#------------------------------------------------------------------------------ #$Date: 2014-04-07 07:16:58 +0100 (Mon, 07 Apr 2014) $ #$Revision: 108980 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/22/7112257.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_7112257 loop_ _publ_author_name 'Kyle T. Horak' 'Alexandra Velian' 'Michael W. Day' 'Theodor Agapie' _publ_section_title ; Arene non-innocence in dinuclear complexes of Fe, Co, and Ni supported by a para-terphenyl diphosphine ; _journal_name_full Chem.Commun. _journal_page_first 4427 _journal_paper_doi 10.1039/C4CC00838C _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C34 H40 Fe2 O4 P2' _chemical_formula_sum 'C34 H40 Fe2 O4 P2' _chemical_formula_weight 686.30 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 108.0292(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.3107(5) _cell_length_b 11.4723(4) _cell_length_c 20.2029(7) _cell_measurement_reflns_used 9785 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 36.40 _cell_measurement_theta_min 2.35 _cell_volume 3153.98(19) _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-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_unetI/netI 0.0197 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 178488 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.829 _diffrn_reflns_theta_min 1.496 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_T_max 0.7472 _exptl_absorpt_correction_T_min 0.6637 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour orange-red _exptl_crystal_density_diffrn 1.445 _exptl_crystal_description block _exptl_crystal_F_000 1432 _exptl_crystal_size_max .94 _exptl_crystal_size_mid .55 _exptl_crystal_size_min .54 _refine_diff_density_max 0.824 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 15800 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.890 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0283 _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^)+(0.1000P)^2^+0.2586P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.1165 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12872 _reflns_number_total 15800 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc00838c2.cif _[local]_cod_data_source_block kth02 _cod_database_code 7112257 _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. ; _diffrn_reflns_laue_measured_fraction_max 0.997 _diffrn_reflns_laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.999 _shelxl_version_number 2013-3 _shelx_res_file ; TITL kth02 in P2(1)/c CELL 0.71073 14.3107 11.4723 20.2029 90 108.0292 90 ZERR 4 0.0005 0.0004 0.0007 0 0.0018 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O P Fe UNIT 136 160 16 8 8 L.S. 16 ACTA BOND FMAP 2 PLAN 30 TEMP 23 