 0.91455(12) 0.0331(6) Uani 1 1 d . . . H23 H 1.1070 0.2085 0.9480 0.040 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 Fe 0.02867(18) 0.02484(19) 0.02714(18) -0.00333(17) -0.00255(17) -0.00007(17) P 0.0247(3) 0.0246(4) 0.0240(3) 0.0000(3) 0.0010(3) 0.0013(3) O 0.0311(11) 0.0425(12) 0.0541(13) 0.0073(10) -0.0042(9) -0.0022(8) B 0.0346(17) 0.0363(19) 0.0317(18) 0.0058(15) 0.0059(15) 0.0025(15) C1 0.0266(13) 0.0290(15) 0.0291(14) -0.0048(12) -0.0075(11) 0.0034(11) C2 0.0280(13) 0.0240(13) 0.0225(13) -0.0020(11) 0.0000(11) 0.0000(12) C3 0.0357(14) 0.0329(15) 0.0242(13) -0.0019(11) 0.0046(13) -0.0009(14) C4 0.0462(18) 0.0301(16) 0.0271(14) 0.0054(12) -0.0010(12) -0.0053(13) C5 0.0381(16) 0.0272(15) 0.0331(16) 0.0016(12) -0.0077(13) 0.0049(13) C6 0.0469(16) 0.059(2) 0.0258(14) -0.0129(14) -0.0059(14) 0.0072(18) C7 0.049(2) 0.0374(17) 0.0434(18) -0.0011(14) -0.0184(14) 0.0052(15) C8 0.0279(15) 0.077(3) 0.053(2) -0.022(2) -0.0120(14) 0.0048(18) C9 0.068(2) 0.055(2) 0.054(2) 0.0007(18) -0.020(2) -0.033(2) C10 0.075(3) 0.0343(18) 0.054(2) -0.0179(16) -0.0275(19) 0.0088(17) C11 0.0301(14) 0.0341(15) 0.0363(16) -0.0027(12) 0.0010(12) 0.0036(13) C12 0.0237(13) 0.0289(16) 0.0276(14) -0.0029(12) 0.0023(11) -0.0031(12) C13 0.0440(16) 0.0325(16) 0.0350(16) -0.0028(14) -0.0094(14) 0.0030(14) C14 0.0461(18) 0.055(2) 0.0380(17) -0.0047(16) -0.0130(15) 0.0051(17) C15 0.0307(15) 0.060(2) 0.0388(17) -0.0205(15) -0.0020(14) -0.0039(15) C16 0.0356(16) 0.0355(18) 0.0486(19) -0.0167(15) 0.0075(14) -0.0086(13) C17 0.0344(16) 0.0270(16) 0.0394(17) -0.0011(13) 0.0036(13) -0.0034(13) C18 0.0250(13) 0.0255(13) 0.0311(14) 0.0014(12) 0.0027(11) -0.0013(11) C19 0.0329(14) 0.0393(17) 0.0326(15) 0.0003(13) 0.0038(13) -0.0015(14) C20 0.0353(15) 0.0429(18) 0.0436(17) -0.0020(16) 0.0132(13) -0.0003(15) C21 0.0258(13) 0.0371(17) 0.062(2) -0.0097(16) -0.0001(14) 0.0016(15) C22 0.0306(13) 0.0411(17) 0.0503(18) 0.0007(17) -0.0087(14) 0.0062(14) C23 0.0333(14) 0.0344(15) 0.0317(16) -0.0037(12) -0.0018(13) 0.0021(12) _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 Fe C9 2.027(3) . ? Fe C3 2.030(3) . ? Fe C4 2.032(3) . ? Fe C2 2.033(3) . ? Fe C8 2.034(3) . ? Fe C5 2.036(3) . ? Fe C10 2.037(3) . ? Fe C1 2.038(3) . ? Fe C6 2.040(3) . ? Fe C7 2.043(3) . ? P C2 1.788(3) . ? P C18 1.817(3) . ? P C12 1.825(3) . ? P B 1.930(3) . ? O C11 1.437(3) . ? O H91 0.9388 . ? B H1B 1.0874 . ? B H2B 1.1098 . ? B H3B 1.1342 . ? C1 C5 1.413(4) . ? C1 C2 1.446(4) . ? C1 C11 1.498(4) . ? C2 C3 1.439(4) . ? C3 C4 1.408(4) . ? C3 H3 0.9300 . ? C4 C5 1.424(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.394(4) . ? C6 C10 1.398(5) . ? C6 H6 0.9300 . ? C7 C8 1.399(5) . ? C7 H7 0.9300 . ? C8 C9 1.393(5) . ? C8 H8 0.9300 . ? C9 C10 1.412(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.379(4) . ? C12 C17 1.392(4) . ? C13 C14 1.387(4) . ? C13 H13 0.9300 . ? C14 C15 1.378(5) . ? C14 H14 0.9300 . ? C15 C16 1.370(5) . ? C15 H15 0.9300 . ? C16 C17 1.379(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.391(4) . ? C18 C23 1.393(4) . ? C19 C20 1.392(4) . ? C19 H19 0.9300 . ? C20 C21 1.379(4) . ? C20 H20 0.9300 . ? C21 C22 1.378(4) . ? C21 H21 0.9300 . ? C22 C23 1.396(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? 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 C9 Fe C3 120.47(14) . . ? C9 Fe C4 105.26(13) . . ? C3 Fe C4 40.54(11) . . ? C9 Fe C2 157.69(14) . . ? C3 Fe C2 41.48(11) . . ? C4 Fe C2 69.20(11) . . ? C9 Fe C8 40.13(16) . . ? C3 Fe C8 108.82(13) . . ? C4 Fe C8 123.53(14) . . ? C2 Fe C8 123.86(14) . . ? C9 Fe C5 121.77(14) . . ? C3 Fe C5 68.65(12) . . ? C4 Fe C5 40.98(12) . . ? C2 Fe C5 69.00(11) . . ? C8 Fe C5 158.98(15) . . ? C9 Fe C10 40.66(15) . . ? C3 Fe C10 154.80(14) . . ? C4 Fe C10 118.85(13) . . ? C2 Fe C10 161.11(14) . . ? C8 Fe C10 67.83(14) . . ? C5 Fe C10 105.10(13) . . ? C9 Fe C1 158.43(14) . . ? C3 Fe C1 69.56(12) . . ? C4 Fe C1 69.10(11) . . ? C2 Fe C1 41.61(11) . . ? C8 Fe C1 159.86(15) . . ? C5 Fe C1 40.58(11) . . ? C10 Fe C1 122.45(13) . . ? C9 Fe C6 67.44(14) . . ? C3 Fe C6 163.76(12) . . ? C4 Fe C6 155.08(12) . . ? C2 Fe C6 126.43(13) . . ? C8 Fe C6 67.16(13) . . ? C5 Fe C6 121.00(13) . . ? C10 Fe C6 40.09(14) . . ? C1 Fe C6 108.45(13) . . ? C9 Fe C7 67.59(14) . . ? C3 Fe C7 126.92(13) . . ? C4 Fe C7 161.42(13) . . ? C2 Fe C7 110.51(12) . . ? C8 Fe C7 40.15(13) . . ? C5 Fe C7 157.44(12) . . ? C10 Fe C7 67.70(13) . . ? C1 Fe C7 123.84(13) . . ? C6 Fe C7 39.92(12) . . ? C2 P C18 107.54(13) . . ? C2 P C12 103.50(13) . . ? C18 P C12 104.16(12) . . ? C2 P B 118.74(14) . . ? C18 P B 110.71(13) . . ? C12 P B 111.02(14) . . ? C11 O H91 103.1 . . ? P B H1B 98.2 . . ? P B H2B 97.8 . . ? H1B B H2B 117.3 . . ? P B H3B 110.7 . . ? H1B B H3B 122.8 . . ? H2B B H3B 106.6 . . ? C5 C1 C2 107.4(2) . . ? C5 C1 C11 125.0(2) . . ? C2 C1 C11 127.5(2) . . ? C5 C1 Fe 69.62(16) . . ? C2 C1 Fe 69.01(15) . . ? C11 C1 Fe 126.38(19) . . ? C3 C2 C1 107.1(2) . . ? C3 C2 P 125.5(2) . . ? C1 C2 P 126.8(2) . . ? C3 C2 Fe 69.15(15) . . ? C1 C2 Fe 69.38(15) . . ? P C2 Fe 133.64(15) . . ? C4 C3 C2 108.4(3) . . ? C4 C3 Fe 69.82(16) . . ? C2 C3 Fe 69.37(14) . . ? C4 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? Fe C3 H3 126.6 . . ? C3 C4 C5 108.1(3) . . ? C3 C4 Fe 69.63(16) . . ? C5 C4 Fe 69.63(15) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe C4 H4 126.4 . . ? C1 C5 C4 108.9(2) . . ? C1 C5 Fe 69.80(16) . . ? C4 C5 Fe 69.39(16) . . ? C1 C5 H5 125.5 . . ? C4 C5 H5 125.5 . . ? Fe C5 H5 126.9 . . ? C7 C6 C10 109.0(3) . . ? C7 C6 Fe 70.16(17) . . ? C10 C6 Fe 69.84(17) . . ? C7 C6 H6 125.5 . . ? C10 C6 H6 125.5 . . ? Fe C6 H6 126.1 . . ? C6 C7 C8 107.5(3) . . ? C6 C7 Fe 69.92(17) . . ? C8 C7 Fe 69.56(17) . . ? C6 C7 H7 126.2 . . ? C8 C7 H7 126.2 . . ? Fe C7 H7 125.9 . . ? C9 C8 C7 108.3(3) . . ? C9 C8 Fe 69.68(19) . . ? C7 C8 Fe 70.29(17) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe C8 H8 125.8 . . ? C8 C9 C10 108.1(3) . . ? C8 C9 Fe 70.19(18) . . ? C10 C9 Fe 70.05(19) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe C9 H9 125.4 . . ? C6 C10 C9 107.0(3) . . ? C6 C10 Fe 70.07(17) . . ? C9 C10 Fe 69.29(18) . . ? C6 C10 H10 126.5 . . ? C9 C10 H10 126.5 . . ? Fe C10 H10 125.7 . . ? O C11 C1 111.0(2) . . ? O C11 H11A 109.4 . . ? C1 C11 H11A 109.4 . . ? O C11 H11B 109.4 . . ? C1 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C17 119.1(3) . . ? C13 C12 P 123.3(2) . . ? C17 C12 P 117.6(2) . . ? C12 C13 C14 120.1(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 119.5(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 120.2(3) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C19 C18 C23 119.0(2) . . ? C19 C18 P 121.8(2) . . ? C23 C18 P 119.3(2) . . ? C18 C19 C20 120.8(3) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 119.5(3) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 120.1(3) . . ? C18 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.401 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.047 data_ps424 _database_code_depnum_ccdc_archive 'CCDC 906408' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H24 B Fe P' _chemical_formula_sum 'C23 H24 B Fe P' _chemical_formula_weight 398.05 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' 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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3300(8) _cell_length_b 17.5284(10) _cell_length_c 34.422(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.118(2) _cell_angle_gamma 90.00 _cell_volume 7917.7(8) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9029 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 26.99 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49847 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.00 _reflns_number_total 17266 _reflns_number_gt 10336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0406P)^2^+1.8174P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17266 _refine_ls_number_parameters 941 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1042 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.50800(3) 0.16123(2) 0.202993(10) 0.01918(9) Uani 1 1 d . . . P1 P 0.41407(5) -0.02058(4) 0.191639(19) 0.01769(15) Uani 1 1 d . . . B1 B 0.4967(2) -0.05558(18) 0.15498(9) 0.0265(7) Uani 1 1 d . . . H1A H 0.4882 -0.1178 0.1539 0.032 Uiso 1 1 d R . . H1B H 0.5756 -0.0364 0.1637 0.032 Uiso 1 1 d R . . H1C H 0.4584 -0.0264 0.1277 0.032 Uiso 1 1 d R . . C101 C 0.39739(18) 0.08024(15) 0.19277(7) 0.0179(6) Uani 1 1 d . . . C102 C 0.38433(18) 0.12758(15) 0.22593(8) 0.0235(6) Uani 1 1 d . . . H102 H 0.3846 0.1105 0.2521 0.028 Uiso 1 1 calc R . . C103 C 0.37100(19) 0.20413(16) 0.21249(8) 0.0291(7) Uani 1 1 d . . . H103 H 0.3610 0.2471 0.2282 0.035 Uiso 1 1 calc R . . C104 C 0.37529(19) 0.20535(16) 0.17158(8) 0.0297(7) Uani 1 1 d . . . H104 H 0.3681 0.2493 0.1552 0.036 Uiso 1 1 calc R . . C105 C 0.39209(19) 0.12979(15) 0.15922(8) 0.0241(6) Uani 1 1 d . . . H105 H 0.3987 0.1147 0.1333 0.029 Uiso 1 1 calc R . . C106 C 0.63273(19) 0.16136(16) 0.24777(8) 0.0274(6) Uani 1 1 d . . . C107 C 0.61867(19) 0.23444(16) 0.22953(8) 0.0287(7) Uani 1 1 d . . . H107 H 0.6079 0.2809 0.2424 0.034 Uiso 1 1 calc R . . C108 C 0.6234(2) 0.22618(17) 0.18905(8) 0.0306(7) Uani 1 1 d . . . H108 H 0.6165 0.2661 0.1701 0.037 Uiso 1 1 calc R . . C109 C 0.6399(2) 0.14834(17) 0.18153(8) 0.0307(7) Uani 1 1 d . . . H109 H 0.6455 0.1266 0.1567 0.037 Uiso 1 1 calc R . . C110 C 0.64672(19) 0.10851(16) 0.21780(8) 0.0276(6) Uani 1 1 d . . . H110 H 0.6586 0.0553 0.2215 0.033 Uiso 1 1 calc R . . C111 C 0.6364(2) 0.14274(19) 0.29039(8) 0.0453(8) Uani 1 1 d . . . H11A H 0.6156 0.0896 0.2929 0.068 Uiso 1 1 calc R . . H11B H 0.5900 0.1766 0.3014 0.068 Uiso 1 1 calc R . . H11C H 0.7060 0.1499 0.3048 0.068 Uiso 1 1 calc R . . C112 C 0.45589(18) -0.04951(14) 0.24236(7) 0.0190(5) Uani 1 1 d . . . C113 C 0.38759(19) -0.04868(15) 0.26886(7) 0.0235(6) Uani 1 1 d . . . H113 H 0.3189 -0.0336 0.2601 0.028 Uiso 1 1 calc R . . C114 C 0.4194(2) -0.06970(15) 0.30780(7) 0.0276(6) Uani 1 1 d . . . H114 H 0.3726 -0.0690 0.3257 0.033 Uiso 1 1 calc R . . C115 C 0.5195(2) -0.09174(15) 0.32074(8) 0.0292(7) Uani 1 1 d . . . H115 H 0.5415 -0.1057 0.3476 0.035 Uiso 1 1 calc R . . C116 C 0.5877(2) -0.09345(15) 0.29457(8) 0.0277(6) Uani 1 1 d . . . H116 H 0.6562 -0.1088 0.3035 0.033 Uiso 1 1 calc R . . C117 C 0.55581(19) -0.07279(14) 0.25541(7) 0.0231(6) Uani 1 1 d . . . H117 H 0.6024 -0.0746 0.2375 0.028 Uiso 1 1 calc R . . C118 C 0.28612(19) -0.05984(15) 0.18004(7) 0.0195(6) Uani 1 1 d . . . C119 C 0.20036(19) -0.01383(15) 0.17164(7) 0.0224(6) Uani 1 1 d . . . H119 H 0.2079 0.0401 0.1716 0.027 Uiso 1 1 calc R . . C120 C 0.1035(2) -0.04576(16) 0.16325(7) 0.0270(6) Uani 1 1 d . . . H120 H 0.0451 -0.0139 0.1573 0.032 Uiso 1 1 calc R . . C121 C 0.0926(2) -0.12429(16) 0.16360(8) 0.0301(7) Uani 1 1 d . . . H121 H 0.0264 -0.1463 0.1581 0.036 Uiso 1 1 calc R . . C122 C 0.1773(2) -0.17103(16) 0.17195(8) 0.0327(7) Uani 1 1 d . . . H122 H 0.1695 -0.2249 0.1721 0.039 Uiso 1 1 calc R . . C123 C 0.2738(2) -0.13859(16) 0.18015(8) 0.0279(7) Uani 1 1 d . . . H123 H 0.3321 -0.1706 0.1859 0.033 Uiso 1 1 calc R . . Fe2 Fe 1.01439(3) 0.43945(2) 0.203389(11) 0.02165(9) Uani 1 1 d . . . P2 P 0.91866(5) 0.62092(4) 0.194991(19) 0.01797(15) Uani 1 1 d . . . B2 B 1.0018(2) 0.65805(19) 0.15877(9) 0.0278(7) Uani 1 1 d . . . H2A H 1.0793 0.6419 0.1673 0.033 Uiso 1 1 d R . . H2B H 0.9891 0.7205 0.1584 0.033 Uiso 1 1 d R . . H2C H 0.9646 0.6309 0.1272 0.033 Uiso 1 1 d R . . C201 C 0.90305(19) 0.51990(16) 0.19501(8) 0.0226(6) Uani 1 1 d . . . C202 C 0.89108(19) 0.47124(15) 0.22724(8) 0.0250(6) Uani 1 1 d . . . H202 H 0.8915 0.4869 0.2537 0.030 Uiso 1 1 calc R . . C203 C 0.8783(2) 0.39484(16) 0.21268(9) 0.0345(7) Uani 1 1 d . . . H203 H 0.8690 0.3509 0.2278 0.041 Uiso 1 1 calc R . . C204 C 0.8819(2) 0.39587(17) 0.17173(9) 0.0356(8) Uani 1 1 d . . . H204 H 0.8750 0.3528 0.1547 0.043 Uiso 1 1 calc R . . C205 C 0.89777(19) 0.47278(16) 0.16050(8) 0.0285(7) Uani 1 1 d . . . H205 H 0.9038 0.4898 0.1348 0.034 Uiso 1 1 calc R . . C206 C 1.1396(2) 0.43600(17) 0.24790(8) 0.0300(7) Uani 1 1 d . . . C207 C 1.1251(2) 0.36440(17) 0.22770(8) 0.0312(7) Uani 1 1 d . . . H207 H 1.1143 0.3166 0.2393 0.037 Uiso 1 1 calc R . . C208 C 1.1297(2) 0.37734(17) 0.18752(8) 0.0333(7) Uani 1 1 d . . . H208 H 1.1228 0.3395 0.1674 0.040 Uiso 1 1 calc R . . C209 C 1.1462(2) 0.45602(17) 0.18227(9) 0.0325(7) Uani 1 1 d . . . H209 H 1.1518 0.4804 0.1581 0.039 Uiso 1 1 calc R . . C210 C 1.15300(18) 0.49200(17) 0.21928(8) 0.0279(6) Uani 1 1 d . . . H210 H 1.1646 0.5449 0.2243 0.033 Uiso 1 1 calc R . . C211 C 1.1437(2) 0.4514(2) 0.29084(9) 0.0468(9) Uani 1 1 d . . . H21A H 1.2142 0.4471 0.3047 0.070 Uiso 1 1 calc R . . H21B H 1.1012 0.4142 0.3017 0.070 Uiso 1 1 calc R . . H21C H 1.1184 0.5030 0.2943 0.070 Uiso 1 1 calc R . . C212 C 0.95975(18) 0.64857(14) 0.24599(7) 0.0199(6) Uani 1 1 d . . . C213 C 0.8922(2) 0.64778(15) 0.27254(7) 0.0257(6) Uani 1 1 d . . . H213 H 0.8231 0.6339 0.2637 0.031 Uiso 1 1 calc R . . C214 C 0.9247(2) 0.66697(15) 0.31184(8) 0.0311(7) Uani 1 1 d . . . H214 H 0.8780 0.6665 0.3298 0.037 Uiso 1 1 calc R . . C215 C 1.0255(2) 0.68677(16) 0.32479(8) 0.0352(7) Uani 1 1 d . . . H215 H 1.0484 0.6991 0.3518 0.042 Uiso 1 1 calc R . . C216 C 1.0929(2) 0.68859(16) 0.29853(8) 0.0340(7) Uani 1 1 d . . . H216 H 1.1620 0.7023 0.3076 0.041 Uiso 1 1 calc R . . C217 C 1.06064(19) 0.67055(15) 0.25909(8) 0.0252(6) Uani 1 1 d . . . H217 H 1.1070 0.6731 0.2411 0.030 Uiso 1 1 calc R . . C218 C 0.78974(19) 0.65876(15) 0.18230(7) 0.0199(6) Uani 1 1 d . . . C219 C 0.70537(18) 0.61099(16) 0.17263(7) 0.0234(6) Uani 1 1 d . . . H219 H 0.7141 0.5572 0.1734 0.028 Uiso 1 1 calc R . . C220 C 0.6081(2) 0.64210(17) 0.16186(8) 0.0300(7) Uani 1 1 d . . . H220 H 0.5506 0.6097 0.1550 0.036 Uiso 1 1 calc R . . C221 C 0.5959(2) 0.72025(17) 0.16125(8) 0.0325(7) Uani 1 1 d . . . H221 H 0.5296 0.7415 0.1542 0.039 Uiso 1 1 calc R . . C222 C 0.6787(2) 0.76793(17) 0.17072(8) 0.0353(7) Uani 1 1 d . . . H222 H 0.6695 0.8217 0.1701 0.042 Uiso 1 1 calc R . . C223 C 0.7757(2) 0.73738(16) 0.18122(8) 0.0289(7) Uani 1 1 d . . . H223 H 0.8327 0.7703 0.1877 0.035 Uiso 1 1 calc R . . Fe3 Fe 0.74267(3) -0.11129(2) 0.046816(10) 0.01956(9) Uani 1 1 d . . . P3 P 0.83546(5) 0.07110(4) 0.056596(19) 0.01844(15) Uani 1 1 d . . . B3 B 0.7566(2) 0.10620(19) 0.09458(9) 0.0295(8) Uani 1 1 d . . . H3A H 0.7617 0.1749 0.0936 0.035 Uiso 1 1 d R . . H3B H 0.6740 0.0899 0.0852 0.035 Uiso 1 1 d R . . H3C H 0.7956 0.0797 0.1239 0.035 Uiso 1 1 d R . . C301 C 0.85267(19) -0.03011(15) 0.05594(8) 0.0200(6) Uani 1 1 d . . . C302 C 0.86516(18) -0.07775(15) 0.02299(8) 0.0230(6) Uani 1 1 d . . . H302 H 0.8641 -0.0611 -0.0033 0.028 Uiso 1 1 calc R . . C303 C 0.87928(19) -0.15379(16) 0.03684(8) 0.0285(7) Uani 1 1 d . . . H303 H 0.8892 -0.1970 0.0213 0.034 Uiso 1 1 calc R . . C304 C 0.8761(2) -0.15461(15) 0.07778(8) 0.0283(7) Uani 1 1 d . . . H304 H 0.8837 -0.1983 0.0944 0.034 Uiso 1 1 calc R . . C305 C 0.85970(19) -0.07866(15) 0.08971(8) 0.0249(6) Uani 1 1 d . . . H305 H 0.8543 -0.0629 0.1157 0.030 Uiso 1 1 calc R . . C306 C 0.6154(2) -0.11237(16) 0.00303(8) 0.0278(6) Uani 1 1 d . . . C307 C 0.63165(19) -0.18537(16) 0.02146(8) 0.0272(6) Uani 1 1 d . . . H307 H 0.6421 -0.2319 0.0086 0.033 Uiso 1 1 calc R . . C308 C 0.6296(2) -0.17642(17) 0.06207(8) 0.0306(7) Uani 1 1 d . . . H308 H 0.6385 -0.2160 0.0812 0.037 Uiso 1 1 calc R . . C309 C 0.6121(2) -0.09828(17) 0.06946(8) 0.0316(7) Uani 1 1 d . . . H309 H 0.6073 -0.0761 0.0943 0.038 Uiso 1 1 calc R . . C310 C 0.60303(19) -0.05960(16) 0.03294(8) 0.0280(6) Uani 1 1 d . . . H310 H 0.5906 -0.0065 0.0291 0.034 Uiso 1 1 calc R . . C311 C 0.6083(2) -0.09517(19) -0.03988(8) 0.0441(8) Uani 1 1 d . . . H31A H 0.6517 -0.1307 -0.0514 0.066 Uiso 1 1 calc R . . H31B H 0.6311 -0.0427 -0.0431 0.066 Uiso 1 1 calc R . . H31C H 0.5375 -0.1008 -0.0533 0.066 Uiso 1 1 calc R . . C312 C 0.78921(18) 0.09939(14) 0.00590(7) 0.0195(6) Uani 1 1 d . . . C313 C 0.8533(2) 0.09762(15) -0.02212(7) 0.0256(6) Uani 1 1 d . . . H313 H 0.9228 0.0836 -0.0144 0.031 Uiso 1 1 calc R . . C314 C 0.8158(2) 0.11617(16) -0.06109(8) 0.0337(7) Uani 1 1 d . . . H314 H 0.8596 0.1148 -0.0801 0.040 Uiso 1 1 calc R . . C315 C 0.7153(2) 0.13652(16) -0.07229(8) 0.0363(8) Uani 1 1 d . . . H315 H 0.6894 0.1482 -0.0991 0.044 Uiso 1 1 calc R . . C316 C 0.6517(2) 0.14002(16) -0.04467(8) 0.0341(7) Uani 1 1 d . . . H316 H 0.5826 0.1550 -0.0525 0.041 Uiso 1 1 calc R . . C317 C 0.68849(19) 0.12173(15) -0.00558(8) 0.0263(6) Uani 1 1 d . . . H317 H 0.6447 0.1245 0.0134 0.032 Uiso 1 1 calc R . . C318 C 0.96390(19) 0.11037(15) 0.06709(7) 0.0194(6) Uani 1 1 d . . . C319 C 1.04964(19) 0.06407(15) 0.07664(7) 0.0228(6) Uani 1 1 d . . . H319 H 1.0420 0.0102 0.0774 0.027 Uiso 1 1 calc R . . C320 C 1.1463(2) 0.09633(16) 0.08512(8) 0.0279(7) Uani 1 1 d . . . H320 H 1.2046 0.0646 0.0915 0.033 Uiso 1 1 calc R . . C321 C 1.1575(2) 0.17461(17) 0.08422(8) 0.0292(7) Uani 1 1 d . . . H321 H 1.2236 0.1966 0.0900 0.035 Uiso 1 1 calc R . . C322 C 1.0728(2) 0.22128(16) 0.07491(8) 0.0321(7) Uani 1 1 d . . . H322 H 1.0809 0.2751 0.0743 0.039 Uiso 1 1 calc R . . C323 C 0.9756(2) 0.18933(16) 0.06648(8) 0.0279(7) Uani 1 1 d . . . H323 H 0.9175 0.2213 0.0603 0.033 Uiso 1 1 calc R . . Fe4 Fe 0.76283(3) 0.38898(2) -0.047783(11) 0.02304(10) Uani 1 1 d . . . P4 P 0.66690(5) 0.57024(4) -0.057170(19) 0.01777(15) Uani 1 1 d . . . B4 B 0.7521(2) 0.60687(19) -0.09262(9) 0.0270(7) Uani 1 1 d . . . H4A H 0.7157 0.5784 -0.1218 0.032 Uiso 1 1 d R . . H4B H 0.7419 0.6685 -0.0919 0.032 Uiso 1 1 d R . . H4C H 0.8285 0.5884 -0.0817 0.032 Uiso 1 1 d R . . C401 C 0.65142(18) 0.46889(15) -0.05718(8) 0.0199(6) Uani 1 1 d . . . C402 C 0.63878(19) 0.42041(15) -0.02456(8) 0.0263(6) Uani 1 1 d . . . H402 H 0.6385 0.4365 0.0018 0.032 Uiso 1 1 calc R . . C403 C 0.6268(2) 0.34454(17) -0.03879(10) 0.0370(8) Uani 1 1 d . . . H403 H 0.6174 0.3008 -0.0236 0.044 Uiso 1 1 calc R . . C404 C 0.6312(2) 0.34511(17) -0.07943(10) 0.0391(8) Uani 1 1 d . . . H404 H 0.6247 0.3017 -0.0962 0.047 Uiso 1 1 calc R . . C405 C 0.6470(2) 0.42110(16) -0.09124(8) 0.0311(7) Uani 1 1 d . . . H405 H 0.6534 0.4373 -0.1170 0.037 Uiso 1 1 calc R . . C406 C 0.8866(2) 0.38603(17) -0.00283(8) 0.0309(7) Uani 1 1 d . . . C407 C 0.8735(2) 0.31456(17) -0.02246(9) 0.0346(7) Uani 1 1 d . . . H407 H 0.8627 0.2670 -0.0106 0.041 Uiso 1 1 calc R . . C408 C 0.8793(2) 0.32611(18) -0.06268(9) 0.0363(8) Uani 1 1 d . . . H408 H 0.8732 0.2878 -0.0825 0.044 Uiso 1 1 calc R . . C409 C 0.8958(2) 0.40508(18) -0.06827(9) 0.0348(7) Uani 1 1 d . . . H409 H 0.9023 0.4290 -0.0925 0.042 Uiso 1 1 calc R . . C410 C 0.90091(19) 0.44160(17) -0.03140(8) 0.0310(7) Uani 1 1 d . . . H410 H 0.9121 0.4945 -0.0265 0.037 Uiso 1 1 calc R . . C411 C 0.8879(3) 0.4021(2) 0.04025(9) 0.0518(9) Uani 1 1 d . . . H41A H 0.9573 0.3955 0.0550 0.078 Uiso 1 1 calc R . . H41B H 0.8419 0.3667 0.0504 0.078 Uiso 1 1 calc R . . H41C H 0.8654 0.4546 0.0434 0.078 Uiso 1 1 calc R . . C412 C 0.70584(18) 0.59860(14) -0.00613(7) 0.0194(5) Uani 1 1 d . . . C413 C 0.80579(19) 0.62160(14) 0.00768(7) 0.0238(6) Uani 1 1 d . . . H413 H 0.8535 0.6230 -0.0098 0.029 Uiso 1 1 calc R . . C414 C 0.8358(2) 0.64244(16) 0.04684(8) 0.0295(7) Uani 1 1 d . . . H414 H 0.9041 0.6577 0.0562 0.035 Uiso 1 1 calc R . . C415 C 0.7664(2) 0.64103(16) 0.07236(8) 0.0295(7) Uani 1 1 d . . . H415 H 0.7872 0.6552 0.0992 0.035 Uiso 1 1 calc R . . C416 C 0.6663(2) 0.61900(15) 0.05886(8) 0.0291(7) Uani 1 1 d . . . H416 H 0.6186 0.6186 0.0764 0.035 Uiso 1 1 calc R . . C417 C 0.63610(19) 0.59759(15) 0.01981(7) 0.0232(6) Uani 1 1 d . . . H417 H 0.5677 0.5822 0.0106 0.028 Uiso 1 1 calc R . . C418 C 0.53790(19) 0.60819(15) -0.07017(7) 0.0199(6) Uani 1 1 d . . . C419 C 0.5248(2) 0.68719(16) -0.07096(8) 0.0285(7) Uani 1 1 d . . . H419 H 0.5823 0.7198 -0.0647 0.034 Uiso 1 1 calc R . . C420 C 0.4277(2) 0.71822(17) -0.08098(8) 0.0348(7) Uani 1 1 d . . . H420 H 0.4189 0.7720 -0.0815 0.042 Uiso 1 1 calc R . . C421 C 0.3441(2) 0.67090(18) -0.09020(8) 0.0343(7) Uani 1 1 d . . . H421 H 0.2777 0.6922 -0.0970 0.041 Uiso 1 1 calc R . . C422 C 0.3568(2) 0.59272(17) -0.08954(8) 0.0307(7) Uani 1 1 d . . . H422 H 0.2992 0.5602 -0.0960 0.037 Uiso 1 1 calc R . . C423 C 0.45357(19) 0.56150(16) -0.07944(7) 0.0251(6) Uani 1 1 d . . . H423 H 0.4619 0.5077 -0.0789 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01679(19) 0.0205(2) 0.02012(19) -0.00052(16) 0.00296(14) -0.00185(16) P1 0.0153(3) 0.0208(4) 0.0164(3) -0.0002(3) 0.0011(3) 0.0013(3) B1 0.0244(16) 0.0303(19) 0.0260(17) -0.0068(14) 0.0076(13) 0.0019(14) C101 0.0154(13) 0.0190(15) 0.0183(13) 0.0016(11) 0.0001(10) 0.0004(11) C102 0.0192(13) 0.0242(16) 0.0277(15) -0.0029(12) 0.0057(11) -0.0023(12) C103 0.0201(14) 0.0277(17) 0.0403(17) -0.0046(13) 0.0075(12) 0.0007(13) C104 0.0217(15) 0.0237(16) 0.0403(17) 0.0048(13) -0.0038(12) 0.0008(12) C105 0.0221(14) 0.0259(16) 0.0215(14) 0.0031(12) -0.0040(11) -0.0024(12) C106 0.0183(14) 0.0317(17) 0.0307(16) -0.0019(13) 0.0003(11) -0.0053(12) C107 0.0214(14) 0.0281(17) 0.0353(16) -0.0024(13) 0.0014(12) -0.0070(13) C108 0.0230(15) 0.0338(18) 0.0360(17) 0.0030(14) 0.0084(12) -0.0067(13) C109 0.0197(15) 0.0401(19) 0.0350(17) -0.0061(14) 0.0121(12) -0.0026(13) C110 0.0172(14) 0.0271(16) 0.0372(17) -0.0029(13) 0.0015(12) 0.0007(12) C111 0.0426(19) 0.055(2) 0.0344(18) -0.0016(16) -0.0053(14) 0.0006(17) C112 0.0200(13) 0.0171(14) 0.0184(13) -0.0013(10) -0.0005(10) -0.0009(11) C113 0.0210(14) 0.0255(15) 0.0234(14) 0.0002(11) 0.0025(11) 0.0039(12) C114 0.0361(16) 0.0262(16) 0.0216(14) 0.0013(12) 0.0079(12) 0.0023(13) C115 0.0387(17) 0.0264(16) 0.0188(14) 0.0050(12) -0.0051(12) -0.0032(13) C116 0.0214(14) 0.0278(16) 0.0300(15) 0.0019(12) -0.0066(12) 0.0010(12) C117 0.0204(14) 0.0210(15) 0.0274(14) 0.0022(11) 0.0027(11) -0.0010(11) C118 0.0202(13) 0.0224(15) 0.0145(12) 0.0005(11) -0.0004(10) -0.0053(12) C119 0.0217(14) 0.0246(15) 0.0206(13) -0.0002(11) 0.0031(11) -0.0008(12) C120 0.0187(14) 0.0345(17) 0.0267(15) 0.0015(13) 0.0009(11) 0.0014(13) C121 0.0221(15) 0.0361(18) 0.0300(16) 0.0037(13) -0.0012(12) -0.0094(14) C122 0.0340(17) 0.0219(16) 0.0387(17) 0.0012(13) -0.0032(13) -0.0089(14) C123 0.0241(15) 0.0238(16) 0.0323(16) 0.0032(12) -0.0046(12) 0.0015(13) Fe2 0.01816(19) 0.0210(2) 0.0250(2) -0.00176(16) 0.00171(15) 0.00237(17) P2 0.0151(3) 0.0210(4) 0.0172(3) 0.0002(3) 0.0012(3) -0.0004(3) B2 0.0218(16) 0.036(2) 0.0271(17) 0.0079(14) 0.0072(13) -0.0017(15) C201 0.0116(13) 0.0315(17) 0.0242(15) -0.0018(13) 0.0016(11) 0.0021(12) C202 0.0171(13) 0.0248(16) 0.0342(16) 0.0009(12) 0.0071(11) -0.0005(12) C203 0.0258(16) 0.0222(17) 0.055(2) 0.0067(15) 0.0051(14) -0.0028(13) C204 0.0271(16) 0.0264(17) 0.049(2) -0.0127(15) -0.0068(14) -0.0028(14) C205 0.0227(15) 0.0309(17) 0.0283(15) -0.0069(13) -0.0055(12) 0.0043(13) C206 0.0222(15) 0.0336(17) 0.0328(16) -0.0007(13) 0.0008(12) 0.0061(13) C207 0.0267(16) 0.0263(17) 0.0394(17) 0.0084(14) 0.0025(13) 0.0076(13) C208 0.0291(16) 0.0365(19) 0.0343(17) -0.0084(14) 0.0060(13) 0.0113(14) C209 0.0206(15) 0.0399(19) 0.0382(17) 0.0092(14) 0.0086(12) 0.0054(14) C210 0.0134(13) 0.0320(17) 0.0366(16) -0.0027(13) -0.0004(11) 0.0018(12) C211 0.0418(19) 0.058(2) 0.0381(19) -0.0007(17) 0.0016(15) 0.0040(17) C212 0.0217(14) 0.0195(14) 0.0172(13) -0.0003(10) 0.0003(10) 0.0052(11) C213 0.0258(15) 0.0269(16) 0.0239(14) -0.0025(12) 0.0030(11) -0.0039(12) C214 0.0468(19) 0.0268(16) 0.0208(14) -0.0002(12) 0.0086(13) -0.0056(14) C215 0.053(2) 0.0277(17) 0.0201(14) -0.0004(12) -0.0061(14) 0.0018(15) C216 0.0267(16) 0.0297(17) 0.0387(17) -0.0074(14) -0.0129(13) 0.0035(13) C217 0.0184(13) 0.0247(15) 0.0311(15) -0.0058(12) -0.0001(11) 0.0015(12) C218 0.0170(13) 0.0260(16) 0.0161(13) 0.0010(11) 0.0011(10) 0.0026(12) C219 0.0187(14) 0.0260(16) 0.0252(14) 0.0043(12) 0.0034(11) 0.0038(12) C220 0.0169(14) 0.0425(19) 0.0295(15) 0.0005(14) 0.0009(12) -0.0002(13) C221 0.0212(15) 0.0417(19) 0.0325(16) 0.0020(14) -0.0014(12) 0.0155(14) C222 0.0353(17) 0.0300(17) 0.0377(17) 0.0010(14) -0.0012(14) 0.0121(14) C223 0.0274(15) 0.0253(16) 0.0310(15) -0.0034(12) -0.0034(12) 0.0016(13) Fe3 0.01754(19) 0.0208(2) 0.02040(19) -0.00152(15) 0.00347(15) -0.00137(16) P3 0.0166(3) 0.0193(4) 0.0192(3) -0.0019(3) 0.0024(3) -0.0001(3) B3 0.0292(18) 0.033(2) 0.0276(17) -0.0070(14) 0.0103(14) 0.0027(15) C301 0.0151(13) 0.0207(15) 0.0239(14) -0.0012(12) 0.0025(11) -0.0012(11) C302 0.0174(13) 0.0263(16) 0.0265(14) -0.0002(12) 0.0069(11) -0.0001(12) C303 0.0212(14) 0.0239(16) 0.0417(18) -0.0037(13) 0.0092(13) 0.0004(12) C304 0.0240(15) 0.0220(16) 0.0357(17) 0.0050(13) -0.0032(12) 0.0008(13) C305 0.0216(14) 0.0290(17) 0.0222(14) 0.0015(12) -0.0010(11) -0.0011(12) C306 0.0221(14) 0.0324(17) 0.0272(15) 0.0000(13) -0.0007(12) -0.0054(13) C307 0.0230(15) 0.0258(16) 0.0318(16) -0.0046(13) 0.0024(12) -0.0049(12) C308 0.0257(15) 0.0313(17) 0.0351(17) 0.0031(14) 0.0061(13) -0.0066(13) C309 0.0211(15) 0.044(2) 0.0320(16) -0.0078(14) 0.0105(12) -0.0036(14) C310 0.0169(14) 0.0264(16) 0.0399(17) -0.0044(13) 0.0030(12) -0.0036(12) C311 0.0392(19) 0.058(2) 0.0328(18) -0.0002(16) 0.0008(14) -0.0039(17) C312 0.0179(13) 0.0142(13) 0.0248(14) -0.0006(10) -0.0003(10) -0.0011(11) C313 0.0256(15) 0.0273(16) 0.0240(14) 0.0022(12) 0.0046(11) 0.0045(12) C314 0.052(2) 0.0277(17) 0.0222(15) 0.0008(12) 0.0073(13) 0.0064(15) C315 0.054(2) 0.0274(17) 0.0216(15) 0.0007(12) -0.0103(14) -0.0001(15) C316 0.0270(16) 0.0250(16) 0.0437(18) 0.0052(14) -0.0125(14) -0.0020(13) C317 0.0205(14) 0.0236(15) 0.0337(16) 0.0035(12) 0.0018(12) -0.0013(12) C318 0.0189(13) 0.0246(15) 0.0143(12) -0.0002(11) 0.0014(10) -0.0012(12) C319 0.0235(14) 0.0246(15) 0.0199(13) -0.0003(11) 0.0029(11) -0.0003(12) C320 0.0190(14) 0.0362(18) 0.0269(15) 0.0003(13) -0.0003(11) 0.0020(13) C321 0.0213(15) 0.0376(18) 0.0272(15) 0.0015(13) -0.0002(12) -0.0083(14) C322 0.0316(16) 0.0244(16) 0.0389(17) 0.0010(13) 0.0022(13) -0.0074(13) C323 0.0250(15) 0.0260(16) 0.0305(15) 0.0033(13) -0.0010(12) 0.0008(13) Fe4 0.0191(2) 0.0215(2) 0.0276(2) -0.00225(16) 0.00168(16) 0.00299(16) P4 0.0152(3) 0.0201(4) 0.0174(3) -0.0010(3) 0.0013(3) 0.0005(3) B4 0.0217(16) 0.0313(19) 0.0282(17) 0.0058(14) 0.0048(13) -0.0021(14) C401 0.0120(13) 0.0191(15) 0.0275(15) -0.0027(12) 0.0003(11) 0.0030(11) C402 0.0182(14) 0.0237(16) 0.0378(16) 0.0016(13) 0.0068(12) 0.0018(12) C403 0.0229(16) 0.0245(17) 0.063(2) 0.0027(15) 0.0051(15) -0.0028(13) C404 0.0276(16) 0.0240(17) 0.059(2) -0.0124(15) -0.0100(15) -0.0001(14) C405 0.0265(15) 0.0316(18) 0.0314(16) -0.0097(13) -0.0051(12) 0.0038(13) C406 0.0215(15) 0.0367(18) 0.0329(16) 0.0012(14) 0.0007(12) 0.0076(13) C407 0.0283(16) 0.0278(17) 0.0463(19) 0.0047(14) 0.0029(14) 0.0116(14) C408 0.0311(17) 0.0369(19) 0.0407(19) -0.0077(15) 0.0056(14) 0.0144(15) C409 0.0235(15) 0.043(2) 0.0397(18) 0.0064(15) 0.0098(13) 0.0080(14) C410 0.0192(14) 0.0300(17) 0.0418(18) -0.0001(14) 0.0002(13) 0.0049(13) C411 0.053(2) 0.061(2) 0.040(2) 0.0037(17) 0.0018(16) 0.0093(19) C412 0.0195(13) 0.0186(14) 0.0190(13) -0.0004(10) 0.0002(10) 0.0016(11) C413 0.0215(14) 0.0239(15) 0.0258(14) -0.0035(12) 0.0034(11) 0.0009(12) C414 0.0236(15) 0.0314(17) 0.0295(15) -0.0019(13) -0.0068(12) -0.0008(13) C415 0.0365(17) 0.0305(17) 0.0185(14) -0.0021(12) -0.0034(12) -0.0028(14) C416 0.0367(17) 0.0298(17) 0.0228(14) -0.0013(12) 0.0107(12) -0.0024(14) C417 0.0213(14) 0.0257(15) 0.0228(14) -0.0016(11) 0.0040(11) -0.0023(12) C418 0.0201(13) 0.0254(15) 0.0136(12) 0.0013(11) 0.0008(10) 0.0036(12) C419 0.0243(15) 0.0284(17) 0.0303(15) -0.0016(13) -0.0015(12) 0.0004(13) C420 0.0376(18) 0.0281(17) 0.0365(17) -0.0023(13) 0.0004(14) 0.0143(14) C421 0.0245(16) 0.043(2) 0.0333(16) 0.0007(14) -0.0008(13) 0.0118(15) C422 0.0175(14) 0.0418(19) 0.0316(16) 0.0028(14) 0.0009(12) 0.0025(14) C423 0.0228(14) 0.0290(16) 0.0223(14) 0.0021(12) 0.0012(11) 0.0008(12) _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 C101 2.033(2) . ? Fe1 C105 2.036(2) . ? Fe1 C109 2.036(3) . ? Fe1 C102 2.036(3) . ? Fe1 C108 2.037(3) . ? Fe1 C107 2.045(3) . ? Fe1 C110 2.050(3) . ? Fe1 C103 2.054(3) . ? Fe1 C104 2.055(3) . ? Fe1 C106 2.059(3) . ? P1 C101 1.782(3) . ? P1 C112 1.809(2) . ? P1 C118 1.817(2) . ? P1 B1 1.916(3) . ? B1 H1A 1.0970 . ? B1 H1B 1.0939 . ? B1 H1C 1.1116 . ? C101 C105 1.437(3) . ? C101 C102 1.446(3) . ? C102 C103 1.420(4) . ? C102 H102 0.9500 . ? C103 C104 1.420(4) . ? C103 H103 0.9500 . ? C104 C105 1.421(4) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C110 1.423(4) . ? C106 C107 1.425(4) . ? C106 C111 1.495(4) . ? C107 C108 1.413(4) . ? C107 H107 0.9500 . ? C108 C109 1.413(4) . ? C108 H108 0.9500 . ? C109 C110 1.419(4) . ? C109 H109 0.9500 . ? C110 H110 0.9500 . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 C117 1.390(3) . ? C112 C113 1.398(3) . ? C113 C114 1.383(3) . ? C113 H113 0.9500 . ? C114 C115 1.386(4) . ? C114 H114 0.9500 . ? C115 C116 1.388(4) . ? C115 H115 0.9500 . ? C116 C117 1.388(3) . ? C116 H116 0.9500 . ? C117 H117 0.9500 . ? C118 C119 1.387(3) . ? C118 C123 1.390(4) . ? C119 C120 1.390(3) . ? C119 H119 0.9500 . ? C120 C121 1.384(4) . ? C120 H120 0.9500 . ? C121 C122 1.384(4) . ? C121 H121 0.9500 . ? C122 C123 1.390(4) . ? C122 H122 0.9500 . ? C123 H123 0.9500 . ? Fe2 C201 2.031(3) . ? Fe2 C205 2.032(3) . ? Fe2 C208 2.035(3) . ? Fe2 C209 2.037(3) . ? Fe2 C202 2.040(3) . ? Fe2 C207 2.043(3) . ? Fe2 C210 2.051(3) . ? Fe2 C203 2.051(3) . ? Fe2 C204 2.053(3) . ? Fe2 C206 2.059(3) . ? P2 C201 1.783(3) . ? P2 C212 1.811(2) . ? P2 C218 1.822(3) . ? P2 B2 1.921(3) . ? B2 H2A 1.0614 . ? B2 H2B 1.1074 . ? B2 H2C 1.2096 . ? C201 C202 1.430(4) . ? C201 C205 1.438(4) . ? C202 C203 1.429(4) . ? C202 H202 0.9500 . ? C203 C204 1.419(4) . ? C203 H203 0.9500 . ? C204 C205 1.428(4) . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? C206 C210 1.424(4) . ? C206 C207 1.431(4) . ? C206 C211 1.494(4) . ? C207 C208 1.413(4) . ? C207 H207 0.9500 . ? C208 C209 1.413(4) . ? C208 H208 0.9500 . ? C209 C210 1.410(4) . ? C209 H209 0.9500 . ? C210 H210 0.9500 . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C212 C213 1.391(3) . ? C212 C217 1.396(3) . ? C213 C214 1.387(3) . ? C213 H213 0.9500 . ? C214 C215 1.384(4) . ? C214 H214 0.9500 . ? C215 C216 1.382(4) . ? C215 H215 0.9500 . ? C216 C217 1.386(4) . ? C216 H216 0.9500 . ? C217 H217 0.9500 . ? C218 C223 1.390(4) . ? C218 C219 1.395(3) . ? C219 C220 1.396(3) . ? C219 H219 0.9500 . ? C220 C221 1.379(4) . ? C220 H220 0.9500 . ? C221 C222 1.378(4) . ? C221 H221 0.9500 . ? C222 C223 1.387(4) . ? C222 H222 0.9500 . ? C223 H223 0.9500 . ? Fe3 C301 2.028(3) . ? Fe3 C308 2.032(3) . ? Fe3 C305 2.033(2) . ? Fe3 C302 2.038(3) . ? Fe3 C309 2.041(3) . ? Fe3 C307 2.045(3) . ? Fe3 C310 2.050(3) . ? Fe3 C303 2.052(3) . ? Fe3 C304 2.052(3) . ? Fe3 C306 2.062(3) . ? P3 C301 1.789(3) . ? P3 C312 1.815(2) . ? P3 C318 1.822(3) . ? P3 B3 1.918(3) . ? B3 H3A 1.2062 . ? B3 H3B 1.1285 . ? B3 H3C 1.1503 . ? C301 C305 1.430(3) . ? C301 C302 1.441(3) . ? C302 C303 1.417(4) . ? C302 H302 0.9500 . ? C303 C304 1.417(4) . ? C303 H303 0.9500 . ? C304 C305 1.421(4) . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? C306 C310 1.415(4) . ? C306 C307 1.428(4) . ? C306 C311 1.494(4) . ? C307 C308 1.412(4) . ? C307 H307 0.9500 . ? C308 C309 1.420(4) . ? C308 H308 0.9500 . ? C309 C310 1.415(4) . ? C309 H309 0.9500 . ? C310 H310 0.9500 . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? C312 C317 1.388(3) . ? C312 C313 1.397(3) . ? C313 C314 1.385(3) . ? C313 H313 0.9500 . ? C314 C315 1.375(4) . ? C314 H314 0.9500 . ? C315 C316 1.381(4) . ? C315 H315 0.9500 . ? C316 C317 1.386(4) . ? C316 H316 0.9500 . ? C317 H317 0.9500 . ? C318 C319 1.393(3) . ? C318 C323 1.393(4) . ? C319 C320 1.390(3) . ? C319 H319 0.9500 . ? C320 C321 1.381(4) . ? C320 H320 0.9500 . ? C321 C322 1.386(4) . ? C321 H321 0.9500 . ? C322 C323 1.393(4) . ? C322 H322 0.9500 . ? C323 H323 0.9500 . ? Fe4 C401 2.026(2) . ? Fe4 C405 2.032(3) . ? Fe4 C402 2.035(3) . ? Fe4 C409 2.040(3) . ? Fe4 C408 2.042(3) . ? Fe4 C404 2.045(3) . ? Fe4 C403 2.046(3) . ? Fe4 C407 2.046(3) . ? Fe4 C410 2.048(3) . ? Fe4 C406 2.055(3) . ? P4 C401 1.788(3) . ? P4 C412 1.812(2) . ? P4 C418 1.825(3) . ? P4 B4 1.918(3) . ? B4 H4A 1.1496 . ? B4 H4B 1.0905 . ? B4 H4C 1.0707 . ? C401 C405 1.434(4) . ? C401 C402 1.441(4) . ? C402 C403 1.416(4) . ? C402 H402 0.9500 . ? C403 C404 1.411(4) . ? C403 H403 0.9500 . ? C404 C405 1.419(4) . ? C404 H404 0.9500 . ? C405 H405 0.9500 . ? C406 C407 1.420(4) . ? C406 C410 1.421(4) . ? C406 C411 1.506(4) . ? C407 C408 1.415(4) . ? C407 H407 0.9500 . ? C408 C409 1.420(4) . ? C408 H408 0.9500 . ? C409 C410 1.413(4) . ? C409 H409 0.9500 . ? C410 H410 0.9500 . ? C411 H41A 0.9800 . ? C411 H41B 0.9800 . ? C411 H41C 0.9800 . ? C412 C413 1.393(3) . ? C412 C417 1.398(3) . ? C413 C414 1.386(3) . ? C413 H413 0.9500 . ? C414 C415 1.384(4) . ? C414 H414 0.9500 . ? C415 C416 1.387(4) . ? C415 H415 0.9500 . ? C416 C417 1.386(3) . ? C416 H416 0.9500 . ? C417 H417 0.9500 . ? C418 C423 1.382(3) . ? C418 C419 1.395(4) . ? C419 C420 1.391(4) . ? C419 H419 0.9500 . ? C420 C421 1.381(4) . ? C420 H420 0.9500 . ? C421 C422 1.380(4) . ? C421 H421 0.9500 . ? C422 C423 1.388(3) . ? C422 H422 0.9500 . ? C423 H423 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 C101 Fe1 C105 41.37(9) . . ? C101 Fe1 C109 120.41(11) . . ? C105 Fe1 C109 107.04(11) . . ? C101 Fe1 C102 41.64(10) . . ? C105 Fe1 C102 69.37(10) . . ? C109 Fe1 C102 156.66(11) . . ? C101 Fe1 C108 154.71(11) . . ? C105 Fe1 C108 118.88(11) . . ? C109 Fe1 C108 40.60(11) . . ? C102 Fe1 C108 161.67(11) . . ? C101 Fe1 C107 163.72(10) . . ? C105 Fe1 C107 153.44(11) . . ? C109 Fe1 C107 68.32(11) . . ? C102 Fe1 C107 125.32(11) . . ? C108 Fe1 C107 40.50(11) . . ? C101 Fe1 C110 108.87(11) . . ? C105 Fe1 C110 126.60(11) . . ? C109 Fe1 C110 40.65(11) . . ? C102 Fe1 C110 121.97(11) . . ? C108 Fe1 C110 67.99(11) . . ? C107 Fe1 C110 67.88(11) . . ? C101 Fe1 C103 69.21(11) . . ? C105 Fe1 C103 68.68(11) . . ? C109 Fe1 C103 161.32(12) . . ? C102 Fe1 C103 40.64(10) . . ? C108 Fe1 C103 124.20(12) . . ? C107 Fe1 C103 106.91(11) . . ? C110 Fe1 C103 156.07(11) . . ? C101 Fe1 C104 68.93(10) . . ? C105 Fe1 C104 40.64(10) . . ? C109 Fe1 C104 124.70(12) . . ? C102 Fe1 C104 68.43(11) . . ? C108 Fe1 C104 106.33(11) . . ? C107 Fe1 C104 119.04(11) . . ? C110 Fe1 C104 162.91(11) . . ? C103 Fe1 C104 40.43(11) . . ? C101 Fe1 C106 126.60(10) . . ? C105 Fe1 C106 164.26(11) . . ? C109 Fe1 C106 68.68(11) . . ? C102 Fe1 C106 108.20(11) . . ? C108 Fe1 C106 68.42(11) . . ? C107 Fe1 C106 40.61(10) . . ? C110 Fe1 C106 40.52(10) . . ? C103 Fe1 C106 120.27(11) . . ? C104 Fe1 C106 154.23(11) . . ? C101 P1 C112 105.98(11) . . ? C101 P1 C118 105.33(11) . . ? C112 P1 C118 102.95(11) . . ? C101 P1 B1 114.84(13) . . ? C112 P1 B1 115.49(13) . . ? C118 P1 B1 111.11(13) . . ? P1 B1 H1A 105.8 . . ? P1 B1 H1B 110.9 . . ? H1A B1 H1B 113.8 . . ? P1 B1 H1C 100.2 . . ? H1A B1 H1C 113.5 . . ? H1B B1 H1C 111.6 . . ? C105 C101 C102 107.0(2) . . ? C105 C101 P1 124.79(19) . . ? C102 C101 P1 128.23(19) . . ? C105 C101 Fe1 69.43(14) . . ? C102 C101 Fe1 69.31(14) . . ? P1 C101 Fe1 127.36(13) . . ? C103 C102 C101 108.1(2) . . ? C103 C102 Fe1 70.34(15) . . ? C101 C102 Fe1 69.04(14) . . ? C103 C102 H102 126.0 . . ? C101 C102 H102 126.0 . . ? Fe1 C102 H102 126.2 . . ? C104 C103 C102 108.2(3) . . ? C104 C103 Fe1 69.86(15) . . ? C102 C103 Fe1 69.02(15) . . ? C104 C103 H103 125.9 . . ? C102 C103 H103 125.9 . . ? Fe1 C103 H103 126.8 . . ? C103 C104 C105 108.6(2) . . ? C103 C104 Fe1 69.72(15) . . ? C105 C104 Fe1 68.93(14) . . ? C103 C104 H104 125.7 . . ? C105 C104 H104 125.7 . . ? Fe1 C104 H104 127.2 . . ? C104 C105 C101 108.1(2) . . ? C104 C105 Fe1 70.43(14) . . ? C101 C105 Fe1 69.20(14) . . ? C104 C105 H105 125.9 . . ? C101 C105 H105 125.9 . . ? Fe1 C105 H105 126.0 . . ? C110 C106 C107 106.8(2) . . ? C110 C106 C111 125.7(3) . . ? C107 C106 C111 127.4(3) . . ? C110 C106 Fe1 69.39(14) . . ? C107 C106 Fe1 69.18(15) . . ? C111 C106 Fe1 128.1(2) . . ? C108 C107 C106 108.5(3) . . ? C108 C107 Fe1 69.44(15) . . ? C106 C107 Fe1 70.21(15) . . ? C108 C107 H107 125.7 . . ? C106 C107 H107 125.7 . . ? Fe1 C107 H107 126.2 . . ? C107 C108 C109 108.3(3) . . ? C107 C108 Fe1 70.06(15) . . ? C109 C108 Fe1 69.65(16) . . ? C107 C108 H108 125.8 . . ? C109 C108 H108 125.8 . . ? Fe1 C108 H108 126.0 . . ? C108 C109 C110 107.6(2) . . ? C108 C109 Fe1 69.75(15) . . ? C110 C109 Fe1 70.20(15) . . ? C108 C109 H109 126.2 . . ? C110 C109 H109 126.2 . . ? Fe1 C109 H109 125.4 . . ? C109 C110 C106 108.7(2) . . ? C109 C110 Fe1 69.15(15) . . ? C106 C110 Fe1 70.09(15) . . ? C109 C110 H110 125.6 . . ? C106 C110 H110 125.6 . . ? Fe1 C110 H110 126.7 . . ? C106 C111 H11A 109.5 . . ? C106 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C106 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C117 C112 C113 119.3(2) . . ? C117 C112 P1 120.63(19) . . ? C113 C112 P1 120.08(18) . . ? C114 C113 C112 120.4(2) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C113 C114 C115 120.0(3) . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C114 C115 C116 120.0(2) . . ? C114 C115 H115 120.0 . . ? C116 C115 H115 120.0 . . ? C115 C116 C117 120.1(2) . . ? C115 C116 H116 120.0 . . ? C117 C116 H116 120.0 . . ? C116 C117 C112 120.2(2) . . ? C116 C117 H117 119.9 . . ? C112 C117 H117 119.9 . . ? C119 C118 C123 119.0(2) . . ? C119 C118 P1 122.2(2) . . ? C123 C118 P1 118.8(2) . . ? C118 C119 C120 120.7(2) . . ? C118 C119 H119 119.6 . . ? C120 C119 H119 119.6 . . ? C121 C120 C119 119.6(3) . . ? C121 C120 H120 120.2 . . ? C119 C120 H120 120.2 . . ? C122 C121 C120 120.5(2) . . ? C122 C121 H121 119.8 . . ? C120 C121 H121 119.8 . . ? C121 C122 C123 119.5(3) . . ? C121 C122 H122 120.2 . . ? C123 C122 H122 120.2 . . ? C122 C123 C118 120.8(3) . . ? C122 C123 H123 119.6 . . ? C118 C123 H123 119.6 . . ? C201 Fe2 C205 41.46(10) . . ? C201 Fe2 C208 154.29(11) . . ? C205 Fe2 C208 118.43(11) . . ? C201 Fe2 C209 120.34(11) . . ? C205 Fe2 C209 107.31(11) . . ? C208 Fe2 C209 40.62(11) . . ? C201 Fe2 C202 41.14(10) . . ? C205 Fe2 C202 69.28(11) . . ? C208 Fe2 C202 162.60(11) . . ? C209 Fe2 C202 155.70(11) . . ? C201 Fe2 C207 164.26(11) . . ? C205 Fe2 C207 152.60(11) . . ? C208 Fe2 C207 40.56(11) . . ? C209 Fe2 C207 68.39(11) . . ? C202 Fe2 C207 125.89(11) . . ? C201 Fe2 C210 109.13(11) . . ? C205 Fe2 C210 127.07(11) . . ? C208 Fe2 C210 67.94(11) . . ? C209 Fe2 C210 40.35(11) . . ? C202 Fe2 C210 121.46(11) . . ? C207 Fe2 C210 68.16(11) . . ? C201 Fe2 C203 69.06(11) . . ? C205 Fe2 C203 68.79(12) . . ? C208 Fe2 C203 124.62(12) . . ? C209 Fe2 C203 162.15(12) . . ? C202 Fe2 C203 40.90(10) . . ? C207 Fe2 C203 106.59(12) . . ? C210 Fe2 C203 155.44(12) . . ? C201 Fe2 C204 69.14(11) . . ? C205 Fe2 C204 40.92(11) . . ? C208 Fe2 C204 106.15(12) . . ? C209 Fe2 C204 125.40(12) . . ? C202 Fe2 C204 68.67(11) . . ? C207 Fe2 C204 118.03(12) . . ? C210 Fe2 C204 163.62(12) . . ? C203 Fe2 C204 40.45(12) . . ? C201 Fe2 C206 127.08(11) . . ? C205 Fe2 C206 164.94(12) . . ? C208 Fe2 C206 68.42(11) . . ? C209 Fe2 C206 68.42(11) . . ? C202 Fe2 C206 108.30(11) . . ? C207 Fe2 C206 40.84(11) . . ? C210 Fe2 C206 40.54(11) . . ? C203 Fe2 C206 119.76(12) . . ? C204 Fe2 C206 153.33(12) . . ? C201 P2 C212 106.31(12) . . ? C201 P2 C218 104.86(12) . . ? C212 P2 C218 104.30(11) . . ? C201 P2 B2 114.66(13) . . ? C212 P2 B2 115.33(13) . . ? C218 P2 B2 110.39(13) . . ? P2 B2 H2A 112.0 . . ? P2 B2 H2B 103.7 . . ? H2A B2 H2B 114.0 . . ? P2 B2 H2C 104.9 . . ? H2A B2 H2C 111.7 . . ? H2B B2 H2C 109.9 . . ? C202 C201 C205 107.6(2) . . ? C202 C201 P2 128.4(2) . . ? C205 C201 P2 124.0(2) . . ? C202 C201 Fe2 69.76(15) . . ? C205 C201 Fe2 69.33(15) . . ? P2 C201 Fe2 127.39(14) . . ? C203 C202 C201 108.0(3) . . ? C203 C202 Fe2 69.99(16) . . ? C201 C202 Fe2 69.09(15) . . ? C203 C202 H202 126.0 . . ? C201 C202 H202 126.0 . . ? Fe2 C202 H202 126.5 . . ? C204 C203 C202 108.3(3) . . ? C204 C203 Fe2 69.83(17) . . ? C202 C203 Fe2 69.11(15) . . ? C204 C203 H203 125.9 . . ? C202 C203 H203 125.9 . . ? Fe2 C203 H203 126.8 . . ? C203 C204 C205 108.3(3) . . ? C203 C204 Fe2 69.72(16) . . ? C205 C204 Fe2 68.78(15) . . ? C203 C204 H204 125.9 . . ? C205 C204 H204 125.9 . . ? Fe2 C204 H204 127.2 . . ? C204 C205 C201 107.9(3) . . ? C204 C205 Fe2 70.30(15) . . ? C201 C205 Fe2 69.21(14) . . ? C204 C205 H205 126.1 . . ? C201 C205 H205 126.1 . . ? Fe2 C205 H205 126.0 . . ? C210 C206 C207 106.9(2) . . ? C210 C206 C211 125.0(3) . . ? C207 C206 C211 128.1(3) . . ? C210 C206 Fe2 69.42(15) . . ? C207 C206 Fe2 68.99(15) . . ? C211 C206 Fe2 127.9(2) . . ? C208 C207 C206 108.0(3) . . ? C208 C207 Fe2 69.39(16) . . ? C206 C207 Fe2 70.17(15) . . ? C208 C207 H207 126.0 . . ? C206 C207 H207 126.0 . . ? Fe2 C207 H207 126.0 . . ? C209 C208 C207 108.4(3) . . ? C209 C208 Fe2 69.79(16) . . ? C207 C208 Fe2 70.04(16) . . ? C209 C208 H208 125.8 . . ? C207 C208 H208 125.8 . . ? Fe2 C208 H208 126.0 . . ? C210 C209 C208 107.9(3) . . ? C210 C209 Fe2 70.35(16) . . ? C208 C209 Fe2 69.60(16) . . ? C210 C209 H209 126.0 . . ? C208 C209 H209 126.0 . . ? Fe2 C209 H209 125.6 . . ? C209 C210 C206 108.7(3) . . ? C209 C210 Fe2 69.30(15) . . ? C206 C210 Fe2 70.03(15) . . ? C209 C210 H210 125.6 . . ? C206 C210 H210 125.6 . . ? Fe2 C210 H210 126.6 . . ? C206 C211 H21A 109.5 . . ? C206 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C206 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C213 C212 C217 119.2(2) . . ? C213 C212 P2 120.92(19) . . ? C217 C212 P2 119.84(19) . . ? C214 C213 C212 120.7(3) . . ? C214 C213 H213 119.6 . . ? C212 C213 H213 119.6 . . ? C215 C214 C213 119.6(3) . . ? C215 C214 H214 120.2 . . ? C213 C214 H214 120.2 . . ? C216 C215 C214 120.1(3) . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C215 C216 C217 120.7(3) . . ? C215 C216 H216 119.7 . . ? C217 C216 H216 119.7 . . ? C216 C217 C212 119.6(3) . . ? C216 C217 H217 120.2 . . ? C212 C217 H217 120.2 . . ? C223 C218 C219 119.3(2) . . ? C223 C218 P2 119.0(2) . . ? C219 C218 P2 121.7(2) . . ? C218 C219 C220 120.1(3) . . ? C218 C219 H219 120.0 . . ? C220 C219 H219 120.0 . . ? C221 C220 C219 119.6(3) . . ? C221 C220 H220 120.2 . . ? C219 C220 H220 120.2 . . ? C222 C221 C220 120.8(2) . . ? C222 C221 H221 119.6 . . ? C220 C221 H221 119.6 . . ? C221 C222 C223 119.9(3) . . ? C221 C222 H222 120.0 . . ? C223 C222 H222 120.0 . . ? C222 C223 C218 120.3(3) . . ? C222 C223 H223 119.8 . . ? C218 C223 H223 119.8 . . ? C301 Fe3 C308 154.60(11) . . ? C301 Fe3 C305 41.25(10) . . ? C308 Fe3 C305 118.67(11) . . ? C301 Fe3 C302 41.52(10) . . ? C308 Fe3 C302 161.61(11) . . ? C305 Fe3 C302 69.16(10) . . ? C301 Fe3 C309 120.30(11) . . ? C308 Fe3 C309 40.81(11) . . ? C305 Fe3 C309 106.76(11) . . ? C302 Fe3 C309 156.72(11) . . ? C301 Fe3 C307 163.91(11) . . ? C308 Fe3 C307 40.51(10) . . ? C305 Fe3 C307 153.38(11) . . ? C302 Fe3 C307 125.59(11) . . ? C309 Fe3 C307 68.43(11) . . ? C301 Fe3 C310 109.17(11) . . ? C308 Fe3 C310 67.93(11) . . ? C305 Fe3 C310 126.49(11) . . ? C302 Fe3 C310 122.52(11) . . ? C309 Fe3 C310 40.46(11) . . ? C307 Fe3 C310 67.78(11) . . ? C301 Fe3 C303 69.01(11) . . ? C308 Fe3 C303 124.03(12) . . ? C305 Fe3 C303 68.48(11) . . ? C302 Fe3 C303 40.54(10) . . ? C309 Fe3 C303 161.10(12) . . ? C307 Fe3 C303 107.15(11) . . ? C310 Fe3 C303 156.63(11) . . ? C301 Fe3 C304 69.01(11) . . ? C308 Fe3 C304 105.81(11) . . ? C305 Fe3 C304 40.72(10) . . ? C302 Fe3 C304 68.47(11) . . ? C309 Fe3 C304 124.24(11) . . ? C307 Fe3 C304 118.87(11) . . ? C310 Fe3 C304 162.46(11) . . ? C303 Fe3 C304 40.41(11) . . ? C301 Fe3 C306 126.83(11) . . ? C308 Fe3 C306 68.37(11) . . ? C305 Fe3 C306 164.05(11) . . ? C302 Fe3 C306 108.85(10) . . ? C309 Fe3 C306 68.45(11) . . ? C307 Fe3 C306 40.67(10) . . ? C310 Fe3 C306 40.25(10) . . ? C303 Fe3 C306 120.99(11) . . ? C304 Fe3 C306 154.57(11) . . ? C301 P3 C312 106.34(11) . . ? C301 P3 C318 105.01(12) . . ? C312 P3 C318 103.66(11) . . ? C301 P3 B3 114.43(13) . . ? C312 P3 B3 115.70(13) . . ? C318 P3 B3 110.64(13) . . ? P3 B3 H3A 105.2 . . ? P3 B3 H3B 110.4 . . ? H3A B3 H3B 107.6 . . ? P3 B3 H3C 104.6 . . ? H3A B3 H3C 114.1 . . ? H3B B3 H3C 114.6 . . ? C305 C301 C302 107.1(2) . . ? C305 C301 P3 124.7(2) . . ? C302 C301 P3 128.1(2) . . ? C305 C301 Fe3 69.55(15) . . ? C302 C301 Fe3 69.63(14) . . ? P3 C301 Fe3 127.36(13) . . ? C303 C302 C301 107.9(2) . . ? C303 C302 Fe3 70.23(15) . . ? C301 C302 Fe3 68.84(14) . . ? C303 C302 H302 126.1 . . ? C301 C302 H302 126.1 . . ? Fe3 C302 H302 126.4 . . ? C302 C303 C304 108.6(3) . . ? C302 C303 Fe3 69.23(15) . . ? C304 C303 Fe3 69.82(15) . . ? C302 C303 H303 125.7 . . ? C304 C303 H303 125.7 . . ? Fe3 C303 H303 126.8 . . ? C303 C304 C305 108.1(2) . . ? C303 C304 Fe3 69.77(15) . . ? C305 C304 Fe3 68.90(14) . . ? C303 C304 H304 125.9 . . ? C305 C304 H304 125.9 . . ? Fe3 C304 H304 126.9 . . ? C304 C305 C301 108.3(2) . . ? C304 C305 Fe3 70.38(15) . . ? C301 C305 Fe3 69.20(14) . . ? C304 C305 H305 125.9 . . ? C301 C305 H305 125.9 . . ? Fe3 C305 H305 126.1 . . ? C310 C306 C307 106.9(2) . . ? C310 C306 C311 126.3(3) . . ? C307 C306 C311 126.8(3) . . ? C310 C306 Fe3 69.39(15) . . ? C307 C306 Fe3 69.03(15) . . ? C311 C306 Fe3 128.4(2) . . ? C308 C307 C306 108.2(3) . . ? C308 C307 Fe3 69.22(15) . . ? C306 C307 Fe3 70.29(15) . . ? C308 C307 H307 125.9 . . ? C306 C307 H307 125.9 . . ? Fe3 C307 H307 126.2 . . ? C307 C308 C309 108.5(3) . . ? C307 C308 Fe3 70.27(16) . . ? C309 C308 Fe3 69.97(16) . . ? C307 C308 H308 125.8 . . ? C309 C308 H308 125.8 . . ? Fe3 C308 H308 125.6 . . ? C310 C309 C308 107.1(2) . . ? C310 C309 Fe3 70.08(15) . . ? C308 C309 Fe3 69.22(15) . . ? C310 C309 H309 126.5 . . ? C308 C309 H309 126.5 . . ? Fe3 C309 H309 125.8 . . ? C309 C310 C306 109.3(3) . . ? C309 C310 Fe3 69.46(15) . . ? C306 C310 Fe3 70.35(15) . . ? C309 C310 H310 125.3 . . ? C306 C310 H310 125.3 . . ? Fe3 C310 H310 126.4 . . ? C306 C311 H31A 109.5 . . ? C306 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? C306 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C317 C312 C313 119.2(2) . . ? C317 C312 P3 119.9(2) . . ? C313 C312 P3 120.82(19) . . ? C314 C313 C312 120.2(3) . . ? C314 C313 H313 119.9 . . ? C312 C313 H313 119.9 . . ? C315 C314 C313 120.0(3) . . ? C315 C314 H314 120.0 . . ? C313 C314 H314 120.0 . . ? C314 C315 C316 120.3(3) . . ? C314 C315 H315 119.9 . . ? C316 C315 H315 119.9 . . ? C315 C316 C317 120.2(3) . . ? C315 C316 H316 119.9 . . ? C317 C316 H316 119.9 . . ? C316 C317 C312 120.1(3) . . ? C316 C317 H317 120.0 . . ? C312 C317 H317 120.0 . . ? C319 C318 C323 119.5(2) . . ? C319 C318 P3 122.0(2) . . ? C323 C318 P3 118.46(19) . . ? C320 C319 C318 120.3(2) . . ? C320 C319 H319 119.9 . . ? C318 C319 H319 119.9 . . ? C321 C320 C319 120.0(3) . . ? C321 C320 H320 120.0 . . ? C319 C320 H320 120.0 . . ? C320 C321 C322 120.3(2) . . ? C320 C321 H321 119.9 . . ? C322 C321 H321 119.9 . . ? C321 C322 C323 120.0(3) . . ? C321 C322 H322 120.0 . . ? C323 C322 H322 120.0 . . ? C318 C323 C322 119.9(3) . . ? C318 C323 H323 120.0 . . ? C322 C323 H323 120.0 . . ? C401 Fe4 C405 41.39(10) . . ? C401 Fe4 C402 41.58(10) . . ? C405 Fe4 C402 69.46(11) . . ? C401 Fe4 C409 120.44(11) . . ? C405 Fe4 C409 107.55(12) . . ? C402 Fe4 C409 156.08(12) . . ? C401 Fe4 C408 154.39(12) . . ? C405 Fe4 C408 118.55(12) . . ? C402 Fe4 C408 162.01(12) . . ? C409 Fe4 C408 40.72(11) . . ? C401 Fe4 C404 68.83(11) . . ? C405 Fe4 C404 40.73(11) . . ? C402 Fe4 C404 68.34(12) . . ? C409 Fe4 C404 125.74(13) . . ? C408 Fe4 C404 106.39(12) . . ? C401 Fe4 C403 69.09(11) . . ? C405 Fe4 C403 68.76(12) . . ? C402 Fe4 C403 40.62(11) . . ? C409 Fe4 C403 162.21(12) . . ? C408 Fe4 C403 124.45(12) . . ? C404 Fe4 C403 40.33(12) . . ? C401 Fe4 C407 164.25(11) . . ? C405 Fe4 C407 152.66(12) . . ? C402 Fe4 C407 125.47(12) . . ? C409 Fe4 C407 68.27(12) . . ? C408 Fe4 C407 40.49(11) . . ? C404 Fe4 C407 118.30(12) . . ? C403 Fe4 C407 106.54(12) . . ? C401 Fe4 C410 109.32(11) . . ? C405 Fe4 C410 127.46(12) . . ? C402 Fe4 C410 121.54(11) . . ? C409 Fe4 C410 40.44(11) . . ? C408 Fe4 C410 68.03(12) . . ? C404 Fe4 C410 164.04(13) . . ? C403 Fe4 C410 155.14(12) . . ? C407 Fe4 C410 67.90(12) . . ? C401 Fe4 C406 127.35(11) . . ? C405 Fe4 C406 165.31(11) . . ? C402 Fe4 C406 108.14(11) . . ? C409 Fe4 C406 68.42(11) . . ? C408 Fe4 C406 68.29(11) . . ? C404 Fe4 C406 153.08(12) . . ? C403 Fe4 C406 119.47(12) . . ? C407 Fe4 C406 40.51(11) . . ? C410 Fe4 C406 40.52(11) . . ? C401 P4 C412 106.62(12) . . ? C401 P4 C418 104.98(12) . . ? C412 P4 C418 103.58(11) . . ? C401 P4 B4 114.43(13) . . ? C412 P4 B4 115.10(13) . . ? C418 P4 B4 111.10(13) . . ? P4 B4 H4A 101.8 . . ? P4 B4 H4B 103.1 . . ? H4A B4 H4B 114.5 . . ? P4 B4 H4C 107.9 . . ? H4A B4 H4C 114.0 . . ? H4B B4 H4C 114.0 . . ? C405 C401 C402 107.4(2) . . ? C405 C401 P4 124.7(2) . . ? C402 C401 P4 127.9(2) . . ? C405 C401 Fe4 69.54(15) . . ? C402 C401 Fe4 69.56(14) . . ? P4 C401 Fe4 127.27(13) . . ? C403 C402 C401 107.8(3) . . ? C403 C402 Fe4 70.12(16) . . ? C401 C402 Fe4 68.86(15) . . ? C403 C402 H402 126.1 . . ? C401 C402 H402 126.1 . . ? Fe4 C402 H402 126.5 . . ? C404 C403 C402 108.3(3) . . ? C404 C403 Fe4 69.80(17) . . ? C402 C403 Fe4 69.27(16) . . ? C404 C403 H403 125.8 . . ? C402 C403 H403 125.8 . . ? Fe4 C403 H403 126.7 . . ? C403 C404 C405 109.0(3) . . ? C403 C404 Fe4 69.86(16) . . ? C405 C404 Fe4 69.12(15) . . ? C403 C404 H404 125.5 . . ? C405 C404 H404 125.5 . . ? Fe4 C404 H404 127.1 . . ? C404 C405 C401 107.5(3) . . ? C404 C405 Fe4 70.15(16) . . ? C401 C405 Fe4 69.07(14) . . ? C404 C405 H405 126.2 . . ? C401 C405 H405 126.2 . . ? Fe4 C405 H405 126.1 . . ? C407 C406 C410 107.2(3) . . ? C407 C406 C411 127.8(3) . . ? C410 C406 C411 125.0(3) . . ? C407 C406 Fe4 69.42(16) . . ? C410 C406 Fe4 69.46(15) . . ? C411 C406 Fe4 127.3(2) . . ? C408 C407 C406 108.4(3) . . ? C408 C407 Fe4 69.58(16) . . ? C406 C407 Fe4 70.07(16) . . ? C408 C407 H407 125.8 . . ? C406 C407 H407 125.8 . . ? Fe4 C407 H407 126.2 . . ? C407 C408 C409 108.0(3) . . ? C407 C408 Fe4 69.93(16) . . ? C409 C408 Fe4 69.56(16) . . ? C407 C408 H408 126.0 . . ? C409 C408 H408 126.0 . . ? Fe4 C408 H408 126.1 . . ? C410 C409 C408 107.7(3) . . ? C410 C409 Fe4 70.08(16) . . ? C408 C409 Fe4 69.72(16) . . ? C410 C409 H409 126.1 . . ? C408 C409 H409 126.1 . . ? Fe4 C409 H409 125.6 . . ? C409 C410 C406 108.7(3) . . ? C409 C410 Fe4 69.48(16) . . ? C406 C410 Fe4 70.01(16) . . ? C409 C410 H410 125.7 . . ? C406 C410 H410 125.7 . . ? Fe4 C410 H410 126.4 . . ? C406 C411 H41A 109.5 . . ? C406 C411 H41B 109.5 . . ? H41A C411 H41B 109.5 . . ? C406 C411 H41C 109.5 . . ? H41A C411 H41C 109.5 . . ? H41B C411 H41C 109.5 . . ? C413 C412 C417 119.3(2) . . ? C413 C412 P4 120.28(19) . . ? C417 C412 P4 120.44(19) . . ? C414 C413 C412 120.2(2) . . ? C414 C413 H413 119.9 . . ? C412 C413 H413 119.9 . . ? C415 C414 C413 120.1(2) . . ? C415 C414 H414 119.9 . . ? C413 C414 H414 119.9 . . ? C414 C415 C416 120.2(2) . . ? C414 C415 H415 119.9 . . ? C416 C415 H415 119.9 . . ? C417 C416 C415 119.9(3) . . ? C417 C416 H416 120.0 . . ? C415 C416 H416 120.0 . . ? C416 C417 C412 120.2(2) . . ? C416 C417 H417 119.9 . . ? C412 C417 H417 119.9 . . ? C423 C418 C419 119.3(2) . . ? C423 C418 P4 122.3(2) . . ? C419 C418 P4 118.4(2) . . ? C420 C419 C418 120.0(3) . . ? C420 C419 H419 120.0 . . ? C418 C419 H419 120.0 . . ? C421 C420 C419 120.1(3) . . ? C421 C420 H420 120.0 . . ? C419 C420 H420 120.0 . . ? C422 C421 C420 120.0(3) . . ? C422 C421 H421 120.0 . . ? C420 C421 H421 120.0 . . ? C421 C422 C423 120.1(3) . . ? C421 C422 H422 120.0 . . ? C423 C422 H422 120.0 . . ? C418 C423 C422 120.5(3) . . ? C418 C423 H423 119.8 . . ? C422 C423 H423 119.