#------------------------------------------------------------------------------ #$Date: 2024-06-19 01:58:56 +0300 (Wed, 19 Jun 2024) $ #$Revision: 292453 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571939.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_1571939 _journal_paper_doi 10.1039/D4DT01433B _chemical_formula_moiety 'C21 H25 Fe I N3 Rh' _chemical_formula_sum 'C21 H25 Fe I N3 Rh' _chemical_formula_weight 605.10 _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' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2024-04-04 deposited with the CCDC. 2024-06-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.6940(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.0867(3) _cell_length_b 13.1442(3) _cell_length_c 13.3802(3) _cell_measurement_reflns_used 9907 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.50 _cell_measurement_theta_min 2.33 _cell_volume 2056.19(8) _computing_cell_refinement 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_data_collection 'Bruker Instrument Service v2020.1.0.0' _computing_data_reduction 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_molecular_graphics 'PLATON (Spek, 2017)' _computing_publication_material 'PLATON (Spek, 2017)' _computing_structure_refinement 'SHELXL-2017 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2018 (Sheldrick, 2018)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker Nonius Kappa Apex II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_unetI/netI 0.0183 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 17730 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.505 _diffrn_reflns_theta_min 2.030 _exptl_absorpt_coefficient_mu 3.020 _exptl_absorpt_correction_T_max 0.55 _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015). J. Appl. Cryst. 48, 3-10. ; _exptl_crystal_colour yellow-orange _exptl_crystal_density_diffrn 1.955 _exptl_crystal_description prism _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _refine_diff_density_max 0.417 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.071 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 4730 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0192 _refine_ls_R_factor_gt 0.0166 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0097P)^2^+1.8300P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0348 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4396 _reflns_number_total 4730 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt01433b3.cif _cod_data_source_block mf76 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1571939 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.393 _shelx_estimated_absorpt_t_max 0.543 _shelx_res_file ; TITL mf76, 120 K, P2(1)/n mf76.res created by SHELXL-2017/1 at 08:20:36 on 16-Jan-2023 CELL 0.71073 12.0867 13.1442 13.3802 90.000 104.694 90.000 ZERR 4 0.0003 0.0003 