WGHT 0.100000 0.258626 FVAR 0.09004 FE1 5 0.258626 0.737886 0.127047 11.00000 0.00821 0.01312 = 0.00908 -0.00013 0.00210 0.00129 FE2 5 0.064507 0.735134 0.123396 11.00000 0.00869 0.01286 = 0.00850 0.00066 0.00288 0.00085 P1 4 0.409325 0.722465 0.117973 11.00000 0.00787 0.01452 = 0.01296 0.00168 0.00221 0.00028 P2 4 -0.091245 0.777082 0.114281 11.00000 0.00979 0.01369 = 0.00934 -0.00016 0.00416 0.00067 O1 3 0.302324 0.933051 0.225460 11.00000 0.02603 0.03028 = 0.02470 -0.01335 0.00400 -0.00107 O2 3 0.290562 0.533314 0.217600 11.00000 0.02096 0.03492 = 0.02853 0.01850 0.01200 0.01013 O3 3 0.068932 0.493989 0.171833 11.00000 0.02315 0.02204 = 0.03158 0.01151 0.01047 0.00297 O4 3 0.127280 0.841944 0.261832 11.00000 0.02616 0.03990 = 0.01338 -0.00645 0.00219 0.00145 C1 1 0.169456 0.653515 0.031387 11.00000 0.01127 0.01267 = 0.01212 -0.00121 0.00398 0.00079 C2 1 0.219870 0.756376 0.022859 11.00000 0.00941 0.01388 = 0.00999 0.00028 0.00351 0.00053 C3 1 0.187813 0.859559 0.048582 11.00000 0.00885 0.01272 = 0.01141 0.00021 0.00260 0.00002 C4 1 0.085955 0.866030 0.050221 11.00000 0.00920 0.01259 = 0.01042 0.00018 0.00296 0.00047 C5 1 0.020294 0.773047 0.020598 11.00000 0.00867 0.01395 = 0.00897 0.00015 0.00294 -0.00068 C6 1 0.065171 0.661884 0.026512 11.00000 0.01148 0.01304 = 0.01170 -0.00111 0.00422 -0.00138 C7 1 0.296940 0.757660 -0.012603 11.00000 0.01068 0.01488 = 0.01242 0.00153 0.00532 0.00148 C8 1 0.395790 0.753311 0.027226 11.00000 0.01070 0.01675 = 0.01564 0.00312 0.00455 0.00005 C9 1 0.468794 0.765389 -0.005216 11.00000 0.01096 0.02587 = 0.02280 0.00724 0.00788 0.00135 AFIX 43 H9 2 0.534767 0.765492 0.021264 11.00000 -1.20000 AFIX 0 C10 1 0.442180 0.777214 -0.077148 11.00000 0.01813 0.02313 = 0.02329 0.00777 0.01334 0.00423 AFIX 43 H10 2 0.490486 0.786918 -0.098651 11.00000 -1.20000 AFIX 0 C11 1 0.343470 0.774606 -0.117232 11.00000 0.01934 0.02268 = 0.01749 0.00504 0.01107 0.00631 AFIX 43 H11 2 0.326275 0.779134 -0.165479 11.00000 -1.20000 AFIX 0 C12 1 0.270769 0.765253 -0.085184 11.00000 0.01360 0.02259 = 0.01306 0.00193 0.00572 0.00386 AFIX 43 H12 2 0.204905 0.764041 -0.111889 11.00000 -1.20000 AFIX 0 C13 1 -0.086176 0.791589 -0.016502 11.00000 0.00860 0.01592 = 0.00987 0.00010 0.00280 -0.00080 C14 1 -0.151976 0.799690 0.021824 11.00000 0.00987 0.01552 = 0.01044 0.00009 0.00330 0.00042 C15 1 -0.252405 0.815877 -0.012921 11.00000 0.00952 0.02290 = 0.01411 0.00146 0.00397 0.00175 AFIX 43 H15 2 -0.296745 0.821359 0.012249 11.00000 -1.20000 AFIX 0 C16 1 -0.285343 0.823681 -0.085064 11.00000 0.00940 0.02441 = 0.01457 0.00146 0.00154 0.00002 AFIX 43 H16 2 -0.351861 0.834819 -0.108109 11.00000 -1.20000 AFIX 0 C17 1 -0.219508 0.814949 -0.123096 11.00000 0.01138 0.02997 = 0.01105 