#------------------------------------------------------------------------------ #$Date: 2020-08-18 05:02:47 +0300 (Tue, 18 Aug 2020) $ #$Revision: 255416 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705185.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_7705185 loop_ _publ_author_name 'Liang, Qiuming' 'Lin, Jack H.' 'DeMuth, Joshua C.' 'Neidig, Michael L.' 'Song, Datong' _publ_section_title ; Syntheses and Characterizations of Iron Complexes of Bulky o-Phenylenediamide ligand ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02087G _journal_year 2020 _chemical_formula_moiety 'C36 H56 Fe N3 Si2' _chemical_formula_sum 'C36 H56 Fe N3 Si2' _chemical_formula_weight 642.86 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-08-11 deposited with the CCDC. 2020-08-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.742(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.5549(12) _cell_length_b 17.0278(19) _cell_length_c 16.221(2) _cell_measurement_reflns_used 4263 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.569 _cell_measurement_theta_min 1.934 _cell_volume 3700.5(7) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_measurement_method 'Phi and Omega Scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0902 _diffrn_reflns_av_unetI/netI 0.0965 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16937 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.569 _diffrn_reflns_theta_min 1.934 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_T_max 0.6997 _exptl_absorpt_correction_T_min 0.5818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.154 _exptl_crystal_description plate _exptl_crystal_F_000 1388 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.322 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 4263 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0536 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+3.2621P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.1274 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2778 _reflns_number_total 4263 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02087g2.cif _cod_data_source_block wl224 _cod_original_cell_volume 3700.4(7) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7705185 _shelx_shelxl_version_number 2016/6 _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 ; TITL wl224 in C2/c wl224.res created by SHELXL-2016/6 at 22:33:53 on 18-Feb-2019 CELL 0.71073 13.5549 17.0278 16.2205 90.000 98.742 90.000 ZERR 4.00 0.0012 0.0019 0.0020 0.000 0.004 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N Si Fe UNIT 144 224 12 8 4 L.S. 16 ACTA BOND SIMU 0.01 C16 C16A FMAP 2 PLAN 5 TEMP -123.000 WGHT 0.039700 3.262100 FVAR 0.10080 FE1 5 0.500000 0.231745 0.250000 10.50000 0.02469 0.01268 = 0.03405 0.00000 0.01690 0.00000 SI1 4 0.525913 0.388220 0.161346 11.00000 0.03179 0.02409 = 0.03109 0.01021 0.00693 -0.00068 N1 3 0.585623 0.143310 0.222118 11.00000 0.02943 0.01997 = 0.03646 0.00586 0.02501 0.00371 C1 1 0.549196 0.072418 0.237406 11.00000 0.04282 0.01802 = 0.03297 0.00055 0.02432 0.00288 N2 3 0.500000 0.342838 0.250000 10.50000 0.01970 0.01574 = 0.02508 0.00000 0.00631 0.00000 C2 1 0.598004 -0.000580 0.232585 11.00000 0.05566 0.02229 = 0.04156 0.00600 0.03062 0.01079 AFIX 43 H2A 2 0.665164 -0.001613 0.222356 11.00000 -1.20000 AFIX 0 C3 1 0.550002 -0.069051 0.242398 11.00000 0.09080 0.01800 = 0.04873 0.00369 0.04666 0.00876 AFIX 43 H3A 2 0.583904 -0.117503 0.239025 11.00000 -1.20000 AFIX 0 C4 1 0.682191 0.150553 0.196385 11.00000 0.03400 0.01564 = 0.04268 0.00767 0.02742 0.00704 C5 1 0.758795 0.185020 0.252502 11.00000 0.04393 0.01452 = 0.05368 -0.00024 0.03586 -0.00020 C6 1 0.850672 0.197996 0.225533 11.00000 0.03919 0.02834 = 0.06202 -0.00485 0.03091 -0.00587 AFIX 43 H6A 2 0.903648 0.221148 0.262674 11.00000 -1.20000 AFIX 0 C7 1 0.865785 0.177904 0.146356 11.00000 0.03887 0.03714 = 0.06121 0.00718 0.03712 0.00406 AFIX 43 H7A 2 0.928782 0.186996 0.129224 11.00000 -1.20000 AFIX 0 C8 1 0.789999 0.144818 0.092323 11.00000 0.03790 0.04529 = 0.04350 0.01323 0.02750 0.01399 AFIX 43 H8A 2 0.801420 0.131251 0.037752 11.00000 -1.20000 AFIX 0 C9 1 0.696509 0.130379 0.114822 11.00000 0.03214 0.03159 = 0.03532 0.01467 0.01876 0.01533 C10 1 0.744058 0.204538 0.340859 11.00000 0.05065 0.03708 = 0.06726 -0.02499 0.04216 -0.02231 AFIX 13 H10A 2 0.671731 0.213567 0.343595 11.00000 -1.20000 AFIX 0 C11 1 0.805715 0.273193 0.379049 11.00000 0.05516 0.04058 = 0.06324 -0.01599 0.02458 -0.01604 AFIX 33 H11A 2 0.801432 0.316378 0.338724 11.00000 -1.50000 H11B 2 0.780138 0.290783 0.429308 11.00000 -1.50000 H11C 2 0.875489 0.256866 0.393839 11.00000 -1.50000 AFIX 0 PART 1 C12 1 0.789588 0.128406 0.406797 10.50000 0.10489 0.03637 = 0.02509 -0.00447 0.01209 -0.00149 AFIX 33 H12A 2 0.780021 0.141085 0.463983 10.50000 -1.50000 H12B 2 0.753591 0.079922 0.388968 10.50000 -1.50000 H12C 2 0.860892 0.121168 0.404719 10.50000 -1.50000 AFIX 0 PART 2 C12A 1 0.739193 0.137325 0.386390 10.50000 0.05434 0.04995 = 0.01457 -0.00121 -0.00189 -0.01927 AFIX 33 H12D 2 0.729657 0.151032 0.443327 10.50000 -1.50000 H12E 2 0.683004 0.105148 0.360401 10.50000 -1.50000 H12F 2 0.801434 0.107685 0.388033 10.50000 -1.50000 AFIX 0 PART 0 C13 1 0.615862 0.094345 0.051328 11.00000 0.03083 0.07775 = 0.03110 0.01863 0.01685 0.01881 AFIX 13 H13A 2 0.554409 0.088522 0.077977 11.00000 -1.20000 AFIX 0 C14 1 0.589951 0.146243 -0.026029 11.00000 0.06519 0.12984 = 0.04357 0.03580 0.01716 0.04207 AFIX 33 H14A 2 0.537628 0.120879 -0.065441 11.00000 -1.50000 H14B 2 0.566089 0.197375 -0.009550 11.00000 -1.50000 H14C 2 0.649552 0.153689 -0.052603 11.00000 -1.50000 AFIX 0 C15 1 0.645374 0.013356 0.024076 11.00000 0.03940 0.07948 = 0.03623 -0.00465 0.01090 0.00224 AFIX 33 H15A 2 0.591528 -0.008077 -0.016910 11.00000 -1.50000 H15B 2 0.706486 0.017431 -0.001089 11.00000 -1.50000 H15C 2 0.657133 -0.021495 0.072659 11.00000 -1.50000 AFIX 0 PART 1 C16 1 0.483928 0.489060 0.142625 10.50000 0.13584 0.04539 = 0.10602 0.04923 0.07666 0.04020 AFIX 33 H16A 2 0.503407 0.507811 0.090291 10.50000 -1.50000 H16B 2 0.411125 0.491277 0.138763 10.50000 -1.50000 H16C 2 0.514643 0.522396 0.188741 10.50000 -1.50000 AFIX 0 C17 1 0.460061 0.330846 0.066537 10.50000 0.06525 0.11995 = 0.02992 0.01639 -0.00208 -0.03639 AFIX 33 H17A 2 0.473967 0.355893 0.015134 10.50000 -1.50000 H17B 2 0.484749 0.276676 0.068840 10.50000 -1.50000 H17C 2 0.387912 0.330734 0.067326 10.50000 -1.50000 AFIX 0 C18 1 0.662555 0.380013 0.153486 10.50000 0.03493 0.06624 = 0.04042 0.01187 0.01444 -0.01531 AFIX 33 H18A 2 0.675912 0.406231 0.102542 10.50000 -1.50000 H18B 2 0.701847 0.405052 0.202136 10.50000 -1.50000 H18C 2 0.681096 0.324481 0.151685 10.50000 -1.50000 AFIX 0 PART 2 C16A 1 0.426105 0.463762 0.125634 10.50000 0.11838 0.03662 = 0.06235 0.02032 0.01305 0.03427 AFIX 33 H16D 2 0.441008 0.489639 0.074983 10.50000 -1.50000 H16E 2 0.360996 0.437751 0.113806 10.50000 -1.50000 H16F 2 0.424633 0.503009 0.169620 10.50000 -1.50000 AFIX 0 C17A 1 0.530394 0.318426 0.079293 10.50000 0.05803 0.03824 = 0.02615 0.00305 0.01189 0.00174 AFIX 33 H17D 2 0.545276 0.345694 0.029416 10.50000 -1.50000 H17E 2 0.582614 0.279557 0.097108 10.50000 -1.50000 H17F 2 0.465742 0.291862 0.066486 10.50000 -1.50000 AFIX 0 C18A 1 0.649472 0.441034 0.181841 10.50000 0.06314 0.07179 = 0.06284 0.01184 0.01611 -0.04215 AFIX 33 H18D 2 0.662704 0.466471 0.130439 10.50000 -1.50000 H18E 2 0.647263 0.480860 0.225138 10.50000 -1.50000 H18F 2 0.702669 0.403222 0.200598 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 REM wl224 in C2/c REM R1 = 0.0536 for 2778 Fo > 4sig(Fo) and 0.1029 for all 4263 data REM 227 parameters refined using 6 restraints END WGHT 0.0397 3.2621 REM Highest difference peak 0.322, deepest hole -0.400, 1-sigma level 0.070 Q1 1 0.5000 0.0713 0.2500 10.50000 0.05 0.32 Q2 1 0.5000 0.2937 0.2500 10.50000 0.05 0.32 Q3 1 0.7825 0.2132 0.3711 11.00000 0.05 0.31 Q4 1 0.5862 0.1892 -0.0106 11.00000 0.05 0.31 Q5 1 0.5242 0.3584 0.2274 11.00000 0.05 0.29 ; _shelx_res_checksum 46942 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 0.500000 0.23174(3) 