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.433 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.061 data_ps311tw _database_code_depnum_ccdc_archive 'CCDC 906409' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-(diphenylphosphino)-1'-(methoxymethyl)ferrocene-borane (1/1) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 B Fe O P' _chemical_formula_sum 'C24 H26 B Fe O P' _chemical_formula_weight 428.08 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4573(2) _cell_length_b 13.4113(3) _cell_length_c 17.4666(4) _cell_angle_alpha 88.5960(10) _cell_angle_beta 81.7640(10) _cell_angle_gamma 75.4980(10) _cell_volume 2122.52(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9552 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 40793 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9711 _reflns_number_gt 8219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 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^)+(0.0299P)^2^+2.5935P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom + difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9711 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _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 0.70625(4) 0.73693(3) -0.12389(2) 0.02432(9) Uani 1 1 d . . . P1 P 0.71010(7) 0.64126(5) 0.06110(4) 0.02219(13) Uani 1 1 d . . . O1 O 0.3106(2) 0.98646(16) -0.09222(13) 0.0377(5) Uani 1 1 d . . . B1 B 0.8582(4) 0.7002(3) 0.09253(19) 0.0330(7) Uani 1 1 d . . . H1B H 0.9711 0.6399 0.0670 0.040 Uiso 1 1 d R . . H2B H 0.8418 0.7788 0.0765 0.040 Uiso 1 1 d R . . H3B H 0.8380 0.6993 0.1541 0.040 Uiso 1 1 d R . . C101 C 0.7178(3) 0.62699(19) -0.04103(14) 0.0229(5) Uani 1 1 d . . . C102 C 0.8512(3) 0.6061(2) -0.09518(15) 0.0269(5) Uani 1 1 d . . . H102 H 0.9456 0.6013 -0.0835 0.032 Uiso 1 1 d R . . C103 C 0.8143(3) 0.5933(2) -0.16955(16) 0.0336(6) Uani 1 1 d . . . H103 H 0.8805 0.5788 -0.2150 0.040 Uiso 1 1 d R . . C104 C 0.6595(3) 0.6070(2) -0.16284(16) 0.0331(6) Uani 1 1 d . . . H104 H 0.6066 0.6030 -0.2031 0.040 Uiso 1 1 d R . . C105 C 0.5992(3) 0.6272(2) -0.08416(16) 0.0274(5) Uani 1 1 d . . . H105 H 0.4999 0.6389 -0.0639 0.033 Uiso 1 1 d R . . C106 C 0.5529(3) 0.8748(2) -0.11648(16) 0.0293(6) Uani 1 1 d . . . C107 C 0.6656(3) 0.8781(2) -0.07134(16) 0.0287(6) Uani 1 1 d . . . H107 H 0.6517 0.8918 -0.0185 0.034 Uiso 1 1 d R . . C108 C 0.8028(3) 0.8571(2) -0.12095(18) 0.0342(6) Uani 1 1 d . . . H108 H 0.8946 0.8534 -0.1061 0.041 Uiso 1 1 d R . . C109 C 0.7753(3) 0.8424(2) -0.19735(17) 0.0356(7) Uani 1 1 d . . . H109 H 0.8456 0.8279 -0.2413 0.043 Uiso 1 1 d R . . C110 C 0.6221(3) 0.8535(2) -0.19482(16) 0.0329(6) Uani 1 1 d . . . H110 H 0.5744 0.8481 -0.2369 0.039 Uiso 1 1 d R . . C111 C 0.3946(3) 0.8834(2) -0.08756(18) 0.0343(6) Uani 1 1 d . . . H11A H 0.3849 0.8616 -0.0341 0.041 Uiso 1 1 d R . . H11B H 0.3571 0.8384 -0.1176 0.041 Uiso 1 1 d R . . C112 C 0.5211(3) 0.7086(2) 0.09735(14) 0.0245(5) Uani 1 1 d . . . C113 C 0.4900(3) 0.8112(2) 0.12120(15) 0.0290(6) Uani 1 1 d . . . H113 H 0.5660 0.8441 0.1199 0.035 Uiso 1 1 d R . . C114 C 0.3456(3) 0.8638(2) 0.14691(16) 0.0367(7) Uani 1 1 d . . . H114 H 0.3245 0.9324 0.1625 0.044 Uiso 1 1 d R . . C115 C 0.2326(3) 0.8148(3) 0.14941(17) 0.0391(7) Uani 1 1 d . . . H115 H 0.1359 0.8507 0.1664 0.047 Uiso 1 1 d R . . C116 C 0.2625(3) 0.7126(2) 0.12657(17) 0.0361(7) Uani 1 1 d . . . H116 H 0.1861 0.6800 0.1281 0.043 Uiso 1 1 d R . . C117 C 0.4070(3) 0.6591(2) 0.10141(15) 0.0289(6) Uani 1 1 d . . . H117 H 0.4279 0.5900 0.0873 0.035 Uiso 1 1 d R . . C118 C 0.7330(3) 0.5114(2) 0.09748(15) 0.0246(5) Uani 1 1 d . . . C119 C 0.7262(3) 0.4955(2) 0.17710(16) 0.0335(6) Uani 1 1 d . . . H119 H 0.7008 0.5519 0.2107 0.040 Uiso 1 1 d R . . C120 C 0.7569(3) 0.3965(2) 0.20628(17) 0.0373(7) Uani 1 1 d . . . H120 H 0.7520 0.3865 0.2594 0.045 Uiso 1 1 d R . . C121 C 0.7952(3) 0.3123(2) 0.15616(17) 0.0333(6) Uani 1 1 d . . . H121 H 0.8160 0.2459 0.1756 0.040 Uiso 1 1 d R . . C122 C 0.8018(3) 0.3273(2) 0.07752(17) 0.0295(6) Uani 1 1 d . . . H122 H 0.8280 0.2709 0.0438 0.035 Uiso 1 1 d R . . C123 C 0.7707(3) 0.4261(2) 0.04820(15) 0.0253(5) Uani 1 1 d . . . H123 H 0.7742 0.4356 -0.0049 0.030 Uiso 1 1 d R . . C124 C 0.1597(3) 0.9935(3) -0.0624(2) 0.0481(8) Uani 1 1 d . . . H24A H 0.1527 0.9686 -0.0103 0.058 Uiso 1 1 d R . . H24B H 0.1046 1.0641 -0.0628 0.058 Uiso 1 1 d R . . H24C H 0.1204 0.9527 -0.0941 0.058 Uiso 1 1 d R . . Fe2 Fe 0.70166(4) 0.22990(3) 0.59992(2) 0.02467(9) Uani 1 1 d . . . P2 P 0.72466(7) 0.14106(5) 0.41505(4) 0.02178(13) Uani 1 1 d . . . O2 O 0.3068(2) 0.48071(15) 0.62072(14) 0.0401(5) Uani 1 1 d . . . B2 B 0.8815(3) 0.1997(3) 0.3695(2) 0.0322(7) Uani 1 1 d . . . H4A H 0.8614 0.2828 0.3934 0.039 Uiso 1 1 d R . . H5B H 0.8683 0.2072 0.3087 0.039 Uiso 1 1 d R . . H6B H 0.9871 0.1455 0.3875 0.039 Uiso 1 1 d R . . C201 C 0.7198(3) 0.12193(19) 0.51690(14) 0.0238(5) Uani 1 1 d . . . C202 C 0.8490(3) 0.0996(2) 0.55466(16) 0.0299(6) Uani 1 1 d . . . H202 H 0.9448 0.0953 0.5308 0.036 Uiso 1 1 d R . . C203 C 0.8057(4) 0.0855(2) 0.63446(17) 0.0369(7) Uani 1 1 d . . . H203 H 0.8682 0.0701 0.6720 0.044 Uiso 1 1 d R . . C204 C 0.6504(4) 0.0991(2) 0.64682(16) 0.0353(6) Uani 1 1 d . . . H204 H 0.5935 0.0939 0.6941 0.042 Uiso 1 1 d R . . C205 C 0.5966(3) 0.1215(2) 0.57473(15) 0.0270(5) Uani 1 1 d . . . H205 H 0.4987 0.1339 0.5666 0.032 Uiso 1 1 d R . . C206 C 0.5476(3) 0.3676(2) 0.61323(16) 0.0286(6) Uani 1 1 d . . . C207 C 0.6618(3) 0.3734(2) 0.55141(16) 0.0295(6) Uani 1 1 d . . . H207 H 0.6493 0.3893 0.5003 0.035 Uiso 1 1 d R . . C208 C 0.7981(3) 0.3511(2) 0.58170(17) 0.0327(6) Uani 1 1 d . . . H208 H 0.8903 0.3486 0.5537 0.039 Uiso 1 1 d R . . C209 C 0.7681(3) 0.3331(2) 0.66226(17) 0.0336(6) Uani 1 1 d . . . H209 H 0.8376 0.3173 0.6962 0.040 Uiso 1 1 d R . . C210 C 0.6153(3) 0.3430(2) 0.68180(16) 0.0315(6) Uani 1 1 d . . . H210 H 0.5668 0.3350 0.7309 0.038 Uiso 1 1 d R . . C211 C 0.3894(3) 0.3776(2) 0.60610(19) 0.0348(6) Uani 1 1 d . . . H11C H 0.3817 0.3572 0.5542 0.042 Uiso 1 1 d R . . H11D H 0.3496 0.3322 0.6424 0.042 Uiso 1 1 d R . . C212 C 0.5403(3) 0.2098(2) 0.40025(14) 0.0236(5) Uani 1 1 d . . . C213 C 0.5111(3) 0.3138(2) 0.38188(15) 0.0287(6) Uani 1 1 d . . . H213 H 0.5872 0.3472 0.3758 0.034 Uiso 1 1 d R . . C214 C 0.3684(3) 0.3683(2) 0.37242(17) 0.0357(7) Uani 1 1 d . . . H214 H 0.3486 0.4380 0.3606 0.043 Uiso 1 1 d R . . C215 C 0.2562(3) 0.3183(3) 0.38126(17) 0.0405(7) Uani 1 1 d . . . H215 H 0.1611 0.3542 0.3745 0.049 Uiso 1 1 d R . . C216 C 0.2834(3) 0.2147(3) 0.39931(17) 0.0375(7) Uani 1 1 d . . . H216 H 0.2069 0.1818 0.4052 0.045 Uiso 1 1 d R . . C217 C 0.4253(3) 0.1602(2) 0.40887(15) 0.0283(6) Uani 1 1 d . . . H217 H 0.4437 0.0907 0.4211 0.034 Uiso 1 1 d R . . C218 C 0.7513(3) 0.01320(19) 0.37428(14) 0.0234(5) Uani 1 1 d . . . C219 C 0.7478(3) 0.0023(2) 0.29545(16) 0.0358(6) Uani 1 1 d . . . H219 H 0.7226 0.0606 0.2654 0.043 Uiso 1 1 d R . . C220 C 0.7811(4) -0.0951(2) 0.26163(17) 0.0393(7) Uani 1 1 d . . . H220 H 0.7783 -0.1021 0.2091 0.047 Uiso 1 1 d R . . C221 C 0.8190(3) -0.1817(2) 0.30669(17) 0.0354(6) Uani 1 1 d . . . H221 H 0.8439 -0.2468 0.2838 0.042 Uiso 1 1 d R . . C222 C 0.8202(3) -0.1719(2) 0.38508(17) 0.0313(6) Uani 1 1 d . . . H222 H 0.8438 -0.2302 0.4152 0.038 Uiso 1 1 d R . . C223 C 0.7860(3) -0.0744(2) 0.41889(15) 0.0245(5) Uani 1 1 d . . . H223 H 0.7858 -0.0676 0.4718 0.029 Uiso 1 1 d R . . C224 C 0.1547(4) 0.4890(3) 0.6161(3) 0.0624(11) Uani 1 1 d . . . H24D H 0.1434 0.4694 0.5652 0.075 Uiso 1 1 d R . . H24E H 0.0987 0.5586 0.6271 0.075 Uiso 1 1 d R . . H24F H 0.1196 0.4439 0.6535 0.075 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02403(19) 0.02603(19) 0.02275(18) 0.00227(14) -0.00271(14) -0.00648(14) P1 0.0227(3) 0.0221(3) 0.0218(3) -0.0011(2) -0.0038(2) -0.0050(2) O1 0.0281(10) 0.0317(11) 0.0504(13) 0.0040(9) -0.0020(9) -0.0046(8) B1 0.0333(16) 0.0365(18) 0.0331(16) -0.0066(13) -0.0078(13) -0.0134(14) C101 0.0259(12) 0.0200(12) 0.0234(12) 0.0024(9) -0.0046(10) -0.0064(10) C102 0.0245(13) 0.0262(13) 0.0276(13) -0.0003(10) -0.0027(10) -0.0024(10) C103 0.0407(16) 0.0301(14) 0.0260(13) -0.0049(11) 0.0007(12) -0.0042(12) C104 0.0443(17) 0.0321(15) 0.0276(14) -0.0004(11) -0.0110(12) -0.0147(13) C105 0.0276(13) 0.0261(13) 0.0317(14) 0.0037(10) -0.0064(11) -0.0118(11) C106 0.0281(14) 0.0280(14) 0.0300(14) 0.0037(11) -0.0030(11) -0.0046(11) C107 0.0331(14) 0.0221(13) 0.0305(14) 0.0041(10) -0.0035(11) -0.0068(11) C108 0.0263(14) 0.0279(14) 0.0490(17) 0.0053(12) -0.0044(12) -0.0087(11) C109 0.0374(16) 0.0309(15) 0.0347(15) 0.0090(12) 0.0062(12) -0.0085(12) C110 0.0378(15) 0.0320(15) 0.0269(14) 0.0082(11) -0.0073(12) -0.0042(12) C111 0.0311(15) 0.0320(15) 0.0371(15) 0.0056(12) -0.0014(12) -0.0051(12) C112 0.0271(13) 0.0240(12) 0.0216(12) 0.0003(10) -0.0046(10) -0.0040(10) C113 0.0361(15) 0.0249(13) 0.0242(13) 0.0014(10) -0.0039(11) -0.0044(11) C114 0.0467(17) 0.0294(15) 0.0265(14) -0.0002(11) -0.0025(12) 0.0027(13) C115 0.0312(15) 0.0472(18) 0.0290(14) -0.0006(13) -0.0031(12) 0.0078(13) C116 0.0273(14) 0.0495(18) 0.0317(15) -0.0034(13) -0.0036(11) -0.0099(13) C117 0.0275(13) 0.0316(14) 0.0271(13) -0.0040(11) -0.0031(10) -0.0062(11) C118 0.0200(12) 0.0260(13) 0.0257(12) 0.0011(10) -0.0031(10) -0.0023(10) C119 0.0385(16) 0.0303(15) 0.0266(14) -0.0004(11) -0.0008(11) -0.0010(12) C120 0.0438(17) 0.0376(16) 0.0274(14) 0.0056(12) -0.0010(12) -0.0070(13) C121 0.0327(15) 0.0267(14) 0.0409(16) 0.0090(12) -0.0065(12) -0.0083(11) C122 0.0270(13) 0.0246(13) 0.0386(15) 0.0006(11) -0.0071(11) -0.0082(11) C123 0.0239(12) 0.0272(13) 0.0257(13) 0.0006(10) -0.0063(10) -0.0067(10) C124 0.0313(16) 0.0388(18) 0.070(2) 0.0014(16) -0.0001(15) -0.0059(13) Fe2 0.02613(19) 0.02287(19) 0.02419(19) -0.00320(14) -0.00604(15) -0.00290(14) P2 0.0191(3) 0.0218(3) 0.0238(3) -0.0009(2) -0.0032(2) -0.0039(2) O2 0.0289(10) 0.0276(10) 0.0601(14) -0.0036(10) -0.0056(10) -0.0002(8) B2 0.0271(15) 0.0318(16) 0.0385(17) 0.0050(13) -0.0014(13) -0.0110(13) C201 0.0247(12) 0.0211(12) 0.0249(12) -0.0031(10) -0.0051(10) -0.0033(10) C202 0.0279(13) 0.0264(13) 0.0338(14) -0.0071(11) -0.0106(11) 0.0007(11) C203 0.0493(18) 0.0269(14) 0.0321(15) -0.0005(11) -0.0194(13) 0.0025(13) C204 0.0513(18) 0.0289(14) 0.0260(14) 0.0009(11) -0.0049(12) -0.0110(13) C205 0.0314(14) 0.0240(13) 0.0269(13) -0.0015(10) -0.0031(11) -0.0096(11) C206 0.0308(14) 0.0218(13) 0.0319(14) -0.0057(10) -0.0061(11) -0.0026(10) C207 0.0347(14) 0.0212(13) 0.0317(14) -0.0016(10) -0.0049(11) -0.0050(11) C208 0.0289(14) 0.0280(14) 0.0418(16) -0.0056(12) -0.0027(12) -0.0090(11) C209 0.0358(15) 0.0306(15) 0.0362(15) -0.0068(12) -0.0137(12) -0.0060(12) C210 0.0363(15) 0.0274(14) 0.0280(14) -0.0070(11) -0.0041(11) -0.0024(11) C211 0.0325(15) 0.0247(14) 0.0447(17) -0.0040(12) -0.0058(13) -0.0020(11) C212 0.0222(12) 0.0266(13) 0.0216(12) -0.0006(10) -0.0044(9) -0.0045(10) C213 0.0322(14) 0.0275(13) 0.0256(13) 0.0001(10) -0.0067(11) -0.0043(11) C214 0.0390(16) 0.0301(15) 0.0317(15) 0.0004(12) -0.0100(12) 0.0059(12) C215 0.0263(14) 0.0523(19) 0.0343(15) -0.0009(14) -0.0089(12) 0.0090(13) C216 0.0223(13) 0.058(2) 0.0329(15) 0.0048(14) -0.0064(11) -0.0109(13) C217 0.0253(13) 0.0320(14) 0.0286(13) 0.0037(11) -0.0061(10) -0.0080(11) C218 0.0207(12) 0.0248(12) 0.0241(12) -0.0027(10) -0.0041(9) -0.0039(10) C219 0.0459(17) 0.0321(15) 0.0279(14) -0.0004(11) -0.0093(12) -0.0047(13) C220 0.0529(19) 0.0388(17) 0.0259(14) -0.0087(12) -0.0074(13) -0.0088(14) C221 0.0377(16) 0.0295(15) 0.0390(16) -0.0097(12) -0.0032(13) -0.0086(12) C222 0.0308(14) 0.0258(14) 0.0378(15) -0.0012(11) -0.0081(12) -0.0058(11) C223 0.0213(12) 0.0269(13) 0.0259(12) -0.0021(10) -0.0033(10) -0.0071(10) C224 0.0333(18) 0.041(2) 0.110(4) 0.004(2) -0.010(2) -0.0036(15) _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 C101 2.035(2) . ? Fe1 C106 2.038(3) . ? Fe1 C102 2.039(3) . ? Fe1 C105 2.041(3) . ? Fe1 C110 2.044(3) . ? Fe1 C108 2.047(3) . ? Fe1 C107 2.048(3) . ? Fe1 C109 2.052(3) . ? Fe1 C104 2.055(3) . ? Fe1 C103 2.061(3) . ? P1 C101 1.788(3) . ? P1 C118 1.811(3) . ? P1 C112 1.818(3) . ? P1 B1 1.919(3) . ? O1 C111 1.418(3) . ? O1 C124 1.427(4) . ? B1 H1B 1.2003 . ? B1 H2B 1.0625 . ? B1 H3B 1.0662 . ? C101 C102 1.435(3) . ? C101 C105 1.437(4) . ? C102 C103 1.418(4) . ? C102 H102 0.9300 . ? C103 C104 1.417(4) . ? C103 H103 0.9299 . ? C104 C105 1.415(4) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? C106 C107 1.423(4) . ? C106 C110 1.432(4) . ? C106 C111 1.487(4) . ? C107 C108 1.422(4) . ? C107 H107 0.9299 . ? C108 C109 1.423(4) . ? C108 H108 0.9299 . ? C109 C110 1.413(4) . ? C109 H109 0.9300 . ? C110 H110 0.9300 . ? C111 H11A 0.9700 . ? C111 H11B 0.9701 . ? C112 C113 1.394(4) . ? C112 C117 1.394(4) . ? C113 C114 1.386(4) . ? C113 H113 0.9300 . ? C114 C115 1.384(5) . ? C114 H114 0.9301 . ? C115 C116 1.385(4) . ? C115 H115 0.9301 . ? C116 C117 1.388(4) . ? C116 H116 0.9299 . ? C117 H117 0.9299 . ? C118 C123 1.391(4) . ? C118 C119 1.397(4) . ? C119 C120 1.387(4) . ? C119 H119 0.9301 . ? C120 C121 1.387(4) . ? C120 H120 0.9301 . ? C121 C122 1.378(4) . ? C121 H121 0.9301 . ? C122 C123 1.386(4) . ? C122 H122 0.9300 . ? C123 H123 0.9300 . ? C124 H24A 0.9599 . ? C124 H24B 0.9601 . ? C124 H24C 0.9599 . ? Fe2 C201 2.034(2) . ? Fe2 C202 2.038(3) . ? Fe2 C206 2.040(3) . ? Fe2 C210 2.041(3) . ? Fe2 C205 2.043(3) . ? Fe2 C209 2.049(3) . ? Fe2 C208 2.052(3) . ? Fe2 C207 2.053(3) . ? Fe2 C204 2.055(3) . ? Fe2 C203 2.060(3) . ? P2 C201 1.787(3) . ? P2 C212 1.808(3) . ? P2 C218 1.817(3) . ? P2 B2 1.915(3) . ? O2 C211 1.417(3) . ? O2 C224 1.429(4) . ? B2 H4A 1.1600 . ? B2 H5B 1.0862 . ? B2 H6B 1.1579 . ? C201 C205 1.429(4) . ? C201 C202 1.434(4) . ? C202 C203 1.418(4) . ? C202 H202 0.9301 . ? C203 C204 1.418(4) . ? C203 H203 0.9301 . ? C204 C205 1.423(4) . ? C204 H204 0.9300 . ? C205 H205 0.9300 . ? C206 C207 1.429(4) . ? C206 C210 1.431(4) . ? C206 C211 1.491(4) . ? C207 C208 1.423(4) . ? C207 H207 0.9299 . ? C208 C209 1.422(4) . ? C208 H208 0.9300 . ? C209 C210 1.410(4) . ? C209 H209 0.9299 . ? C210 H210 0.9301 . ? C211 H11C 0.9700 . ? C211 H11D 0.9699 . ? C212 C213 1.392(4) . ? C212 C217 1.399(4) . ? C213 C214 1.396(4) . ? C213 H213 0.9300 . ? C214 C215 1.380(5) . ? C214 H214 0.9299 . ? C215 C216 1.384(5) . ? C215 H215 0.9300 . ? C216 C217 1.390(4) . ? C216 H216 0.9300 . ? C217 H217 0.9300 . ? C218 C223 1.389(4) . ? C218 C219 1.394(4) . ? C219 C220 1.390(4) . ? C219 H219 0.9300 . ? C220 C221 1.387(4) . ? C220 H220 0.9300 . ? C221 C222 1.381(4) . ? C221 H221 0.9300 . ? C222 C223 1.390(4) . ? C222 H222 0.9300 . ? C223 H223 0.9300 . ? C224 H24D 0.9599 . ? C224 H24E 0.9599 . ? C224 H24F 0.9600 . ? 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 C101 Fe1 C106 124.50(10) . . ? C101 Fe1 C102 41.25(10) . . ? C106 Fe1 C102 162.20(11) . . ? C101 Fe1 C105 41.29(10) . . ? C106 Fe1 C105 107.24(11) . . ? C102 Fe1 C105 68.93(11) . . ? C101 Fe1 C110 161.03(11) . . ? C106 Fe1 C110 41.08(11) . . ? C102 Fe1 C110 155.64(11) . . ? C105 Fe1 C110 123.23(12) . . ? C101 Fe1 C108 122.71(11) . . ? C106 Fe1 C108 68.72(11) . . ? C102 Fe1 C108 108.21(11) . . ? C105 Fe1 C108 158.87(12) . . ? C110 Fe1 C108 68.23(12) . . ? C101 Fe1 C107 108.81(10) . . ? C106 Fe1 C107 40.77(11) . . ? C102 Fe1 C107 125.64(11) . . ? C105 Fe1 C107 122.90(11) . . ? C110 Fe1 C107 68.37(11) . . ? C108 Fe1 C107 40.63(11) . . ? C101 Fe1 C109 157.70(12) . . ? C106 Fe1 C109 68.74(11) . . ? C102 Fe1 C109 121.14(11) . . ? C105 Fe1 C109 159.09(12) . . ? C110 Fe1 C109 40.38(12) . . ? C108 Fe1 C109 40.63(12) . . ? C107 Fe1 C109 68.31(11) . . ? C101 Fe1 C104 68.80(11) . . ? C106 Fe1 C104 120.78(12) . . ? C102 Fe1 C104 68.32(11) . . ? C105 Fe1 C104 40.43(11) . . ? C110 Fe1 C104 106.21(12) . . ? C108 Fe1 C104 159.69(12) . . ? C107 Fe1 C104 157.42(12) . . ? C109 Fe1 C104 122.63(12) . . ? C101 Fe1 C103 68.64(11) . . ? C106 Fe1 C103 155.82(12) . . ? C102 Fe1 C103 40.46(11) . . ? C105 Fe1 C103 68.06(11) . . ? C110 Fe1 C103 120.14(12) . . ? C108 Fe1 C103 124.21(12) . . ? C107 Fe1 C103 161.58(12) . . ? C109 Fe1 C103 106.73(12) . . ? C104 Fe1 C103 40.27(12) . . ? C101 P1 C118 104.34(12) . . ? C101 P1 C112 106.25(12) . . ? C118 P1 C112 105.58(11) . . ? C101 P1 B1 115.37(13) . . ? C118 P1 B1 109.48(14) . . ? C112 P1 B1 114.88(13) . . ? C111 O1 C124 109.7(2) . . ? P1 B1 H1B 102.9 . . ? P1 B1 H2B 111.3 . . ? H1B B1 H2B 119.1 . . ? P1 B1 H3B 103.9 . . ? H1B B1 H3B 112.1 . . ? H2B B1 H3B 106.5 . . ? C102 C101 C105 107.0(2) . . ? C102 C101 P1 124.44(19) . . ? C105 C101 P1 128.4(2) . . ? C102 C101 Fe1 69.55(14) . . ? C105 C101 Fe1 69.59(14) . . ? P1 C101 Fe1 128.78(14) . . ? C103 C102 C101 108.1(2) . . ? C103 C102 Fe1 70.58(16) . . ? C101 C102 Fe1 69.20(14) . . ? C103 C102 H102 126.0 . . ? C101 C102 H102 126.0 . . ? Fe1 C102 H102 126.2 . . ? C104 C103 C102 108.4(2) . . ? C104 C103 Fe1 69.66(16) . . ? C102 C103 Fe1 68.96(15) . . ? C104 C103 H103 125.9 . . ? C102 C103 H103 125.7 . . ? Fe1 C103 H103 126.8 . . ? C105 C104 C103 108.3(2) . . ? C105 C104 Fe1 69.24(15) . . ? C103 C104 Fe1 70.07(16) . . ? C105 C104 H104 125.8 . . ? C103 C104 H104 125.9 . . ? Fe1 C104 H104 126.7 . . ? C104 C105 C101 108.2(2) . . ? C104 C105 Fe1 70.33(15) . . ? C101 C105 Fe1 69.12(14) . . ? C104 C105 H105 125.9 . . ? C101 C105 H105 125.9 . . ? Fe1 C105 H105 126.1 . . ? C107 C106 C110 107.3(2) . . ? C107 C106 C111 126.8(3) . . ? C110 C106 C111 125.8(3) . . ? C107 C106 Fe1 70.01(15) . . ? C110 C106 Fe1 69.68(15) . . ? C111 C106 Fe1 122.0(2) . . ? C108 C107 C106 108.3(3) . . ? C108 C107 Fe1 69.63(16) . . ? C106 C107 Fe1 69.22(16) . . ? C108 C107 H107 125.9 . . ? C106 C107 H107 125.8 . . ? Fe1 C107 H107 126.9 . . ? C107 C108 C109 108.0(3) . . ? C107 C108 Fe1 69.74(15) . . ? C109 C108 Fe1 69.86(17) . . ? C107 C108 H108 126.0 . . ? C109 C108 H108 125.9 . . ? Fe1 C108 H108 125.8 . . ? C110 C109 C108 108.0(2) . . ? C110 C109 Fe1 69.51(15) . . ? C108 C109 Fe1 69.51(16) . . ? C110 C109 H109 125.9 . . ? C108 C109 H109 126.2 . . ? Fe1 C109 H109 126.4 . . ? C109 C110 C106 108.5(3) . . ? C109 C110 Fe1 70.11(16) . . ? C106 C110 Fe1 69.24(15) . . ? C109 C110 H110 125.7 . . ? C106 C110 H110 125.8 . . ? Fe1 C110 H110 126.6 . . ? O1 C111 C106 110.7(2) . . ? O1 C111 H11A 109.2 . . ? C106 C111 H11A 109.2 . . ? O1 C111 H11B 109.8 . . ? C106 C111 H11B 109.9 . . ? H11A C111 H11B 108.1 . . ? C113 C112 C117 119.6(2) . . ? C113 C112 P1 119.5(2) . . ? C117 C112 P1 120.9(2) . . ? C114 C113 C112 119.8(3) . . ? C114 C113 H113 120.2 . . ? C112 C113 H113 120.0 . . ? C115 C114 C113 120.2(3) . . ? C115 C114 H114 119.8 . . ? C113 C114 H114 120.0 . . ? C114 C115 C116 120.4(3) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C117 119.6(3) . . ? C115 C116 H116 120.1 . . ? C117 C116 H116 120.3 . . ? C116 C117 C112 120.3(3) . . ? C116 C117 H117 119.9 . . ? C112 C117 H117 119.8 . . ? C123 C118 C119 118.7(2) . . ? C123 C118 P1 121.89(19) . . ? C119 C118 P1 119.2(2) . . ? C120 C119 C118 120.5(3) . . ? C120 C119 H119 120.0 . . ? C118 C119 H119 119.5 . . ? C119 C120 C121 119.9(3) . . ? C119 C120 H120 120.1 . . ? C121 C120 H120 120.0 . . ? C122 C121 C120 119.9(3) . . ? C122 C121 H121 120.0 . . ? C120 C121 H121 120.1 . . ? C121 C122 C123 120.3(3) . . ? C121 C122 H122 120.0 . . ? C123 C122 H122 119.7 . . ? C122 C123 C118 120.6(2) . . ? C122 C123 H123 119.9 . . ? C118 C123 H123 119.5 . . ? O1 C124 H24A 109.7 . . ? O1 C124 H24B 109.4 . . ? H24A C124 H24B 109.5 . . ? O1 C124 H24C 109.4 . . ? H24A C124 H24C 109.5 . . ? H24B C124 H24C 109.5 . . ? C201 Fe2 C202 41.24(10) . . ? C201 Fe2 C206 125.64(10) . . ? C202 Fe2 C206 163.81(11) . . ? C201 Fe2 C210 162.06(11) . . ? C202 Fe2 C210 154.26(11) . . ? C206 Fe2 C210 41.04(11) . . ? C201 Fe2 C205 41.05(10) . . ? C202 Fe2 C205 68.85(11) . . ? C206 Fe2 C205 107.25(11) . . ? C210 Fe2 C205 123.84(11) . . ? C201 Fe2 C209 156.94(11) . . ? C202 Fe2 C209 120.55(11) . . ? C206 Fe2 C209 68.55(11) . . ? C210 Fe2 C209 40.32(11) . . ? C205 Fe2 C209 160.06(11) . . ? C201 Fe2 C208 122.48(11) . . ? C202 Fe2 C208 108.61(12) . . ? C206 Fe2 C208 68.73(11) . . ? C210 Fe2 C208 68.28(12) . . ? C205 Fe2 C208 157.90(11) . . ? C209 Fe2 C208 40.58(12) . . ? C201 Fe2 C207 109.37(11) . . ? C202 Fe2 C207 126.87(11) . . ? C206 Fe2 C207 40.88(11) . . ? C210 Fe2 C207 68.46(11) . . ? C205 Fe2 C207 122.26(11) . . ? C209 Fe2 C207 68.17(11) . . ? C208 Fe2 C207 40.58(11) . . ? C201 Fe2 C204 68.63(11) . . ? C202 Fe2 C204 68.15(12) . . ? C206 Fe2 C204 119.83(12) . . ? C210 Fe2 C204 105.85(12) . . ? C205 Fe2 C204 40.63(11) . . ? C209 Fe2 C204 123.17(12) . . ? C208 Fe2 C204 160.56(12) . . ? C207 Fe2 C204 156.41(12) . . ? C201 Fe2 C203 68.77(11) . . ? C202 Fe2 C203 40.48(11) . . ? C206 Fe2 C203 154.24(12) . . ? C210 Fe2 C203 118.79(12) . . ? C205 Fe2 C203 68.41(12) . . ? C209 Fe2 C203 106.42(12) . . ? C208 Fe2 C203 124.82(12) . . ? C207 Fe2 C203 162.72(12) . . ? C204 Fe2 C203 40.33(13) . . ? C201 P2 C212 106.45(11) . . ? C201 P2 C218 104.92(12) . . ? C212 P2 C218 105.29(12) . . ? C201 P2 B2 113.58(14) . . ? C212 P2 B2 116.31(13) . . ? C218 P2 B2 109.39(13) . . ? C211 O2 C224 109.9(2) . . ? P2 B2 H4A 109.3 . . ? P2 B2 H5B 104.4 . . ? H4A B2 H5B 106.3 . . ? P2 B2 H6B 104.6 . . ? H4A B2 H6B 112.0 . . ? H5B B2 H6B 119.6 . . ? C205 C201 C202 107.3(2) . . ? C205 C201 P2 129.3(2) . . ? C202 C201 P2 123.3(2) . . ? C205 C201 Fe2 69.81(14) . . ? C202 C201 Fe2 69.52(14) . . ? P2 C201 Fe2 127.48(14) . . ? C203 C202 C201 108.4(2) . . ? C203 C202 Fe2 70.60(16) . . ? C201 C202 Fe2 69.24(14) . . ? C203 C202 H202 125.9 . . ? C201 C202 H202 125.7 . . ? Fe2 C202 H202 125.9 . . ? C202 C203 C204 107.9(2) . . ? C202 C203 Fe2 68.92(15) . . ? C204 C203 Fe2 69.65(16) . . ? C202 C203 H203 125.9 . . ? C204 C203 H203 126.2 . . ? Fe2 C203 H203 126.8 . . ? C203 C204 C205 108.6(3) . . ? C203 C204 Fe2 70.02(17) . . ? C205 C204 Fe2 69.23(15) . . ? C203 C204 H204 125.7 . . ? C205 C204 H204 125.7 . . ? Fe2 C204 H204 126.9 . . ? C204 C205 C201 107.8(2) . . ? C204 C205 Fe2 70.14(16) . . ? C201 C205 Fe2 69.14(14) . . ? C204 C205 H205 126.1 . . ? C201 C205 H205 126.0 . . ? Fe2 C205 H205 126.1 . . ? C207 C206 C210 107.3(2) . . ? C207 C206 C211 126.1(3) . . ? C210 C206 C211 126.5(3) . . ? C207 C206 Fe2 70.03(15) . . ? C210 C206 Fe2 69.50(15) . . ? C211 C206 Fe2 122.38(19) . . ? C208 C207 C206 108.1(2) . . ? C208 C207 Fe2 69.66(16) . . ? C206 C207 Fe2 69.09(15) . . ? C208 C207 H207 125.9 . . ? C206 C207 H207 126.0 . . ? Fe2 C207 H207 127.0 . . ? C209 C208 C207 107.8(2) . . ? C209 C208 Fe2 69.63(16) . . ? C207 C208 Fe2 69.77(15) . . ? C209 C208 H208 126.2 . . ? C207 C208 H208 126.0 . . ? Fe2 C208 H208 125.9 . . ? C210 C209 C208 108.4(3) . . ? C210 C209 Fe2 69.52(16) . . ? C208 C209 Fe2 69.79(16) . . ? C210 C209 H209 125.9 . . ? C208 C209 H209 125.7 . . ? Fe2 C209 H209 126.4 . . ? C209 C210 C206 108.4(3) . . ? C209 C210 Fe2 70.16(16) . . ? C206 C210 Fe2 69.46(15) . . ? C209 C210 H210 125.8 . . ? C206 C210 H210 125.9 . . ? Fe2 C210 H210 126.1 . . ? O2 C211 C206 110.3(2) . . ? O2 C211 H11C 109.5 . . ? C206 C211 H11C 109.3 . . ? O2 C211 H11D 109.8 . . ? C206 C211 H11D 109.9 . . ? H11C C211 H11D 108.1 . . ? C213 C212 C217 119.4(2) . . ? C213 C212 P2 119.8(2) . . ? C217 C212 P2 120.7(2) . . ? C212 C213 C214 120.3(3) . . ? C212 C213 H213 119.9 . . ? C214 C213 H213 119.9 . . ? C215 C214 C213 119.6(3) . . ? C215 C214 H214 120.1 . . ? C213 C214 H214 120.4 . . ? C214 C215 C216 120.9(3) . . ? C214 C215 H215 119.8 . . ? C216 C215 H215 119.3 . . ? C215 C216 C217 119.8(3) . . ? C215 C216 H216 120.2 . . ? C217 C216 H216 120.1 . . ? C216 C217 C212 120.1(3) . . ? C216 C217 H217 119.9 . . ? C212 C217 H217 120.1 . . ? C223 C218 C219 119.2(2) . . ? C223 C218 P2 121.25(19) . . ? C219 C218 P2 119.3(2) . . ? C220 C219 C218 120.4(3) . . ? C220 C219 H219 119.9 . . ? C218 C219 H219 119.7 . . ? C221 C220 C219 119.6(3) . . ? C221 C220 H220 120.2 . . ? C219 C220 H220 120.2 . . ? C222 C221 C220 120.5(3) . . ? C222 C221 H221 119.8 . . ? C220 C221 H221 119.7 . . ? C221 C222 C223 119.8(3) . . ? C221 C222 H222 120.1 . . ? C223 C222 H222 120.1 . . ? C218 C223 C222 120.5(2) . . ? C218 C223 H223 119.6 . . ? C222 C223 H223 119.9 . . ? O2 C224 H24D 110.1 . . ? O2 C224 H24E 109.7 . . ? H24D C224 H24E 109.5 . . ? O2 C224 H24F 108.6 . . ? H24D C224 H24F 109.5 . . ? H24E C224 H24F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.456 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.065 data_ps312 _database_code_depnum_ccdc_archive 'CCDC 906410' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-(diphenylphosphino)-1'-(methoxymethyl)ferrocene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H23 Fe O P' _chemical_formula_sum 'C24 H23 Fe O P' _chemical_formula_weight 414.24 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 10.8960(2) _cell_length_b 17.2531(3) _cell_length_c 10.9826(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.3430(11) _cell_angle_gamma 90.00 _cell_volume 1981.19(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4642 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 31152 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4529 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 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^)+(0.0368P)^2^+0.6031P] 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 4529 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Fe Fe 0.663523(18) -0.110329(12) 0.379183(18) 0.02291(7) Uani 1 1 d . . . P P 0.57130(3) 0.07957(2) 0.31054(3) 0.02441(9) Uani 1 1 d . . . O O 1.05256(10) -0.10127(6) 0.35068(10) 0.0296(2) Uani 1 1 d . . . C1 C 0.54743(13) -0.02384(9) 0.28424(13) 0.0244(3) Uani 1 1 d . . . C2 C 0.48183(13) -0.07102(9) 0.35392(14) 0.0279(3) Uani 1 1 d . . . H2 H 0.4471 -0.0538 0.4173 0.033 Uiso 1 1 calc R . . C3 C 0.47914(14) -0.14877(10) 0.30907(15) 0.0330(4) Uani 1 1 d . . . H3 H 0.4422 -0.1909 0.3380 0.040 Uiso 1 1 calc R . . C4 C 0.54258(14) -0.15067(9) 0.21274(14) 0.0310(3) Uani 1 1 d . . . H4 H 0.5544 -0.1943 0.1676 0.037 Uiso 1 1 calc R . . C5 C 0.58507(14) -0.07425(9) 0.19693(13) 0.0261(3) Uani 1 1 d . . . H5 H 0.6296 -0.0595 0.1398 0.031 Uiso 1 1 calc R . . C6 C 0.85624(13) -0.11330(8) 0.40621(13) 0.0242(3) Uani 1 1 d . . . C7 C 0.82583(13) -0.06036(9) 0.49335(13) 0.0258(3) Uani 1 1 d . . . H7 H 0.8454 -0.0078 0.5002 0.031 Uiso 1 1 calc R . . C8 C 0.76051(14) -0.10199(10) 0.56792(14) 0.0300(3) Uani 1 1 d . . . H8 H 0.7291 -0.0813 0.6314 0.036 Uiso 1 1 calc R . . C9 C 0.75163(14) -0.18058(10) 0.52844(14) 0.0312(3) Uani 1 1 d . . . H9 H 0.7136 -0.2205 0.5618 0.037 Uiso 1 1 calc R . . C10 C 0.81076(14) -0.18778(9) 0.42921(14) 0.0282(3) Uani 1 1 d . . . H10 H 0.8185 -0.2333 0.3865 0.034 Uiso 1 1 calc R . . C11 C 0.91674(14) -0.09312(9) 0.30452(14) 0.0271(3) Uani 1 1 d . . . H11A H 0.8841 -0.1270 0.2321 0.033 Uiso 1 1 calc R . . H11B H 0.8954 -0.0402 0.2770 0.033 Uiso 1 1 calc R . . C12 C 0.42772(13) 0.11743(8) 0.19324(13) 0.0238(3) Uani 1 1 d . . . C13 C 0.41639(15) 0.19759(9) 0.17399(16) 0.0332(3) Uani 1 1 d . . . H13 H 0.4829 0.2299 0.2167 0.040 Uiso 1 1 calc R . . C14 C 0.30711(16) 0.22949(10) 0.09202(16) 0.0371(4) Uani 1 1 d . . . H14 H 0.3014 0.2828 0.0790 0.045 Uiso 1 1 calc R . . C15 C 0.20673(15) 0.18193(10) 0.02972(15) 0.0335(4) Uani 1 1 d . . . H15 H 0.1329 0.2032 -0.0243 0.040 Uiso 1 1 calc R . . C16 C 0.21659(15) 0.10281(9) 0.04804(15) 0.0310(3) Uani 1 1 d . . . H16 H 0.1494 0.0708 0.0059 0.037 Uiso 1 1 calc R . . C17 C 0.32630(14) 0.07073(9) 0.12906(13) 0.0261(3) Uani 1 1 d . . . H17 H 0.3319 0.0173 0.1405 0.031 Uiso 1 