Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Jim Thomas' 'Harry Adams' 'Veronica Gonzalez' _publ_contact_author_name 'Jim Thomas' _publ_contact_author_address ; Department of Chemistry University of Sheffield Brook Hill Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_email JAMES.THOMAS@SHEFFIELD.AC.UK _publ_section_title ; A convenient synthetic route to half-sandwich rhodium(III) complexes of the tripodal ligand (tris(3,5-dimethylpyrazolyl)methane. ; #2.CIF data_iaj184m _database_code_depnum_ccdc_archive 'CCDC 244903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 Cl F12 N8 O P2 Rh' _chemical_formula_weight 928.95 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 8.1797(16) _cell_length_b 11.725(2) _cell_length_c 38.021(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.162(4) _cell_angle_gamma 90.00 _cell_volume 3643.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4521 _cell_measurement_theta_min 4.734 _cell_measurement_theta_max 50.610 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7543 _exptl_absorpt_correction_T_max 0.8800 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23217 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8243 _reflns_number_gt 5019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0839P)^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 8243 _refine_ls_number_parameters 464 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1648 _refine_ls_wR_factor_gt 0.1481 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Rh1 Rh 0.10115(5) 0.72838(4) 0.617411(10) 0.02409(13) Uani 1 1 d . . . Cl1 Cl -0.07941(17) 0.84951(12) 0.58753(4) 0.0394(4) Uani 1 1 d . . . N1 N 0.2604(4) 0.6202(3) 0.64427(10) 0.0218(9) Uani 1 1 d . . . N2 N 0.1904(4) 0.5339(4) 0.66228(11) 0.0260(10) Uani 1 1 d . . . N3 N -0.0385(5) 0.7301(4) 0.66122(11) 0.0272(9) Uani 1 1 d . . . N4 N -0.0537(5) 0.6291(4) 0.67842(11) 0.0263(10) Uani 1 1 d . . . N5 N -0.0410(5) 0.5884(4) 0.60304(11) 0.0260(9) Uani 1 1 d . . . N6 N -0.0564(5) 0.5074(4) 0.62842(10) 0.0275(10) Uani 1 1 d . . . N7 N 0.2421(5) 0.7352(4) 0.57501(11) 0.0270(10) Uani 1 1 d . . . N8 N 0.2415(5) 0.8644(4) 0.63036(11) 0.0266(10) Uani 1 1 d . . . C1 C 0.0152(5) 0.5269(5) 0.66318(13) 0.0268(11) Uani 1 1 d . . . H1A H -0.0130 0.4606 0.6783 0.032 Uiso 1 1 calc R . . C2 C 0.4212(6) 0.6023(4) 0.64728(12) 0.0249(11) Uani 1 1 d . . . C3 C 0.4522(6) 0.5065(5) 0.66759(14) 0.0323(13) Uani 1 1 d . . . H3 H 0.5569 0.4765 0.6741 0.039 Uiso 1 1 calc R . . C4 C 0.3046(6) 0.4627(4) 0.67672(13) 0.0280(12) Uani 1 1 d . . . C5 C -0.1251(6) 0.8065(5) 0.67927(14) 0.0327(13) Uani 1 1 d . . . C6 C -0.1938(7) 0.7510(5) 0.70775(15) 0.0380(14) Uani 1 1 d . . . H6 H -0.2610 0.7852 0.7246 0.046 Uiso 1 1 calc R . . C7 C -0.1474(6) 0.6392(5) 0.70709(14) 0.0342(13) Uani 1 1 d . . . C8 C -0.1267(6) 0.5493(5) 0.57451(14) 0.0320(13) Uani 1 1 d . . . C9 C -0.1990(6) 0.4456(5) 0.58262(14) 0.0355(13) Uani 1 1 d . . . H9 H -0.2688 0.4015 0.5674 0.043 Uiso 1 1 calc R . . C10 C -0.1515(6) 0.4189(5) 0.61625(14) 0.0335(13) Uani 1 1 d . . . C11 C 0.2589(6) 0.6526(5) 0.55085(14) 0.0323(13) Uani 1 1 d . . . H11 H 0.2052 0.5817 0.5539 0.039 Uiso 1 1 calc R . . C12 C 0.3520(7) 0.6684(5) 0.52189(15) 0.0396(14) Uani 1 1 d . . . H12 H 0.3601 0.6095 0.5049 0.048 Uiso 1 1 calc R . . C13 C 0.4337(8) 0.7700(6) 0.51756(16) 0.0495(17) Uani 1 1 d . . . H13 H 0.4977 0.7820 0.4975 0.059 Uiso 1 1 calc R . . C14 C 0.4210(7) 0.8553(5) 0.54307(15) 0.0415(15) Uani 1 1 d . . . H14 H 0.4774 0.9256 0.5407 0.050 Uiso 1 1 calc R . . C15 C 0.3250(6) 0.8360(5) 0.57187(14) 0.0341(13) Uani 1 1 d . . . C16 C 0.3222(6) 0.9089(5) 0.60292(14) 0.0314(12) Uani 1 1 d . . . C17 C 0.4110(7) 1.0090(5) 0.60702(16) 0.0416(15) Uani 1 1 d . . . H17 H 0.4627 1.0419 0.5875 0.050 Uiso 1 1 calc R . . C18 C 0.4239(7) 1.0606(5) 0.63972(17) 0.0447(15) Uani 1 1 d . . . H18 H 0.4831 1.1297 0.6429 0.054 Uiso 1 1 calc R . . C19 C 0.3487(7) 1.0095(5) 0.66781(16) 0.0385(14) Uani 1 1 d . . . H19 H 0.3604 1.0418 0.6907 0.046 Uiso 1 1 calc R . . C20 C 0.2566(7) 0.9115(5) 0.66240(14) 0.0343(13) Uani 1 1 d . . . H20 H 0.2038 0.8773 0.6816 0.041 Uiso 1 1 calc R . . C21 C 0.5469(6) 0.6751(5) 0.63053(15) 0.0363(13) Uani 1 1 d . . . H21A H 0.4923 0.7371 0.6174 0.054 Uiso 1 1 calc R . . H21B H 0.6097 0.6286 0.6144 0.054 Uiso 1 1 calc R . . H21C H 0.6209 0.7072 0.6488 0.054 Uiso 1 1 calc R . . C22 C 0.2586(7) 0.3591(5) 0.69700(16) 0.0401(14) Uani 1 1 d . . . H22A H 0.1393 0.3551 0.6982 0.060 Uiso 1 1 calc R . . H22B H 0.3077 0.3635 0.7209 0.060 Uiso 1 1 calc R . . H22C H 0.2988 0.2909 0.6852 0.060 Uiso 1 1 calc R . . C23 C -0.1430(7) 0.9276(5) 0.66999(16) 0.0459(16) Uani 1 1 d . . . H23A H -0.0827 0.9436 0.6487 0.069 Uiso 1 1 calc R . . H23B H -0.0992 0.9747 0.6894 0.069 Uiso 1 1 calc R . . H23C H -0.2591 0.9454 0.6656 0.069 Uiso 1 1 calc R . . C24 C -0.1763(7) 0.5446(6) 0.73230(15) 0.0445(15) Uani 1 1 d . . . H24A H -0.1259 0.4745 0.7238 0.067 Uiso 1 1 calc R . . H24B H -0.2942 0.5328 0.7342 0.067 Uiso 1 1 calc R . . H24C H -0.1277 0.5644 0.7555 0.067 Uiso 1 1 calc R . . C25 C -0.1429(7) 0.6109(5) 0.54026(14) 0.0421(15) Uani 1 1 d . . . H25A H -0.0799 0.6819 0.5417 0.063 Uiso 1 1 calc R . . H25B H -0.2584 0.6285 0.5350 0.063 Uiso 1 1 calc R . . H25C H -0.1012 0.5627 0.5215 0.063 Uiso 1 1 calc R . . C26 C -0.1823(7) 0.3159(5) 0.63829(16) 0.0412(14) Uani 1 1 d . . . H26A H -0.1297 0.3260 0.6617 0.062 Uiso 1 1 calc R . . H26B H -0.1370 0.2483 0.6270 0.062 Uiso 1 1 calc R . . H26C H -0.3004 0.3060 0.6406 0.062 Uiso 1 1 calc R . . P1 P 0.70698(17) 0.19342(13) 0.73915(4) 0.0347(4) Uani 1 1 d . . . F1 F 0.8784(5) 0.2313(4) 0.72537(14) 0.0984(18) Uani 1 1 d . . . F2 F 0.6357(5) 0.3139(3) 0.73044(17) 0.104(2) Uani 1 1 d . . . F3 F 0.7635(6) 0.2264(5) 0.77729(12) 0.1058(19) Uani 1 1 d . . . F4 F 0.6513(6) 0.1567(5) 0.70065(12) 0.1017(17) Uani 1 1 d . . . F5 F 0.5329(5) 0.1525(4) 0.75099(13) 0.0874(15) Uani 1 1 d . . . F6 F 0.7793(6) 0.0705(3) 0.74656(13) 0.0894(15) Uani 1 1 d . . . P2 P 0.69276(19) 0.67653(14) 0.42874(4) 0.0389(4) Uani 1 1 d . . . F7 F 0.8073(5) 0.7404(4) 0.40206(11) 0.0765(13) Uani 1 1 d . . . F8 F 0.8493(4) 0.6359(4) 0.45192(11) 0.0743(13) Uani 1 1 d . . . F9 F 0.7028(8) 0.5634(3) 0.40664(10) 0.106(2) Uani 1 1 d . . . F10 F 0.6843(5) 0.7903(3) 0.45122(10) 0.0556(10) Uani 1 1 d . . . F11 F 0.5379(5) 0.7156(3) 0.40616(12) 0.0716(13) Uani 1 1 d . . . F12 F 0.5803(4) 0.6125(3) 0.45597(10) 0.0550(10) Uani 1 1 d . . . O1S O 0.6911(11) 0.0614(9) 0.5408(3) 0.194(4) Uiso 1 1 d D . . H1SA H 0.6345 0.0838 0.5574 0.291 Uiso 1 1 d R . . C1S C 0.8280(11) 0.0965(9) 0.5444(3) 0.102(3) Uiso 1 1 d D . . H1S1 H 0.8578 0.0701 0.5685 0.122 Uiso 1 1 calc R . . H1S2 H 0.8085 0.1794 0.5470 0.122 Uiso 1 1 calc R . . C2S C 0.991(2) 0.0958(16) 0.5278(5) 0.258(9) Uiso 1 1 d . . . H2S1 H 1.0050 0.0236 0.5153 0.387 Uiso 1 1 calc R . . H2S2 H 1.0776 0.1040 0.5461 0.387 Uiso 1 1 calc R . . H2S3 H 0.9965 0.1593 0.5112 0.387 Uiso 1 1 calc R . . 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 0.0220(2) 0.0291(2) 0.0214(2) 0.00331(19) 0.00412(14) 0.00605(18) Cl1 0.0407(8) 0.0411(8) 0.0362(8) 0.0062(7) -0.0028(6) 0.0161(6) N1 0.022(2) 0.025(2) 0.018(2) 0.0037(18) 0.0034(16) 0.0019(17) N2 0.0170(19) 0.033(2) 0.028(2) 0.006(2) 0.0039(17) 0.0038(18) N3 0.022(2) 0.031(2) 0.028(2) 0.001(2) 0.0040(17) 0.0068(19) N4 0.021(2) 0.037(3) 0.021(2) 0.004(2) 0.0040(17) 0.0046(19) N5 0.023(2) 0.031(2) 0.024(2) 0.008(2) 0.0035(17) 0.0024(18) N6 0.021(2) 0.038(3) 0.024(2) 0.007(2) 0.0050(17) 0.0037(19) N7 0.028(2) 0.032(2) 0.021(2) 0.007(2) 0.0053(17) 0.0057(19) N8 0.031(2) 0.026(2) 0.023(2) 0.0043(19) 0.0061(18) 0.0052(19) C1 0.022(2) 0.036(3) 0.023(3) 0.005(2) 0.002(2) 0.001(2) C2 0.023(2) 0.035(3) 0.017(2) 0.001(2) 0.0045(19) 0.005(2) C3 0.023(3) 0.041(3) 0.033(3) 0.003(3) -0.001(2) 0.013(2) C4 0.027(3) 0.034(3) 0.023(3) 0.005(2) 0.000(2) 0.010(2) C5 0.025(3) 0.044(3) 0.029(3) -0.009(3) -0.002(2) 0.007(2) C6 0.027(3) 0.053(4) 0.035(3) -0.009(3) 0.010(2) 0.002(3) C7 0.021(3) 0.059(4) 0.023(3) 0.000(3) 0.005(2) -0.003(3) C8 0.022(3) 0.046(4) 0.027(3) -0.002(3) 0.002(2) 0.006(2) C9 0.028(3) 0.049(4) 0.029(3) -0.001(3) -0.003(2) -0.002(3) C10 0.024(3) 0.043(3) 0.033(3) 0.004(3) 0.005(2) 0.000(2) C11 0.034(3) 0.036(3) 0.027(3) 0.005(3) 0.001(2) 0.009(2) C12 0.050(4) 0.044(4) 0.026(3) -0.002(3) 0.009(3) 0.010(3) C13 0.062(4) 0.059(4) 0.029(3) 0.012(3) 0.024(3) 0.017(4) C14 0.054(4) 0.035(3) 0.036(3) 0.013(3) 0.014(3) 0.005(3) C15 0.034(3) 0.039(3) 0.031(3) 0.013(3) 0.010(2) 0.009(3) C16 0.035(3) 0.034(3) 0.026(3) 0.010(3) 0.004(2) 0.005(2) C17 0.051(4) 0.033(3) 0.042(4) 0.013(3) 0.014(3) 0.000(3) C18 0.048(4) 0.037(3) 0.049(4) 0.007(3) 0.007(3) -0.007(3) C19 0.040(3) 0.038(3) 0.037(3) 0.002(3) 0.002(3) -0.002(3) C20 0.041(3) 0.036(3) 0.026(3) 0.004(3) 0.007(2) 0.004(3) C21 0.021(3) 0.047(4) 0.041(3) 0.006(3) 0.006(2) 0.000(2) C22 0.038(3) 0.035(3) 0.048(4) 0.016(3) -0.001(3) 0.002(3) C23 0.049(4) 0.045(4) 0.044(4) -0.019(3) 0.006(3) 0.013(3) C24 0.032(3) 0.071(4) 0.032(3) 0.005(3) 0.014(2) -0.004(3) C25 0.039(3) 0.054(4) 0.033(3) 0.001(3) -0.006(3) 0.003(3) C26 0.040(3) 0.042(3) 0.042(4) 0.005(3) 0.001(3) -0.014(3) P1 0.0299(7) 0.0371(8) 0.0369(9) 0.0026(7) -0.0016(6) -0.0003(6) F1 0.035(2) 0.146(4) 0.113(4) 0.073(3) 0.000(2) -0.011(2) F2 0.066(3) 0.038(2) 0.205(6) 0.021(3) -0.039(3) 0.008(2) F3 0.108(4) 0.142(5) 0.065(3) -0.054(3) -0.030(3) 0.035(3) F4 0.106(4) 0.133(4) 0.064(3) -0.018(3) -0.030(3) -0.017(3) F5 0.048(2) 0.113(4) 0.103(4) 0.033(3) 0.019(2) -0.009(2) F6 0.096(3) 0.054(3) 0.121(4) 0.028(3) 0.034(3) 0.029(2) P2 0.0458(9) 0.0417(9) 0.0296(8) -0.0010(7) 0.0049(7) 0.0116(7) F7 0.071(3) 0.102(3) 0.058(3) 0.036(2) 0.030(2) 0.026(2) F8 0.048(2) 0.109(4) 0.066(3) 0.035(3) 0.008(2) 0.027(2) F9 0.236(6) 0.050(3) 0.030(2) -0.008(2) -0.005(3) 0.054(3) F10 0.070(2) 0.038(2) 0.059(2) -0.0126(18) 0.018(2) -0.0131(18) F11 0.064(2) 0.055(3) 0.093(3) 0.023(2) -0.032(2) -0.005(2) F12 0.062(2) 0.043(2) 0.060(2) 0.0069(19) 0.0113(19) -0.0059(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 Rh1 N8 2.015(4) . ? Rh1 N7 2.019(4) . ? Rh1 N3 2.055(4) . ? Rh1 N1 2.062(4) . ? Rh1 N5 2.073(4) . ? Rh1 Cl1 2.3157(13) . ? N1 C2 1.332(6) . ? N1 N2 1.360(5) . ? N2 C4 1.353(6) . ? N2 C1 1.438(6) . ? N3 C5 1.346(6) . ? N3 N4 1.361(6) . ? N4 C7 1.361(6) . ? N4 C1 1.453(6) . ? N5 C8 1.349(6) . ? N5 N6 1.363(5) . ? N6 C10 1.367(7) . ? N6 C1 1.443(6) . ? N7 C11 1.346(7) . ? N7 C15 1.369(7) . ? N8 C20 1.339(7) . ? N8 C16 1.360(6) . ? C1 H1A 1.0000 . ? C2 C3 1.380(7) . ? C2 C21 1.497(7) . ? C3 C4 1.369(7) . ? C3 H3 0.9500 . ? C4 C22 1.494(7) . ? C5 C6 1.399(8) . ? C5 C23 1.470(8) . ? C6 C7 1.365(8) . ? C6 H6 0.9500 . ? C7 C24 1.491(8) . ? C8 C9 1.392(8) . ? C8 C25 1.490(7) . ? C9 C10 1.359(7) . ? C9 H9 0.9500 . ? C10 C26 1.496(7) . ? C11 C12 1.374(7) . ? C11 H11 0.9500 . ? C12 C13 1.379(9) . ? C12 H12 0.9500 . ? C13 C14 1.400(8) . ? C13 H13 0.9500 . ? C14 C15 1.390(8) . ? C14 H14 0.9500 . ? C15 C16 1.459(8) . ? C16 C17 1.385(8) . ? C17 C18 1.383(8) . ? C17 H17 0.9500 . ? C18 C19 1.388(8) . ? C18 H18 0.9500 . ? C19 C20 1.386(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? P1 F3 1.554(4) . ? P1 F2 1.560(4) . ? P1 F4 1.576(5) . ? P1 F1 1.579(4) . ? P1 F6 1.580(4) . ? P1 F5 1.584(4) . ? P2 F11 1.571(4) . ? P2 F9 1.574(4) . ? P2 F10 1.588(4) . ? P2 F7 1.594(4) . ? P2 F12 1.598(4) . ? P2 F8 1.600(4) . ? O1S C1S 1.196(2) . ? O1S H1SA 0.8400 . ? C1S C2S 1.495(18) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? 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 N8 Rh1 N7 80.00(17) . . ? N8 Rh1 N3 97.07(17) . . ? N7 Rh1 N3 176.94(18) . . ? N8 Rh1 N1 91.29(16) . . ? N7 Rh1 N1 92.90(16) . . ? N3 Rh1 N1 88.00(16) . . ? N8 Rh1 N5 178.77(17) . . ? N7 Rh1 N5 98.78(17) . . ? N3 Rh1 N5 84.16(17) . . ? N1 Rh1 N5 88.91(15) . . ? N8 Rh1 Cl1 88.93(12) . . ? N7 Rh1 Cl1 87.53(12) . . ? N3 Rh1 Cl1 91.58(12) . . ? N1 Rh1 Cl1 179.55(12) . . ? N5 Rh1 Cl1 90.88(11) . . ? C2 N1 N2 105.8(4) . . ? C2 N1 Rh1 138.0(3) . . ? N2 N1 Rh1 115.9(3) . . ? C4 N2 N1 111.4(4) . . ? C4 N2 C1 129.0(4) . . ? N1 N2 C1 119.6(4) . . ? C5 N3 N4 106.0(4) . . ? C5 N3 Rh1 137.7(4) . . ? N4 N3 Rh1 116.4(3) . . ? N3 N4 C7 111.9(4) . . ? N3 N4 C1 118.8(4) . . ? C7 N4 C1 129.0(5) . . ? C8 N5 N6 105.9(4) . . ? C8 N5 Rh1 138.6(4) . . ? N6 N5 Rh1 115.5(3) . . ? N5 N6 C10 110.8(4) . . ? N5 N6 C1 119.5(4) . . ? C10 N6 C1 129.5(4) . . ? C11 N7 C15 119.9(5) . . ? C11 N7 Rh1 126.3(4) . . ? C15 N7 Rh1 113.8(3) . . ? C20 N8 C16 120.6(5) . . ? C20 N8 Rh1 125.5(4) . . ? C16 N8 Rh1 113.9(3) . . ? N2 C1 N6 110.9(4) . . ? N2 C1 N4 111.4(4) . . ? N6 C1 N4 110.2(4) . . ? N2 C1 H1A 108.1 . . ? N6 C1 H1A 108.1 . . ? N4 C1 H1A 108.1 . . ? N1 C2 C3 109.6(4) . . ? N1 C2 C21 124.4(4) . . ? C3 C2 C21 126.0(4) . . ? C4 C3 C2 107.6(4) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? N2 C4 C3 105.5(4) . . ? N2 C4 C22 121.8(5) . . ? C3 C4 C22 132.6(5) . . ? N3 C5 C6 108.7(5) . . ? N3 C5 C23 124.8(5) . . ? C6 C5 C23 126.6(5) . . ? C7 C6 C5 108.2(5) . . ? C7 C6 H6 125.9 . . ? C5 C6 H6 125.9 . . ? N4 C7 C6 105.3(5) . . ? N4 C7 C24 123.9(5) . . ? C6 C7 C24 130.7(5) . . ? N5 C8 C9 109.3(5) . . ? N5 C8 C25 124.4(5) . . ? C9 C8 C25 126.3(5) . . ? C10 C9 C8 107.5(5) . . ? C10 C9 H9 126.3 . . ? C8 C9 H9 126.3 . . ? C9 C10 N6 106.4(5) . . ? C9 C10 C26 131.6(5) . . ? N6 C10 C26 121.9(5) . . ? N7 C11 C12 121.6(5) . . ? N7 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C13 119.8(6) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 119.1(6) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 119.2(6) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N7 C15 C14 120.4(5) . . ? N7 C15 C16 114.4(5) . . ? C14 C15 C16 124.6(5) . . ? N8 C16 C17 120.4(5) . . ? N8 C16 C15 114.8(5) . . ? C17 C16 C15 124.3(5) . . ? C18 C17 C16 119.6(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 118.8(6) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C20 C19 C18 119.8(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? N8 C20 C19 120.6(5) . . ? N8 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C4 C22 H22A 109.5 . . ? C4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C5 C23 H23A 109.5 . . ? C5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C7 C24 H24A 109.5 . . ? C7 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C7 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 C25 H25A 109.5 . . ? C8 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C8 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C10 C26 H26A 109.5 . . ? C10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F3 P1 F2 93.9(3) . . ? F3 P1 F4 178.5(3) . . ? F2 P1 F4 87.6(3) . . ? F3 P1 F1 90.2(3) . . ? F2 P1 F1 90.2(3) . . ? F4 P1 F1 89.9(3) . . ? F3 P1 F6 87.9(3) . . ? F2 P1 F6 178.0(3) . . ? F4 P1 F6 90.6(3) . . ? F1 P1 F6 89.1(3) . . ? F3 P1 F5 92.8(3) . . ? F2 P1 F5 90.1(3) . . ? F4 P1 F5 87.1(3) . . ? F1 P1 F5 177.0(3) . . ? F6 P1 F5 90.4(3) . . ? F11 P2 F9 90.7(3) . . ? F11 P2 F10 89.9(2) . . ? F9 P2 F10 179.4(3) . . ? F11 P2 F7 89.8(2) . . ? F9 P2 F7 90.7(3) . . ? F10 P2 F7 89.2(2) . . ? F11 P2 F12 91.1(2) . . ? F9 P2 F12 89.6(3) . . ? F10 P2 F12 90.5(2) . . ? F7 P2 F12 179.0(2) . . ? F11 P2 F8 179.4(3) . . ? F9 P2 F8 89.2(3) . . ? F10 P2 F8 90.2(2) . . ? F7 P2 F8 90.7(2) . . ? F12 P2 F8 88.3(2) . . ? C1S O1S H1SA 110.1 . . ? O1S C1S C2S 142.5(13) . . ? O1S C1S H1S1 101.3 . . ? C2S C1S H1S1 101.3 . . ? O1S C1S H1S2 101.3 . . ? C2S C1S H1S2 101.3 . . ? H1S1 C1S H1S2 104.6 . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? 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 N8 Rh1 N1 C2 -46.1(5) . . . . ? N7 Rh1 N1 C2 34.0(5) . . . . ? N3 Rh1 N1 C2 -143.1(5) . . . . ? N5 Rh1 N1 C2 132.7(5) . . . . ? Cl1 Rh1 N1 C2 -165(100) . . . . ? N8 Rh1 N1 N2 141.4(3) . . . . ? N7 Rh1 N1 N2 -138.6(3) . . . . ? N3 Rh1 N1 N2 44.3(3) . . . . ? N5 Rh1 N1 N2 -39.8(3) . . . . ? Cl1 Rh1 N1 N2 22(18) . . . . ? C2 N1 N2 C4 0.4(5) . . . . ? Rh1 N1 N2 C4 175.3(3) . . . . ? C2 N1 N2 C1 -178.2(4) . . . . ? Rh1 N1 N2 C1 -3.4(5) . . . . ? N8 Rh1 N3 C5 49.3(5) . . . . ? N7 Rh1 N3 C5 33(3) . . . . ? N1 Rh1 N3 C5 140.3(5) . . . . ? N5 Rh1 N3 C5 -130.6(5) . . . . ? Cl1 Rh1 N3 C5 -39.9(5) . . . . ? N8 Rh1 N3 N4 -130.6(3) . . . . ? N7 Rh1 N3 N4 -147(3) . . . . ? N1 Rh1 N3 N4 -39.5(3) . . . . ? N5 Rh1 N3 N4 49.6(3) . . . . ? Cl1 Rh1 N3 N4 140.3(3) . . . . ? C5 N3 N4 C7 -0.2(5) . . . . ? Rh1 N3 N4 C7 179.6(3) . . . . ? C5 N3 N4 C1 174.5(4) . . . . ? Rh1 N3 N4 C1 -5.7(5) . . . . ? N8 Rh1 N5 C8 -40(8) . . . . ? N7 Rh1 N5 C8 -46.8(5) . . . . ? N3 Rh1 N5 C8 132.3(5) . . . . ? N1 Rh1 N5 C8 -139.6(5) . . . . ? Cl1 Rh1 N5 C8 40.8(5) . . . . ? N8 Rh1 N5 N6 139(7) . . . . ? N7 Rh1 N5 N6 132.1(3) . . . . ? N3 Rh1 N5 N6 -48.7(3) . . . . ? N1 Rh1 N5 N6 39.4(3) . . . . ? Cl1 Rh1 N5 N6 -140.2(3) . . . . ? C8 N5 N6 C10 -0.5(5) . . . . ? Rh1 N5 N6 C10 -179.7(3) . . . . ? C8 N5 N6 C1 -176.7(4) . . . . ? Rh1 N5 N6 C1 4.1(5) . . . . ? N8 Rh1 N7 C11 165.4(4) . . . . ? N3 Rh1 N7 C11 -178(100) . . . . ? N1 Rh1 N7 C11 74.6(4) . . . . ? N5 Rh1 N7 C11 -14.8(4) . . . . ? Cl1 Rh1 N7 C11 -105.3(4) . . . . ? N8 Rh1 N7 C15 -15.0(3) . . . . ? N3 Rh1 N7 C15 1(3) . . . . ? N1 Rh1 N7 C15 -105.8(3) . . . . ? N5 Rh1 N7 C15 164.9(3) . . . . ? Cl1 Rh1 N7 C15 74.4(3) . . . . ? N7 Rh1 N8 C20 -165.2(4) . . . . ? N3 Rh1 N8 C20 15.7(4) . . . . ? N1 Rh1 N8 C20 -72.5(4) . . . . ? N5 Rh1 N8 C20 -172(7) . . . . ? Cl1 Rh1 N8 C20 107.1(4) . . . . ? N7 Rh1 N8 C16 15.9(3) . . . . ? N3 Rh1 N8 C16 -163.3(3) . . . . ? N1 Rh1 N8 C16 108.6(3) . . . . ? N5 Rh1 N8 C16 9(8) . . . . ? Cl1 Rh1 N8 C16 -71.8(3) . . . . ? C4 N2 C1 N6 -114.3(6) . . . . ? N1 N2 C1 N6 64.0(6) . . . . ? C4 N2 C1 N4 122.5(5) . . . . ? N1 N2 C1 N4 -59.2(6) . . . . ? N5 N6 C1 N2 -64.4(6) . . . . ? C10 N6 C1 N2 120.2(5) . . . . ? N5 N6 C1 N4 59.5(5) . . . . ? C10 N6 C1 N4 -115.9(5) . . . . ? N3 N4 C1 N2 64.9(5) . . . . ? C7 N4 C1 N2 -121.4(5) . . . . ? N3 N4 C1 N6 -58.6(5) . . . . ? C7 N4 C1 N6 115.0(5) . . . . ? N2 N1 C2 C3 -1.1(5) . . . . ? Rh1 N1 C2 C3 -174.1(4) . . . . ? N2 N1 C2 C21 178.1(5) . . . . ? Rh1 N1 C2 C21 5.1(8) . . . . ? N1 C2 C3 C4 1.3(6) . . . . ? C21 C2 C3 C4 -177.9(5) . . . . ? N1 N2 C4 C3 0.4(6) . . . . ? C1 N2 C4 C3 178.8(5) . . . . ? N1 N2 C4 C22 -178.2(5) . . . . ? C1 N2 C4 C22 0.2(8) . . . . ? C2 C3 C4 N2 -1.0(6) . . . . ? C2 C3 C4 C22 177.4(6) . . . . ? N4 N3 C5 C6 0.0(5) . . . . ? Rh1 N3 C5 C6 -179.9(4) . . . . ? N4 N3 C5 C23 -179.9(5) . . . . ? Rh1 N3 C5 C23 0.2(8) . . . . ? N3 C5 C6 C7 0.3(6) . . . . ? C23 C5 C6 C7 -179.8(5) . . . . ? N3 N4 C7 C6 0.4(5) . . . . ? C1 N4 C7 C6 -173.6(4) . . . . ? N3 N4 C7 C24 -175.8(4) . . . . ? C1 N4 C7 C24 10.2(8) . . . . ? C5 C6 C7 N4 -0.4(6) . . . . ? C5 C6 C7 C24 175.5(5) . . . . ? N6 N5 C8 C9 1.7(5) . . . . ? Rh1 N5 C8 C9 -179.3(4) . . . . ? N6 N5 C8 C25 -179.7(5) . . . . ? Rh1 N5 C8 C25 -0.8(8) . . . . ? N5 C8 C9 C10 -2.3(6) . . . . ? C25 C8 C9 C10 179.2(5) . . . . ? C8 C9 C10 N6 1.9(6) . . . . ? C8 C9 C10 C26 -176.1(6) . . . . ? N5 N6 C10 C9 -0.9(6) . . . . ? C1 N6 C10 C9 174.8(5) . . . . ? N5 N6 C10 C26 177.3(5) . . . . ? C1 N6 C10 C26 -7.0(8) . . . . ? C15 N7 C11 C12 -3.0(7) . . . . ? Rh1 N7 C11 C12 176.6(4) . . . . ? N7 C11 C12 C13 1.4(8) . . . . ? C11 C12 C13 C14 0.5(9) . . . . ? C12 C13 C14 C15 -0.8(9) . . . . ? C11 N7 C15 C14 2.7(7) . . . . ? Rh1 N7 C15 C14 -177.0(4) . . . . ? C11 N7 C15 C16 -168.6(4) . . . . ? Rh1 N7 C15 C16 11.7(5) . . . . ? C13 C14 C15 N7 -0.8(8) . . . . ? C13 C14 C15 C16 169.5(5) . . . . ? C20 N8 C16 C17 -5.1(7) . . . . ? Rh1 N8 C16 C17 173.9(4) . . . . ? C20 N8 C16 C15 166.8(5) . . . . ? Rh1 N8 C16 C15 -14.2(5) . . . . ? N7 C15 C16 N8 1.6(6) . . . . ? C14 C15 C16 N8 -169.3(5) . . . . ? N7 C15 C16 C17 173.2(5) . . . . ? C14 C15 C16 C17 2.3(8) . . . . ? N8 C16 C17 C18 3.1(8) . . . . ? C15 C16 C17 C18 -168.0(5) . . . . ? C16 C17 C18 C19 0.9(9) . . . . ? C17 C18 C19 C20 -2.9(9) . . . . ? C16 N8 C20 C19 3.0(7) . . . . ? Rh1 N8 C20 C19 -175.9(4) . . . . ? C18 C19 C20 N8 1.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.341 _refine_diff_density_min -0.936 _refine_diff_density_rms 0.120 #3.CIF data_iaj177m _database_code_depnum_ccdc_archive 'CCDC 244904' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 Cl F12 N8 P2 Rh' _chemical_formula_weight 906.90 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 8.8314(13) _cell_length_b 11.1993(17) _cell_length_c 33.990(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.057(3) _cell_angle_gamma 90.00 _cell_volume 3359.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7276 _cell_measurement_theta_min 4.357 _cell_measurement_theta_max 54.997 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8099 _exptl_absorpt_correction_T_max 0.9255 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37573 _diffrn_reflns_av_R_equivalents 0.1258 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.62 _reflns_number_total 7759 _reflns_number_gt 5252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0687P)^2^+14.7424P] 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 7759 _refine_ls_number_parameters 472 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1753 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Rh1 Rh 0.32182(5) 0.37226(4) 0.602999(12) 0.02161(14) Uani 1 1 d . . . Cl1 Cl 0.41107(17) 0.51177(13) 0.55900(4) 0.0284(3) Uani 1 1 d . . . N1 N 0.4873(6) 0.4120(4) 0.64495(13) 0.0247(10) Uani 1 1 d . . . N2 N 0.5473(6) 0.3170(4) 0.66546(14) 0.0258(11) Uani 1 1 d . . . N3 N 0.4715(6) 0.2458(4) 0.58404(13) 0.0240(10) Uani 1 1 d . . . N4 N 0.5403(6) 0.1764(4) 0.61287(13) 0.0249(11) Uani 1 1 d . . . N5 N 0.2410(6) 0.2467(4) 0.64115(13) 0.0232(10) Uani 1 1 d . . . N6 N 0.3466(6) 0.1766(4) 0.65969(14) 0.0260(11) Uani 1 1 d . . . N7 N 0.1518(6) 0.3376(5) 0.56309(14) 0.0264(11) Uani 1 1 d . . . N8 N 0.1708(5) 0.4955(4) 0.62077(14) 0.0241(10) Uani 1 1 d . . . C1 C 0.5033(7) 0.1975(5) 0.65375(16) 0.0249(12) Uani 1 1 d . . . H1 H 0.5631 0.1399 0.6706 0.030 Uiso 1 1 calc R . . C2 C 0.5557(7) 0.5104(6) 0.65988(17) 0.0273(13) Uani 1 1 d . . . C3 C 0.6589(7) 0.4759(6) 0.68996(17) 0.0299(14) Uani 1 1 d . . . H3 H 0.7221 0.5277 0.7054 0.036 Uiso 1 1 calc R . . C4 C 0.6525(7) 0.3546(6) 0.69317(17) 0.0285(13) Uani 1 1 d . . . C5 C 0.5274(7) 0.2081(5) 0.55000(16) 0.0253(12) Uani 1 1 d . . . C6 C 0.6286(7) 0.1143(6) 0.55730(17) 0.0302(13) Uani 1 1 d . . . H6 H 0.6835 0.0721 0.5382 0.036 Uiso 1 1 calc R . . C7 C 0.6342(7) 0.0941(5) 0.59756(17) 0.0257(13) Uani 1 1 d . . . C8 C 0.1052(8) 0.2043(6) 0.65066(18) 0.0306(14) Uani 1 1 d . . . C9 C 0.1287(8) 0.1057(6) 0.67552(18) 0.0344(15) Uani 1 1 d . . . H9 H 0.0519 0.0582 0.6866 0.041 Uiso 1 1 calc R . . C10 C 0.2789(8) 0.0897(6) 0.68100(17) 0.0310(14) Uani 1 1 d . . . C11 C 0.1314(7) 0.2441(6) 0.53907(18) 0.0312(14) Uani 1 1 d . . . H11 H 0.2015 0.1798 0.5407 0.037 Uiso 1 1 calc R . . C12 C 0.0099(8) 0.2383(7) 0.5117(2) 0.0390(16) Uani 1 1 d . . . H12 H 0.0004 0.1720 0.4943 0.047 Uiso 1 1 calc R . . C13 C -0.0958(8) 0.3282(7) 0.50974(19) 0.0402(17) Uani 1 1 d . . . H13 H -0.1767 0.3256 0.4906 0.048 Uiso 1 1 calc R . . C14 C -0.0832(7) 0.4247(6) 0.53660(17) 0.0307(14) Uani 1 1 d . . . C15 C -0.1931(8) 0.5167(7) 0.5398(2) 0.0399(17) Uani 1 1 d . . . H15 H -0.2754 0.5209 0.5211 0.048 Uiso 1 1 calc R . . C16 C -0.1824(7) 0.5982(6) 0.5690(2) 0.0363(15) Uani 1 1 d . . . H16 H -0.2570 0.6591 0.5702 0.044 Uiso 1 1 calc R . . C17 C -0.0615(7) 0.5954(6) 0.59836(19) 0.0317(14) Uani 1 1 d . . . C18 C -0.0515(8) 0.6652(6) 0.6327(2) 0.0364(15) Uani 1 1 d . . . H18 H -0.1235 0.7267 0.6366 0.044 Uiso 1 1 calc R . . C19 C 0.0612(7) 0.6450(6) 0.6607(2) 0.0337(14) Uani 1 1 d . . . H19 H 0.0653 0.6902 0.6843 0.040 Uiso 1 1 calc R . . C20 C 0.1699(7) 0.5574(6) 0.65414(18) 0.0294(13) Uani 1 1 d . . . H20 H 0.2453 0.5416 0.6741 0.035 Uiso 1 1 calc R . . C21 C 0.0537(7) 0.5113(6) 0.59390(18) 0.0270(13) Uani 1 1 d . . . C22 C 0.0434(6) 0.4262(6) 0.56258(17) 0.0249(12) Uani 1 1 d . . . C23 C 0.5191(8) 0.6347(6) 0.64635(19) 0.0351(14) Uani 1 1 d . . . H23A H 0.4561 0.6314 0.6220 0.053 Uiso 1 1 calc R . . H23B H 0.6132 0.6776 0.6414 0.053 Uiso 1 1 calc R . . H23C H 0.4640 0.6765 0.6668 0.053 Uiso 1 1 calc R . . C24 C 0.7277(8) 0.2705(7) 0.72191(18) 0.0375(16) Uani 1 1 d . . . H24A H 0.6577 0.2512 0.7427 0.056 Uiso 1 1 calc R . . H24B H 0.8189 0.3081 0.7336 0.056 Uiso 1 1 calc R . . H24C H 0.7558 0.1971 0.7083 0.056 Uiso 1 1 calc R . . C25 C 0.4827(8) 0.2574(6) 0.51051(17) 0.0337(15) Uani 1 1 d . . . H25A H 0.3944 0.3095 0.5128 0.051 Uiso 1 1 calc R . . H25B H 0.4573 0.1916 0.4924 0.051 Uiso 1 1 calc R . . H25C H 0.5672 0.3034 0.5003 0.051 Uiso 1 1 calc R . . C26 C 0.7147(8) -0.0001(6) 0.62122(19) 0.0347(15) Uani 1 1 d . . . H26A H 0.7592 0.0353 0.6453 0.052 Uiso 1 1 calc R . . H26B H 0.7952 -0.0349 0.6058 0.052 Uiso 1 1 calc R . . H26C H 0.6427 -0.0627 0.6281 0.052 Uiso 1 1 calc R . . C27 C -0.0406(8) 0.2564(7) 0.6369(2) 0.0401(16) Uani 1 1 d . . . H27A H -0.0413 0.3420 0.6428 0.060 Uiso 1 1 calc R . . H27B H -0.1235 0.2171 0.6502 0.060 Uiso 1 1 calc R . . H27C H -0.0538 0.2446 0.6084 0.060 Uiso 1 1 calc R . . C28 C 0.3683(9) -0.0009(7) 0.7035(2) 0.0431(17) Uani 1 1 d . . . H28A H 0.4417 -0.0378 0.6863 0.065 Uiso 1 1 calc R . . H28B H 0.3001 -0.0623 0.7132 0.065 Uiso 1 1 calc R . . H28C H 0.4222 0.0375 0.7258 0.065 Uiso 1 1 calc R . . P1 P 0.2385(2) 0.89715(16) 0.58131(5) 0.0349(4) Uani 1 1 d . . . F1 F 0.2401(8) 0.8670(4) 0.62658(13) 0.0789(18) Uani 1 1 d . . . F2 F 0.0665(6) 0.9286(6) 0.58167(19) 0.0836(17) Uani 1 1 d . . . F3 F 0.2832(6) 1.0325(4) 0.59077(12) 0.0507(11) Uani 1 1 d . . . F4 F 0.2401(6) 0.9274(4) 0.53505(11) 0.0579(13) Uani 1 1 d . . . F5 F 0.4138(6) 0.8649(5) 0.58023(17) 0.0732(15) Uani 1 1 d . . . F6 F 0.1985(6) 0.7620(4) 0.57144(13) 0.0596(13) Uani 1 1 d . . . P2 P 0.2040(2) 0.35840(16) 0.76252(5) 0.0352(4) Uani 1 1 d D . . F7 F 0.3048(17) 0.3544(14) 0.7258(4) 0.062(3) Uiso 0.361(11) 1 d PDU A 1 F7' F 0.3523(10) 0.3209(9) 0.7407(3) 0.070(2) Uiso 0.639(11) 1 d PDU A 2 F8 F 0.0680(19) 0.4022(17) 0.7339(5) 0.085(4) Uiso 0.361(11) 1 d PDU A 1 F8' F 0.1162(10) 0.3724(8) 0.7210(2) 0.065(2) Uiso 0.639(11) 1 d PDU A 2 F9 F 0.103(2) 0.3759(15) 0.8002(5) 0.074(3) Uiso 0.361(11) 1 d PDU A 1 F9' F 0.0497(10) 0.3835(8) 0.7843(3) 0.066(2) Uiso 0.639(11) 1 d PDU A 2 F10 F 0.3415(18) 0.3349(15) 0.7932(5) 0.072(4) Uiso 0.361(11) 1 d PDU A 1 F10' F 0.2801(13) 0.3330(9) 0.8043(3) 0.076(2) Uiso 0.639(11) 1 d PDU A 2 F11 F 0.2525(7) 0.4934(4) 0.76573(19) 0.0875(19) Uani 1 1 d D A . F12 F 0.1530(6) 0.2223(4) 0.76104(15) 0.0673(14) Uani 1 1 d D A . 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 0.0258(2) 0.0197(2) 0.0195(2) -0.00122(18) 0.00181(16) 0.00031(19) Cl1 0.0317(8) 0.0265(8) 0.0271(7) 0.0056(6) 0.0026(6) -0.0009(6) N1 0.030(3) 0.024(3) 0.020(2) 0.0012(19) 0.000(2) 0.002(2) N2 0.034(3) 0.022(3) 0.022(2) -0.001(2) -0.005(2) 0.000(2) N3 0.033(3) 0.021(3) 0.019(2) 0.0012(19) -0.0002(19) 0.004(2) N4 0.037(3) 0.019(2) 0.019(2) 0.0012(19) 0.001(2) 0.005(2) N5 0.031(3) 0.020(2) 0.019(2) -0.0004(19) 0.0017(19) -0.003(2) N6 0.038(3) 0.019(2) 0.022(2) -0.0034(19) 0.004(2) -0.003(2) N7 0.027(3) 0.026(3) 0.027(3) -0.004(2) 0.004(2) -0.003(2) N8 0.027(3) 0.023(3) 0.022(2) 0.0011(19) 0.001(2) -0.003(2) C1 0.033(3) 0.024(3) 0.018(3) 0.001(2) 0.001(2) 0.004(2) C2 0.024(3) 0.033(3) 0.025(3) -0.004(2) 0.004(2) -0.002(3) C3 0.034(3) 0.031(3) 0.025(3) -0.001(3) 0.005(3) -0.004(3) C4 0.033(3) 0.032(4) 0.020(3) -0.002(2) 0.001(2) -0.001(3) C5 0.032(3) 0.023(3) 0.021(3) 0.000(2) 0.007(2) 0.001(2) C6 0.035(3) 0.032(4) 0.024(3) -0.002(3) 0.007(2) 0.001(3) C7 0.029(3) 0.021(3) 0.028(3) 0.000(2) 0.006(2) 0.002(2) C8 0.041(4) 0.025(3) 0.026(3) -0.007(2) 0.009(3) -0.007(3) C9 0.050(4) 0.027(4) 0.027(3) -0.003(3) 0.010(3) -0.014(3) C10 0.049(4) 0.024(3) 0.020(3) 0.000(2) 0.004(3) -0.007(3) C11 0.031(3) 0.036(4) 0.027(3) -0.009(3) 0.001(3) -0.002(3) C12 0.034(4) 0.048(4) 0.036(4) -0.017(3) 0.001(3) -0.008(3) C13 0.031(4) 0.059(5) 0.029(3) -0.009(3) -0.005(3) -0.005(3) C14 0.030(3) 0.039(4) 0.023(3) 0.000(3) 0.001(2) -0.003(3) C15 0.028(3) 0.058(5) 0.033(4) 0.004(3) 0.000(3) 0.006(3) C16 0.026(3) 0.037(4) 0.045(4) 0.002(3) 0.003(3) 0.010(3) C17 0.031(3) 0.029(3) 0.036(3) 0.004(3) 0.009(3) 0.004(3) C18 0.035(4) 0.027(3) 0.049(4) -0.001(3) 0.011(3) 0.004(3) C19 0.034(3) 0.029(4) 0.038(3) -0.010(3) 0.008(3) -0.001(3) C20 0.030(3) 0.031(3) 0.028(3) -0.005(3) 0.006(3) -0.002(3) C21 0.023(3) 0.027(3) 0.030(3) 0.000(2) 0.002(2) 0.000(2) C22 0.019(3) 0.030(3) 0.025(3) 0.003(2) 0.003(2) -0.004(2) C23 0.042(4) 0.025(3) 0.038(3) -0.004(3) 0.001(3) -0.007(3) C24 0.042(4) 0.046(4) 0.025(3) -0.001(3) -0.007(3) 0.003(3) C25 0.043(4) 0.038(4) 0.020(3) 0.002(3) 0.006(3) 0.007(3) C26 0.040(4) 0.028(3) 0.035(3) -0.001(3) 0.001(3) 0.003(3) C27 0.037(4) 0.040(4) 0.045(4) 0.001(3) 0.013(3) -0.010(3) C28 0.062(5) 0.038(4) 0.029(3) 0.011(3) 0.000(3) -0.004(4) P1 0.0500(11) 0.0285(9) 0.0261(8) -0.0059(7) 0.0024(7) -0.0079(8) F1 0.162(6) 0.044(3) 0.031(2) -0.003(2) 0.011(3) -0.021(3) F2 0.050(3) 0.085(4) 0.117(5) -0.006(4) 0.022(3) 0.006(3) F3 0.084(3) 0.030(2) 0.038(2) -0.0055(17) 0.006(2) -0.016(2) F4 0.091(4) 0.057(3) 0.026(2) -0.0031(19) -0.001(2) -0.014(3) F5 0.057(3) 0.064(4) 0.098(4) -0.001(3) -0.009(3) 0.004(3) F6 0.097(4) 0.030(2) 0.052(3) -0.013(2) 0.008(2) -0.018(2) P2 0.0448(10) 0.0328(10) 0.0281(8) -0.0055(7) 0.0010(7) -0.0018(8) F11 0.113(5) 0.035(3) 0.115(5) -0.015(3) 0.007(4) -0.018(3) F12 0.097(4) 0.041(3) 0.064(3) -0.006(2) 0.020(3) -0.017(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 Rh1 N7 2.025(5) . ? Rh1 N8 2.026(5) . ? Rh1 N1 2.054(5) . ? Rh1 N3 2.056(5) . ? Rh1 N5 2.058(5) . ? Rh1 Cl1 2.3202(15) . ? N1 C2 1.347(8) . ? N1 N2 1.368(7) . ? N2 C4 1.366(8) . ? N2 C1 1.446(8) . ? N3 C5 1.342(7) . ? N3 N4 1.376(6) . ? N4 C7 1.355(8) . ? N4 C1 1.458(7) . ? N5 C8 1.340(8) . ? N5 N6 1.357(7) . ? N6 C10 1.364(8) . ? N6 C1 1.425(8) . ? N7 C11 1.336(8) . ? N7 C22 1.378(8) . ? N8 C20 1.330(7) . ? N8 C21 1.366(8) . ? C2 C3 1.399(9) . ? C2 C23 1.498(9) . ? C3 C4 1.364(9) . ? C4 C24 1.495(9) . ? C5 C6 1.396(9) . ? C5 C25 1.491(8) . ? C6 C7 1.386(8) . ? C7 C26 1.492(8) . ? C8 C9 1.402(9) . ? C8 C27 1.474(10) . ? C9 C10 1.345(10) . ? C10 C28 1.480(9) . ? C11 C12 1.398(9) . ? C12 C13 1.373(10) . ? C13 C14 1.417(9) . ? C14 C22 1.400(8) . ? C14 C15 1.423(9) . ? C15 C16 1.349(10) . ? C16 C17 1.436(9) . ? C17 C21 1.399(8) . ? C17 C18 1.405(9) . ? C18 C19 1.370(10) . ? C19 C20 1.396(9) . ? C21 C22 1.429(8) . ? P1 F2 1.559(6) . ? P1 F1 1.575(5) . ? P1 F6 1.587(4) . ? P1 F5 1.591(6) . ? P1 F3 1.597(4) . ? P1 F4 1.609(4) . ? P2 F7 1.561(11) . ? P2 F11 1.574(5) . ? P2 F10' 1.576(8) . ? P2 F7' 1.585(8) . ? P2 F12 1.590(5) . ? P2 F8' 1.592(7) . ? P2 F10 1.594(11) . ? P2 F8 1.595(12) . ? P2 F9' 1.598(8) . ? P2 F9 1.599(11) . ? 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 N7 Rh1 N8 81.38(19) . . ? N7 Rh1 N1 177.3(2) . . ? N8 Rh1 N1 96.02(19) . . ? N7 Rh1 N3 97.33(19) . . ? N8 Rh1 N3 178.7(2) . . ? N1 Rh1 N3 85.26(19) . . ? N7 Rh1 N5 91.5(2) . . ? N8 Rh1 N5 91.76(19) . . ? N1 Rh1 N5 87.99(19) . . ? N3 Rh1 N5 88.18(19) . . ? N7 Rh1 Cl1 87.61(15) . . ? N8 Rh1 Cl1 88.63(14) . . ? N1 Rh1 Cl1 92.97(14) . . ? N3 Rh1 Cl1 91.41(14) . . ? N5 Rh1 Cl1 178.92(13) . . ? C2 N1 N2 106.5(5) . . ? C2 N1 Rh1 137.5(4) . . ? N2 N1 Rh1 116.0(4) . . ? C4 N2 N1 110.7(5) . . ? C4 N2 C1 130.1(5) . . ? N1 N2 C1 119.0(5) . . ? C5 N3 N4 105.6(5) . . ? C5 N3 Rh1 138.3(4) . . ? N4 N3 Rh1 116.0(3) . . ? C7 N4 N3 111.8(5) . . ? C7 N4 C1 129.6(5) . . ? N3 N4 C1 118.6(5) . . ? C8 N5 N6 106.9(5) . . ? C8 N5 Rh1 136.7(4) . . ? N6 N5 Rh1 116.1(4) . . ? N5 N6 C10 110.6(5) . . ? N5 N6 C1 119.6(5) . . ? C10 N6 C1 129.7(5) . . ? C11 N7 C22 118.6(5) . . ? C11 N7 Rh1 129.8(4) . . ? C22 N7 Rh1 111.6(4) . . ? C20 N8 C21 118.4(5) . . ? C20 N8 Rh1 129.3(4) . . ? C21 N8 Rh1 112.3(4) . . ? N6 C1 N2 111.5(5) . . ? N6 C1 N4 111.1(5) . . ? N2 C1 N4 110.2(5) . . ? N1 C2 C3 108.7(6) . . ? N1 C2 C23 123.7(5) . . ? C3 C2 C23 127.5(6) . . ? C4 C3 C2 107.9(6) . . ? C3 C4 N2 106.3(5) . . ? C3 C4 C24 131.4(6) . . ? N2 C4 C24 122.2(6) . . ? N3 C5 C6 109.7(5) . . ? N3 C5 C25 124.5(5) . . ? C6 C5 C25 125.8(5) . . ? C7 C6 C5 107.3(5) . . ? N4 C7 C6 105.5(5) . . ? N4 C7 C26 124.1(5) . . ? C6 C7 C26 130.3(6) . . ? N5 C8 C9 108.0(6) . . ? N5 C8 C27 124.2(6) . . ? C9 C8 C27 127.8(6) . . ? C10 C9 C8 108.2(6) . . ? C9 C10 N6 106.3(6) . . ? C9 C10 C28 131.8(6) . . ? N6 C10 C28 121.8(6) . . ? N7 C11 C12 121.8(6) . . ? C13 C12 C11 120.2(6) . . ? C12 C13 C14 119.4(6) . . ? C22 C14 C13 117.2(6) . . ? C22 C14 C15 118.4(6) . . ? C13 C14 C15 124.3(6) . . ? C16 C15 C14 121.1(6) . . ? C15 C16 C17 121.8(6) . . ? C21 C17 C18 116.1(6) . . ? C21 C17 C16 117.7(6) . . ? C18 C17 C16 126.0(6) . . ? C19 C18 C17 120.4(6) . . ? C18 C19 C20 119.5(6) . . ? N8 C20 C19 121.8(6) . . ? N8 C21 C17 123.4(6) . . ? N8 C21 C22 116.0(5) . . ? C17 C21 C22 120.2(6) . . ? N7 C22 C14 122.6(6) . . ? N7 C22 C21 116.4(5) . . ? C14 C22 C21 120.4(6) . . ? F2 P1 F1 90.9(4) . . ? F2 P1 F6 90.4(3) . . ? F1 P1 F6 89.8(3) . . ? F2 P1 F5 179.1(3) . . ? F1 P1 F5 90.0(3) . . ? F6 P1 F5 89.3(3) . . ? F2 P1 F3 91.0(3) . . ? F1 P1 F3 90.8(2) . . ? F6 P1 F3 178.4(3) . . ? F5 P1 F3 89.2(3) . . ? F2 P1 F4 90.2(3) . . ? F1 P1 F4 179.0(3) . . ? F6 P1 F4 90.2(2) . . ? F5 P1 F4 89.0(3) . . ? F3 P1 F4 89.2(2) . . ? F7 P2 F11 85.5(6) . . ? F7 P2 F10' 118.7(7) . . ? F11 P2 F10' 90.3(5) . . ? F7 P2 F7' 27.5(5) . . ? F11 P2 F7' 93.4(4) . . ? F10' P2 F7' 92.3(5) . . ? F7 P2 F12 96.7(6) . . ? F11 P2 F12 177.7(3) . . ? F10' P2 F12 88.1(4) . . ? F7' P2 F12 88.2(4) . . ? F7 P2 F8' 64.4(7) . . ? F11 P2 F8' 95.1(4) . . ? F10' P2 F8' 174.1(5) . . ? F7' P2 F8' 89.8(5) . . ? F12 P2 F8' 86.5(4) . . ? F7 P2 F10 94.3(9) . . ? F11 P2 F10 85.1(7) . . ? F10' P2 F10 24.5(6) . . ? F7' P2 F10 68.8(7) . . ? F12 P2 F10 94.0(7) . . ? F8' P2 F10 158.6(8) . . ? F7 P2 F8 87.7(9) . . ? F11 P2 F8 86.8(7) . . ? F10' P2 F8 153.2(8) . . ? F7' P2 F8 114.4(8) . . ? F12 P2 F8 94.0(7) . . ? F8' P2 F8 25.5(7) . . ? F10 P2 F8 171.5(10) . . ? F7 P2 F9' 153.6(7) . . ? F11 P2 F9' 91.9(4) . . ? F10' P2 F9' 87.6(5) . . ? F7' P2 F9' 174.7(5) . . ? F12 P2 F9' 86.4(4) . . ? F8' P2 F9' 89.8(5) . . ? F10 P2 F9' 111.6(7) . . ? F8 P2 F9' 65.9(8) . . ? F7 P2 F9 174.6(8) . . ? F11 P2 F9 89.2(7) . . ? F10' P2 F9 62.2(7) . . ? F7' P2 F9 154.4(8) . . ? F12 P2 F9 88.6(6) . . ? F8' P2 F9 115.3(8) . . ? F10 P2 F9 86.1(9) . . ? F8 P2 F9 91.1(10) . . ? F9' P2 F9 25.5(6) . . ? 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 N7 Rh1 N1 C2 -61(4) . . . . ? N8 Rh1 N1 C2 -47.3(6) . . . . ? N3 Rh1 N1 C2 132.8(6) . . . . ? N5 Rh1 N1 C2 -138.9(6) . . . . ? Cl1 Rh1 N1 C2 41.6(6) . . . . ? N7 Rh1 N1 N2 117(4) . . . . ? N8 Rh1 N1 N2 130.3(4) . . . . ? N3 Rh1 N1 N2 -49.6(4) . . . . ? N5 Rh1 N1 N2 38.8(4) . . . . ? Cl1 Rh1 N1 N2 -140.7(4) . . . . ? C2 N1 N2 C4 0.1(6) . . . . ? Rh1 N1 N2 C4 -178.2(4) . . . . ? C2 N1 N2 C1 -175.3(5) . . . . ? Rh1 N1 N2 C1 6.4(6) . . . . ? N7 Rh1 N3 C5 47.4(6) . . . . ? N8 Rh1 N3 C5 51(9) . . . . ? N1 Rh1 N3 C5 -133.3(6) . . . . ? N5 Rh1 N3 C5 138.6(6) . . . . ? Cl1 Rh1 N3 C5 -40.4(6) . . . . ? N7 Rh1 N3 N4 -133.3(4) . . . . ? N8 Rh1 N3 N4 -129(9) . . . . ? N1 Rh1 N3 N4 46.1(4) . . . . ? N5 Rh1 N3 N4 -42.0(4) . . . . ? Cl1 Rh1 N3 N4 139.0(4) . . . . ? C5 N3 N4 C7 -1.8(7) . . . . ? Rh1 N3 N4 C7 178.6(4) . . . . ? C5 N3 N4 C1 179.3(5) . . . . ? Rh1 N3 N4 C1 -0.3(7) . . . . ? N7 Rh1 N5 C8 -33.3(6) . . . . ? N8 Rh1 N5 C8 48.1(6) . . . . ? N1 Rh1 N5 C8 144.1(6) . . . . ? N3 Rh1 N5 C8 -130.6(6) . . . . ? Cl1 Rh1 N5 C8 -63(8) . . . . ? N7 Rh1 N5 N6 138.3(4) . . . . ? N8 Rh1 N5 N6 -140.3(4) . . . . ? N1 Rh1 N5 N6 -44.3(4) . . . . ? N3 Rh1 N5 N6 41.0(4) . . . . ? Cl1 Rh1 N5 N6 109(8) . . . . ? C8 N5 N6 C10 0.0(6) . . . . ? Rh1 N5 N6 C10 -174.0(4) . . . . ? C8 N5 N6 C1 177.5(5) . . . . ? Rh1 N5 N6 C1 3.5(6) . . . . ? N8 Rh1 N7 C11 -165.8(6) . . . . ? N1 Rh1 N7 C11 -152(4) . . . . ? N3 Rh1 N7 C11 14.1(6) . . . . ? N5 Rh1 N7 C11 -74.2(5) . . . . ? Cl1 Rh1 N7 C11 105.2(5) . . . . ? N8 Rh1 N7 C22 13.0(4) . . . . ? N1 Rh1 N7 C22 27(4) . . . . ? N3 Rh1 N7 C22 -167.0(4) . . . . ? N5 Rh1 N7 C22 104.6(4) . . . . ? Cl1 Rh1 N7 C22 -75.9(4) . . . . ? N7 Rh1 N8 C20 165.2(5) . . . . ? N1 Rh1 N8 C20 -14.2(5) . . . . ? N3 Rh1 N8 C20 161(9) . . . . ? N5 Rh1 N8 C20 74.0(5) . . . . ? Cl1 Rh1 N8 C20 -107.0(5) . . . . ? N7 Rh1 N8 C21 -13.0(4) . . . . ? N1 Rh1 N8 C21 167.6(4) . . . . ? N3 Rh1 N8 C21 -17(9) . . . . ? N5 Rh1 N8 C21 -104.2(4) . . . . ? Cl1 Rh1 N8 C21 74.8(4) . . . . ? N5 N6 C1 N2 59.2(6) . . . . ? C10 N6 C1 N2 -123.9(6) . . . . ? N5 N6 C1 N4 -64.2(6) . . . . ? C10 N6 C1 N4 112.7(6) . . . . ? C4 N2 C1 N6 120.1(6) . . . . ? N1 N2 C1 N6 -65.5(6) . . . . ? C4 N2 C1 N4 -116.0(6) . . . . ? N1 N2 C1 N4 58.4(7) . . . . ? C7 N4 C1 N6 -116.7(7) . . . . ? N3 N4 C1 N6 62.0(7) . . . . ? C7 N4 C1 N2 119.2(6) . . . . ? N3 N4 C1 N2 -62.1(7) . . . . ? N2 N1 C2 C3 -0.1(6) . . . . ? Rh1 N1 C2 C3 177.7(4) . . . . ? N2 N1 C2 C23 -178.1(5) . . . . ? Rh1 N1 C2 C23 -0.4(10) . . . . ? N1 C2 C3 C4 0.0(7) . . . . ? C23 C2 C3 C4 178.0(6) . . . . ? C2 C3 C4 N2 0.0(7) . . . . ? C2 C3 C4 C24 -174.7(6) . . . . ? N1 N2 C4 C3 -0.1(7) . . . . ? C1 N2 C4 C3 174.6(6) . . . . ? N1 N2 C4 C24 175.2(5) . . . . ? C1 N2 C4 C24 -10.1(10) . . . . ? N4 N3 C5 C6 1.0(7) . . . . ? Rh1 N3 C5 C6 -179.6(5) . . . . ? N4 N3 C5 C25 179.1(6) . . . . ? Rh1 N3 C5 C25 -1.5(10) . . . . ? N3 C5 C6 C7 0.1(7) . . . . ? C25 C5 C6 C7 -178.0(6) . . . . ? N3 N4 C7 C6 1.9(7) . . . . ? C1 N4 C7 C6 -179.4(6) . . . . ? N3 N4 C7 C26 -174.9(6) . . . . ? C1 N4 C7 C26 3.9(10) . . . . ? C5 C6 C7 N4 -1.2(7) . . . . ? C5 C6 C7 C26 175.3(6) . . . . ? N6 N5 C8 C9 -0.2(6) . . . . ? Rh1 N5 C8 C9 171.9(4) . . . . ? N6 N5 C8 C27 179.3(6) . . . . ? Rh1 N5 C8 C27 -8.6(10) . . . . ? N5 C8 C9 C10 0.4(7) . . . . ? C27 C8 C9 C10 -179.2(6) . . . . ? C8 C9 C10 N6 -0.4(7) . . . . ? C8 C9 C10 C28 -178.6(7) . . . . ? N5 N6 C10 C9 0.2(7) . . . . ? C1 N6 C10 C9 -176.9(5) . . . . ? N5 N6 C10 C28 178.6(5) . . . . ? C1 N6 C10 C28 1.5(9) . . . . ? C22 N7 C11 C12 4.8(9) . . . . ? Rh1 N7 C11 C12 -176.5(5) . . . . ? N7 C11 C12 C13 -2.3(10) . . . . ? C11 C12 C13 C14 -2.0(11) . . . . ? C12 C13 C14 C22 3.5(10) . . . . ? C12 C13 C14 C15 -173.9(7) . . . . ? C22 C14 C15 C16 -5.1(10) . . . . ? C13 C14 C15 C16 172.3(7) . . . . ? C14 C15 C16 C17 -0.7(11) . . . . ? C15 C16 C17 C21 5.5(10) . . . . ? C15 C16 C17 C18 -170.6(7) . . . . ? C21 C17 C18 C19 -3.5(10) . . . . ? C16 C17 C18 C19 172.7(6) . . . . ? C17 C18 C19 C20 2.4(10) . . . . ? C21 N8 C20 C19 -6.0(9) . . . . ? Rh1 N8 C20 C19 175.9(5) . . . . ? C18 C19 C20 N8 2.5(10) . . . . ? C20 N8 C21 C17 4.7(9) . . . . ? Rh1 N8 C21 C17 -176.8(5) . . . . ? C20 N8 C21 C22 -167.7(5) . . . . ? Rh1 N8 C21 C22 10.7(6) . . . . ? C18 C17 C21 N8 0.0(9) . . . . ? C16 C17 C21 N8 -176.6(6) . . . . ? C18 C17 C21 C22 172.1(6) . . . . ? C16 C17 C21 C22 -4.4(9) . . . . ? C11 N7 C22 C14 -3.1(9) . . . . ? Rh1 N7 C22 C14 177.9(5) . . . . ? C11 N7 C22 C21 167.8(5) . . . . ? Rh1 N7 C22 C21 -11.2(6) . . . . ? C13 C14 C22 N7 -1.0(9) . . . . ? C15 C14 C22 N7 176.5(6) . . . . ? C13 C14 C22 C21 -171.5(6) . . . . ? C15 C14 C22 C21 6.1(9) . . . . ? N8 C21 C22 N7 0.4(8) . . . . ? C17 C21 C22 N7 -172.3(5) . . . . ? N8 C21 C22 C14 171.4(5) . . . . ? C17 C21 C22 C14 -1.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.898 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.148 #4.CIF data_iaj186m _database_code_depnum_ccdc_archive 'CCDC 244905' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H30 Cl2 F6 N8 P Rh' _chemical_formula_weight 737.33 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.0197(8) _cell_length_b 11.8664(12) _cell_length_c 16.0172(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.709(2) _cell_angle_gamma 90.00 _cell_volume 1516.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4891 _cell_measurement_theta_min 5.101 _cell_measurement_theta_max 54.803 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7534 _exptl_absorpt_correction_T_max 0.9191 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9325 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6299 _reflns_number_gt 5647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0353P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.55(2) _refine_ls_number_reflns 6299 _refine_ls_number_parameters 372 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Rh1 Rh -0.13491(3) 0.50040(2) 0.176882(15) 0.01779(7) Uani 1 1 d . . . N1 N -0.0009(4) 0.3631(3) 0.1406(2) 0.0195(7) Uani 1 1 d . . . N2 N 0.0340(4) 0.2811(3) 0.20096(18) 0.0203(7) Uani 1 1 d . . . N3 N 0.0182(3) 0.5008(4) 0.28665(15) 0.0201(5) Uani 1 1 d . . . N4 N 0.0580(4) 0.3980(3) 0.32257(19) 0.0209(8) Uani 1 1 d . . . N5 N -0.2823(5) 0.3868(3) 0.2332(2) 0.0221(8) Uani 1 1 d . . . N6 N -0.1989(4) 0.3042(3) 0.28065(19) 0.0218(7) Uani 1 1 d . . . N7 N -0.2695(5) 0.6312(3) 0.2174(2) 0.0213(8) Uani 1 1 d . . . C1 C -0.0204(5) 0.2975(3) 0.2837(2) 0.0211(8) Uani 1 1 d . . . H1A H 0.0175 0.2310 0.3191 0.025 Uiso 1 1 calc R . . C2 C 0.0609(5) 0.3261(3) 0.0719(2) 0.0218(8) Uani 1 1 d . . . C3 C 0.1305(5) 0.2180(3) 0.0869(3) 0.0276(9) Uani 1 1 d . . . H3 H 0.1815 0.1727 0.0476 0.033 Uiso 1 1 calc R . . C4 C 0.1113(5) 0.1903(3) 0.1684(2) 0.0274(9) Uani 1 1 d . . . C5 C 0.1045(5) 0.5793(4) 0.3347(3) 0.0266(10) Uani 1 1 d . . . C6 C 0.1977(5) 0.5227(4) 0.4008(2) 0.0271(11) Uani 1 1 d . . . H6 H 0.2702 0.5570 0.4440 0.033 Uiso 1 1 calc R . . C7 C 0.1663(5) 0.4107(4) 0.3924(2) 0.0255(9) Uani 1 1 d . . . C8 C -0.4464(5) 0.3701(3) 0.2399(2) 0.0253(9) Uani 1 1 d . . . C9 C -0.4640(6) 0.2751(4) 0.2901(3) 0.0322(11) Uani 1 1 d . . . H9 H -0.5668 0.2440 0.3040 0.039 Uiso 1 1 calc R . . C10 C -0.3086(5) 0.2352(3) 0.3153(2) 0.0261(9) Uani 1 1 d . . . C11 C -0.3163(5) 0.6330(3) 0.2955(2) 0.0252(9) Uani 1 1 d . . . H11 H -0.2854 0.5720 0.3322 0.030 Uiso 1 1 calc R . . C12 C -0.4084(6) 0.7212(4) 0.3243(3) 0.0334(11) Uani 1 1 d . . . H12 H -0.4424 0.7186 0.3794 0.040 Uiso 1 1 calc R . . C13 C -0.4505(6) 0.8114(4) 0.2742(3) 0.0440(12) Uani 1 1 d . . . H13 H -0.5124 0.8725 0.2938 0.053 Uiso 1 1 calc R . . C14 C -0.4001(6) 0.8116(4) 0.1932(3) 0.0424(12) Uani 1 1 d . . . H14 H -0.4274 0.8732 0.1566 0.051 Uiso 1 1 calc R . . C15 C -0.3104(5) 0.7214(4) 0.1671(3) 0.0327(10) Uani 1 1 d . . . H15 H -0.2760 0.7222 0.1121 0.039 Uiso 1 1 calc R . . C16 C 0.0532(6) 0.3925(3) -0.0081(2) 0.0299(9) Uani 1 1 d . . . H16A H -0.0025 0.4647 -0.0005 0.045 Uiso 1 1 calc R . . H16B H -0.0102 0.3500 -0.0532 0.045 Uiso 1 1 calc R . . H16C H 0.1671 0.4060 -0.0230 0.045 Uiso 1 1 calc R . . C17 C 0.1542(6) 0.0850(4) 0.2170(3) 0.0382(11) Uani 1 1 d . . . H17A H 0.1234 0.0938 0.2744 0.057 Uiso 1 1 calc R . . H17B H 0.2748 0.0708 0.2187 0.057 Uiso 1 1 calc R . . H17C H 0.0924 0.0214 0.1899 0.057 Uiso 1 1 calc R . . C18 C 0.0931(6) 0.7025(4) 0.3198(3) 0.0353(11) Uani 1 1 d . . . H18A H 0.0180 0.7173 0.2689 0.053 Uiso 1 1 calc R . . H18B H 0.2047 0.7325 0.3128 0.053 Uiso 1 1 calc R . . H18C H 0.0489 0.7392 0.3678 0.053 Uiso 1 1 calc R . . C19 C 0.2233(6) 0.3139(4) 0.4487(3) 0.0367(11) Uani 1 1 d . . . H19A H 0.1777 0.2433 0.4242 0.055 Uiso 1 1 calc R . . H19B H 0.1833 0.3249 0.5040 0.055 Uiso 1 1 calc R . . H19C H 0.3460 0.3104 0.4547 0.055 Uiso 1 1 calc R . . C20 C -0.5815(5) 0.4444(4) 0.1997(3) 0.0354(10) Uani 1 1 d . . . H20A H -0.5313 0.5045 0.1684 0.053 Uiso 1 1 calc R . . H20B H -0.6440 0.4779 0.2431 0.053 Uiso 1 1 calc R . . H20C H -0.6578 0.3998 0.1612 0.053 Uiso 1 1 calc R . . C21 C -0.2497(6) 0.1373(4) 0.3692(3) 0.0381(11) Uani 1 1 d . . . H21A H -0.1269 0.1346 0.3746 0.057 Uiso 1 1 calc R . . H21B H -0.2946 0.0673 0.3435 0.057 Uiso 1 1 calc R . . H21C H -0.2889 0.1459 0.4249 0.057 Uiso 1 1 calc R . . Cl1 Cl -0.31108(10) 0.49497(12) 0.05142(5) 0.02679(18) Uani 1 1 d . . . Cl2 Cl 0.04684(14) 0.62243(8) 0.11767(7) 0.0274(2) Uani 1 1 d . . . P1 P 0.26700(13) -0.03465(9) -0.52301(7) 0.0279(3) Uani 1 1 d . . . F1 F 0.3647(5) 0.0512(3) -0.5776(3) 0.0937(14) Uani 1 1 d . . . F2 F 0.3674(4) -0.1375(3) -0.55803(18) 0.0541(8) Uani 1 1 d . . . F3 F 0.4086(4) -0.0233(4) -0.44890(19) 0.0845(13) Uani 1 1 d . . . F4 F 0.1685(4) -0.1187(3) -0.4709(3) 0.0804(12) Uani 1 1 d . . . F5 F 0.1659(4) 0.0679(3) -0.4876(2) 0.0568(8) Uani 1 1 d . . . F6 F 0.1266(4) -0.0464(3) -0.59807(19) 0.0717(10) Uani 1 1 d . . . N1S N 0.7276(7) 0.0802(5) 0.1561(3) 0.0729(15) Uani 1 1 d . . . C1S C 0.6863(7) 0.1295(5) 0.0973(4) 0.0506(14) Uani 1 1 d . . . C2S C 0.6374(6) 0.1934(4) 0.0220(3) 0.0478(13) Uani 1 1 d . . . H2S1 H 0.6166 0.2719 0.0369 0.072 Uiso 1 1 calc R . . H2S2 H 0.5349 0.1610 -0.0069 0.072 Uiso 1 1 calc R . . H2S3 H 0.7273 0.1906 -0.0152 0.072 Uiso 1 1 calc R . . 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 0.01682(12) 0.01939(13) 0.01743(12) 0.00022(15) 0.00294(9) -0.00048(15) N1 0.0196(18) 0.0196(17) 0.0188(18) -0.0003(14) -0.0009(14) 0.0015(14) N2 0.0229(17) 0.0205(17) 0.0182(16) 0.0024(13) 0.0050(13) 0.0025(13) N3 0.0185(13) 0.0225(14) 0.0193(13) -0.003(2) 0.0018(10) -0.002(2) N4 0.0188(18) 0.030(2) 0.0140(16) 0.0015(14) 0.0026(13) -0.0013(14) N5 0.0191(18) 0.028(2) 0.0192(18) -0.0007(15) 0.0025(15) -0.0001(15) N6 0.0211(16) 0.0238(17) 0.0204(16) 0.0034(13) 0.0019(13) -0.0019(13) N7 0.0217(19) 0.0194(19) 0.0229(19) -0.0029(15) 0.0026(15) 0.0008(15) C1 0.0185(19) 0.023(2) 0.023(2) 0.0011(16) 0.0055(16) -0.0016(15) C2 0.0201(19) 0.023(2) 0.023(2) -0.0043(16) 0.0072(16) -0.0013(16) C3 0.031(2) 0.026(2) 0.026(2) -0.0060(17) 0.0052(18) 0.0047(17) C4 0.028(2) 0.025(2) 0.028(2) -0.0017(18) 0.0027(17) 0.0003(17) C5 0.021(2) 0.026(2) 0.034(3) -0.0096(18) 0.0073(19) -0.0015(18) C6 0.0170(17) 0.038(4) 0.0246(19) -0.0029(18) -0.0045(14) -0.0032(17) C7 0.020(2) 0.041(3) 0.016(2) -0.0019(18) 0.0001(16) 0.0017(19) C8 0.020(2) 0.030(2) 0.026(2) -0.0031(17) 0.0016(16) -0.0027(17) C9 0.028(2) 0.039(3) 0.030(3) 0.001(2) 0.007(2) -0.012(2) C10 0.027(2) 0.026(2) 0.025(2) -0.0026(17) 0.0051(17) -0.0061(18) C11 0.024(2) 0.026(2) 0.026(2) 0.0002(17) 0.0042(17) 0.0027(17) C12 0.039(3) 0.034(3) 0.028(2) -0.011(2) 0.011(2) 0.006(2) C13 0.050(3) 0.035(3) 0.050(3) -0.005(2) 0.018(2) 0.009(2) C14 0.063(3) 0.023(2) 0.043(3) 0.006(2) 0.014(2) 0.013(2) C15 0.036(3) 0.027(2) 0.036(3) 0.0039(19) 0.010(2) 0.0040(19) C16 0.044(3) 0.027(2) 0.020(2) -0.0035(17) 0.0111(18) 0.0043(19) C17 0.049(3) 0.022(2) 0.043(3) -0.0025(19) 0.003(2) 0.008(2) C18 0.041(3) 0.029(2) 0.035(2) -0.0089(19) 0.002(2) -0.006(2) C19 0.030(2) 0.048(3) 0.031(2) 0.010(2) -0.0010(19) 0.002(2) C20 0.016(2) 0.045(3) 0.045(3) 0.003(2) 0.0006(18) 0.0013(18) C21 0.040(3) 0.032(3) 0.043(3) 0.013(2) 0.007(2) -0.012(2) Cl1 0.0272(4) 0.0304(5) 0.0220(4) 0.0020(6) -0.0013(3) 0.0007(6) Cl2 0.0280(6) 0.0243(6) 0.0311(6) 0.0037(4) 0.0095(4) -0.0031(4) P1 0.0254(5) 0.0323(6) 0.0268(5) -0.0025(4) 0.0063(4) -0.0005(4) F1 0.087(3) 0.064(2) 0.142(4) 0.031(2) 0.075(3) -0.0007(19) F2 0.0480(17) 0.0527(19) 0.0615(19) -0.0249(15) 0.0050(14) 0.0135(15) F3 0.0486(17) 0.123(4) 0.076(2) -0.060(2) -0.0218(15) 0.028(2) F4 0.057(2) 0.074(2) 0.117(3) 0.059(2) 0.045(2) 0.0198(19) F5 0.0517(18) 0.0482(18) 0.072(2) -0.0235(16) 0.0142(16) 0.0083(15) F6 0.072(2) 0.081(2) 0.0561(19) -0.0159(16) -0.0250(16) 0.0221(18) N1S 0.090(4) 0.061(3) 0.067(4) -0.013(3) 0.003(3) -0.012(3) C1S 0.056(3) 0.042(3) 0.055(4) -0.022(3) 0.011(3) -0.017(3) C2S 0.039(3) 0.042(3) 0.062(3) -0.010(3) 0.005(2) -0.013(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 Rh1 N7 2.034(4) . ? Rh1 N3 2.042(2) . ? Rh1 N5 2.059(4) . ? Rh1 N1 2.067(3) . ? Rh1 Cl2 2.3229(10) . ? Rh1 Cl1 2.3396(8) . ? N1 C2 1.326(5) . ? N1 N2 1.380(4) . ? N2 C4 1.372(5) . ? N2 C1 1.449(4) . ? N3 C5 1.354(5) . ? N3 N4 1.373(6) . ? N4 C7 1.354(5) . ? N4 C1 1.458(5) . ? N5 C8 1.346(5) . ? N5 N6 1.373(5) . ? N6 C10 1.360(5) . ? N6 C1 1.430(5) . ? N7 C11 1.342(5) . ? N7 C15 1.359(5) . ? C1 H1A 1.0000 . ? C2 C3 1.410(5) . ? C2 C16 1.500(5) . ? C3 C4 1.370(5) . ? C3 H3 0.9500 . ? C4 C17 1.495(6) . ? C5 C6 1.404(6) . ? C5 C18 1.483(6) . ? C6 C7 1.358(6) . ? C6 H6 0.9500 . ? C7 C19 1.503(6) . ? C8 C9 1.399(6) . ? C8 C20 1.493(6) . ? C9 C10 1.356(6) . ? C9 H9 0.9500 . ? C10 C21 1.496(6) . ? C11 C12 1.385(6) . ? C11 H11 0.9500 . ? C12 C13 1.360(7) . ? C12 H12 0.9500 . ? C13 C14 1.396(6) . ? C13 H13 0.9500 . ? C14 C15 1.378(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? 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 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? P1 F4 1.564(3) . ? P1 F3 1.565(3) . ? P1 F6 1.569(3) . ? P1 F2 1.595(3) . ? P1 F5 1.597(3) . ? P1 F1 1.598(3) . ? N1S C1S 1.131(7) . ? C1S C2S 1.446(8) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? 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 N7 Rh1 N3 90.92(15) . . ? N7 Rh1 N5 90.81(13) . . ? N3 Rh1 N5 86.95(14) . . ? N7 Rh1 N1 177.28(15) . . ? N3 Rh1 N1 87.67(15) . . ? N5 Rh1 N1 86.80(15) . . ? N7 Rh1 Cl2 91.65(11) . . ? N3 Rh1 Cl2 90.12(10) . . ? N5 Rh1 Cl2 176.20(11) . . ? N1 Rh1 Cl2 90.68(10) . . ? N7 Rh1 Cl1 90.05(11) . . ? N3 Rh1 Cl1 178.55(15) . . ? N5 Rh1 Cl1 91.95(11) . . ? N1 Rh1 Cl1 91.32(9) . . ? Cl2 Rh1 Cl1 90.94(4) . . ? C2 N1 N2 106.3(3) . . ? C2 N1 Rh1 137.9(3) . . ? N2 N1 Rh1 115.7(2) . . ? C4 N2 N1 110.8(3) . . ? C4 N2 C1 129.9(3) . . ? N1 N2 C1 119.2(3) . . ? C5 N3 N4 106.8(3) . . ? C5 N3 Rh1 136.1(4) . . ? N4 N3 Rh1 117.0(3) . . ? C7 N4 N3 110.5(3) . . ? C7 N4 C1 131.1(4) . . ? N3 N4 C1 118.4(3) . . ? C8 N5 N6 106.1(3) . . ? C8 N5 Rh1 137.7(3) . . ? N6 N5 Rh1 116.1(3) . . ? C10 N6 N5 110.9(3) . . ? C10 N6 C1 129.7(3) . . ? N5 N6 C1 119.3(3) . . ? C11 N7 C15 117.8(4) . . ? C11 N7 Rh1 121.1(3) . . ? C15 N7 Rh1 121.1(3) . . ? N6 C1 N2 111.6(3) . . ? N6 C1 N4 110.9(3) . . ? N2 C1 N4 110.1(3) . . ? N6 C1 H1A 108.1 . . ? N2 C1 H1A 108.1 . . ? N4 C1 H1A 108.1 . . ? N1 C2 C3 109.6(4) . . ? N1 C2 C16 123.2(4) . . ? C3 C2 C16 127.2(3) . . ? C4 C3 C2 107.4(4) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? C3 C4 N2 105.8(3) . . ? C3 C4 C17 130.9(4) . . ? N2 C4 C17 123.2(4) . . ? N3 C5 C6 107.6(4) . . ? N3 C5 C18 124.5(4) . . ? C6 C5 C18 127.8(4) . . ? C7 C6 C5 108.3(4) . . ? C7 C6 H6 125.8 . . ? C5 C6 H6 125.8 . . ? N4 C7 C6 106.8(4) . . ? N4 C7 C19 122.8(4) . . ? C6 C7 C19 130.3(4) . . ? N5 C8 C9 108.6(4) . . ? N5 C8 C20 123.5(4) . . ? C9 C8 C20 127.9(4) . . ? C10 C9 C8 108.1(4) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? C9 C10 N6 106.3(4) . . ? C9 C10 C21 132.1(4) . . ? N6 C10 C21 121.5(4) . . ? N7 C11 C12 122.0(4) . . ? N7 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 120.5(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 118.1(4) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? C15 C14 C13 119.3(4) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N7 C15 C14 122.3(4) . . ? N7 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C2 C16 H16A 109.5 . . ? C2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C4 C17 H17A 109.5 . . ? C4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C5 C18 H18A 109.5 . . ? C5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 C19 H19A 109.5 . . ? C7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C8 C20 H20A 109.5 . . ? C8 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C8 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C10 C21 H21A 109.5 . . ? C10 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C10 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? F4 P1 F3 91.0(2) . . ? F4 P1 F6 89.4(2) . . ? F3 P1 F6 179.31(19) . . ? F4 P1 F2 89.93(19) . . ? F3 P1 F2 88.79(17) . . ? F6 P1 F2 90.66(16) . . ? F4 P1 F5 89.73(18) . . ? F3 P1 F5 91.19(17) . . ? F6 P1 F5 89.37(17) . . ? F2 P1 F5 179.7(2) . . ? F4 P1 F1 178.9(2) . . ? F3 P1 F1 90.1(2) . . ? F6 P1 F1 89.5(2) . . ? F2 P1 F1 90.17(19) . . ? F5 P1 F1 90.17(19) . . ? N1S C1S C2S 178.7(6) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? 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 N7 Rh1 N1 C2 162(3) . . . . ? N3 Rh1 N1 C2 -138.7(4) . . . . ? N5 Rh1 N1 C2 134.2(4) . . . . ? Cl2 Rh1 N1 C2 -48.6(4) . . . . ? Cl1 Rh1 N1 C2 42.3(4) . . . . ? N7 Rh1 N1 N2 -15(3) . . . . ? N3 Rh1 N1 N2 44.1(3) . . . . ? N5 Rh1 N1 N2 -43.0(2) . . . . ? Cl2 Rh1 N1 N2 134.2(2) . . . . ? Cl1 Rh1 N1 N2 -134.9(2) . . . . ? C2 N1 N2 C4 -2.8(4) . . . . ? Rh1 N1 N2 C4 175.2(3) . . . . ? C2 N1 N2 C1 -179.4(3) . . . . ? Rh1 N1 N2 C1 -1.4(4) . . . . ? N7 Rh1 N3 C5 -48.3(4) . . . . ? N5 Rh1 N3 C5 -139.1(4) . . . . ? N1 Rh1 N3 C5 134.0(4) . . . . ? Cl2 Rh1 N3 C5 43.3(4) . . . . ? Cl1 Rh1 N3 C5 180(100) . . . . ? N7 Rh1 N3 N4 136.5(2) . . . . ? N5 Rh1 N3 N4 45.7(2) . . . . ? N1 Rh1 N3 N4 -41.2(2) . . . . ? Cl2 Rh1 N3 N4 -131.9(2) . . . . ? Cl1 Rh1 N3 N4 4(3) . . . . ? C5 N3 N4 C7 0.4(4) . . . . ? Rh1 N3 N4 C7 177.0(2) . . . . ? C5 N3 N4 C1 179.1(4) . . . . ? Rh1 N3 N4 C1 -4.3(4) . . . . ? N7 Rh1 N5 C8 44.7(4) . . . . ? N3 Rh1 N5 C8 135.6(5) . . . . ? N1 Rh1 N5 C8 -136.6(5) . . . . ? Cl2 Rh1 N5 C8 175.1(14) . . . . ? Cl1 Rh1 N5 C8 -45.4(4) . . . . ? N7 Rh1 N5 N6 -132.5(3) . . . . ? N3 Rh1 N5 N6 -41.6(3) . . . . ? N1 Rh1 N5 N6 46.2(3) . . . . ? Cl2 Rh1 N5 N6 -2.1(19) . . . . ? Cl1 Rh1 N5 N6 137.4(3) . . . . ? C8 N5 N6 C10 1.3(4) . . . . ? Rh1 N5 N6 C10 179.4(3) . . . . ? C8 N5 N6 C1 178.0(3) . . . . ? Rh1 N5 N6 C1 -4.0(4) . . . . ? N3 Rh1 N7 C11 -44.5(3) . . . . ? N5 Rh1 N7 C11 42.5(3) . . . . ? N1 Rh1 N7 C11 14(4) . . . . ? Cl2 Rh1 N7 C11 -134.6(3) . . . . ? Cl1 Rh1 N7 C11 134.5(3) . . . . ? N3 Rh1 N7 C15 133.5(3) . . . . ? N5 Rh1 N7 C15 -139.6(4) . . . . ? N1 Rh1 N7 C15 -168(3) . . . . ? Cl2 Rh1 N7 C15 43.3(3) . . . . ? Cl1 Rh1 N7 C15 -47.6(3) . . . . ? C10 N6 C1 N2 116.9(4) . . . . ? N5 N6 C1 N2 -59.1(4) . . . . ? C10 N6 C1 N4 -120.0(4) . . . . ? N5 N6 C1 N4 64.1(4) . . . . ? C4 N2 C1 N6 -113.4(4) . . . . ? N1 N2 C1 N6 62.4(4) . . . . ? C4 N2 C1 N4 123.0(4) . . . . ? N1 N2 C1 N4 -61.1(4) . . . . ? C7 N4 C1 N6 119.4(4) . . . . ? N3 N4 C1 N6 -59.0(4) . . . . ? C7 N4 C1 N2 -116.6(4) . . . . ? N3 N4 C1 N2 65.0(4) . . . . ? N2 N1 C2 C3 2.2(4) . . . . ? Rh1 N1 C2 C3 -175.2(3) . . . . ? N2 N1 C2 C16 -178.3(3) . . . . ? Rh1 N1 C2 C16 4.3(6) . . . . ? N1 C2 C3 C4 -0.9(5) . . . . ? C16 C2 C3 C4 179.6(4) . . . . ? C2 C3 C4 N2 -0.8(4) . . . . ? C2 C3 C4 C17 177.0(4) . . . . ? N1 N2 C4 C3 2.3(4) . . . . ? C1 N2 C4 C3 178.4(4) . . . . ? N1 N2 C4 C17 -175.7(4) . . . . ? C1 N2 C4 C17 0.4(6) . . . . ? N4 N3 C5 C6 -0.1(4) . . . . ? Rh1 N3 C5 C6 -175.6(3) . . . . ? N4 N3 C5 C18 -177.7(4) . . . . ? Rh1 N3 C5 C18 6.7(6) . . . . ? N3 C5 C6 C7 -0.3(5) . . . . ? C18 C5 C6 C7 177.3(4) . . . . ? N3 N4 C7 C6 -0.6(4) . . . . ? C1 N4 C7 C6 -179.1(4) . . . . ? N3 N4 C7 C19 175.5(3) . . . . ? C1 N4 C7 C19 -3.0(7) . . . . ? C5 C6 C7 N4 0.5(5) . . . . ? C5 C6 C7 C19 -175.2(4) . . . . ? N6 N5 C8 C9 -1.5(5) . . . . ? Rh1 N5 C8 C9 -178.9(3) . . . . ? N6 N5 C8 C20 178.0(4) . . . . ? Rh1 N5 C8 C20 0.6(7) . . . . ? N5 C8 C9 C10 1.2(5) . . . . ? C20 C8 C9 C10 -178.2(4) . . . . ? C8 C9 C10 N6 -0.3(5) . . . . ? C8 C9 C10 C21 179.8(4) . . . . ? N5 N6 C10 C9 -0.6(5) . . . . ? C1 N6 C10 C9 -176.8(4) . . . . ? N5 N6 C10 C21 179.3(4) . . . . ? C1 N6 C10 C21 3.1(6) . . . . ? C15 N7 C11 C12 2.2(6) . . . . ? Rh1 N7 C11 C12 -179.8(3) . . . . ? N7 C11 C12 C13 -2.0(7) . . . . ? C11 C12 C13 C14 0.8(7) . . . . ? C12 C13 C14 C15 0.0(7) . . . . ? C11 N7 C15 C14 -1.4(6) . . . . ? Rh1 N7 C15 C14 -179.4(4) . . . . ? C13 C14 C15 N7 0.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.559 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.077 #5.CIF data_iaj185m _database_code_depnum_ccdc_archive 'CCDC 244906' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H41 Cl F12 N11 P2 Rh' _chemical_formula_weight 1008.06 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.822(4) _cell_length_b 10.362(4) _cell_length_c 36.801(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.243(8) _cell_angle_gamma 90.00 _cell_volume 4481(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2155 _cell_measurement_theta_min 5.179 _cell_measurement_theta_max 46.264 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7869 _exptl_absorpt_correction_T_max 0.9315 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18740 _diffrn_reflns_av_R_equivalents 0.1228 _diffrn_reflns_av_sigmaI/netI 0.1584 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.34 _reflns_number_total 6430 _reflns_number_gt 3170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1229P)^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 6430 _refine_ls_number_parameters 490 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1482 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.2234 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.894 _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 Rh1 Rh 0.18999(7) 1.04987(8) 0.39560(2) 0.0342(3) Uani 1 1 d . . . Cl1 Cl 0.2433(2) 1.0151(3) 0.45728(8) 0.0451(7) Uani 1 1 d . . . N1 N 0.2953(7) 0.9075(7) 0.3823(2) 0.034(2) Uani 1 1 d . . . N2 N 0.2553(7) 0.8240(7) 0.3564(2) 0.036(2) Uani 1 1 d . . . N3 N 0.0681(8) 0.9112(8) 0.3955(2) 0.041(2) Uani 1 1 d . . . N4 N 0.0596(8) 0.8242(8) 0.3670(2) 0.039(2) Uani 1 1 d . . . N5 N 0.1439(7) 1.0722(7) 0.3413(2) 0.032(2) Uani 1 1 d . . . N6 N 0.1236(7) 0.9596(8) 0.3205(2) 0.036(2) Uani 1 1 d . . . N7 N 0.3168(8) 1.1810(7) 0.3923(2) 0.039(2) Uani 1 1 d . . . N8 N 0.0724(8) 1.1820(8) 0.4083(2) 0.038(2) Uani 1 1 d . . . C1 C 0.1367(10) 0.8353(10) 0.3397(3) 0.048(3) Uani 1 1 d . . . H1A H 0.1208 0.7642 0.3215 0.057 Uiso 1 1 calc R . . C2 C 0.4017(9) 0.8657(10) 0.3930(3) 0.035(3) Uani 1 1 d . . . C3 C 0.4237(10) 0.7547(10) 0.3731(3) 0.046(3) Uani 1 1 d . . . H3 H 0.4923 0.7064 0.3756 0.056 Uiso 1 1 calc R . . C4 C 0.3305(9) 0.7288(10) 0.3501(3) 0.039(3) Uani 1 1 d . . . C5 C -0.0153(9) 0.8781(10) 0.4166(3) 0.039(3) Uani 1 1 d . . . C6 C -0.0724(9) 0.7675(10) 0.4006(3) 0.042(3) Uani 1 1 d . . . H6 H -0.1342 0.7232 0.4094 0.050 Uiso 1 1 calc R . . C7 C -0.0212(10) 0.7375(10) 0.3701(3) 0.040(3) Uani 1 1 d . . . C8 C 0.1217(9) 1.1676(9) 0.3163(3) 0.035(3) Uani 1 1 d . . . C9 C 0.0884(8) 1.1151(10) 0.2829(3) 0.035(3) Uani 1 1 d . . . H9 H 0.0676 1.1631 0.2612 0.042 Uiso 1 1 calc R . . C10 C 0.0892(9) 0.9862(10) 0.2851(3) 0.036(3) Uani 1 1 d . . . C11 C -0.0248(10) 1.1952(11) 0.3857(3) 0.048(3) Uani 1 1 d . . . H11 H -0.0332 1.1459 0.3638 0.057 Uiso 1 1 calc R . . C12 C -0.1131(11) 1.2767(12) 0.3927(4) 0.065(4) Uani 1 1 d . . . H12 H -0.1818 1.2802 0.3768 0.078 Uiso 1 1 calc R . . C13 C -0.0967(12) 1.3554(12) 0.4250(4) 0.067(4) Uani 1 1 d . . . H13 H -0.1521 1.4170 0.4303 0.081 Uiso 1 1 calc R . . C14 C -0.0019(11) 1.3390(12) 0.4470(4) 0.063(4) Uani 1 1 d . . . H14 H 0.0081 1.3857 0.4693 0.076 Uiso 1 1 calc R . . C15 C 0.0844(10) 1.2552(11) 0.4386(3) 0.047(3) Uani 1 1 d . . . H15 H 0.1528 1.2500 0.4546 0.057 Uiso 1 1 calc R . . C16 C 0.3491(9) 1.2683(10) 0.4184(3) 0.042(3) Uani 1 1 d . . . H16 H 0.3124 1.2671 0.4401 0.051 Uiso 1 1 calc R . . C17 C 0.4336(10) 1.3607(11) 0.4153(3) 0.052(3) Uani 1 1 d . . . H17 H 0.4497 1.4243 0.4338 0.062 Uiso 1 1 calc R . . C18 C 0.4927(11) 1.3584(11) 0.3855(3) 0.055(3) Uani 1 1 d . . . H18 H 0.5525 1.4180 0.3830 0.066 Uiso 1 1 calc R . . C19 C 0.4630(9) 1.2678(10) 0.3595(3) 0.042(3) Uani 1 1 d . . . H19 H 0.5019 1.2634 0.3382 0.051 Uiso 1 1 calc R . . C20 C 0.3777(9) 1.1837(10) 0.3639(3) 0.038(3) Uani 1 1 d . . . H20 H 0.3599 1.1214 0.3452 0.045 Uiso 1 1 calc R . . C21 C 0.4826(9) 0.9352(10) 0.4207(3) 0.048(3) Uani 1 1 d . . . H21A H 0.4442 1.0099 0.4301 0.072 Uiso 1 1 calc R . . H21B H 0.5489 0.9644 0.4091 0.072 Uiso 1 1 calc R . . H21C H 0.5074 0.8766 0.4409 0.072 Uiso 1 1 calc R . . C22 C 0.3078(10) 0.6219(11) 0.3223(3) 0.057(3) Uani 1 1 d . . . H22A H 0.2305 0.6307 0.3100 0.085 Uiso 1 1 calc R . . H22B H 0.3154 0.5382 0.3348 0.085 Uiso 1 1 calc R . . H22C H 0.3627 0.6273 0.3043 0.085 Uiso 1 1 calc R . . C23 C -0.0416(10) 0.9461(11) 0.4496(3) 0.050(3) Uani 1 1 d . . . H23A H 0.0108 1.0189 0.4545 0.075 Uiso 1 1 calc R . . H23B H -0.0332 0.8867 0.4705 0.075 Uiso 1 1 calc R . . H23C H -0.1200 0.9783 0.4460 0.075 Uiso 1 1 calc R . . C24 C -0.0474(9) 0.6287(10) 0.3436(3) 0.046(3) Uani 1 1 d . . . H24A H 0.0040 0.6329 0.3245 0.069 Uiso 1 1 calc R . . H24B H -0.1263 0.6359 0.3325 0.069 Uiso 1 1 calc R . . H24C H -0.0370 0.5461 0.3565 0.069 Uiso 1 1 calc R . . C25 C 0.1363(10) 1.3071(9) 0.3274(3) 0.045(3) Uani 1 1 d . . . H25A H 0.1610 1.3124 0.3536 0.068 Uiso 1 1 calc R . . H25B H 0.0637 1.3525 0.3220 0.068 Uiso 1 1 calc R . . H25C H 0.1938 1.3472 0.3137 0.068 Uiso 1 1 calc R . . C26 C 0.0649(10) 0.8802(10) 0.2582(3) 0.046(3) Uani 1 1 d . . . H26A H 0.0750 0.7969 0.2708 0.069 Uiso 1 1 calc R . . H26B H 0.1173 0.8860 0.2394 0.069 Uiso 1 1 calc R . . H26C H -0.0136 0.8877 0.2468 0.069 Uiso 1 1 calc R . . P1 P 0.6880(2) 0.6182(2) 0.46404(7) 0.0426(8) Uani 1 1 d D . . F1 F 0.6824(7) 0.6107(8) 0.50678(11) 0.078(2) Uani 1 1 d D . . F2 F 0.5542(3) 0.6348(6) 0.45655(18) 0.0550(18) Uani 1 1 d D . . F3 F 0.7023(7) 0.7699(4) 0.4669(3) 0.100(3) Uani 1 1 d D . . F4 F 0.6944(6) 0.6249(9) 0.42132(11) 0.086(3) Uani 1 1 d D . . F5 F 0.8221(3) 0.6036(6) 0.47107(18) 0.0574(18) Uani 1 1 d D . . F6 F 0.6746(6) 0.4665(4) 0.4610(2) 0.065(2) Uani 1 1 d D . . P2 P 0.0592(3) 0.5018(3) 0.23119(9) 0.0445(8) Uani 1 1 d . . . F7 F 0.0656(8) 0.4511(7) 0.19144(19) 0.092(3) Uani 1 1 d . . . F8 F 0.1448(6) 0.6159(6) 0.22330(19) 0.065(2) Uani 1 1 d . . . F9 F -0.0447(6) 0.5919(7) 0.2167(2) 0.074(2) Uani 1 1 d . . . F19 F -0.0248(7) 0.3911(7) 0.2387(3) 0.092(3) Uani 1 1 d . . . F11 F 0.1603(6) 0.4111(7) 0.2460(2) 0.080(2) Uani 1 1 d . . . F12 F 0.0558(8) 0.5598(7) 0.27139(19) 0.085(3) Uani 1 1 d . . . N1S N 0.7012(12) 0.1396(14) 0.4393(4) 0.109(5) Uiso 1 1 d D . . C1S C 0.6462(13) 0.1707(15) 0.4606(4) 0.088(5) Uiso 1 1 d D . . C2S C 0.5736(14) 0.2039(16) 0.4898(4) 0.103(6) Uiso 1 1 d D . . H2S1 H 0.6211 0.2106 0.5133 0.155 Uiso 1 1 calc R . . H2S2 H 0.5162 0.1364 0.4913 0.155 Uiso 1 1 calc R . . H2S3 H 0.5356 0.2867 0.4841 0.155 Uiso 1 1 calc R . . N2S N 0.8435(12) 0.9427(13) 0.3123(4) 0.108(5) Uiso 1 1 d D . . C3S C 0.7798(12) 0.9476(14) 0.3326(4) 0.075(4) Uiso 1 1 d D . . C4S C 0.6894(15) 0.9444(18) 0.3578(5) 0.135(7) Uiso 1 1 d D . . H4S1 H 0.6932 1.0234 0.3725 0.203 Uiso 1 1 calc R . . H4S2 H 0.7009 0.8692 0.3739 0.203 Uiso 1 1 calc R . . H4S3 H 0.6147 0.9385 0.3434 0.203 Uiso 1 1 calc R . . N3S N 0.1846(10) 0.5406(11) 0.4002(3) 0.080(3) Uiso 1 1 d D . . C5S C 0.1909(13) 0.5940(14) 0.4267(4) 0.080(4) Uiso 1 1 d D . . C6S C 0.173(2) 0.662(2) 0.4612(5) 0.164(9) Uiso 1 1 d D . . H6S1 H 0.0976 0.6410 0.4682 0.246 Uiso 1 1 calc R . . H6S2 H 0.1787 0.7555 0.4576 0.246 Uiso 1 1 calc R . . H6S3 H 0.2314 0.6347 0.4807 0.246 Uiso 1 1 calc R . . 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 0.0329(5) 0.0306(5) 0.0422(5) -0.0035(4) 0.0173(4) -0.0004(4) Cl1 0.0487(19) 0.0394(16) 0.0490(18) -0.0021(13) 0.0132(14) 0.0001(13) N1 0.038(6) 0.031(5) 0.033(5) 0.000(4) 0.001(4) -0.009(4) N2 0.040(6) 0.023(5) 0.044(6) -0.004(4) 0.010(5) 0.002(4) N3 0.056(6) 0.034(5) 0.038(6) 0.004(4) 0.025(5) 0.005(4) N4 0.048(6) 0.028(5) 0.045(6) -0.006(4) 0.022(5) -0.010(4) N5 0.029(5) 0.029(5) 0.039(5) -0.013(4) 0.011(4) -0.005(4) N6 0.034(5) 0.031(5) 0.047(6) -0.006(5) 0.018(4) 0.002(4) N7 0.043(6) 0.025(5) 0.051(6) 0.001(4) 0.014(5) 0.006(4) N8 0.042(6) 0.044(6) 0.031(6) -0.004(4) 0.015(5) -0.005(4) C1 0.058(9) 0.032(6) 0.060(8) 0.008(6) 0.038(7) 0.006(6) C2 0.032(7) 0.040(6) 0.036(7) 0.001(5) 0.020(5) -0.006(5) C3 0.032(7) 0.046(7) 0.068(9) 0.000(6) 0.033(7) 0.012(6) C4 0.026(7) 0.047(7) 0.046(7) 0.000(6) 0.011(6) -0.003(5) C5 0.033(7) 0.042(7) 0.046(7) 0.002(6) 0.022(6) -0.004(5) C6 0.035(7) 0.054(7) 0.040(7) -0.006(5) 0.024(5) -0.005(6) C7 0.051(8) 0.034(6) 0.039(7) 0.008(5) 0.019(6) -0.004(6) C8 0.042(7) 0.023(6) 0.044(7) 0.006(5) 0.020(5) 0.002(5) C9 0.037(7) 0.032(7) 0.036(7) -0.007(5) 0.006(5) -0.012(5) C10 0.036(7) 0.032(7) 0.045(8) 0.004(5) 0.020(6) -0.011(5) C11 0.034(7) 0.057(8) 0.054(8) -0.010(6) 0.013(6) -0.003(6) C12 0.042(8) 0.070(9) 0.084(11) 0.007(8) 0.016(7) 0.018(7) C13 0.055(10) 0.048(8) 0.109(13) -0.007(8) 0.056(9) 0.005(7) C14 0.044(9) 0.059(8) 0.090(11) -0.025(7) 0.022(8) 0.011(7) C15 0.035(7) 0.050(7) 0.060(9) -0.004(6) 0.020(6) -0.002(6) C16 0.041(7) 0.043(7) 0.048(8) -0.017(6) 0.024(6) -0.008(6) C17 0.042(8) 0.044(7) 0.069(9) -0.026(6) 0.008(7) -0.013(6) C18 0.060(9) 0.045(7) 0.066(9) -0.001(7) 0.029(7) -0.010(6) C19 0.034(7) 0.050(7) 0.047(8) -0.007(6) 0.022(6) 0.000(6) C20 0.030(7) 0.040(6) 0.047(7) -0.005(5) 0.024(6) -0.008(5) C21 0.039(7) 0.040(7) 0.068(9) 0.002(6) 0.016(6) -0.007(5) C22 0.050(8) 0.047(7) 0.077(10) -0.015(7) 0.024(7) -0.002(6) C23 0.058(8) 0.053(7) 0.046(7) -0.006(6) 0.033(6) -0.009(6) C24 0.042(7) 0.046(7) 0.054(8) -0.015(6) 0.023(6) -0.022(6) C25 0.056(8) 0.021(6) 0.061(8) -0.005(5) 0.018(6) 0.000(5) C26 0.056(8) 0.050(7) 0.034(7) -0.016(5) 0.014(6) -0.017(6) P1 0.0397(19) 0.0427(18) 0.047(2) -0.0026(15) 0.0100(15) -0.0051(14) F1 0.084(6) 0.107(6) 0.047(5) -0.020(4) 0.034(4) -0.001(5) F2 0.035(4) 0.050(4) 0.081(5) 0.001(3) 0.010(3) 0.007(3) F3 0.077(6) 0.033(4) 0.180(9) 0.004(5) -0.026(6) -0.007(4) F4 0.063(5) 0.151(8) 0.045(5) 0.027(5) 0.013(4) -0.024(5) F5 0.033(4) 0.073(5) 0.065(5) -0.001(4) -0.002(3) -0.011(3) F6 0.054(4) 0.038(4) 0.104(6) -0.011(4) 0.021(4) -0.009(3) P2 0.046(2) 0.0422(16) 0.048(2) -0.0059(14) 0.0194(16) 0.0018(14) F7 0.159(9) 0.074(5) 0.046(5) -0.015(4) 0.025(5) 0.011(5) F8 0.064(5) 0.056(4) 0.079(5) -0.006(4) 0.026(4) -0.018(4) F9 0.051(5) 0.065(5) 0.107(6) 0.018(4) 0.009(4) 0.012(4) F19 0.069(6) 0.063(5) 0.147(8) 0.028(5) 0.032(5) -0.023(4) F11 0.074(6) 0.084(5) 0.085(6) 0.026(4) 0.025(4) 0.037(4) F12 0.139(8) 0.070(5) 0.051(5) -0.009(4) 0.039(5) 0.009(5) _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 2.025(9) . ? Rh1 N5 2.027(8) . ? Rh1 N3 2.035(9) . ? Rh1 N7 2.037(9) . ? Rh1 N8 2.042(9) . ? Rh1 Cl1 2.317(3) . ? N1 N2 1.335(10) . ? N1 C2 1.349(13) . ? N2 C4 1.365(13) . ? N2 C1 1.473(14) . ? N3 C5 1.363(13) . ? N3 N4 1.379(11) . ? N4 C7 1.326(13) . ? N4 C1 1.433(13) . ? N5 C8 1.357(12) . ? N5 N6 1.401(10) . ? N6 C10 1.351(12) . ? N6 C1 1.469(13) . ? N7 C20 1.331(13) . ? N7 C16 1.345(12) . ? N8 C15 1.341(13) . ? N8 C11 1.351(13) . ? C1 H1A 1.0000 . ? C2 C3 1.402(14) . ? C2 C21 1.503(14) . ? C3 C4 1.343(15) . ? C3 H3 0.9500 . ? C4 C22 1.510(15) . ? C5 C6 1.423(14) . ? C5 C23 1.469(14) . ? C6 C7 1.367(14) . ? C6 H6 0.9500 . ? C7 C24 1.501(14) . ? C8 C9 1.361(13) . ? C8 C25 1.507(13) . ? C9 C10 1.338(13) . ? C9 H9 0.9500 . ? C10 C26 1.485(14) . ? C11 C12 1.389(16) . ? C11 H11 0.9500 . ? C12 C13 1.435(18) . ? C12 H12 0.9500 . ? C13 C14 1.320(17) . ? C13 H13 0.9500 . ? C14 C15 1.399(16) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.398(14) . ? C16 H16 0.9500 . ? C17 C18 1.364(16) . ? C17 H17 0.9500 . ? C18 C19 1.361(15) . ? C18 H18 0.9500 . ? C19 C20 1.356(14) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? P1 F3 1.583(3) . ? P1 F1 1.583(3) . ? P1 F6 1.583(3) . ? P1 F4 1.584(3) . ? P1 F2 1.585(3) . ? P1 F5 1.585(3) . ? P2 F19 1.561(7) . ? P2 F7 1.564(7) . ? P2 F11 1.571(7) . ? P2 F9 1.587(7) . ? P2 F12 1.601(7) . ? P2 F8 1.603(7) . ? N1S C1S 1.120(10) . ? C1S C2S 1.487(13) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? N2S C3S 1.119(10) . ? C3S C4S 1.487(13) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? N3S C5S 1.119(10) . ? C5S C6S 1.487(13) . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? 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 N5 87.2(3) . . ? N1 Rh1 N3 86.5(3) . . ? N5 Rh1 N3 87.9(3) . . ? N1 Rh1 N7 89.7(3) . . ? N5 Rh1 N7 89.2(3) . . ? N3 Rh1 N7 175.3(4) . . ? N1 Rh1 N8 175.0(3) . . ? N5 Rh1 N8 91.9(3) . . ? N3 Rh1 N8 88.5(3) . . ? N7 Rh1 N8 95.2(3) . . ? N1 Rh1 Cl1 90.9(2) . . ? N5 Rh1 Cl1 177.6(2) . . ? N3 Rh1 Cl1 90.5(3) . . ? N7 Rh1 Cl1 92.3(3) . . ? N8 Rh1 Cl1 89.9(3) . . ? N2 N1 C2 104.3(8) . . ? N2 N1 Rh1 117.8(6) . . ? C2 N1 Rh1 137.9(7) . . ? N1 N2 C4 113.8(9) . . ? N1 N2 C1 119.5(8) . . ? C4 N2 C1 126.5(9) . . ? C5 N3 N4 105.7(8) . . ? C5 N3 Rh1 137.1(8) . . ? N4 N3 Rh1 117.2(6) . . ? C7 N4 N3 111.8(8) . . ? C7 N4 C1 129.4(9) . . ? N3 N4 C1 118.8(9) . . ? C8 N5 N6 103.1(8) . . ? C8 N5 Rh1 139.8(7) . . ? N6 N5 Rh1 117.1(6) . . ? C10 N6 N5 111.9(8) . . ? C10 N6 C1 130.3(9) . . ? N5 N6 C1 117.7(9) . . ? C20 N7 C16 114.3(9) . . ? C20 N7 Rh1 121.7(7) . . ? C16 N7 Rh1 124.0(7) . . ? C15 N8 C11 117.4(10) . . ? C15 N8 Rh1 123.8(8) . . ? C11 N8 Rh1 118.8(7) . . ? N4 C1 N6 111.5(8) . . ? N4 C1 N2 110.5(9) . . ? N6 C1 N2 108.4(9) . . ? N4 C1 H1A 108.8 . . ? N6 C1 H1A 108.8 . . ? N2 C1 H1A 108.8 . . ? N1 C2 C3 109.3(10) . . ? N1 C2 C21 123.3(9) . . ? C3 C2 C21 127.3(10) . . ? C4 C3 C2 108.0(10) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? C3 C4 N2 104.6(9) . . ? C3 C4 C22 130.4(10) . . ? N2 C4 C22 125.0(10) . . ? N3 C5 C6 107.9(9) . . ? N3 C5 C23 125.6(10) . . ? C6 C5 C23 126.5(10) . . ? C7 C6 C5 106.8(10) . . ? C7 C6 H6 126.6 . . ? C5 C6 H6 126.6 . . ? N4 C7 C6 107.7(10) . . ? N4 C7 C24 123.5(9) . . ? C6 C7 C24 128.8(10) . . ? N5 C8 C9 109.6(9) . . ? N5 C8 C25 120.5(10) . . ? C9 C8 C25 129.9(10) . . ? C10 C9 C8 110.3(10) . . ? C10 C9 H9 124.9 . . ? C8 C9 H9 124.9 . . ? C9 C10 N6 105.0(9) . . ? C9 C10 C26 134.4(11) . . ? N6 C10 C26 120.5(9) . . ? N8 C11 C12 123.6(11) . . ? N8 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C11 C12 C13 117.5(12) . . ? C11 C12 H12 121.2 . . ? C13 C12 H12 121.2 . . ? C14 C13 C12 117.6(12) . . ? C14 C13 H13 121.2 . . ? C12 C13 H13 121.2 . . ? C13 C14 C15 122.4(13) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? N8 C15 C14 121.3(11) . . ? N8 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? N7 C16 C17 123.5(10) . . ? N7 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C18 C17 C16 119.1(11) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 117.6(11) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? C20 C19 C18 119.8(11) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? N7 C20 C19 125.5(10) . . ? N7 C20 H20 117.3 . . ? C19 C20 H20 117.3 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C4 C22 H22A 109.5 . . ? C4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C5 C23 H23A 109.5 . . ? C5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C7 C24 H24A 109.5 . . ? C7 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C7 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 C25 H25A 109.5 . . ? C8 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C8 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C10 C26 H26A 109.5 . . ? C10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F3 P1 F1 90.0(5) . . ? F3 P1 F6 179.5(5) . . ? F1 P1 F6 90.4(4) . . ? F3 P1 F4 90.3(5) . . ? F1 P1 F4 179.5(5) . . ? F6 P1 F4 89.3(4) . . ? F3 P1 F2 90.1(4) . . ? F1 P1 F2 91.7(4) . . ? F6 P1 F2 90.3(4) . . ? F4 P1 F2 88.7(4) . . ? F3 P1 F5 89.2(4) . . ? F1 P1 F5 89.0(4) . . ? F6 P1 F5 90.4(4) . . ? F4 P1 F5 90.6(4) . . ? F2 P1 F5 179.0(4) . . ? F19 P2 F7 90.9(5) . . ? F19 P2 F11 88.5(4) . . ? F7 P2 F11 90.6(5) . . ? F19 P2 F9 90.4(4) . . ? F7 P2 F9 89.9(5) . . ? F11 P2 F9 178.8(5) . . ? F19 P2 F12 91.8(5) . . ? F7 P2 F12 177.3(5) . . ? F11 P2 F12 89.9(5) . . ? F9 P2 F12 89.6(5) . . ? F19 P2 F8 179.6(5) . . ? F7 P2 F8 89.0(4) . . ? F11 P2 F8 91.9(4) . . ? F9 P2 F8 89.2(4) . . ? F12 P2 F8 88.3(4) . . ? N1S C1S C2S 176.5(19) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 174.7(18) . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N3S C5S C6S 168.1(19) . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? 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 N5 Rh1 N1 N2 -43.2(7) . . . . ? N3 Rh1 N1 N2 44.9(7) . . . . ? N7 Rh1 N1 N2 -132.4(7) . . . . ? N8 Rh1 N1 N2 36(4) . . . . ? Cl1 Rh1 N1 N2 135.4(7) . . . . ? N5 Rh1 N1 C2 138.7(10) . . . . ? N3 Rh1 N1 C2 -133.2(10) . . . . ? N7 Rh1 N1 C2 49.6(10) . . . . ? N8 Rh1 N1 C2 -142(4) . . . . ? Cl1 Rh1 N1 C2 -42.7(10) . . . . ? C2 N1 N2 C4 0.9(11) . . . . ? Rh1 N1 N2 C4 -177.8(7) . . . . ? C2 N1 N2 C1 176.3(9) . . . . ? Rh1 N1 N2 C1 -2.3(11) . . . . ? N1 Rh1 N3 C5 137.5(11) . . . . ? N5 Rh1 N3 C5 -135.2(11) . . . . ? N7 Rh1 N3 C5 174(4) . . . . ? N8 Rh1 N3 C5 -43.3(11) . . . . ? Cl1 Rh1 N3 C5 46.6(11) . . . . ? N1 Rh1 N3 N4 -44.1(7) . . . . ? N5 Rh1 N3 N4 43.2(7) . . . . ? N7 Rh1 N3 N4 -8(5) . . . . ? N8 Rh1 N3 N4 135.1(7) . . . . ? Cl1 Rh1 N3 N4 -135.0(7) . . . . ? C5 N3 N4 C7 -2.1(12) . . . . ? Rh1 N3 N4 C7 179.0(7) . . . . ? C5 N3 N4 C1 179.5(9) . . . . ? Rh1 N3 N4 C1 0.6(12) . . . . ? N1 Rh1 N5 C8 -138.4(11) . . . . ? N3 Rh1 N5 C8 135.0(11) . . . . ? N7 Rh1 N5 C8 -48.6(11) . . . . ? N8 Rh1 N5 C8 46.5(11) . . . . ? Cl1 Rh1 N5 C8 -175(5) . . . . ? N1 Rh1 N5 N6 43.6(6) . . . . ? N3 Rh1 N5 N6 -43.0(6) . . . . ? N7 Rh1 N5 N6 133.4(6) . . . . ? N8 Rh1 N5 N6 -131.4(6) . . . . ? Cl1 Rh1 N5 N6 7(6) . . . . ? C8 N5 N6 C10 -1.1(10) . . . . ? Rh1 N5 N6 C10 177.6(6) . . . . ? C8 N5 N6 C1 -178.2(9) . . . . ? Rh1 N5 N6 C1 0.4(10) . . . . ? N1 Rh1 N7 C20 47.8(8) . . . . ? N5 Rh1 N7 C20 -39.4(8) . . . . ? N3 Rh1 N7 C20 12(5) . . . . ? N8 Rh1 N7 C20 -131.2(8) . . . . ? Cl1 Rh1 N7 C20 138.7(8) . . . . ? N1 Rh1 N7 C16 -129.9(8) . . . . ? N5 Rh1 N7 C16 142.9(8) . . . . ? N3 Rh1 N7 C16 -166(4) . . . . ? N8 Rh1 N7 C16 51.1(9) . . . . ? Cl1 Rh1 N7 C16 -39.1(8) . . . . ? N1 Rh1 N8 C15 129(4) . . . . ? N5 Rh1 N8 C15 -151.3(8) . . . . ? N3 Rh1 N8 C15 120.8(9) . . . . ? N7 Rh1 N8 C15 -62.0(9) . . . . ? Cl1 Rh1 N8 C15 30.3(8) . . . . ? N1 Rh1 N8 C11 -49(4) . . . . ? N5 Rh1 N8 C11 30.5(8) . . . . ? N3 Rh1 N8 C11 -57.3(8) . . . . ? N7 Rh1 N8 C11 119.9(8) . . . . ? Cl1 Rh1 N8 C11 -147.9(8) . . . . ? C7 N4 C1 N6 120.5(12) . . . . ? N3 N4 C1 N6 -61.5(13) . . . . ? C7 N4 C1 N2 -118.9(12) . . . . ? N3 N4 C1 N2 59.1(12) . . . . ? C10 N6 C1 N4 -115.8(11) . . . . ? N5 N6 C1 N4 60.8(12) . . . . ? C10 N6 C1 N2 122.4(11) . . . . ? N5 N6 C1 N2 -61.1(11) . . . . ? N1 N2 C1 N4 -59.1(11) . . . . ? C4 N2 C1 N4 115.8(11) . . . . ? N1 N2 C1 N6 63.4(12) . . . . ? C4 N2 C1 N6 -121.7(10) . . . . ? N2 N1 C2 C3 -0.7(11) . . . . ? Rh1 N1 C2 C3 177.5(8) . . . . ? N2 N1 C2 C21 176.6(9) . . . . ? Rh1 N1 C2 C21 -5.2(16) . . . . ? N1 C2 C3 C4 0.3(12) . . . . ? C21 C2 C3 C4 -176.8(10) . . . . ? C2 C3 C4 N2 0.2(12) . . . . ? C2 C3 C4 C22 179.5(11) . . . . ? N1 N2 C4 C3 -0.7(12) . . . . ? C1 N2 C4 C3 -175.8(10) . . . . ? N1 N2 C4 C22 -180.0(10) . . . . ? C1 N2 C4 C22 4.9(17) . . . . ? N4 N3 C5 C6 1.3(12) . . . . ? Rh1 N3 C5 C6 179.8(8) . . . . ? N4 N3 C5 C23 -178.0(11) . . . . ? Rh1 N3 C5 C23 0.5(18) . . . . ? N3 C5 C6 C7 -0.1(13) . . . . ? C23 C5 C6 C7 179.2(11) . . . . ? N3 N4 C7 C6 2.1(13) . . . . ? C1 N4 C7 C6 -179.7(11) . . . . ? N3 N4 C7 C24 -178.2(10) . . . . ? C1 N4 C7 C24 -0.1(18) . . . . ? C5 C6 C7 N4 -1.2(13) . . . . ? C5 C6 C7 C24 179.2(11) . . . . ? N6 N5 C8 C9 1.1(10) . . . . ? Rh1 N5 C8 C9 -177.1(8) . . . . ? N6 N5 C8 C25 -178.4(9) . . . . ? Rh1 N5 C8 C25 3.4(16) . . . . ? N5 C8 C9 C10 -0.8(12) . . . . ? C25 C8 C9 C10 178.7(11) . . . . ? C8 C9 C10 N6 0.0(12) . . . . ? C8 C9 C10 C26 -178.0(11) . . . . ? N5 N6 C10 C9 0.7(11) . . . . ? C1 N6 C10 C9 177.4(10) . . . . ? N5 N6 C10 C26 179.1(9) . . . . ? C1 N6 C10 C26 -4.2(16) . . . . ? C15 N8 C11 C12 -2.0(17) . . . . ? Rh1 N8 C11 C12 176.3(9) . . . . ? N8 C11 C12 C13 3.1(19) . . . . ? C11 C12 C13 C14 -4.2(19) . . . . ? C12 C13 C14 C15 4(2) . . . . ? C11 N8 C15 C14 1.9(16) . . . . ? Rh1 N8 C15 C14 -176.3(9) . . . . ? C13 C14 C15 N8 -3(2) . . . . ? C20 N7 C16 C17 4.4(15) . . . . ? Rh1 N7 C16 C17 -177.8(8) . . . . ? N7 C16 C17 C18 -4.5(18) . . . . ? C16 C17 C18 C19 2.2(18) . . . . ? C17 C18 C19 C20 -0.4(18) . . . . ? C16 N7 C20 C19 -2.4(16) . . . . ? Rh1 N7 C20 C19 179.7(8) . . . . ? C18 C19 C20 N7 0.5(18) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.211 _refine_diff_density_min -1.429 _refine_diff_density_rms 0.137