#------------------------------------------------------------------------------ #$Date: 2021-06-15 04:54:23 +0300 (Tue, 15 Jun 2021) $ #$Revision: 266453 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/76/7707656.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7707656 loop_ _publ_author_name 'Petit, Julien' 'Cavaill\'e, Anthony' 'Saffon, Nathalie' 'Fustier-Boutignon, Marie' 'M\'ezailles, Nicolas' _publ_section_title ; Double \a,\a CH Bond Insertion into sp3 CH2 Moiety: Synthesis of a Fe Carbene bis-Hydride Dinitrogen Complex. ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00610J _journal_year 2021 _chemical_formula_sum 'C43 H68 Cl2 Fe N2 O1.5 P2' _chemical_formula_weight 825.68 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-02-12 deposited with the CCDC. 2021-06-14 downloaded from the CCDC. ; _cell_angle_alpha 80.9776(13) _cell_angle_beta 77.2074(14) _cell_angle_gamma 86.6279(14) _cell_formula_units_Z 2 _cell_length_a 11.0591(4) _cell_length_b 11.1758(4) _cell_length_c 18.3680(7) _cell_measurement_reflns_used 9955 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 29.32 _cell_measurement_theta_min 2.86 _cell_volume 2185.75(14) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 193(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker-AXS D8-Venture CMOS detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 47842 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.282 _diffrn_reflns_theta_min 2.858 _diffrn_source 'fine focus sealed tube' _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_correction_T_min 0.6828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.255 _exptl_crystal_description block _exptl_crystal_F_000 884 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.492 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 533 _refine_ls_number_reflns 10829 _refine_ls_number_restraints 214 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0471 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+1.6838P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1073 _refine_ls_wR_factor_ref 0.1254 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7615 _reflns_number_total 10829 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00610j3.cif _cod_data_source_block 2 _cod_original_formula_sum 'C43 H68 Cl2 Fe N2 O1.50 P2' _cod_database_code 7707656 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.894 _shelx_estimated_absorpt_t_max 0.919 _shelx_res_file ; Anthony19_a.res created by SHELXL-2014/7 TITL Anthony19_a.res in P-1 CELL 0.71073 11.05910 11.17580 18.36800 80.9776 77.2074 86.6279 ZERR 2.00 0.00040 0.00040 0.00070 0.0013 0.0014 0.0014 LATT 1 SFAC C H N P Cl Fe O UNIT 86 136 4 4 4 2 3 L.S. 10 SHEL 40 0.75 OMIT -3 6 0 OMIT -4 6 0 OMIT -1 6 0 OMIT -1 6 2 OMIT 6 5 4 OMIT -5 6 0 BOND $H DELU C43 > C46 SIMU 0.01 C43 > C46 FMAP 2 ACTA PLAN 20 DELU C38 > C41' SIMU 0.01 C38 > C41' SIZE 0.15 0.16 0.20 TEMP -80.150 WGHT 0.050800 1.683800 FVAR 0.15124 0.63105 FE1 6 0.503067 0.291250 0.677856 11.00000 0.02102 0.02442 = 0.02797 -0.00490 -0.00480 -0.00086 CL1 5 0.389048 0.380758 0.595645 11.00000 0.03195 0.05099 = 0.03614 -0.00806 -0.01527 0.00356 CL2 5 0.462555 0.108996 0.746200 11.00000 0.05350 0.02814 = 0.05801 0.00052 0.00388 -0.00613 P1 4 0.717359 0.286046 0.601956 11.00000 0.01956 0.02057 = 0.02661 -0.00530 -0.00336 0.00083 P2 4 0.474197 0.451232 0.760302 11.00000 0.01849 0.02557 = 0.02620 -0.00521 -0.00440 0.00011 N1 3 0.727667 0.530055 0.602257 11.00000 0.02378 0.02195 = 0.02915 -0.00806 -0.00620 0.00177 N2 3 0.569150 0.663091 0.660270 11.00000 0.02652 0.02306 = 0.03399 -0.00634 -0.00336 0.00129 C1 1 0.621763 0.612717 0.592580 11.00000 0.02724 0.02433 = 0.02945 -0.00365 -0.00715 0.00178 AFIX 23 H1A 2 0.649624 0.679195 0.550759 11.00000 -1.20000 H1B 2 0.557446 0.567990 0.578855 11.00000 -1.20000 AFIX 0 C2 1 0.755552 0.440651 0.550477 11.00000 0.02343 0.02491 = 0.02468 -0.00653 -0.00279 -0.00015 AFIX 23 H2A 2 0.844683 0.442913 0.525695 11.00000 -1.20000 H2B 2 0.706900 0.460768 0.510770 11.00000 -1.20000 AFIX 0 C3 1 0.458126 0.609015 0.709595 11.00000 0.02531 0.02583 = 0.03500 -0.00676 -0.00412 0.00390 AFIX 23 H3A 2 0.394907 0.608336 0.679020 11.00000 -1.20000 H3B 2 0.425468 0.662579 0.747981 11.00000 -1.20000 AFIX 0 C4 1 0.821191 0.584593 0.624662 11.00000 0.02752 0.01947 = 0.02447 -0.00099 -0.00325 -0.00448 C5 1 0.783160 0.680525 0.669348 11.00000 0.03009 0.01970 = 0.02594 -0.00149 -0.00181 -0.00512 C6 1 0.655842 0.717008 0.689639 11.00000 0.03228 0.02033 = 0.03125 -0.00185 -0.00130 -0.00379 C7 1 0.620707 