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H FE I N RH UNIT 84 100 4 4 12 4 TEMP -153 SIZE 0.23 0.23 0.38 L.S. 9 BOND $H LIST 4 ACTA FMAP 2 PLAN -10 WGHT 0.009700 1.830000 FVAR 0.26054 RH1 6 0.229846 0.437497 0.428488 11.00000 0.01118 0.01375 = 0.00729 0.00106 0.00162 -0.00088 I1 4 0.085967 0.295716 0.466670 11.00000 0.01994 0.01928 = 0.01351 0.00259 0.00057 -0.00702 FE1 3 0.277771 0.495553 0.819277 11.00000 0.01492 0.01182 = 0.00816 -0.00021 0.00429 0.00018 N1 5 0.378779 0.398830 0.646617 11.00000 0.01133 0.01272 = 0.00861 0.00063 0.00256 0.00052 N2 5 0.416396 0.292366 0.541725 11.00000 0.01495 0.01446 = 0.01008 -0.00129 0.00317 0.00086 N3 5 0.482671 0.262541 0.637630 11.00000 0.01588 0.01473 = 0.01553 0.00355 0.00333 0.00269 C1 1 0.335246 0.484912 0.689499 11.00000 0.01514 0.01302 = 0.00818 0.00133 0.00496 0.00012 C2 1 0.402265 0.557662 0.758569 11.00000 0.01803 0.01663 = 0.01188 0.00014 0.00568 -0.00417 AFIX 43 H2 2 0.482536 0.555398 0.787759 11.00000 -1.20000 AFIX 0 C3 1 0.325249 0.634301 0.775157 11.00000 0.02903 0.01200 = 0.01452 -0.00024 0.00882 -0.00140 AFIX 43 H3 2 0.345424 0.692526 0.817973 11.00000 -1.20000 AFIX 0 C4 1 0.213199 0.608756 0.716749 11.00000 0.02498 0.01766 = 0.01407 0.00449 0.00811 0.00895 AFIX 43 H4 2 0.145798 0.647001 0.713994 11.00000 -1.20000 AFIX 0 C5 1 0.219015 0.516416 0.663209 11.00000 0.01472 0.01902 = 0.00929 0.00150 0.00224 0.00221 AFIX 43 H5 2 0.156763 0.482100 0.618191 11.00000 -1.20000 AFIX 0 C6 1 0.286689 0.357437 0.892527 11.00000 0.02985 0.01366 = 0.01872 0.00289 0.01089 -0.00087 AFIX 43 H6 2 0.315294 0.295801 0.871694 11.00000 -1.20000 AFIX 0 C7 1 0.351484 0.430961 0.960475 11.00000 0.02356 0.02238 = 0.01200 0.00532 0.00281 -0.00066 AFIX 43 H7 2 0.430903 0.427179 0.993221 11.00000 -1.20000 AFIX 0 C8 1 0.276445 0.511302 0.970850 11.00000 0.03623 0.01965 = 0.00946 -0.00075 0.01034 -0.00268 AFIX 43 H8 2 0.297025 0.570845 1.011569 11.00000 -1.20000 AFIX 0 C9 1 0.165444 0.487035 0.909775 11.00000 0.02445 0.02987 = 0.01802 0.00477 0.01385 0.00448 AFIX 43 H9 2 0.098622 0.527298 0.902672 11.00000 -1.20000 AFIX 0 C10 1 0.171843 0.391807 0.861058 11.00000 0.02361 0.02543 = 0.01756 0.00122 0.00878 -0.00895 AFIX 43 H10 2 0.110128 0.357334 0.815511 11.00000 -1.20000 AFIX 0 C11 1 0.350882 0.373836 0.543404 11.00000 0.01258 0.01285 = 0.01024 -0.00055 0.00487 -0.00211 C12 1 0.457103 0.329829 0.699223 11.00000 0.01288 0.01563 = 0.01257 0.00407 0.00255 0.00026 AFIX 43 H12 2 0.488822 0.331050 0.771847 11.00000 -1.20000 AFIX 0 C13 1 0.421357 0.232522 0.451565 11.00000 0.03287 0.02018 = 0.01630 -0.00648 0.00892 0.00219 PART 1 AFIX 3 H13A 2 0.386819 0.267943 0.391531 10.50000 -1.50000 H13B 2 0.493019 0.242844 0.444231 10.50000 -1.50000 H13C 2 0.383219 0.164943 0.451031 10.50000 -1.50000 AFIX 3 PART 2 H13D 2 0.474204 0.175412 0.472876 10.50000 -1.50000 H13E 2 0.448206 0.275421 