#------------------------------------------------------------------------------ #$Date: 2019-11-17 09:59:28 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229233 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045407.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_7045407 loop_ _publ_author_name 'Lin, Hsiu-Jung' 'Lutz, Sean' 'O'Kane, Catherine' 'Zeller, Matthias' 'Chen, Chun-Hsing' 'Al Assil, Talal' 'Lee, Wei-Tsung' _publ_section_title ; Synthesis and characterization of an iron complex bearing a hemilabile NNN-pincer for catalytic hydrosilylation of organic carbonyl compounds. ; _journal_issue 10 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 3243 _journal_page_last 3247 _journal_paper_doi 10.1039/c7dt04928e _journal_volume 47 _journal_year 2018 _chemical_formula_sum 'C68 H86 Fe2 N10' _chemical_formula_weight 1155.16 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-01-06 deposited with the CCDC. 2018-01-26 downloaded from the CCDC. ; _cell_angle_alpha 108.574(3) _cell_angle_beta 101.586(4) _cell_angle_gamma 98.224(4) _cell_formula_units_Z 1 _cell_length_a 10.6257(7) _cell_length_b 11.7461(7) _cell_length_c 13.3730(9) _cell_measurement_reflns_used 9471 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.5407 _cell_measurement_theta_min 2.2448 _cell_volume 1510.91(18) _computing_cell_refinement 'SAINT V8.34A (Bruker, 2014)' _computing_data_collection 'Apex2 v2014.11 (Bruker, 2014)' _computing_data_reduction 'SAINT V8.34A (Bruker, 2014)' _computing_structure_refinement ; SHELXL-2014/7 (Sheldrick, 2014), SHELXLE Rev714 (H\"ubschle et al., 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker AXS D8 Quest CMOS diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'laterally graded multilayer (Goebel) mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_unetI/netI 0.0497 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 75126 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.282 _diffrn_reflns_theta_min 2.246 _diffrn_source 'I-mu-S microsource X-ray tube' _exptl_absorpt_coefficient_mu 0.530 _exptl_absorpt_correction_T_max 0.746070 _exptl_absorpt_correction_T_min 0.491463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2012)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.270 _exptl_crystal_description plate _exptl_crystal_F_000 616 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.682 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 374 _refine_ls_number_reflns 7475 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0566 _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^)+(0.0331P)^2^+4.0051P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1283 _refine_ls_wR_factor_ref 0.1383 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6811 _reflns_number_total 7475 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04928e2.cif _cod_data_source_block Quest15mz333_0m _cod_depositor_comments 'Adding full bibliography for 7045406--7045408.cif.' _cod_original_cell_volume 1510.91(17) _cod_database_code 7045407 _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_res_file ; Quest15mz333_0m.res created by SHELXL-2014/7 TITL Quest15mz333_0m in P-1 CELL 0.71073 10.6257 11.7461 13.3730 108.574 101.586 98.224 ZERR 1.00 0.0007 0.0007 0.0009 0.003 0.004 0.004 LATT 1 SFAC C H Fe N UNIT 68 86 2 10 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.160 L.S. 14 BOND $H ACTA CONF FMAP 2 PLAN 20 SHEL 99 0.75 OMIT 0 1 1 WGHT 0.033100 4.005100 BASF 0.20757 FVAR 0.55714 FE1 3 1.041776 0.099383 -0.024433 11.00000 0.01184 0.01036 = 0.00898 0.00356 0.00339 0.00339 N1 4 1.104262 0.142518 0.315270 11.00000 0.01172 0.01435 = 0.01024 0.00475 0.00067 0.00498 N2 4 1.045565 0.151370 0.218447 11.00000 0.00974 0.01140 = 0.00846 0.00579 0.00284 0.00365 N3 4 0.968642 0.241804 0.038713 11.00000 0.01118 0.01128 = 0.00657 0.00345 0.00199 0.00447 N4 4 1.046889 0.279575 -0.152012 11.00000 0.01118 0.01067 = 0.01119 0.00445 0.00380 0.00478 N5 4 1.109736 0.197523 -0.118777 11.00000 0.01066 0.00948 = 0.00999 0.00259 0.00306 0.00347 C1 1 1.083320 0.079319 0.128916 11.00000 0.01131 0.00992 = 0.01561 0.00348 0.00705 0.00369 C2 1 1.172804 0.022548 0.177937 11.00000 0.01076 0.01299 = 0.01032 0.00395 0.00277 0.00509 AFIX 43 H2 2 1.219279 -0.033521 0.141283 11.00000 -1.20000 AFIX 0 C3 1 1.181316 0.063380 0.290626 11.00000 0.00897 0.01181 = 0.01192 0.00345 0.00043 0.00073 C4 1 1.259741 0.029377 0.380559 11.00000 0.01512 0.01497 = 0.01079 0.00356 -0.00070 0.00640 C5 1 1.329742 0.146030 0.479324 11.00000 0.01801 0.01900 = 0.01424 0.00157 -0.00502 0.00297 AFIX 137 H5A 2 1.387044 0.201130 0.457102 11.00000 -1.50000 H5B 2 1.382952 0.123901 0.536169 11.00000 -1.50000 H5C 2 1.264113 0.187855 0.508028 11.00000 -1.50000 AFIX 0 C6 1 1.165586 -0.053349 0.414536 11.00000 0.03189 0.02100 = 0.01732 0.01018 -0.00487 -0.00568 AFIX 137 H6A 2 1.119798 -0.127906 0.351254 11.00000 -1.50000 H6B 2 1.100896 -0.008918 0.441858 11.00000 -1.50000 H6C 2 1.215711 -0.076253 0.472276 11.00000 -1.50000 AFIX 0 C7 1 1.360791 -0.039996 0.338318 11.00000 0.02971 0.03471 = 0.02276 0.00771 0.00074 0.02513 AFIX 137 H7A 2 1.315236 -0.113930 0.274351 11.00000 -1.50000 H7B 2 1.409757 -0.063940 0.395837 11.00000 -1.50000 H7C 2 1.422165 0.013407 0.317685 11.00000 -1.50000 AFIX 0 C8 1 0.956723 0.230777 0.219088 11.00000 0.00884 0.00933 = 0.00960 0.00242 0.00030 0.00202 C9 1 0.905643 0.276879 0.308607 11.00000 0.01210 0.01336 = 0.00976 0.00574 0.00252 0.00395 AFIX 43 H9 2 0.933072 0.255850 0.371268 11.00000 -1.20000 AFIX 0 C10 1 0.815209 0.353188 0.309205 11.00000 0.01136 0.01280 = 0.01270 0.00607 0.00640 0.00347 C11 1 0.775450 0.384385 0.216846 11.00000 0.00929 0.01483 = 0.01278 0.00691 0.00408 0.00462 AFIX 43 H11 2 0.711583 0.433060 0.214388 11.00000 -1.20000 AFIX 0 C12 1 0.829535 0.344058 0.128455 11.00000 0.00830 0.00907 = 0.01100 0.00367 0.00110 -0.00029 C13 1 0.920812 0.267369 0.129819 11.00000 0.00913 0.01099 = 0.01043 0.00275 0.00152 0.00195 C14 1 0.912050 0.306200 -0.020072 11.00000 0.00926 0.01026 = 0.01060 0.00270 0.00141 0.00337 C15 1 0.820062 0.366143 0.026430 11.00000 0.01054 0.01042 = 0.00957 0.00191 0.00286 0.00062 C16 1 0.744406 0.427937 -0.027326 11.00000 0.00893 0.01188 = 0.01252 0.00250 0.00098 0.00320 AFIX 43 H16 2 0.682646 0.467829 0.004317 11.00000 -1.20000 AFIX 0 C17 1 0.760132 0.430614 -0.127236 11.00000 0.01026 0.01212 = 0.00996 0.00351 -0.00164 0.00129 C18 1 0.859123 0.378965 -0.168442 11.00000 0.01295 0.01365 = 0.00916 0.00428 0.00187 0.00231 AFIX 43 H18 2 0.872833 0.384872 -0.234828 11.00000 -1.20000 AFIX 0 C19 1 0.937456 0.319613 -0.115169 11.00000 0.00842 0.01209 = 0.01002 0.00211 0.00272 0.00243 C20 1 0.756789 0.398813 0.407503 11.00000 0.01662 0.01606 = 0.01274 0.00714 0.00686 0.00692 C21 1 0.833818 0.379340 0.508294 11.00000 0.03364 0.03741 = 0.01260 0.01185 0.01346 0.01989 AFIX 137 H21A 2 0.826816 0.290973 0.492755 11.00000 -1.50000 H21B 2 0.797256 0.413810 0.570176 11.00000 -1.50000 H21C 2 0.926670 0.420779 0.526441 11.00000 -1.50000 AFIX 0 C22 1 0.613579 0.326916 0.376434 11.00000 0.02014 0.03215 = 0.02897 0.01336 0.01643 0.00843 AFIX 137 H22A 2 0.565148 0.332286 0.308127 11.00000 -1.50000 H22B 2 0.571992 0.362188 0.434767 11.00000 -1.50000 H22C 2 0.612168 0.240374 0.366572 11.00000 -1.50000 AFIX 0 C23 1 0.758238 0.536458 0.437923 11.00000 0.03118 0.02050 = 0.02027 0.00587 0.01450 0.01249 AFIX 137 H23A 2 0.705542 0.550300 0.375557 11.00000 -1.50000 H23B 2 0.849163 0.583290 0.457083 11.00000 -1.50000 H23C 2 0.720937 0.563757 0.500570 11.00000 -1.50000 AFIX 0 C24 1 0.669047 0.484271 -0.196481 11.00000 0.01227 0.01595 = 0.01080 0.00462 0.00024 0.00319 C25 1 0.574560 0.543796 -0.134824 11.00000 0.02189 0.03224 = 0.01694 0.01265 0.00429 0.01632 AFIX 137 H25A 2 0.519093 0.578509 -0.179948 11.00000 -1.50000 H25B 2 0.625371 0.609550 -0.066197 11.00000 -1.50000 H25C 2 0.518719 0.481440 -0.118851 11.00000 -1.50000 AFIX 0 C26 1 0.748213 0.582894 -0.225193 11.00000 0.01814 0.01842 = 0.02151 0.01135 0.00135 0.00296 AFIX 137 H26A 2 0.814407 0.549242 -0.259918 11.00000 -1.50000 H26B 2 0.792264 0.654066 -0.158388 11.00000 -1.50000 H26C 2 0.688779 0.608672 -0.275701 11.00000 -1.50000 AFIX 0 C27 1 0.587433 0.379355 -0.301822 11.00000 0.01588 0.02238 = 0.01446 0.00719 -0.00086 -0.00022 AFIX 137 H27A 2 0.532900 0.413067 -0.348521 11.00000 -1.50000 H27B 2 0.530572 0.319893 -0.283517 11.00000 -1.50000 H27C 2 0.646683 0.338075 -0.340731 11.00000 -1.50000 AFIX 0 C28 1 1.110355 0.324161 -0.214212 11.00000 0.01587 0.01523 = 0.01620 0.00845 0.00691 0.00341 AFIX 43 H28 2 1.085881 0.382053 -0.246091 11.00000 -1.20000 AFIX 0 C29 1 1.216623 0.270977 -0.223246 11.00000 0.01794 0.01623 = 0.02006 0.00858 0.01046 0.00476 AFIX 43 H29 2 1.279031 0.283999 -0.262597 11.00000 -1.20000 AFIX 0 C30 1 1.213859 0.193383 -0.162251 11.00000 0.00905 0.01261 = 0.01524 0.00282 0.00595 0.00022 C31 1 1.307608 0.110743 -0.148548 11.00000 0.01221 0.01383 = 0.01828 0.00488 0.00905 0.00420 C32 1 1.451123 0.184420 -0.113943 11.00000 0.01350 0.02284 = 0.03167 0.00938 0.01159 0.00388 AFIX 137 H32A 2 1.511150 0.128850 -0.110819 11.00000 -1.50000 H32B 2 1.468487 0.248609 -0.041703 11.00000 -1.50000 H32C 2 1.465044 0.222677 -0.167292 11.00000 -1.50000 AFIX 0 C33 1 1.283671 0.008021 -0.261090 11.00000 0.02953 0.01725 = 0.02473 0.00408 0.01163 0.00859 AFIX 137 H33A 2 1.308475 0.044306 -0.312896 11.00000 -1.50000 H33B 2 1.190223 -0.033676 -0.288029 11.00000 -1.50000 H33C 2 1.337132 -0.051720 -0.253728 11.00000 -1.50000 AFIX 0 C34 1 1.288082 0.053751 -0.063201 11.00000 0.01537 0.02529 = 0.02544 0.01451 0.01075 0.00814 AFIX 137 H34A 2 1.199901 -0.000059 -0.087533 11.00000 -1.50000 H34B 2 1.297265 0.119346 0.006721 11.00000 -1.50000 H34C 2 1.354561 0.005421 -0.054067 11.00000 -1.50000 AFIX 0 HKLF 5 REM Quest15mz333_0m in P-1 REM R1 = 0.0566 for 6811 Fo > 4sig(Fo) and 0.0678 for all 7475 data REM 374 parameters refined using 0 restraints END WGHT 0.0331 4.0025 REM Highest difference peak 0.682, deepest hole -0.952, 1-sigma level 0.101 Q1 1 1.0484 0.0877 0.0437 11.00000 0.05 0.68 Q2 1 1.0195 0.0602 -0.0961 11.00000 0.05 0.62 Q3 1 1.0414 0.1133 -0.0891 11.00000 0.05 0.59 Q4 1 0.8189 0.3682 0.0743 11.00000 0.05 0.51 Q5 1 1.1103 0.2088 -0.0494 11.00000 0.05 0.49 Q6 1 0.9386 0.3191 -0.0561 11.00000 0.05 0.48 Q7 1 1.0458 0.1149 0.1609 11.00000 0.05 0.47 Q8 1 0.7424 0.4019 -0.0910 11.00000 0.05 0.46 Q9 1 0.8640 0.3366 -0.0012 11.00000 0.05 0.46 Q10 1 1.2137 0.0748 0.2514 11.00000 0.05 0.45 Q11 1 0.7088 0.5354 -0.2003 11.00000 0.05 0.41 Q12 1 1.1181 0.1008 0.0980 11.00000 0.05 0.40 Q13 1 1.2997 0.1036 -0.0961 11.00000 0.05 0.40 Q14 1 1.1621 0.0214 0.2302 11.00000 0.05 0.40 Q15 1 1.0736 0.1967 0.1271 11.00000 0.05 0.39 Q16 1 1.4586 0.0538 -0.1102 11.00000 0.05 0.39 Q17 1 0.8055 0.3761 0.2672 11.00000 0.05 0.39 Q18 1 1.0316 -0.0196 -0.0461 11.00000 0.05 0.38 Q19 1 1.2083 -0.0039 0.4043 11.00000 0.05 0.38 Q20 1 0.9507 0.2574 0.1772 11.00000 0.05 0.38 ; _shelx_res_checksum 73739 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 Fe1 Fe 1.04178(4) 0.09938(4) -0.02443(4) 0.01017(10) Uani 1 1 d . . N1 N 1.1043(3) 0.1425(2) 0.3153(2) 0.0121(5) Uani 1 1 d . . N2 N 1.0456(3) 0.1514(2) 0.21845(19) 0.0091(4) Uani 1 1 d . . N3 N 0.9686(3) 0.2418(2) 0.03871(19) 0.0095(4) Uani 1 1 d . . N4 N 1.0469(3) 0.2796(2) -0.15201(19) 0.0105(4) Uani 1 1 d . . N5 N 1.1097(2) 0.1975(2) -0.1188(2) 0.0101(5) Uani 1 1 d . . C1 C 1.0833(3) 0.0793(3) 0.1289(2) 0.0119(5) Uani 1 1 d . . C2 C 1.1728(3) 0.0225(3) 0.1779(2) 0.0111(5) Uani 1 1 d . . H2 H 1.2193 -0.0335 0.1413 0.013 Uiso 1 1 calc R U C3 C 1.1813(3) 0.0634(3) 0.2906(2) 0.0116(5) Uani 1 1 d . . C4 C 1.2597(3) 0.0294(3) 0.3806(2) 0.0142(6) Uani 1 1 d . . C5 C 1.3297(3) 0.1460(3) 0.4793(3) 0.0197(7) Uani 1 1 d . . H5A H 1.3870 0.2011 0.4571 0.030 Uiso 1 1 calc R U H5B H 1.3830 0.1239 0.5362 0.030 Uiso 1 1 calc R U H5C H 1.2641 0.1879 0.5080 0.030 Uiso 1 1 calc R U C6 C 1.1656(4) -0.0533(3) 0.4145(3) 0.0256(8) Uani 1 1 d . . H6A H 1.1198 -0.1279 0.3513 0.038 Uiso 1 1 calc R U H6B H 1.1009 -0.0089 0.4419 0.038 Uiso 1 1 calc R U H6C H 1.2157 -0.0763 0.4723 0.038 Uiso 1 1 calc R U C7 C 1.3608(4) -0.0400(4) 0.3383(3) 0.0287(8) Uani 1 1 d . . H7A H 1.3152 -0.1139 0.2744 0.043 Uiso 1 1 calc R U H7B H 1.4098 -0.0639 0.3958 0.043 Uiso 1 1 calc R U H7C H 1.4222 0.0134 0.3177 0.043 Uiso 1 1 calc R U C8 C 0.9567(3) 0.2308(2) 0.2191(2) 0.0098(5) Uani 1 1 d . . C9 C 0.9056(3) 0.2769(3) 0.3086(2) 0.0113(5) Uani 1 1 d . . H9 H 0.9331 0.2558 0.3713 0.014 Uiso 1 1 calc R U C10 C 0.8152(3) 0.3532(3) 0.3092(2) 0.0113(5) Uani 1 1 d . . C11 C 0.7754(3) 0.3844(3) 0.2168(2) 0.0114(5) Uani 1 1 d . . H11 H 0.7116 0.4331 0.2144 0.014 Uiso 1 1 calc R U C12 C 0.8295(3) 0.3441(3) 0.1285(2) 0.0099(5) Uani 1 1 d . . C13 C 0.9208(3) 0.2674(3) 0.1298(2) 0.0106(5) Uani 1 1 d . . C14 C 0.9121(3) 0.3062(3) -0.0201(2) 0.0104(5) Uani 1 1 d . . C15 C 0.8201(3) 0.3661(3) 0.0264(2) 0.0107(5) Uani 1 1 d . . C16 C 0.7444(3) 0.4279(3) -0.0273(2) 0.0118(5) Uani 1 1 d . . H16 H 0.6826 0.4678 0.0043 0.014 Uiso 1 1 calc R U C17 C 0.7601(3) 0.4306(3) -0.1272(2) 0.0117(5) Uani 1 1 d . . C18 C 0.8591(3) 0.3790(3) -0.1684(2) 0.0121(5) Uani 1 1 d . . H18 H 0.8728 0.3849 -0.2348 0.015 Uiso 1 1 calc R U C19 C 0.9375(3) 0.3196(3) -0.1152(2) 0.0106(5) Uani 1 1 d . . C20 C 0.7568(3) 0.3988(3) 0.4075(2) 0.0138(6) Uani 1 1 d . . C21 C 0.8338(4) 0.3793(4) 0.5083(3) 0.0247(7) Uani 1 1 d . . H21A H 0.8268 0.2910 0.4928 0.037 Uiso 1 1 calc R U H21B H 0.7973 0.4138 0.5702 0.037 Uiso 1 1 calc R U H21C H 0.9267 0.4208 0.5264 0.037 Uiso 1 1 calc R U C22 C 0.6136(3) 0.3269(4) 0.3764(3) 0.0247(7) Uani 1 1 d . . H22A H 0.5651 0.3323 0.3081 0.037 Uiso 1 1 calc R U H22B