0.803326 0.736851 11.00000 0.04239 0.02410 = 0.04855 -0.01146 0.00169 -0.00070 AFIX 43 H7 2 0.536018 0.828151 0.749907 11.00000 -1.20000 AFIX 0 C8 1 0.709657 0.854508 0.765612 11.00000 0.06070 0.03017 = 0.04900 -0.01838 0.00229 -0.01317 AFIX 43 H8 2 0.684421 0.913584 0.798290 11.00000 -1.20000 AFIX 0 C9 1 0.831817 0.820810 0.747410 11.00000 0.05384 0.03114 = 0.04398 -0.01048 -0.00526 -0.01730 AFIX 43 H9 2 0.890415 0.856891 0.767522 11.00000 -1.20000 AFIX 0 C10 1 0.872769 0.732797 0.698955 11.00000 0.04151 0.02345 = 0.03243 -0.00280 -0.00501 -0.01087 C11 1 0.997983 0.692606 0.681967 11.00000 0.03428 0.04177 = 0.04219 -0.00486 -0.00912 -0.01479 AFIX 43 H11 2 1.058438 0.728422 0.700716 11.00000 -1.20000 AFIX 0 C12 1 1.032160 0.602989 0.638945 11.00000 0.02570 0.03990 = 0.04204 -0.00419 -0.00617 -0.00491 AFIX 43 H12 2 1.116569 0.576451 0.628200 11.00000 -1.20000 AFIX 0 C13 1 0.944748 0.548461 0.609861 11.00000 0.02705 0.02788 = 0.03067 -0.00395 -0.00238 -0.00338 AFIX 43 H13 2 0.971187 0.486125 0.579726 11.00000 -1.20000 AFIX 0 C14 1 0.744095 0.191884 0.525116 11.00000 0.02455 0.02545 = 0.03007 -0.00894 -0.00384 0.00122 AFIX 13 H14 2 0.828049 0.210708 0.492676 11.00000 -1.20000 AFIX 0 C15 1 0.648964 0.221406 0.475089 11.00000 0.04002 0.03370 = 0.05119 -0.02100 -0.02081 0.01065 AFIX 23 H15A 2 0.653043 0.308296 0.453338 11.00000 -1.20000 H15B 2 0.564505 0.206242 0.506240 11.00000 -1.20000 AFIX 0 C16 1 0.673547 0.144062 0.411011 11.00000 0.04966 0.04475 = 0.05100 -0.02205 -0.02546 0.00840 AFIX 23 H16A 2 0.607595 0.161324 0.381852 11.00000 -1.20000 H16B 2 0.753726 0.166614 0.376415 11.00000 -1.20000 AFIX 0 C17 1 0.677111 0.009562 0.440601 11.00000 0.03676 0.04170 = 0.06207 -0.02993 -0.00485 -0.00106 AFIX 23 H17A 2 0.699908 -0.036741 0.397592 11.00000 -1.20000 H17B 2 0.593728 -0.015528 0.469729 11.00000 -1.20000 AFIX 0 C18 1 0.770560 -0.019369 0.490857 11.00000 0.06807 0.02845 = 0.05219 -0.01896 -0.01602 0.00954 AFIX 23 H18A 2 0.855125 -0.002602 0.460286 11.00000 -1.20000 H18B 2 0.767590 -0.106584 0.511852 11.00000 -1.20000 AFIX 0 C19 1 0.743510 0.056067 0.555643 11.00000 0.06451 0.02683 = 0.04040 -0.00975 -0.00966 0.00130 AFIX 23 H19A 2 0.807010 0.037013 0.586482 11.00000 -1.20000 H19B 2 0.661536 0.034896 0.588491 11.00000 -1.20000 AFIX 0 C20 1 0.848527 0.251787 0.650215 11.00000 0.02304 0.02273 = 0.03149 -0.00728 -0.00605 0.00335 AFIX 13 H20 2 0.855352 0.324397 0.674556 11.00000 -1.20000 AFIX 0 C21 1 0.828925 0.144229 0.714152 11.00000 0.03493 0.02516 = 0.03299 -0.00460 -0.00541 0.00328 AFIX 23 H21A 2 0.747233 0.153357 0.748410 11.00000 -1.20000 H21B 2 0.829588 0.068076 0.692841 11.00000 -1.20000 AFIX 0 C22 1 0.931673 0.137966 0.758479 11.00000 0.05500 0.03788 = 0.03841 -0.00818 -0.02058 0.01093 AFIX 23 H22A 2 0.926284 0.211287 0.783198 11.00000 -1.20000 H22B 2 0.919844 0.066453 0.798426 11.00000 -1.20000 AFIX 0 C23 1 1.059573 0.129049 0.706956 11.00000 0.04185 0.04821 = 0.05896 -0.01688 -0.02756 0.01554 AFIX 23 H23A 2 1.124032 0.131857 0.736391 11.00000 -1.20000 H23B 2 1.068918 0.050377 0.687663 11.00000 -1.20000 AFIX 0 C24 1 1.078815 0.231351 0.640767 11.00000 0.02653 0.04253 = 0.05751 -0.01824 -0.01266 0.00580 AFIX 23 H24A 2 1.159821 0.219193 0.606492 11.00000 -1.20000 H24B 2 1.080173 0.309480 0.659557 11.00000 -1.20000 AFIX 0 C25 1 0.975335 0.235855 0.597289 11.00000 0.02187 0.03048 = 0.03993 -0.00874 -0.00478 0.00476 AFIX 23 H25A 2 0.977324 0.159919 0.575563 11.00000 -1.20000 H25B 2 0.988304 0.304274 0.555253 11.00000 -1.20000 AFIX 0 C26 1 0.320832 0.440602 0.826842 11.00000 0.02173 0.03315 = 0.03324 -0.00943 -0.00445 -0.00081 AFIX 13 H26 2 0.309282 0.512132 0.854496 11.00000 -1.20000 AFIX 0 C27 1 0.310831 0.325490 0.884894 11.00000 0.02443 0.04708 = 0.03329 -0.00094 -0.00347 -0.00350 AFIX 23 H27A 2 0.328381 0.253935 0.858203 11.00000 -1.20000 H27B 2 0.374049 0.326170 0.915469 11.00000 -1.20000 AFIX 0 C28 1 0.182635 0.314417 0.937110 11.00000 0.02812 0.06390 = 0.03546 -0.00181 -0.00114 -0.00973 AFIX 23 H28A 2 0.178553 0.236574 0.971645 11.00000 -1.20000 H28B 2 0.168716 0.380860 0.968128 11.00000 -1.20000 AFIX 0 C29 1 0.081315 0.320198 0.892421 11.00000 0.02580 0.07668 = 0.04926 -0.00228 -0.00516 -0.01704 AFIX 23 H29A 2 0.089287 0.248295 0.866182 11.00000 -1.20000 H29B 2 -0.000856 0.318538 0.927492 11.00000 -1.20000 AFIX 0 C30 1 0.089533 0.433046 0.835513 11.00000 0.02190 0.08554 = 0.06513 0.00804 -0.00879 -0.00441 AFIX 23 H30A 2 0.071751 0.504580 0.862215 11.00000 -1.20000 H30B 2 0.025858 0.431695 0.805335 11.00000 -1.20000 AFIX 0 C31 1 0.216907 0.444992 0.782850 