data_2fa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H56 B2 Fe N2 O2 P2' _chemical_formula_weight 784.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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' 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 9.28400(10) _cell_length_b 19.3628(2) _cell_length_c 24.2448(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4358.35(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; HKL SCALEPACK (Otwinowski & Minor, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39917 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9953 _reflns_number_gt 8253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.7669P] 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 -0.007(13) _chemical_absolute_configuration rmad _refine_ls_number_reflns 9953 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.13115(4) 0.341086(17) 0.896409(13) 0.03872(9) Uani 1 1 d . . . P1 P -0.05111(7) 0.50031(3) 0.85991(2) 0.03888(14) Uani 1 1 d . . . P2 P 0.07315(6) 0.16027(3) 0.90575(2) 0.03358(12) Uani 1 1 d . . . B1 B 0.0901(4) 0.54117(18) 0.81307(13) 0.0585(9) Uani 1 1 d . . . H1A H 0.0483 0.5796 0.7938 0.088 Uiso 1 1 calc R . . H1B H 0.1234 0.5075 0.7869 0.088 Uiso 1 1 calc R . . H1C H 0.1698 0.5570 0.8349 0.088 Uiso 1 1 calc R . . B2 B 0.0876(3) 0.15674(16) 0.98473(10) 0.0441(6) Uani 1 1 d . . . H2A H 0.0538 0.1128 0.9976 0.066 Uiso 1 1 calc R . . H2B H 0.0300 0.1928 1.0005 0.066 Uiso 1 1 calc R . . H2C H 0.1863 0.1629 0.9955 0.066 Uiso 1 1 calc R . . O1 O -0.0799(3) 0.73865(11) 0.93243(11) 0.0896(8) Uani 1 1 d . . . O2 O 0.2425(3) -0.08001(9) 0.92089(8) 0.0656(6) Uani 1 1 d . . . N1 N -0.1320(2) 0.55552(10) 0.90263(8) 0.0455(5) Uani 1 1 d . . . N2 N 0.1553(2) 0.09530(10) 0.87370(8) 0.0397(5) Uani 1 1 d . . . C1 C -0.1660(4) 0.67818(14) 0.92953(12) 0.0610(8) Uani 1 1 d . . . H1 H -0.2088 0.6700 0.9659 0.073 Uiso 1 1 calc R . . C1N C -0.2294(4) 0.52599(15) 0.94472(12) 0.0645(8) Uani 1 1 d . . . H1N1 H -0.1737 0.5091 0.9752 0.097 Uiso 1 1 calc R . . H1N2 H -0.2834 0.4886 0.9288 0.097 Uiso 1 1 calc R . . H1N3 H -0.2945 0.5611 0.9574 0.097 Uiso 1 1 calc R . . C1O C -0.1520(7) 0.79447(18) 0.95906(19) 0.1216(19) Uani 1 1 d . . . H1O1 H -0.2187 0.8154 0.9338 0.182 Uiso 1 1 calc R . . H1O2 H -0.0825 0.8282 0.9707 0.182 Uiso 1 1 calc R . . H1O3 H -0.2033 0.7774 0.9906 0.182 Uiso 1 1 calc R . . C2N C 0.1910(3) 0.10046(15) 0.81500(10) 0.0526(7) Uani 1 1 d . . . H2N1 H 0.2937 0.1026 0.8107 0.079 Uiso 1 1 calc R . . H2N2 H 