0.00171 0.00164 -0.00174 AFIX 43 H17 2 -0.242202 0.820160 -0.171391 11.00000 -1.20000 AFIX 0 C18 1 -0.120063 0.798486 -0.089175 11.00000 0.01070 0.02696 = 0.00996 0.00089 0.00279 -0.00128 AFIX 43 H18 2 -0.076175 0.792071 -0.114652 11.00000 -1.20000 AFIX 0 C19 1 0.464981 0.573780 0.132432 11.00000 0.01176 0.01682 = 0.01670 0.00262 0.00479 0.00258 AFIX 13 H19 2 0.468863 0.550965 0.179956 11.00000 -1.20000 AFIX 0 C20 1 0.397104 0.486060 0.083517 11.00000 0.01723 0.01775 = 0.02461 -0.00260 0.00537 0.00252 AFIX 137 H20A 2 0.390550 0.506069 0.036152 11.00000 -1.50000 H20B 2 0.333649 0.487801 0.090346 11.00000 -1.50000 H20C 2 0.424503 0.409244 0.093346 11.00000 -1.50000 AFIX 0 C21 1 0.569296 0.563666 0.126912 11.00000 0.01269 0.02569 = 0.02821 0.00606 0.00771 0.00591 AFIX 137 H21A 2 0.591862 0.484742 0.136143 11.00000 -1.50000 H21B 2 0.612566 0.614664 0.160270 11.00000 -1.50000 H21C 2 0.568683 0.585267 0.080872 11.00000 -1.50000 AFIX 0 C22 1 0.511830 0.816990 0.167724 11.00000 0.01131 0.01916 = 0.02105 0.00221 0.00097 -0.00237 AFIX 13 H22 2 0.569270 0.796968 0.153357 11.00000 -1.20000 AFIX 0 C23 1 0.538622 0.793019 0.245890 11.00000 0.01876 0.02527 = 0.02077 0.00070 -0.00364 -0.00233 AFIX 137 H23A 2 0.593249 0.841133 0.270421 11.00000 -1.50000 H23B 2 0.556141 0.712447 0.254765 11.00000 -1.50000 H23C 2 0.483285 0.810439 0.261521 11.00000 -1.50000 AFIX 0 C24 1 0.489145 0.946151 0.150626 11.00000 0.02124 0.01873 = 0.03020 0.00268 0.00066 -0.00516 AFIX 137 H24A 2 0.432916 0.968603 0.164008 11.00000 -1.50000 H24B 2 0.475594 0.958237 0.101530 11.00000 -1.50000 H24C 2 0.544722 0.992481 0.175635 11.00000 -1.50000 AFIX 0 C25 1 -0.111753 0.911333 0.159122 11.00000 0.01631 0.01557 = 0.01317 -0.00163 0.00613 0.00224 AFIX 13 H25 2 -0.077676 0.899977 0.208837 11.00000 -1.20000 AFIX 0 C26 1 -0.063474 1.016393 0.136247 11.00000 0.01968 0.01515 = 0.01751 -0.00201 0.00612 0.00062 AFIX 137 H26A 2 -0.094435 1.030390 0.087509 11.00000 -1.50000 H26B 2 0.005124 1.000830 0.144584 11.00000 -1.50000 H26C 2 -0.070820 1.083873 0.162298 11.00000 -1.50000 AFIX 0 C27 1 -0.218973 0.939367 0.152362 11.00000 0.01917 0.02380 = 0.02993 -0.00524 0.01316 0.00426 AFIX 137 H27A 2 -0.221586 1.008174 0.178774 11.00000 -1.50000 H27B 2 -0.247451 0.875143 0.169781 11.00000 -1.50000 H27C 2 -0.255072 0.952353 0.104293 11.00000 -1.50000 AFIX 0 C28 1 -0.171775 0.670077 0.138746 11.00000 0.01348 0.01735 = 0.01509 0.00040 0.00725 -0.00052 AFIX 13 H28 2 -0.237141 0.705253 0.128355 11.00000 -1.20000 AFIX 0 C29 1 -0.134709 0.645051 0.216947 11.00000 0.02587 0.02624 = 0.01594 0.00349 0.01065 -0.00241 AFIX 137 H29A 2 -0.178629 0.591628 0.228824 11.00000 -1.50000 H29B 2 -0.132021 0.716468 0.242234 11.00000 -1.50000 H29C 2 -0.070220 