11.00000 0.02212 0.07141 = 0.04513 0.00939 -0.01079 -0.00758 AFIX 23 H31A 2 0.219752 0.522660 0.748226 11.00000 -1.20000 H31B 2 0.230835 0.378424 0.751927 11.00000 -1.20000 AFIX 0 C32 1 0.591032 0.466869 0.815688 11.00000 0.01897 0.02850 = 0.02757 -0.00693 -0.00210 -0.00298 AFIX 13 H32 2 0.662707 0.507657 0.778989 11.00000 -1.20000 AFIX 0 C33 1 0.641845 0.344260 0.847310 11.00000 0.02656 0.03492 = 0.03810 -0.01218 -0.00834 0.00348 AFIX 23 H33A 2 0.668154 0.294206 0.806330 11.00000 -1.20000 H33B 2 0.575758 0.301161 0.886278 11.00000 -1.20000 AFIX 0 C34 1 0.752177 0.360962 0.881952 11.00000 0.02521 0.05442 = 0.04307 -0.01396 -0.01278 0.00684 AFIX 23 H34A 2 0.780931 0.280955 0.904439 11.00000 -1.20000 H34B 2 0.821304 0.396621 0.841856 11.00000 -1.20000 AFIX 0 C35 1 0.717368 0.443143 0.942473 11.00000 0.04663 0.06236 = 0.04463 -0.01947 -0.02448 0.00484 AFIX 23 H35A 2 0.655922 0.402545 0.985590 11.00000 -1.20000 H35B 2 0.792020 0.457358 0.961033 11.00000 -1.20000 AFIX 0 C36 1 0.663211 0.563961 0.912200 11.00000 0.04885 0.04892 = 0.04328 -0.01909 -0.01703 -0.00529 AFIX 23 H36A 2 0.727995 0.608903 0.873248 11.00000 -1.20000 H36B 2 0.636455 0.612873 0.953732 11.00000 -1.20000 AFIX 0 C37 1 0.552881 0.546954 0.878033 11.00000 0.03247 0.03291 = 0.03332 -0.01250 -0.00779 0.00224 AFIX 23 H37A 2 0.522190 0.626885 0.856704 11.00000 -1.20000 H37B 2 0.484844 0.508684 0.917855 11.00000 -1.20000 AFIX 0 SAME C38' > C41' PART 1 21 C38 1 0.092558 0.874899 0.931247 21.00000 0.16147 0.11381 = 0.08908 -0.02195 0.03067 -0.04095 AFIX 23 H38A 2 0.011756 0.919419 0.939203 21.00000 -1.20000 H38B 2 0.118848 0.855321 0.979983 21.00000 -1.20000 AFIX 0 C39 1 0.085073 0.761286 0.897109 21.00000 0.16303 0.11194 = 0.08586 -0.02653 0.02228 -0.05114 AFIX 23 H39A 2 0.097984 0.688873 0.933451 21.00000 -1.20000 H39B 2 0.001756 0.757133 0.886260 21.00000 -1.20000 AFIX 0 O1 7 0.178705 0.762282 0.827978 21.00000 0.16629 0.11356 = 0.12383 -0.04879 0.01594 -0.03950 C40 1 0.234810 0.867347 0.815814 21.00000 0.13318 0.08612 = 0.10298 -0.03090 0.02555 -0.03290 AFIX 23 H40A 2 0.225228 0.911767 0.766287 21.00000 -1.20000 H40B 2 0.324556 0.851790 0.813436 21.00000 -1.20000 AFIX 0 C41 1 0.185293 0.944295 0.874859 21.00000 0.13713 0.08784 = 0.08906 -0.02291 0.02326 -0.02633 AFIX 23 H41A 2 0.252644 0.965581 0.897795 21.00000 -1.20000 H41B 2 0.147653 1.020112 0.852860 21.00000 -1.20000 AFIX 0 PART 2 -21 C38' 1 0.073666 0.879799 0.895396 -21.00000 0.15029 0.11148 = 0.09843 -0.01617 0.01785 -0.02398 AFIX 23 H38C 2 0.022099 0.823743 0.935950 -21.00000 -1.20000 H38D 2 0.021741 0.949143 0.878303 -21.00000 -1.20000 AFIX 0 C39' 1 0.139476 0.817850 0.832611 -21.00000 0.15309 0.10923 = 0.10570 -0.02811 0.01297 -0.03114 AFIX 23 H39C 2 0.152869 0.874316 0.784468 -21.00000 -1.20000 H39D 2 0.091585 0.748504 0.827746 -21.00000 -1.20000 AFIX 0 O1' 7 0.267970 0.772478 0.853205 -21.00000 0.14705 0.10810 = 0.11779 -0.03946 -0.00480 -0.01910 C40' 1 0.292275 0.843254 0.893808 -21.00000 0.14360 0.09243 = 0.10724 -0.02833 0.01511 -0.02304 AFIX 23 H40C 2 0.362057 0.894514 0.864973 -21.00000 -1.20000 H40D 2 0.318591 0.795879 0.938154 -21.00000 -1.20000 AFIX 0 C41' 1 0.185298 0.920713 0.919523 -21.00000 0.14629 0.10225 = 0.09997 -0.02959 0.02533 -0.02951 AFIX 23 H41C 2 0.202660 1.006159 0.897285 -21.00000 -1.20000 H41D 2 0.168257 0.915038 0.975171 -21.00000 -1.20000 AFIX 0 PART 0 SAME C43 > C46 PART -1 C43 1 0.440151 -0.011206 1.041461 10.50000 0.29380 0.09583 = 0.09962 -0.01204 0.03626 -0.04109 AFIX 23 H43A 2 0.364078 0.001696 1.020924 10.50000 -1.20000 H43B 2 0.421822 -0.065510 1.090399 10.50000 -1.20000 AFIX 0 C44 1 0.485605 0.096372 1.048850 10.50000 0.28531 0.09799 = 0.08396 -0.01342 0.02816 -0.03352 AFIX 23 H44A 2 0.421936 0.161704 1.044803 10.50000 -1.20000 H44B 2 0.506333 0.090494 1.099056 10.50000 -1.20000 AFIX 0 O2 7 0.587347 0.122618 0.994614 10.50000 0.29933 0.09594 = 0.07622 -0.01426 0.02178 -0.05494 C45 1 0.605687 0.037000 0.944243 10.50000 0.29637 0.08526 = 0.08737 -0.01451 0.03022 -0.03885 AFIX 23 H45A 2 0.568544 0.066669 0.900200 10.50000 -1.20000 H45B 2 0.695209 0.019699 0.926116 10.50000 -1.20000 AFIX 0 C46 1 0.548058 -0.062904 0.985199 10.50000 0.29376 0.08237 = 0.10778 -0.00967 0.03288 -0.03121 AFIX 23 H46A 2 0.604847 -0.114877 1.012082 10.50000 -1.20000 H46B 2 0.516579 -0.110784 0.952624 10.50000 -1.20000 PART 0 AFIX 0 HKLF 4 REM Anthony19_a.res in P-1 REM R1 = 0.0471 for 7615 Fo > 4sig(Fo) and 0.0828 for all 10829 data REM 533 parameters refined using 214 restraints END WGHT 0.0508 1.6782 REM Highest difference