0.1483 0.1415 0.7999 0.079 Uiso 1 1 calc R . . H2N3 H 0.1544 0.0607 0.7959 0.079 Uiso 1 1 calc R . . C2 C -0.0586(4) 0.61991(13) 0.91735(12) 0.0566(7) Uani 1 1 d . . . H2 H -0.0024 0.6342 0.8851 0.068 Uiso 1 1 calc R . . C2O C 0.2534(5) -0.14763(15) 0.89920(15) 0.0874(12) Uani 1 1 d . . . H2O1 H 0.1591 -0.1642 0.8897 0.131 Uiso 1 1 calc R . . H2O2 H 0.2954 -0.1776 0.9263 0.131 Uiso 1 1 calc R . . H2O3 H 0.3129 -0.1470 0.8668 0.131 Uiso 1 1 calc R . . C3 C 0.0466(5) 0.61198(19) 0.96492(17) 0.0949(13) Uani 1 1 d . . . H3A H -0.0035 0.5949 0.9967 0.142 Uiso 1 1 calc R . . H3B H 0.0887 0.6560 0.9733 0.142 Uiso 1 1 calc R . . H3C H 0.1212 0.5801 0.9547 0.142 Uiso 1 1 calc R . . C4 C 0.1783(3) -0.03112(13) 0.88434(11) 0.0477(6) Uani 1 1 d . . . H4 H 0.2174 -0.0385 0.8473 0.057 Uiso 1 1 calc R . . C5 C 0.2268(3) 0.04002(12) 0.90465(10) 0.0431(5) Uani 1 1 d . . . H5 H 0.1952 0.0442 0.9431 0.052 Uiso 1 1 calc R . . C6 C 0.3903(3) 0.04730(17) 0.90463(14) 0.0645(8) Uani 1 1 d . . . H6A H 0.4267 0.0381 0.8683 0.097 Uiso 1 1 calc R . . H6B H 0.4312 0.0150 0.9303 0.097 Uiso 1 1 calc R . . H6C H 0.4160 0.0934 0.9153 0.097 Uiso 1 1 calc R . . C11 C -0.2865(4) 0.68540(14) 0.88773(12) 0.0569(7) Uani 1 1 d . . . C12 C -0.4271(4) 0.67291(19) 0.90158(15) 0.0821(10) Uani 1 1 d . . . H12 H -0.4492 0.6592 0.9374 0.099 Uiso 1 1 calc R . . C13 C -0.5375(5) 0.6803(3) 0.8633(2) 0.1049(14) Uani 1 1 d . . . H13 H -0.6321 0.6705 0.8731 0.126 Uiso 1 1 calc R . . C14 C -0.5055(7) 0.7020(2) 0.8114(2) 0.1074(16) Uani 1 1 d . . . H14 H -0.5785 0.7073 0.7855 0.129 Uiso 1 1 calc R . . C15 C -0.3654(7) 0.7163(2) 0.79733(16) 0.0965(14) Uani 1 1 d . . . H15 H -0.3445 0.7319 0.7620 0.116 Uiso 1 1 calc R . . C16 C -0.2561(5) 0.70775(18) 0.83443(14) 0.0759(10) Uani 1 1 d . . . H16 H -0.1616 0.7169 0.8241 0.091 Uiso 1 1 calc R . . C21 C -0.2006(3) 0.46252(13) 0.82205(10) 0.0433(6) Uani 1 1 d . . . C22 C -0.1941(4) 0.39649(15) 0.80100(12) 0.0617(8) Uani 1 1 d . . . H22 H -0.1136 0.3693 0.8080 0.074 Uiso 1 1 calc R . . C23 C -0.3056(4) 0.37000(19) 0.76952(14) 0.0773(10) Uani 1 1 d . . . H23 H -0.2994 0.3253 0.7556 0.093 Uiso 1 1 calc R . . C24 C -0.4237(4) 0.4088(2) 0.75885(14) 0.0770(10) Uani 1 1 d . . . H24 H -0.4987 0.3907 0.7379 0.092 Uiso 1 1 calc R . . C25 C -0.4322(4) 0.4747(2) 0.77903(16) 0.0829(10) Uani 1 1 d . . . H25 H -0.5130 0.5015 0.7714 0.099 Uiso 1 1 calc R . . C26 C -0.3220(3) 0.50181(18) 0.81051(13) 0.0667(8) Uani 1 1 d . . . H26 H -0.3292 0.5466 0.8241 0.080 Uiso 1 1 calc R . . C31 C -0.1107(2) 0.16470(12) 0.88062(9) 0.0370(5) Uani 1 1 d . . . C32 C -0.1616(3) 0.12395(14) 0.83792(11) 0.0504(6) Uani 1 1 d . . . H32 H -0.1031 0.0900 0.8226 0.060 Uiso 1 1 calc R . . C33 C -0.2999(4) 0.13403(17) 0.81817(13) 0.0656(8) Uani 1 1 d . . . H33 H -0.3337 0.1069 0.7893 0.079 Uiso 1 1 calc R . . C34 C -0.3877(3) 0.18354(17) 0.84060(12) 0.0629(8) Uani 1 1 d . . . H34 H -0.4800 0.1903 0.8266 0.075 Uiso 1 1 calc R . . C35 C -0.3392(3) 0.22330(15) 0.88386(12) 0.0542(7) Uani 1 1 d . . . H35 H -0.3989 0.2565 0.8995 0.065 Uiso 1 1 calc R . . C36 C -0.2021(3) 0.21368(13) 0.90381(11) 0.0445(5) Uani 1 1 d . . . H36 H -0.1700 0.2403 0.9333 0.053 Uiso 1 1 calc R . . C41 C 0.0171(3) -0.04010(12) 0.88208(11) 0.0471(6) Uani 1 1 d . . . C42 C -0.0500(4) -0.06621(19) 0.83546(13) 0.0701(9) Uani 1 1 d . . . H42 H 0.0054 -0.0776 0.8048 0.084 Uiso 1 1 calc R . . C43 C -0.1962(4) -0.0755(2) 0.83362(17) 0.0886(12) Uani 1 1 d . . . H43 H -0.2382 -0.0942 0.8022 0.106 Uiso 1 1 calc R . . C44 C -0.2803(4) -0.05789(19) 0.87697(16) 0.0770(10) Uani 1 1 d . . . H44 H -0.3795 -0.0638 0.8751 0.092 Uiso 1 1 calc R . . C45 C -0.2187(4) -0.03137(16) 0.92344(15) 0.0703(9) Uani 1 1 d . . . H45 H -0.2760 -0.0191 0.9533 0.084 Uiso 1 1 calc R . . C46 C -0.0699(4) -0.02258(14) 0.92619(12) 0.0577(7) Uani 1 1 d . . . H46 H -0.0287 -0.0047 0.9581 0.069 Uiso 1 1 calc R . . C51 C 0.0216(3) 0.43311(11) 0.90325(10) 0.0384(5) Uani 1 1 d . . . C52 C 0.1614(3) 0.43743(13) 0.92812(11) 0.0519(7) Uani 1 1 d . . . H52 H 0.2349 0.4676 0.9181 0.062 Uiso 1 1 calc R . . C53 C 0.1674(4) 0.38729(15) 0.97096(12) 0.0593(8) Uani 1 1 d . . . H53 H 0.2456 0.3794 0.9941 0.071 Uiso 1 1 calc R . . C54 C 0.0363(3) 0.35196(14) 0.97248(10) 0.0527(7) Uani 1 1 d . . . H54 H 0.0127 0.3163 0.9965 0.063 Uiso 1 1 calc R . . C55 C -0.0544(3) 0.37966(12) 0.93117(10) 0.0437(6) Uani 1 1 d . . . H55 H -0.1479 0.3654 0.9235 0.052 Uiso 1 1 calc R . . C61 C 0.1508(3) 0.23798(12) 0.87690(10) 0.0390(5) Uani 1 1 d . . . C62 C 0.2864(3) 0.26694(13) 0.89214(13) 0.0488(6) Uani 1 1 d . . . H62 H 0.3440 0.2527 0.9214 0.059 Uiso 1 1 calc R . . C63 C 0.3179(3) 0.32103(15) 0.85502(14) 0.0649(8) Uani 1 1 d . . . H63 H 0.4009 0.3480 0.8552 0.078 Uiso 1 1 calc R . . C64 C 0.2032(4) 0.32736(15) 0.81783(12) 0.0638(8) Uani 1 1 d . . . H64 H 0.1962 0.3598 0.7897 0.077 Uiso 1 1 calc R . . C65 C 0.0997(3) 0.27594(13) 0.83041(10) 0.0475(6) Uani 1 1 d . . . H65 H 0.0137 0.2683 0.8117 0.057 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 0.03521(18) 0.03627(16) 0.04469(18) 0.00302(15) 0.00179(15) 0.00407(15) P1 0.0414(3) 0.0362(3) 0.0390(3) 0.0052(2) 0.0004(3) 0.0018(3) P2 0.0308(3) 0.0358(3) 0.0341(3) -0.0005(2) -0.0003(2) 0.0045(2) B1 0.062(2) 0.0605(19) 0.0535(17) 0.0095(15) 0.0098(16) -0.0096(16) B2 0.0506(17) 0.0476(15) 0.0341(12) -0.0035(12) 0.0012(11) 0.0049(14) O1 0.110(2) 0.0458(12) 0.113(2) -0.0169(12) -0.0218(17) 0.0072(13) O2 0.0946(17) 0.0439(10) 0.0585(11) -0.0026(9) -0.0136(11) 0.0284(11) N1 0.0554(13) 0.0369(10) 0.0443(10) 0.0055(9) 0.0036(11) 0.0074(9) N2 0.0447(13) 0.0391(10) 0.0353(10) -0.0001(8) 0.0014(9) 0.0106(9) C1 0.078(2) 0.0444(15) 0.0604(16) -0.0030(12) -0.0040(15) 0.0115(14) C1N 0.084(2) 0.0539(16) 0.0554(16) 0.0121(13) 0.0250(17) 0.0131(16) C1O 0.196(6) 0.0486(19) 0.120(3) -0.029(2) -0.026(4) 0.029(3) C2N 0.0608(18) 0.0560(16) 0.0408(13) -0.0014(12) 0.0062(13) 0.0133(13) C2 0.068(2) 0.0428(14) 0.0586(16) -0.0018(12) -0.0103(15) 0.0075(14) C2O 0.131(3) 0.0490(17) 0.082(2) -0.0056(17) -0.014(2) 0.0349(19) C3 0.103(3) 0.074(2) 0.108(3) -0.028(2) -0.051(3) 0.025(2) C4 0.0598(17) 0.0407(13) 0.0425(13) -0.0022(10) 0.0003(12) 0.0156(12) C5 0.0440(14) 0.0424(13) 0.0428(13) -0.0014(11) 0.0003(11) 0.0115(10) C6 0.0450(16) 0.0703(19) 0.0781(19) 0.0000(16) -0.0015(15) 0.0137(14) C11 0.076(2) 0.0432(14) 0.0521(16) -0.0017(12) -0.0011(15) 0.0188(14) C12 0.084(3) 0.089(2) 0.073(2) 0.0097(19) 0.007(2) 0.025(2) C13 0.076(3) 0.121(4) 0.118(4) 0.004(3) -0.006(3) 0.027(3) C14 0.128(5) 0.101(3) 0.094(3) -0.012(3) -0.040(3) 0.043(3) C15 0.137(4) 0.088(3) 0.064(2) 0.0146(19) -0.012(3) 0.034(3) C16 0.091(3) 0.072(2) 0.065(2) 0.0119(17) 0.004(2) 0.0170(19) C21 0.0424(14) 0.0485(14) 0.0392(12) 0.0085(10) -0.0026(11) -0.0014(11) C22 0.0606(19) 0.0556(17) 0.0689(18) -0.0054(14) -0.0183(16) 0.0020(14) C23 0.083(3) 0.076(2) 0.072(2) -0.0088(17) -0.022(2) -0.016(2) C24 0.058(2) 0.105(3) 0.068(2) 0.0136(19) -0.0159(17) -0.020(2) C25 0.053(2) 0.104(3) 0.092(3) 0.015(2) -0.0219(19) 0.007(2) C26 0.0566(19) 0.0671(18) 0.076(2) 0.0113(16) -0.0157(16) 0.0074(16) C31 0.0315(11) 0.0408(12) 0.0386(11) 0.0022(10) -0.0009(9) -0.0004(10) C32 0.0469(16) 0.0520(15) 0.0522(14) -0.0076(12) -0.0069(12) 0.0046(12) C33 0.0558(19) 0.072(2) 0.0686(19) -0.0124(16) -0.0219(16) -0.0021(16) C34 0.0375(15) 0.082(2) 0.0689(18) 0.0093(16) -0.0147(14) 0.0033(15) C35 0.0368(15) 0.0651(17) 0.0605(16) -0.0003(14) 0.0021(12) 0.0081(13) C36 0.0314(12) 0.0521(14) 0.0500(14) -0.0034(12) 0.0026(11) 0.0014(10) C41 0.0607(17) 0.0349(12) 0.0456(14) -0.0025(10) 0.0055(12) 0.0070(12) C42 0.065(2) 0.089(2) 0.0561(17) -0.0176(16) 0.0065(16) 0.0051(19) C43 0.064(2) 0.123(3) 0.079(2) -0.032(2) -0.007(2) -0.001(2) C44 0.059(2) 0.077(2) 0.095(3) -0.0122(19) 0.0055(19) -0.0046(18) C45 0.072(2) 0.0563(18) 0.083(2) -0.0058(16) 0.0342(19) -0.0047(16) C46 0.074(2) 0.0472(15) 0.0517(15) -0.0040(12) 0.0168(15) -0.0070(15) C51 0.0400(13) 0.0343(11) 0.0410(12) 0.0001(10) -0.0013(11) 0.0052(9) C52 0.0520(17) 0.0378(13) 0.0658(17) -0.0051(12) -0.0131(13) 0.0022(12) C53 0.070(2) 0.0541(16) 0.0532(16) -0.0041(13) -0.0203(14) 0.0189(15) C54 0.073(2) 0.0456(14) 0.0401(13) 0.0035(11) 0.0070(13) 0.0155(14) C55 0.0473(15) 0.0389(12) 0.0450(13) 0.0015(10) 0.0093(12) 0.0067(11) C61 0.0350(14) 0.0382(12) 0.0438(12) 0.0008(9) 0.0067(11) 0.0085(10) C62 0.0293(13) 0.0442(13) 0.0729(18) 0.0022(13) 0.0037(13) 0.0075(10) C63 0.0492(17) 0.0532(16) 0.092(2) 0.0028(15) 0.0291(17) -0.0006(13) C64 0.081(2) 0.0538(17) 0.0566(16) 0.0124(13) 0.0323(16) 0.0108(16) C65 0.0576(17) 0.0460(13) 0.0387(12) 0.0010(10) 0.0058(12) 0.0100(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 C64 2.037(3) . ? Fe1 C52 2.037(3) . ? Fe1 C62 2.037(2) . ? Fe1 C63 2.041(3) . ? Fe1 C53 2.045(3) . ? Fe1 C54 2.054(3) . ? Fe1 C55 2.058(3) . ? Fe1 C51 2.058(2) . ? Fe1 C65 2.058(3) . ? Fe1 C61 2.060(2) . ? P1 N1 1.667(2) . ? P1 C51 1.804(2) . ? P1 C21 1.818(3) . ? P1 B1 1.906(3) . ? P2 N2 1.6638(19) . ? P2 C61 1.809(2) . ? P2 C31 1.814(2) . ? P2 B2 1.921(2) . ? B1 H1A 0.9600 . ? B1 H1B 0.9600 . ? B1 H1C 0.9600 . ? B2 H2A 0.9600 . ? B2 H2B 0.9600 . ? B2 H2C 0.9600 . ? O1 C1 1.419(4) . ? O1 C1O 1.426(5) . ? O2 C2O 1.415(3) . ? O2 C4 1.427(3) . ? N1 C2 1.465(3) . ? N1 C1N 1.479(3) . ? N2 C2N 1.465(3) . ? N2 C5 1.466(3) . ? C1 C11 1.516(4) . ? C1 C2 1.535(4) . ? C1 H1 0.9800 . ? C1N H1N1 0.9600 . ? C1N H1N2 0.9600 . ? C1N H1N3 0.9600 . ? C1O H1O1 0.9600 . ? C1O H1O2 0.9600 . ? C1O H1O3 0.9600 . ? C2N H2N1 0.9600 . ? C2N H2N2 0.9600 . ? C2N H2N3 0.9600 . ? C2 C3 1.519(4) . ? C2 H2 0.9800 . ? C2O H2O1 0.9600 . ? C2O H2O2 0.9600 . ? C2O H2O3 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C41 1.508(4) . ? C4 C5 1.531(4) . ? C4 H4 0.9800 . ? C5 C6 1.524(4) . ? C5 H5 0.9800 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C11 C12 1.369(5) . ? C11 C16 1.392(4) . ? C12 C13 1.389(5) . ? C12 H12 0.9300 . ? C13 C14 1.361(6) . ? C13 H13 0.9300 . ? C14 C15 1.373(7) . ? C14 H14 0.9300 . ? C15 C16 1.365(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C22 1.378(4) . ? C21 