#------------------------------------------------------------------------------ #$Date: 2019-10-12 03:58:18 +0300 (Sat, 12 Oct 2019) $ #$Revision: 219306 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/13/7701356.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_7701356 loop_ _publ_author_name 'Shimamura, Takehiko' 'Maeno, Yuki' 'Kubo, Kazuyuki' 'Kume, Shoko' 'Greco, Claudio' 'Mizuta, Tsutomu' _publ_section_title ; Protonation and Electrochemical Properties of Bisphosphide Diiron Hexacarbonyl Complex Bearing Amino Groups on the Bridge ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT03427G _journal_year 2019 _chemical_formula_sum 'C24 H26 Fe2 N2 O6 P2' _chemical_formula_weight 612.11 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_update_record ; 2019-08-22 deposited with the CCDC. 2019-10-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.151(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.352(3) _cell_length_b 12.479(3) _cell_length_c 17.703(4) _cell_measurement_reflns_used 1408 _cell_measurement_temperature 100.0(2) _cell_measurement_theta_max 27.9233 _cell_measurement_theta_min 2.3809 _cell_volume 2607.4(11) _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_collection 'APEX2(Bruker AXS)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_molecular_graphics 'XSHELL V6.3.1(Bruker AXS)' _computing_publication_material 'Generate Report (Bruker AXS)' _diffrn_ambient_temperature 100.0(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker D8 goniometer' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator 'multilayered conforcal mirror' _diffrn_radiation_type MoKa _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 15432 _diffrn_reflns_theta_full 27.90 _diffrn_reflns_theta_max 27.90 _diffrn_reflns_theta_min 1.79 _diffrn_source 'rotating-anode X-ray tube' _diffrn_source_type 'Bruker Turbo X-ray Source' _exptl_absorpt_coefficient_mu 1.277 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_crystal_colour 'clear light yellow' _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.122 _exptl_crystal_size_mid 0.113 _exptl_crystal_size_min 0.087 _refine_diff_density_max 0.443 _refine_diff_density_min -0.198 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 6180 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.0267P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.0669 _reflns_number_gt 5526 _reflns_number_total 6180 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt03427g2.cif _cod_data_source_block I _cod_original_cell_volume 2607.4(9) _cod_database_code 7701356 _shelx_res_file ; TITL 20141002shimamura01 in P2(1)/n CELL 0.71073 12.35150 12.47880 17.70330 90.0000 107.1510 