peak 0.492, deepest hole -0.430, 1-sigma level 0.067 Q1 1 0.2001 0.7437 0.9035 11.00000 0.05 0.49 Q2 1 0.4796 0.2775 0.7325 11.00000 0.05 0.45 Q3 1 0.5358 0.3043 0.6192 11.00000 0.05 0.39 Q4 1 0.6205 0.2682 0.6364 11.00000 0.05 0.34 Q5 1 0.0514 0.8220 0.8868 11.00000 0.05 0.34 Q6 1 0.4943 0.1196 0.6776 11.00000 0.05 0.34 Q7 1 0.6036 0.3805 0.5206 11.00000 0.05 0.32 Q8 1 0.7411 0.1253 0.5317 11.00000 0.05 0.31 Q9 1 0.6922 -0.0274 0.4959 11.00000 0.05 0.31 Q10 1 0.6385 0.7364 0.7274 11.00000 0.05 0.31 Q11 1 0.1747 0.8521 0.9392 11.00000 0.05 0.31 Q12 1 0.0827 0.7348 0.8861 11.00000 0.05 0.31 Q13 1 0.8408 0.2012 0.6775 11.00000 0.05 0.30 Q14 1 0.7397 0.3721 0.5724 11.00000 0.05 0.29 Q15 1 0.6755 0.2646 0.6634 11.00000 0.05 0.29 Q16 1 0.3515 0.3668 0.6570 11.00000 0.05 0.29 Q17 1 0.9175 0.2402 0.6272 11.00000 0.05 0.29 Q18 1 0.3976 0.4403 0.7927 11.00000 0.05 0.28 Q19 1 0.0775 0.8892 0.8227 11.00000 0.05 0.27 Q20 1 0.4946 0.4048 0.7173 11.00000 0.05 0.27 ; _shelx_res_checksum 6820 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.50307(3) 0.29125(3) 0.67786(2) 0.02442(9) Uani 1 1 d . . . . . Cl1 Cl 0.38905(6) 0.38076(7) 0.59565(4) 0.03846(16) Uani 1 1 d . . . . . Cl2 Cl 0.46256(8) 0.10900(7) 0.74620(5) 0.0496(2) Uani 1 1 d . . . . . P1 P 0.71736(5) 0.28605(5) 0.60196(3) 0.02236(13) Uani 1 1 d . . . . . P2 P 0.47420(5) 0.45123(6) 0.76030(3) 0.02336(13) Uani 1 1 d . . . . . N1 N 0.72767(18) 0.53005(18) 0.60226(11) 0.0245(4) Uani 1 1 d . . . . . N2 N 0.56915(19) 0.66309(18) 0.66027(12) 0.0282(4) Uani 1 1 d . . . . . C1 C 0.6218(2) 0.6127(2) 0.59258(14) 0.0270(5) Uani 1 1 d . . . . . H1A H 0.6496 0.6792 0.5508 0.032 Uiso 1 1 calc R U . . . H1B H 0.5574 0.5680 0.5789 0.032 Uiso 1 1 calc R U . . . C2 C 0.7556(2) 0.4407(2) 0.55048(13) 0.0244(5) Uani 1 1 d . . . . . H2A H 0.8447 0.4429 0.5257 0.029 Uiso 1 1 calc R U . . . H2B H 0.7069 0.4608 0.5108 0.029 Uiso 1 1 calc R U . . . C3 C 0.4581(2) 0.6090(2) 0.70959(15) 0.0290(5) Uani 1 1 d . . . . . H3A H 0.3949 0.6083 0.6790 0.035 Uiso 1 1 calc R U . . . H3B H 0.4255 0.6626 0.7480 0.035 Uiso 1 1 calc R U . . . C4 C 0.8212(2) 0.5846(2) 0.62466(13) 0.0243(5) Uani 1 1 d . . . . . C5 C 0.7832(2) 0.6805(2) 0.66935(13) 0.0259(5) Uani 1 1 d . . . . . C6 C 0.6558(2) 0.7170(2) 0.68964(14) 0.0289(5) Uani 1 1 d . . . . . C7 C 0.6207(3) 0.8033(2) 0.73685(17) 0.0395(7) Uani 1 1 d . . . . . H7 H 0.5360 0.8282 0.7499 0.047 Uiso 1 1 calc R U . . . C8 C 0.7097(3) 0.8545(3) 0.76561(18) 0.0470(8) Uani 1 1 d . . . . . H8 H 0.6844 0.9136 0.7983 0.056 Uiso 1 1 calc R U . . . C9 C 0.8318(3) 0.8208(3) 0.74741(17) 0.0426(7) Uani 1 1 d . . . . . H9 H 0.8904 0.8569 0.7675 0.051 Uiso 1 1 calc R U . . . C10 C 0.8728(3) 0.7328(2) 0.69896(15) 0.0327(6) Uani 1 1 d . . . . . C11 C 0.9980(3) 0.6926(3) 0.68197(16) 0.0389(6) Uani 1 1 d . . . . . H11 H 1.0584 0.7284 0.7007 0.047 Uiso 1 1 calc R U . . . C12 C 1.0322(2) 0.6030(3) 0.63894(16) 0.0361(6) Uani 1 1 d . . . . . H12 H 1.1166 0.5765 0.6282 0.043 Uiso 1 1 calc R U . . . C13 C 0.9447(2) 0.5485(2) 0.60986(14) 0.0291(5) Uani 1 1 d . . . . . H13 H 0.9712 0.4861 0.5797 0.035 Uiso 1 1 calc R U . . . C14 C 0.7441(2) 0.1919(2) 0.52512(14) 0.0266(5) Uani 1 1 d . . . . . H14 H 0.8280 0.2107 0.4927 0.032 Uiso 1 1 calc R U . . . C15 C 0.6490(3) 0.2214(3) 0.47509(17) 0.0388(7) Uani 1 1 d . . . . . H15A H 0.6530 0.3083 0.4533 0.047 Uiso 1 1 calc R U . . . H15B H 0.5645 0.2062 0.5062 0.047 Uiso 1 1 calc R U . . . C16 C 0.6735(3) 0.1441(3) 0.41101(18) 0.0449(7) Uani 1 1 d . . . . . H16A H 0.6076 0.1613 0.3819 0.054 Uiso 1 1 calc R U . . . H16B H 0.7537 0.1666 0.3764 0.054 Uiso 1 1 calc R U . . . C17 C 0.6771(3) 0.0096(3) 0.44060(19) 0.0453(7) Uani 1 1 d . . . . . H17A H 0.6999 -0.0367 0.3976 0.054 Uiso 1 1 calc R U . . . H17B H 0.5937 -0.0155 0.4697 0.054 Uiso 1 1 calc R U . . . C18 C 0.7706(3) -0.0194(3) 0.49086(18) 0.0481(8) Uani 1 1 d . . . . . H18A H 0.8551 -0.0026 0.4603 0.058 Uiso 1 1 calc R U . . . H18B H 0.7676 -0.1066 0.5119 0.058 Uiso 1 1 calc R U . . . C19 C 0.7435(3) 0.0561(3) 0.55564(17) 0.0437(7) Uani 1 1 d . . . . . H19A H 0.8070 0.0370 0.5865 0.052 Uiso 1 1 calc R U . . . H19B H 0.6615 0.0349 0.5885 0.052 Uiso 1 1 calc R U . . . C20 C 0.8485(2) 0.2518(2) 0.65022(14) 0.0255(5) Uani 1 1 d . . . . . H20 H 0.8554 0.3244 0.6746 0.031 Uiso 1 1 calc R U . . . C21 C 0.8289(2) 0.1442(2) 0.71415(15) 0.0315(6) Uani 1 1 d . . . . . H21A H 0.7472 0.1534 0.7484 0.038 Uiso 1 1 calc R U . . . H21B H 0.8296 0.0681 0.6928 0.038 Uiso 1 1 calc R U . . . C22 C 0.9317(3) 0.1380(3) 0.75848(17) 0.0423(7) Uani 1 1 d . . . . . H22A H 0.9263 0.2113 0.7832 0.051 Uiso 1 1 calc R U . . . H22B H 0.9198 0.0665 0.7984 0.051 Uiso 1 1 calc R U . . . C23 C 1.0596(3) 0.1290(3) 0.70696(18) 0.0467(8) Uani 1 1 d . . . . . H23A H 1.1240 0.1319 0.7364 0.056 Uiso 1 1 calc R U . . . H23B H 1.0689 0.0504 0.6877 0.056 Uiso 1 1 calc R U . . . C24 C 1.0788(2) 0.2314(3) 0.64077(18) 0.0407(7) Uani 1 1 d . . . . . H24A H 1.1598 0.2192 0.6065 0.049 Uiso 1 1 calc R U . . . H24B H 1.0802 0.3095 0.6596 0.049 Uiso 1 1 calc R U . . . C25 C 0.9753(2) 0.2359(2) 0.59729(15) 0.0309(5) Uani 1 1 d . . . . . H25A H 0.9773 0.1599 0.5756 0.037 Uiso 1 1 calc R U . . . H25B H 0.9883 0.3043 0.5553 0.037 Uiso 1 1 calc R U . . . C26 C 0.3208(2) 0.4406(2) 0.82684(14) 0.0291(5) Uani 1 1 d . . . . . H26 H 0.3093 0.5121 0.8545 0.035 Uiso 1 1 calc R U . . . C27 C 0.3108(2) 0.3255(3) 0.88489(15) 0.0358(6) Uani 1 1 d . . . . . H27A H 0.3284 0.2539 0.8582 0.043 Uiso 1 1 calc R U . . . H27B H 0.3740 0.3262 0.9155 0.043 Uiso 1 1 calc R U . . . C28 C 0.1826(2) 0.3144(3) 0.93711(16) 0.0436(7) Uani 1 1 d . . . . . H28A H 0.1786 0.2366 0.9716 0.052 Uiso 1 1 calc R U . . . H28B H 0.1687 0.3809 0.9681 0.052 Uiso 1 1 calc R U . . . C29 C 0.0813(3) 0.3202(3) 0.89242(18) 0.0512(8) Uani 1 1 d . . . . . H29A H 0.0893 0.2483 0.8662 0.061 Uiso 1 1 calc R U . . . H29B H -0.0009 0.3185 0.9275 0.061 Uiso 1 1 calc R U . . . C30 C 0.0895(3) 0.4330(4) 0.8355(2) 0.0596(10) Uani 1 1 d . . . . . H30A H 0.0718 0.5046 0.8622 0.072 Uiso 1 1 calc R U . . . H30B H 0.0259 0.4317 0.8053 0.072 Uiso 1 1 calc R U . . . C31 C 0.2169(2) 0.4450(3) 0.78285(17) 0.0474(8) Uani 1 1 d . . . . . H31A H 0.2198 0.5227 0.7482 0.057 Uiso 1 1 calc R U . . . H31B H 0.2308 0.3784 0.7519 0.057 Uiso 1 1 calc R U . . . C32 C 0.5910(2) 0.4669(2) 0.81569(13) 0.0251(5) Uani 1 1 d . . . . . H32 H 0.6627 0.5077 0.7790 0.030 Uiso 1 1 calc R U . . . C33 C 0.6418(2) 0.3443(2) 0.84731(15) 0.0324(6) Uani 1 1 d . . . . . H33A H 0.6682 0.2942 0.8063 0.039 Uiso 1 1 calc R U . . . H33B H 0.5758 0.3012 0.8863 0.039 Uiso 1 1 calc R U . . . C34 C 0.7522(2) 0.3610(3) 0.88195(17) 0.0396(7) Uani 1 1 d . . . . . H34A H 0.7809 0.2810 0.9044 0.048 Uiso 1 1 calc R U . . . H34B H 0.8213 0.3966 0.8419 0.048 Uiso 1 1 calc R U . . . C35 C 0.7174(3) 0.4431(3) 0.94247(18) 0.0479(8) Uani 1 1 d . . . . . H35A H 0.6559 0.4025 0.9856 0.057 Uiso 1 1 calc R U . . . H35B H 0.7920 0.4574 0.9610 0.057 Uiso 1 1 calc R U . . . C36 C 0.6632(3) 0.5640(3) 0.91220(18) 0.0444(7) Uani 1 1 d . . . . . H36A H 0.7280 0.6089 0.8732 0.053 Uiso 1 1 calc R U . . . H36B H 0.6365 0.6129 0.9537 0.053 Uiso 1 1 calc R U . . . C37 C 0.5529(2) 0.5470(2) 0.87803(15) 0.0321(6) Uani 1 1 d . . . . . H37A H 0.5222 0.6269 0.8567 0.038 Uiso 1 1 calc R U . . . H37B H 0.4848 0.5087 0.9179 0.038 Uiso 1 1 calc R U . . . C38 C 0.0926(12) 0.8749(10) 0.9312(6) 0.128(3) Uani 0.631(5) 1 d D U P A 1 H38A H 0.0118 0.9194 0.9392 0.154 Uiso 0.631(5) 1 calc R U P A 1 H38B H 0.1188 0.8553 0.9800 0.154 Uiso 0.631(5) 1 calc R U P A 1 C39 C 0.0851(10) 0.7613(9) 0.8971(5) 0.125(3) Uani 0.631(5) 1 d D U P A 1 H39A H 0.0980 0.6889 0.9335 0.150 Uiso 0.631(5) 1 calc R U P A 1 H39B H 0.0018 0.7571 0.8863 0.150 Uiso 0.631(5) 1 calc R U P A 1 O1 O 0.1787(9) 0.7623(7) 0.8280(5) 0.137(2) Uani 0.631(5) 1 d D U P A 1 C40 C 0.2348(10) 0.8673(8) 0.8158(6) 0.112(2) Uani 0.631(5) 1 d D U P A 1 H40A H 0.2252 0.9118 0.7663 0.135 Uiso 0.631(5) 1 calc R U P A 1 H40B H 0.3246 0.8518 0.8134 0.135 Uiso 0.631(5) 1 calc R U P A 1 C41 C 0.1853(10) 0.9443(8) 0.8749(6) 0.110(2) Uani 0.631(5) 1 d D U P A 1 H41A H 0.2526 0.9656 0.8978 0.132 Uiso 0.631(5) 1 calc R U P A 1 H41B H 0.1477 1.0201 0.8529 0.132 Uiso 0.631(5) 1 calc R U P A 1 C38' C 0.0737(15) 0.8798(19) 0.8954(11) 0.126(3) Uani 0.369(5) 1 d D U P A 2 H38C H 0.0221 0.8237 0.9359 0.151 Uiso 0.369(5) 1 calc R U P A 2 H38D H 0.0217 0.9491 0.8783 0.151 Uiso 0.369(5) 1 calc R U P A 2 C39' C 0.1395(18) 0.8179(19) 0.8326(11) 0.127(2) Uani 0.369(5) 1 d D U P A 2 H39C H 0.1529 0.8743 0.7845 0.152 Uiso 0.369(5) 1 calc R U P A 2 H39D H 0.0916 0.7485 0.8277 0.152 Uiso 0.369(5) 1 calc R U P A 2 O1' O 0.2680(12) 0.7725(12) 0.8532(7) 0.125(3) Uani 0.369(5) 1 d D U P A 2 C40' C 0.2923(14) 0.8433(14) 0.8938(9) 0.119(3) Uani 0.369(5) 1 d D U P A 2 H40C H 0.3621 0.8945 0.8650 0.142 Uiso 0.369(5) 1 calc R U P A 2 H40D H 0.3186 0.7959 0.9382 0.142 Uiso 0.369(5) 1 calc R U P A 2 C41' C 0.1853(16) 0.9207(16) 0.9195(11) 0.122(3) Uani 0.369(5) 1 d D U P A 2 H41C H 0.2027 1.0062 0.8973 0.146 Uiso 0.369(5) 1 calc R U P A 2 H41D H 0.1683 0.9150 0.9752 0.146 