data_rob556_mo_b _audit_creation_date 2014-09-15 _audit_creation_method ; Olex2 1.2 (compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H26 N3 Rh, 2(F6 Sb)' _chemical_formula_sum 'C16 H26 F12 N3 Rh Sb2' _chemical_formula_weight 834.81 _chemical_melting_point ? _chemical_oxdiff_formula 'Rh1 C16 H26 N3 Sb2 F12' 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' 'F' 'F' 0.0171 0.0103 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.72575(16) _cell_length_b 17.2034(4) _cell_length_c 18.9758(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.856(2) _cell_angle_gamma 90.00 _cell_volume 2498.40(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13845 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 30.9100 _cell_measurement_theta_min 3.4400 _exptl_absorpt_coefficient_mu 2.899 _exptl_absorpt_correction_T_max 0.727 _exptl_absorpt_correction_T_min 0.506 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light orange' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.219 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1592 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_unetI/netI 0.0547 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 30615 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 2.91 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3095 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 31.00 73.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 57.0000 30.0000 42 #__ type_ start__ end____ width___ exp.time_ 2 omega 3.00 75.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 37.0000 -150.0000 72 #__ type_ start__ end____ width___ exp.time_ 3 omega 15.00 78.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 37.0000 -90.0000 63 #__ type_ start__ end____ width___ exp.time_ 4 omega 58.00 84.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 37.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega -29.00 -2.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 -57.0000 -60.0000 27 #__ type_ start__ end____ width___ exp.time_ 6 omega -22.00 38.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 -57.0000 60.0000 60 #__ type_ start__ end____ width___ exp.time_ 7 omega -11.00 79.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 57.0000 -30.0000 90 #__ type_ start__ end____ width___ exp.time_ 8 omega 21.00 63.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 37.0000 150.0000 42 #__ type_ start__ end____ width___ exp.time_ 9 omega -14.00 11.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -13.7322 -57.0000 -120.0000 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0272226000 _diffrn_orient_matrix_UB_12 -0.0314542000 _diffrn_orient_matrix_UB_13 0.0230389000 _diffrn_orient_matrix_UB_21 0.0090665000 _diffrn_orient_matrix_UB_22 -0.0237150000 _diffrn_orient_matrix_UB_23 -0.0298614000 _diffrn_orient_matrix_UB_31 0.0881165000 _diffrn_orient_matrix_UB_32 0.0121559000 _diffrn_orient_matrix_UB_33 0.0013774000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5413 _reflns_number_total 6199 _reflns_odcompleteness_completeness 99.84 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.22 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.755 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.189 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 309 _refine_ls_number_reflns 6199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0353 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.5212P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.0905 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B) 2.b Me refined with riding coordinates: C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C) 2.c Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C16(H16A,H16B,H16C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn Rh1 Rh 0.46048(3) 0.229279(17) 0.394921(14) 0.01341(8) Uani 1 d . . . N1 N 0.3209(4) 0.30423(19) 0.31746(16) 0.0189(6) Uani 1 d . . . H1A H 0.3193 0.3520 0.3367 0.023 Uiso 1 calc . . R H1B H 0.3822 0.3076 0.2805 0.023 Uiso 1 calc . . R C1 C 0.1385(5) 0.2830(2) 0.28900(19) 0.0205(8) Uani 1 d . . . H1C H 0.1388 0.2348 0.2626 0.025 Uiso 1 calc . . R H1D H 0.0890 0.3231 0.2564 0.025 Uiso 1 calc . . R N2 N 0.6297(4) 0.3246(2) 0.41140(16) 0.0193(7) Uani 1 d . . . C2 C 0.0249(4) 0.2735(2) 0.3479(2) 0.0205(8) Uani 1 d . . . H2A H -0.0967 0.2776 0.3271 0.025 Uiso 1 calc . . R H2B H 0.0492 0.3162 0.3812 0.025 Uiso 1 calc . . R N3 N 0.5956(4) 0.18688(19) 0.31276(16) 0.0184(6) Uani 1 d . . . C3 C 0.0495(5) 0.1971(2) 0.3893(2) 0.0225(8) Uani 1 d . . . H3A H -0.0325 0.1961 0.4237 0.027 Uiso 1 calc . . R H3B H 0.0193 0.1546 0.3563 0.027 Uiso 1 calc . . R C4 C 0.2294(5) 0.1824(2) 0.42803(18) 0.0182(7) Uani 1 d . . . C5 C 0.3197(5) 0.2307(2) 0.48382(19) 0.0175(7) Uani 1 d . . . C6 C 0.4882(5) 0.1941(2) 0.50638(19) 0.0178(7) Uani 1 d . . . C7 C 0.5042(4) 0.1286(2) 0.46298(18) 0.0169(7) Uani 1 d . . . C8 C 0.3428(5) 0.1203(2) 0.41429(19) 0.0182(7) Uani 1 d . . . C9 C 0.2457(5) 0.2975(2) 0.5191(2) 0.0230(8) Uani 1 d . . . H9A H 0.3380 0.3325 0.5371 0.034 Uiso 1 calc . . R H9B H 0.1885 0.2790 0.5577 0.034 Uiso 1 calc . . R H9C H 0.1627 0.3242 0.4853 0.034 Uiso 1 calc . . R C10 C 0.6216(5) 0.2242(3) 0.5643(2) 0.0279(9) Uani 1 d . . . H10A H 0.7364 0.2130 0.5530 0.042 Uiso 1 calc . . R H10B H 0.6062 0.1995 0.6084 0.042 Uiso 1 calc . . R H10C H 0.6079 0.2794 0.5687 0.042 Uiso 1 calc . . R C11 C 0.6582(5) 0.0747(2) 0.4676(2) 0.0257(9) Uani 1 d . . . H11A H 0.6637 0.0518 0.4219 0.039 Uiso 1 calc . . R H11B H 0.6459 0.0345 0.5017 0.039 Uiso 1 calc . . R H11C H 0.7636 0.1034 0.4823 0.039 Uiso 1 calc . . R C12 C 0.3023(5) 0.0567(2) 0.36141(19) 0.0205(8) Uani 1 d . . . H12A H 0.2223 0.0755 0.3219 0.031 Uiso 1 calc . . R H12B H 0.2503 0.0139 0.3833 0.031 Uiso 1 calc . . R H12C H 0.4081 0.0398 0.3449 0.031 Uiso 1 calc . . R C13 C 0.7027(5) 0.3821(2) 0.41711(19) 0.0186(8) Uani 1 d . . . C14 C 0.7986(5) 0.4549(2) 0.4228(2) 0.0230(8) Uani 1 d . . . H14A H 0.8316 0.4681 0.3773 0.034 Uiso 1 calc . . GR H14B H 0.9016 0.4494 0.4570 0.034 Uiso 1 calc . . GR H14C H 0.7260 0.4952 0.4378 0.034 Uiso 1 calc . . GR C15 C 0.6624(4) 0.1567(2) 0.27057(19) 0.0166(7) Uani 1 d . . . C16 C 0.7519(5) 0.1176(2) 0.2178(2) 0.0231(8) Uani 1 d . . . H16A H 0.6779 0.1172 0.1728 0.035 Uiso 1 calc . . GR H16B H 0.7785 0.0652 0.2328 0.035 Uiso 1 calc . . GR H16C H 0.8582 0.1448 0.2130 0.035 Uiso 1 calc . . GR Sb2 Sb 0.23735(3) 0.040294(15) 0.135464(13) 0.01839(8) Uani 1 d . . . F7 F 0.0731(3) -0.01265(17) 0.18114(14) 0.0398(7) Uani 1 d . . . F8 F 0.2011(4) 0.13049(16) 0.18623(14) 0.0389(6) Uani 1 d . . . F9 F 0.4009(3) 0.09169(16) 0.08794(13) 0.0331(6) Uani 1 d . . . F10 F 0.2717(3) -0.05137(15) 0.08543(14) 0.0350(6) Uani 1 d . . . F11 F 0.0613(3) 0.06984(16) 0.06290(13) 0.0343(6) Uani 1 d . . . F12 F 0.4170(3) 0.00986(17) 0.20619(12) 0.0345(6) Uani 1 d . . . Sb1 Sb 0.66333(3) 0.389308(15) 0.161686(12) 0.01855(8) Uani 1 d . . . F1 F 0.4433(3) 0.36548(18) 0.18657(14) 0.0402(7) Uani 1 d . . . F2 F 0.6037(3) 0.49479(15) 0.15166(14) 0.0338(6) Uani 1 d . . . F3 F 0.8833(3) 0.41103(16) 0.13563(15) 0.0377(6) Uani 1 d . . . F4 F 0.7298(4) 0.28502(15) 0.17374(14) 0.0412(7) Uani 1 d . . . F5 F 0.7466(3) 0.40620(17) 0.25770(13) 0.0374(6) Uani 1 d . . . F6 F 0.5760(3) 0.37093(17) 0.06621(12) 0.0351(6) Uani 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 Rh1 0.01363(14) 0.01338(16) 0.01338(14) 0.00054(10) 0.00244(10) -0.00250(10) N1 0.0172(14) 0.0191(18) 0.0207(15) 0.0002(13) 0.0041(12) 0.0001(12) C1 0.0208(18) 0.023(2) 0.0169(17) -0.0022(15) -0.0004(14) 0.0037(15) N2 0.0155(14) 0.0253(19) 0.0176(15) 0.0002(13) 0.0040(12) -0.0022(13) C2 0.0138(16) 0.018(2) 0.029(2) 0.0022(16) 0.0021(15) 0.0002(14) N3 0.0186(14) 0.0176(17) 0.0186(15) 0.0005(13) 0.0012(12) -0.0039(12) C3 0.0171(17) 0.022(2) 0.029(2) -0.0023(17) 0.0055(15) -0.0009(15) C4 0.0203(17) 0.020(2) 0.0157(16) 0.0019(14) 0.0072(14) -0.0065(15) C5 0.0216(17) 0.017(2) 0.0150(16) 0.0019(14) 0.0053(14) -0.0058(14) C6 0.0215(17) 0.016(2) 0.0150(16) 0.0006(14) -0.0013(14) -0.0065(14) C7 0.0183(16) 0.0164(19) 0.0154(16) 0.0053(14) 0.0002(14) -0.0059(14) C8 0.0208(17) 0.017(2) 0.0169(17) 0.0014(14) 0.0037(14) -0.0076(14) C9 0.030(2) 0.020(2) 0.0208(18) -0.0025(15) 0.0102(16) -0.0046(16) C10 0.036(2) 0.026(2) 0.0199(19) -0.0006(16) -0.0011(17) -0.0044(18) C11 0.0225(19) 0.022(2) 0.030(2) 0.0035(17) -0.0026(16) -0.0038(16) C12 0.0278(19) 0.0137(19) 0.0194(18) -0.0003(14) 0.0016(15) -0.0024(15) C13 0.0188(17) 0.021(2) 0.0154(16) 0.0014(14) 0.0002(14) -0.0008(15) C14 0.0260(19) 0.020(2) 0.0233(19) -0.0018(15) 0.0055(16) -0.0081(15) C15 0.0175(16) 0.0114(18) 0.0196(17) 0.0012(14) -0.0021(14) -0.0035(13) C16 0.0284(19) 0.020(2) 0.0230(19) -0.0039(15) 0.0104(16) 0.0045(16) Sb2 0.02043(13) 0.01537(15) 0.01957(13) 0.00018(9) 0.00346(10) 0.00230(9) F7 0.0367(14) 0.0413(17) 0.0443(15) 0.0117(13) 0.0159(12) -0.0048(12) F8 0.0639(17) 0.0228(14) 0.0312(13) -0.0064(11) 0.0109(12) 0.0099(12) F9 0.0326(12) 0.0384(16) 0.0299(13) 0.0021(11) 0.0093(10) -0.0098(11) F10 0.0473(14) 0.0191(13) 0.0377(14) -0.0095(11) 0.0030(12) 0.0044(11) F11 0.0295(12) 0.0333(16) 0.0371(14) 0.0096(12) -0.0059(11) 0.0064(11) F12 0.0333(13) 0.0427(17) 0.0260(12) 0.0032(12) -0.0019(10) 0.0078(11) Sb1 0.02245(14) 0.01658(15) 0.01673(13) 0.00032(9) 0.00308(10) -0.00006(9) F1 0.0337(13) 0.0564(19) 0.0329(14) 0.0010(13) 0.0134(11) -0.0177(13) F2 0.0383(13) 0.0220(14) 0.0433(15) 0.0060(11) 0.0134(11) 0.0097(11) F3 0.0239(12) 0.0391(17) 0.0525(16) 0.0030(13) 0.0143(12) 0.0043(11) F4 0.0736(19) 0.0175(14) 0.0319(14) 0.0026(11) 0.0052(13) 0.0060(13) F5 0.0448(15) 0.0427(17) 0.0219(12) -0.0089(11) -0.0055(11) 0.0053(12) F6 0.0428(14) 0.0455(17) 0.0168(11) -0.0009(11) 0.0037(10) 0.0046(12) _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 Rh1 N1 2.134(3) . ? Rh1 N2 2.094(3) . ? Rh1 N3 2.121(3) . ? Rh1 C4 2.130(3) . ? Rh1 C5 2.129(3) . ? Rh1 C6 2.182(4) . ? Rh1 C7 2.160(4) . ? Rh1 C8 2.138(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N1 C1 1.484(5) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C1 C2 1.522(5) . ? N2 C13 1.137(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.529(6) . ? N3 C15 1.135(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.502(5) . ? C4 C5 1.447(5) . ? C4 C8 1.429(5) . ? C5 C6 1.456(5) . ? C5 C9 1.483(5) . ? C6 C7 1.412(5) . ? C6 C10 1.492(5) . ? C7 C8 1.454(5) . ? C7 C11 1.501(5) . ? C8 C12 1.488(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.450(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.457(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Sb2 F7 1.869(2) . ? Sb2 F8 1.868(3) . ? Sb2 F9 1.872(2) . ? Sb2 F10 1.878(2) . ? Sb2 F11 1.869(2) . ? Sb2 F12 1.869(2) . ? Sb1 F1 1.871(2) . ? Sb1 F2 1.876(2) . ? Sb1 F3 1.872(2) . ? Sb1 F4 1.872(3) . ? Sb1 F5 1.870(2) . ? Sb1 F6 1.872(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 Rh1 C6 143.96(13) . . ? N1 Rh1 C7 156.90(12) . . ? N1 Rh1 C8 117.51(13) . . ? N2 Rh1 N1 82.88(12) . . ? N2 Rh1 N3 91.09(12) . . ? N2 Rh1 C4 141.60(13) . . ? N2 Rh1 C5 104.42(13) . . ? N2 Rh1 C6 95.49(13) . . ? N2 Rh1 C7 119.70(12) . . ? N2 Rh1 C8 158.89(13) . . ? N3 Rh1 N1 87.39(12) . . ? N3 Rh1 C4 127.10(13) . . ? N3 Rh1 C5 160.52(13) . . ? N3 Rh1 C6 128.65(13) . . ? N3 Rh1 C7 96.39(13) . . ? N3 Rh1 C8 95.07(13) . . ? C4 Rh1 N1 93.85(13) . . ? C4 Rh1 C6 65.44(13) . . ? C4 Rh1 C7 65.73(14) . . ? C4 Rh1 C8 39.11(15) . . ? C5 Rh1 N1 105.92(13) . . ? C5 Rh1 C4 39.74(13) . . ? C5 Rh1 C6 39.46(14) . . ? C5 Rh1 C7 65.82(14) . . ? C5 Rh1 C8 66.32(14) . . ? C7 Rh1 C6 37.96(14) . . ? C8 Rh1 C6 65.04(13) . . ? C8 Rh1 C7 39.55(13) . . ? Rh1 N1 H1A 107.8 . . ? Rh1 N1 H1B 107.8 . . ? H1A N1 H1B 107.2 . . ? C1 N1 Rh1 117.9(2) . . ? C1 N1 H1A 107.8 . . ? C1 N1 H1B 107.8 . . ? N1 C1 H1C 109.2 . . ? N1 C1 H1D 109.2 . . ? N1 C1 C2 111.9(3) . . ? H1C C1 H1D 107.9 . . ? C2 C1 H1C 109.2 . . ? C2 C1 H1D 109.2 . . ? C13 N2 Rh1 170.9(3) . . ? C1 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? C1 C2 C3 115.2(3) . . ? H2A C2 H2B 107.5 . . ? C3 C2 H2A 108.5 . . ? C3 C2 H2B 108.5 . . ? C15 N3 Rh1 172.9(3) . . ? C2 C3 H3A 108.3 . . ? C2 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C4 C3 C2 116.0(3) . . ? C4 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? C3 C4 Rh1 123.3(3) . . ? C5 C4 Rh1 70.08(19) . . ? C5 C4 C3 125.6(3) . . ? C8 C4 Rh1 70.7(2) . . ? C8 C4 C3 125.9(3) . . ? C8 C4 C5 108.5(3) . . ? C4 C5 Rh1 70.19(19) . . ? C4 C5 C6 106.8(3) . . ? C4 C5 C9 126.7(3) . . ? C6 C5 Rh1 72.2(2) . . ? C6 C5 C9 125.9(3) . . ? C9 C5 Rh1 129.5(3) . . ? C5 C6 Rh1 68.3(2) . . ? C5 C6 C10 124.5(3) . . ? C7 C6 Rh1 70.2(2) . . ? C7 C6 C5 108.7(3) . . ? C7 C6 C10 126.8(3) . . ? C10 C6 Rh1 125.7(3) . . ? C6 C7 Rh1 71.9(2) . . ? C6 C7 C8 108.2(3) . . ? C6 C7 C11 126.2(3) . . ? C8 C7 Rh1 69.4(2) . . ? C8 C7 C11 125.5(3) . . ? C11 C7 Rh1 126.0(3) . . ? C4 C8 Rh1 70.2(2) . . ? C4 C8 C7 107.7(3) . . ? C4 C8 C12 126.5(3) . . ? C7 C8 Rh1 71.0(2) . . ? C7 C8 C12 125.7(3) . . ? C12 C8 Rh1 125.7(3) . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 178.4(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 178.5(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? F7 Sb2 F9 178.67(12) . . ? F7 Sb2 F10 88.69(12) . . ? F7 Sb2 F11 90.13(11) . . ? F7 Sb2 F12 90.86(11) . . ? F8 Sb2 F7 90.38(13) . . ? F8 Sb2 F9 90.84(12) . . ? F8 Sb2 F10 179.04(12) . . ? F8 Sb2 F11 90.51(12) . . ? F8 Sb2 F12 90.65(12) . . ? F9 Sb2 F10 90.10(12) . . ? F11 Sb2 F9 89.30(11) . . ? F11 Sb2 F10 89.71(12) . . ? F11 Sb2 F12 178.47(11) . . ? F12 Sb2 F9 89.68(11) . . ? F12 Sb2 F10 89.16(12) . . ? F1 Sb1 F2 91.05(12) . . ? F1 Sb1 F3 178.69(13) . . ? F1 Sb1 F4 90.15(13) . . ? F1 Sb1 F6 89.28(11) . . ? F3 Sb1 F2 89.98(11) . . ? F3 Sb1 F6 89.90(12) . . ? F4 Sb1 F2 178.04(12) . . ? F4 Sb1 F3 88.84(13) . . ? F4 Sb1 F6 90.74(12) . . ? F5 Sb1 F1 89.51(12) . . ? F5 Sb1 F2 89.74(12) . . ? F5 Sb1 F3 91.30(12) . . ? F5 Sb1 F4 88.73(12) . . ? F5 Sb1 F6 178.68(12) . . ? F6 Sb1 F2 90.81(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 N1 C1 C2 56.0(4) . . . . ? Rh1 N2 C13 C14 -111(15) . . . . ? Rh1 N3 C15 C16 -84(16) . . . . ? Rh1 C4 C5 C6 -63.4(2) . . . . ? Rh1 C4 C5 C9 125.1(4) . . . . ? Rh1 C4 C8 C7 61.4(2) . . . . ? Rh1 C4 C8 C12 -120.3(4) . . . . ? Rh1 C5 C6 C7 -58.7(3) . . . . ? Rh1 C5 C6 C10 119.3(4) . . . . ? Rh1 C6 C7 C8 -60.2(2) . . . . ? Rh1 C6 C7 C11 121.8(4) . . . . ? Rh1 C7 C8 C4 -60.9(2) . . . . ? Rh1 C7 C8 C12 120.9(4) . . . . ? N1 Rh1 N2 C13 26.3(19) . . . . ? N1 Rh1 N3 C15 -125(2) . . . . ? N1 Rh1 C4 C3 9.7(3) . . . . ? N1 Rh1 C4 C5 -110.4(2) . . . . ? N1 Rh1 C4 C8 130.6(2) . . . . ? N1 Rh1 C5 C4 76.5(2) . . . . ? N1 Rh1 C5 C6 -167.5(2) . . . . ? N1 Rh1 C5 C9 -45.3(3) . . . . ? N1 Rh1 C6 C5 20.6(3) . . . . ? N1 Rh1 C6 C7 141.3(2) . . . . ? N1 Rh1 C6 C10 -97.1(4) . . . . ? N1 Rh1 C7 C6 -110.2(3) . . . . ? N1 Rh1 C7 C8 8.1(4) . . . . ? N1 Rh1 C7 C11 127.7(3) . . . . ? N1 Rh1 C8 C4 -58.6(2) . . . . ? N1 Rh1 C8 C7 -176.4(2) . . . . ? N1 Rh1 C8 C12 62.7(3) . . . . ? N1 C1 C2 C3 -77.6(4) . . . . ? C1 C2 C3 C4 60.8(5) . . . . ? N2 Rh1 N1 C1 -165.0(3) . . . . ? N2 Rh1 N3 C15 152(2) . . . . ? N2 Rh1 C4 C3 93.1(3) . . . . ? N2 Rh1 C4 C5 -27.0(3) . . . . ? N2 Rh1 C4 C8 -146.0(2) . . . . ? N2 Rh1 C5 C4 163.0(2) . . . . ? N2 Rh1 C5 C6 -81.0(2) . . . . ? N2 Rh1 C5 C9 41.3(3) . . . . ? N2 Rh1 C6 C5 106.1(2) . . . . ? N2 Rh1 C6 C7 -133.3(2) . . . . ? N2 Rh1 C6 C10 -11.6(3) . . . . ? N2 Rh1 C7 C6 56.5(2) . . . . ? N2 Rh1 C7 C8 174.8(2) . . . . ? N2 Rh1 C7 C11 -65.6(3) . . . . ? N2 Rh1 C8 C4 105.3(4) . . . . ? N2 Rh1 C8 C7 -12.5(5) . . . . ? N2 Rh1 C8 C12 -133.4(4) . . . . ? C2 C3 C4 Rh1 -27.6(5) . . . . ? C2 C3 C4 C5 60.6(5) . . . . ? C2 C3 C4 C8 -116.9(4) . . . . ? N3 Rh1 N1 C1 103.6(3) . . . . ? N3 Rh1 N2 C13 113.5(19) . . . . ? N3 Rh1 C4 C3 -79.9(3) . . . . ? N3 Rh1 C4 C5 159.9(2) . . . . ? N3 Rh1 C4 C8 41.0(3) . . . . ? N3 Rh1 C5 C4 -55.2(5) . . . . ? N3 Rh1 C5 C6 60.8(4) . . . . ? N3 Rh1 C5 C9 -176.9(3) . . . . ? N3 Rh1 C6 C5 -158.11(19) . . . . ? N3 Rh1 C6 C7 -37.5(3) . . . . ? N3 Rh1 C6 C10 84.2(4) . . . . ? N3 Rh1 C7 C6 151.4(2) . . . . ? N3 Rh1 C7 C8 -90.2(2) . . . . ? N3 Rh1 C7 C11 29.4(3) . . . . ? N3 Rh1 C8 C4 -148.3(2) . . . . ? N3 Rh1 C8 C7 93.9(2) . . . . ? N3 Rh1 C8 C12 -27.0(3) . . . . ? C3 C4 C5 Rh1 -117.3(4) . . . . ? C3 C4 C5 C6 179.3(3) . . . . ? C3 C4 C5 C9 7.9(6) . . . . ? C3 C4 C8 Rh1 117.7(4) . . . . ? C3 C4 C8 C7 179.1(3) . . . . ? C3 C4 C8 C12 -2.7(6) . . . . ? C4 Rh1 N1 C1 -23.4(3) . . . . ? C4 Rh1 N2 C13 -61(2) . . . . ? C4 Rh1 N3 C15 -32(2) . . . . ? C4 Rh1 C5 C6 116.0(3) . . . . ? C4 Rh1 C5 C9 -121.8(4) . . . . ? C4 Rh1 C6 C5 -39.2(2) . . . . ? C4 Rh1 C6 C7 81.4(2) . . . . ? C4 Rh1 C6 C10 -156.9(4) . . . . ? C4 Rh1 C7 C6 -80.6(2) . . . . ? C4 Rh1 C7 C8 37.7(2) . . . . ? C4 Rh1 C7 C11 157.3(4) . . . . ? C4 Rh1 C8 C7 -117.8(3) . . . . ? C4 Rh1 C8 C12 121.3(4) . . . . ? C4 C5 C6 Rh1 62.1(2) . . . . ? C4 C5 C6 C7 3.4(4) . . . . ? C4 C5 C6 C10 -178.7(3) . . . . ? C5 Rh1 N1 C1 -62.0(3) . . . . ? C5 Rh1 N2 C13 -78.4(19) . . . . ? C5 Rh1 N3 C15 9(2) . . . . ? C5 Rh1 C4 C3 120.2(4) . . . . ? C5 Rh1 C4 C8 -118.9(3) . . . . ? C5 Rh1 C6 C7 120.6(3) . . . . ? C5 Rh1 C6 C10 -117.7(4) . . . . ? C5 Rh1 C7 C6 -36.8(2) . . . . ? C5 Rh1 C7 C8 81.5(2) . . . . ? C5 Rh1 C7 C11 -158.9(3) . . . . ? C5 Rh1 C8 C4 37.7(2) . . . . ? C5 Rh1 C8 C7 -80.1(2) . . . . ? C5 Rh1 C8 C12 159.0(4) . . . . ? C5 C4 C8 Rh1 -60.2(2) . . . . ? C5 C4 C8 C7 1.3(4) . . . . ? C5 C4 C8 C12 179.5(3) . . . . ? C5 C6 C7 Rh1 57.6(2) . . . . ? C5 C6 C7 C8 -2.6(4) . . . . ? C5 C6 C7 C11 179.4(3) . . . . ? C6 Rh1 N1 C1 -75.4(3) . . . . ? C6 Rh1 N2 C13 -117.5(19) . . . . ? C6 Rh1 N3 C15 54(2) . . . . ? C6 Rh1 C4 C3 159.1(4) . . . . ? C6 Rh1 C4 C5 38.9(2) . . . . ? C6 Rh1 C4 C8 -80.0(2) . . . . ? C6 Rh1 C5 C4 -116.0(3) . . . . ? C6 Rh1 C5 C9 122.2(4) . . . . ? C6 Rh1 C7 C8 118.3(3) . . . . ? C6 Rh1 C7 C11 -122.1(4) . . . . ? C6 Rh1 C8 C4 81.1(2) . . . . ? C6 Rh1 C8 C7 -36.7(2) . . . . ? C6 Rh1 C8 C12 -157.6(4) . . . . ? C6 C7 C8 Rh1 61.7(3) . . . . ? C6 C7 C8 C4 0.8(4) . . . . ? C6 C7 C8 C12 -177.4(3) . . . . ? C7 Rh1 N1 C1 3.4(5) . . . . ? C7 Rh1 N2 C13 -148.5(19) . . . . ? C7 Rh1 N3 C15 32(2) . . . . ? C7 Rh1 C4 C3 -159.0(4) . . . . ? C7 Rh1 C4 C5 80.8(2) . . . . ? C7 Rh1 C4 C8 -38.2(2) . . . . ? C7 Rh1 C5 C4 -80.5(2) . . . . ? C7 Rh1 C5 C6 35.5(2) . . . . ? C7 Rh1 C5 C9 157.7(4) . . . . ? C7 Rh1 C6 C5 -120.6(3) . . . . ? C7 Rh1 C6 C10 121.7(4) . . . . ? C7 Rh1 C8 C4 117.8(3) . . . . ? C7 Rh1 C8 C12 -120.9(4) . . . . ? C8 Rh1 N1 C1 9.2(3) . . . . ? C8 Rh1 N2 C13 -139.4(18) . . . . ? C8 Rh1 N3 C15 -8(2) . . . . ? C8 Rh1 C4 C3 -120.9(4) . . . . ? C8 Rh1 C4 C5 118.9(3) . . . . ? C8 Rh1 C5 C4 -37.1(2) . . . . ? C8 Rh1 C5 C6 78.9(2) . . . . ? C8 Rh1 C5 C9 -158.8(4) . . . . ? C8 Rh1 C6 C5 -82.4(2) . . . . ? C8 Rh1 C6 C7 38.2(2) . . . . ? C8 Rh1 C6 C10 159.9(4) . . . . ? C8 Rh1 C7 C6 -118.3(3) . . . . ? C8 Rh1 C7 C11 119.6(4) . . . . ? C8 C4 C5 Rh1 60.6(2) . . . . ? C8 C4 C5 C6 -2.8(4) . . . . ? C8 C4 C5 C9 -174.3(3) . . . . ? C9 C5 C6 Rh1 -126.4(4) . . . . ? C9 C5 C6 C7 174.9(3) . . . . ? C9 C5 C6 C10 -7.1(6) . . . . ? C10 C6 C7 Rh1 -120.4(4) . . . . ? C10 C6 C7 C8 179.5(4) . . . . ? C10 C6 C7 C11 1.5(6) . . . . ? C11 C7 C8 Rh1 -120.3(4) . . . . ? C11 C7 C8 C4 178.9(3) . . . . ? C11 C7 C8 C12 0.6(6) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -10 0 -7 0.1157 -10.0012 -0.0033 -7.0023 -0.4335 0.1185 -0.8910 -4 14 20 0.1858 -3.9846 14.0127 20.0013 -0.0884 -0.9657 -0.1532 3 -14 -21 0.1021 2.9844 -14.0132 -21.0015 0.0382 0.9865 0.0637 1 22 -12 0.0441 1.0025 21.9941 -11.9987 -0.9410 -0.1542 0.3392 -9 -6 -12 0.1146 -9.0060 -6.0066 -12.0029 -0.3328 0.4192 -0.8831 9 4 13 0.1093 9.0057 4.0071 13.0028 0.4187 -0.4017 0.8602 -8 -16 6 0.1340 -8.0016 -15.9967 5.9974 0.4235 0.1277 -0.8913 7 18 -1 0.0902 7.0049 17.9998 -0.9972 -0.3985 -0.3336 0.8347 7 -1 -22 0.1012 6.9880 -1.0134 -21.9998 -0.2847 0.7443 0.5731 -1 -18 18 0.0959 -0.9982 -17.9904 17.9993 0.9534 -0.1199 -0.2819 10 -7 -4 0.1115 9.9935 -7.0035 -3.9987 0.4002 0.3761 0.7899 -7 -11 18 0.1551 -6.9944 -10.9896 17.9986 0.5699 -0.3403 -0.7251 0 -24 0 0.0964 -0.0090 -24.0013 -0.0019 0.7547 0.5692 -0.2926 -1 24 -1 0.1000 -0.9912 24.0008 -0.9984 -0.8049 -0.5484 0.2030 2 -5 25 0.1389 2.0093 -4.9859 25.0012 0.7875 -0.6101 0.1509 -1 6 -25 0.0754 -1.0091 5.9859 -25.0010 -0.7917 0.5955 -0.0506 0 -8 25 0.1299 0.0086 -7.9859 25.0006 0.8274 -0.5571 -0.0619 10 2 9 0.0984 10.0029 2.0046 9.0026 0.4167 -0.2257 0.9182 0 -23 9 0.0798 -0.0045 -22.9960 8.9986 0.9305 0.2766 -0.2675 _olex2_submission_special_instructions 'No special instructions were received'