0.402598 10.50000 -1.50000 H13F 2 0.344911 0.206393 0.418435 10.50000 -1.50000 AFIX 0 C21 1 0.329002 0.571784 0.439012 11.00000 0.01730 0.01654 = 0.01415 0.00229 0.00171 -0.00631 AFIX 3 H21 2 0.386872 0.566590 0.502009 11.00000 -1.20000 AFIX 0 C22 1 0.346539 0.511145 0.357449 11.00000 0.01157 0.02142 = 0.01508 0.00459 0.00541 -0.00200 AFIX 3 H22 2 0.420439 0.474293 0.374180 11.00000 -1.20000 AFIX 0 C23 1 0.294576 0.534934 0.243521 11.00000 0.01888 0.02730 = 0.01333 0.00376 0.00648 0.00153 AFIX 23 H23A 2 0.349438 0.515091 0.203210 11.00000 -1.20000 H23B 2 0.281692 0.609175 0.235204 11.00000 -1.20000 AFIX 0 C24 1 0.180993 0.479298 0.200163 11.00000 0.02524 0.02613 = 0.00946 0.00325 0.00198 -0.00088 AFIX 23 H24A 2 0.136243 0.516795 0.139029 11.00000 -1.20000 H24B 2 0.197180 0.410635 0.176952 11.00000 -1.20000 AFIX 0 C25 1 0.110047 0.468888 0.277152 11.00000 0.01415 0.02632 = 0.01136 0.00726 -0.00332 -0.00204 AFIX 3 H25 2 0.054290 0.414439 0.269214 11.00000 -1.20000 AFIX 0 C26 1 0.093824 0.542500 0.344816 11.00000 0.01282 0.02725 = 0.01910 0.01037 0.00395 0.00434 AFIX 3 H26 2 0.032915 0.533953 0.380290 11.00000 -1.20000 AFIX 0 C27 1 0.137778 0.650850 0.348700 11.00000 0.02668 0.02140 = 0.02677 0.00709 0.01167 0.01057 AFIX 23 H27A 2 0.081166 0.697112 0.366749 11.00000 -1.20000 H27B 2 0.145699 0.670356 0.279385 11.00000 -1.20000 AFIX 0 C28 1 0.253791 0.664269 0.427848 11.00000 0.03392 0.01672 = 0.02310 -0.00032 0.01058 -0.00054 AFIX 23 H28A 2 0.294425 0.722596 0.406649 11.00000 -1.20000 H28B 2 0.240176 0.680776 0.495933 11.00000 -1.20000 AFIX 0 HKLF 4 REM mf76, 120 K, P2(1)/n REM R1 = 0.0166 for 4396 Fo > 4sig(Fo) and 0.0192 for all 4730 data REM 244 parameters refined using 0 restraints END WGHT 0.0097 1.8301 REM Highest difference peak 0.417, deepest hole -0.588, 1-sigma level 0.071 Q1 1 0.1364 0.2716 0.4415 11.00000 0.05 0.42 Q2 1 0.3502 0.3872 0.5934 11.00000 0.05 0.40 Q3 1 0.3154 0.5174 0.2972 11.00000 0.05 0.36 Q4 1 0.4132 0.3657 0.6736 11.00000 0.05 0.35 Q5 1 0.1525 0.4764 0.2492 11.00000 0.05 0.35 Q6 1 0.3351 0.4159 0.5041 11.00000 0.05 0.34 Q7 1 0.3761 0.5200 0.7155 11.00000 0.05 0.33 Q8 1 0.1108 0.5906 0.3481 11.00000 0.05 0.32 Q9 1 0.4582 0.2712 0.5869 11.00000 0.05 0.31 Q10 1 0.2261 0.3650 0.8991 11.00000 0.05 0.31 ; _shelx_res_checksum 17676 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_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 Rh1 Rh 0.22985(2) 0.43750(2) 0.42849(2) 0.01087(4) Uani 1 1 d . . . . . I1 I 0.08597(2) 0.29572(2) 0.46667(2) 0.01824(4) Uani 1 1 d . . . . . Fe1 Fe 0.27777(2) 0.49555(2) 0.81928(2) 0.01139(6) Uani 1 1 d . . . . . N1 N 0.37878(13) 0.39883(11) 0.64662(11) 0.0109(3) Uani 1 1 d . . . . . N2 N 0.41640(13) 0.29237(11) 0.54172(11) 0.0132(3) Uani 1 1 d . . . . . N3 N 0.48267(14) 0.26254(12) 0.63763(12) 0.0155(3) Uani 1 1 d . . . . . C1 C 0.33525(16) 0.48491(13) 