Uiso 0.369(5) 1 calc R U P A 2 C43 C 0.440(3) -0.011(2) 1.0415(13) 0.174(5) Uani 0.5 1 d . U P B -1 H43A H 0.3641 0.0017 1.0209 0.209 Uiso 0.5 1 calc R U P B -1 H43B H 0.4218 -0.0655 1.0904 0.209 Uiso 0.5 1 calc R U P B -1 C44 C 0.486(2) 0.0964(15) 1.0489(9) 0.165(4) Uani 0.5 1 d . U P B -1 H44A H 0.4219 0.1617 1.0448 0.198 Uiso 0.5 1 calc R U P B -1 H44B H 0.5063 0.0905 1.0991 0.198 Uiso 0.5 1 calc R U P B -1 O2 O 0.5873(12) 0.1226(8) 0.9946(5) 0.165(4) Uani 0.5 1 d . U P B -1 C45 C 0.606(3) 0.0370(18) 0.9442(12) 0.166(4) Uani 0.5 1 d . U P B -1 H45A H 0.5685 0.0667 0.9002 0.199 Uiso 0.5 1 calc R U P B -1 H45B H 0.6952 0.0197 0.9261 0.199 Uiso 0.5 1 calc R U P B -1 C46 C 0.548(2) -0.0629(16) 0.9852(10) 0.173(5) Uani 0.5 1 d . U P B -1 H46A H 0.6048 -0.1149 1.0121 0.207 Uiso 0.5 1 calc R U P B -1 H46B H 0.5166 -0.1108 0.9526 0.207 Uiso 0.5 1 calc R U P B -1 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 0.02102(17) 0.02442(18) 0.02797(19) -0.00490(14) -0.00480(13) -0.00086(13) Cl1 0.0320(3) 0.0510(4) 0.0361(3) -0.0081(3) -0.0153(3) 0.0036(3) Cl2 0.0535(4) 0.0281(4) 0.0580(5) 0.0005(3) 0.0039(4) -0.0061(3) P1 0.0196(3) 0.0206(3) 0.0266(3) -0.0053(2) -0.0034(2) 0.0008(2) P2 0.0185(3) 0.0256(3) 0.0262(3) -0.0052(2) -0.0044(2) 0.0001(2) N1 0.0238(10) 0.0220(10) 0.0291(10) -0.0081(8) -0.0062(8) 0.0018(8) N2 0.0265(10) 0.0231(10) 0.0340(11) -0.0063(9) -0.0034(9) 0.0013(8) C1 0.0272(12) 0.0243(12) 0.0295(12) -0.0036(10) -0.0071(10) 0.0018(10) C2 0.0234(11) 0.0249(12) 0.0247(12) -0.0065(9) -0.0028(9) -0.0001(9) C3 0.0253(12) 0.0258(13) 0.0350(14) -0.0068(10) -0.0041(10) 0.0039(10) C4 0.0275(12) 0.0195(11) 0.0245(12) -0.0010(9) -0.0032(9) -0.0045(9) C5 0.0301(12) 0.0197(11) 0.0259(12) -0.0015(9) -0.0018(10) -0.0051(9) C6 0.0323(13) 0.0203(12) 0.0313(13) -0.0018(10) -0.0013(10) -0.0038(10) C7 0.0424(16) 0.0241(13) 0.0486(17) -0.0115(12) 0.0017(13) -0.0007(11) C8 0.061(2) 0.0302(15) 0.0490(18) -0.0184(13) 0.0023(15) -0.0132(14) C9 0.0538(18) 0.0311(15) 0.0440(17) -0.0105(12) -0.0053(14) -0.0173(13) C10 0.0415(15) 0.0234(13) 0.0324(13) -0.0028(10) -0.0050(11) -0.0109(11) C11 0.0343(14) 0.0418(16) 0.0422(16) -0.0049(13) -0.0091(12) -0.0148(12) C12 0.0257(13) 0.0399(16) 0.0420(15) -0.0042(12) -0.0062(11) -0.0049(11) C13 0.0271(12) 0.0279(13) 0.0307(13) -0.0040(10) -0.0024(10) -0.0034(10) C14 0.0245(12) 0.0255(12) 0.0301(13) -0.0089(10) -0.0038(9) 0.0012(9) C15 0.0400(15) 0.0337(15) 0.0512(17) -0.0210(13) -0.0208(13) 0.0106(12) C16 0.0497(18) 0.0448(17) 0.0510(18) -0.0221(14) -0.0255(15) 0.0084(14) C17 0.0368(15) 0.0417(17) 0.062(2) -0.0299(15) -0.0049(14) -0.0011(13) C18 0.068(2) 0.0285(15) 0.0522(19) -0.0190(13) -0.0160(16) 0.0095(14) C19 0.065(2) 0.0268(14) 0.0404(16) -0.0098(12) -0.0097(14) 0.0013(13) C20 0.0230(11) 0.0227(12) 0.0315(13) -0.0073(10) -0.0060(9) 0.0034(9) C21 0.0349(14) 0.0252(13) 0.0330(14) -0.0046(10) -0.0054(11) 0.0033(10) C22 0.0550(18) 0.0379(16) 0.0384(16) -0.0082(13) -0.0206(14) 0.0109(14) C23 0.0419(16) 0.0482(18) 0.059(2) -0.0169(15) -0.0276(15) 0.0155(14) C24 0.0265(13) 0.0425(16) 0.0575(19) -0.0182(14) -0.0127(13) 0.0058(12) C25 0.0219(12) 0.0305(13) 0.0399(14) -0.0087(11) -0.0048(10) 0.0048(10) C26 0.0217(11) 0.0332(14) 0.0332(13) -0.0094(11) -0.0044(10) -0.0008(10) C27 0.0244(12) 0.0471(17) 0.0333(14) -0.0009(12) -0.0035(10) -0.0035(11) C28 0.0281(14) 0.064(2) 0.0355(15) -0.0018(14) -0.0011(11) -0.0097(13) C29 0.0258(14) 0.077(2) 0.0493(18) -0.0023(17) -0.0052(13) -0.0170(15) C30 0.0219(14) 0.086(3) 0.065(2) 0.008(2) -0.0088(14) -0.0044(15) C31 0.0221(13) 0.071(2) 0.0451(17) 0.0094(16) -0.0108(12) -0.0076(13) C32 0.0190(11) 0.0285(12) 0.0276(12) -0.0069(10) -0.0021(9) -0.0030(9) C33 0.0266(12) 0.0349(14) 0.0381(14) -0.0122(11) -0.0083(11) 0.0035(11) C34 0.0252(13) 0.0544(18) 0.0431(16) -0.0140(14) -0.0128(11) 0.0068(12) C35 0.0466(17) 0.062(2) 0.0446(17) -0.0195(15) -0.0245(14) 0.0048(15) C36 0.0489(17) 0.0489(18) 0.0433(17) -0.0191(14) -0.0170(14) -0.0053(14) C37 0.0325(13) 0.0329(14) 0.0333(14) -0.0125(11) -0.0078(11) 0.0022(11) C38 0.161(5) 0.114(4) 0.089(5) -0.022(4) 0.031(4) -0.041(4) C39 0.163(5) 0.112(5) 0.086(4) -0.027(4) 0.022(4) -0.051(4) O1 0.166(5) 0.114(4) 0.124(4) -0.049(4) 0.016(4) -0.039(4) C40 0.133(5) 0.086(4) 0.103(4) -0.031(4) 0.026(4) -0.033(4) C41 0.137(5) 0.088(4) 0.089(4) -0.023(4) 0.023(4) -0.026(4) C38' 0.150(5) 0.111(5) 0.098(5) -0.016(5) 0.018(5) -0.024(5) C39' 0.153(5) 0.109(5) 0.106(4) -0.028(4) 0.013(4) -0.031(4) O1' 0.147(5) 0.108(5) 0.118(5) -0.039(4) -0.005(5) -0.019(5) C40' 0.144(5) 0.092(5) 