0.611354 0.228847 11.00000 -1.50000 AFIX 0 C30 1 -0.182648 0.558169 0.095944 11.00000 0.01780 0.01721 = 0.02303 -0.00265 0.00695 -0.00298 AFIX 137 H30A 2 -0.119724 0.521068 0.105532 11.00000 -1.50000 H30B 2 -0.207598 0.576730 0.047295 11.00000 -1.50000 H30C 2 -0.227450 0.506434 0.108127 11.00000 -1.50000 AFIX 0 C31 1 0.285502 0.854446 0.187783 11.00000 0.01303 0.02225 = 0.01578 -0.00292 0.00151 0.00160 C32 1 0.275497 0.614315 0.182021 11.00000 0.01198 0.02365 = 0.01516 0.00406 0.00597 0.00334 C33 1 0.066909 0.589642 0.154021 11.00000 0.01315 0.02030 = 0.01747 0.00456 0.00622 0.00272 C34 1 0.105336 0.803092 0.206308 11.00000 0.01423 0.02377 = 0.01276 -0.00003 0.00272 0.00206 H3 2 0.220550 0.934049 0.046788 11.00000 0.01900 H1 2 0.191374 0.579515 0.019261 11.00000 0.01809 H4 2 0.056434 0.941013 0.049836 11.00000 0.01387 H6 2 0.025937 0.595000 0.009622 11.00000 0.01297 HKLF 4 REM kth02 in P2(1)/c REM R1 = 0.0283 for 12872 Fo > 4sig(Fo) and 0.0421 for all 15800 data REM 403 parameters refined using 0 restraints END WGHT 0.0444 0.8524 REM Highest difference peak 0.824, deepest hole -0.609, 1-sigma level 0.095 Q1 1 -0.1335 0.7316 0.1213 11.00000 0.05 0.72 Q2 1 0.2824 0.7624 -0.0494 11.00000 0.05 0.65 Q3 1 0.4999 0.8833 0.1596 11.00000 0.05 0.61 Q4 1 0.4580 0.7693 -0.0416 11.00000 0.05 0.61 Q5 1 0.3495 0.7559 0.0071 11.00000 0.05 0.59 Q6 1 0.4350 0.6462 0.1241 11.00000 0.05 0.58 Q7 1 0.3905 0.7686 -0.1021 11.00000 0.05 0.58 Q8 1 0.4590 0.7516 0.1360 11.00000 0.05 0.58 Q9 1 0.3099 0.7725 -0.1013 11.00000 0.05 0.55 Q10 1 0.2408 0.7963 0.1314 11.00000 0.05 0.54 Q11 1 -0.2546 0.8203 -0.1059 11.00000 0.05 0.54 Q12 1 0.4331 0.7621 0.0113 11.00000 0.05 0.54 Q13 1 0.5271 0.8058 0.2085 11.00000 0.05 0.53 Q14 1 0.0429 0.7181 0.0207 11.00000 0.05 0.52 Q15 1 0.0502 0.8200 0.0323 11.00000 0.05 0.51 Q16 1 -0.2745 0.8204 -0.0511 11.00000 0.05 0.51 Q17 1 0.2650 0.6751 0.1207 11.00000 0.05 0.51 Q18 1 0.1995 0.8045 0.0327 11.00000 0.05 0.50 Q19 1 0.4300 0.5352 0.1092 11.00000 0.05 0.49 Q20 1 -0.1015 0.7855 -0.0517 11.00000 0.05 0.49 Q21 1 -0.2073 0.8096 0.0053 11.00000 0.05 0.49 Q22 1 0.0728 0.6586 0.1309 11.00000 0.05 0.49 Q23 1 0.2162 0.7197 0.1112 11.00000 0.05 0.48 Q24 1 0.2873 0.7903 0.1688 11.00000 0.05 0.47 Q25 1 -0.1717 0.8085 -0.1064 11.00000 0.05 0.46 Q26 1 0.1953 0.7084 0.0284 11.00000 0.05 0.46 Q27 1 0.2645 0.7539 0.0021 11.00000 0.05 0.45 Q28 1 -0.1209 0.7895 0.0027 11.00000 0.05 0.45 Q29 1 0.1041 0.7804 0.1152 11.00000 0.05 0.45 Q30 1 0.0632 0.8064 0.1295 11.00000 0.05 0.44 ; _shelx_res_checksum 84220 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Fe1 Fe 0.25863(2) 0.73789(2) 0.12705(2) 0.01027(4) Uani 1 1 d . . Fe2 Fe 0.06451(2) 0.73513(2) 0.12340(2) 0.00997(4) Uani 1 1 d . . P1 