H 0.5720 0.3622 0.4348 0.037 Uiso 1 1 calc R U H22C H 0.6122 0.2404 0.3666 0.037 Uiso 1 1 calc R U C23 C 0.7582(4) 0.5365(3) 0.4379(3) 0.0224(7) Uani 1 1 d . . H23A H 0.7055 0.5503 0.3756 0.034 Uiso 1 1 calc R U H23B H 0.8492 0.5833 0.4571 0.034 Uiso 1 1 calc R U H23C H 0.7209 0.5638 0.5006 0.034 Uiso 1 1 calc R U C24 C 0.6690(3) 0.4843(3) -0.1965(2) 0.0135(6) Uani 1 1 d . . C25 C 0.5746(3) 0.5438(3) -0.1348(3) 0.0217(7) Uani 1 1 d . . H25A H 0.5191 0.5785 -0.1799 0.033 Uiso 1 1 calc R U H25B H 0.6254 0.6096 -0.0662 0.033 Uiso 1 1 calc R U H25C H 0.5187 0.4814 -0.1189 0.033 Uiso 1 1 calc R U C26 C 0.7482(3) 0.5829(3) -0.2252(3) 0.0190(6) Uani 1 1 d . . H26A H 0.8144 0.5492 -0.2599 0.029 Uiso 1 1 calc R U H26B H 0.7923 0.6541 -0.1584 0.029 Uiso 1 1 calc R U H26C H 0.6888 0.6087 -0.2757 0.029 Uiso 1 1 calc R U C27 C 0.5874(3) 0.3794(3) -0.3018(3) 0.0187(6) Uani 1 1 d . . H27A H 0.5329 0.4131 -0.3485 0.028 Uiso 1 1 calc R U H27B H 0.5306 0.3199 -0.2835 0.028 Uiso 1 1 calc R U H27C H 0.6467 0.3381 -0.3407 0.028 Uiso 1 1 calc R U C28 C 1.1104(3) 0.3242(3) -0.2142(3) 0.0147(6) Uani 1 1 d . . H28 H 1.0859 0.3821 -0.2461 0.018 Uiso 1 1 calc R U C29 C 1.2166(3) 0.2710(3) -0.2232(3) 0.0166(6) Uani 1 1 d . . H29 H 1.2790 0.2840 -0.2626 0.020 Uiso 1 1 calc R U C30 C 1.2139(3) 0.1934(3) -0.1623(2) 0.0127(6) Uani 1 1 d . . C31 C 1.3076(3) 0.1107(3) -0.1485(3) 0.0141(6) Uani 1 1 d . . C32 C 1.4511(3) 0.1844(3) -0.1139(3) 0.0219(7) Uani 1 1 d . . H32A H 1.5111 0.1288 -0.1108 0.033 Uiso 1 1 calc R U H32B H 1.4685 0.2486 -0.0417 0.033 Uiso 1 1 calc R U H32C H 1.4650 0.2227 -0.1673 0.033 Uiso 1 1 calc R U C33 C 1.2837(4) 0.0080(3) -0.2611(3) 0.0236(7) Uani 1 1 d . . H33A H 1.3085 0.0443 -0.3129 0.035 Uiso 1 1 calc R U H33B H 1.1902 -0.0337 -0.2880 0.035 Uiso 1 1 calc R U H33C H 1.3371 -0.0517 -0.2537 0.035 Uiso 1 1 calc R U C34 C 1.2881(3) 0.0538(3) -0.0632(3) 0.0195(7) Uani 1 1 d . . H34A H 1.1999 -0.0001 -0.0875 0.029 Uiso 1 1 calc R U H34B H 1.2973 0.1193 0.0067 0.029 Uiso 1 1 calc R U H34C H 1.3546 0.0054 -0.0541 0.029 Uiso 1 1 calc R U 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 0.01184(19) 0.01036(19) 0.00898(19) 0.00356(14) 0.00339(16) 0.00339(16) N1 0.0117(12) 0.0144(12) 0.0102(12) 0.0048(9) 0.0007(9) 0.0050(10) N2 0.0097(10) 0.0114(10) 0.0085(11) 0.0058(9) 0.0028(9) 0.0036(9) N3 0.0112(11) 0.0113(11) 0.0066(10) 0.0034(8) 0.0020(9) 0.0045(9) N4 0.0112(11) 0.0107(11) 0.0112(11) 0.0045(9) 0.0038(10) 0.0048(10) N5 0.0107(11) 0.0095(11) 0.0100(11) 0.0026(9) 0.0031(9) 0.0035(9) C1 0.0113(13) 0.0099(12) 0.0156(14) 0.0035(11) 0.0071(11) 0.0037(10) C2 0.0108(13) 0.0130(13) 0.0103(13) 0.0040(11) 0.0028(10) 0.0051(11) C3 0.0090(13) 0.0118(13) 0.0119(13) 0.0034(11) 0.0004(10) 0.0007(10) C4 0.0151(14) 0.0150(14) 0.0108(13) 0.0036(11) -0.0007(11) 0.0064(11) C5 0.0180(15) 0.0190(15) 0.0142(15) 0.0016(12) -0.0050(12) 0.0030(12) C6 0.0319(19) 0.0210(16) 0.0173(16) 0.0102(14) -0.0049(14) -0.0057(14) C7 0.0297(19) 0.035(2) 0.0228(18) 0.0077(15) 0.0007(15) 0.0251(17) C8 0.0088(11) 0.0093(12) 0.0096(12) 0.0024(10) 0.0003(10) 0.0020(10) C9 0.0121(13) 0.0134(13) 0.0098(13) 0.0057(11) 0.0025(11) 0.0040(11) C10 0.0114(13) 0.0128(13) 0.0127(13) 0.0061(11) 0.0064(11) 0.0035(11) C11 0.0093(13) 0.0148(13) 0.0128(13) 0.0069(11) 0.0041(11) 0.0046(11) C12 0.0083(12) 0.0091(12) 0.0110(13) 0.0037(10) 0.0011(10) -0.0003(10) C13 0.0091(12) 0.0110(13) 0.0104(13) 0.0028(10) 0.0015(10) 0.0020(10) C14 0.0093(12) 0.0103(12) 0.0106(13) 0.0027(10) 0.0014(10) 0.0034(10) C15 0.0105(13) 0.0104(12) 0.0096(13) 0.0019(10) 0.0029(10) 0.0006(10) C16 0.0089(13) 0.0119(13) 0.0125(13) 0.0025(11) 0.0010(10) 0.0032(10) C17 0.0103(13) 0.0121(13) 0.0100(13) 0.0035(11) -0.0016(10) 0.0013(10) C18 0.0129(13) 0.0137(13) 0.0092(13) 0.0043(11) 0.0019(11) 0.0023(11) C19 0.0084(13) 0.0121(12) 0.0100(13) 0.0021(10) 0.0027(10) 0.0024(10) C20 0.0166(14) 0.0161(14) 0.0127(14) 0.0071(12) 0.0069(11) 0.0069(11) C21 0.0336(19) 0.037(2) 0.0126(15) 0.0119(15) 0.0135(14) 0.0199(17) C22 0.0201(17) 0.0322(19) 0.0290(18) 0.0134(15) 0.0164(15) 0.0084(14) C23 0.0312(19) 0.0205(16) 0.0203(17) 0.0059(14) 0.0145(14) 0.0125(14) C24 0.0123(13) 0.0159(14) 0.0108(13) 0.0046(11) 0.0002(11) 0.0032(11) C25 0.0219(17) 0.0322(19) 0.0169(16) 0.0126(14) 0.0043(13) 0.0163(15) C26 0.0181(15) 0.0184(15) 0.0215(16) 0.0113(13) 0.0014(13) 0.0030(12) C27 0.0159(15) 0.0224(16) 0.0145(15) 0.0072(13) -0.0009(12) -0.0002(12) C28 0.0159(14) 0.0152(14) 0.0162(14) 0.0084(12) 0.0069(12) 0.0034(12) C29 0.0179(15) 0.0162(14) 0.0201(15) 0.0086(12) 0.0105(12) 0.0048(12) C30 0.0091(13) 0.0126(13) 0.0152(14) 0.0028(11) 0.0059(11) 0.0002(10) C31 0.0122(13) 0.0138(14) 0.0183(15) 0.0049(12) 0.0090(12) 0.0042(11) C32 0.0135(15) 0.0228(16) 0.0317(19) 0.0094(14) 0.0116(14) 0.0039(13) C33 0.0295(18) 0.0172(16) 0.0247(18) 0.0041(14) 0.0116(15) 0.0086(14) C34 0.0154(15) 0.0253(17) 0.0254(17) 0.0145(14) 0.0107(13) 0.0081(13) 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' 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' 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 N3 Fe1 C1 88.91(10) . . N3 Fe1 N5 85.86(10) . . C1 Fe1 N5 144.25(10) . . N3 Fe1 C1 121.99(11) . 2_755 C1 Fe1 C1 101.77(10) . 2_755 N5 Fe1 C1 110.94(10) . 2_755 N3 Fe1 Fe1 114.30(8) . 2_755 C1 Fe1 Fe1 51.98(8) . 2_755 N5 Fe1 Fe1 157.04(7) . 2_755 C1 Fe1 Fe1 49.80(8) 2_755 2_755 C3 N1 N2 105.2(2) . . N1 N2 C1 114.0(2) . . N1 N2 C8 118.2(2) . . C1 N2 C8 127.8(2) . . C14 N3 C13 105.3(2) . . C14 N3 Fe1 123.76(19) . . C13 N3 Fe1 127.08(19) . . C28 N4 N5 110.7(2) . . C28 N4 C19 125.5(2) . . N5 N4 C19 123.5(2) . . C30 N5 N4 105.3(2) . . C30 N5 Fe1 130.5(2) . . N4 N5 Fe1 124.17(18) . . N2 C1 C2 102.1(2) . . N2 C1 Fe1 123.1(2) . . C2 C1 Fe1 133.2(2) . . N2 C1 Fe1 119.4(2) . 2_755 C2 C1 Fe1 90.71(18) . 2_755 Fe1 C1 Fe1 78.23(10) . 2_755 C3 C2 C1 108.1(3) . . C3 C2 H2 125.9 . . C1 C2 H2 125.9 . . N1 C3 C2 110.5(3) . . N1 C3 C4 119.2(3) . . C2 C3 C4 130.2(3) . . C3 C4 C5 109.7(3) . . C3 C4 C7 109.5(3) . . C5 C4 C7 110.0(3) . . C3 C4 C6 109.0(3) . . C5 C4 C6 109.2(3) . . C7 C4 C6 109.4(3) . . C4 C5 H5A 109.5 . . C4 C5 H5B 109.5 . . H5A C5 H5B 109.5 . . C4 C5 H5C 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . C4 C6 H6A 109.5 . . C4 C6 H6B 109.5 . . H6A C6 H6B 109.5 . . C4 C6 H6C 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . C4 C7 H7A 109.5 . . C4 C7 H7B 109.5 . . H7A C7 H7B 109.5 . . C4 C7 H7C 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . C13 C8 C9 118.2(3) . . C13 C8 N2 119.9(2) . . C9 C8 N2 121.8(2) . . C8 C9 C10 122.3(3) . . C8 C9 H9 118.8 . . C10 C9 H9 118.8 . . C11 C10 C9 118.7(3) . . C11 C10 C20 120.2(3) . . C9 C10 C20 121.1(3) . . C12 C11 C10 120.1(3) . . C12 C11 H11 120.0 . . C10 C11 H11 120.0 . . C11 C12 C13 120.2(3) . . C11 C12 C15 134.8(3) . . C13 C12 C15 105.0(2) . . N3 C13 C8 127.4(3) . . N3 C13 