90.0000 ZERR 4.00 0.00250 0.00250 0.00350 0.0000 0.0022 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O P Fe UNIT 96 104 8 24 8 8 L.S. 10 ACTA 50 BOND $h FMAP 2 PLAN 20 SIZE 0.122 0.113 0.087 TEMP -173 WGHT 0.032200 1.026700 FVAR 0.10825 MOLE 1 FE1 6 0.865798 0.770237 1.028219 11.00000 0.00943 0.01168 = 0.01206 0.00060 0.00086 0.00099 FE2 6 0.754547 0.636985 0.919741 11.00000 0.01410 0.00947 = 0.01315 -0.00057 0.00367 0.00057 P1 5 0.755196 0.814842 0.910603 11.00000 0.00952 0.01005 = 0.01072 -0.00011 0.00248 0.00022 P2 5 0.705549 0.688280 1.024967 11.00000 0.01191 0.01088 = 0.01107 0.00113 0.00183 -0.00013 O7 4 0.530411 0.608877 0.805801 11.00000 0.02108 0.03808 = 0.02624 -0.00725 0.00067 -0.00755 O8 4 0.825775 0.422304 0.984435 11.00000 0.05886 0.01830 = 0.04697 0.01159 0.02563 0.01476 O9 4 0.923336 0.620615 0.832570 11.00000 0.02867 0.02345 = 0.03209 0.00086 0.01774 0.00670 O10 4 0.857982 0.952260 1.130263 11.00000 0.01564 0.02631 = 0.03060 -0.01222 0.00645 -0.00084 O11 4 0.993690 0.609360 1.141273 11.00000 0.02415 0.03142 = 0.03400 0.01525 0.00118 0.00859 O12 4 1.069097 0.808495 0.976941 11.00000 0.01638 0.03026 = 0.02969 0.00485 0.00868 0.00301 N1 3 0.811761 0.875299 0.846759 11.00000 0.01294 0.01306 = 0.01322 0.00018 0.00464 -0.00221 N2 3 0.707747 0.606474 1.100351 11.00000 0.01888 0.01421 = 0.01159 0.00253 0.00188 -0.00238 C1 1 0.573055 0.763433 1.002850 11.00000 0.01156 0.01340 = 0.01167 -0.00199 0.00189 -0.00071 C2 1 0.494071 0.734943 1.040633 11.00000 0.01742 0.01815 = 0.01392 0.00234 0.00481 -0.00085 AFIX 43 H2 2 0.511389 0.678552 1.078349 11.00000 -1.20000 AFIX 0 C3 1 0.388554 0.787194 1.024786 11.00000 0.01600 0.02590 = 0.01931 0.00065 0.00960 -0.00188 AFIX 43 H3 2 0.335606 0.765217 1.051224 11.00000 -1.20000 AFIX 0 C4 1 0.362302 0.869212 0.971594 11.00000 0.01234 0.02360 = 0.01870 -0.00212 0.00516 0.00159 AFIX 43 H4 2 0.291673 0.905067 0.961941 11.00000 -1.20000 AFIX 0 C5 1 0.410649 0.985564 0.874686 11.00000 0.01186 0.01758 = 0.01813 -0.00025 0.00212 0.00398 AFIX 43 H5 2 0.340852 1.022413 0.866632 11.00000 -1.20000 AFIX 0 C6 1 0.481871 1.014415 0.832215 11.00000 0.01600 0.01472 = 0.01689 0.00356 0.00146 0.00307 AFIX 43 H6 2 0.461651 1.070902 0.794700 11.00000 -1.20000 AFIX 0 C7 1 0.585457 0.960169 0.844182 11.00000 0.01333 0.01445 = 0.01387 0.00076 0.00337 -0.00084 AFIX 43 H7 2 0.633448 0.979374 0.813157 11.00000 -1.20000 AFIX 0 C8 1 0.619323 0.879666 0.899867 11.00000 0.00960 0.01226 = 0.01127 -0.00183 0.00093 -0.00067 C9 1 0.545967 0.847401 0.944882 11.00000 0.01203 0.01164 = 0.00957 -0.00253 0.00131 -0.00075 C10 1 0.439478 0.901277 0.930694 11.00000 0.01228 0.01599 = 0.01284 -0.00232 0.00265 -0.00008 C11 1 