C26 1.388(4) . ? C22 C23 1.385(4) . ? C22 H22 0.9300 . ? C23 C24 1.354(5) . ? C23 H23 0.9300 . ? C24 C25 1.369(5) . ? C24 H24 0.9300 . ? C25 C26 1.380(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.385(3) . ? C31 C36 1.392(3) . ? C32 C33 1.384(4) . ? C32 H32 0.9300 . ? C33 C34 1.371(4) . ? C33 H33 0.9300 . ? C34 C35 1.377(4) . ? C34 H34 0.9300 . ? C35 C36 1.374(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C46 1.383(4) . ? C41 C42 1.386(4) . ? C42 C43 1.370(5) . ? C42 H42 0.9300 . ? C43 C44 1.353(5) . ? C43 H43 0.9300 . ? C44 C45 1.364(5) . ? C44 H44 0.9300 . ? C45 C46 1.393(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C55 1.424(3) . ? C51 C52 1.434(4) . ? C52 C53 1.423(4) . ? C52 H52 0.9300 . ? C53 C54 1.397(4) . ? C53 H53 0.9300 . ? C54 C55 1.414(4) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C61 C62 1.427(4) . ? C61 C65 1.427(3) . ? C62 C63 1.412(4) . ? C62 H62 0.9300 . ? C63 C64 1.401(5) . ? C63 H63 0.9300 . ? C64 C65 1.417(4) . ? C64 H64 0.9300 . ? C65 H65 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 C64 Fe1 C52 115.29(12) . . ? C64 Fe1 C62 68.16(12) . . ? C52 Fe1 C62 124.54(11) . . ? C64 Fe1 C63 40.19(13) . . ? C52 Fe1 C63 104.04(12) . . ? C62 Fe1 C63 40.50(12) . . ? C64 Fe1 C53 146.09(14) . . ? C52 Fe1 C53 40.80(11) . . ? C62 Fe1 C53 103.69(12) . . ? C63 Fe1 C53 112.21(14) . . ? C64 Fe1 C54 173.66(14) . . ? C52 Fe1 C54 68.07(11) . . ? C62 Fe1 C54 114.90(11) . . ? C63 Fe1 C54 145.59(14) . . ? C53 Fe1 C54 39.84(12) . . ? C64 Fe1 C55 134.86(12) . . ? C52 Fe1 C55 68.19(11) . . ? C62 Fe1 C55 150.33(10) . . ? C63 Fe1 C55 169.00(11) . . ? C53 Fe1 C55 67.48(12) . . ? C54 Fe1 C55 40.23(10) . . ? C64 Fe1 C51 110.53(11) . . ? C52 Fe1 C51 40.98(10) . . ? C62 Fe1 C51 164.54(10) . . ? C63 Fe1 C51 128.62(11) . . ? C53 Fe1 C51 68.37(10) . . ? C54 Fe1 C51 68.12(10) . . ? C55 Fe1 C51 40.47(9) . . ? C64 Fe1 C65 40.49(12) . . ? C52 Fe1 C65 150.94(10) . . ? C62 Fe1 C65 68.23(11) . . ? C63 Fe1 C65 67.77(12) . . ? C53 Fe1 C65 168.16(11) . . ? C54 Fe1 C65 134.41(12) . . ? C55 Fe1 C65 114.96(11) . . ? C51 Fe1 C65 121.53(10) . . ? C64 Fe1 C61 68.26(11) . . ? C52 Fe1 C61 164.14(11) . . ? C62 Fe1 C61 40.75(10) . . ? C63 Fe1 C61 68.11(11) . . ? C53 Fe1 C61 127.76(10) . . ? C54 Fe1 C61 110.09(10) . . ? C55 Fe1 C61 121.34(10) . . ? C51 Fe1 C61 154.34(10) . . ? C65 Fe1 C61 40.55(10) . . ? N1 P1 C51 105.62(10) . . ? N1 P1 C21 103.17(12) . . ? C51 P1 C21 106.83(11) . . ? N1 P1 B1 114.44(14) . . ? C51 P1 B1 112.89(14) . . ? C21 P1 B1 