P 0.40933(2) 0.72247(2) 0.11797(2) 0.01202(5) Uani 1 1 d . . P2 P -0.09124(2) 0.77708(2) 0.11428(2) 0.01066(5) Uani 1 1 d . . O1 O 0.30232(7) 0.93305(9) 0.22546(5) 0.02788(19) Uani 1 1 d . . O2 O 0.29056(6) 0.53331(9) 0.21760(5) 0.02715(19) Uani 1 1 d . . O3 O 0.06893(7) 0.49399(8) 0.17183(5) 0.02513(17) Uani 1 1 d . . O4 O 0.12728(7) 0.84194(10) 0.26183(4) 0.02738(18) Uani 1 1 d . . C1 C 0.16946(6) 0.65351(8) 0.03139(5) 0.01194(14) Uani 1 1 d . . C2 C 0.21987(7) 0.75638(8) 0.02286(5) 0.01098(14) Uani 1 1 d . . C3 C 0.18781(6) 0.85956(8) 0.04858(4) 0.01111(13) Uani 1 1 d . . C4 C 0.08595(6) 0.86603(8) 0.05022(4) 0.01075(13) Uani 1 1 d . . C5 C 0.02029(6) 0.77305(8) 0.02060(5) 0.01048(14) Uani 1 1 d . . C6 C 0.06517(6) 0.66188(8) 0.02651(5) 0.01193(14) Uani 1 1 d . . C7 C 0.29694(7) 0.75766(8) -0.01260(5) 0.01226(14) Uani 1 1 d . . C8 C 0.39579(7) 0.75331(9) 0.02723(5) 0.01425(15) Uani 1 1 d . . C9 C 0.46879(8) 0.76539(10) -0.00522(6) 0.01927(19) Uani 1 1 d . . H9 H 0.5348 0.7655 0.0213 0.023 Uiso 1 1 calc R U C10 C 0.44218(8) 0.77721(10) -0.07715(6) 0.01993(19) Uani 1 1 d . . H10 H 0.4905 0.7869 -0.0987 0.024 Uiso 1 1 calc R U C11 C 0.34347(8) 0.77461(10) -0.11723(6) 0.01861(18) Uani 1 1 d . . H11 H 0.3263 0.7791 -0.1655 0.022 Uiso 1 1 calc R U C12 C 0.27077(8) 0.76525(10) -0.08518(5) 0.01606(17) Uani 1 1 d . . H12 H 0.2049 0.7640 -0.1119 0.019 Uiso 1 1 calc R U C13 C -0.08618(6) 0.79159(9) -0.01650(4) 0.01148(14) Uani 1 1 d . . C14 C -0.15198(6) 0.79969(9) 0.02182(5) 0.01191(14) Uani 1 1 d . . C15 C -0.25241(7) 0.81588(10) -0.01292(5) 0.01544(16) Uani 1 1 d . . H15 H -0.2967 0.8214 0.0122 0.019 Uiso 1 1 calc R U C16 C -0.28534(7) 0.82368(10) -0.08506(5) 0.01662(17) Uani 1 1 d . . H16 H -0.3519 0.8348 -0.1081 0.020 Uiso 1 1 calc R U C17 C -0.21951(7) 0.81495(11) -0.12310(5) 0.01788(18) Uani 1 1 d . . H17 H -0.2422 0.8202 -0.1714 0.021 Uiso 1 1 calc R U C18 C -0.12006(7) 0.79849(10) -0.08918(5) 0.01596(16) Uani 1 1 d . . H18 H -0.0762 0.7921 -0.1147 0.019 Uiso 1 1 calc R U C19 C 0.46498(7) 0.57378(9) 0.13243(5) 0.01501(16) Uani 1 1 d . . H19 H 0.4689 0.5510 0.1800 0.018 Uiso 1 1 calc R U C20 C 0.39710(8) 0.48606(10) 0.08352(6) 0.02012(18) Uani 1 1 d . . H20A H 0.3906 0.5061 0.0362 0.030 Uiso 1 1 calc R U H20B H 0.3336 0.4878 0.0903 0.030 Uiso 1 1 calc R U H20C H 0.4245 0.4092 0.0933 0.030 Uiso 1 1 calc R U C21 C 0.56930(7) 0.56367(11) 0.12691(6) 0.0219(2) Uani 1 1 d . . H21A H 0.5919 0.4847 0.1361 0.033 Uiso 1 1 calc R U H21B H 0.6126 0.6147 0.1603 0.033 Uiso 1 1 calc R U H21C H 0.5687 0.5853 0.0809 0.033 Uiso 1 1 calc R U C22 C 0.51183(7) 0.81699(10) 0.16772(6) 0.01809(17) Uani 1 1 d . . H22 H 0.5693 0.7970 0.1534 0.022 Uiso 1 1 calc R U C23 C 0.53862(9) 0.79302(11) 0.24589(6) 0.0238(2) Uani 1 1 d . . H23A H 0.5932 0.8411 0.2704 0.036 Uiso 1 1 calc R U H23B H 0.5561 0.7124 0.2548 0.036 Uiso 1 1 calc R U H23C H 0.4833 0.8104 0.2615 0.036 Uiso 1 1 calc R U C24 C 0.48915(9) 0.94615(11) 0.15063(7) 0.0251(2) Uani 1 1 d . . H24A H 0.4329 0.9686 0.1640 0.038 Uiso 1 1 calc R U H24B H 0.4756 0.9582 0.1015 0.038 Uiso 1 1 calc R U H24C H 0.5447 0.9925 0.1756 0.038 Uiso 1 1 calc R U C25 C -0.11175(7) 0.91133(9) 0.15912(5) 0.01466(15) Uani 1 1 d . . H25 H -0.0777 0.9000 0.2088 0.018 Uiso 1 1 calc R U C26 C -0.06347(8) 1.01639(9) 0.13625(5) 0.01736(16) Uani 1 1 d . . H26A H -0.0944 1.0304 0.0875 0.026 Uiso 1 1 calc R U H26B H 0.0051 1.0008 0.1446 0.026 Uiso 1 1 calc R U H26C H -0.0708 1.0839 0.1623 0.026 Uiso 1 1 calc R U C27 C -0.21897(8) 0.93937(11) 0.15236(6) 0.0230(2) Uani 1 1 d . . H27A H -0.2216 1.0082 0.1788 0.035 Uiso 1 1 calc R U H27B H -0.2475 0.8751 0.1698 0.035 Uiso 1 1 calc R U H27C H -0.2551 0.9524 0.1043 0.035 Uiso 1 1 calc R U C28 C -0.17177(7) 0.67008(9) 0.13875(5) 0.01466(15) Uani 1 1 d . . H28 H -0.2371 0.7053 0.1284 0.018 Uiso 1 1 calc R U C29 C -0.13471(9) 0.64505(11) 0.21695(5) 0.0217(2) Uani 1 1 d . . H29A H -0.1786 0.5916 0.2288 0.033 Uiso 1 1 calc R U H29B H -0.1320 0.7165 0.2422 0.033 Uiso 1 1 calc R U H29C H -0.0702 0.6114 0.2288 0.033 Uiso 1 1 calc R U C30 C -0.18265(8) 0.55817(10) 0.09594(6) 0.01921(18) Uani 1 1 d . . H30A H -0.1197 0.5211 0.1055 0.029 Uiso 1 1 calc R U H30B H -0.2076 0.5767 0.0473 0.029 Uiso 1 1 calc R U H30C H -0.2274 0.5064 0.1081 0.029 Uiso 1 1 calc R U C31 C 0.28550(7) 0.85445(10) 0.18778(5) 0.01769(17) Uani 1 1 d . . C32 C 0.27550(7) 0.61431(10) 0.18202(5) 0.01652(17) Uani 1 1 d . . C33 C 0.06691(7) 0.58964(10) 0.15402(5) 0.01664(17) Uani 1 1 d . . C34 C 0.10534(7) 0.80309(10) 0.20631(5) 0.01725(17) Uani 1 1 d . . H3 H 0.2206(11) 0.9340(15) 0.0468(8) 0.019(4) Uiso 1 1 d . . H1 H 0.1914(11) 0.5795(15) 0.0193(8) 0.018(4) Uiso 1 1 d . . H4 H 0.0564(10) 0.9410(14) 0.0498(7) 0.014(3) Uiso 1 1 d . . H6 H 0.0259(10) 0.5950(14) 0.0096(7) 0.013(3) Uiso 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 0.00821(6) 0.01312(7) 0.00908(6) -0.00013(4) 0.00210(4) 0.00129(4) Fe2 0.00869(6) 0.01286(7) 0.00850(6) 0.00066(4) 0.00288(4) 0.00085(4) P1 0.00787(9) 0.01452(11) 0.01296(10) 0.00168(7) 0.00221(7) 0.00028(7) P2 0.00979(9) 0.01369(11) 0.00934(9) -0.00016(7) 0.00416(7) 0.00067(7) O1 0.0260(4) 0.0303(5) 0.0247(4) -0.0134(3) 0.0040(3) -0.0011(3) O2 0.0210(4) 0.0349(5) 0.0285(4) 0.0185(4) 0.0120(3) 0.0101(3) O3 0.0231(4) 0.0220(4) 0.0316(4) 0.0115(3) 0.0105(3) 0.0030(3) O4 0.0262(4) 0.0399(5) 0.0134(3) -0.0065(3) 0.0022(3) 0.0015(4) C1 0.0113(3) 0.0127(4) 0.0121(3) -0.0012(3) 0.0040(3) 0.0008(3) C2 0.0094(3) 0.0139(4) 0.0100(3) 0.0003(3) 0.0035(3) 0.0005(3) C3 0.0089(3) 0.0127(4) 0.0114(3) 0.0002(3) 0.0026(2) 0.0000(3) C4 0.0092(3) 0.0126(4) 0.0104(3) 0.0002(3) 0.0030(2) 0.0005(3) C5 0.0087(3) 0.0140(4) 0.0090(3) 0.0001(2) 0.0029(2) -0.0007(3) C6 0.0115(3) 0.0130(4) 0.0117(3) -0.0011(3) 0.0042(3) -0.0014(3) C7 0.0107(3) 0.0149(4) 0.0124(3) 0.0015(3) 0.0053(3) 0.0015(3) C8 0.0107(3) 0.0168(4) 0.0156(4) 0.0031(3) 0.0046(3) 0.0000(3) C9 0.0110(4) 0.0259(5) 0.0228(5) 0.0072(4) 0.0079(3) 0.0014(3) C10 0.0181(4) 0.0231(5) 0.0233(5) 0.0078(4) 0.0133(4) 0.0042(4) C11 0.0193(4) 0.0227(5) 0.0175(4) 0.0050(3) 0.0111(3) 0.0063(3) C12 0.0136(4) 0.0226(5) 0.0131(4) 0.0019(3) 0.0057(3) 0.0039(3) C13 0.0086(3) 0.0159(4) 0.0099(3) 0.0001(3) 0.0028(2) -0.0008(3) C14 0.0099(3) 0.0155(4) 0.0104(3) 0.0001(3) 0.0033(3) 0.0004(3) C15 0.0095(3) 0.0229(5) 0.0141(4) 0.0015(3) 0.0040(3) 0.0018(3) C16 0.0094(3) 0.0244(5) 0.0146(4) 0.0015(3) 0.0015(3) 0.0000(3) C17 0.0114(3) 0.0300(5) 0.0110(3) 0.0017(3) 0.0016(3) -0.0017(3) C18 0.0107(3) 0.0270(5) 0.0100(3) 0.0009(3) 0.0028(3) -0.0013(3) C19 0.0118(3) 0.0168(4) 0.0167(4) 0.0026(3) 0.0048(3) 0.0026(3) C20 0.0172(4) 0.0177(4) 0.0246(5) -0.0026(4) 0.0054(3) 0.0025(3) C21 0.0127(4) 0.0257(5) 0.0282(5) 0.0061(4) 0.0077(4) 0.0059(3) C22 0.0113(4) 0.0192(4) 0.0210(4) 0.0022(3) 0.0010(3) -0.0024(3) C23 0.0188(4) 0.0253(5) 0.0208(5) 0.0007(4) -0.0036(4) -0.0023(4) C24 0.0212(5) 0.0187(5) 0.0302(5) 0.0027(4) 0.0007(4) -0.0052(4) C25 0.0163(4) 0.0156(4) 0.0132(3) -0.0016(3) 0.0061(3) 0.0022(3) C26 0.0197(4) 0.0152(4) 0.0175(4) -0.0020(3) 0.0061(3) 0.0006(3) C27 0.0192(4) 0.0238(5) 0.0299(5) -0.0052(4) 0.0132(4) 0.0043(4) C28 0.0135(3) 0.0174(4) 0.0151(4) 0.0004(3) 0.0072(3) -0.0005(3) C29 0.0259(5) 0.0262(5) 0.0159(4) 0.0035(4) 0.0106(4) -0.0024(4) C30 0.0178(4) 0.0172(4) 0.0230(5) -0.0026(3) 0.0069(3) -0.0030(3) C31 0.0130(4) 0.0222(5) 0.0158(4) -0.0029(3) 0.0015(3) 0.0016(3) C32 0.0120(3) 0.0236(5) 0.0152(4) 0.0041(3) 0.0060(3) 0.0033(3) C33 0.0132(4) 0.0203(4) 0.0175(4) 0.0046(3) 0.0062(3) 0.0027(3) C34 0.0142(4) 0.0238(5) 0.0128(4) 0.0000(3) 0.0027(3) 0.0021(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C32 Fe1 C31 102.20(5) C32 Fe1 C2 132.80(4) C31 Fe1 C2 125.00(5) C32 Fe1 C3 159.55(4) C31 Fe1 C3 88.40(4) C2 Fe1 C3 40.20(4) C32 Fe1 C1 97.41(4) C31 Fe1 C1 152.58(4) C2 Fe1 C1 39.29(4) C3 Fe1 C1 67.49(3) C32 Fe1 P1 92.32(3) C31 Fe1 P1 96.23(3) C2 Fe1 P1 83.27(3) C3 Fe1 P1 103.99(2) C1 Fe1 P1 101.97(2) C32 Fe1 Fe2 87.03(3) C31 Fe1 Fe2 91.61(3) C2 Fe1 Fe2 91.37(3) C3 Fe1 Fe2 75.10(2) C1 Fe1 Fe2 70.33(2) P1 Fe1 Fe2 172.085(10) C34 Fe2 C33 96.82(5) C34 Fe2 C5 141.43(5) C33 Fe2 C5 121.73(4) C34 Fe2 C6 161.02(4) C33 Fe2 C6 86.81(4) C5 Fe2 C6 39.74(4) C34 Fe2 C4 105.15(4) C33 Fe2 C4 152.35(4) C5 Fe2 C4 39.24(3) C6 Fe2 C4 67.05(3) C34 Fe2 P2 90.68(3) C33 Fe2 P2 98.19(3) C5 Fe2 P2 83.21(3) C6 Fe2 P2 107.29(3) C4 Fe2 P2 98.12(2) C34 Fe2 Fe1 86.28(3) C33 Fe2 Fe1 95.21(3) C5 Fe2 Fe1 91.00(3) C6 Fe2 Fe1 74.83(2) C4 Fe2 Fe1 70.14(2) P2 Fe2 Fe1 166.522(9) C8 P1 C22 104.64(5) C8 P1 C19 104.05(5) C22 P1 C19 102.85(5) C8 P1 Fe1 105.30(3) C22 P1 Fe1 122.25(4) C19 P1 Fe1 115.90(3) C14 P2 C28 103.27(4) C14 P2 C25 106.59(4) C28 P2 C25 102.37(4) C14 P2 Fe2 105.26(3) C28 P2 Fe2 121.54(3) C25 P2 Fe2 116.33(3) C2 C1 C6 118.77(8) C2 C1 Fe1 63.89(5) C6 C1 Fe1 109.49(6) C1 C2 C3 114.39(8) C1 C2 C7 123.07(8) C3 C2 C7 122.49(8) C1 C2 Fe1 76.81(5) C3 C2 Fe1 73.86(5) C7 C2 Fe1 119.87(6) C2 C3 C4 118.93(8) C2 C3 Fe1 65.94(5) C4 C3 Fe1 105.32(6) C5 C4 C3 118.83(8) C5 C4 Fe2 63.84(5) C3 C4 Fe2 109.09(6) C6 C5 C4 114.57(8) C6 C5 C13 122.50(8) C4 C5 C13 122.88(8) C6 C5 Fe2 74.34(5) C4 C5 Fe2 76.92(5) C13 C5 Fe2 119.56(6) C5 C6 C1 119.31(8) C5 C6 Fe2 65.91(5) C1 C6 Fe2 104.91(6) C8 C7 C12 120.09(9) C8 C7 C2 119.46(9) C12 C7 C2 120.45(8) C7 C8 C9 119.76(10) C7 C8 P1 111.17(7) C9 C8 P1 128.96(8) C10 C9 C8 119.72(10) C9 C10 C11 120.37(9) C12 C11 C10 120.08(10) C11 C12 C7 119.80(10) C14 C13 C18 120.30(8) C14 C13 C5 119.40(8) C18 C13 C5 120.28(8) C13 C14 C15 119.61(8) C13 C14 P2 111.75(6) C15 C14 P2 128.52(7) C16 C15 C14 119.73(8) C15 C16 C17 120.46(8) C18 C17 C16 120.21(9) C17 C18 C13 119.69(9) C20 C19 C21 109.92(9) C20 C19 P1 110.20(7) C21 C19 P1 115.78(7) C23 C22 C24 111.97(10) C23 C22 P1 111.01(7) C24 C22 P1 111.53(7) C26 C25 C27 109.95(9) C26 C25 P2 110.60(6) C27 C25 P2 115.86(7) C30 C28 C29 111.63(9) C30 C28 P2 111.62(6) C29 C28 P2 110.75(7) O1 C31 Fe1 177.64(10) O2 C32 Fe1 177.01(9) O3 C33 Fe2 177.69(10) O4 C34 Fe2 174.92(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 C32 1.7707(11) Fe1 C31 1.7747(11) Fe1 C2 2.0151(9) Fe1 C3 2.1199(9) Fe1 C1 2.1849(9) Fe1 P1 2.2272(3) Fe1 Fe2 2.7562(2) Fe2 C34 1.7746(10) Fe2 C33 1.7767(11) Fe2 C5 2.0222(9) Fe2 C6 2.1328(9) Fe2 C4 2.1944(9) Fe2 P2 2.2315(3) P1 C8 1.8177(10) P1 C22 1.8508(10) P1 C19 1.8669(10) P2 C14 1.8184(9) P2 C28 1.8526(10) P2 C25 1.8557(10) O1 C31 1.1563(13) O2 C32 1.1536(13) O3 C33 1.1524(13) O4 C34 1.1565(13) C1 C2 1.4212(13) C1 C6 1.4680(12) C2 C3 1.4246(13) C2 C7 1.4896(13) C3 C4 1.4701(12) C4 C5 1.4251(13) C5 C6 1.4162(13) C5 C13 1.4905(12) C7 C8 1.3952(14) C7 C12 1.3993(14) C8 C9 1.4015(14) C9 C10 1.3902(16) C10 C11 1.3943(16) C11 C12 1.3893(14) C13 C14 1.3951(12) C13 C18 1.3987(13) C14 C15 1.4030(13) C15 C16 1.3890(13) C16 C17 1.3915(14) C17 C18 1.3881(13) C19 C20 1.5293(15) C19 C21 1.5354(14) C22 C23 1.5302(16) C22 C24 1.5333(16) C25 C26 1.5301(15) C25 C27 1.5319(14) C28 C30 1.5287(15) C28 C29 1.5301(14)