0.107(5) -0.028(5) 0.015(5) -0.023(5) C41' 0.146(6) 0.102(5) 0.100(6) -0.030(5) 0.025(5) -0.030(5) C43 0.294(12) 0.096(8) 0.100(9) -0.012(7) 0.036(7) -0.041(7) C44 0.285(12) 0.098(7) 0.084(7) -0.013(6) 0.028(7) -0.034(7) O2 0.299(11) 0.096(5) 0.076(5) -0.014(4) 0.022(5) -0.055(6) C45 0.296(12) 0.085(7) 0.087(7) -0.015(5) 0.030(7) -0.039(7) C46 0.294(12) 0.082(7) 0.108(8) -0.010(6) 0.033(8) -0.031(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl2 Fe1 Cl1 123.30(3) . . ? Cl2 Fe1 P1 108.44(3) . . ? Cl1 Fe1 P1 104.60(3) . . ? Cl2 Fe1 P2 110.91(3) . . ? Cl1 Fe1 P2 97.69(3) . . ? P1 Fe1 P2 111.35(2) . . ? C14 P1 C20 106.46(11) . . ? C14 P1 C2 103.01(11) . . ? C20 P1 C2 101.27(11) . . ? C14 P1 Fe1 115.80(8) . . ? C20 P1 Fe1 119.55(8) . . ? C2 P1 Fe1 108.56(8) . . ? C32 P2 C26 107.22(11) . . ? C32 P2 C3 103.14(12) . . ? C26 P2 C3 99.31(11) . . ? C32 P2 Fe1 119.61(8) . . ? C26 P2 Fe1 111.16(9) . . ? C3 P2 Fe1 114.19(8) . . ? C4 N1 C2 121.86(19) . . ? C4 N1 C1 113.24(19) . . ? C2 N1 C1 114.89(19) . . ? C6 N2 C1 114.1(2) . . ? C6 N2 C3 120.9(2) . . ? C1 N2 C3 118.2(2) . . ? N2 C1 N1 111.5(2) . . ? N2 C1 H1A 109.3 . . ? N1 C1 H1A 109.3 . . ? N2 C1 H1B 109.3 . . ? N1 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N1 C2 P1 110.58(16) . . ? N1 C2 H2A 109.5 . . ? P1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N2 C3 P2 117.35(16) . . ? N2 C3 H3A 108.0 . . ? P2 C3 H3A 108.0 . . ? N2 C3 H3B 108.0 . . ? P2 C3 H3B 108.0 . . ? H3A C3 H3B 107.2 . . ? C13 C4 N1 124.4(2) . . ? C13 C4 C5 118.8(2) . . ? N1 C4 C5 116.7(2) . . ? C10 C5 C6 119.4(2) . . ? C10 C5 C4 119.2(2) . . ? C6 C5 C4 121.1(2) . . ? C7 C6 N2 121.7(2) . . ? C7 C6 C5 120.0(2) . . ? N2 C6 C5 118.3(2) . . ? C6 C7 C8 120.2(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 122.0(3) . . ? C11 C10 C5 119.6(2) . . ? C9 C10 C5 118.4(3) . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 121.3(3) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C4 C13 C12 120.8(2) . . ? C4 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C19 C14 C15 109.8(2) . . ? C19 C14 P1 111.92(18) . . ? C15 C14 P1 111.84(17) . . ? C19 C14 H14 107.7 . . ? C15 C14 H14 107.7 . . ? P1 C14 H14 107.7 . . ? C14 C15 C16 111.2(2) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 111.9(3) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 110.9(2) . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C19 111.3(3) . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C14 110.8(2) . . ? C18 C19 H19A 109.5 . . ? C14 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C25 109.0(2) . . ? C21 C20 P1 114.70(17) . . ? C25 C20 P1 114.70(17) . . ? C21 C20 H20 105.9 . . ? C25 C20 H20 105.9 . . ? P1 C20 H20 105.9 . . ? C22 C21 C20 110.1(2) . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 111.2(2) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 111.7(2) . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C25 110.8(2) . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C20 110.1(2) . . ? C24 C25 H25A 109.6 . . ? C20 C25 H25A 109.6 . . ? C24 C25 H25B 109.6 . . ? C20 C25 H25B 109.6 . . ? H25A C25 H25B 108.2 . . ? C27 C26 C31 109.6(2) . . ? C27 C26 P2 112.28(17) . . ? C31 C26 P2 109.98(18) . . ? C27 C26 H26 108.3 . . ? C31 C26 H26 108.3 . . ? P2 C26 H26 108.3 . . ? C28 C27 C26 112.0(2) . . ? C28 C27 H27A 109.2 . . ? C26 C27 H27A 109.2 . . ? C28 C27 H27B 109.2 . . ? C26 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C29 C28 C27 111.3(2) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 111.2(3) . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C31 112.0(3) . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C30 C31 C26 111.7(3) . . ? C30 C31 H31A 109.3 . . ? C26 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C26 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? C33 C32 C37 110.2(2) . . ? C33 C32 P2 112.30(17) . . ? C37 C32 P2 116.15(16) . . ? C33 C32 H32 105.8 . . ? C37 C32 H32 105.8 . . ? P2 C32 H32 105.8 . . ? C32 C33 C34 110.6(2) . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C33 111.2(2) . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 111.4(2) . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C34 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C37 111.5(2) . . ? C35 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C36 C37 C32 110.2(2) . . ? C36 C37 H37A 109.6 . . ? C32 C37 H37A 109.6 . . ? C36 C37 H37B 109.6 . . ? C32 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C41 C38 C39 103.0(7) . . ? C41 C38 H38A 111.2 . . ? C39 C38 H38A 111.2 . . ? C41 C38 H38B 111.2 . . ? C39 C38 H38B 111.2 . . ? H38A C38 H38B 109.1 . . ? O1 C39 C38 110.0(7) . . ? O1 C39 H39A 109.7 . . ? C38 C39 H39A 109.7 . . ? O1 C39 H39B 109.7 . . ? C38 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C40 O1 C39 106.7(7) . . ? O1 C40 C41 113.0(7) . . ? O1 C40 H40A 109.0 . . ? C41 C40 H40A 109.0 . . ? O1 C40 H40B 109.0 . . ? C41 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C38 C41 C40 107.0(8) . . ? C38 C41 H41A 110.3 . . ? C40 C41 H41A 110.3 . . ? C38 C41 H41B 110.3 . . ? C40 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C39' C38' C41' 98.6(13) . . ? C39' C38' H38C 112.0 . . ? C41' C38' H38C 112.0 . . ? C39' C38' H38D 112.0 . . ? C41' C38' H38D 112.0 . . ? H38C C38' H38D 109.7 . . ? C38' C39' O1' 105.4(13) . . ? C38' C39' H39C 110.7 . . ? O1' C39' H39C 110.7 . . ? C38' C39' H39D 110.7 . . ? O1' C39' H39D 110.7 . . ? H39C C39' H39D 108.8 . . ? C40' O1' C39' 106.6(12) . . ? O1' C40' C41' 111.6(14) . . ? O1' C40' H40C 109.3 . . ? C41' C40' H40C 109.3 . . ? O1' C40' H40D 109.3 . . ? C41' C40' H40D 109.3 . . ? H40C C40' H40D 108.0 . . ? C40' C41' C38' 108.9(12) . . ? C40' C41' H41C 109.9 . . ? C38' C41' H41C 109.9 . . ? C40' C41' H41D 109.9 . . ? C38' C41' H41D 109.9 . . ? H41C C41' H41D 108.3 . . ? C44 C43 C46 102.4(18) . . ? C44 C43 H43A 111.3 . . ? C46 C43 H43A 111.3 . . ? C44 C43 H43B 111.3 . . ? C46 C43 H43B 111.3 . . ? H43A C43 H43B 109.2 . . ? O2 C44 C43 109.5(15) . . ? O2 C44 H44A 109.8 . . ? C43 C44 H44A 109.8 . . ? O2 C44 H44B 109.8 . . ? C43 C44 H44B 109.8 . . ? H44A C44 H44B 108.2 . . ? C44 O2 C45 109.9(13) . . ? C46 C45 O2 104.6(15) . . ? C46 C45 H45A 110.8 . . ? O2 C45 H45A 110.8 . . ? C46 C45 H45B 110.8 . . ? O2 C45 H45B 110.8 . . ? H45A C45 H45B 108.9 . . ? C45 C46 C43 104(2) . . ? C45 C46 H46A 111.0 . . ? C43 C46 H46A 111.0 . . ? C45 C46 H46B 111.0 . . ? C43 C46 H46B 111.0 . . ? H46A C46 H46B 109.0 . . ? 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 Cl2 2.2320(8) . ? Fe1 Cl1 2.2565(7) . ? Fe1 P1 2.4717(7) . ? Fe1 P2 2.4819(7) . ? P1 C14 1.852(2) . ? P1 C20 1.853(2) . ? P1 C2 1.859(2) . ? P2 C32 1.844(2) . ? P2 C26 1.856(2) . ? P2 C3 1.879(3) . ? N1 C4 1.397(3) . ? N1 C2 1.459(3) . ? N1 C1 1.473(3) . ? N2 C6 1.404(3) . ? N2 C1 1.436(3) . ? N2 C3 1.455(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C13 1.382(3) . ? C4 C5 1.439(3) . ? C5 C10 1.423(3) . ? C5 C6 1.427(3) . ? C6 C7 1.379(4) . ? C7 C8 1.402(4) . ? C7 H7 0.9500 . ? C8 C9 1.363(4) . ? C8 H8 0.9500 . ? C9 C10 1.417(4) . ? C9 H9 0.9500 . ? C10 C11 1.413(4) . ? C11 C12 1.357(4) . ? C11 H11 0.9500 . ? C12 C13 1.411(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.533(4) . ? C14 C15 1.534(3) . ? C14 H14 1.0000 . ? C15 C16 1.535(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.517(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.521(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.531(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.532(3) . ? C20 C25 1.538(3) . ? C20 H20 1.0000 . ? C21 C22 1.530(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.525(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.519(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.528(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.529(4) . ? C26 C31 1.539(4) . ? C26 H26 1.0000 . ? C27 C28 1.525(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.522(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.500(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.522(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.528(3) . ? C32 C37 1.534(3) . ? C32 H32 1.0000 . ? C33 C34 1.529(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.522(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.519(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.524(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C41 1.448(11) . ? C38 C39 1.516(12) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O1 1.449(11) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? O1 C40 1.325(11) . ? C40 C41 1.480(11) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C38' C39' 1.469(17) . ? C38' C41' 1.517(16) . ? C38' H38C 0.9900 . ? C38' H38D 0.9900 . ? C39' O1' 1.585(17) . ? C39' H39C 0.9900 . ? C39' H39D 0.9900 . ? O1' C40' 1.246(15) . ? C40' C41' 1.460(16) . ? C40' H40C 0.9900 . ? C40' H40D 0.9900 . ? C41' H41C 0.9900 . ? C41' H41D 0.9900 . ? C43 C44 1.37(3) . ? C43 C46 1.54(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O2 1.34(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O2 C45 1.41(2) . ? C45 C46 1.35(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ?