# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Pascal Le Floch' _publ_contact_author_email LEFLOCH@POLY.POLYTECHNIQUE.FR _publ_section_title ; Coordination of tetradentate X2N2 (X = P, S, O) ligands to iron(II) metal center and catalytic application in the transfer hydrogenation of ketones ; loop_ _publ_author_name 'Pascal Le Floch' 'Audrey Auffrant' 'Antoine Buchard' 'Hadrien Heuclin' 'Xavier F. Le Goff' # Attachment 'buchard-dalton.cif' data_ab774 _database_code_depnum_ccdc_archive 'CCDC 702897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Cl2 Fe N2 P4,1.5(C4 H8 O),C H2 Cl2' _chemical_formula_sum 'C59 H62 Cl4 Fe N2 O1.50 P4' _chemical_formula_weight 1144.64 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' 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' _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 36.269(1) _cell_length_b 15.077(1) _cell_length_c 19.211(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.424(1) _cell_angle_gamma 90.00 _cell_volume 10504.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 26666 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4768 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7786 _exptl_absorpt_correction_T_max 0.8907 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34140 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 28.70 _reflns_number_total 13547 _reflns_number_gt 9652 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. One and half C4H8O and one CH2Cl2 molecules present in two cavity (0 0 0) and (0.5 0.5 0.25) were accounted by squeeze platon's function. The phenyl define by C34 to C39 shows large thermal ellispoid indicating possible disorder. We find a model without contrain to explain this disorder. ; _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^)+(0.1007P)^2^+8.2237P] 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 13547 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 Fe1 Fe 0.193284(12) 0.27145(3) 0.22856(2) 0.02814(12) Uani 1 1 d . . . Cl1 Cl 0.19962(2) 0.41792(4) 0.18858(4) 0.03078(16) Uani 1 1 d . . . Cl2 Cl 0.172502(17) 0.15033(4) 0.15678(3) 0.02410(14) Uani 1 1 d . . . P1 P 0.24219(2) 0.16405(4) 0.34476(4) 0.02560(16) Uani 1 1 d . . . P2 P 0.26113(2) 0.21365(4) 0.19882(4) 0.02623(16) Uani 1 1 d . . . P3 P 0.10466(2) 0.30959(6) 0.26549(4) 0.03465(19) Uani 1 1 d . . . P4 P 0.06003(2) 0.34163(6) 0.12832(4) 0.0402(2) Uani 1 1 d . . . N1 N 0.21532(7) 0.24434(15) 0.32622(12) 0.0299(5) Uani 1 1 d . . . N2 N 0.14593(7) 0.29446(18) 0.28970(13) 0.0362(6) Uani 1 1 d . A . C1 C 0.19336(10) 0.2879(2) 0.38014(16) 0.0384(7) Uani 1 1 d . A . H1A H 0.1992 0.3520 0.3815 0.046 Uiso 1 1 calc R . . H1B H 0.1995 0.2622 0.4262 0.046 Uiso 1 1 calc R . . C2 C 0.15280(10) 0.2750(2) 0.36462(16) 0.0420(8) Uani 1 1 d . . . H2A H 0.1455 0.2132 0.3752 0.050 Uiso 1 1 calc R A . H2B H 0.1380 0.3154 0.3939 0.050 Uiso 1 1 calc R . . C3 C 0.21980(8) 0.07631(17) 0.39323(15) 0.0282(6) Uani 1 1 d . . . C4 C 0.23284(9) 0.0442(2) 0.45720(16) 0.0355(7) Uani 1 1 d . . . H4 H 0.2549 0.0675 0.4768 0.043 Uiso 1 1 calc R . . C5 C 0.21343(10) -0.0220(2) 0.49217(18) 0.0419(8) Uani 1 1 d . . . H5 H 0.2224 -0.0441 0.5353 0.050 Uiso 1 1 calc R . . C6 C 0.18136(10) -0.0550(2) 0.46423(19) 0.0438(8) Uani 1 1 d . . . H6 H 0.1681 -0.0999 0.4882 0.053 Uiso 1 1 calc R . . C7 C 0.16819(11) -0.0231(3) 0.4012(2) 0.0542(10) Uani 1 1 d . . . H7 H 0.1459 -0.0462 0.3821 0.065 Uiso 1 1 calc R . . C8 C 0.18714(10) 0.0421(2) 0.36585(18) 0.0443(8) Uani 1 1 d . . . H8 H 0.1779 0.0637 0.3227 0.053 Uiso 1 1 calc R . . C9 C 0.28343(8) 0.19314(18) 0.39294(14) 0.0287(6) Uani 1 1 d . . . C10 C 0.28963(9) 0.28052(19) 0.41319(15) 0.0334(6) Uani 1 1 d . . . H10 H 0.2712 0.3243 0.4051 0.040 Uiso 1 1 calc R . . C11 C 0.32257(10) 0.3038(2) 0.44512(17) 0.0409(7) Uani 1 1 d . . . H11 H 0.3269 0.3636 0.4583 0.049 Uiso 1 1 calc R . . C12 C 0.34922(9) 0.2396(2) 0.45797(17) 0.0411(7) Uani 1 1 d . . . H12 H 0.3719 0.2558 0.4795 0.049 Uiso 1 1 calc R . . C13 C 0.34286(9) 0.1521(2) 0.43949(16) 0.0395(7) Uani 1 1 d . . . H13 H 0.3609 0.1081 0.4496 0.047 Uiso 1 1 calc R . . C14 C 0.31049(9) 0.1287(2) 0.40645(15) 0.0331(6) Uani 1 1 d . . . H14 H 0.3065 0.0689 0.3928 0.040 Uiso 1 1 calc R . . C15 C 0.25779(8) 0.12118(17) 0.26232(14) 0.0270(6) Uani 1 1 d . . . H15A H 0.2402 0.0759 0.2448 0.032 Uiso 1 1 calc R . . H15B H 0.2822 0.0927 0.2683 0.032 Uiso 1 1 calc R . . C16 C 0.30134(9) 0.27530(19) 0.23079(15) 0.0322(6) Uani 1 1 d . . . C17 C 0.33643(10) 0.2381(2) 0.23410(18) 0.0441(8) Uani 1 1 d . . . H17 H 0.3399 0.1785 0.2195 0.053 Uiso 1 1 calc R . . C18 C 0.36634(11) 0.2864(3) 0.2583(2) 0.0571(10) Uani 1 1 d . . . H18 H 0.3902 0.2605 0.2598 0.069 Uiso 1 1 calc R . . C19 C 0.36106(13) 0.3729(3) 0.2801(2) 0.0633(12) Uani 1 1 d . . . H19 H 0.3815 0.4063 0.2967 0.076 Uiso 1 1 calc R . . C20 C 0.32676(13) 0.4112(2) 0.2781(2) 0.0551(10) Uani 1 1 d . . . H20 H 0.3233 0.4701 0.2943 0.066 Uiso 1 1 calc R . . C21 C 0.29668(10) 0.3622(2) 0.25162(17) 0.0432(8) Uani 1 1 d . . . H21 H 0.2731 0.3891 0.2481 0.052 Uiso 1 1 calc R . . C22 C 0.28075(8) 0.15910(18) 0.12266(14) 0.0280(6) Uani 1 1 d . . . C23 C 0.29400(8) 0.07256(18) 0.12038(15) 0.0316(6) Uani 1 1 d . . . H23 H 0.2924 0.0357 0.1604 0.038 Uiso 1 1 calc R . . C24 C 0.30959(9) 0.03982(19) 0.05930(15) 0.0336(6) Uani 1 1 d . . . H24 H 0.3186 -0.0194 0.0580 0.040 Uiso 1 1 calc R . . C25 C 0.31211(9) 0.0929(2) 0.00050(16) 0.0352(7) Uani 1 1 d . . . H25 H 0.3229 0.0705 -0.0408 0.042 Uiso 1 1 calc R . . C26 C 0.29870(9) 0.1788(2) 0.00258(16) 0.0366(7) Uani 1 1 d . . . H26 H 0.3001 0.2154 -0.0375 0.044 Uiso 1 1 calc R . . C27 C 0.28323(9) 0.21136(19) 0.06281(15) 0.0325(6) Uani 1 1 d . . . H27 H 0.2741 0.2704 0.0636 0.039 Uiso 1 1 calc R . . C28 C 0.08426(9) 0.4088(2) 0.30285(16) 0.0342(6) Uani 1 1 d . A . C29 C 0.04683(10) 0.4269(3) 0.3019(2) 0.0490(9) Uani 1 1 d . . . H29 H 0.0299 0.3847 0.2835 0.059 Uiso 1 1 calc R A . C30 C 0.03395(11) 0.5077(3) 0.3280(2) 0.0565(10) Uani 1 1 d . A . H30 H 0.0083 0.5202 0.3277 0.068 Uiso 1 1 calc R . . C31 C 0.05841(12) 0.5692(3) 0.3542(2) 0.0543(10) Uani 1 1 d . . . H31 H 0.0496 0.6237 0.3724 0.065 Uiso 1 1 calc R A . C32 C 0.09566(11) 0.5519(2) 0.3539(2) 0.0515(9) Uani 1 1 d . A . H32 H 0.1126 0.5948 0.3713 0.062 Uiso 1 1 calc R . . C33 C 0.10851(9) 0.4717(2) 0.32826(18) 0.0428(8) Uani 1 1 d . . . H33 H 0.1342 0.4599 0.3282 0.051 Uiso 1 1 calc R A . C34A C 0.0724(2) 0.2169(4) 0.2868(4) 0.039(3) Uani 0.464(10) 1 d PG A 1 C35A C 0.0882(2) 0.1345(4) 0.2745(6) 0.054(3) Uani 0.464(10) 1 d PG A 1 H35A H 0.1124 0.1307 0.2560 0.064 Uiso 0.464(10) 1 calc PR A 1 C36A C 0.0687(3) 0.0575(3) 0.2893(7) 0.074(4) Uani 0.464(10) 1 d PG A 1 H36A H 0.0795 0.0012 0.2809 0.089 Uiso 0.464(10) 1 calc PR A 1 C37A C 0.0333(3) 0.0630(4) 0.3164(7) 0.102(6) Uani 0.464(10) 1 d PG A 1 H37A H 0.0199 0.0105 0.3265 0.122 Uiso 0.464(10) 1 calc PR A 1 C38A C 0.0175(2) 0.1455(6) 0.3287(7) 0.104(6) Uani 0.464(10) 1 d PG A 1 H38A H -0.0067 0.1492 0.3472 0.124 Uiso 0.464(10) 1 calc PR A 1 C39A C 0.0370(2) 0.2224(4) 0.3139(5) 0.075(4) Uani 0.464(10) 1 d PG A 1 H39A H 0.0262 0.2788 0.3223 0.090 Uiso 0.464(10) 1 calc PR A 1 C34B C 0.07807(13) 0.2141(3) 0.28853(11) 0.055(4) Uani 0.536(10) 1 d PG A 2 C35B C 0.08053(15) 0.1374(2) 0.24865(14) 0.104(7) Uani 0.536(10) 1 d PG A 2 H35B H 0.0942 0.1377 0.2067 0.125 Uiso 0.536(10) 1 calc PR A 2 C36B C 0.0630(2) 0.0603(2) 0.2702(2) 0.148(11) Uani 0.536(10) 1 d PG A 2 H36B H 0.0647 0.0079 0.2429 0.178 Uiso 0.536(10) 1 calc PR A 2 C37B C 0.0430(2) 0.0598(3) 0.3316(2) 0.152(10) Uani 0.536(10) 1 d PG A 2 H37B H 0.0310 0.0071 0.3463 0.183 Uiso 0.536(10) 1 calc PR A 2 C38B C 0.04050(19) 0.1365(4) 0.37150(18) 0.119(7) Uani 0.536(10) 1 d PG A 2 H38B H 0.0268 0.1362 0.4135 0.143 Uiso 0.536(10) 1 calc PR A 2 C39B C 0.05805(15) 0.2136(3) 0.34996(13) 0.077(4) Uani 0.536(10) 1 d PG A 2 H39B H 0.0564 0.2660 0.3772 0.092 Uiso 0.536(10) 1 calc PR A 2 C40 C 0.10513(7) 0.32416(18) 0.17205(10) 0.0398(7) Uani 1 1 d G A . H40A H 0.1168 0.2712 0.1512 0.048 Uiso 1 1 calc R . . H40B H 0.1211 0.3756 0.1614 0.048 Uiso 1 1 calc R . . C41 C 0.06784(6) 0.28377(17) 0.04540(11) 0.0391(7) Uani 1 1 d G A . C42 C 0.10166(7) 0.27966(16) 0.01227(10) 0.0407(7) Uani 1 1 d G . . H42 H 0.1224 0.3074 0.0333 0.049 Uiso 1 1 calc R A . C43 C 0.10593(11) 0.2365(2) -0.05026(19) 0.0484(9) Uani 1 1 d . A . H43 H 0.1294 0.2343 -0.0720 0.058 Uiso 1 1 calc R . . C44 C 0.07552(14) 0.1961(3) -0.0812(2) 0.0606(11) Uani 1 1 d . . . H44 H 0.0781 0.1660 -0.1244 0.073 Uiso 1 1 calc R A . C45 C 0.04188(13) 0.1995(3) -0.0498(2) 0.0634(11) Uani 1 1 d . A . H45 H 0.0212 0.1722 -0.0715 0.076 Uiso 1 1 calc R . . C46 C 0.03759(11) 0.2420(3) 0.0128(2) 0.0519(9) Uani 1 1 d . . . H46 H 0.0141 0.2433 0.0343 0.062 Uiso 1 1 calc R A . C47 C 0.06294(9) 0.4572(2) 0.09902(18) 0.0433(8) Uani 1 1 d . A . C48 C 0.07531(11) 0.5246(3) 0.1420(2) 0.0542(9) Uani 1 1 d . . . H48 H 0.0861 0.5105 0.1859 0.065 Uiso 1 1 calc R A . C49 C 0.07217(13) 0.6128(3) 0.1217(2) 0.0634(11) Uani 1 1 d . A . H49 H 0.0807 0.6581 0.1521 0.076 Uiso 1 1 calc R . . C50 C 0.05700(12) 0.6357(3) 0.0588(3) 0.0645(11) Uani 1 1 d . . . H50 H 0.0541 0.6962 0.0463 0.077 Uiso 1 1 calc R A . C51 C 0.04611(17) 0.5704(3) 0.0144(3) 0.0855(16) Uani 1 1 d . A . H51 H 0.0370 0.5851 -0.0306 0.103 Uiso 1 1 calc R . . C52 C 0.04822(15) 0.4816(3) 0.0350(2) 0.0719(13) Uani 1 1 d . . . H52 H 0.0394 0.4368 0.0043 0.086 Uiso 1 1 calc R A . 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 0.0337(2) 0.0274(2) 0.0233(2) 0.00085(15) 0.00053(16) 0.00422(16) Cl1 0.0461(4) 0.0156(3) 0.0305(3) 0.0062(2) -0.0069(3) -0.0010(2) Cl2 0.0256(3) 0.0205(3) 0.0262(3) -0.0042(2) 0.0014(2) -0.0004(2) P1 0.0296(4) 0.0236(3) 0.0236(3) 0.0007(3) 0.0007(3) 0.0025(3) P2 0.0295(4) 0.0243(3) 0.0249(4) 0.0005(3) 0.0018(3) 0.0007(3) P3 0.0327(4) 0.0410(4) 0.0302(4) -0.0028(3) 0.0015(3) 0.0060(3) P4 0.0296(4) 0.0553(5) 0.0356(4) -0.0023(4) -0.0003(3) 0.0027(4) N1 0.0368(14) 0.0302(11) 0.0227(11) 0.0009(9) 0.0018(10) 0.0071(10) N2 0.0368(15) 0.0479(15) 0.0239(12) 0.0004(11) 0.0024(10) 0.0102(11) C1 0.050(2) 0.0414(16) 0.0240(14) -0.0035(12) -0.0024(13) 0.0160(14) C2 0.0445(19) 0.057(2) 0.0248(15) 0.0029(14) 0.0051(13) 0.0196(15) C3 0.0303(15) 0.0254(13) 0.0289(14) 0.0000(11) 0.0029(11) 0.0010(11) C4 0.0350(16) 0.0369(15) 0.0344(16) 0.0092(13) 0.0011(13) 0.0014(12) C5 0.045(2) 0.0373(16) 0.0438(18) 0.0131(14) 0.0063(15) 0.0039(14) C6 0.048(2) 0.0349(16) 0.049(2) 0.0064(14) 0.0135(16) -0.0061(14) C7 0.051(2) 0.064(2) 0.048(2) 0.0036(18) 0.0014(17) -0.0275(18) C8 0.043(2) 0.054(2) 0.0360(17) 0.0052(15) -0.0049(14) -0.0130(15) C9 0.0307(15) 0.0317(14) 0.0236(13) 0.0018(11) 0.0012(11) 0.0006(11) C10 0.0388(17) 0.0316(14) 0.0299(15) -0.0010(12) -0.0011(12) 0.0008(12) C11 0.047(2) 0.0396(16) 0.0359(17) -0.0045(14) -0.0001(14) -0.0081(14) C12 0.0322(17) 0.057(2) 0.0338(16) -0.0006(15) -0.0014(13) -0.0089(14) C13 0.0347(17) 0.0487(18) 0.0350(16) 0.0072(14) 0.0002(13) 0.0034(14) C14 0.0353(16) 0.0330(14) 0.0310(15) 0.0013(12) 0.0003(12) 0.0020(12) C15 0.0311(15) 0.0237(12) 0.0261(13) 0.0007(10) 0.0024(11) 0.0026(10) C16 0.0370(16) 0.0347(15) 0.0250(14) 0.0032(12) 0.0007(12) -0.0068(12) C17 0.0384(19) 0.0516(19) 0.0423(19) -0.0020(15) -0.0018(15) -0.0039(15) C18 0.036(2) 0.080(3) 0.054(2) 0.005(2) -0.0075(17) -0.0136(18) C19 0.066(3) 0.077(3) 0.047(2) 0.013(2) -0.0126(19) -0.043(2) C20 0.073(3) 0.0398(18) 0.052(2) 0.0007(16) -0.0080(19) -0.0238(18) C21 0.053(2) 0.0356(16) 0.0409(18) 0.0004(14) -0.0045(15) -0.0065(14) C22 0.0274(14) 0.0296(13) 0.0270(14) -0.0003(11) 0.0001(11) -0.0023(11) C23 0.0370(16) 0.0288(13) 0.0291(14) 0.0015(11) 0.0026(12) -0.0006(11) C24 0.0397(17) 0.0303(14) 0.0310(15) -0.0038(12) 0.0044(13) -0.0003(12) C25 0.0367(17) 0.0401(16) 0.0289(15) -0.0055(13) 0.0043(12) -0.0039(13) C26 0.0385(17) 0.0426(16) 0.0289(15) 0.0061(13) 0.0028(13) -0.0025(13) C27 0.0348(16) 0.0318(14) 0.0310(15) 0.0041(12) 0.0001(12) 0.0012(12) C28 0.0325(16) 0.0403(16) 0.0297(15) -0.0025(12) 0.0036(12) 0.0057(12) C29 0.0321(18) 0.062(2) 0.053(2) -0.0177(18) 0.0022(15) 0.0031(15) C30 0.0345(19) 0.074(3) 0.061(2) -0.015(2) 0.0039(17) 0.0175(18) C31 0.061(3) 0.046(2) 0.056(2) -0.0111(17) 0.0058(19) 0.0135(18) C32 0.050(2) 0.0469(19) 0.058(2) -0.0097(17) 0.0082(18) -0.0026(16) C33 0.0316(17) 0.0508(19) 0.0459(19) -0.0058(15) -0.0021(14) 0.0003(14) C34A 0.036(5) 0.025(6) 0.054(9) -0.004(5) 0.000(5) 0.007(4) C35A 0.043(5) 0.038(5) 0.080(7) -0.025(4) 0.017(5) 0.001(4) C36A 0.078(10) 0.041(7) 0.104(9) -0.012(6) 0.040(8) 0.002(6) C37A 0.115(12) 0.069(11) 0.122(13) -0.034(9) 0.068(10) -0.033(8) C38A 0.051(7) 0.079(8) 0.182(17) 0.002(9) 0.047(9) -0.004(6) C39A 0.064(7) 0.055(6) 0.106(10) 0.014(6) 0.031(7) 0.008(5) C34B 0.040(5) 0.074(9) 0.050(9) -0.011(6) 0.020(5) -0.004(5) C35B 0.127(12) 0.076(8) 0.110(11) -0.054(7) 0.068(10) -0.053(8) C36B 0.139(16) 0.084(11) 0.22(2) -0.081(12) 0.122(15) -0.062(10) C37B 0.151(15) 0.044(8) 0.26(3) 0.010(11) 0.116(17) -0.014(8) C38B 0.140(13) 0.050(5) 0.170(14) 0.000(7) 0.111(12) -0.012(7) C39B 0.092(8) 0.048(4) 0.091(8) -0.004(5) 0.049(6) 0.001(5) C40 0.0328(17) 0.0549(19) 0.0317(16) -0.0047(14) 0.0005(13) 0.0090(14) C41 0.0369(17) 0.0418(17) 0.0386(17) 0.0017(14) -0.0033(14) -0.0011(13) C42 0.0393(18) 0.0463(18) 0.0366(17) -0.0007(14) 0.0002(14) 0.0005(14) C43 0.055(2) 0.051(2) 0.0396(19) 0.0014(16) 0.0011(16) 0.0077(17) C44 0.083(3) 0.052(2) 0.046(2) -0.0101(18) -0.008(2) 0.005(2) C45 0.070(3) 0.064(3) 0.055(2) -0.007(2) -0.020(2) -0.019(2) C46 0.046(2) 0.061(2) 0.049(2) 0.0017(18) -0.0081(17) -0.0082(17) C47 0.0321(17) 0.055(2) 0.0424(18) -0.0066(15) -0.0014(14) 0.0076(14) C48 0.055(2) 0.060(2) 0.047(2) -0.0032(18) -0.0051(17) -0.0081(18) C49 0.070(3) 0.060(2) 0.061(3) -0.012(2) 0.002(2) -0.010(2) C50 0.053(3) 0.054(2) 0.086(3) 0.004(2) -0.003(2) 0.0056(19) C51 0.103(4) 0.069(3) 0.084(4) 0.013(3) -0.041(3) 0.005(3) C52 0.095(4) 0.056(2) 0.065(3) -0.007(2) -0.035(2) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.074(2) . ? Fe1 N2 2.116(2) . ? Fe1 Cl1 2.3498(7) . ? Fe1 Cl2 2.4061(7) . ? Fe1 P2 2.6762(8) . ? P1 N1 1.593(2) . ? P1 C15 1.805(3) . ? P1 C9 1.807(3) . ? P1 C3 1.813(3) . ? P2 C22 1.827(3) . ? P2 C16 1.832(3) . ? P2 C15 1.857(3) . ? P3 N2 1.581(3) . ? P3 C34B 1.791(4) . ? P3 C40 1.809(2) . ? P3 C28 1.819(3) . ? P3 C34A 1.870(5) . ? P4 C47 1.835(4) . ? P4 C41 1.840(2) . ? P4 C40 1.852(3) . ? N1 C1 1.466(4) . ? N2 C2 1.488(4) . ? C1 C2 1.511(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.392(4) . ? C3 C4 1.400(4) . ? C4 C5 1.396(4) . ? C4 H4 0.9500 . ? C5 C6 1.371(5) . ? C5 H5 0.9500 . ? C6 C7 1.385(5) . ? C6 H6 0.9500 . ? C7 C8 1.380(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.392(4) . ? C9 C14 1.404(4) . ? C10 C11 1.384(5) . ? C10 H10 0.9500 . ? C11 C12 1.388(5) . ? C11 H11 0.9500 . ? C12 C13 1.385(5) . ? C12 H12 0.9500 . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.380(4) . ? C16 C17 1.392(5) . ? C17 C18 1.385(5) . ? C17 H17 0.9500 . ? C18 C19 1.384(6) . ? C18 H18 0.9500 . ? C19 C20 1.372(6) . ? C19 H19 0.9500 . ? C20 C21 1.409(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.391(4) . ? C22 C27 1.397(4) . ? C23 C24 1.397(4) . ? C23 H23 0.9500 . ? C24 C25 1.388(4) . ? C24 H24 0.9500 . ? C25 C26 1.384(4) . ? C25 H25 0.9500 . ? C26 C27 1.380(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.379(5) . ? C28 C29 1.385(5) . ? C29 C30 1.400(5) . ? C29 H29 0.9500 . ? C30 C31 1.375(6) . ? C30 H30 0.9500 . ? C31 C32 1.376(6) . ? C31 H31 0.9500 . ? C32 C33 1.388(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34A C35A 1.3900 . ? C34A C39A 1.3900 . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A C37A 1.3900 . ? C36A H36A 0.9500 . ? C37A C38A 1.3900 . ? C37A H37A 0.9500 . ? C38A C39A 1.3900 . ? C38A H38A 0.9500 . ? C39A H39A 0.9500 . ? C34B C35B 1.3900 . ? C34B C39B 1.3900 . ? C35B C36B 1.3900 . ? C35B H35B 0.9500 . ? C36B C37B 1.3900 . ? C36B H36B 0.9500 . ? C37B C38B 1.3900 . ? C37B H37B 0.9500 . ? C38B C39B 1.3900 . ? C38B H38B 0.9500 . ? C39B H39B 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.3872 . ? C41 C46 1.408(4) . ? C42 C43 1.376(4) . ? C42 H42 0.9500 . ? C43 C44 1.390(6) . ? C43 H43 0.9500 . ? C44 C45 1.367(6) . ? C44 H44 0.9500 . ? C45 C46 1.372(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.382(5) . ? C47 C52 1.387(5) . ? C48 C49 1.391(6) . ? C48 H48 0.9500 . ? C49 C50 1.368(6) . ? C49 H49 0.9500 . ? C50 C51 1.358(7) . ? C50 H50 0.9500 . ? C51 C52 1.398(6) . ? C51 H51 0.9500 . ? C52 H52 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 N1 Fe1 N2 80.75(10) . . ? N1 Fe1 Cl1 116.28(7) . . ? N2 Fe1 Cl1 96.26(8) . . ? N1 Fe1 Cl2 119.06(7) . . ? N2 Fe1 Cl2 100.98(8) . . ? Cl1 Fe1 Cl2 123.84(3) . . ? N1 Fe1 P2 77.30(7) . . ? N2 Fe1 P2 157.38(7) . . ? Cl1 Fe1 P2 98.27(3) . . ? Cl2 Fe1 P2 85.13(2) . . ? N1 P1 C15 105.74(12) . . ? N1 P1 C9 115.64(13) . . ? C15 P1 C9 105.81(13) . . ? N1 P1 C3 113.20(13) . . ? C15 P1 C3 109.49(12) . . ? C9 P1 C3 106.63(13) . . ? C22 P2 C16 100.55(13) . . ? C22 P2 C15 102.46(12) . . ? C16 P2 C15 102.49(13) . . ? C22 P2 Fe1 132.97(10) . . ? C16 P2 Fe1 119.62(10) . . ? C15 P2 Fe1 92.28(9) . . ? N2 P3 C34B 108.77(17) . . ? N2 P3 C40 107.09(13) . . ? C34B P3 C40 110.61(15) . . ? N2 P3 C28 112.93(15) . . ? C34B P3 C28 110.04(16) . . ? C40 P3 C28 107.37(14) . . ? N2 P3 C34A 114.9(3) . . ? C34B P3 C34A 6.2(3) . . ? C40 P3 C34A 108.6(3) . . ? C28 P3 C34A 105.7(2) . . ? C47 P4 C41 100.09(14) . . ? C47 P4 C40 102.81(14) . . ? C41 P4 C40 100.61(10) . . ? C1 N1 P1 121.11(19) . . ? C1 N1 Fe1 110.06(18) . . ? P1 N1 Fe1 125.67(13) . . ? C2 N2 P3 117.7(2) . . ? C2 N2 Fe1 111.95(19) . . ? P3 N2 Fe1 129.11(14) . . ? N1 C1 C2 109.7(3) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 108.7(3) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C8 C3 C4 119.0(3) . . ? C8 C3 P1 117.4(2) . . ? C4 C3 P1 123.6(2) . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.0(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.1(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C3 120.2(3) . . ? C7 C8 H8 119.9 . . ? C3 C8 H8 119.9 . . ? C10 C9 C14 119.5(3) . . ? C10 C9 P1 120.3(2) . . ? C14 C9 P1 120.1(2) . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 120.1(3) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? P1 C15 P2 109.25(14) . . ? P1 C15 H15A 109.8 . . ? P2 C15 H15A 109.8 . . ? P1 C15 H15B 109.8 . . ? P2 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? C21 C16 C17 118.9(3) . . ? C21 C16 P2 118.7(3) . . ? C17 C16 P2 122.4(2) . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C17 119.2(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C18 121.0(4) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 119.3(4) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C16 C21 C20 120.4(4) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C27 118.6(3) . . ? C23 C22 P2 125.7(2) . . ? C27 C22 P2 115.7(2) . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.6(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 119.4(3) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C27 C26 C25 120.1(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C22 121.2(3) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C33 C28 C29 119.5(3) . . ? C33 C28 P3 116.4(2) . . ? C29 C28 P3 123.9(3) . . ? C28 C29 C30 119.8(3) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.1(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 119.9(4) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C28 C33 C32 120.6(3) . . ? C28 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35A C34A C39A 120.0 . . ? C35A C34A P3 111.8(4) . . ? C39A C34A P3 128.2(4) . . ? C34A C35A C36A 120.0 . . ? C34A C35A H35A 120.0 . . ? C36A C35A H35A 120.0 . . ? C35A C36A C37A 120.0 . . ? C35A C36A H36A 120.0 . . ? C37A C36A H36A 120.0 . . ? C38A C37A C36A 120.0 . . ? C38A C37A H37A 120.0 . . ? C36A C37A H37A 120.0 . . ? C39A C38A C37A 120.0 . . ? C39A C38A H38A 120.0 . . ? C37A C38A H38A 120.0 . . ? C38A C39A C34A 120.0 . . ? C38A C39A H39A 120.0 . . ? C34A C39A H39A 120.0 . . ? C35B C34B C39B 120.0 . . ? C35B C34B P3 119.72(10) . . ? C39B C34B P3 119.95(9) . . ? C34B C35B C36B 120.0 . . ? C34B C35B H35B 120.0 . . ? C36B C35B H35B 120.0 . . ? C37B C36B C35B 120.0 . . ? C37B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C36B C37B C38B 120.0 . . ? C36B C37B H37B 120.0 . . ? C38B C37B H37B 120.0 . . ? C39B C38B C37B 120.0 . . ? C39B C38B H38B 120.0 . . ? C37B C38B H38B 120.0 . . ? C38B C39B C34B 120.0 . . ? C38B C39B H39B 120.0 . . ? C34B C39B H39B 120.0 . . ? P3 C40 P4 116.92(14) . . ? P3 C40 H40A 108.1 . . ? P4 C40 H40A 108.1 . . ? P3 C40 H40B 108.1 . . ? P4 C40 H40B 108.1 . . ? H40A C40 H40B 107.3 . . ? C42 C41 C46 117.7(2) . . ? C42 C41 P4 124.10(9) . . ? C46 C41 P4 118.2(2) . . ? C43 C42 C41 121.8(2) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C42 C43 C44 119.1(4) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 120.1(4) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.8(4) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C45 C46 C41 120.4(4) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C48 C47 C52 117.2(4) . . ? C48 C47 P4 122.3(3) . . ? C52 C47 P4 120.0(3) . . ? C47 C48 C49 120.6(4) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C50 C49 C48 121.4(4) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C51 C50 C49 119.0(4) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C50 C51 C52 120.1(5) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C47 C52 C51 121.6(4) . . ? C47 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.499 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.086 #===END #Compound 6 data_ab651 _database_code_depnum_ccdc_archive 'CCDC 702898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C52H46Cl2FeN2P4S2,3(CH2Cl2) _chemical_formula_sum 'C55 H52 Cl8 Fe N2 P4 S2' _chemical_formula_weight 1268.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 13.700(1) _cell_length_b 15.476(1) _cell_length_c 15.866(1) _cell_angle_alpha 91.952(1) _cell_angle_beta 114.158(1) _cell_angle_gamma 103.426(1) _cell_volume 2953.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 3509 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7879 _exptl_absorpt_correction_T_max 0.9212 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39926 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 30.03 _reflns_number_total 17238 _reflns_number_gt 12502 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0623P)^2^+2.2673P] 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 17238 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.78527(3) 0.21892(2) 0.48239(2) 0.02053(8) Uani 1 1 d . . . Cl1 Cl 0.65992(5) 0.16286(4) 0.54306(5) 0.02986(14) Uani 1 1 d . . . Cl2 Cl 0.80695(5) 0.36456(4) 0.45137(4) 0.02697(13) Uani 1 1 d . . . S1 S 1.16390(6) 0.36352(5) 0.89537(5) 0.03402(16) Uani 1 1 d . . . S2 S 0.38812(5) 0.08801(4) 0.08051(4) 0.02752(14) Uani 1 1 d . . . P1 P 1.01624(5) 0.21840(4) 0.65533(4) 0.02025(12) Uani 1 1 d . . . P2 P 0.67552(5) 0.11617(4) 0.27019(4) 0.02019(12) Uani 1 1 d . . . P3 P 1.00413(5) 0.30979(4) 0.83063(4) 0.02497(14) Uani 1 1 d . . . P4 P 0.47617(5) 0.20091(4) 0.16315(4) 0.02125(13) Uani 1 1 d . . . N1 N 0.92847(16) 0.18460(14) 0.54890(13) 0.0226(4) Uani 1 1 d . . . N2 N 0.77076(16) 0.13632(13) 0.37418(14) 0.0230(4) Uani 1 1 d . . . C1 C 0.9564(2) 0.13401(17) 0.48522(17) 0.0247(5) Uani 1 1 d . . . H1A H 1.0004 0.0935 0.5192 0.030 Uiso 1 1 calc R . . H1B H 1.0014 0.1761 0.4608 0.030 Uiso 1 1 calc R . . C2 C 0.8489(2) 0.07954(17) 0.40493(17) 0.0251(5) Uani 1 1 d . . . H2A H 0.8641 0.0602 0.3525 0.030 Uiso 1 1 calc R . . H2B H 0.8160 0.0253 0.4256 0.030 Uiso 1 1 calc R . . C3 C 1.14797(19) 0.29090(16) 0.67111(16) 0.0227(5) Uani 1 1 d . . . C4 C 1.1606(2) 0.38323(18) 0.66817(19) 0.0308(6) Uani 1 1 d . . . H4 H 1.1012 0.4079 0.6624 0.037 Uiso 1 1 calc R . . C5 C 1.2586(2) 0.43847(19) 0.6736(2) 0.0358(6) Uani 1 1 d . . . H5 H 1.2666 0.5009 0.6718 0.043 Uiso 1 1 calc R . . C6 C 1.3449(2) 0.4028(2) 0.6818(2) 0.0370(6) Uani 1 1 d . . . H6 H 1.4127 0.4409 0.6865 0.044 Uiso 1 1 calc R . . C7 C 1.3329(2) 0.3116(2) 0.6831(2) 0.0379(7) Uani 1 1 d . . . H7 H 1.3921 0.2871 0.6877 0.045 Uiso 1 1 calc R . . C8 C 1.2347(2) 0.25571(18) 0.67772(19) 0.0294(5) Uani 1 1 d . . . H8 H 1.2269 0.1932 0.6786 0.035 Uiso 1 1 calc R . . C9 C 1.04274(19) 0.12514(16) 0.71847(16) 0.0222(5) Uani 1 1 d . . . C10 C 0.9626(2) 0.04295(17) 0.68148(18) 0.0278(5) Uani 1 1 d . . . H10 H 0.8991 0.0374 0.6243 0.033 Uiso 1 1 calc R . . C11 C 0.9756(2) -0.03109(19) 0.7283(2) 0.0344(6) Uani 1 1 d . . . H11 H 0.9216 -0.0874 0.7028 0.041 Uiso 1 1 calc R . . C12 C 1.0676(2) -0.0220(2) 0.8122(2) 0.0340(6) Uani 1 1 d . . . H12 H 1.0763 -0.0722 0.8445 0.041 Uiso 1 1 calc R . . C13 C 1.1467(2) 0.0593(2) 0.84936(19) 0.0322(6) Uani 1 1 d . . . H13 H 1.2093 0.0648 0.9073 0.039 Uiso 1 1 calc R . . C14 C 1.1355(2) 0.13310(18) 0.80271(17) 0.0274(5) Uani 1 1 d . . . H14 H 1.1908 0.1888 0.8280 0.033 Uiso 1 1 calc R . . C15 C 0.9498(2) 0.28120(17) 0.70360(16) 0.0239(5) Uani 1 1 d . . . H15 H 0.8870 0.2993 0.6632 0.029 Uiso 1 1 calc R . . C16 C 0.9557(2) 0.20786(17) 0.87176(17) 0.0248(5) Uani 1 1 d . . . C17 C 1.0236(2) 0.19316(18) 0.96023(18) 0.0281(5) Uani 1 1 d . . . H17 H 1.0943 0.2343 0.9957 0.034 Uiso 1 1 calc R . . C18 C 0.9876(2) 0.11791(19) 0.99670(19) 0.0317(6) Uani 1 1 d . . . H18 H 1.0343 0.1076 1.0568 0.038 Uiso 1 1 calc R . . C19 C 0.8843(2) 0.05814(18) 0.9458(2) 0.0320(6) Uani 1 1 d . . . H19 H 0.8599 0.0075 0.9713 0.038 Uiso 1 1 calc R . . C20 C 0.8166(2) 0.07222(18) 0.85762(19) 0.0324(6) Uani 1 1 d . . . H20 H 0.7456 0.0312 0.8228 0.039 Uiso 1 1 calc R . . C21 C 0.8525(2) 0.14664(18) 0.81994(18) 0.0300(6) Uani 1 1 d . . . H21 H 0.8066 0.1556 0.7589 0.036 Uiso 1 1 calc R . . C22 C 0.9245(3) 0.38468(19) 0.8422(2) 0.0356(6) Uani 1 1 d . . . C23 C 0.9779(3) 0.4741(2) 0.8773(3) 0.0526(9) Uani 1 1 d . . . H23 H 1.0552 0.4959 0.8941 0.063 Uiso 1 1 calc R . . C24 C 0.9194(4) 0.5326(3) 0.8882(3) 0.0647(11) Uani 1 1 d . . . H24 H 0.9566 0.5943 0.9107 0.078 Uiso 1 1 calc R . . C25 C 0.8094(4) 0.5020(3) 0.8669(3) 0.0694(12) Uani 1 1 d . . . H25 H 0.7708 0.5410 0.8789 0.083 Uiso 1 1 calc R . . C26 C 0.7557(5) 0.4154(3) 0.8285(6) 0.129(3) Uani 1 1 d . . . H26 H 0.6779 0.3945 0.8097 0.155 Uiso 1 1 calc R . . C27 C 0.8127(4) 0.3569(3) 0.8163(5) 0.106(2) Uani 1 1 d . . . H27 H 0.7735 0.2962 0.7894 0.127 Uiso 1 1 calc R . . C28 C 0.72858(19) 0.14680(16) 0.18509(17) 0.0227(5) Uani 1 1 d . . . C29 C 0.8323(2) 0.20919(17) 0.21907(19) 0.0286(5) Uani 1 1 d . . . H29 H 0.8738 0.2284 0.2843 0.034 Uiso 1 1 calc R . . C30 C 0.8753(2) 0.24347(19) 0.1577(2) 0.0353(6) Uani 1 1 d . . . H30 H 0.9456 0.2867 0.1809 0.042 Uiso 1 1 calc R . . C31 C 0.8157(3) 0.2145(2) 0.0628(2) 0.0367(6) Uani 1 1 d . . . H31 H 0.8451 0.2381 0.0210 0.044 Uiso 1 1 calc R . . C32 C 0.7134(2) 0.1514(2) 0.02843(19) 0.0342(6) Uani 1 1 d . . . H32 H 0.6738 0.1307 -0.0367 0.041 Uiso 1 1 calc R . . C33 C 0.6685(2) 0.11810(18) 0.08902(18) 0.0278(5) Uani 1 1 d . . . H33 H 0.5973 0.0761 0.0652 0.033 Uiso 1 1 calc R . . C34 C 0.59306(19) 0.00087(16) 0.23992(16) 0.0224(5) Uani 1 1 d . . . C35 C 0.6005(2) -0.06190(18) 0.1802(2) 0.0316(6) Uani 1 1 d . . . H35 H 0.6467 -0.0440 0.1493 0.038 Uiso 1 1 calc R . . C36 C 0.5402(3) -0.15125(19) 0.1655(2) 0.0412(7) Uani 1 1 d . . . H36 H 0.5446 -0.1941 0.1238 0.049 Uiso 1 1 calc R . . C37 C 0.4740(2) -0.17772(19) 0.2114(2) 0.0399(7) Uani 1 1 d . . . H37 H 0.4327 -0.2387 0.2009 0.048 Uiso 1 1 calc R . . C38 C 0.4677(2) -0.1161(2) 0.2725(2) 0.0376(7) Uani 1 1 d . . . H38 H 0.4225 -0.1346 0.3042 0.045 Uiso 1 1 calc R . . C39 C 0.5275(2) -0.02692(19) 0.2873(2) 0.0329(6) Uani 1 1 d . . . H39 H 0.5239 0.0154 0.3300 0.039 Uiso 1 1 calc R . . C40 C 0.58899(19) 0.18840(16) 0.27107(16) 0.0237(5) Uani 1 1 d . . . H40 H 0.6024 0.2204 0.3286 0.028 Uiso 1 1 calc R . . C41 C 0.5329(2) 0.28750(16) 0.10916(18) 0.0254(5) Uani 1 1 d . . . C42 C 0.4584(3) 0.30401(19) 0.0240(2) 0.0369(6) Uani 1 1 d . . . H42 H 0.3834 0.2685 -0.0038 0.044 Uiso 1 1 calc R . . C43 C 0.4934(3) 0.3721(2) -0.0203(2) 0.0488(8) Uani 1 1 d . . . H43 H 0.4423 0.3835 -0.0779 0.059 Uiso 1 1 calc R . . C44 C 0.6032(3) 0.4235(2) 0.0198(3) 0.0507(9) Uani 1 1 d . . . H44 H 0.6275 0.4695 -0.0109 0.061 Uiso 1 1 calc R . . C45 C 0.6774(3) 0.4078(2) 0.1044(3) 0.0520(9) Uani 1 1 d . . . H45 H 0.7524 0.4433 0.1317 0.062 Uiso 1 1 calc R . . C46 C 0.6426(2) 0.34008(18) 0.1498(2) 0.0379(7) Uani 1 1 d . . . H46 H 0.6935 0.3299 0.2083 0.045 Uiso 1 1 calc R . . C47 C 0.3986(2) 0.25447(17) 0.20776(17) 0.0255(5) Uani 1 1 d . . . C48 C 0.2859(2) 0.2169(2) 0.1802(2) 0.0343(6) Uani 1 1 d . . . H48 H 0.2485 0.1625 0.1378 0.041 Uiso 1 1 calc R . . C49 C 0.2282(2) 0.2589(2) 0.2146(2) 0.0425(7) Uani 1 1 d . . . H49 H 0.1511 0.2330 0.1957 0.051 Uiso 1 1 calc R . . C50 C 0.2811(3) 0.3376(2) 0.2758(2) 0.0430(7) Uani 1 1 d . . . H50 H 0.2407 0.3660 0.2991 0.052 Uiso 1 1 calc R . . C51 C 0.3937(3) 0.3754(2) 0.3035(3) 0.0526(9) Uani 1 1 d . . . H51 H 0.4306 0.4296 0.3462 0.063 Uiso 1 1 calc R . . C52 C 0.4523(3) 0.3346(2) 0.2695(2) 0.0444(8) Uani 1 1 d . . . H52 H 0.5293 0.3612 0.2882 0.053 Uiso 1 1 calc R . . Cl3 Cl 0.27542(7) 0.13624(6) 0.50123(7) 0.0569(2) Uani 1 1 d . . . Cl4 Cl 0.34433(9) 0.08818(11) 0.36002(7) 0.0825(4) Uani 1 1 d . . . C53 C 0.3667(3) 0.0877(3) 0.4758(2) 0.0512(8) Uani 1 1 d . . . H53A H 0.4444 0.1215 0.5168 0.061 Uiso 1 1 calc R . . H53B H 0.3562 0.0251 0.4893 0.061 Uiso 1 1 calc R . . Cl5 Cl 0.64332(8) 0.48738(6) 0.52359(8) 0.0558(2) Uani 1 1 d . . . Cl6 Cl 0.51554(14) 0.34163(9) 0.57814(14) 0.1165(6) Uani 1 1 d . . . C54 C 0.6280(5) 0.3797(3) 0.5507(5) 0.114(2) Uani 1 1 d . . . H54A H 0.6970 0.3772 0.6044 0.136 Uiso 1 1 calc R . . H54B H 0.6183 0.3386 0.4969 0.136 Uiso 1 1 calc R . . Cl7 Cl 0.12392(7) 0.32211(5) 0.41747(6) 0.0481(2) Uani 1 1 d . . . Cl8 Cl 0.02475(12) 0.45750(7) 0.32198(7) 0.0823(4) Uani 1 1 d . . . C55 C 0.0691(3) 0.4119(2) 0.4274(2) 0.0429(7) Uani 1 1 d . . . H55A H 0.1265 0.4590 0.4785 0.051 Uiso 1 1 calc R . . H55B H 0.0055 0.3905 0.4431 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01937(16) 0.02364(17) 0.01785(16) 0.00242(12) 0.00668(13) 0.00701(13) Cl1 0.0242(3) 0.0367(3) 0.0330(3) 0.0062(3) 0.0176(2) 0.0060(2) Cl2 0.0290(3) 0.0185(3) 0.0339(3) 0.0033(2) 0.0136(2) 0.0072(2) S1 0.0298(3) 0.0346(4) 0.0267(3) 0.0006(3) 0.0089(3) -0.0046(3) S2 0.0236(3) 0.0246(3) 0.0251(3) -0.0018(2) 0.0042(2) 0.0023(2) P1 0.0189(3) 0.0229(3) 0.0174(3) 0.0046(2) 0.0058(2) 0.0062(2) P2 0.0198(3) 0.0217(3) 0.0176(3) 0.0007(2) 0.0066(2) 0.0058(2) P3 0.0278(3) 0.0245(3) 0.0207(3) 0.0019(2) 0.0106(2) 0.0035(2) P4 0.0180(3) 0.0218(3) 0.0206(3) 0.0008(2) 0.0056(2) 0.0046(2) N1 0.0203(9) 0.0293(10) 0.0174(9) 0.0029(8) 0.0054(7) 0.0103(8) N2 0.0226(10) 0.0249(10) 0.0193(10) 0.0005(8) 0.0054(8) 0.0097(8) C1 0.0224(11) 0.0298(12) 0.0221(11) 0.0024(9) 0.0078(9) 0.0107(9) C2 0.0255(12) 0.0271(12) 0.0222(12) 0.0024(9) 0.0076(9) 0.0112(10) C3 0.0226(11) 0.0247(12) 0.0202(11) 0.0053(9) 0.0087(9) 0.0055(9) C4 0.0302(13) 0.0298(13) 0.0372(15) 0.0110(11) 0.0170(11) 0.0112(11) C5 0.0399(15) 0.0256(13) 0.0435(17) 0.0076(11) 0.0228(13) 0.0024(11) C6 0.0289(13) 0.0395(16) 0.0411(16) 0.0103(12) 0.0177(12) 0.0007(12) C7 0.0294(14) 0.0439(17) 0.0472(18) 0.0155(13) 0.0212(13) 0.0121(12) C8 0.0285(13) 0.0279(13) 0.0355(14) 0.0095(11) 0.0168(11) 0.0082(10) C9 0.0203(11) 0.0270(12) 0.0206(11) 0.0074(9) 0.0089(9) 0.0082(9) C10 0.0254(12) 0.0286(13) 0.0273(13) 0.0078(10) 0.0092(10) 0.0066(10) C11 0.0382(15) 0.0275(13) 0.0416(16) 0.0111(11) 0.0213(13) 0.0078(11) C12 0.0441(16) 0.0386(15) 0.0345(15) 0.0195(12) 0.0243(13) 0.0225(13) C13 0.0326(13) 0.0462(16) 0.0247(13) 0.0153(11) 0.0118(11) 0.0227(12) C14 0.0226(12) 0.0355(14) 0.0234(12) 0.0066(10) 0.0080(10) 0.0100(10) C15 0.0232(11) 0.0300(12) 0.0186(11) 0.0057(9) 0.0073(9) 0.0102(9) C16 0.0270(12) 0.0264(12) 0.0228(12) 0.0043(9) 0.0134(10) 0.0056(10) C17 0.0260(12) 0.0352(14) 0.0242(12) 0.0063(10) 0.0121(10) 0.0071(10) C18 0.0323(13) 0.0396(15) 0.0284(13) 0.0128(11) 0.0153(11) 0.0139(11) C19 0.0355(14) 0.0306(13) 0.0364(15) 0.0098(11) 0.0217(12) 0.0082(11) C20 0.0316(14) 0.0314(14) 0.0303(14) 0.0014(11) 0.0141(11) 0.0002(11) C21 0.0316(13) 0.0306(13) 0.0223(12) 0.0038(10) 0.0091(10) 0.0029(11) C22 0.0497(17) 0.0325(14) 0.0320(14) 0.0057(11) 0.0227(13) 0.0149(12) C23 0.070(2) 0.0365(17) 0.053(2) 0.0006(15) 0.0278(18) 0.0160(16) C24 0.102(3) 0.0389(19) 0.065(3) 0.0056(17) 0.040(2) 0.032(2) C25 0.104(4) 0.054(2) 0.093(3) 0.024(2) 0.071(3) 0.045(2) C26 0.079(3) 0.054(3) 0.287(10) 0.003(4) 0.109(5) 0.024(3) C27 0.063(3) 0.038(2) 0.232(7) -0.015(3) 0.082(4) 0.0095(19) C28 0.0246(11) 0.0233(11) 0.0223(11) 0.0027(9) 0.0110(9) 0.0082(9) C29 0.0290(13) 0.0267(12) 0.0291(13) 0.0007(10) 0.0131(11) 0.0050(10) C30 0.0364(15) 0.0286(14) 0.0456(17) 0.0055(12) 0.0240(13) 0.0052(11) C31 0.0486(17) 0.0367(15) 0.0406(16) 0.0149(12) 0.0306(14) 0.0174(13) C32 0.0416(15) 0.0442(16) 0.0230(13) 0.0084(11) 0.0160(11) 0.0182(13) C33 0.0263(12) 0.0341(14) 0.0234(12) 0.0033(10) 0.0104(10) 0.0095(10) C34 0.0207(11) 0.0237(11) 0.0206(11) 0.0032(9) 0.0066(9) 0.0059(9) C35 0.0321(13) 0.0262(13) 0.0369(15) 0.0011(11) 0.0156(12) 0.0075(10) C36 0.0432(17) 0.0275(14) 0.0488(18) -0.0038(12) 0.0169(14) 0.0088(12) C37 0.0319(14) 0.0259(14) 0.0508(18) 0.0093(12) 0.0097(13) 0.0020(11) C38 0.0319(14) 0.0373(15) 0.0419(16) 0.0145(12) 0.0163(12) 0.0039(12) C39 0.0331(14) 0.0347(14) 0.0329(14) 0.0061(11) 0.0165(12) 0.0085(11) C40 0.0240(11) 0.0267(12) 0.0172(11) -0.0011(9) 0.0045(9) 0.0097(9) C41 0.0297(12) 0.0205(11) 0.0290(13) 0.0018(9) 0.0149(10) 0.0079(9) C42 0.0444(16) 0.0326(14) 0.0280(14) 0.0043(11) 0.0111(12) 0.0080(12) C43 0.078(2) 0.0365(16) 0.0353(17) 0.0135(13) 0.0252(17) 0.0186(16) C44 0.074(2) 0.0321(16) 0.062(2) 0.0170(15) 0.045(2) 0.0122(16) C45 0.0459(18) 0.0329(16) 0.084(3) 0.0195(17) 0.0356(19) 0.0077(14) C46 0.0316(14) 0.0276(14) 0.0549(19) 0.0117(12) 0.0189(13) 0.0075(11) C47 0.0232(11) 0.0287(12) 0.0249(12) 0.0040(9) 0.0096(10) 0.0091(10) C48 0.0250(13) 0.0393(15) 0.0368(15) 0.0014(12) 0.0122(11) 0.0080(11) C49 0.0271(14) 0.0550(19) 0.0490(19) 0.0054(15) 0.0186(13) 0.0134(13) C50 0.0428(17) 0.0511(19) 0.0490(19) 0.0065(15) 0.0277(15) 0.0229(14) C51 0.0475(19) 0.0476(19) 0.065(2) -0.0162(16) 0.0302(17) 0.0095(15) C52 0.0322(15) 0.0420(17) 0.057(2) -0.0101(14) 0.0216(14) 0.0054(13) Cl3 0.0495(5) 0.0585(5) 0.0628(6) -0.0095(4) 0.0290(4) 0.0077(4) Cl4 0.0595(6) 0.1545(12) 0.0400(5) 0.0117(6) 0.0227(5) 0.0382(7) C53 0.0448(18) 0.067(2) 0.0434(19) 0.0130(16) 0.0196(15) 0.0168(17) Cl5 0.0545(5) 0.0384(4) 0.0866(7) 0.0011(4) 0.0441(5) 0.0094(4) Cl6 0.1465(13) 0.0678(7) 0.2257(19) 0.0427(9) 0.1629(15) 0.0348(8) C54 0.150(5) 0.076(3) 0.225(7) 0.075(4) 0.166(6) 0.059(3) Cl7 0.0548(5) 0.0363(4) 0.0600(5) 0.0108(3) 0.0320(4) 0.0106(3) Cl8 0.1336(11) 0.0548(6) 0.0418(5) 0.0033(4) 0.0114(6) 0.0448(6) C55 0.0445(17) 0.0436(17) 0.0404(17) 0.0024(13) 0.0192(14) 0.0107(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 Fe1 N1 2.018(2) . ? Fe1 N2 2.019(2) . ? Fe1 Cl2 2.3010(7) . ? Fe1 Cl1 2.3122(7) . ? S1 P3 1.9478(9) . ? S2 P4 1.9487(8) . ? P1 N1 1.599(2) . ? P1 C3 1.803(2) . ? P1 C9 1.806(2) . ? P1 C15 1.814(3) . ? P2 N2 1.592(2) . ? P2 C34 1.803(2) . ? P2 C28 1.806(2) . ? P2 C40 1.812(3) . ? P3 C16 1.815(2) . ? P3 C22 1.818(3) . ? P3 C15 1.836(2) . ? P4 C41 1.809(3) . ? P4 C47 1.817(3) . ? P4 C40 1.831(2) . ? N1 C1 1.477(3) . ? N2 C2 1.482(3) . ? C1 C2 1.522(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.386(4) . ? C3 C4 1.404(4) . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 C7 1.384(4) . ? C6 H6 0.9500 . ? C7 C8 1.387(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.393(3) . ? C9 C14 1.394(3) . ? C10 C11 1.393(4) . ? C10 H10 0.9500 . ? C11 C12 1.383(4) . ? C11 H11 0.9500 . ? C12 C13 1.378(4) . ? C12 H12 0.9500 . ? C13 C14 1.386(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.393(4) . ? C16 C21 1.395(3) . ? C17 C18 1.395(4) . ? C17 H17 0.9500 . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 C20 1.385(4) . ? C19 H19 0.9500 . ? C20 C21 1.397(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.366(5) . ? C22 C23 1.380(4) . ? C23 C24 1.388(5) . ? C23 H23 0.9500 . ? C24 C25 1.361(6) . ? C24 H24 0.9500 . ? C25 C26 1.353(7) . ? C25 H25 0.9500 . ? C26 C27 1.382(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.394(3) . ? C28 C33 1.398(3) . ? C29 C30 1.392(4) . ? C29 H29 0.9500 . ? C30 C31 1.382(4) . ? C30 H30 0.9500 . ? C31 C32 1.385(4) . ? C31 H31 0.9500 . ? C32 C33 1.393(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.383(4) . ? C34 C39 1.397(3) . ? C35 C36 1.392(4) . ? C35 H35 0.9500 . ? C36 C37 1.381(5) . ? C36 H36 0.9500 . ? C37 C38 1.378(5) . ? C37 H37 0.9500 . ? C38 C39 1.388(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C46 1.392(4) . ? C41 C42 1.397(4) . ? C42 C43 1.387(4) . ? C42 H42 0.9500 . ? C43 C44 1.388(5) . ? C43 H43 0.9500 . ? C44 C45 1.384(5) . ? C44 H44 0.9500 . ? C45 C46 1.394(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.387(3) . ? C47 C52 1.395(4) . ? C48 C49 1.384(4) . ? C48 H48 0.9500 . ? C49 C50 1.373(5) . ? C49 H49 0.9500 . ? C50 C51 1.387(5) . ? C50 H50 0.9500 . ? C51 C52 1.379(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? Cl3 C53 1.766(4) . ? Cl4 C53 1.735(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? Cl5 C54 1.723(4) . ? Cl6 C54 1.749(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? Cl7 C55 1.756(3) . ? Cl8 C55 1.764(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 82.74(8) . . ? N1 Fe1 Cl2 114.79(6) . . ? N2 Fe1 Cl2 110.46(6) . . ? N1 Fe1 Cl1 111.26(6) . . ? N2 Fe1 Cl1 113.88(6) . . ? Cl2 Fe1 Cl1 118.42(3) . . ? N1 P1 C3 114.77(11) . . ? N1 P1 C9 111.38(11) . . ? C3 P1 C9 108.00(11) . . ? N1 P1 C15 104.56(11) . . ? C3 P1 C15 108.56(12) . . ? C9 P1 C15 109.42(11) . . ? N2 P2 C34 112.00(11) . . ? N2 P2 C28 112.69(11) . . ? C34 P2 C28 110.65(11) . . ? N2 P2 C40 104.00(11) . . ? C34 P2 C40 109.07(11) . . ? C28 P2 C40 108.10(11) . . ? C16 P3 C22 105.47(13) . . ? C16 P3 C15 105.87(11) . . ? C22 P3 C15 102.89(13) . . ? C16 P3 S1 113.92(9) . . ? C22 P3 S1 112.70(10) . . ? C15 P3 S1 114.94(8) . . ? C41 P4 C47 103.13(12) . . ? C41 P4 C40 108.60(12) . . ? C47 P4 C40 101.84(11) . . ? C41 P4 S2 114.50(9) . . ? C47 P4 S2 113.90(8) . . ? C40 P4 S2 113.63(8) . . ? C1 N1 P1 120.19(16) . . ? C1 N1 Fe1 112.91(14) . . ? P1 N1 Fe1 126.28(12) . . ? C2 N2 P2 119.94(16) . . ? C2 N2 Fe1 111.83(14) . . ? P2 N2 Fe1 127.30(12) . . ? N1 C1 C2 108.63(19) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 108.6(2) . . ? N2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C8 C3 C4 118.9(2) . . ? C8 C3 P1 120.81(19) . . ? C4 C3 P1 120.03(19) . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.2(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C8 120.3(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C3 C8 C7 120.2(3) . . ? C3 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C14 119.7(2) . . ? C10 C9 P1 116.96(18) . . ? C14 C9 P1 123.23(19) . . ? C11 C10 C9 120.1(2) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.6(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.4(2) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 119.7(2) . . ? C13 C14 H14 120.2 . . ? C9 C14 H14 120.2 . . ? P1 C15 P3 119.91(13) . . ? P1 C15 H15 120.0 . . ? P3 C15 H15 120.0 . . ? C17 C16 C21 119.6(2) . . ? C17 C16 P3 117.74(18) . . ? C21 C16 P3 122.60(19) . . ? C16 C17 C18 119.8(2) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 120.4(2) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.0(2) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 120.0(2) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C16 C21 C20 120.1(2) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C27 C22 C23 117.8(3) . . ? C27 C22 P3 122.9(3) . . ? C23 C22 P3 119.2(3) . . ? C22 C23 C24 120.4(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 119.1(4) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 120.7(5) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C22 C27 C26 121.2(4) . . ? C22 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C29 C28 C33 119.6(2) . . ? C29 C28 P2 116.02(18) . . ? C33 C28 P2 124.12(18) . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 119.9(3) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.4(2) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 120.2(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 119.7(2) . . ? C32 C33 H33 120.2 . . ? C28 C33 H33 120.2 . . ? C35 C34 C39 119.3(2) . . ? C35 C34 P2 123.31(19) . . ? C39 C34 P2 117.04(19) . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 120.3(3) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 119.8(3) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C38 C39 C34 120.4(3) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? P2 C40 P4 121.28(13) . . ? P2 C40 H40 119.4 . . ? P4 C40 H40 119.4 . . ? C46 C41 C42 119.7(2) . . ? C46 C41 P4 124.0(2) . . ? C42 C41 P4 116.3(2) . . ? C43 C42 C41 120.2(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.9(3) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.1(3) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C41 C46 C45 119.7(3) . . ? C41 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C48 C47 C52 119.5(3) . . ? C48 C47 P4 120.7(2) . . ? C52 C47 P4 119.8(2) . . ? C49 C48 C47 119.8(3) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C50 C49 C48 120.7(3) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C49 C50 C51 119.6(3) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 120.4(3) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C47 119.9(3) . . ? C51 C52 H52 120.0 . . ? C47 C52 H52 120.0 . . ? Cl4 C53 Cl3 111.8(2) . . ? Cl4 C53 H53A 109.3 . . ? Cl3 C53 H53A 109.3 . . ? Cl4 C53 H53B 109.3 . . ? Cl3 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? Cl5 C54 Cl6 113.6(3) . . ? Cl5 C54 H54A 108.8 . . ? Cl6 C54 H54A 108.8 . . ? Cl5 C54 H54B 108.8 . . ? Cl6 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? Cl7 C55 Cl8 110.68(18) . . ? Cl7 C55 H55A 109.5 . . ? Cl8 C55 H55A 109.5 . . ? Cl7 C55 H55B 109.5 . . ? Cl8 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.451 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.085 #===END data_ab855 _database_code_depnum_ccdc_archive 'CCDC 702899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Cl Fe N2 O2 P4, Cl, 2(C H2 Cl2)' _chemical_formula_sum 'C54 H52 Cl6 Fe N2 O2 P4' _chemical_formula_weight 1153.41 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.611(1) _cell_length_b 20.231(1) _cell_length_c 25.508(1) _cell_angle_alpha 108.182(1) _cell_angle_beta 102.266(1) _cell_angle_gamma 92.630(1) _cell_volume 5522.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 12779 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8575 _exptl_absorpt_correction_T_max 0.9058 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24439 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.47 _reflns_number_total 24439 _reflns_number_gt 17218 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. Two highly disordered CH2Cl2 molecule centered in (0 0 0) and (0.5 0.5 0.5) cavity were accounted for using the Platon SQUEEZE function. Two hight density (> 2e/A3) were found close to the metal center (Fe) To explain these density, we propose to model with two positions for the ligand (with occupacy 3/4 and 1/4). For the convergence of this model, we used contrains to define Fe-O and Fe-N distance. With this model, the phenyl define by C74 to C79 and C99 to C14A show large thermal ellispoid indicating possible disorder. We use the occupacy parameter to explain this disorder with unique contrain the equivalence of thermal ellipsoid between the equivalent atom of phenyl group. ; _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^)+(0.0908P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24439 _refine_ls_number_parameters 1142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1510 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.77614(3) 0.182814(18) 0.517874(16) 0.02621(10) Uani 1 1 d . . . Cl1 Cl 0.75169(6) 0.29385(3) 0.57496(3) 0.03662(16) Uani 1 1 d . . . P1 P 1.02857(6) 0.18417(3) 0.60505(3) 0.02627(15) Uani 1 1 d . . . P2 P 0.79671(6) 0.12295(3) 0.62078(3) 0.02625(15) Uani 1 1 d . . . P3 P 0.76897(6) 0.22426(3) 0.40390(3) 0.02752(15) Uani 1 1 d . . . P4 P 0.53580(6) 0.18614(4) 0.43253(3) 0.02924(16) Uani 1 1 d . . . O1 O 0.74100(15) 0.10977(9) 0.55900(8) 0.0299(4) Uani 1 1 d . . . O2 O 0.59734(16) 0.14827(10) 0.47076(9) 0.0340(4) Uani 1 1 d . . . N1 N 0.95938(18) 0.17987(11) 0.54318(10) 0.0279(5) Uani 1 1 d . . . N2 N 0.82597(19) 0.18023(11) 0.44285(10) 0.0290(5) Uani 1 1 d . . . C1 C 1.0246(2) 0.19649(14) 0.50410(12) 0.0299(6) Uani 1 1 d . . . H1A H 1.1014 0.1769 0.5074 0.036 Uiso 1 1 calc R . . H1B H 1.0410 0.2479 0.5140 0.036 Uiso 1 1 calc R . . C2 C 0.9499(2) 0.16519(14) 0.44404(12) 0.0322(6) Uani 1 1 d . . . H2A H 0.9818 0.1855 0.4187 0.039 Uiso 1 1 calc R . . H2B H 0.9523 0.1139 0.4304 0.039 Uiso 1 1 calc R . . C3 C 1.1285(2) 0.26456(14) 0.64199(12) 0.0308(6) Uani 1 1 d . . . C4 C 1.0936(3) 0.32444(15) 0.63063(14) 0.0393(7) Uani 1 1 d . . . H4 H 1.0206 0.3220 0.6044 0.047 Uiso 1 1 calc R . . C5 C 1.1659(3) 0.38793(15) 0.65779(15) 0.0454(8) Uani 1 1 d . . . H5 H 1.1423 0.4291 0.6503 0.054 Uiso 1 1 calc R . . C6 C 1.2736(3) 0.39096(17) 0.69618(17) 0.0527(9) Uani 1 1 d . . . H6 H 1.3247 0.4339 0.7135 0.063 Uiso 1 1 calc R . . C7 C 1.3056(3) 0.33276(17) 0.70884(16) 0.0481(8) Uani 1 1 d . . . H7 H 1.3765 0.3360 0.7366 0.058 Uiso 1 1 calc R . . C8 C 1.2350(2) 0.26866(16) 0.68137(14) 0.0387(7) Uani 1 1 d . . . H8 H 1.2591 0.2278 0.6893 0.046 Uiso 1 1 calc R . . C9 C 1.1122(2) 0.11131(13) 0.60663(12) 0.0285(6) Uani 1 1 d . . . C10 C 1.1685(2) 0.10062(14) 0.65759(13) 0.0331(6) Uani 1 1 d . . . H10 H 1.1616 0.1314 0.6932 0.040 Uiso 1 1 calc R . . C11 C 1.2333(2) 0.04530(14) 0.65509(13) 0.0362(7) Uani 1 1 d . . . H11 H 1.2716 0.0381 0.6893 0.043 Uiso 1 1 calc R . . C12 C 1.2438(3) -0.00030(14) 0.60355(14) 0.0386(7) Uani 1 1 d . . . H12 H 1.2900 -0.0380 0.6026 0.046 Uiso 1 1 calc R . . C13 C 1.1871(3) 0.00912(15) 0.55340(14) 0.0406(7) Uani 1 1 d . . . H13 H 1.1935 -0.0224 0.5179 0.049 Uiso 1 1 calc R . . C14 C 1.1215(3) 0.06430(14) 0.55511(13) 0.0341(6) Uani 1 1 d . . . H14 H 1.0820 0.0704 0.5206 0.041 Uiso 1 1 calc R . . C15 C 0.9240(2) 0.18925(13) 0.64857(11) 0.0274(6) Uani 1 1 d . . . H15A H 0.8949 0.2357 0.6556 0.033 Uiso 1 1 calc R . . H15B H 0.9668 0.1869 0.6858 0.033 Uiso 1 1 calc R . . C16 C 0.8377(2) 0.04377(14) 0.63377(13) 0.0308(6) Uani 1 1 d . . . C17 C 0.9095(3) 0.04459(16) 0.68542(14) 0.0393(7) Uani 1 1 d . . . H17 H 0.9446 0.0878 0.7138 0.047 Uiso 1 1 calc R . . C18 C 0.9292(3) -0.01808(18) 0.69498(16) 0.0503(8) Uani 1 1 d . . . H18 H 0.9768 -0.0176 0.7304 0.060 Uiso 1 1 calc R . . C19 C 0.8808(3) -0.08089(17) 0.65401(16) 0.0499(9) Uani 1 1 d . . . H19 H 0.8951 -0.1234 0.6613 0.060 Uiso 1 1 calc R . . C20 C 0.8111(3) -0.08274(16) 0.60202(15) 0.0439(8) Uani 1 1 d . . . H20 H 0.7788 -0.1264 0.5735 0.053 Uiso 1 1 calc R . . C21 C 0.7889(2) -0.02015(14) 0.59195(13) 0.0351(6) Uani 1 1 d . . . H21 H 0.7405 -0.0210 0.5566 0.042 Uiso 1 1 calc R . . C22 C 0.6936(2) 0.15481(13) 0.66385(13) 0.0319(6) Uani 1 1 d . . . C23 C 0.7278(3) 0.18233(15) 0.72270(14) 0.0394(7) Uani 1 1 d . . . H23 H 0.8092 0.1878 0.7417 0.047 Uiso 1 1 calc R . . C24 C 0.6433(3) 0.20167(16) 0.75346(16) 0.0493(8) Uani 1 1 d . . . H24 H 0.6662 0.2194 0.7938 0.059 Uiso 1 1 calc R . . C25 C 0.5252(3) 0.19524(18) 0.72568(19) 0.0564(10) Uani 1 1 d . . . H25 H 0.4675 0.2097 0.7469 0.068 Uiso 1 1 calc R . . C26 C 0.4907(3) 0.16770(19) 0.66675(18) 0.0535(9) Uani 1 1 d . . . H26 H 0.4093 0.1626 0.6478 0.064 Uiso 1 1 calc R . . C27 C 0.5741(3) 0.14789(17) 0.63607(16) 0.0446(8) Uani 1 1 d . . . H27 H 0.5506 0.1294 0.5958 0.054 Uiso 1 1 calc R . . C28 C 0.8669(2) 0.30309(14) 0.41620(13) 0.0324(6) Uani 1 1 d . . . C29 C 0.9054(2) 0.34749(14) 0.47251(14) 0.0360(7) Uani 1 1 d . . . H29 H 0.8733 0.3388 0.5013 0.043 Uiso 1 1 calc R . . C30 C 0.9908(3) 0.40425(15) 0.48604(15) 0.0424(7) Uani 1 1 d . . . H30 H 1.0178 0.4342 0.5243 0.051 Uiso 1 1 calc R . . C31 C 1.0368(3) 0.41736(16) 0.44369(16) 0.0441(8) Uani 1 1 d . . . H31 H 1.0950 0.4564 0.4531 0.053 Uiso 1 1 calc R . . C32 C 0.9979(3) 0.37366(17) 0.38792(16) 0.0460(8) Uani 1 1 d . . . H32 H 1.0291 0.3830 0.3591 0.055 Uiso 1 1 calc R . . C33 C 0.9128(3) 0.31588(16) 0.37388(14) 0.0404(7) Uani 1 1 d . . . H33 H 0.8865 0.2856 0.3357 0.048 Uiso 1 1 calc R . . C34 C 0.7346(2) 0.17968(14) 0.32845(12) 0.0329(6) Uani 1 1 d . . . C35 C 0.7744(3) 0.11411(15) 0.30827(14) 0.0395(7) Uani 1 1 d . . . H35 H 0.8180 0.0941 0.3343 0.047 Uiso 1 1 calc R . . C36 C 0.7498(3) 0.07830(17) 0.24995(15) 0.0528(9) Uani 1 1 d . . . H36 H 0.7758 0.0336 0.2362 0.063 Uiso 1 1 calc R . . C37 C 0.6883(3) 0.1076(2) 0.21266(15) 0.0568(9) Uani 1 1 d . . . H37 H 0.6727 0.0832 0.1730 0.068 Uiso 1 1 calc R . . C38 C 0.6485(3) 0.17199(19) 0.23160(15) 0.0512(8) Uani 1 1 d . . . H38 H 0.6053 0.1914 0.2051 0.061 Uiso 1 1 calc R . . C39 C 0.6720(3) 0.20839(16) 0.28964(14) 0.0404(7) Uani 1 1 d . . . H39 H 0.6452 0.2529 0.3028 0.049 Uiso 1 1 calc R . . C40 C 0.6340(2) 0.25158(13) 0.42344(12) 0.0297(6) Uani 1 1 d . . . H40A H 0.5891 0.2691 0.3939 0.036 Uiso 1 1 calc R . . H40B H 0.6558 0.2915 0.4595 0.036 Uiso 1 1 calc R . . C41 C 0.4675(2) 0.12508(14) 0.36331(13) 0.0320(6) Uani 1 1 d . . . C42 C 0.4612(3) 0.05408(15) 0.35606(14) 0.0392(7) Uani 1 1 d . . . H42 H 0.4892 0.0389 0.3877 0.047 Uiso 1 1 calc R . . C43 C 0.4143(3) 0.00529(17) 0.30288(16) 0.0509(9) Uani 1 1 d . . . H43 H 0.4102 -0.0433 0.2980 0.061 Uiso 1 1 calc R . . C44 C 0.3733(3) 0.02726(19) 0.25688(16) 0.0586(10) Uani 1 1 d . . . H44 H 0.3410 -0.0063 0.2204 0.070 Uiso 1 1 calc R . . C45 C 0.3793(3) 0.0977(2) 0.26373(16) 0.0585(10) Uani 1 1 d . . . H45 H 0.3523 0.1123 0.2318 0.070 Uiso 1 1 calc R . . C46 C 0.4244(3) 0.14744(16) 0.31696(14) 0.0435(8) Uani 1 1 d . . . H46 H 0.4259 0.1960 0.3218 0.052 Uiso 1 1 calc R . . C47 C 0.4279(2) 0.23588(14) 0.46369(13) 0.0355(6) Uani 1 1 d . . . C48 C 0.4226(3) 0.23968(18) 0.51830(14) 0.0448(8) Uani 1 1 d . . . H48 H 0.4718 0.2141 0.5376 0.054 Uiso 1 1 calc R . . C49 C 0.3443(3) 0.2814(2) 0.54510(17) 0.0573(9) Uani 1 1 d . . . H49 H 0.3402 0.2838 0.5824 0.069 Uiso 1 1 calc R . . C50 C 0.2736(3) 0.31864(18) 0.51694(18) 0.0560(9) Uani 1 1 d . . . H50 H 0.2209 0.3471 0.5349 0.067 Uiso 1 1 calc R . . C51 C 0.2795(4) 0.3146(2) 0.4634(2) 0.0715(13) Uani 1 1 d . . . H51 H 0.2303 0.3403 0.4442 0.086 Uiso 1 1 calc R . . C52 C 0.3568(3) 0.2733(2) 0.43590(18) 0.0593(10) Uani 1 1 d . . . H52 H 0.3602 0.2712 0.3985 0.071 Uiso 1 1 calc R . . Fe2 Fe 0.24552(3) 0.35032(2) 0.070362(17) 0.03058(10) Uani 1 1 d . . . Cl2 Cl 0.29455(9) 0.23702(4) 0.04956(4) 0.0594(2) Uani 1 1 d . A . P5 P 0.44123(6) 0.40775(4) 0.19180(3) 0.02942(16) Uani 1 1 d . . . P6 P 0.18964(6) 0.34890(4) 0.18796(3) 0.03227(17) Uani 1 1 d . . . P7 P 0.29485(6) 0.36991(4) -0.04503(3) 0.03213(16) Uani 1 1 d . . . P8 P 0.04923(6) 0.30529(4) -0.04711(3) 0.03567(18) Uani 1 1 d . . . C53A C 0.4794(3) 0.4376(2) 0.10254(18) 0.0437(10) Uani 0.777(2) 1 d P A 1 H53A H 0.5330 0.4031 0.0886 0.052 Uiso 0.777(2) 1 calc PR A 1 H53B H 0.5288 0.4798 0.1313 0.052 Uiso 0.777(2) 1 calc PR A 1 C54A C 0.4112(4) 0.4565(2) 0.05512(17) 0.0417(9) Uani 0.777(2) 1 d P A 1 H54A H 0.4639 0.4615 0.0304 0.050 Uiso 0.777(2) 1 calc PR A 1 H54B H 0.3828 0.5025 0.0703 0.050 Uiso 0.777(2) 1 calc PR A 1 O3A O 0.1443(7) 0.3634(4) 0.1313(2) 0.0388(11) Uani 0.777(2) 1 d P A 1 O4A O 0.0768(4) 0.3371(4) 0.0162(3) 0.0461(12) Uani 0.777(2) 1 d P A 1 N3A N 0.4009(4) 0.4084(3) 0.1279(2) 0.0254(9) Uani 0.777(2) 1 d P A 1 N4A N 0.3068(8) 0.4033(5) 0.0202(5) 0.0302(16) Uani 0.777(2) 1 d P A 1 C53B C -0.0081(12) 0.3042(9) 0.0423(6) 0.049(4) Uani 0.223(2) 1 d P A 2 H53C H 0.0152 0.2568 0.0384 0.059 Uiso 0.223(2) 1 calc PR A 2 H53D H -0.0942 0.3006 0.0255 0.059 Uiso 0.223(2) 1 calc PR A 2 C54B C 0.0259(14) 0.3524(9) 0.1041(7) 0.054(4) Uani 0.223(2) 1 d P A 2 H54C H 0.0054 0.3994 0.1042 0.065 Uiso 0.223(2) 1 calc PR A 2 H54D H -0.0268 0.3355 0.1242 0.065 Uiso 0.223(2) 1 calc PR A 2 O3 O 0.322(3) 0.4013(19) 0.0230(17) 0.0388(11) Uani 0.223(2) 1 d P A 2 O4 O 0.3810(17) 0.4152(12) 0.1362(9) 0.0461(12) Uani 0.223(2) 1 d P A 2 N3 N 0.056(2) 0.3384(12) 0.0200(12) 0.0254(9) Uani 0.223(2) 1 d P A 2 N4 N 0.151(3) 0.3626(13) 0.1401(12) 0.0302(16) Uani 0.223(2) 1 d P A 2 C55 C 0.5891(2) 0.38034(15) 0.20381(13) 0.0347(6) Uani 1 1 d . A . C56 C 0.6757(3) 0.41033(17) 0.25387(15) 0.0434(8) Uani 1 1 d . . . H56 H 0.6590 0.4465 0.2844 0.052 Uiso 1 1 calc R A . C57 C 0.7867(3) 0.3872(2) 0.25908(18) 0.0544(9) Uani 1 1 d . A . H57 H 0.8465 0.4080 0.2931 0.065 Uiso 1 1 calc R . . C58 C 0.8102(3) 0.3352(2) 0.2157(2) 0.0611(11) Uani 1 1 d . . . H58 H 0.8872 0.3205 0.2193 0.073 Uiso 1 1 calc R A . C59 C 0.7254(4) 0.3039(2) 0.1675(2) 0.0657(11) Uani 1 1 d . A . H59 H 0.7418 0.2657 0.1383 0.079 Uiso 1 1 calc R . . C60 C 0.6128(3) 0.32763(18) 0.16034(17) 0.0524(9) Uani 1 1 d . . . H60 H 0.5542 0.3073 0.1258 0.063 Uiso 1 1 calc R A . C61 C 0.4389(2) 0.49049(14) 0.24567(13) 0.0348(6) Uani 1 1 d . A . C62 C 0.4577(3) 0.49851(16) 0.30302(14) 0.0431(7) Uani 1 1 d . . . H62 H 0.4783 0.4606 0.3162 0.052 Uiso 1 1 calc R A . C63 C 0.4461(3) 0.56251(17) 0.34064(17) 0.0535(9) Uani 1 1 d . A . H63 H 0.4587 0.5687 0.3800 0.064 Uiso 1 1 calc R . . C64 C 0.4163(3) 0.61735(17) 0.32132(19) 0.0552(10) Uani 1 1 d . . . H64 H 0.4072 0.6609 0.3474 0.066 Uiso 1 1 calc R A . C65 C 0.3998(3) 0.60995(17) 0.26551(18) 0.0527(9) Uani 1 1 d . A . H65 H 0.3806 0.6484 0.2528 0.063 Uiso 1 1 calc R . . C66 C 0.4108(2) 0.54695(15) 0.22745(15) 0.0427(8) Uani 1 1 d . . . H66 H 0.3992 0.5419 0.1883 0.051 Uiso 1 1 calc R A . C67 C 0.3473(2) 0.34108(14) 0.20180(12) 0.0309(6) Uani 1 1 d . A . H67A H 0.3743 0.3417 0.2415 0.037 Uiso 1 1 calc R . . H67B H 0.3590 0.2948 0.1767 0.037 Uiso 1 1 calc R . . C68 C 0.1613(2) 0.41709(15) 0.24693(12) 0.0345(6) Uani 1 1 d . A . C69 C 0.2086(3) 0.41935(19) 0.30298(14) 0.0453(8) Uani 1 1 d . . . H69 H 0.2529 0.3835 0.3104 0.054 Uiso 1 1 calc R A . C70 C 0.1898(3) 0.4747(2) 0.34734(15) 0.0566(10) Uani 1 1 d . A . H70 H 0.2220 0.4769 0.3854 0.068 Uiso 1 1 calc R . . C71 C 0.1242(3) 0.52705(19) 0.33689(17) 0.0581(10) Uani 1 1 d . . . H71 H 0.1117 0.5646 0.3677 0.070 Uiso 1 1 calc R A . C72 C 0.0776(4) 0.5244(2) 0.28203(18) 0.0615(10) Uani 1 1 d . A . H72 H 0.0329 0.5602 0.2749 0.074 Uiso 1 1 calc R . . C73 C 0.0961(3) 0.46914(17) 0.23671(15) 0.0470(8) Uani 1 1 d . . . H73 H 0.0636 0.4673 0.1987 0.056 Uiso 1 1 calc R A . C74A C 0.1159(2) 0.26858(14) 0.18567(13) 0.0344(9) Uani 0.777(2) 1 d PG A 1 C75A C 0.1495(4) 0.2394(2) 0.22845(15) 0.110(3) Uani 0.777(2) 1 d PG A 1 H75A H 0.2137 0.2624 0.2601 0.132 Uiso 0.777(2) 1 calc PR A 1 C76A C 0.0891(5) 0.1766(2) 0.2249(2) 0.127(3) Uani 0.777(2) 1 d PG A 1 H76A H 0.1121 0.1567 0.2541 0.152 Uiso 0.777(2) 1 calc PR A 1 C77A C -0.0047(4) 0.14298(18) 0.1785(2) 0.090(2) Uani 0.777(2) 1 d PG A 1 H77A H -0.0460 0.1001 0.1761 0.108 Uiso 0.777(2) 1 calc PR A 1 C78A C -0.0383(3) 0.17212(17) 0.13574(18) 0.0828(18) Uani 0.777(2) 1 d PG A 1 H78A H -0.1025 0.1491 0.1041 0.099 Uiso 0.777(2) 1 calc PR A 1 C79A C 0.0220(3) 0.23492(16) 0.13931(13) 0.0641(13) Uani 0.777(2) 1 d PG A 1 H79A H -0.0009 0.2548 0.1101 0.077 Uiso 0.777(2) 1 calc PR A 1 C74B C 0.1462(8) 0.2579(5) 0.1862(3) 0.0344(9) Uani 0.223(2) 1 d PG A 2 C75B C 0.1134(10) 0.2508(6) 0.2336(4) 0.110(3) Uani 0.223(2) 1 d PG A 2 H75B H 0.1290 0.2894 0.2679 0.132 Uiso 0.223(2) 1 calc PR A 2 C76B C 0.0579(9) 0.1870(7) 0.2309(4) 0.127(3) Uani 0.223(2) 1 d PG A 2 H76B H 0.0355 0.1821 0.2634 0.152 Uiso 0.223(2) 1 calc PR A 2 C77B C 0.0351(9) 0.1305(6) 0.1807(4) 0.090(2) Uani 0.223(2) 1 d PG A 2 H77B H -0.0029 0.0869 0.1789 0.108 Uiso 0.223(2) 1 calc PR A 2 C78B C 0.0678(8) 0.1376(5) 0.1333(4) 0.0828(18) Uani 0.223(2) 1 d PG A 2 H78B H 0.0523 0.0990 0.0990 0.099 Uiso 0.223(2) 1 calc PR A 2 C79B C 0.1234(7) 0.2014(5) 0.1360(3) 0.0641(13) Uani 0.223(2) 1 d PG A 2 H79B H 0.1458 0.2063 0.1035 0.077 Uiso 0.223(2) 1 calc PR A 2 C80 C 0.4302(2) 0.33826(16) -0.06366(12) 0.0430(7) Uani 1 1 d G A . C81 C 0.4849(3) 0.2933(2) -0.03515(16) 0.0725(12) Uani 1 1 d G . . H81 H 0.4495 0.2797 -0.0092 0.087 Uiso 1 1 calc R A . C82 C 0.5886(4) 0.2703(3) -0.0457(2) 0.0885(15) Uani 1 1 d . A . H82 H 0.6240 0.2389 -0.0279 0.106 Uiso 1 1 calc R . . C83 C 0.6442(3) 0.2917(2) -0.08212(19) 0.0655(11) Uani 1 1 d . . . H83 H 0.7182 0.2765 -0.0878 0.079 Uiso 1 1 calc R A . C84 C 0.5936(4) 0.3330(2) -0.1085(2) 0.0649(11) Uani 1 1 d . A . H84 H 0.6314 0.3472 -0.1334 0.078 Uiso 1 1 calc R . . C85 C 0.4846(3) 0.35663(18) -0.10064(17) 0.0535(9) Uani 1 1 d . . . H85 H 0.4486 0.3854 -0.1210 0.064 Uiso 1 1 calc R A . C86 C 0.2516(3) 0.42886(17) -0.08413(14) 0.0421(7) Uani 1 1 d . A . C87 C 0.2551(3) 0.49988(18) -0.05403(17) 0.0521(9) Uani 1 1 d . . . H87 H 0.2779 0.5161 -0.0137 0.063 Uiso 1 1 calc R A . C88 C 0.2255(3) 0.5463(2) -0.0828(2) 0.0669(12) Uani 1 1 d . A . H88 H 0.2279 0.5947 -0.0624 0.080 Uiso 1 1 calc R . . C89 C 0.1921(4) 0.5222(3) -0.1416(2) 0.0792(15) Uani 1 1 d . . . H89 H 0.1715 0.5543 -0.1614 0.095 Uiso 1 1 calc R A . C90 C 0.1882(4) 0.4527(3) -0.1717(2) 0.0737(13) Uani 1 1 d . A . H90 H 0.1653 0.4372 -0.2120 0.088 Uiso 1 1 calc R . . C91 C 0.2173(3) 0.4047(2) -0.14382(16) 0.0594(10) Uani 1 1 d . . . H91 H 0.2140 0.3564 -0.1646 0.071 Uiso 1 1 calc R A . C92 C 0.1846(2) 0.29377(14) -0.07147(12) 0.0327(6) Uani 1 1 d . A . H92A H 0.2210 0.2553 -0.0605 0.039 Uiso 1 1 calc R . . H92B H 0.1636 0.2787 -0.1135 0.039 Uiso 1 1 calc R . . C93 C -0.0337(2) 0.35912(15) -0.08215(13) 0.0335(6) Uani 1 1 d . A . C94 C -0.0695(2) 0.41868(16) -0.04797(14) 0.0411(7) Uani 1 1 d . . . H94 H -0.0541 0.4282 -0.0081 0.049 Uiso 1 1 calc R A . C95 C -0.1283(3) 0.46482(17) -0.07252(16) 0.0476(8) Uani 1 1 d . A . H95 H -0.1532 0.5056 -0.0493 0.057 Uiso 1 1 calc R . . C96 C -0.1498(3) 0.45067(17) -0.13038(16) 0.0471(8) Uani 1 1 d . . . H96 H -0.1884 0.4822 -0.1471 0.057 Uiso 1 1 calc R A . C97 C -0.1154(3) 0.39077(19) -0.16425(16) 0.0513(8) Uani 1 1 d . A . H97 H -0.1321 0.3809 -0.2042 0.062 Uiso 1 1 calc R . . C98 C -0.0567(3) 0.34492(17) -0.14033(14) 0.0434(7) Uani 1 1 d . . . H98 H -0.0324 0.3041 -0.1638 0.052 Uiso 1 1 calc R A . C99A C -0.0372(2) 0.22262(13) -0.06857(13) 0.0430(10) Uani 0.777(2) 1 d PG A 1 C10A C -0.0869(3) 0.20553(16) -0.02879(11) 0.0606(12) Uani 0.777(2) 1 d PG A 1 H10A H -0.0723 0.2372 0.0090 0.073 Uiso 0.777(2) 1 calc PR A 1 C11A C -0.1580(3) 0.14211(19) -0.04426(15) 0.0821(18) Uani 0.777(2) 1 d PG A 1 H11A H -0.1920 0.1304 -0.0171 0.099 Uiso 0.777(2) 1 calc PR A 1 C12A C -0.1794(4) 0.09578(15) -0.09951(17) 0.093(2) Uani 0.777(2) 1 d PG A 1 H12A H -0.2281 0.0524 -0.1101 0.112 Uiso 0.777(2) 1 calc PR A 1 C13A C -0.1297(4) 0.11287(16) -0.13929(13) 0.093(2) Uani 0.777(2) 1 d PG A 1 H13A H -0.1444 0.0812 -0.1771 0.111 Uiso 0.777(2) 1 calc PR A 1 C14A C -0.0586(3) 0.17629(17) -0.12382(12) 0.0683(16) Uani 0.777(2) 1 d PG A 1 H14A H -0.0246 0.1880 -0.1510 0.082 Uiso 0.777(2) 1 calc PR A 1 C99B C -0.0201(5) 0.2091(3) -0.08048(12) 0.0430(10) Uani 0.223(2) 1 d PG A 2 C10B C 0.0282(5) 0.1588(2) -0.05857(9) 0.0606(12) Uani 0.223(2) 1 d PG A 2 H10B H 0.0887 0.1728 -0.0244 0.073 Uiso 0.223(2) 1 calc PR A 2 C11B C -0.0122(6) 0.0882(3) -0.08673(8) 0.0821(18) Uani 0.223(2) 1 d PG A 2 H11B H 0.0208 0.0539 -0.0718 0.099 Uiso 0.223(2) 1 calc PR A 2 C12B C -0.1007(7) 0.0678(3) -0.13678(10) 0.093(2) Uani 0.223(2) 1 d PG A 2 H12B H -0.1283 0.0195 -0.1560 0.112 Uiso 0.223(2) 1 calc PR A 2 C13B C -0.1489(7) 0.1180(3) -0.15869(13) 0.093(2) Uani 0.223(2) 1 d PG A 2 H13B H -0.2094 0.1041 -0.1929 0.111 Uiso 0.223(2) 1 calc PR A 2 C14B C -0.1086(6) 0.1887(3) -0.13054(14) 0.0683(16) Uani 0.223(2) 1 d PG A 2 H14B H -0.1416 0.2230 -0.1455 0.082 Uiso 0.223(2) 1 calc PR A 2 Cl3 Cl 0.46220(6) 0.33303(3) 0.33438(3) 0.04278(19) Uani 1 1 d G . . Cl4 Cl 0.89616(6) 0.78713(3) 0.21761(3) 0.04258(18) Uani 1 1 d G . . 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 0.02122(18) 0.02833(19) 0.0300(2) 0.01011(16) 0.00725(15) 0.00360(14) Cl1 0.0349(4) 0.0332(3) 0.0393(4) 0.0068(3) 0.0105(3) 0.0089(3) P1 0.0207(3) 0.0268(3) 0.0303(4) 0.0079(3) 0.0061(3) 0.0028(3) P2 0.0225(3) 0.0283(3) 0.0287(4) 0.0098(3) 0.0071(3) 0.0028(3) P3 0.0254(3) 0.0279(3) 0.0300(4) 0.0108(3) 0.0065(3) 0.0019(3) P4 0.0221(3) 0.0315(3) 0.0346(4) 0.0130(3) 0.0047(3) 0.0026(3) O1 0.0271(9) 0.0330(9) 0.0275(10) 0.0091(8) 0.0047(8) -0.0011(7) O2 0.0254(9) 0.0359(10) 0.0404(12) 0.0165(9) 0.0026(8) -0.0008(8) N1 0.0205(10) 0.0336(11) 0.0315(13) 0.0132(10) 0.0060(9) 0.0040(9) N2 0.0296(11) 0.0300(11) 0.0290(13) 0.0110(10) 0.0080(9) 0.0068(9) C1 0.0222(12) 0.0357(14) 0.0372(16) 0.0169(12) 0.0105(11) 0.0058(11) C2 0.0275(13) 0.0335(14) 0.0368(17) 0.0115(12) 0.0097(12) 0.0077(11) C3 0.0245(13) 0.0319(13) 0.0342(16) 0.0063(12) 0.0113(11) -0.0019(11) C4 0.0365(16) 0.0349(15) 0.0433(19) 0.0098(13) 0.0083(13) 0.0017(12) C5 0.0467(18) 0.0320(15) 0.062(2) 0.0174(15) 0.0188(16) 0.0051(13) C6 0.0417(18) 0.0404(17) 0.066(2) 0.0080(16) 0.0099(17) -0.0120(14) C7 0.0264(15) 0.0534(19) 0.056(2) 0.0124(16) 0.0024(14) -0.0063(14) C8 0.0247(14) 0.0430(16) 0.0452(19) 0.0118(14) 0.0069(13) -0.0007(12) C9 0.0235(13) 0.0289(13) 0.0360(16) 0.0122(12) 0.0099(11) 0.0061(10) C10 0.0299(14) 0.0342(14) 0.0321(16) 0.0072(12) 0.0064(12) 0.0049(11) C11 0.0318(15) 0.0354(14) 0.0374(17) 0.0110(13) 0.0019(12) 0.0030(12) C12 0.0322(15) 0.0288(14) 0.056(2) 0.0142(14) 0.0118(14) 0.0073(12) C13 0.0488(18) 0.0310(14) 0.0439(19) 0.0080(13) 0.0210(14) 0.0086(13) C14 0.0371(15) 0.0307(14) 0.0321(16) 0.0070(12) 0.0085(12) 0.0018(12) C15 0.0253(13) 0.0266(12) 0.0281(15) 0.0063(11) 0.0057(11) 0.0042(10) C16 0.0259(13) 0.0325(13) 0.0390(17) 0.0143(12) 0.0136(12) 0.0073(11) C17 0.0360(16) 0.0449(16) 0.0389(18) 0.0166(14) 0.0083(13) 0.0088(13) C18 0.0511(19) 0.057(2) 0.053(2) 0.0289(18) 0.0144(16) 0.0188(16) C19 0.060(2) 0.0450(18) 0.066(3) 0.0317(18) 0.0363(18) 0.0234(16) C20 0.0461(18) 0.0328(15) 0.059(2) 0.0141(15) 0.0280(16) 0.0048(13) C21 0.0296(14) 0.0368(15) 0.0428(18) 0.0142(13) 0.0147(13) 0.0057(12) C22 0.0324(14) 0.0263(13) 0.0421(18) 0.0133(12) 0.0164(12) 0.0043(11) C23 0.0398(16) 0.0400(15) 0.0381(18) 0.0089(13) 0.0152(13) 0.0048(13) C24 0.065(2) 0.0442(17) 0.043(2) 0.0082(15) 0.0307(17) 0.0144(16) C25 0.056(2) 0.051(2) 0.083(3) 0.029(2) 0.046(2) 0.0226(17) C26 0.0354(17) 0.062(2) 0.071(3) 0.024(2) 0.0232(17) 0.0158(15) C27 0.0326(16) 0.0503(18) 0.056(2) 0.0205(16) 0.0152(14) 0.0126(14) C28 0.0228(13) 0.0348(14) 0.0437(18) 0.0181(13) 0.0082(12) 0.0057(11) C29 0.0308(14) 0.0352(14) 0.0422(18) 0.0136(13) 0.0078(13) 0.0028(12) C30 0.0358(16) 0.0330(15) 0.052(2) 0.0089(14) 0.0052(14) 0.0030(12) C31 0.0342(16) 0.0334(15) 0.068(2) 0.0208(16) 0.0126(15) 0.0023(12) C32 0.0359(16) 0.0502(18) 0.061(2) 0.0316(18) 0.0120(15) 0.0003(14) C33 0.0368(16) 0.0405(16) 0.0464(19) 0.0184(14) 0.0103(14) -0.0019(13) C34 0.0331(15) 0.0371(15) 0.0290(16) 0.0107(12) 0.0095(12) -0.0014(12) C35 0.0430(17) 0.0354(15) 0.0381(18) 0.0102(13) 0.0094(14) 0.0002(13) C36 0.072(2) 0.0394(17) 0.045(2) 0.0055(15) 0.0222(18) 0.0060(16) C37 0.071(2) 0.067(2) 0.0267(18) 0.0091(16) 0.0116(16) -0.0041(19) C38 0.054(2) 0.064(2) 0.037(2) 0.0227(17) 0.0060(15) 0.0023(17) C39 0.0395(16) 0.0421(16) 0.0406(19) 0.0165(14) 0.0070(14) 0.0052(13) C40 0.0263(13) 0.0288(13) 0.0329(16) 0.0114(11) 0.0028(11) 0.0041(11) C41 0.0210(13) 0.0358(14) 0.0368(17) 0.0092(12) 0.0063(11) 0.0015(11) C42 0.0367(16) 0.0398(16) 0.0430(19) 0.0137(14) 0.0135(13) 0.0047(13) C43 0.0494(19) 0.0350(16) 0.062(2) 0.0054(16) 0.0175(17) -0.0049(14) C44 0.060(2) 0.052(2) 0.045(2) -0.0020(16) 0.0048(17) -0.0171(17) C45 0.056(2) 0.070(2) 0.040(2) 0.0178(18) -0.0022(17) -0.0124(18) C46 0.0400(17) 0.0410(16) 0.046(2) 0.0164(15) 0.0015(14) -0.0039(13) C47 0.0265(14) 0.0354(14) 0.0425(18) 0.0096(13) 0.0093(12) -0.0004(11) C48 0.0286(15) 0.066(2) 0.0389(19) 0.0160(16) 0.0073(13) 0.0078(14) C49 0.0417(19) 0.076(2) 0.048(2) 0.0089(19) 0.0180(16) 0.0002(18) C50 0.0402(18) 0.0503(19) 0.079(3) 0.0136(19) 0.0288(18) 0.0070(15) C51 0.068(3) 0.084(3) 0.098(4) 0.055(3) 0.048(2) 0.050(2) C52 0.060(2) 0.076(2) 0.068(3) 0.046(2) 0.0329(19) 0.0349(19) Fe2 0.0262(2) 0.0341(2) 0.0296(2) 0.00992(17) 0.00453(16) -0.00041(16) Cl2 0.0874(7) 0.0348(4) 0.0476(5) 0.0093(4) 0.0037(5) 0.0121(4) P5 0.0235(3) 0.0318(3) 0.0321(4) 0.0116(3) 0.0040(3) 0.0005(3) P6 0.0255(3) 0.0401(4) 0.0306(4) 0.0113(3) 0.0069(3) -0.0005(3) P7 0.0279(4) 0.0395(4) 0.0279(4) 0.0093(3) 0.0078(3) 0.0012(3) P8 0.0248(3) 0.0467(4) 0.0352(4) 0.0159(4) 0.0036(3) 0.0006(3) C53A 0.033(2) 0.056(2) 0.041(2) 0.019(2) 0.0034(17) -0.0092(17) C54A 0.041(2) 0.046(2) 0.031(2) 0.0066(17) 0.0066(17) -0.0095(18) O3A 0.0279(17) 0.0670(19) 0.026(2) 0.0232(18) 0.0039(17) 0.0098(14) O4A 0.021(2) 0.084(2) 0.0331(19) 0.0160(16) 0.0125(17) -0.0023(18) N3A 0.021(2) 0.0327(17) 0.025(2) 0.0122(16) 0.0085(14) 0.0004(14) N4A 0.028(4) 0.0262(16) 0.031(3) 0.0016(16) 0.008(3) -0.006(2) C53B 0.035(7) 0.077(10) 0.030(8) 0.017(7) -0.001(6) -0.001(7) C54B 0.051(9) 0.060(9) 0.053(10) 0.021(8) 0.015(8) -0.013(7) O3 0.0279(17) 0.0670(19) 0.026(2) 0.0232(18) 0.0039(17) 0.0098(14) O4 0.021(2) 0.084(2) 0.0331(19) 0.0160(16) 0.0125(17) -0.0023(18) N3 0.021(2) 0.0327(17) 0.025(2) 0.0122(16) 0.0085(14) 0.0004(14) N4 0.028(4) 0.0262(16) 0.031(3) 0.0016(16) 0.008(3) -0.006(2) C55 0.0270(14) 0.0378(15) 0.0429(18) 0.0177(13) 0.0091(12) 0.0039(11) C56 0.0340(16) 0.0477(17) 0.052(2) 0.0240(16) 0.0056(14) 0.0040(13) C57 0.0328(17) 0.068(2) 0.069(3) 0.036(2) 0.0038(17) 0.0072(16) C58 0.0360(18) 0.078(3) 0.095(3) 0.054(3) 0.029(2) 0.0245(18) C59 0.066(3) 0.062(2) 0.079(3) 0.021(2) 0.037(2) 0.026(2) C60 0.0395(18) 0.056(2) 0.057(2) 0.0096(17) 0.0147(16) 0.0090(15) C61 0.0261(14) 0.0328(14) 0.0415(18) 0.0075(12) 0.0080(12) -0.0034(11) C62 0.0447(18) 0.0366(15) 0.044(2) 0.0071(14) 0.0129(14) -0.0052(13) C63 0.060(2) 0.0468(19) 0.052(2) 0.0067(16) 0.0284(18) -0.0042(16) C64 0.0412(18) 0.0366(17) 0.080(3) -0.0004(17) 0.0285(18) -0.0025(14) C65 0.0350(17) 0.0408(18) 0.080(3) 0.0181(18) 0.0109(17) 0.0075(14) C66 0.0278(14) 0.0361(16) 0.058(2) 0.0151(15) -0.0005(14) 0.0002(12) C67 0.0284(14) 0.0340(14) 0.0306(16) 0.0106(12) 0.0078(11) 0.0023(11) C68 0.0257(13) 0.0444(16) 0.0308(16) 0.0081(13) 0.0098(11) -0.0046(12) C69 0.0352(16) 0.065(2) 0.0361(18) 0.0150(16) 0.0145(13) -0.0013(15) C70 0.0451(19) 0.085(3) 0.0319(19) 0.0084(18) 0.0147(15) -0.0163(19) C71 0.062(2) 0.0470(19) 0.054(2) -0.0056(17) 0.0278(19) -0.0114(17) C72 0.072(3) 0.053(2) 0.066(3) 0.0161(19) 0.036(2) 0.0081(18) C73 0.053(2) 0.0491(18) 0.048(2) 0.0195(16) 0.0244(16) 0.0130(15) C74A 0.0151(18) 0.0398(18) 0.045(2) 0.0048(15) 0.0136(15) 0.0034(14) C75A 0.172(7) 0.062(3) 0.087(4) 0.046(3) -0.010(4) -0.036(4) C76A 0.192(8) 0.075(4) 0.110(5) 0.057(4) 0.001(5) -0.046(4) C77A 0.062(4) 0.071(3) 0.134(5) 0.028(4) 0.036(4) -0.025(3) C78A 0.062(3) 0.055(3) 0.109(5) 0.010(3) 0.005(3) -0.020(2) C79A 0.061(3) 0.055(3) 0.065(3) 0.012(2) 0.007(2) -0.007(2) C74B 0.0151(18) 0.0398(18) 0.045(2) 0.0048(15) 0.0136(15) 0.0034(14) C75B 0.172(7) 0.062(3) 0.087(4) 0.046(3) -0.010(4) -0.036(4) C76B 0.192(8) 0.075(4) 0.110(5) 0.057(4) 0.001(5) -0.046(4) C77B 0.062(4) 0.071(3) 0.134(5) 0.028(4) 0.036(4) -0.025(3) C78B 0.062(3) 0.055(3) 0.109(5) 0.010(3) 0.005(3) -0.020(2) C79B 0.061(3) 0.055(3) 0.065(3) 0.012(2) 0.007(2) -0.007(2) C80 0.0300(15) 0.0618(19) 0.0338(18) 0.0121(15) 0.0064(13) 0.0048(14) C81 0.058(2) 0.115(4) 0.062(3) 0.042(3) 0.026(2) 0.041(2) C82 0.063(3) 0.140(4) 0.077(3) 0.047(3) 0.024(2) 0.048(3) C83 0.0323(18) 0.080(3) 0.071(3) 0.005(2) 0.0145(18) 0.0054(18) C84 0.065(2) 0.054(2) 0.083(3) 0.013(2) 0.049(2) 0.0030(19) C85 0.055(2) 0.0468(18) 0.067(3) 0.0161(18) 0.0356(18) 0.0093(16) C86 0.0340(16) 0.0530(18) 0.0427(19) 0.0232(16) 0.0064(13) -0.0022(13) C87 0.0460(19) 0.055(2) 0.064(2) 0.0282(19) 0.0184(17) 0.0077(16) C88 0.060(2) 0.063(2) 0.096(4) 0.051(2) 0.021(2) 0.0141(19) C89 0.050(2) 0.107(4) 0.111(4) 0.083(4) 0.014(2) 0.006(2) C90 0.061(2) 0.111(4) 0.063(3) 0.057(3) 0.005(2) -0.005(2) C91 0.056(2) 0.083(3) 0.040(2) 0.028(2) 0.0040(17) -0.0110(19) C92 0.0307(14) 0.0336(14) 0.0311(16) 0.0069(12) 0.0067(12) 0.0064(11) C93 0.0223(13) 0.0429(15) 0.0337(16) 0.0121(13) 0.0042(11) 0.0039(11) C94 0.0289(15) 0.0522(18) 0.0358(18) 0.0071(14) 0.0060(12) 0.0020(13) C95 0.0287(15) 0.0430(17) 0.061(2) 0.0059(16) 0.0063(15) 0.0046(13) C96 0.0313(16) 0.0481(18) 0.060(2) 0.0195(17) 0.0031(15) 0.0089(14) C97 0.0458(19) 0.068(2) 0.042(2) 0.0225(18) 0.0075(15) 0.0113(17) C98 0.0394(17) 0.0533(18) 0.0376(18) 0.0131(15) 0.0104(14) 0.0158(14) C99A 0.0291(18) 0.047(2) 0.054(3) 0.021(2) 0.0058(17) 0.0022(16) C10A 0.068(3) 0.061(3) 0.054(3) 0.027(2) 0.009(2) -0.007(2) C11A 0.083(4) 0.087(4) 0.084(4) 0.048(4) 0.016(3) -0.028(3) C12A 0.087(4) 0.083(4) 0.097(5) 0.036(4) -0.002(3) -0.048(3) C13A 0.115(5) 0.064(3) 0.079(5) 0.001(3) 0.023(4) -0.044(3) C14A 0.076(4) 0.065(3) 0.060(3) 0.012(2) 0.024(3) -0.019(3) C99B 0.0291(18) 0.047(2) 0.054(3) 0.021(2) 0.0058(17) 0.0022(16) C10B 0.068(3) 0.061(3) 0.054(3) 0.027(2) 0.009(2) -0.007(2) C11B 0.083(4) 0.087(4) 0.084(4) 0.048(4) 0.016(3) -0.028(3) C12B 0.087(4) 0.083(4) 0.097(5) 0.036(4) -0.002(3) -0.048(3) C13B 0.115(5) 0.064(3) 0.079(5) 0.001(3) 0.023(4) -0.044(3) C14B 0.076(4) 0.065(3) 0.060(3) 0.012(2) 0.024(3) -0.019(3) Cl3 0.0523(4) 0.0380(4) 0.0393(4) 0.0202(3) 0.0012(3) 0.0109(3) Cl4 0.0450(4) 0.0495(4) 0.0233(4) -0.0004(3) 0.0056(3) 0.0079(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 Fe1 N1 2.097(2) . ? Fe1 N2 2.100(2) . ? Fe1 O2 2.1272(18) . ? Fe1 O1 2.1317(18) . ? Fe1 Cl1 2.3323(8) . ? P1 N1 1.585(2) . ? P1 C15 1.797(3) . ? P1 C9 1.808(2) . ? P1 C3 1.813(3) . ? P2 O1 1.5040(19) . ? P2 C16 1.799(3) . ? P2 C22 1.801(3) . ? P2 C15 1.807(3) . ? P3 N2 1.596(2) . ? P3 C34 1.798(3) . ? P3 C40 1.803(3) . ? P3 C28 1.818(3) . ? P4 O2 1.5065(18) . ? P4 C41 1.796(3) . ? P4 C47 1.804(3) . ? P4 C40 1.809(3) . ? N1 C1 1.479(3) . ? N2 C2 1.480(3) . ? C1 C2 1.510(4) . ? C3 C4 1.389(4) . ? C3 C8 1.399(4) . ? C4 C5 1.391(4) . ? C5 C6 1.401(5) . ? C6 C7 1.362(5) . ? C7 C8 1.391(4) . ? C9 C14 1.390(4) . ? C9 C10 1.411(4) . ? C10 C11 1.369(4) . ? C11 C12 1.384(4) . ? C12 C13 1.383(4) . ? C13 C14 1.375(4) . ? C16 C21 1.395(4) . ? C16 C17 1.396(4) . ? C17 C18 1.384(4) . ? C18 C19 1.371(5) . ? C19 C20 1.387(5) . ? C20 C21 1.393(4) . ? C22 C23 1.388(4) . ? C22 C27 1.396(4) . ? C23 C24 1.380(4) . ? C24 C25 1.382(5) . ? C25 C26 1.390(5) . ? C26 C27 1.369(5) . ? C28 C33 1.386(4) . ? C28 C29 1.398(4) . ? C29 C30 1.386(4) . ? C30 C31 1.391(5) . ? C31 C32 1.384(5) . ? C32 C33 1.398(4) . ? C34 C39 1.392(4) . ? C34 C35 1.403(4) . ? C35 C36 1.396(5) . ? C36 C37 1.367(5) . ? C37 C38 1.378(5) . ? C38 C39 1.392(5) . ? C41 C42 1.386(4) . ? C41 C46 1.399(4) . ? C42 C43 1.383(5) . ? C43 C44 1.381(5) . ? C44 C45 1.376(5) . ? C45 C46 1.389(5) . ? C47 C52 1.379(4) . ? C47 C48 1.386(4) . ? C48 C49 1.407(5) . ? C49 C50 1.379(5) . ? C50 C51 1.360(6) . ? C51 C52 1.401(5) . ? Fe2 O4 2.08(2) . ? Fe2 O4A 2.095(6) . ? Fe2 N3A 2.097(6) . ? Fe2 O3A 2.102(7) . ? Fe2 N4A 2.112(12) . ? Fe2 O3 2.12(4) . ? Fe2 N4 2.24(3) . ? Fe2 N3 2.26(3) . ? Fe2 Cl2 2.3127(9) . ? P5 O4 1.50(2) . ? P5 N3A 1.601(5) . ? P5 C67 1.809(3) . ? P5 C61 1.810(3) . ? P5 C55 1.821(3) . ? P6 N4 1.32(3) . ? P6 O3A 1.552(5) . ? P6 C74A 1.780(3) . ? P6 C68 1.798(3) . ? P6 C67 1.813(3) . ? P6 C74B 1.870(9) . ? P7 N4A 1.562(12) . ? P7 O3 1.60(4) . ? P7 C86 1.804(3) . ? P7 C92 1.808(3) . ? P7 C80 1.823(3) . ? P8 O4A 1.496(7) . ? P8 N3 1.62(3) . ? P8 C99A 1.773(2) . ? P8 C93 1.803(3) . ? P8 C92 1.808(3) . ? P8 C99B 1.922(3) . ? C53A N3A 1.429(6) . ? C53A C54A 1.465(5) . ? C54A N4A 1.498(9) . ? C53B N3 1.31(3) . ? C53B C54B 1.53(2) . ? C54B N4 1.52(3) . ? C55 C60 1.364(5) . ? C55 C56 1.388(4) . ? C56 C57 1.385(4) . ? C57 C58 1.355(6) . ? C58 C59 1.351(6) . ? C59 C60 1.409(5) . ? C61 C62 1.388(4) . ? C61 C66 1.388(4) . ? C62 C63 1.382(5) . ? C63 C64 1.378(5) . ? C64 C65 1.354(5) . ? C65 C66 1.371(5) . ? C68 C73 1.383(4) . ? C68 C69 1.404(4) . ? C69 C70 1.385(5) . ? C70 C71 1.392(6) . ? C71 C72 1.372(6) . ? C72 C73 1.397(5) . ? C74A C75A 1.3900 . ? C74A C79A 1.3900 . ? C75A C76A 1.3900 . ? C76A C77A 1.3900 . ? C77A C78A 1.3900 . ? C78A C79A 1.3900 . ? C74B C75B 1.3900 . ? C74B C79B 1.3900 . ? C75B C76B 1.3900 . ? C76B C77B 1.3900 . ? C77B C78B 1.3900 . ? C78B C79B 1.3900 . ? C80 C85 1.370(4) . ? C80 C81 1.4236 . ? C81 C82 1.361(5) . ? C82 C83 1.396(6) . ? C83 C84 1.313(6) . ? C84 C85 1.404(5) . ? C86 C87 1.396(5) . ? C86 C91 1.405(5) . ? C87 C88 1.375(5) . ? C88 C89 1.385(7) . ? C89 C90 1.369(7) . ? C90 C91 1.385(5) . ? C93 C98 1.384(4) . ? C93 C94 1.388(4) . ? C94 C95 1.404(4) . ? C95 C96 1.377(5) . ? C96 C97 1.383(5) . ? C97 C98 1.390(4) . ? C99A C10A 1.3900 . ? C99A C14A 1.3900 . ? C10A C11A 1.3900 . ? C11A C12A 1.3900 . ? C12A C13A 1.3900 . ? C13A C14A 1.3900 . ? C99B C10B 1.3900 . ? C99B C14B 1.3900 . ? C10B C11B 1.3900 . ? C11B C12B 1.3900 . ? C12B C13B 1.3900 . ? C13B C14B 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 79.98(9) . . ? N1 Fe1 O2 158.19(9) . . ? N2 Fe1 O2 89.80(8) . . ? N1 Fe1 O1 90.78(7) . . ? N2 Fe1 O1 137.26(8) . . ? O2 Fe1 O1 83.69(7) . . ? N1 Fe1 Cl1 102.54(7) . . ? N2 Fe1 Cl1 114.85(6) . . ? O2 Fe1 Cl1 99.23(6) . . ? O1 Fe1 Cl1 107.89(6) . . ? N1 P1 C15 108.91(12) . . ? N1 P1 C9 113.84(13) . . ? C15 P1 C9 109.44(12) . . ? N1 P1 C3 112.93(12) . . ? C15 P1 C3 103.04(13) . . ? C9 P1 C3 108.09(12) . . ? O1 P2 C16 111.69(12) . . ? O1 P2 C22 110.89(12) . . ? C16 P2 C22 105.85(12) . . ? O1 P2 C15 113.00(11) . . ? C16 P2 C15 109.61(12) . . ? C22 P2 C15 105.38(13) . . ? N2 P3 C34 116.10(12) . . ? N2 P3 C40 107.97(12) . . ? C34 P3 C40 108.22(13) . . ? N2 P3 C28 111.21(12) . . ? C34 P3 C28 105.65(13) . . ? C40 P3 C28 107.34(12) . . ? O2 P4 C41 110.40(12) . . ? O2 P4 C47 110.35(13) . . ? C41 P4 C47 111.03(13) . . ? O2 P4 C40 113.54(11) . . ? C41 P4 C40 107.72(13) . . ? C47 P4 C40 103.59(13) . . ? P2 O1 Fe1 121.52(10) . . ? P4 O2 Fe1 120.62(10) . . ? C1 N1 P1 120.03(17) . . ? C1 N1 Fe1 112.32(15) . . ? P1 N1 Fe1 124.95(13) . . ? C2 N2 P3 118.20(18) . . ? C2 N2 Fe1 112.74(16) . . ? P3 N2 Fe1 122.81(13) . . ? N1 C1 C2 108.8(2) . . ? N2 C2 C1 109.3(2) . . ? C4 C3 C8 119.9(3) . . ? C4 C3 P1 116.8(2) . . ? C8 C3 P1 123.3(2) . . ? C3 C4 C5 119.7(3) . . ? C4 C5 C6 119.8(3) . . ? C7 C6 C5 120.4(3) . . ? C6 C7 C8 120.4(3) . . ? C7 C8 C3 119.7(3) . . ? C14 C9 C10 119.0(2) . . ? C14 C9 P1 118.0(2) . . ? C10 C9 P1 122.9(2) . . ? C11 C10 C9 119.2(3) . . ? C10 C11 C12 121.1(3) . . ? C13 C12 C11 120.0(3) . . ? C14 C13 C12 119.7(3) . . ? C13 C14 C9 121.0(3) . . ? P1 C15 P2 116.62(15) . . ? C21 C16 C17 119.7(2) . . ? C21 C16 P2 118.1(2) . . ? C17 C16 P2 122.0(2) . . ? C18 C17 C16 119.5(3) . . ? C19 C18 C17 120.8(3) . . ? C18 C19 C20 120.5(3) . . ? C19 C20 C21 119.5(3) . . ? C20 C21 C16 120.0(3) . . ? C23 C22 C27 119.8(3) . . ? C23 C22 P2 122.6(2) . . ? C27 C22 P2 117.5(2) . . ? C24 C23 C22 119.8(3) . . ? C23 C24 C25 120.1(3) . . ? C24 C25 C26 120.3(3) . . ? C27 C26 C25 119.9(3) . . ? C26 C27 C22 120.2(3) . . ? C33 C28 C29 120.4(3) . . ? C33 C28 P3 122.8(2) . . ? C29 C28 P3 116.5(2) . . ? C30 C29 C28 119.7(3) . . ? C29 C30 C31 120.1(3) . . ? C32 C31 C30 120.1(3) . . ? C31 C32 C33 120.2(3) . . ? C28 C33 C32 119.4(3) . . ? C39 C34 C35 119.2(3) . . ? C39 C34 P3 122.4(2) . . ? C35 C34 P3 118.4(2) . . ? C36 C35 C34 119.9(3) . . ? C37 C36 C35 119.9(3) . . ? C36 C37 C38 121.2(3) . . ? C37 C38 C39 119.8(3) . . ? C38 C39 C34 120.1(3) . . ? P3 C40 P4 116.76(14) . . ? C42 C41 C46 120.0(3) . . ? C42 C41 P4 118.3(2) . . ? C46 C41 P4 121.7(2) . . ? C43 C42 C41 120.1(3) . . ? C44 C43 C42 120.0(3) . . ? C45 C44 C43 120.2(3) . . ? C44 C45 C46 120.6(3) . . ? C45 C46 C41 119.1(3) . . ? C52 C47 C48 119.8(3) . . ? C52 C47 P4 121.5(3) . . ? C48 C47 P4 118.5(2) . . ? C47 C48 C49 120.0(3) . . ? C50 C49 C48 119.8(4) . . ? C51 C50 C49 119.9(3) . . ? C50 C51 C52 121.3(3) . . ? C47 C52 C51 119.3(4) . . ? O4 Fe2 O4A 149.3(6) . . ? O4 Fe2 N3A 9.6(5) . . ? O4A Fe2 N3A 155.0(3) . . ? O4 Fe2 O3A 86.2(5) . . ? O4A Fe2 O3A 81.6(2) . . ? N3A Fe2 O3A 95.3(2) . . ? O4 Fe2 N4A 84.9(7) . . ? O4A Fe2 N4A 87.1(3) . . ? N3A Fe2 N4A 79.8(3) . . ? O3A Fe2 N4A 141.2(3) . . ? O4 Fe2 O3 81.6(11) . . ? O4A Fe2 O3 91.9(10) . . ? N3A Fe2 O3 76.0(10) . . ? O3A Fe2 O3 144.2(10) . . ? N4A Fe2 O3 5.1(12) . . ? O4 Fe2 N4 82.8(9) . . ? O4A Fe2 N4 86.3(8) . . ? N3A Fe2 N4 91.6(7) . . ? O3A Fe2 N4 4.9(9) . . ? N4A Fe2 N4 143.6(7) . . ? O3 Fe2 N4 146.1(13) . . ? O4 Fe2 N3 146.4(9) . . ? O4A Fe2 N3 6.0(8) . . ? N3A Fe2 N3 153.5(6) . . ? O3A Fe2 N3 75.7(7) . . ? N4A Fe2 N3 91.7(6) . . ? O3 Fe2 N3 96.6(11) . . ? N4 Fe2 N3 80.4(10) . . ? O4 Fe2 Cl2 107.9(6) . . ? O4A Fe2 Cl2 102.57(19) . . ? N3A Fe2 Cl2 102.11(12) . . ? O3A Fe2 Cl2 106.71(19) . . ? N4A Fe2 Cl2 112.0(3) . . ? O3 Fe2 Cl2 109.0(10) . . ? N4 Fe2 Cl2 104.4(7) . . ? N3 Fe2 Cl2 104.4(6) . . ? O4 P5 N3A 12.4(7) . . ? O4 P5 C67 105.8(9) . . ? N3A P5 C67 110.0(2) . . ? O4 P5 C61 106.1(9) . . ? N3A P5 C61 114.33(19) . . ? C67 P5 C61 108.34(14) . . ? O4 P5 C55 122.0(7) . . ? N3A P5 C55 109.69(17) . . ? C67 P5 C55 104.35(12) . . ? C61 P5 C55 109.65(13) . . ? N4 P6 O3A 1.1(13) . . ? N4 P6 C74A 111.5(11) . . ? O3A P6 C74A 110.5(3) . . ? N4 P6 C68 110.2(13) . . ? O3A P6 C68 111.1(3) . . ? C74A P6 C68 107.48(14) . . ? N4 P6 C67 111.9(15) . . ? O3A P6 C67 112.0(3) . . ? C74A P6 C67 106.87(13) . . ? C68 P6 C67 108.71(13) . . ? N4 P6 C74B 116.2(11) . . ? O3A P6 C74B 115.1(4) . . ? C74A P6 C74B 12.9(3) . . ? C68 P6 C74B 114.5(2) . . ? C67 P6 C74B 94.1(3) . . ? N4A P7 O3 6.7(15) . . ? N4A P7 C86 113.4(4) . . ? O3 P7 C86 117.4(13) . . ? N4A P7 C92 108.1(4) . . ? O3 P7 C92 110.4(13) . . ? C86 P7 C92 108.95(13) . . ? N4A P7 C80 114.0(3) . . ? O3 P7 C80 107.3(12) . . ? C86 P7 C80 106.24(14) . . ? C92 P7 C80 105.81(14) . . ? O4A P8 N3 9.5(10) . . ? O4A P8 C99A 109.7(3) . . ? N3 P8 C99A 104.4(8) . . ? O4A P8 C93 112.1(3) . . ? N3 P8 C93 107.5(8) . . ? C99A P8 C93 107.70(14) . . ? O4A P8 C92 110.54(19) . . ? N3 P8 C92 120.0(9) . . ? C99A P8 C92 109.14(14) . . ? C93 P8 C92 107.57(13) . . ? O4A P8 C99B 117.9(3) . . ? N3 P8 C99B 114.1(8) . . ? C99A P8 C99B 12.6(3) . . ? C93 P8 C99B 110.46(17) . . ? C92 P8 C99B 96.8(3) . . ? N3A C53A C54A 110.1(4) . . ? C53A C54A N4A 112.6(5) . . ? P6 O3A Fe2 122.2(4) . . ? P8 O4A Fe2 124.8(3) . . ? C53A N3A P5 121.7(4) . . ? C53A N3A Fe2 114.0(3) . . ? P5 N3A Fe2 123.1(3) . . ? C54A N4A P7 118.9(7) . . ? C54A N4A Fe2 110.6(7) . . ? P7 N4A Fe2 123.8(5) . . ? N3 C53B C54B 99.8(16) . . ? N4 C54B C53B 121.6(18) . . ? P7 O3 Fe2 121.3(19) . . ? P5 O4 Fe2 130.5(14) . . ? C53B N3 P8 117.9(19) . . ? C53B N3 Fe2 105.9(16) . . ? P8 N3 Fe2 109.7(12) . . ? P6 N4 C54B 129(2) . . ? P6 N4 Fe2 127(2) . . ? C54B N4 Fe2 97.4(15) . . ? C60 C55 C56 120.0(3) . . ? C60 C55 P5 116.6(2) . . ? C56 C55 P5 123.4(3) . . ? C57 C56 C55 119.7(3) . . ? C58 C57 C56 120.2(3) . . ? C59 C58 C57 120.7(3) . . ? C58 C59 C60 120.3(4) . . ? C55 C60 C59 119.0(3) . . ? C62 C61 C66 119.5(3) . . ? C62 C61 P5 123.0(2) . . ? C66 C61 P5 117.3(2) . . ? C63 C62 C61 119.0(3) . . ? C64 C63 C62 120.3(4) . . ? C65 C64 C63 120.8(3) . . ? C64 C65 C66 119.9(3) . . ? C65 C66 C61 120.5(3) . . ? P5 C67 P6 116.12(14) . . ? C73 C68 C69 120.0(3) . . ? C73 C68 P6 119.3(2) . . ? C69 C68 P6 120.6(2) . . ? C70 C69 C68 118.9(3) . . ? C69 C70 C71 120.9(3) . . ? C72 C71 C70 120.0(4) . . ? C71 C72 C73 120.0(4) . . ? C68 C73 C72 120.2(3) . . ? C75A C74A C79A 120.0 . . ? C75A C74A P6 122.04(17) . . ? C79A C74A P6 117.96(17) . . ? C76A C75A C74A 120.0 . . ? C75A C76A C77A 120.0 . . ? C78A C77A C76A 120.0 . . ? C77A C78A C79A 120.0 . . ? C78A C79A C74A 120.0 . . ? C75B C74B C79B 120.0 . . ? C75B C74B P6 117.18(13) . . ? C79B C74B P6 121.5(2) . . ? C74B C75B C76B 120.0 . . ? C77B C76B C75B 120.0 . . ? C76B C77B C78B 120.0 . . ? C77B C78B C79B 120.0 . . ? C78B C79B C74B 120.0 . . ? C85 C80 C81 118.4(2) . . ? C85 C80 P7 125.2(2) . . ? C81 C80 P7 116.30(11) . . ? C82 C81 C80 118.9(3) . . ? C81 C82 C83 121.4(4) . . ? C84 C83 C82 119.6(4) . . ? C83 C84 C85 121.5(4) . . ? C80 C85 C84 120.1(3) . . ? C87 C86 C91 120.1(3) . . ? C87 C86 P7 118.7(3) . . ? C91 C86 P7 121.2(3) . . ? C88 C87 C86 120.0(4) . . ? C87 C88 C89 119.6(4) . . ? C90 C89 C88 121.0(4) . . ? C89 C90 C91 120.6(4) . . ? C90 C91 C86 118.7(4) . . ? P7 C92 P8 115.89(15) . . ? C98 C93 C94 120.2(3) . . ? C98 C93 P8 122.5(2) . . ? C94 C93 P8 117.2(2) . . ? C93 C94 C95 119.9(3) . . ? C96 C95 C94 119.6(3) . . ? C95 C96 C97 120.2(3) . . ? C96 C97 C98 120.6(3) . . ? C93 C98 C97 119.5(3) . . ? C10A C99A C14A 120.0 . . ? C10A C99A P8 118.11(18) . . ? C14A C99A P8 121.86(18) . . ? C99A C10A C11A 120.0 . . ? C12A C11A C10A 120.0 . . ? C11A C12A C13A 120.0 . . ? C14A C13A C12A 120.0 . . ? C13A C14A C99A 120.0 . . ? C10B C99B C14B 120.0 . . ? C10B C99B P8 119.89(11) . . ? C14B C99B P8 119.63(8) . . ? C11B C10B C99B 120.0 . . ? C10B C11B C12B 120.0 . . ? C13B C12B C11B 120.0 . . ? C12B C13B C14B 120.0 . . ? C13B C14B C99B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.820 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.074 #===END #Compound 8 data_ab706 _database_code_depnum_ccdc_archive 'CCDC 702900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Cl Fe N2 P4,C H2 Cl2,B F4' _chemical_formula_sum 'C53 H50 B Cl3 F4 Fe N2 P4' _chemical_formula_weight 1087.84 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.868(1) _cell_length_b 13.934(1) _cell_length_c 18.166(1) _cell_angle_alpha 100.819(1) _cell_angle_beta 101.043(1) _cell_angle_gamma 102.516(1) _cell_volume 2559.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 19642 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7959 _exptl_absorpt_correction_T_max 0.8534 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29603 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 30.02 _reflns_number_total 14716 _reflns_number_gt 11542 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0457P)^2^+0.7764P] 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 14716 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.59184(2) 0.789576(17) 0.274567(13) 0.01810(6) Uani 1 1 d . . . Cl1 Cl 0.79530(4) 0.77127(3) 0.32572(2) 0.02191(8) Uani 1 1 d . . . P1 P 0.65027(4) 1.03607(3) 0.29626(2) 0.01833(9) Uani 1 1 d . . . P2 P 0.43436(4) 0.65904(3) 0.37430(2) 0.01929(9) Uani 1 1 d . . . P3 P 0.63373(4) 0.86236(3) 0.16426(2) 0.01872(9) Uani 1 1 d . . . P4 P 0.48836(4) 0.60231(3) 0.21958(2) 0.01896(9) Uani 1 1 d . . . N1 N 0.58281(14) 0.93639(10) 0.31991(8) 0.0211(3) Uani 1 1 d . . . N2 N 0.46705(14) 0.76161(10) 0.34625(8) 0.0209(3) Uani 1 1 d . . . C1 C 0.54744(19) 0.94473(13) 0.39507(10) 0.0264(4) Uani 1 1 d . . . H1A H 0.5195 1.0075 0.4086 0.032 Uiso 1 1 calc R . . H1B H 0.6232 0.9471 0.4362 0.032 Uiso 1 1 calc R . . C2 C 0.43761(18) 0.85296(13) 0.38775(11) 0.0267(4) Uani 1 1 d . . . H2A H 0.4280 0.8457 0.4397 0.032 Uiso 1 1 calc R . . H2B H 0.3550 0.8612 0.3589 0.032 Uiso 1 1 calc R . . C3 C 0.77694(16) 1.12051(12) 0.37492(10) 0.0215(3) Uani 1 1 d . . . C4 C 0.86905(18) 1.07878(14) 0.41318(11) 0.0276(4) Uani 1 1 d . . . H4 H 0.8652 1.0093 0.3955 0.033 Uiso 1 1 calc R . . C5 C 0.96549(19) 1.13782(15) 0.47646(11) 0.0322(4) Uani 1 1 d . . . H5 H 1.0281 1.1091 0.5018 0.039 Uiso 1 1 calc R . . C6 C 0.97100(19) 1.23907(15) 0.50312(12) 0.0336(4) Uani 1 1 d . . . H6 H 1.0372 1.2797 0.5468 0.040 Uiso 1 1 calc R . . C7 C 0.8798(2) 1.28064(15) 0.46595(12) 0.0353(4) Uani 1 1 d . . . H7 H 0.8836 1.3499 0.4844 0.042 Uiso 1 1 calc R . . C8 C 0.78327(18) 1.22247(13) 0.40223(11) 0.0286(4) Uani 1 1 d . . . H8 H 0.7213 1.2519 0.3770 0.034 Uiso 1 1 calc R . . C9 C 0.54177(16) 1.10686(12) 0.25949(9) 0.0202(3) Uani 1 1 d . . . C10 C 0.58582(17) 1.18676(13) 0.22648(10) 0.0242(3) Uani 1 1 d . . . H10 H 0.6758 1.2104 0.2291 0.029 Uiso 1 1 calc R . . C11 C 0.4965(2) 1.23157(15) 0.18956(11) 0.0312(4) Uani 1 1 d . . . H11 H 0.5258 1.2862 0.1674 0.037 Uiso 1 1 calc R . . C12 C 0.3655(2) 1.19670(15) 0.18520(11) 0.0331(4) Uani 1 1 d . . . H12 H 0.3051 1.2261 0.1586 0.040 Uiso 1 1 calc R . . C13 C 0.32190(18) 1.11939(14) 0.21925(12) 0.0322(4) Uani 1 1 d . . . H13 H 0.2320 1.0968 0.2169 0.039 Uiso 1 1 calc R . . C14 C 0.40968(17) 1.07472(13) 0.25689(11) 0.0267(4) Uani 1 1 d . . . H14 H 0.3798 1.0222 0.2809 0.032 Uiso 1 1 calc R . . C15 C 0.72134(16) 0.99348(12) 0.21764(9) 0.0201(3) Uani 1 1 d . . . H15A H 0.8137 0.9969 0.2386 0.024 Uiso 1 1 calc R . . H15B H 0.7180 1.0389 0.1819 0.024 Uiso 1 1 calc R . . C16 C 0.49227(16) 0.87277(12) 0.09637(10) 0.0204(3) Uani 1 1 d . . . C17 C 0.48663(18) 0.87118(14) 0.01898(10) 0.0273(4) Uani 1 1 d . . . H17 H 0.5613 0.8687 -0.0005 0.033 Uiso 1 1 calc R . . C18 C 0.3725(2) 0.87316(15) -0.02997(11) 0.0327(4) Uani 1 1 d . . . H18 H 0.3695 0.8716 -0.0828 0.039 Uiso 1 1 calc R . . C19 C 0.26287(19) 0.87732(14) -0.00226(11) 0.0310(4) Uani 1 1 d . . . H19 H 0.1849 0.8782 -0.0360 0.037 Uiso 1 1 calc R . . C20 C 0.26758(18) 0.88019(14) 0.07430(12) 0.0310(4) Uani 1 1 d . . . H20 H 0.1932 0.8844 0.0937 0.037 Uiso 1 1 calc R . . C21 C 0.38098(17) 0.87689(13) 0.12344(10) 0.0256(4) Uani 1 1 d . . . H21 H 0.3828 0.8775 0.1760 0.031 Uiso 1 1 calc R . . C22 C 0.74069(16) 0.82580(12) 0.10487(10) 0.0214(3) Uani 1 1 d . . . C23 C 0.74669(18) 0.72529(13) 0.09049(11) 0.0270(4) Uani 1 1 d . . . H23 H 0.7010 0.6794 0.1148 0.032 Uiso 1 1 calc R . . C24 C 0.8194(2) 0.69213(14) 0.04065(12) 0.0342(4) Uani 1 1 d . . . H24 H 0.8227 0.6234 0.0307 0.041 Uiso 1 1 calc R . . C25 C 0.88679(19) 0.75829(16) 0.00561(12) 0.0353(4) Uani 1 1 d . . . H25 H 0.9347 0.7347 -0.0292 0.042 Uiso 1 1 calc R . . C26 C 0.8848(2) 0.85895(16) 0.02103(13) 0.0379(5) Uani 1 1 d . . . H26 H 0.9329 0.9049 -0.0022 0.045 Uiso 1 1 calc R . . C27 C 0.8118(2) 0.89277(14) 0.07084(12) 0.0323(4) Uani 1 1 d . . . H27 H 0.8107 0.9619 0.0816 0.039 Uiso 1 1 calc R . . C28 C 0.51702(17) 0.67234(12) 0.47330(10) 0.0231(3) Uani 1 1 d . . . C29 C 0.65200(19) 0.71028(15) 0.49295(11) 0.0312(4) Uani 1 1 d . . . H29 H 0.6959 0.7252 0.4543 0.037 Uiso 1 1 calc R . . C30 C 0.7227(2) 0.72637(15) 0.56855(12) 0.0343(4) Uani 1 1 d . . . H30 H 0.8145 0.7516 0.5814 0.041 Uiso 1 1 calc R . . C31 C 0.6589(2) 0.70549(15) 0.62507(11) 0.0344(4) Uani 1 1 d . . . H31 H 0.7071 0.7158 0.6767 0.041 Uiso 1 1 calc R . . C32 C 0.5255(2) 0.66976(16) 0.60653(11) 0.0363(5) Uani 1 1 d . . . H32 H 0.4820 0.6566 0.6457 0.044 Uiso 1 1 calc R . . C33 C 0.45400(19) 0.65284(14) 0.53086(11) 0.0294(4) Uani 1 1 d . . . H33 H 0.3621 0.6280 0.5185 0.035 Uiso 1 1 calc R . . C34 C 0.26442(16) 0.60172(12) 0.36343(10) 0.0222(3) Uani 1 1 d . . . C35 C 0.22408(19) 0.50898(14) 0.38224(12) 0.0298(4) Uani 1 1 d . . . H35 H 0.2867 0.4772 0.4034 0.036 Uiso 1 1 calc R . . C36 C 0.0927(2) 0.46343(15) 0.36995(13) 0.0372(5) Uani 1 1 d . . . H36 H 0.0652 0.3999 0.3820 0.045 Uiso 1 1 calc R . . C37 C 0.0018(2) 0.51056(16) 0.34022(13) 0.0375(5) Uani 1 1 d . . . H37 H -0.0880 0.4798 0.3329 0.045 Uiso 1 1 calc R . . C38 C 0.04018(19) 0.60192(16) 0.32106(12) 0.0339(4) Uani 1 1 d . . . H38 H -0.0231 0.6336 0.3004 0.041 Uiso 1 1 calc R . . C39 C 0.17183(17) 0.64750(13) 0.33205(10) 0.0260(4) Uani 1 1 d . . . H39 H 0.1985 0.7098 0.3181 0.031 Uiso 1 1 calc R . . C40 C 0.49418(16) 0.56959(12) 0.31381(10) 0.0210(3) Uani 1 1 d . . . H40A H 0.4398 0.5000 0.3063 0.025 Uiso 1 1 calc R . . H40B H 0.5846 0.5724 0.3390 0.025 Uiso 1 1 calc R . . C41 C 0.31656(16) 0.56281(12) 0.17156(10) 0.0211(3) Uani 1 1 d . . . C42 C 0.23009(17) 0.47572(13) 0.17652(10) 0.0239(3) Uani 1 1 d . . . H42 H 0.2615 0.4300 0.2031 0.029 Uiso 1 1 calc R . . C43 C 0.09854(17) 0.45534(13) 0.14292(11) 0.0264(4) Uani 1 1 d . . . H43 H 0.0399 0.3966 0.1475 0.032 Uiso 1 1 calc R . . C44 C 0.05256(19) 0.52104(16) 0.10254(12) 0.0352(4) Uani 1 1 d . . . H44 H -0.0376 0.5073 0.0796 0.042 Uiso 1 1 calc R . . C45 C 0.1380(2) 0.60635(17) 0.09572(13) 0.0407(5) Uani 1 1 d . . . H45 H 0.1067 0.6504 0.0673 0.049 Uiso 1 1 calc R . . C46 C 0.26879(19) 0.62761(15) 0.13021(12) 0.0313(4) Uani 1 1 d . . . H46 H 0.3268 0.6868 0.1258 0.038 Uiso 1 1 calc R . . C47 C 0.56126(16) 0.51235(12) 0.16871(10) 0.0210(3) Uani 1 1 d . . . C48 C 0.50278(18) 0.45825(13) 0.09313(10) 0.0261(4) Uani 1 1 d . . . H48 H 0.4184 0.4614 0.0694 0.031 Uiso 1 1 calc R . . C49 C 0.5672(2) 0.39931(14) 0.05179(11) 0.0307(4) Uani 1 1 d . . . H49 H 0.5269 0.3632 -0.0001 0.037 Uiso 1 1 calc R . . C50 C 0.68853(19) 0.39335(14) 0.08587(12) 0.0316(4) Uani 1 1 d . . . H50 H 0.7316 0.3525 0.0577 0.038 Uiso 1 1 calc R . . C51 C 0.74810(19) 0.44660(16) 0.16105(13) 0.0364(5) Uani 1 1 d . . . H51 H 0.8319 0.4421 0.1846 0.044 Uiso 1 1 calc R . . C52 C 0.68541(17) 0.50693(14) 0.20229(11) 0.0303(4) Uani 1 1 d . . . H52 H 0.7275 0.5446 0.2536 0.036 Uiso 1 1 calc R . . Cl2 Cl 0.18168(9) 0.99229(7) 0.38490(6) 0.0848(3) Uani 1 1 d . . . Cl3 Cl 0.10909(7) 0.85229(7) 0.23267(5) 0.0684(2) Uani 1 1 d . . . C53 C 0.0643(3) 0.9427(2) 0.2958(2) 0.0798(11) Uani 1 1 d . . . H53A H -0.0200 0.9112 0.3055 0.096 Uiso 1 1 calc R . . H53B H 0.0528 0.9987 0.2710 0.096 Uiso 1 1 calc R . . F1 F 0.10935(12) 0.27223(9) 0.21784(9) 0.0484(3) Uani 1 1 d . . . F2 F -0.00895(17) 0.11716(13) 0.15103(11) 0.0838(6) Uani 1 1 d . . . F3 F 0.01216(16) 0.16256(15) 0.27772(10) 0.0776(5) Uani 1 1 d . . . F4 F -0.11074(13) 0.22929(12) 0.19651(10) 0.0620(4) Uani 1 1 d . . . B1 B 0.0002(2) 0.19671(16) 0.21125(14) 0.0302(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01804(12) 0.01852(11) 0.01777(12) 0.00391(9) 0.00386(9) 0.00561(9) Cl1 0.01511(17) 0.02495(18) 0.0251(2) 0.00775(16) 0.00129(15) 0.00581(15) P1 0.0188(2) 0.01792(18) 0.0185(2) 0.00358(15) 0.00464(16) 0.00599(16) P2 0.0198(2) 0.02005(19) 0.0195(2) 0.00562(16) 0.00560(16) 0.00680(16) P3 0.0199(2) 0.01820(18) 0.0182(2) 0.00379(16) 0.00480(16) 0.00575(16) P4 0.0184(2) 0.01826(18) 0.0197(2) 0.00378(16) 0.00450(16) 0.00464(16) N1 0.0263(7) 0.0187(6) 0.0194(7) 0.0034(5) 0.0085(6) 0.0067(6) N2 0.0225(7) 0.0195(6) 0.0225(7) 0.0048(5) 0.0080(6) 0.0072(6) C1 0.0363(10) 0.0219(8) 0.0220(9) 0.0033(7) 0.0120(8) 0.0074(7) C2 0.0320(10) 0.0229(8) 0.0299(9) 0.0054(7) 0.0159(8) 0.0101(7) C3 0.0212(8) 0.0233(8) 0.0196(8) 0.0030(6) 0.0054(6) 0.0063(7) C4 0.0278(9) 0.0276(9) 0.0259(9) 0.0046(7) 0.0012(7) 0.0102(8) C5 0.0270(9) 0.0395(10) 0.0278(10) 0.0052(8) -0.0008(8) 0.0130(8) C6 0.0261(9) 0.0390(10) 0.0270(10) -0.0038(8) 0.0005(8) 0.0055(8) C7 0.0330(10) 0.0282(9) 0.0356(11) -0.0071(8) -0.0001(9) 0.0092(8) C8 0.0277(9) 0.0250(8) 0.0291(10) -0.0012(7) 0.0007(8) 0.0104(8) C9 0.0215(8) 0.0205(7) 0.0195(8) 0.0035(6) 0.0051(6) 0.0082(6) C10 0.0250(9) 0.0278(8) 0.0240(9) 0.0089(7) 0.0094(7) 0.0100(7) C11 0.0408(11) 0.0349(10) 0.0292(10) 0.0163(8) 0.0151(9) 0.0199(9) C12 0.0363(11) 0.0412(11) 0.0280(10) 0.0097(8) 0.0056(8) 0.0237(9) C13 0.0219(9) 0.0336(10) 0.0400(11) 0.0037(8) 0.0057(8) 0.0106(8) C14 0.0243(9) 0.0247(8) 0.0319(10) 0.0056(7) 0.0088(7) 0.0075(7) C15 0.0191(8) 0.0207(7) 0.0205(8) 0.0039(6) 0.0052(6) 0.0056(6) C16 0.0218(8) 0.0170(7) 0.0204(8) 0.0026(6) 0.0031(6) 0.0039(6) C17 0.0296(9) 0.0311(9) 0.0230(9) 0.0071(7) 0.0070(7) 0.0108(8) C18 0.0415(11) 0.0363(10) 0.0189(9) 0.0069(8) 0.0017(8) 0.0122(9) C19 0.0317(10) 0.0275(9) 0.0297(10) 0.0065(8) -0.0036(8) 0.0091(8) C20 0.0237(9) 0.0352(10) 0.0337(10) 0.0074(8) 0.0041(8) 0.0106(8) C21 0.0253(9) 0.0299(9) 0.0215(8) 0.0062(7) 0.0045(7) 0.0079(7) C22 0.0213(8) 0.0214(7) 0.0205(8) 0.0014(6) 0.0045(6) 0.0069(7) C23 0.0260(9) 0.0230(8) 0.0321(10) 0.0054(7) 0.0068(8) 0.0079(7) C24 0.0331(10) 0.0275(9) 0.0421(12) 0.0005(8) 0.0103(9) 0.0137(8) C25 0.0292(10) 0.0407(11) 0.0352(11) -0.0019(9) 0.0130(9) 0.0122(9) C26 0.0402(11) 0.0366(10) 0.0424(12) 0.0089(9) 0.0242(10) 0.0095(9) C27 0.0376(11) 0.0270(9) 0.0384(11) 0.0085(8) 0.0201(9) 0.0110(8) C28 0.0273(9) 0.0225(8) 0.0201(8) 0.0048(6) 0.0042(7) 0.0089(7) C29 0.0305(10) 0.0361(10) 0.0260(10) 0.0118(8) 0.0046(8) 0.0048(8) C30 0.0313(10) 0.0352(10) 0.0307(10) 0.0058(8) -0.0015(8) 0.0071(9) C31 0.0460(12) 0.0366(10) 0.0222(9) 0.0034(8) 0.0014(8) 0.0230(10) C32 0.0470(12) 0.0496(12) 0.0232(9) 0.0119(9) 0.0143(9) 0.0277(10) C33 0.0314(10) 0.0377(10) 0.0251(9) 0.0093(8) 0.0108(8) 0.0163(8) C34 0.0215(8) 0.0228(8) 0.0221(8) 0.0035(6) 0.0066(7) 0.0061(7) C35 0.0290(9) 0.0268(9) 0.0362(11) 0.0100(8) 0.0107(8) 0.0084(8) C36 0.0342(11) 0.0314(10) 0.0438(12) 0.0101(9) 0.0138(9) -0.0007(9) C37 0.0238(9) 0.0433(11) 0.0396(12) 0.0033(9) 0.0102(8) 0.0008(9) C38 0.0252(9) 0.0404(11) 0.0328(11) 0.0033(9) 0.0028(8) 0.0104(9) C39 0.0244(9) 0.0267(8) 0.0255(9) 0.0049(7) 0.0042(7) 0.0067(7) C40 0.0215(8) 0.0206(7) 0.0224(8) 0.0060(6) 0.0054(6) 0.0081(7) C41 0.0196(8) 0.0218(7) 0.0216(8) 0.0040(6) 0.0051(6) 0.0053(7) C42 0.0234(8) 0.0218(8) 0.0250(9) 0.0040(7) 0.0049(7) 0.0053(7) C43 0.0222(8) 0.0265(8) 0.0276(9) 0.0038(7) 0.0065(7) 0.0023(7) C44 0.0203(9) 0.0436(11) 0.0381(11) 0.0112(9) -0.0001(8) 0.0063(8) C45 0.0287(10) 0.0459(12) 0.0497(13) 0.0260(11) 0.0002(9) 0.0098(9) C46 0.0258(9) 0.0319(9) 0.0369(11) 0.0170(8) 0.0045(8) 0.0040(8) C47 0.0223(8) 0.0174(7) 0.0240(8) 0.0047(6) 0.0089(7) 0.0039(6) C48 0.0305(9) 0.0245(8) 0.0241(9) 0.0058(7) 0.0060(7) 0.0096(7) C49 0.0396(11) 0.0285(9) 0.0239(9) 0.0023(7) 0.0096(8) 0.0105(8) C50 0.0310(10) 0.0288(9) 0.0359(11) 0.0012(8) 0.0173(8) 0.0073(8) C51 0.0226(9) 0.0411(11) 0.0424(12) -0.0016(9) 0.0098(8) 0.0105(9) C52 0.0202(8) 0.0349(10) 0.0300(10) -0.0036(8) 0.0044(7) 0.0063(8) Cl2 0.0940(6) 0.0789(5) 0.1164(7) 0.0306(5) 0.0680(6) 0.0516(5) Cl3 0.0467(4) 0.1001(6) 0.0696(5) 0.0485(4) 0.0146(3) 0.0179(4) C53 0.0409(15) 0.0759(19) 0.164(4) 0.078(2) 0.0511(19) 0.0345(15) F1 0.0303(6) 0.0394(7) 0.0756(10) 0.0279(7) 0.0066(6) 0.0023(6) F2 0.0679(11) 0.0728(11) 0.0790(13) -0.0308(9) -0.0101(9) 0.0194(9) F3 0.0545(9) 0.1135(14) 0.0711(11) 0.0650(11) 0.0091(8) 0.0034(9) F4 0.0301(7) 0.0804(10) 0.0843(12) 0.0296(9) 0.0117(7) 0.0263(7) B1 0.0219(10) 0.0309(10) 0.0356(12) 0.0118(9) 0.0021(9) 0.0036(9) _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 N2 2.0796(14) . ? Fe1 N1 2.0876(13) . ? Fe1 Cl1 2.3161(5) . ? Fe1 P3 2.4826(5) . ? Fe1 P4 2.5279(5) . ? P1 N1 1.5983(14) . ? P1 C3 1.7984(18) . ? P1 C9 1.8053(16) . ? P1 C15 1.8144(16) . ? P2 N2 1.5971(14) . ? P2 C34 1.8027(18) . ? P2 C28 1.8056(17) . ? P2 C40 1.8150(16) . ? P3 C22 1.8181(16) . ? P3 C16 1.8284(17) . ? P3 C15 1.8472(17) . ? P4 C41 1.8168(17) . ? P4 C47 1.8246(16) . ? P4 C40 1.8456(17) . ? N1 C1 1.479(2) . ? N2 C2 1.483(2) . ? C1 C2 1.514(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.396(2) . ? C3 C4 1.400(2) . ? C4 C5 1.381(3) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 C7 1.383(3) . ? C6 H6 0.9500 . ? C7 C8 1.383(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.397(2) . ? C9 C10 1.399(2) . ? C10 C11 1.397(2) . ? C10 H10 0.9500 . ? C11 C12 1.382(3) . ? C11 H11 0.9500 . ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 C14 1.390(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.391(2) . ? C16 C21 1.398(2) . ? C17 C18 1.390(3) . ? C17 H17 0.9500 . ? C18 C19 1.388(3) . ? C18 H18 0.9500 . ? C19 C20 1.375(3) . ? C19 H19 0.9500 . ? C20 C21 1.392(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.392(2) . ? C22 C23 1.394(2) . ? C23 C24 1.391(2) . ? C23 H23 0.9500 . ? C24 C25 1.377(3) . ? C24 H24 0.9500 . ? C25 C26 1.384(3) . ? C25 H25 0.9500 . ? C26 C27 1.395(2) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.392(2) . ? C28 C29 1.397(3) . ? C29 C30 1.390(3) . ? C29 H29 0.9500 . ? C30 C31 1.384(3) . ? C30 H30 0.9500 . ? C31 C32 1.379(3) . ? C31 H31 0.9500 . ? C32 C33 1.392(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.393(2) . ? C34 C35 1.399(2) . ? C35 C36 1.387(3) . ? C35 H35 0.9500 . ? C36 C37 1.381(3) . ? C36 H36 0.9500 . ? C37 C38 1.381(3) . ? C37 H37 0.9500 . ? C38 C39 1.393(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.394(2) . ? C41 C46 1.399(2) . ? C42 C43 1.386(2) . ? C42 H42 0.9500 . ? C43 C44 1.391(3) . ? C43 H43 0.9500 . ? C44 C45 1.383(3) . ? C44 H44 0.9500 . ? C45 C46 1.381(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.388(2) . ? C47 C52 1.394(2) . ? C48 C49 1.396(2) . ? C48 H48 0.9500 . ? C49 C50 1.372(3) . ? C49 H49 0.9500 . ? C50 C51 1.381(3) . ? C50 H50 0.9500 . ? C51 C52 1.393(2) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? Cl2 C53 1.770(4) . ? Cl3 C53 1.753(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? F1 B1 1.373(2) . ? F2 B1 1.375(3) . ? F3 B1 1.373(3) . ? F4 B1 1.375(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 79.38(5) . . ? N2 Fe1 Cl1 111.40(4) . . ? N1 Fe1 Cl1 109.42(4) . . ? N2 Fe1 P3 146.68(4) . . ? N1 Fe1 P3 82.21(4) . . ? Cl1 Fe1 P3 100.823(16) . . ? N2 Fe1 P4 79.42(4) . . ? N1 Fe1 P4 152.04(4) . . ? Cl1 Fe1 P4 95.200(16) . . ? P3 Fe1 P4 106.554(16) . . ? N1 P1 C3 111.71(8) . . ? N1 P1 C9 115.48(8) . . ? C3 P1 C9 108.48(8) . . ? N1 P1 C15 106.13(7) . . ? C3 P1 C15 108.88(8) . . ? C9 P1 C15 105.81(7) . . ? N2 P2 C34 115.82(7) . . ? N2 P2 C28 112.95(8) . . ? C34 P2 C28 107.63(8) . . ? N2 P2 C40 105.65(7) . . ? C34 P2 C40 106.88(8) . . ? C28 P2 C40 107.44(7) . . ? C22 P3 C16 105.14(8) . . ? C22 P3 C15 103.46(7) . . ? C16 P3 C15 105.61(7) . . ? C22 P3 Fe1 123.99(5) . . ? C16 P3 Fe1 116.83(6) . . ? C15 P3 Fe1 99.25(5) . . ? C41 P4 C47 105.66(8) . . ? C41 P4 C40 104.02(8) . . ? C47 P4 C40 103.56(7) . . ? C41 P4 Fe1 117.80(5) . . ? C47 P4 Fe1 125.99(6) . . ? C40 P4 Fe1 95.75(5) . . ? C1 N1 P1 119.94(11) . . ? C1 N1 Fe1 111.22(10) . . ? P1 N1 Fe1 125.69(8) . . ? C2 N2 P2 119.31(11) . . ? C2 N2 Fe1 114.65(10) . . ? P2 N2 Fe1 124.05(7) . . ? N1 C1 C2 107.82(14) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C1 108.94(13) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C8 C3 C4 118.99(16) . . ? C8 C3 P1 123.71(13) . . ? C4 C3 P1 117.19(13) . . ? C5 C4 C3 120.51(16) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.06(17) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 119.75(18) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C6 120.74(17) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C3 119.94(16) . . ? C7 C8 H8 120.0 . . ? C3 C8 H8 120.0 . . ? C14 C9 C10 119.61(15) . . ? C14 C9 P1 119.28(12) . . ? C10 C9 P1 120.78(12) . . ? C11 C10 C9 119.48(16) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 120.23(17) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C11 120.49(17) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.97(18) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C9 120.16(17) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? P1 C15 P3 111.02(9) . . ? P1 C15 H15A 109.4 . . ? P3 C15 H15A 109.4 . . ? P1 C15 H15B 109.4 . . ? P3 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C21 118.43(16) . . ? C17 C16 P3 124.04(13) . . ? C21 C16 P3 117.42(13) . . ? C18 C17 C16 120.43(17) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.49(17) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 119.69(17) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.16(17) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 120.80(17) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C27 C22 C23 119.12(16) . . ? C27 C22 P3 122.71(12) . . ? C23 C22 P3 118.11(13) . . ? C24 C23 C22 120.09(17) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.40(17) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.17(17) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C27 119.76(19) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C22 C27 C26 120.41(17) . . ? C22 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C33 C28 C29 119.02(17) . . ? C33 C28 P2 124.04(14) . . ? C29 C28 P2 116.83(13) . . ? C30 C29 C28 120.53(18) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 119.86(19) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 120.04(18) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.48(18) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C28 C33 C32 120.05(18) . . ? C28 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C39 C34 C35 119.54(16) . . ? C39 C34 P2 119.63(13) . . ? C35 C34 P2 120.74(13) . . ? C36 C35 C34 120.04(17) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 119.87(18) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C36 120.74(19) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 119.82(18) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C34 C39 C38 119.98(17) . . ? C34 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? P2 C40 P4 108.87(8) . . ? P2 C40 H40A 109.9 . . ? P4 C40 H40A 109.9 . . ? P2 C40 H40B 109.9 . . ? P4 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? C42 C41 C46 118.84(16) . . ? C42 C41 P4 124.29(13) . . ? C46 C41 P4 116.80(13) . . ? C43 C42 C41 120.47(16) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 119.90(17) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C45 C44 C43 120.05(18) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.11(18) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C41 120.60(17) . . ? C45 C46 H46 119.7 . . ? C41 C46 H46 119.7 . . ? C48 C47 C52 118.79(15) . . ? C48 C47 P4 121.12(13) . . ? C52 C47 P4 119.58(13) . . ? C47 C48 C49 120.43(17) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 120.23(18) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 120.10(17) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C52 120.04(18) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C51 C52 C47 120.38(18) . . ? C51 C52 H52 119.8 . . ? C47 C52 H52 119.8 . . ? Cl3 C53 Cl2 112.15(13) . . ? Cl3 C53 H53A 109.2 . . ? Cl2 C53 H53A 109.2 . . ? Cl3 C53 H53B 109.2 . . ? Cl2 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? F3 B1 F1 109.02(18) . . ? F3 B1 F4 110.94(18) . . ? F1 B1 F4 111.60(17) . . ? F3 B1 F2 107.95(19) . . ? F1 B1 F2 109.03(19) . . ? F4 B1 F2 108.20(18) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.816 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.064 #===END