1 calc R . . C18 C 0.69480(13) 0.10070(8) 0.23119(13) 0.0232(3) Uani 1 1 d . . . C19 C 0.81616(14) 0.12211(8) 0.30601(15) 0.0281(3) Uani 1 1 d . . . H19 H 0.8322 0.1256 0.3936 0.034 Uiso 1 1 calc R . . C20 C 0.91323(15) 0.13826(9) 0.25038(17) 0.0341(4) Uani 1 1 d . . . H20 H 0.9939 0.1522 0.3010 0.041 Uiso 1 1 calc R . . C21 C 0.89040(15) 0.13369(10) 0.12030(17) 0.0355(4) Uani 1 1 d . . . H21 H 0.9557 0.1442 0.0835 0.043 Uiso 1 1 calc R . . C22 C 0.76944(16) 0.11324(9) 0.04433(16) 0.0316(3) Uani 1 1 d . . . H22 H 0.7536 0.1106 -0.0433 0.038 Uiso 1 1 calc R . . C23 C 0.67280(14) 0.09684(9) 0.09970(14) 0.0266(3) Uani 1 1 d . . . H23 H 0.5922 0.0831 0.0487 0.032 Uiso 1 1 calc R . . C24 C 1.11134(16) -0.08163(12) 0.25522(17) 0.0421(4) Uani 1 1 d . . . H24A H 1.0848 -0.1176 0.1860 0.063 Uiso 1 1 calc R . . H24B H 1.2026 -0.0839 0.2896 0.063 Uiso 1 1 calc R . . H24C H 1.0865 -0.0301 0.2252 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.01904(11) 0.02832(12) 0.02098(12) 0.00268(8) 0.00497(8) -0.00063(8) P 0.02249(18) 0.0309(2) 0.02059(18) -0.00081(14) 0.00722(14) -0.00059(15) O 0.0195(5) 0.0407(6) 0.0293(6) 0.0008(4) 0.0082(4) 0.0001(4) C1 0.0188(6) 0.0318(8) 0.0215(7) 0.0031(6) 0.0042(5) 0.0006(6) C2 0.0182(7) 0.0383(9) 0.0273(7) 0.0059(6) 0.0066(6) 0.0003(6) C3 0.0218(7) 0.0362(9) 0.0374(9) 0.0068(7) 0.0026(6) -0.0055(6) C4 0.0286(8) 0.0319(8) 0.0272(8) -0.0011(6) -0.0008(6) -0.0026(6) C5 0.0245(7) 0.0326(8) 0.0199(7) 0.0019(6) 0.0042(6) -0.0003(6) C6 0.0189(7) 0.0301(8) 0.0225(7) 0.0018(6) 0.0038(5) 0.0018(6) C7 0.0207(7) 0.0318(8) 0.0227(7) -0.0004(6) 0.0022(5) 0.0001(6) C8 0.0239(7) 0.0468(9) 0.0187(7) 0.0016(6) 0.0052(6) 0.0019(7) C9 0.0260(7) 0.0374(9) 0.0285(8) 0.0113(6) 0.0048(6) 0.0001(6) C10 0.0250(7) 0.0292(8) 0.0288(8) 0.0038(6) 0.0050(6) 0.0025(6) C11 0.0209(7) 0.0350(8) 0.0256(7) 0.0017(6) 0.0067(6) 0.0010(6) C12 0.0212(7) 0.0304(8) 0.0226(7) -0.0003(5) 0.0107(6) 0.0007(6) C13 0.0267(8) 0.0309(8) 0.0421(9) -0.0006(7) 0.0096(7) -0.0032(6) C14 0.0353(9) 0.0299(8) 0.0468(10) 0.0053(7) 0.0128(7) 0.0036(7) C15 0.0274(8) 0.0403(9) 0.0328(8) 0.0042(7) 0.0083(6) 0.0082(7) C16 0.0268(8) 0.0379(9) 0.0277(8) -0.0030(6) 0.0066(6) -0.0014(6) C17 0.0273(7) 0.0275(8) 0.0253(7) -0.0007(6) 0.0103(6) 0.0012(6) C18 0.0202(7) 0.0237(7) 0.0256(7) 0.0001(5) 0.0063(6) -0.0004(5) C19 0.0256(7) 0.0259(7) 0.0291(8) 0.0015(6) 0.0015(6) -0.0010(6) C20 0.0198(7) 0.0299(8) 0.0488(10) 0.0039(7) 0.0035(7) -0.0020(6) C21 0.0269(8) 0.0318(8) 0.0541(11) 0.0027(7) 0.0216(7) 0.0000(7) C22 0.0371(9) 0.0311(8) 0.0310(8) -0.0021(6) 0.0169(7) -0.0022(7) C23 0.0240(7) 0.0302(8) 0.0258(7) -0.0018(6) 0.0071(6) -0.0035(6) C24 0.0270(8) 0.0618(12) 0.0422(10) -0.0002(9) 0.0176(7) -0.0035(8) _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 Fe C2 2.0365(14) . ? Fe C6 2.0370(14) . ? Fe C5 2.0400(14) . ? Fe C10 2.0408(15) . ? Fe C1 2.0424(14) . ? Fe C9 2.0475(15) . ? Fe C7 2.0482(14) . ? Fe C3 2.0490(15) . ? Fe C8 2.0497(15) . ? Fe C4 2.0511(14) . ? P C1 1.8144(16) . ? P C18 1.8339(15) . ? P C12 1.8438(15) . ? O C24 1.4149(19) . ? O C11 1.4299(17) . ? C1 C5 1.437(2) . ? C1 C2 1.438(2) . ? C2 C3 1.427(2) . ? C2 H2 0.9300 . ? C3 C4 1.418(2) . ? C3 H3 0.9300 . ? C4 C5 1.424(2) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.425(2) . ? C6 C7 1.428(2) . ? C6 C11 1.489(2) . ? C7 C8 1.422(2) . ? C7 H7 0.9300 . ? C8 C9 1.419(2) . ? C8 H8 0.9300 . ? C9 C10 1.419(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.389(2) . ? C12 C13 1.399(2) . ? C13 C14 1.388(2) . ? C13 H13 0.9300 . ? C14 C15 1.384(2) . ? C14 H14 0.9300 . ? C15 C16 1.380(2) . ? C15 H15 0.9300 . ? C16 C17 1.389(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.396(2) . ? C18 C23 1.397(2) . ? C19 C20 1.390(2) . ? C19 H19 0.9300 . ? C20 C21 1.382(2) . ? C20 H20 0.9300 . ? C21 C22 1.392(2) . ? C21 H21 0.9300 . ? C22 C23 1.385(2) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 C2 Fe C6 161.99(6) . . ? C2 Fe C5 69.01(6) . . ? C6 Fe C5 106.31(6) . . ? C2 Fe C10 156.23(6) . . ? C6 Fe C10 40.91(6) . . ? C5 Fe C10 122.99(6) . . ? C2 Fe C1 41.28(6) . . ? C6 Fe C1 123.90(6) . . ? C5 Fe C1 41.22(6) . . ? C10 Fe C1 160.52(6) . . ? C2 Fe C9 121.67(6) . . ? C6 Fe C9 68.69(6) . . ? C5 Fe C9 159.85(7) . . ? C10 Fe C9 40.61(6) . . ? C1 Fe C9 157.63(6) . . ? C2 Fe C7 125.59(6) . . ? C6 Fe C7 40.91(6) . . ? C5 Fe C7 121.57(6) . . ? C10 Fe C7 68.46(6) . . ? C1 Fe C7 108.00(6) . . ? C9 Fe C7 68.25(6) . . ? C2 Fe C3 40.87(7) . . ? C6 Fe C3 155.25(7) . . ? C5 Fe C3 68.54(6) . . ? C10 Fe C3 120.17(6) . . ? C1 Fe C3 69.13(6) . . ? C9 Fe C3 107.37(6) . . ? C7 Fe C3 162.31(6) . . ? C2 Fe C8 108.61(6) . . ? C6 Fe C8 68.74(6) . . ? C5 Fe C8 157.71(6) . . ? C10 Fe C8 68.36(6) . . ? C1 Fe C8 122.27(6) . . ? C9 Fe C8 40.51(6) . . ? C7 Fe C8 40.60(6) . . ? C3 Fe C8 125.08(6) . . ? C2 Fe C4 68.62(6) . . ? C6 Fe C4 119.92(6) . . ? C5 Fe C4 40.74(6) . . ? C10 Fe C4 106.08(6) . . ? C1 Fe C4 69.06(6) . . ? C9 Fe C4 123.48(6) . . ? C7 Fe C4 156.34(6) . . ? C3 Fe C4 40.46(7) . . ? C8 Fe C4 160.78(6) . . ? C1 P C18 102.20(6) . . ? C1 P C12 100.47(6) . . ? C18 P C12 100.91(6) . . ? C24 O C11 110.66(12) . . ? C5 C1 C2 106.89(13) . . ? C5 C1 P 130.26(11) . . ? C2 C1 P 122.85(11) . . ? C5 C1 Fe 69.30(8) . . ? C2 C1 Fe 69.14(8) . . ? P C1 Fe 126.64(7) . . ? C3 C2 C1 108.27(13) . . ? C3 C2 Fe 70.04(9) . . ? C1 C2 Fe 69.58(8) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe C2 H2 126.1 . . ? C4 C3 C2 108.21(14) . . ? C4 C3 Fe 69.85(8) . . ? C2 C3 Fe 69.09(8) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe C3 H3 126.7 . . ? C3 C4 C5 108.25(14) . . ? C3 C4 Fe 69.69(9) . . ? C5 C4 Fe 69.21(8) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe C4 H4 126.8 . . ? C4 C5 C1 108.38(13) . . ? C4 C5 Fe 70.05(8) . . ? C1 C5 Fe 69.48(8) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? Fe C5 H5 126.2 . . ? C10 C6 C7 107.47(13) . . ? C10 C6 C11 126.38(14) . . ? C7 C6 C11 126.04(13) . . ? C10 C6 Fe 69.69(8) . . ? C7 C6 Fe 69.97(8) . . ? C11 C6 Fe 122.72(10) . . ? C8 C7 C6 108.13(13) . . ? C8 C7 Fe 69.76(8) . . ? C6 C7 Fe 69.12(8) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe C7 H7 126.8 . . ? C9 C8 C7 107.99(13) . . ? C9 C8 Fe 69.66(8) . . ? C7 C8 Fe 69.64(8) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? Fe C8 H8 126.3 . . ? C8 C9 C10 108.17(14) . . ? C8 C9 Fe 69.83(9) . . ? C10 C9 Fe 69.44(8) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe C9 H9 126.4 . . ? C9 C10 C6 108.24(14) . . ? C9 C10 Fe 69.94(9) . . ? C6 C10 Fe 69.40(8) . . ? C9 C10 H10 125.9 . . ? C6 C10 H10 125.9 . . ? Fe C10 H10 126.3 . . ? O C11 C6 110.09(12) . . ? O C11 H11A 109.6 . . ? C6 C11 H11A 109.6 . . ? O C11 H11B 109.6 . . ? C6 C11 H11B 109.6 . . ? H11A C11 H11B 108.2 . . ? C17 C12 C13 118.22(14) . . ? C17 C12 P 123.13(11) . . ? C13 C12 P 118.51(11) . . ? C14 C13 C12 120.86(15) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.97(15) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 119.75(15) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.36(15) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.83(14) . . ? C16 C17 H17 119.6 . . ? C12 C17 H17 119.6 . . ? C19 C18 C23 118.66(14) . . ? C19 C18 P 118.24(11) . . ? C23 C18 P 123.10(11) . . ? C20 C19 C18 120.41(14) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.33(14) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.91(14) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 119.80(15) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 120.89(14) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? O C24 H24A 109.5 . . ? O C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.271 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.049 data_ps314a _database_code_depnum_ccdc_archive 'CCDC 906411' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H37 Cl2 Fe O P Ru' _chemical_formula_sum 'C34 H37 Cl2 Fe O P Ru' _chemical_formula_weight 722.27 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.7055(8) _cell_length_b 10.2413(11) _cell_length_c 30.665(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.795(8) _cell_angle_gamma 90.00 _cell_volume 3012.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30359 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 26.0 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 1.287 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 1 0.031 -1 0 -1 0.024 0 0 -1 0.124 0 0 1 0.100 0 -1 0 0.056 0 1 0 0.042 0 1 -3 0.074 0 -1 3 0.071 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_reflns_number 33228 _diffrn_reflns_av_R_equivalents 0.0952 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5871 _reflns_number_gt 4416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 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^)+(0.0201P)^2^+10.5681P] 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 5871 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Ru Ru 0.93167(5) 0.80471(4) 0.058577(13) 0.02499(12) Uani 1 1 d . . . Cl1 Cl 1.14871(14) 0.90787(13) 0.08818(4) 0.0320(3) Uani 1 1 d . . . Cl2 Cl 0.81273(14) 0.99850(12) 0.07728(4) 0.0311(3) Uani 1 1 d . . . Fe Fe 0.62677(8) 0.81693(7) 0.17982(2) 0.02807(19) Uani 1 1 d . . . P P 0.91662(14) 0.72636(12) 0.13021(4) 0.0217(3) Uani 1 1 d . . . O O 0.4547(4) 1.2044(4) 0.14398(15) 0.0453(10) Uani 1 1 d . . . C1 C 0.7420(5) 0.7068(5) 0.14288(17) 0.0263(11) Uani 1 1 d . . . C2 C 0.6165(5) 0.7480(5) 0.11713(18) 0.0288(12) Uani 1 1 d . . . H2 H 0.6098 0.7981 0.0916 0.035 Uiso 1 1 calc R . . C3 C 0.5019(6) 0.7007(6) 0.1363(2) 0.0402(14) Uani 1 1 d . . . H3 H 0.4079 0.7140 0.1257 0.048 Uiso 1 1 calc R . . C4 C 0.5567(7) 0.6300(5) 0.1743(2) 0.0430(16) Uani 1 1 d . . . H4 H 0.5047 0.5881 0.1932 0.052 Uiso 1 1 calc R . . C5 C 0.7036(6) 0.6329(5) 0.17910(19) 0.0352(14) Uani 1 1 d . . . H5 H 0.7648 0.5940 0.2017 0.042 Uiso 1 1 calc R . . C6 C 0.5603(6) 1.0065(5) 0.17722(19) 0.0309(13) Uani 1 1 d . . . C7 C 0.4977(6) 0.9350(6) 0.2091(2) 0.0431(16) Uani 1 1 d . . . H7 H 0.4025 0.9241 0.2089 0.052 Uiso 1 1 calc R . . C8 C 0.6041(7) 0.8838(6) 0.2410(2) 0.0477(17) Uani 1 1 d . . . H8 H 0.5910 0.8324 0.2650 0.057 Uiso 1 1 calc R . . C9 C 0.7345(7) 0.9241(6) 0.23013(18) 0.0393(14) Uani 1 1 d . . . H9 H 0.8219 0.9046 0.2458 0.047 Uiso 1 1 calc R . . C10 C 0.7069(6) 0.9999(5) 0.19092(18) 0.0319(13) Uani 1 1 d . . . H10 H 0.7739 1.0389 0.1765 0.038 Uiso 1 1 calc R . . C11 C 0.4872(6) 1.0712(5) 0.1368(2) 0.0385(14) Uani 1 1 d . . . H11A H 0.5457 1.0666 0.1138 0.046 Uiso 1 1 calc R . . H11B H 0.4017 1.0242 0.1265 0.046 Uiso 1 1 calc R . . C12 C 1.0130(5) 0.8048(5) 0.17885(16) 0.0259(11) Uani 1 1 d . . . C13 C 1.0367(5) 0.9394(5) 0.17885(17) 0.0278(12) Uani 1 1 d . . . H13 H 1.0061 0.9882 0.1536 0.033 Uiso 1 1 calc R . . C14 C 1.1055(6) 1.0005(6) 0.21630(18) 0.0336(13) Uani 1 1 d . . . H14 H 1.1201 1.0903 0.2163 0.040 Uiso 1 1 calc R . . C15 C 1.1523(6) 0.9279(6) 0.25342(19) 0.0405(15) Uani 1 1 d . . . H15 H 1.2008 0.9687 0.2782 0.049 Uiso 1 1 calc R . . C16 C 1.1278(6) 0.7950(6) 0.25421(18) 0.0394(14) Uani 1 1 d . . . H16 H 1.1572 0.7468 0.2796 0.047 Uiso 1 1 calc R . . C17 C 1.0594(6) 0.7351(6) 0.21697(17) 0.0342(13) Uani 1 1 d . . . H17 H 1.0439 0.6455 0.2174 0.041 Uiso 1 1 calc R . . C18 C 0.9865(6) 0.5596(5) 0.13363(16) 0.0275(12) Uani 1 1 d . . . C19 C 1.1301(6) 0.5437(6) 0.13610(17) 0.0333(13) Uani 1 1 d . . . H19 H 1.1885 0.6161 0.1403 0.040 Uiso 1 1 calc R . . C20 C 1.1859(7) 0.4215(6) 0.13236(18) 0.0401(15) Uani 1 1 d . . . H20 H 1.2818 0.4123 0.1340 0.048 Uiso 1 1 calc R . . C21 C 1.1022(7) 0.3132(6) 0.12625(19) 0.0450(16) Uani 1 1 d . . . H21 H 1.1414 0.2312 0.1238 0.054 Uiso 1 1 calc R . . C22 C 0.9591(7) 0.3263(5) 0.1237(2) 0.0468(17) Uani 1 1 d . . . H22 H 0.9014 0.2535 0.1192 0.056 Uiso 1 1 calc R . . C23 C 0.9029(7) 0.4497(5) 0.12796(19) 0.0389(15) Uani 1 1 d . . . H23 H 0.8071 0.4585 0.1270 0.047 Uiso 1 1 calc R . . C24 C 0.5752(7) 1.2819(5) 0.1533(3) 0.0557(19) Uani 1 1 d . . . H24A H 0.5489 1.3718 0.1554 0.083 Uiso 1 1 calc R . . H24B H 0.6306 1.2723 0.1302 0.083 Uiso 1 1 calc R . . H24C H 0.6284 1.2546 0.1808 0.083 Uiso 1 1 calc R . . C25 C 0.7601(6) 0.7297(6) 0.00745(18) 0.0420(15) Uani 1 1 d . . . C26 C 0.8333(7) 0.6276(6) 0.03041(17) 0.0415(16) Uani 1 1 d . . . H26 H 0.7853 0.5669 0.0449 0.050 Uiso 1 1 calc R . . C27 C 0.9791(8) 0.6141(6) 0.03215(19) 0.0445(16) Uani 1 1 d . . . H27 H 1.0259 0.5434 0.0466 0.053 Uiso 1 1 calc R . . C28 C 1.0525(7) 0.7092(6) 0.0117(2) 0.0464(16) Uani 1 1 d . . . C29 C 0.9791(8) 0.8128(6) -0.01046(18) 0.0457(17) Uani 1 1 d . . . H29 H 1.0272 0.8749 -0.0244 0.055 Uiso 1 1 calc R . . C30 C 0.8371(7) 0.8253(6) -0.01225(18) 0.0422(15) Uani 1 1 d . . . H30 H 0.7912 0.8969 -0.0264 0.051 Uiso 1 1 calc R . . C31 C 0.6029(8) 0.7267(9) 0.0008(2) 0.063(2) Uani 1 1 d . . . H31 H 0.5717 0.6856 0.0264 0.075 Uiso 1 1 calc R . . C32 C 0.5423(10) 0.8552(12) -0.0056(4) 0.115(4) Uani 1 1 d . . . H32A H 0.4428 0.8489 -0.0078 0.172 Uiso 1 1 calc R . . H32B H 0.5657 0.8924 -0.0323 0.172 Uiso 1 1 calc R . . H32C H 0.5781 0.9097 0.0190 0.172 Uiso 1 1 calc R . . C33 C 0.5520(10) 0.6445(13) -0.0409(3) 0.126(5) Uani 1 1 d . . . H33A H 0.5869 0.5570 -0.0366 0.189 Uiso 1 1 calc R . . H33B H 0.5855 0.6827 -0.0658 0.189 Uiso 1 1 calc R . . H33C H 0.4519 0.6429 -0.0460 0.189 Uiso 1 1 calc R . . C34 C 1.2076(8) 0.6970(9) 0.0146(3) 0.083(3) Uani 1 1 d . . . H34A H 1.2417 0.6332 0.0365 0.124 Uiso 1 1 calc R . . H34B H 1.2505 0.7798 0.0226 0.124 Uiso 1 1 calc R . . H34C H 1.2299 0.6702 -0.0135 0.124 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 Ru 0.0314(2) 0.0232(2) 0.0222(2) 0.00023(19) 0.00999(17) -0.0063(2) Cl1 0.0304(7) 0.0363(7) 0.0317(7) -0.0034(6) 0.0120(6) -0.0104(6) Cl2 0.0344(7) 0.0263(6) 0.0340(7) 0.0047(6) 0.0100(6) -0.0004(6) Fe 0.0319(4) 0.0231(4) 0.0332(4) 0.0001(3) 0.0175(3) 0.0011(3) P 0.0267(7) 0.0177(6) 0.0229(7) 0.0001(5) 0.0105(5) -0.0001(5) O 0.037(2) 0.025(2) 0.073(3) -0.004(2) 0.006(2) 0.0069(19) C1 0.034(3) 0.014(2) 0.035(3) -0.001(2) 0.019(2) -0.003(2) C2 0.031(3) 0.027(3) 0.031(3) -0.005(2) 0.010(2) -0.002(2) C3 0.034(3) 0.031(3) 0.059(4) -0.014(3) 0.021(3) -0.004(3) C4 0.048(4) 0.028(3) 0.061(4) -0.002(3) 0.036(3) -0.007(3) C5 0.045(4) 0.022(3) 0.044(3) 0.006(2) 0.022(3) 0.004(3) C6 0.026(3) 0.023(3) 0.046(3) -0.012(2) 0.012(3) 0.005(2) C7 0.033(3) 0.040(3) 0.064(4) -0.011(3) 0.031(3) 0.005(3) C8 0.066(5) 0.040(4) 0.043(4) -0.005(3) 0.028(3) 0.006(3) C9 0.048(4) 0.040(3) 0.030(3) -0.010(3) 0.006(3) 0.007(3) C10 0.036(3) 0.025(3) 0.037(3) -0.011(2) 0.011(3) -0.001(2) C11 0.031(3) 0.022(3) 0.061(4) -0.010(3) 0.002(3) 0.001(2) C12 0.028(3) 0.028(3) 0.025(3) -0.002(2) 0.014(2) -0.001(2) C13 0.027(3) 0.032(3) 0.026(3) -0.003(2) 0.010(2) 0.001(2) C14 0.034(3) 0.034(3) 0.035(3) -0.009(3) 0.011(3) -0.003(3) C15 0.027(3) 0.063(4) 0.031(3) -0.018(3) 0.004(3) 0.007(3) C16 0.042(4) 0.052(4) 0.024(3) -0.002(3) 0.007(3) 0.014(3) C17 0.041(3) 0.035(3) 0.029(3) -0.002(2) 0.014(3) 0.008(3) C18 0.036(3) 0.026(3) 0.023(3) 0.003(2) 0.011(2) 0.002(2) C19 0.036(3) 0.035(3) 0.030(3) -0.005(2) 0.009(3) 0.002(3) C20 0.042(4) 0.048(4) 0.030(3) -0.010(3) 0.004(3) 0.020(3) C21 0.070(5) 0.028(3) 0.041(4) -0.003(3) 0.018(3) 0.020(3) C22 0.066(5) 0.020(3) 0.060(4) -0.004(3) 0.027(4) -0.001(3) C23 0.045(4) 0.029(3) 0.049(4) 0.002(3) 0.026(3) 0.006(3) C24 0.045(4) 0.021(3) 0.097(6) -0.009(3) -0.001(4) -0.001(3) C25 0.043(4) 0.057(4) 0.025(3) -0.003(3) 0.004(3) -0.017(3) C26 0.071(5) 0.032(3) 0.020(3) -0.004(2) 0.004(3) -0.023(3) C27 0.078(5) 0.027(3) 0.030(3) -0.011(3) 0.010(3) -0.002(3) C28 0.056(4) 0.050(4) 0.037(3) -0.027(3) 0.017(3) -0.011(3) C29 0.080(5) 0.039(3) 0.025(3) -0.006(3) 0.026(3) -0.022(4) C30 0.058(4) 0.043(4) 0.023(3) 0.006(3) 0.000(3) -0.003(3) C31 0.045(4) 0.091(6) 0.048(4) -0.001(4) -0.005(3) -0.001(4) C32 0.066(7) 0.164(12) 0.112(8) 0.004(8) 0.003(6) -0.020(7) C33 0.074(7) 0.241(14) 0.060(5) -0.040(7) -0.003(5) -0.068(8) C34 0.055(5) 0.104(7) 0.098(6) -0.063(6) 0.040(5) -0.008(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 Ru C26 2.167(5) . ? Ru C27 2.190(6) . ? Ru C28 2.217(6) . ? Ru C30 2.235(6) . ? Ru C29 2.236(5) . ? Ru C25 2.241(6) . ? Ru P 2.3640(13) . ? Ru Cl1 2.4068(14) . ? Ru Cl2 2.4089(14) . ? Fe C5 2.028(5) . ? Fe C4 2.030(6) . ? Fe C2 2.036(5) . ? Fe C10 2.037(5) . ? Fe C8 2.039(6) . ? Fe C3 2.043(6) . ? Fe C6 2.044(5) . ? Fe C7 2.045(5) . ? Fe C9 2.046(6) . ? Fe C1 2.048(5) . ? P C1 1.807(5) . ? P C12 1.822(5) . ? P C18 1.835(5) . ? O C24 1.407(7) . ? O C11 1.425(6) . ? C1 C2 1.411(7) . ? C1 C5 1.439(7) . ? C2 C3 1.420(7) . ? C2 H2 0.9300 . ? C3 C4 1.405(9) . ? C3 H3 0.9300 . ? C4 C5 1.411(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.422(7) . ? C6 C7 1.429(8) . ? C6 C11 1.487(8) . ? C7 C8 1.410(9) . ? C7 H7 0.9300 . ? C8 C9 1.418(9) . ? C8 H8 0.9300 . ? C9 C10 1.422(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.385(7) . ? C12 C13 1.398(7) . ? C13 C14 1.386(7) . ? C13 H13 0.9300 . ? C14 C15 1.377(8) . ? C14 H14 0.9300 . ? C15 C16 1.383(9) . ? C15 H15 0.9300 . ? C16 C17 1.375(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.383(8) . ? C18 C19 1.394(7) . ? C19 C20 1.375(8) . ? C19 H19 0.9300 . ? C20 C21 1.370(9) . ? C20 H20 0.9300 . ? C21 C22 1.386(9) . ? C21 H21 0.9300 . ? C22 C23 1.391(8) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.393(9) . ? C25 C30 1.422(8) . ? C25 C31 1.508(9) . ? C26 C27 1.415(9) . ? C26 H26 0.9300 . ? C27 C28 1.410(9) . ? C27 H27 0.9300 . ? C28 C29 1.395(9) . ? C28 C34 1.499(9) . ? C29 C30 1.377(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.443(13) . ? C31 C33 1.546(11) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? 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 C26 Ru C27 37.9(2) . . ? C26 Ru C28 67.5(2) . . ? C27 Ru C28 37.3(2) . . ? C26 Ru C30 66.5(2) . . ? C27 Ru C30 78.6(2) . . ? C28 Ru C30 65.9(2) . . ? C26 Ru C29 78.2(2) . . ? C27 Ru C29 66.2(2) . . ? C28 Ru C29 36.5(2) . . ? C30 Ru C29 35.9(2) . . ? C26 Ru C25 36.8(2) . . ? C27 Ru C25 67.1(3) . . ? C28 Ru C25 78.8(2) . . ? C30 Ru C25 37.0(2) . . ? C29 Ru C25 65.7(2) . . ? C26 Ru P 90.01(15) . . ? C27 Ru P 95.03(16) . . ? C28 Ru P 124.54(19) . . ? C30 Ru P 149.37(17) . . ? C29 Ru P 160.62(18) . . ? C25 Ru P 112.88(15) . . ? C26 Ru Cl1 145.5(2) . . ? C27 Ru Cl1 108.02(19) . . ? C28 Ru Cl1 85.35(17) . . ? C30 Ru Cl1 122.06(17) . . ? C29 Ru Cl1 92.63(17) . . ? C25 Ru Cl1 158.15(15) . . ? P Ru Cl1 88.48(5) . . ? C26 Ru Cl2 125.9(2) . . ? C27 Ru Cl2 163.39(19) . . ? C28 Ru Cl2 146.94(19) . . ? C30 Ru Cl2 90.74(17) . . ? C29 Ru Cl2 111.74(18) . . ? C25 Ru Cl2 96.73(18) . . ? P Ru Cl2 87.62(4) . . ? Cl1 Ru Cl2 88.41(5) . . ? C5 Fe C4 40.7(2) . . ? C5 Fe C2 68.4(2) . . ? C4 Fe C2 68.1(2) . . ? C5 Fe C10 136.5(2) . . ? C4 Fe C10 174.7(3) . . ? C2 Fe C10 116.1(2) . . ? C5 Fe C8 114.4(2) . . ? C4 Fe C8 108.2(3) . . ? C2 Fe C8 171.1(3) . . ? C10 Fe C8 68.3(2) . . ? C5 Fe C3 68.5(3) . . ? C4 Fe C3 40.4(2) . . ? C2 Fe C3 40.8(2) . . ? C10 Fe C3 144.9(2) . . ? C8 Fe C3 131.3(3) . . ? C5 Fe C6 175.4(2) . . ? C4 Fe C6 142.5(2) . . ? C2 Fe C6 108.8(2) . . ? C10 Fe C6 40.8(2) . . ? C8 Fe C6 68.8(2) . . ? C3 Fe C6 112.1(2) . . ? C5 Fe C7 143.6(2) . . ? C4 Fe C7 112.0(2) . . ? C2 Fe C7 132.4(3) . . ? C10 Fe C7 68.1(2) . . ? C8 Fe C7 40.4(3) . . ? C3 Fe C7 106.8(2) . . ? C6 Fe C7 40.9(2) . . ? C5 Fe C9 111.1(2) . . ? C4 Fe C9 134.0(3) . . ? C2 Fe C9 147.5(2) . . ? C10 Fe C9 40.8(2) . . ? C8 Fe C9 40.6(2) . . ? C3 Fe C9 171.6(2) . . ? C6 Fe C9 69.0(2) . . ? C7 Fe C9 68.2(3) . . ? C5 Fe C1 41.4(2) . . ? C4 Fe C1 68.8(2) . . ? C2 Fe C1 40.4(2) . . ? C10 Fe C1 111.8(2) . . ? C8 Fe C1 147.0(3) . . ? C3 Fe C1 68.8(2) . . ? C6 Fe C1 134.2(2) . . ? C7 Fe C1 172.6(3) . . ? C9 Fe C1 116.9(2) . . ? C1 P C12 104.7(2) . . ? C1 P C18 103.6(2) . . ? C12 P C18 103.0(2) . . ? C1 P Ru 115.51(18) . . ? C12 P Ru 120.95(17) . . ? C18 P Ru 107.11(16) . . ? C24 O C11 112.0(4) . . ? C2 C1 C5 106.6(5) . . ? C2 C1 P 127.2(4) . . ? C5 C1 P 125.9(4) . . ? C2 C1 Fe 69.3(3) . . ? C5 C1 Fe 68.6(3) . . ? P C1 Fe 131.9(3) . . ? C1 C2 C3 109.3(5) . . ? C1 C2 Fe 70.2(3) . . ? C3 C2 Fe 69.9(3) . . ? C1 C2 H2 125.4 . . ? C3 C2 H2 125.4 . . ? Fe C2 H2 126.1 . . ? C4 C3 C2 107.3(5) . . ? C4 C3 Fe 69.3(4) . . ? C2 C3 Fe 69.4(3) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? Fe C3 H3 126.5 . . ? C3 C4 C5 108.9(5) . . ? C3 C4 Fe 70.3(3) . . ? C5 C4 Fe 69.6(3) . . ? C3 C4 H4 125.5 . . ? C5 C4 H4 125.5 . . ? Fe C4 H4 126.2 . . ? C4 C5 C1 107.9(5) . . ? C4 C5 Fe 69.7(3) . . ? C1 C5 Fe 70.0(3) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe C5 H5 125.8 . . ? C10 C6 C7 106.5(5) . . ? C10 C6 C11 126.6(5) . . ? C7 C6 C11 126.9(5) . . ? C10 C6 Fe 69.4(3) . . ? C7 C6 Fe 69.6(3) . . ? C11 C6 Fe 124.3(4) . . ? C8 C7 C6 108.8(5) . . ? C8 C7 Fe 69.6(3) . . ? C6 C7 Fe 69.5(3) . . ? C8 C7 H7 125.6 . . ? C6 C7 H7 125.6 . . ? Fe C7 H7 126.9 . . ? C7 C8 C9 108.4(6) . . ? C7 C8 Fe 70.0(3) . . ? C9 C8 Fe 69.9(3) . . ? C7 C8 H8 125.8 . . ? C9 C8 H8 125.8 . . ? Fe C8 H8 125.8 . . ? C8 C9 C10 107.3(6) . . ? C8 C9 Fe 69.4(4) . . ? C10 C9 Fe 69.3(3) . . ? C8 C9 H9 126.4 . . ? C10 C9 H9 126.4 . . ? Fe C9 H9 126.5 . . ? C9 C10 C6 109.1(5) . . ? C9 C10 Fe 69.9(3) . . ? C6 C10 Fe 69.9(3) . . ? C9 C10 H10 125.5 . . ? C6 C10 H10 125.5 . . ? Fe C10 H10 126.3 . . ? O C11 C6 112.7(5) . . ? O C11 H11A 109.1 . . ? C6 C11 H11A 109.1 . . ? O C11 H11B 109.1 . . ? C6 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C17 C12 C13 118.4(5) . . ? C17 C12 P 121.6(4) . . ? C13 C12 P 119.9(4) . . ? C14 C13 C12 120.3(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 119.8(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.7(6) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.2(6) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C12 121.6(5) . . ? C16 C17 H17 119.2 . . ? C12 C17 H17 119.2 . . ? C23 C18 C19 118.3(5) . . ? C23 C18 P 123.1(4) . . ? C19 C18 P 118.0(4) . . ? C20 C19 C18 120.3(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 121.0(6) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.8(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 119.1(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C18 C23 C22 121.3(6) . . ? C18 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? O C24 H24A 109.5 . . ? O C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 118.1(6) . . ? C26 C25 C31 118.7(6) . . ? C30 C25 C31 122.9(6) . . ? C26 C25 Ru 68.7(3) . . ? C30 C25 Ru 71.3(3) . . ? C31 C25 Ru 136.9(5) . . ? C25 C26 C27 121.5(6) . . ? C25 C26 Ru 74.5(3) . . ? C27 C26 Ru 71.9(3) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? Ru C26 H26 126.2 . . ? C28 C27 C26 119.1(6) . . ? C28 C27 Ru 72.4(3) . . ? C26 C27 Ru 70.2(3) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? Ru C27 H27 129.2 . . ? C29 C28 C27 119.1(6) . . ? C29 C28 C34 121.7(7) . . ? C27 C28 C34 119.2(7) . . ? C29 C28 Ru 72.5(3) . . ? C27 C28 Ru 70.3(3) . . ? C34 C28 Ru 128.6(4) . . ? C30 C29 C28 121.6(6) . . ? C30 C29 Ru 72.0(3) . . ? C28 C29 Ru 71.0(3) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? Ru C29 H29 130.5 . . ? C29 C30 C25 120.4(6) . . ? C29 C30 Ru 72.1(3) . . ? C25 C30 Ru 71.7(3) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? Ru C30 H30 128.7 . . ? C32 C31 C25 112.5(7) . . ? C32 C31 C33 108.2(8) . . ? C25 C31 C33 108.2(7) . . ? C32 C31 H31 109.3 . . ? C25 C31 H31 109.3 . . ? C33 C31 H31 109.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C28 C34 H34A 109.5 . . ? C28 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C28 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.911 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.110 data_ps314b _database_code_depnum_ccdc_archive 'CCDC 906412' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 Cl Fe N O P Ru, Sb F6, 0.5 (C H Cl3)' _chemical_formula_sum 'C36.50 H40.50 Cl2.50 F6 Fe N O P Ru Sb' _chemical_formula_weight 1021.46 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' Ru Ru -1.2594 0.8363 '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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.5750(7) _cell_length_b 13.9675(8) _cell_length_c 14.6000(8) _cell_angle_alpha 96.764(4) _cell_angle_beta 97.044(5) _cell_angle_gamma 111.478(6) _cell_volume 1960.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40516 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 1.700 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.669 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43999 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8948 _reflns_number_gt 7819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 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^)+(0.0195P)^2^+4.2072P] 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 8948 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.48588(2) 0.928813(15) 0.234149(14) 0.01477(5) Uani 1 1 d . . . Fe Fe 0.02763(4) 0.72431(3) 0.37646(3) 0.01745(8) Uani 1 1 d . . . Cl Cl 0.52534(8) 0.82760(5) 0.10535(5) 0.02702(15) Uani 1 1 d . . . P P 0.29313(7) 0.77761(5) 0.23927(5) 0.01599(13) Uani 1 1 d . . . N N 0.3615(2) 0.96229(17) 0.13534(15) 0.0199(5) Uani 1 1 d . . . O O -0.2250(2) 0.46901(17) 0.50151(17) 0.0337(5) Uani 1 1 d . . . C1 C 0.2189(3) 0.79152(19) 0.34257(18) 0.0167(5) Uani 1 1 d . . . C2 C 0.2249(3) 0.7381(2) 0.42088(18) 0.0195(5) Uani 1 1 d . . . H2 H 0.2554 0.6837 0.4230 0.023 Uiso 1 1 calc R . . C3 C 0.1762(3) 0.7830(2) 0.49411(19) 0.0247(6) Uani 1 1 d . . . H3 H 0.1690 0.7628 0.5523 0.030 Uiso 1 1 calc R . . C4 C 0.1406(3) 0.8638(2) 0.4637(2) 0.0269(6) Uani 1 1 d . . . H4 H 0.1060 0.9057 0.4984 0.032 Uiso 1 1 calc R . . C5 C 0.1666(3) 0.8698(2) 0.3711(2) 0.0226(6) Uani 1 1 d . . . H5 H 0.1522 0.9166 0.3348 0.027 Uiso 1 1 calc R . . C6 C -0.1298(3) 0.6108(2) 0.4169(2) 0.0229(6) Uani 1 1 d . . . C7 C -0.1701(3) 0.6935(2) 0.3954(2) 0.0278(6) Uani 1 1 d . . . H7 H -0.1989 0.7344 0.4362 0.033 Uiso 1 1 calc R . . C8 C -0.1586(3) 0.7025(3) 0.3004(2) 0.0313(7) Uani 1 1 d . . . H8 H -0.1775 0.7509 0.2685 0.038 Uiso 1 1 calc R . . C9 C -0.1134(3) 0.6252(2) 0.2628(2) 0.0285(6) Uani 1 1 d . . . H9 H -0.0983 0.6133 0.2019 0.034 Uiso 1 1 calc R . . C10 C -0.0952(3) 0.5690(2) 0.3349(2) 0.0250(6) Uani 1 1 d . . . H10 H -0.0655 0.5139 0.3292 0.030 Uiso 1 1 calc R . . C11 C -0.1254(3) 0.5722(2) 0.5084(2) 0.0283(6) Uani 1 1 d . . . H11A H -0.0340 0.5733 0.5286 0.034 Uiso 1 1 calc R . . H11B H -0.1423 0.6189 0.5555 0.034 Uiso 1 1 calc R . . C12 C 0.1558(3) 0.7426(2) 0.13831(19) 0.0234(6) Uani 1 1 d . . . C13 C 0.0632(3) 0.7926(3) 0.1341(2) 0.0313(7) Uani 1 1 d . . . H13 H 0.0704 0.8437 0.1838 0.038 Uiso 1 1 calc R . . C14 C -0.0402(4) 0.7659(3) 0.0554(3) 0.0441(9) Uani 1 1 d . . . H14 H -0.1024 0.7988 0.0530 0.053 Uiso 1 1 calc R . . C15 C -0.0506(4) 0.6909(3) -0.0188(3) 0.0497(11) Uani 1 1 d . . . H15 H -0.1200 0.6729 -0.0709 0.060 Uiso 1 1 calc R . . C16 C 0.0419(4) 0.6430(3) -0.0154(2) 0.0484(10) Uani 1 1 d . . . H16 H 0.0349 0.5928 -0.0658 0.058 Uiso 1 1 calc R . . C17 C 0.1466(3) 0.6682(3) 0.0626(2) 0.0331(7) Uani 1 1 d . . . H17 H 0.2094 0.6358 0.0638 0.040 Uiso 1 1 calc R . . C18 C 0.3232(3) 0.6578(2) 0.24444(18) 0.0196(5) Uani 1 1 d . . . C19 C 0.4538(3) 0.6559(2) 0.2513(2) 0.0236(6) Uani 1 1 d . . . H19 H 0.5294 0.7167 0.2510 0.028 Uiso 1 1 calc R . . C20 C 0.4728(3) 0.5635(2) 0.2586(2) 0.0303(6) Uani 1 1 d . . . H20 H 0.5608 0.5625 0.2625 0.036 Uiso 1 1 calc R . . C21 C 0.3612(4) 0.4733(2) 0.2600(2) 0.0332(7) Uani 1 1 d . . . H21 H 0.3745 0.4119 0.2662 0.040 Uiso 1 1 calc R . . C22 C 0.2295(3) 0.4737(2) 0.2523(2) 0.0293(6) Uani 1 1 d . . . H22 H 0.1543 0.4127 0.2527 0.035 Uiso 1 1 calc R . . C23 C 0.2101(3) 0.5655(2) 0.2440(2) 0.0250(6) Uani 1 1 d . . . H23 H 0.1216 0.5657 0.2382 0.030 Uiso 1 1 calc R . . C24 C -0.3612(4) 0.4656(3) 0.4857(3) 0.0453(9) Uani 1 1 d . . . H24A H -0.4251 0.3966 0.4878 0.068 Uiso 1 1 calc R . . H24B H -0.3807 0.4828 0.4252 0.068 Uiso 1 1 calc R . . H24C H -0.3704 0.5150 0.5332 0.068 Uiso 1 1 calc R . . C25 C 0.6190(3) 1.1019(2) 0.26964(19) 0.0223(6) Uani 1 1 d . . . C26 C 0.7037(3) 1.0456(2) 0.2613(2) 0.0239(6) Uani 1 1 d . . . H26 H 0.7678 1.0618 0.2214 0.029 Uiso 1 1 calc R . . C27 C 0.6930(3) 0.9636(2) 0.3135(2) 0.0232(6) Uani 1 1 d . . . H27 H 0.7482 0.9257 0.3051 0.028 Uiso 1 1 calc R . . C28 C 0.6014(3) 0.9385(2) 0.37704(18) 0.0196(5) Uani 1 1 d . . . C29 C 0.5109(3) 0.9930(2) 0.38207(18) 0.0188(5) Uani 1 1 d . . . H29 H 0.4456 0.9758 0.4210 0.023 Uiso 1 1 calc R . . C30 C 0.5188(3) 1.0720(2) 0.32927(19) 0.0209(5) Uani 1 1 d . . . H30 H 0.4577 1.1056 0.3331 0.025 Uiso 1 1 calc R . . C31 C 0.6217(4) 1.1865(2) 0.2128(2) 0.0338(7) Uani 1 1 d . . . H31 H 0.5265 1.1810 0.1955 0.041 Uiso 1 1 calc R . . C32 C 0.7044(5) 1.2933(3) 0.2747(3) 0.0584(13) Uani 1 1 d . . . H32A H 0.7032 1.3474 0.2401 0.088 Uiso 1 1 calc R . . H32B H 0.7980 1.3003 0.2935 0.088 Uiso 1 1 calc R . . H32C H 0.6637 1.2992 0.3293 0.088 Uiso 1 1 calc R . . C33 C 0.6783(4) 1.1765(3) 0.1228(3) 0.0512(10) Uani 1 1 d . . . H33A H 0.6682 1.2275 0.0870 0.077 Uiso 1 1 calc R . . H33B H 0.6281 1.1077 0.0868 0.077 Uiso 1 1 calc R . . H33C H 0.7743 1.1881 0.1380 0.077 Uiso 1 1 calc R . . C34 C 0.6002(3) 0.8595(2) 0.4387(2) 0.0286(6) Uani 1 1 d . . . H34A H 0.5091 0.8271 0.4523 0.043 Uiso 1 1 calc R . . H34B H 0.6645 0.8937 0.4961 0.043 Uiso 1 1 calc R . . H34C H 0.6263 0.8073 0.4070 0.043 Uiso 1 1 calc R . . C35 C 0.2968(3) 0.9876(2) 0.08342(19) 0.0231(6) Uani 1 1 d . . . C36 C 0.2123(3) 1.0207(3) 0.0184(2) 0.0353(7) Uani 1 1 d . . . H36A H 0.1406 0.9603 -0.0204 0.053 Uiso 1 1 calc R . . H36B H 0.2689 1.0624 -0.0202 0.053 Uiso 1 1 calc R . . H36C H 0.1717 1.0611 0.0530 0.053 Uiso 1 1 calc R . . Sb Sb 0.116669(19) 1.146482(14) 0.282025(14) 0.02341(5) Uani 1 1 d . . . F1 F 0.2261(2) 1.06921(17) 0.26690(17) 0.0459(5) Uani 1 1 d . . . F2 F 0.1924(3) 1.21889(19) 0.19013(17) 0.0625(7) Uani 1 1 d . . . F3 F 0.2560(2) 1.2460(2) 0.37342(17) 0.0599(7) Uani 1 1 d . . . F4 F 0.0414(3) 1.0717(2) 0.3724(2) 0.0708(8) Uani 1 1 d . . . F5 F -0.0209(2) 1.04642(19) 0.18952(19) 0.0642(8) Uani 1 1 d . . . F6 F 0.0057(2) 1.22275(18) 0.2957(2) 0.0593(7) Uani 1 1 d . . . C90 C 0.4882(9) 1.4150(7) -0.0041(5) 0.0491(19) Uani 0.50 1 d P . . H90 H 0.4819 1.3696 -0.0624 0.059 Uiso 0.50 1 d PR . . Cl91 Cl 0.4167(3) 1.33243(19) 0.07470(15) 0.0620(6) Uani 0.50 1 d P . . Cl92 Cl 0.6616(4) 1.4894(3) 0.0376(3) 0.0931(8) Uani 0.50 1 d P . . Cl93 Cl 0.3909(4) 1.4860(3) -0.0300(3) 0.0931(8) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01362(10) 0.01336(10) 0.01396(10) 0.00156(7) 0.00148(7) 0.00192(7) Fe 0.01431(17) 0.01579(18) 0.01871(18) 0.00311(14) 0.00178(14) 0.00210(14) Cl 0.0324(4) 0.0234(3) 0.0223(3) -0.0001(3) 0.0110(3) 0.0068(3) P 0.0144(3) 0.0141(3) 0.0158(3) 0.0028(2) 0.0008(2) 0.0018(2) N 0.0188(11) 0.0171(11) 0.0182(11) 0.0037(9) 0.0027(9) 0.0007(9) O 0.0344(12) 0.0284(11) 0.0432(13) 0.0194(10) 0.0140(10) 0.0115(10) C1 0.0130(11) 0.0148(12) 0.0183(12) 0.0037(9) 0.0011(9) 0.0012(9) C2 0.0157(12) 0.0194(13) 0.0183(12) 0.0028(10) -0.0019(9) 0.0027(10) C3 0.0187(13) 0.0291(15) 0.0165(12) -0.0015(11) -0.0005(10) 0.0007(11) C4 0.0217(14) 0.0202(13) 0.0312(15) -0.0053(11) 0.0054(11) 0.0021(11) C5 0.0183(13) 0.0143(12) 0.0317(15) 0.0029(11) 0.0029(11) 0.0032(10) C6 0.0161(12) 0.0213(13) 0.0257(14) 0.0050(11) 0.0046(10) 0.0002(10) C7 0.0168(13) 0.0306(16) 0.0367(16) 0.0109(13) 0.0073(12) 0.0077(12) C8 0.0174(13) 0.0355(17) 0.0367(17) 0.0170(14) -0.0013(12) 0.0039(12) C9 0.0189(13) 0.0300(16) 0.0218(14) 0.0028(12) -0.0009(11) -0.0056(12) C10 0.0215(13) 0.0174(13) 0.0269(14) 0.0027(11) 0.0040(11) -0.0026(11) C11 0.0305(16) 0.0270(15) 0.0277(15) 0.0074(12) 0.0065(12) 0.0104(13) C12 0.0191(13) 0.0215(13) 0.0202(13) 0.0093(11) -0.0006(10) -0.0034(10) C13 0.0247(15) 0.0312(16) 0.0314(16) 0.0128(13) -0.0018(12) 0.0031(13) C14 0.0295(17) 0.048(2) 0.047(2) 0.0270(18) -0.0080(15) 0.0045(15) C15 0.041(2) 0.047(2) 0.0358(19) 0.0196(17) -0.0176(16) -0.0077(17) C16 0.057(2) 0.041(2) 0.0232(16) 0.0037(14) -0.0105(16) -0.0022(18) C17 0.0364(17) 0.0297(16) 0.0201(14) 0.0035(12) -0.0024(12) 0.0005(13) C18 0.0255(14) 0.0145(12) 0.0161(12) 0.0009(10) 0.0028(10) 0.0053(10) C19 0.0219(14) 0.0185(13) 0.0253(14) 0.0011(11) 0.0027(11) 0.0033(11) C20 0.0268(15) 0.0255(15) 0.0370(17) 0.0030(13) 0.0030(13) 0.0100(12) C21 0.0402(18) 0.0194(14) 0.0403(18) 0.0041(13) 0.0059(14) 0.0127(13) C22 0.0328(16) 0.0159(13) 0.0344(16) 0.0042(12) 0.0081(13) 0.0034(12) C23 0.0248(14) 0.0197(13) 0.0280(14) 0.0024(11) 0.0072(11) 0.0052(11) C24 0.0309(18) 0.054(2) 0.052(2) 0.0281(19) 0.0156(16) 0.0096(16) C25 0.0223(13) 0.0138(12) 0.0200(13) 0.0008(10) -0.0025(10) -0.0026(10) C26 0.0140(12) 0.0239(14) 0.0247(14) 0.0006(11) 0.0022(10) -0.0018(10) C27 0.0152(12) 0.0245(14) 0.0247(14) -0.0011(11) -0.0025(10) 0.0052(11) C28 0.0159(12) 0.0185(12) 0.0175(12) 0.0005(10) -0.0056(9) 0.0023(10) C29 0.0172(12) 0.0191(13) 0.0146(11) -0.0016(10) -0.0007(9) 0.0031(10) C30 0.0200(13) 0.0189(13) 0.0194(12) -0.0018(10) -0.0026(10) 0.0058(10) C31 0.0396(18) 0.0194(14) 0.0290(16) 0.0080(12) -0.0067(13) -0.0010(13) C32 0.079(3) 0.0192(16) 0.052(2) 0.0078(16) -0.022(2) 0.0008(18) C33 0.052(2) 0.056(2) 0.038(2) 0.0255(18) 0.0093(17) 0.0070(19) C34 0.0294(15) 0.0265(15) 0.0244(14) 0.0056(12) -0.0066(12) 0.0079(12) C35 0.0216(13) 0.0230(14) 0.0214(13) 0.0061(11) 0.0046(11) 0.0039(11) C36 0.0310(16) 0.049(2) 0.0331(17) 0.0232(15) 0.0054(13) 0.0184(15) Sb 0.01975(9) 0.01959(10) 0.03110(11) 0.00439(7) 0.00362(7) 0.00815(7) F1 0.0392(11) 0.0458(12) 0.0704(15) 0.0222(11) 0.0218(10) 0.0294(10) F2 0.093(2) 0.0480(14) 0.0547(14) 0.0318(12) 0.0259(14) 0.0261(14) F3 0.0398(12) 0.0638(16) 0.0548(14) -0.0151(12) -0.0094(10) 0.0089(11) F4 0.090(2) 0.0656(17) 0.0784(18) 0.0379(15) 0.0601(17) 0.0332(15) F5 0.0342(12) 0.0557(15) 0.0784(18) -0.0347(13) -0.0087(11) 0.0096(11) F6 0.0405(12) 0.0425(13) 0.0940(19) -0.0144(12) -0.0027(12) 0.0275(11) C90 0.056(5) 0.062(5) 0.036(4) -0.001(4) 0.006(3) 0.033(4) Cl91 0.0831(16) 0.0599(13) 0.0478(11) 0.0032(10) 0.0278(11) 0.0300(12) Cl92 0.065(2) 0.0873(19) 0.1177(17) -0.0015(14) 0.0181(18) 0.0237(12) Cl93 0.065(2) 0.0873(19) 0.1177(17) -0.0015(14) 0.0181(18) 0.0237(12) _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 Ru N 2.043(2) . ? Ru C29 2.183(3) . ? Ru C30 2.184(3) . ? Ru C27 2.200(3) . ? Ru C26 2.236(3) . ? Ru C28 2.247(2) . ? Ru C25 2.265(3) . ? Ru P 2.3543(7) . ? Ru Cl 2.3890(7) . ? Fe C7 2.036(3) . ? Fe C8 2.037(3) . ? Fe C2 2.038(3) . ? Fe C3 2.038(3) . ? Fe C6 2.040(3) . ? Fe C5 2.044(3) . ? Fe C1 2.045(3) . ? Fe C4 2.045(3) . ? Fe C10 2.048(3) . ? Fe C9 2.057(3) . ? P C1 1.806(3) . ? P C12 1.818(3) . ? P C18 1.823(3) . ? N C35 1.131(4) . ? O C24 1.413(4) . ? O C11 1.423(4) . ? C1 C5 1.438(4) . ? C1 C2 1.444(4) . ? C2 C3 1.420(4) . ? C2 H2 0.9300 . ? C3 C4 1.415(4) . ? C3 H3 0.9300 . ? C4 C5 1.419(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.417(4) . ? C6 C7 1.424(4) . ? C6 C11 1.501(4) . ? C7 C8 1.423(4) . ? C7 H7 0.9300 . ? C8 C9 1.413(5) . ? C8 H8 0.9300 . ? C9 C10 1.420(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.393(4) . ? C12 C13 1.395(4) . ? C13 C14 1.396(4) . ? C13 H13 0.9300 . ? C14 C15 1.379(6) . ? C14 H14 0.9300 . ? C15 C16 1.372(6) . ? C15 H15 0.9300 . ? C16 C17 1.398(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.383(4) . ? C18 C23 1.400(4) . ? C19 C20 1.391(4) . ? C19 H19 0.9300 . ? C20 C21 1.380(4) . ? C20 H20 0.9300 . ? C21 C22 1.387(5) . ? C21 H21 0.9300 . ? C22 C23 1.386(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.398(4) . ? C25 C30 1.430(4) . ? C25 C31 1.516(4) . ? C26 C27 1.427(4) . ? C26 H26 0.9300 . ? C27 C28 1.404(4) . ? C27 H27 0.9300 . ? C28 C29 1.427(4) . ? C28 C34 1.501(4) . ? C29 C30 1.403(4) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C33 1.521(5) . ? C31 C32 1.530(4) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.453(4) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? Sb F4 1.855(2) . ? Sb F2 1.858(2) . ? Sb F3 1.862(2) . ? Sb F6 1.864(2) . ? Sb F1 1.8642(19) . ? Sb F5 1.865(2) . ? C90 Cl93 1.477(10) 2_685 ? C90 Cl93 1.710(9) . ? C90 Cl92 1.731(9) . ? C90 Cl91 1.765(9) . ? C90 H90 0.9800 . ? Cl92 Cl93 0.757(4) 2_685 ? Cl93 Cl92 0.757(4) 2_685 ? Cl93 C90 1.477(10) 2_685 ? Cl93 Cl93 2.237(8) 2_685 ? 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 N Ru C29 119.99(10) . . ? N Ru C30 90.94(10) . . ? C29 Ru C30 37.49(10) . . ? N Ru C27 149.50(10) . . ? C29 Ru C27 66.88(10) . . ? C30 Ru C27 79.20(10) . . ? N Ru C26 112.15(10) . . ? C29 Ru C26 78.96(10) . . ? C30 Ru C26 66.44(11) . . ? C27 Ru C26 37.53(11) . . ? N Ru C28 157.32(10) . . ? C29 Ru C28 37.54(10) . . ? C30 Ru C28 67.60(10) . . ? C27 Ru C28 36.79(10) . . ? C26 Ru C28 67.01(10) . . ? N Ru C25 87.90(9) . . ? C29 Ru C25 67.38(10) . . ? C30 Ru C25 37.44(10) . . ? C27 Ru C25 66.71(10) . . ? C26 Ru C25 36.19(11) . . ? C28 Ru C25 79.40(10) . . ? N Ru P 87.54(6) . . ? C29 Ru P 93.68(7) . . ? C30 Ru P 117.78(8) . . ? C27 Ru P 122.64(8) . . ? C26 Ru P 160.15(8) . . ? C28 Ru P 95.92(7) . . ? C25 Ru P 154.68(8) . . ? N Ru Cl 85.49(7) . . ? C29 Ru Cl 154.52(7) . . ? C30 Ru Cl 155.22(8) . . ? C27 Ru Cl 91.57(8) . . ? C26 Ru Cl 92.25(8) . . ? C28 Ru Cl 117.04(7) . . ? C25 Ru Cl 117.82(8) . . ? P Ru Cl 86.61(3) . . ? C7 Fe C8 40.89(13) . . ? C7 Fe C2 152.13(12) . . ? C8 Fe C2 165.90(12) . . ? C7 Fe C3 116.34(12) . . ? C8 Fe C3 152.65(13) . . ? C2 Fe C3 40.76(11) . . ? C7 Fe C6 40.91(12) . . ? C8 Fe C6 68.72(12) . . ? C2 Fe C6 118.43(11) . . ? C3 Fe C6 103.79(12) . . ? C7 Fe C5 123.90(12) . . ? C8 Fe C5 108.95(12) . . ? C2 Fe C5 68.89(11) . . ? C3 Fe C5 68.42(12) . . ? C6 Fe C5 159.38(12) . . ? C7 Fe C1 163.09(11) . . ? C8 Fe C1 127.86(12) . . ? C2 Fe C1 41.43(10) . . ? C3 Fe C1 69.23(11) . . ? C6 Fe C1 155.85(11) . . ? C5 Fe C1 41.19(11) . . ? C7 Fe C4 104.12(13) . . ? C8 Fe C4 119.50(13) . . ? C2 Fe C4 68.58(12) . . ? C3 Fe C4 40.53(12) . . ? C6 Fe C4 121.33(12) . . ? C5 Fe C4 40.61(12) . . ? C1 Fe C4 69.12(11) . . ? C7 Fe C10 68.29(13) . . ? C8 Fe C10 68.12(13) . . ? C2 Fe C10 108.64(12) . . ? C3 Fe C10 124.04(12) . . ? C6 Fe C10 40.57(11) . . ? C5 Fe C10 159.25(12) . . ? C1 Fe C10 123.26(11) . . ? C4 Fe C10 159.35(12) . . ? C7 Fe C9 68.34(13) . . ? C8 Fe C9 40.39(14) . . ? C2 Fe C9 128.40(12) . . ? C3 Fe C9 162.97(13) . . ? C6 Fe C9 68.40(12) . . ? C5 Fe C9 123.99(12) . . ? C1 Fe C9 111.37(11) . . ? C4 Fe C9 156.46(13) . . ? C10 Fe C9 40.45(12) . . ? C1 P C12 107.14(13) . . ? C1 P C18 102.65(12) . . ? C12 P C18 104.02(13) . . ? C1 P Ru 112.08(8) . . ? C12 P Ru 113.07(9) . . ? C18 P Ru 116.86(9) . . ? C35 N Ru 175.5(2) . . ? C24 O C11 111.7(3) . . ? C5 C1 C2 106.5(2) . . ? C5 C1 P 127.1(2) . . ? C2 C1 P 125.5(2) . . ? C5 C1 Fe 69.37(15) . . ? C2 C1 Fe 69.05(14) . . ? P C1 Fe 134.82(14) . . ? C3 C2 C1 108.2(2) . . ? C3 C2 Fe 69.63(16) . . ? C1 C2 Fe 69.53(14) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe C2 H2 126.5 . . ? C4 C3 C2 108.5(3) . . ? C4 C3 Fe 69.99(16) . . ? C2 C3 Fe 69.62(15) . . ? C4 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? Fe C3 H3 126.2 . . ? C3 C4 C5 108.2(3) . . ? C3 C4 Fe 69.48(16) . . ? C5 C4 Fe 69.64(16) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe C4 H4 126.6 . . ? C4 C5 C1 108.6(2) . . ? C4 C5 Fe 69.75(16) . . ? C1 C5 Fe 69.45(15) . . ? C4 C5 H5 125.7 . . ? C1 C5 H5 125.7 . . ? Fe C5 H5 126.7 . . ? C10 C6 C7 107.6(3) . . ? C10 C6 C11 125.1(3) . . ? C7 C6 C11 127.3(3) . . ? C10 C6 Fe 70.04(15) . . ? C7 C6 Fe 69.41(16) . . ? C11 C6 Fe 126.5(2) . . ? C8 C7 C6 107.8(3) . . ? C8 C7 Fe 69.57(17) . . ? C6 C7 Fe 69.69(16) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe C7 H7 126.2 . . ? C9 C8 C7 108.3(3) . . ? C9 C8 Fe 70.59(17) . . ? C7 C8 Fe 69.54(17) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe C8 H8 125.6 . . ? C8 C9 C10 107.7(3) . . ? C8 C9 Fe 69.02(17) . . ? C10 C9 Fe 69.43(16) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe C9 H9 127.0 . . ? C6 C10 C9 108.6(3) . . ? C6 C10 Fe 69.40(16) . . ? C9 C10 Fe 70.11(16) . . ? C6 C10 H10 125.7 . . ? C9 C10 H10 125.7 . . ? Fe C10 H10 126.3 . . ? O C11 C6 112.1(2) . . ? O C11 H11A 109.2 . . ? C6 C11 H11A 109.2 . . ? O C11 H11B 109.2 . . ? C6 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C17 C12 C13 119.6(3) . . ? C17 C12 P 119.6(2) . . ? C13 C12 P 120.7(2) . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 119.7(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.2(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C12 C17 C16 119.2(4) . . ? C12 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C23 119.3(3) . . ? C19 C18 P 122.2(2) . . ? C23 C18 P 118.4(2) . . ? C18 C19 C20 120.3(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.3(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 120.2(3) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? O C24 H24A 109.5 . . ? O C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 117.8(3) . . ? C26 C25 C31 122.9(3) . . ? C30 C25 C31 119.2(3) . . ? C26 C25 Ru 70.77(15) . . ? C30 C25 Ru 68.20(15) . . ? C31 C25 Ru 128.52(19) . . ? C25 C26 C27 120.7(3) . . ? C25 C26 Ru 73.04(15) . . ? C27 C26 Ru 69.89(15) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? Ru C26 H26 130.0 . . ? C28 C27 C26 121.8(3) . . ? C28 C27 Ru 73.42(15) . . ? C26 C27 Ru 72.58(15) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? Ru C27 H27 127.0 . . ? C27 C28 C29 117.1(2) . . ? C27 C28 C34 121.7(3) . . ? C29 C28 C34 121.2(3) . . ? C27 C28 Ru 69.78(15) . . ? C29 C28 Ru 68.80(14) . . ? C34 C28 Ru 133.74(19) . . ? C30 C29 C28 121.1(3) . . ? C30 C29 Ru 71.26(15) . . ? C28 C29 Ru 73.65(15) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? Ru C29 H29 127.8 . . ? C29 C30 C25 121.2(3) . . ? C29 C30 Ru 71.25(15) . . ? C25 C30 Ru 74.36(16) . . ? C29 C30 H30 119.4 . . ? C25 C30 H30 119.4 . . ? Ru C30 H30 127.0 . . ? C25 C31 C33 113.5(3) . . ? C25 C31 C32 108.9(3) . . ? C33 C31 C32 111.0(3) . . ? C25 C31 H31 107.7 . . ? C33 C31 H31 107.7 . . ? C32 C31 H31 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C28 C34 H34A 109.5 . . ? C28 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C28 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N C35 C36 178.7(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? F4 Sb F2 178.79(12) . . ? F4 Sb F3 90.90(13) . . ? F2 Sb F3 89.76(12) . . ? F4 Sb F6 89.75(13) . . ? F2 Sb F6 91.25(13) . . ? F3 Sb F6 90.04(11) . . ? F4 Sb F1 90.43(11) . . ? F2 Sb F1 88.56(11) . . ? F3 Sb F1 90.67(11) . . ? F6 Sb F1 179.26(11) . . ? F4 Sb F5 89.58(14) . . ? F2 Sb F5 89.74(13) . . ? F3 Sb F5 179.13(11) . . ? F6 Sb F5 90.68(11) . . ? F1 Sb F5 88.61(11) . . ? Cl93 C90 Cl93 88.9(5) 2_685 . ? Cl93 C90 Cl92 114.5(6) . . ? Cl93 C90 Cl91 120.4(5) 2_685 . ? Cl93 C90 Cl91 110.1(5) . . ? Cl92 C90 Cl91 110.8(5) . . ? Cl93 C90 H90 121.0 2_685 . ? Cl93 C90 H90 107.1 . . ? Cl92 C90 H90 107.3 . . ? Cl91 C90 H90 106.8 . . ? Cl93 Cl92 C90 58.0(6) 2_685 . ? Cl92 Cl93 C90 96.2(7) 2_685 2_685 ? Cl92 Cl93 C90 169.8(8) 2_685 . ? C90 Cl93 C90 91.1(5) 2_685 . ? Cl92 Cl93 Cl93 145.4(7) 2_685 2_685 ? C90 Cl93 Cl93 49.8(4) 2_685 2_685 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.426 _refine_diff_density_min -1.617 _refine_diff_density_rms 0.094 data_ps333b _database_code_depnum_ccdc_archive 'CCDC 906413' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H46 Cl2 Fe2 O2 P2 Pd' _chemical_formula_sum 'C48 H46 Cl2 Fe2 O2 P2 Pd' _chemical_formula_weight 1005.79 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.4772(3) _cell_length_b 9.1167(2) _cell_length_c 17.3793(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.4850(10) _cell_angle_gamma 90.00 _cell_volume 2111.98(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17048 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.341 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 13 -1 0.120 0 -13 1 0.140 1 0 1 0.050 -1 0 -1 0.040 -1 0 1 0.070 1 0 -1 0.050 -1 -2 1 0.121 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 29903 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4854 _reflns_number_gt 3943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 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^)+(0.0406P)^2^+0.2840P] 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 4854 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Pd Pd 0.0000 0.0000 0.0000 0.01689(8) Uani 1 2 d S . . Fe Fe 0.25608(2) 0.33186(3) 0.087311(17) 0.01964(9) Uani 1 1 d . . . P P 0.15511(4) 0.05544(6) -0.03831(3) 0.01696(13) Uani 1 1 d . . . O O 0.02529(13) 0.43086(19) 0.22857(9) 0.0342(4) Uani 1 1 d . . . ClA Cl 0.0565(3) -0.2000(3) 0.06918(19) 0.0396(5) Uani 0.405(3) 1 d P . . ClB Cl 0.05644(16) -0.2322(2) 0.03809(13) 0.0396(5) Uani 0.60 1 d P . . C1 C 0.21470(16) 0.2315(2) -0.01702(12) 0.0193(4) Uani 1 1 d . . . C2 C 0.32182(17) 0.2512(2) -0.00211(12) 0.0216(5) Uani 1 1 d . . . H2 H 0.3698 0.1773 0.0009 0.026 Uiso 1 1 calc R . . C3 C 0.34093(17) 0.4039(2) 0.00725(13) 0.0240(5) Uani 1 1 d . . . H3 H 0.4040 0.4470 0.0178 0.029 Uiso 1 1 calc R . . C4 C 0.24806(18) 0.4798(2) -0.00216(13) 0.0237(5) Uani 1 1 d . . . H4 H 0.2397 0.5808 0.0007 0.028 Uiso 1 1 calc R . . C5 C 0.17016(17) 0.3742(2) -0.01679(12) 0.0219(5) Uani 1 1 d . . . H5 H 0.1018 0.3942 -0.0249 0.026 Uiso 1 1 calc R . . C6 C 0.16787(18) 0.3729(2) 0.17030(12) 0.0243(5) Uani 1 1 d . . . C7 C 0.19727(18) 0.2224(2) 0.17245(12) 0.0243(5) Uani 1 1 d . . . H7 H 0.1540 0.1425 0.1656 0.029 Uiso 1 1 calc R . . C8 C 0.30349(18) 0.2149(3) 0.18680(13) 0.0292(5) Uani 1 1 d . . . H8 H 0.3419 0.1297 0.1906 0.035 Uiso 1 1 calc R . . C9 C 0.34054(19) 0.3603(3) 0.19427(14) 0.0330(6) Uani 1 1 d . . . H9 H 0.4078 0.3874 0.2041 0.040 Uiso 1 1 calc R . . C10 C 0.2580(2) 0.4572(3) 0.18428(14) 0.0302(6) Uani 1 1 d . . . H10 H 0.2618 0.5590 0.1864 0.036 Uiso 1 1 calc R . . C11 C 0.06427(19) 0.4330(3) 0.15670(13) 0.0285(5) Uani 1 1 d . . . H11A H 0.0651 0.5327 0.1373 0.034 Uiso 1 1 calc R . . H11B H 0.0224 0.3740 0.1183 0.034 Uiso 1 1 calc R . . C12 C 0.14254(16) 0.0399(2) -0.14395(12) 0.0200(5) Uani 1 1 d . . . C13 C 0.09155(17) -0.0801(3) -0.17967(13) 0.0265(5) Uani 1 1 d . . . H13 H 0.0610 -0.1464 -0.1499 0.032 Uiso 1 1 calc R . . C14 C 0.08566(19) -0.1021(3) -0.25876(14) 0.0337(6) Uani 1 1 d . . . H14 H 0.0514 -0.1828 -0.2821 0.040 Uiso 1 1 calc R . . C15 C 0.1309(2) -0.0038(3) -0.30334(14) 0.0337(6) Uani 1 1 d . . . H15 H 0.1277 -0.0191 -0.3565 0.040 Uiso 1 1 calc R . . C16 C 0.18037(19) 0.1163(3) -0.26895(13) 0.0312(6) Uani 1 1 d . . . H16 H 0.2097 0.1831 -0.2992 0.037 Uiso 1 1 calc R . . C17 C 0.18716(17) 0.1391(2) -0.18910(13) 0.0242(5) Uani 1 1 d . . . H17 H 0.2213 0.2203 -0.1661 0.029 Uiso 1 1 calc R . . C18 C 0.25987(16) -0.0675(2) -0.00542(12) 0.0189(4) Uani 1 1 d . . . C19 C 0.32367(16) -0.1182(2) -0.05622(13) 0.0227(5) Uani 1 1 d . . . H19 H 0.3092 -0.0975 -0.1091 0.027 Uiso 1 1 calc R . . C20 C 0.40830(17) -0.1991(2) -0.02806(14) 0.0273(5) Uani 1 1 d . . . H20 H 0.4506 -0.2322 -0.0620 0.033 Uiso 1 1 calc R . . C21 C 0.42996(17) -0.2305(2) 0.05044(14) 0.0269(5) Uani 1 1 d . . . H21 H 0.4870 -0.2844 0.0692 0.032 Uiso 1 1 calc R . . C22 C 0.36710(17) -0.1822(2) 0.10120(14) 0.0253(5) Uani 1 1 d . . . H22 H 0.3819 -0.2036 0.1540 0.030 Uiso 1 1 calc R . . C23 C 0.28210(17) -0.1019(2) 0.07338(12) 0.0221(5) Uani 1 1 d . . . H23 H 0.2395 -0.0707 0.1076 0.027 Uiso 1 1 calc R . . C24 C -0.0624(2) 0.5161(4) 0.2248(2) 0.0606(10) Uani 1 1 d . . . H24A H -0.0478 0.6157 0.2125 0.091 Uiso 1 1 calc R . . H24B H -0.0864 0.5131 0.2741 0.091 Uiso 1 1 calc R . . H24C H -0.1129 0.4777 0.1852 0.091 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 Pd 0.01772(13) 0.01639(13) 0.01701(13) 0.00183(9) 0.00399(9) 0.00015(9) Fe 0.02298(18) 0.01957(17) 0.01667(17) -0.00082(12) 0.00394(13) -0.00192(12) P 0.0178(3) 0.0178(3) 0.0157(3) 0.0009(2) 0.0038(2) 0.0000(2) O 0.0351(10) 0.0427(10) 0.0280(9) 0.0061(8) 0.0153(8) 0.0118(8) ClA 0.0235(4) 0.0164(9) 0.0789(16) 0.0138(7) 0.0074(10) 0.0029(5) ClB 0.0235(4) 0.0164(9) 0.0789(16) 0.0138(7) 0.0074(10) 0.0029(5) C1 0.0213(12) 0.0221(11) 0.0148(10) 0.0001(8) 0.0038(9) -0.0025(9) C2 0.0223(12) 0.0211(11) 0.0224(11) -0.0037(9) 0.0067(9) -0.0024(9) C3 0.0249(12) 0.0257(12) 0.0233(12) -0.0016(9) 0.0097(10) -0.0061(9) C4 0.0342(14) 0.0182(11) 0.0197(12) 0.0020(9) 0.0069(10) -0.0013(9) C5 0.0237(12) 0.0258(12) 0.0160(11) 0.0027(9) 0.0021(9) 0.0018(9) C6 0.0304(13) 0.0274(12) 0.0165(11) 0.0005(9) 0.0082(9) 0.0019(10) C7 0.0322(13) 0.0250(12) 0.0166(11) 0.0024(9) 0.0066(10) -0.0016(10) C8 0.0338(14) 0.0344(13) 0.0189(11) 0.0040(10) 0.0020(10) 0.0054(11) C9 0.0293(14) 0.0489(16) 0.0194(12) -0.0072(11) -0.0008(10) -0.0064(11) C10 0.0439(16) 0.0278(12) 0.0203(12) -0.0095(10) 0.0095(11) -0.0076(11) C11 0.0371(14) 0.0290(13) 0.0216(12) 0.0065(10) 0.0116(11) 0.0057(10) C12 0.0193(11) 0.0214(11) 0.0192(11) -0.0008(9) 0.0021(9) 0.0038(8) C13 0.0270(13) 0.0293(13) 0.0235(12) 0.0002(10) 0.0041(10) -0.0054(9) C14 0.0352(15) 0.0368(14) 0.0275(13) -0.0093(11) -0.0007(11) -0.0022(11) C15 0.0418(16) 0.0434(16) 0.0156(12) -0.0034(10) 0.0033(11) 0.0070(12) C16 0.0379(15) 0.0347(13) 0.0226(12) 0.0070(10) 0.0094(11) 0.0044(11) C17 0.0294(13) 0.0228(11) 0.0209(11) 0.0002(9) 0.0056(10) 0.0001(9) C18 0.0189(11) 0.0164(10) 0.0213(11) -0.0018(8) 0.0027(9) -0.0023(8) C19 0.0241(12) 0.0239(11) 0.0207(11) -0.0012(9) 0.0053(9) -0.0001(9) C20 0.0204(12) 0.0304(12) 0.0322(13) -0.0046(10) 0.0076(10) 0.0027(10) C21 0.0201(12) 0.0262(12) 0.0327(13) -0.0002(10) -0.0017(10) 0.0039(9) C22 0.0250(13) 0.0261(12) 0.0227(12) 0.0016(9) -0.0035(10) -0.0021(9) C23 0.0248(12) 0.0214(11) 0.0202(11) -0.0019(9) 0.0035(9) -0.0017(9) C24 0.050(2) 0.084(3) 0.053(2) 0.0113(17) 0.0255(16) 0.0317(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 Pd ClA 2.254(4) . ? Pd ClA 2.254(4) 3 ? Pd ClB 2.313(2) . ? Pd ClB 2.313(2) 3 ? Pd P 2.3408(5) . ? Pd P 2.3408(5) 3 ? Fe C10 2.033(2) . ? Fe C1 2.034(2) . ? Fe C6 2.035(2) . ? Fe C5 2.036(2) . ? Fe C3 2.036(2) . ? Fe C2 2.036(2) . ? Fe C7 2.040(2) . ? Fe C9 2.048(2) . ? Fe C4 2.049(2) . ? Fe C8 2.052(2) . ? P C1 1.808(2) . ? P C12 1.824(2) . ? P C18 1.827(2) . ? O C24 1.408(3) . ? O C11 1.425(3) . ? ClA ClB 0.614(3) . ? C1 C5 1.433(3) . ? C1 C2 1.440(3) . ? C2 C3 1.421(3) . ? C2 H2 0.9300 . ? C3 C4 1.419(3) . ? C3 H3 0.9300 . ? C4 C5 1.420(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.427(3) . ? C6 C10 1.428(3) . ? C6 C11 1.486(3) . ? C7 C8 1.418(3) . ? C7 H7 0.9300 . ? C8 C9 1.416(3) . ? C8 H8 0.9300 . ? C9 C10 1.410(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.389(3) . ? C12 C17 1.391(3) . ? C13 C14 1.380(3) . ? C13 H13 0.9300 . ? C14 C15 1.383(4) . ? C14 H14 0.9300 . ? C15 C16 1.373(3) . ? C15 H15 0.9300 . ? C16 C17 1.393(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.394(3) . ? C18 C19 1.399(3) . ? C19 C20 1.385(3) . ? C19 H19 0.9300 . ? C20 C21 1.382(3) . ? C20 H20 0.9300 . ? C21 C22 1.382(3) . ? C21 H21 0.9300 . ? C22 C23 1.385(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 ClA Pd ClA 180.00(15) . 3 ? ClA Pd ClB 15.39(8) . . ? ClA Pd ClB 164.61(8) 3 . ? ClA Pd ClB 164.61(8) . 3 ? ClA Pd ClB 15.39(8) 3 3 ? ClB Pd ClB 180.00(16) . 3 ? ClA Pd P 94.62(9) . . ? ClA Pd P 85.38(9) 3 . ? ClB Pd P 90.53(6) . . ? ClB Pd P 89.47(6) 3 . ? ClA Pd P 85.38(9) . 3 ? ClA Pd P 94.62(9) 3 3 ? ClB Pd P 89.47(6) . 3 ? ClB Pd P 90.53(6) 3 3 ? P Pd P 180.00(4) . 3 ? C10 Fe C1 163.76(10) . . ? C10 Fe C6 41.11(9) . . ? C1 Fe C6 127.06(9) . . ? C10 Fe C5 124.50(10) . . ? C1 Fe C5 41.23(8) . . ? C6 Fe C5 106.25(9) . . ? C10 Fe C3 116.45(9) . . ? C1 Fe C3 69.12(9) . . ? C6 Fe C3 150.59(9) . . ? C5 Fe C3 68.57(9) . . ? C10 Fe C2 151.84(10) . . ? C1 Fe C2 41.43(9) . . ? C6 Fe C2 166.62(9) . . ? C5 Fe C2 69.19(9) . . ? C3 Fe C2 40.84(8) . . ? C10 Fe C7 68.44(9) . . ? C1 Fe C7 109.98(9) . . ? C6 Fe C7 41.01(9) . . ? C5 Fe C7 120.43(9) . . ? C3 Fe C7 166.24(9) . . ? C2 Fe C7 129.51(9) . . ? C10 Fe C9 40.43(10) . . ? C1 Fe C9 155.32(9) . . ? C6 Fe C9 68.77(10) . . ? C5 Fe C9 161.75(9) . . ? C3 Fe C9 106.65(10) . . ? C2 Fe C9 119.49(10) . . ? C7 Fe C9 68.10(10) . . ? C10 Fe C4 104.59(10) . . ? C1 Fe C4 69.08(8) . . ? C6 Fe C4 116.48(9) . . ? C5 Fe C4 40.67(9) . . ? C3 Fe C4 40.64(9) . . ? C2 Fe C4 68.83(9) . . ? C7 Fe C4 152.87(9) . . ? C9 Fe C4 124.43(10) . . ? C10 Fe C8 68.23(10) . . ? C1 Fe C8 121.84(9) . . ? C6 Fe C8 68.90(9) . . ? C5 Fe C8 155.92(9) . . ? C3 Fe C8 127.39(10) . . ? C2 Fe C8 109.81(9) . . ? C7 Fe C8 40.56(9) . . ? C9 Fe C8 40.42(10) . . ? C4 Fe C8 163.07(10) . . ? C1 P C12 104.32(10) . . ? C1 P C18 100.42(10) . . ? C12 P C18 102.71(10) . . ? C1 P Pd 121.45(7) . . ? C12 P Pd 108.38(7) . . ? C18 P Pd 117.38(7) . . ? C24 O C11 111.6(2) . . ? ClB ClA Pd 87.7(5) . . ? ClA ClB Pd 76.9(5) . . ? C5 C1 C2 107.18(18) . . ? C5 C1 P 129.25(17) . . ? C2 C1 P 123.43(16) . . ? C5 C1 Fe 69.45(12) . . ? C2 C1 Fe 69.37(12) . . ? P C1 Fe 129.55(11) . . ? C3 C2 C1 107.64(19) . . ? C3 C2 Fe 69.56(12) . . ? C1 C2 Fe 69.20(12) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? Fe C2 H2 126.6 . . ? C4 C3 C2 108.8(2) . . ? C4 C3 Fe 70.19(13) . . ? C2 C3 Fe 69.60(12) . . ? C4 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? Fe C3 H3 126.2 . . ? C3 C4 C5 107.83(19) . . ? C3 C4 Fe 69.17(12) . . ? C5 C4 Fe 69.15(12) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? Fe C4 H4 127.2 . . ? C4 C5 C1 108.5(2) . . ? C4 C5 Fe 70.18(13) . . ? C1 C5 Fe 69.32(12) . . ? C4 C5 H5 125.7 . . ? C1 C5 H5 125.7 . . ? Fe C5 H5 126.3 . . ? C7 C6 C10 106.7(2) . . ? C7 C6 C11 127.5(2) . . ? C10 C6 C11 125.8(2) . . ? C7 C6 Fe 69.68(12) . . ? C10 C6 Fe 69.38(13) . . ? C11 C6 Fe 126.06(16) . . ? C8 C7 C6 108.7(2) . . ? C8 C7 Fe 70.18(13) . . ? C6 C7 Fe 69.30(12) . . ? C8 C7 H7 125.7 . . ? C6 C7 H7 125.7 . . ? Fe C7 H7 126.4 . . ? C9 C8 C7 107.7(2) . . ? C9 C8 Fe 69.64(13) . . ? C7 C8 Fe 69.26(13) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? Fe C8 H8 126.5 . . ? C10 C9 C8 108.3(2) . . ? C10 C9 Fe 69.21(13) . . ? C8 C9 Fe 69.94(13) . . ? C10 C9 H9 125.8 . . ? C8 C9 H9 125.8 . . ? Fe C9 H9 126.6 . . ? C9 C10 C6 108.7(2) . . ? C9 C10 Fe 70.36(13) . . ? C6 C10 Fe 69.51(12) . . ? C9 C10 H10 125.7 . . ? C6 C10 H10 125.7 . . ? Fe C10 H10 126.0 . . ? O C11 C6 108.35(18) . . ? O C11 H11A 110.0 . . ? C6 C11 H11A 110.0 . . ? O C11 H11B 110.0 . . ? C6 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C13 C12 C17 119.1(2) . . ? C13 C12 P 118.52(17) . . ? C17 C12 P 122.25(17) . . ? C14 C13 C12 120.8(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 119.9(2) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.6(2) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 119.6(2) . . ? C12 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C23 C18 C19 118.9(2) . . ? C23 C18 P 119.32(16) . . ? C19 C18 P 121.58(16) . . ? C20 C19 C18 120.2(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.1(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 119.9(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C18 120.6(2) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? O C24 H24A 109.5 . . ? O C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.020 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.084 data_ps333a _database_code_depnum_ccdc_archive 'CCDC 906414' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H46 Cl4 Fe2 O2 P2 Pd2, C H2 Cl2' _chemical_formula_sum 'C49 H48 Cl6 Fe2 O2 P2 Pd2' _chemical_formula_weight 1268.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 22.7193(3) _cell_length_b 18.7832(3) _cell_length_c 15.3334(2) _cell_angle_alpha 90.00 _cell_angle_beta 131.4336(6) _cell_angle_gamma 90.00 _cell_volume 4905.73(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 33525 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description bar _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 1.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 1.000 0.461 0.250 108 42 ' ' 2 0.500 0.961 0.250 108 42 ' ' 3 0.500 0.344 0.250 11 1 ' ' 4 1.000 0.844 0.250 11 1 ' ' 5 0.500 0.039 0.750 108 42 ' ' 6 1.000 0.539 0.750 108 42 ' ' 7 1.000 0.156 0.750 11 1 ' ' 8 0.500 0.656 0.750 11 1 ' ' _platon_squeeze_details ; Total 172; four molecules of CH2Cl2 require 168 electrons. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 53794 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5622 _reflns_number_gt 5069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 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^)+(0.0510P)^2^+31.9300P] 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 5622 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Pd Pd 0.227591(13) 0.312613(13) -0.10275(2) 0.02009(9) Uani 1 1 d . . . Fe Fe 0.30361(3) 0.39978(3) -0.28909(5) 0.03379(14) Uani 1 1 d . . . Cl1 Cl 0.24023(7) 0.43250(5) -0.09064(9) 0.0422(2) Uani 1 1 d . . . Cl2 Cl 0.20812(6) 0.19104(4) -0.10169(7) 0.03089(19) Uani 1 1 d . . . P P 0.16601(4) 0.31433(4) -0.29141(6) 0.02016(17) Uani 1 1 d . . . C1 C 0.19432(4) 0.37473(4) -0.35091(6) 0.0263(7) Uani 1 1 d R A . C2 C 0.20255(4) 0.35489(4) -0.43174(6) 0.0327(8) Uani 1 1 d R A . H2 H 0.1977 0.3091 -0.4588 0.039 Uiso 1 1 calc R . . C3 C 0.21948(4) 0.41730(4) -0.46390(6) 0.0391(9) Uani 1 1 d R A . H3 H 0.2277 0.4195 -0.5158 0.047 Uiso 1 1 calc R . . C4 C 0.22172(4) 0.47570(4) -0.40295(6) 0.0382(9) Uani 1 1 d R A . H4 H 0.2316 0.5229 -0.4079 0.046 Uiso 1 1 calc R . . C5 C 0.20616(4) 0.44939(4) -0.33312(6) 0.0306(7) Uani 1 1 d R A . H5 H 0.2041 0.4763 -0.2843 0.037 Uiso 1 1 calc R . . C6 C 0.40103(4) 0.34618(4) -0.22395(6) 0.0326(15) Uiso 0.50 1 d PR A 1 C7 C 0.41022(4) 0.41574(4) -0.24977(6) 0.0392(18) Uiso 0.50 1 d PR A 1 H7 H 0.4175 0.4271 -0.3012 0.047 Uiso 0.50 1 calc PR B 1 C8 C 0.40641(4) 0.46496(4) -0.18334(6) 0.047(2) Uiso 0.50 1 d PR A 1 H8 H 0.4107 0.5142 -0.1836 0.057 Uiso 0.50 1 calc PR C 1 C9 C 0.39487(4) 0.42583(4) -0.11646(6) 0.036(2) Uiso 0.50 1 d PR A 1 H9 H 0.3903 0.4449 -0.0652 0.043 Uiso 0.50 1 calc PR D 1 C10 C 0.39155(4) 0.35242(4) -0.14156(6) 0.038(2) Uiso 0.50 1 d PR A 1 H10 H 0.3844 0.3150 -0.1096 0.046 Uiso 0.50 1 calc PR E 1 C11 C 0.4030(2) 0.28084(19) -0.2704(3) 0.0433(19) Uiso 0.50 1 d P A 1 H11A H 0.3741 0.2441 -0.2679 0.052 Uiso 0.50 1 calc PR A 1 H11B H 0.3792 0.2875 -0.3507 0.052 Uiso 0.50 1 calc PR A 1 C12 C 0.0628(2) 0.32969(19) -0.3671(3) 0.0233(7) Uiso 0.50 1 d PR A 1 C13 C 0.0220(2) 0.38593(19) -0.4447(3) 0.0346(10) Uiso 0.50 1 d PR A 1 H13 H 0.0472 0.4161 -0.4591 0.041 Uiso 0.50 1 calc PR A 1 C14 C -0.0565(2) 0.39708(19) -0.5009(3) 0.0411(12) Uiso 0.50 1 d PR A 1 H14 H -0.0838 0.4347 -0.5529 0.049 Uiso 0.50 1 calc PR A 1 C15 C -0.0941(2) 0.35199(19) -0.4794(3) 0.0346(11) Uiso 0.50 1 d PR A 1 H15 H -0.1466 0.3595 -0.5170 0.042 Uiso 0.50 1 calc PR A 1 C16 C -0.0533(2) 0.29576(19) -0.4017(3) 0.0347(11) Uiso 0.50 1 d PR A 1 H16 H -0.0786 0.2656 -0.3873 0.042 Uiso 0.50 1 calc PR A 1 C17 C 0.0251(2) 0.28461(19) -0.3456(3) 0.0344(9) Uiso 0.50 1 d PR A 1 H17 H 0.0524 0.2470 -0.2936 0.041 Uiso 0.50 1 calc PR A 1 C24 C 0.4919(8) 0.2041(5) -0.2364(12) 0.061(3) Uiso 0.50 1 d P . 1 H24A H 0.4471 0.1731 -0.2771 0.091 Uiso 0.50 1 d PR . 1 H24B H 0.5372 0.1800 -0.1693 0.091 Uiso 0.50 1 d PR . 1 H24C H 0.5012 0.2170 -0.2870 0.091 Uiso 0.50 1 d PR . 1 O1 O 0.4826(4) 0.2606(4) -0.2017(6) 0.0538(16) Uiso 0.50 1 d P . 1 C18 C 0.16842(19) 0.22786(18) -0.3413(3) 0.0238(6) Uani 1 1 d . A . C19 C 0.1010(2) 0.1942(2) -0.4363(3) 0.0314(8) Uani 1 1 d . . . H19 H 0.0523 0.2156 -0.4758 0.038 Uiso 1 1 calc R A . C20 C 0.1059(2) 0.1285(2) -0.4727(4) 0.0384(9) Uani 1 1 d . A . H20 H 0.0604 0.1058 -0.5361 0.046 Uiso 1 1 calc R . . C21 C 0.1779(2) 0.0969(2) -0.4154(4) 0.0378(9) Uani 1 1 d . . . H21 H 0.1808 0.0529 -0.4401 0.045 Uiso 1 1 calc R A . C22 C 0.2459(2) 0.1304(2) -0.3210(4) 0.0357(8) Uani 1 1 d . A . H22 H 0.2945 0.1090 -0.2822 0.043 Uiso 1 1 calc R . . C23 C 0.24120(15) 0.19486(14) -0.2855(2) 0.0311(8) Uani 1 1 d . . . H23 H 0.2871 0.2176 -0.2230 0.037 Uiso 1 1 calc R A . C6B C 0.40948(15) 0.43852(14) -0.2066(2) 0.0335(16) Uiso 0.50 1 d PR A 2 C7B C 0.40348(15) 0.37447(14) -0.2613(2) 0.0340(16) Uiso 0.50 1 d PR A 2 H7B H 0.4070 0.3704 -0.3181 0.041 Uiso 0.50 1 calc PR F 2 C8B C 0.39118(15) 0.31765(14) -0.2138(2) 0.0352(16) Uiso 0.50 1 d PR A 2 H8B H 0.3852 0.2699 -0.2341 0.042 Uiso 0.50 1 calc PR G 2 C9B C 0.38958(15) 0.34659(14) -0.1298(2) 0.0298(19) Uiso 0.50 1 d PR A 2 H9B H 0.3824 0.3211 -0.0855 0.036 Uiso 0.50 1 calc PR H 2 C10B C 0.40089(15) 0.42129(14) -0.1254(2) 0.049(3) Uiso 0.50 1 d PR A 2 H10B H 0.4024 0.4533 -0.0777 0.059 Uiso 0.50 1 calc PR I 2 C11B C 0.4237(5) 0.5101(5) -0.2358(8) 0.0401(18) Uiso 0.50 1 d P A 2 H11C H 0.3955 0.5124 -0.3184 0.048 Uiso 0.50 1 calc PR A 2 H11D H 0.4043 0.5479 -0.2175 0.048 Uiso 0.50 1 calc PR A 2 C24B C 0.5282(7) 0.5808(6) -0.1809(10) 0.060(3) Uiso 0.50 1 d P . 2 H24D H 0.5026 0.5859 -0.2614 0.091 Uiso 0.50 1 d PR . 2 H24E H 0.5840 0.5845 -0.1339 0.091 Uiso 0.50 1 d PR . 2 H24F H 0.5105 0.6175 -0.1594 0.091 Uiso 0.50 1 d PR . 2 O1B O 0.50610(19) 0.51991(17) -0.1705(3) 0.0419(13) Uiso 0.50 1 d P A 2 C12B C 0.06199(19) 0.33488(17) -0.3812(3) 0.0233(7) Uiso 0.50 1 d PR A 2 C13B C 0.02579(19) 0.38894(17) -0.4638(3) 0.0346(10) Uiso 0.50 1 d PR A 2 H13B H 0.0540 0.4141 -0.4779 0.041 Uiso 0.50 1 calc PR A 2 C14B C -0.05257(19) 0.40538(17) -0.5252(3) 0.0411(12) Uiso 0.50 1 d PR A 2 H14B H -0.0768 0.4415 -0.5804 0.049 Uiso 0.50 1 calc PR A 2 C15B C -0.09472(19) 0.36775(17) -0.5041(3) 0.0346(11) Uiso 0.50 1 d PR A 2 H15B H -0.1471 0.3787 -0.5452 0.042 Uiso 0.50 1 calc PR A 2 C16B C -0.05852(19) 0.31369(17) -0.4215(3) 0.0347(11) Uiso 0.50 1 d PR A 2 H16B H -0.0867 0.2885 -0.4074 0.042 Uiso 0.50 1 calc PR A 2 C17B C 0.01984(19) 0.29725(17) -0.3601(3) 0.0344(9) Uiso 0.50 1 d PR A 2 H17B H 0.0441 0.2611 -0.3048 0.041 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01987(13) 0.02326(14) 0.01855(13) -0.00132(8) 0.01331(11) -0.00062(8) Fe 0.0247(3) 0.0497(3) 0.0301(3) 0.0130(2) 0.0195(2) 0.0068(2) Cl1 0.0738(7) 0.0241(4) 0.0410(5) -0.0036(4) 0.0432(5) -0.0044(4) Cl2 0.0423(5) 0.0252(4) 0.0211(4) -0.0034(3) 0.0192(4) -0.0055(3) P 0.0176(4) 0.0256(4) 0.0181(4) 0.0005(3) 0.0122(3) 0.0029(3) C1 0.0238(15) 0.0318(18) 0.0263(16) 0.0055(13) 0.0178(14) 0.0064(13) C2 0.0322(18) 0.045(2) 0.0247(16) 0.0058(15) 0.0206(15) 0.0071(16) C3 0.038(2) 0.056(3) 0.0293(19) 0.0142(18) 0.0252(17) 0.0097(18) C4 0.0347(19) 0.043(2) 0.036(2) 0.0149(17) 0.0228(17) 0.0055(17) C5 0.0281(17) 0.0319(18) 0.0302(17) 0.0074(14) 0.0186(15) 0.0047(14) C18 0.0234(15) 0.0270(16) 0.0244(15) 0.0010(13) 0.0173(13) 0.0020(12) C19 0.0253(17) 0.0351(19) 0.0320(18) -0.0044(15) 0.0182(15) 0.0008(14) C20 0.036(2) 0.035(2) 0.044(2) -0.0139(17) 0.0262(18) -0.0064(16) C21 0.044(2) 0.0309(19) 0.049(2) -0.0055(17) 0.036(2) 0.0000(16) C22 0.0319(18) 0.037(2) 0.043(2) 0.0021(16) 0.0268(18) 0.0088(15) C23 0.0255(17) 0.0341(19) 0.0307(18) -0.0016(14) 0.0173(15) 0.0033(14) _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 Pd P 2.2295(7) . ? Pd Cl1 2.2622(10) . ? Pd Cl2 2.3281(9) . ? Pd Cl2 2.4300(8) 7 ? Fe C6B 1.972(3) . ? Fe C10 1.9795 . ? Fe C6 1.9960 . ? Fe C10B 2.002(3) . ? Fe C2 2.0298 . ? Fe C3 2.0410 . ? Fe C1 2.0422 . ? Fe C4 2.0602 . ? Fe C5 2.0609 . ? Fe C7B 2.068(3) . ? Fe C9 2.0691 . ? Fe C7 2.0946 . ? Cl2 Pd 2.4300(8) 7 ? P C18 1.812(3) . ? P C1 1.8191 . ? P C12B 1.823(3) . ? P C12 1.824(4) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C2 C3 1.4200 . ? C2 H2 0.9300 . ? C3 C4 1.4200 . ? C3 H3 0.9300 . ? C4 C5 1.4200 . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.4200 . ? C6 C7 1.4200 . ? C6 C11 1.435(4) . ? C7 C8 1.4200 . ? C7 H7 0.9300 . ? C8 C9 1.4200 . ? C8 H8 0.9300 . ? C9 C10 1.4200 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 O1 1.416(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.3900 . ? C12 C17 1.3901 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C24 C24 0.72(2) 6_655 ? C24 O1 1.266(12) . ? C24 O1 1.757(12) 6_655 ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? O1 C24 1.757(12) 6_655 ? C18 C19 1.384(5) . ? C18 C23 1.406(4) . ? C19 C20 1.389(5) . ? C19 H19 0.9300 . ? C20 C21 1.378(6) . ? C20 H20 0.9300 . ? C21 C22 1.385(6) . ? C21 H21 0.9300 . ? C22 C23 1.361(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C6B C7B 1.4200 . ? C6B C10B 1.4200 . ? C6B C11B 1.519(9) . ? C7B C8B 1.4200 . ? C7B H7B 0.9300 . ? C8B C9B 1.4200 . ? C8B H8B 0.9300 . ? C9B C10B 1.4200 . ? C9B H9B 0.9300 . ? C10B H10B 0.9300 . ? C11B O1B 1.435(9) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C24B O1B 1.300(12) . ? C24B C24B 1.59(2) 6_655 ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 0.9601 . ? C12B C13B 1.3900 . ? C12B C17B 1.3900 . ? C13B C14B 1.3900 . ? C13B H13B 0.9300 . ? C14B C15B 1.3900 . ? C14B H14B 0.9300 . ? C15B C16B 1.3900 . ? C15B H15B 0.9300 . ? C16B C17B 1.3900 . ? C16B H16B 0.9300 . ? C17B H17B 0.9300 . ? 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 P Pd Cl1 91.64(3) . . ? P Pd Cl2 93.68(3) . . ? Cl1 Pd Cl2 171.98(4) . . ? P Pd Cl2 178.50(3) . 7 ? Cl1 Pd Cl2 89.25(3) . 7 ? Cl2 Pd Cl2 85.30(3) . 7 ? C6B Fe C10 63.43(8) . . ? C6B Fe C6 52.20(8) . . ? C10 Fe C6 41.9 . . ? C6B Fe C10B 41.87(5) . . ? C10 Fe C10B 38.35(8) . . ? C6 Fe C10B 62.34(8) . . ? C6B Fe C2 150.95(9) . . ? C10 Fe C2 127.7 . . ? C6 Fe C2 114.8 . . ? C10B Fe C2 163.36(9) . . ? C6B Fe C3 117.86(9) . . ? C10 Fe C3 158.92(5) . . ? C6 Fe C3 120.2 . . ? C10B Fe C3 155.73(9) . . ? C2 Fe C3 40.8 . . ? C6B Fe C1 167.21(9) . . ? C10 Fe C1 115.1 . . ? C6 Fe C1 136.15(5) . . ? C10B Fe C1 128.54(9) . . ? C2 Fe C1 40.8 . . ? C3 Fe C1 68.5 . . ? C6B Fe C4 108.80(9) . . ? C10 Fe C4 160.39(5) . . ? C6 Fe C4 148.6 . . ? C10B Fe C4 123.47(8) . . ? C2 Fe C4 68.4 . . ? C3 Fe C4 40.5 . . ? C1 Fe C4 68.1 . . ? C6B Fe C5 129.29(9) . . ? C10 Fe C5 129.1 . . ? C6 Fe C5 170.8 . . ? C10B Fe C5 112.02(8) . . ? C2 Fe C5 68.3 . . ? C3 Fe C5 68.1 . . ? C1 Fe C5 40.5 . . ? C4 Fe C5 40.3 . . ? C6B Fe C7B 41.07(5) . . ? C10 Fe C7B 61.38(8) . . ? C6 Fe C7B 22.88(8) . . ? C10B Fe C7B 68.74(8) . . ? C2 Fe C7B 115.55(8) . . ? C3 Fe C7B 104.72(8) . . ? C1 Fe C7B 150.93(8) . . ? C4 Fe C7B 125.90(8) . . ? C5 Fe C7B 164.98(9) . . ? C6B Fe C9 47.78(9) . . ? C10 Fe C9 41.0 . . ? C6 Fe C9 68.8 . . ? C10B Fe C9 7.18(8) . . ? C2 Fe C9 159.7 . . ? C3 Fe C9 156.45(5) . . ? C1 Fe C9 122.0 . . ? C4 Fe C9 119.9 . . ? C5 Fe C9 105.2 . . ? C7B Fe C9 75.91(8) . . ? C6B Fe C7 22.35(8) . . ? C10 Fe C7 68.6 . . ? C6 Fe C7 40.5 . . ? C10B Fe C7 60.21(8) . . ? C2 Fe C7 129.6 . . ? C3 Fe C7 104.7 . . ? C1 Fe C7 170.34(5) . . ? C4 Fe C7 111.6 . . ? C5 Fe C7 144.74(5) . . ? C7B Fe C7 21.79(8) . . ? C9 Fe C7 67.0 . . ? Pd Cl2 Pd 94.70(3) . 7 ? C18 P C1 103.15(10) . . ? C18 P C12B 104.91(15) . . ? C1 P C12B 101.60(10) . . ? C18 P C12 104.99(16) . . ? C1 P C12 108.34(11) . . ? C18 P Pd 111.52(11) . . ? C1 P Pd 122.22(2) . . ? C12B P Pd 111.70(11) . . ? C12 P Pd 105.44(11) . . ? C2 C1 C5 108.0 . . ? C2 C1 P 124.6 . . ? C5 C1 P 127.2 . . ? C2 C1 Fe 69.1 . . ? C5 C1 Fe 70.5 . . ? P C1 Fe 129.47(3) . . ? C1 C2 C3 108.0 . . ? C1 C2 Fe 70.1 . . ? C3 C2 Fe 70.0 . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Fe C2 H2 125.5 . . ? C2 C3 C4 108.0 . . ? C2 C3 Fe 69.2 . . ? C4 C3 Fe 70.5 . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? Fe C3 H3 125.9 . . ? C5 C4 C3 108.0 . . ? C5 C4 Fe 69.9 . . ? C3 C4 Fe 69.0 . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Fe C4 H4 126.7 . . ? C4 C5 C1 108.0 . . ? C4 C5 Fe 69.8 . . ? C1 C5 Fe 69.0 . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe C5 H5 126.7 . . ? C10 C6 C7 108.0 . . ? C10 C6 C11 125.83(14) . . ? C7 C6 C11 126.16(14) . . ? C10 C6 Fe 68.5 . . ? C7 C6 Fe 73.5 . . ? C11 C6 Fe 124.87(15) . . ? C8 C7 C6 108.0 . . ? C8 C7 Fe 72.1 . . ? C6 C7 Fe 66.0 . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe C7 H7 127.5 . . ? C7 C8 C9 108.0 . . ? C7 C8 Fe 68.8 . . ? C9 C8 Fe 67.7 . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe C8 H8 129.1 . . ? C10 C9 C8 108.0 . . ? C10 C9 Fe 66.1 . . ? C8 C9 Fe 72.9 . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe C9 H9 126.5 . . ? C9 C10 C6 108.0 . . ? C9 C10 Fe 72.9 . . ? C6 C10 Fe 69.7 . . ? C9 C10 H10 126.0 . . ? C6 C10 H10 126.0 . . ? Fe C10 H10 123.1 . . ? O1 C11 C6 107.8(4) . . ? O1 C11 H11A 110.2 . . ? C6 C11 H11A 110.2 . . ? O1 C11 H11B 110.2 . . ? C6 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C13 C12 C17 120.0 . . ? C13 C12 P 120.85(11) . . ? C17 C12 P 119.15(11) . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C12 120.0 . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C24 C24 O1 122.5(6) 6_655 . ? O1 C24 O1 85.8(8) . 6_655 ? C24 C24 H24A 110.7 6_655 . ? O1 C24 H24A 112.5 . . ? O1 C24 H24A 126.9 6_655 . ? C24 C24 H24B 91.4 6_655 . ? O1 C24 H24B 107.6 . . ? O1 C24 H24B 111.2 6_655 . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C24 O1 C11 113.5(8) . . ? C11 O1 C24 118.4(7) . 6_655 ? C19 C18 C23 118.5(3) . . ? C19 C18 P 122.1(3) . . ? C23 C18 P 119.3(2) . . ? C18 C19 C20 120.1(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 120.2(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.3(4) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 119.5(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C18 121.4(3) . . ? C22 C23 H23 119.3 . . ? C18 C23 H23 119.3 . . ? C7B C6B C10B 108.0 . . ? C7B C6B C11B 122.2(3) . . ? C10B C6B C11B 129.8(3) . . ? C7B C6B Fe 73.08(8) . . ? C10B C6B Fe 70.18(8) . . ? C11B C6B Fe 123.1(4) . . ? C6B C7B C8B 108.0 . . ? C6B C7B Fe 65.85(8) . . ? C8B C7B Fe 73.57(8) . . ? C6B C7B H7B 126.0 . . ? C8B C7B H7B 126.0 . . ? Fe C7B H7B 126.1 . . ? C9B C8B C7B 108.0 . . ? C9B C8B Fe 69.08(8) . . ? C7B C8B Fe 67.16(8) . . ? C9B C8B H8B 126.0 . . ? C7B C8B H8B 126.0 . . ? Fe C8B H8B 129.3 . . ? C8B C9B C10B 108.0 . . ? C8B C9B Fe 72.04(8) . . ? C10B C9B Fe 65.64(7) . . ? C8B C9B H9B 126.0 . . ? C10B C9B H9B 126.0 . . ? Fe C9B H9B 127.8 . . ? C9B C10B C6B 108.0 . . ? C9B C10B Fe 74.09(8) . . ? C6B C10B Fe 67.95(8) . . ? C9B C10B H10B 126.0 . . ? C6B C10B H10B 126.0 . . ? Fe C10B H10B 123.5 . . ? O1B C11B C6B 110.0(6) . . ? O1B C11B H11C 109.7 . . ? C6B C11B H11C 109.7 . . ? O1B C11B H11D 109.7 . . ? C6B C11B H11D 109.7 . . ? H11C C11B H11D 108.2 . . ? O1B C24B C24B 97.3(7) . 6_655 ? O1B C24B H24D 107.0 . . ? O1B C24B H24E 113.4 . . ? C24B C24B H24E 119.9 6_655 . ? H24D C24B H24E 109.5 . . ? O1B C24B H24F 107.9 . . ? C24B C24B H24F 107.8 6_655 . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C24B O1B C11B 117.3(7) . . ? C13B C12B C17B 120.0 . . ? C13B C12B P 122.17(10) . . ? C17B C12B P 117.72(10) . . ? C14B C13B C12B 120.0 . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C13B C14B C15B 120.0 . . ? C13B C14B H14B 120.0 . . ? C15B C14B H14B 120.0 . . ? C16B C15B C14B 120.0 . . ? C16B C15B H15B 120.0 . . ? C14B C15B H15B 120.0 . . ? C17B C16B C15B 120.0 . . ? C17B C16B H16B 120.0 . . ? C15B C16B H16B 120.0 . . ? C16B C17B C12B 120.0 . . ? C16B C17B H17B 120.0 . . ? C12B C17B H17B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.589 _refine_diff_density_min -1.581 _refine_diff_density_rms 0.113 ### CIF validation report _vrf_CHEMW03_ps333a ; Problem: CHEMW03_ALERT_2_B WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 Response: The quoted formula includes disordered water molecules whose contribution was removed using SQUEEZE routine. ; _vrf_PLAT051_ps333a ; PROBLEM: PLAT051_ALERT_1_B Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by 6.42 Perc RESPONSE: The quoted formula includes disordered water molecules whose contribution was removed using SQUEEZE routine. ; data_ps418c _database_code_depnum_ccdc_archive 'CCDC 906415' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H46 Cl2 Fe2 O2 P2 Pt' _chemical_formula_sum 'C48 H46 Cl2 Fe2 O2 P2 Pt' _chemical_formula_weight 1094.48 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.4348(4) _cell_length_b 9.1071(3) _cell_length_c 17.4178(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.8600(10) _cell_angle_gamma 90.00 _cell_volume 2105.67(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.51 _exptl_crystal_description bar _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 4.236 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2356 _exptl_absorpt_correction_T_max 0.7558 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32707 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4846 _reflns_number_gt 4301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0163P)^2^+1.2897P] 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 4846 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0168 _refine_ls_wR_factor_ref 0.0382 _refine_ls_wR_factor_gt 0.0368 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Pt Pt 0.0000 0.0000 0.0000 0.01261(3) Uani 1 2 d S . . Fe Fe 0.25514(2) 0.32977(3) 0.087634(16) 0.01553(6) Uani 1 1 d . . . P P 0.15384(4) 0.05276(6) -0.03886(3) 0.01303(10) Uani 1 1 d . . . O O 0.02402(12) 0.42803(19) 0.22774(9) 0.0306(4) Uani 1 1 d . . . ClB Cl 0.05897(12) -0.2047(2) 0.07198(17) 0.0365(5) Uani 0.663(5) 1 d P . . ClA Cl 0.0565(3) -0.2257(4) 0.0393(3) 0.0365(5) Uani 0.337(5) 1 d P . . C1 C 0.21292(14) 0.2289(2) -0.01650(11) 0.0147(4) Uani 1 1 d . . . C2 C 0.32035(15) 0.2499(2) -0.00160(11) 0.0175(4) Uani 1 1 d . . . H2 H 0.3698 0.1747 0.0017 0.021 Uiso 1 1 calc R . . C3 C 0.33941(16) 0.4028(2) 0.00728(12) 0.0206(4) Uani 1 1 d . . . H3 H 0.4040 0.4476 0.0176 0.025 Uiso 1 1 calc R . . C4 C 0.24572(17) 0.4772(2) -0.00181(12) 0.0205(4) Uani 1 1 d . . . H4 H 0.2368 0.5804 0.0014 0.025 Uiso 1 1 calc R . . C5 C 0.16772(16) 0.3718(2) -0.01640(11) 0.0184(4) Uani 1 1 d . . . H5 H 0.0975 0.3920 -0.0247 0.022 Uiso 1 1 calc R . . C6 C 0.16740(16) 0.3698(2) 0.17031(11) 0.0201(4) Uani 1 1 d . . . C7 C 0.19691(16) 0.2193(2) 0.17260(11) 0.0199(4) Uani 1 1 d . . . H7 H 0.1527 0.1373 0.1654 0.024 Uiso 1 1 calc R . . C8 C 0.30406(16) 0.2128(3) 0.18746(12) 0.0248(5) Uani 1 1 d . . . H8 H 0.3438 0.1261 0.1917 0.030 Uiso 1 1 calc R . . C9 C 0.34081(17) 0.3592(3) 0.19476(12) 0.0285(5) Uani 1 1 d . . . H9 H 0.4096 0.3876 0.2049 0.034 Uiso 1 1 calc R . . C10 C 0.25712(18) 0.4553(3) 0.18427(13) 0.0263(5) Uani 1 1 d . . . H10 H 0.2603 0.5595 0.1862 0.032 Uiso 1 1 calc R . . C11 C 0.06328(17) 0.4290(3) 0.15593(12) 0.0244(5) Uani 1 1 d . . . H11A H 0.0637 0.5305 0.1356 0.029 Uiso 1 1 calc R . . H11B H 0.0206 0.3677 0.1170 0.029 Uiso 1 1 calc R . . C12 C 0.14211(15) 0.0397(2) -0.14423(11) 0.0156(4) Uani 1 1 d . . . C13 C 0.09040(16) -0.0798(2) -0.18122(12) 0.0226(5) Uani 1 1 d . . . H13 H 0.0579 -0.1476 -0.1518 0.027 Uiso 1 1 calc R . . C14 C 0.08599(17) -0.1005(3) -0.26016(13) 0.0285(5) Uani 1 1 d . . . H14 H 0.0511 -0.1827 -0.2848 0.034 Uiso 1 1 calc R . . C15 C 0.13266(18) -0.0011(3) -0.30338(13) 0.0290(5) Uani 1 1 d . . . H15 H 0.1302 -0.0155 -0.3577 0.035 Uiso 1 1 calc R . . C16 C 0.18258(18) 0.1186(3) -0.26763(13) 0.0275(5) Uani 1 1 d . . . H16 H 0.2135 0.1873 -0.2975 0.033 Uiso 1 1 calc R . . C17 C 0.18802(16) 0.1393(2) -0.18820(12) 0.0218(4) Uani 1 1 d . . . H17 H 0.2231 0.2216 -0.1638 0.026 Uiso 1 1 calc R . . C18 C 0.25937(14) -0.0702(2) -0.00578(12) 0.0149(4) Uani 1 1 d . . . C19 C 0.32216(15) -0.1220(2) -0.05661(12) 0.0185(4) Uani 1 1 d . . . H19 H 0.3062 -0.1017 -0.1106 0.022 Uiso 1 1 calc R . . C20 C 0.40772(16) -0.2029(2) -0.02884(13) 0.0236(5) Uani 1 1 d . . . H20 H 0.4502 -0.2378 -0.0637 0.028 Uiso 1 1 calc R . . C21 C 0.43101(15) -0.2325(2) 0.04976(13) 0.0234(5) Uani 1 1 d . . . H21 H 0.4898 -0.2873 0.0688 0.028 Uiso 1 1 calc R . . C22 C 0.36916(16) -0.1827(2) 0.10075(12) 0.0219(4) Uani 1 1 d . . . H22 H 0.3854 -0.2038 0.1546 0.026 Uiso 1 1 calc R . . C23 C 0.28338(15) -0.1019(2) 0.07325(12) 0.0183(4) Uani 1 1 d . . . H23 H 0.2409 -0.0680 0.1084 0.022 Uiso 1 1 calc R . . C24 C -0.0633(2) 0.5147(4) 0.22383(19) 0.0555(9) Uani 1 1 d . . . H24A H -0.0478 0.6159 0.2105 0.083 Uiso 1 1 calc R . . H24B H -0.0869 0.5135 0.2743 0.083 Uiso 1 1 calc R . . H24C H -0.1159 0.4752 0.1840 0.083 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 Pt 0.01275(5) 0.01232(5) 0.01323(5) 0.00171(4) 0.00348(4) -0.00029(4) Fe 0.01800(14) 0.01535(14) 0.01353(13) -0.00098(11) 0.00342(11) -0.00229(11) P 0.0130(2) 0.0138(2) 0.0126(2) 0.00049(19) 0.00270(19) -0.00037(19) O 0.0323(9) 0.0374(10) 0.0257(9) 0.0074(7) 0.0155(7) 0.0109(8) ClB 0.0178(3) 0.0337(6) 0.0567(13) 0.0333(9) 0.0014(8) 0.0007(4) ClA 0.0178(3) 0.0337(6) 0.0567(13) 0.0333(9) 0.0014(8) 0.0007(4) C1 0.0178(10) 0.0164(10) 0.0108(9) -0.0003(7) 0.0045(7) -0.0020(8) C2 0.0171(10) 0.0184(10) 0.0179(10) -0.0028(8) 0.0057(8) -0.0029(8) C3 0.0238(11) 0.0200(10) 0.0196(10) -0.0014(8) 0.0085(9) -0.0076(9) C4 0.0325(12) 0.0119(11) 0.0181(10) 0.0010(8) 0.0072(9) -0.0018(8) C5 0.0230(11) 0.0186(10) 0.0138(10) 0.0020(8) 0.0031(8) 0.0017(8) C6 0.0261(11) 0.0233(11) 0.0122(10) -0.0001(8) 0.0073(8) -0.0009(9) C7 0.0253(11) 0.0212(11) 0.0139(10) 0.0028(8) 0.0049(8) -0.0006(9) C8 0.0268(12) 0.0310(13) 0.0159(10) 0.0040(9) 0.0008(9) 0.0041(9) C9 0.0250(12) 0.0434(15) 0.0162(11) -0.0055(10) 0.0002(9) -0.0072(10) C10 0.0376(13) 0.0254(11) 0.0170(11) -0.0080(9) 0.0080(10) -0.0076(10) C11 0.0333(12) 0.0229(11) 0.0190(11) 0.0060(9) 0.0104(9) 0.0042(10) C12 0.0145(9) 0.0185(10) 0.0139(9) 0.0018(7) 0.0022(7) 0.0030(7) C13 0.0208(11) 0.0272(12) 0.0199(11) -0.0016(9) 0.0033(9) -0.0051(9) C14 0.0293(12) 0.0329(13) 0.0218(12) -0.0075(10) -0.0006(9) -0.0027(10) C15 0.0349(12) 0.0385(13) 0.0133(10) -0.0024(10) 0.0030(9) 0.0067(11) C16 0.0353(13) 0.0313(13) 0.0180(11) 0.0062(9) 0.0104(10) 0.0007(10) C17 0.0271(11) 0.0202(11) 0.0184(10) 0.0007(8) 0.0049(9) -0.0017(9) C18 0.0126(9) 0.0122(9) 0.0197(10) -0.0011(8) 0.0019(8) -0.0013(7) C19 0.0179(10) 0.0210(10) 0.0170(10) -0.0004(8) 0.0038(8) -0.0005(8) C20 0.0171(10) 0.0260(12) 0.0286(12) -0.0036(9) 0.0064(9) 0.0027(9) C21 0.0162(10) 0.0225(11) 0.0299(12) 0.0003(9) -0.0014(9) 0.0018(8) C22 0.0222(11) 0.0219(11) 0.0196(10) 0.0018(9) -0.0028(8) -0.0008(9) C23 0.0189(10) 0.0170(10) 0.0190(10) -0.0009(8) 0.0026(8) -0.0010(8) C24 0.0426(16) 0.077(2) 0.0528(19) 0.0139(17) 0.0259(14) 0.0292(16) _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 Pt ClA 2.261(4) 3 ? Pt ClA 2.261(4) . ? Pt ClB 2.3173(16) 3 ? Pt ClB 2.3173(16) . ? Pt P 2.3220(5) . ? Pt P 2.3220(5) 3 ? Fe C6 2.030(2) . ? Fe C10 2.032(2) . ? Fe C2 2.0326(19) . ? Fe C1 2.0342(19) . ? Fe C5 2.038(2) . ? Fe C3 2.042(2) . ? Fe C7 2.042(2) . ? Fe C4 2.046(2) . ? Fe C9 2.053(2) . ? Fe C8 2.059(2) . ? P C1 1.806(2) . ? P C12 1.822(2) . ? P C18 1.829(2) . ? O C24 1.407(3) . ? O C11 1.430(2) . ? ClB ClA 0.596(3) . ? C1 C5 1.436(3) . ? C1 C2 1.439(3) . ? C2 C3 1.420(3) . ? C2 H2 0.9500 . ? C3 C4 1.417(3) . ? C3 H3 0.9500 . ? C4 C5 1.415(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.424(3) . ? C6 C7 1.426(3) . ? C6 C11 1.484(3) . ? C7 C8 1.424(3) . ? C7 H7 0.9500 . ? C8 C9 1.421(3) . ? C8 H8 0.9500 . ? C9 C10 1.415(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.391(3) . ? C12 C13 1.394(3) . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 C15 1.388(3) . ? C14 H14 0.9500 . ? C15 C16 1.377(3) . ? C15 H15 0.9500 . ? C16 C17 1.387(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.395(3) . ? C18 C19 1.396(3) . ? C19 C20 1.388(3) . ? C19 H19 0.9500 . ? C20 C21 1.383(3) . ? C20 H20 0.9500 . ? C21 C22 1.383(3) . ? C21 H21 0.9500 . ? C22 C23 1.389(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 ClA Pt ClA 180.0(3) 3 . ? ClA Pt ClB 14.89(9) 3 3 ? ClA Pt ClB 165.11(9) . 3 ? ClA Pt ClB 165.11(9) 3 . ? ClA Pt ClB 14.89(9) . . ? ClB Pt ClB 180.00(14) 3 . ? ClA Pt P 89.75(9) 3 . ? ClA Pt P 90.25(9) . . ? ClB Pt P 85.49(4) 3 . ? ClB Pt P 94.51(4) . . ? ClA Pt P 90.25(9) 3 3 ? ClA Pt P 89.75(9) . 3 ? ClB Pt P 94.51(4) 3 3 ? ClB Pt P 85.49(4) . 3 ? P Pt P 180.00(2) . 3 ? C6 Fe C10 41.06(9) . . ? C6 Fe C2 166.58(8) . . ? C10 Fe C2 151.96(9) . . ? C6 Fe C1 126.95(8) . . ? C10 Fe C1 163.55(9) . . ? C2 Fe C1 41.46(8) . . ? C6 Fe C5 106.20(8) . . ? C10 Fe C5 124.27(9) . . ? C2 Fe C5 69.18(8) . . ? C1 Fe C5 41.30(8) . . ? C6 Fe C3 150.63(9) . . ? C10 Fe C3 116.52(9) . . ? C2 Fe C3 40.78(8) . . ? C1 Fe C3 69.14(8) . . ? C5 Fe C3 68.53(8) . . ? C6 Fe C7 41.01(8) . . ? C10 Fe C7 68.57(9) . . ? C2 Fe C7 129.50(8) . . ? C1 Fe C7 109.77(8) . . ? C5 Fe C7 120.28(8) . . ? C3 Fe C7 166.32(9) . . ? C6 Fe C4 116.60(8) . . ? C10 Fe C4 104.64(9) . . ? C2 Fe C4 68.65(8) . . ? C1 Fe C4 68.98(8) . . ? C5 Fe C4 40.55(8) . . ? C3 Fe C4 40.55(9) . . ? C7 Fe C4 152.81(9) . . ? C6 Fe C9 68.73(9) . . ? C10 Fe C9 40.52(9) . . ? C2 Fe C9 119.62(9) . . ? C1 Fe C9 155.42(9) . . ? C5 Fe C9 161.62(9) . . ? C3 Fe C9 106.74(9) . . ? C7 Fe C9 68.25(9) . . ? C4 Fe C9 124.51(9) . . ? C6 Fe C8 68.81(9) . . ? C10 Fe C8 68.28(9) . . ? C2 Fe C8 109.97(9) . . ? C1 Fe C8 121.89(9) . . ? C5 Fe C8 155.97(9) . . ? C3 Fe C8 127.51(9) . . ? C7 Fe C8 40.63(8) . . ? C4 Fe C8 163.16(9) . . ? C9 Fe C8 40.42(9) . . ? C1 P C12 104.01(9) . . ? C1 P C18 100.52(9) . . ? C12 P C18 102.71(9) . . ? C1 P Pt 120.16(6) . . ? C12 P Pt 109.72(7) . . ? C18 P Pt 117.58(6) . . ? C24 O C11 111.79(19) . . ? ClA ClB Pt 77.1(5) . . ? ClB ClA Pt 88.0(5) . . ? C5 C1 C2 106.98(17) . . ? C5 C1 P 129.30(15) . . ? C2 C1 P 123.52(15) . . ? C5 C1 Fe 69.50(11) . . ? C2 C1 Fe 69.21(11) . . ? P C1 Fe 130.27(10) . . ? C3 C2 C1 107.99(18) . . ? C3 C2 Fe 69.98(11) . . ? C1 C2 Fe 69.33(11) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe C2 H2 126.3 . . ? C4 C3 C2 108.35(18) . . ? C4 C3 Fe 69.86(11) . . ? C2 C3 Fe 69.24(11) . . ? C4 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? Fe C3 H3 126.6 . . ? C5 C4 C3 108.42(17) . . ? C5 C4 Fe 69.43(11) . . ? C3 C4 Fe 69.59(12) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe C4 H4 126.8 . . ? C4 C5 C1 108.26(18) . . ? C4 C5 Fe 70.03(12) . . ? C1 C5 Fe 69.21(11) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe C5 H5 126.5 . . ? C10 C6 C7 107.25(19) . . ? C10 C6 C11 125.5(2) . . ? C7 C6 C11 127.2(2) . . ? C10 C6 Fe 69.55(12) . . ? C7 C6 Fe 69.98(11) . . ? C11 C6 Fe 125.51(14) . . ? C8 C7 C6 108.29(19) . . ? C8 C7 Fe 70.30(12) . . ? C6 C7 Fe 69.01(11) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe C7 H7 126.4 . . ? C9 C8 C7 107.8(2) . . ? C9 C8 Fe 69.59(13) . . ? C7 C8 Fe 69.07(12) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? Fe C8 H8 126.8 . . ? C10 C9 C8 108.1(2) . . ? C10 C9 Fe 68.91(12) . . ? C8 C9 Fe 69.99(12) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Fe C9 H9 126.7 . . ? C9 C10 C6 108.6(2) . . ? C9 C10 Fe 70.57(13) . . ? C6 C10 Fe 69.40(12) . . ? C9 C10 H10 125.7 . . ? C6 C10 H10 125.7 . . ? Fe C10 H10 125.9 . . ? O C11 C6 108.36(17) . . ? O C11 H11A 110.0 . . ? C6 C11 H11A 110.0 . . ? O C11 H11B 110.0 . . ? C6 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C17 C12 C13 119.09(19) . . ? C17 C12 P 122.36(16) . . ? C13 C12 P 118.42(15) . . ? C14 C13 C12 120.6(2) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.4(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.0(2) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C23 C18 C19 119.07(18) . . ? C23 C18 P 119.18(15) . . ? C19 C18 P 121.47(15) . . ? C20 C19 C18 120.5(2) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 119.8(2) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.3(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.1(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C18 120.21(19) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? O C24 H24A 109.5 . . ? O C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.564 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.071 data_cupome _database_code_depnum_ccdc_archive 'CCDC 906416' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H48 Cu F3 Fe2 O6 P2 S' _chemical_formula_sum 'C49 H48 Cu F3 Fe2 O6 P2 S' _chemical_formula_weight 1057.10 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' 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' S S 0.1246 0.1234 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.1234(3) _cell_length_b 26.0560(6) _cell_length_c 13.6517(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.4890(10) _cell_angle_gamma 90.00 _cell_volume 4557.65(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9972 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.502 _exptl_absorpt_correction_T_max 0.697 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67700 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10455 _reflns_number_gt 9231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0750P)^2^+16.5567P] 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 10455 _refine_ls_number_parameters 550 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1602 _refine_ls_wR_factor_gt 0.1527 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Cu Cu 0.78765(3) 0.890223(16) 0.74737(3) 0.02552(12) Uani 1 1 d . . . Fe1 Fe 0.68741(4) 1.014303(19) 0.92962(4) 0.02376(12) Uani 1 1 d . . . P1 P 0.62710(6) 0.91142(3) 0.76772(6) 0.02164(18) Uani 1 1 d . . . O1 O 0.8928(2) 1.13132(11) 1.0876(2) 0.0410(7) Uani 1 1 d . . . C101 C 0.6082(3) 0.97665(13) 0.8057(2) 0.0237(6) Uani 1 1 d . . . C102 C 0.5369(3) 0.99498(14) 0.8642(3) 0.0283(7) Uani 1 1 d . . . H102 H 0.4911 0.9744 0.8928 0.034 Uiso 1 1 calc R . . C103 C 0.5471(3) 1.04947(15) 0.8718(3) 0.0324(8) Uani 1 1 d . . . H103 H 0.5094 1.0716 0.9065 0.039 Uiso 1 1 calc R . . C104 C 0.6240(3) 1.06487(14) 0.8181(3) 0.0310(8) Uani 1 1 d . . . H104 H 0.6462 1.0991 0.8108 0.037 Uiso 1 1 calc R . . C105 C 0.6618(3) 1.02024(14) 0.7775(3) 0.0276(7) Uani 1 1 d . . . H105 H 0.7136 1.0195 0.7384 0.033 Uiso 1 1 calc R . . C106 C 0.8033(3) 1.05450(15) 1.0205(3) 0.0294(7) Uani 1 1 d . . . C107 C 0.8450(3) 1.01007(16) 0.9812(3) 0.0332(8) Uani 1 1 d . . . H107 H 0.8965 1.0102 0.9420 0.040 Uiso 1 1 calc R . . C108 C 0.7964(3) 0.96583(16) 1.0108(3) 0.0367(9) Uani 1 1 d . . . H108 H 0.8093 0.9314 0.9942 0.044 Uiso 1 1 calc R . . C109 C 0.7251(3) 0.98201(16) 1.0697(3) 0.0365(9) Uani 1 1 d . . . H109 H 0.6819 0.9603 1.0993 0.044 Uiso 1 1 calc R . . C110 C 0.7302(3) 1.03658(16) 1.0762(3) 0.0330(8) Uani 1 1 d . . . H110 H 0.6913 1.0575 1.1118 0.040 Uiso 1 1 calc R . . C111 C 0.8256(3) 1.10929(15) 1.0013(3) 0.0352(8) Uani 1 1 d . . . H11A H 0.8593 1.1115 0.9431 0.042 Uiso 1 1 calc R . . H11B H 0.7593 1.1288 0.9848 0.042 Uiso 1 1 calc R . . C112 C 0.5342(2) 0.90575(13) 0.6474(2) 0.0227(6) Uani 1 1 d . . . C113 C 0.5227(3) 0.85801(14) 0.5997(3) 0.0297(7) Uani 1 1 d . . . H113 H 0.5598 0.8291 0.6318 0.036 Uiso 1 1 calc R . . C114 C 0.4574(3) 0.85257(16) 0.5057(3) 0.0360(9) Uani 1 1 d . . . H114 H 0.4486 0.8198 0.4744 0.043 Uiso 1 1 calc R . . C115 C 0.4051(3) 0.89470(17) 0.4573(3) 0.0353(8) Uani 1 1 d . . . H115 H 0.3617 0.8910 0.3923 0.042 Uiso 1 1 calc R . . C116 C 0.4162(3) 0.94227(16) 0.5040(3) 0.0323(8) Uani 1 1 d . . . H116 H 0.3802 0.9712 0.4709 0.039 Uiso 1 1 calc R . . C117 C 0.4798(3) 0.94783(14) 0.5991(3) 0.0266(7) Uani 1 1 d . . . H117 H 0.4862 0.9804 0.6312 0.032 Uiso 1 1 calc R . . C118 C 0.5636(3) 0.87351(13) 0.8500(3) 0.0285(7) Uani 1 1 d . . . C119 C 0.4555(4) 0.86751(18) 0.8291(3) 0.0405(9) Uani 1 1 d . . . H119 H 0.4138 0.8832 0.7713 0.049 Uiso 1 1 calc R . . C120 C 0.4087(5) 0.8385(2) 0.8929(4) 0.0611(15) Uani 1 1 d . . . H120 H 0.3351 0.8341 0.8774 0.073 Uiso 1 1 calc R . . C121 C 0.4666(6) 0.8166(2) 0.9769(4) 0.0625(16) Uani 1 1 d . . . H121 H 0.4336 0.7976 1.0207 0.075 Uiso 1 1 calc R . . C122 C 0.5730(6) 0.8221(2) 0.9979(4) 0.0651(16) Uani 1 1 d . . . H122 H 0.6137 0.8067 1.0565 0.078 Uiso 1 1 calc R . . C123 C 0.6224(4) 0.85008(18) 0.9340(3) 0.0459(10) Uani 1 1 d . . . H123 H 0.6963 0.8529 0.9485 0.055 Uiso 1 1 calc R . . C124 C 0.8888(4) 1.18628(17) 1.0819(4) 0.0465(11) Uani 1 1 d . . . H12A H 0.9159 1.1978 1.0241 0.070 Uiso 1 1 calc R . . H12B H 0.9315 1.2008 1.1435 0.070 Uiso 1 1 calc R . . H12C H 0.8165 1.1978 1.0744 0.070 Uiso 1 1 calc R . . Fe2 Fe 0.76758(4) 0.87237(2) 0.40269(4) 0.02941(14) Uani 1 1 d . A . P2 P 0.87905(7) 0.92271(3) 0.64037(6) 0.02284(18) Uani 1 1 d . . . O2A O 0.7864(5) 0.7967(3) 0.1197(5) 0.0459(11) Uiso 0.50 1 d P A 1 O2B O 0.8070(5) 0.7715(3) 0.1629(5) 0.0459(11) Uiso 0.50 1 d P B 2 C201 C 0.8161(3) 0.92688(13) 0.5097(3) 0.0241(6) Uani 1 1 d . . . C202 C 0.8653(3) 0.93430(15) 0.4266(3) 0.0296(7) Uani 1 1 d . . . H202 H 0.9383 0.9339 0.4295 0.036 Uiso 1 1 calc R . . C203 C 0.7859(3) 0.94231(15) 0.3391(3) 0.0335(8) Uani 1 1 d . . . H203 H 0.7968 0.9484 0.2735 0.040 Uiso 1 1 calc R . . C204 C 0.6873(3) 0.93960(15) 0.3662(3) 0.0317(8) Uani 1 1 d . . . H204 H 0.6211 0.9436 0.3220 0.038 Uiso 1 1 calc R . . C205 C 0.7052(3) 0.92986(13) 0.4714(3) 0.0265(7) Uani 1 1 d . . . H205 H 0.6531 0.9260 0.5094 0.032 Uiso 1 1 calc R . . C206 C 0.7808(4) 0.8195(2) 0.2975(4) 0.0559(14) Uani 1 1 d D . . C207 C 0.6806(4) 0.81725(18) 0.3166(4) 0.0484(11) Uani 1 1 d . A . H207 H 0.6167 0.8219 0.2692 0.058 Uiso 1 1 calc R . . C208 C 0.6927(6) 0.80646(19) 0.4222(5) 0.076(2) Uani 1 1 d . . . H208 H 0.6391 0.8035 0.4588 0.091 Uiso 1 1 calc R A . C209 C 0.8028(7) 0.80124(19) 0.4599(5) 0.081(2) Uani 1 1 d . A . H209 H 0.8351 0.7932 0.5273 0.097 Uiso 1 1 calc R . . C210 C 0.8544(5) 0.8095(2) 0.3849(6) 0.077(2) Uani 1 1 d . A . H210 H 0.9279 0.8085 0.3912 0.092 Uiso 1 1 calc R . . C21A C 0.7900(8) 0.8372(4) 0.1945(5) 0.0502(16) Uiso 0.50 1 d PD A 1 H21A H 0.7328 0.8618 0.1691 0.060 Uiso 0.50 1 calc PR A 1 H21B H 0.8567 0.8560 0.2010 0.060 Uiso 0.50 1 calc PR A 1 C21B C 0.8397(8) 0.8150(4) 0.2159(6) 0.0502(16) Uiso 0.50 1 d PD B 2 H21C H 0.8262 0.8453 0.1713 0.060 Uiso 0.50 1 calc PR B 2 H21D H 0.9155 0.8131 0.2449 0.060 Uiso 0.50 1 calc PR B 2 C212 C 0.9076(3) 0.99007(13) 0.6719(3) 0.0233(6) Uani 1 1 d . . . C213 C 0.9727(3) 1.00276(15) 0.7640(3) 0.0319(8) Uani 1 1 d . . . H213 H 1.0062 0.9764 0.8072 0.038 Uiso 1 1 calc R . . C214 C 0.9887(3) 1.05368(16) 0.7924(3) 0.0364(9) Uani 1 1 d . . . H214 H 1.0336 1.0620 0.8548 0.044 Uiso 1 1 calc R . . C215 C 0.9396(3) 1.09248(15) 0.7302(3) 0.0345(8) Uani 1 1 d . . . H215 H 0.9496 1.1273 0.7507 0.041 Uiso 1 1 calc R . . C216 C 0.8760(3) 1.08058(14) 0.6382(3) 0.0307(7) Uani 1 1 d . . . H216 H 0.8431 1.1072 0.5952 0.037 Uiso 1 1 calc R . . C217 C 0.8603(3) 1.02954(14) 0.6087(3) 0.0259(7) Uani 1 1 d . . . H217 H 0.8172 1.0215 0.5453 0.031 Uiso 1 1 calc R . . C218 C 1.0083(3) 0.89581(14) 0.6411(3) 0.0282(7) Uani 1 1 d . . . C219 C 1.0927(3) 0.92592(16) 0.6309(3) 0.0345(8) Uani 1 1 d . . . H219 H 1.0846 0.9620 0.6233 0.041 Uiso 1 1 calc R . . C220 C 1.1891(3) 0.9034(2) 0.6318(3) 0.0437(10) Uani 1 1 d . . . H220 H 1.2469 0.9242 0.6262 0.052 Uiso 1 1 calc R . . C221 C 1.2008(3) 0.8510(2) 0.6407(4) 0.0481(11) Uani 1 1 d . . . H221 H 1.2662 0.8357 0.6396 0.058 Uiso 1 1 calc R . . C222 C 1.1173(4) 0.8206(2) 0.6513(4) 0.0556(13) Uani 1 1 d . . . H222 H 1.1256 0.7845 0.6577 0.067 Uiso 1 1 calc R . . C223 C 1.0210(4) 0.84296(17) 0.6526(4) 0.0439(10) Uani 1 1 d . . . H223 H 0.9641 0.8221 0.6613 0.053 Uiso 1 1 calc R . . C22A C 0.8817(10) 0.7659(5) 0.1432(10) 0.062(2) Uiso 0.50 1 d P A 1 H22A H 0.9423 0.7881 0.1451 0.092 Uiso 0.50 1 calc PR A 1 H22B H 0.8792 0.7396 0.0916 0.092 Uiso 0.50 1 calc PR A 1 H22C H 0.8873 0.7495 0.2087 0.092 Uiso 0.50 1 calc PR A 1 C22B C 0.8607(10) 0.7694(5) 0.0887(10) 0.062(2) Uiso 0.50 1 d P B 2 H22D H 0.8414 0.7987 0.0435 0.092 Uiso 0.50 1 calc PR B 2 H22E H 0.8438 0.7374 0.0509 0.092 Uiso 0.50 1 calc PR B 2 H22F H 0.9358 0.7705 0.1180 0.092 Uiso 0.50 1 calc PR B 2 O1W O 0.88965(8) 0.87060(3) 0.88781(8) 0.0394(7) Uani 1 1 d . . . H1W H 0.9588 0.8770 0.8999 0.047 Uiso 1 1 d R . . H2W H 0.8871 0.8343 0.8937 0.047 Uiso 1 1 d R . . S S 0.81866(8) 0.75894(3) 0.75898(8) 0.0511(3) Uani 1 1 d R . . C1 C 0.70378(8) 0.72010(3) 0.75987(8) 0.0637(16) Uani 1 1 d R . . O4 O 0.77801(8) 0.80547(3) 0.71078(8) 0.0525(9) Uani 1 1 d R . . O5 O 0.86764(8) 0.76399(3) 0.86213(8) 0.0853(17) Uani 1 1 d R . . O6 O 0.87431(8) 0.72683(3) 0.70254(8) 0.118(2) Uani 1 1 d R . . F1 F 0.63468(8) 0.74404(3) 0.79965(8) 0.127(2) Uani 1 1 d R . . F2 F 0.73157(8) 0.67799(3) 0.81342(8) 0.164(3) Uani 1 1 d R . . F3 F 0.65614(8) 0.70604(3) 0.66861(8) 0.1154(19) Uani 1 1 d 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 Cu 0.0233(2) 0.0248(2) 0.0278(2) 0.00575(16) 0.00409(16) 0.00139(15) Fe1 0.0241(2) 0.0244(2) 0.0205(2) -0.00097(18) -0.00013(18) -0.00105(18) P1 0.0210(4) 0.0221(4) 0.0202(4) 0.0012(3) 0.0009(3) -0.0012(3) O1 0.0362(15) 0.0322(15) 0.0465(17) -0.0026(12) -0.0092(13) -0.0036(12) C101 0.0233(15) 0.0247(16) 0.0208(15) -0.0005(12) -0.0001(12) -0.0011(12) C102 0.0240(16) 0.0312(18) 0.0273(17) -0.0028(14) 0.0004(13) -0.0007(14) C103 0.0305(18) 0.0314(19) 0.0315(18) -0.0058(15) -0.0014(15) 0.0045(15) C104 0.0368(19) 0.0248(17) 0.0268(17) 0.0009(13) -0.0035(14) -0.0001(14) C105 0.0315(18) 0.0285(17) 0.0197(15) 0.0022(13) -0.0011(13) -0.0030(14) C106 0.0261(17) 0.0319(18) 0.0259(17) -0.0040(14) -0.0035(13) -0.0013(14) C107 0.0284(18) 0.041(2) 0.0273(17) -0.0028(15) -0.0009(14) 0.0062(15) C108 0.041(2) 0.0326(19) 0.0294(18) -0.0008(15) -0.0088(16) 0.0052(16) C109 0.044(2) 0.038(2) 0.0232(17) 0.0059(15) -0.0029(15) -0.0061(17) C110 0.0325(19) 0.041(2) 0.0231(17) -0.0049(15) 0.0002(14) -0.0015(16) C111 0.0319(19) 0.033(2) 0.036(2) -0.0013(16) -0.0024(16) -0.0056(15) C112 0.0188(14) 0.0279(16) 0.0209(15) 0.0007(12) 0.0032(12) -0.0026(12) C113 0.0314(18) 0.0263(17) 0.0288(17) 0.0015(14) 0.0008(14) -0.0036(14) C114 0.039(2) 0.035(2) 0.0309(19) -0.0074(15) 0.0023(16) -0.0121(16) C115 0.0298(18) 0.048(2) 0.0242(17) -0.0007(16) -0.0025(14) -0.0081(16) C116 0.0240(17) 0.039(2) 0.0298(18) 0.0076(15) -0.0026(14) -0.0015(15) C117 0.0221(15) 0.0288(17) 0.0283(17) -0.0001(14) 0.0039(13) 0.0005(13) C118 0.0371(19) 0.0234(16) 0.0257(17) -0.0002(13) 0.0085(14) -0.0054(14) C119 0.042(2) 0.045(2) 0.038(2) -0.0011(18) 0.0155(18) -0.0137(18) C120 0.074(4) 0.060(3) 0.060(3) -0.012(3) 0.037(3) -0.036(3) C121 0.104(5) 0.040(3) 0.057(3) 0.000(2) 0.047(3) -0.025(3) C122 0.107(5) 0.049(3) 0.041(3) 0.019(2) 0.019(3) -0.003(3) C123 0.060(3) 0.041(2) 0.036(2) 0.0120(18) 0.008(2) 0.002(2) C124 0.038(2) 0.032(2) 0.065(3) -0.007(2) 0.001(2) -0.0023(17) Fe2 0.0358(3) 0.0244(3) 0.0285(3) -0.0042(2) 0.0078(2) 0.0018(2) P2 0.0218(4) 0.0223(4) 0.0242(4) 0.0042(3) 0.0044(3) 0.0020(3) C201 0.0247(16) 0.0209(15) 0.0262(16) 0.0010(12) 0.0045(13) 0.0005(12) C202 0.0277(17) 0.0332(18) 0.0286(17) 0.0020(14) 0.0074(14) -0.0019(14) C203 0.040(2) 0.0344(19) 0.0262(17) 0.0046(15) 0.0065(15) -0.0023(16) C204 0.0330(19) 0.0287(18) 0.0300(18) -0.0011(14) -0.0006(15) 0.0030(14) C205 0.0250(16) 0.0241(16) 0.0303(17) -0.0033(13) 0.0053(13) 0.0010(13) C206 0.047(3) 0.058(3) 0.067(3) -0.041(3) 0.021(2) -0.014(2) C207 0.042(2) 0.037(2) 0.067(3) -0.021(2) 0.014(2) -0.0117(19) C208 0.128(6) 0.026(2) 0.097(5) -0.019(3) 0.077(5) -0.024(3) C209 0.132(7) 0.021(2) 0.072(4) -0.001(2) -0.015(4) 0.006(3) C210 0.065(4) 0.050(3) 0.103(5) -0.037(3) -0.009(4) 0.019(3) C212 0.0204(15) 0.0242(16) 0.0254(16) 0.0026(12) 0.0056(12) -0.0002(12) C213 0.0323(19) 0.0347(19) 0.0259(17) 0.0029(14) 0.0003(14) 0.0008(15) C214 0.0331(19) 0.040(2) 0.0325(19) -0.0052(16) -0.0012(15) -0.0057(16) C215 0.0332(19) 0.0295(19) 0.040(2) -0.0060(16) 0.0066(16) -0.0039(15) C216 0.0303(18) 0.0250(17) 0.0360(19) 0.0021(14) 0.0053(15) 0.0017(14) C217 0.0234(16) 0.0274(17) 0.0259(16) 0.0011(13) 0.0029(13) 0.0006(13) C218 0.0261(17) 0.0315(18) 0.0260(17) 0.0039(14) 0.0037(13) 0.0074(14) C219 0.0264(18) 0.040(2) 0.037(2) 0.0092(16) 0.0072(15) 0.0051(15) C220 0.0245(18) 0.067(3) 0.041(2) 0.007(2) 0.0088(16) 0.0047(19) C221 0.031(2) 0.065(3) 0.047(2) -0.003(2) 0.0041(18) 0.021(2) C222 0.049(3) 0.042(3) 0.071(3) 0.000(2) 0.004(2) 0.022(2) C223 0.038(2) 0.034(2) 0.059(3) 0.0051(19) 0.010(2) 0.0093(17) O1W 0.0347(15) 0.0401(16) 0.0372(15) 0.0055(12) -0.0059(12) 0.0044(12) S 0.0449(6) 0.0315(5) 0.0747(8) 0.0109(5) 0.0077(6) -0.0021(5) C1 0.055(3) 0.046(3) 0.080(4) 0.017(3) -0.008(3) -0.021(2) O4 0.070(2) 0.0275(15) 0.0531(19) 0.0048(14) -0.0003(17) -0.0037(15) O5 0.082(3) 0.051(2) 0.094(3) 0.029(2) -0.046(3) -0.026(2) O6 0.133(5) 0.065(3) 0.182(6) 0.004(4) 0.093(5) 0.037(3) F1 0.094(3) 0.143(5) 0.165(5) -0.024(4) 0.074(4) -0.045(3) F2 0.110(4) 0.089(3) 0.243(7) 0.111(4) -0.075(4) -0.060(3) F3 0.118(4) 0.092(3) 0.106(3) 0.000(3) -0.041(3) -0.047(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 Cu O1W 2.1493(11) . ? Cu P2 2.2465(10) . ? Cu P1 2.2526(10) . ? Cu O4 2.2616(10) . ? Fe1 C106 2.033(4) . ? Fe1 C101 2.035(3) . ? Fe1 C105 2.037(3) . ? Fe1 C107 2.038(4) . ? Fe1 C110 2.042(4) . ? Fe1 C108 2.046(4) . ? Fe1 C102 2.046(4) . ? Fe1 C104 2.049(4) . ? Fe1 C109 2.049(4) . ? Fe1 C103 2.055(4) . ? P1 C101 1.810(4) . ? P1 C118 1.826(4) . ? P1 C112 1.827(3) . ? O1 C111 1.431(5) . ? O1 C124 1.434(5) . ? C101 C105 1.432(5) . ? C101 C102 1.437(5) . ? C102 C103 1.428(5) . ? C102 H102 0.9500 . ? C103 C104 1.427(6) . ? C103 H103 0.9500 . ? C104 C105 1.423(5) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C110 1.426(6) . ? C106 C107 1.433(5) . ? C106 C111 1.492(5) . ? C107 C108 1.417(6) . ? C107 H107 0.9500 . ? C108 C109 1.423(6) . ? C108 H108 0.9500 . ? C109 C110 1.425(6) . ? C109 H109 0.9500 . ? C110 H110 0.9500 . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? C112 C117 1.394(5) . ? C112 C113 1.397(5) . ? C113 C114 1.389(5) . ? C113 H113 0.9500 . ? C114 C115 1.385(6) . ? C114 H114 0.9500 . ? C115 C116 1.387(6) . ? C115 H115 0.9500 . ? C116 C117 1.391(5) . ? C116 H116 0.9500 . ? C117 H117 0.9500 . ? C118 C123 1.379(6) . ? C118 C119 1.394(6) . ? C119 C120 1.392(6) . ? C119 H119 0.9500 . ? C120 C121 1.357(9) . ? C120 H120 0.9500 . ? C121 C122 1.372(9) . ? C121 H121 0.9500 . ? C122 C123 1.399(7) . ? C122 H122 0.9500 . ? C123 H123 0.9500 . ? C124 H12A 0.9800 . ? C124 H12B 0.9800 . ? C124 H12C 0.9800 . ? Fe2 C206 2.023(4) . ? Fe2 C208 2.024(5) . ? Fe2 C209 2.025(5) . ? Fe2 C205 2.031(4) . ? Fe2 C201 2.038(3) . ? Fe2 C210 2.040(5) . ? Fe2 C207 2.041(4) . ? Fe2 C202 2.043(4) . ? Fe2 C204 2.049(4) . ? Fe2 C203 2.055(4) . ? P2 C201 1.800(4) . ? P2 C212 1.826(4) . ? P2 C218 1.833(4) . ? O2A C21A 1.461(12) . ? O2A C22A 1.462(14) . ? O2B C22B 1.354(14) . ? O2B C21B 1.363(12) . ? C201 C202 1.435(5) . ? C201 C205 1.438(5) . ? C202 C203 1.420(5) . ? C202 H202 0.9500 . ? C203 C204 1.423(6) . ? C203 H203 0.9500 . ? C204 C205 1.427(5) . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? C206 C210 1.388(9) . ? C206 C207 1.395(6) . ? C206 C21B 1.492(3) . ? C206 C21A 1.510(3) . ? C207 C208 1.443(9) . ? C207 H207 0.9500 . ? C208 C209 1.432(10) . ? C208 H208 0.9500 . ? C209 C210 1.361(11) . ? C209 H209 0.9500 . ? C210 H210 0.9500 . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C212 C217 1.398(5) . ? C212 C213 1.399(5) . ? C213 C214 1.385(6) . ? C213 H213 0.9500 . ? C214 C215 1.386(6) . ? C214 H214 0.9500 . ? C215 C216 1.385(5) . ? C215 H215 0.9500 . ? C216 C217 1.392(5) . ? C216 H216 0.9500 . ? C217 H217 0.9500 . ? C218 C219 1.388(5) . ? C218 C223 1.392(6) . ? C219 C220 1.393(6) . ? C219 H219 0.9500 . ? C220 C221 1.376(7) . ? C220 H220 0.9500 . ? C221 C222 1.385(8) . ? C221 H221 0.9500 . ? C222 C223 1.395(6) . ? C222 H222 0.9500 . ? C223 H223 0.9500 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? O1W H1W 0.9024 . ? O1W H2W 0.9494 . ? S O5 1.4219 . ? S O4 1.4267 . ? S O6 1.4390 . ? S C1 1.8181 . ? C1 F1 1.3112 . ? C1 F3 1.3193 . ? C1 F2 1.3251 . ? 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 O1W Cu P2 110.64(4) . . ? O1W Cu P1 111.53(4) . . ? P2 Cu P1 129.27(4) . . ? O1W Cu O4 87.66(4) . . ? P2 Cu O4 103.68(4) . . ? P1 Cu O4 104.92(4) . . ? C106 Fe1 C101 159.32(15) . . ? C106 Fe1 C105 121.33(15) . . ? C101 Fe1 C105 41.17(14) . . ? C106 Fe1 C107 41.22(15) . . ? C101 Fe1 C107 123.96(15) . . ? C105 Fe1 C107 106.74(16) . . ? C106 Fe1 C110 40.95(16) . . ? C101 Fe1 C110 159.06(15) . . ? C105 Fe1 C110 158.03(16) . . ? C107 Fe1 C110 68.49(16) . . ? C106 Fe1 C108 69.15(16) . . ? C101 Fe1 C108 108.91(15) . . ? C105 Fe1 C108 122.76(17) . . ? C107 Fe1 C108 40.61(17) . . ? C110 Fe1 C108 68.46(16) . . ? C106 Fe1 C102 156.49(15) . . ? C101 Fe1 C102 41.21(14) . . ? C105 Fe1 C102 69.08(15) . . ? C107 Fe1 C102 161.56(16) . . ? C110 Fe1 C102 122.16(16) . . ? C108 Fe1 C102 125.47(16) . . ? C106 Fe1 C104 104.60(15) . . ? C101 Fe1 C104 68.92(14) . . ? C105 Fe1 C104 40.77(15) . . ? C107 Fe1 C104 120.69(17) . . ? C110 Fe1 C104 121.78(16) . . ? C108 Fe1 C104 157.47(18) . . ? C102 Fe1 C104 68.63(15) . . ? C106 Fe1 C109 69.17(16) . . ? C101 Fe1 C109 123.66(15) . . ? C105 Fe1 C109 159.38(16) . . ? C107 Fe1 C109 68.48(17) . . ? C110 Fe1 C109 40.77(16) . . ? C108 Fe1 C109 40.68(18) . . ? C102 Fe1 C109 108.75(16) . . ? C104 Fe1 C109 159.15(17) . . ? C106 Fe1 C103 119.63(15) . . ? C101 Fe1 C103 69.02(14) . . ? C105 Fe1 C103 68.78(16) . . ? C107 Fe1 C103 156.14(17) . . ? C110 Fe1 C103 106.44(16) . . ? C108 Fe1 C103 161.23(18) . . ? C102 Fe1 C103 40.75(15) . . ? C104 Fe1 C103 40.70(16) . . ? C109 Fe1 C103 123.82(18) . . ? C101 P1 C118 102.87(16) . . ? C101 P1 C112 103.15(16) . . ? C118 P1 C112 101.80(16) . . ? C101 P1 Cu 117.07(12) . . ? C118 P1 Cu 120.42(13) . . ? C112 P1 Cu 109.24(11) . . ? C111 O1 C124 110.3(3) . . ? C105 C101 C102 107.6(3) . . ? C105 C101 P1 124.2(3) . . ? C102 C101 P1 128.1(3) . . ? C105 C101 Fe1 69.47(19) . . ? C102 C101 Fe1 69.80(19) . . ? P1 C101 Fe1 127.89(18) . . ? C103 C102 C101 108.0(3) . . ? C103 C102 Fe1 69.9(2) . . ? C101 C102 Fe1 68.98(19) . . ? C103 C102 H102 126.0 . . ? C101 C102 H102 126.0 . . ? Fe1 C102 H102 126.6 . . ? C104 C103 C102 107.9(3) . . ? C104 C103 Fe1 69.4(2) . . ? C102 C103 Fe1 69.3(2) . . ? C104 C103 H103 126.0 . . ? C102 C103 H103 126.0 . . ? Fe1 C103 H103 126.8 . . ? C105 C104 C103 108.4(3) . . ? C105 C104 Fe1 69.2(2) . . ? C103 C104 Fe1 69.9(2) . . ? C105 C104 H104 125.8 . . ? C103 C104 H104 125.8 . . ? Fe1 C104 H104 126.7 . . ? C104 C105 C101 108.1(3) . . ? C104 C105 Fe1 70.1(2) . . ? C101 C105 Fe1 69.35(19) . . ? C104 C105 H105 126.0 . . ? C101 C105 H105 126.0 . . ? Fe1 C105 H105 126.2 . . ? C110 C106 C107 106.9(3) . . ? C110 C106 C111 126.0(4) . . ? C107 C106 C111 127.0(4) . . ? C110 C106 Fe1 69.9(2) . . ? C107 C106 Fe1 69.6(2) . . ? C111 C106 Fe1 122.3(3) . . ? C108 C107 C106 108.6(4) . . ? C108 C107 Fe1 70.0(2) . . ? C106 C107 Fe1 69.2(2) . . ? C108 C107 H107 125.7 . . ? C106 C107 H107 125.7 . . ? Fe1 C107 H107 126.7 . . ? C107 C108 C109 108.1(4) . . ? C107 C108 Fe1 69.4(2) . . ? C109 C108 Fe1 69.8(2) . . ? C107 C108 H108 125.9 . . ? C109 C108 H108 125.9 . . ? Fe1 C108 H108 126.4 . . ? C108 C109 C110 107.6(4) . . ? C108 C109 Fe1 69.5(2) . . ? C110 C109 Fe1 69.3(2) . . ? C108 C109 H109 126.2 . . ? C110 C109 H109 126.2 . . ? Fe1 C109 H109 126.5 . . ? C109 C110 C106 108.7(4) . . ? C109 C110 Fe1 69.9(2) . . ? C106 C110 Fe1 69.2(2) . . ? C109 C110 H110 125.6 . . ? C106 C110 H110 125.6 . . ? Fe1 C110 H110 126.9 . . ? O1 C111 C106 110.4(3) . . ? O1 C111 H11A 109.6 . . ? C106 C111 H11A 109.6 . . ? O1 C111 H11B 109.6 . . ? C106 C111 H11B 109.6 . . ? H11A C111 H11B 108.1 . . ? C117 C112 C113 119.2(3) . . ? C117 C112 P1 122.4(3) . . ? C113 C112 P1 118.3(3) . . ? C114 C113 C112 120.3(4) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C115 C114 C113 120.2(4) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C114 C115 C116 119.8(3) . . ? C114 C115 H115 120.1 . . ? C116 C115 H115 120.1 . . ? C115 C116 C117 120.3(4) . . ? C115 C116 H116 119.9 . . ? C117 C116 H116 119.9 . . ? C116 C117 C112 120.2(3) . . ? C116 C117 H117 119.9 . . ? C112 C117 H117 119.9 . . ? C123 C118 C119 118.8(4) . . ? C123 C118 P1 120.3(3) . . ? C119 C118 P1 120.9(3) . . ? C120 C119 C118 120.0(5) . . ? C120 C119 H119 120.0 . . ? C118 C119 H119 120.0 . . ? C121 C120 C119 121.0(5) . . ? C121 C120 H120 119.5 . . ? C119 C120 H120 119.5 . . ? C120 C121 C122 119.4(5) . . ? C120 C121 H121 120.3 . . ? C122 C121 H121 120.3 . . ? C121 C122 C123 120.9(5) . . ? C121 C122 H122 119.6 . . ? C123 C122 H122 119.6 . . ? C118 C123 C122 119.9(5) . . ? C118 C123 H123 120.1 . . ? C122 C123 H123 120.1 . . ? O1 C124 H12A 109.5 . . ? O1 C124 H12B 109.5 . . ? H12A C124 H12B 109.5 . . ? O1 C124 H12C 109.5 . . ? H12A C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? C206 Fe2 C208 68.6(2) . . ? C206 Fe2 C209 66.6(3) . . ? C208 Fe2 C209 41.4(3) . . ? C206 Fe2 C205 159.12(19) . . ? C208 Fe2 C205 108.05(19) . . ? C209 Fe2 C205 125.3(3) . . ? C206 Fe2 C201 157.12(17) . . ? C208 Fe2 C201 125.6(2) . . ? C209 Fe2 C201 110.6(2) . . ? C205 Fe2 C201 41.38(13) . . ? C206 Fe2 C210 39.9(3) . . ? C208 Fe2 C210 68.5(3) . . ? C209 Fe2 C210 39.1(3) . . ? C205 Fe2 C210 159.8(2) . . ? C201 Fe2 C210 123.3(2) . . ? C206 Fe2 C207 40.16(19) . . ? C208 Fe2 C207 41.6(2) . . ? C209 Fe2 C207 68.3(2) . . ? C205 Fe2 C207 123.63(17) . . ? C201 Fe2 C207 162.18(17) . . ? C210 Fe2 C207 67.9(2) . . ? C206 Fe2 C202 120.23(17) . . ? C208 Fe2 C202 162.7(3) . . ? C209 Fe2 C202 125.3(3) . . ? C205 Fe2 C202 69.24(15) . . ? C201 Fe2 C202 41.18(14) . . ? C210 Fe2 C202 107.8(2) . . ? C207 Fe2 C202 154.30(19) . . ? C206 Fe2 C204 121.8(2) . . ? C208 Fe2 C204 121.2(3) . . ? C209 Fe2 C204 159.8(3) . . ? C205 Fe2 C204 40.93(15) . . ? C201 Fe2 C204 69.09(14) . . ? C210 Fe2 C204 158.2(3) . . ? C207 Fe2 C204 105.50(19) . . ? C202 Fe2 C204 68.64(15) . . ? C206 Fe2 C203 105.53(19) . . ? C208 Fe2 C203 155.8(3) . . ? C209 Fe2 C203 159.5(3) . . ? C205 Fe2 C203 68.70(15) . . ? C201 Fe2 C203 68.77(14) . . ? C210 Fe2 C203 122.8(3) . . ? C207 Fe2 C203 118.9(2) . . ? C202 Fe2 C203 40.55(15) . . ? C204 Fe2 C203 40.58(16) . . ? C201 P2 C212 101.66(16) . . ? C201 P2 C218 104.73(16) . . ? C212 P2 C218 102.93(17) . . ? C201 P2 Cu 118.16(12) . . ? C212 P2 Cu 108.67(11) . . ? C218 P2 Cu 118.42(12) . . ? C21A O2A C22A 110.2(8) . . ? C22B O2B C21B 106.1(8) . . ? C202 C201 C205 107.3(3) . . ? C202 C201 P2 127.1(3) . . ? C205 C201 P2 125.2(3) . . ? C202 C201 Fe2 69.6(2) . . ? C205 C201 Fe2 69.03(19) . . ? P2 C201 Fe2 132.34(18) . . ? C203 C202 C201 108.1(3) . . ? C203 C202 Fe2 70.2(2) . . ? C201 C202 Fe2 69.2(2) . . ? C203 C202 H202 125.9 . . ? C201 C202 H202 125.9 . . ? Fe2 C202 H202 126.2 . . ? C202 C203 C204 108.5(3) . . ? C202 C203 Fe2 69.3(2) . . ? C204 C203 Fe2 69.5(2) . . ? C202 C203 H203 125.8 . . ? C204 C203 H203 125.8 . . ? Fe2 C203 H203 127.1 . . ? C203 C204 C205 108.0(3) . . ? C203 C204 Fe2 69.9(2) . . ? C205 C204 Fe2 68.8(2) . . ? C203 C204 H204 126.0 . . ? C205 C204 H204 126.0 . . ? Fe2 C204 H204 126.8 . . ? C204 C205 C201 108.1(3) . . ? C204 C205 Fe2 70.2(2) . . ? C201 C205 Fe2 69.6(2) . . ? C204 C205 H205 126.0 . . ? C201 C205 H205 126.0 . . ? Fe2 C205 H205 125.8 . . ? C210 C206 C207 109.9(5) . . ? C210 C206 C21B 104.5(6) . . ? C207 C206 C21B 142.8(6) . . ? C210 C206 C21A 132.6(7) . . ? C207 C206 C21A 117.1(6) . . ? C210 C206 Fe2 70.7(3) . . ? C207 C206 Fe2 70.6(2) . . ? C21B C206 Fe2 136.2(5) . . ? C21A C206 Fe2 119.4(5) . . ? C206 C207 C208 106.8(5) . . ? C206 C207 Fe2 69.2(2) . . ? C208 C207 Fe2 68.6(3) . . ? C206 C207 H207 126.6 . . ? C208 C207 H207 126.6 . . ? Fe2 C207 H207 127.2 . . ? C209 C208 C207 105.2(5) . . ? C209 C208 Fe2 69.3(3) . . ? C207 C208 Fe2 69.8(3) . . ? C209 C208 H208 127.4 . . ? C207 C208 H208 127.4 . . ? Fe2 C208 H208 125.0 . . ? C210 C209 C208 110.0(6) . . ? C210 C209 Fe2 71.0(4) . . ? C208 C209 Fe2 69.3(3) . . ? C210 C209 H209 125.0 . . ? C208 C209 H209 125.0 . . ? Fe2 C209 H209 126.3 . . ? C209 C210 C206 108.0(6) . . ? C209 C210 Fe2 69.9(3) . . ? C206 C210 Fe2 69.4(3) . . ? C209 C210 H210 126.0 . . ? C206 C210 H210 126.0 . . ? Fe2 C210 H210 126.3 . . ? O2A C21A C206 115.7(7) . . ? O2A C21A H21A 108.4 . . ? C206 C21A H21A 108.4 . . ? O2A C21A H21B 108.4 . . ? C206 C21A H21B 108.4 . . ? H21A C21A H21B 107.4 . . ? O2B C21B C206 108.0(7) . . ? O2B C21B H21C 110.1 . . ? C206 C21B H21C 110.1 . . ? O2B C21B H21D 110.1 . . ? C206 C21B H21D 110.1 . . ? H21C C21B H21D 108.4 . . ? C217 C212 C213 118.9(3) . . ? C217 C212 P2 121.4(3) . . ? C213 C212 P2 119.6(3) . . ? C214 C213 C212 120.3(4) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C213 C214 C215 120.3(4) . . ? C213 C214 H214 119.8 . . ? C215 C214 H214 119.8 . . ? C216 C215 C214 120.1(4) . . ? C216 C215 H215 119.9 . . ? C214 C215 H215 119.9 . . ? C215 C216 C217 119.9(3) . . ? C215 C216 H216 120.0 . . ? C217 C216 H216 120.0 . . ? C216 C217 C212 120.4(3) . . ? C216 C217 H217 119.8 . . ? C212 C217 H217 119.8 . . ? C219 C218 C223 119.5(4) . . ? C219 C218 P2 122.7(3) . . ? C223 C218 P2 117.8(3) . . ? C218 C219 C220 120.2(4) . . ? C218 C219 H219 119.9 . . ? C220 C219 H219 119.9 . . ? C221 C220 C219 120.2(4) . . ? C221 C220 H220 119.9 . . ? C219 C220 H220 119.9 . . ? C220 C221 C222 120.0(4) . . ? C220 C221 H221 120.0 . . ? C222 C221 H221 120.0 . . ? C221 C222 C223 120.2(5) . . ? C221 C222 H222 119.9 . . ? C223 C222 H222 119.9 . . ? C218 C223 C222 119.9(4) . . ? C218 C223 H223 120.1 . . ? C222 C223 H223 120.1 . . ? O2B C22B H22D 109.5 . . ? O2B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? O2B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? Cu O1W H1W 121.8 . . ? Cu O1W H2W 106.6 . . ? H1W O1W H2W 102.8 . . ? O5 S O4 115.0 . . ? O5 S O6 114.3 . . ? O4 S O6 115.4 . . ? O5 S C1 104.1 . . ? O4 S C1 104.4 . . ? O6 S C1 101.4 . . ? F1 C1 F3 107.1 . . ? F1 C1 F2 107.3 . . ? F3 C1 F2 108.0 . . ? F1 C1 S 112.8 . . ? F3 C1 S 111.9 . . ? F2 C1 S 109.6 . . ? S O4 Cu 136.9 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.968 _refine_diff_density_min -1.995 _refine_diff_density_rms 0.111 data_ps350 _database_code_depnum_ccdc_archive 'CCDC 906417' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H31 Fe O P' _chemical_formula_sum 'C23 H31 Fe O P' _chemical_formula_weight 410.30 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.4488(3) _cell_length_b 7.7891(4) _cell_length_c 39.978(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2008.11(17) _cell_measurement_temperature 150(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2569 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.840 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 12140 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4545 _reflns_number_gt 3362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 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^)+(0.0511P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(5) _refine_ls_number_reflns 4545 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Fe Fe 0.23292(7) 0.98138(5) 0.065940(11) 0.02699(14) Uani 1 1 d . . . P P 0.19385(13) 0.82971(10) 0.14769(2) 0.0268(2) Uani 1 1 d . . . O O 0.1763(4) 1.1593(4) -0.02361(7) 0.0548(8) Uani 1 1 d . . . C1 C 0.1733(4) 1.0013(4) 0.11658(7) 0.0267(7) Uani 1 1 d . . . C2 C 0.3486(5) 1.1032(4) 0.10657(9) 0.0323(8) Uani 1 1 d . . . H2 H 0.4835 1.0915 0.1145 0.039 Uiso 1 1 calc R . . C3 C 0.2798(5) 1.2262(4) 0.08222(8) 0.0330(8) Uani 1 1 d . . . H3 H 0.3616 1.3089 0.0718 0.040 Uiso 1 1 calc R . . C4 C 0.0671(5) 1.1995(4) 0.07686(8) 0.0334(8) Uani 1 1 d . . . H4 H -0.0165 1.2611 0.0622 0.040 Uiso 1 1 calc R . . C5 C 0.0016(5) 1.0616(4) 0.09780(8) 0.0296(8) Uani 1 1 d . . . H5 H -0.1325 1.0181 0.0990 0.035 Uiso 1 1 calc R . . C6 C 0.2115(5) 0.9374(4) 0.01599(8) 0.0293(8) Uani 1 1 d . . . C7 C 0.1290(6) 0.7953(4) 0.03440(8) 0.0349(9) Uani 1 1 d . . . H7 H -0.0065 0.7548 0.0333 0.042 Uiso 1 1 calc R . . C8 C 0.2885(5) 0.7277(4) 0.05439(8) 0.0333(8) Uani 1 1 d . . . H8 H 0.2775 0.6336 0.0686 0.040 Uiso 1 1 calc R . . C9 C 0.4695(5) 0.8281(4) 0.04912(9) 0.0345(9) Uani 1 1 d . . . H9 H 0.5971 0.8112 0.0595 0.041 Uiso 1 1 calc R . . C10 C 0.4240(5) 0.9567(4) 0.02570(8) 0.0320(8) Uani 1 1 d . . . H10 H 0.5155 1.0398 0.0179 0.038 Uiso 1 1 calc R . . C11 C 0.0946(7) 1.0503(5) -0.00574(9) 0.0435(10) Uani 1 1 d . . . H11 H -0.0490 1.0398 -0.0062 0.052 Uiso 1 1 calc R . . C12 C 0.1915(5) 0.9581(4) 0.18737(8) 0.0268(7) Uani 1 1 d . . . H12 H 0.1637 0.8767 0.2055 0.032 Uiso 1 1 calc R . . C13 C 0.4105(5) 1.0320(5) 0.19389(8) 0.0313(8) Uani 1 1 d . . . H13A H 0.5112 0.9395 0.1937 0.038 Uiso 1 1 calc R . . H13B H 0.4463 1.1119 0.1762 0.038 Uiso 1 1 calc R . . C14 C 0.4191(5) 1.1246(4) 0.22771(9) 0.0336(9) Uani 1 1 d . . . H14A H 0.3983 1.0418 0.2455 0.040 Uiso 1 1 calc R . . H14B H 0.5553 1.1752 0.2306 0.040 Uiso 1 1 calc R . . C15 C 0.2565(5) 1.2634(4) 0.23032(8) 0.0335(8) Uani 1 1 d . . . H15A H 0.2853 1.3526 0.2140 0.040 Uiso 1 1 calc R . . H15B H 0.2617 1.3147 0.2524 0.040 Uiso 1 1 calc R . . C16 C 0.0393(5) 1.1898(5) 0.22407(9) 0.0358(9) Uani 1 1 d . . . H16A H 0.0048 1.1092 0.2417 0.043 Uiso 1 1 calc R . . H16B H -0.0617 1.2820 0.2246 0.043 Uiso 1 1 calc R . . C17 C 0.0289(5) 1.0987(5) 0.19028(9) 0.0319(9) Uani 1 1 d . . . H17A H -0.1078 1.0489 0.1874 0.038 Uiso 1 1 calc R . . H17B H 0.0498 1.1819 0.1725 0.038 Uiso 1 1 calc R . . C18 C -0.0712(5) 0.7353(4) 0.14705(8) 0.0277(7) Uani 1 1 d . . . H18 H -0.1736 0.8283 0.1474 0.033 Uiso 1 1 calc R . . C19 C -0.1044(5) 0.6201(4) 0.17772(8) 0.0316(8) Uani 1 1 d . . . H19A H 0.0029 0.5329 0.1784 0.038 Uiso 1 1 calc R . . H19B H -0.0930 0.6886 0.1979 0.038 Uiso 1 1 calc R . . C20 C -0.3168(5) 0.5337(4) 0.17675(8) 0.0335(8) Uani 1 1 d . . . H20A H -0.3290 0.4561 0.1956 0.040 Uiso 1 1 calc R . . H20B H -0.4237 0.6206 0.1790 0.040 Uiso 1 1 calc R . . C21 C -0.3526(5) 0.4337(4) 0.14453(9) 0.0341(9) Uani 1 1 d . . . H21A H -0.2593 0.3361 0.1438 0.041 Uiso 1 1 calc R . . H21B H -0.4937 0.3905 0.1442 0.041 Uiso 1 1 calc R . . C22 C -0.3164(5) 0.5458(4) 0.11413(8) 0.0316(8) Uani 1 1 d . . . H22A H -0.4217 0.6347 0.1133 0.038 Uiso 1 1 calc R . . H22B H -0.3287 0.4767 0.0940 0.038 Uiso 1 1 calc R . . C23 C -0.1008(5) 0.6293(4) 0.11519(8) 0.0292(8) Uani 1 1 d . . . H23A H 0.0046 0.5406 0.1142 0.035 Uiso 1 1 calc R . . H23B H -0.0837 0.7030 0.0958 0.035 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 Fe 0.0340(3) 0.0225(2) 0.0244(2) -0.00302(19) 0.0012(2) -0.0007(2) P 0.0298(5) 0.0224(4) 0.0281(5) -0.0019(4) -0.0007(4) -0.0007(3) O 0.0614(19) 0.0556(17) 0.0476(17) 0.0151(15) 0.0056(14) 0.0095(15) C1 0.0326(16) 0.0263(17) 0.0211(17) -0.0049(15) 0.0008(13) -0.0017(15) C2 0.039(2) 0.0287(18) 0.029(2) -0.0055(16) -0.0004(16) -0.0082(15) C3 0.050(2) 0.0211(15) 0.0280(19) -0.0003(13) -0.0010(18) -0.0092(17) C4 0.046(2) 0.0263(18) 0.028(2) -0.0014(15) 0.0029(17) 0.0100(16) C5 0.0310(18) 0.0257(19) 0.032(2) -0.0025(15) 0.0057(15) 0.0030(14) C6 0.0377(19) 0.0292(17) 0.0211(17) -0.0043(13) -0.0025(15) 0.0029(15) C7 0.039(2) 0.031(2) 0.035(2) -0.0117(16) -0.0003(17) -0.0027(16) C8 0.046(2) 0.0213(15) 0.0322(18) -0.0064(13) 0.0016(17) 0.0039(16) C9 0.035(2) 0.035(2) 0.034(2) -0.0038(17) 0.0019(16) 0.0118(17) C10 0.0373(18) 0.0312(19) 0.0275(19) -0.0051(16) 0.0062(15) 0.0010(16) C11 0.056(2) 0.045(2) 0.030(2) -0.0013(19) -0.0002(18) 0.007(2) C12 0.0317(17) 0.0236(16) 0.0250(17) 0.0009(14) -0.0026(14) 0.0009(14) C13 0.0261(16) 0.032(2) 0.036(2) 0.0018(17) -0.0028(14) 0.0036(16) C14 0.037(2) 0.034(2) 0.030(2) -0.0044(17) -0.0057(16) -0.0067(16) C15 0.0384(19) 0.0313(17) 0.0308(19) -0.0041(14) -0.0038(18) -0.0078(18) C16 0.040(2) 0.035(2) 0.033(2) -0.0062(18) 0.0046(16) -0.0003(17) C17 0.0282(19) 0.034(2) 0.033(2) -0.0053(17) -0.0011(15) -0.0025(15) C18 0.0314(18) 0.0225(16) 0.0293(19) -0.0018(15) 0.0019(16) -0.0006(14) C19 0.037(2) 0.0296(19) 0.028(2) 0.0023(16) -0.0045(15) -0.0043(16) C20 0.0360(17) 0.0289(17) 0.036(2) 0.0062(16) 0.0002(14) -0.0050(15) C21 0.0361(19) 0.0266(19) 0.040(2) -0.0002(16) -0.0018(16) -0.0093(14) C22 0.0347(18) 0.0302(17) 0.0298(19) -0.0049(15) 0.0003(15) -0.0081(15) C23 0.0329(19) 0.0254(18) 0.029(2) -0.0007(15) 0.0010(15) -0.0017(15) _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 Fe C2 2.024(3) . ? Fe C6 2.031(3) . ? Fe C7 2.035(3) . ? Fe C10 2.035(3) . ? Fe C3 2.038(3) . ? Fe C9 2.051(3) . ? Fe C4 2.055(3) . ? Fe C5 2.059(3) . ? Fe C8 2.060(3) . ? Fe C1 2.067(3) . ? P C1 1.831(3) . ? P C18 1.861(3) . ? P C12 1.875(3) . ? O C11 1.228(4) . ? C1 C5 1.418(4) . ? C1 C2 1.438(4) . ? C2 C3 1.436(5) . ? C2 H2 0.9300 . ? C3 C4 1.404(5) . ? C3 H3 0.9300 . ? C4 C5 1.426(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.432(5) . ? C6 C10 1.432(5) . ? C6 C11 1.448(5) . ? C7 C8 1.405(5) . ? C7 H7 0.9300 . ? C8 C9 1.421(4) . ? C8 H8 0.9300 . ? C9 C10 1.403(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.521(4) . ? C12 C13 1.547(4) . ? C12 H12 0.9800 . ? C13 C14 1.533(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.510(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.534(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.527(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.530(4) . ? C18 C19 1.535(4) . ? C18 H18 0.9800 . ? C19 C20 1.527(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.523(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.515(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.536(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? 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 C2 Fe C6 153.30(13) . . ? C2 Fe C7 162.34(14) . . ? C6 Fe C7 41.25(13) . . ? C2 Fe C10 117.08(14) . . ? C6 Fe C10 41.25(13) . . ? C7 Fe C10 69.06(14) . . ? C2 Fe C3 41.41(13) . . ? C6 Fe C3 118.82(13) . . ? C7 Fe C3 156.00(14) . . ? C10 Fe C3 104.53(14) . . ? C2 Fe C9 105.18(14) . . ? C6 Fe C9 68.29(13) . . ? C7 Fe C9 68.11(14) . . ? C10 Fe C9 40.14(13) . . ? C3 Fe C9 122.64(14) . . ? C2 Fe C4 68.50(14) . . ? C6 Fe C4 108.24(13) . . ? C7 Fe C4 123.32(14) . . ? C10 Fe C4 124.12(13) . . ? C3 Fe C4 40.12(13) . . ? C9 Fe C4 159.78(14) . . ? C2 Fe C5 68.18(14) . . ? C6 Fe C5 127.61(13) . . ? C7 Fe C5 111.15(14) . . ? C10 Fe C5 162.99(13) . . ? C3 Fe C5 68.02(13) . . ? C9 Fe C5 156.74(14) . . ? C4 Fe C5 40.57(13) . . ? C2 Fe C8 124.43(14) . . ? C6 Fe C8 68.27(13) . . ? C7 Fe C8 40.12(13) . . ? C10 Fe C8 68.11(14) . . ? C3 Fe C8 160.60(15) . . ? C9 Fe C8 40.43(13) . . ? C4 Fe C8 158.63(14) . . ? C5 Fe C8 123.77(14) . . ? C2 Fe C1 41.15(12) . . ? C6 Fe C1 164.45(13) . . ? C7 Fe C1 126.82(13) . . ? C10 Fe C1 153.37(12) . . ? C3 Fe C1 69.16(13) . . ? C9 Fe C1 120.22(13) . . ? C4 Fe C1 68.47(13) . . ? C5 Fe C1 40.22(12) . . ? C8 Fe C1 108.90(13) . . ? C1 P C18 102.28(14) . . ? C1 P C12 100.64(14) . . ? C18 P C12 102.42(14) . . ? C5 C1 C2 106.5(3) . . ? C5 C1 P 131.2(2) . . ? C2 C1 P 122.4(2) . . ? C5 C1 Fe 69.60(18) . . ? C2 C1 Fe 67.83(18) . . ? P C1 Fe 126.67(17) . . ? C3 C2 C1 108.3(3) . . ? C3 C2 Fe 69.81(18) . . ? C1 C2 Fe 71.02(18) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe C2 H2 124.9 . . ? C4 C3 C2 107.9(3) . . ? C4 C3 Fe 70.59(19) . . ? C2 C3 Fe 68.78(18) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Fe C3 H3 126.1 . . ? C3 C4 C5 108.1(3) . . ? C3 C4 Fe 69.29(19) . . ? C5 C4 Fe 69.87(19) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe C4 H4 126.5 . . ? C1 C5 C4 109.2(3) . . ? C1 C5 Fe 70.19(18) . . ? C4 C5 Fe 69.56(18) . . ? C1 C5 H5 125.4 . . ? C4 C5 H5 125.4 . . ? Fe C5 H5 126.4 . . ? C7 C6 C10 107.3(3) . . ? C7 C6 C11 125.7(3) . . ? C10 C6 C11 126.7(3) . . ? C7 C6 Fe 69.53(19) . . ? C10 C6 Fe 69.55(18) . . ? C11 C6 Fe 121.5(2) . . ? C8 C7 C6 108.0(3) . . ? C8 C7 Fe 70.92(19) . . ? C6 C7 Fe 69.23(19) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe C7 H7 125.5 . . ? C7 C8 C9 108.1(3) . . ? C7 C8 Fe 68.96(19) . . ? C9 C8 Fe 69.43(17) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe C8 H8 127.3 . . ? C10 C9 C8 108.7(3) . . ? C10 C9 Fe 69.33(19) . . ? C8 C9 Fe 70.14(17) . . ? C10 C9 H9 125.7 . . ? C8 C9 H9 125.7 . . ? Fe C9 H9 126.4 . . ? C9 C10 C6 107.8(3) . . ? C9 C10 Fe 70.53(19) . . ? C6 C10 Fe 69.20(18) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 125.8 . . ? O C11 C6 123.0(4) . . ? O C11 H11 118.5 . . ? C6 C11 H11 118.5 . . ? C17 C12 C13 110.4(3) . . ? C17 C12 P 117.0(2) . . ? C13 C12 P 109.5(2) . . ? C17 C12 H12 106.4 . . ? C13 C12 H12 106.4 . . ? P C12 H12 106.4 . . ? C14 C13 C12 110.9(3) . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 111.9(3) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 110.8(3) . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 111.0(3) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C12 C17 C16 111.8(3) . . ? C12 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? C12 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C23 C18 C19 109.4(3) . . ? C23 C18 P 109.8(2) . . ? C19 C18 P 110.4(2) . . ? C23 C18 H18 109.1 . . ? C19 C18 H18 109.1 . . ? P C18 H18 109.1 . . ? C20 C19 C18 111.3(3) . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C19 112.5(3) . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 111.1(3) . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 111.2(3) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C18 C23 C22 111.4(3) . . ? C18 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C18 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.358 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.074 data_ps349 _database_code_depnum_ccdc_archive 'CCDC 906418' #TrackingRef 'deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H30 Br Fe P' _chemical_formula_sum 'C22 H30 Br Fe P' _chemical_formula_weight 461.19 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.37690(10) _cell_length_b 7.9364(2) _cell_length_c 39.9711(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2022.92(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 59050 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 2.802 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.200 0 0 -1 0.100 0 1 0 0.192 0 -1 0 0.132 6 1 0 0.180 0 1 -6 0.114 0 -1 6 0.168 -4 0 -1 0.203 0 1 11 0.189 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.376 _exptl_absorpt_correction_T_max 0.535 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 16600 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4616 _reflns_number_gt 4070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 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^)+(0.0471P)^2^+3.2746P] 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 SHELXL _refine_ls_extinction_coef 0.0033(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 4616 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 Fe Fe -0.23159(10) 0.47187(8) 0.433493(15) 0.02301(16) Uani 1 1 d . . . Br Br -0.60277(9) 0.61865(7) 0.491211(13) 0.04107(17) Uani 1 1 d . . . P P -0.19974(19) 0.31340(15) 0.35210(3) 0.0253(3) Uani 1 1 d . . . C1 C -0.1733(7) 0.4832(6) 0.38294(11) 0.0261(9) Uani 1 1 d . . . C2 C -0.3425(8) 0.5898(6) 0.39237(11) 0.0302(11) Uani 1 1 d . . . H2 H -0.4793 0.5815 0.3845 0.036 Uiso 1 1 calc R . . C3 C -0.2693(9) 0.7112(6) 0.41583(12) 0.0332(11) Uani 1 1 d . . . H3 H -0.3485 0.7962 0.4257 0.040 Uiso 1 1 calc R . . C4 C -0.0557(8) 0.6790(6) 0.42135(12) 0.0317(11) Uani 1 1 d . . . H4 H 0.0311 0.7387 0.4358 0.038 Uiso 1 1 calc R . . C5 C 0.0064(7) 0.5394(6) 0.40113(11) 0.0275(9) Uani 1 1 d . . . H5 H 0.1402 0.4932 0.4000 0.033 Uiso 1 1 calc R . . C6 C -0.4147(8) 0.4553(6) 0.47436(12) 0.0308(10) Uani 1 1 d . . . C7 C -0.2038(8) 0.4359(6) 0.48406(11) 0.0286(10) Uani 1 1 d . . . H7 H -0.1306 0.5033 0.4991 0.034 Uiso 1 1 calc R . . C8 C -0.1236(8) 0.2933(6) 0.46652(11) 0.0313(10) Uani 1 1 d . . . H8 H 0.0124 0.2515 0.4679 0.038 Uiso 1 1 calc R . . C9 C -0.2906(8) 0.2252(6) 0.44627(12) 0.0302(10) Uani 1 1 d . . . H9 H -0.2813 0.1316 0.4324 0.036 Uiso 1 1 calc R . . C10 C -0.4714(8) 0.3262(6) 0.45131(11) 0.0271(10) Uani 1 1 d . . . H10 H -0.6021 0.3111 0.4414 0.032 Uiso 1 1 calc R . . C11 C -0.1958(8) 0.4385(6) 0.31228(11) 0.0281(10) Uani 1 1 d . . . H11 H -0.1666 0.3583 0.2942 0.034 Uiso 1 1 calc R . . C12 C -0.4166(7) 0.5117(6) 0.30535(12) 0.0301(10) Uani 1 1 d . . . H12A H -0.5191 0.4214 0.3055 0.036 Uiso 1 1 calc R . . H12B H -0.4536 0.5907 0.3229 0.036 Uiso 1 1 calc R . . C13 C -0.4218(8) 0.6012(6) 0.27157(12) 0.0331(11) Uani 1 1 d . . . H13A H -0.3991 0.5196 0.2539 0.040 Uiso 1 1 calc R . . H13B H -0.5591 0.6512 0.2683 0.040 Uiso 1 1 calc R . . C14 C -0.2558(8) 0.7376(6) 0.26939(13) 0.0348(11) Uani 1 1 d . . . H14A H -0.2855 0.8247 0.2857 0.042 Uiso 1 1 calc R . . H14B H -0.2594 0.7886 0.2473 0.042 Uiso 1 1 calc R . . C15 C -0.0380(8) 0.6648(7) 0.27586(12) 0.0326(11) Uani 1 1 d . . . H15A H 0.0648 0.7548 0.2754 0.039 Uiso 1 1 calc R . . H15B H -0.0029 0.5854 0.2583 0.039 Uiso 1 1 calc R . . C16 C -0.0296(7) 0.5754(6) 0.30983(12) 0.0298(11) Uani 1 1 d . . . H16A H 0.1081 0.5258 0.3129 0.036 Uiso 1 1 calc R . . H16B H -0.0513 0.6572 0.3275 0.036 Uiso 1 1 calc R . . C17 C 0.0643(7) 0.2159(5) 0.35290(11) 0.0253(9) Uani 1 1 d . . . H17 H 0.1699 0.3055 0.3520 0.030 Uiso 1 1 calc R . . C18 C 0.0956(8) 0.0994(6) 0.32266(11) 0.0312(10) Uani 1 1 d . . . H18A H 0.0842 0.1644 0.3022 0.037 Uiso 1 1 calc R . . H18B H -0.0132 0.0140 0.3225 0.037 Uiso 1 1 calc R . . C19 C 0.3116(8) 0.0144(6) 0.32418(12) 0.0342(11) Uani 1 1 d . . . H19A H 0.3261 -0.0614 0.3053 0.041 Uiso 1 1 calc R . . H19B H 0.4197 0.0998 0.3223 0.041 Uiso 1 1 calc R . . C20 C 0.3439(8) -0.0832(6) 0.35604(12) 0.0336(11) Uani 1 1 d . . . H20A H 0.4852 -0.1284 0.3565 0.040 Uiso 1 1 calc R . . H20B H 0.2464 -0.1769 0.3569 0.040 Uiso 1 1 calc R . . C21 C 0.3095(8) 0.0314(7) 0.38657(12) 0.0337(11) Uani 1 1 d . . . H21A H 0.3212 -0.0349 0.4069 0.040 Uiso 1 1 calc R . . H21B H 0.4173 0.1176 0.3871 0.040 Uiso 1 1 calc R . . C22 C 0.0960(8) 0.1139(6) 0.38526(11) 0.0301(9) Uani 1 1 d . . . H22A H 0.0804 0.1882 0.4044 0.036 Uiso 1 1 calc R . . H22B H -0.0115 0.0278 0.3867 0.036 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 Fe 0.0256(3) 0.0208(3) 0.0226(3) 0.0035(2) 0.0008(3) 0.0003(2) Br 0.0477(3) 0.0337(3) 0.0417(3) -0.0025(2) 0.0116(2) 0.0049(2) P 0.0265(6) 0.0226(5) 0.0269(6) 0.0026(5) -0.0010(5) -0.0012(5) C1 0.030(2) 0.022(2) 0.026(2) 0.0079(18) 0.0020(17) -0.0004(18) C2 0.037(3) 0.025(2) 0.029(2) 0.0065(19) 0.0042(19) 0.008(2) C3 0.044(3) 0.025(2) 0.031(2) 0.0106(19) 0.002(2) 0.003(2) C4 0.046(3) 0.021(2) 0.028(2) 0.0014(18) 0.005(2) -0.011(2) C5 0.027(2) 0.029(2) 0.027(2) 0.0019(19) 0.0032(18) -0.006(2) C6 0.041(3) 0.024(2) 0.027(2) 0.0010(19) 0.005(2) -0.002(2) C7 0.034(2) 0.029(2) 0.022(2) 0.0016(18) -0.0033(18) -0.0021(19) C8 0.032(2) 0.033(2) 0.028(2) 0.012(2) -0.003(2) 0.007(2) C9 0.037(3) 0.023(2) 0.031(2) 0.0005(18) -0.001(2) -0.003(2) C10 0.031(2) 0.026(2) 0.024(2) -0.0008(19) -0.0016(18) -0.0037(19) C11 0.032(2) 0.027(2) 0.026(2) -0.0019(18) -0.0018(18) 0.0023(19) C12 0.024(2) 0.035(3) 0.031(2) -0.001(2) -0.0030(19) -0.001(2) C13 0.036(3) 0.035(3) 0.029(2) 0.000(2) -0.008(2) 0.006(2) C14 0.040(3) 0.029(2) 0.035(3) 0.007(2) 0.001(2) 0.015(2) C15 0.031(3) 0.037(3) 0.030(2) 0.013(2) 0.0034(19) 0.001(2) C16 0.022(2) 0.037(3) 0.030(2) 0.009(2) -0.0029(18) -0.0010(19) C17 0.030(2) 0.020(2) 0.026(2) 0.0008(17) 0.0020(19) 0.0007(17) C18 0.040(3) 0.025(2) 0.028(2) -0.0002(19) -0.002(2) 0.005(2) C19 0.039(3) 0.031(3) 0.033(2) -0.004(2) 0.002(2) 0.007(2) C20 0.039(3) 0.022(2) 0.039(3) 0.003(2) -0.002(2) 0.0092(19) C21 0.040(3) 0.031(2) 0.030(2) 0.004(2) 0.000(2) 0.004(2) C22 0.032(2) 0.029(2) 0.029(2) 0.000(2) 0.002(2) 0.001(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 Fe C6 2.012(5) . ? Fe C2 2.019(5) . ? Fe C3 2.041(4) . ? Fe C10 2.045(5) . ? Fe C4 2.048(5) . ? Fe C7 2.049(4) . ? Fe C8 2.056(4) . ? Fe C1 2.057(4) . ? Fe C9 2.058(5) . ? Fe C5 2.065(5) . ? Br C6 1.890(5) . ? P C1 1.834(5) . ? P C17 1.854(5) . ? P C11 1.876(5) . ? C1 C2 1.422(7) . ? C1 C5 1.428(6) . ? C2 C3 1.423(7) . ? C2 H2 0.9300 . ? C3 C4 1.403(8) . ? C3 H3 0.9300 . ? C4 C5 1.427(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.408(7) . ? C6 C10 1.424(7) . ? C7 C8 1.426(7) . ? C7 H7 0.9300 . ? C8 C9 1.442(7) . ? C8 H8 0.9300 . ? C9 C10 1.419(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.521(7) . ? C11 C12 1.549(7) . ? C11 H11 0.9800 . ? C12 C13 1.526(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.517(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.526(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.533(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.534(6) . ? C17 C22 1.539(6) . ? C17 H17 0.9800 . ? C18 C19 1.535(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.504(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.537(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.512(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? 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 C6 Fe C2 119.2(2) . . ? C6 Fe C3 105.9(2) . . ? C2 Fe C3 41.0(2) . . ? C6 Fe C10 41.10(19) . . ? C2 Fe C10 106.5(2) . . ? C3 Fe C10 123.9(2) . . ? C6 Fe C4 124.2(2) . . ? C2 Fe C4 68.1(2) . . ? C3 Fe C4 40.1(2) . . ? C10 Fe C4 161.0(2) . . ? C6 Fe C7 40.6(2) . . ? C2 Fe C7 153.87(19) . . ? C3 Fe C7 118.77(19) . . ? C10 Fe C7 69.04(19) . . ? C4 Fe C7 107.4(2) . . ? C6 Fe C8 68.2(2) . . ? C2 Fe C8 163.7(2) . . ? C3 Fe C8 154.6(2) . . ? C10 Fe C8 68.7(2) . . ? C4 Fe C8 121.5(2) . . ? C7 Fe C8 40.66(19) . . ? C6 Fe C1 154.9(2) . . ? C2 Fe C1 40.83(18) . . ? C3 Fe C1 68.94(19) . . ? C10 Fe C1 120.14(19) . . ? C4 Fe C1 68.48(19) . . ? C7 Fe C1 163.67(19) . . ? C8 Fe C1 126.91(19) . . ? C6 Fe C9 68.3(2) . . ? C2 Fe C9 125.4(2) . . ? C3 Fe C9 161.8(2) . . ? C10 Fe C9 40.47(19) . . ? C4 Fe C9 157.3(2) . . ? C7 Fe C9 68.80(19) . . ? C8 Fe C9 41.1(2) . . ? C1 Fe C9 108.57(19) . . ? C6 Fe C5 162.2(2) . . ? C2 Fe C5 68.1(2) . . ? C3 Fe C5 68.2(2) . . ? C10 Fe C5 156.13(19) . . ? C4 Fe C5 40.61(19) . . ? C7 Fe C5 126.2(2) . . ? C8 Fe C5 109.6(2) . . ? C1 Fe C5 40.55(18) . . ? C9 Fe C5 122.5(2) . . ? C1 P C17 102.2(2) . . ? C1 P C11 100.4(2) . . ? C17 P C11 102.9(2) . . ? C2 C1 C5 106.7(4) . . ? C2 C1 P 123.1(4) . . ? C5 C1 P 130.2(4) . . ? C2 C1 Fe 68.2(3) . . ? C5 C1 Fe 70.0(3) . . ? P C1 Fe 127.7(2) . . ? C1 C2 C3 109.2(5) . . ? C1 C2 Fe 71.0(3) . . ? C3 C2 Fe 70.3(3) . . ? C1 C2 H2 125.4 . . ? C3 C2 H2 125.4 . . ? Fe C2 H2 124.9 . . ? C4 C3 C2 107.4(4) . . ? C4 C3 Fe 70.2(3) . . ? C2 C3 Fe 68.7(3) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? Fe C3 H3 126.4 . . ? C3 C4 C5 108.8(4) . . ? C3 C4 Fe 69.6(3) . . ? C5 C4 Fe 70.3(3) . . ? C3 C4 H4 125.6 . . ? C5 C4 H4 125.6 . . ? Fe C4 H4 126.0 . . ? C4 C5 C1 107.9(4) . . ? C4 C5 Fe 69.1(3) . . ? C1 C5 Fe 69.4(3) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe C5 H5 127.1 . . ? C7 C6 C10 110.0(4) . . ? C7 C6 Br 125.7(4) . . ? C10 C6 Br 124.2(4) . . ? C7 C6 Fe 71.1(3) . . ? C10 C6 Fe 70.7(3) . . ? Br C6 Fe 127.8(2) . . ? C6 C7 C8 107.1(4) . . ? C6 C7 Fe 68.3(3) . . ? C8 C7 Fe 69.9(2) . . ? C6 C7 H7 126.5 . . ? C8 C7 H7 126.5 . . ? Fe C7 H7 126.9 . . ? C7 C8 C9 108.0(4) . . ? C7 C8 Fe 69.4(3) . . ? C9 C8 Fe 69.5(3) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe C8 H8 126.6 . . ? C10 C9 C8 108.0(4) . . ? C10 C9 Fe 69.3(3) . . ? C8 C9 Fe 69.4(3) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe C9 H9 126.9 . . ? C9 C10 C6 107.0(4) . . ? C9 C10 Fe 70.2(3) . . ? C6 C10 Fe 68.2(3) . . ? C9 C10 H10 126.5 . . ? C6 C10 H10 126.5 . . ? Fe C10 H10 126.6 . . ? C16 C11 C12 110.7(4) . . ? C16 C11 P 116.2(3) . . ? C12 C11 P 109.8(3) . . ? C16 C11 H11 106.5 . . ? C12 C11 H11 106.5 . . ? P C11 H11 106.5 . . ? C13 C12 C11 110.7(4) . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 111.6(4) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C15 110.8(4) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 110.9(4) . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.0 . . ? C11 C16 C15 111.3(4) . . ? C11 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C11 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C22 109.1(4) . . ? C18 C17 P 110.9(3) . . ? C22 C17 P 110.7(3) . . ? C18 C17 H17 108.7 . . ? C22 C17 H17 108.7 . . ? P C17 H17 108.7 . . ? C17 C18 C19 110.5(4) . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 112.5(4) . . ? C20 C19 H19A 109.1 . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 C21 110.4(4) . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C20 110.9(4) . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C17 112.0(4) . . ? C21 C22 H22A 109.2 . . ? C17 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C17 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.564 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.099 #===END