0.884383 0.970604 0.869719 11.00000 0.01426 0.01702 = 0.02162 0.00260 0.00128 -0.00437 AFIX 23 H11A 2 0.952641 0.960178 0.852101 11.00000 -1.20000 H11B 2 0.909869 0.974963 0.928153 11.00000 -1.20000 AFIX 0 C12 1 0.830822 1.077519 0.837443 11.00000 0.02046 0.01647 = 0.02012 0.00181 0.00046 -0.00542 AFIX 137 H12A 2 0.795129 1.071491 0.780299 11.00000 -1.50000 H12B 2 0.889457 1.133084 0.847999 11.00000 -1.50000 H12C 2 0.773428 1.096753 0.863271 11.00000 -1.50000 AFIX 0 C13 1 0.769997 0.851240 0.761755 11.00000 0.03040 0.01778 = 0.01559 -0.00250 0.01012 -0.00263 AFIX 23 H13A 2 0.719210 0.909858 0.734764 11.00000 -1.20000 H13B 2 0.724783 0.784462 0.754174 11.00000 -1.20000 AFIX 0 C14 1 0.864245 0.838060 0.723405 11.00000 0.06084 0.02572 = 0.03819 0.00603 0.03714 0.00927 AFIX 137 H14A 2 0.904959 0.906042 0.726176 11.00000 -1.50000 H14B 2 0.831616 0.817211 0.667955 11.00000 -1.50000 H14C 2 0.916939 0.782429 0.751351 11.00000 -1.50000 AFIX 0 C15 1 0.754516 0.643910 1.182730 11.00000 0.02376 0.02056 = 0.01325 0.00223 0.00184 -0.00272 AFIX 23 H15A 2 0.791885 0.713933 1.182028 11.00000 -1.20000 H15B 2 0.813680 0.592694 1.211280 11.00000 -1.20000 AFIX 0 C16 1 0.669404 0.656487 1.229094 11.00000 0.03264 0.03163 = 0.01625 0.00168 0.00718 0.00097 AFIX 137 H16A 2 0.615661 0.713620 1.205434 11.00000 -1.50000 H16B 2 0.709442 0.674936 1.284052 11.00000 -1.50000 H16C 2 0.628257 0.589010 1.227676 11.00000 -1.50000 AFIX 0 C17 1 0.647764 0.503013 1.088551 11.00000 0.02393 0.01558 = 0.01872 0.00374 0.00338 -0.00396 AFIX 23 H17A 2 0.627995 0.483354 1.031933 11.00000 -1.20000 H17B 2 0.576196 0.511072 1.102435 11.00000 -1.20000 AFIX 0 C18 1 0.716942 0.412587 1.137751 11.00000 0.04225 0.01709 = 0.02465 0.00606 0.00614 0.00105 AFIX 137 H18A 2 0.790518 0.407781 1.127454 11.00000 -1.50000 H18B 2 0.676145 0.344703 1.123439 11.00000 -1.50000 H18C 2 0.728643 0.427134 1.193995 11.00000 -1.50000 AFIX 0 C19 1 0.618996 0.616576 0.850017 11.00000 0.02307 0.01650 = 0.01958 -0.00400 0.00917 -0.00323 C20 1 0.796423 0.505671 0.960661 11.00000 0.02946 0.01814 = 0.02436 0.00041 0.01293 0.00216 C21 1 0.855992 0.628301 0.864911 11.00000 0.02055 0.01115 = 0.01893 -0.00095 0.00399 0.00208 C22 1 0.862415 0.881943 1.089778 11.00000 0.00793 0.02006 = 0.01729 0.00045 0.00139 -0.00083 C23 1 0.942889 0.671830 1.098246 11.00000 0.01448 0.02097 = 0.02134 0.00033 0.00305 -0.00144 C24 1 0.989747 0.794922 0.996180 11.00000 0.01578 0.01554 = 0.01644 0.00088 0.00097 0.00247 HKLF 4 REM 20141002shimamura01 in P2(1)/n REM R1 = 0.0250 for 5526 Fo > 4sig(Fo) and 0.0293 for all 6180 data REM 329 parameters refined using 0 restraints END WGHT 0.0320 1.0271 REM Highest difference peak 0.443, deepest hole -0.198, 1-sigma level 0.065 Q1 1 0.8238 0.6330 0.9089 11.00000 0.05 0.44 Q2 1 0.7001 0.6428 1.0628 11.00000 0.05 0.43 Q3 1 0.4970 0.8797 0.9396 11.00000 0.05 0.42 Q4 1 0.7756 0.8509 0.8741 11.00000 0.05 0.41 Q5 1 0.6353 0.7242 1.0157 11.00000 0.05 0.40 Q6 1 0.7985 0.8621 0.8067 11.00000 0.05 0.38 Q7 1 0.6800 0.8436 0.9064 11.00000 0.05 0.37 Q8 1 0.5371 0.7590 1.0276 11.00000 0.05 0.37 Q9 1 0.5692 0.8032 0.9715 11.00000 0.05 0.37 Q10 1 0.4326 0.9459 0.9062 11.00000 0.05 0.37 Q11 1 0.8420 0.8405 1.0438 11.00000 0.05 0.36 Q12 1 0.3812 0.8166 0.9891 11.00000 0.05 0.35 Q13 1 0.7035 0.6557 1.2006 11.00000 0.05 0.34 Q14 1 0.8481 0.7779 0.9736 11.00000 0.05 0.34 Q15 1 0.7946 0.7939 1.0273 11.00000 0.05 0.33 Q16 1 0.5788 0.8555 0.9211 11.00000 0.05 0.33 Q17 1 0.3982 0.8649 0.9416 11.00000 0.05 0.33 Q18 1 0.6112 0.9341 0.8845 11.00000 0.05 0.33 Q19 1 0.7231 0.6326 1.1384 11.00000 0.05 0.32 Q20 1 0.7223 0.6408 0.9855 11.00000 0.05 0.31 ; _shelx_res_checksum 71495 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_posn _atom_site_occupancy Fe Fe1 0.86580(2) 0.77024(2) 1.02822(2) 0.01155(6) Uani d . . 1 Fe Fe2 0.75455(2) 0.63699(2) 0.91974(2) 0.01231(6) Uani d . . 1 P P1 0.75520(3) 0.81484(3) 0.91060(2) 0.01020(8) Uani d . . 1 P P2 0.70555(3) 0.68828(3) 1.02497(2) 0.01162(8) Uani d . . 1 O O7 0.53041(10) 0.60888(11) 0.80580(7) 0.0298(3) Uani d . . 1 O O8 0.82578(13) 0.42230(10) 0.98443(8) 0.0392(3) Uani d . . 1 O O9 0.92334(10) 0.62061(10) 0.83257(7) 0.0262(3) Uani d . . 1 O O10 0.85798(9) 0.95226(10) 1.13026(7) 0.0243(3) Uani d . . 1 O O11 0.99369(10) 0.60936(11) 1.14127(8) 0.0314(3) Uani d . . 1 O O12 1.06910(9) 0.80849(10) 0.97694(7) 0.0250(3) Uani d . . 1 N N1 0.81176(10) 0.87530(10) 0.84676(7) 0.0129(2) Uani d . . 1 N N2 0.70775(11) 0.60647(10) 1.10035(7) 0.0155(3) Uani d . . 1 C C1 0.57306(12) 0.76343(11) 1.00285(8) 0.0125(3) Uani d . . 1 C C2 0.49407(13) 0.73494(12) 1.04063(9) 0.0165(3) Uani d . . 1 H H2 0.5114 0.6786 1.0783 0.02 Uiso calc U R 1 C C3 0.38855(13) 0.78719(13) 1.02479(9) 0.0195(3) Uani d . . 1 H H3 0.3356 0.7652 1.0512 0.023 Uiso calc U R 1 C C4 0.36230(12) 0.86921(13) 0.97159(9) 0.0181(3) Uani d . . 1 H H4 0.2917 0.9051 0.9619 0.022 Uiso calc U R 1 C C5 0.41065(12) 0.98556(12) 0.87469(9) 0.0163(3) Uani d . . 1 H H5 0.3409 1.0224 0.8666 0.02 Uiso calc U R 1 C C6 0.48187(12) 1.01441(12) 0.83221(9) 0.0166(3) Uani d . . 1 H H6 0.4617 1.0709 0.7947 0.02 Uiso calc U R 1 C C7 0.58546(12) 0.96017(12) 0.84418(8) 0.0140(3) Uani d . . 1 H H7 0.6334 0.9794 0.8132 0.017 Uiso calc U R 1 C C8 0.61932(11) 0.87967(11) 0.89987(8) 0.0115(3) Uani d . . 1 C C9 0.54597(12) 0.84740(11) 0.94488(8) 0.0115(3) Uani d . . 1 C C10 0.43948(12) 0.90128(12) 0.93069(8) 0.0139(3) Uani d . . 1 C C11 0.88438(13) 0.97060(12) 0.86972(9) 0.0185(3) Uani d . . 1 H H11A 0.9526 0.9602 0.8521 0.022 Uiso calc U R 1 H H11B 0.9099 0.975 0.9282 0.022 Uiso calc U R 1 C C12 0.83082(13) 1.07752(12) 0.83744(9) 0.0202(3) Uani d . . 1 H H12A 0.7951 1.0715 0.7803 0.03 Uiso calc U R 1 H H12B 0.8895 1.1331 0.848 0.03 Uiso calc U R 1 H H12C 0.7734 1.0968 0.8633 0.03 Uiso calc U R 1 C C13 0.77000(14) 0.85124(13) 0.76176(9) 0.0205(3) Uani d . . 1 H H13A 0.7192 0.9099 0.7348 0.025 Uiso calc U R 1 H H13B 0.7248 0.7845 0.7542 0.025 Uiso calc U R 1 C C14 0.86424(19) 0.83806(16) 0.72340(12) 0.0367(5) Uani d . . 1 H H14A 0.905 0.906 0.7262 0.055 Uiso calc U R 1 H H14B 0.8316 0.8172 0.668 0.055 Uiso calc U R 1 H H14C 0.9169 0.7824 0.7514 0.055 Uiso calc U R 1 C C15 0.75452(14) 0.64391(13) 1.18273(9) 0.0200(3) Uani d . . 1 H H15A 0.7919 0.7139 1.182 0.024 Uiso calc U R 1 H H15B 0.8137 0.5927 1.2113 0.024 Uiso calc U R 1 C C16 0.66940(16) 0.65649(15) 1.22909(10) 0.0268(4) Uani d . . 1 H H16A 0.6157 0.7136 1.2054 0.04 Uiso calc U R 1 H H16B 0.7094 0.6749 1.2841 0.04 Uiso calc U R 1 H H16C 0.6283 0.589 1.2277 0.04 Uiso calc U R 1 C C17 0.64776(14) 0.50301(12) 1.08855(9) 0.0200(3) Uani d . . 1 H H17A 0.628 0.4834 1.0319 0.024 Uiso calc U R 1 H H17B 0.5762 0.5111 1.1024 0.024 Uiso calc U R 1 C C18 0.71694(17) 0.41259(14) 1.13775(10) 0.0288(4) Uani d . . 1 H H18A 0.7905 0.4078 1.1275 0.043 Uiso calc U R 1 H H18B 0.6761 0.3447 1.1234 0.043 Uiso calc U R 1 H H18C 0.7286 0.4271 1.194 0.043 Uiso calc U R 1 C C19 0.61900(14) 0.61658(12) 0.85002(9) 0.0191(3) Uani d . . 1 C C20 0.79642(14) 0.50567(13) 0.96066(10) 0.0229(3) Uani d . . 1 C C21 0.85599(13) 0.62830(12) 0.86491(9) 0.0173(3) Uani d . . 1 C C22 0.86242(12) 0.88194(12) 1.08978(9) 0.0156(3) Uani d . . 1 C C23 0.94289(13) 0.67183(13) 1.09825(9) 0.0194(3) Uani d . . 1 C C24 0.98975(13) 0.79492(12) 0.99618(9) 0.0167(3) Uani d . . 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.00943(10) 0.01168(11) 0.01206(10) 0.00099(7) 0.00086(8) 0.00060(7) Fe2 0.01410(11) 0.00947(10) 0.01315(10) 0.00057(7) 0.00367(8) -0.00057(7) P1 0.00952(16) 0.01005(17) 0.01072(16) 0.00022(13) 0.00248(13) -0.00011(13) P2 0.01191(17) 0.01088(17) 0.01107(17) -0.00013(13) 0.00183(13) 0.00113(13) O7 0.0211(6) 0.0381(7) 0.0262(6) -0.0076(5) 0.0007(5) -0.0073(6) O8 0.0589(9) 0.0183(7) 0.0470(8) 0.0148(6) 0.0256(7) 0.0116(6) O9 0.0287(6) 0.0235(6) 0.0321(7) 0.0067(5) 0.0177(5) 0.0009(5) O10 0.0156(5) 0.0263(6) 0.0306(6) -0.0008(5) 0.0064(5) -0.0122(5) O11 0.0241(6) 0.0314(7) 0.0340(7) 0.0086(5) 0.0012(5) 0.0153(6) O12 0.0164(6) 0.0303(7) 0.0297(6) 0.0030(5) 0.0087(5) 0.0048(5) N1 0.0129(6) 0.0131(6) 0.0132(6) -0.0022(5) 0.0046(5) 0.0002(5) N2 0.0189(6) 0.0142(6) 0.0116(6) -0.0024(5) 0.0019(5) 0.0025(5) C1 0.0116(7) 0.0134(7) 0.0117(6) -0.0007(5) 0.0019(5) -0.0020(5) C2 0.0174(7) 0.0181(7) 0.0139(7) -0.0008(6) 0.0048(6) 0.0023(6) C3 0.0160(7) 0.0259(8) 0.0193(8) -0.0019(6) 0.0096(6) 0.0007(6) C4 0.0123(7) 0.0236(8) 0.0187(7) 0.0016(6) 0.0052(6) -0.0021(6) C5 0.0119(7) 0.0176(7) 0.0181(7) 0.0040(6) 0.0021(5) -0.0002(6) C6 0.0160(7) 0.0147(7) 0.0169(7) 0.0031(6) 0.0015(6) 0.0036(6) C7 0.0133(7) 0.0144(7) 0.0139(7) -0.0008(5) 0.0034(5) 0.0008(5) C8 0.0096(6) 0.0123(6) 0.0113(6) -0.0007(5) 0.0009(5) -0.0018(5) C9 0.0120(6) 0.0116(6) 0.0096(6) -0.0008(5) 0.0013(5) -0.0025(5) C10 0.0123(6) 0.0160(7) 0.0128(6) -0.0001(5) 0.0026(5) -0.0023(5) C11 0.0143(7) 0.0170(7) 0.0216(8) -0.0044(6) 0.0013(6) 0.0026(6) C12 0.0205(8) 0.0165(7) 0.0201(8) -0.0054(6) 0.0005(6) 0.0018(6) C13 0.0304(9) 0.0178(8) 0.0156(7) -0.0026(6) 0.0101(6) -0.0025(6) C14 0.0608(13) 0.0257(9) 0.0382(10) 0.0093(9) 0.0371(10) 0.0060(8) C15 0.0238(8) 0.0206(8) 0.0132(7) -0.0027(6) 0.0018(6) 0.0022(6) C16 0.0326(9) 0.0316(9) 0.0163(8) 0.0010(8) 0.0072(7) 0.0017(7) C17 0.0239(8) 0.0156(7) 0.0187(7) -0.0040(6) 0.0034(6) 0.0037(6) C18 0.0422(10) 0.0171(8) 0.0246(8) 0.0010(7) 0.0061(7) 0.0061(7) C19 0.0231(8) 0.0165(7) 0.0196(7) -0.0032(6) 0.0092(6) -0.0040(6) C20 0.0295(9) 0.0181(8) 0.0244(8) 0.0022(7) 0.0129(7) 0.0004(7) C21 0.0205(7) 0.0111(7) 0.0189(7) 0.0021(6) 0.0040(6) -0.0009(6) C22 0.0079(6) 0.0201(7) 0.0173(7) -0.0008(5) 0.0014(5) 0.0005(6) C23 0.0145(7) 0.0210(8) 0.0213(8) -0.0014(6) 0.0030(6) 0.0003(6) C24 0.0158(7) 0.0155(7) 0.0164(7) 0.0025(6) 0.0010(6) 0.0009(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C22 Fe1 C23 102.45(7) C22 Fe1 C24 103.52(7) C23 Fe1 C24 90.42(7) C22 Fe1 P1 105.17(5) C23 Fe1 P1 151.36(5) C24 Fe1 P1 90.40(5) C22 Fe1 P2 101.29(5) C23 Fe1 P2 89.43(5) C24 Fe1 P2 154.61(5) P1 Fe1 P2 77.950(17) C22 Fe1 Fe2 148.21(5) C23 Fe1 Fe2 97.40(5) C24 Fe1 Fe2 100.88(5) P1 Fe1 Fe2 54.410(15) P2 Fe1 Fe2 54.028(13) C19 Fe2 C21 106.21(7) C19 Fe2 C20 104.35(8) C21 Fe2 C20 89.95(7) C19 Fe2 P2 100.95(5) C21 Fe2 P2 151.24(5) C20 Fe2 P2 92.40(5) C19 Fe2 P1 96.60(5) C21 Fe2 P1 90.16(5) C20 Fe2 P1 158.13(6) P2 Fe2 P1 77.337(16) C19 Fe2 Fe1 141.80(5) C21 Fe2 Fe1 97.83(5) C20 Fe2 Fe1 104.91(6) P2 Fe2 Fe1 53.937(15) P1 Fe2 Fe1 53.454(14) N1 P1 C8 106.53(6) N1 P1 Fe1 119.16(5) C8 P1 Fe1 120.48(5) N1 P1 Fe2 120.65(5) C8 P1 Fe2 115.31(5) Fe1 P1 Fe2 72.135(13) N2 P2 C1 106.68(7) N2 P2 Fe1 117.18(5) C1 P2 Fe1 120.42(5) N2 P2 Fe2 123.35(5) C1 P2 Fe2 114.70(5) Fe1 P2 Fe2 72.035(15) C13 N1 C11 116.65(12) C13 N1 P1 120.58(10) C11 N1 P1 121.28(10) C17 N2 C15 116.83(12) C17 N2 P2 122.17(10) C15 N2 P2 120.26(10) C2 C1 C9 119.00(13) C2 C1 P2 118.69(11) C9 C1 P2 122.24(11) C1 C2 C3 121.86(14) C1 C2 H2 119.1 C3 C2 H2 119.1 C4 C3 C2 120.15(14) C4 C3 H3 119.9 C2 C3 H3 119.9 C3 C4 C10 120.47(14) C3 C4 H4 119.8 C10 C4 H4 119.8 C6 C5 C10 120.80(13) C6 C5 H5 119.6 C10 C5 H5 119.6 C5 C6 C7 119.72(14) C5 C6 H6 120.1 C7 C6 H6 120.1 C8 C7 C6 121.82(14) C8 C7 H7 119.1 C6 C7 H7 119.1 C7 C8 C9 119.58(13) C7 C8 P1 118.20(11) C9 C8 P1 122.18(10) C8 C9 C10 118.06(13) C8 C9 C1 123.48(13) C10 C9 C1 118.46(13) C4 C10 C5 120.00(13) C4 C10 C9 120.02(13) C5 C10 C9 119.97(13) N1 C11 C12 116.22(12) N1 C11 H11A 108.2 C12 C11 H11A 108.2 N1 C11 H11B 108.2 C12 C11 H11B 108.2 H11A C11 H11B 107.4 C11 C12 H12A 109.5 C11 C12 H12B 109.5 H12A C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 N1 C13 C14 113.30(15) N1 C13 H13A 108.9 C14 C13 H13A 108.9 N1 C13 H13B 108.9 C14 C13 H13B 108.9 H13A C13 H13B 107.7 C13 C14 H14A 109.5 C13 C14 H14B 109.5 H14A C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 N2 C15 C16 115.74(13) N2 C15 H15A 108.3 C16 C15 H15A 108.3 N2 C15 H15B 108.3 C16 C15 H15B 108.3 H15A C15 H15B 107.4 C15 C16 H16A 109.5 C15 C16 H16B 109.5 H16A C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 N2 C17 C18 113.22(13) N2 C17 H17A 108.9 C18 C17 H17A 108.9 N2 C17 H17B 108.9 C18 C17 H17B 108.9 H17A C17 H17B 107.7 C17 C18 H18A 109.5 C17 C18 H18B 109.5 H18A C18 H18B 109.5 C17 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 O7 C19 Fe2 176.42(15) O8 C20 Fe2 177.05(15) O9 C21 Fe2 177.24(14) O10 C22 Fe1 177.97(14) O11 C23 Fe1 178.07(15) O12 C24 Fe1 178.43(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 C22 1.7775(16) Fe1 C23 1.8043(16) Fe1 C24 1.8090(16) Fe1 P1 2.1986(5) Fe1 P2 2.2135(6) Fe1 Fe2 2.6048(4) Fe2 C19 1.7812(16) Fe2 C21 1.8003(16) Fe2 C20 1.8046(17) Fe2 P2 2.2161(5) Fe2 P1 2.2255(6) P1 N1 1.6735(13) P1 C8 1.8218(15) P2 N2 1.6741(13) P2 C1 1.8257(15) O7 C19 1.1463(19) O8 C20 1.141(2) O9 C21 1.1445(19) O10 C22 1.1445(19) O11 C23 1.1401(19) O12 C24 1.141(2) N1 C13 1.4707(19) N1 C11 1.4728(19) N2 C17 1.4725(19) N2 C15 1.4772(19) C1 C2 1.382(2) C1 C9 1.435(2) C2 C3 1.410(2) C2 H2 0.95 C3 C4 1.364(2) C3 H3 0.95 C4 C10 1.414(2) C4 H4 0.95 C5 C6 1.363(2) C5 C10 1.417(2) C5 H5 0.95 C6 C7 1.407(2) C6 H6 0.95 C7 C8 1.383(2) C7 H7 0.95 C8 C9 1.4297(19) C9 C10 1.432(2) C11 C12 1.524(2) C11 H11A 0.99 C11 H11B 0.99 C12 H12A 0.98 C12 H12B 0.98 C12 H12C 0.98 C13 C14 1.520(2) C13 H13A 0.99 C13 H13B 0.99 C14 H14A 0.98 C14 H14B 0.98 C14 H14C 0.98 C15 C16 1.521(2) C15 H15A 0.99 C15 H15B 0.99 C16 H16A 0.98 C16 H16B 0.98 C16 H16C 0.98 C17 C18 1.524(2) C17 H17A 0.99 C17 H17B 0.99 C18 H18A 0.98 C18 H18B 0.98 C18 H18C 0.98