C12 112.2(3) . . C8 C13 C12 120.4(3) . . N3 C14 C19 127.8(3) . . N3 C14 C15 112.7(3) . . C19 C14 C15 119.5(3) . . C16 C15 C14 120.7(3) . . C16 C15 C12 134.6(3) . . C14 C15 C12 104.7(2) . . C17 C16 C15 119.6(3) . . C17 C16 H16 120.2 . . C15 C16 H16 120.2 . . C16 C17 C18 119.1(3) . . C16 C17 C24 122.0(3) . . C18 C17 C24 118.9(3) . . C19 C18 C17 122.1(3) . . C19 C18 H18 118.9 . . C17 C18 H18 118.9 . . C18 C19 C14 118.4(3) . . C18 C19 N4 121.1(3) . . C14 C19 N4 120.4(2) . . C21 C20 C23 108.2(3) . . C21 C20 C22 108.6(3) . . C23 C20 C22 108.7(3) . . C21 C20 C10 111.8(3) . . C23 C20 C10 110.7(2) . . C22 C20 C10 108.8(3) . . C20 C21 H21A 109.5 . . C20 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . C20 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C20 C22 H22A 109.5 . . C20 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . C20 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C20 C23 H23A 109.5 . . C20 C23 H23B 109.5 . . H23A C23 H23B 109.5 . . C20 C23 H23C 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C26 C24 C25 107.5(3) . . C26 C24 C27 109.6(3) . . C25 C24 C27 108.5(3) . . C26 C24 C17 111.3(2) . . C25 C24 C17 111.1(2) . . C27 C24 C17 108.7(2) . . C24 C25 H25A 109.5 . . C24 C25 H25B 109.5 . . H25A C25 H25B 109.5 . . C24 C25 H25C 109.5 . . H25A C25 H25C 109.5 . . H25B C25 H25C 109.5 . . C24 C26 H26A 109.5 . . C24 C26 H26B 109.5 . . H26A C26 H26B 109.5 . . C24 C26 H26C 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . C24 C27 H27A 109.5 . . C24 C27 H27B 109.5 . . H27A C27 H27B 109.5 . . C24 C27 H27C 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . N4 C28 C29 107.9(3) . . N4 C28 H28 126.1 . . C29 C28 H28 126.1 . . C28 C29 C30 105.7(3) . . C28 C29 H29 127.1 . . C30 C29 H29 127.1 . . N5 C30 C29 110.4(3) . . N5 C30 C31 122.7(3) . . C29 C30 C31 126.9(3) . . C30 C31 C34 112.7(2) . . C30 C31 C32 110.0(3) . . C34 C31 C32 108.4(3) . . C30 C31 C33 107.3(3) . . C34 C31 C33 109.9(3) . . C32 C31 C33 108.5(3) . . C31 C32 H32A 109.5 . . C31 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . C31 C32 H32C 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . C31 C33 H33A 109.5 . . C31 C33 H33B 109.5 . . H33A C33 H33B 109.5 . . C31 C33 H33C 109.5 . . H33A C33 H33C 109.5 . . H33B C33 H33C 109.5 . . C31 C34 H34A 109.5 . . C31 C34 H34B 109.5 . . H34A C34 H34B 109.5 . . C31 C34 H34C 109.5 . . H34A C34 H34C 109.5 . . H34B C34 H34C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Fe1 N3 1.962(2) . Fe1 C1 2.105(3) . Fe1 N5 2.120(2) . Fe1 C1 2.171(3) 2_755 Fe1 Fe1 2.6978(9) 2_755 N1 C3 1.332(4) . N1 N2 1.362(3) . N2 C1 1.398(4) . N2 C8 1.418(4) . N3 C14 1.368(4) . N3 C13 1.376(4) . N4 C28 1.350(4) . N4 N5 1.382(3) . N4 C19 1.434(4) . N5 C30 1.349(4) . C1 C2 1.410(4) . C1 Fe1 2.171(3) 2_755 C2 C3 1.408(4) . C2 H2 0.9500 . C3 C4 1.516(4) . C4 C5 1.528(4) . C4 C7 1.529(4) . C4 C6 1.529(5) . C5 H5A 0.9800 . C5 H5B 0.9800 . C5 H5C 0.9800 . C6 H6A 0.9800 . C6 H6B 0.9800 . C6 H6C 0.9800 . C7 H7A 0.9800 . C7 H7B 0.9800 . C7 H7C 0.9800 . C8 C13 1.395(4) . C8 C9 1.398(4) . C9 C10 1.404(4) . C9 H9 0.9500 . C10 C11 1.400(4) . C10 C20 1.541(4) . C11 C12 1.395(4) . C11 H11 0.9500 . C12 C13 1.416(4) . C12 C15 1.455(4) . C14 C19 1.403(4) . C14 C15 1.414(4) . C15 C16 1.399(4) . C16 C17 1.389(4) . C16 H16 0.9500 . C17 C18 1.407(4) . C17 C24 1.542(4) . C18 C19 1.389(4) . C18 H18 0.9500 . C20 C21 1.532(4) . C20 C23 1.533(4) . C20 C22 1.535(5) . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C24 C26 1.527(4) . C24 C25 1.531(4) . C24 C27 1.534(4) . C25 H25A 0.9800 . C25 H25B 0.9800 . C25 H25C 0.9800 . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C28 C29 1.374(4) . C28 H28 0.9500 . C29 C30 1.404(4) . C29 H29 0.9500 . C30 C31 1.512(4) . C31 C34 1.528(4) . C31 C32 1.540(4) . C31 C33 1.545(4) . C32 H32A 0.9800 . C32 H32B 0.9800 . C32 H32C 0.9800 . C33 H33A 0.9800 . C33 H33B 0.9800 . C33 H33C 0.9800 . C34 H34A 0.9800 . C34 H34B 0.9800 . C34 H34C 0.9800 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 C3 N1 N2 C1 -0.4(3) . . C3 N1 N2 C8 -179.8(2) . . C28 N4 N5 C30 0.2(3) . . C19 N4 N5 C30 -174.0(3) . . C28 N4 N5 Fe1 -177.7(2) . . C19 N4 N5 Fe1 8.1(4) . . N1 N2 C1 C2 0.1(3) . . C8 N2 C1 C2 179.4(3) . . N1 N2 C1 Fe1 -167.10(19) . . C8 N2 C1 Fe1 12.2(4) . . N1 N2 C1 Fe1 97.8(3) . 2_755 C8 N2 C1 Fe1 -82.8(3) . 2_755 N2 C1 C2 C3 0.3(3) . . Fe1 C1 C2 C3 165.5(2) . . Fe1 C1 C2 C3 -120.0(2) 2_755 . N2 N1 C3 C2 0.6(3) . . N2 N1 C3 C4 -178.5(3) . . C1 C2 C3 N1 -0.6(3) . . C1 C2 C3 C4 178.3(3) . . N1 C3 C4 C5 -47.5(4) . . C2 C3 C4 C5 133.7(3) . . N1 C3 C4 C7 -168.3(3) . . C2 C3 C4 C7 12.9(5) . . N1 C3 C4 C6 72.1(4) . . C2 C3 C4 C6 -106.8(4) . . N1 N2 C8 C13 163.6(3) . . C1 N2 C8 C13 -15.8(4) . . N1 N2 C8 C9 -14.8(4) . . C1 N2 C8 C9 165.9(3) . . C13 C8 C9 C10 3.2(4) . . N2 C8 C9 C10 -178.4(3) . . C8 C9 C10 C11 -0.3(4) . . C8 C9 C10 C20 177.8(3) . . C9 C10 C11 C12 -2.6(4) . . C20 C10 C11 C12 179.3(3) . . C10 C11 C12 C13 2.5(4) . . C10 C11 C12 C15 -174.1(3) . . C14 N3 C13 C8 -174.9(3) . . Fe1 N3 C13 C8 26.9(4) . . C14 N3 C13 C12 2.3(3) . . Fe1 N3 C13 C12 -155.9(2) . . C9 C8 C13 N3 173.7(3) . . N2 C8 C13 N3 -4.6(5) . . C9 C8 C13 C12 -3.2(4) . . N2 C8 C13 C12 178.4(3) . . C11 C12 C13 N3 -177.0(3) . . C15 C12 C13 N3 0.6(3) . . C11 C12 C13 C8 0.5(4) . . C15 C12 C13 C8 178.0(3) . . C13 N3 C14 C19 174.0(3) . . Fe1 N3 C14 C19 -26.9(4) . . C13 N3 C14 C15 -4.6(3) . . Fe1 N3 C14 C15 154.6(2) . . N3 C14 C15 C16 -174.7(3) . . C19 C14 C15 C16 6.6(4) . . N3 C14 C15 C12 4.9(3) . . C19 C14 C15 C12 -173.8(3) . . C11 C12 C15 C16 -6.7(6) . . C13 C12 C15 C16 176.3(3) . . C11 C12 C15 C14 173.9(3) . . C13 C12 C15 C14 -3.2(3) . . C14 C15 C16 C17 -0.2(4) . . C12 C15 C16 C17 -179.6(3) . . C15 C16 C17 C18 -4.8(4) . . C15 C16 C17 C24 172.9(3) . . C16 C17 C18 C19 3.4(4) . . C24 C17 C18 C19 -174.4(3) . . C17 C18 C19 C14 3.1(4) . . C17 C18 C19 N4 -173.1(3) . . N3 C14 C19 C18 173.6(3) . . C15 C14 C19 C18 -8.0(4) . . N3 C14 C19 N4 -10.2(5) . . C15 C14 C19 N4 168.3(3) . . C28 N4 C19 C18 21.5(4) . . N5 N4 C19 C18 -165.2(3) . . C28 N4 C19 C14 -154.6(3) . . N5 N4 C19 C14 18.7(4) . . C11 C10 C20 C21 -167.5(3) . . C9 C10 C20 C21 14.5(4) . . C11 C10 C20 C23 -46.8(4) . . C9 C10 C20 C23 135.2(3) . . C11 C10 C20 C22 72.6(4) . . C9 C10 C20 C22 -105.4(3) . . C16 C17 C24 C26 126.0(3) . . C18 C17 C24 C26 -56.3(4) . . C16 C17 C24 C25 6.2(4) . . C18 C17 C24 C25 -176.1(3) . . C16 C17 C24 C27 -113.2(3) . . C18 C17 C24 C27 64.5(3) . . N5 N4 C28 C29 0.3(3) . . C19 N4 C28 C29 174.3(3) . . N4 C28 C29 C30 -0.6(4) . . N4 N5 C30 C29 -0.5(3) . . Fe1 N5 C30 C29 177.1(2) . . N4 N5 C30 C31 -178.1(3) . . Fe1 N5 C30 C31 -0.4(4) . . C28 C29 C30 N5 0.7(4) . . C28 C29 C30 C31 178.1(3) . . N5 C30 C31 C34 -11.4(4) . . C29 C30 C31 C34 171.5(3) . . N5 C30 C31 C32 -132.4(3) . . C29 C30 C31 C32 50.5(4) . . N5 C30 C31 C33 109.7(3) . . C29 C30 C31 C33 -67.4(4) . .