0.68950(13) 0.0118(3) Uani 1 1 d . . . . . C2 C 0.40227(17) 0.55766(14) 0.75857(14) 0.0152(4) Uani 1 1 d . . . . . H2 H 0.482536 0.555398 0.787759 0.018 Uiso 1 1 calc R U . . . C3 C 0.32525(18) 0.63430(14) 0.77516(14) 0.0179(4) Uani 1 1 d . . . . . H3 H 0.345424 0.692526 0.817973 0.022 Uiso 1 1 calc R U . . . C4 C 0.21320(18) 0.60876(14) 0.71675(14) 0.0183(4) Uani 1 1 d . . . . . H4 H 0.145798 0.647001 0.713994 0.022 Uiso 1 1 calc R U . . . C5 C 0.21901(16) 0.51642(14) 0.66321(13) 0.0145(4) Uani 1 1 d . . . . . H5 H 0.156763 0.482100 0.618191 0.017 Uiso 1 1 calc R U . . . C6 C 0.28669(19) 0.35744(15) 0.89253(15) 0.0199(4) Uani 1 1 d . . . . . H6 H 0.315294 0.295801 0.871694 0.024 Uiso 1 1 calc R U . . . C7 C 0.35148(18) 0.43096(15) 0.96048(14) 0.0196(4) Uani 1 1 d . . . . . H7 H 0.430903 0.427179 0.993221 0.024 Uiso 1 1 calc R U . . . C8 C 0.27645(19) 0.51130(15) 0.97085(14) 0.0210(4) Uani 1 1 d . . . . . H8 H 0.297025 0.570845 1.011569 0.025 Uiso 1 1 calc R U . . . C9 C 0.16544(19) 0.48703(16) 0.90977(15) 0.0226(4) Uani 1 1 d . . . . . H9 H 0.098622 0.527298 0.902672 0.027 Uiso 1 1 calc R U . . . C10 C 0.17184(18) 0.39181(16) 0.86106(15) 0.0216(4) Uani 1 1 d . . . . . H10 H 0.110128 0.357334 0.815511 0.026 Uiso 1 1 calc R U . . . C11 C 0.35088(15) 0.37384(13) 0.54340(13) 0.0115(3) Uani 1 1 d . . . . . C12 C 0.45710(16) 0.32983(14) 0.69922(14) 0.0138(4) Uani 1 1 d . . . . . H12 H 0.488822 0.331050 0.771847 0.017 Uiso 1 1 calc R U . . . C13 C 0.4214(2) 0.23252(15) 0.45157(15) 0.0226(4) Uani 1 1 d . . . . . H13A H 0.386819 0.267943 0.391531 0.034 Uiso 0.5 1 d R U P A 1 H13B H 0.493019 0.242844 0.444231 0.034 Uiso 0.5 1 d R U P A 1 H13C H 0.383219 0.164943 0.451031 0.034 Uiso 0.5 1 d R U P A 1 H13D H 0.474204 0.175412 0.472876 0.034 Uiso 0.5 1 d R U P B 2 H13E H 0.448206 0.275421 0.402598 0.034 Uiso 0.5 1 d R U P B 2 H13F H 0.344911 0.206393 0.418435 0.034 Uiso 0.5 1 d R U P B 2 C21 C 0.32900(17) 0.57178(14) 0.43901(14) 0.0164(4) Uani 1 1 d . . . C 2 H21 H 0.386872 0.566590 0.502009 0.020 Uiso 1 1 d R U . C 2 C22 C 0.34654(16) 0.51114(14) 0.35745(14) 0.0157(4) Uani 1 1 d . . . C 2 H22 H 0.420439 0.474293 0.374180 0.019 Uiso 1 1 d R U . C 2 C23 C 0.29458(17) 0.53493(16) 0.24352(14) 0.0194(4) Uani 1 1 d . . . C 2 H23A H 0.349438 0.515091 0.203210 0.023 Uiso 1 1 calc R U . C 2 H23B H 0.281692 0.609175 0.235204 0.023 Uiso 1 1 calc R U . C 2 C24 C 0.18099(18) 0.47930(16) 0.20016(14) 0.0207(4) Uani 1 1 d . . . C 2 H24A H 0.136243 0.516795 0.139029 0.025 Uiso 1 1 calc R U . C 2 H24B H 0.197180 0.410635 0.176952 0.025 Uiso 1 1 calc R U . C 2 C25 C 0.11005(17) 0.46889(16) 0.27715(14) 0.0185(4) Uani 1 1 d . . . C 2 H25 H 0.054290 0.414439 0.269214 0.022 Uiso 1 1 d R U . C 2 C26 C 0.09382(17) 0.54250(15) 0.34482(15) 0.0197(4) Uani 1 1 d . . . C 2 H26 H 0.032915 0.533953 0.380290 0.024 Uiso 1 1 d R U . C 2 C27 C 0.13778(19) 0.65085(16) 0.34870(16) 0.0241(5) Uani 1 1 d . . . C 2 H27A H 0.081166 0.697112 0.366749 0.029 Uiso 1 1 calc R U . C 2 H27B H 0.145699 0.670356 0.279385 0.029 Uiso 1 1 calc R U . C 2 C28 C 0.25379(19) 0.66427(15) 0.42785(16) 0.0240(5) Uani 1 1 d . . . C 2 H28A H 0.294425 0.722596 0.406649 0.029 Uiso 1 1 calc R U . C 2 H28B H 0.240176 0.680776 0.495933 0.029 Uiso 1 1 calc R U . 