113.05(14) . . ? N2 P2 C61 105.40(10) . . ? N2 P2 C31 108.08(11) . . ? C61 P2 C31 101.88(11) . . ? N2 P2 B2 113.99(11) . . ? C61 P2 B2 112.77(13) . . ? C31 P2 B2 113.72(12) . . ? P1 B1 H1A 109.5 . . ? P1 B1 H1B 109.5 . . ? H1A B1 H1B 109.5 . . ? P1 B1 H1C 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? P2 B2 H2A 109.5 . . ? P2 B2 H2B 109.5 . . ? H2A B2 H2B 109.5 . . ? P2 B2 H2C 109.5 . . ? H2A B2 H2C 109.5 . . ? H2B B2 H2C 109.5 . . ? C1 O1 C1O 112.6(3) . . ? C2O O2 C4 114.4(2) . . ? C2 N1 C1N 116.5(2) . . ? C2 N1 P1 119.17(19) . . ? C1N N1 P1 117.15(17) . . ? C2N N2 C5 116.41(19) . . ? C2N N2 P2 120.39(16) . . ? C5 N2 P2 121.37(15) . . ? O1 C1 C11 111.9(2) . . ? O1 C1 C2 104.5(3) . . ? C11 C1 C2 114.8(2) . . ? O1 C1 H1 108.5 . . ? C11 C1 H1 108.5 . . ? C2 C1 H1 108.5 . . ? N1 C1N H1N1 109.5 . . ? N1 C1N H1N2 109.5 . . ? H1N1 C1N H1N2 109.5 . . ? N1 C1N H1N3 109.5 . . ? H1N1 C1N H1N3 109.5 . . ? H1N2 C1N H1N3 109.5 . . ? O1 C1O H1O1 109.5 . . ? O1 C1O H1O2 109.5 . . ? H1O1 C1O H1O2 109.5 . . ? O1 C1O H1O3 109.5 . . ? H1O1 C1O H1O3 109.5 . . ? H1O2 C1O H1O3 109.5 . . ? N2 C2N H2N1 109.5 . . ? N2 C2N H2N2 109.5 . . ? H2N1 C2N H2N2 109.5 . . ? N2 C2N H2N3 109.5 . . ? H2N1 C2N H2N3 109.5 . . ? H2N2 C2N H2N3 109.5 . . ? N1 C2 C3 113.5(2) . . ? N1 C2 C1 111.7(3) . . ? C3 C2 C1 110.3(2) . . ? N1 C2 H2 107.0 . . ? C3 C2 H2 107.0 . . ? C1 C2 H2 107.0 . . ? O2 C2O H2O1 109.5 . . ? O2 C2O H2O2 109.5 . . ? H2O1 C2O H2O2 109.5 . . ? O2 C2O H2O3 109.5 . . ? H2O1 C2O H2O3 109.5 . . ? H2O2 C2O H2O3 109.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C41 111.1(2) . . ? O2 C4 C5 105.9(2) . . ? C41 C4 C5 114.1(2) . . ? O2 C4 H4 108.5 . . ? C41 C4 H4 108.5 . . ? C5 C4 H4 108.5 . . ? N2 C5 C6 112.5(2) . . ? N2 C5 C4 111.0(2) . . ? C6 C5 C4 112.1(2) . . ? N2 C5 H5 106.9 . . ? C6 C5 H5 106.9 . . ? C4 C5 H5 106.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C16 118.4(3) . . ? C12 C11 C1 121.5(3) . . ? C16 C11 C1 120.0(3) . . ? C11 C12 C13 121.4(4) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 119.2(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 119.9(4) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C22 C21 C26 118.0(3) . . ? C22 C21 P1 121.8(2) . . ? C26 C21 P1 120.1(2) . . ? C21 C22 C23 121.0(3) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 120.3(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.7(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.6(3) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 120.3(3) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C32 C31 C36 118.8(2) . . ? C32 C31 P2 123.04(18) . . ? C36 C31 P2 118.07(18) . . ? C33 C32 C31 119.7(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C34 C33 C32 120.9(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 119.9(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C31 121.0(2) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? C46 C41 C42 117.2(3) . . ? C46 C41 C4 121.6(3) . . ? C42 C41 C4 121.2(3) . . ? C43 C42 C41 121.3(3) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C44 C43 C42 120.9(4) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 119.7(4) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C44 C45 C46 120.1(3) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 120.8(3) . . ? C41 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C55 C51 C52 106.9(2) . . ? C55 C51 P1 128.03(19) . . ? C52 C51 P1 122.81(18) . . ? C55 C51 Fe1 69.74(13) . . ? C52 C51 Fe1 68.72(13) . . ? P1 C51 Fe1 139.69(13) . . ? C53 C52 C51 107.6(2) . . ? C53 C52 Fe1 69.88(15) . . ? C51 C52 Fe1 70.30(13) . . ? C53 C52 H52 126.2 . . ? C51 C52 H52 126.2 . . ? Fe1 C52 H52 125.2 . . ? C54 C53 C52 108.6(2) . . ? C54 C53 Fe1 70.46(16) . . ? C52 C53 Fe1 69.32(15) . . ? C54 C53 H53 125.7 . . ? C52 C53 H53 125.7 . . ? Fe1 C53 H53 126.1 . . ? C53 C54 C55 108.3(2) . . ? C53 C54 Fe1 69.70(17) . . ? C55 C54 Fe1 70.01(14) . . ? C53 C54 H54 125.8 . . ? C55 C54 H54 125.8 . . ? Fe1 C54 H54 126.0 . . ? C54 C55 C51 108.5(2) . . ? C54 C55 Fe1 69.77(15) . . ? C51 C55 Fe1 69.79(14) . . ? C54 C55 H55 125.7 . . ? C51 C55 H55 125.7 . . ? Fe1 C55 H55 126.3 . . ? C62 C61 C65 107.2(2) . . ? C62 C61 P2 125.35(19) . . ? C65 C61 P2 126.9(2) . . ? C62 C61 Fe1 68.78(13) . . ? C65 C61 Fe1 69.67(14) . . ? P2 C61 Fe1 133.00(13) . . ? C63 C62 C61 108.0(3) . . ? C63 C62 Fe1 69.87(16) . . ? C61 C62 Fe1 70.47(13) . . ? C63 C62 H62 126.0 . . ? C61 C62 H62 126.0 . . ? Fe1 C62 H62 125.2 . . ? C64 C63 C62 108.5(3) . . ? C64 C63 Fe1 69.76(17) . . ? C62 C63 Fe1 69.62(15) . . ? C64 C63 H63 125.7 . . ? C62 C63 H63 125.7 . . ? Fe1 C63 H63 126.5 . . ? C63 C64 C65 108.4(2) . . ? C63 C64 Fe1 70.06(17) . . ? C65 C64 Fe1 70.58(15) . . ? C63 C64 H64 125.8 . . ? C65 C64 H64 125.8 . . ? Fe1 C64 H64 125.2 . . ? C64 C65 C61 107.8(3) . . ? C64 C65 Fe1 68.93(16) . . ? C61 C65 Fe1 69.77(14) . . ? C64 C65 H65 126.1 . . ? C61 C65 H65 126.1 . . ? Fe1 C65 H65 126.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.308 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.116