0.250000 0.02252(17) Uani 1 2 d S T P . . Si1 Si 0.52591(6) 0.38822(5) 0.16135(5) 0.0288(2) Uani 1 1 d . . . . . N1 N 0.58562(16) 0.14331(12) 0.22212(15) 0.0265(6) Uani 1 1 d . . . . . C1 C 0.5492(2) 0.07242(15) 0.23741(18) 0.0293(7) Uani 1 1 d . . . . . N2 N 0.500000 0.34284(16) 0.250000 0.0199(7) Uani 1 2 d S T P C . C2 C 0.5980(2) -0.00058(16) 0.2326(2) 0.0374(8) Uani 1 1 d . . . . . H2A H 0.665164 -0.001613 0.222356 0.045 Uiso 1 1 calc R U . . . C3 C 0.5500(3) -0.06905(17) 0.2424(2) 0.0488(10) Uani 1 1 d . . . . . H3A H 0.583904 -0.117503 0.239025 0.059 Uiso 1 1 calc R U . . . C4 C 0.6822(2) 0.15055(15) 0.19638(19) 0.0285(7) Uani 1 1 d . . . . . C5 C 0.7588(2) 0.18502(15) 0.2525(2) 0.0344(8) Uani 1 1 d . . . . . C6 C 0.8507(2) 0.19800(17) 0.2255(2) 0.0408(9) Uani 1 1 d . . . . . H6A H 0.903648 0.221148 0.262674 0.049 Uiso 1 1 calc R U . . . C7 C 0.8658(2) 0.17790(18) 0.1464(2) 0.0427(9) Uani 1 1 d . . . . . H7A H 0.928782 0.186996 0.129224 0.051 Uiso 1 1 calc R U . . . C8 C 0.7900(2) 0.14482(19) 0.0923(2) 0.0400(8) Uani 1 1 d . . . . . H8A H 0.801420 0.131251 0.037752 0.048 Uiso 1 1 calc R U . . . C9 C 0.6965(2) 0.13038(17) 0.11482(19) 0.0316(7) Uani 1 1 d . . . . . C10 C 0.7441(3) 0.20454(18) 0.3409(2) 0.0482(10) Uani 1 1 d . . . . . H10A H 0.671731 0.213567 0.343595 0.058 Uiso 1 1 calc R U . A 1 C11 C 0.8057(3) 0.27319(19) 0.3790(2) 0.0514(10) Uani 1 1 d . . . . . H11A H 0.801432 0.316378 0.338724 0.077 Uiso 1 1 calc R U . . . H11B H 0.780138 0.290783 0.429308 0.077 Uiso 1 1 calc R U . . . H11C H 0.875489 0.256866 0.393839 0.077 Uiso 1 1 calc R U . . . C12 C 0.7896(8) 0.1284(6) 0.4068(6) 0.055(3) Uani 0.5 1 d . . P B 1 H12A H 0.780021 0.141085 0.463983 0.083 Uiso 0.5 1 calc R U P B 1 H12B H 0.753591 0.079922 0.388968 0.083 Uiso 0.5 1 calc R U P B 1 H12C H 0.860892 0.121168 0.404719 0.083 Uiso 0.5 1 calc R U P B 1 C12A C 0.7392(6) 0.1373(6) 0.3864(6) 0.040(2) Uani 0.5 1 d . . P B 2 H12D H 0.729657 0.151032 0.443327 0.061 Uiso 0.5 1 calc R U P B 2 H12E H 0.683004 0.105148 0.360401 0.061 Uiso 0.5 1 calc R U P B 2 H12F H 0.801434 0.107685 0.388033 0.061 Uiso 0.5 1 calc R U P B 2 C13 C 0.6159(2) 0.0943(2) 0.0513(2) 0.0453(9) Uani 1 1 d . . . . . H13A H 0.554409 0.088522 0.077977 0.054 Uiso 1 1 calc R U . . . C14 C 0.5900(3) 0.1462(3) -0.0260(3) 0.0786(15) Uani 1 1 d . . . . . H14A H 0.537628 0.120879 -0.065441 0.118 Uiso 1 1 calc R U . . . H14B H 0.566089 0.197375 -0.009550 0.118 Uiso 1 1 calc R U . . . H14C H 0.649552 0.153689 -0.052603 0.118 Uiso 1 1 calc R U . . . C15 C 0.6454(2) 0.0134(2) 0.0241(2) 0.0512(10) Uani 1 1 d . . . . . H15A H 0.591528 -0.008077 -0.016910 0.077 Uiso 1 1 calc R U . . . H15B H 0.706486 0.017431 -0.001089 0.077 Uiso 1 1 calc R U . . . H15C H 0.657133 -0.021495 0.072659 0.077 Uiso 1 1 calc R U . . . C16 C 0.4839(10) 0.4891(7) 0.1426(10) 0.090(5) Uani 0.5 1 d . U P C 1 H16A H 0.503407 0.507811 0.090291 0.135 Uiso 0.5 1 calc R U P C 1 H16B H 0.411125 0.491277 0.138763 0.135 Uiso 0.5 1 calc R U P C 1 H16C H 0.514643 0.522396 0.188741 0.135 Uiso 0.5 1 calc R U P C 1 C17 C 0.4601(7) 0.3308(6) 0.0665(5) 0.073(3) Uani 0.5 1 d . . P C 1 H17A H 0.473967 0.355893 0.015134 0.109 Uiso 0.5 1 calc R U P C 1 H17B H 0.484749 0.276676 0.068840 0.109 Uiso 0.5 1 calc R U P C 1 H17C H 0.387912 0.330734 0.067326 0.109 Uiso 0.5 1 calc R U P C 1 C18 C 0.6626(5) 0.3800(5) 0.1535(5) 0.0463(18) Uani 0.5 1 d . . P C 1 H18A H 0.675912 0.406231 0.102542 0.069 Uiso 0.5 1 calc R U P C 1 H18B H 0.701847 0.405052 0.202136 0.069 Uiso 0.5 1 calc R U P C 1 H18C H 0.681096 0.324481 0.151685 0.069 Uiso 0.5 1 calc R U P C 1 C16A C 0.4261(9) 0.4638(6) 0.1256(8) 0.073(4) Uani 0.5 1 d . U P C 2 H16D H 0.441008 0.489639 0.074983 0.109 Uiso 0.5 1 calc R U P C 2 H16E H 0.360996 0.437751 0.113806 0.109 Uiso 0.5 1 calc R U P C 2 H16F H 0.424633 0.503009 0.169620 0.109 Uiso 0.5 1 calc R U P C 2 C17A C 0.5304(6) 0.3184(4) 0.0793(4) 0.0402(16) Uani 0.5 1 d . . P C 2 H17D H 0.545276 0.345694 0.029416 0.060 Uiso 0.5 1 calc R U P C 2 H17E H 0.582614 0.279557 0.097108 0.060 Uiso 0.5 1 calc R U P C 2 H17F H 0.465742 0.291862 0.066486 0.060 Uiso 0.5 1 calc R U P C 2 C18A C 0.6495(6) 0.4410(5) 0.1818(5) 0.065(2) Uani 0.5 1 d . . P C 2 H18D H 0.662704 0.466471 0.130439 0.098 Uiso 0.5 1 calc R U P C 2 H18E H 0.647263 0.480860 0.225138 0.098 Uiso 0.5 1 calc R U P C 2 H18F H 0.702669 0.403222 0.200598 0.098 Uiso 0.5 1 calc R U P C 2 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 0.0247(3) 0.0127(3) 0.0341(4) 0.000 0.0169(3) 0.000 Si1 0.0318(4) 0.0241(4) 0.0311(5) 0.0102(3) 0.0069(4) -0.0007(3) N1 0.0294(12) 0.0200(12) 0.0365(15) 0.0059(10) 0.0250(11) 0.0037(9) C1 0.0428(17) 0.0180(14) 0.0330(18) 0.0005(12) 0.0243(14) 0.0029(12) N2 0.0197(15) 0.0157(15) 0.0251(19) 0.000 0.0063(14) 0.000 C2 0.056(2) 0.0223(15) 0.042(2) 0.0060(14) 0.0306(17) 0.0108(14) C3 0.091(3) 0.0180(15) 0.049(2) 0.0037(15) 0.047(2) 0.0088(16) C4 0.0340(16) 0.0156(13) 0.043(2) 0.0077(13) 0.0274(15) 0.0070(11) C5 0.0439(18) 0.0145(13) 0.054(2) -0.0002(14) 0.0359(17) -0.0002(12) C6 0.0392(18) 0.0283(16) 0.062(2) -0.0049(15) 0.0309(18) -0.0059(13) C7 0.0389(18) 0.0371(18) 0.061(3) 0.0072(17) 0.0371(19) 0.0041(15) C8 0.0379(18) 0.0453(19) 0.043(2) 0.0132(16) 0.0275(17) 0.0140(15) C9 0.0321(16) 0.0316(16) 0.0353(19) 0.0147(13) 0.0188(14) 0.0153(12) C10 0.051(2) 0.0371(18) 0.067(3) -0.0250(17) 0.0422(19) -0.0223(15) C11 0.055(2) 0.041(2) 0.063(3) -0.0160(18) 0.0246(19) -0.0160(16) C12 0.105(9) 0.036(4) 0.025(6) -0.004(4) 0.012(6) -0.001(6) C12A 0.054(6) 0.050(5) 0.015(5) -0.001(4) -0.002(4) -0.019(5) C13 0.0308(17) 0.078(3) 0.031(2) 0.0186(18) 0.0169(15) 0.0188(16) C14 0.065(3) 0.130(4) 0.044(3) 0.036(3) 0.017(2) 0.042(3) C15 0.0394(19) 0.079(3) 0.036(2) -0.0046(19) 0.0109(17) 0.0022(18) C16 0.136(12) 0.045(7) 0.106(10) 0.049(7) 0.077(9) 0.040(6) C17 0.065(6) 0.120(8) 0.030(5) 0.016(5) -0.002(5) -0.036(6) C18 0.035(4) 0.066(5) 0.040(5) 0.012(4) 0.014(3) -0.015(3) C16A 0.118(11) 0.037(6) 0.062(6) 0.020(5) 0.013(8) 0.034(6) C17A 0.058(5) 0.038(4) 0.026(4) 0.003(3) 0.012(4) 0.002(4) C18A 0.063(5) 0.072(6) 0.063(6) 0.012(5) 0.016(4) -0.042(5) 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' Si Si 0.0817 0.0704 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 139.02(6) . . ? N2 Fe1 N1 139.02(6) . 2_655 ? N1 Fe1 N1 81.96(12) . 2_655 ? N2 Si1 C17A 111.0(2) . . ? N2 Si1 C16 117.8(4) . . ? N2 Si1 C18 110.6(2) . . ? C16 Si1 C18 110.2(4) . . ? N2 Si1 C18A 110.9(3) . . ? C17A Si1 C18A 108.5(4) . . ? N2 Si1 C16A 109.6(4) . . ? C17A Si1 C16A 109.1(5) . . ? C18A Si1 C16A 107.7(4) . . ? N2 Si1 C17 108.2(3) . . ? C16 Si1 C17 104.5(6) . . ? C18 Si1 C17 104.5(4) . . ? C1 N1 C4 120.5(2) . . ? C1 N1 Fe1 113.22(16) . . ? C4 N1 Fe1 125.99(16) . . ? N1 C1 C2 126.3(2) . . ? N1 C1 C1 115.55(14) . 2_655 ? C2 C1 C1 118.17(16) . 2_655 ? Si1 N2 Si1 126.44(17) 2_655 . ? Si1 N2 Fe1 116.78(9) 2_655 . ? Si1 N2 Fe1 116.78(9) . . ? C3 C2 C1 120.8(3) . . ? C2 C3 C3 120.67(18) . 2_655 ? C5 C4 C9 121.2(2) . . ? C5 C4 N1 117.7(2) . . ? C9 C4 N1 120.9(3) . . ? C6 C5 C4 118.0(3) . . ? C6 C5 C10 120.9(3) . . ? C4 C5 C10 121.0(2) . . ? C7 C6 C5 121.3(3) . . ? C8 C7 C6 119.9(3) . . ? C7 C8 C9 122.0(3) . . ? C8 C9 C4 117.6(3) . . ? C8 C9 C13 119.0(3) . . ? C4 C9 C13 123.3(2) . . ? C12A C10 C5 110.6(5) . . ? C12A C10 C11 119.6(5) . . ? C5 C10 C11 114.4(3) . . ? C5 C10 C12 109.5(4) . . ? C11 C10 C12 101.7(4) . . ? C9 C13 C15 111.8(2) . . ? C9 C13 C14 112.1(3) . . ? C15 C13 C14 108.8(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.892(3) . ? Fe1 N1 1.995(2) . ? Fe1 N1 1.995(2) 2_655 ? Si1 N2 1.7152(14) . ? Si1 C17A 1.792(7) . ? Si1 C16 1.820(11) . ? Si1 C18 1.881(6) . ? Si1 C18A 1.885(7) . ? Si1 C16A 1.893(11) . ? Si1 C17 1.923(9) . ? N1 C1 1.342(3) . ? N1 C4 1.438(3) . ? C1 C2 1.416(4) . ? C1 C1 1.453(5) 2_655 ? C2 C3 1.356(4) . ? C3 C3 1.414(6) 2_655 ? C4 C5 1.401(4) . ? C4 C9 1.409(4) . ? C5 C6 1.399(4) . ? C5 C10 1.514(4) . ? C6 C7 1.374(5) . ? C7 C8 1.366(5) . ? C8 C9 1.393(4) . ? C9 C13 1.513(5) . ? C10 C12A 1.369(10) . ? C10 C11 1.514(4) . ? C10 C12 1.733(11) . ? C13 C15 1.520(5) . ? C13 C14 1.531(5) . ?