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 Rh1 0.01118(7) 0.01375(7) 0.00729(7) 0.00106(5) 0.00162(5) -0.00088(5) I1 0.01994(7) 0.01928(7) 0.01351(6) 0.00259(5) 0.00057(5) -0.00702(5) Fe1 0.01492(13) 0.01182(12) 0.00816(12) -0.00021(10) 0.00429(10) 0.00018(10) N1 0.0113(7) 0.0127(7) 0.0086(7) 0.0006(6) 0.0026(6) 0.0005(6) N2 0.0150(8) 0.0145(7) 0.0101(7) -0.0013(6) 0.0032(6) 0.0009(6) N3 0.0159(8) 0.0147(8) 0.0155(8) 0.0035(6) 0.0033(6) 0.0027(6) C1 0.0151(9) 0.0130(8) 0.0082(8) 0.0013(7) 0.0050(7) 0.0001(7) C2 0.0180(10) 0.0166(9) 0.0119(9) 0.0001(7) 0.0057(7) -0.0042(7) C3 0.0290(11) 0.0120(9) 0.0145(9) -0.0002(7) 0.0088(8) -0.0014(8) C4 0.0250(11) 0.0177(9) 0.0141(9) 0.0045(7) 0.0081(8) 0.0090(8) C5 0.0147(9) 0.0190(9) 0.0093(8) 0.0015(7) 0.0022(7) 0.0022(7) C6 0.0299(11) 0.0137(9) 0.0187(10) 0.0029(8) 0.0109(8) -0.0009(8) C7 0.0236(11) 0.0224(10) 0.0120(9) 0.0053(8) 0.0028(8) -0.0007(8) C8 0.0362(12) 0.0197(10) 0.0095(9) -0.0008(8) 0.0103(8) -0.0027(9) C9 0.0244(11) 0.0299(11) 0.0180(10) 0.0048(9) 0.0138(9) 0.0045(9) C10 0.0236(11) 0.0254(11) 0.0176(10) 0.0012(8) 0.0088(8) -0.0089(9) C11 0.0126(9) 0.0128(8) 0.0102(8) -0.0006(7) 0.0049(7) -0.0021(7) C12 0.0129(9) 0.0156(9) 0.0126(9) 0.0041(7) 0.0026(7) 0.0003(7) C13 0.0329(12) 0.0202(10) 0.0163(10) -0.0065(8) 0.0089(9) 0.0022(9) C21 0.0173(10) 0.0165(9) 0.0141(9) 0.0023(7) 0.0017(7) -0.0063(7) C22 0.0116(9) 0.0214(10) 0.0151(9) 0.0046(8) 0.0054(7) -0.0020(7) C23 0.0189(10) 0.0273(11) 0.0133(9) 0.0038(8) 0.0065(8) 0.0015(8) C24 0.0252(11) 0.0261(10) 0.0095(9) 0.0032(8) 0.0020(8) -0.0009(9) C25 0.0141(10) 0.0263(10) 0.0114(9) 0.0073(8) -0.0033(7) -0.0020(8) C26 0.0128(9) 0.0273(11) 0.0191(10) 0.0104(8) 0.0039(8) 0.0043(8) C27 0.0267(12) 0.0214(10) 0.0268(11) 0.0071(9) 0.0117(9) 0.0106(9) C28 0.0339(13) 0.0167(10) 0.0231(11) -0.0003(8) 0.0106(9) -0.0005(9) 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' I I -0.4742 1.8119 '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' Rh Rh -1.1178 0.9187 '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 C11 Rh1 C21 90.36(7) . . ? C11 Rh1 C22 95.44(7) . . ? C21 Rh1 C22 38.84(7) . . ? C11 Rh1 C25 163.11(7) . . ? C21 Rh1 C25 97.68(7) . . ? C22 Rh1 C25 81.95(7) . . ? C11 Rh1 C26 160.76(7) . . ? C21 Rh1 C26 81.35(8) . . ? C22 Rh1 C26 88.96(7) . . ? C25 Rh1 C26 36.11(8) . . ? C11 Rh1 I1 86.93(5) . . ? C21 Rh1 I1 161.56(5) . . ? C22 Rh1 I1 159.60(5) . . ? C25 Rh1 I1 89.91(5) . . ? C26 Rh1 I1 95.45(5) . . ? C1 Fe1 C9 158.02(8) . . ? C1 Fe1 C4 68.34(7) . . ? C9 Fe1 C4 103.92(8) . . ? C1 Fe1 C8 161.06(8) . . ? C9 Fe1 C8 40.69(9) . . ? C4 Fe1 C8 119.72(8) . . ? C1 Fe1 C10 124.17(8) . . ? C9 Fe1 C10 40.79(8) . . ? C4 Fe1 C10 120.76(9) . . ? C8 Fe1 C10 68.45(8) . . ? C1 Fe1 C3 68.45(7) . . ? C9 Fe1 C3 119.92(8) . . ? C4 Fe1 C3 40.74(8) . . ? C8 Fe1 C3 105.66(8) . . ? C10 Fe1 C3 156.36(9) . . ? C1 Fe1 C5 40.77(7) . . ? C9 Fe1 C5 120.16(8) . . ? C4 Fe1 C5 40.67(7) . . ? C8 Fe1 C5 155.71(8) . . ? C10 Fe1 C5 106.82(8) . . ? C3 Fe1 C5 68.64(8) . . ? C1 Fe1 C2 40.99(7) . . ? C9 Fe1 C2 157.32(8) . . ? C4 Fe1 C2 68.75(8) . . ? C8 Fe1 C2 122.95(8) . . ? C10 Fe1 C2 161.30(8) . . ? C3 Fe1 C2 40.77(8) . . ? C5 Fe1 C2 69.04(8) . . ? C1 Fe1 C6 111.05(8) . . ? C9 Fe1 C6 68.29(8) . . ? C4 Fe1 C6 158.57(9) . . ? C8 Fe1 C6 68.18(8) . . ? C10 Fe1 C6 40.52(8) . . ? C3 Fe1 C6 160.49(9) . . ? C5 Fe1 C6 124.63(8) . . ? C2 Fe1 C6 125.86(8) . . ? C1 Fe1 C7 126.46(8) . . ? C9 Fe1 C7 68.30(8) . . ? C4 Fe1 C7 157.14(8) . . ? C8 Fe1 C7 40.58(8) . . ? C10 Fe1 C7 68.20(8) . . ? C3 Fe1 C7 123.08(8) . . ? C5 Fe1 C7 161.81(8) . . ? C2 Fe1 C7 109.73(8) . . ? C6 Fe1 C7 40.39(8) . . ? C12 N1 C11 108.61(15) . . ? C12 N1 C1 126.53(15) . . ? C11 N1 C1 124.82(15) . . ? C11 N2 N3 114.66(14) . . ? C11 N2 C13 126.67(16) . . ? N3 N2 C13 118.65(15) . . ? C12 N3 N2 102.73(15) . . ? C5 C1 N1 124.99(16) . . ? C5 C1 C2 109.12(16) . . ? N1 C1 C2 125.69(17) . . ? C5 C1 Fe1 70.16(10) . . ? N1 C1 Fe1 129.68(12) . . ? C2 C1 Fe1 70.25(10) . . ? C3 C2 C1 106.72(17) . . ? C3 C2 Fe1 69.29(11) . . ? C1 C2 Fe1 68.76(10) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? Fe1 C2 H2 126.9 . . ? C4 C3 C2 108.42(16) . . ? C4 C3 Fe1 69.50(11) . . ? C2 C3 Fe1 69.93(10) . . ? C4 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? Fe1 C3 H3 126.3 . . ? C5 C4 C3 108.48(17) . . ? C5 C4 Fe1 69.90(10) . . ? C3 C4 Fe1 69.75(11) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe1 C4 H4 126.2 . . ? C4 C5 C1 107.25(17) . . ? C4 C5 Fe1 69.42(10) . . ? C1 C5 Fe1 69.07(10) . . ? C4 C5 H5 126.4 . . ? C1 C5 H5 126.4 . . ? Fe1 C5 H5 126.7 . . ? C10 C6 C7 108.23(18) . . ? C10 C6 Fe1 69.37(11) . . ? C7 C6 Fe1 69.95(11) . . ? C10 C6 H6 125.9 . . ? C7 C6 H6 125.9 . . ? Fe1 C6 H6 126.4 . . ? C6 C7 C8 107.84(19) . . ? C6 C7 Fe1 69.66(11) . . ? C8 C7 Fe1 69.18(11) . . ? C6 C7 H7 126.1 . . ? C8 C7 H7 126.1 . . ? Fe1 C7 H7 126.6 . . ? C9 C8 C7 108.07(18) . . ? C9 C8 Fe1 69.50(11) . . ? C7 C8 Fe1 70.24(11) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? Fe1 C8 H8 125.9 . . ? C8 C9 C10 107.96(18) . . ? C8 C9 Fe1 69.81(11) . . ? C10 C9 Fe1 69.78(11) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? Fe1 C9 H9 126.0 . . ? C6 C10 C9 107.89(18) . . ? C6 C10 Fe1 70.11(11) . . ? C9 C10 Fe1 69.44(11) . . ? C6 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? Fe1 C10 H10 126.0 . . ? N2 C11 N1 102.30(15) . . ? N2 C11 Rh1 129.70(13) . . ? N1 C11 Rh1 127.75(13) . . ? N3 C12 N1 111.69(16) . . ? N3 C12 H12 124.2 . . ? N1 C12 H12 124.2 . . ? N2 C13 H13A 110.0 . . ? N2 C13 H13B 104.5 . . ? H13A C13 H13B 93.6 . . ? N2 C13 H13C 111.7 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 125.7 . . ? N2 C13 H13D 109.5 . . ? N2 C13 H13E 109.5 . . ? H13D C13 H13E 109.5 . . ? N2 C13 H13F 109.4 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? C22 C21 C28 125.89(17) . . ? C22 C21 Rh1 70.80(10) . . ? C28 C21 Rh1 110.47(13) . . ? C22 C21 H21 115.1 . . ? C28 C21 H21 115.9 . . ? Rh1 C21 H21 106.0 . . ? C21 C22 C23 123.54(17) . . ? C21 C22 Rh1 70.37(10) . . ? C23 C22 Rh1 112.87(13) . . ? C21 C22 H22 113.9 . . ? C23 C22 H22 116.4 . . ? Rh1 C22 H22 109.8 . . ? C22 C23 C24 112.47(16) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 113.29(16) . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 126.09(19) . . ? C26 C25 Rh1 72.37(11) . . ? C24 C25 Rh1 106.84(13) . . ? C26 C25 H25 112.4 . . ? C24 C25 H25 119.5 . . ? Rh1 C25 H25 103.8 . . ? C25 C26 C27 125.25(18) . . ? C25 C26 Rh1 71.52(11) . . ? C27 C26 Rh1 111.01(13) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 113.0 . . ? Rh1 C26 H26 103.7 . . ? C26 C27 C28 112.43(16) . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C21 C28 C27 113.49(17) . . ? C21 C28 H28A 108.9 . . ? C27 C28 H28A 108.9 . . ? C21 C28 H28B 108.9 . . ? C27 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? 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 Rh1 C11 2.0158(18) . ? Rh1 C21 2.1180(18) . ? Rh1 C22 2.1237(18) . ? Rh1 C25 2.2090(18) . ? Rh1 C26 2.2198(19) . ? Rh1 I1 2.68494(19) . ? Fe1 C1 2.0321(17) . ? Fe1 C9 2.0386(19) . ? Fe1 C4 2.0401(19) . ? Fe1 C8 2.0427(18) . ? Fe1 C10 2.043(2) . ? Fe1 C3 2.0434(19) . ? Fe1 C5 2.0464(18) . ? Fe1 C2 2.0520(18) . ? Fe1 C6 2.0529(19) . ? Fe1 C7 2.0567(19) . ? N1 C12 1.370(2) . ? N1 C11 1.376(2) . ? N1 C1 1.428(2) . ? N2 C11 1.335(2) . ? N2 N3 1.386(2) . ? N2 C13 1.454(2) . ? N3 C12 1.299(2) . ? C1 C5 1.421(3) . ? C1 C2 1.430(3) . ? C2 C3 1.427(3) . ? C2 H2 0.9500 . ? C3 C4 1.422(3) . ? C3 H3 0.9500 . ? C4 C5 1.420(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.418(3) . ? C6 C7 1.419(3) . ? C6 H6 0.9500 . ? C7 C8 1.422(3) . ? C7 H7 0.9500 . ? C8 C9 1.419(3) . ? C8 H8 0.9500 . ? C9 C10 1.422(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9307 . ? C13 H13B 0.9063 . ? C13 H13C 0.9999 . ? C13 H13D 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? C21 C22 1.410(3) . ? C21 C28 1.503(3) . ? C21 H21 0.9515 . ? C22 C23 1.527(3) . ? C22 H22 0.9905 . ? C23 C24 1.534(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.504(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.373(3) . ? C25 H25 0.9702 . ? C26 C27 1.516(3) . ? C26 H26 0.9783 . ? C27 C28 1.538(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ?