# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_i0438 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 Fe N2' _chemical_formula_weight 292.16 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.082(2) _cell_length_b 13.8650(10) _cell_length_c 9.3820(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2612.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7364 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.46 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8111 _exptl_absorpt_correction_T_max 0.9698 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 32 _diffrn_source_power 1.60 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 15758 _diffrn_reflns_av_R_equivalents 0.1050 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2297 _reflns_number_gt 1538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie. 2006)' _computing_cell_refinement 'X-Area (Stoe & Cie. 2006)' _computing_data_reduction 'X-Area (Stoe & Cie. 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 win. (Farrugia 2008)' _computing_publication_material 'PLATON (Spek 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2297 _refine_ls_number_parameters 181 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.877 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.16623(14) 0.45507(19) 0.3478(3) 0.0329(6) Uani 1 1 d . . . C2 C 0.16449(15) 0.5373(2) 0.2536(3) 0.0344(7) Uani 1 1 d . . . H2 H 0.2020 0.5681 0.2118 0.041 Uiso 1 1 calc R . . C3 C 0.09700(14) 0.5640(2) 0.2348(3) 0.0371(7) Uani 1 1 d . . . H3A H 0.0817 0.6162 0.1780 0.044 Uiso 1 1 calc R . . C4 C 0.05593(15) 0.5004(2) 0.3142(3) 0.0385(7) Uani 1 1 d . . . H4A H 0.0088 0.5029 0.3210 0.046 Uiso 1 1 calc R . . C5 C 0.09847(13) 0.4320(2) 0.3819(3) 0.0339(7) Uani 1 1 d . . . H5A H 0.0843 0.3798 0.4400 0.041 Uiso 1 1 calc R . . C6 C 0.14288(14) 0.2947(2) 0.0893(3) 0.0333(7) Uani 1 1 d . . . C7 C 0.16133(15) 0.3702(2) -0.0063(3) 0.0362(7) Uani 1 1 d . . . H7A H 0.2054 0.3865 -0.0341 0.043 Uiso 1 1 calc R . . C8 C 0.10169(15) 0.4171(2) -0.0528(3) 0.0402(7) Uani 1 1 d . . . H8A H 0.0992 0.4698 -0.1173 0.048 Uiso 1 1 calc R . . C9 C 0.04675(15) 0.3710(2) 0.0144(3) 0.0390(7) Uani 1 1 d . . . H9A H 0.0012 0.3876 0.0030 0.047 Uiso 1 1 calc R . . C10 C 0.07228(15) 0.2951(2) 0.1025(3) 0.0364(7) Uani 1 1 d . . . H10A H 0.0466 0.2525 0.1597 0.044 Uiso 1 1 calc R . . C11 C 0.28193(12) 0.3839(2) 0.3420(3) 0.0321(6) Uani 1 1 d . . . C12 C 0.30217(14) 0.4196(2) 0.2088(3) 0.0336(6) Uani 1 1 d . . . H12A H 0.2741 0.4622 0.1570 0.040 Uiso 1 1 calc R . . C13 C 0.36391(14) 0.3921(2) 0.1525(3) 0.0365(7) Uani 1 1 d . . . H13A H 0.3770 0.4164 0.0620 0.044 Uiso 1 1 calc R . . C14 C 0.40620(14) 0.3308(2) 0.2247(3) 0.0364(7) Uani 1 1 d . . . H14A H 0.4482 0.3136 0.1857 0.044 Uiso 1 1 calc R . . C15 C 0.38581(15) 0.2947(2) 0.3567(3) 0.0363(6) Uani 1 1 d . . . H15A H 0.4140 0.2516 0.4075 0.044 Uiso 1 1 calc R . . C16 C 0.32522(14) 0.3209(2) 0.4140(3) 0.0334(7) Uani 1 1 d . . . H16A H 0.3124 0.2957 0.5041 0.040 Uiso 1 1 calc R . . N1 N 0.22129(11) 0.40659(19) 0.4067(3) 0.0347(6) Uani 1 1 d . . . H1 H 0.2100(15) 0.373(2) 0.474(4) 0.042 Uiso 1 1 d . . . Fe Fe 0.11013(2) 0.42552(3) 0.16560(4) 0.03090(12) Uani 1 1 d . . . N2 N 0.18657(13) 0.22575(19) 0.1535(3) 0.0390(6) Uani 1 1 d D . . H2A H 0.2242(12) 0.252(2) 0.186(3) 0.047 Uiso 1 1 d D . . H2B H 0.1677(15) 0.204(2) 0.232(3) 0.047 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0375(15) 0.0331(14) 0.0280(15) -0.0040(14) -0.0028(14) 0.0013(12) C2 0.0377(16) 0.0322(14) 0.0334(16) -0.0026(14) -0.0046(15) -0.0029(12) C3 0.045(2) 0.0316(15) 0.0350(14) -0.0045(14) -0.0088(13) 0.0052(14) C4 0.0352(15) 0.0436(16) 0.0368(18) -0.0086(15) 0.0014(14) 0.0053(14) C5 0.0351(16) 0.0356(15) 0.0311(15) -0.0010(13) 0.0014(11) 0.0004(13) C6 0.0373(16) 0.0359(16) 0.0267(16) -0.0073(13) 0.0014(13) 0.0007(14) C7 0.0375(17) 0.0451(18) 0.0260(16) -0.0066(14) 0.0039(13) -0.0046(14) C8 0.0485(18) 0.0425(16) 0.0297(14) 0.0013(14) -0.0055(14) -0.0028(17) C9 0.0369(17) 0.0449(19) 0.0351(17) -0.0054(15) -0.0080(14) -0.0014(14) C10 0.0389(17) 0.0372(16) 0.0331(16) -0.0076(14) 0.0043(14) -0.0062(14) C11 0.0298(14) 0.0340(13) 0.0325(15) -0.0027(15) -0.0033(14) -0.0038(11) C12 0.0353(15) 0.0383(15) 0.0272(14) 0.0067(14) -0.0041(11) -0.0039(14) C13 0.0399(15) 0.0408(15) 0.0288(15) 0.0016(15) -0.0002(14) -0.0078(12) C14 0.0307(17) 0.0423(17) 0.0363(16) -0.0027(14) -0.0010(12) -0.0012(12) C15 0.0379(14) 0.0358(14) 0.0351(16) 0.0008(13) -0.0046(15) 0.0013(14) C16 0.0374(16) 0.0348(16) 0.0279(15) 0.0031(13) -0.0036(13) -0.0020(13) N1 0.0342(13) 0.0426(17) 0.0273(12) 0.0068(12) -0.0011(10) 0.0012(11) Fe 0.03174(19) 0.0329(2) 0.02801(19) -0.0018(2) -0.0019(2) 0.0004(2) N2 0.0416(14) 0.0411(14) 0.0342(14) -0.0043(14) -0.0012(13) 0.0061(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.407(4) . ? C1 C5 1.434(4) . ? C1 C2 1.443(4) . ? C1 Fe 2.088(3) . ? C2 C3 1.416(4) . ? C2 Fe 2.068(3) . ? C2 H2 0.9500 . ? C3 C4 1.419(4) . ? C3 Fe 2.044(3) . ? C3 H3A 0.9500 . ? C4 C5 1.426(4) . ? C4 Fe 2.051(3) . ? C4 H4A 0.9500 . ? C5 Fe 2.045(3) . ? C5 H5A 0.9500 . ? C6 C10 1.423(4) . ? C6 C7 1.428(4) . ? C6 N2 1.430(4) . ? C6 Fe 2.058(3) . ? C7 C8 1.430(4) . ? C7 Fe 2.061(3) . ? C7 H7A 0.9500 . ? C8 C9 1.423(4) . ? C8 Fe 2.059(3) . ? C8 H8A 0.9500 . ? C9 C10 1.433(4) . ? C9 Fe 2.050(3) . ? C9 H9A 0.9500 . ? C10 Fe 2.049(3) . ? C10 H10A 0.9500 . ? C11 N1 1.397(3) . ? C11 C12 1.404(4) . ? C11 C16 1.406(4) . ? C12 C13 1.401(4) . ? C12 H12A 0.9500 . ? C13 C14 1.380(4) . ? C13 H13A 0.9500 . ? C14 C15 1.397(4) . ? C14 H14A 0.9500 . ? C15 C16 1.379(4) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N1 H1 0.82(3) . ? N2 H2A 0.89(2) . ? N2 H2B 0.89(2) . ? 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 N1 C1 C5 123.5(3) . . ? N1 C1 C2 129.6(3) . . ? C5 C1 C2 106.9(3) . . ? N1 C1 Fe 130.7(2) . . ? C5 C1 Fe 68.10(16) . . ? C2 C1 Fe 68.95(16) . . ? C3 C2 C1 107.8(3) . . ? C3 C2 Fe 68.94(16) . . ? C1 C2 Fe 70.41(16) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe C2 H2 126.1 . . ? C2 C3 C4 109.2(3) . . ? C2 C3 Fe 70.78(16) . . ? C4 C3 Fe 69.98(16) . . ? C2 C3 H3A 125.4 . . ? C4 C3 H3A 125.4 . . ? Fe C3 H3A 125.4 . . ? C3 C4 C5 107.4(3) . . ? C3 C4 Fe 69.47(16) . . ? C5 C4 Fe 69.41(16) . . ? C3 C4 H4A 126.3 . . ? C5 C4 H4A 126.3 . . ? Fe C4 H4A 126.4 . . ? C4 C5 C1 108.7(3) . . ? C4 C5 Fe 69.84(16) . . ? C1 C5 Fe 71.32(17) . . ? C4 C5 H5A 125.7 . . ? C1 C5 H5A 125.7 . . ? Fe C5 H5A 124.8 . . ? C10 C6 C7 108.1(3) . . ? C10 C6 N2 125.2(3) . . ? C7 C6 N2 126.6(3) . . ? C10 C6 Fe 69.37(18) . . ? C7 C6 Fe 69.81(17) . . ? N2 C6 Fe 129.7(2) . . ? C6 C7 C8 107.9(3) . . ? C6 C7 Fe 69.63(16) . . ? C8 C7 Fe 69.63(16) . . ? C6 C7 H7A 126.0 . . ? C8 C7 H7A 126.0 . . ? Fe C7 H7A 126.3 . . ? C9 C8 C7 108.1(3) . . ? C9 C8 Fe 69.40(16) . . ? C7 C8 Fe 69.74(16) . . ? C9 C8 H8A 126.0 . . ? C7 C8 H8A 126.0 . . ? Fe C8 H8A 126.5 . . ? C8 C9 C10 107.9(3) . . ? C8 C9 Fe 70.09(16) . . ? C10 C9 Fe 69.50(17) . . ? C8 C9 H9A 126.0 . . ? C10 C9 H9A 126.0 . . ? Fe C9 H9A 126.0 . . ? C6 C10 C9 108.0(3) . . ? C6 C10 Fe 70.08(18) . . ? C9 C10 Fe 69.59(17) . . ? C6 C10 H10A 126.0 . . ? C9 C10 H10A 126.0 . . ? Fe C10 H10A 125.9 . . ? N1 C11 C12 124.0(3) . . ? N1 C11 C16 118.1(3) . . ? C12 C11 C16 117.9(3) . . ? C13 C12 C11 119.7(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C12 121.8(3) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C13 C14 C15 118.4(3) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? C16 C15 C14 120.6(3) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C11 121.5(3) . . ? C15 C16 H16A 119.3 . . ? C11 C16 H16A 119.3 . . ? C11 N1 C1 128.5(3) . . ? C11 N1 H1 117(2) . . ? C1 N1 H1 111(2) . . ? C3 Fe C5 68.22(12) . . ? C3 Fe C10 150.81(12) . . ? C5 Fe C10 106.44(12) . . ? C3 Fe C9 119.08(12) . . ? C5 Fe C9 129.17(12) . . ? C10 Fe C9 40.91(12) . . ? C3 Fe C4 40.55(12) . . ? C5 Fe C4 40.75(12) . . ? C10 Fe C4 116.51(12) . . ? C9 Fe C4 109.11(12) . . ? C3 Fe C6 168.43(12) . . ? C5 Fe C6 114.87(12) . . ? C10 Fe C6 40.55(11) . . ? C9 Fe C6 68.45(12) . . ? C4 Fe C6 148.47(12) . . ? C3 Fe C8 111.01(13) . . ? C5 Fe C8 168.68(11) . . ? C10 Fe C8 68.40(13) . . ? C9 Fe C8 40.51(12) . . ? C4 Fe C8 131.40(13) . . ? C6 Fe C8 68.29(12) . . ? C3 Fe C7 131.47(12) . . ? C5 Fe C7 148.24(12) . . ? C10 Fe C7 68.32(12) . . ? C9 Fe C7 68.35(12) . . ? C4 Fe C7 170.12(12) . . ? C6 Fe C7 40.57(11) . . ? C8 Fe C7 40.63(11) . . ? C3 Fe C2 40.28(11) . . ? C5 Fe C2 68.36(12) . . ? C10 Fe C2 166.60(12) . . ? C9 Fe C2 151.69(12) . . ? C4 Fe C2 68.23(12) . . ? C6 Fe C2 129.12(12) . . ? C8 Fe C2 118.90(12) . . ? C7 Fe C2 109.15(12) . . ? C3 Fe C1 68.00(11) . . ? C5 Fe C1 40.58(11) . . ? C10 Fe C1 127.58(11) . . ? C9 Fe C1 166.84(12) . . ? C4 Fe C1 68.31(11) . . ? C6 Fe C1 106.59(11) . . ? C8 Fe C1 150.48(12) . . ? C7 Fe C1 116.40(11) . . ? C2 Fe C1 40.64(11) . . ? C6 N2 H2A 113(2) . . ? C6 N2 H2B 109(2) . . ? H2A N2 H2B 102(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.306 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.052 _database_code_depnum_ccdc_archive 'CCDC 961488' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_i0593 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H35 B F4 Fe N2' _chemical_formula_weight 518.22 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_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' _cell_length_a 26.917(2) _cell_length_b 13.8187(7) _cell_length_c 17.8272(14) _cell_angle_alpha 90.00 _cell_angle_beta 125.348(5) _cell_angle_gamma 90.00 _cell_volume 5408.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22872 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 25.63 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8521 _exptl_absorpt_correction_T_max 0.9453 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 4846 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.24 _reflns_number_total 4846 _reflns_number_gt 3647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie. 2006)' _computing_cell_refinement 'X-Area (Stoe & Cie. 2006)' _computing_data_reduction 'X-Area (Stoe & Cie. 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 win. (Farrugia 2008)' _computing_publication_material 'PLATON (Spek 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4846 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.26812(10) 0.32780(16) 0.36781(14) 0.0428(5) Uani 1 1 d . . . H1 H 0.2494 0.3382 0.3989 0.051 Uiso 1 1 calc R . . C2 C 0.36683(10) 0.32324(18) 0.38906(15) 0.0456(5) Uani 1 1 d . . . C3 C 0.38263(11) 0.3886(2) 0.34304(16) 0.0540(6) Uani 1 1 d . . . H3 H 0.3707 0.4532 0.3282 0.065 Uiso 1 1 d R . . C4 C 0.41990(11) 0.3362(2) 0.32472(18) 0.0594(7) Uani 1 1 d . . . H4 H 0.4367 0.3609 0.2956 0.071 Uiso 1 1 d R . . C5 C 0.42714(11) 0.2400(2) 0.35853(17) 0.0575(6) Uani 1 1 d . . . H5 H 0.4488 0.1906 0.3541 0.069 Uiso 1 1 d R . . C6 C 0.39524(10) 0.23188(19) 0.40063(16) 0.0509(6) Uani 1 1 d . . . H6 H 0.3936 0.1774 0.4300 0.061 Uiso 1 1 d R . . C7 C 0.25012(10) 0.27127(17) 0.22381(14) 0.0428(5) Uani 1 1 d . . . C8 C 0.26687(10) 0.17492(17) 0.21668(16) 0.0476(6) Uani 1 1 d . . . H8 H 0.2663 0.1198 0.2464 0.057 Uiso 1 1 d R . . C9 C 0.28450(11) 0.1795(2) 0.15520(17) 0.0554(6) Uani 1 1 d . . . H9 H 0.2982 0.1276 0.1384 0.066 Uiso 1 1 d R . . C10 C 0.27799(11) 0.2765(2) 0.12385(16) 0.0554(6) Uani 1 1 d . . . H10 H 0.2862 0.2989 0.0829 0.066 Uiso 1 1 d R . . C11 C 0.25614(10) 0.33359(18) 0.16516(15) 0.0488(6) Uani 1 1 d . . . H11 H 0.2475 0.3997 0.1559 0.059 Uiso 1 1 d R . . C12 C 0.35957(11) 0.36747(18) 0.51814(14) 0.0497(6) Uani 1 1 d . . . H12A H 0.3911 0.3177 0.5550 0.060 Uiso 1 1 calc R . . H12B H 0.3294 0.3628 0.5328 0.060 Uiso 1 1 calc R . . C13 C 0.39009(11) 0.46823(18) 0.54893(16) 0.0529(6) Uani 1 1 d . . . C14 C 0.45127(13) 0.4712(2) 0.5610(2) 0.0711(8) Uani 1 1 d . . . H14A H 0.4443 0.4637 0.5010 0.085 Uiso 1 1 calc R . . H14B H 0.4773 0.4184 0.6017 0.085 Uiso 1 1 calc R . . H14C H 0.4713 0.5333 0.5881 0.085 Uiso 1 1 calc R . . C15 C 0.34703(16) 0.5463(2) 0.4820(2) 0.0764(9) Uani 1 1 d . . . H15A H 0.3081 0.5424 0.4748 0.092 Uiso 1 1 calc R . . H15B H 0.3401 0.5364 0.4221 0.092 Uiso 1 1 calc R . . H15C H 0.3652 0.6102 0.5060 0.092 Uiso 1 1 calc R . . C16 C 0.40239(17) 0.4870(2) 0.6441(2) 0.0788(9) Uani 1 1 d . . . H16A H 0.4296 0.4367 0.6874 0.095 Uiso 1 1 calc R . . H16B H 0.3638 0.4855 0.6380 0.095 Uiso 1 1 calc R . . H16C H 0.4216 0.5505 0.6669 0.095 Uiso 1 1 calc R . . C17 C 0.16457(10) 0.27621(18) 0.23972(16) 0.0483(5) Uani 1 1 d . . . H17 H 0.1607 0.2041 0.2365 0.058 Uiso 1 1 calc R . . C18 C 0.12329(12) 0.3150(2) 0.13871(18) 0.0651(7) Uani 1 1 d . . . H18 H 0.1398 0.2938 0.1035 0.078 Uiso 1 1 calc R . . C19 C 0.05970(13) 0.2742(3) 0.0946(2) 0.0842(10) Uani 1 1 d . . . H19A H 0.0613 0.2026 0.0946 0.101 Uiso 1 1 calc R . . H19B H 0.0328 0.2963 0.0300 0.101 Uiso 1 1 calc R . . C20 C 0.03343(12) 0.3074(3) 0.1477(2) 0.0706(8) Uani 1 1 d . . . H20 H -0.0082 0.2794 0.1184 0.085 Uiso 1 1 calc R . . C21 C 0.07512(13) 0.2716(3) 0.2450(2) 0.0785(9) Uani 1 1 d . . . H21A H 0.0765 0.2000 0.2450 0.094 Uiso 1 1 calc R . . H21B H 0.0588 0.2915 0.2802 0.094 Uiso 1 1 calc R . . C22 C 0.14009(12) 0.3121(2) 0.29216(18) 0.0618(7) Uani 1 1 d . . . H22 H 0.1666 0.2887 0.3572 0.074 Uiso 1 1 calc R . . C23 C 0.13642(15) 0.4215(2) 0.2908(2) 0.0808(9) Uani 1 1 d . . . H23A H 0.1204 0.4426 0.3261 0.097 Uiso 1 1 calc R . . H23B H 0.1777 0.4490 0.3208 0.097 Uiso 1 1 calc R . . C24 C 0.09569(16) 0.4587(3) 0.1938(3) 0.0894(11) Uani 1 1 d . . . H24 H 0.0942 0.5310 0.1946 0.107 Uiso 1 1 calc R . . C25 C 0.12123(15) 0.4267(3) 0.1408(2) 0.0898(11) Uani 1 1 d . . . H25A H 0.1628 0.4532 0.1705 0.108 Uiso 1 1 calc R . . H25B H 0.0953 0.4520 0.0771 0.108 Uiso 1 1 calc R . . C26 C 0.02979(15) 0.4170(3) 0.1448(3) 0.0921(11) Uani 1 1 d . . . H26A H 0.0115 0.4397 0.1765 0.110 Uiso 1 1 calc R . . H26B H 0.0039 0.4395 0.0802 0.110 Uiso 1 1 calc R . . B1 B 0.28214(18) 0.0788(2) 0.4517(2) 0.0643(9) Uani 1 1 d . . . F1 F 0.26790(11) 0.16316(13) 0.47601(14) 0.0941(6) Uani 1 1 d . . . F2 F 0.27369(10) 0.00174(13) 0.49259(13) 0.0901(6) Uani 1 1 d . . . F3 F 0.24456(15) 0.07087(15) 0.35696(14) 0.1281(11) Uani 1 1 d . . . F4 F 0.34056(14) 0.0810(2) 0.4799(2) 0.1586(14) Uani 1 1 d . . . Fe1 Fe 0.335644(14) 0.27183(2) 0.26656(2) 0.04347(12) Uani 1 1 d . . . N1 N 0.32814(8) 0.34374(14) 0.41832(12) 0.0445(4) Uani 1 1 d . . . N2 N 0.23068(8) 0.29966(13) 0.28099(12) 0.0411(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0447(11) 0.0440(12) 0.0383(11) 0.0007(9) 0.0233(10) -0.0026(10) C2 0.0378(11) 0.0530(14) 0.0387(11) -0.0030(10) 0.0180(9) -0.0111(10) C3 0.0545(14) 0.0545(15) 0.0487(13) -0.0025(11) 0.0274(12) -0.0158(11) C4 0.0501(13) 0.0778(19) 0.0537(14) -0.0058(13) 0.0319(12) -0.0184(13) C5 0.0419(12) 0.0731(18) 0.0513(14) -0.0026(12) 0.0235(11) -0.0033(12) C6 0.0400(11) 0.0582(14) 0.0443(12) 0.0045(11) 0.0187(10) -0.0018(11) C7 0.0394(11) 0.0475(12) 0.0344(10) -0.0017(10) 0.0172(9) -0.0048(10) C8 0.0433(12) 0.0434(13) 0.0477(12) -0.0042(10) 0.0215(10) -0.0053(10) C9 0.0515(13) 0.0615(16) 0.0519(14) -0.0135(12) 0.0293(12) -0.0044(12) C10 0.0530(13) 0.0707(17) 0.0394(12) -0.0020(12) 0.0250(11) -0.0063(12) C11 0.0487(12) 0.0534(14) 0.0364(11) 0.0013(10) 0.0201(10) -0.0029(10) C12 0.0523(13) 0.0559(14) 0.0333(11) -0.0029(10) 0.0205(10) -0.0042(11) C13 0.0548(14) 0.0490(14) 0.0433(13) -0.0048(10) 0.0216(11) -0.0001(11) C14 0.0562(16) 0.0753(19) 0.0654(17) -0.0210(14) 0.0257(14) -0.0225(14) C15 0.090(2) 0.0556(17) 0.0689(18) 0.0024(14) 0.0372(17) 0.0138(15) C16 0.099(2) 0.073(2) 0.0529(16) -0.0188(14) 0.0367(17) -0.0104(17) C17 0.0392(11) 0.0462(13) 0.0540(13) 0.0000(11) 0.0237(10) -0.0065(10) C18 0.0455(13) 0.094(2) 0.0487(14) -0.0068(14) 0.0234(12) -0.0056(14) C19 0.0487(15) 0.118(3) 0.0651(18) -0.0205(18) 0.0212(14) -0.0086(17) C20 0.0432(14) 0.092(2) 0.0713(18) 0.0043(16) 0.0300(13) -0.0039(14) C21 0.0536(15) 0.102(2) 0.088(2) 0.0183(19) 0.0454(16) 0.0052(16) C22 0.0520(14) 0.0784(18) 0.0525(14) 0.0060(13) 0.0288(12) 0.0045(13) C23 0.0660(18) 0.077(2) 0.087(2) -0.0134(17) 0.0378(17) 0.0084(16) C24 0.082(2) 0.0597(18) 0.113(3) 0.0141(18) 0.049(2) 0.0134(16) C25 0.0636(18) 0.096(3) 0.090(2) 0.048(2) 0.0332(18) 0.0117(17) C26 0.0588(18) 0.103(3) 0.101(3) 0.029(2) 0.0389(18) 0.0241(18) B1 0.103(3) 0.0439(16) 0.075(2) 0.0058(14) 0.068(2) 0.0091(16) F1 0.1415(18) 0.0618(11) 0.0971(13) -0.0056(9) 0.0795(14) 0.0196(11) F2 0.1291(16) 0.0670(11) 0.0763(11) 0.0141(9) 0.0607(12) -0.0163(10) F3 0.245(3) 0.0686(13) 0.0758(13) 0.0059(10) 0.0957(17) 0.0006(15) F4 0.157(2) 0.175(3) 0.235(3) 0.100(3) 0.166(3) 0.067(2) Fe1 0.04031(18) 0.0486(2) 0.03838(18) -0.00040(14) 0.02099(14) -0.00532(14) N1 0.0410(10) 0.0514(11) 0.0349(9) -0.0029(8) 0.0185(8) -0.0072(8) N2 0.0373(9) 0.0426(10) 0.0386(9) 0.0008(7) 0.0192(8) -0.0024(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N2 1.326(3) . ? C1 N1 1.337(3) . ? C1 H1 0.9500 . ? C2 C6 1.428(4) . ? C2 N1 1.437(3) . ? C2 C3 1.440(3) . ? C2 Fe1 1.964(2) . ? C3 C4 1.420(4) . ? C3 Fe1 2.017(2) . ? C3 H3 0.9333 . ? C4 C5 1.425(4) . ? C4 Fe1 2.071(2) . ? C4 H4 0.9293 . ? C5 C6 1.435(4) . ? C5 Fe1 2.068(2) . ? C5 H5 0.9310 . ? C6 Fe1 2.038(2) . ? C6 H6 0.9325 . ? C7 C11 1.434(3) . ? C7 C8 1.435(3) . ? C7 N2 1.444(3) . ? C7 Fe1 1.962(2) . ? C8 C9 1.426(4) . ? C8 Fe1 2.026(2) . ? C8 H8 0.9326 . ? C9 C10 1.424(4) . ? C9 Fe1 2.074(2) . ? C9 H9 0.9314 . ? C10 C11 1.419(4) . ? C10 Fe1 2.078(2) . ? C10 H10 0.9304 . ? C11 Fe1 2.025(2) . ? C11 H11 0.9334 . ? C12 N1 1.499(3) . ? C12 C13 1.547(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C15 1.527(4) . ? C13 C14 1.533(4) . ? C13 C16 1.550(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.506(4) . ? C17 N2 1.516(3) . ? C17 C18 1.565(4) . ? C17 H17 1.0000 . ? C18 C19 1.520(4) . ? C18 C25 1.546(5) . ? C18 H18 1.0000 . ? C19 C20 1.542(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.504(4) . ? C20 C26 1.516(5) . ? C20 H20 1.0000 . ? C21 C22 1.542(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.513(4) . ? C22 H22 1.0000 . ? C23 C24 1.505(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.522(5) . ? C24 C26 1.565(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? B1 F4 1.346(5) . ? B1 F1 1.373(4) . ? B1 F2 1.381(4) . ? B1 F3 1.383(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 C1 N1 129.9(2) . . ? N2 C1 H1 115.1 . . ? N1 C1 H1 115.1 . . ? C6 C2 N1 124.2(2) . . ? C6 C2 C3 109.1(2) . . ? N1 C2 C3 126.7(2) . . ? C6 C2 Fe1 71.91(14) . . ? N1 C2 Fe1 122.79(14) . . ? C3 C2 Fe1 70.77(13) . . ? C4 C3 C2 107.0(2) . . ? C4 C3 Fe1 71.74(15) . . ? C2 C3 Fe1 66.85(13) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? Fe1 C3 H3 126.5 . . ? C3 C4 C5 108.7(2) . . ? C3 C4 Fe1 67.63(14) . . ? C5 C4 Fe1 69.72(14) . . ? C3 C4 H4 125.4 . . ? C5 C4 H4 125.9 . . ? Fe1 C4 H4 128.6 . . ? C4 C5 C6 108.5(2) . . ? C4 C5 Fe1 69.99(15) . . ? C6 C5 Fe1 68.45(13) . . ? C4 C5 H5 126.0 . . ? C6 C5 H5 125.5 . . ? Fe1 C5 H5 127.3 . . ? C2 C6 C5 106.7(2) . . ? C2 C6 Fe1 66.34(13) . . ? C5 C6 Fe1 70.64(14) . . ? C2 C6 H6 126.8 . . ? C5 C6 H6 126.5 . . ? Fe1 C6 H6 128.1 . . ? C11 C7 C8 108.6(2) . . ? C11 C7 N2 126.3(2) . . ? C8 C7 N2 125.1(2) . . ? C11 C7 Fe1 71.26(13) . . ? C8 C7 Fe1 71.33(13) . . ? N2 C7 Fe1 123.21(14) . . ? C9 C8 C7 106.8(2) . . ? C9 C8 Fe1 71.47(14) . . ? C7 C8 Fe1 66.55(12) . . ? C9 C8 H8 126.5 . . ? C7 C8 H8 126.8 . . ? Fe1 C8 H8 126.9 . . ? C10 C9 C8 108.9(2) . . ? C10 C9 Fe1 70.07(14) . . ? C8 C9 Fe1 67.86(13) . . ? C10 C9 H9 125.5 . . ? C8 C9 H9 125.6 . . ? Fe1 C9 H9 127.9 . . ? C11 C10 C9 108.3(2) . . ? C11 C10 Fe1 67.78(13) . . ? C9 C10 Fe1 69.82(14) . . ? C11 C10 H10 125.5 . . ? C9 C10 H10 126.2 . . ? Fe1 C10 H10 128.5 . . ? C10 C11 C7 107.5(2) . . ? C10 C11 Fe1 71.79(14) . . ? C7 C11 Fe1 66.61(12) . . ? C10 C11 H11 126.1 . . ? C7 C11 H11 126.4 . . ? Fe1 C11 H11 126.6 . . ? N1 C12 C13 115.9(2) . . ? N1 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? N1 C12 H12B 108.3 . . ? C13 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C15 C13 C14 111.0(3) . . ? C15 C13 C12 110.6(2) . . ? C14 C13 C12 112.4(2) . . ? C15 C13 C16 108.8(2) . . ? C14 C13 C16 108.0(2) . . ? C12 C13 C16 105.8(2) . . ? 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 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 N2 116.15(19) . . ? C22 C17 C18 109.1(2) . . ? N2 C17 C18 109.74(19) . . ? C22 C17 H17 107.2 . . ? N2 C17 H17 107.2 . . ? C18 C17 H17 107.2 . . ? C19 C18 C25 109.8(3) . . ? C19 C18 C17 107.8(3) . . ? C25 C18 C17 109.0(2) . . ? C19 C18 H18 110.1 . . ? C25 C18 H18 110.1 . . ? C17 C18 H18 110.1 . . ? C18 C19 C20 110.6(3) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C26 111.0(3) . . ? C21 C20 C19 108.0(3) . . ? C26 C20 C19 108.7(3) . . ? C21 C20 H20 109.7 . . ? C26 C20 H20 109.7 . . ? C19 C20 H20 109.7 . . ? C20 C21 C22 111.3(3) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C17 C22 C23 111.6(3) . . ? C17 C22 C21 107.9(2) . . ? C23 C22 C21 108.1(3) . . ? C17 C22 H22 109.7 . . ? C23 C22 H22 109.7 . . ? C21 C22 H22 109.7 . . ? C24 C23 C22 110.9(3) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 108.9(3) . . ? C23 C24 C26 110.6(3) . . ? C25 C24 C26 108.6(3) . . ? C23 C24 H24 109.5 . . ? C25 C24 H24 109.5 . . ? C26 C24 H24 109.5 . . ? C24 C25 C18 109.9(3) . . ? C24 C25 H25A 109.7 . . ? C18 C25 H25A 109.7 . . ? C24 C25 H25B 109.7 . . ? C18 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C20 C26 C24 108.6(3) . . ? C20 C26 H26A 110.0 . . ? C24 C26 H26A 110.0 . . ? C20 C26 H26B 110.0 . . ? C24 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? F4 B1 F1 110.0(3) . . ? F4 B1 F2 109.5(3) . . ? F1 B1 F2 109.1(3) . . ? F4 B1 F3 109.2(3) . . ? F1 B1 F3 108.2(3) . . ? F2 B1 F3 110.8(3) . . ? C7 Fe1 C2 94.82(9) . . ? C7 Fe1 C3 113.68(11) . . ? C2 Fe1 C3 42.38(10) . . ? C7 Fe1 C11 42.13(10) . . ? C2 Fe1 C11 113.04(10) . . ? C3 Fe1 C11 101.06(10) . . ? C7 Fe1 C8 42.12(10) . . ? C2 Fe1 C8 114.91(10) . . ? C3 Fe1 C8 151.85(11) . . ? C11 Fe1 C8 70.21(10) . . ? C7 Fe1 C6 113.89(10) . . ? C2 Fe1 C6 41.75(11) . . ? C3 Fe1 C6 70.35(10) . . ? C11 Fe1 C6 150.38(10) . . ? C8 Fe1 C6 103.59(10) . . ? C7 Fe1 C5 153.99(10) . . ? C2 Fe1 C5 69.41(10) . . ? C3 Fe1 C5 68.93(11) . . ? C11 Fe1 C5 163.03(11) . . ? C8 Fe1 C5 125.05(10) . . ? C6 Fe1 C5 40.90(10) . . ? C7 Fe1 C4 153.50(11) . . ? C2 Fe1 C4 69.39(10) . . ? C3 Fe1 C4 40.63(11) . . ? C11 Fe1 C4 123.48(11) . . ? C8 Fe1 C4 164.03(11) . . ? C6 Fe1 C4 68.79(11) . . ? C5 Fe1 C4 40.29(11) . . ? C7 Fe1 C9 69.27(10) . . ? C2 Fe1 C9 155.06(10) . . ? C3 Fe1 C9 161.57(11) . . ? C11 Fe1 C9 68.38(10) . . ? C8 Fe1 C9 40.67(10) . . ? C6 Fe1 C9 126.29(11) . . ? C5 Fe1 C9 117.05(11) . . ? C4 Fe1 C9 132.20(11) . . ? C7 Fe1 C10 69.34(10) . . ? C2 Fe1 C10 152.41(11) . . ? C3 Fe1 C10 122.35(11) . . ? C11 Fe1 C10 40.43(10) . . ? C8 Fe1 C10 68.76(10) . . ? C6 Fe1 C10 165.44(11) . . ? C5 Fe1 C10 132.91(11) . . ? C4 Fe1 C10 115.19(11) . . ? C9 Fe1 C10 40.11(11) . . ? C1 N1 C2 124.77(18) . . ? C1 N1 C12 117.9(2) . . ? C2 N1 C12 116.37(17) . . ? C1 N2 C7 124.26(18) . . ? C1 N2 C17 121.01(19) . . ? C7 N2 C17 113.73(17) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.258 _refine_diff_density_min -0.322 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.173 0.250 156 49 ' ' 2 0.000 0.327 0.750 156 49 ' ' 3 0.000 0.673 0.250 156 49 ' ' 4 0.500 0.827 0.750 156 49 ' ' _platon_squeeze_details ; ; _refine_diff_density_rms 0.042 _database_code_depnum_ccdc_archive 'CCDC 961489' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_i0794 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 Cl Fe N2 Rh' _chemical_formula_weight 618.82 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' Cl Cl 0.1484 0.1585 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_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' _cell_length_a 24.2589(15) _cell_length_b 12.7596(4) _cell_length_c 21.9110(14) _cell_angle_alpha 90.00 _cell_angle_beta 119.247(4) _cell_angle_gamma 90.00 _cell_volume 5917.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18264 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 25.53 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 1.158 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5586 _exptl_absorpt_correction_T_max 0.9328 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 154 frames, detector distance = 135 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 5191 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5191 _reflns_number_gt 4294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie. 2006)' _computing_cell_refinement 'X-Area (Stoe & Cie. 2006)' _computing_data_reduction 'X-Area (Stoe & Cie. 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 win. (Farrugia 2008)' _computing_publication_material 'PLATON (Spek 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5191 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.153 0.250 221 75 ' ' 2 0.500 0.152 0.750 221 75 ' ' 3 0.000 0.347 0.250 221 75 ' ' 4 0.000 0.652 0.750 221 75 ' ' _platon_squeeze_details ; ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.74741(13) 0.3917(2) 0.26162(14) 0.0238(6) Uani 1 1 d . . . C2 C 0.79854(13) 0.3977(2) 0.39250(15) 0.0273(6) Uani 1 1 d . . . C3 C 0.83428(13) 0.3112(2) 0.43549(15) 0.0293(6) Uani 1 1 d . . . H3A H 0.8277 0.2391 0.4231 0.035 Uiso 1 1 calc R . . C4 C 0.88180(15) 0.3540(3) 0.50068(16) 0.0371(7) Uani 1 1 d . . . H4A H 0.9129 0.3148 0.5389 0.044 Uiso 1 1 calc R . . C5 C 0.87473(15) 0.4643(3) 0.49854(16) 0.0368(7) Uani 1 1 d . . . H5A H 0.9003 0.5116 0.5350 0.044 Uiso 1 1 calc R . . C6 C 0.82249(14) 0.4924(2) 0.43227(15) 0.0303(6) Uani 1 1 d . . . H6A H 0.8065 0.5611 0.4173 0.036 Uiso 1 1 calc R . . C7 C 0.86648(13) 0.4012(2) 0.31861(15) 0.0266(6) Uani 1 1 d . . . C8 C 0.91285(13) 0.3237(3) 0.35852(16) 0.0321(7) Uani 1 1 d . . . H8A H 0.9083 0.2500 0.3521 0.039 Uiso 1 1 calc R . . C9 C 0.96733(15) 0.3781(3) 0.40987(18) 0.0383(7) Uani 1 1 d . . . H9A H 1.0053 0.3464 0.4443 0.046 Uiso 1 1 calc R . . C10 C 0.95510(15) 0.4882(3) 0.40075(18) 0.0397(7) Uani 1 1 d . . . H10A H 0.9833 0.5421 0.4284 0.048 Uiso 1 1 calc R . . C11 C 0.89294(14) 0.5033(3) 0.34264(16) 0.0334(7) Uani 1 1 d . . . H11A H 0.8731 0.5686 0.3237 0.040 Uiso 1 1 calc R . . C12 C 0.68432(14) 0.4211(2) 0.31918(16) 0.0304(6) Uani 1 1 d . . . H12A H 0.6509 0.4173 0.2696 0.036 Uiso 1 1 calc R . . H12B H 0.6868 0.4948 0.3343 0.036 Uiso 1 1 calc R . . C13 C 0.66306(15) 0.3532(3) 0.36273(17) 0.0364(7) Uani 1 1 d . . . C14 C 0.67229(16) 0.2364(3) 0.35555(18) 0.0394(7) Uani 1 1 d . . . H14A H 0.7174 0.2215 0.3748 0.047 Uiso 1 1 calc R . . H14B H 0.6495 0.2167 0.3060 0.047 Uiso 1 1 calc R . . H14C H 0.6558 0.1960 0.3812 0.047 Uiso 1 1 calc R . . C15 C 0.69555(18) 0.3844(3) 0.44038(18) 0.0456(8) Uani 1 1 d . . . H15A H 0.6910 0.4600 0.4443 0.055 Uiso 1 1 calc R . . H15B H 0.7405 0.3665 0.4626 0.055 Uiso 1 1 calc R . . H15C H 0.6759 0.3466 0.4637 0.055 Uiso 1 1 calc R . . C16 C 0.59136(17) 0.3761(4) 0.3303(2) 0.0553(10) Uani 1 1 d . . . H16A H 0.5695 0.3543 0.2811 0.066 Uiso 1 1 calc R . . H16B H 0.5849 0.4513 0.3334 0.066 Uiso 1 1 calc R . . H16C H 0.5744 0.3370 0.3560 0.066 Uiso 1 1 calc R . . C17 C 0.80292(14) 0.3702(2) 0.19530(15) 0.0305(6) Uani 1 1 d . . . C18 C 0.81440(16) 0.2722(3) 0.17681(17) 0.0392(7) Uani 1 1 d . . . H18A H 0.8206 0.2133 0.2060 0.047 Uiso 1 1 calc R . . C19 C 0.81674(19) 0.2610(3) 0.11523(19) 0.0503(9) Uani 1 1 d . . . H19A H 0.8240 0.1938 0.1018 0.060 Uiso 1 1 calc R . . C20 C 0.8085(2) 0.3466(3) 0.0732(2) 0.0529(10) Uani 1 1 d . . . H20A H 0.8095 0.3381 0.0307 0.064 Uiso 1 1 calc R . . C21 C 0.7989(2) 0.4446(3) 0.0928(2) 0.0501(9) Uani 1 1 d . . . H21A H 0.7942 0.5036 0.0642 0.060 Uiso 1 1 calc R . . C22 C 0.79613(16) 0.4573(3) 0.15436(17) 0.0382(7) Uani 1 1 d . . . H22A H 0.7897 0.5248 0.1681 0.046 Uiso 1 1 calc R . . C23 C 0.65787(15) 0.2745(2) 0.12589(16) 0.0339(7) Uani 1 1 d . . . H23A H 0.7017 0.2629 0.1562 0.041 Uiso 1 1 calc R . . C24 C 0.61911(15) 0.2838(2) 0.15713(17) 0.0352(7) Uani 1 1 d . . . H24A H 0.6386 0.2821 0.2067 0.042 Uiso 1 1 calc R . . C25 C 0.54751(16) 0.2965(3) 0.1151(2) 0.0495(9) Uani 1 1 d . . . H25A H 0.5317 0.2575 0.0706 0.059 Uiso 1 1 calc R . . H25B H 0.5286 0.2643 0.1417 0.059 Uiso 1 1 calc R . . C26 C 0.52527(18) 0.4088(3) 0.0987(2) 0.0586(11) Uani 1 1 d . . . H26A H 0.5157 0.4347 0.1351 0.070 Uiso 1 1 calc R . . H26B H 0.4856 0.4107 0.0534 0.070 Uiso 1 1 calc R . . C27 C 0.57277(15) 0.4823(3) 0.09483(17) 0.0427(8) Uani 1 1 d . . . H27A H 0.5816 0.5455 0.1208 0.051 Uiso 1 1 calc R . . C28 C 0.60422(17) 0.4671(3) 0.05786(16) 0.0429(8) Uani 1 1 d . . . H28A H 0.6342 0.5183 0.0618 0.051 Uiso 1 1 calc R . . C29 C 0.5937(2) 0.3733(3) 0.01112(19) 0.0578(11) Uani 1 1 d . . . H29A H 0.5491 0.3508 -0.0095 0.069 Uiso 1 1 calc R . . H29B H 0.6011 0.3948 -0.0278 0.069 Uiso 1 1 calc R . . C30 C 0.63588(19) 0.2813(3) 0.04842(18) 0.0501(9) Uani 1 1 d . . . H30A H 0.6735 0.2849 0.0421 0.060 Uiso 1 1 calc R . . H30B H 0.6129 0.2161 0.0258 0.060 Uiso 1 1 calc R . . N1 N 0.74569(11) 0.39380(19) 0.32288(12) 0.0245(5) Uani 1 1 d . . . N2 N 0.80359(11) 0.38320(19) 0.26189(12) 0.0253(5) Uani 1 1 d . . . Cl1 Cl 0.70183(4) 0.60466(6) 0.20100(4) 0.03328(17) Uani 1 1 d . . . Fe1 Fe 0.887136(19) 0.41436(3) 0.41628(2) 0.02822(12) Uani 1 1 d . . . Rh1 Rh 0.668401(10) 0.426510(17) 0.168753(11) 0.02605(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0225(13) 0.0189(13) 0.0272(14) -0.0006(11) 0.0099(11) 0.0008(11) C2 0.0254(14) 0.0321(16) 0.0240(14) -0.0032(12) 0.0118(12) -0.0022(12) C3 0.0271(14) 0.0334(16) 0.0274(14) 0.0032(12) 0.0132(12) -0.0031(12) C4 0.0289(15) 0.049(2) 0.0253(14) 0.0041(14) 0.0069(13) -0.0003(14) C5 0.0321(16) 0.0449(19) 0.0280(15) -0.0096(14) 0.0103(13) -0.0073(14) C6 0.0298(14) 0.0284(15) 0.0321(15) -0.0048(13) 0.0145(12) -0.0011(12) C7 0.0233(14) 0.0280(15) 0.0288(14) 0.0021(12) 0.0130(12) 0.0011(11) C8 0.0261(15) 0.0342(17) 0.0381(16) 0.0028(13) 0.0174(13) 0.0012(13) C9 0.0237(15) 0.0415(19) 0.0457(18) 0.0044(15) 0.0138(14) 0.0029(14) C10 0.0286(15) 0.0404(19) 0.0474(18) -0.0053(15) 0.0164(14) -0.0116(14) C11 0.0300(15) 0.0318(17) 0.0373(15) 0.0012(14) 0.0157(13) -0.0037(13) C12 0.0268(15) 0.0337(17) 0.0310(15) -0.0009(13) 0.0145(13) 0.0003(12) C13 0.0338(16) 0.0406(18) 0.0411(17) 0.0076(14) 0.0232(14) 0.0040(14) C14 0.0370(17) 0.0391(18) 0.0432(17) 0.0075(15) 0.0204(15) 0.0005(14) C15 0.054(2) 0.052(2) 0.0431(19) 0.0059(17) 0.0336(18) 0.0071(17) C16 0.040(2) 0.067(3) 0.072(3) 0.021(2) 0.037(2) 0.0138(18) C17 0.0336(15) 0.0347(17) 0.0285(15) -0.0008(13) 0.0193(13) -0.0004(13) C18 0.052(2) 0.0311(17) 0.0418(17) 0.0035(14) 0.0289(16) 0.0020(15) C19 0.077(3) 0.0364(19) 0.056(2) -0.0098(17) 0.047(2) -0.0025(18) C20 0.082(3) 0.049(2) 0.047(2) -0.0026(17) 0.047(2) -0.002(2) C21 0.073(3) 0.045(2) 0.050(2) 0.0106(17) 0.044(2) 0.0046(18) C22 0.0505(19) 0.0318(17) 0.0391(17) 0.0018(14) 0.0272(16) 0.0017(15) C23 0.0319(15) 0.0223(15) 0.0342(15) -0.0059(13) 0.0057(13) -0.0001(12) C24 0.0333(16) 0.0245(15) 0.0387(16) -0.0035(13) 0.0105(14) -0.0039(13) C25 0.0341(18) 0.049(2) 0.056(2) -0.0049(18) 0.0147(16) -0.0041(16) C26 0.0287(18) 0.066(3) 0.061(2) 0.013(2) 0.0064(17) 0.0047(17) C27 0.0323(16) 0.0414(19) 0.0329(16) 0.0072(15) -0.0009(14) 0.0104(15) C28 0.0460(19) 0.0386(19) 0.0249(15) 0.0038(14) 0.0024(14) 0.0067(16) C29 0.082(3) 0.047(2) 0.0292(17) -0.0022(17) 0.0155(18) 0.005(2) C30 0.053(2) 0.047(2) 0.0376(18) -0.0092(16) 0.0121(16) 0.0085(17) N1 0.0222(12) 0.0256(12) 0.0233(12) 0.0002(10) 0.0093(10) 0.0010(9) N2 0.0257(12) 0.0257(12) 0.0236(11) -0.0006(10) 0.0113(10) 0.0014(10) Cl1 0.0397(4) 0.0236(4) 0.0349(4) -0.0004(3) 0.0169(3) 0.0023(3) Fe1 0.0225(2) 0.0296(2) 0.0274(2) -0.00152(17) 0.00823(18) -0.00245(17) Rh1 0.02642(14) 0.02306(14) 0.02262(13) 0.00022(9) 0.00726(10) 0.00267(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.363(4) . ? C1 N2 1.364(4) . ? C1 Rh1 2.050(3) . ? C2 C3 1.435(4) . ? C2 N1 1.436(4) . ? C2 C6 1.436(4) . ? C2 Fe1 1.960(3) . ? C3 C4 1.435(4) . ? C3 Fe1 2.020(3) . ? C3 H3A 0.9500 . ? C4 C5 1.416(5) . ? C4 Fe1 2.065(3) . ? C4 H4A 0.9500 . ? C5 C6 1.430(4) . ? C5 Fe1 2.068(3) . ? C5 H5A 0.9500 . ? C6 Fe1 2.027(3) . ? C6 H6A 0.9500 . ? C7 C8 1.431(4) . ? C7 C11 1.434(4) . ? C7 N2 1.439(4) . ? C7 Fe1 1.952(3) . ? C8 C9 1.429(5) . ? C8 Fe1 2.025(3) . ? C8 H8A 0.9500 . ? C9 C10 1.430(5) . ? C9 Fe1 2.070(3) . ? C9 H9A 0.9500 . ? C10 C11 1.434(4) . ? C10 Fe1 2.067(3) . ? C10 H10A 0.9500 . ? C11 Fe1 2.033(3) . ? C11 H11A 0.9500 . ? C12 N1 1.492(4) . ? C12 C13 1.552(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.526(5) . ? C13 C15 1.538(5) . ? C13 C16 1.552(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.385(5) . ? C17 C22 1.386(5) . ? C17 N2 1.461(4) . ? C18 C19 1.385(5) . ? C18 H18A 0.9500 . ? C19 C20 1.380(5) . ? C19 H19A 0.9500 . ? C20 C21 1.377(5) . ? C20 H20A 0.9500 . ? C21 C22 1.394(5) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.413(5) . ? C23 C30 1.513(5) . ? C23 Rh1 2.116(3) . ? C23 H23A 0.9500 . ? C24 C25 1.526(5) . ? C24 Rh1 2.124(3) . ? C24 H24A 0.9500 . ? C25 C26 1.511(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.520(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.371(5) . ? C27 Rh1 2.200(3) . ? C27 H27A 0.9500 . ? C28 C29 1.514(5) . ? C28 Rh1 2.213(3) . ? C28 H28A 0.9500 . ? C29 C30 1.508(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? Cl1 Rh1 2.4008(8) . ? 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 N1 C1 N2 120.6(2) . . ? N1 C1 Rh1 120.63(19) . . ? N2 C1 Rh1 117.97(19) . . ? C3 C2 N1 127.6(3) . . ? C3 C2 C6 108.3(2) . . ? N1 C2 C6 124.1(3) . . ? C3 C2 Fe1 71.12(16) . . ? N1 C2 Fe1 125.45(19) . . ? C6 C2 Fe1 71.42(16) . . ? C4 C3 C2 107.2(3) . . ? C4 C3 Fe1 71.12(17) . . ? C2 C3 Fe1 66.66(16) . . ? C4 C3 H3A 126.4 . . ? C2 C3 H3A 126.4 . . ? Fe1 C3 H3A 127.3 . . ? C5 C4 C3 108.7(3) . . ? C5 C4 Fe1 70.07(18) . . ? C3 C4 Fe1 67.77(16) . . ? C5 C4 H4A 125.7 . . ? C3 C4 H4A 125.7 . . ? Fe1 C4 H4A 128.1 . . ? C4 C5 C6 108.4(3) . . ? C4 C5 Fe1 69.85(17) . . ? C6 C5 Fe1 68.06(16) . . ? C4 C5 H5A 125.8 . . ? C6 C5 H5A 125.8 . . ? Fe1 C5 H5A 127.9 . . ? C5 C6 C2 107.5(3) . . ? C5 C6 Fe1 71.08(17) . . ? C2 C6 Fe1 66.41(16) . . ? C5 C6 H6A 126.3 . . ? C2 C6 H6A 126.3 . . ? Fe1 C6 H6A 127.8 . . ? C8 C7 C11 109.0(3) . . ? C8 C7 N2 127.0(3) . . ? C11 C7 N2 123.9(3) . . ? C8 C7 Fe1 71.65(17) . . ? C11 C7 Fe1 71.96(17) . . ? N2 C7 Fe1 123.81(19) . . ? C9 C8 C7 107.1(3) . . ? C9 C8 Fe1 71.31(19) . . ? C7 C8 Fe1 66.23(17) . . ? C9 C8 H8A 126.4 . . ? C7 C8 H8A 126.4 . . ? Fe1 C8 H8A 127.5 . . ? C8 C9 C10 108.5(3) . . ? C8 C9 Fe1 67.88(17) . . ? C10 C9 Fe1 69.63(17) . . ? C8 C9 H9A 125.7 . . ? C10 C9 H9A 125.7 . . ? Fe1 C9 H9A 128.3 . . ? C9 C10 C11 108.2(3) . . ? C9 C10 Fe1 69.92(18) . . ? C11 C10 Fe1 68.29(17) . . ? C9 C10 H10A 125.9 . . ? C11 C10 H10A 125.9 . . ? Fe1 C10 H10A 127.5 . . ? C10 C11 C7 107.0(3) . . ? C10 C11 Fe1 70.78(18) . . ? C7 C11 Fe1 65.92(16) . . ? C10 C11 H11A 126.5 . . ? C7 C11 H11A 126.5 . . ? Fe1 C11 H11A 128.3 . . ? N1 C12 C13 117.3(2) . . ? N1 C12 H12A 108.0 . . ? C13 C12 H12A 108.0 . . ? N1 C12 H12B 108.0 . . ? C13 C12 H12B 108.0 . . ? H12A C12 H12B 107.2 . . ? C14 C13 C15 110.2(3) . . ? C14 C13 C16 108.9(3) . . ? C15 C13 C16 108.2(3) . . ? C14 C13 C12 111.8(3) . . ? C15 C13 C12 113.0(3) . . ? C16 C13 C12 104.4(3) . . ? 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 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 120.8(3) . . ? C18 C17 N2 119.3(3) . . ? C22 C17 N2 119.7(3) . . ? C17 C18 C19 119.2(3) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? C21 C20 C19 120.1(3) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C17 C22 C21 119.1(3) . . ? C17 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C24 C23 C30 125.8(3) . . ? C24 C23 Rh1 70.87(17) . . ? C30 C23 Rh1 110.2(2) . . ? C24 C23 H23A 117.1 . . ? C30 C23 H23A 117.1 . . ? Rh1 C23 H23A 88.9 . . ? C23 C24 C25 123.2(3) . . ? C23 C24 Rh1 70.21(17) . . ? C25 C24 Rh1 112.9(2) . . ? C23 C24 H24A 118.4 . . ? C25 C24 H24A 118.4 . . ? Rh1 C24 H24A 86.9 . . ? C26 C25 C24 114.4(3) . . ? C26 C25 H25A 108.7 . . ? C24 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C25 C26 C27 114.0(3) . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C28 C27 C26 127.0(4) . . ? C28 C27 Rh1 72.43(19) . . ? C26 C27 Rh1 108.4(2) . . ? C28 C27 H27A 116.5 . . ? C26 C27 H27A 116.5 . . ? Rh1 C27 H27A 89.2 . . ? C27 C28 C29 123.6(4) . . ? C27 C28 Rh1 71.37(17) . . ? C29 C28 Rh1 110.7(2) . . ? C27 C28 H28A 118.2 . . ? C29 C28 H28A 118.2 . . ? Rh1 C28 H28A 88.0 . . ? C30 C29 C28 113.8(3) . . ? C30 C29 H29A 108.8 . . ? C28 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? C28 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 C23 115.3(3) . . ? C29 C30 H30A 108.5 . . ? C23 C30 H30A 108.5 . . ? C29 C30 H30B 108.5 . . ? C23 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? C1 N1 C2 127.3(2) . . ? C1 N1 C12 117.4(2) . . ? C2 N1 C12 113.5(2) . . ? C1 N2 C7 128.8(2) . . ? C1 N2 C17 118.8(2) . . ? C7 N2 C17 111.7(2) . . ? C7 Fe1 C2 92.20(12) . . ? C7 Fe1 C3 108.86(12) . . ? C2 Fe1 C3 42.22(12) . . ? C7 Fe1 C8 42.12(12) . . ? C2 Fe1 C8 113.86(12) . . ? C3 Fe1 C8 100.31(13) . . ? C7 Fe1 C6 115.19(12) . . ? C2 Fe1 C6 42.18(12) . . ? C3 Fe1 C6 70.16(12) . . ? C8 Fe1 C6 152.75(12) . . ? C7 Fe1 C11 42.12(12) . . ? C2 Fe1 C11 109.98(12) . . ? C3 Fe1 C11 145.71(12) . . ? C8 Fe1 C11 70.18(13) . . ? C6 Fe1 C11 102.84(12) . . ? C7 Fe1 C4 148.75(13) . . ? C2 Fe1 C4 69.95(12) . . ? C3 Fe1 C4 41.11(12) . . ? C8 Fe1 C4 121.33(13) . . ? C6 Fe1 C4 68.67(13) . . ? C11 Fe1 C4 167.94(14) . . ? C7 Fe1 C10 69.93(13) . . ? C2 Fe1 C10 149.90(13) . . ? C3 Fe1 C10 165.96(13) . . ? C8 Fe1 C10 69.10(13) . . ? C6 Fe1 C10 123.45(13) . . ? C11 Fe1 C10 40.93(12) . . ? C4 Fe1 C10 136.20(13) . . ? C7 Fe1 C5 155.97(13) . . ? C2 Fe1 C5 69.97(12) . . ? C3 Fe1 C5 69.00(13) . . ? C8 Fe1 C5 160.29(13) . . ? C6 Fe1 C5 40.86(12) . . ? C11 Fe1 C5 128.00(14) . . ? C4 Fe1 C5 40.07(14) . . ? C10 Fe1 C5 118.08(13) . . ? C7 Fe1 C9 69.69(13) . . ? C2 Fe1 C9 154.48(13) . . ? C3 Fe1 C9 125.57(13) . . ? C8 Fe1 C9 40.82(13) . . ? C6 Fe1 C9 162.44(13) . . ? C11 Fe1 C9 68.86(13) . . ? C4 Fe1 C9 116.71(13) . . ? C10 Fe1 C9 40.45(14) . . ? C5 Fe1 C9 132.06(13) . . ? C1 Rh1 C23 95.36(11) . . ? C1 Rh1 C24 97.56(12) . . ? C23 Rh1 C24 38.92(12) . . ? C1 Rh1 C27 159.93(12) . . ? C23 Rh1 C27 96.58(13) . . ? C24 Rh1 C27 81.94(13) . . ? C1 Rh1 C28 162.87(13) . . ? C23 Rh1 C28 81.94(12) . . ? C24 Rh1 C28 90.93(13) . . ? C27 Rh1 C28 36.19(14) . . ? C1 Rh1 Cl1 84.01(8) . . ? C23 Rh1 Cl1 161.61(9) . . ? C24 Rh1 Cl1 159.44(9) . . ? C27 Rh1 Cl1 89.62(10) . . ? C28 Rh1 Cl1 93.25(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.573 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 961491' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_i1092 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 Cl Fe N2 O2 Rh' _chemical_formula_sum 'C28 H34 Cl Fe N2 O2 Rh' _chemical_formula_weight 624.78 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' Cl Cl 0.1484 0.1585 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_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' _cell_length_a 11.797(3) _cell_length_b 19.483(3) _cell_length_c 12.948(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.250(14) _cell_angle_gamma 90.00 _cell_volume 2691.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8963 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 25.42 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.279 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7218 _exptl_absorpt_correction_T_max 0.9765 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 104 frames, detector distance = 135 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 12059 _diffrn_reflns_av_R_equivalents 0.1398 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4696 _reflns_number_gt 3158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie. 2006)' _computing_cell_refinement 'X-Area (Stoe & Cie. 2006)' _computing_data_reduction 'X-Area (Stoe & Cie. 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 win. (Farrugia 2008)' _computing_publication_material 'PLATON (Spek 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1211P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4696 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1923 _refine_ls_wR_factor_gt 0.1771 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5596(6) 0.2361(3) 0.7693(6) 0.0447(15) Uani 1 1 d . . . C2 C 0.5343(8) 0.2241(4) 1.0681(8) 0.063(2) Uani 1 1 d . . . C3 C 0.3696(9) 0.2095(4) 0.8475(7) 0.063(2) Uani 1 1 d . . . C4 C 0.6310(7) 0.1690(3) 0.6424(6) 0.0509(17) Uani 1 1 d . . . C5 C 0.5557(8) 0.1595(4) 0.5223(7) 0.0584(19) Uani 1 1 d . . . H5A H 0.4669 0.1565 0.4859 0.070 Uiso 1 1 calc R . . C6 C 0.6383(10) 0.1552(4) 0.4667(8) 0.069(2) Uani 1 1 d . . . H6A H 0.6135 0.1492 0.3872 0.083 Uiso 1 1 calc R . . C7 C 0.7638(9) 0.1617(4) 0.5519(8) 0.069(2) Uani 1 1 d . . . H7A H 0.8373 0.1613 0.5390 0.083 Uiso 1 1 calc R . . C8 C 0.7597(8) 0.1688(3) 0.6609(7) 0.0565(18) Uani 1 1 d . . . H8A H 0.8301 0.1728 0.7327 0.068 Uiso 1 1 calc R . . C9 C 0.5956(6) 0.3148(3) 0.6340(6) 0.0455(15) Uani 1 1 d . . . C10 C 0.7222(7) 0.3334(3) 0.6531(7) 0.0492(16) Uani 1 1 d . . . H10A H 0.7919 0.3378 0.7253 0.059 Uiso 1 1 calc R . . C11 C 0.7239(8) 0.3439(4) 0.5442(7) 0.060(2) Uani 1 1 d . . . H11A H 0.7954 0.3555 0.5319 0.072 Uiso 1 1 calc R . . C12 C 0.6011(9) 0.3342(4) 0.4581(7) 0.062(2) Uani 1 1 d . . . H12A H 0.5761 0.3381 0.3782 0.074 Uiso 1 1 calc R . . C13 C 0.5209(8) 0.3176(4) 0.5119(7) 0.0573(18) Uani 1 1 d . . . H13A H 0.4332 0.3097 0.4737 0.069 Uiso 1 1 calc R . . C14 C 0.6104(7) 0.1127(3) 0.8017(6) 0.0500(16) Uani 1 1 d . . . H14B H 0.5945 0.1238 0.8689 0.060 Uiso 1 1 calc R . . H14A H 0.7003 0.1007 0.8304 0.060 Uiso 1 1 calc R . . C15 C 0.5325(8) 0.0480(4) 0.7436(7) 0.0561(18) Uani 1 1 d . . . C16 C 0.5389(12) 0.0004(4) 0.8433(9) 0.088(3) Uani 1 1 d . . . H16A H 0.4957 0.0225 0.8843 0.105 Uiso 1 1 calc R . . H16B H 0.6268 -0.0077 0.8959 0.105 Uiso 1 1 calc R . . H16C H 0.4984 -0.0436 0.8120 0.105 Uiso 1 1 calc R . . C17 C 0.5896(9) 0.0079(4) 0.6741(8) 0.071(2) Uani 1 1 d . . . H17A H 0.6782 -0.0017 0.7225 0.086 Uiso 1 1 calc R . . H17B H 0.5825 0.0354 0.6082 0.086 Uiso 1 1 calc R . . H17C H 0.5444 -0.0355 0.6474 0.086 Uiso 1 1 calc R . . C18 C 0.3930(8) 0.0650(4) 0.6665(8) 0.070(2) Uani 1 1 d . . . H18C H 0.3469 0.0223 0.6355 0.085 Uiso 1 1 calc R . . H18B H 0.3878 0.0947 0.6036 0.085 Uiso 1 1 calc R . . H18A H 0.3562 0.0886 0.7118 0.085 Uiso 1 1 calc R . . C19 C 0.5207(8) 0.3598(3) 0.7751(6) 0.0532(18) Uani 1 1 d . . . H19A H 0.5441 0.3458 0.8560 0.064 Uiso 1 1 calc R . . C20 C 0.3782(8) 0.3745(4) 0.7244(7) 0.0577(19) Uani 1 1 d . . . H20A H 0.3309 0.3303 0.7107 0.069 Uiso 1 1 calc R . . C21 C 0.3333(9) 0.4154(4) 0.6130(7) 0.066(2) Uani 1 1 d . . . H21B H 0.2424 0.4247 0.5842 0.079 Uiso 1 1 calc R . . H21A H 0.3466 0.3880 0.5547 0.079 Uiso 1 1 calc R . . C22 C 0.4048(9) 0.4840(4) 0.6317(7) 0.068(2) Uani 1 1 d . . . H22A H 0.3726 0.5100 0.5581 0.082 Uiso 1 1 calc R . . C23 C 0.5417(9) 0.4697(4) 0.6701(7) 0.062(2) Uani 1 1 d . . . H23B H 0.5882 0.5136 0.6828 0.074 Uiso 1 1 calc R . . H23A H 0.5544 0.4438 0.6100 0.074 Uiso 1 1 calc R . . C24 C 0.5934(8) 0.4269(4) 0.7837(7) 0.0586(19) Uani 1 1 d . . . H24A H 0.6847 0.4171 0.8098 0.070 Uiso 1 1 calc R . . C25 C 0.3544(9) 0.4179(5) 0.8131(8) 0.073(2) Uani 1 1 d . . . H25B H 0.3798 0.3918 0.8851 0.088 Uiso 1 1 calc R . . H25A H 0.2641 0.4289 0.7839 0.088 Uiso 1 1 calc R . . C26 C 0.4328(9) 0.4858(4) 0.8355(7) 0.068(2) Uani 1 1 d . . . H26A H 0.4212 0.5135 0.8954 0.082 Uiso 1 1 calc R . . C27 C 0.5717(10) 0.4701(4) 0.8745(8) 0.076(3) Uani 1 1 d . . . H27A H 0.6036 0.4446 0.9476 0.091 Uiso 1 1 calc R . . H27B H 0.6190 0.5137 0.8877 0.091 Uiso 1 1 calc R . . C28 C 0.3829(10) 0.5269(5) 0.7219(8) 0.079(3) Uani 1 1 d . . . H28A H 0.2924 0.5364 0.6953 0.095 Uiso 1 1 calc R . . H28B H 0.4275 0.5713 0.7338 0.095 Uiso 1 1 calc R . . N1 N 0.5880(5) 0.1768(3) 0.7308(5) 0.0442(13) Uani 1 1 d . . . N2 N 0.5563(6) 0.2992(3) 0.7216(5) 0.0457(13) Uani 1 1 d . . . O1 O 0.5356(7) 0.2154(5) 1.1591(6) 0.103(3) Uani 1 1 d . . . O2 O 0.2646(6) 0.1973(4) 0.8025(5) 0.0785(18) Uani 1 1 d . . . Cl3 Cl 0.75090(18) 0.26621(10) 1.01257(17) 0.0585(5) Uani 1 1 d . . . Fe2 Fe 0.65931(11) 0.24649(5) 0.55785(10) 0.0494(3) Uani 1 1 d . . . Rh1 Rh 0.53768(5) 0.23210(3) 0.92468(5) 0.0476(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(3) 0.035(3) 0.059(4) -0.001(3) 0.020(3) 0.002(3) C2 0.056(5) 0.064(5) 0.075(5) -0.003(4) 0.033(4) -0.014(4) C3 0.077(6) 0.062(5) 0.059(5) 0.009(4) 0.038(5) -0.001(4) C4 0.069(5) 0.031(3) 0.060(4) -0.007(3) 0.035(4) -0.006(3) C5 0.074(5) 0.046(4) 0.060(5) -0.015(3) 0.033(4) -0.019(4) C6 0.102(7) 0.047(4) 0.078(6) -0.010(4) 0.058(6) -0.010(4) C7 0.091(7) 0.049(4) 0.092(6) 0.000(4) 0.063(6) 0.003(4) C8 0.067(5) 0.038(4) 0.071(5) -0.001(3) 0.035(4) 0.001(3) C9 0.047(4) 0.037(3) 0.055(4) 0.000(3) 0.024(3) 0.004(3) C10 0.057(4) 0.033(3) 0.064(4) 0.001(3) 0.032(4) 0.003(3) C11 0.073(6) 0.044(4) 0.082(5) -0.005(4) 0.052(5) -0.005(4) C12 0.088(6) 0.052(4) 0.066(5) 0.009(4) 0.053(5) 0.003(4) C13 0.066(5) 0.046(4) 0.060(4) 0.008(3) 0.027(4) 0.001(3) C14 0.064(5) 0.032(3) 0.051(4) 0.002(3) 0.023(4) 0.003(3) C15 0.069(5) 0.042(4) 0.055(4) 0.001(3) 0.024(4) 0.001(3) C16 0.126(9) 0.039(4) 0.088(7) 0.015(4) 0.035(7) -0.001(5) C17 0.073(6) 0.044(4) 0.090(6) -0.016(4) 0.028(5) -0.009(4) C18 0.064(5) 0.059(5) 0.080(6) 0.011(4) 0.022(5) -0.013(4) C19 0.081(5) 0.035(3) 0.055(4) 0.007(3) 0.040(4) 0.013(3) C20 0.068(5) 0.050(4) 0.062(4) 0.004(3) 0.035(4) 0.002(4) C21 0.068(5) 0.065(5) 0.062(5) 0.007(4) 0.026(4) 0.016(4) C22 0.104(7) 0.052(4) 0.067(5) 0.023(4) 0.054(5) 0.027(4) C23 0.098(6) 0.034(3) 0.075(5) 0.001(3) 0.058(5) -0.002(4) C24 0.073(5) 0.040(4) 0.069(5) -0.005(3) 0.035(4) -0.003(3) C25 0.091(7) 0.069(5) 0.078(6) 0.012(4) 0.055(6) 0.019(5) C26 0.105(7) 0.049(4) 0.062(5) 0.002(4) 0.046(5) 0.020(4) C27 0.118(8) 0.043(4) 0.073(6) -0.007(4) 0.046(6) 0.001(5) C28 0.116(8) 0.047(4) 0.092(6) 0.011(4) 0.061(6) 0.022(5) N1 0.051(3) 0.033(3) 0.049(3) -0.002(2) 0.023(3) -0.002(2) N2 0.058(3) 0.038(3) 0.045(3) 0.000(2) 0.025(3) -0.002(3) O1 0.098(5) 0.157(8) 0.058(4) 0.007(4) 0.037(4) -0.030(5) O2 0.056(4) 0.109(5) 0.070(4) 0.004(4) 0.026(3) -0.013(4) Cl3 0.0527(11) 0.0572(10) 0.0612(11) -0.0003(8) 0.0201(9) -0.0008(8) Fe2 0.0631(7) 0.0371(5) 0.0576(6) -0.0027(4) 0.0348(6) -0.0021(4) Rh1 0.0531(4) 0.0442(3) 0.0490(4) 0.0032(2) 0.0251(3) 0.0000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.357(8) . ? C1 N2 1.369(9) . ? C1 Rh1 2.137(7) . ? C2 O1 1.183(10) . ? C2 Rh1 1.881(9) . ? C3 O2 1.147(10) . ? C3 Rh1 1.853(10) . ? C4 C8 1.432(11) . ? C4 C5 1.436(11) . ? C4 N1 1.445(8) . ? C4 Fe2 1.975(7) . ? C5 C6 1.440(11) . ? C5 Fe2 2.025(7) . ? C5 H5A 0.9500 . ? C6 C7 1.425(13) . ? C6 Fe2 2.089(8) . ? C6 H6A 0.9500 . ? C7 C8 1.440(11) . ? C7 Fe2 2.083(8) . ? C7 H7A 0.9500 . ? C8 Fe2 2.031(8) . ? C8 H8A 0.9500 . ? C9 N2 1.429(8) . ? C9 C13 1.446(10) . ? C9 C10 1.451(10) . ? C9 Fe2 1.985(6) . ? C10 C11 1.434(10) . ? C10 Fe2 2.038(7) . ? C10 H10A 0.9500 . ? C11 C12 1.413(12) . ? C11 Fe2 2.081(7) . ? C11 H11A 0.9500 . ? C12 C13 1.431(10) . ? C12 Fe2 2.075(8) . ? C12 H12A 0.9500 . ? C13 Fe2 2.027(8) . ? C13 H13A 0.9500 . ? C14 N1 1.504(8) . ? C14 C15 1.553(10) . ? C14 H14B 0.9900 . ? C14 H14A 0.9900 . ? C15 C17 1.546(11) . ? C15 C18 1.554(12) . ? C15 C16 1.564(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18C 0.9800 . ? C18 H18B 0.9800 . ? C18 H18A 0.9800 . ? C19 N2 1.516(8) . ? C19 C24 1.541(10) . ? C19 C20 1.548(11) . ? C19 H19A 1.0000 . ? C20 C21 1.532(11) . ? C20 C25 1.544(11) . ? C20 H20A 1.0000 . ? C21 C22 1.544(13) . ? C21 H21B 0.9900 . ? C21 H21A 0.9900 . ? C22 C23 1.499(12) . ? C22 C28 1.545(11) . ? C22 H22A 1.0000 . ? C23 C24 1.571(11) . ? C23 H23B 0.9900 . ? C23 H23A 0.9900 . ? C24 C27 1.554(11) . ? C24 H24A 1.0000 . ? C25 C26 1.568(13) . ? C25 H25B 0.9900 . ? C25 H25A 0.9900 . ? C26 C27 1.526(14) . ? C26 C28 1.554(12) . ? C26 H26A 1.0000 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? Cl3 Rh1 2.371(2) . ? 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 N1 C1 N2 124.3(6) . . ? N1 C1 Rh1 117.6(5) . . ? N2 C1 Rh1 117.8(4) . . ? O1 C2 Rh1 176.1(9) . . ? O2 C3 Rh1 177.3(8) . . ? C8 C4 C5 107.6(6) . . ? C8 C4 N1 125.0(7) . . ? C5 C4 N1 127.4(7) . . ? C8 C4 Fe2 71.2(4) . . ? C5 C4 Fe2 70.8(4) . . ? N1 C4 Fe2 123.9(4) . . ? C4 C5 C6 108.1(7) . . ? C4 C5 Fe2 67.1(4) . . ? C6 C5 Fe2 71.9(4) . . ? C4 C5 H5A 126.0 . . ? C6 C5 H5A 126.0 . . ? Fe2 C5 H5A 126.5 . . ? C7 C6 C5 108.0(7) . . ? C7 C6 Fe2 69.8(5) . . ? C5 C6 Fe2 67.1(4) . . ? C7 C6 H6A 126.0 . . ? C5 C6 H6A 126.0 . . ? Fe2 C6 H6A 128.6 . . ? C6 C7 C8 108.0(7) . . ? C6 C7 Fe2 70.3(5) . . ? C8 C7 Fe2 67.6(4) . . ? C6 C7 H7A 126.0 . . ? C8 C7 H7A 126.0 . . ? Fe2 C7 H7A 127.7 . . ? C4 C8 C7 108.2(8) . . ? C4 C8 Fe2 67.0(4) . . ? C7 C8 Fe2 71.5(5) . . ? C4 C8 H8A 125.9 . . ? C7 C8 H8A 125.9 . . ? Fe2 C8 H8A 127.2 . . ? N2 C9 C13 128.5(6) . . ? N2 C9 C10 125.2(6) . . ? C13 C9 C10 106.2(6) . . ? N2 C9 Fe2 124.9(4) . . ? C13 C9 Fe2 70.4(4) . . ? C10 C9 Fe2 70.8(4) . . ? C11 C10 C9 108.3(7) . . ? C11 C10 Fe2 71.2(4) . . ? C9 C10 Fe2 66.9(4) . . ? C11 C10 H10A 125.9 . . ? C9 C10 H10A 125.9 . . ? Fe2 C10 H10A 127.5 . . ? C12 C11 C10 108.5(6) . . ? C12 C11 Fe2 69.9(4) . . ? C10 C11 Fe2 68.0(4) . . ? C12 C11 H11A 125.8 . . ? C10 C11 H11A 125.8 . . ? Fe2 C11 H11A 127.9 . . ? C11 C12 C13 108.3(7) . . ? C11 C12 Fe2 70.4(5) . . ? C13 C12 Fe2 67.8(4) . . ? C11 C12 H12A 125.8 . . ? C13 C12 H12A 125.8 . . ? Fe2 C12 H12A 127.6 . . ? C12 C13 C9 108.6(7) . . ? C12 C13 Fe2 71.4(5) . . ? C9 C13 Fe2 67.3(4) . . ? C12 C13 H13A 125.7 . . ? C9 C13 H13A 125.7 . . ? Fe2 C13 H13A 127.2 . . ? N1 C14 C15 117.7(6) . . ? N1 C14 H14B 107.9 . . ? C15 C14 H14B 107.9 . . ? N1 C14 H14A 107.9 . . ? C15 C14 H14A 107.9 . . ? H14B C14 H14A 107.2 . . ? C17 C15 C14 112.2(6) . . ? C17 C15 C18 109.8(7) . . ? C14 C15 C18 112.6(6) . . ? C17 C15 C16 107.5(7) . . ? C14 C15 C16 105.8(6) . . ? C18 C15 C16 108.8(7) . . ? 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 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18C 109.5 . . ? C15 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? C15 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? N2 C19 C24 116.0(6) . . ? N2 C19 C20 114.4(6) . . ? C24 C19 C20 110.1(6) . . ? N2 C19 H19A 105.0 . . ? C24 C19 H19A 105.0 . . ? C20 C19 H19A 105.0 . . ? C21 C20 C25 108.5(7) . . ? C21 C20 C19 111.9(6) . . ? C25 C20 C19 107.1(7) . . ? C21 C20 H20A 109.8 . . ? C25 C20 H20A 109.8 . . ? C19 C20 H20A 109.8 . . ? C20 C21 C22 110.9(7) . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? H21B C21 H21A 108.1 . . ? C23 C22 C21 109.3(6) . . ? C23 C22 C28 110.7(8) . . ? C21 C22 C28 109.3(7) . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C28 C22 H22A 109.2 . . ? C22 C23 C24 110.0(6) . . ? C22 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? C22 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? H23B C23 H23A 108.2 . . ? C19 C24 C27 104.3(6) . . ? C19 C24 C23 113.6(7) . . ? C27 C24 C23 107.3(6) . . ? C19 C24 H24A 110.5 . . ? C27 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? C20 C25 C26 108.6(6) . . ? C20 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? C20 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? H25B C25 H25A 108.3 . . ? C27 C26 C28 109.6(7) . . ? C27 C26 C25 111.0(7) . . ? C28 C26 C25 107.7(8) . . ? C27 C26 H26A 109.5 . . ? C28 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C26 C27 C24 111.0(8) . . ? C26 C27 H27A 109.4 . . ? C24 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C24 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C22 C28 C26 108.6(6) . . ? C22 C28 H28A 110.0 . . ? C26 C28 H28A 110.0 . . ? C22 C28 H28B 110.0 . . ? C26 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? C1 N1 C4 127.3(5) . . ? C1 N1 C14 119.3(5) . . ? C4 N1 C14 111.5(5) . . ? C1 N2 C9 126.3(5) . . ? C1 N2 C19 117.0(5) . . ? C9 N2 C19 116.4(5) . . ? C4 Fe2 C9 92.8(3) . . ? C4 Fe2 C5 42.1(3) . . ? C9 Fe2 C5 110.8(3) . . ? C4 Fe2 C13 112.3(3) . . ? C9 Fe2 C13 42.2(3) . . ? C5 Fe2 C13 100.0(4) . . ? C4 Fe2 C8 41.9(3) . . ? C9 Fe2 C8 114.3(3) . . ? C5 Fe2 C8 69.6(3) . . ? C13 Fe2 C8 150.8(3) . . ? C4 Fe2 C10 113.8(3) . . ? C9 Fe2 C10 42.3(3) . . ? C5 Fe2 C10 149.5(3) . . ? C13 Fe2 C10 69.5(3) . . ? C8 Fe2 C10 105.2(3) . . ? C4 Fe2 C12 152.3(3) . . ? C9 Fe2 C12 70.2(3) . . ? C5 Fe2 C12 122.8(4) . . ? C13 Fe2 C12 40.8(3) . . ? C8 Fe2 C12 165.5(3) . . ? C10 Fe2 C12 68.3(3) . . ? C4 Fe2 C11 154.1(3) . . ? C9 Fe2 C11 70.1(3) . . ? C5 Fe2 C11 162.1(4) . . ? C13 Fe2 C11 68.3(3) . . ? C8 Fe2 C11 127.1(4) . . ? C10 Fe2 C11 40.7(3) . . ? C12 Fe2 C11 39.8(3) . . ? C4 Fe2 C7 69.9(3) . . ? C9 Fe2 C7 154.9(3) . . ? C5 Fe2 C7 68.7(4) . . ? C13 Fe2 C7 161.2(4) . . ? C8 Fe2 C7 41.0(3) . . ? C10 Fe2 C7 127.8(4) . . ? C12 Fe2 C7 132.4(3) . . ? C11 Fe2 C7 118.5(3) . . ? C4 Fe2 C6 69.8(3) . . ? C9 Fe2 C6 150.7(3) . . ? C5 Fe2 C6 40.9(3) . . ? C13 Fe2 C6 122.0(4) . . ? C8 Fe2 C6 68.4(4) . . ? C10 Fe2 C6 166.7(3) . . ? C12 Fe2 C6 114.9(4) . . ? C11 Fe2 C6 133.4(3) . . ? C7 Fe2 C6 39.9(4) . . ? C3 Rh1 C2 92.5(3) . . ? C3 Rh1 C1 91.9(3) . . ? C2 Rh1 C1 174.2(3) . . ? C3 Rh1 Cl3 176.0(2) . . ? C2 Rh1 Cl3 90.8(3) . . ? C1 Rh1 Cl3 84.94(19) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.250 _refine_diff_density_min -1.745 _refine_diff_density_rms 0.149 _database_code_depnum_ccdc_archive 'CCDC 961493' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_i1123 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C39 H42 Cl Fe N2 Rh), C H2 Cl2' _chemical_formula_sum 'C39.25 H42.50 Cl1.50 Fe N2 Rh' _chemical_formula_weight 754.19 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' Cl Cl 0.1484 0.1585 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6403(7) _cell_length_b 14.8878(10) _cell_length_c 20.1701(12) _cell_angle_alpha 98.297(5) _cell_angle_beta 91.535(5) _cell_angle_gamma 103.422(5) _cell_volume 3357.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 21102 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 25.59 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1554 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8319 _exptl_absorpt_correction_T_max 0.9587 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 222 frames, detector distance = 135 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 26910 _diffrn_reflns_av_R_equivalents 0.1013 _diffrn_reflns_av_unetI/netI 0.1028 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.15 _reflns_number_total 11890 _reflns_number_gt 8185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie. 2006)' _computing_cell_refinement 'X-Area (Stoe & Cie. 2006)' _computing_data_reduction 'X-Area (Stoe & Cie. 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 win. (Farrugia 2008)' _computing_publication_material 'PLATON (Spek 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11890 _refine_ls_number_parameters 962 _refine_ls_number_restraints 886 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1079(4) 0.5472(3) 0.2573(2) 0.0286(11) Uani 1 1 d U . . C2 C 0.1793(5) 0.5586(4) 0.1420(3) 0.0322(12) Uani 1 1 d U . . C3 C 0.2514(5) 0.6485(4) 0.1320(3) 0.0395(13) Uani 1 1 d U . . H3A H 0.3028 0.6928 0.1648 0.047 Uiso 1 1 calc R . . C4 C 0.2307(5) 0.6581(4) 0.0635(3) 0.0410(13) Uani 1 1 d U . . H4A H 0.2652 0.7109 0.0431 0.049 Uiso 1 1 calc R . . C5 C 0.1501(5) 0.5757(4) 0.0311(3) 0.0397(13) Uani 1 1 d U . . H5A H 0.1215 0.5641 -0.0147 0.048 Uiso 1 1 calc R . . C6 C 0.1192(5) 0.5136(4) 0.0781(3) 0.0342(12) Uani 1 1 d U . . H6A H 0.0680 0.4528 0.0693 0.041 Uiso 1 1 calc R . . C7 C -0.0101(5) 0.6324(4) 0.1958(3) 0.0317(11) Uani 1 1 d U . . C8 C 0.0376(6) 0.7274(4) 0.1877(3) 0.0393(13) Uani 1 1 d U . . H8A H 0.0906 0.7731 0.2190 0.047 Uiso 1 1 calc R . . C9 C -0.0076(6) 0.7421(4) 0.1250(3) 0.0466(15) Uani 1 1 d U . . H9A H 0.0129 0.7982 0.1062 0.056 Uiso 1 1 calc R . . C10 C -0.0885(5) 0.6582(4) 0.0955(3) 0.0403(13) Uani 1 1 d U . . H10A H -0.1329 0.6491 0.0538 0.048 Uiso 1 1 calc R . . C11 C -0.0923(5) 0.5901(4) 0.1383(3) 0.0389(13) Uani 1 1 d U . . H11A H -0.1400 0.5280 0.1308 0.047 Uiso 1 1 calc R . . C12 C 0.2556(5) 0.4657(4) 0.2161(3) 0.0366(12) Uani 1 1 d U . . H12A H 0.2242 0.4241 0.2489 0.044 Uiso 1 1 calc R . . H12B H 0.3319 0.5071 0.2356 0.044 Uiso 1 1 calc R . . C13 C 0.2764(5) 0.4070(4) 0.1517(3) 0.0358(12) Uani 1 1 d U . . C14 C 0.1866(5) 0.3289(4) 0.1223(3) 0.0366(12) Uani 1 1 d U . . C15 C 0.0722(6) 0.3060(4) 0.1495(3) 0.0436(14) Uani 1 1 d U . . H15A H 0.0580 0.3407 0.1906 0.052 Uiso 1 1 calc R . . C16 C -0.0159(6) 0.2352(5) 0.1169(4) 0.0516(16) Uani 1 1 d U . . H16A H -0.0907 0.2215 0.1358 0.062 Uiso 1 1 calc R . . C17 C 0.0010(7) 0.1818(5) 0.0559(3) 0.0550(18) Uani 1 1 d U . . H17A H -0.0625 0.1343 0.0332 0.066 Uiso 1 1 calc R . . C18 C 0.1092(6) 0.1989(4) 0.0300(3) 0.0456(15) Uani 1 1 d U . . H18A H 0.1220 0.1603 -0.0096 0.055 Uiso 1 1 calc R . . C19 C 0.2039(5) 0.2737(4) 0.0610(3) 0.0391(13) Uani 1 1 d U . . C20 C 0.3135(5) 0.2952(4) 0.0327(3) 0.0407(14) Uani 1 1 d U . . H20A H 0.3259 0.2571 -0.0072 0.049 Uiso 1 1 calc R . . C21 C 0.4053(5) 0.3708(4) 0.0609(3) 0.0388(13) Uani 1 1 d U . . C22 C 0.5159(5) 0.3926(5) 0.0307(3) 0.0455(15) Uani 1 1 d U . . H22A H 0.5291 0.3530 -0.0083 0.055 Uiso 1 1 calc R . . C23 C 0.6024(6) 0.4684(5) 0.0565(3) 0.0517(16) Uani 1 1 d U . . H23A H 0.6762 0.4808 0.0364 0.062 Uiso 1 1 calc R . . C24 C 0.5823(5) 0.5292(5) 0.1136(3) 0.0502(16) Uani 1 1 d U . . H24A H 0.6415 0.5841 0.1302 0.060 Uiso 1 1 calc R . . C25 C 0.4790(5) 0.5097(5) 0.1449(3) 0.0434(14) Uani 1 1 d U . . H25A H 0.4687 0.5508 0.1838 0.052 Uiso 1 1 calc R . . C26 C 0.3860(5) 0.4295(4) 0.1211(3) 0.0360(12) Uani 1 1 d U . . C27 C -0.0468(5) 0.6106(4) 0.3117(3) 0.0321(11) Uani 1 1 d U . . H27A H -0.0396 0.6789 0.3213 0.039 Uiso 1 1 calc R . . H27B H -0.0068 0.5932 0.3501 0.039 Uiso 1 1 calc R . . C28 C -0.1798(5) 0.5610(4) 0.3087(3) 0.0345(12) Uani 1 1 d U . . C29 C -0.2062(6) 0.4622(4) 0.2679(3) 0.0433(14) Uani 1 1 d U . . H29A H -0.1578 0.4253 0.2869 0.052 Uiso 1 1 calc R . . H29B H -0.1875 0.4663 0.2211 0.052 Uiso 1 1 calc R . . H29C H -0.2902 0.4320 0.2694 0.052 Uiso 1 1 calc R . . C30 C -0.2570(5) 0.6215(5) 0.2820(3) 0.0438(14) Uani 1 1 d U . . H30A H -0.2334 0.6343 0.2374 0.053 Uiso 1 1 calc R . . H30B H -0.2460 0.6806 0.3127 0.053 Uiso 1 1 calc R . . H30C H -0.3405 0.5878 0.2791 0.053 Uiso 1 1 calc R . . C31 C -0.2065(5) 0.5535(5) 0.3827(3) 0.0425(14) Uani 1 1 d U . . H31A H -0.1770 0.6147 0.4105 0.051 Uiso 1 1 calc R . . H31C H -0.1671 0.5083 0.3985 0.051 Uiso 1 1 calc R . . H31B H -0.2921 0.5326 0.3861 0.051 Uiso 1 1 calc R . . C32 C 0.1638(6) 0.5309(5) 0.4606(3) 0.0416(14) Uani 1 1 d U . . H32A H 0.0922 0.4837 0.4551 0.050 Uiso 1 1 calc R . . C33 C 0.2637(6) 0.5046(5) 0.4401(3) 0.0417(14) Uani 1 1 d U . . H33A H 0.2546 0.4415 0.4197 0.050 Uiso 1 1 calc R . . C34 C 0.3878(5) 0.5671(5) 0.4471(3) 0.0444(14) Uani 1 1 d U . . H34A H 0.4452 0.5292 0.4542 0.053 Uiso 1 1 calc R . . H34B H 0.3949 0.6155 0.4872 0.053 Uiso 1 1 calc R . . C35 C 0.4194(5) 0.6153(5) 0.3852(3) 0.0428(14) Uani 1 1 d U . . H35A H 0.4791 0.6748 0.3993 0.051 Uiso 1 1 calc R . . H35B H 0.4555 0.5748 0.3530 0.051 Uiso 1 1 calc R . . C36 C 0.3137(5) 0.6355(4) 0.3500(3) 0.0347(12) Uani 1 1 d U . . H36 H 0.3052 0.6198 0.3025 0.042 Uiso 1 1 calc R . . C37 C 0.2281(5) 0.6750(4) 0.3812(3) 0.0354(12) Uani 1 1 d U . . H37 H 0.1652 0.6831 0.3534 0.042 Uiso 1 1 calc R . . C38 C 0.2273(5) 0.7061(4) 0.4559(3) 0.0423(14) Uani 1 1 d U . . H38A H 0.1926 0.7612 0.4637 0.051 Uiso 1 1 calc R . . H38B H 0.3097 0.7252 0.4756 0.051 Uiso 1 1 calc R . . C39 C 0.1565(6) 0.6290(5) 0.4916(3) 0.0473(15) Uani 1 1 d U . . H39A H 0.1861 0.6406 0.5392 0.057 Uiso 1 1 calc R . . H39B H 0.0725 0.6323 0.4903 0.057 Uiso 1 1 calc R . . C40 C 0.2199(5) 0.0822(4) 0.2973(3) 0.0315(11) Uani 1 1 d U A . C41 C 0.3950(5) 0.1232(4) 0.2272(3) 0.0329(12) Uani 1 1 d U A . C42 C 0.3959(5) 0.1966(4) 0.1874(3) 0.0383(13) Uani 1 1 d U . . H42 H 0.3282 0.2107 0.1680 0.046 Uiso 1 1 calc R . . C43 C 0.5152(5) 0.2439(4) 0.1824(3) 0.0368(13) Uani 1 1 d U . . H43 H 0.5412 0.2967 0.1605 0.044 Uiso 1 1 calc R . . C44 C 0.5881(5) 0.1991(4) 0.2154(3) 0.0404(13) Uani 1 1 d U . . H44 H 0.6721 0.2167 0.2192 0.048 Uiso 1 1 calc R . . C45 C 0.5161(5) 0.1224(4) 0.2426(3) 0.0377(13) Uani 1 1 d U . . H45 H 0.5432 0.0796 0.2661 0.045 Uiso 1 1 calc R . . C46 C 0.3604(5) 0.2294(4) 0.3519(3) 0.0348(12) Uani 1 1 d U A . C47 C 0.3653(5) 0.3162(4) 0.3295(3) 0.0396(13) Uani 1 1 d U . . H47 H 0.3004 0.3349 0.3107 0.048 Uiso 1 1 calc R . . C48 C 0.4838(6) 0.3704(4) 0.3398(3) 0.0468(15) Uani 1 1 d U . . H48 H 0.5127 0.4306 0.3277 0.056 Uiso 1 1 calc R . . C49 C 0.5509(6) 0.3194(5) 0.3710(3) 0.0469(15) Uani 1 1 d U . . H49 H 0.6329 0.3402 0.3844 0.056 Uiso 1 1 calc R . . C50 C 0.4774(5) 0.2316(5) 0.3796(3) 0.0411(14) Uani 1 1 d U . . H50 H 0.5004 0.1840 0.3996 0.049 Uiso 1 1 calc R . . C51 C 0.1700(5) 0.1729(4) 0.3986(3) 0.0336(12) Uani 1 1 d U A . H51A H 0.0943 0.1261 0.3856 0.040 Uiso 1 1 calc R . . H51B H 0.1553 0.2349 0.3950 0.040 Uiso 1 1 calc R . . C52 C 0.2009(5) 0.1718(4) 0.4729(3) 0.0393(13) Uani 1 1 d U . . C53 C 0.2982(6) 0.2554(5) 0.5053(3) 0.0504(16) Uani 1 1 d U . . H53A H 0.3751 0.2473 0.4903 0.060 Uiso 1 1 calc R . . H53B H 0.2985 0.2598 0.5542 0.060 Uiso 1 1 calc R . . H53C H 0.2836 0.3127 0.4921 0.060 Uiso 1 1 calc R . . C54 C 0.2348(8) 0.0802(5) 0.4823(4) 0.0618(19) Uani 1 1 d U . . H54A H 0.3091 0.0779 0.4612 0.074 Uiso 1 1 calc R . . H54B H 0.1720 0.0269 0.4613 0.074 Uiso 1 1 calc R . . H54C H 0.2447 0.0776 0.5303 0.074 Uiso 1 1 calc R . . C55 C 0.0860(6) 0.1764(6) 0.5076(3) 0.0549(18) Uani 1 1 d U . . H55A H 0.1012 0.1841 0.5563 0.066 Uiso 1 1 calc R . . H55B H 0.0258 0.1184 0.4925 0.066 Uiso 1 1 calc R . . H55C H 0.0577 0.2295 0.4959 0.066 Uiso 1 1 calc R . . C56 C 0.251(2) -0.0301(16) 0.2020(14) 0.040(7) Uani 0.50 1 d PDU A 1 H56A H 0.1791 -0.0283 0.1757 0.048 Uiso 0.50 1 calc PR A 1 H56B H 0.2280 -0.0788 0.2309 0.048 Uiso 0.50 1 calc PR A 1 C56A C 0.236(2) -0.0193(15) 0.1941(12) 0.023(5) Uani 0.50 1 d PDU A 2 H56C H 0.1997 0.0023 0.1565 0.028 Uiso 0.50 1 calc PR A 2 H56D H 0.1745 -0.0644 0.2131 0.028 Uiso 0.50 1 calc PR A 2 C57 C 0.336(2) -0.062(2) 0.1527(13) 0.029(5) Uani 0.50 1 d PDU A 1 C57A C 0.335(3) -0.065(2) 0.1696(15) 0.042(7) Uani 0.50 1 d PDU A 2 C58 C 0.333(2) -0.0516(14) 0.0832(12) 0.030(5) Uani 0.50 1 d PU A 1 C58A C 0.354(2) -0.0703(17) 0.0987(12) 0.031(5) Uani 0.50 1 d PU A 2 C59 C 0.2737(18) 0.0039(11) 0.0519(10) 0.033(4) Uani 0.50 1 d PU A 1 H59 H 0.2306 0.0420 0.0775 0.040 Uiso 0.50 1 calc PR A 1 C59A C 0.2931(17) -0.0268(13) 0.0575(11) 0.036(4) Uani 0.50 1 d PU A 2 H59A H 0.2418 0.0098 0.0765 0.043 Uiso 0.50 1 calc PR A 2 C60 C 0.2780(13) 0.0030(12) -0.0142(7) 0.043(3) Uani 0.50 1 d PU A 1 H60 H 0.2377 0.0417 -0.0346 0.052 Uiso 0.50 1 calc PR A 1 C60A C 0.3077(13) -0.0372(14) -0.0128(10) 0.051(4) Uani 0.50 1 d PU A 2 H60A H 0.2667 -0.0061 -0.0399 0.061 Uiso 0.50 1 calc PR A 2 C61 C 0.3405(16) -0.0534(12) -0.0560(8) 0.046(3) Uani 0.50 1 d PU A 1 H61 H 0.3364 -0.0561 -0.1034 0.055 Uiso 0.50 1 calc PR A 1 C61A C 0.378(2) -0.0894(19) -0.0420(12) 0.047(6) Uani 0.50 1 d PU A 2 H61A H 0.3814 -0.0975 -0.0895 0.056 Uiso 0.50 1 calc PR A 2 C62 C 0.4063(18) -0.1032(15) -0.0256(10) 0.034(5) Uani 0.50 1 d PU A 1 H62 H 0.4505 -0.1392 -0.0524 0.041 Uiso 0.50 1 calc PR A 1 C62A C 0.4447(14) -0.1320(12) -0.0038(8) 0.047(4) Uani 0.50 1 d PU A 2 H62A H 0.4958 -0.1664 -0.0258 0.056 Uiso 0.50 1 calc PR A 2 C63 C 0.4098(14) -0.1023(10) 0.0454(9) 0.034(3) Uani 0.50 1 d PU A 1 C63A C 0.4389(15) -0.1255(13) 0.0671(8) 0.032(4) Uani 0.50 1 d PU A 2 C64 C 0.4801(16) -0.1481(11) 0.0773(12) 0.036(4) Uani 0.50 1 d PU A 1 H64 H 0.5315 -0.1772 0.0506 0.044 Uiso 0.50 1 calc PR A 1 C64A C 0.5037(17) -0.1631(13) 0.1091(13) 0.042(4) Uani 0.50 1 d PU A 2 H64A H 0.5606 -0.1944 0.0906 0.051 Uiso 0.50 1 calc PR A 2 C65 C 0.4818(17) -0.1551(13) 0.1452(14) 0.040(5) Uani 0.50 1 d PU A 1 C65A C 0.4887(19) -0.1568(14) 0.1787(10) 0.044(5) Uani 0.50 1 d PU A 2 C66 C 0.5483(13) -0.2084(10) 0.1733(10) 0.049(3) Uani 0.50 1 d PU A 1 H66 H 0.5955 -0.2410 0.1461 0.059 Uiso 0.50 1 calc PR A 1 C66A C 0.560(2) -0.1987(18) 0.2170(14) 0.043(6) Uani 0.50 1 d PU A 2 H66A H 0.6165 -0.2284 0.1960 0.052 Uiso 0.50 1 calc PR A 2 C67 C 0.545(2) -0.2133(18) 0.2407(15) 0.049(6) Uani 0.50 1 d PU A 1 H67 H 0.5936 -0.2469 0.2601 0.059 Uiso 0.50 1 calc PR A 1 C67A C 0.5464(13) -0.1957(11) 0.2861(10) 0.048(3) Uani 0.50 1 d PU A 2 H67A H 0.5923 -0.2242 0.3125 0.058 Uiso 0.50 1 calc PR A 2 C68 C 0.4713(18) -0.1700(13) 0.2817(10) 0.057(4) Uani 0.50 1 d PU A 1 H68 H 0.4691 -0.1757 0.3280 0.068 Uiso 0.50 1 calc PR A 1 C68A C 0.4610(15) -0.1484(11) 0.3165(9) 0.046(3) Uani 0.50 1 d PU A 2 H68A H 0.4547 -0.1430 0.3637 0.055 Uiso 0.50 1 calc PR A 2 C69 C 0.4055(19) -0.1214(16) 0.2555(12) 0.037(5) Uani 0.50 1 d PU A 1 H69 H 0.3552 -0.0932 0.2835 0.044 Uiso 0.50 1 calc PR A 1 C69A C 0.388(2) -0.1105(17) 0.2788(12) 0.042(5) Uani 0.50 1 d PU A 2 H69A H 0.3288 -0.0834 0.2997 0.051 Uiso 0.50 1 calc PR A 2 C70 C 0.407(3) -0.109(2) 0.1845(11) 0.034(5) Uani 0.50 1 d PU A 1 C70A C 0.401(3) -0.113(2) 0.2083(12) 0.037(5) Uani 0.50 1 d PU A 2 C71 C -0.1220(5) -0.0991(4) 0.2522(3) 0.0414(14) Uani 1 1 d U A . H71 H -0.0822 -0.1483 0.2505 0.050 Uiso 1 1 calc R . . C72 C -0.1374(5) -0.0529(4) 0.3144(3) 0.0414(14) Uani 1 1 d U A . H72 H -0.1099 -0.0748 0.3524 0.050 Uiso 1 1 calc R . . C73 C -0.1938(6) 0.0293(5) 0.3281(4) 0.0519(16) Uani 1 1 d U . . H73A H -0.1756 0.0581 0.3757 0.062 Uiso 1 1 calc R . . H73B H -0.2808 0.0062 0.3211 0.062 Uiso 1 1 calc R . . C74 C -0.1516(6) 0.1051(5) 0.2830(4) 0.0493(15) Uani 1 1 d U . . H74A H -0.2025 0.0894 0.2409 0.059 Uiso 1 1 calc R . . H74B H -0.1604 0.1662 0.3064 0.059 Uiso 1 1 calc R . . C75 C -0.0225(5) 0.1135(4) 0.2662(3) 0.0390(13) Uani 1 1 d U A . H75A H 0.0378 0.1538 0.2965 0.047 Uiso 1 1 calc R . . C76 C 0.0107(5) 0.0650(4) 0.2090(3) 0.0360(12) Uani 1 1 d U A . H76A H 0.0930 0.0773 0.2024 0.043 Uiso 1 1 calc R . . C77 C -0.0704(5) -0.0061(4) 0.1551(3) 0.0412(14) Uani 1 1 d U . . H77A H -0.0220 -0.0408 0.1266 0.049 Uiso 1 1 calc R . . H77B H -0.1099 0.0275 0.1261 0.049 Uiso 1 1 calc R . . C78 C -0.1650(5) -0.0760(4) 0.1856(3) 0.0446(14) Uani 1 1 d U . . H78B H -0.2352 -0.0498 0.1931 0.054 Uiso 1 1 calc R . . H78A H -0.1899 -0.1345 0.1531 0.054 Uiso 1 1 calc R . . C79 C 0.4192(17) -0.0729(14) 0.4593(9) 0.081(5) Uani 0.50 1 d PU . . H79A H 0.3426 -0.0743 0.4360 0.097 Uiso 0.50 1 calc PR . . H79B H 0.4359 -0.1352 0.4469 0.097 Uiso 0.50 1 calc PR . . Cl1 Cl 0.04361(13) 0.36981(10) 0.33654(7) 0.0412(3) Uani 1 1 d . . . Cl2 Cl 0.10828(14) -0.11406(10) 0.34627(7) 0.0419(6) Uani 0.998(7) 1 d P A . Cl3 Cl 0.4046(6) -0.0545(4) 0.5431(2) 0.0781(13) Uani 0.50 1 d PU . . Cl4 Cl 0.5311(5) 0.0111(4) 0.4294(3) 0.0854(14) Uani 0.50 1 d P . . Fe1 Fe 0.07538(7) 0.63443(5) 0.11276(4) 0.03073(18) Uani 1 1 d . . . Fe2 Fe 0.47384(7) 0.24303(5) 0.28133(4) 0.03227(19) Uani 1 1 d . . . N1 N 0.1700(4) 0.5240(3) 0.2041(2) 0.0305(10) Uani 1 1 d U . . N2 N 0.0183(4) 0.5913(3) 0.2512(2) 0.0285(9) Uani 1 1 d U . . N3 N 0.2919(4) 0.0623(3) 0.2472(2) 0.0334(10) Uani 1 1 d DU . . N4 N 0.2561(4) 0.1544(3) 0.3480(2) 0.0324(10) Uani 1 1 d U . . Rh1 Rh 0.16061(4) 0.52709(3) 0.35169(2) 0.03063(12) Uani 1 1 d . . . Rh2 Rh 0.04783(4) 0.00097(3) 0.29096(2) 0.03147(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(3) 0.029(3) 0.032(3) 0.002(2) 0.001(2) 0.003(2) C2 0.023(3) 0.040(3) 0.032(3) 0.000(2) 0.003(2) 0.009(2) C3 0.030(3) 0.047(3) 0.039(3) 0.004(2) 0.002(2) 0.005(2) C4 0.029(3) 0.050(3) 0.047(3) 0.014(3) 0.006(3) 0.009(3) C5 0.030(3) 0.056(4) 0.033(3) 0.001(3) 0.006(2) 0.015(3) C6 0.029(3) 0.039(3) 0.034(3) -0.001(2) 0.001(2) 0.012(2) C7 0.025(3) 0.041(3) 0.034(3) 0.004(2) 0.005(2) 0.016(2) C8 0.051(4) 0.033(3) 0.033(3) -0.003(2) 0.008(3) 0.013(3) C9 0.062(4) 0.042(3) 0.041(3) 0.009(3) 0.011(3) 0.020(3) C10 0.037(3) 0.057(4) 0.036(3) 0.009(3) 0.003(2) 0.028(3) C11 0.029(3) 0.051(3) 0.037(3) 0.004(2) 0.004(2) 0.012(3) C12 0.033(3) 0.046(3) 0.036(3) 0.002(2) 0.002(2) 0.022(3) C13 0.033(3) 0.043(3) 0.035(3) 0.003(2) -0.003(2) 0.018(2) C14 0.036(3) 0.038(3) 0.040(3) 0.008(2) 0.001(2) 0.015(2) C15 0.043(3) 0.046(3) 0.046(3) 0.013(3) 0.004(3) 0.015(3) C16 0.045(4) 0.046(4) 0.065(4) 0.018(3) 0.004(3) 0.008(3) C17 0.056(4) 0.051(4) 0.052(4) 0.016(3) -0.012(3) -0.003(3) C18 0.049(4) 0.039(3) 0.044(3) 0.004(3) -0.005(3) 0.005(3) C19 0.042(3) 0.041(3) 0.036(3) 0.006(2) -0.002(3) 0.016(3) C20 0.044(3) 0.047(3) 0.035(3) -0.002(2) 0.002(3) 0.025(3) C21 0.037(3) 0.046(3) 0.039(3) 0.002(2) -0.003(3) 0.024(3) C22 0.033(3) 0.063(4) 0.042(3) -0.002(3) 0.006(3) 0.022(3) C23 0.030(3) 0.070(4) 0.055(4) -0.002(3) 0.003(3) 0.019(3) C24 0.026(3) 0.071(4) 0.049(4) -0.007(3) -0.006(3) 0.013(3) C25 0.034(3) 0.055(4) 0.041(3) -0.008(3) -0.001(3) 0.022(3) C26 0.031(3) 0.049(3) 0.031(3) 0.003(2) -0.004(2) 0.018(2) C27 0.025(3) 0.037(3) 0.034(3) 0.001(2) 0.000(2) 0.009(2) C28 0.026(3) 0.041(3) 0.036(3) 0.003(2) 0.006(2) 0.009(2) C29 0.038(3) 0.040(3) 0.046(3) 0.003(3) 0.007(3) -0.002(3) C30 0.028(3) 0.055(4) 0.053(4) 0.004(3) 0.001(3) 0.021(3) C31 0.030(3) 0.053(4) 0.041(3) 0.003(3) 0.007(3) 0.005(3) C32 0.044(3) 0.056(4) 0.027(3) 0.008(2) 0.001(2) 0.015(3) C33 0.046(4) 0.054(4) 0.029(3) 0.010(2) -0.003(3) 0.018(3) C34 0.031(3) 0.062(4) 0.042(3) -0.001(3) -0.009(3) 0.020(3) C35 0.023(3) 0.055(4) 0.047(3) 0.000(3) -0.007(2) 0.009(3) C36 0.025(3) 0.039(3) 0.037(3) 0.000(2) -0.002(2) 0.006(2) C37 0.031(3) 0.030(3) 0.041(3) 0.000(2) 0.001(2) 0.003(2) C38 0.037(3) 0.043(3) 0.043(3) -0.007(3) -0.001(3) 0.010(3) C39 0.048(4) 0.057(4) 0.036(3) 0.000(3) 0.003(3) 0.015(3) C40 0.030(3) 0.035(3) 0.033(3) 0.009(2) -0.001(2) 0.013(2) C41 0.025(3) 0.035(3) 0.035(3) -0.002(2) 0.000(2) 0.006(2) C42 0.037(3) 0.045(3) 0.034(3) 0.002(2) -0.001(2) 0.014(3) C43 0.034(3) 0.042(3) 0.032(3) 0.009(2) 0.001(2) 0.004(2) C44 0.035(3) 0.041(3) 0.044(3) 0.001(2) 0.001(3) 0.009(3) C45 0.029(3) 0.039(3) 0.045(3) 0.005(2) 0.000(2) 0.008(2) C46 0.026(3) 0.041(3) 0.033(3) -0.001(2) 0.001(2) 0.003(2) C47 0.038(3) 0.038(3) 0.042(3) 0.000(2) 0.012(3) 0.010(3) C48 0.045(4) 0.033(3) 0.054(4) -0.008(3) 0.012(3) 0.001(3) C49 0.034(3) 0.052(4) 0.043(3) -0.009(3) 0.000(3) -0.001(3) C50 0.034(3) 0.059(4) 0.032(3) 0.005(3) 0.001(2) 0.014(3) C51 0.022(3) 0.039(3) 0.038(3) -0.002(2) 0.003(2) 0.008(2) C52 0.038(3) 0.045(3) 0.035(3) 0.002(2) 0.007(2) 0.012(3) C53 0.044(4) 0.070(4) 0.033(3) -0.008(3) 0.007(3) 0.012(3) C54 0.087(6) 0.061(4) 0.045(4) 0.012(3) 0.004(4) 0.029(4) C55 0.041(4) 0.078(5) 0.042(3) 0.000(3) 0.012(3) 0.011(3) C56 0.027(10) 0.049(10) 0.042(9) 0.007(7) -0.007(8) 0.005(9) C56A 0.013(7) 0.027(7) 0.032(8) -0.005(6) -0.004(6) 0.016(5) C57 0.018(6) 0.039(8) 0.027(12) -0.011(8) 0.004(6) 0.011(6) C57A 0.042(9) 0.033(8) 0.035(12) -0.012(9) 0.010(8) -0.015(7) C58 0.024(11) 0.027(9) 0.043(13) 0.010(7) 0.003(8) 0.012(7) C58A 0.018(7) 0.041(10) 0.033(10) 0.002(7) -0.010(6) 0.011(6) C59 0.038(8) 0.027(9) 0.039(7) 0.014(7) -0.007(6) 0.014(7) C59A 0.036(10) 0.031(10) 0.051(9) 0.023(8) -0.005(7) 0.017(7) C60 0.028(7) 0.054(8) 0.044(7) 0.003(7) -0.014(6) 0.005(6) C60A 0.027(7) 0.074(10) 0.053(9) 0.001(8) -0.011(6) 0.026(7) C61 0.042(9) 0.056(9) 0.030(7) -0.003(6) -0.008(7) 0.000(7) C61A 0.029(12) 0.064(12) 0.046(11) 0.009(8) -0.022(8) 0.009(8) C62 0.016(10) 0.042(9) 0.044(12) -0.008(8) 0.000(8) 0.016(7) C62A 0.023(7) 0.057(9) 0.051(9) -0.013(7) 0.002(6) 0.002(6) C63 0.019(7) 0.034(7) 0.050(9) -0.001(6) 0.001(6) 0.010(5) C63A 0.011(8) 0.040(10) 0.041(8) -0.005(7) -0.012(6) 0.012(6) C64 0.016(9) 0.034(8) 0.067(11) 0.011(7) 0.006(8) 0.019(6) C64A 0.025(8) 0.036(7) 0.066(13) 0.008(9) 0.000(9) 0.006(6) C65 0.021(7) 0.034(7) 0.069(14) 0.013(11) 0.020(10) 0.006(5) C65A 0.032(7) 0.035(7) 0.063(10) 0.008(9) 0.013(9) 0.001(6) C66 0.036(7) 0.038(7) 0.076(10) 0.012(7) 0.016(8) 0.013(6) C66A 0.024(7) 0.051(11) 0.057(15) 0.006(10) 0.020(10) 0.012(7) C67 0.032(10) 0.042(9) 0.073(17) 0.008(11) -0.002(12) 0.010(7) C67A 0.026(7) 0.050(8) 0.068(10) 0.005(7) 0.013(7) 0.010(6) C68 0.047(9) 0.052(9) 0.063(10) 0.010(8) -0.001(9) -0.005(8) C68A 0.040(7) 0.047(8) 0.054(9) 0.014(7) 0.007(8) 0.015(6) C69 0.028(8) 0.035(8) 0.052(13) 0.010(9) 0.010(9) 0.014(6) C69A 0.036(8) 0.028(7) 0.063(13) 0.002(8) 0.029(8) 0.008(6) C70 0.021(7) 0.034(7) 0.049(12) 0.016(10) 0.022(9) 0.001(5) C70A 0.035(8) 0.030(7) 0.047(13) 0.012(11) 0.020(11) 0.003(6) C71 0.025(3) 0.043(3) 0.050(3) 0.005(3) -0.002(3) -0.002(2) C72 0.022(3) 0.048(3) 0.054(3) 0.012(3) 0.013(3) 0.005(2) C73 0.031(3) 0.058(4) 0.067(4) 0.000(3) 0.012(3) 0.017(3) C74 0.034(3) 0.053(4) 0.064(4) 0.004(3) 0.000(3) 0.020(3) C75 0.032(3) 0.041(3) 0.044(3) 0.004(2) -0.006(3) 0.010(2) C76 0.026(3) 0.044(3) 0.039(3) 0.008(2) -0.008(2) 0.010(2) C77 0.037(3) 0.042(3) 0.040(3) 0.003(2) -0.006(3) 0.006(3) C78 0.029(3) 0.045(3) 0.055(4) -0.003(3) -0.002(3) 0.004(3) C79 0.070(11) 0.093(12) 0.083(11) 0.011(9) 0.020(9) 0.025(10) Cl1 0.0404(8) 0.0350(7) 0.0476(8) 0.0069(6) 0.0028(6) 0.0076(6) Cl2 0.0499(10) 0.0384(9) 0.0400(9) 0.0075(6) 0.0046(6) 0.0151(6) Cl3 0.095(4) 0.078(3) 0.071(3) 0.014(2) 0.006(3) 0.040(3) Cl4 0.076(3) 0.089(4) 0.102(4) 0.032(3) 0.026(3) 0.030(3) Fe1 0.0259(4) 0.0339(4) 0.0315(4) 0.0026(3) 0.0019(3) 0.0067(3) Fe2 0.0270(4) 0.0346(4) 0.0340(4) 0.0015(3) 0.0024(3) 0.0072(3) N1 0.027(2) 0.038(2) 0.028(2) 0.0024(18) -0.0028(18) 0.0126(19) N2 0.024(2) 0.032(2) 0.030(2) 0.0028(17) 0.0038(18) 0.0094(18) N3 0.030(2) 0.035(2) 0.034(2) 0.0008(19) 0.003(2) 0.0090(19) N4 0.029(2) 0.036(2) 0.033(2) 0.0040(18) 0.0020(19) 0.0095(19) Rh1 0.0272(2) 0.0344(2) 0.0302(2) 0.00340(16) 0.00051(17) 0.00838(17) Rh2 0.0253(2) 0.0325(2) 0.0363(2) 0.00388(17) 0.00238(18) 0.00733(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.358(7) . ? C1 N2 1.366(7) . ? C1 Rh1 2.068(5) . ? C2 N1 1.420(7) . ? C2 C6 1.443(7) . ? C2 C3 1.449(8) . ? C2 Fe1 1.968(6) . ? C3 C4 1.428(8) . ? C3 Fe1 2.031(6) . ? C3 H3A 0.9500 . ? C4 C5 1.420(8) . ? C4 Fe1 2.069(6) . ? C4 H4A 0.9500 . ? C5 C6 1.415(8) . ? C5 Fe1 2.062(6) . ? C5 H5A 0.9500 . ? C6 Fe1 2.017(6) . ? C6 H6A 0.9500 . ? C7 N2 1.417(7) . ? C7 C8 1.430(8) . ? C7 C11 1.451(8) . ? C7 Fe1 1.971(5) . ? C8 C9 1.422(9) . ? C8 Fe1 2.028(5) . ? C8 H8A 0.9500 . ? C9 C10 1.419(9) . ? C9 Fe1 2.045(7) . ? C9 H9A 0.9500 . ? C10 C11 1.419(8) . ? C10 Fe1 2.050(6) . ? C10 H10A 0.9500 . ? C11 Fe1 2.017(6) . ? C11 H11A 0.9500 . ? C12 N1 1.502(7) . ? C12 C13 1.515(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.415(8) . ? C13 C26 1.423(8) . ? C14 C19 1.428(8) . ? C14 C15 1.440(9) . ? C15 C16 1.363(9) . ? C15 H15A 0.9500 . ? C16 C17 1.410(10) . ? C16 H16A 0.9500 . ? C17 C18 1.360(10) . ? C17 H17A 0.9500 . ? C18 C19 1.428(8) . ? C18 H18A 0.9500 . ? C19 C20 1.399(9) . ? C20 C21 1.399(9) . ? C20 H20A 0.9500 . ? C21 C22 1.429(9) . ? C21 C26 1.444(8) . ? C22 C23 1.354(9) . ? C22 H22A 0.9500 . ? C23 C24 1.420(9) . ? C23 H23A 0.9500 . ? C24 C25 1.364(9) . ? C24 H24A 0.9500 . ? C25 C26 1.427(8) . ? C25 H25A 0.9500 . ? C27 N2 1.481(7) . ? C27 C28 1.549(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.537(8) . ? C28 C31 1.548(8) . ? C28 C30 1.548(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31C 0.9800 . ? C31 H31B 0.9800 . ? C32 C33 1.366(9) . ? C32 C39 1.526(9) . ? C32 Rh1 2.189(5) . ? C32 H32A 0.9500 . ? C33 C34 1.517(9) . ? C33 Rh1 2.231(5) . ? C33 H33A 0.9500 . ? C34 C35 1.539(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.515(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.391(8) . ? C36 Rh1 2.113(5) . ? C36 H36 0.9500 . ? C37 C38 1.513(8) . ? C37 Rh1 2.148(5) . ? C37 H37 0.9500 . ? C38 C39 1.530(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N4 1.352(7) . ? C40 N3 1.373(7) . ? C40 Rh2 2.075(5) . ? C41 N3 1.433(7) . ? C41 C45 1.438(8) . ? C41 C42 1.444(8) . ? C41 Fe2 1.960(5) . ? C42 C43 1.417(8) . ? C42 Fe2 2.032(5) . ? C42 H42 0.9500 . ? C43 C44 1.404(8) . ? C43 Fe2 2.067(6) . ? C43 H43 0.9500 . ? C44 C45 1.438(8) . ? C44 Fe2 2.053(6) . ? C44 H44 0.9500 . ? C45 Fe2 2.026(6) . ? C45 H45 0.9500 . ? C46 C47 1.419(8) . ? C46 N4 1.438(7) . ? C46 C50 1.449(8) . ? C46 Fe2 1.968(6) . ? C47 C48 1.420(9) . ? C47 Fe2 2.031(6) . ? C47 H47 0.9500 . ? C48 C49 1.404(10) . ? C48 Fe2 2.060(6) . ? C48 H48 0.9500 . ? C49 C50 1.422(9) . ? C49 Fe2 2.054(6) . ? C49 H49 0.9500 . ? C50 Fe2 2.014(6) . ? C50 H50 0.9500 . ? C51 N4 1.493(7) . ? C51 C52 1.535(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.526(9) . ? C52 C55 1.537(9) . ? C52 C54 1.539(9) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 N3 1.504(16) . ? C56 C57 1.518(17) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C56A N3 1.504(14) . ? C56A C57A 1.525(18) . ? C56A H56C 0.9900 . ? C56A H56D 0.9900 . ? C57 C70 1.40(4) . ? C57 C58 1.43(3) . ? C57A C70A 1.44(4) . ? C57A C58A 1.45(3) . ? C58 C59 1.39(2) . ? C58 C63 1.46(3) . ? C58A C59A 1.398(19) . ? C58A C63A 1.52(3) . ? C59 C60 1.33(2) . ? C59 H59 0.9500 . ? C59A C60A 1.42(3) . ? C59A H59A 0.9500 . ? C60 C61 1.43(2) . ? C60 H60 0.9500 . ? C60A C61A 1.34(3) . ? C60A H60A 0.9500 . ? C61 C62 1.37(2) . ? C61 H61 0.9500 . ? C61A C62A 1.39(2) . ? C61A H61A 0.9500 . ? C62 C63 1.43(3) . ? C62 H62 0.9500 . ? C62A C63A 1.42(2) . ? C62A H62A 0.9500 . ? C63 C64 1.38(2) . ? C63A C64A 1.38(3) . ? C64 C65 1.39(3) . ? C64 H64 0.9500 . ? C64A C65A 1.41(3) . ? C64A H64A 0.9500 . ? C65 C66 1.39(3) . ? C65 C70 1.42(4) . ? C65A C66A 1.42(4) . ? C65A C70A 1.43(4) . ? C66 C67 1.37(3) . ? C66 H66 0.9500 . ? C66A C67A 1.40(3) . ? C66A H66A 0.9500 . ? C67 C68 1.40(4) . ? C67 H67 0.9500 . ? C67A C68A 1.45(2) . ? C67A H67A 0.9500 . ? C68 C69 1.32(3) . ? C68 H68 0.9500 . ? C68A C69A 1.39(3) . ? C68A H68A 0.9500 . ? C69 C70 1.47(2) . ? C69 H69 0.9500 . ? C69A C70A 1.43(3) . ? C69A H69A 0.9500 . ? C71 C72 1.379(9) . ? C71 C78 1.534(9) . ? C71 Rh2 2.225(5) . ? C71 H71 0.9500 . ? C72 C73 1.513(9) . ? C72 Rh2 2.209(5) . ? C72 H72 0.9500 . ? C73 C74 1.551(10) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.531(9) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.384(8) . ? C75 Rh2 2.140(6) . ? C75 H75A 0.9500 . ? C76 C77 1.530(7) . ? C76 Rh2 2.107(5) . ? C76 H76A 0.9500 . ? C77 C78 1.537(8) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78B 0.9900 . ? C78 H78A 0.9900 . ? C79 Cl3 1.692(18) . ? C79 Cl4 1.769(19) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? Cl1 Rh1 2.3920(14) . ? Cl2 Rh2 2.3961(15) . ? Cl3 Cl4 0.967(6) 2_656 ? Cl4 Cl3 0.967(6) 2_656 ? 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 N1 C1 N2 121.7(4) . . ? N1 C1 Rh1 119.1(4) . . ? N2 C1 Rh1 118.9(4) . . ? N1 C2 C6 127.5(5) . . ? N1 C2 C3 125.2(5) . . ? C6 C2 C3 107.3(5) . . ? N1 C2 Fe1 122.8(4) . . ? C6 C2 Fe1 70.6(3) . . ? C3 C2 Fe1 71.1(3) . . ? C4 C3 C2 107.3(5) . . ? C4 C3 Fe1 71.1(3) . . ? C2 C3 Fe1 66.4(3) . . ? C4 C3 H3A 126.3 . . ? C2 C3 H3A 126.3 . . ? Fe1 C3 H3A 127.7 . . ? C5 C4 C3 108.6(5) . . ? C5 C4 Fe1 69.6(3) . . ? C3 C4 Fe1 68.2(3) . . ? C5 C4 H4A 125.7 . . ? C3 C4 H4A 125.7 . . ? Fe1 C4 H4A 128.1 . . ? C6 C5 C4 108.7(5) . . ? C6 C5 Fe1 68.0(3) . . ? C4 C5 Fe1 70.2(3) . . ? C6 C5 H5A 125.6 . . ? C4 C5 H5A 125.6 . . ? Fe1 C5 H5A 127.7 . . ? C5 C6 C2 108.0(5) . . ? C5 C6 Fe1 71.4(3) . . ? C2 C6 Fe1 66.9(3) . . ? C5 C6 H6A 126.0 . . ? C2 C6 H6A 126.0 . . ? Fe1 C6 H6A 127.2 . . ? N2 C7 C8 124.6(5) . . ? N2 C7 C11 128.4(5) . . ? C8 C7 C11 107.0(5) . . ? N2 C7 Fe1 124.7(4) . . ? C8 C7 Fe1 71.2(3) . . ? C11 C7 Fe1 70.4(3) . . ? C9 C8 C7 108.5(5) . . ? C9 C8 Fe1 70.2(3) . . ? C7 C8 Fe1 66.9(3) . . ? C9 C8 H8A 125.7 . . ? C7 C8 H8A 125.7 . . ? Fe1 C8 H8A 128.7 . . ? C10 C9 C8 107.9(5) . . ? C10 C9 Fe1 69.9(3) . . ? C8 C9 Fe1 68.9(3) . . ? C10 C9 H9A 126.0 . . ? C8 C9 H9A 126.0 . . ? Fe1 C9 H9A 126.7 . . ? C11 C10 C9 108.8(5) . . ? C11 C10 Fe1 68.3(3) . . ? C9 C10 Fe1 69.5(4) . . ? C11 C10 H10A 125.6 . . ? C9 C10 H10A 125.6 . . ? Fe1 C10 H10A 128.1 . . ? C10 C11 C7 107.6(5) . . ? C10 C11 Fe1 70.8(3) . . ? C7 C11 Fe1 67.0(3) . . ? C10 C11 H11A 126.2 . . ? C7 C11 H11A 126.2 . . ? Fe1 C11 H11A 127.5 . . ? N1 C12 C13 111.5(4) . . ? N1 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N1 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C26 119.9(5) . . ? C14 C13 C12 119.7(5) . . ? C26 C13 C12 120.4(5) . . ? C13 C14 C19 120.5(5) . . ? C13 C14 C15 121.9(5) . . ? C19 C14 C15 117.5(5) . . ? C16 C15 C14 120.6(6) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 121.7(7) . . ? C15 C16 H16A 119.1 . . ? C17 C16 H16A 119.1 . . ? C18 C17 C16 119.4(6) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C20 C19 C14 118.8(5) . . ? C20 C19 C18 121.7(5) . . ? C14 C19 C18 119.4(6) . . ? C21 C20 C19 122.4(5) . . ? C21 C20 H20A 118.8 . . ? C19 C20 H20A 118.8 . . ? C20 C21 C22 121.6(5) . . ? C20 C21 C26 118.9(5) . . ? C22 C21 C26 119.5(5) . . ? C23 C22 C21 121.3(6) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C24 119.7(6) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C25 C24 C23 120.8(6) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 121.9(6) . . ? C24 C25 H25A 119.0 . . ? C26 C25 H25A 119.0 . . ? C13 C26 C25 123.8(5) . . ? C13 C26 C21 119.4(5) . . ? C25 C26 C21 116.7(5) . . ? N2 C27 C28 117.1(4) . . ? N2 C27 H27A 108.0 . . ? C28 C27 H27A 108.0 . . ? N2 C27 H27B 108.0 . . ? C28 C27 H27B 108.0 . . ? H27A C27 H27B 107.3 . . ? C29 C28 C31 109.0(5) . . ? C29 C28 C30 111.7(5) . . ? C31 C28 C30 108.4(5) . . ? C29 C28 C27 112.1(5) . . ? C31 C28 C27 104.5(4) . . ? C30 C28 C27 110.9(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? H31C C31 H31B 109.5 . . ? C33 C32 C39 126.1(6) . . ? C33 C32 Rh1 73.7(3) . . ? C39 C32 Rh1 107.0(4) . . ? C33 C32 H32A 116.9 . . ? C39 C32 H32A 116.9 . . ? Rh1 C32 H32A 89.3 . . ? C32 C33 C34 125.8(6) . . ? C32 C33 Rh1 70.3(3) . . ? C34 C33 Rh1 111.1(4) . . ? C32 C33 H33A 117.1 . . ? C34 C33 H33A 117.1 . . ? Rh1 C33 H33A 88.6 . . ? C33 C34 C35 112.8(5) . . ? C33 C34 H34A 109.0 . . ? C35 C34 H34A 109.0 . . ? C33 C34 H34B 109.0 . . ? C35 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C36 C35 C34 113.3(5) . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C34 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C35 125.7(5) . . ? C37 C36 Rh1 72.3(3) . . ? C35 C36 Rh1 111.0(4) . . ? C37 C36 H36 117.2 . . ? C35 C36 H36 117.2 . . ? Rh1 C36 H36 86.6 . . ? C36 C37 C38 125.1(5) . . ? C36 C37 Rh1 69.6(3) . . ? C38 C37 Rh1 113.2(4) . . ? C36 C37 H37 117.5 . . ? C38 C37 H37 117.5 . . ? Rh1 C37 H37 87.2 . . ? C37 C38 C39 112.4(5) . . ? C37 C38 H38A 109.1 . . ? C39 C38 H38A 109.1 . . ? C37 C38 H38B 109.1 . . ? C39 C38 H38B 109.1 . . ? H38A C38 H38B 107.9 . . ? C32 C39 C38 113.6(5) . . ? C32 C39 H39A 108.9 . . ? C38 C39 H39A 108.9 . . ? C32 C39 H39B 108.9 . . ? C38 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? N4 C40 N3 122.2(5) . . ? N4 C40 Rh2 120.0(4) . . ? N3 C40 Rh2 117.8(4) . . ? N3 C41 C45 126.6(5) . . ? N3 C41 C42 125.9(5) . . ? C45 C41 C42 107.5(5) . . ? N3 C41 Fe2 122.8(4) . . ? C45 C41 Fe2 71.3(3) . . ? C42 C41 Fe2 71.5(3) . . ? C43 C42 C41 108.2(5) . . ? C43 C42 Fe2 71.1(3) . . ? C41 C42 Fe2 66.2(3) . . ? C43 C42 H42 125.9 . . ? C41 C42 H42 125.9 . . ? Fe2 C42 H42 128.4 . . ? C44 C43 C42 108.1(5) . . ? C44 C43 Fe2 69.5(3) . . ? C42 C43 Fe2 68.4(3) . . ? C44 C43 H43 126.0 . . ? C42 C43 H43 126.0 . . ? Fe2 C43 H43 127.6 . . ? C43 C44 C45 109.5(5) . . ? C43 C44 Fe2 70.6(3) . . ? C45 C44 Fe2 68.4(3) . . ? C43 C44 H44 125.2 . . ? C45 C44 H44 125.2 . . ? Fe2 C44 H44 127.4 . . ? C44 C45 C41 106.5(5) . . ? C44 C45 Fe2 70.4(3) . . ? C41 C45 Fe2 66.4(3) . . ? C44 C45 H45 126.7 . . ? C41 C45 H45 126.7 . . ? Fe2 C45 H45 127.9 . . ? C47 C46 N4 125.0(5) . . ? C47 C46 C50 107.8(5) . . ? N4 C46 C50 127.2(5) . . ? C47 C46 Fe2 71.6(3) . . ? N4 C46 Fe2 124.1(4) . . ? C50 C46 Fe2 70.4(3) . . ? C46 C47 C48 108.2(6) . . ? C46 C47 Fe2 66.8(3) . . ? C48 C47 Fe2 70.8(4) . . ? C46 C47 H47 125.9 . . ? C48 C47 H47 125.9 . . ? Fe2 C47 H47 128.1 . . ? C49 C48 C47 108.0(6) . . ? C49 C48 Fe2 69.8(4) . . ? C47 C48 Fe2 68.6(3) . . ? C49 C48 H48 126.0 . . ? C47 C48 H48 126.0 . . ? Fe2 C48 H48 127.2 . . ? C48 C49 C50 109.5(6) . . ? C48 C49 Fe2 70.3(3) . . ? C50 C49 Fe2 68.1(3) . . ? C48 C49 H49 125.2 . . ? C50 C49 H49 125.2 . . ? Fe2 C49 H49 128.0 . . ? C49 C50 C46 106.4(6) . . ? C49 C50 Fe2 71.0(3) . . ? C46 C50 Fe2 66.9(3) . . ? C49 C50 H50 126.8 . . ? C46 C50 H50 126.8 . . ? Fe2 C50 H50 126.7 . . ? N4 C51 C52 119.0(5) . . ? N4 C51 H51A 107.6 . . ? C52 C51 H51A 107.6 . . ? N4 C51 H51B 107.6 . . ? C52 C51 H51B 107.6 . . ? H51A C51 H51B 107.0 . . ? C53 C52 C51 113.8(5) . . ? C53 C52 C55 108.3(5) . . ? C51 C52 C55 104.4(5) . . ? C53 C52 C54 109.9(6) . . ? C51 C52 C54 110.9(5) . . ? C55 C52 C54 109.3(6) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N3 C56 C57 119(2) . . ? N3 C56 H56A 107.5 . . ? C57 C56 H56A 107.5 . . ? N3 C56 H56B 107.5 . . ? C57 C56 H56B 107.5 . . ? H56A C56 H56B 107.0 . . ? N3 C56A C57A 107.1(19) . . ? N3 C56A H56C 110.3 . . ? C57A C56A H56C 110.3 . . ? N3 C56A H56D 110.3 . . ? C57A C56A H56D 110.3 . . ? H56C C56A H56D 108.6 . . ? C70 C57 C58 126.5(19) . . ? C70 C57 C56 110(2) . . ? C58 C57 C56 124(2) . . ? C70A C57A C58A 117(2) . . ? C70A C57A C56A 126(2) . . ? C58A C57A C56A 116(2) . . ? C59 C58 C57 128(2) . . ? C59 C58 C63 120.3(19) . . ? C57 C58 C63 111.9(19) . . ? C59A C58A C57A 121(2) . . ? C59A C58A C63A 119(2) . . ? C57A C58A C63A 120.6(19) . . ? C60 C59 C58 119.6(18) . . ? C60 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? C58A C59A C60A 120(2) . . ? C58A C59A H59A 120.0 . . ? C60A C59A H59A 120.0 . . ? C59 C60 C61 123.2(16) . . ? C59 C60 H60 118.4 . . ? C61 C60 H60 118.4 . . ? C61A C60A C59A 122.2(18) . . ? C61A C60A H60A 118.9 . . ? C59A C60A H60A 118.9 . . ? C62 C61 C60 118.1(15) . . ? C62 C61 H61 120.9 . . ? C60 C61 H61 120.9 . . ? C60A C61A C62A 121(2) . . ? C60A C61A H61A 119.5 . . ? C62A C61A H61A 119.5 . . ? C61 C62 C63 121.5(17) . . ? C61 C62 H62 119.2 . . ? C63 C62 H62 119.2 . . ? C61A C62A C63A 122(2) . . ? C61A C62A H62A 119.0 . . ? C63A C62A H62A 119.0 . . ? C64 C63 C62 122.4(17) . . ? C64 C63 C58 121.0(17) . . ? C62 C63 C58 116.6(17) . . ? C64A C63A C62A 126(2) . . ? C64A C63A C58A 117.7(16) . . ? C62A C63A C58A 116.1(19) . . ? C63 C64 C65 125.2(17) . . ? C63 C64 H64 117.4 . . ? C65 C64 H64 117.4 . . ? C63A C64A C65A 122(2) . . ? C63A C64A H64A 118.8 . . ? C65A C64A H64A 118.8 . . ? C64 C65 C66 122(2) . . ? C64 C65 C70 116.6(19) . . ? C66 C65 C70 121(2) . . ? C64A C65A C66A 117(2) . . ? C64A C65A C70A 120(2) . . ? C66A C65A C70A 122.0(19) . . ? C67 C66 C65 119(2) . . ? C67 C66 H66 120.3 . . ? C65 C66 H66 120.3 . . ? C67A C66A C65A 119(2) . . ? C67A C66A H66A 120.3 . . ? C65A C66A H66A 120.3 . . ? C66 C67 C68 122(2) . . ? C66 C67 H67 119.1 . . ? C68 C67 H67 119.1 . . ? C66A C67A C68A 118.6(19) . . ? C66A C67A H67A 120.7 . . ? C68A C67A H67A 120.7 . . ? C69 C68 C67 119(2) . . ? C69 C68 H68 120.3 . . ? C67 C68 H68 120.3 . . ? C69A C68A C67A 122.2(17) . . ? C69A C68A H68A 118.9 . . ? C67A C68A H68A 118.9 . . ? C68 C69 C70 123(2) . . ? C68 C69 H69 118.7 . . ? C70 C69 H69 118.7 . . ? C68A C69A C70A 120(2) . . ? C68A C69A H69A 120.2 . . ? C70A C69A H69A 120.2 . . ? C57 C70 C65 118.7(18) . . ? C57 C70 C69 125(2) . . ? C65 C70 C69 116(3) . . ? C69A C70A C65A 118(2) . . ? C69A C70A C57A 121(2) . . ? C65A C70A C57A 121(2) . . ? C72 C71 C78 124.0(6) . . ? C72 C71 Rh2 71.2(3) . . ? C78 C71 Rh2 110.2(4) . . ? C72 C71 H71 118.0 . . ? C78 C71 H71 118.0 . . ? Rh2 C71 H71 88.5 . . ? C71 C72 C73 126.3(6) . . ? C71 C72 Rh2 72.5(3) . . ? C73 C72 Rh2 107.9(4) . . ? C71 C72 H72 116.8 . . ? C73 C72 H72 116.8 . . ? Rh2 C72 H72 89.5 . . ? C72 C73 C74 113.5(5) . . ? C72 C73 H73A 108.9 . . ? C74 C73 H73A 108.9 . . ? C72 C73 H73B 108.9 . . ? C74 C73 H73B 108.9 . . ? H73A C73 H73B 107.7 . . ? C75 C74 C73 112.0(5) . . ? C75 C74 H74A 109.2 . . ? C73 C74 H74A 109.2 . . ? C75 C74 H74B 109.2 . . ? C73 C74 H74B 109.2 . . ? H74A C74 H74B 107.9 . . ? C76 C75 C74 123.1(5) . . ? C76 C75 Rh2 69.7(3) . . ? C74 C75 Rh2 113.6(4) . . ? C76 C75 H75A 118.4 . . ? C74 C75 H75A 118.4 . . ? Rh2 C75 H75A 86.8 . . ? C75 C76 C77 127.3(5) . . ? C75 C76 Rh2 72.3(3) . . ? C77 C76 Rh2 110.7(4) . . ? C75 C76 H76A 116.3 . . ? C77 C76 H76A 116.3 . . ? Rh2 C76 H76A 86.8 . . ? C76 C77 C78 112.2(5) . . ? C76 C77 H77A 109.2 . . ? C78 C77 H77A 109.2 . . ? C76 C77 H77B 109.2 . . ? C78 C77 H77B 109.2 . . ? H77A C77 H77B 107.9 . . ? C71 C78 C77 113.2(5) . . ? C71 C78 H78B 108.9 . . ? C77 C78 H78B 108.9 . . ? C71 C78 H78A 108.9 . . ? C77 C78 H78A 108.9 . . ? H78B C78 H78A 107.8 . . ? Cl3 C79 Cl4 115.2(11) . . ? Cl3 C79 H79A 108.5 . . ? Cl4 C79 H79A 108.5 . . ? Cl3 C79 H79B 108.5 . . ? Cl4 C79 H79B 108.5 . . ? H79A C79 H79B 107.5 . . ? Cl4 Cl3 C79 117.5(9) 2_656 . ? Cl3 Cl4 C79 125.1(9) 2_656 . ? C2 Fe1 C7 92.9(2) . . ? C2 Fe1 C11 112.0(2) . . ? C7 Fe1 C11 42.7(2) . . ? C2 Fe1 C6 42.4(2) . . ? C7 Fe1 C6 114.4(2) . . ? C11 Fe1 C6 102.5(2) . . ? C2 Fe1 C8 114.0(2) . . ? C7 Fe1 C8 41.9(2) . . ? C11 Fe1 C8 69.8(2) . . ? C6 Fe1 C8 152.2(2) . . ? C2 Fe1 C3 42.5(2) . . ? C7 Fe1 C3 111.5(2) . . ? C11 Fe1 C3 149.1(2) . . ? C6 Fe1 C3 70.2(2) . . ? C8 Fe1 C3 102.1(3) . . ? C2 Fe1 C9 154.3(2) . . ? C7 Fe1 C9 70.4(2) . . ? C11 Fe1 C9 69.2(3) . . ? C6 Fe1 C9 162.8(2) . . ? C8 Fe1 C9 40.9(2) . . ? C3 Fe1 C9 124.7(3) . . ? C2 Fe1 C10 151.9(2) . . ? C7 Fe1 C10 70.3(2) . . ? C11 Fe1 C10 40.8(2) . . ? C6 Fe1 C10 123.7(2) . . ? C8 Fe1 C10 68.6(2) . . ? C3 Fe1 C10 164.7(3) . . ? C9 Fe1 C10 40.6(3) . . ? C2 Fe1 C5 70.0(2) . . ? C7 Fe1 C5 154.7(2) . . ? C11 Fe1 C5 125.6(2) . . ? C6 Fe1 C5 40.6(2) . . ? C8 Fe1 C5 162.6(2) . . ? C3 Fe1 C5 68.8(2) . . ? C9 Fe1 C5 131.7(2) . . ? C10 Fe1 C5 116.5(2) . . ? C2 Fe1 C4 70.0(2) . . ? C7 Fe1 C4 151.3(2) . . ? C11 Fe1 C4 165.3(2) . . ? C6 Fe1 C4 68.6(2) . . ? C8 Fe1 C4 123.5(3) . . ? C3 Fe1 C4 40.7(2) . . ? C9 Fe1 C4 115.8(3) . . ? C10 Fe1 C4 133.8(2) . . ? C5 Fe1 C4 40.2(2) . . ? C41 Fe2 C46 93.6(2) . . ? C41 Fe2 C50 110.6(2) . . ? C46 Fe2 C50 42.7(2) . . ? C41 Fe2 C45 42.2(2) . . ? C46 Fe2 C45 114.1(2) . . ? C50 Fe2 C45 100.2(3) . . ? C41 Fe2 C47 115.7(2) . . ? C46 Fe2 C47 41.5(2) . . ? C50 Fe2 C47 69.9(3) . . ? C45 Fe2 C47 152.6(2) . . ? C41 Fe2 C42 42.4(2) . . ? C46 Fe2 C42 113.0(2) . . ? C50 Fe2 C42 148.9(2) . . ? C45 Fe2 C42 69.9(2) . . ? C47 Fe2 C42 105.0(2) . . ? C41 Fe2 C44 70.1(2) . . ? C46 Fe2 C44 154.9(2) . . ? C50 Fe2 C44 124.2(3) . . ? C45 Fe2 C44 41.3(2) . . ? C47 Fe2 C44 163.2(2) . . ? C42 Fe2 C44 68.0(2) . . ? C41 Fe2 C49 150.4(3) . . ? C46 Fe2 C49 69.7(2) . . ? C50 Fe2 C49 40.9(3) . . ? C45 Fe2 C49 121.6(3) . . ? C47 Fe2 C49 68.0(3) . . ? C42 Fe2 C49 166.9(3) . . ? C44 Fe2 C49 115.5(3) . . ? C41 Fe2 C48 156.1(2) . . ? C46 Fe2 C48 69.6(2) . . ? C50 Fe2 C48 69.0(3) . . ? C45 Fe2 C48 160.4(3) . . ? C47 Fe2 C48 40.6(2) . . ? C42 Fe2 C48 127.7(3) . . ? C44 Fe2 C48 131.2(2) . . ? C49 Fe2 C48 39.9(3) . . ? C41 Fe2 C43 70.2(2) . . ? C46 Fe2 C43 152.4(2) . . ? C50 Fe2 C43 163.7(2) . . ? C45 Fe2 C43 69.1(2) . . ? C47 Fe2 C43 125.2(2) . . ? C42 Fe2 C43 40.4(2) . . ? C44 Fe2 C43 39.8(2) . . ? C49 Fe2 C43 134.0(2) . . ? C48 Fe2 C43 117.3(3) . . ? C1 N1 C2 128.9(4) . . ? C1 N1 C12 115.8(4) . . ? C2 N1 C12 114.5(4) . . ? C1 N2 C7 127.1(4) . . ? C1 N2 C27 117.6(4) . . ? C7 N2 C27 114.8(4) . . ? C40 N3 C41 127.9(4) . . ? C40 N3 C56 117.0(12) . . ? C41 N3 C56 114.6(12) . . ? C40 N3 C56A 115.1(11) . . ? C41 N3 C56A 113.9(11) . . ? C56 N3 C56A 12(2) . . ? C40 N4 C46 127.1(5) . . ? C40 N4 C51 118.3(4) . . ? C46 N4 C51 113.1(4) . . ? C1 Rh1 C36 88.7(2) . . ? C1 Rh1 C37 90.9(2) . . ? C36 Rh1 C37 38.1(2) . . ? C1 Rh1 C32 158.9(2) . . ? C36 Rh1 C32 97.1(2) . . ? C37 Rh1 C32 81.7(2) . . ? C1 Rh1 C33 164.3(2) . . ? C36 Rh1 C33 81.2(2) . . ? C37 Rh1 C33 88.6(2) . . ? C32 Rh1 C33 36.0(2) . . ? C1 Rh1 Cl1 92.63(14) . . ? C36 Rh1 Cl1 156.74(16) . . ? C37 Rh1 Cl1 164.80(16) . . ? C32 Rh1 Cl1 89.91(18) . . ? C33 Rh1 Cl1 91.99(17) . . ? C40 Rh2 C76 88.5(2) . . ? C40 Rh2 C75 91.8(2) . . ? C76 Rh2 C75 38.0(2) . . ? C40 Rh2 C72 161.1(2) . . ? C76 Rh2 C72 97.0(2) . . ? C75 Rh2 C72 81.7(2) . . ? C40 Rh2 C71 162.3(2) . . ? C76 Rh2 C71 81.8(2) . . ? C75 Rh2 C71 89.6(2) . . ? C72 Rh2 C71 36.2(2) . . ? C40 Rh2 Cl2 91.67(15) . . ? C76 Rh2 Cl2 156.44(17) . . ? C75 Rh2 Cl2 165.26(17) . . ? C72 Rh2 Cl2 90.43(17) . . ? C71 Rh2 Cl2 91.42(17) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.228 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.132 _database_code_depnum_ccdc_archive 'CCDC 961494' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_i1125 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H30 Cl Fe N2 O2 Rh' _chemical_formula_sum 'C33 H30 Cl Fe N2 O2 Rh' _chemical_formula_weight 680.80 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_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' _cell_length_a 21.200(2) _cell_length_b 6.6361(5) _cell_length_c 21.901(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.394(8) _cell_angle_gamma 90.00 _cell_volume 2848.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4577 _cell_measurement_theta_min 1.14 _cell_measurement_theta_max 24.41 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.216 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7432 _exptl_absorpt_correction_T_max 0.8831 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 150 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 14762 _diffrn_reflns_av_R_equivalents 0.1343 _diffrn_reflns_av_sigmaI/netI 0.1978 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.19 _reflns_number_total 5061 _reflns_number_gt 2202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie. 2006)' _computing_cell_refinement 'X-Area (Stoe & Cie. 2006)' _computing_data_reduction 'X-Area (Stoe & Cie. 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 win. (Farrugia 2008)' _computing_publication_material 'PLATON (Spek 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5061 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1472 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 0.766 _refine_ls_restrained_S_all 0.766 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0081(3) 0.1450(13) 0.2460(4) 0.031(2) Uani 1 1 d . . . C2 C 0.0540(3) 0.2029(13) 0.3675(4) 0.0334(19) Uani 1 1 d . . . C3 C 0.0506(4) 0.0812(14) 0.4189(4) 0.042(2) Uani 1 1 d . . . H3A H 0.0435 -0.0603 0.4168 0.051 Uiso 1 1 calc R . . C4 C 0.0597(4) 0.2062(17) 0.4748(4) 0.054(3) Uani 1 1 d . . . H4A H 0.0591 0.1642 0.5160 0.065 Uiso 1 1 calc R . . C5 C 0.0699(4) 0.4050(15) 0.4566(5) 0.051(3) Uani 1 1 d . . . H5A H 0.0766 0.5206 0.4839 0.061 Uiso 1 1 calc R . . C6 C 0.0686(3) 0.4047(14) 0.3917(4) 0.040(2) Uani 1 1 d . . . H6A H 0.0761 0.5173 0.3685 0.048 Uiso 1 1 calc R . . C7 C -0.0862(4) 0.2688(13) 0.2993(4) 0.038(2) Uani 1 1 d . . . C8 C -0.0889(3) 0.4722(17) 0.3205(4) 0.042(2) Uani 1 1 d . . . H8A H -0.0798 0.5914 0.3013 0.051 Uiso 1 1 calc R . . C9 C -0.1080(4) 0.4600(18) 0.3763(4) 0.049(3) Uani 1 1 d . . . H9A H -0.1135 0.5711 0.4011 0.059 Uiso 1 1 calc R . . C10 C -0.1172(4) 0.2549(15) 0.3884(4) 0.047(2) Uani 1 1 d . . . H10A H -0.1290 0.2056 0.4234 0.056 Uiso 1 1 calc R . . C11 C -0.1063(4) 0.1362(14) 0.3403(4) 0.042(2) Uani 1 1 d . . . H11A H -0.1112 -0.0059 0.3358 0.051 Uiso 1 1 calc R . . C12 C -0.0003(4) -0.1234(13) 0.0855(4) 0.039(2) Uani 1 1 d . . . C13 C 0.0153(4) 0.2454(14) 0.1286(4) 0.039(2) Uani 1 1 d . . . C14 C 0.1104(3) 0.0397(13) 0.3021(3) 0.032(2) Uani 1 1 d . . . H14B H 0.1086 0.0415 0.2563 0.038 Uiso 1 1 calc R . . H14A H 0.1097 -0.1032 0.3148 0.038 Uiso 1 1 calc R . . C15 C 0.1768(4) 0.1298(13) 0.3462(4) 0.035(2) Uani 1 1 d . . . C16 C 0.2225(3) 0.0261(15) 0.4024(4) 0.037(2) Uani 1 1 d . . . C17 C 0.2035(4) -0.1574(13) 0.4267(4) 0.038(2) Uani 1 1 d . . . H17A H 0.1585 -0.2086 0.4054 0.045 Uiso 1 1 calc R . . C18 C 0.2492(4) -0.2597(16) 0.4799(5) 0.054(3) Uani 1 1 d . . . H18A H 0.2347 -0.3767 0.4960 0.065 Uiso 1 1 calc R . . C19 C 0.3180(4) -0.1922(17) 0.5112(4) 0.052(3) Uani 1 1 d . . . H19A H 0.3497 -0.2670 0.5466 0.063 Uiso 1 1 calc R . . C20 C 0.3374(4) -0.021(2) 0.4901(4) 0.051(2) Uani 1 1 d . . . H20A H 0.3833 0.0231 0.5113 0.062 Uiso 1 1 calc R . . C21 C 0.2911(4) 0.0970(13) 0.4363(4) 0.039(2) Uani 1 1 d . . . C22 C 0.3110(4) 0.2772(15) 0.4164(4) 0.043(2) Uani 1 1 d . . . H22A H 0.3563 0.3237 0.4392 0.052 Uiso 1 1 calc R . . C23 C 0.2675(4) 0.3910(15) 0.3647(5) 0.043(2) Uani 1 1 d . . . C24 C 0.2861(4) 0.5798(14) 0.3441(5) 0.043(2) Uani 1 1 d . . . H24A H 0.3307 0.6312 0.3673 0.052 Uiso 1 1 calc R . . C25 C 0.2422(4) 0.6879(14) 0.2924(4) 0.044(2) Uani 1 1 d . . . H25A H 0.2568 0.8099 0.2792 0.053 Uiso 1 1 calc R . . C26 C 0.1742(4) 0.6171(15) 0.2582(4) 0.042(2) Uani 1 1 d . . . H26A H 0.1433 0.6947 0.2231 0.051 Uiso 1 1 calc R . . C27 C 0.1531(4) 0.4380(13) 0.2754(4) 0.038(2) Uani 1 1 d . . . H27A H 0.1080 0.3914 0.2514 0.045 Uiso 1 1 calc R . . C28 C 0.1985(4) 0.3200(13) 0.3294(4) 0.0326(19) Uani 1 1 d . . . C29 C -0.1242(3) 0.2649(13) 0.1767(3) 0.0338(19) Uani 1 1 d . . . H29B H -0.1078 0.2164 0.1426 0.041 Uiso 1 1 calc R . . H29A H -0.1271 0.4136 0.1732 0.041 Uiso 1 1 calc R . . C30 C -0.1968(4) 0.1833(15) 0.1594(4) 0.042(2) Uani 1 1 d . . . C31 C -0.2357(4) 0.2895(15) 0.1969(4) 0.048(2) Uani 1 1 d . . . H31C H -0.2833 0.2445 0.1794 0.057 Uiso 1 1 calc R . . H31B H -0.2340 0.4356 0.1912 0.057 Uiso 1 1 calc R . . H31A H -0.2145 0.2561 0.2440 0.057 Uiso 1 1 calc R . . C32 C -0.1940(4) -0.0499(14) 0.1721(4) 0.046(3) Uani 1 1 d . . . H32A H -0.1746 -0.0758 0.2197 0.055 Uiso 1 1 calc R . . H32B H -0.1655 -0.1139 0.1514 0.055 Uiso 1 1 calc R . . H32C H -0.2403 -0.1057 0.1530 0.055 Uiso 1 1 calc R . . C33 C -0.2347(4) 0.2274(15) 0.0867(4) 0.046(2) Uani 1 1 d . . . H33C H -0.2789 0.1589 0.0710 0.055 Uiso 1 1 calc R . . H33B H -0.2078 0.1788 0.0618 0.055 Uiso 1 1 calc R . . H33A H -0.2417 0.3730 0.0803 0.055 Uiso 1 1 calc R . . Cl1 Cl -0.02017(10) -0.2948(4) 0.20856(11) 0.0456(5) Uani 1 1 d . . . Fe1 Fe -0.02116(5) 0.2969(2) 0.39033(6) 0.0395(3) Uani 1 1 d . . . N1 N 0.0477(3) 0.1396(11) 0.3027(3) 0.0377(17) Uani 1 1 d . . . N2 N -0.0706(3) 0.2127(11) 0.2434(3) 0.0364(16) Uani 1 1 d . . . Rh1 Rh -0.00222(3) 0.01044(15) 0.16102(3) 0.03574(17) Uani 1 1 d . . . O2 O 0.0302(3) 0.3916(10) 0.1078(3) 0.0559(17) Uani 1 1 d . . . O1 O -0.0005(3) -0.2048(10) 0.0377(3) 0.0507(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(4) 0.039(6) 0.024(4) -0.001(4) 0.008(3) -0.004(3) C2 0.029(4) 0.037(5) 0.029(4) -0.002(4) 0.005(3) -0.004(4) C3 0.037(4) 0.061(7) 0.027(4) 0.002(4) 0.010(3) 0.001(4) C4 0.045(5) 0.081(8) 0.036(5) -0.002(6) 0.015(4) 0.010(5) C5 0.048(5) 0.052(7) 0.054(6) -0.021(5) 0.020(5) -0.008(4) C6 0.032(4) 0.054(6) 0.027(4) -0.008(4) 0.004(3) -0.006(4) C7 0.033(4) 0.041(6) 0.040(5) -0.011(4) 0.014(4) -0.003(4) C8 0.047(4) 0.044(6) 0.036(4) -0.001(5) 0.015(3) -0.004(5) C9 0.047(4) 0.070(9) 0.027(4) -0.003(5) 0.010(3) 0.014(5) C10 0.041(5) 0.065(8) 0.033(5) -0.004(5) 0.011(4) -0.006(5) C11 0.042(5) 0.041(6) 0.042(5) 0.007(5) 0.015(4) 0.002(4) C12 0.040(5) 0.038(6) 0.033(5) 0.001(4) 0.006(4) -0.005(4) C13 0.040(5) 0.030(6) 0.045(5) 0.005(5) 0.014(4) 0.002(4) C14 0.022(3) 0.035(6) 0.034(4) -0.006(4) 0.004(3) 0.002(3) C15 0.034(4) 0.035(5) 0.033(5) -0.007(4) 0.008(4) 0.000(4) C16 0.036(4) 0.032(6) 0.045(4) -0.004(5) 0.018(3) 0.000(4) C17 0.034(4) 0.037(6) 0.038(5) 0.005(4) 0.010(4) 0.007(4) C18 0.065(6) 0.050(7) 0.061(6) 0.016(5) 0.040(5) 0.016(5) C19 0.042(5) 0.075(8) 0.040(5) 0.014(6) 0.016(4) 0.020(5) C20 0.034(4) 0.067(7) 0.042(5) -0.001(7) 0.002(3) 0.015(6) C21 0.032(4) 0.053(6) 0.030(5) -0.004(4) 0.009(4) 0.002(4) C22 0.031(4) 0.050(6) 0.048(5) -0.007(5) 0.015(4) -0.004(4) C23 0.033(5) 0.050(7) 0.048(6) -0.002(5) 0.017(4) 0.000(4) C24 0.047(5) 0.045(7) 0.043(6) -0.001(4) 0.023(4) -0.006(4) C25 0.061(6) 0.029(6) 0.060(6) -0.004(5) 0.043(5) -0.002(4) C26 0.043(5) 0.051(7) 0.040(5) 0.007(5) 0.023(4) 0.015(4) C27 0.044(5) 0.037(6) 0.034(5) 0.003(4) 0.017(4) 0.005(4) C28 0.033(4) 0.033(5) 0.034(4) -0.001(4) 0.015(3) -0.001(4) C29 0.026(4) 0.041(6) 0.030(4) 0.000(4) 0.006(3) 0.001(4) C30 0.037(4) 0.059(7) 0.030(5) -0.006(5) 0.012(4) -0.006(4) C31 0.040(5) 0.062(7) 0.035(5) -0.007(5) 0.007(4) 0.003(4) C32 0.030(4) 0.059(9) 0.042(5) -0.015(5) 0.007(3) -0.007(4) C33 0.040(5) 0.053(6) 0.041(5) -0.005(5) 0.013(4) -0.006(4) Cl1 0.0491(12) 0.0418(14) 0.0475(13) -0.0051(12) 0.0200(10) -0.0052(11) Fe1 0.0367(6) 0.0497(9) 0.0308(7) -0.0042(7) 0.0115(5) -0.0002(6) N1 0.030(3) 0.040(5) 0.044(4) -0.012(4) 0.014(3) -0.001(3) N2 0.037(4) 0.039(5) 0.034(4) -0.003(3) 0.015(3) -0.002(3) Rh1 0.0364(3) 0.0380(4) 0.0319(3) -0.0026(5) 0.0120(2) -0.0006(4) O2 0.064(4) 0.058(5) 0.047(4) -0.005(3) 0.024(3) -0.002(3) O1 0.066(4) 0.051(4) 0.038(4) -0.007(3) 0.023(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.348(9) . ? C1 N2 1.380(8) . ? C1 Rh1 2.111(8) . ? C2 C3 1.410(10) . ? C2 C6 1.431(11) . ? C2 N1 1.437(9) . ? C2 Fe1 1.946(7) . ? C3 C4 1.429(11) . ? C3 Fe1 2.007(8) . ? C3 H3A 0.9500 . ? C4 C5 1.418(13) . ? C4 Fe1 2.075(9) . ? C4 H4A 0.9500 . ? C5 C6 1.411(11) . ? C5 Fe1 2.053(8) . ? C5 H5A 0.9500 . ? C6 Fe1 2.023(7) . ? C6 H6A 0.9500 . ? C7 C11 1.432(11) . ? C7 C8 1.436(13) . ? C7 N2 1.435(9) . ? C7 Fe1 1.953(8) . ? C8 C9 1.426(10) . ? C8 Fe1 2.020(9) . ? C8 H8A 0.9500 . ? C9 C10 1.415(14) . ? C9 Fe1 2.054(8) . ? C9 H9A 0.9500 . ? C10 C11 1.404(11) . ? C10 Fe1 2.040(8) . ? C10 H10A 0.9500 . ? C11 Fe1 2.021(8) . ? C11 H11A 0.9500 . ? C12 O1 1.177(10) . ? C12 Rh1 1.891(9) . ? C13 O2 1.167(9) . ? C13 Rh1 1.809(9) . ? C14 N1 1.491(8) . ? C14 C15 1.496(9) . ? C14 H14B 0.9900 . ? C14 H14A 0.9900 . ? C15 C16 1.420(11) . ? C15 C28 1.439(11) . ? C16 C21 1.438(10) . ? C16 C17 1.446(12) . ? C17 C18 1.378(11) . ? C17 H17A 0.9500 . ? C18 C19 1.427(12) . ? C18 H18A 0.9500 . ? C19 C20 1.349(14) . ? C19 H19A 0.9500 . ? C20 C21 1.444(12) . ? C20 H20A 0.9500 . ? C21 C22 1.392(12) . ? C22 C23 1.380(12) . ? C22 H22A 0.9500 . ? C23 C24 1.437(11) . ? C23 C28 1.450(11) . ? C24 C25 1.364(12) . ? C24 H24A 0.9500 . ? C25 C26 1.427(11) . ? C25 H25A 0.9500 . ? C26 C27 1.372(11) . ? C26 H26A 0.9500 . ? C27 C28 1.438(11) . ? C27 H27A 0.9500 . ? C29 N2 1.509(9) . ? C29 C30 1.537(10) . ? C29 H29B 0.9900 . ? C29 H29A 0.9900 . ? C30 C33 1.513(11) . ? C30 C31 1.538(11) . ? C30 C32 1.570(14) . ? C31 H31C 0.9800 . ? C31 H31B 0.9800 . ? C31 H31A 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33C 0.9800 . ? C33 H33B 0.9800 . ? C33 H33A 0.9800 . ? Cl1 Rh1 2.373(3) . ? 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 N1 C1 N2 122.6(7) . . ? N1 C1 Rh1 118.3(5) . . ? N2 C1 Rh1 118.6(5) . . ? C3 C2 C6 108.0(7) . . ? C3 C2 N1 127.4(8) . . ? C6 C2 N1 124.5(7) . . ? C3 C2 Fe1 71.5(4) . . ? C6 C2 Fe1 71.8(4) . . ? N1 C2 Fe1 124.8(5) . . ? C2 C3 C4 108.7(8) . . ? C2 C3 Fe1 66.8(5) . . ? C4 C3 Fe1 72.1(5) . . ? C2 C3 H3A 125.7 . . ? C4 C3 H3A 125.7 . . ? Fe1 C3 H3A 127.0 . . ? C5 C4 C3 106.6(8) . . ? C5 C4 Fe1 69.1(5) . . ? C3 C4 Fe1 67.0(5) . . ? C5 C4 H4A 126.7 . . ? C3 C4 H4A 126.7 . . ? Fe1 C4 H4A 128.7 . . ? C6 C5 C4 109.5(8) . . ? C6 C5 Fe1 68.6(5) . . ? C4 C5 Fe1 70.7(5) . . ? C6 C5 H5A 125.2 . . ? C4 C5 H5A 125.2 . . ? Fe1 C5 H5A 127.0 . . ? C5 C6 C2 107.1(8) . . ? C5 C6 Fe1 70.9(5) . . ? C2 C6 Fe1 66.0(4) . . ? C5 C6 H6A 126.5 . . ? C2 C6 H6A 126.5 . . ? Fe1 C6 H6A 128.1 . . ? C11 C7 C8 108.5(7) . . ? C11 C7 N2 126.6(8) . . ? C8 C7 N2 124.8(8) . . ? C11 C7 Fe1 71.4(5) . . ? C8 C7 Fe1 71.3(4) . . ? N2 C7 Fe1 126.3(5) . . ? C9 C8 C7 106.4(9) . . ? C9 C8 Fe1 70.8(5) . . ? C7 C8 Fe1 66.4(5) . . ? C9 C8 H8A 126.8 . . ? C7 C8 H8A 126.8 . . ? Fe1 C8 H8A 127.5 . . ? C10 C9 C8 108.7(9) . . ? C10 C9 Fe1 69.3(5) . . ? C8 C9 Fe1 68.2(5) . . ? C10 C9 H9A 125.6 . . ? C8 C9 H9A 125.6 . . ? Fe1 C9 H9A 128.5 . . ? C11 C10 C9 108.9(8) . . ? C11 C10 Fe1 69.0(4) . . ? C9 C10 Fe1 70.3(5) . . ? C11 C10 H10A 125.6 . . ? C9 C10 H10A 125.6 . . ? Fe1 C10 H10A 126.7 . . ? C10 C11 C7 107.4(8) . . ? C10 C11 Fe1 70.5(5) . . ? C7 C11 Fe1 66.4(4) . . ? C10 C11 H11A 126.3 . . ? C7 C11 H11A 126.3 . . ? Fe1 C11 H11A 128.3 . . ? O1 C12 Rh1 178.5(8) . . ? O2 C13 Rh1 175.8(7) . . ? N1 C14 C15 116.1(7) . . ? N1 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? N1 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? H14B C14 H14A 107.4 . . ? C16 C15 C28 118.0(7) . . ? C16 C15 C14 121.9(8) . . ? C28 C15 C14 119.9(7) . . ? C15 C16 C21 120.7(8) . . ? C15 C16 C17 122.2(7) . . ? C21 C16 C17 117.0(7) . . ? C18 C17 C16 121.4(8) . . ? C18 C17 H17A 119.3 . . ? C16 C17 H17A 119.3 . . ? C17 C18 C19 120.8(9) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C20 C19 C18 119.3(8) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C19 C20 C21 122.3(8) . . ? C19 C20 H20A 118.8 . . ? C21 C20 H20A 118.8 . . ? C22 C21 C16 119.1(8) . . ? C22 C21 C20 122.0(8) . . ? C16 C21 C20 118.9(9) . . ? C23 C22 C21 122.7(8) . . ? C23 C22 H22A 118.6 . . ? C21 C22 H22A 118.6 . . ? C22 C23 C24 123.9(9) . . ? C22 C23 C28 118.8(8) . . ? C24 C23 C28 117.3(8) . . ? C25 C24 C23 122.5(9) . . ? C25 C24 H24A 118.7 . . ? C23 C24 H24A 118.7 . . ? C24 C25 C26 119.7(9) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C27 C26 C25 120.8(9) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 120.7(8) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C15 C28 C27 120.7(7) . . ? C15 C28 C23 120.3(7) . . ? C27 C28 C23 119.0(8) . . ? N2 C29 C30 118.2(6) . . ? N2 C29 H29B 107.8 . . ? C30 C29 H29B 107.8 . . ? N2 C29 H29A 107.8 . . ? C30 C29 H29A 107.8 . . ? H29B C29 H29A 107.1 . . ? C33 C30 C29 105.8(6) . . ? C33 C30 C31 107.2(7) . . ? C29 C30 C31 113.4(7) . . ? C33 C30 C32 110.2(8) . . ? C29 C30 C32 109.7(7) . . ? C31 C30 C32 110.4(7) . . ? C30 C31 H31C 109.5 . . ? C30 C31 H31B 109.5 . . ? H31C C31 H31B 109.5 . . ? C30 C31 H31A 109.5 . . ? H31C C31 H31A 109.5 . . ? H31B C31 H31A 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33C 109.5 . . ? C30 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? C30 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C2 Fe1 C7 92.1(3) . . ? C2 Fe1 C3 41.7(3) . . ? C7 Fe1 C3 114.0(3) . . ? C2 Fe1 C8 113.9(3) . . ? C7 Fe1 C8 42.3(4) . . ? C3 Fe1 C8 151.9(3) . . ? C2 Fe1 C11 109.9(3) . . ? C7 Fe1 C11 42.2(3) . . ? C3 Fe1 C11 101.9(3) . . ? C8 Fe1 C11 70.3(4) . . ? C2 Fe1 C6 42.2(3) . . ? C7 Fe1 C6 110.1(3) . . ? C3 Fe1 C6 69.5(3) . . ? C8 Fe1 C6 101.6(3) . . ? C11 Fe1 C6 146.7(3) . . ? C2 Fe1 C10 149.3(4) . . ? C7 Fe1 C10 69.8(3) . . ? C3 Fe1 C10 122.8(4) . . ? C8 Fe1 C10 69.3(3) . . ? C11 Fe1 C10 40.4(3) . . ? C6 Fe1 C10 167.1(4) . . ? C2 Fe1 C5 69.7(3) . . ? C7 Fe1 C5 149.7(4) . . ? C3 Fe1 C5 68.4(4) . . ? C8 Fe1 C5 122.7(4) . . ? C11 Fe1 C5 166.5(4) . . ? C6 Fe1 C5 40.5(3) . . ? C10 Fe1 C5 136.4(3) . . ? C2 Fe1 C9 154.8(3) . . ? C7 Fe1 C9 69.7(3) . . ? C3 Fe1 C9 162.1(4) . . ? C8 Fe1 C9 41.0(3) . . ? C11 Fe1 C9 68.5(4) . . ? C6 Fe1 C9 126.8(4) . . ? C10 Fe1 C9 40.4(4) . . ? C5 Fe1 C9 118.0(4) . . ? C2 Fe1 C4 69.9(3) . . ? C7 Fe1 C4 154.7(4) . . ? C3 Fe1 C4 40.9(3) . . ? C8 Fe1 C4 161.7(4) . . ? C11 Fe1 C4 126.4(4) . . ? C6 Fe1 C4 68.6(3) . . ? C10 Fe1 C4 117.3(4) . . ? C5 Fe1 C4 40.2(4) . . ? C9 Fe1 C4 132.5(3) . . ? C1 N1 C2 128.3(6) . . ? C1 N1 C14 118.5(6) . . ? C2 N1 C14 113.0(6) . . ? C1 N2 C7 125.4(6) . . ? C1 N2 C29 118.2(6) . . ? C7 N2 C29 115.6(6) . . ? C13 Rh1 C12 89.2(4) . . ? C13 Rh1 C1 94.1(4) . . ? C12 Rh1 C1 176.4(4) . . ? C13 Rh1 Cl1 177.0(3) . . ? C12 Rh1 Cl1 92.5(3) . . ? C1 Rh1 Cl1 84.3(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.490 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 961495' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_i1144a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Cl Fe N2 O2 Rh' _chemical_formula_sum 'C24 H24 Cl Fe N2 O2 Rh' _chemical_formula_weight 566.66 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' Cl Cl 0.1484 0.1585 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8531(8) _cell_length_b 18.9358(7) _cell_length_c 20.6272(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.753(4) _cell_angle_gamma 90.00 _cell_volume 4854.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16788 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 25.59 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 1.409 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8331 _exptl_absorpt_correction_T_max 0.9472 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 124 frames, detector distance = 135 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 21353 _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.16 _reflns_number_total 8551 _reflns_number_gt 5790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie. 2006)' _computing_cell_refinement 'X-Area (Stoe & Cie. 2006)' _computing_data_reduction 'X-Area (Stoe & Cie. 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 win. (Farrugia 2008)' _computing_publication_material 'PLATON (Spek 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8551 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9270(4) 0.1792(3) 0.7535(2) 0.0326(11) Uani 1 1 d . . . C2 C 0.7475(5) 0.2968(3) 0.6050(3) 0.0472(14) Uani 1 1 d . . . C3 C 0.9578(4) 0.2665(3) 0.6447(3) 0.0459(13) Uani 1 1 d . . . C4 C 0.9615(4) 0.0506(3) 0.7814(2) 0.0342(11) Uani 1 1 d . . . C5 C 1.0656(4) 0.0191(3) 0.8114(2) 0.0359(11) Uani 1 1 d . . . H5A H 1.1329 0.0333 0.8046 0.043 Uiso 1 1 calc R . . C6 C 1.0474(4) -0.0374(3) 0.8528(2) 0.0426(13) Uani 1 1 d . . . H6A H 1.1017 -0.0663 0.8800 0.051 Uiso 1 1 calc R . . C7 C 0.9346(4) -0.0436(3) 0.8471(2) 0.0412(12) Uani 1 1 d . . . H7A H 0.9008 -0.0774 0.8690 0.049 Uiso 1 1 calc R . . C8 C 0.8821(4) 0.0103(3) 0.8024(2) 0.0405(12) Uani 1 1 d . . . H8A H 0.8066 0.0181 0.7889 0.049 Uiso 1 1 calc R . . C9 C 0.9770(4) 0.1620(3) 0.8775(2) 0.0337(11) Uani 1 1 d . . . C10 C 1.0831(4) 0.1413(3) 0.9151(2) 0.0385(12) Uani 1 1 d . . . H10A H 1.1490 0.1536 0.9052 0.046 Uiso 1 1 calc R . . C11 C 1.0708(5) 0.0985(3) 0.9704(2) 0.0424(13) Uani 1 1 d . . . H11A H 1.1272 0.0768 1.0031 0.051 Uiso 1 1 calc R . . C12 C 0.9598(5) 0.0946(3) 0.9673(3) 0.0484(14) Uani 1 1 d . . . H12A H 0.9294 0.0698 0.9981 0.058 Uiso 1 1 calc R . . C13 C 0.9004(4) 0.1337(3) 0.9107(2) 0.0391(12) Uani 1 1 d . . . H13A H 0.8245 0.1398 0.8975 0.047 Uiso 1 1 calc R . . C14 C 0.9261(4) 0.0926(3) 0.6676(2) 0.0375(12) Uani 1 1 d . . . C15 C 0.8294(5) 0.0649(3) 0.6325(3) 0.0485(14) Uani 1 1 d . . . H15A H 0.7721 0.0584 0.6533 0.058 Uiso 1 1 calc R . . C16 C 0.8173(6) 0.0465(4) 0.5651(3) 0.064(2) Uani 1 1 d . . . H16A H 0.7512 0.0271 0.5398 0.076 Uiso 1 1 calc R . . C17 C 0.9004(7) 0.0564(4) 0.5353(3) 0.070(2) Uani 1 1 d . . . H17A H 0.8908 0.0443 0.4895 0.084 Uiso 1 1 calc R . . C18 C 0.9976(7) 0.0839(4) 0.5711(3) 0.0641(19) Uani 1 1 d . . . H18A H 1.0546 0.0902 0.5500 0.077 Uiso 1 1 calc R . . C19 C 1.0120(5) 0.1025(3) 0.6389(3) 0.0464(13) Uani 1 1 d . . . H19A H 1.0784 0.1212 0.6643 0.056 Uiso 1 1 calc R . . C20 C 0.9171(4) 0.2776(3) 0.8281(2) 0.0369(12) Uani 1 1 d . . . H20B H 0.8755 0.2760 0.8623 0.044 Uiso 1 1 calc R . . H20A H 0.8674 0.2940 0.7858 0.044 Uiso 1 1 calc R . . C21 C 1.0049(5) 0.3342(3) 0.8500(3) 0.0439(13) Uani 1 1 d . . . C22 C 1.0722(5) 0.3434(3) 0.7981(3) 0.0539(15) Uani 1 1 d . . . H22A H 1.0260 0.3611 0.7559 0.065 Uiso 1 1 calc R . . H22B H 1.1028 0.2978 0.7903 0.065 Uiso 1 1 calc R . . H22C H 1.1305 0.3772 0.8154 0.065 Uiso 1 1 calc R . . C23 C 1.0818(6) 0.3180(3) 0.9187(3) 0.064(2) Uani 1 1 d . . . H23A H 1.1256 0.2766 0.9149 0.076 Uiso 1 1 calc R . . H23B H 1.0399 0.3083 0.9513 0.076 Uiso 1 1 calc R . . H23C H 1.1288 0.3587 0.9337 0.076 Uiso 1 1 calc R . . C24 C 0.9445(5) 0.4033(3) 0.8536(3) 0.0530(15) Uani 1 1 d . . . H24A H 0.9059 0.3996 0.8887 0.064 Uiso 1 1 calc R . . H24B H 0.8930 0.4120 0.8103 0.064 Uiso 1 1 calc R . . H24C H 0.9960 0.4424 0.8640 0.064 Uiso 1 1 calc R . . C25 C 0.4316(4) 0.1943(3) 0.7550(2) 0.0330(11) Uani 1 1 d . . . C26 C 0.3769(5) 0.0833(4) 0.9086(3) 0.0528(15) Uani 1 1 d . . . C27 C 0.5512(5) 0.1065(3) 0.8631(3) 0.0482(14) Uani 1 1 d . . . C28 C 0.4406(4) 0.3217(3) 0.7227(2) 0.0348(11) Uani 1 1 d . . . C29 C 0.3425(4) 0.3598(3) 0.7013(3) 0.0434(13) Uani 1 1 d . . . H29A H 0.2789 0.3519 0.7158 0.052 Uiso 1 1 calc R . . C30 C 0.3564(5) 0.4123(3) 0.6539(3) 0.0460(14) Uani 1 1 d . . . H30A H 0.3032 0.4447 0.6310 0.055 Uiso 1 1 calc R . . C31 C 0.4638(5) 0.4075(3) 0.6474(2) 0.0427(13) Uani 1 1 d . . . H31A H 0.4944 0.4360 0.6191 0.051 Uiso 1 1 calc R . . C32 C 0.5185(4) 0.3520(3) 0.6909(2) 0.0376(12) Uani 1 1 d . . . H32A H 0.5914 0.3381 0.6974 0.045 Uiso 1 1 calc R . . C33 C 0.3783(4) 0.2075(3) 0.6310(2) 0.0376(12) Uani 1 1 d . . . C34 C 0.4525(5) 0.2248(3) 0.5921(2) 0.0429(13) Uani 1 1 d . . . H34A H 0.5261 0.2113 0.6015 0.051 Uiso 1 1 calc R . . C35 C 0.3958(6) 0.2660(3) 0.5366(3) 0.0594(18) Uani 1 1 d . . . H35A H 0.4260 0.2871 0.5038 0.071 Uiso 1 1 calc R . . C36 C 0.2886(6) 0.2703(3) 0.5385(3) 0.069(2) Uani 1 1 d . . . H36A H 0.2333 0.2934 0.5060 0.082 Uiso 1 1 calc R . . C37 C 0.2743(5) 0.2345(3) 0.5972(3) 0.0579(18) Uani 1 1 d . . . H37A H 0.2094 0.2297 0.6108 0.069 Uiso 1 1 calc R . . C38 C 0.5059(4) 0.2839(3) 0.8376(2) 0.0363(11) Uani 1 1 d . . . C39 C 0.4413(5) 0.3187(3) 0.8724(3) 0.0494(14) Uani 1 1 d . . . H39A H 0.3672 0.3270 0.8525 0.059 Uiso 1 1 calc R . . C40 C 0.4901(6) 0.3410(3) 0.9380(3) 0.0548(16) Uani 1 1 d . . . H40A H 0.4480 0.3648 0.9628 0.066 Uiso 1 1 calc R . . C41 C 0.5974(6) 0.3293(3) 0.9672(3) 0.0590(18) Uani 1 1 d . . . H41A H 0.6283 0.3445 1.0118 0.071 Uiso 1 1 calc R . . C42 C 0.6606(5) 0.2949(3) 0.9313(3) 0.0496(15) Uani 1 1 d . . . H42A H 0.7348 0.2871 0.9515 0.060 Uiso 1 1 calc R . . C43 C 0.6162(5) 0.2720(3) 0.8658(3) 0.0459(14) Uani 1 1 d . . . H43A H 0.6592 0.2489 0.8409 0.055 Uiso 1 1 calc R . . C44 C 0.3543(4) 0.0941(3) 0.6833(3) 0.0414(12) Uani 1 1 d . . . H44A H 0.2808 0.0973 0.6533 0.050 Uiso 1 1 calc R . . H44B H 0.3468 0.0772 0.7273 0.050 Uiso 1 1 calc R . . C45 C 0.4150(4) 0.0372(3) 0.6549(3) 0.0410(12) Uani 1 1 d . . . C46 C 0.5306(5) 0.0282(3) 0.6994(3) 0.0541(15) Uani 1 1 d . . . H46A H 0.5278 0.0146 0.7447 0.065 Uiso 1 1 calc R . . H46B H 0.5697 0.0730 0.7012 0.065 Uiso 1 1 calc R . . H46C H 0.5677 -0.0086 0.6804 0.065 Uiso 1 1 calc R . . C47 C 0.4196(7) 0.0515(3) 0.5828(3) 0.0647(18) Uani 1 1 d . . . H47A H 0.4692 0.0907 0.5821 0.078 Uiso 1 1 calc R . . H47B H 0.3476 0.0639 0.5557 0.078 Uiso 1 1 calc R . . H47C H 0.4449 0.0091 0.5642 0.078 Uiso 1 1 calc R . . C48 C 0.3532(5) -0.0319(3) 0.6575(3) 0.0547(15) Uani 1 1 d . . . H48C H 0.3889 -0.0708 0.6404 0.066 Uiso 1 1 calc R . . H48B H 0.2793 -0.0271 0.6298 0.066 Uiso 1 1 calc R . . H48A H 0.3520 -0.0418 0.7039 0.066 Uiso 1 1 calc R . . N1 N 0.9411(3) 0.1112(2) 0.73865(18) 0.0303(9) Uani 1 1 d . . . N2 N 0.9496(3) 0.2039(2) 0.81704(18) 0.0333(9) Uani 1 1 d . . . N3 N 0.4590(3) 0.2623(2) 0.76813(19) 0.0330(9) Uani 1 1 d . . . N4 N 0.3992(3) 0.1670(2) 0.6928(2) 0.0344(9) Uani 1 1 d . . . O1 O 0.6926(4) 0.3316(3) 0.5651(2) 0.0680(13) Uani 1 1 d . . . O2 O 1.0308(4) 0.2833(2) 0.6249(2) 0.0582(11) Uani 1 1 d . . . O3 O 0.3558(4) 0.0528(3) 0.9518(2) 0.0742(14) Uani 1 1 d . . . O4 O 0.6402(3) 0.0865(2) 0.8797(2) 0.0624(12) Uani 1 1 d . . . Cl1 Cl 0.69401(10) 0.19856(8) 0.71388(7) 0.0459(3) Uani 1 1 d . . . Cl2 Cl 0.23135(11) 0.17616(8) 0.79818(7) 0.0504(3) Uani 1 1 d . . . Fe1 Fe 0.98855(6) 0.05758(4) 0.87912(3) 0.03433(17) Uani 1 1 d . . . Fe2 Fe 0.38713(6) 0.31067(4) 0.62584(4) 0.03993(19) Uani 1 1 d . . . Rh1 Rh 0.83931(3) 0.24097(2) 0.673126(19) 0.03481(11) Uani 1 1 d . . . Rh2 Rh 0.41122(3) 0.13470(2) 0.83758(2) 0.03822(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(2) 0.033(3) 0.036(2) -0.006(2) 0.0126(19) -0.007(2) C2 0.051(3) 0.044(3) 0.047(3) -0.009(3) 0.013(3) -0.008(3) C3 0.043(3) 0.041(3) 0.056(3) 0.002(3) 0.016(3) 0.002(3) C4 0.039(3) 0.033(3) 0.031(2) 0.001(2) 0.009(2) -0.001(2) C5 0.039(3) 0.036(3) 0.032(2) 0.000(2) 0.008(2) -0.001(2) C6 0.049(3) 0.039(3) 0.036(3) 0.002(2) 0.004(2) 0.007(3) C7 0.056(3) 0.036(3) 0.032(2) -0.002(2) 0.011(2) -0.001(3) C8 0.045(3) 0.041(3) 0.032(2) -0.004(2) 0.004(2) -0.007(2) C9 0.037(3) 0.032(3) 0.035(2) -0.003(2) 0.016(2) -0.005(2) C10 0.043(3) 0.040(3) 0.031(2) -0.003(2) 0.004(2) -0.002(2) C11 0.055(3) 0.038(3) 0.031(2) -0.003(2) 0.005(2) -0.005(3) C12 0.069(4) 0.044(3) 0.036(3) -0.003(2) 0.020(3) -0.010(3) C13 0.045(3) 0.038(3) 0.037(3) -0.007(2) 0.016(2) -0.007(2) C14 0.054(3) 0.029(3) 0.028(2) 0.003(2) 0.007(2) 0.010(2) C15 0.056(3) 0.047(4) 0.037(3) -0.008(3) 0.003(2) 0.011(3) C16 0.078(4) 0.062(4) 0.038(3) -0.010(3) -0.010(3) 0.018(4) C17 0.122(6) 0.052(4) 0.031(3) -0.001(3) 0.011(4) 0.026(4) C18 0.111(6) 0.045(4) 0.048(3) 0.006(3) 0.041(4) 0.019(4) C19 0.067(4) 0.037(3) 0.042(3) 0.003(2) 0.027(3) 0.006(3) C20 0.044(3) 0.035(3) 0.033(2) -0.002(2) 0.013(2) 0.005(2) C21 0.058(3) 0.031(3) 0.039(3) -0.004(2) 0.006(2) 0.003(3) C22 0.056(3) 0.044(4) 0.062(4) -0.001(3) 0.016(3) -0.006(3) C23 0.083(4) 0.044(4) 0.046(3) 0.003(3) -0.018(3) -0.011(3) C24 0.064(4) 0.037(3) 0.056(3) -0.011(3) 0.012(3) 0.006(3) C25 0.026(2) 0.034(3) 0.040(3) -0.002(2) 0.0094(19) 0.002(2) C26 0.052(3) 0.051(4) 0.058(4) 0.002(3) 0.020(3) 0.007(3) C27 0.052(3) 0.040(3) 0.051(3) -0.003(3) 0.010(3) -0.010(3) C28 0.035(2) 0.034(3) 0.036(2) -0.006(2) 0.011(2) 0.000(2) C29 0.040(3) 0.035(3) 0.052(3) -0.004(3) 0.006(2) 0.005(2) C30 0.056(3) 0.034(3) 0.045(3) -0.004(2) 0.008(3) 0.005(3) C31 0.058(3) 0.037(3) 0.032(2) 0.000(2) 0.010(2) -0.001(3) C32 0.040(3) 0.036(3) 0.037(3) -0.004(2) 0.009(2) -0.005(2) C33 0.037(3) 0.035(3) 0.038(3) -0.006(2) 0.003(2) 0.002(2) C34 0.058(3) 0.036(3) 0.034(2) -0.006(2) 0.012(2) 0.003(3) C35 0.091(5) 0.039(3) 0.038(3) 0.002(3) -0.002(3) 0.000(3) C36 0.091(5) 0.041(4) 0.049(3) -0.008(3) -0.028(4) 0.011(3) C37 0.044(3) 0.040(3) 0.073(4) -0.010(3) -0.014(3) 0.002(3) C38 0.054(3) 0.026(3) 0.033(2) -0.002(2) 0.020(2) -0.008(2) C39 0.064(4) 0.044(3) 0.046(3) -0.002(3) 0.025(3) -0.002(3) C40 0.086(5) 0.043(3) 0.044(3) -0.006(3) 0.031(3) -0.007(3) C41 0.093(5) 0.051(4) 0.033(3) -0.002(3) 0.016(3) -0.020(4) C42 0.056(3) 0.047(4) 0.040(3) 0.005(3) 0.002(3) -0.013(3) C43 0.055(3) 0.046(3) 0.034(3) 0.005(2) 0.006(2) -0.007(3) C44 0.041(3) 0.035(3) 0.047(3) -0.004(2) 0.010(2) -0.009(2) C45 0.056(3) 0.029(3) 0.042(3) -0.006(2) 0.020(2) -0.007(2) C46 0.051(3) 0.039(3) 0.074(4) -0.007(3) 0.020(3) 0.005(3) C47 0.114(6) 0.035(3) 0.053(3) -0.003(3) 0.036(4) 0.006(4) C48 0.066(4) 0.033(3) 0.066(4) -0.006(3) 0.019(3) -0.009(3) N1 0.036(2) 0.029(2) 0.0274(18) -0.0002(16) 0.0100(16) -0.0013(17) N2 0.035(2) 0.035(2) 0.0290(19) -0.0020(18) 0.0073(16) 0.0007(18) N3 0.034(2) 0.030(2) 0.036(2) -0.0007(18) 0.0117(16) -0.0002(18) N4 0.032(2) 0.031(2) 0.040(2) -0.0008(19) 0.0097(17) 0.0032(17) O1 0.075(3) 0.064(3) 0.054(2) 0.015(2) -0.005(2) 0.013(3) O2 0.065(3) 0.045(3) 0.074(3) 0.003(2) 0.037(2) 0.002(2) O3 0.097(4) 0.066(3) 0.068(3) 0.026(3) 0.038(3) -0.007(3) O4 0.044(2) 0.052(3) 0.084(3) 0.001(2) 0.003(2) -0.002(2) Cl1 0.0350(6) 0.0497(8) 0.0538(7) 0.0038(6) 0.0129(5) -0.0003(6) Cl2 0.0415(7) 0.0510(9) 0.0654(8) 0.0062(7) 0.0257(6) 0.0052(6) Fe1 0.0395(4) 0.0334(4) 0.0301(3) -0.0004(3) 0.0090(3) -0.0023(3) Fe2 0.0465(4) 0.0328(4) 0.0358(4) -0.0018(3) 0.0019(3) 0.0062(3) Rh1 0.0365(2) 0.0340(2) 0.03302(19) 0.00190(17) 0.00716(15) 0.00125(17) Rh2 0.0412(2) 0.0347(2) 0.0419(2) 0.00158(18) 0.01640(17) -0.00122(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.345(6) . ? C1 N2 1.351(6) . ? C1 Rh1 2.107(5) . ? C1 Fe1 3.405(5) . ? C2 O1 1.146(7) . ? C2 Rh1 1.908(6) . ? C3 O2 1.159(7) . ? C3 Rh1 1.831(6) . ? C4 C8 1.428(8) . ? C4 N1 1.431(6) . ? C4 C5 1.452(7) . ? C4 Fe1 1.961(5) . ? C5 C6 1.425(8) . ? C5 Fe1 2.043(5) . ? C5 H5A 0.9500 . ? C6 C7 1.430(8) . ? C6 Fe1 2.076(6) . ? C6 H6A 0.9500 . ? C7 C8 1.423(7) . ? C7 Fe1 2.087(5) . ? C7 H7A 0.9500 . ? C8 Fe1 2.019(5) . ? C8 H8A 0.9500 . ? C9 C13 1.439(7) . ? C9 C10 1.442(7) . ? C9 N2 1.443(6) . ? C9 Fe1 1.983(5) . ? C10 C11 1.439(8) . ? C10 Fe1 2.020(5) . ? C10 H10A 0.9500 . ? C11 C12 1.413(9) . ? C11 Fe1 2.061(5) . ? C11 H11A 0.9500 . ? C12 C13 1.428(8) . ? C12 Fe1 2.068(6) . ? C12 H12A 0.9500 . ? C13 Fe1 2.040(6) . ? C13 H13A 0.9500 . ? C14 C15 1.373(8) . ? C14 C19 1.392(8) . ? C14 N1 1.472(6) . ? C15 C16 1.404(8) . ? C15 H15A 0.9500 . ? C16 C17 1.373(11) . ? C16 H16A 0.9500 . ? C17 C18 1.380(10) . ? C17 H17A 0.9500 . ? C18 C19 1.407(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 N2 1.492(7) . ? C20 C21 1.538(8) . ? C20 H20B 0.9900 . ? C20 H20A 0.9900 . ? C21 C24 1.532(8) . ? C21 C23 1.539(7) . ? C21 C22 1.548(9) . ? 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 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N3 1.344(6) . ? C25 N4 1.348(6) . ? C25 Rh2 2.114(5) . ? C25 Fe2 3.392(5) . ? C26 O3 1.152(7) . ? C26 Rh2 1.901(7) . ? C27 O4 1.170(7) . ? C27 Rh2 1.821(6) . ? C28 C29 1.422(7) . ? C28 N3 1.445(7) . ? C28 C32 1.448(7) . ? C28 Fe2 1.951(5) . ? C29 C30 1.438(8) . ? C29 Fe2 2.018(6) . ? C29 H29A 0.9500 . ? C30 C31 1.424(8) . ? C30 Fe2 2.077(6) . ? C30 H30A 0.9500 . ? C31 C32 1.443(7) . ? C31 Fe2 2.075(6) . ? C31 H31A 0.9500 . ? C32 Fe2 2.027(5) . ? C32 H32A 0.9500 . ? C33 C34 1.434(8) . ? C33 C37 1.434(7) . ? C33 N4 1.453(7) . ? C33 Fe2 1.961(5) . ? C34 C35 1.423(8) . ? C34 Fe2 2.033(6) . ? C34 H34A 0.9500 . ? C35 C36 1.390(11) . ? C35 Fe2 2.054(7) . ? C35 H35A 0.9500 . ? C36 C37 1.441(11) . ? C36 Fe2 2.067(5) . ? C36 H36A 0.9500 . ? C37 Fe2 2.024(6) . ? C37 H37A 0.9500 . ? C38 C39 1.393(8) . ? C38 C43 1.407(8) . ? C38 N3 1.465(6) . ? C39 C40 1.403(8) . ? C39 H39A 0.9500 . ? C40 C41 1.375(9) . ? C40 H40A 0.9500 . ? C41 C42 1.392(10) . ? C41 H41A 0.9500 . ? C42 C43 1.396(7) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 N4 1.490(7) . ? C44 C45 1.532(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C47 1.527(8) . ? C45 C48 1.539(8) . ? C45 C46 1.544(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48C 0.9800 . ? C48 H48B 0.9800 . ? C48 H48A 0.9800 . ? Cl1 Rh1 2.3746(14) . ? Cl2 Rh2 2.3801(14) . ? 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 N1 C1 N2 122.9(4) . . ? N1 C1 Rh1 115.3(3) . . ? N2 C1 Rh1 120.7(4) . . ? N1 C1 Fe1 60.5(2) . . ? N2 C1 Fe1 63.0(3) . . ? Rh1 C1 Fe1 161.6(2) . . ? O1 C2 Rh1 178.4(5) . . ? O2 C3 Rh1 177.9(5) . . ? C8 C4 N1 125.7(4) . . ? C8 C4 C5 107.7(4) . . ? N1 C4 C5 126.6(4) . . ? C8 C4 Fe1 71.2(3) . . ? N1 C4 Fe1 122.4(3) . . ? C5 C4 Fe1 71.8(3) . . ? C6 C5 C4 106.8(5) . . ? C6 C5 Fe1 71.0(3) . . ? C4 C5 Fe1 65.7(3) . . ? C6 C5 H5A 126.6 . . ? C4 C5 H5A 126.6 . . ? Fe1 C5 H5A 128.1 . . ? C5 C6 C7 109.3(5) . . ? C5 C6 Fe1 68.5(3) . . ? C7 C6 Fe1 70.3(3) . . ? C5 C6 H6A 125.4 . . ? C7 C6 H6A 125.4 . . ? Fe1 C6 H6A 127.4 . . ? C8 C7 C6 107.4(5) . . ? C8 C7 Fe1 67.2(3) . . ? C6 C7 Fe1 69.5(3) . . ? C8 C7 H7A 126.3 . . ? C6 C7 H7A 126.3 . . ? Fe1 C7 H7A 128.5 . . ? C7 C8 C4 108.8(5) . . ? C7 C8 Fe1 72.3(3) . . ? C4 C8 Fe1 66.8(3) . . ? C7 C8 H8A 125.6 . . ? C4 C8 H8A 125.6 . . ? Fe1 C8 H8A 126.8 . . ? C13 C9 C10 108.1(4) . . ? C13 C9 N2 124.8(4) . . ? C10 C9 N2 127.1(5) . . ? C13 C9 Fe1 71.2(3) . . ? C10 C9 Fe1 70.3(3) . . ? N2 C9 Fe1 124.3(3) . . ? C11 C10 C9 107.4(5) . . ? C11 C10 Fe1 70.9(3) . . ? C9 C10 Fe1 67.5(3) . . ? C11 C10 H10A 126.3 . . ? C9 C10 H10A 126.3 . . ? Fe1 C10 H10A 126.8 . . ? C12 C11 C10 107.9(5) . . ? C12 C11 Fe1 70.2(3) . . ? C10 C11 Fe1 67.8(3) . . ? C12 C11 H11A 126.1 . . ? C10 C11 H11A 126.1 . . ? Fe1 C11 H11A 127.4 . . ? C11 C12 C13 109.5(5) . . ? C11 C12 Fe1 69.7(3) . . ? C13 C12 Fe1 68.6(3) . . ? C11 C12 H12A 125.3 . . ? C13 C12 H12A 125.3 . . ? Fe1 C12 H12A 128.0 . . ? C12 C13 C9 107.1(5) . . ? C12 C13 Fe1 70.7(3) . . ? C9 C13 Fe1 66.9(3) . . ? C12 C13 H13A 126.5 . . ? C9 C13 H13A 126.5 . . ? Fe1 C13 H13A 127.4 . . ? C15 C14 C19 122.4(5) . . ? C15 C14 N1 119.2(5) . . ? C19 C14 N1 118.4(5) . . ? C14 C15 C16 118.3(6) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? C17 C16 C15 120.4(6) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 120.9(6) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C17 C18 C19 119.8(7) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C14 C19 C18 118.1(6) . . ? C14 C19 H19A 120.9 . . ? C18 C19 H19A 120.9 . . ? N2 C20 C21 119.0(4) . . ? N2 C20 H20B 107.6 . . ? C21 C20 H20B 107.6 . . ? N2 C20 H20A 107.6 . . ? C21 C20 H20A 107.6 . . ? H20B C20 H20A 107.0 . . ? C24 C21 C20 105.4(5) . . ? C24 C21 C23 109.9(5) . . ? C20 C21 C23 112.5(5) . . ? C24 C21 C22 108.5(5) . . ? C20 C21 C22 111.9(4) . . ? C23 C21 C22 108.6(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 N4 124.1(5) . . ? N3 C25 Rh2 115.4(3) . . ? N4 C25 Rh2 119.4(4) . . ? N3 C25 Fe2 61.2(2) . . ? N4 C25 Fe2 63.4(3) . . ? Rh2 C25 Fe2 161.6(2) . . ? O3 C26 Rh2 179.3(6) . . ? O4 C27 Rh2 178.2(5) . . ? C29 C28 N3 125.5(5) . . ? C29 C28 C32 108.7(5) . . ? N3 C28 C32 125.8(4) . . ? C29 C28 Fe2 71.6(3) . . ? N3 C28 Fe2 122.5(3) . . ? C32 C28 Fe2 71.5(3) . . ? C28 C29 C30 107.9(5) . . ? C28 C29 Fe2 66.5(3) . . ? C30 C29 Fe2 71.6(3) . . ? C28 C29 H29A 126.1 . . ? C30 C29 H29A 126.1 . . ? Fe2 C29 H29A 127.3 . . ? C31 C30 C29 108.2(5) . . ? C31 C30 Fe2 69.9(3) . . ? C29 C30 Fe2 67.3(3) . . ? C31 C30 H30A 125.9 . . ? C29 C30 H30A 125.9 . . ? Fe2 C30 H30A 128.5 . . ? C30 C31 C32 108.5(5) . . ? C30 C31 Fe2 70.0(3) . . ? C32 C31 Fe2 67.6(3) . . ? C30 C31 H31A 125.7 . . ? C32 C31 H31A 125.7 . . ? Fe2 C31 H31A 128.2 . . ? C31 C32 C28 106.7(5) . . ? C31 C32 Fe2 71.2(3) . . ? C28 C32 Fe2 65.9(3) . . ? C31 C32 H32A 126.7 . . ? C28 C32 H32A 126.7 . . ? Fe2 C32 H32A 127.7 . . ? C34 C33 C37 108.5(5) . . ? C34 C33 N4 127.7(4) . . ? C37 C33 N4 123.8(5) . . ? C34 C33 Fe2 71.7(3) . . ? C37 C33 Fe2 71.3(3) . . ? N4 C33 Fe2 125.0(3) . . ? C35 C34 C33 107.3(5) . . ? C35 C34 Fe2 70.4(4) . . ? C33 C34 Fe2 66.3(3) . . ? C35 C34 H34A 126.3 . . ? C33 C34 H34A 126.3 . . ? Fe2 C34 H34A 128.4 . . ? C36 C35 C34 108.6(6) . . ? C36 C35 Fe2 70.8(4) . . ? C34 C35 Fe2 68.8(3) . . ? C36 C35 H35A 125.7 . . ? C34 C35 H35A 125.7 . . ? Fe2 C35 H35A 126.2 . . ? C35 C36 C37 109.6(5) . . ? C35 C36 Fe2 69.8(3) . . ? C37 C36 Fe2 67.8(3) . . ? C35 C36 H36A 125.2 . . ? C37 C36 H36A 125.2 . . ? Fe2 C36 H36A 128.9 . . ? C33 C37 C36 105.9(6) . . ? C33 C37 Fe2 66.6(3) . . ? C36 C37 Fe2 71.0(4) . . ? C33 C37 H37A 127.1 . . ? C36 C37 H37A 127.1 . . ? Fe2 C37 H37A 126.9 . . ? C39 C38 C43 122.3(5) . . ? C39 C38 N3 119.0(5) . . ? C43 C38 N3 118.7(5) . . ? C38 C39 C40 117.4(6) . . ? C38 C39 H39A 121.3 . . ? C40 C39 H39A 121.3 . . ? C41 C40 C39 121.7(6) . . ? C41 C40 H40A 119.1 . . ? C39 C40 H40A 119.1 . . ? C40 C41 C42 119.9(5) . . ? C40 C41 H41A 120.1 . . ? C42 C41 H41A 120.1 . . ? C41 C42 C43 120.7(6) . . ? C41 C42 H42A 119.7 . . ? C43 C42 H42A 119.7 . . ? C42 C43 C38 118.0(6) . . ? C42 C43 H43A 121.0 . . ? C38 C43 H43A 121.0 . . ? N4 C44 C45 118.9(5) . . ? N4 C44 H44A 107.6 . . ? C45 C44 H44A 107.6 . . ? N4 C44 H44B 107.6 . . ? C45 C44 H44B 107.6 . . ? H44A C44 H44B 107.0 . . ? C47 C45 C44 113.4(5) . . ? C47 C45 C48 109.4(5) . . ? C44 C45 C48 105.4(5) . . ? C47 C45 C46 109.2(5) . . ? C44 C45 C46 110.9(4) . . ? C48 C45 C46 108.2(5) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48C 109.5 . . ? C45 C48 H48B 109.5 . . ? H48C C48 H48B 109.5 . . ? C45 C48 H48A 109.5 . . ? H48C C48 H48A 109.5 . . ? H48B C48 H48A 109.5 . . ? C1 N1 C4 129.9(4) . . ? C1 N1 C14 117.7(4) . . ? C4 N1 C14 112.3(4) . . ? C1 N2 C9 126.3(4) . . ? C1 N2 C20 118.2(4) . . ? C9 N2 C20 113.5(4) . . ? C25 N3 C28 128.6(4) . . ? C25 N3 C38 119.0(4) . . ? C28 N3 C38 112.1(4) . . ? C25 N4 C33 125.2(4) . . ? C25 N4 C44 119.8(4) . . ? C33 N4 C44 113.2(4) . . ? C4 Fe1 C9 93.3(2) . . ? C4 Fe1 C8 42.0(2) . . ? C9 Fe1 C8 113.3(2) . . ? C4 Fe1 C10 111.3(2) . . ? C9 Fe1 C10 42.2(2) . . ? C8 Fe1 C10 149.4(2) . . ? C4 Fe1 C13 114.1(2) . . ? C9 Fe1 C13 41.9(2) . . ? C8 Fe1 C13 104.1(2) . . ? C10 Fe1 C13 70.1(2) . . ? C4 Fe1 C5 42.48(19) . . ? C9 Fe1 C5 113.1(2) . . ? C8 Fe1 C5 69.8(2) . . ? C10 Fe1 C5 100.4(2) . . ? C13 Fe1 C5 151.2(2) . . ? C4 Fe1 C11 151.6(2) . . ? C9 Fe1 C11 70.1(2) . . ? C8 Fe1 C11 166.0(2) . . ? C10 Fe1 C11 41.3(2) . . ? C13 Fe1 C11 68.9(2) . . ? C5 Fe1 C11 122.3(2) . . ? C4 Fe1 C12 154.4(2) . . ? C9 Fe1 C12 69.3(2) . . ? C8 Fe1 C12 127.0(2) . . ? C10 Fe1 C12 68.7(2) . . ? C13 Fe1 C12 40.7(2) . . ? C5 Fe1 C12 161.7(2) . . ? C11 Fe1 C12 40.0(2) . . ? C4 Fe1 C6 69.7(2) . . ? C9 Fe1 C6 152.9(2) . . ? C8 Fe1 C6 68.3(2) . . ? C10 Fe1 C6 123.4(2) . . ? C13 Fe1 C6 164.7(2) . . ? C5 Fe1 C6 40.5(2) . . ? C11 Fe1 C6 115.4(2) . . ? C12 Fe1 C6 133.0(2) . . ? C4 Fe1 C7 69.8(2) . . ? C9 Fe1 C7 153.20(19) . . ? C8 Fe1 C7 40.5(2) . . ? C10 Fe1 C7 163.2(2) . . ? C13 Fe1 C7 125.6(2) . . ? C5 Fe1 C7 68.6(2) . . ? C11 Fe1 C7 133.4(2) . . ? C12 Fe1 C7 118.1(2) . . ? C6 Fe1 C7 40.2(2) . . ? C4 Fe1 C1 46.95(17) . . ? C9 Fe1 C1 46.44(16) . . ? C8 Fe1 C1 73.97(17) . . ? C10 Fe1 C1 75.57(15) . . ? C13 Fe1 C1 74.04(17) . . ? C5 Fe1 C1 77.29(16) . . ? C11 Fe1 C1 113.97(18) . . ? C12 Fe1 C1 112.38(19) . . ? C6 Fe1 C1 114.60(17) . . ? C7 Fe1 C1 112.67(15) . . ? C28 Fe2 C33 93.5(2) . . ? C28 Fe2 C29 41.9(2) . . ? C33 Fe2 C29 112.7(2) . . ? C28 Fe2 C37 114.5(3) . . ? C33 Fe2 C37 42.1(2) . . ? C29 Fe2 C37 103.3(3) . . ? C28 Fe2 C32 42.6(2) . . ? C33 Fe2 C32 113.5(2) . . ? C29 Fe2 C32 70.4(2) . . ? C37 Fe2 C32 151.9(2) . . ? C28 Fe2 C34 111.6(2) . . ? C33 Fe2 C34 42.0(2) . . ? C29 Fe2 C34 148.9(2) . . ? C37 Fe2 C34 70.0(3) . . ? C32 Fe2 C34 100.8(2) . . ? C28 Fe2 C35 151.2(2) . . ? C33 Fe2 C35 69.9(2) . . ? C29 Fe2 C35 166.4(2) . . ? C37 Fe2 C35 69.1(3) . . ? C32 Fe2 C35 121.7(3) . . ? C34 Fe2 C35 40.7(2) . . ? C28 Fe2 C36 155.5(3) . . ? C33 Fe2 C36 69.4(2) . . ? C29 Fe2 C36 127.7(3) . . ? C37 Fe2 C36 41.2(3) . . ? C32 Fe2 C36 160.3(3) . . ? C34 Fe2 C36 67.7(3) . . ? C35 Fe2 C36 39.4(3) . . ? C28 Fe2 C31 70.2(2) . . ? C33 Fe2 C31 154.1(2) . . ? C29 Fe2 C31 69.0(2) . . ? C37 Fe2 C31 163.4(2) . . ? C32 Fe2 C31 41.2(2) . . ? C34 Fe2 C31 124.3(2) . . ? C35 Fe2 C31 115.1(3) . . ? C36 Fe2 C31 131.7(2) . . ? C28 Fe2 C30 70.0(2) . . ? C33 Fe2 C30 152.9(2) . . ? C29 Fe2 C30 41.1(2) . . ? C37 Fe2 C30 124.7(3) . . ? C32 Fe2 C30 69.1(2) . . ? C34 Fe2 C30 164.0(3) . . ? C35 Fe2 C30 133.6(2) . . ? C36 Fe2 C30 117.9(2) . . ? C31 Fe2 C30 40.1(2) . . ? C28 Fe2 C25 47.19(18) . . ? C33 Fe2 C25 46.45(16) . . ? C29 Fe2 C25 73.57(18) . . ? C37 Fe2 C25 74.4(2) . . ? C32 Fe2 C25 77.62(17) . . ? C34 Fe2 C25 75.43(17) . . ? C35 Fe2 C25 113.57(19) . . ? C36 Fe2 C25 112.8(2) . . ? C31 Fe2 C25 115.45(16) . . ? C30 Fe2 C25 112.87(18) . . ? C3 Rh1 C2 91.5(3) . . ? C3 Rh1 C1 94.4(2) . . ? C2 Rh1 C1 173.8(2) . . ? C3 Rh1 Cl1 174.91(18) . . ? C2 Rh1 Cl1 93.08(19) . . ? C1 Rh1 Cl1 81.06(14) . . ? C27 Rh2 C26 91.9(3) . . ? C27 Rh2 C25 94.3(2) . . ? C26 Rh2 C25 173.8(2) . . ? C27 Rh2 Cl2 176.1(2) . . ? C26 Rh2 Cl2 92.08(18) . . ? C25 Rh2 Cl2 81.80(13) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.936 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.101 _database_code_depnum_ccdc_archive 'CCDC 976855' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_i1254-sr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Cl Fe N2 Rh' _chemical_formula_weight 676.94 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' Cl Cl 0.1484 0.1585 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7145(17) _cell_length_b 12.8372(17) _cell_length_c 21.686(3) _cell_angle_alpha 81.088(10) _cell_angle_beta 82.726(11) _cell_angle_gamma 76.040(11) _cell_volume 3113.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 11836 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 24.89 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8364 _exptl_absorpt_correction_T_max 0.9424 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 196 frames, detector distance = 138 mm ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 21217 _diffrn_reflns_av_R_equivalents 0.1310 _diffrn_reflns_av_unetI/netI 0.1384 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 24.91 _reflns_number_total 10545 _reflns_number_gt 5186 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie. 2006)' _computing_cell_refinement 'X-Area (Stoe & Cie. 2006)' _computing_data_reduction 'X-Area (Stoe & Cie. 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 win. (Farrugia 2008)' _computing_publication_material 'PLATON (Spek 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1701P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10545 _refine_ls_number_parameters 899 _refine_ls_number_restraints 907 _refine_ls_R_factor_all 0.1486 _refine_ls_R_factor_gt 0.0989 _refine_ls_wR_factor_ref 0.2738 _refine_ls_wR_factor_gt 0.2454 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2736(9) 0.8647(8) 0.2296(5) 0.072(3) Uani 1 1 d U . . C2 C 0.0638(10) 0.9208(9) 0.2043(5) 0.077(3) Uani 1 1 d U . . C3 C 0.0116(10) 0.8412(10) 0.1871(5) 0.084(3) Uani 1 1 d U . . H3A H 0.0321 0.7671 0.1998 0.100 Uiso 1 1 calc R . . C4 C -0.0773(13) 0.8955(15) 0.1471(6) 0.109(4) Uani 1 1 d U . . H4A H -0.1247 0.8626 0.1288 0.131 Uiso 1 1 calc R . . C5 C -0.0819(11) 1.0053(14) 0.1400(6) 0.108(4) Uani 1 1 d U . . H5A H -0.1338 1.0570 0.1157 0.129 Uiso 1 1 calc R . . C6 C 0.0046(11) 1.0304(10) 0.1751(6) 0.094(4) Uani 1 1 d U . . H6A H 0.0190 1.0974 0.1783 0.113 Uiso 1 1 calc R . . C7 C 0.2617(11) 0.8892(9) 0.1121(5) 0.082(3) Uani 1 1 d U . . C8 C 0.2238(11) 0.8119(11) 0.0823(6) 0.090(3) Uani 1 1 d U . . H8A H 0.2353 0.7380 0.0956 0.108 Uiso 1 1 calc R . . C9 C 0.1672(13) 0.8673(12) 0.0302(6) 0.103(4) Uani 1 1 d U . . H9A H 0.1350 0.8367 0.0023 0.124 Uiso 1 1 calc R . . C10 C 0.1669(12) 0.9780(13) 0.0269(5) 0.102(4) Uani 1 1 d U . . H10A H 0.1342 1.0327 -0.0035 0.123 Uiso 1 1 calc R . . C11 C 0.2249(12) 0.9920(10) 0.0778(5) 0.086(3) Uani 1 1 d U . . H11A H 0.2364 1.0571 0.0868 0.104 Uiso 1 1 calc R . . C12 C 0.1184(10) 0.8983(10) 0.3115(5) 0.077(3) Uani 1 1 d U . . H12A H 0.1918 0.8715 0.3318 0.092 Uiso 1 1 calc R . . C13 C 0.0659(12) 1.0158(10) 0.3326(6) 0.091(3) Uani 1 1 d U . . H13A H 0.1113 1.0673 0.3102 0.109 Uiso 1 1 calc R . . C14 C 0.0809(13) 0.9987(11) 0.4039(5) 0.096(4) Uani 1 1 d U . . H14B H 0.0506 1.0666 0.4211 0.115 Uiso 1 1 calc R . . H14A H 0.1640 0.9741 0.4106 0.115 Uiso 1 1 calc R . . C15 C 0.0112(17) 0.9118(14) 0.4380(7) 0.122(5) Uani 1 1 d U . . H15A H 0.0225 0.8999 0.4828 0.147 Uiso 1 1 calc R . . C16 C 0.0542(16) 0.8088(14) 0.4123(6) 0.119(5) Uani 1 1 d U . . H16B H 0.0073 0.7579 0.4324 0.143 Uiso 1 1 calc R . . H16A H 0.1355 0.7786 0.4211 0.143 Uiso 1 1 calc R . . C17 C 0.0461(13) 0.8250(13) 0.3388(6) 0.102(4) Uani 1 1 d U . . H17A H 0.0736 0.7557 0.3220 0.122 Uiso 1 1 calc R . . C18 C -0.0637(14) 1.0581(12) 0.3248(7) 0.110(4) Uani 1 1 d U . . H18B H -0.0756 1.0729 0.2806 0.133 Uiso 1 1 calc R . . H18A H -0.0919 1.1253 0.3428 0.133 Uiso 1 1 calc R . . C19 C -0.1342(15) 0.9758(14) 0.3571(7) 0.115(4) Uani 1 1 d U . . H19A H -0.2178 1.0053 0.3509 0.138 Uiso 1 1 calc R . . C20 C -0.0962(14) 0.8721(16) 0.3328(7) 0.127(5) Uani 1 1 d U . . H20A H -0.1121 0.8811 0.2892 0.153 Uiso 1 1 calc R . . H20B H -0.1398 0.8212 0.3563 0.153 Uiso 1 1 calc R . . C21 C -0.1193(15) 0.9590(14) 0.4300(6) 0.117(5) Uani 1 1 d U . . H21A H -0.1452 1.0276 0.4466 0.141 Uiso 1 1 calc R . . H21B H -0.1664 0.9099 0.4521 0.141 Uiso 1 1 calc R . . C22 C 0.4479(9) 0.7909(12) 0.1560(5) 0.088(3) Uani 1 1 d U . . H22A H 0.4403 0.7202 0.1489 0.106 Uiso 1 1 calc R . . H22B H 0.4856 0.7805 0.1945 0.106 Uiso 1 1 calc R . . C23 C 0.5358(13) 0.8306(13) 0.1010(7) 0.106(4) Uani 1 1 d U . . C24 C 0.5175(17) 0.8127(17) 0.0384(7) 0.153(7) Uani 1 1 d U . . H24A H 0.4458 0.8607 0.0254 0.183 Uiso 1 1 calc R . . H24B H 0.5119 0.7391 0.0393 0.183 Uiso 1 1 calc R . . H24C H 0.5829 0.8264 0.0094 0.183 Uiso 1 1 calc R . . C25 C 0.5376(15) 0.9395(12) 0.1051(9) 0.132(6) Uani 1 1 d U . . H25A H 0.6178 0.9453 0.1052 0.158 Uiso 1 1 calc R . . H25B H 0.4930 0.9611 0.1431 0.158 Uiso 1 1 calc R . . H25C H 0.5033 0.9856 0.0698 0.158 Uiso 1 1 calc R . . C26 C 0.6593(14) 0.7531(16) 0.1173(10) 0.155(7) Uani 1 1 d U . . H26C H 0.7137 0.7505 0.0803 0.186 Uiso 1 1 calc R . . H26B H 0.6483 0.6817 0.1328 0.186 Uiso 1 1 calc R . . H26A H 0.6903 0.7806 0.1488 0.186 Uiso 1 1 calc R . . C27 C 0.4475(14) 0.7241(9) 0.3912(6) 0.096(4) Uani 1 1 d U . . H27A H 0.3956 0.6786 0.3939 0.115 Uiso 1 1 calc R . . C28 C 0.5415(13) 0.7066(11) 0.3466(7) 0.096(4) Uani 1 1 d U . . H28A H 0.5467 0.6533 0.3211 0.115 Uiso 1 1 calc R . . C29 C 0.6374(14) 0.7697(13) 0.3369(8) 0.118(5) Uani 1 1 d U . . H29A H 0.7122 0.7220 0.3251 0.142 Uiso 1 1 calc R . . H29B H 0.6441 0.7938 0.3762 0.142 Uiso 1 1 calc R . . C30 C 0.6146(12) 0.8694(14) 0.2860(8) 0.115(4) Uani 1 1 d U . . H30A H 0.6531 0.9233 0.2954 0.138 Uiso 1 1 calc R . . H30B H 0.6500 0.8476 0.2457 0.138 Uiso 1 1 calc R . . C31 C 0.4833(12) 0.9205(10) 0.2812(7) 0.095(4) Uani 1 1 d U . . H31A H 0.4587 0.9407 0.2411 0.113 Uiso 1 1 calc R . . C32 C 0.3963(14) 0.9398(9) 0.3314(6) 0.093(4) Uani 1 1 d U . . H32A H 0.3180 0.9664 0.3228 0.112 Uiso 1 1 calc R . . C33 C 0.4254(16) 0.9187(13) 0.4009(6) 0.117(5) Uani 1 1 d U . . H33A H 0.5051 0.9275 0.4019 0.141 Uiso 1 1 calc R . . H33B H 0.3723 0.9738 0.4233 0.141 Uiso 1 1 calc R . . C34 C 0.4165(15) 0.8068(12) 0.4364(6) 0.114(5) Uani 1 1 d U . . H34A H 0.4702 0.7865 0.4690 0.137 Uiso 1 1 calc R . . H34B H 0.3368 0.8098 0.4560 0.137 Uiso 1 1 calc R . . C35 C 0.2810(11) 1.3568(8) 0.2614(5) 0.075(3) Uani 1 1 d U A . C36 C 0.4722(10) 1.2980(9) 0.3115(5) 0.075(3) Uani 1 1 d U A . C37 C 0.5194(10) 1.3672(10) 0.3423(5) 0.080(3) Uani 1 1 d U A . H37A H 0.5121 1.4415 0.3325 0.096 Uiso 1 1 calc R . . C38 C 0.5803(11) 1.2963(11) 0.3914(5) 0.087(3) Uani 1 1 d U A . H38A H 0.6192 1.3183 0.4201 0.104 Uiso 1 1 calc R . . C39 C 0.5733(11) 1.1893(10) 0.3901(5) 0.083(3) Uani 1 1 d U A . H39A H 0.6052 1.1286 0.4173 0.099 Uiso 1 1 calc R . . C40 C 0.5081(11) 1.1925(10) 0.3393(5) 0.087(3) Uani 1 1 d U A . H40A H 0.4915 1.1324 0.3263 0.104 Uiso 1 1 calc R . . C41 C 0.2444(10) 1.3401(8) 0.3789(5) 0.074(3) Uani 1 1 d U A . C42 C 0.2712(11) 1.4164(10) 0.4142(5) 0.083(3) Uani 1 1 d U A . H42A H 0.2690 1.4894 0.4015 0.100 Uiso 1 1 calc R . . C43 C 0.3023(12) 1.3539(13) 0.4736(5) 0.097(4) Uani 1 1 d U A . H43A H 0.3262 1.3799 0.5064 0.117 Uiso 1 1 calc R . . C44 C 0.2905(12) 1.2473(14) 0.4737(5) 0.102(4) Uani 1 1 d U A . H44A H 0.3046 1.1918 0.5068 0.122 Uiso 1 1 calc R . . C45 C 0.2541(10) 1.2375(10) 0.4161(5) 0.079(3) Uani 1 1 d U A . H45A H 0.2393 1.1756 0.4044 0.095 Uiso 1 1 calc R . . C46 C 0.465(3) 1.340(3) 0.1954(15) 0.083(7) Uani 0.50 1 d PU A 2 H46A H 0.4031 1.3513 0.1669 0.100 Uiso 0.50 1 calc PR A 2 C47 C 0.540(2) 1.228(2) 0.1869(9) 0.080(5) Uani 0.50 1 d PU A 2 H47A H 0.4986 1.1718 0.2067 0.097 Uiso 0.50 1 calc PR A 2 C48 C 0.657(3) 1.210(3) 0.2098(17) 0.098(8) Uani 0.50 1 d PU A 2 H48A H 0.7036 1.1407 0.1997 0.117 Uiso 0.50 1 calc PR A 2 H48B H 0.6469 1.2070 0.2551 0.117 Uiso 0.50 1 calc PR A 2 C49 C 0.726(3) 1.299(3) 0.1823(12) 0.097(7) Uani 0.50 1 d PU A 2 H49A H 0.8033 1.2838 0.1988 0.117 Uiso 0.50 1 calc PR A 2 C50 C 0.647(2) 1.402(3) 0.2018(11) 0.089(6) Uani 0.50 1 d PU A 2 H50A H 0.6831 1.4620 0.1848 0.107 Uiso 0.50 1 calc PR A 2 H50B H 0.6399 1.3971 0.2471 0.107 Uiso 0.50 1 calc PR A 2 C51 C 0.514(3) 1.426(3) 0.1779(12) 0.078(6) Uani 0.50 1 d PU A 2 H51A H 0.4629 1.4926 0.1916 0.094 Uiso 0.50 1 calc PR A 2 C52 C 0.553(3) 1.233(3) 0.1139(11) 0.091(7) Uani 0.50 1 d PU A 2 H52A H 0.5981 1.1637 0.1021 0.110 Uiso 0.50 1 calc PR A 2 H52B H 0.4760 1.2476 0.0986 0.110 Uiso 0.50 1 calc PR A 2 C53 C 0.618(3) 1.323(3) 0.0841(11) 0.083(7) Uani 0.50 1 d PU A 2 H53A H 0.6281 1.3256 0.0384 0.099 Uiso 0.50 1 calc PR A 2 C54 C 0.543(2) 1.437(2) 0.1035(9) 0.085(6) Uani 0.50 1 d PU A 2 H54A H 0.5874 1.4922 0.0898 0.102 Uiso 0.50 1 calc PR A 2 H54B H 0.4697 1.4581 0.0834 0.102 Uiso 0.50 1 calc PR A 2 C55 C 0.739(2) 1.305(3) 0.1103(10) 0.095(7) Uani 0.50 1 d PU A 2 H55B H 0.7893 1.2383 0.0982 0.114 Uiso 0.50 1 calc PR A 2 H55A H 0.7757 1.3640 0.0922 0.114 Uiso 0.50 1 calc PR A 2 C56 C 0.070(2) 1.355(2) 0.3171(13) 0.064(6) Uani 0.50 1 d PU B 3 H56B H 0.0668 1.2804 0.3309 0.077 Uiso 0.50 1 calc PR B 3 H56A H 0.0480 1.3723 0.2744 0.077 Uiso 0.50 1 calc PR B 3 C57 C -0.0308(18) 1.4315(18) 0.3611(10) 0.073(5) Uani 0.50 1 d PU B 3 C58 C -0.019(2) 1.550(3) 0.3483(15) 0.085(7) Uani 0.50 1 d PU B 3 H58A H -0.0209 1.5747 0.3042 0.102 Uiso 0.50 1 calc PR B 3 H58B H 0.0553 1.5544 0.3612 0.102 Uiso 0.50 1 calc PR B 3 H58C H -0.0823 1.5942 0.3713 0.102 Uiso 0.50 1 calc PR B 3 C59 C -0.034(3) 1.383(3) 0.4300(14) 0.092(8) Uani 0.50 1 d PU B 3 H59A H 0.0341 1.3917 0.4476 0.111 Uiso 0.50 1 calc PR B 3 H59B H -0.0332 1.3075 0.4334 0.111 Uiso 0.50 1 calc PR B 3 H59C H -0.1044 1.4197 0.4525 0.111 Uiso 0.50 1 calc PR B 3 C60 C -0.148(3) 1.427(3) 0.3382(15) 0.089(8) Uani 0.50 1 d PU B 3 H60C H -0.2102 1.4811 0.3551 0.106 Uiso 0.50 1 calc PR B 3 H60B H -0.1635 1.3567 0.3519 0.106 Uiso 0.50 1 calc PR B 3 H60A H -0.1420 1.4402 0.2933 0.106 Uiso 0.50 1 calc PR B 3 C71 C 0.095(2) 1.4068(19) 0.3052(12) 0.063(5) Uani 0.50 1 d PU B 4 H71A H 0.0922 1.4147 0.2597 0.076 Uiso 0.50 1 calc PR B 4 C72 C 0.039(2) 1.5235(19) 0.3255(14) 0.072(5) Uani 0.50 1 d PU B 4 H72A H 0.0903 1.5738 0.3109 0.086 Uiso 0.50 1 calc PR B 4 C73 C -0.077(2) 1.556(2) 0.2923(13) 0.099(7) Uani 0.50 1 d PU B 4 H73A H -0.1171 1.6290 0.2997 0.119 Uiso 0.50 1 calc PR B 4 H73B H -0.0564 1.5566 0.2475 0.119 Uiso 0.50 1 calc PR B 4 C74 C -0.159(3) 1.482(3) 0.3141(14) 0.083(7) Uani 0.50 1 d PU B 4 H74A H -0.2300 1.5074 0.2912 0.100 Uiso 0.50 1 calc PR B 4 C75 C -0.103(2) 1.368(2) 0.3015(14) 0.090(6) Uani 0.50 1 d PU B 4 H75A H -0.0867 1.3655 0.2567 0.108 Uiso 0.50 1 calc PR B 4 H75B H -0.1549 1.3203 0.3184 0.108 Uiso 0.50 1 calc PR B 4 C76 C 0.014(2) 1.332(2) 0.3331(13) 0.079(6) Uani 0.50 1 d PU B 4 H76A H 0.0524 1.2580 0.3247 0.094 Uiso 0.50 1 calc PR B 4 C77 C -0.022(3) 1.331(3) 0.4071(14) 0.096(7) Uani 0.50 1 d PU B 4 H77A H -0.0741 1.2820 0.4214 0.115 Uiso 0.50 1 calc PR B 4 H77B H 0.0485 1.3053 0.4295 0.115 Uiso 0.50 1 calc PR B 4 C78 C -0.084(3) 1.446(3) 0.4205(12) 0.091(6) Uani 0.50 1 d PU B 4 H78A H -0.1026 1.4465 0.4657 0.109 Uiso 0.50 1 calc PR B 4 C79 C -0.198(2) 1.484(3) 0.3868(12) 0.102(7) Uani 0.50 1 d PU B 4 H79A H -0.2376 1.5572 0.3948 0.122 Uiso 0.50 1 calc PR B 4 H79B H -0.2516 1.4368 0.4016 0.122 Uiso 0.50 1 calc PR B 4 C80 C 0.002(2) 1.520(2) 0.3954(13) 0.085(6) Uani 0.50 1 d PU B 4 H80B H -0.0344 1.5928 0.4045 0.103 Uiso 0.50 1 calc PR B 4 H80A H 0.0729 1.4951 0.4176 0.103 Uiso 0.50 1 calc PR B 4 N1 N 0.1563(8) 0.9004(6) 0.2441(3) 0.065(2) Uani 1 1 d U . . N2 N 0.3247(8) 0.8591(7) 0.1675(4) 0.072(2) Uani 1 1 d U . . N3 N 0.2078(8) 1.3648(6) 0.3156(4) 0.069(2) Uani 1 1 d U . . N4 N 0.3996(9) 1.3313(8) 0.2595(3) 0.079(2) Uani 1 1 d DU . . Cl1 Cl 0.3289(3) 0.6319(2) 0.28758(13) 0.0819(7) Uani 1 1 d . . . Cl2 Cl 0.2277(3) 1.1751(2) 0.20368(14) 0.0908(9) Uani 1 1 d . A . Fe1 Fe 0.08742(15) 0.92522(14) 0.11306(7) 0.0827(5) Uani 1 1 d . . . Fe2 Fe 0.40684(15) 1.28832(13) 0.39998(6) 0.0761(5) Uani 1 1 d . . . Rh1 Rh 0.38347(8) 0.79499(7) 0.30044(4) 0.0742(3) Uani 1 1 d . . . Rh2 Rh 0.20288(9) 1.36620(7) 0.17717(4) 0.0793(3) Uani 1 1 d . . . C81 C 0.201(2) 1.356(2) 0.0740(11) 0.068(6) Uiso 0.50 1 d PU A 2 H81A H 0.2490 1.2863 0.0777 0.081 Uiso 0.50 1 calc PR A 2 C82 C 0.063(3) 1.366(3) 0.1185(15) 0.083(7) Uiso 0.50 1 d PU A 2 H82A H 0.0309 1.3142 0.1452 0.099 Uiso 0.50 1 calc PR A 2 C83 C 0.009(3) 1.493(3) 0.0985(12) 0.085(7) Uani 0.50 1 d PU A 2 H83B H 0.0177 1.5046 0.0530 0.101 Uiso 0.50 1 calc PR A 2 H83A H -0.0752 1.5051 0.1110 0.101 Uiso 0.50 1 calc PR A 2 C84 C 0.049(3) 1.576(2) 0.1191(14) 0.101(7) Uani 0.50 1 d PU A 2 H84B H -0.0155 1.6151 0.1453 0.121 Uiso 0.50 1 calc PR A 2 H84A H 0.0645 1.6264 0.0825 0.121 Uiso 0.50 1 calc PR A 2 C85 C 0.161(4) 1.545(3) 0.1565(19) 0.086(9) Uani 0.50 1 d PU A 2 H85A H 0.1503 1.5543 0.1986 0.103 Uiso 0.50 1 calc PR A 2 C86 C 0.276(3) 1.505(2) 0.1317(12) 0.075(7) Uani 0.50 1 d PU A 2 H86A H 0.3330 1.4816 0.1599 0.090 Uiso 0.50 1 calc PR A 2 C87 C 0.317(3) 1.494(2) 0.0631(11) 0.100(7) Uani 0.50 1 d PU A 2 H87A H 0.3090 1.5660 0.0401 0.121 Uiso 0.50 1 calc PR A 2 H87B H 0.4004 1.4590 0.0601 0.121 Uiso 0.50 1 calc PR A 2 C88 C 0.256(3) 1.435(3) 0.0329(16) 0.084(7) Uani 0.50 1 d PU A 2 H88A H 0.1953 1.4859 0.0105 0.100 Uiso 0.50 1 calc PR A 2 H88B H 0.3117 1.3971 0.0021 0.100 Uiso 0.50 1 calc PR A 2 C100 C 0.153(3) 1.359(2) 0.0845(11) 0.068(6) Uiso 0.50 1 d PU A 1 H100 H 0.1873 1.2857 0.0930 0.082 Uiso 0.50 1 calc PR A 1 C101 C 0.072(3) 1.396(3) 0.1048(16) 0.091(8) Uiso 0.50 1 d PDU A 1 H101 H 0.0499 1.3380 0.1310 0.109 Uiso 0.50 1 calc PR A 1 C102 C -0.034(2) 1.491(3) 0.1168(16) 0.082(7) Uani 0.50 1 d PDU A 1 H102 H -0.0513 1.5342 0.0769 0.099 Uiso 0.50 1 calc PR A 1 H103 H -0.1019 1.4616 0.1332 0.099 Uiso 0.50 1 calc PR A 1 C103 C -0.019(2) 1.558(3) 0.1572(14) 0.103(7) Uani 0.50 1 d PU A 1 H104 H -0.0749 1.5533 0.1940 0.124 Uiso 0.50 1 calc PR A 1 H105 H -0.0364 1.6324 0.1369 0.124 Uiso 0.50 1 calc PR A 1 C104 C 0.108(3) 1.530(3) 0.1782(14) 0.084(7) Uani 0.50 1 d PU A 1 H106 H 0.1147 1.5167 0.2211 0.101 Uiso 0.50 1 calc PR A 1 C105 C 0.211(3) 1.523(3) 0.1400(16) 0.077(8) Uani 0.50 1 d PU A 1 H107 H 0.2804 1.5108 0.1589 0.092 Uiso 0.50 1 calc PR A 1 C106 C 0.220(2) 1.535(2) 0.0675(9) 0.084(6) Uani 0.50 1 d PU A 1 H108 H 0.1573 1.5949 0.0528 0.100 Uiso 0.50 1 calc PR A 1 H109 H 0.2945 1.5526 0.0512 0.100 Uiso 0.50 1 calc PR A 1 C107 C 0.211(3) 1.435(4) 0.041(2) 0.096(9) Uani 0.50 1 d PU A 1 H110 H 0.1667 1.4584 0.0042 0.115 Uiso 0.50 1 calc PR A 1 H111 H 0.2895 1.3973 0.0271 0.115 Uiso 0.50 1 calc PR A 1 C90A C 0.470(3) 1.288(3) 0.2002(13) 0.086(7) Uani 0.50 1 d PDU A 1 H90A H 0.4195 1.3144 0.1664 0.103 Uiso 0.50 1 calc PR A 1 H90B H 0.4806 1.2101 0.2072 0.103 Uiso 0.50 1 calc PR A 1 C91A C 0.602(2) 1.313(3) 0.1729(12) 0.097(6) Uani 0.50 1 d PU A 1 C92A C 0.705(3) 1.246(3) 0.213(2) 0.107(11) Uani 0.50 1 d PU A 1 H92A H 0.7139 1.1699 0.2114 0.129 Uiso 0.50 1 calc PR A 1 H92B H 0.6873 1.2602 0.2556 0.129 Uiso 0.50 1 calc PR A 1 H92C H 0.7779 1.2662 0.1962 0.129 Uiso 0.50 1 calc PR A 1 C93A C 0.586(4) 1.428(3) 0.1749(18) 0.126(12) Uani 0.50 1 d PU A 1 H93A H 0.5235 1.4509 0.2067 0.151 Uiso 0.50 1 calc PR A 1 H93B H 0.5644 1.4674 0.1349 0.151 Uiso 0.50 1 calc PR A 1 H93C H 0.6575 1.4433 0.1842 0.151 Uiso 0.50 1 calc PR A 1 C94A C 0.625(4) 1.276(4) 0.1081(14) 0.121(13) Uani 0.50 1 d PU A 1 H94A H 0.5578 1.3087 0.0848 0.145 Uiso 0.50 1 calc PR A 1 H94B H 0.6360 1.1983 0.1125 0.145 Uiso 0.50 1 calc PR A 1 H94C H 0.6939 1.2964 0.0863 0.145 Uiso 0.50 1 calc PR A 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.066(6) 0.059(6) 0.094(7) -0.008(5) -0.029(5) -0.012(5) C2 0.087(7) 0.068(6) 0.077(6) -0.008(5) -0.033(5) -0.011(5) C3 0.098(8) 0.082(7) 0.085(7) -0.028(6) -0.019(6) -0.033(6) C4 0.106(9) 0.146(12) 0.092(8) -0.036(8) -0.034(7) -0.036(9) C5 0.087(8) 0.134(11) 0.095(8) -0.019(8) -0.049(7) 0.010(8) C6 0.100(8) 0.083(8) 0.090(7) -0.017(6) -0.032(6) 0.014(6) C7 0.089(7) 0.078(7) 0.076(6) -0.008(5) -0.028(6) -0.005(6) C8 0.096(8) 0.087(8) 0.095(8) -0.034(6) -0.029(6) -0.014(6) C9 0.124(10) 0.109(10) 0.076(7) -0.030(7) -0.034(7) -0.001(8) C10 0.116(9) 0.118(10) 0.061(6) 0.003(7) -0.033(6) -0.001(8) C11 0.120(9) 0.077(7) 0.067(6) -0.007(5) -0.020(6) -0.028(7) C12 0.074(6) 0.086(7) 0.063(6) -0.029(5) -0.006(5) 0.008(6) C13 0.114(9) 0.080(7) 0.081(7) -0.008(6) -0.006(6) -0.029(7) C14 0.123(10) 0.096(9) 0.075(7) -0.023(6) 0.005(7) -0.036(8) C15 0.161(13) 0.127(11) 0.072(7) -0.019(8) 0.023(8) -0.033(10) C16 0.154(12) 0.136(12) 0.083(8) -0.014(8) -0.015(8) -0.062(10) C17 0.125(10) 0.121(10) 0.066(6) -0.024(7) -0.009(7) -0.033(8) C18 0.137(11) 0.091(9) 0.095(9) -0.028(7) 0.002(8) -0.005(8) C19 0.109(10) 0.123(11) 0.116(10) -0.030(9) 0.001(8) -0.028(9) C20 0.124(11) 0.180(15) 0.104(9) -0.039(10) 0.006(8) -0.081(11) C21 0.145(12) 0.129(11) 0.090(8) -0.040(8) 0.029(8) -0.061(10) C22 0.064(6) 0.134(10) 0.063(6) 0.026(6) -0.013(5) -0.038(7) C23 0.104(9) 0.118(10) 0.112(9) -0.053(8) -0.021(7) -0.028(8) C24 0.157(15) 0.168(17) 0.100(10) -0.049(11) 0.015(10) 0.034(13) C25 0.119(12) 0.090(10) 0.178(16) -0.021(11) 0.011(11) -0.018(9) C26 0.091(11) 0.141(15) 0.21(2) -0.050(14) -0.005(11) 0.025(10) C27 0.143(11) 0.066(7) 0.086(7) 0.023(6) -0.070(8) -0.030(7) C28 0.112(10) 0.088(8) 0.090(8) 0.000(7) -0.040(7) -0.016(7) C29 0.113(10) 0.122(11) 0.130(11) 0.008(9) -0.065(9) -0.031(9) C30 0.089(9) 0.137(12) 0.130(11) -0.018(9) -0.019(8) -0.043(8) C31 0.099(9) 0.087(8) 0.111(9) -0.012(7) -0.036(7) -0.034(7) C32 0.142(10) 0.071(7) 0.080(7) -0.010(6) -0.058(7) -0.027(7) C33 0.153(12) 0.126(11) 0.082(8) -0.011(8) -0.025(8) -0.045(10) C34 0.148(12) 0.124(11) 0.073(7) 0.013(7) -0.052(8) -0.030(9) C35 0.108(8) 0.061(6) 0.068(6) -0.020(5) -0.021(6) -0.031(6) C36 0.087(7) 0.082(7) 0.057(5) 0.001(5) -0.014(5) -0.027(6) C37 0.099(8) 0.091(7) 0.061(5) 0.000(5) -0.016(5) -0.046(6) C38 0.095(8) 0.104(9) 0.071(6) -0.003(6) -0.023(6) -0.036(7) C39 0.094(8) 0.083(7) 0.071(6) -0.001(6) -0.018(6) -0.019(6) C40 0.111(9) 0.075(7) 0.076(7) -0.017(6) -0.010(6) -0.022(6) C41 0.093(7) 0.062(6) 0.068(6) -0.012(5) -0.021(5) -0.013(5) C42 0.110(8) 0.082(7) 0.066(6) -0.025(5) -0.012(6) -0.027(6) C43 0.112(9) 0.117(10) 0.064(6) -0.005(7) -0.021(6) -0.026(8) C44 0.096(8) 0.138(11) 0.065(6) 0.016(7) -0.024(6) -0.024(8) C45 0.090(7) 0.077(7) 0.073(6) 0.002(5) -0.024(5) -0.022(6) C46 0.097(12) 0.111(15) 0.057(11) -0.001(12) -0.007(10) -0.061(14) C47 0.100(14) 0.101(14) 0.046(9) 0.001(10) 0.014(10) -0.051(11) C48 0.103(18) 0.115(17) 0.071(13) -0.023(13) 0.022(15) -0.025(15) C49 0.083(13) 0.153(18) 0.053(11) -0.020(12) 0.005(11) -0.024(14) C50 0.084(14) 0.138(17) 0.056(11) -0.032(12) -0.004(10) -0.038(13) C51 0.092(14) 0.099(13) 0.054(10) -0.026(10) 0.000(12) -0.033(13) C52 0.118(17) 0.124(17) 0.051(11) -0.027(11) 0.021(12) -0.069(14) C53 0.115(15) 0.105(16) 0.036(11) -0.018(10) 0.042(12) -0.060(13) C54 0.089(13) 0.117(16) 0.045(9) 0.010(10) 0.001(9) -0.030(12) C55 0.095(15) 0.139(18) 0.056(11) -0.027(12) 0.014(11) -0.038(14) C56 0.067(13) 0.054(12) 0.082(13) -0.022(11) -0.012(11) -0.024(11) C57 0.066(10) 0.073(10) 0.078(10) -0.017(9) -0.003(8) -0.013(9) C58 0.052(14) 0.107(19) 0.095(19) -0.014(15) -0.002(13) -0.021(13) C59 0.11(2) 0.073(18) 0.081(17) -0.017(14) 0.023(15) -0.003(16) C60 0.084(17) 0.10(2) 0.086(19) -0.005(16) -0.013(15) -0.032(16) C71 0.065(11) 0.060(12) 0.076(11) -0.035(10) -0.015(9) -0.012(10) C72 0.056(12) 0.066(11) 0.099(14) -0.020(10) -0.010(10) -0.017(10) C73 0.090(15) 0.085(14) 0.094(15) 0.006(12) 0.015(13) 0.012(12) C74 0.064(12) 0.113(18) 0.071(14) -0.013(13) 0.000(11) -0.019(14) C75 0.085(14) 0.082(14) 0.104(15) -0.018(13) -0.015(12) -0.015(12) C76 0.084(13) 0.064(12) 0.096(13) -0.016(10) -0.022(12) -0.023(11) C77 0.083(14) 0.090(16) 0.098(15) 0.002(13) 0.004(13) -0.005(13) C78 0.102(15) 0.102(15) 0.068(12) -0.033(12) 0.007(11) -0.019(13) C79 0.097(15) 0.109(17) 0.085(14) -0.024(13) 0.009(12) 0.004(13) C80 0.091(13) 0.074(12) 0.102(14) -0.050(11) -0.012(12) -0.014(11) N1 0.089(6) 0.054(4) 0.057(4) -0.005(3) -0.029(4) -0.014(4) N2 0.075(5) 0.071(5) 0.070(5) -0.008(4) -0.022(4) -0.007(4) N3 0.100(6) 0.054(4) 0.056(4) -0.019(4) -0.019(4) -0.012(4) N4 0.111(7) 0.093(6) 0.044(4) -0.007(4) -0.010(4) -0.040(5) Cl1 0.0979(19) 0.0652(15) 0.0858(17) -0.0096(13) -0.0136(14) -0.0220(14) Cl2 0.127(2) 0.0661(16) 0.0867(18) -0.0160(14) -0.0116(17) -0.0310(16) Fe1 0.0926(11) 0.0847(11) 0.0720(9) -0.0155(8) -0.0351(8) -0.0051(9) Fe2 0.0970(11) 0.0803(10) 0.0567(8) -0.0035(7) -0.0210(7) -0.0276(9) Rh1 0.0876(6) 0.0626(5) 0.0776(5) -0.0033(4) -0.0367(4) -0.0158(4) Rh2 0.1146(7) 0.0670(5) 0.0627(5) -0.0140(4) -0.0303(5) -0.0183(5) C83 0.096(16) 0.101(13) 0.049(12) -0.031(10) 0.000(11) 0.002(14) C84 0.112(15) 0.107(14) 0.081(13) 0.000(12) -0.030(12) -0.015(13) C85 0.10(2) 0.087(16) 0.073(18) -0.005(14) -0.016(15) -0.016(16) C86 0.087(16) 0.073(13) 0.056(10) -0.014(9) -0.010(12) 0.005(13) C87 0.119(17) 0.102(15) 0.067(12) -0.004(12) 0.005(13) -0.012(14) C88 0.094(18) 0.096(13) 0.066(12) -0.046(10) -0.008(13) -0.009(15) C102 0.062(13) 0.097(13) 0.075(15) 0.005(13) 0.002(11) -0.008(11) C103 0.076(13) 0.128(16) 0.093(14) -0.031(13) -0.020(11) 0.017(13) C104 0.085(15) 0.102(14) 0.071(14) -0.003(12) -0.023(12) -0.026(13) C105 0.09(2) 0.075(16) 0.069(16) -0.005(13) -0.032(16) -0.007(17) C106 0.092(13) 0.099(13) 0.050(9) -0.005(9) -0.021(10) 0.003(11) C107 0.071(16) 0.108(15) 0.089(15) -0.007(13) -0.002(13) 0.012(15) C90A 0.094(14) 0.120(18) 0.057(12) -0.014(15) -0.008(11) -0.046(17) C91A 0.099(12) 0.124(13) 0.069(10) -0.023(10) 0.001(10) -0.026(11) C92A 0.072(19) 0.14(3) 0.09(2) 0.01(2) -0.006(18) -0.001(18) C93A 0.14(3) 0.14(2) 0.077(18) 0.012(18) 0.01(2) -0.03(3) C94A 0.13(2) 0.17(3) 0.045(15) -0.021(18) 0.03(2) 0.00(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 N1 1.353(13) . ? C1 N2 1.408(14) . ? C1 Rh1 2.083(10) . ? C2 N1 1.420(12) . ? C2 C3 1.427(14) . ? C2 C6 1.493(16) . ? C2 Fe1 1.958(11) . ? C3 C4 1.419(18) . ? C3 Fe1 2.023(12) . ? C3 H3A 0.9300 . ? C4 C5 1.38(2) . ? C4 Fe1 2.079(15) . ? C4 H4A 0.9300 . ? C5 C6 1.462(17) . ? C5 Fe1 2.059(13) . ? C5 H5A 0.9300 . ? C6 Fe1 2.043(12) . ? C6 H6A 0.9300 . ? C7 C11 1.408(16) . ? C7 C8 1.443(15) . ? C7 N2 1.443(13) . ? C7 Fe1 1.979(12) . ? C8 C9 1.392(17) . ? C8 Fe1 2.006(12) . ? C8 H8A 0.9300 . ? C9 C10 1.41(2) . ? C9 Fe1 2.076(12) . ? C9 H9A 0.9300 . ? C10 C11 1.423(15) . ? C10 Fe1 2.070(13) . ? C10 H10A 0.9300 . ? C11 Fe1 2.016(13) . ? C11 H11A 0.9300 . ? C12 C17 1.427(18) . ? C12 N1 1.470(13) . ? C12 C13 1.599(16) . ? C12 H12A 0.9800 . ? C13 C18 1.506(19) . ? C13 C14 1.555(17) . ? C13 H13A 0.9800 . ? C14 C15 1.58(2) . ? C14 H14B 0.9700 . ? C14 H14A 0.9700 . ? C15 C16 1.47(2) . ? C15 C21 1.52(2) . ? C15 H15A 0.9800 . ? C16 C17 1.588(17) . ? C16 H16B 0.9700 . ? C16 H16A 0.9700 . ? C17 C20 1.65(2) . ? C17 H17A 0.9800 . ? C18 C19 1.53(2) . ? C18 H18B 0.9700 . ? C18 H18A 0.9700 . ? C19 C20 1.46(2) . ? C19 C21 1.59(2) . ? C19 H19A 0.9800 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N2 1.510(15) . ? C22 C23 1.580(19) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C25 1.42(2) . ? C23 C24 1.46(2) . ? C23 C26 1.59(2) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26C 0.9600 . ? C26 H26B 0.9600 . ? C26 H26A 0.9600 . ? C27 C28 1.37(2) . ? C27 C34 1.506(19) . ? C27 Rh1 2.180(10) . ? C27 H27A 0.9300 . ? C28 C29 1.51(2) . ? C28 Rh1 2.196(12) . ? C28 H28A 0.9300 . ? C29 C30 1.55(2) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.530(19) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.402(19) . ? C31 Rh1 2.171(12) . ? C31 H31A 0.9300 . ? C32 C33 1.555(16) . ? C32 Rh1 2.116(10) . ? C32 H32A 0.9300 . ? C33 C34 1.54(2) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N4 1.344(15) . ? C35 N3 1.367(14) . ? C35 Rh2 2.120(10) . ? C36 C40 1.382(16) . ? C36 C37 1.434(14) . ? C36 N4 1.448(13) . ? C36 Fe2 1.971(10) . ? C37 C38 1.432(16) . ? C37 Fe2 2.041(11) . ? C37 H37A 0.9300 . ? C38 C39 1.401(17) . ? C38 Fe2 2.043(12) . ? C38 H38A 0.9300 . ? C39 C40 1.410(16) . ? C39 Fe2 2.061(12) . ? C39 H39A 0.9300 . ? C40 Fe2 2.014(12) . ? C40 H40A 0.9300 . ? C41 C45 1.422(15) . ? C41 C42 1.444(13) . ? C41 N3 1.454(12) . ? C41 Fe2 1.947(11) . ? C42 C43 1.448(17) . ? C42 Fe2 2.023(12) . ? C42 H42A 0.9300 . ? C43 C44 1.41(2) . ? C43 Fe2 2.045(13) . ? C43 H43A 0.9300 . ? C44 C45 1.402(15) . ? C44 Fe2 2.055(13) . ? C44 H44A 0.9300 . ? C45 Fe2 2.021(12) . ? C45 H45A 0.9300 . ? C46 C51 1.35(4) . ? C46 N4 1.50(3) . ? C46 C47 1.52(4) . ? C46 H46A 0.9800 . ? C47 C48 1.47(4) . ? C47 C52 1.56(3) . ? C47 H47A 0.9800 . ? C48 C49 1.55(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.51(4) . ? C49 C55 1.54(3) . ? C49 H49A 0.9800 . ? C50 C51 1.65(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C54 1.60(3) . ? C51 H51A 0.9800 . ? C52 C53 1.55(4) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C55 1.54(5) . ? C53 C54 1.60(4) . ? C53 H53A 0.9800 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55B 0.9700 . ? C55 H55A 0.9700 . ? C56 N3 1.64(3) . ? C56 C57 1.65(3) . ? C56 H56B 0.9700 . ? C56 H56A 0.9700 . ? C57 C59 1.53(4) . ? C57 C60 1.53(4) . ? C57 C58 1.54(4) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60C 0.9600 . ? C60 H60B 0.9600 . ? C60 H60A 0.9600 . ? C71 N3 1.34(2) . ? C71 C76 1.52(3) . ? C71 C72 1.59(3) . ? C71 H71A 0.9800 . ? C72 C80 1.52(4) . ? C72 C73 1.55(4) . ? C72 H72A 0.9800 . ? C73 C74 1.51(4) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.50(4) . ? C74 C79 1.59(4) . ? C74 H74A 0.9800 . ? C75 C76 1.54(4) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 C77 1.60(4) . ? C76 H76A 0.9800 . ? C77 C78 1.53(4) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C80 1.54(4) . ? C78 C79 1.55(4) . ? C78 H78A 0.9800 . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 H80B 0.9700 . ? C80 H80A 0.9700 . ? N4 C90A 1.541(18) . ? Cl1 Rh1 2.396(3) . ? Cl2 Rh2 2.386(3) . ? Rh2 C105 2.07(4) . ? Rh2 C104 2.13(3) . ? Rh2 C100 2.18(2) . ? Rh2 C86 2.20(3) . ? Rh2 C82 2.20(3) . ? Rh2 C85 2.21(4) . ? Rh2 C101 2.26(3) . ? Rh2 C81 2.26(2) . ? C81 C88 1.45(5) . ? C81 C82 1.77(4) . ? C81 H81A 0.9300 . ? C82 C83 1.61(4) . ? C82 H82A 0.9300 . ? C83 C84 1.42(4) . ? C83 H83B 0.9700 . ? C83 H83A 0.9700 . ? C84 C85 1.57(4) . ? C84 H84B 0.9700 . ? C84 H84A 0.9700 . ? C85 C86 1.39(4) . ? C85 H85A 0.9300 . ? C86 C87 1.52(3) . ? C86 H86A 0.9300 . ? C87 C88 1.43(4) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C100 C101 1.03(3) . ? C100 C107 1.47(5) . ? C100 H100 0.9300 . ? C101 C102 1.548(19) . ? C101 H101 0.9300 . ? C102 C103 1.37(4) . ? C102 H102 0.9700 . ? C102 H103 0.9700 . ? C103 C104 1.55(4) . ? C103 H104 0.9700 . ? C103 H105 0.9700 . ? C104 C105 1.36(5) . ? C104 H106 0.9300 . ? C105 C106 1.55(4) . ? C105 H107 0.9300 . ? C106 C107 1.51(5) . ? C106 H108 0.9700 . ? C106 H109 0.9700 . ? C107 H110 0.9700 . ? C107 H111 0.9700 . ? C90A C91A 1.67(4) . ? C90A H90A 0.9700 . ? C90A H90B 0.9700 . ? C91A C93A 1.45(5) . ? C91A C94A 1.53(4) . ? C91A C92A 1.58(5) . ? C92A H92A 0.9600 . ? C92A H92B 0.9600 . ? C92A H92C 0.9600 . ? C93A H93A 0.9600 . ? C93A H93B 0.9600 . ? C93A H93C 0.9600 . ? C94A H94A 0.9600 . ? C94A H94B 0.9600 . ? C94A H94C 0.9600 . ? 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 N1 C1 N2 122.8(8) . . ? N1 C1 Rh1 119.9(8) . . ? N2 C1 Rh1 116.8(7) . . ? N1 C2 C3 125.8(10) . . ? N1 C2 C6 124.7(10) . . ? C3 C2 C6 109.5(10) . . ? N1 C2 Fe1 124.6(8) . . ? C3 C2 Fe1 71.5(6) . . ? C6 C2 Fe1 71.2(6) . . ? C4 C3 C2 107.8(12) . . ? C4 C3 Fe1 71.9(8) . . ? C2 C3 Fe1 66.6(7) . . ? C4 C3 H3A 126.1 . . ? C2 C3 H3A 126.1 . . ? Fe1 C3 H3A 126.9 . . ? C5 C4 C3 108.7(11) . . ? C5 C4 Fe1 69.7(9) . . ? C3 C4 Fe1 67.7(7) . . ? C5 C4 H4A 125.7 . . ? C3 C4 H4A 125.7 . . ? Fe1 C4 H4A 128.6 . . ? C4 C5 C6 112.0(11) . . ? C4 C5 Fe1 71.3(9) . . ? C6 C5 Fe1 68.5(7) . . ? C4 C5 H5A 124.0 . . ? C6 C5 H5A 124.0 . . ? Fe1 C5 H5A 127.9 . . ? C5 C6 C2 102.1(11) . . ? C5 C6 Fe1 69.7(7) . . ? C2 C6 Fe1 65.1(6) . . ? C5 C6 H6A 129.0 . . ? C2 C6 H6A 129.0 . . ? Fe1 C6 H6A 127.6 . . ? C11 C7 C8 107.7(9) . . ? C11 C7 N2 129.4(10) . . ? C8 C7 N2 122.9(10) . . ? C11 C7 Fe1 70.8(7) . . ? C8 C7 Fe1 69.8(7) . . ? N2 C7 Fe1 124.3(8) . . ? C9 C8 C7 108.0(12) . . ? C9 C8 Fe1 72.8(8) . . ? C7 C8 Fe1 67.8(7) . . ? C9 C8 H8A 126.0 . . ? C7 C8 H8A 126.0 . . ? Fe1 C8 H8A 125.0 . . ? C8 C9 C10 108.2(11) . . ? C8 C9 Fe1 67.4(7) . . ? C10 C9 Fe1 69.9(7) . . ? C8 C9 H9A 125.9 . . ? C10 C9 H9A 125.9 . . ? Fe1 C9 H9A 128.4 . . ? C9 C10 C11 108.7(11) . . ? C9 C10 Fe1 70.3(8) . . ? C11 C10 Fe1 67.6(7) . . ? C9 C10 H10A 125.7 . . ? C11 C10 H10A 125.7 . . ? Fe1 C10 H10A 128.0 . . ? C7 C11 C10 107.3(11) . . ? C7 C11 Fe1 68.0(7) . . ? C10 C11 Fe1 71.7(8) . . ? C7 C11 H11A 126.3 . . ? C10 C11 H11A 126.3 . . ? Fe1 C11 H11A 125.5 . . ? C17 C12 N1 117.4(9) . . ? C17 C12 C13 111.1(10) . . ? N1 C12 C13 113.6(10) . . ? C17 C12 H12A 104.4 . . ? N1 C12 H12A 104.4 . . ? C13 C12 H12A 104.4 . . ? C18 C13 C14 107.6(11) . . ? C18 C13 C12 113.7(10) . . ? C14 C13 C12 104.0(10) . . ? C18 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? C12 C13 H13A 110.5 . . ? C13 C14 C15 109.1(11) . . ? C13 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? C13 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? H14B C14 H14A 108.3 . . ? C16 C15 C21 111.9(15) . . ? C16 C15 C14 111.0(12) . . ? C21 C15 C14 107.2(14) . . ? C16 C15 H15A 108.9 . . ? C21 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? C15 C16 C17 111.0(14) . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? H16B C16 H16A 108.0 . . ? C12 C17 C16 107.1(11) . . ? C12 C17 C20 114.8(13) . . ? C16 C17 C20 102.8(12) . . ? C12 C17 H17A 110.6 . . ? C16 C17 H17A 110.6 . . ? C20 C17 H17A 110.6 . . ? C13 C18 C19 110.7(13) . . ? C13 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? C13 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? H18B C18 H18A 108.1 . . ? C20 C19 C18 112.7(13) . . ? C20 C19 C21 109.7(14) . . ? C18 C19 C21 108.2(12) . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19A 108.7 . . ? C21 C19 H19A 108.7 . . ? C19 C20 C17 109.4(12) . . ? C19 C20 H20A 109.8 . . ? C17 C20 H20A 109.8 . . ? C19 C20 H20B 109.8 . . ? C17 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? C15 C21 C19 107.4(12) . . ? C15 C21 H21A 110.2 . . ? C19 C21 H21A 110.2 . . ? C15 C21 H21B 110.2 . . ? C19 C21 H21B 110.2 . . ? H21A C21 H21B 108.5 . . ? N2 C22 C23 119.8(10) . . ? N2 C22 H22A 107.4 . . ? C23 C22 H22A 107.4 . . ? N2 C22 H22B 107.4 . . ? C23 C22 H22B 107.4 . . ? H22A C22 H22B 106.9 . . ? C25 C23 C24 113.4(17) . . ? C25 C23 C22 109.1(12) . . ? C24 C23 C22 115.4(13) . . ? C25 C23 C26 109.7(13) . . ? C24 C23 C26 106.3(13) . . ? C22 C23 C26 102.1(13) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26C 109.5 . . ? C23 C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? C23 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? C28 C27 C34 129.0(13) . . ? C28 C27 Rh1 72.4(7) . . ? C34 C27 Rh1 110.5(8) . . ? C28 C27 H27A 115.5 . . ? C34 C27 H27A 115.5 . . ? Rh1 C27 H27A 86.8 . . ? C27 C28 C29 123.1(13) . . ? C27 C28 Rh1 71.1(7) . . ? C29 C28 Rh1 112.3(9) . . ? C27 C28 H28A 118.4 . . ? C29 C28 H28A 118.4 . . ? Rh1 C28 H28A 86.7 . . ? C28 C29 C30 113.5(10) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C31 C30 C29 113.2(12) . . ? C31 C30 H30A 108.9 . . ? C29 C30 H30A 108.9 . . ? C31 C30 H30B 108.9 . . ? C29 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 126.4(13) . . ? C32 C31 Rh1 68.8(7) . . ? C30 C31 Rh1 109.6(9) . . ? C32 C31 H31A 116.8 . . ? C30 C31 H31A 116.8 . . ? Rh1 C31 H31A 91.7 . . ? C31 C32 C33 122.6(13) . . ? C31 C32 Rh1 73.1(7) . . ? C33 C32 Rh1 110.7(9) . . ? C31 C32 H32A 118.7 . . ? C33 C32 H32A 118.7 . . ? Rh1 C32 H32A 86.3 . . ? C34 C33 C32 116.0(11) . . ? C34 C33 H33A 108.3 . . ? C32 C33 H33A 108.3 . . ? C34 C33 H33B 108.3 . . ? C32 C33 H33B 108.3 . . ? H33A C33 H33B 107.4 . . ? C27 C34 C33 109.4(11) . . ? C27 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? C27 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? N4 C35 N3 123.8(9) . . ? N4 C35 Rh2 118.2(7) . . ? N3 C35 Rh2 117.6(8) . . ? C40 C36 C37 108.8(9) . . ? C40 C36 N4 124.9(10) . . ? C37 C36 N4 126.3(10) . . ? C40 C36 Fe2 71.4(6) . . ? C37 C36 Fe2 71.7(6) . . ? N4 C36 Fe2 123.3(8) . . ? C38 C37 C36 104.6(10) . . ? C38 C37 Fe2 69.6(7) . . ? C36 C37 Fe2 66.5(6) . . ? C38 C37 H37A 127.7 . . ? C36 C37 H37A 127.7 . . ? Fe2 C37 H37A 127.7 . . ? C39 C38 C37 110.7(10) . . ? C39 C38 Fe2 70.7(7) . . ? C37 C38 Fe2 69.4(7) . . ? C39 C38 H38A 124.7 . . ? C37 C38 H38A 124.7 . . ? Fe2 C38 H38A 126.8 . . ? C38 C39 C40 105.7(10) . . ? C38 C39 Fe2 69.4(7) . . ? C40 C39 Fe2 68.0(7) . . ? C38 C39 H39A 127.1 . . ? C40 C39 H39A 127.1 . . ? Fe2 C39 H39A 127.1 . . ? C36 C40 C39 110.1(10) . . ? C36 C40 Fe2 68.1(7) . . ? C39 C40 Fe2 71.6(7) . . ? C36 C40 H40A 124.9 . . ? C39 C40 H40A 124.9 . . ? Fe2 C40 H40A 127.0 . . ? C45 C41 C42 110.0(9) . . ? C45 C41 N3 124.5(9) . . ? C42 C41 N3 125.5(9) . . ? C45 C41 Fe2 71.8(6) . . ? C42 C41 Fe2 71.5(7) . . ? N3 C41 Fe2 125.2(8) . . ? C41 C42 C43 104.6(11) . . ? C41 C42 Fe2 65.9(6) . . ? C43 C42 Fe2 69.9(8) . . ? C41 C42 H42A 127.7 . . ? C43 C42 H42A 127.7 . . ? Fe2 C42 H42A 127.9 . . ? C44 C43 C42 108.9(11) . . ? C44 C43 Fe2 70.3(8) . . ? C42 C43 Fe2 68.4(7) . . ? C44 C43 H43A 125.6 . . ? C42 C43 H43A 125.6 . . ? Fe2 C43 H43A 127.4 . . ? C45 C44 C43 109.6(12) . . ? C45 C44 Fe2 68.6(7) . . ? C43 C44 Fe2 69.5(8) . . ? C45 C44 H44A 125.2 . . ? C43 C44 H44A 125.2 . . ? Fe2 C44 H44A 128.3 . . ? C44 C45 C41 106.9(11) . . ? C44 C45 Fe2 71.2(7) . . ? C41 C45 Fe2 66.3(6) . . ? C44 C45 H45A 126.5 . . ? C41 C45 H45A 126.5 . . ? Fe2 C45 H45A 127.5 . . ? C51 C46 N4 117(3) . . ? C51 C46 C47 119(3) . . ? N4 C46 C47 107(2) . . ? C51 C46 H46A 104.0 . . ? N4 C46 H46A 104.0 . . ? C47 C46 H46A 104.0 . . ? C48 C47 C46 112(2) . . ? C48 C47 C52 110(2) . . ? C46 C47 C52 102(2) . . ? C48 C47 H47A 111.1 . . ? C46 C47 H47A 111.1 . . ? C52 C47 H47A 111.1 . . ? C47 C48 C49 114(3) . . ? C47 C48 H48A 108.7 . . ? C49 C48 H48A 108.7 . . ? C47 C48 H48B 108.7 . . ? C49 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? C50 C49 C55 110(3) . . ? C50 C49 C48 104(2) . . ? C55 C49 C48 108(2) . . ? C50 C49 H49A 111.6 . . ? C55 C49 H49A 111.6 . . ? C48 C49 H49A 111.6 . . ? C49 C50 C51 113(2) . . ? C49 C50 H50A 109.0 . . ? C51 C50 H50A 109.0 . . ? C49 C50 H50B 109.0 . . ? C51 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? C46 C51 C54 108(2) . . ? C46 C51 C50 111(3) . . ? C54 C51 C50 102(2) . . ? C46 C51 H51A 112.0 . . ? C54 C51 H51A 112.0 . . ? C50 C51 H51A 112.0 . . ? C53 C52 C47 109.7(19) . . ? C53 C52 H52A 109.7 . . ? C47 C52 H52A 109.7 . . ? C53 C52 H52B 109.7 . . ? C47 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? C52 C53 C55 111(3) . . ? C52 C53 C54 109(3) . . ? C55 C53 C54 106(2) . . ? C52 C53 H53A 110.3 . . ? C55 C53 H53A 110.3 . . ? C54 C53 H53A 110.3 . . ? C51 C54 C53 109(2) . . ? C51 C54 H54A 109.8 . . ? C53 C54 H54A 109.8 . . ? C51 C54 H54B 109.8 . . ? C53 C54 H54B 109.8 . . ? H54A C54 H54B 108.3 . . ? C49 C55 C53 112(2) . . ? C49 C55 H55B 109.2 . . ? C53 C55 H55B 109.2 . . ? C49 C55 H55A 109.2 . . ? C53 C55 H55A 109.2 . . ? H55B C55 H55A 107.9 . . ? N3 C56 C57 117.7(17) . . ? N3 C56 H56B 107.9 . . ? C57 C56 H56B 107.9 . . ? N3 C56 H56A 107.9 . . ? C57 C56 H56A 107.9 . . ? H56B C56 H56A 107.2 . . ? C59 C57 C60 107(2) . . ? C59 C57 C58 115(2) . . ? C60 C57 C58 108(2) . . ? C59 C57 C56 112(2) . . ? C60 C57 C56 103.8(19) . . ? C58 C57 C56 111(2) . . ? N3 C71 C76 113(2) . . ? N3 C71 C72 116.4(17) . . ? C76 C71 C72 109(2) . . ? N3 C71 H71A 106.0 . . ? C76 C71 H71A 106.0 . . ? C72 C71 H71A 106.0 . . ? C80 C72 C73 107(2) . . ? C80 C72 C71 113(2) . . ? C73 C72 C71 101.5(18) . . ? C80 C72 H72A 111.8 . . ? C73 C72 H72A 111.8 . . ? C71 C72 H72A 111.8 . . ? C74 C73 C72 113(2) . . ? C74 C73 H73A 108.9 . . ? C72 C73 H73A 108.9 . . ? C74 C73 H73B 108.9 . . ? C72 C73 H73B 108.9 . . ? H73A C73 H73B 107.7 . . ? C75 C74 C73 111(2) . . ? C75 C74 C79 110(3) . . ? C73 C74 C79 109(2) . . ? C75 C74 H74A 108.7 . . ? C73 C74 H74A 108.7 . . ? C79 C74 H74A 108.7 . . ? C74 C75 C76 108(2) . . ? C74 C75 H75A 110.1 . . ? C76 C75 H75A 110.1 . . ? C74 C75 H75B 110.1 . . ? C76 C75 H75B 110.1 . . ? H75A C75 H75B 108.4 . . ? C71 C76 C75 109(2) . . ? C71 C76 C77 115(2) . . ? C75 C76 C77 106(2) . . ? C71 C76 H76A 108.9 . . ? C75 C76 H76A 108.9 . . ? C77 C76 H76A 108.9 . . ? C78 C77 C76 109(2) . . ? C78 C77 H77A 109.9 . . ? C76 C77 H77A 109.9 . . ? C78 C77 H77B 109.9 . . ? C76 C77 H77B 109.9 . . ? H77A C77 H77B 108.3 . . ? C77 C78 C80 108(2) . . ? C77 C78 C79 110(2) . . ? C80 C78 C79 110(3) . . ? C77 C78 H78A 109.8 . . ? C80 C78 H78A 109.8 . . ? C79 C78 H78A 109.8 . . ? C78 C79 C74 107(2) . . ? C78 C79 H79A 110.4 . . ? C74 C79 H79A 110.4 . . ? C78 C79 H79B 110.4 . . ? C74 C79 H79B 110.4 . . ? H79A C79 H79B 108.6 . . ? C72 C80 C78 114.0(19) . . ? C72 C80 H80B 108.8 . . ? C78 C80 H80B 108.8 . . ? C72 C80 H80A 108.8 . . ? C78 C80 H80A 108.8 . . ? H80B C80 H80A 107.6 . . ? C1 N1 C2 128.2(9) . . ? C1 N1 C12 115.3(8) . . ? C2 N1 C12 115.4(9) . . ? C1 N2 C7 125.7(9) . . ? C1 N2 C22 119.0(8) . . ? C7 N2 C22 113.4(8) . . ? C71 N3 C35 112.6(13) . . ? C71 N3 C41 121.2(13) . . ? C35 N3 C41 126.0(9) . . ? C71 N3 C56 28.0(12) . . ? C35 N3 C56 120.2(11) . . ? C41 N3 C56 109.7(12) . . ? C35 N4 C36 128.2(9) . . ? C35 N4 C46 115.9(17) . . ? C36 N4 C46 115.9(18) . . ? C35 N4 C90A 118.0(16) . . ? C36 N4 C90A 109.4(17) . . ? C46 N4 C90A 24.6(15) . . ? C2 Fe1 C7 93.1(5) . . ? C2 Fe1 C8 114.4(5) . . ? C7 Fe1 C8 42.4(4) . . ? C2 Fe1 C11 110.6(4) . . ? C7 Fe1 C11 41.2(5) . . ? C8 Fe1 C11 69.8(5) . . ? C2 Fe1 C3 42.0(4) . . ? C7 Fe1 C3 111.6(5) . . ? C8 Fe1 C3 102.5(5) . . ? C11 Fe1 C3 147.2(4) . . ? C2 Fe1 C6 43.8(5) . . ? C7 Fe1 C6 113.5(5) . . ? C8 Fe1 C6 152.7(4) . . ? C11 Fe1 C6 100.1(5) . . ? C3 Fe1 C6 71.8(5) . . ? C2 Fe1 C5 69.7(5) . . ? C7 Fe1 C5 155.1(5) . . ? C8 Fe1 C5 161.4(6) . . ? C11 Fe1 C5 127.1(6) . . ? C3 Fe1 C5 67.8(6) . . ? C6 Fe1 C5 41.8(5) . . ? C2 Fe1 C10 150.5(5) . . ? C7 Fe1 C10 68.5(5) . . ? C8 Fe1 C10 67.7(6) . . ? C11 Fe1 C10 40.7(5) . . ? C3 Fe1 C10 166.0(5) . . ? C6 Fe1 C10 121.6(6) . . ? C5 Fe1 C10 118.5(6) . . ? C2 Fe1 C9 154.0(5) . . ? C7 Fe1 C9 68.8(5) . . ? C8 Fe1 C9 39.8(5) . . ? C11 Fe1 C9 68.4(6) . . ? C3 Fe1 C9 126.4(6) . . ? C6 Fe1 C9 160.6(6) . . ? C5 Fe1 C9 132.9(5) . . ? C10 Fe1 C9 39.8(6) . . ? C2 Fe1 C4 69.3(5) . . ? C7 Fe1 C4 151.2(6) . . ? C8 Fe1 C4 123.6(6) . . ? C11 Fe1 C4 166.0(6) . . ? C3 Fe1 C4 40.4(5) . . ? C6 Fe1 C4 69.8(6) . . ? C5 Fe1 C4 39.0(6) . . ? C10 Fe1 C4 136.2(5) . . ? C9 Fe1 C4 118.2(6) . . ? C41 Fe2 C36 93.3(4) . . ? C41 Fe2 C40 112.8(5) . . ? C36 Fe2 C40 40.6(5) . . ? C41 Fe2 C45 41.9(4) . . ? C36 Fe2 C45 114.1(4) . . ? C40 Fe2 C45 104.5(5) . . ? C41 Fe2 C42 42.6(4) . . ? C36 Fe2 C42 110.8(5) . . ? C40 Fe2 C42 147.9(5) . . ? C45 Fe2 C42 70.9(5) . . ? C41 Fe2 C37 112.1(5) . . ? C36 Fe2 C37 41.8(4) . . ? C40 Fe2 C37 68.8(5) . . ? C45 Fe2 C37 150.2(4) . . ? C42 Fe2 C37 99.0(5) . . ? C41 Fe2 C38 152.7(5) . . ? C36 Fe2 C38 68.7(4) . . ? C40 Fe2 C38 67.1(5) . . ? C45 Fe2 C38 164.4(5) . . ? C42 Fe2 C38 123.4(5) . . ? C37 Fe2 C38 41.0(5) . . ? C41 Fe2 C43 69.9(5) . . ? C36 Fe2 C43 151.6(5) . . ? C40 Fe2 C43 167.3(6) . . ? C45 Fe2 C43 68.8(5) . . ? C42 Fe2 C43 41.7(5) . . ? C37 Fe2 C43 122.5(5) . . ? C38 Fe2 C43 116.7(5) . . ? C41 Fe2 C44 69.0(5) . . ? C36 Fe2 C44 154.0(5) . . ? C40 Fe2 C44 128.0(6) . . ? C45 Fe2 C44 40.2(5) . . ? C42 Fe2 C44 69.4(6) . . ? C37 Fe2 C44 162.3(6) . . ? C38 Fe2 C44 134.3(4) . . ? C43 Fe2 C44 40.2(6) . . ? C41 Fe2 C39 152.4(4) . . ? C36 Fe2 C39 69.1(5) . . ? C40 Fe2 C39 40.5(5) . . ? C45 Fe2 C39 125.3(5) . . ? C42 Fe2 C39 163.1(5) . . ? C37 Fe2 C39 69.2(5) . . ? C38 Fe2 C39 39.9(5) . . ? C43 Fe2 C39 134.3(5) . . ? C44 Fe2 C39 118.6(5) . . ? C1 Rh1 C32 97.7(4) . . ? C1 Rh1 C31 93.4(5) . . ? C32 Rh1 C31 38.1(5) . . ? C1 Rh1 C27 162.8(6) . . ? C32 Rh1 C27 82.3(4) . . ? C31 Rh1 C27 96.9(5) . . ? C1 Rh1 C28 160.1(5) . . ? C32 Rh1 C28 90.3(5) . . ? C31 Rh1 C28 81.7(5) . . ? C27 Rh1 C28 36.5(5) . . ? C1 Rh1 Cl1 84.0(3) . . ? C32 Rh1 Cl1 164.9(4) . . ? C31 Rh1 Cl1 156.9(4) . . ? C27 Rh1 Cl1 91.6(3) . . ? C28 Rh1 Cl1 92.9(4) . . ? C105 Rh2 C35 98.9(9) . . ? C105 Rh2 C104 37.8(12) . . ? C35 Rh2 C104 95.0(8) . . ? C105 Rh2 C100 83.4(11) . . ? C35 Rh2 C100 169.7(9) . . ? C104 Rh2 C100 92.9(10) . . ? C105 Rh2 C86 20.0(9) . . ? C35 Rh2 C86 93.2(8) . . ? C104 Rh2 C86 57.0(10) . . ? C100 Rh2 C86 85.5(10) . . ? C105 Rh2 C82 92.1(13) . . ? C35 Rh2 C82 156.7(9) . . ? C104 Rh2 C82 81.2(11) . . ? C100 Rh2 C82 31.9(10) . . ? C86 Rh2 C82 103.6(11) . . ? C105 Rh2 C85 17.3(12) . . ? C35 Rh2 C85 96.5(10) . . ? C104 Rh2 C85 20.5(10) . . ? C100 Rh2 C85 88.6(12) . . ? C86 Rh2 C85 36.6(11) . . ? C82 Rh2 C85 87.9(13) . . ? C105 Rh2 C101 80.7(12) . . ? C35 Rh2 C101 163.5(9) . . ? C104 Rh2 C101 74.5(10) . . ? C100 Rh2 C101 26.7(9) . . ? C86 Rh2 C101 91.5(12) . . ? C82 Rh2 C101 12.0(13) . . ? C85 Rh2 C101 78.2(13) . . ? C105 Rh2 C81 80.0(11) . . ? C35 Rh2 C81 155.7(8) . . ? C104 Rh2 C81 98.3(10) . . ? C100 Rh2 C81 14.7(8) . . ? C86 Rh2 C81 77.4(9) . . ? C82 Rh2 C81 46.6(10) . . ? C85 Rh2 C81 89.2(12) . . ? C101 Rh2 C81 40.7(10) . . ? C105 Rh2 Cl2 168.0(11) . . ? C35 Rh2 Cl2 84.4(3) . . ? C104 Rh2 Cl2 153.9(9) . . ? C100 Rh2 Cl2 91.4(7) . . ? C86 Rh2 Cl2 149.1(7) . . ? C82 Rh2 Cl2 89.1(8) . . ? C85 Rh2 Cl2 174.3(11) . . ? C101 Rh2 Cl2 99.4(8) . . ? C81 Rh2 Cl2 92.3(7) . . ? C88 C81 C82 133(2) . . ? C88 C81 Rh2 113.5(17) . . ? C82 C81 Rh2 64.8(13) . . ? C88 C81 H81A 113.5 . . ? C82 C81 H81A 113.5 . . ? Rh2 C81 H81A 91.9 . . ? C83 C82 C81 98(2) . . ? C83 C82 Rh2 103.3(19) . . ? C81 C82 Rh2 68.6(12) . . ? C83 C82 H82A 130.9 . . ? C81 C82 H82A 130.9 . . ? Rh2 C82 H82A 96.0 . . ? C84 C83 C82 123(3) . . ? C84 C83 H83B 106.5 . . ? C82 C83 H83B 106.5 . . ? C84 C83 H83A 106.5 . . ? C82 C83 H83A 106.5 . . ? H83B C83 H83A 106.5 . . ? C83 C84 C85 119(3) . . ? C83 C84 H84B 107.6 . . ? C85 C84 H84B 107.6 . . ? C83 C84 H84A 107.6 . . ? C85 C84 H84A 107.6 . . ? H84B C84 H84A 107.0 . . ? C86 C85 C84 125(3) . . ? C86 C85 Rh2 71(2) . . ? C84 C85 Rh2 106(2) . . ? C86 C85 H85A 117.3 . . ? C84 C85 H85A 117.3 . . ? Rh2 C85 H85A 93.1 . . ? C85 C86 C87 127(3) . . ? C85 C86 Rh2 72(2) . . ? C87 C86 Rh2 111.1(19) . . ? C85 C86 H86A 116.7 . . ? C87 C86 H86A 116.7 . . ? Rh2 C86 H86A 86.4 . . ? C88 C87 C86 116(3) . . ? C88 C87 H87A 108.3 . . ? C86 C87 H87A 108.3 . . ? C88 C87 H87B 108.3 . . ? C86 C87 H87B 108.3 . . ? H87A C87 H87B 107.4 . . ? C81 C88 C87 116(3) . . ? C81 C88 H88A 108.4 . . ? C87 C88 H88A 108.4 . . ? C81 C88 H88B 108.3 . . ? C87 C88 H88B 108.3 . . ? H88A C88 H88B 107.4 . . ? C101 C100 C107 113(3) . . ? C101 C100 Rh2 81(2) . . ? C107 C100 Rh2 106(2) . . ? C101 C100 H100 123.4 . . ? C107 C100 H100 123.4 . . ? Rh2 C100 H100 84.0 . . ? C100 C101 C102 155(4) . . ? C100 C101 Rh2 73(2) . . ? C102 C101 Rh2 112(2) . . ? C100 C101 H101 102.3 . . ? C102 C101 H101 102.3 . . ? Rh2 C101 H101 80.1 . . ? C103 C102 C101 116(3) . . ? C103 C102 H102 108.3 . . ? C101 C102 H102 108.3 . . ? C103 C102 H103 108.3 . . ? C101 C102 H103 108.3 . . ? H102 C102 H103 107.4 . . ? C102 C103 C104 113(2) . . ? C102 C103 H104 109.0 . . ? C104 C103 H104 109.0 . . ? C102 C103 H105 109.0 . . ? C104 C103 H105 109.0 . . ? H104 C103 H105 107.8 . . ? C105 C104 C103 127(3) . . ? C105 C104 Rh2 68.7(19) . . ? C103 C104 Rh2 116(2) . . ? C105 C104 H106 116.7 . . ? C103 C104 H106 116.7 . . ? Rh2 C104 H106 85.0 . . ? C104 C105 C106 125(3) . . ? C104 C105 Rh2 74(2) . . ? C106 C105 Rh2 110(2) . . ? C104 C105 H107 117.5 . . ? C106 C105 H107 117.5 . . ? Rh2 C105 H107 86.5 . . ? C107 C106 C105 115(3) . . ? C107 C106 H108 108.5 . . ? C105 C106 H108 108.5 . . ? C107 C106 H109 108.5 . . ? C105 C106 H109 108.5 . . ? H108 C106 H109 107.5 . . ? C100 C107 C106 115(3) . . ? C100 C107 H110 108.5 . . ? C106 C107 H110 108.5 . . ? C100 C107 H111 108.5 . . ? C106 C107 H111 108.5 . . ? H110 C107 H111 107.5 . . ? N4 C90A C91A 123(2) . . ? N4 C90A H90A 106.6 . . ? C91A C90A H90A 106.6 . . ? N4 C90A H90B 106.6 . . ? C91A C90A H90B 106.6 . . ? H90A C90A H90B 106.6 . . ? C93A C91A C94A 117(3) . . ? C93A C91A C92A 111(3) . . ? C94A C91A C92A 108(3) . . ? C93A C91A C90A 104(3) . . ? C94A C91A C90A 104(3) . . ? C92A C91A C90A 114(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 24.91 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.056 _refine_diff_density_min -1.528 _refine_diff_density_rms 0.184 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.057 0.234 0.004 16 2 ' ' 2 0.500 0.500 0.500 34 5 ' ' 3 0.942 0.766 -0.004 16 2 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 976856'