Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'N. Connelly' 'Christopher J. Adams' 'David J. H. Emslie' 'Owen D. Hayward' 'Tania Manson' 'A. Guy Orpen' 'P. Rieger' _publ_contact_author_name 'Prof N. Connelly ' _publ_contact_author_address ; Prof N. Connelly School of Chemistry University of Bristol Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email NEIL.CONNELLY@BRISTOL.AC.UK _publ_section_title ; The substitution chemistry of the tris(3,5-dimethylpyrazolyl)methanerhodium complex [Rh(CO)2{HC(pz')3}]+ ; data_1+ _database_code_CSD 205489 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 F6 N6 O2 P Rh' _chemical_formula_weight 602.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 14.4245(19) _cell_length_b 11.5540(12) _cell_length_c 28.1766(18) _cell_angle_alpha 90.000(8) _cell_angle_beta 97.188(9) _cell_angle_gamma 90.000(10) _cell_volume 4659.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.259 _exptl_absorpt_correction_T_max 0.333 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker CCD area detector' _diffrn_measurement_method 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 29260 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10635 _reflns_number_gt 7998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10635 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.004 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 0.143790(13) 0.700410(16) 0.502352(6) 0.02572(6) Uani 1 1 d . . . Rh2 Rh -0.459044(15) 0.898252(18) 0.122095(7) 0.03392(6) Uani 1 1 d . . . O1 O 0.22165(16) 0.86869(19) 0.43703(7) 0.0557(6) Uani 1 1 d . . . O2 O 0.14804(16) 0.52855(18) 0.42395(6) 0.0487(5) Uani 1 1 d . . . O3 O -0.6298(2) 0.9556(3) 0.05605(10) 0.0928(10) Uani 1 1 d . . . O4 O -0.37775(19) 1.0980(2) 0.07398(9) 0.0783(8) Uani 1 1 d . . . N2 N -0.00005(14) 0.79848(17) 0.51531(6) 0.0255(4) Uani 1 1 d . . . N1 N -0.02770(13) 0.78069(16) 0.55967(7) 0.0252(4) Uani 1 1 d . . . N4 N 0.10645(14) 0.57774(16) 0.55174(7) 0.0258(4) Uani 1 1 d . . . N3 N 0.06016(14) 0.61256(16) 0.58923(6) 0.0256(4) Uani 1 1 d . . . N6 N 0.18450(13) 0.79839(16) 0.56683(6) 0.0249(4) Uani 1 1 d . . . N5 N 0.12518(13) 0.80128(16) 0.60147(6) 0.0239(4) Uani 1 1 d . . . N16 N -0.53106(14) 0.79012(17) 0.16759(7) 0.0292(4) Uani 1 1 d . . . N15 N -0.48567(14) 0.69638(17) 0.18985(7) 0.0278(4) Uani 1 1 d . . . N14 N -0.34131(14) 0.86502(18) 0.17316(7) 0.0293(5) Uani 1 1 d . . . N13 N -0.32626(14) 0.75411(18) 0.19096(7) 0.0291(4) Uani 1 1 d . . . N12 N -0.41298(15) 0.70865(18) 0.09495(7) 0.0322(5) Uani 1 1 d . . . N11 N -0.39536(14) 0.62664(17) 0.12980(7) 0.0291(5) Uani 1 1 d . . . C1 C 0.1915(2) 0.8035(2) 0.46200(9) 0.0371(6) Uani 1 1 d . . . C2 C 0.14537(19) 0.5943(2) 0.45343(9) 0.0339(6) Uani 1 1 d . . . C3 C 0.04020(16) 0.7339(2) 0.59649(8) 0.0240(5) Uani 1 1 d . . . H3 H 0.0131 0.7400 0.6274 0.029 Uiso 1 1 calc R . . C6 C -0.0647(2) 0.8942(2) 0.44034(9) 0.0382(6) Uani 1 1 d . . . H6A H -0.0475 0.9761 0.4392 0.057 Uiso 1 1 calc R . . H6B H -0.1259 0.8823 0.4216 0.057 Uiso 1 1 calc R . . H6C H -0.0178 0.8471 0.4269 0.057 Uiso 1 1 calc R . . C7 C -0.06930(17) 0.8590(2) 0.49124(8) 0.0282(5) Uani 1 1 d . . . C8 C -0.14039(18) 0.8791(2) 0.52024(9) 0.0318(6) Uani 1 1 d . . . H8 H -0.1973 0.9194 0.5112 0.038 Uiso 1 1 calc R . . C9 C -0.11269(17) 0.8301(2) 0.56373(9) 0.0285(5) Uani 1 1 d . . . C10 C -0.15930(19) 0.8210(2) 0.60817(10) 0.0398(7) Uani 1 1 d . . . H10A H -0.1783 0.7406 0.6125 0.060 Uiso 1 1 calc R . . H10B H -0.2145 0.8711 0.6052 0.060 Uiso 1 1 calc R . . H10C H -0.1156 0.8452 0.6358 0.060 Uiso 1 1 calc R . . C11 C 0.1804(2) 0.3958(2) 0.52789(10) 0.0400(6) Uani 1 1 d . . . H11A H 0.1368 0.3714 0.5002 0.060 Uiso 1 1 calc R . . H11B H 0.2073 0.3274 0.5450 0.060 Uiso 1 1 calc R . . H11C H 0.2305 0.4423 0.5170 0.060 Uiso 1 1 calc R . . C12 C 0.12932(17) 0.4667(2) 0.56073(9) 0.0296(5) Uani 1 1 d . . . C13 C 0.09784(19) 0.4319(2) 0.60365(9) 0.0359(6) Uani 1 1 d . . . H13 H 0.1047 0.3571 0.6177 0.043 Uiso 1 1 calc R . . C14 C 0.05569(18) 0.5247(2) 0.62149(8) 0.0319(6) Uani 1 1 d . . . C15 C 0.0110(2) 0.5399(3) 0.66630(9) 0.0457(7) Uani 1 1 d . . . H15A H 0.0074 0.4648 0.6822 0.069 Uiso 1 1 calc R . . H15B H -0.0522 0.5712 0.6582 0.069 Uiso 1 1 calc R . . H15C H 0.0483 0.5935 0.6878 0.069 Uiso 1 1 calc R . . C16 C 0.33887(18) 0.8835(2) 0.55668(9) 0.0392(6) Uani 1 1 d . . . H16A H 0.3447 0.8173 0.5355 0.059 Uiso 1 1 calc R . . H16B H 0.3959 0.8905 0.5794 0.059 Uiso 1 1 calc R . . H16C H 0.3298 0.9544 0.5375 0.059 Uiso 1 1 calc R . . C17 C 0.25700(17) 0.8658(2) 0.58346(8) 0.0272(5) Uani 1 1 d . . . C18 C 0.24313(18) 0.9120(2) 0.62804(8) 0.0304(6) Uani 1 1 d . . . H18 H 0.2841 0.9629 0.6471 0.036 Uiso 1 1 calc R . . C19 C 0.15966(18) 0.8701(2) 0.63901(8) 0.0275(5) Uani 1 1 d . . . C20 C 0.1095(2) 0.8895(2) 0.68160(9) 0.0427(7) Uani 1 1 d . . . H20A H 0.0463 0.9179 0.6711 0.064 Uiso 1 1 calc R . . H20B H 0.1436 0.9468 0.7027 0.064 Uiso 1 1 calc R . . H20C H 0.1059 0.8164 0.6989 0.064 Uiso 1 1 calc R . . C21 C -0.5654(3) 0.9358(3) 0.08233(12) 0.0561(9) Uani 1 1 d . . . C22 C -0.4067(2) 1.0212(3) 0.09305(11) 0.0502(8) Uani 1 1 d . . . C23 C -0.39385(17) 0.6628(2) 0.17913(8) 0.0280(5) Uani 1 1 d . . . H23 H -0.3735 0.5947 0.1998 0.034 Uiso 1 1 calc R . . C26 C -0.6847(2) 0.8863(2) 0.16916(11) 0.0448(7) Uani 1 1 d . . . H26A H -0.6545 0.9617 0.1667 0.067 Uiso 1 1 calc R . . H26B H -0.7298 0.8913 0.1923 0.067 Uiso 1 1 calc R . . H26C H -0.7172 0.8644 0.1378 0.067 Uiso 1 1 calc R . . C27 C -0.61222(17) 0.7971(2) 0.18536(9) 0.0322(6) Uani 1 1 d . . . C28 C -0.61805(18) 0.7095(2) 0.21913(9) 0.0344(6) Uani 1 1 d . . . H28 H -0.6685 0.6967 0.2372 0.041 Uiso 1 1 calc R . . C29 C -0.53769(18) 0.6458(2) 0.22135(8) 0.0301(5) Uani 1 1 d . . . C30 C -0.5066(2) 0.5409(2) 0.25021(9) 0.0399(6) Uani 1 1 d . . . H30A H -0.5497 0.5265 0.2738 0.060 Uiso 1 1 calc R . . H30B H -0.4435 0.5538 0.2668 0.060 Uiso 1 1 calc R . . H30C H -0.5061 0.4738 0.2290 0.060 Uiso 1 1 calc R . . C31 C -0.2578(2) 1.0522(2) 0.18253(10) 0.0431(7) Uani 1 1 d . . . H31A H -0.2333 1.0620 0.1519 0.065 Uiso 1 1 calc R . . H31B H -0.2146 1.0873 0.2081 0.065 Uiso 1 1 calc R . . H31C H -0.3189 1.0899 0.1810 0.065 Uiso 1 1 calc R . . C32 C -0.26788(18) 0.9269(2) 0.19246(8) 0.0321(6) Uani 1 1 d . . . C33 C -0.20612(18) 0.8553(2) 0.22189(9) 0.0362(6) Uani 1 1 d . . . H33 H -0.1482 0.8780 0.2392 0.043 Uiso 1 1 calc R . . C34 C -0.24465(18) 0.7472(2) 0.22091(8) 0.0335(6) Uani 1 1 d . . . C35 C -0.2111(2) 0.6384(3) 0.24568(11) 0.0503(8) Uani 1 1 d . . . H35A H -0.2547 0.6152 0.2680 0.076 Uiso 1 1 calc R . . H35B H -0.1490 0.6513 0.2634 0.076 Uiso 1 1 calc R . . H35C H -0.2073 0.5770 0.2220 0.076 Uiso 1 1 calc R . . C36 C -0.4308(2) 0.7135(3) 0.00705(9) 0.0494(8) Uani 1 1 d . . . H36A H -0.4856 0.7638 0.0066 0.074 Uiso 1 1 calc R . . H36B H -0.4413 0.6576 -0.0192 0.074 Uiso 1 1 calc R . . H36C H -0.3757 0.7606 0.0032 0.074 Uiso 1 1 calc R . . C37 C -0.41513(18) 0.6503(2) 0.05363(9) 0.0355(6) Uani 1 1 d . . . C38 C -0.39996(19) 0.5324(2) 0.06280(10) 0.0386(6) Uani 1 1 d . . . H38 H -0.3986 0.4732 0.0395 0.046 Uiso 1 1 calc R . . C39 C -0.38737(17) 0.5176(2) 0.11158(9) 0.0327(6) Uani 1 1 d . . . C40 C -0.3646(2) 0.4133(2) 0.14236(11) 0.0448(7) Uani 1 1 d . . . H40A H -0.3000 0.4186 0.1577 0.067 Uiso 1 1 calc R . . H40B H -0.3720 0.3434 0.1225 0.067 Uiso 1 1 calc R . . H40C H -0.4070 0.4096 0.1669 0.067 Uiso 1 1 calc R . . P1 P 0.06635(6) 0.82659(6) 0.30999(2) 0.03852(17) Uani 1 1 d . . . P2 P -0.62901(6) 0.28043(7) 0.14382(3) 0.04605(19) Uani 1 1 d . . . F1 F 0.16028(14) 0.83095(19) 0.28573(9) 0.0820(7) Uani 1 1 d . . . F2 F 0.1099(2) 0.73796(19) 0.34915(7) 0.0960(9) Uani 1 1 d . . . F3 F 0.03283(16) 0.72096(17) 0.27585(7) 0.0717(6) Uani 1 1 d . . . F4 F -0.03017(16) 0.82162(18) 0.33224(7) 0.0775(6) Uani 1 1 d . . . F5 F 0.01985(14) 0.91626(17) 0.27161(6) 0.0630(5) Uani 1 1 d . . . F6 F 0.09973(17) 0.93156(17) 0.34391(7) 0.0861(8) Uani 1 1 d . . . F7 F -0.5827(9) 0.2512(6) 0.1935(3) 0.126(4) Uani 0.572(12) 1 d P A . F7' F -0.6674(12) 0.1575(13) 0.1623(8) 0.141(8) Uani 0.428(12) 1 d P A 2 F8 F -0.6748(10) 0.1602(7) 0.1399(4) 0.094(3) Uani 0.572(12) 1 d P A . F8' F -0.5818(13) 0.2157(14) 0.1048(3) 0.175(7) Uani 0.428(12) 1 d P A 2 F9 F -0.6861(6) 0.3180(7) 0.09334(19) 0.0711(19) Uani 0.572(12) 1 d P A . F9' F -0.5834(9) 0.3984(10) 0.1304(5) 0.123(5) Uani 0.428(12) 1 d P A 2 F10 F -0.5486(5) 0.2346(5) 0.1190(4) 0.107(4) Uani 0.572(12) 1 d P A . F10' F -0.5276(6) 0.2513(9) 0.1774(5) 0.101(4) Uani 0.428(12) 1 d P A 2 F11 F -0.5864(5) 0.4072(5) 0.1467(3) 0.069(2) Uani 0.572(12) 1 d P A . F11' F -0.6605(12) 0.3471(8) 0.1857(3) 0.113(4) Uani 0.428(12) 1 d P A 2 F12 F -0.7208(6) 0.3303(5) 0.1657(3) 0.085(3) Uani 0.572(12) 1 d P A . F12' F -0.7177(8) 0.3069(8) 0.1129(6) 0.118(6) Uani 0.428(12) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02659(10) 0.02848(11) 0.02306(9) -0.00222(8) 0.00695(7) -0.00316(8) Rh2 0.03282(12) 0.03146(12) 0.03599(11) 0.00376(9) -0.00153(9) 0.00177(9) O1 0.0707(16) 0.0589(14) 0.0398(11) 0.0082(10) 0.0153(11) -0.0256(12) O2 0.0636(14) 0.0501(13) 0.0339(10) -0.0144(9) 0.0121(10) -0.0032(11) O3 0.0711(19) 0.089(2) 0.104(2) 0.0261(17) -0.0464(17) 0.0105(16) O4 0.0695(18) 0.0812(19) 0.0842(18) 0.0449(15) 0.0093(14) -0.0123(14) N2 0.0241(10) 0.0320(11) 0.0207(9) 0.0017(8) 0.0038(8) 0.0007(9) N1 0.0211(10) 0.0313(11) 0.0238(9) 0.0014(8) 0.0047(8) 0.0023(8) N4 0.0263(11) 0.0247(11) 0.0269(10) -0.0019(8) 0.0050(8) -0.0030(8) N3 0.0282(11) 0.0255(11) 0.0235(9) -0.0003(8) 0.0050(8) -0.0012(8) N6 0.0220(10) 0.0288(11) 0.0239(9) 0.0004(8) 0.0031(8) -0.0012(8) N5 0.0251(10) 0.0256(10) 0.0208(9) -0.0014(8) 0.0020(8) -0.0014(8) N16 0.0251(11) 0.0278(11) 0.0340(11) -0.0022(9) 0.0013(9) 0.0015(9) N15 0.0247(10) 0.0302(11) 0.0284(10) -0.0015(9) 0.0026(8) 0.0006(9) N14 0.0274(11) 0.0323(11) 0.0280(10) 0.0007(9) 0.0027(9) -0.0018(9) N13 0.0242(11) 0.0338(11) 0.0286(10) 0.0001(9) 0.0001(9) -0.0004(9) N12 0.0324(12) 0.0337(12) 0.0299(10) -0.0010(9) 0.0022(9) 0.0020(9) N11 0.0274(11) 0.0297(11) 0.0309(10) -0.0027(9) 0.0060(9) 0.0011(9) C1 0.0407(16) 0.0415(16) 0.0290(12) -0.0105(12) 0.0033(12) 0.0006(13) C2 0.0340(15) 0.0385(15) 0.0305(13) -0.0018(12) 0.0084(11) -0.0045(12) C3 0.0239(12) 0.0271(12) 0.0212(11) 0.0009(9) 0.0031(9) -0.0002(10) C6 0.0413(16) 0.0375(15) 0.0335(13) 0.0072(12) -0.0042(12) -0.0010(12) C7 0.0306(13) 0.0221(12) 0.0301(12) -0.0016(10) -0.0031(11) -0.0010(10) C8 0.0241(13) 0.0274(13) 0.0425(14) -0.0037(11) -0.0009(11) 0.0050(10) C9 0.0236(13) 0.0269(13) 0.0356(13) -0.0061(10) 0.0056(11) 0.0005(10) C10 0.0308(14) 0.0473(17) 0.0437(15) -0.0052(13) 0.0144(12) 0.0031(12) C11 0.0433(16) 0.0294(14) 0.0476(16) -0.0062(12) 0.0060(13) 0.0020(12) C12 0.0276(13) 0.0245(13) 0.0351(13) -0.0035(10) -0.0017(11) -0.0024(10) C13 0.0436(16) 0.0253(13) 0.0371(14) 0.0055(11) -0.0016(12) -0.0031(12) C14 0.0360(15) 0.0310(14) 0.0277(12) 0.0055(10) 0.0005(11) -0.0073(11) C15 0.067(2) 0.0427(17) 0.0292(13) 0.0076(12) 0.0142(14) -0.0081(15) C16 0.0285(14) 0.0457(16) 0.0425(15) 0.0041(13) 0.0003(12) -0.0091(12) C17 0.0241(12) 0.0238(12) 0.0319(12) 0.0048(10) -0.0035(10) -0.0025(10) C18 0.0322(14) 0.0246(13) 0.0314(12) 0.0016(10) -0.0072(11) -0.0034(10) C19 0.0359(14) 0.0222(12) 0.0224(11) 0.0010(9) -0.0041(10) 0.0037(10) C20 0.0568(19) 0.0437(17) 0.0276(13) -0.0101(12) 0.0058(13) -0.0005(14) C21 0.060(2) 0.0414(18) 0.064(2) 0.0115(16) -0.0056(18) 0.0030(16) C22 0.0445(18) 0.055(2) 0.0509(17) 0.0145(16) 0.0045(15) 0.0035(15) C23 0.0217(12) 0.0294(13) 0.0322(13) 0.0017(10) 0.0010(10) 0.0015(10) C26 0.0312(15) 0.0365(16) 0.0658(19) -0.0098(14) 0.0022(14) 0.0044(12) C27 0.0227(12) 0.0346(14) 0.0386(13) -0.0134(11) 0.0006(11) -0.0030(11) C28 0.0254(13) 0.0434(16) 0.0354(13) -0.0067(12) 0.0077(11) -0.0059(12) C29 0.0305(14) 0.0359(14) 0.0235(11) -0.0058(10) 0.0016(10) -0.0074(11) C30 0.0436(16) 0.0452(17) 0.0309(13) 0.0038(12) 0.0048(12) -0.0040(13) C31 0.0494(18) 0.0416(16) 0.0399(15) -0.0076(13) 0.0125(13) -0.0157(14) C32 0.0300(14) 0.0419(15) 0.0261(12) -0.0080(11) 0.0102(11) -0.0084(12) C33 0.0249(13) 0.0545(17) 0.0289(13) -0.0085(12) 0.0025(11) -0.0061(12) C34 0.0254(13) 0.0487(16) 0.0259(12) -0.0031(11) 0.0009(10) 0.0011(12) C35 0.0390(17) 0.058(2) 0.0485(17) 0.0090(15) -0.0144(14) 0.0032(15) C36 0.0510(19) 0.065(2) 0.0322(14) -0.0034(14) 0.0050(13) 0.0018(16) C37 0.0263(14) 0.0478(16) 0.0332(13) -0.0083(12) 0.0065(11) -0.0001(12) C38 0.0327(15) 0.0418(16) 0.0428(15) -0.0173(12) 0.0107(12) -0.0032(12) C39 0.0229(13) 0.0301(14) 0.0466(15) -0.0059(11) 0.0098(11) -0.0016(10) C40 0.0407(17) 0.0331(15) 0.0617(18) -0.0024(13) 0.0110(14) 0.0016(13) P1 0.0490(5) 0.0333(4) 0.0320(3) -0.0036(3) 0.0001(3) 0.0018(3) P2 0.0512(5) 0.0382(4) 0.0474(4) -0.0007(3) 0.0007(4) 0.0034(4) F1 0.0428(11) 0.0737(14) 0.133(2) -0.0123(13) 0.0253(13) -0.0055(10) F2 0.156(2) 0.0601(13) 0.0633(13) 0.0068(11) -0.0182(14) 0.0486(15) F3 0.0877(15) 0.0676(13) 0.0640(12) -0.0343(10) 0.0260(11) -0.0297(11) F4 0.0951(17) 0.0809(15) 0.0667(13) 0.0040(11) 0.0503(12) 0.0045(12) F5 0.0711(13) 0.0782(13) 0.0391(9) 0.0175(9) 0.0046(9) 0.0168(11) F6 0.1157(19) 0.0483(12) 0.0805(14) -0.0274(10) -0.0419(13) 0.0127(12) F7 0.183(9) 0.087(4) 0.086(4) 0.023(3) -0.073(5) 0.028(6) F7' 0.081(8) 0.071(6) 0.29(2) 0.078(10) 0.078(12) 0.011(5) F8 0.107(5) 0.024(3) 0.153(7) 0.011(4) 0.028(5) -0.012(3) F8' 0.274(17) 0.210(13) 0.043(4) 0.009(5) 0.026(6) 0.183(12) F9 0.090(5) 0.077(3) 0.042(2) 0.0014(19) -0.009(2) -0.011(3) F9' 0.062(5) 0.116(8) 0.192(10) 0.131(8) 0.020(6) 0.014(6) F10 0.054(3) 0.051(3) 0.225(11) -0.035(4) 0.053(5) 0.004(3) F10' 0.056(4) 0.084(5) 0.146(9) 0.079(5) -0.049(5) -0.026(4) F11 0.044(3) 0.037(3) 0.117(5) -0.034(4) -0.026(3) 0.005(2) F11' 0.190(12) 0.088(5) 0.067(5) -0.013(4) 0.041(6) 0.021(7) F12 0.112(5) 0.062(3) 0.095(5) 0.030(3) 0.066(4) 0.026(3) F12' 0.070(7) 0.054(5) 0.208(15) -0.034(7) -0.076(8) 0.027(4) _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 C1 1.839(3) . ? Rh1 C2 1.847(3) . ? Rh1 N4 2.1032(19) . ? Rh1 N6 2.1587(19) . ? Rh1 N2 2.431(2) . ? Rh1 C3 3.226(2) . ? Rh2 C21 1.835(3) . ? Rh2 C22 1.848(3) . ? Rh2 N14 2.119(2) . ? Rh2 N16 2.149(2) . ? Rh2 N12 2.440(2) . ? Rh2 C23 3.239(2) . ? O1 C1 1.152(3) . ? O2 C2 1.130(3) . ? O3 C21 1.137(4) . ? O4 C22 1.143(4) . ? N2 C7 1.333(3) . ? N2 N1 1.374(2) . ? N1 C9 1.370(3) . ? N1 C3 1.440(3) . ? N4 C12 1.341(3) . ? N4 N3 1.378(3) . ? N3 C14 1.369(3) . ? N3 C3 1.451(3) . ? N6 C17 1.341(3) . ? N6 N5 1.377(3) . ? N5 C19 1.366(3) . ? N5 C3 1.444(3) . ? N16 C27 1.332(3) . ? N16 N15 1.376(3) . ? N15 C29 1.364(3) . ? N15 C23 1.448(3) . ? N14 C32 1.336(3) . ? N14 N13 1.383(3) . ? N13 C34 1.362(3) . ? N13 C23 1.447(3) . ? N12 C37 1.342(3) . ? N12 N11 1.365(3) . ? N11 C39 1.371(3) . ? N11 C23 1.449(3) . ? C6 C7 1.500(3) . ? C7 C8 1.408(3) . ? C8 C9 1.363(3) . ? C9 C10 1.497(3) . ? C11 C12 1.496(4) . ? C12 C13 1.403(3) . ? C13 C14 1.360(4) . ? C14 C15 1.498(3) . ? C16 C17 1.493(3) . ? C17 C18 1.402(3) . ? C18 C19 1.368(4) . ? C19 C20 1.493(3) . ? C26 C27 1.498(4) . ? C27 C28 1.398(4) . ? C28 C29 1.368(4) . ? C29 C30 1.496(4) . ? C31 C32 1.484(4) . ? C32 C33 1.408(4) . ? C33 C34 1.366(4) . ? C34 C35 1.489(4) . ? C36 C37 1.494(4) . ? C37 C38 1.399(4) . ? C38 C39 1.375(4) . ? C39 C40 1.497(4) . ? P1 F2 1.577(2) . ? P1 F6 1.5815(19) . ? P1 F5 1.5846(18) . ? P1 F3 1.5912(18) . ? P1 F1 1.593(2) . ? P1 F4 1.598(2) . ? P2 F12' 1.487(8) . ? P2 F7 1.512(5) . ? P2 F11' 1.525(8) . ? P2 F10 1.523(7) . ? P2 F8 1.536(9) . ? P2 F8' 1.555(10) . ? P2 F9' 1.580(10) . ? P2 F11 1.587(6) . ? P2 F9 1.612(6) . ? P2 F12 1.634(5) . ? P2 F7' 1.633(15) . ? P2 F10' 1.675(7) . ? F7 F10' 0.964(11) . ? F7 F11' 1.572(12) . ? F7' F8 0.63(3) . ? F8' F10 0.623(17) . ? F9 F12' 0.769(18) . ? F10 F10' 1.648(13) . ? F11 F11' 1.768(13) . ? F11' F12 0.996(10) . ? F12 F12' 1.518(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C2 85.89(11) . . ? C1 Rh1 N4 172.93(10) . . ? C2 Rh1 N4 94.27(10) . . ? C1 Rh1 N6 95.58(9) . . ? C2 Rh1 N6 161.56(10) . . ? N4 Rh1 N6 82.05(7) . . ? C1 Rh1 N2 100.55(10) . . ? C2 Rh1 N2 120.79(10) . . ? N4 Rh1 N2 85.45(7) . . ? N6 Rh1 N2 77.09(7) . . ? C1 Rh1 C3 132.69(9) . . ? C2 Rh1 C3 138.02(9) . . ? N4 Rh1 C3 49.73(7) . . ? N6 Rh1 C3 49.49(7) . . ? N2 Rh1 C3 47.85(6) . . ? C21 Rh2 C22 84.51(14) . . ? C21 Rh2 N14 174.39(12) . . ? C22 Rh2 N14 95.90(11) . . ? C21 Rh2 N16 94.14(12) . . ? C22 Rh2 N16 165.10(12) . . ? N14 Rh2 N16 84.02(8) . . ? C21 Rh2 N12 105.12(12) . . ? C22 Rh2 N12 114.15(11) . . ? N14 Rh2 N12 79.84(7) . . ? N16 Rh2 N12 80.56(7) . . ? C21 Rh2 C23 132.09(11) . . ? C22 Rh2 C23 139.15(11) . . ? N14 Rh2 C23 49.66(7) . . ? N16 Rh2 C23 49.28(7) . . ? N12 Rh2 C23 47.76(6) . . ? C7 N2 N1 104.89(19) . . ? C7 N2 Rh1 140.11(16) . . ? N1 N2 Rh1 114.65(13) . . ? C9 N1 N2 112.23(18) . . ? C9 N1 C3 129.14(19) . . ? N2 N1 C3 117.57(18) . . ? C12 N4 N3 105.42(19) . . ? C12 N4 Rh1 133.82(17) . . ? N3 N4 Rh1 119.94(14) . . ? C14 N3 N4 111.10(19) . . ? C14 N3 C3 126.58(19) . . ? N4 N3 C3 120.91(18) . . ? C17 N6 N5 105.37(18) . . ? C17 N6 Rh1 135.80(16) . . ? N5 N6 Rh1 118.80(14) . . ? C19 N5 N6 111.38(19) . . ? C19 N5 C3 127.7(2) . . ? N6 N5 C3 120.89(18) . . ? C27 N16 N15 105.5(2) . . ? C27 N16 Rh2 134.62(18) . . ? N15 N16 Rh2 119.46(15) . . ? C29 N15 N16 111.4(2) . . ? C29 N15 C23 127.8(2) . . ? N16 N15 C23 120.78(19) . . ? C32 N14 N13 105.5(2) . . ? C32 N14 Rh2 134.97(18) . . ? N13 N14 Rh2 119.34(15) . . ? C34 N13 N14 111.3(2) . . ? C34 N13 C23 127.2(2) . . ? N14 N13 C23 121.44(19) . . ? C37 N12 N11 104.9(2) . . ? C37 N12 Rh2 138.16(18) . . ? N11 N12 Rh2 115.53(14) . . ? N12 N11 C39 112.7(2) . . ? N12 N11 C23 117.99(19) . . ? C39 N11 C23 129.2(2) . . ? O1 C1 Rh1 179.4(2) . . ? O2 C2 Rh1 178.6(3) . . ? N1 C3 N5 111.14(18) . . ? N1 C3 N3 112.96(18) . . ? N5 C3 N3 110.70(19) . . ? N1 C3 Rh1 78.23(12) . . ? N5 C3 Rh1 70.72(11) . . ? N3 C3 Rh1 69.37(11) . . ? N2 C7 C8 110.2(2) . . ? N2 C7 C6 120.6(2) . . ? C8 C7 C6 129.3(2) . . ? C9 C8 C7 107.5(2) . . ? C8 C9 N1 105.2(2) . . ? C8 C9 C10 132.0(2) . . ? N1 C9 C10 122.7(2) . . ? N4 C12 C13 109.8(2) . . ? N4 C12 C11 122.4(2) . . ? C13 C12 C11 127.9(2) . . ? C14 C13 C12 107.5(2) . . ? C13 C14 N3 106.2(2) . . ? C13 C14 C15 131.5(2) . . ? N3 C14 C15 122.3(2) . . ? N6 C17 C18 110.0(2) . . ? N6 C17 C16 122.3(2) . . ? C18 C17 C16 127.7(2) . . ? C19 C18 C17 107.2(2) . . ? N5 C19 C18 106.0(2) . . ? N5 C19 C20 122.9(2) . . ? C18 C19 C20 131.1(2) . . ? O3 C21 Rh2 176.6(4) . . ? O4 C22 Rh2 177.2(3) . . ? N13 C23 N15 111.3(2) . . ? N13 C23 N11 111.1(2) . . ? N15 C23 N11 111.90(19) . . ? N13 C23 Rh2 69.33(12) . . ? N15 C23 Rh2 70.23(12) . . ? N11 C23 Rh2 78.31(13) . . ? N16 C27 C28 110.0(2) . . ? N16 C27 C26 122.6(2) . . ? C28 C27 C26 127.3(2) . . ? C29 C28 C27 107.3(2) . . ? N15 C29 C28 105.7(2) . . ? N15 C29 C30 123.3(2) . . ? C28 C29 C30 131.0(2) . . ? N14 C32 C33 109.7(2) . . ? N14 C32 C31 122.4(2) . . ? C33 C32 C31 127.9(2) . . ? C34 C33 C32 107.4(2) . . ? N13 C34 C33 106.0(2) . . ? N13 C34 C35 123.1(2) . . ? C33 C34 C35 130.9(2) . . ? N12 C37 C38 110.0(2) . . ? N12 C37 C36 120.1(3) . . ? C38 C37 C36 129.9(2) . . ? C39 C38 C37 107.7(2) . . ? N11 C39 C38 104.7(2) . . ? N11 C39 C40 123.1(2) . . ? C38 C39 C40 132.2(2) . . ? F2 P1 F6 90.61(12) . . ? F2 P1 F5 178.14(14) . . ? F6 P1 F5 88.96(11) . . ? F2 P1 F3 89.38(12) . . ? F6 P1 F3 179.97(16) . . ? F5 P1 F3 91.05(12) . . ? F2 P1 F1 92.01(14) . . ? F6 P1 F1 91.38(13) . . ? F5 P1 F1 89.81(12) . . ? F3 P1 F1 88.59(11) . . ? F2 P1 F4 89.57(14) . . ? F6 P1 F4 90.27(13) . . ? F5 P1 F4 88.63(11) . . ? F3 P1 F4 89.76(12) . . ? F1 P1 F4 177.70(13) . . ? F12' P2 F7 146.8(6) . . ? F12' P2 F11' 91.8(5) . . ? F7 P2 F11' 62.3(5) . . ? F12' P2 F10 116.8(7) . . ? F7 P2 F10 94.3(5) . . ? F11' P2 F10 148.1(6) . . ? F12' P2 F8 79.2(6) . . ? F7 P2 F8 90.1(5) . . ? F11' P2 F8 110.2(6) . . ? F10 P2 F8 89.9(5) . . ? F12' P2 F8' 96.1(7) . . ? F7 P2 F8' 111.4(5) . . ? F11' P2 F8' 171.4(7) . . ? F10 P2 F8' 23.3(7) . . ? F8 P2 F8' 74.7(9) . . ? F12' P2 F9' 92.0(7) . . ? F7 P2 F9' 105.4(5) . . ? F11' P2 F9' 85.6(6) . . ? F10 P2 F9' 80.0(6) . . ? F8 P2 F9' 162.0(7) . . ? F8' P2 F9' 90.8(7) . . ? F12' P2 F11 98.0(5) . . ? F7 P2 F11 92.0(4) . . ? F11' P2 F11 69.2(5) . . ? F10 P2 F11 91.9(4) . . ? F8 P2 F11 177.2(6) . . ? F8' P2 F11 106.2(7) . . ? F9' P2 F11 17.4(7) . . ? F12' P2 F9 28.4(7) . . ? F7 P2 F9 174.4(5) . . ? F11' P2 F9 112.2(5) . . ? F10 P2 F9 91.3(4) . . ? F8 P2 F9 90.7(5) . . ? F8' P2 F9 74.1(5) . . ? F9' P2 F9 74.8(5) . . ? F11 P2 F9 87.1(4) . . ? F12' P2 F12 58.0(5) . . ? F7 P2 F12 90.8(4) . . ? F11' P2 F12 36.5(4) . . ? F10 P2 F12 174.8(4) . . ? F8 P2 F12 89.1(6) . . ? F8' P2 F12 152.1(6) . . ? F9' P2 F12 99.6(5) . . ? F11 P2 F12 89.0(4) . . ? F9 P2 F12 83.6(3) . . ? F12' P2 F7' 93.7(8) . . ? F7 P2 F7' 68.8(7) . . ? F11' P2 F7' 92.7(8) . . ? F10 P2 F7' 98.7(7) . . ? F8 P2 F7' 22.6(10) . . ? F8' P2 F7' 90.1(8) . . ? F9' P2 F7' 174.1(8) . . ? F11 P2 F7' 158.6(8) . . ? F9 P2 F7' 111.1(8) . . ? F12 P2 F7' 82.2(7) . . ? F12' P2 F10' 178.5(7) . . ? F7 P2 F10' 34.7(4) . . ? F11' P2 F10' 89.3(6) . . ? F10 P2 F10' 61.8(5) . . ? F8 P2 F10' 101.3(6) . . ? F8' P2 F10' 82.7(6) . . ? F9' P2 F10' 87.1(5) . . ? F11 P2 F10' 81.4(4) . . ? F9 P2 F10' 150.1(4) . . ? F12 P2 F10' 123.4(5) . . ? F7' P2 F10' 87.2(7) . . ? F10' F7 P2 81.9(8) . . ? F10' F7 F11' 123.4(10) . . ? P2 F7 F11' 59.2(3) . . ? F8 F7' P2 70(2) . . ? F7' F8 P2 87(2) . . ? F10 F8' P2 75.5(14) . . ? F12' F9 P2 66.8(10) . . ? F8' F10 P2 81.2(15) . . ? F8' F10 F10' 135.3(19) . . ? P2 F10 F10' 63.6(4) . . ? F7 F10' F10 114.2(9) . . ? F7 F10' P2 63.3(6) . . ? F10 F10' P2 54.6(3) . . ? P2 F11 F11' 53.8(4) . . ? F12 F11' P2 77.7(6) . . ? F12 F11' F7 120.0(9) . . ? P2 F11' F7 58.4(4) . . ? F12 F11' F11 106.2(8) . . ? P2 F11' F11 57.1(4) . . ? F7 F11' F11 83.5(6) . . ? F11' F12 F12' 117.3(9) . . ? F11' F12 P2 65.8(7) . . ? F12' F12 P2 56.2(4) . . ? F9 F12' P2 84.8(11) . . ? F9 F12' F12 139.9(15) . . ? P2 F12' F12 65.9(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 Rh1 C3 N1 N2 -10.84(16) . . . . ? Rh2 C23 N11 N12 5.32(18) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.319 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.070 data_2+ _database_code_CSD 205490 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H41 Cl4 F6 N6 O P2 Rh' _chemical_formula_weight 1006.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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)/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 14.565(3) _cell_length_b 16.151(3) _cell_length_c 38.248(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.187(12) _cell_angle_gamma 90.00 _cell_volume 8882(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 45331 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15606 _reflns_number_gt 9178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0855P)^2^+12.3720P] 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 15606 _refine_ls_number_parameters 1067 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1284 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1865 _refine_ls_wR_factor_gt 0.1550 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.021 _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 0.41139(3) 0.57561(3) 0.092327(14) 0.02304(15) Uani 1 1 d . . . Rh2 Rh 0.90147(3) 0.87771(3) 0.094097(14) 0.02569(15) Uani 1 1 d . . . P1 P 0.41752(11) 0.63208(11) 0.14684(5) 0.0237(4) Uani 1 1 d . . . P2 P 0.91465(11) 0.82204(11) 0.14905(5) 0.0248(4) Uani 1 1 d . . . O1 O 0.2492(4) 0.6852(4) 0.07016(15) 0.0543(16) Uani 1 1 d . . . O2 O 0.7305(4) 0.7776(4) 0.07557(15) 0.0536(16) Uani 1 1 d . . . N6 N 0.5381(3) 0.5106(3) 0.10206(14) 0.0252(13) Uani 1 1 d . . . N3 N 0.5398(3) 0.4270(3) 0.09568(14) 0.0237(12) Uani 1 1 d . . . N2 N 0.4189(4) 0.3788(4) 0.13764(15) 0.0311(14) Uani 1 1 d . . . N1 N 0.3863(4) 0.3877(3) 0.10181(15) 0.0273(13) Uani 1 1 d . . . N4 N 0.3959(3) 0.5082(3) 0.04416(14) 0.0247(13) Uani 1 1 d . . . N5 N 0.4219(3) 0.4256(3) 0.04532(15) 0.0262(13) Uani 1 1 d . . . N16 N 1.0296(3) 0.9409(3) 0.10044(15) 0.0247(13) Uani 1 1 d . . . N15 N 1.0298(3) 1.0250(3) 0.09544(14) 0.0233(12) Uani 1 1 d . . . N12 N 0.9143(4) 1.0737(3) 0.13929(15) 0.0284(13) Uani 1 1 d . . . N11 N 0.8788(3) 1.0674(3) 0.10392(15) 0.0257(13) Uani 1 1 d . . . N14 N 0.8816(4) 0.9449(3) 0.04571(15) 0.0288(13) Uani 1 1 d . . . N13 N 0.9076(3) 1.0264(4) 0.04640(15) 0.0277(13) Uani 1 1 d . . . C1 C 0.3107(5) 0.6416(5) 0.07911(19) 0.0335(17) Uani 1 1 d . . . C2 C 0.4562(4) 0.3863(4) 0.07844(18) 0.0242(15) Uani 1 1 d . . . H2A H 0.4711 0.3286 0.0739 0.029 Uiso 1 1 calc R . . C3 C 0.6549(4) 0.6208(4) 0.1173(2) 0.0348(18) Uani 1 1 d . . . H3B H 0.6012 0.6558 0.1120 0.052 Uiso 1 1 calc R . . H3C H 0.6998 0.6360 0.1026 0.052 Uiso 1 1 calc R . . H3D H 0.6817 0.6271 0.1417 0.052 Uiso 1 1 calc R . . C4 C 0.6270(4) 0.5333(4) 0.11036(18) 0.0271(16) Uani 1 1 d . . . C5 C 0.6848(5) 0.4641(4) 0.10969(19) 0.0315(17) Uani 1 1 d . . . H5 H 0.7494 0.4639 0.1148 0.038 Uiso 1 1 calc R . . C6 C 0.6287(4) 0.3963(4) 0.10009(19) 0.0285(16) Uani 1 1 d . . . C7 C 0.6524(5) 0.3090(4) 0.0959(2) 0.043(2) Uani 1 1 d . . . H7A H 0.6276 0.2910 0.0724 0.064 Uiso 1 1 calc R . . H7B H 0.6262 0.2761 0.1128 0.064 Uiso 1 1 calc R . . H7C H 0.7187 0.3027 0.0998 0.064 Uiso 1 1 calc R . . C9 C 0.3511(7) 0.3557(6) 0.1912(2) 0.064(3) Uani 1 1 d . . . H9A H 0.4150 0.3612 0.2019 0.096 Uiso 1 1 calc R . . H9B H 0.3282 0.3025 0.1970 0.096 Uiso 1 1 calc R . . H9C H 0.3149 0.3985 0.1999 0.096 Uiso 1 1 calc R . . C10 C 0.3436(5) 0.3630(5) 0.1522(2) 0.041(2) Uani 1 1 d . . . C11 C 0.2638(5) 0.3583(5) 0.1258(2) 0.043(2) Uani 1 1 d . . . H11A H 0.2032 0.3479 0.1294 0.051 Uiso 1 1 calc R . . C12 C 0.2924(5) 0.3719(4) 0.0941(2) 0.0344(18) Uani 1 1 d . . . C13 C 0.2366(4) 0.3723(5) 0.0584(2) 0.046(2) Uani 1 1 d . . . H13A H 0.1742 0.3551 0.0598 0.068 Uiso 1 1 calc R . . H13B H 0.2636 0.3349 0.0434 0.068 Uiso 1 1 calc R . . H13C H 0.2356 0.4272 0.0487 0.068 Uiso 1 1 calc R . . C14 C 0.3309(5) 0.6076(5) -0.0020(2) 0.043(2) Uani 1 1 d . . . H14A H 0.3619 0.6498 0.0132 0.065 Uiso 1 1 calc R . . H14B H 0.2654 0.6095 -0.0012 0.065 Uiso 1 1 calc R . . H14C H 0.3413 0.6166 -0.0258 0.065 Uiso 1 1 calc R . . C15 C 0.3677(4) 0.5260(5) 0.01023(19) 0.0296(17) Uani 1 1 d . . . C16 C 0.3774(5) 0.4546(5) -0.0102(2) 0.0365(18) Uani 1 1 d . . . H16A H 0.3627 0.4509 -0.0347 0.044 Uiso 1 1 calc R . . C17 C 0.4114(5) 0.3930(5) 0.01170(19) 0.0331(18) Uani 1 1 d . . . C18 C 0.4311(5) 0.3047(5) 0.0048(2) 0.045(2) Uani 1 1 d . . . H18A H 0.4207 0.2948 -0.0203 0.067 Uiso 1 1 calc R . . H18B H 0.3907 0.2699 0.0158 0.067 Uiso 1 1 calc R . . H18C H 0.4947 0.2924 0.0143 0.067 Uiso 1 1 calc R . . C19 C 0.4066(4) 0.7445(4) 0.1483(2) 0.0295(17) Uani 1 1 d . . . C20 C 0.4377(5) 0.7911(4) 0.12205(19) 0.0321(17) Uani 1 1 d . . . H20A H 0.4582 0.7643 0.1032 0.038 Uiso 1 1 calc R . . C21 C 0.4386(5) 0.8775(5) 0.1234(2) 0.0417(19) Uani 1 1 d . . . H21A H 0.4590 0.9082 0.1056 0.050 Uiso 1 1 calc R . . C22 C 0.4087(5) 0.9169(5) 0.1519(2) 0.042(2) Uani 1 1 d . . . H22A H 0.4105 0.9743 0.1535 0.050 Uiso 1 1 calc R . . C23 C 0.3766(5) 0.8711(5) 0.1775(2) 0.041(2) Uani 1 1 d . . . H23A H 0.3558 0.8980 0.1962 0.049 Uiso 1 1 calc R . . C24 C 0.3745(5) 0.7854(4) 0.1760(2) 0.0353(18) Uani 1 1 d . . . H24A H 0.3516 0.7553 0.1934 0.042 Uiso 1 1 calc R . . C25 C 0.5205(4) 0.6112(4) 0.17972(18) 0.0265(16) Uani 1 1 d . . . C26 C 0.5748(5) 0.6739(5) 0.1969(2) 0.0385(19) Uani 1 1 d . . . H26A H 0.5598 0.7289 0.1916 0.046 Uiso 1 1 calc R . . C27 C 0.6518(5) 0.6550(5) 0.2221(2) 0.054(2) Uani 1 1 d . . . H27A H 0.6883 0.6973 0.2335 0.065 Uiso 1 1 calc R . . C28 C 0.6737(6) 0.5743(6) 0.2302(3) 0.068(3) Uani 1 1 d . . . H28A H 0.7249 0.5615 0.2471 0.082 Uiso 1 1 calc R . . C29 C 0.6200(6) 0.5122(6) 0.2132(3) 0.060(3) Uani 1 1 d . . . H29A H 0.6345 0.4572 0.2189 0.072 Uiso 1 1 calc R . . C30 C 0.5451(5) 0.5305(5) 0.1880(2) 0.0355(18) Uani 1 1 d . . . H30A H 0.5102 0.4877 0.1762 0.043 Uiso 1 1 calc R . . C31 C 0.3246(4) 0.5937(4) 0.16964(19) 0.0282(16) Uani 1 1 d . . . C32 C 0.3326(5) 0.5978(5) 0.2061(2) 0.0399(19) Uani 1 1 d . . . H32A H 0.3880 0.6163 0.2193 0.048 Uiso 1 1 calc R . . C33 C 0.2596(6) 0.5747(5) 0.2235(2) 0.052(2) Uani 1 1 d . . . H33A H 0.2656 0.5782 0.2481 0.063 Uiso 1 1 calc R . . C34 C 0.1767(6) 0.5461(6) 0.2034(3) 0.060(3) Uani 1 1 d . . . H34A H 0.1268 0.5318 0.2145 0.072 Uiso 1 1 calc R . . C35 C 0.1688(5) 0.5392(5) 0.1675(3) 0.054(2) Uani 1 1 d . . . H35A H 0.1145 0.5178 0.1546 0.065 Uiso 1 1 calc R . . C36 C 0.2415(5) 0.5638(5) 0.1501(2) 0.041(2) Uani 1 1 d . . . H36A H 0.2348 0.5604 0.1256 0.049 Uiso 1 1 calc R . . C51 C 0.7958(5) 0.8164(5) 0.08327(19) 0.0349(18) Uani 1 1 d . . . C52 C 0.9461(4) 1.0670(4) 0.07887(17) 0.0247(15) Uani 1 1 d . . . H52A H 0.9616 1.1243 0.0737 0.030 Uiso 1 1 calc R . . C53 C 1.1472(5) 0.8302(4) 0.1146(2) 0.0397(19) Uani 1 1 d . . . H53A H 1.0932 0.7953 0.1107 0.060 Uiso 1 1 calc R . . H53B H 1.1792 0.8226 0.1384 0.060 Uiso 1 1 calc R . . H53C H 1.1879 0.8158 0.0981 0.060 Uiso 1 1 calc R . . C54 C 1.1183(4) 0.9185(4) 0.10940(18) 0.0279(16) Uani 1 1 d . . . C55 C 1.1751(4) 0.9892(5) 0.11003(19) 0.0326(17) Uani 1 1 d . . . H55A H 1.2397 0.9902 0.1154 0.039 Uiso 1 1 calc R . . C56 C 1.1186(4) 1.0558(4) 0.10140(18) 0.0278(16) Uani 1 1 d . . . C57 C 1.1389(5) 1.1457(5) 0.0989(2) 0.043(2) Uani 1 1 d . . . H57A H 1.1179 1.1646 0.0752 0.065 Uiso 1 1 calc R . . H57B H 1.2047 1.1547 0.1049 0.065 Uiso 1 1 calc R . . H57C H 1.1073 1.1759 0.1150 0.065 Uiso 1 1 calc R . . C58 C 0.8521(6) 1.0954(6) 0.1935(2) 0.053(2) Uani 1 1 d . . . H58A H 0.9168 1.0905 0.2033 0.079 Uiso 1 1 calc R . . H58B H 0.8179 1.0513 0.2023 0.079 Uiso 1 1 calc R . . H58C H 0.8290 1.1477 0.2003 0.079 Uiso 1 1 calc R . . C59 C 0.8410(5) 1.0905(4) 0.1544(2) 0.0354(18) Uani 1 1 d . . . C60 C 0.7603(5) 1.0966(5) 0.1295(2) 0.0377(19) Uani 1 1 d . . . H60A H 0.7007 1.1070 0.1342 0.045 Uiso 1 1 calc R . . C61 C 0.7851(4) 1.0845(4) 0.09682(19) 0.0316(17) Uani 1 1 d . . . C62 C 0.7260(5) 1.0879(6) 0.0615(2) 0.050(2) Uani 1 1 d . . . H62A H 0.6627 1.0985 0.0643 0.074 Uiso 1 1 calc R . . H62B H 0.7294 1.0359 0.0496 0.074 Uiso 1 1 calc R . . H62C H 0.7475 1.1314 0.0478 0.074 Uiso 1 1 calc R . . C63 C 0.8127(6) 0.8424(5) 0.0012(2) 0.053(2) Uani 1 1 d . . . H63A H 0.8560 0.8020 0.0125 0.080 Uiso 1 1 calc R . . H63B H 0.8068 0.8369 -0.0240 0.080 Uiso 1 1 calc R . . H63C H 0.7531 0.8339 0.0084 0.080 Uiso 1 1 calc R . . C64 C 0.8473(5) 0.9278(5) 0.01200(19) 0.0344(17) Uani 1 1 d . . . C65 C 0.8544(5) 0.9964(5) -0.0090(2) 0.0396(19) Uani 1 1 d . . . H65A H 0.8362 0.9997 -0.0334 0.048 Uiso 1 1 calc R . . C66 C 0.8934(5) 1.0588(4) 0.01299(19) 0.0317(17) Uani 1 1 d . . . C67 C 0.9156(6) 1.1453(5) 0.0047(2) 0.048(2) Uani 1 1 d . . . H67A H 0.9772 1.1586 0.0163 0.072 Uiso 1 1 calc R . . H67B H 0.8717 1.1820 0.0129 0.072 Uiso 1 1 calc R . . H67C H 0.9123 1.1514 -0.0204 0.072 Uiso 1 1 calc R . . C68 C 1.0217(4) 0.8432(4) 0.18001(18) 0.0283(16) Uani 1 1 d . . . C69 C 1.0789(5) 0.7810(5) 0.19655(19) 0.0352(18) Uani 1 1 d . . . H69A H 1.0649 0.7257 0.1913 0.042 Uiso 1 1 calc R . . C70 C 1.1572(5) 0.8016(5) 0.2210(2) 0.043(2) Uani 1 1 d . . . H70A H 1.1958 0.7600 0.2318 0.051 Uiso 1 1 calc R . . C71 C 1.1774(5) 0.8829(6) 0.2290(2) 0.050(2) Uani 1 1 d . . . H71A H 1.2283 0.8961 0.2461 0.060 Uiso 1 1 calc R . . C72 C 1.1234(5) 0.9450(5) 0.2122(2) 0.049(2) Uani 1 1 d . . . H72A H 1.1390 1.0000 0.2173 0.058 Uiso 1 1 calc R . . C73 C 1.0445(5) 0.9261(5) 0.1870(2) 0.0371(18) Uani 1 1 d . . . H73A H 1.0082 0.9681 0.1754 0.045 Uiso 1 1 calc R . . C74 C 0.8250(5) 0.8600(4) 0.1740(2) 0.0320(17) Uani 1 1 d . . . C75 C 0.7411(5) 0.8900(5) 0.1565(2) 0.042(2) Uani 1 1 d . . . H75A H 0.7308 0.8946 0.1319 0.050 Uiso 1 1 calc R . . C76 C 0.6721(5) 0.9134(6) 0.1760(3) 0.057(3) Uani 1 1 d . . . H76A H 0.6156 0.9331 0.1642 0.068 Uiso 1 1 calc R . . C77 C 0.6864(6) 0.9079(5) 0.2123(3) 0.057(3) Uani 1 1 d . . . H77A H 0.6396 0.9235 0.2249 0.068 Uiso 1 1 calc R . . C78 C 0.7713(6) 0.8788(5) 0.2303(2) 0.048(2) Uani 1 1 d . . . H78A H 0.7817 0.8747 0.2548 0.058 Uiso 1 1 calc R . . C79 C 0.8404(5) 0.8561(4) 0.2107(2) 0.0384(18) Uani 1 1 d . . . H79A H 0.8977 0.8380 0.2224 0.046 Uiso 1 1 calc R . . C80 C 0.9054(4) 0.7095(4) 0.15076(19) 0.0288(16) Uani 1 1 d . . . C81 C 0.8819(5) 0.6679(5) 0.1803(2) 0.044(2) Uani 1 1 d . . . H81A H 0.8648 0.6979 0.1990 0.053 Uiso 1 1 calc R . . C82 C 0.8842(5) 0.5817(5) 0.1817(3) 0.052(2) Uani 1 1 d . . . H82A H 0.8681 0.5543 0.2012 0.062 Uiso 1 1 calc R . . C83 C 0.9102(5) 0.5368(5) 0.1540(3) 0.048(2) Uani 1 1 d . . . H83A H 0.9133 0.4794 0.1552 0.057 Uiso 1 1 calc R . . C84 C 0.9310(5) 0.5766(5) 0.1256(2) 0.047(2) Uani 1 1 d . . . H84A H 0.9462 0.5462 0.1067 0.056 Uiso 1 1 calc R . . C85 C 0.9302(5) 0.6628(5) 0.1238(2) 0.0393(19) Uani 1 1 d . . . H85A H 0.9467 0.6890 0.1041 0.047 Uiso 1 1 calc R . . C100 C 0.4414(6) 0.9128(5) 0.0190(2) 0.057(2) Uani 1 1 d . . . H10A H 0.4201 0.9656 0.0268 0.069 Uiso 1 1 calc R . . H10B H 0.4424 0.9166 -0.0062 0.069 Uiso 1 1 calc R . . C102 C 0.9634(9) 0.7556(8) 0.3190(3) 0.104(4) Uani 1 1 d . . . H10C H 1.0061 0.7170 0.3325 0.125 Uiso 1 1 calc R . . H10D H 0.9371 0.7902 0.3356 0.125 Uiso 1 1 calc R . . C103 C 0.9524(9) 0.5926(12) 0.0191(4) 0.171(8) Uani 1 1 d . . . H10E H 0.9509 0.6121 -0.0050 0.205 Uiso 1 1 calc R . . H10F H 0.9523 0.5326 0.0182 0.205 Uiso 1 1 calc R . . P3 P 0.42817(13) 0.12475(12) 0.08650(6) 0.0367(5) Uani 1 1 d . . . F1 F 0.3768(3) 0.1155(3) 0.12016(14) 0.0675(16) Uani 1 1 d . . . F2 F 0.3520(3) 0.1914(3) 0.06979(14) 0.0643(15) Uani 1 1 d . . . F3 F 0.4878(4) 0.1976(3) 0.10510(19) 0.093(2) Uani 1 1 d . . . F4 F 0.4799(4) 0.1358(5) 0.05373(16) 0.110(3) Uani 1 1 d . . . F5 F 0.5052(3) 0.0610(3) 0.10326(17) 0.0776(18) Uani 1 1 d . . . F6 F 0.3645(4) 0.0526(4) 0.0694(2) 0.108(2) Uani 1 1 d . . . Cl1 Cl 0.55541(17) 0.89343(17) 0.04131(7) 0.0694(7) Uani 1 1 d . . . Cl2 Cl 0.36397(17) 0.83530(15) 0.02689(7) 0.0669(7) Uani 1 1 d . . . Cl5 Cl 1.0258(3) 0.8188(3) 0.29312(10) 0.1344(15) Uani 1 1 d . . . Cl6 Cl 0.8763(3) 0.7016(2) 0.29394(12) 0.1309(14) Uani 1 1 d . . . Cl7 Cl 0.8538(3) 0.6220(3) 0.03198(11) 0.1472(16) Uani 1 1 d . . . Cl8 Cl 1.0533(3) 0.6219(5) 0.04235(14) 0.250(4) Uani 1 1 d . . . P4 P 0.94009(14) 0.33760(13) 0.07842(6) 0.0436(5) Uani 1 1 d D . . F7 F 0.8787(4) 0.3720(4) 0.10486(19) 0.103(2) Uani 1 1 d D . . F8 F 0.9409(6) 0.2513(3) 0.0965(2) 0.124(3) Uani 1 1 d D . . F9 F 1.0052(4) 0.2993(4) 0.05251(15) 0.0787(18) Uani 1 1 d D . . F10 F 1.0262(4) 0.3670(5) 0.10447(17) 0.120(3) Uani 1 1 d D . . F11 F 0.8527(4) 0.3045(5) 0.0537(2) 0.144(4) Uani 1 1 d D . . F12 F 0.9402(10) 0.4210(4) 0.0602(2) 0.215(6) Uani 1 1 d D . . Cl3 Cl 0.5024(6) 0.6216(6) 0.29140(16) 0.244(5) Uani 0.783(6) 1 d PD A 1 Cl4 Cl 0.3712(5) 0.7542(4) 0.2923(2) 0.161(4) Uani 0.783(6) 1 d PD A 1 C101 C 0.4609(9) 0.6979(9) 0.3158(4) 0.110(6) Uani 0.783(6) 1 d PD A 1 H10G H 0.5114 0.7354 0.3246 0.132 Uiso 0.783(6) 1 calc PR A 1 H10H H 0.4395 0.6730 0.3361 0.132 Uiso 0.783(6) 1 calc PR A 1 Cl11 Cl 0.2818(10) 0.8010(9) 0.3162(3) 0.094(6) Uani 0.217(6) 1 d PD A 2 Cl12 Cl 0.4234(11) 0.7783(9) 0.2706(3) 0.083(5) Uani 0.217(6) 1 d PD A 2 C105 C 0.3980(19) 0.770(3) 0.3144(7) 0.051(11) Uani 0.217(6) 1 d PDU A 2 H10I H 0.4071 0.7137 0.3226 0.061 Uiso 0.217(6) 1 calc PR A 2 H10J H 0.4404 0.8054 0.3301 0.061 Uiso 0.217(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0185(3) 0.0239(3) 0.0262(3) 0.0001(2) 0.0022(2) 0.0018(2) Rh2 0.0205(3) 0.0286(3) 0.0267(3) -0.0037(3) -0.0005(2) -0.0001(2) P1 0.0200(9) 0.0210(9) 0.0297(10) 0.0008(8) 0.0024(7) 0.0023(7) P2 0.0224(9) 0.0240(10) 0.0266(10) -0.0035(8) -0.0006(7) -0.0004(7) O1 0.049(4) 0.060(4) 0.049(4) -0.001(3) -0.007(3) 0.028(3) O2 0.045(3) 0.058(4) 0.051(4) 0.008(3) -0.012(3) -0.026(3) N6 0.017(3) 0.027(3) 0.031(3) 0.000(3) 0.003(2) -0.002(2) N3 0.019(3) 0.019(3) 0.034(3) -0.001(3) 0.007(2) 0.001(2) N2 0.033(3) 0.032(3) 0.031(4) -0.001(3) 0.012(3) -0.006(3) N1 0.026(3) 0.027(3) 0.031(4) 0.000(3) 0.010(2) -0.004(2) N4 0.017(3) 0.030(3) 0.026(3) -0.001(3) -0.001(2) -0.003(2) N5 0.023(3) 0.024(3) 0.032(3) -0.003(3) 0.007(2) -0.004(2) N16 0.021(3) 0.024(3) 0.030(3) -0.001(3) 0.005(2) 0.002(2) N15 0.017(3) 0.030(3) 0.023(3) -0.005(3) 0.005(2) 0.002(2) N12 0.030(3) 0.030(3) 0.025(3) -0.007(3) 0.004(3) 0.003(3) N11 0.018(3) 0.031(3) 0.029(3) -0.005(3) 0.005(2) 0.006(2) N14 0.025(3) 0.031(3) 0.030(4) -0.002(3) 0.001(2) -0.003(3) N13 0.020(3) 0.035(4) 0.028(3) -0.003(3) 0.004(2) 0.006(3) C1 0.033(4) 0.036(4) 0.030(4) -0.003(3) 0.001(3) 0.005(3) C2 0.019(3) 0.019(4) 0.035(4) 0.002(3) 0.006(3) 0.000(3) C3 0.020(4) 0.027(4) 0.058(5) 0.000(4) 0.008(3) -0.006(3) C4 0.026(4) 0.028(4) 0.028(4) -0.003(3) 0.009(3) -0.001(3) C5 0.020(4) 0.030(4) 0.044(5) -0.001(4) 0.005(3) 0.001(3) C6 0.018(3) 0.029(4) 0.039(4) 0.007(3) 0.006(3) 0.002(3) C7 0.031(4) 0.031(4) 0.069(6) 0.007(4) 0.016(4) 0.008(3) C9 0.082(7) 0.075(7) 0.044(6) 0.003(5) 0.036(5) -0.002(5) C10 0.052(5) 0.032(4) 0.043(5) 0.002(4) 0.027(4) -0.004(4) C11 0.034(4) 0.039(5) 0.060(6) 0.000(4) 0.026(4) -0.006(4) C12 0.023(4) 0.026(4) 0.055(5) -0.001(4) 0.008(3) -0.007(3) C13 0.014(4) 0.061(6) 0.062(6) 0.001(5) 0.006(3) -0.004(4) C14 0.049(5) 0.046(5) 0.033(5) 0.009(4) 0.000(4) 0.001(4) C15 0.016(3) 0.039(4) 0.034(4) 0.011(4) 0.004(3) -0.004(3) C16 0.038(4) 0.043(5) 0.030(4) -0.004(4) 0.009(3) -0.012(4) C17 0.029(4) 0.042(5) 0.029(4) -0.010(4) 0.006(3) -0.010(3) C18 0.050(5) 0.043(5) 0.043(5) -0.023(4) 0.013(4) -0.009(4) C19 0.026(4) 0.018(4) 0.044(5) 0.008(3) 0.002(3) 0.008(3) C20 0.036(4) 0.026(4) 0.033(4) 0.003(3) 0.002(3) 0.003(3) C21 0.051(5) 0.027(4) 0.044(5) 0.005(4) 0.000(4) -0.003(4) C22 0.027(4) 0.030(4) 0.064(6) 0.004(4) -0.006(4) -0.002(3) C23 0.044(5) 0.029(4) 0.052(5) -0.014(4) 0.012(4) 0.003(4) C24 0.036(4) 0.030(4) 0.042(5) -0.001(4) 0.012(3) 0.003(3) C25 0.021(3) 0.027(4) 0.030(4) -0.002(3) -0.001(3) -0.001(3) C26 0.039(4) 0.037(5) 0.038(5) -0.002(4) 0.001(3) 0.005(4) C27 0.040(5) 0.045(5) 0.069(7) -0.021(5) -0.018(4) 0.000(4) C28 0.046(5) 0.065(7) 0.079(7) -0.013(6) -0.037(5) 0.023(5) C29 0.048(5) 0.047(6) 0.074(7) 0.003(5) -0.026(5) 0.014(4) C30 0.032(4) 0.030(4) 0.042(5) 0.000(4) 0.000(3) 0.002(3) C31 0.024(4) 0.026(4) 0.035(4) 0.003(3) 0.007(3) 0.007(3) C32 0.047(5) 0.037(5) 0.041(5) 0.001(4) 0.022(4) 0.005(4) C33 0.081(7) 0.041(5) 0.044(5) 0.013(4) 0.037(5) 0.008(5) C34 0.052(6) 0.058(6) 0.079(8) 0.021(5) 0.037(5) 0.007(5) C35 0.030(5) 0.055(6) 0.081(7) 0.013(5) 0.014(4) -0.001(4) C36 0.025(4) 0.050(5) 0.048(5) 0.007(4) 0.008(3) 0.006(3) C51 0.038(4) 0.039(5) 0.026(4) 0.008(3) 0.000(3) 0.004(4) C52 0.023(3) 0.032(4) 0.020(4) 0.002(3) 0.006(3) 0.004(3) C53 0.032(4) 0.039(5) 0.048(5) 0.000(4) 0.007(3) 0.013(3) C54 0.018(3) 0.035(4) 0.029(4) -0.004(3) 0.000(3) 0.009(3) C55 0.015(3) 0.046(5) 0.037(4) 0.001(4) 0.004(3) 0.000(3) C56 0.022(4) 0.036(4) 0.026(4) -0.002(3) 0.004(3) -0.001(3) C57 0.027(4) 0.047(5) 0.058(6) 0.005(4) 0.011(4) -0.008(4) C58 0.062(6) 0.064(6) 0.038(5) -0.003(4) 0.028(4) 0.015(5) C59 0.039(4) 0.033(4) 0.039(5) -0.001(4) 0.019(4) 0.009(3) C60 0.022(4) 0.046(5) 0.048(5) 0.002(4) 0.016(3) 0.012(3) C61 0.020(4) 0.037(4) 0.039(5) 0.002(4) 0.007(3) 0.011(3) C62 0.021(4) 0.077(6) 0.049(5) -0.001(5) 0.000(3) 0.014(4) C63 0.061(6) 0.066(6) 0.033(5) -0.009(4) 0.006(4) -0.011(5) C64 0.028(4) 0.044(5) 0.029(4) -0.006(4) -0.002(3) 0.003(3) C65 0.043(5) 0.052(5) 0.023(4) 0.000(4) 0.007(3) 0.007(4) C66 0.035(4) 0.030(4) 0.029(4) -0.001(3) 0.003(3) 0.002(3) C67 0.056(5) 0.043(5) 0.046(5) 0.007(4) 0.013(4) 0.006(4) C68 0.026(4) 0.031(4) 0.027(4) -0.001(3) 0.002(3) 0.000(3) C69 0.035(4) 0.036(4) 0.033(4) -0.004(4) -0.002(3) -0.003(3) C70 0.027(4) 0.053(5) 0.042(5) -0.001(4) -0.012(3) 0.004(4) C71 0.028(4) 0.060(6) 0.052(6) -0.002(5) -0.025(4) -0.009(4) C72 0.044(5) 0.043(5) 0.054(6) -0.005(4) -0.007(4) -0.017(4) C73 0.029(4) 0.031(4) 0.047(5) 0.003(4) -0.006(3) -0.002(3) C74 0.028(4) 0.029(4) 0.040(5) -0.005(3) 0.008(3) -0.010(3) C75 0.029(4) 0.053(5) 0.042(5) -0.012(4) 0.002(3) 0.000(4) C76 0.022(4) 0.074(7) 0.074(7) -0.017(5) 0.010(4) 0.000(4) C77 0.049(6) 0.054(6) 0.077(7) -0.006(5) 0.042(5) 0.003(4) C78 0.055(5) 0.047(5) 0.049(6) -0.007(4) 0.025(4) -0.005(4) C79 0.044(5) 0.033(4) 0.039(5) 0.001(4) 0.008(4) -0.001(4) C80 0.019(3) 0.027(4) 0.036(4) -0.004(3) -0.010(3) -0.003(3) C81 0.045(5) 0.036(5) 0.051(5) -0.003(4) 0.003(4) -0.006(4) C82 0.043(5) 0.032(5) 0.079(7) 0.012(5) 0.004(4) -0.003(4) C83 0.038(5) 0.022(4) 0.079(7) -0.005(5) -0.004(4) -0.001(4) C84 0.047(5) 0.038(5) 0.051(6) -0.017(4) -0.006(4) 0.011(4) C85 0.034(4) 0.040(5) 0.042(5) -0.009(4) -0.002(3) 0.004(4) C100 0.074(6) 0.050(6) 0.047(6) 0.002(4) 0.007(5) 0.006(5) C102 0.149(12) 0.113(11) 0.057(8) 0.011(7) 0.039(8) 0.038(9) C103 0.089(11) 0.29(2) 0.132(15) 0.067(15) 0.010(10) -0.068(13) P3 0.0299(10) 0.0315(11) 0.0496(13) 0.0035(10) 0.0094(9) 0.0002(9) F1 0.051(3) 0.081(4) 0.075(4) 0.036(3) 0.025(3) 0.007(3) F2 0.055(3) 0.073(4) 0.067(4) 0.031(3) 0.016(3) 0.026(3) F3 0.075(4) 0.059(4) 0.138(6) -0.004(4) -0.005(4) -0.030(3) F4 0.108(5) 0.162(7) 0.076(5) 0.051(4) 0.061(4) 0.072(5) F5 0.049(3) 0.055(3) 0.132(5) 0.044(3) 0.025(3) 0.021(3) F6 0.081(4) 0.082(5) 0.150(7) -0.055(4) -0.015(4) -0.013(4) Cl1 0.0579(15) 0.0788(18) 0.0709(18) -0.0133(14) 0.0082(12) 0.0063(13) Cl2 0.0731(16) 0.0621(16) 0.0601(16) 0.0175(13) -0.0059(12) -0.0110(13) Cl5 0.141(3) 0.180(4) 0.076(3) 0.014(3) 0.000(2) -0.029(3) Cl6 0.116(3) 0.121(3) 0.140(4) 0.035(3) -0.028(2) -0.001(2) Cl7 0.140(4) 0.192(5) 0.097(3) 0.002(3) -0.019(2) -0.005(3) Cl8 0.138(4) 0.486(11) 0.129(4) -0.043(5) 0.027(3) -0.162(6) P4 0.0352(11) 0.0352(12) 0.0583(15) -0.0044(11) 0.0015(10) 0.0036(9) F7 0.048(3) 0.114(5) 0.151(6) -0.081(5) 0.031(4) 0.013(3) F8 0.205(8) 0.041(4) 0.153(7) 0.004(4) 0.109(6) 0.011(4) F9 0.067(4) 0.099(5) 0.077(4) -0.032(3) 0.034(3) -0.026(3) F10 0.049(4) 0.224(8) 0.091(5) -0.072(5) 0.021(3) -0.048(4) F11 0.058(4) 0.213(9) 0.147(7) -0.109(7) -0.030(4) 0.048(5) F12 0.476(19) 0.060(5) 0.115(8) 0.036(5) 0.072(10) 0.057(8) Cl3 0.281(9) 0.325(11) 0.092(5) -0.069(6) -0.080(5) 0.141(8) Cl4 0.156(6) 0.107(5) 0.182(8) -0.019(5) -0.090(6) 0.009(4) C101 0.077(11) 0.138(16) 0.106(14) -0.026(12) -0.011(9) -0.014(11) Cl11 0.139(13) 0.079(10) 0.050(8) 0.016(7) -0.023(7) -0.056(9) Cl12 0.115(12) 0.082(10) 0.041(7) -0.007(7) -0.017(7) -0.040(8) C105 0.058(14) 0.053(14) 0.039(13) 0.007(9) 0.001(9) -0.007(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.818(7) . ? Rh1 N6 2.104(5) . ? Rh1 N4 2.121(5) . ? Rh1 P1 2.2642(19) . ? Rh1 C2 3.188(6) . ? Rh1 N2 3.614(6) . ? Rh2 C51 1.821(8) . ? Rh2 N16 2.106(5) . ? Rh2 N14 2.125(6) . ? Rh2 P2 2.266(2) . ? Rh2 C52 3.198(7) . ? Rh2 N12 3.597(5) . ? P1 C19 1.824(7) . ? P1 C25 1.829(7) . ? P1 C31 1.831(7) . ? P2 C80 1.825(7) . ? P2 C68 1.833(7) . ? P2 C74 1.842(7) . ? O1 C1 1.148(8) . ? O2 C51 1.138(8) . ? N6 C4 1.334(8) . ? N6 N3 1.373(7) . ? N3 C6 1.371(7) . ? N3 C2 1.446(8) . ? N2 C10 1.330(8) . ? N2 N1 1.384(8) . ? N1 C12 1.377(8) . ? N1 C2 1.458(8) . ? N4 C15 1.329(8) . ? N4 N5 1.385(7) . ? N5 C17 1.375(9) . ? N5 C2 1.433(8) . ? N16 C54 1.332(8) . ? N16 N15 1.372(7) . ? N15 C56 1.370(8) . ? N15 C52 1.449(8) . ? N12 C59 1.321(8) . ? N12 N11 1.372(7) . ? N11 C61 1.378(8) . ? N11 C52 1.476(8) . ? N14 C64 1.335(9) . ? N14 N13 1.369(7) . ? N13 C66 1.366(9) . ? N13 C52 1.437(8) . ? C3 C4 1.482(9) . ? C4 C5 1.402(9) . ? C5 C6 1.380(9) . ? C6 C7 1.467(9) . ? C9 C10 1.484(11) . ? C10 C11 1.415(11) . ? C11 C12 1.359(10) . ? C12 C13 1.475(10) . ? C14 C15 1.470(10) . ? C15 C16 1.412(10) . ? C16 C17 1.345(10) . ? C17 C18 1.486(10) . ? C19 C20 1.388(9) . ? C19 C24 1.389(9) . ? C20 C21 1.397(9) . ? C21 C22 1.389(11) . ? C22 C23 1.367(11) . ? C23 C24 1.386(9) . ? C25 C30 1.375(9) . ? C25 C26 1.385(9) . ? C26 C27 1.391(10) . ? C27 C28 1.365(12) . ? C28 C29 1.369(12) . ? C29 C30 1.370(10) . ? C31 C32 1.382(10) . ? C31 C36 1.403(10) . ? C32 C33 1.395(10) . ? C33 C34 1.403(13) . ? C34 C35 1.360(12) . ? C35 C36 1.396(10) . ? C53 C54 1.492(9) . ? C54 C55 1.408(9) . ? C55 C56 1.363(9) . ? C56 C57 1.489(10) . ? C58 C59 1.481(10) . ? C59 C60 1.394(10) . ? C60 C61 1.368(10) . ? C61 C62 1.482(10) . ? C63 C64 1.503(10) . ? C64 C65 1.380(10) . ? C65 C66 1.375(10) . ? C66 C67 1.480(10) . ? C68 C69 1.391(10) . ? C68 C73 1.395(9) . ? C69 C70 1.394(10) . ? C70 C71 1.370(11) . ? C71 C72 1.371(11) . ? C72 C73 1.409(10) . ? C74 C79 1.384(10) . ? C74 C75 1.385(10) . ? C75 C76 1.395(10) . ? C76 C77 1.374(12) . ? C77 C78 1.396(12) . ? C78 C79 1.396(10) . ? C80 C85 1.370(10) . ? C80 C81 1.402(10) . ? C81 C82 1.394(10) . ? C82 C83 1.384(12) . ? C83 C84 1.338(11) . ? C84 C85 1.394(10) . ? C100 Cl2 1.743(9) . ? C100 Cl1 1.769(9) . ? C102 Cl6 1.703(14) . ? C102 Cl5 1.770(12) . ? C103 Cl7 1.660(16) . ? C103 Cl8 1.661(14) . ? P3 F3 1.564(6) . ? P3 F6 1.567(6) . ? P3 F4 1.572(5) . ? P3 F5 1.581(5) . ? P3 F1 1.596(5) . ? P3 F2 1.603(5) . ? P4 F12 1.517(7) . ? P4 F10 1.546(6) . ? P4 F11 1.554(6) . ? P4 F7 1.556(5) . ? P4 F8 1.556(6) . ? P4 F9 1.601(5) . ? Cl3 C101 1.713(13) . ? Cl4 C101 1.722(13) . ? Cl11 C105 1.775(19) . ? Cl12 C105 1.776(19) . ? 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 C1 Rh1 N6 170.9(3) . . ? C1 Rh1 N4 95.2(3) . . ? N6 Rh1 N4 82.3(2) . . ? C1 Rh1 P1 86.1(2) . . ? N6 Rh1 P1 97.68(16) . . ? N4 Rh1 P1 171.76(15) . . ? C1 Rh1 C2 133.9(3) . . ? N6 Rh1 C2 49.75(18) . . ? N4 Rh1 C2 50.13(19) . . ? P1 Rh1 C2 124.10(13) . . ? C1 Rh1 N2 127.6(2) . . ? N6 Rh1 N2 61.17(17) . . ? N4 Rh1 N2 87.45(18) . . ? P1 Rh1 N2 85.36(10) . . ? C2 Rh1 N2 40.98(15) . . ? C51 Rh2 N16 172.0(3) . . ? C51 Rh2 N14 95.0(3) . . ? N16 Rh2 N14 81.3(2) . . ? C51 Rh2 P2 86.5(2) . . ? N16 Rh2 P2 98.22(16) . . ? N14 Rh2 P2 171.94(16) . . ? C51 Rh2 C52 131.9(2) . . ? N16 Rh2 C52 49.91(18) . . ? N14 Rh2 C52 49.96(19) . . ? P2 Rh2 C52 123.96(13) . . ? C51 Rh2 N12 124.4(2) . . ? N16 Rh2 N12 62.71(16) . . ? N14 Rh2 N12 87.63(18) . . ? P2 Rh2 N12 85.02(10) . . ? C52 Rh2 N12 41.40(14) . . ? C19 P1 C25 103.2(3) . . ? C19 P1 C31 104.3(3) . . ? C25 P1 C31 101.4(3) . . ? C19 P1 Rh1 116.0(2) . . ? C25 P1 Rh1 117.8(2) . . ? C31 P1 Rh1 112.3(2) . . ? C80 P2 C68 102.9(3) . . ? C80 P2 C74 104.5(3) . . ? C68 P2 C74 101.7(3) . . ? C80 P2 Rh2 115.6(2) . . ? C68 P2 Rh2 117.6(2) . . ? C74 P2 Rh2 112.8(2) . . ? C4 N6 N3 105.6(5) . . ? C4 N6 Rh1 134.1(5) . . ? N3 N6 Rh1 119.9(4) . . ? C6 N3 N6 112.1(5) . . ? C6 N3 C2 127.0(5) . . ? N6 N3 C2 119.4(5) . . ? C10 N2 N1 105.0(6) . . ? C10 N2 Rh1 113.9(5) . . ? N1 N2 Rh1 57.0(3) . . ? C12 N1 N2 111.3(5) . . ? C12 N1 C2 129.3(6) . . ? N2 N1 C2 116.3(5) . . ? C15 N4 N5 106.3(5) . . ? C15 N4 Rh1 135.3(5) . . ? N5 N4 Rh1 118.4(4) . . ? C17 N5 N4 110.5(6) . . ? C17 N5 C2 128.9(6) . . ? N4 N5 C2 120.6(5) . . ? C54 N16 N15 106.3(5) . . ? C54 N16 Rh2 134.7(5) . . ? N15 N16 Rh2 119.0(4) . . ? C56 N15 N16 111.1(5) . . ? C56 N15 C52 127.4(6) . . ? N16 N15 C52 120.3(5) . . ? C59 N12 N11 104.1(6) . . ? C59 N12 Rh2 114.0(4) . . ? N11 N12 Rh2 58.6(3) . . ? N12 N11 C61 112.6(5) . . ? N12 N11 C52 117.1(5) . . ? C61 N11 C52 127.8(6) . . ? C64 N14 N13 106.1(6) . . ? C64 N14 Rh2 135.5(5) . . ? N13 N14 Rh2 118.4(4) . . ? C66 N13 N14 110.5(6) . . ? C66 N13 C52 127.9(6) . . ? N14 N13 C52 121.6(6) . . ? O1 C1 Rh1 177.4(7) . . ? N5 C2 N3 110.6(5) . . ? N5 C2 N1 110.9(5) . . ? N3 C2 N1 109.4(5) . . ? N5 C2 Rh1 70.8(3) . . ? N3 C2 Rh1 70.6(3) . . ? N1 C2 Rh1 72.7(3) . . ? N6 C4 C5 109.9(6) . . ? N6 C4 C3 122.1(6) . . ? C5 C4 C3 127.9(6) . . ? C6 C5 C4 107.7(6) . . ? N3 C6 C5 104.7(6) . . ? N3 C6 C7 124.6(6) . . ? C5 C6 C7 130.7(6) . . ? N2 C10 C11 110.5(7) . . ? N2 C10 C9 120.2(8) . . ? C11 C10 C9 129.2(7) . . ? C12 C11 C10 107.0(6) . . ? C11 C12 N1 106.0(7) . . ? C11 C12 C13 128.7(7) . . ? N1 C12 C13 125.3(6) . . ? N4 C15 C16 108.8(6) . . ? N4 C15 C14 123.0(7) . . ? C16 C15 C14 128.3(7) . . ? C17 C16 C15 108.6(7) . . ? C16 C17 N5 105.9(7) . . ? C16 C17 C18 131.4(7) . . ? N5 C17 C18 122.6(7) . . ? C20 C19 C24 118.8(6) . . ? C20 C19 P1 118.4(5) . . ? C24 C19 P1 122.6(5) . . ? C19 C20 C21 121.1(7) . . ? C22 C21 C20 119.0(7) . . ? C23 C22 C21 119.9(7) . . ? C22 C23 C24 121.2(7) . . ? C23 C24 C19 119.9(7) . . ? C30 C25 C26 118.4(7) . . ? C30 C25 P1 119.2(5) . . ? C26 C25 P1 122.4(5) . . ? C25 C26 C27 120.3(7) . . ? C28 C27 C26 120.0(8) . . ? C27 C28 C29 119.8(8) . . ? C28 C29 C30 120.4(8) . . ? C29 C30 C25 121.1(7) . . ? C32 C31 C36 118.6(6) . . ? C32 C31 P1 121.0(5) . . ? C36 C31 P1 120.3(6) . . ? C31 C32 C33 121.5(8) . . ? C32 C33 C34 118.6(8) . . ? C35 C34 C33 120.6(8) . . ? C34 C35 C36 120.5(9) . . ? C35 C36 C31 120.0(8) . . ? O2 C51 Rh2 178.0(7) . . ? N13 C52 N15 110.5(5) . . ? N13 C52 N11 110.8(5) . . ? N15 C52 N11 108.5(5) . . ? N13 C52 Rh2 70.0(4) . . ? N15 C52 Rh2 69.8(3) . . ? N11 C52 Rh2 73.2(3) . . ? N16 C54 C55 109.2(6) . . ? N16 C54 C53 122.3(6) . . ? C55 C54 C53 128.3(6) . . ? C56 C55 C54 107.7(6) . . ? C55 C56 N15 105.7(6) . . ? C55 C56 C57 131.8(6) . . ? N15 C56 C57 122.4(6) . . ? N12 C59 C60 111.5(7) . . ? N12 C59 C58 119.2(7) . . ? C60 C59 C58 129.2(6) . . ? C61 C60 C59 107.4(6) . . ? C60 C61 N11 104.3(6) . . ? C60 C61 C62 128.8(6) . . ? N11 C61 C62 126.9(6) . . ? N14 C64 C65 110.2(7) . . ? N14 C64 C63 120.7(7) . . ? C65 C64 C63 129.0(7) . . ? C66 C65 C64 107.1(7) . . ? N13 C66 C65 106.1(6) . . ? N13 C66 C67 123.8(7) . . ? C65 C66 C67 130.1(7) . . ? C69 C68 C73 119.9(6) . . ? C69 C68 P2 123.1(5) . . ? C73 C68 P2 117.1(5) . . ? C68 C69 C70 119.9(7) . . ? C71 C70 C69 120.3(7) . . ? C70 C71 C72 120.5(7) . . ? C71 C72 C73 120.4(7) . . ? C68 C73 C72 118.9(7) . . ? C79 C74 C75 119.6(7) . . ? C79 C74 P2 119.8(6) . . ? C75 C74 P2 120.6(6) . . ? C74 C75 C76 119.4(8) . . ? C77 C76 C75 121.1(8) . . ? C76 C77 C78 119.9(7) . . ? C79 C78 C77 118.8(8) . . ? C74 C79 C78 121.2(8) . . ? C85 C80 C81 118.0(7) . . ? C85 C80 P2 119.4(6) . . ? C81 C80 P2 122.3(6) . . ? C82 C81 C80 120.1(8) . . ? C83 C82 C81 120.1(8) . . ? C84 C83 C82 119.6(8) . . ? C83 C84 C85 121.2(8) . . ? C80 C85 C84 120.9(8) . . ? Cl2 C100 Cl1 111.9(5) . . ? Cl6 C102 Cl5 112.6(7) . . ? Cl7 C103 Cl8 119.5(12) . . ? F3 P3 F6 176.7(4) . . ? F3 P3 F4 88.6(4) . . ? F6 P3 F4 94.5(4) . . ? F3 P3 F5 90.0(3) . . ? F6 P3 F5 91.1(3) . . ? F4 P3 F5 89.9(3) . . ? F3 P3 F1 90.0(3) . . ? F6 P3 F1 86.9(4) . . ? F4 P3 F1 178.7(4) . . ? F5 P3 F1 90.3(3) . . ? F3 P3 F2 88.6(3) . . ? F6 P3 F2 90.4(3) . . ? F4 P3 F2 89.7(3) . . ? F5 P3 F2 178.5(3) . . ? F1 P3 F2 90.0(3) . . ? F12 P4 F10 87.9(6) . . ? F12 P4 F11 95.0(6) . . ? F10 P4 F11 176.9(5) . . ? F12 P4 F7 91.4(5) . . ? F10 P4 F7 87.9(3) . . ? F11 P4 F7 91.0(3) . . ? F12 P4 F8 178.9(5) . . ? F10 P4 F8 92.3(5) . . ? F11 P4 F8 84.8(5) . . ? F7 P4 F8 89.7(4) . . ? F12 P4 F9 90.8(5) . . ? F10 P4 F9 91.0(3) . . ? F11 P4 F9 89.9(3) . . ? F7 P4 F9 177.5(4) . . ? F8 P4 F9 88.1(3) . . ? Cl3 C101 Cl4 113.5(9) . . ? Cl11 C105 Cl12 111.1(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 C2 N1 N2 -97.6(5) . . . . ? Rh2 C52 N11 N12 95.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.750 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.111 data_6 _database_code_CSD 205491 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H44 F6 N6 O2.50 P Rh' _chemical_formula_weight 860.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y, -z-1/2' _cell_length_a 18.231(6) _cell_length_b 10.710(3) _cell_length_c 19.500(5) _cell_angle_alpha 90.00(2) _cell_angle_beta 93.40(3) _cell_angle_gamma 90.00(3) _cell_volume 3800.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 20281 _diffrn_reflns_av_R_equivalents 0.1245 _diffrn_reflns_av_sigmaI/netI 0.1402 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6705 _reflns_number_gt 3275 _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^)+(0.0953P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6705 _refine_ls_number_parameters 530 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1646 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2049 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.002 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 -0.01007(4) -0.49737(7) 0.19836(3) 0.0461(2) Uani 1 1 d . . . O1 O -0.0763(4) -0.3247(6) 0.0932(3) 0.0667(19) Uani 1 1 d . . . N1 N -0.0622(4) -0.6692(6) 0.1596(3) 0.0417(16) Uani 1 1 d . . . N2 N -0.0866(4) -0.7527(6) 0.2067(3) 0.0416(16) Uani 1 1 d . . . N3 N 0.0385(4) -0.6223(8) 0.2758(3) 0.065(2) Uani 1 1 d . . . N4 N -0.0081(4) -0.7055(7) 0.3043(3) 0.055(2) Uani 1 1 d . . . N5 N -0.1048(4) -0.4972(7) 0.2632(3) 0.0466(16) Uani 1 1 d . . . N6 N -0.1254(4) -0.6094(6) 0.2913(3) 0.0404(17) Uani 1 1 d . . . C1 C -0.0520(5) -0.3943(8) 0.1348(4) 0.047(2) Uani 1 1 d . . . C2 C -0.0833(5) -0.7189(8) 0.2787(4) 0.047(2) Uani 1 1 d . . . H2 H -0.1051 -0.7894 0.3043 0.057 Uiso 1 1 calc R . . C3 C 0.0897(5) -0.4349(8) 0.1666(4) 0.044(2) Uani 1 1 d . . . C4 C 0.0711(5) -0.3646(9) 0.2138(5) 0.068(3) Uani 1 1 d . . . C6 C -0.1389(7) -0.9702(7) 0.2140(5) 0.076(3) Uani 1 1 d . . . H6A H -0.1546 -1.0361 0.1815 0.114 Uiso 1 1 calc R . . H6B H -0.1808 -0.9440 0.2398 0.114 Uiso 1 1 calc R . . H6C H -0.0998 -1.0020 0.2459 0.114 Uiso 1 1 calc R . . C7 C -0.1107(5) -0.8598(7) 0.1750(4) 0.048(2) Uani 1 1 d . . . C8 C -0.1026(5) -0.8419(7) 0.1074(4) 0.053(2) Uani 1 1 d . . . H8 H -0.1153 -0.9001 0.0719 0.063 Uiso 1 1 calc R . . C9 C -0.0726(5) -0.7243(7) 0.0984(4) 0.041(2) Uani 1 1 d . . . C10 C -0.0534(5) -0.6613(8) 0.0342(4) 0.055(2) Uani 1 1 d . . . H10A H -0.0539 -0.7224 -0.0032 0.082 Uiso 1 1 calc R . . H10B H -0.0044 -0.6243 0.0408 0.082 Uiso 1 1 calc R . . H10C H -0.0894 -0.5955 0.0227 0.082 Uiso 1 1 calc R . . C11 C -0.0112(6) -0.8681(12) 0.3970(5) 0.114(5) Uani 1 1 d . . . H11A H -0.0503 -0.8273 0.4212 0.171 Uiso 1 1 calc R . . H11B H 0.0237 -0.9073 0.4305 0.171 Uiso 1 1 calc R . . H11C H -0.0327 -0.9319 0.3659 0.171 Uiso 1 1 calc R . . C12 C 0.0277(6) -0.7732(12) 0.3566(5) 0.088(4) Uani 1 1 d . . . C13 C 0.0974(7) -0.7309(15) 0.3590(6) 0.128(6) Uani 1 1 d . . . H13 H 0.1361 -0.7595 0.3898 0.154 Uiso 1 1 calc R . . C14 C 0.1036(6) -0.6403(14) 0.3103(5) 0.106(5) Uani 1 1 d . . . C15 C 0.1722(6) -0.5727(16) 0.2936(6) 0.154(7) Uani 1 1 d . . . H15A H 0.2136 -0.6028 0.3235 0.232 Uiso 1 1 calc R . . H15B H 0.1657 -0.4829 0.3008 0.232 Uiso 1 1 calc R . . H15C H 0.1823 -0.5880 0.2455 0.232 Uiso 1 1 calc R . . C16 C -0.2191(5) -0.7000(8) 0.3665(4) 0.058(2) Uani 1 1 d . . . H16A H -0.2664 -0.6722 0.3824 0.087 Uiso 1 1 calc R . . H16B H -0.1870 -0.7263 0.4060 0.087 Uiso 1 1 calc R . . H16C H -0.2270 -0.7704 0.3348 0.087 Uiso 1 1 calc R . . C17 C -0.1839(5) -0.5955(8) 0.3305(4) 0.047(2) Uani 1 1 d . . . C18 C -0.2008(5) -0.4698(8) 0.3287(4) 0.057(3) Uani 1 1 d . . . H18 H -0.2385 -0.4293 0.3519 0.068 Uiso 1 1 calc R . . C19 C -0.1510(5) -0.4141(9) 0.2858(4) 0.054(2) Uani 1 1 d . . . C20 C -0.1467(6) -0.2788(7) 0.2654(5) 0.066(3) Uani 1 1 d . . . H20A H -0.0951 -0.2530 0.2659 0.099 Uiso 1 1 calc R . . H20B H -0.1725 -0.2275 0.2979 0.099 Uiso 1 1 calc R . . H20C H -0.1697 -0.2678 0.2191 0.099 Uiso 1 1 calc R . . C21 C 0.1438(5) -0.4661(7) 0.1178(4) 0.044(2) Uani 1 1 d . . . C22 C 0.1445(6) -0.5889(9) 0.0884(5) 0.064(3) Uani 1 1 d . . . H22 H 0.1097 -0.6493 0.1011 0.076 Uiso 1 1 calc R . . C23 C 0.1946(7) -0.6190(12) 0.0425(6) 0.089(4) Uani 1 1 d . . . H23 H 0.1948 -0.7000 0.0226 0.107 Uiso 1 1 calc R . . C24 C 0.2451(7) -0.5311(16) 0.0250(6) 0.108(5) Uani 1 1 d . . . H24 H 0.2802 -0.5524 -0.0072 0.130 Uiso 1 1 calc R . . C25 C 0.2461(5) -0.4135(14) 0.0527(5) 0.091(4) Uani 1 1 d . . . H25 H 0.2818 -0.3546 0.0398 0.109 Uiso 1 1 calc R . . C26 C 0.1950(5) -0.3801(9) 0.0998(4) 0.054(2) Uani 1 1 d . . . H26 H 0.1956 -0.2987 0.1192 0.065 Uiso 1 1 calc R . . C31 C 0.0900(7) -0.2785(12) 0.2683(7) 0.116(5) Uani 1 1 d D . . C32 C 0.1549(9) -0.2110(12) 0.2686(7) 0.137(6) Uani 1 1 d D . . H32 H 0.1868 -0.2210 0.2322 0.164 Uiso 1 1 calc R . . C33 C 0.1737(10) -0.1278(13) 0.3228(9) 0.158(7) Uani 1 1 d D . . H33 H 0.2185 -0.0826 0.3235 0.189 Uiso 1 1 calc R . . C34 C 0.1275(13) -0.1127(19) 0.3737(10) 0.231(13) Uani 1 1 d D . . H34 H 0.1392 -0.0531 0.4087 0.277 Uiso 1 1 calc R . . C35 C 0.0681(10) -0.1764(19) 0.3763(9) 0.211(12) Uani 1 1 d D . . H35 H 0.0368 -0.1679 0.4132 0.253 Uiso 1 1 calc R . . C36 C 0.0523(8) -0.2567(14) 0.3235(6) 0.142(7) Uani 1 1 d D . . H36 H 0.0084 -0.3037 0.3263 0.171 Uiso 1 1 calc R . . C201 C 0.123(4) 0.076(3) 0.1671(14) 0.66(7) Uani 1 1 d . . . H20D H 0.1633 0.1109 0.1980 0.787 Uiso 1 1 calc R . . H20E H 0.0933 0.1489 0.1523 0.787 Uiso 1 1 calc R . . C202 C 0.156(2) 0.053(3) 0.115(3) 0.54(5) Uani 1 1 d . . . H20F H 0.2094 0.0395 0.1260 0.647 Uiso 1 1 calc R . . H20G H 0.1500 0.1216 0.0809 0.647 Uiso 1 1 calc R . . C203 C 0.120(2) -0.062(3) 0.0898(9) 0.290(19) Uani 1 1 d . . . H20H H 0.1515 -0.1366 0.0968 0.348 Uiso 1 1 calc R . . H20I H 0.1021 -0.0563 0.0409 0.348 Uiso 1 1 calc R . . C204 C 0.0565(15) -0.062(2) 0.1374(18) 0.33(2) Uani 1 1 d . . . H20J H 0.0467 -0.1473 0.1548 0.398 Uiso 1 1 calc R . . H20K H 0.0109 -0.0283 0.1143 0.398 Uiso 1 1 calc R . . C211 C -0.0452(14) -0.547(6) 0.5198(15) 0.54(5) Uani 1 1 d . . . O12 O -0.0660(13) -0.592(3) 0.4632(10) 0.149(9) Uani 0.50 1 d P . . C212 C -0.0309(13) -0.463(3) 0.4516(13) 0.234(13) Uani 1 1 d . . . O11 O 0.0906(19) 0.034(3) 0.202(3) 0.67(5) Uani 1 1 d . . . P1 P -0.3083(2) -0.0792(3) 0.05680(13) 0.0723(9) Uani 1 1 d . . . F1 F -0.2736(15) -0.200(2) 0.0877(12) 0.095(11) Uani 0.50(4) 1 d P A 1 F1' F -0.232(3) -0.133(4) 0.0844(18) 0.21(3) Uani 0.50(4) 1 d P A 2 F2 F -0.229(2) -0.043(3) 0.0522(10) 0.128(14) Uani 0.50(4) 1 d P A 1 F2' F -0.2669(14) 0.044(3) 0.0387(12) 0.102(9) Uani 0.50(4) 1 d P A 2 F3 F -0.3873(10) -0.134(4) 0.0692(16) 0.162(15) Uani 0.50(4) 1 d P A 1 F3' F -0.338(4) -0.214(3) 0.0727(14) 0.25(3) Uani 0.50(4) 1 d P A 2 F4 F -0.2994(4) -0.1305(6) -0.0187(3) 0.104(2) Uani 1 1 d . A . F5 F -0.333(3) 0.051(2) 0.0301(9) 0.16(2) Uani 0.50(4) 1 d P A 1 F5' F -0.3815(10) -0.032(3) 0.0259(10) 0.101(11) Uani 0.50(4) 1 d P A 2 F6 F -0.3175(5) -0.0263(6) 0.1317(3) 0.127(3) Uani 1 1 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 0.0514(4) 0.0549(4) 0.0313(3) 0.0011(4) -0.0042(2) -0.0177(4) O1 0.087(5) 0.059(4) 0.053(4) 0.012(3) -0.006(4) 0.004(4) N1 0.049(4) 0.039(4) 0.036(4) 0.009(3) -0.004(3) -0.001(3) N2 0.047(4) 0.044(4) 0.034(4) 0.009(3) -0.004(3) -0.001(3) N3 0.043(5) 0.116(7) 0.034(4) 0.021(4) -0.011(3) -0.020(5) N4 0.040(5) 0.083(5) 0.040(4) 0.021(4) -0.009(4) -0.011(4) N5 0.050(4) 0.048(4) 0.041(3) 0.002(4) 0.002(3) -0.012(4) N6 0.041(4) 0.043(4) 0.037(4) 0.001(3) -0.001(3) -0.006(4) C1 0.057(6) 0.047(5) 0.035(5) -0.009(4) -0.001(4) -0.020(5) C2 0.045(6) 0.065(6) 0.030(4) 0.018(4) -0.011(4) -0.007(5) C3 0.050(5) 0.042(5) 0.038(5) 0.002(4) -0.006(4) -0.015(4) C4 0.062(7) 0.085(7) 0.059(6) -0.023(6) 0.004(5) -0.025(6) C6 0.118(9) 0.034(6) 0.078(7) 0.007(4) 0.018(6) -0.015(5) C7 0.060(6) 0.030(4) 0.053(5) -0.003(4) 0.000(4) 0.001(4) C8 0.071(7) 0.041(5) 0.047(5) -0.006(4) 0.003(5) 0.002(5) C9 0.054(6) 0.031(4) 0.036(5) -0.002(4) -0.005(4) 0.001(4) C10 0.066(6) 0.065(6) 0.033(5) 0.008(4) -0.003(4) -0.004(5) C11 0.081(9) 0.176(13) 0.080(8) 0.088(9) -0.026(7) -0.018(9) C12 0.053(7) 0.156(11) 0.054(6) 0.064(7) -0.014(5) -0.005(7) C13 0.070(9) 0.230(17) 0.081(8) 0.095(10) -0.032(7) -0.032(10) C14 0.064(8) 0.187(14) 0.062(7) 0.045(8) -0.032(6) -0.046(9) C15 0.058(8) 0.30(2) 0.095(9) 0.094(11) -0.044(7) -0.090(11) C16 0.055(6) 0.066(6) 0.053(5) 0.010(5) 0.005(5) -0.019(5) C17 0.043(5) 0.068(6) 0.030(4) 0.006(4) -0.003(4) -0.017(5) C18 0.064(6) 0.059(7) 0.048(5) 0.011(4) 0.014(5) 0.001(5) C19 0.058(7) 0.055(6) 0.047(5) -0.004(5) -0.001(5) -0.011(5) C20 0.077(7) 0.046(5) 0.077(7) -0.002(5) 0.023(6) -0.013(5) C21 0.042(5) 0.054(6) 0.034(4) -0.005(4) -0.013(4) 0.000(4) C22 0.068(7) 0.065(6) 0.054(6) -0.026(5) -0.026(5) 0.016(6) C23 0.061(8) 0.107(10) 0.094(9) -0.050(8) -0.036(7) 0.036(8) C24 0.065(8) 0.189(16) 0.069(7) -0.071(9) -0.006(6) 0.041(9) C25 0.041(7) 0.166(13) 0.068(7) -0.020(8) 0.014(6) -0.006(7) C26 0.038(5) 0.080(7) 0.044(5) 0.002(5) -0.006(4) -0.006(5) C31 0.079(9) 0.137(11) 0.135(11) -0.093(10) 0.023(8) -0.050(9) C32 0.160(15) 0.121(12) 0.129(12) -0.050(10) 0.011(11) -0.050(11) C33 0.146(16) 0.133(13) 0.194(18) -0.074(13) 0.000(14) -0.059(12) C34 0.19(2) 0.28(3) 0.24(2) -0.20(2) 0.07(2) -0.04(2) C35 0.113(15) 0.36(3) 0.164(17) -0.145(19) 0.009(13) -0.060(19) C36 0.103(11) 0.221(17) 0.101(10) -0.122(11) -0.012(9) -0.012(11) C201 1.57(18) 0.21(3) 0.14(2) -0.09(2) -0.35(5) 0.44(6) C202 0.37(5) 0.24(4) 1.04(14) -0.07(6) 0.38(7) -0.18(4) C203 0.47(5) 0.31(3) 0.082(12) -0.047(16) -0.009(19) 0.24(3) C204 0.30(3) 0.18(2) 0.54(5) -0.22(3) 0.22(4) -0.13(2) C211 0.14(2) 1.34(15) 0.126(19) -0.20(5) -0.051(18) 0.18(5) O12 0.131(19) 0.25(3) 0.061(12) 0.018(14) -0.030(12) 0.002(18) C212 0.13(2) 0.40(4) 0.17(2) 0.08(3) -0.003(17) -0.01(2) O11 0.36(4) 0.33(3) 1.36(14) -0.27(6) 0.43(6) -0.16(3) P1 0.117(3) 0.0534(18) 0.0455(15) -0.0086(13) -0.0079(17) 0.0146(19) F1 0.15(2) 0.053(13) 0.084(16) 0.019(11) 0.051(16) 0.032(12) F1' 0.28(5) 0.17(3) 0.16(3) -0.07(2) -0.13(3) 0.18(4) F2 0.15(3) 0.16(3) 0.079(13) -0.011(16) 0.032(16) -0.06(2) F2' 0.093(16) 0.11(2) 0.106(14) -0.030(13) 0.003(12) -0.020(13) F3 0.055(12) 0.23(4) 0.20(2) 0.01(3) 0.033(12) -0.020(16) F3' 0.54(9) 0.10(2) 0.111(17) -0.028(15) 0.04(4) -0.16(4) F4 0.158(6) 0.090(4) 0.060(4) -0.034(3) -0.026(4) 0.030(4) F5 0.36(7) 0.064(15) 0.066(11) 0.004(11) 0.02(2) 0.11(3) F5' 0.085(12) 0.14(3) 0.072(11) -0.044(13) -0.020(8) 0.025(12) F6 0.238(10) 0.093(5) 0.052(4) -0.016(3) 0.027(5) 0.006(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 C1 1.796(9) . ? Rh1 C4 2.061(9) . ? Rh1 C3 2.068(8) . ? Rh1 N3 2.167(7) . ? Rh1 N1 2.185(6) . ? Rh1 N5 2.200(6) . ? Rh1 C2 3.180(8) . ? O1 C1 1.168(9) . ? N1 C9 1.334(9) . ? N1 N2 1.375(8) . ? N2 C7 1.364(9) . ? N2 C2 1.447(9) . ? N3 C14 1.343(11) . ? N3 N4 1.371(9) . ? N4 C12 1.383(10) . ? N4 C2 1.439(10) . ? N5 C19 1.319(11) . ? N5 N6 1.383(8) . ? N6 C17 1.356(10) . ? N6 C2 1.430(10) . ? C3 C4 1.251(11) . ? C3 C21 1.450(11) . ? C4 C31 1.434(13) . ? C6 C7 1.513(11) . ? C7 C8 1.348(11) . ? C8 C9 1.388(11) . ? C9 C10 1.482(10) . ? C11 C12 1.491(13) . ? C12 C13 1.346(14) . ? C13 C14 1.367(15) . ? C14 C15 1.499(14) . ? C16 C17 1.487(10) . ? C17 C18 1.381(12) . ? C18 C19 1.403(12) . ? C19 C20 1.506(11) . ? C21 C26 1.371(11) . ? C21 C22 1.435(11) . ? C22 C23 1.355(14) . ? C23 C24 1.374(17) . ? C24 C25 1.370(18) . ? C25 C26 1.393(12) . ? C31 C36 1.330(16) . ? C31 C32 1.387(17) . ? C32 C33 1.409(18) . ? C33 C34 1.35(2) . ? C34 C35 1.28(2) . ? C35 C36 1.360(18) . ? C201 O11 1.03(8) . ? C201 C202 1.24(6) . ? C202 C203 1.48(4) . ? C203 C204 1.52(3) . ? C204 O11 1.71(5) . ? C211 O12 1.24(3) . ? C211 C212 1.47(3) 3_546 ? C211 C212 1.64(5) . ? O12 C212 1.54(3) . ? C212 C211 1.47(3) 3_546 ? P1 F2 1.51(3) . ? P1 F5' 1.520(16) . ? P1 F5 1.553(14) . ? P1 F1 1.551(19) . ? P1 F1' 1.57(3) . ? P1 F2' 1.57(2) . ? P1 F3' 1.58(2) . ? P1 F6 1.585(6) . ? P1 F4 1.588(6) . ? P1 F3 1.59(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C4 87.1(4) . . ? C1 Rh1 C3 86.6(3) . . ? C4 Rh1 C3 35.3(3) . . ? C1 Rh1 N3 178.9(3) . . ? C4 Rh1 N3 93.7(3) . . ? C3 Rh1 N3 94.5(3) . . ? C1 Rh1 N1 96.9(3) . . ? C4 Rh1 N1 157.7(3) . . ? C3 Rh1 N1 122.8(3) . . ? N3 Rh1 N1 82.7(3) . . ? C1 Rh1 N5 94.6(3) . . ? C4 Rh1 N5 119.8(3) . . ? C3 Rh1 N5 155.0(3) . . ? N3 Rh1 N5 84.4(3) . . ? N1 Rh1 N5 81.9(2) . . ? C1 Rh1 C2 128.6(3) . . ? C4 Rh1 C2 139.6(3) . . ? C3 Rh1 C2 142.4(3) . . ? N3 Rh1 C2 50.4(2) . . ? N1 Rh1 C2 49.9(2) . . ? N5 Rh1 C2 49.5(3) . . ? C9 N1 N2 106.0(6) . . ? C9 N1 Rh1 135.9(5) . . ? N2 N1 Rh1 117.9(4) . . ? C7 N2 N1 110.6(6) . . ? C7 N2 C2 130.1(7) . . ? N1 N2 C2 119.3(6) . . ? C14 N3 N4 104.7(8) . . ? C14 N3 Rh1 138.6(7) . . ? N4 N3 Rh1 116.5(5) . . ? N3 N4 C12 111.3(7) . . ? N3 N4 C2 121.6(6) . . ? C12 N4 C2 127.0(7) . . ? C19 N5 N6 105.0(6) . . ? C19 N5 Rh1 137.0(6) . . ? N6 N5 Rh1 117.9(5) . . ? C17 N6 N5 111.7(7) . . ? C17 N6 C2 129.4(7) . . ? N5 N6 C2 118.9(7) . . ? O1 C1 Rh1 177.0(7) . . ? N6 C2 N4 111.7(7) . . ? N6 C2 N2 112.4(6) . . ? N4 C2 N2 110.2(7) . . ? N6 C2 Rh1 73.7(4) . . ? N4 C2 Rh1 71.2(4) . . ? N2 C2 Rh1 72.7(4) . . ? C4 C3 C21 147.8(9) . . ? C4 C3 Rh1 72.1(6) . . ? C21 C3 Rh1 140.1(6) . . ? C3 C4 C31 150.3(10) . . ? C3 C4 Rh1 72.6(6) . . ? C31 C4 Rh1 133.7(8) . . ? C8 C7 N2 105.8(7) . . ? C8 C7 C6 131.5(8) . . ? N2 C7 C6 122.7(7) . . ? C7 C8 C9 108.6(7) . . ? N1 C9 C8 108.9(7) . . ? N1 C9 C10 121.7(7) . . ? C8 C9 C10 129.4(7) . . ? C13 C12 N4 104.6(9) . . ? C13 C12 C11 133.5(9) . . ? N4 C12 C11 121.9(9) . . ? C12 C13 C14 109.4(10) . . ? N3 C14 C13 110.0(10) . . ? N3 C14 C15 123.1(10) . . ? C13 C14 C15 126.8(10) . . ? N6 C17 C18 106.0(7) . . ? N6 C17 C16 124.0(8) . . ? C18 C17 C16 130.0(8) . . ? C17 C18 C19 106.1(8) . . ? N5 C19 C18 111.2(8) . . ? N5 C19 C20 121.0(8) . . ? C18 C19 C20 127.8(9) . . ? C26 C21 C22 119.4(9) . . ? C26 C21 C3 120.8(8) . . ? C22 C21 C3 119.8(8) . . ? C23 C22 C21 120.3(11) . . ? C22 C23 C24 119.2(11) . . ? C25 C24 C23 121.8(12) . . ? C24 C25 C26 120.1(12) . . ? C21 C26 C25 119.3(10) . . ? C36 C31 C32 112.8(12) . . ? C36 C31 C4 126.8(12) . . ? C32 C31 C4 120.3(12) . . ? C31 C32 C33 120.1(15) . . ? C34 C33 C32 119.5(17) . . ? C35 C34 C33 122.1(19) . . ? C34 C35 C36 116.6(19) . . ? C31 C36 C35 128.8(16) . . ? O11 C201 C202 142(5) . . ? C201 C202 C203 102(4) . . ? C202 C203 C204 98(2) . . ? C203 C204 O11 101(2) . . ? O12 C211 C212 127(3) . 3_546 ? O12 C211 C212 63(2) . . ? C212 C211 C212 94(3) 3_546 . ? C211 O12 C212 71(3) . . ? C211 C212 O12 114(3) 3_546 . ? C211 C212 C211 86(3) 3_546 . ? O12 C212 C211 45.8(19) . . ? C201 O11 C204 89(5) . . ? F2 P1 F5' 135.5(14) . . ? F2 P1 F5 90.7(17) . . ? F5' P1 F5 47.8(14) . . ? F2 P1 F1 82.5(15) . . ? F5' P1 F1 139.8(14) . . ? F5 P1 F1 172(2) . . ? F2 P1 F1' 44.0(16) . . ? F5' P1 F1' 176.5(12) . . ? F5 P1 F1' 133(2) . . ? F1 P1 F1' 39.5(19) . . ? F2 P1 F2' 45.0(11) . . ? F5' P1 F2' 92.9(12) . . ? F5 P1 F2' 45.9(15) . . ? F1 P1 F2' 126.9(13) . . ? F1' P1 F2' 87(2) . . ? F2 P1 F3' 126(2) . . ? F5' P1 F3' 95(2) . . ? F5 P1 F3' 142(3) . . ? F1 P1 F3' 45(2) . . ? F1' P1 F3' 85(2) . . ? F2' P1 F3' 171(2) . . ? F2 P1 F6 96.7(8) . . ? F5' P1 F6 96.1(8) . . ? F5 P1 F6 86.7(7) . . ? F1 P1 F6 90.3(9) . . ? F1' P1 F6 87.4(12) . . ? F2' P1 F6 89.2(8) . . ? F3' P1 F6 95.2(12) . . ? F2 P1 F4 83.3(8) . . ? F5' P1 F4 83.3(7) . . ? F5 P1 F4 92.6(7) . . ? F1 P1 F4 90.5(9) . . ? F1' P1 F4 93.2(12) . . ? F2' P1 F4 90.4(8) . . ? F3' P1 F4 85.4(11) . . ? F6 P1 F4 179.3(4) . . ? F2 P1 F3 171.2(15) . . ? F5' P1 F3 53.3(11) . . ? F5 P1 F3 97.6(18) . . ? F1 P1 F3 89.1(14) . . ? F1' P1 F3 127(2) . . ? F2' P1 F3 142.9(13) . . ? F3' P1 F3 46(2) . . ? F6 P1 F3 81.1(12) . . ? F4 P1 F3 99.0(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 N5 N6 C2 1.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.626 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.095 data_7 _database_code_CSD 205492 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H34 F6 N6 O P Rh' _chemical_formula_weight 682.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 8.806(4) _cell_length_b 13.867(5) _cell_length_c 22.785(6) _cell_angle_alpha 90.00(2) _cell_angle_beta 94.952(19) _cell_angle_gamma 90.00(3) _cell_volume 2771.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 14408 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4887 _reflns_number_gt 3374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0809P)^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 4887 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 0.832 _refine_ls_restrained_S_all 0.832 _refine_ls_shift/su_max 0.002 _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 0.86331(4) 0.76332(3) 0.858714(16) 0.01977(14) Uani 1 1 d . . . O1 O 0.9966(4) 0.8574(2) 0.73492(16) 0.0337(9) Uani 1 1 d . . . N6 N 0.7104(4) 0.6427(3) 0.86333(16) 0.0201(9) Uani 1 1 d . . . N5 N 0.7740(4) 0.5540(3) 0.85636(16) 0.0191(9) Uani 1 1 d . . . N4 N 1.0081(4) 0.6747(3) 0.91671(16) 0.0205(9) Uani 1 1 d . . . N3 N 1.0231(4) 0.5806(3) 0.89945(17) 0.0206(9) Uani 1 1 d . . . N2 N 1.1212(4) 0.6158(3) 0.79344(18) 0.0264(10) Uani 1 1 d . . . N1 N 0.9671(4) 0.6031(3) 0.79724(17) 0.0226(9) Uani 1 1 d . . . C1 C 0.9336(5) 0.5461(3) 0.8481(2) 0.0220(11) Uani 1 1 d . . . H1A H 0.9594 0.4771 0.8412 0.026 Uiso 1 1 calc R . . C2 C 0.7120(6) 0.3781(4) 0.8565(2) 0.0301(12) Uani 1 1 d . . . H2A H 0.7960 0.3610 0.8857 0.045 Uiso 1 1 calc R . . H2B H 0.7429 0.3669 0.8168 0.045 Uiso 1 1 calc R . . H2C H 0.6228 0.3383 0.8627 0.045 Uiso 1 1 calc R . . C3 C 0.6728(6) 0.4813(3) 0.8632(2) 0.0237(11) Uani 1 1 d . . . C4 C 0.5399(6) 0.5257(4) 0.8746(2) 0.0291(12) Uani 1 1 d . . . H4A H 0.4469 0.4949 0.8816 0.035 Uiso 1 1 calc R . . C5 C 0.5666(5) 0.6254(4) 0.8739(2) 0.0247(11) Uani 1 1 d . . . C6 C 0.4572(6) 0.7030(4) 0.8835(2) 0.0325(13) Uani 1 1 d . . . H6A H 0.4795 0.7592 0.8596 0.049 Uiso 1 1 calc R . . H6B H 0.4658 0.7210 0.9253 0.049 Uiso 1 1 calc R . . H6C H 0.3534 0.6804 0.8720 0.049 Uiso 1 1 calc R . . C7 C 1.1616(6) 0.4276(4) 0.9279(2) 0.0339(13) Uani 1 1 d . . . H7A H 1.1797 0.4162 0.8866 0.051 Uiso 1 1 calc R . . H7B H 1.0753 0.3882 0.9382 0.051 Uiso 1 1 calc R . . H7C H 1.2528 0.4101 0.9533 0.051 Uiso 1 1 calc R . . C8 C 1.1262(5) 0.5314(4) 0.9364(2) 0.0246(11) Uani 1 1 d . . . C9 C 1.1764(6) 0.5961(4) 0.9789(2) 0.0267(12) Uani 1 1 d . . . H9A H 1.2489 0.5838 1.0114 0.032 Uiso 1 1 calc R . . C10 C 1.1020(5) 0.6841(4) 0.9662(2) 0.0229(11) Uani 1 1 d . . . C11 C 1.1127(6) 0.7749(4) 1.0007(2) 0.0294(12) Uani 1 1 d . . . H11A H 1.0116 0.8045 1.0002 0.044 Uiso 1 1 calc R . . H11B H 1.1827 0.8194 0.9833 0.044 Uiso 1 1 calc R . . H11C H 1.1510 0.7607 1.0415 0.044 Uiso 1 1 calc R . . C12 C 0.7208(6) 0.5859(4) 0.7301(2) 0.0297(12) Uani 1 1 d . . . H12A H 0.6643 0.6306 0.7535 0.045 Uiso 1 1 calc R . . H12B H 0.6978 0.5194 0.7409 0.045 Uiso 1 1 calc R . . H12C H 0.6906 0.5960 0.6881 0.045 Uiso 1 1 calc R . . C13 C 0.8865(6) 0.6038(4) 0.7419(2) 0.0255(11) Uani 1 1 d . . . C14 C 0.9916(6) 0.6268(3) 0.7035(2) 0.0266(12) Uani 1 1 d . . . H14A H 0.9726 0.6371 0.6623 0.032 Uiso 1 1 calc R . . C15 C 1.1346(6) 0.6324(4) 0.7371(2) 0.0276(12) Uani 1 1 d . . . C16 C 1.2871(6) 0.6530(4) 0.7166(3) 0.0395(14) Uani 1 1 d . . . H16A H 1.3585 0.6018 0.7302 0.059 Uiso 1 1 calc R . . H16B H 1.3243 0.7150 0.7326 0.059 Uiso 1 1 calc R . . H16C H 1.2792 0.6556 0.6735 0.059 Uiso 1 1 calc R . . C19 C 0.7464(5) 0.8985(3) 0.8459(2) 0.0233(11) Uani 1 1 d . . . C20 C 0.8951(6) 0.9130(3) 0.8775(2) 0.0219(11) Uani 1 1 d . . . C21 C 1.0078(5) 0.8823(3) 0.8406(2) 0.0228(11) Uani 1 1 d . . . C17 C 0.9351(5) 0.8679(3) 0.7809(2) 0.0222(11) Uani 1 1 d . . . C18 C 0.7699(5) 0.8602(3) 0.7898(2) 0.0216(11) Uani 1 1 d . . . C22 C 0.6007(6) 0.9313(4) 0.8677(3) 0.0358(14) Uani 1 1 d . . . H22A H 0.5898 0.9028 0.9065 0.054 Uiso 1 1 calc R . . H22B H 0.5153 0.9108 0.8401 0.054 Uiso 1 1 calc R . . H22C H 0.6009 1.0017 0.8710 0.054 Uiso 1 1 calc R . . C23 C 0.9168(6) 0.9663(4) 0.9343(2) 0.0326(13) Uani 1 1 d . . . H23A H 0.8522 0.9376 0.9626 0.049 Uiso 1 1 calc R . . H23B H 0.8887 1.0340 0.9279 0.049 Uiso 1 1 calc R . . H23C H 1.0239 0.9621 0.9499 0.049 Uiso 1 1 calc R . . C24 C 1.1775(5) 0.8843(4) 0.8545(2) 0.0301(12) Uani 1 1 d . . . H24A H 1.2271 0.8565 0.8215 0.045 Uiso 1 1 calc R . . H24B H 1.2048 0.8467 0.8902 0.045 Uiso 1 1 calc R . . H24C H 1.2114 0.9511 0.8607 0.045 Uiso 1 1 calc R . . C25 C 0.6518(6) 0.8402(4) 0.7400(2) 0.0370(14) Uani 1 1 d . . . H25A H 0.6960 0.7997 0.7106 0.055 Uiso 1 1 calc R . . H25B H 0.6169 0.9012 0.7218 0.055 Uiso 1 1 calc R . . H25C H 0.5653 0.8066 0.7551 0.055 Uiso 1 1 calc R . . P1 P 0.59785(16) 0.68740(10) 0.55363(6) 0.0298(3) Uani 1 1 d . . . F1 F 0.7174(5) 0.7322(3) 0.60278(15) 0.0638(11) Uani 1 1 d . . . F2 F 0.4838(5) 0.6660(3) 0.60270(16) 0.0647(11) Uani 1 1 d . . . F3 F 0.4795(4) 0.6428(3) 0.50446(15) 0.0527(9) Uani 1 1 d . . . F4 F 0.6735(4) 0.5841(2) 0.56530(16) 0.0582(10) Uani 1 1 d . . . F5 F 0.5222(4) 0.7910(2) 0.54248(14) 0.0475(9) Uani 1 1 d . . . F6 F 0.7103(4) 0.7109(3) 0.50459(15) 0.0517(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0217(2) 0.0115(2) 0.0259(2) 0.00282(17) 0.00073(14) -0.00161(17) O1 0.050(2) 0.021(2) 0.033(2) 0.0008(16) 0.0155(18) 0.0001(17) N6 0.025(2) 0.011(2) 0.025(2) -0.0019(17) 0.0054(17) 0.0003(17) N5 0.022(2) 0.009(2) 0.027(2) -0.0005(17) 0.0059(17) -0.0021(17) N4 0.029(2) 0.012(2) 0.021(2) -0.0007(17) 0.0015(17) 0.0015(17) N3 0.022(2) 0.012(2) 0.027(2) -0.0002(17) 0.0015(17) 0.0001(17) N2 0.024(2) 0.025(3) 0.031(2) 0.002(2) 0.0065(18) -0.0035(19) N1 0.023(2) 0.022(2) 0.023(2) -0.0004(18) 0.0054(17) -0.0049(18) C1 0.023(3) 0.013(3) 0.030(3) 0.000(2) 0.005(2) -0.001(2) C2 0.038(3) 0.015(3) 0.039(3) 0.000(2) 0.010(2) -0.005(2) C3 0.033(3) 0.014(3) 0.025(3) -0.004(2) 0.005(2) -0.009(2) C4 0.030(3) 0.024(3) 0.034(3) -0.003(2) 0.007(2) -0.011(2) C5 0.024(3) 0.024(3) 0.027(3) -0.004(2) 0.008(2) -0.005(2) C6 0.025(3) 0.025(3) 0.049(3) -0.002(3) 0.011(2) -0.001(2) C7 0.031(3) 0.024(3) 0.048(3) 0.006(3) 0.011(3) 0.008(2) C8 0.025(3) 0.019(3) 0.031(3) 0.005(2) 0.007(2) 0.004(2) C9 0.028(3) 0.025(3) 0.027(3) 0.009(2) 0.002(2) 0.003(2) C10 0.026(3) 0.023(3) 0.021(3) 0.002(2) 0.004(2) -0.001(2) C11 0.036(3) 0.025(3) 0.026(3) -0.001(2) -0.004(2) 0.003(2) C12 0.031(3) 0.031(3) 0.026(3) -0.001(2) -0.001(2) -0.003(2) C13 0.037(3) 0.014(3) 0.026(3) -0.003(2) 0.002(2) 0.003(2) C14 0.042(3) 0.016(3) 0.025(3) 0.000(2) 0.014(2) 0.003(2) C15 0.036(3) 0.013(3) 0.035(3) 0.002(2) 0.015(2) 0.000(2) C16 0.038(3) 0.032(3) 0.051(4) 0.001(3) 0.021(3) -0.004(3) C19 0.025(3) 0.011(3) 0.034(3) 0.008(2) 0.005(2) 0.002(2) C20 0.034(3) 0.005(2) 0.027(3) 0.0024(19) 0.004(2) 0.000(2) C21 0.023(3) 0.011(3) 0.034(3) 0.002(2) 0.004(2) -0.003(2) C17 0.032(3) 0.006(2) 0.029(3) 0.004(2) 0.006(2) 0.001(2) C18 0.025(3) 0.012(3) 0.027(3) 0.004(2) 0.000(2) 0.004(2) C22 0.041(3) 0.017(3) 0.051(3) 0.003(3) 0.013(3) 0.008(2) C23 0.053(4) 0.017(3) 0.028(3) -0.003(2) 0.006(3) -0.003(2) C24 0.030(3) 0.017(3) 0.044(3) 0.004(2) 0.006(2) -0.003(2) C25 0.039(3) 0.034(3) 0.036(3) 0.011(3) -0.008(3) 0.000(3) P1 0.0393(8) 0.0221(8) 0.0287(7) 0.0008(6) 0.0076(6) -0.0007(6) F1 0.094(3) 0.045(2) 0.047(2) 0.0060(18) -0.023(2) -0.025(2) F2 0.098(3) 0.040(2) 0.064(2) 0.0081(19) 0.052(2) -0.005(2) F3 0.056(2) 0.043(2) 0.057(2) -0.0056(17) -0.0057(17) -0.0120(18) F4 0.071(3) 0.027(2) 0.076(3) 0.0056(18) 0.002(2) 0.0153(18) F5 0.063(2) 0.0243(19) 0.057(2) 0.0067(16) 0.0192(18) 0.0088(16) F6 0.047(2) 0.057(2) 0.054(2) 0.0069(19) 0.0217(17) 0.0005(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 C20 2.133(5) . ? Rh1 N4 2.143(4) . ? Rh1 C21 2.145(5) . ? Rh1 C19 2.147(5) . ? Rh1 N6 2.155(4) . ? Rh1 C18 2.173(5) . ? Rh1 C17 2.416(5) . ? Rh1 C1 3.088(5) . ? Rh1 N2 3.484(4) . ? O1 C17 1.230(6) . ? N6 C5 1.331(6) . ? N6 N5 1.367(5) . ? N5 C3 1.363(6) . ? N5 C1 1.438(6) . ? N4 C10 1.345(6) . ? N4 N3 1.372(5) . ? N3 C8 1.366(6) . ? N3 C1 1.434(6) . ? N2 C15 1.320(6) . ? N2 N1 1.378(5) . ? N1 C13 1.392(6) . ? N1 C1 1.454(6) . ? C2 C3 1.482(7) . ? C3 C4 1.367(7) . ? C4 C5 1.402(7) . ? C5 C6 1.473(7) . ? C7 C8 1.489(7) . ? C8 C9 1.366(7) . ? C9 C10 1.403(7) . ? C10 C11 1.485(7) . ? C12 C13 1.482(7) . ? C13 C14 1.365(7) . ? C14 C15 1.418(7) . ? C15 C16 1.487(7) . ? C19 C18 1.416(7) . ? C19 C20 1.453(7) . ? C19 C22 1.486(7) . ? C20 C21 1.420(7) . ? C20 C23 1.489(7) . ? C21 C17 1.465(7) . ? C21 C24 1.501(7) . ? C17 C18 1.490(7) . ? C18 C25 1.497(7) . ? P1 F3 1.588(4) . ? P1 F6 1.590(3) . ? P1 F4 1.593(4) . ? P1 F2 1.594(3) . ? P1 F5 1.595(4) . ? P1 F1 1.595(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Rh1 N4 111.96(16) . . ? C20 Rh1 C21 38.75(18) . . ? N4 Rh1 C21 103.23(17) . . ? C20 Rh1 C19 39.68(18) . . ? N4 Rh1 C19 146.89(17) . . ? C21 Rh1 C19 65.63(19) . . ? C20 Rh1 N6 144.82(17) . . ? N4 Rh1 N6 82.28(15) . . ? C21 Rh1 N6 171.71(16) . . ? C19 Rh1 N6 112.97(17) . . ? C20 Rh1 C18 65.06(18) . . ? N4 Rh1 C18 165.47(16) . . ? C21 Rh1 C18 65.13(18) . . ? C19 Rh1 C18 38.28(18) . . ? N6 Rh1 C18 108.40(16) . . ? C20 Rh1 C17 61.62(17) . . ? N4 Rh1 C17 128.11(16) . . ? C21 Rh1 C17 36.87(17) . . ? C19 Rh1 C17 61.90(17) . . ? N6 Rh1 C17 134.89(16) . . ? C18 Rh1 C17 37.43(17) . . ? C20 Rh1 C1 160.21(16) . . ? N4 Rh1 C1 51.40(13) . . ? C21 Rh1 C1 127.50(16) . . ? C19 Rh1 C1 159.74(16) . . ? N6 Rh1 C1 51.49(13) . . ? C18 Rh1 C1 127.74(16) . . ? C17 Rh1 C1 117.45(14) . . ? C20 Rh1 N2 125.28(15) . . ? N4 Rh1 N2 63.34(12) . . ? C21 Rh1 N2 87.14(15) . . ? C19 Rh1 N2 141.02(15) . . ? N6 Rh1 N2 89.90(12) . . ? C18 Rh1 N2 105.93(14) . . ? C17 Rh1 N2 79.49(13) . . ? C1 Rh1 N2 41.55(11) . . ? C5 N6 N5 105.3(4) . . ? C5 N6 Rh1 139.2(3) . . ? N5 N6 Rh1 115.4(3) . . ? C3 N5 N6 112.0(4) . . ? C3 N5 C1 128.0(4) . . ? N6 N5 C1 119.9(4) . . ? C10 N4 N3 105.4(4) . . ? C10 N4 Rh1 138.7(3) . . ? N3 N4 Rh1 115.8(3) . . ? C8 N3 N4 111.9(4) . . ? C8 N3 C1 128.7(4) . . ? N4 N3 C1 119.4(4) . . ? C15 N2 N1 104.8(4) . . ? C15 N2 Rh1 115.5(3) . . ? N1 N2 Rh1 50.7(2) . . ? N2 N1 C13 111.7(4) . . ? N2 N1 C1 112.8(4) . . ? C13 N1 C1 127.0(4) . . ? N3 C1 N5 110.0(4) . . ? N3 C1 N1 109.5(4) . . ? N5 C1 N1 109.3(4) . . ? N3 C1 Rh1 73.2(2) . . ? N5 C1 Rh1 73.2(2) . . ? N1 C1 Rh1 65.7(2) . . ? N5 C3 C4 105.5(4) . . ? N5 C3 C2 122.8(4) . . ? C4 C3 C2 131.7(5) . . ? C3 C4 C5 107.2(4) . . ? N6 C5 C4 110.0(4) . . ? N6 C5 C6 122.7(5) . . ? C4 C5 C6 127.3(5) . . ? N3 C8 C9 105.5(4) . . ? N3 C8 C7 122.5(5) . . ? C9 C8 C7 132.0(5) . . ? C8 C9 C10 107.9(4) . . ? N4 C10 C9 109.4(4) . . ? N4 C10 C11 122.2(4) . . ? C9 C10 C11 128.3(4) . . ? C14 C13 N1 105.1(4) . . ? C14 C13 C12 129.3(5) . . ? N1 C13 C12 125.5(4) . . ? C13 C14 C15 106.7(5) . . ? N2 C15 C14 111.4(4) . . ? N2 C15 C16 119.9(5) . . ? C14 C15 C16 128.7(5) . . ? C18 C19 C20 107.7(4) . . ? C18 C19 C22 127.9(5) . . ? C20 C19 C22 124.0(5) . . ? C18 C19 Rh1 71.9(3) . . ? C20 C19 Rh1 69.7(3) . . ? C22 C19 Rh1 129.7(3) . . ? C21 C20 C19 108.2(4) . . ? C21 C20 C23 128.3(5) . . ? C19 C20 C23 122.8(5) . . ? C21 C20 Rh1 71.1(3) . . ? C19 C20 Rh1 70.7(3) . . ? C23 C20 Rh1 131.4(3) . . ? C20 C21 C17 108.6(4) . . ? C20 C21 C24 127.1(5) . . ? C17 C21 C24 123.0(4) . . ? C20 C21 Rh1 70.2(3) . . ? C17 C21 Rh1 81.7(3) . . ? C24 C21 Rh1 124.7(3) . . ? O1 C17 C21 128.2(5) . . ? O1 C17 C18 127.9(5) . . ? C21 C17 C18 103.7(4) . . ? O1 C17 Rh1 135.8(3) . . ? C21 C17 Rh1 61.5(2) . . ? C18 C17 Rh1 62.4(2) . . ? C19 C18 C17 108.4(4) . . ? C19 C18 C25 127.4(5) . . ? C17 C18 C25 122.2(4) . . ? C19 C18 Rh1 69.9(3) . . ? C17 C18 Rh1 80.2(3) . . ? C25 C18 Rh1 128.9(4) . . ? F3 P1 F6 89.7(2) . . ? F3 P1 F4 90.4(2) . . ? F6 P1 F4 91.4(2) . . ? F3 P1 F2 90.4(2) . . ? F6 P1 F2 178.8(2) . . ? F4 P1 F2 89.7(2) . . ? F3 P1 F5 89.9(2) . . ? F6 P1 F5 88.86(19) . . ? F4 P1 F5 179.6(2) . . ? F2 P1 F5 89.96(19) . . ? F3 P1 F1 179.7(2) . . ? F6 P1 F1 90.0(2) . . ? F4 P1 F1 89.5(2) . . ? F2 P1 F1 89.8(2) . . ? F5 P1 F1 90.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 C1 N1 N2 107.0(3) . . . . ? C17 C18 C19 C20 -10.9(5) . . . . ? C18 C19 C20 C21 -0.7(5) . . . . ? C19 C20 C21 C17 12.2(5) . . . . ? C20 C21 C17 C18 -18.2(5) . . . . ? C21 C17 C18 C19 17.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.383 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.110 data_8 _database_code_CSD 205493 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H40 F6 N6 O2 P Rh' _chemical_formula_weight 726.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 8.960(2) _cell_length_b 12.110(3) _cell_length_c 14.639(4) _cell_angle_alpha 90.00(3) _cell_angle_beta 101.89(2) _cell_angle_gamma 90.00(2) _cell_volume 1554.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10053 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.56 _reflns_number_total 4700 _reflns_number_gt 3605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(4) _refine_ls_number_reflns 4700 _refine_ls_number_parameters 399 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 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 0.66294(4) 0.80144(4) 0.57908(4) 0.02863(11) Uani 1 1 d . . . O1 O 0.5863(5) 0.5856(3) 0.6992(3) 0.0378(11) Uani 1 1 d . . . O2 O -0.6433(6) 0.4775(5) -0.2440(4) 0.0745(17) Uani 1 1 d . . . N1 N 0.4985(6) 0.6294(4) 0.4511(3) 0.0278(11) Uani 1 1 d . . . N2 N 0.3511(6) 0.6327(5) 0.4681(4) 0.0332(14) Uani 1 1 d . . . N3 N 0.4468(5) 0.8090(4) 0.3914(3) 0.0296(10) Uani 1 1 d . . . N6 N 0.7711(7) 0.7683(5) 0.4663(5) 0.0264(14) Uani 1 1 d . . . N4 N 0.4860(5) 0.8667(4) 0.4724(4) 0.0270(12) Uani 1 1 d . . . N5 N 0.6829(5) 0.7267(4) 0.3856(3) 0.0281(11) Uani 1 1 d . . . C1 C 0.5239(6) 0.7068(5) 0.3801(4) 0.0305(13) Uani 1 1 d . . . H1 H 0.4792 0.6754 0.3172 0.037 Uiso 1 1 calc R . . C2 C 0.6944(7) 0.6782(5) 0.2207(4) 0.0415(16) Uani 1 1 d . . . H2A H 0.7724 0.6764 0.1827 0.062 Uiso 1 1 calc R . . H2B H 0.6120 0.7282 0.1921 0.062 Uiso 1 1 calc R . . H2C H 0.6531 0.6037 0.2245 0.062 Uiso 1 1 calc R . . C3 C 0.7632(7) 0.7177(5) 0.3157(4) 0.0340(15) Uani 1 1 d . . . C4 C 0.9062(9) 0.7522(7) 0.3544(6) 0.045(2) Uani 1 1 d . . . H4 H 0.9898 0.7555 0.3238 0.054 Uiso 1 1 calc R . . C5 C 0.9094(9) 0.7825(6) 0.4479(6) 0.0305(19) Uani 1 1 d . . . C6 C 1.0402(6) 0.8306(6) 0.5161(4) 0.0409(16) Uani 1 1 d . . . H6A H 1.0439 0.9105 0.5064 0.061 Uiso 1 1 calc R . . H6B H 1.1356 0.7970 0.5069 0.061 Uiso 1 1 calc R . . H6C H 1.0271 0.8157 0.5798 0.061 Uiso 1 1 calc R . . C7 C 0.2628(7) 0.8079(6) 0.2377(4) 0.0446(17) Uani 1 1 d . . . H7A H 0.1716 0.8492 0.2079 0.067 Uiso 1 1 calc R . . H7B H 0.2351 0.7308 0.2462 0.067 Uiso 1 1 calc R . . H7C H 0.3385 0.8108 0.1981 0.067 Uiso 1 1 calc R . . C8 C 0.3286(6) 0.8581(5) 0.3311(4) 0.0319(14) Uani 1 1 d . . . C9 C 0.2965(7) 0.9520(5) 0.3740(4) 0.0364(15) Uani 1 1 d . . . H9 H 0.2212 1.0051 0.3490 0.044 Uiso 1 1 calc R . . C10 C 0.3955(6) 0.9566(5) 0.4630(4) 0.0296(14) Uani 1 1 d . . . C11 C 0.4025(7) 1.0430(5) 0.5340(5) 0.0398(16) Uani 1 1 d . . . H11A H 0.3588 1.0150 0.5856 0.060 Uiso 1 1 calc R . . H11B H 0.3444 1.1076 0.5062 0.060 Uiso 1 1 calc R . . H11C H 0.5091 1.0642 0.5576 0.060 Uiso 1 1 calc R . . C12 C 0.7127(7) 0.4932(6) 0.4463(5) 0.0462(18) Uani 1 1 d . . . H12A H 0.7407 0.4196 0.4720 0.069 Uiso 1 1 calc R . . H12B H 0.7903 0.5467 0.4752 0.069 Uiso 1 1 calc R . . H12C H 0.7063 0.4922 0.3787 0.069 Uiso 1 1 calc R . . C13 C 0.5614(7) 0.5255(5) 0.4663(4) 0.0291(13) Uani 1 1 d . . . C14 C 0.4592(7) 0.4638(5) 0.5021(4) 0.0336(14) Uani 1 1 d . . . H14 H 0.4723 0.3899 0.5240 0.040 Uiso 1 1 calc R . . C15 C 0.3298(7) 0.5318(5) 0.4999(4) 0.0359(15) Uani 1 1 d . . . C16 C 0.1842(8) 0.5027(6) 0.5310(5) 0.055(2) Uani 1 1 d . . . H16A H 0.2023 0.5039 0.5994 0.083 Uiso 1 1 calc R . . H16B H 0.1508 0.4288 0.5084 0.083 Uiso 1 1 calc R . . H16C H 0.1050 0.5567 0.5056 0.083 Uiso 1 1 calc R . . C17 C 0.6410(6) 0.6795(5) 0.7003(4) 0.0291(13) Uani 1 1 d . . . C18 C 0.7982(6) 0.7101(5) 0.6917(4) 0.0310(14) Uani 1 1 d . . . C19 C 0.8186(7) 0.8233(5) 0.7108(5) 0.0312(16) Uani 1 1 d . . . C20 C 0.6720(7) 0.8715(5) 0.7144(4) 0.0313(14) Uani 1 1 d . . . C21 C 0.5631(9) 0.7861(6) 0.7005(5) 0.0288(19) Uani 1 1 d . . . C22 C 0.9163(8) 0.6224(7) 0.6853(6) 0.043(2) Uani 1 1 d . . . H22A H 0.9954 0.6543 0.6549 0.051 Uiso 1 1 calc R . . H22B H 0.8668 0.5610 0.6457 0.051 Uiso 1 1 calc R . . C23 C 0.9915(7) 0.5775(6) 0.7804(5) 0.0496(18) Uani 1 1 d . . . H23A H 1.0484 0.6367 0.8179 0.074 Uiso 1 1 calc R . . H23B H 1.0616 0.5177 0.7728 0.074 Uiso 1 1 calc R . . H23C H 0.9131 0.5490 0.8121 0.074 Uiso 1 1 calc R . . C24 C 0.9650(7) 0.8872(6) 0.7367(5) 0.0459(17) Uani 1 1 d . . . H24A H 0.9861 0.9033 0.8037 0.069 Uiso 1 1 calc R . . H24B H 0.9555 0.9566 0.7015 0.069 Uiso 1 1 calc R . . H24C H 1.0487 0.8434 0.7216 0.069 Uiso 1 1 calc R . . C25 C 0.6527(7) 0.9883(5) 0.7450(4) 0.0378(15) Uani 1 1 d . . . H25A H 0.5439 1.0042 0.7394 0.057 Uiso 1 1 calc R . . H25B H 0.6958 1.0394 0.7054 0.057 Uiso 1 1 calc R . . H25C H 0.7057 0.9974 0.8101 0.057 Uiso 1 1 calc R . . C26 C 0.3991(9) 0.7899(6) 0.7107(6) 0.034(2) Uani 1 1 d . . . H26A H 0.3393 0.7327 0.6706 0.041 Uiso 1 1 calc R . . H26B H 0.3545 0.8629 0.6907 0.041 Uiso 1 1 calc R . . C27 C 0.3925(8) 0.7693(6) 0.8126(5) 0.0358(19) Uani 1 1 d . . . H27A H 0.4407 0.6983 0.8327 0.054 Uiso 1 1 calc R . . H27B H 0.2858 0.7678 0.8191 0.054 Uiso 1 1 calc R . . H27C H 0.4467 0.8285 0.8514 0.054 Uiso 1 1 calc R . . P1 P -0.1210(2) 0.83054(15) 0.01597(13) 0.0466(5) Uani 1 1 d . . . F1 F 0.0419(6) 0.8722(5) 0.0131(5) 0.117(2) Uani 1 1 d . . . F2 F -0.1008(6) 0.8781(4) 0.1192(4) 0.0930(18) Uani 1 1 d . . . F3 F -0.1522(7) 0.7798(4) -0.0854(3) 0.0938(18) Uani 1 1 d . . . F4 F -0.2879(5) 0.7895(4) 0.0227(3) 0.0753(14) Uani 1 1 d . . . F5 F -0.0567(5) 0.7177(3) 0.0593(3) 0.0655(12) Uani 1 1 d . . . F6 F -0.1897(7) 0.9452(4) -0.0259(5) 0.117(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02037(19) 0.0394(2) 0.0265(2) 0.0053(4) 0.00555(14) 0.0062(3) O1 0.038(2) 0.034(3) 0.041(3) 0.001(2) 0.007(2) 0.001(2) O2 0.059(4) 0.079(4) 0.083(4) 0.008(3) 0.009(3) 0.005(3) N1 0.022(3) 0.027(3) 0.035(3) 0.004(2) 0.007(2) 0.000(2) N2 0.025(3) 0.036(3) 0.039(3) 0.001(3) 0.007(2) -0.003(2) N3 0.031(3) 0.030(3) 0.027(3) 0.003(2) 0.003(2) -0.001(2) N6 0.017(3) 0.031(3) 0.031(3) 0.003(3) 0.005(2) 0.003(3) N4 0.019(3) 0.031(3) 0.031(3) 0.005(2) 0.007(2) 0.001(2) N5 0.023(2) 0.034(3) 0.029(3) 0.005(2) 0.009(2) 0.001(2) C1 0.029(3) 0.040(3) 0.023(3) 0.003(3) 0.008(2) 0.001(3) C2 0.049(4) 0.048(4) 0.034(4) -0.003(3) 0.023(3) -0.009(3) C3 0.046(4) 0.032(4) 0.029(3) 0.000(3) 0.019(3) -0.002(3) C4 0.039(4) 0.051(5) 0.053(5) -0.001(4) 0.031(4) -0.008(4) C5 0.028(4) 0.032(4) 0.031(5) 0.002(3) 0.005(3) -0.001(3) C6 0.020(3) 0.062(4) 0.042(4) 0.009(3) 0.009(3) -0.002(3) C7 0.032(3) 0.058(4) 0.036(4) 0.010(4) -0.010(3) 0.000(3) C8 0.019(3) 0.039(4) 0.037(4) 0.010(3) 0.006(3) -0.001(3) C9 0.029(3) 0.040(4) 0.038(4) 0.015(3) 0.002(3) 0.006(3) C10 0.023(3) 0.030(3) 0.037(4) 0.003(3) 0.008(3) 0.002(3) C11 0.037(4) 0.035(4) 0.049(4) 0.005(3) 0.012(3) 0.007(3) C12 0.046(4) 0.046(4) 0.052(4) 0.011(4) 0.021(3) 0.018(3) C13 0.034(3) 0.030(3) 0.023(3) -0.002(3) 0.006(3) 0.001(3) C14 0.043(4) 0.026(3) 0.030(3) 0.003(3) 0.004(3) -0.007(3) C15 0.037(4) 0.040(4) 0.032(4) -0.006(3) 0.010(3) -0.011(3) C16 0.054(4) 0.062(5) 0.057(5) -0.007(4) 0.031(4) -0.022(4) C17 0.031(3) 0.033(4) 0.021(3) 0.002(3) -0.001(2) -0.001(3) C18 0.024(3) 0.044(4) 0.025(3) 0.003(3) 0.004(2) 0.009(3) C19 0.025(3) 0.039(4) 0.030(4) 0.010(3) 0.007(3) -0.004(3) C20 0.026(3) 0.036(3) 0.030(3) 0.005(3) 0.003(3) 0.001(3) C21 0.032(4) 0.037(4) 0.017(4) 0.001(3) 0.006(3) 0.010(3) C22 0.034(5) 0.050(5) 0.044(5) 0.017(4) 0.009(4) 0.014(4) C23 0.033(4) 0.065(5) 0.051(4) 0.019(4) 0.009(3) 0.016(3) C24 0.029(4) 0.063(5) 0.044(4) 0.004(4) 0.007(3) -0.006(3) C25 0.042(4) 0.037(4) 0.034(4) -0.001(3) 0.007(3) 0.004(3) C26 0.022(4) 0.038(5) 0.049(5) 0.004(4) 0.021(4) 0.004(3) C27 0.025(4) 0.045(4) 0.040(4) 0.005(3) 0.014(3) 0.004(3) P1 0.0516(12) 0.0454(11) 0.0398(11) -0.0027(8) 0.0022(9) -0.0033(8) F1 0.056(3) 0.119(4) 0.180(7) 0.028(5) 0.030(4) -0.032(3) F2 0.119(4) 0.084(4) 0.065(3) -0.036(3) -0.006(3) 0.018(3) F3 0.150(5) 0.098(4) 0.035(3) -0.016(3) 0.024(3) -0.032(3) F4 0.046(3) 0.098(4) 0.081(3) 0.009(3) 0.009(2) 0.001(2) F5 0.059(3) 0.060(3) 0.075(3) 0.002(2) 0.008(2) 0.018(2) F6 0.138(5) 0.048(3) 0.136(5) 0.020(3) -0.041(4) -0.005(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 N6 2.118(7) . ? Rh1 N4 2.135(5) . ? Rh1 C20 2.141(6) . ? Rh1 C18 2.142(6) . ? Rh1 C19 2.151(7) . ? Rh1 C21 2.156(8) . ? Rh1 C17 2.348(6) . ? Rh1 C1 3.140(6) . ? Rh1 N2 3.570(6) . ? O1 C17 1.237(7) . ? N1 C13 1.377(7) . ? N1 N2 1.394(6) . ? N1 C1 1.453(7) . ? N2 C15 1.336(8) . ? N3 N4 1.359(7) . ? N3 C8 1.367(7) . ? N3 C1 1.444(7) . ? N6 C5 1.333(10) . ? N6 N5 1.375(8) . ? N4 C10 1.347(7) . ? N5 C3 1.371(7) . ? N5 C1 1.430(7) . ? C2 C3 1.480(8) . ? C3 C4 1.355(10) . ? C4 C5 1.411(12) . ? C5 C6 1.493(9) . ? C7 C8 1.501(8) . ? C8 C9 1.359(9) . ? C9 C10 1.418(8) . ? C10 C11 1.467(9) . ? C12 C13 1.497(8) . ? C13 C14 1.368(8) . ? C14 C15 1.417(8) . ? C15 C16 1.509(9) . ? C17 C21 1.468(9) . ? C17 C18 1.486(8) . ? C18 C19 1.403(9) . ? C18 C22 1.516(9) . ? C19 C20 1.448(9) . ? C19 C24 1.503(8) . ? C20 C21 1.407(10) . ? C20 C25 1.505(8) . ? C21 C26 1.508(11) . ? C22 C23 1.518(9) . ? C26 C27 1.526(11) . ? P1 F1 1.553(5) . ? P1 F5 1.565(4) . ? P1 F3 1.577(5) . ? P1 F6 1.590(5) . ? P1 F2 1.592(5) . ? P1 F4 1.598(5) . ? 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 N6 Rh1 N4 83.7(2) . . ? N6 Rh1 C20 149.3(2) . . ? N4 Rh1 C20 114.3(2) . . ? N6 Rh1 C18 103.0(2) . . ? N4 Rh1 C18 166.3(2) . . ? C20 Rh1 C18 65.5(2) . . ? N6 Rh1 C19 114.0(2) . . ? N4 Rh1 C19 149.0(2) . . ? C20 Rh1 C19 39.4(2) . . ? C18 Rh1 C19 38.2(2) . . ? N6 Rh1 C21 163.85(19) . . ? N4 Rh1 C21 105.2(2) . . ? C20 Rh1 C21 38.2(3) . . ? C18 Rh1 C21 65.5(3) . . ? C19 Rh1 C21 64.8(3) . . ? N6 Rh1 C17 126.4(2) . . ? N4 Rh1 C17 128.35(19) . . ? C20 Rh1 C17 62.8(2) . . ? C18 Rh1 C17 38.3(2) . . ? C19 Rh1 C17 62.6(2) . . ? C21 Rh1 C17 37.7(2) . . ? N6 Rh1 C1 50.6(2) . . ? N4 Rh1 C1 50.46(18) . . ? C20 Rh1 C1 159.28(19) . . ? C18 Rh1 C1 125.4(2) . . ? C19 Rh1 C1 159.6(2) . . ? C21 Rh1 C1 125.5(2) . . ? C17 Rh1 C1 113.15(18) . . ? N6 Rh1 N2 88.7(2) . . ? N4 Rh1 N2 59.03(17) . . ? C20 Rh1 N2 121.6(2) . . ? C18 Rh1 N2 108.7(2) . . ? C19 Rh1 N2 141.3(2) . . ? C21 Rh1 N2 84.7(2) . . ? C17 Rh1 N2 78.73(17) . . ? C1 Rh1 N2 41.01(14) . . ? C13 N1 N2 111.7(5) . . ? C13 N1 C1 125.8(5) . . ? N2 N1 C1 113.7(5) . . ? C15 N2 N1 104.1(5) . . ? C15 N2 Rh1 121.3(4) . . ? N1 N2 Rh1 54.3(3) . . ? N4 N3 C8 111.5(5) . . ? N4 N3 C1 119.8(5) . . ? C8 N3 C1 128.6(5) . . ? C5 N6 N5 105.5(7) . . ? C5 N6 Rh1 136.6(6) . . ? N5 N6 Rh1 117.7(4) . . ? C10 N4 N3 106.5(5) . . ? C10 N4 Rh1 135.6(4) . . ? N3 N4 Rh1 117.9(4) . . ? C3 N5 N6 111.9(5) . . ? C3 N5 C1 127.9(5) . . ? N6 N5 C1 120.0(5) . . ? N5 C1 N3 110.2(5) . . ? N5 C1 N1 111.6(4) . . ? N3 C1 N1 108.8(5) . . ? N5 C1 Rh1 71.7(3) . . ? N3 C1 Rh1 71.9(3) . . ? N1 C1 Rh1 70.2(3) . . ? C4 C3 N5 105.1(6) . . ? C4 C3 C2 131.9(6) . . ? N5 C3 C2 123.1(6) . . ? C3 C4 C5 108.3(7) . . ? N6 C5 C4 109.2(7) . . ? N6 C5 C6 123.3(8) . . ? C4 C5 C6 127.4(8) . . ? C9 C8 N3 105.9(5) . . ? C9 C8 C7 132.8(5) . . ? N3 C8 C7 121.2(6) . . ? C8 C9 C10 107.8(5) . . ? N4 C10 C9 108.2(6) . . ? N4 C10 C11 124.5(6) . . ? C9 C10 C11 127.3(5) . . ? C14 C13 N1 106.1(5) . . ? C14 C13 C12 129.5(6) . . ? N1 C13 C12 124.4(5) . . ? C13 C14 C15 106.4(5) . . ? N2 C15 C14 111.4(5) . . ? N2 C15 C16 120.9(6) . . ? C14 C15 C16 127.7(6) . . ? O1 C17 C21 128.4(6) . . ? O1 C17 C18 127.4(6) . . ? C21 C17 C18 103.9(5) . . ? O1 C17 Rh1 131.5(4) . . ? C21 C17 Rh1 64.0(4) . . ? C18 C17 Rh1 63.3(3) . . ? C19 C18 C17 108.3(5) . . ? C19 C18 C22 129.2(6) . . ? C17 C18 C22 121.1(6) . . ? C19 C18 Rh1 71.3(4) . . ? C17 C18 Rh1 78.4(3) . . ? C22 C18 Rh1 127.2(5) . . ? C18 C19 C20 108.6(5) . . ? C18 C19 C24 128.6(6) . . ? C20 C19 C24 122.3(6) . . ? C18 C19 Rh1 70.6(3) . . ? C20 C19 Rh1 69.9(4) . . ? C24 C19 Rh1 131.3(5) . . ? C21 C20 C19 107.8(6) . . ? C21 C20 C25 127.9(6) . . ? C19 C20 C25 123.4(5) . . ? C21 C20 Rh1 71.5(4) . . ? C19 C20 Rh1 70.7(4) . . ? C25 C20 Rh1 131.6(4) . . ? C20 C21 C17 109.3(6) . . ? C20 C21 C26 128.7(7) . . ? C17 C21 C26 120.0(6) . . ? C20 C21 Rh1 70.3(4) . . ? C17 C21 Rh1 78.3(4) . . ? C26 C21 Rh1 131.1(6) . . ? C18 C22 C23 112.2(6) . . ? C21 C26 C27 109.1(7) . . ? F1 P1 F5 91.5(3) . . ? F1 P1 F3 95.0(4) . . ? F5 P1 F3 91.2(3) . . ? F1 P1 F6 89.8(3) . . ? F5 P1 F6 178.3(4) . . ? F3 P1 F6 89.9(3) . . ? F1 P1 F2 89.1(3) . . ? F5 P1 F2 88.3(3) . . ? F3 P1 F2 175.9(3) . . ? F6 P1 F2 90.5(3) . . ? F1 P1 F4 177.9(4) . . ? F5 P1 F4 88.5(3) . . ? F3 P1 F4 87.1(3) . . ? F6 P1 F4 90.2(3) . . ? F2 P1 F4 88.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 C1 N1 N2 101.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.548 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.084 data_9 _database_code_CSD 205494 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H38 Cl4 F6 N6 O P Rh' _chemical_formula_weight 948.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 18.5922(5) _cell_length_b 12.7967(3) _cell_length_c 16.7223(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.7780(10) _cell_angle_gamma 90.00 _cell_volume 3976.63(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20233 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6971 _reflns_number_gt 5601 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^+12.3410P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6971 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 -0.285926(17) -0.04277(3) 0.632891(19) 0.02220(11) Uani 1 1 d . . . O1 O -0.42921(18) -0.1289(3) 0.6756(2) 0.0428(9) Uani 1 1 d . . . N6 N -0.22061(19) -0.1019(3) 0.7339(2) 0.0268(8) Uani 1 1 d . . . N5 N -0.16804(18) -0.0372(3) 0.7648(2) 0.0263(8) Uani 1 1 d . . . N4 N -0.28871(18) 0.1018(3) 0.7032(2) 0.0251(8) Uani 1 1 d . . . N3 N -0.22589(19) 0.1273(3) 0.7448(2) 0.0269(8) Uani 1 1 d . . . N2 N -0.18714(18) 0.0150(3) 0.5926(2) 0.0248(8) Uani 1 1 d . . . N1 N -0.14297(18) 0.0639(3) 0.6486(2) 0.0258(8) Uani 1 1 d . . . C1 C -0.3746(3) -0.0955(4) 0.6624(3) 0.0303(10) Uani 1 1 d . . . C2 C -0.2630(3) -0.2820(4) 0.7626(3) 0.0365(11) Uani 1 1 d . . . H2A H -0.3074 -0.2586 0.7350 0.055 Uiso 1 1 calc R . . H2B H -0.2745 -0.3131 0.8142 0.055 Uiso 1 1 calc R . . H2C H -0.2391 -0.3341 0.7296 0.055 Uiso 1 1 calc R . . C3 C -0.2140(2) -0.1906(4) 0.7761(3) 0.0292(10) Uani 1 1 d . . . C4 C -0.1568(2) -0.1817(4) 0.8322(3) 0.0336(11) Uani 1 1 d . . . H4A H -0.1406 -0.2342 0.8686 0.040 Uiso 1 1 calc R . . C5 C -0.1286(2) -0.0837(4) 0.8251(3) 0.0321(10) Uani 1 1 d . . . C6 C -0.0688(3) -0.0297(5) 0.8701(3) 0.0474(14) Uani 1 1 d . . . H6A H -0.0391 0.0085 0.8326 0.071 Uiso 1 1 calc R . . H6B H -0.0392 -0.0815 0.8990 0.071 Uiso 1 1 calc R . . H6C H -0.0890 0.0195 0.9084 0.071 Uiso 1 1 calc R . . C7 C -0.4158(2) 0.1630(4) 0.7044(3) 0.0346(11) Uani 1 1 d . . . H7A H -0.4276 0.0934 0.6834 0.052 Uiso 1 1 calc R . . H7B H -0.4230 0.2150 0.6618 0.052 Uiso 1 1 calc R . . H7C H -0.4471 0.1793 0.7487 0.052 Uiso 1 1 calc R . . C8 C -0.3391(2) 0.1648(3) 0.7334(3) 0.0258(9) Uani 1 1 d . . . C9 C -0.3083(2) 0.2278(4) 0.7943(3) 0.0303(10) Uani 1 1 d . . . H9A H -0.3325 0.2786 0.8249 0.036 Uiso 1 1 calc R . . C10 C -0.2368(3) 0.2023(3) 0.8012(3) 0.0299(10) Uani 1 1 d . . . C11 C -0.1787(3) 0.2419(4) 0.8567(3) 0.0440(13) Uani 1 1 d . . . H11A H -0.1598 0.1841 0.8896 0.066 Uiso 1 1 calc R . . H11B H -0.1983 0.2959 0.8915 0.066 Uiso 1 1 calc R . . H11C H -0.1399 0.2717 0.8256 0.066 Uiso 1 1 calc R . . C12 C -0.1814(3) -0.0235(4) 0.4466(3) 0.0377(12) Uani 1 1 d . . . H12A H -0.1958 -0.0963 0.4550 0.057 Uiso 1 1 calc R . . H12B H -0.1441 -0.0209 0.4064 0.057 Uiso 1 1 calc R . . H12C H -0.2232 0.0172 0.4278 0.057 Uiso 1 1 calc R . . C13 C -0.1525(2) 0.0211(3) 0.5233(3) 0.0279(10) Uani 1 1 d . . . C14 C -0.0865(2) 0.0726(4) 0.5364(3) 0.0341(11) Uani 1 1 d . . . H14A H -0.0519 0.0872 0.4973 0.041 Uiso 1 1 calc R . . C15 C -0.0814(2) 0.0976(4) 0.6158(3) 0.0312(10) Uani 1 1 d . . . C16 C -0.0221(3) 0.1494(4) 0.6639(3) 0.0432(13) Uani 1 1 d . . . H16A H -0.0408 0.2119 0.6900 0.065 Uiso 1 1 calc R . . H16B H 0.0166 0.1696 0.6285 0.065 Uiso 1 1 calc R . . H16C H -0.0032 0.1008 0.7046 0.065 Uiso 1 1 calc R . . C17 C -0.1613(2) 0.0672(3) 0.7323(2) 0.0256(9) Uani 1 1 d . . . H17A H -0.1208 0.1026 0.7623 0.031 Uiso 1 1 calc R . . C18 C -0.3426(2) 0.0010(3) 0.5304(2) 0.0248(9) Uani 1 1 d . . . C19 C -0.3652(2) 0.1093(3) 0.5131(2) 0.0269(9) Uani 1 1 d . . . C20 C -0.3206(2) 0.1954(3) 0.5297(3) 0.0287(10) Uani 1 1 d . . . H20A H -0.2736 0.1841 0.5520 0.034 Uiso 1 1 calc R . . C21 C -0.3436(3) 0.2964(4) 0.5144(3) 0.0329(10) Uani 1 1 d . . . H21A H -0.3125 0.3536 0.5260 0.039 Uiso 1 1 calc R . . C22 C -0.4122(3) 0.3142(4) 0.4821(3) 0.0354(11) Uani 1 1 d . . . H22A H -0.4284 0.3837 0.4726 0.043 Uiso 1 1 calc R . . C23 C -0.4570(3) 0.2304(4) 0.4638(3) 0.0341(11) Uani 1 1 d . . . H23A H -0.5037 0.2423 0.4410 0.041 Uiso 1 1 calc R . . C24 C -0.4335(2) 0.1293(4) 0.4787(3) 0.0299(10) Uani 1 1 d . . . H24A H -0.4643 0.0724 0.4653 0.036 Uiso 1 1 calc R . . C25 C -0.3567(2) -0.0799(3) 0.4809(3) 0.0274(9) Uani 1 1 d . . . H25A H -0.3856 -0.0714 0.4335 0.033 Uiso 1 1 calc R . . C26 C -0.3258(2) -0.1812(3) 0.5025(2) 0.0269(9) Uani 1 1 d . . . C27 C -0.3403(2) -0.2765(3) 0.4546(2) 0.0281(10) Uani 1 1 d . . . C28 C -0.4039(3) -0.2857(4) 0.4082(3) 0.0340(11) Uani 1 1 d . . . H28A H -0.4365 -0.2285 0.4050 0.041 Uiso 1 1 calc R . . C29 C -0.4200(3) -0.3769(4) 0.3670(3) 0.0441(13) Uani 1 1 d . . . H29A H -0.4638 -0.3824 0.3364 0.053 Uiso 1 1 calc R . . C30 C -0.3729(3) -0.4594(4) 0.3703(3) 0.0476(14) Uani 1 1 d . . . H30A H -0.3842 -0.5220 0.3420 0.057 Uiso 1 1 calc R . . C31 C -0.3091(3) -0.4518(4) 0.4146(3) 0.0412(12) Uani 1 1 d . . . H31A H -0.2763 -0.5087 0.4159 0.049 Uiso 1 1 calc R . . C32 C -0.2932(3) -0.3617(4) 0.4567(3) 0.0348(11) Uani 1 1 d . . . H32A H -0.2495 -0.3575 0.4876 0.042 Uiso 1 1 calc R . . C33 C -0.2851(2) -0.1791(3) 0.5705(3) 0.0272(9) Uani 1 1 d . . . H33 H -0.2576 -0.2377 0.5882 0.033 Uiso 1 1 calc R . . P1 P -0.15301(7) 0.44764(13) 0.65707(10) 0.0507(4) Uani 1 1 d . . . F1 F -0.2004(2) 0.4560(3) 0.7362(3) 0.0836(12) Uani 1 1 d . . . F2 F -0.1057(2) 0.4411(5) 0.5828(3) 0.1133(19) Uani 1 1 d . . . F3 F -0.2033(3) 0.3595(6) 0.6303(4) 0.170(3) Uani 1 1 d . . . F4 F -0.1031(3) 0.3685(5) 0.7009(4) 0.135(2) Uani 1 1 d . . . F5 F -0.1022(3) 0.5340(5) 0.6931(4) 0.142(2) Uani 1 1 d . . . F6 F -0.2025(3) 0.5332(6) 0.6193(3) 0.147(3) Uani 1 1 d . . . C100 C 0.0854(3) 0.2282(5) 0.3816(4) 0.0555(15) Uani 1 1 d . . . H10A H 0.1283 0.1832 0.3901 0.067 Uiso 1 1 calc R . . H10B H 0.0994 0.2887 0.3487 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.05676(16) 0.2721(2) 0.47314(11) 0.1201(10) Uani 1 1 d . . . Cl2 Cl 0.01789(8) 0.15728(12) 0.33052(8) 0.0532(4) Uani 1 1 d . . . C101 C 0.6265(3) 0.0167(5) 0.1783(3) 0.0513(14) Uani 1 1 d . . . H10C H 0.6224 0.0859 0.1520 0.062 Uiso 1 1 calc R . . H10D H 0.6783 -0.0002 0.1849 0.062 Uiso 1 1 calc R . . Cl3 Cl 0.58855(10) 0.02375(14) 0.27297(9) 0.0656(4) Uani 1 1 d . . . Cl4 Cl 0.58522(11) -0.07608(17) 0.11778(12) 0.0864(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02314(18) 0.02247(18) 0.02080(17) -0.00132(14) -0.00217(12) -0.00100(14) O1 0.034(2) 0.056(2) 0.0385(19) -0.0053(17) 0.0029(15) -0.0149(17) N6 0.0264(19) 0.028(2) 0.0256(18) -0.0016(16) 0.0010(15) -0.0003(16) N5 0.0221(18) 0.0288(19) 0.0277(18) -0.0009(16) -0.0044(15) -0.0003(16) N4 0.0213(18) 0.029(2) 0.0244(18) -0.0007(15) -0.0027(14) -0.0027(15) N3 0.0271(19) 0.0238(19) 0.0298(19) -0.0062(16) -0.0011(15) -0.0013(15) N2 0.0255(19) 0.026(2) 0.0223(18) -0.0033(15) -0.0012(14) -0.0022(15) N1 0.0217(18) 0.031(2) 0.0248(18) -0.0046(15) -0.0013(14) -0.0015(15) C1 0.032(3) 0.037(3) 0.022(2) -0.0025(19) -0.0030(18) 0.003(2) C2 0.045(3) 0.031(3) 0.033(2) 0.006(2) 0.005(2) -0.001(2) C3 0.032(2) 0.030(2) 0.026(2) 0.0017(19) 0.0061(19) 0.0091(19) C4 0.032(3) 0.039(3) 0.030(2) 0.011(2) 0.002(2) 0.009(2) C5 0.026(2) 0.042(3) 0.028(2) 0.004(2) 0.0004(18) 0.006(2) C6 0.034(3) 0.063(4) 0.045(3) 0.011(3) -0.014(2) -0.004(3) C7 0.032(3) 0.033(3) 0.039(3) 0.001(2) 0.002(2) 0.005(2) C8 0.029(2) 0.022(2) 0.026(2) 0.0037(18) 0.0029(18) 0.0013(18) C9 0.036(3) 0.025(2) 0.031(2) -0.0035(19) 0.0084(19) -0.001(2) C10 0.039(3) 0.023(2) 0.027(2) -0.0033(19) 0.0041(19) -0.007(2) C11 0.046(3) 0.041(3) 0.045(3) -0.019(2) -0.005(2) -0.008(2) C12 0.049(3) 0.040(3) 0.024(2) -0.004(2) 0.007(2) -0.008(2) C13 0.030(2) 0.027(2) 0.027(2) 0.0037(18) 0.0037(18) 0.0002(18) C14 0.033(3) 0.037(3) 0.033(2) 0.001(2) 0.008(2) -0.004(2) C15 0.026(2) 0.029(3) 0.039(3) 0.002(2) 0.0061(19) -0.0017(19) C16 0.034(3) 0.049(3) 0.047(3) -0.002(3) 0.004(2) -0.014(2) C17 0.022(2) 0.032(2) 0.022(2) -0.0043(18) -0.0047(16) -0.0034(18) C18 0.026(2) 0.026(2) 0.022(2) 0.0014(18) -0.0004(17) -0.0026(18) C19 0.032(2) 0.028(2) 0.021(2) 0.0019(18) 0.0012(18) 0.0017(19) C20 0.031(2) 0.027(2) 0.027(2) -0.0003(19) 0.0010(18) -0.0018(19) C21 0.043(3) 0.024(2) 0.032(2) -0.001(2) 0.004(2) -0.009(2) C22 0.043(3) 0.029(3) 0.034(3) 0.001(2) 0.000(2) 0.008(2) C23 0.032(3) 0.038(3) 0.032(2) 0.006(2) -0.0061(19) 0.007(2) C24 0.030(2) 0.030(2) 0.029(2) -0.002(2) -0.0014(19) -0.002(2) C25 0.029(2) 0.029(2) 0.025(2) 0.0010(18) -0.0066(18) -0.0025(19) C26 0.030(2) 0.028(2) 0.022(2) -0.0010(18) -0.0001(18) -0.0025(19) C27 0.037(3) 0.025(2) 0.022(2) -0.0023(18) 0.0052(18) -0.0074(19) C28 0.038(3) 0.032(3) 0.032(2) -0.006(2) 0.004(2) -0.003(2) C29 0.050(3) 0.046(3) 0.037(3) -0.011(2) 0.004(2) -0.017(3) C30 0.073(4) 0.034(3) 0.037(3) -0.015(2) 0.018(3) -0.016(3) C31 0.061(3) 0.026(2) 0.038(3) -0.002(2) 0.021(2) 0.001(2) C32 0.044(3) 0.033(3) 0.028(2) 0.001(2) 0.009(2) -0.001(2) C33 0.032(2) 0.021(2) 0.029(2) -0.0005(18) 0.0045(19) 0.0001(18) P1 0.0319(7) 0.0508(9) 0.0690(10) 0.0110(8) -0.0071(7) 0.0013(6) F1 0.081(3) 0.088(3) 0.084(3) 0.016(2) 0.020(2) 0.018(2) F2 0.073(3) 0.194(6) 0.074(3) 0.008(3) 0.015(2) 0.019(3) F3 0.130(5) 0.202(7) 0.179(6) -0.093(6) 0.019(4) -0.100(5) F4 0.112(4) 0.150(5) 0.143(5) 0.060(4) 0.012(3) 0.076(4) F5 0.119(4) 0.123(5) 0.185(6) -0.051(4) 0.017(4) -0.058(4) F6 0.098(4) 0.221(7) 0.123(4) 0.100(5) 0.034(3) 0.084(4) C100 0.050(3) 0.057(4) 0.058(4) 0.011(3) -0.003(3) 0.002(3) Cl1 0.189(3) 0.125(2) 0.0474(10) -0.0255(11) 0.0233(13) -0.0746(19) Cl2 0.0543(8) 0.0605(9) 0.0447(7) -0.0017(7) -0.0015(6) 0.0097(7) C101 0.046(3) 0.052(4) 0.056(3) -0.003(3) 0.007(3) -0.006(3) Cl3 0.0804(11) 0.0777(12) 0.0391(7) 0.0026(7) 0.0067(7) -0.0172(9) Cl4 0.0961(14) 0.0817(13) 0.0810(12) -0.0433(11) -0.0022(10) -0.0011(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.861(5) . ? Rh1 C33 2.033(4) . ? Rh1 C18 2.061(4) . ? Rh1 N2 2.110(3) . ? Rh1 N6 2.185(4) . ? Rh1 N4 2.194(4) . ? Rh1 C17 3.142(4) . ? O1 C1 1.130(5) . ? N6 C3 1.340(6) . ? N6 N5 1.369(5) . ? N5 C5 1.364(6) . ? N5 C17 1.450(6) . ? N4 C8 1.347(5) . ? N4 N3 1.380(5) . ? N3 C10 1.366(6) . ? N3 C17 1.447(5) . ? N2 C13 1.345(5) . ? N2 N1 1.377(5) . ? N1 C15 1.355(5) . ? N1 C17 1.451(5) . ? C2 C3 1.495(7) . ? C3 C4 1.400(6) . ? C4 C5 1.365(7) . ? C5 C6 1.492(7) . ? C7 C8 1.491(6) . ? C8 C9 1.406(6) . ? C9 C10 1.370(6) . ? C10 C11 1.491(6) . ? C12 C13 1.489(6) . ? C13 C14 1.403(6) . ? C14 C15 1.367(6) . ? C15 C16 1.499(6) . ? C18 C25 1.347(6) . ? C18 C19 1.474(6) . ? C19 C24 1.401(6) . ? C19 C20 1.402(6) . ? C20 C21 1.383(6) . ? C21 C22 1.388(7) . ? C22 C23 1.386(7) . ? C23 C24 1.386(6) . ? C25 C26 1.458(6) . ? C26 C33 1.346(6) . ? C26 C27 1.479(6) . ? C27 C32 1.399(7) . ? C27 C28 1.400(6) . ? C28 C29 1.384(7) . ? C29 C30 1.371(8) . ? C30 C31 1.383(8) . ? C31 C32 1.379(7) . ? P1 F3 1.523(5) . ? P1 F4 1.544(5) . ? P1 F2 1.547(5) . ? P1 F6 1.552(5) . ? P1 F5 1.563(5) . ? P1 F1 1.615(4) . ? C100 Cl1 1.730(6) . ? C100 Cl2 1.750(6) . ? C101 Cl4 1.726(6) . ? C101 Cl3 1.755(6) . ? 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 C1 Rh1 C33 81.14(18) . . ? C1 Rh1 C18 83.37(17) . . ? C33 Rh1 C18 79.56(17) . . ? C1 Rh1 N2 176.71(16) . . ? C33 Rh1 N2 96.66(15) . . ? C18 Rh1 N2 93.85(15) . . ? C1 Rh1 N6 98.33(16) . . ? C33 Rh1 N6 94.98(16) . . ? C18 Rh1 N6 174.00(15) . . ? N2 Rh1 N6 84.26(13) . . ? C1 Rh1 N4 97.36(17) . . ? C33 Rh1 N4 178.19(15) . . ? C18 Rh1 N4 101.30(15) . . ? N2 Rh1 N4 84.89(13) . . ? N6 Rh1 N4 84.23(13) . . ? C1 Rh1 C17 131.81(15) . . ? C33 Rh1 C17 129.65(15) . . ? C18 Rh1 C17 131.90(14) . . ? N2 Rh1 C17 51.46(12) . . ? N6 Rh1 C17 50.42(12) . . ? N4 Rh1 C17 50.82(12) . . ? C3 N6 N5 105.1(3) . . ? C3 N6 Rh1 137.7(3) . . ? N5 N6 Rh1 117.1(3) . . ? C5 N5 N6 112.1(4) . . ? C5 N5 C17 128.9(4) . . ? N6 N5 C17 118.9(3) . . ? C8 N4 N3 104.9(3) . . ? C8 N4 Rh1 137.3(3) . . ? N3 N4 Rh1 115.8(2) . . ? C10 N3 N4 111.9(3) . . ? C10 N3 C17 128.0(4) . . ? N4 N3 C17 119.7(3) . . ? C13 N2 N1 105.5(3) . . ? C13 N2 Rh1 137.8(3) . . ? N1 N2 Rh1 116.7(2) . . ? C15 N1 N2 111.3(3) . . ? C15 N1 C17 127.4(4) . . ? N2 N1 C17 121.1(3) . . ? O1 C1 Rh1 175.8(4) . . ? N6 C3 C4 109.8(4) . . ? N6 C3 C2 122.5(4) . . ? C4 C3 C2 127.7(4) . . ? C5 C4 C3 107.6(4) . . ? N5 C5 C4 105.4(4) . . ? N5 C5 C6 123.0(4) . . ? C4 C5 C6 131.6(4) . . ? N4 C8 C9 110.0(4) . . ? N4 C8 C7 122.5(4) . . ? C9 C8 C7 127.5(4) . . ? C10 C9 C8 107.4(4) . . ? N3 C10 C9 105.8(4) . . ? N3 C10 C11 123.3(4) . . ? C9 C10 C11 130.9(4) . . ? N2 C13 C14 109.4(4) . . ? N2 C13 C12 123.4(4) . . ? C14 C13 C12 127.2(4) . . ? C15 C14 C13 107.2(4) . . ? N1 C15 C14 106.5(4) . . ? N1 C15 C16 122.7(4) . . ? C14 C15 C16 130.8(4) . . ? N3 C17 N5 110.7(3) . . ? N3 C17 N1 112.1(3) . . ? N5 C17 N1 111.2(3) . . ? N3 C17 Rh1 73.3(2) . . ? N5 C17 Rh1 73.4(2) . . ? N1 C17 Rh1 70.6(2) . . ? C25 C18 C19 123.6(4) . . ? C25 C18 Rh1 112.8(3) . . ? C19 C18 Rh1 123.6(3) . . ? C24 C19 C20 117.5(4) . . ? C24 C19 C18 120.1(4) . . ? C20 C19 C18 122.4(4) . . ? C21 C20 C19 121.3(4) . . ? C20 C21 C22 120.1(4) . . ? C23 C22 C21 119.8(4) . . ? C24 C23 C22 119.9(4) . . ? C23 C24 C19 121.4(4) . . ? C18 C25 C26 117.6(4) . . ? C33 C26 C25 113.5(4) . . ? C33 C26 C27 124.2(4) . . ? C25 C26 C27 122.3(4) . . ? C32 C27 C28 117.7(4) . . ? C32 C27 C26 121.8(4) . . ? C28 C27 C26 120.4(4) . . ? C29 C28 C27 120.9(5) . . ? C30 C29 C28 120.1(5) . . ? C29 C30 C31 120.2(5) . . ? C32 C31 C30 120.0(5) . . ? C31 C32 C27 121.0(5) . . ? C26 C33 Rh1 115.9(3) . . ? F3 P1 F4 90.5(4) . . ? F3 P1 F2 94.7(4) . . ? F4 P1 F2 89.9(3) . . ? F3 P1 F6 93.0(4) . . ? F4 P1 F6 175.2(4) . . ? F2 P1 F6 93.2(3) . . ? F3 P1 F5 174.4(4) . . ? F4 P1 F5 86.2(4) . . ? F2 P1 F5 89.7(3) . . ? F6 P1 F5 90.1(4) . . ? F3 P1 F1 86.9(3) . . ? F4 P1 F1 89.4(3) . . ? F2 P1 F1 178.2(3) . . ? F6 P1 F1 87.4(3) . . ? F5 P1 F1 88.6(3) . . ? Cl1 C100 Cl2 111.4(3) . . ? Cl4 C101 Cl3 112.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 C17 N1 N2 -3.2(3) . . . . ? Rh1 C33 C26 C25 7.0(5) . . . . ? C33 C26 C25 C18 -1.3(6) . . . . ? C26 C25 C18 Rh1 -4.9(5) . . . . ? C25 C18 Rh1 C33 6.5(3) . . . . ? C18 Rh1 C33 C26 -7.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.744 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.092 data_11 _database_code_CSD 205495 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H28 F6 N6 O P Rh' _chemical_formula_weight 652.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.899(4) _cell_length_b 11.025(2) _cell_length_c 24.751(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5157.1(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.288 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% none _diffrn_reflns_number 26359 _diffrn_reflns_av_R_equivalents 0.2224 _diffrn_reflns_av_sigmaI/netI 0.1259 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4538 _reflns_number_gt 2429 _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^)+(0.0597P)^2^+12.4854P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4538 _refine_ls_number_parameters 404 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1390 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1802 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.005 _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 0.01734(4) -0.08166(6) 0.82303(3) 0.0318(2) Uani 1 1 d . . . N1 N -0.0293(3) 0.0841(7) 0.8549(3) 0.0300(16) Uani 1 1 d . . . N6 N 0.1314(4) 0.0983(7) 0.8598(3) 0.0359(17) Uani 1 1 d . . . N2 N 0.0157(4) 0.1569(6) 0.8839(3) 0.0325(16) Uani 1 1 d . . . C12 C -0.0170(5) 0.2637(8) 0.8972(3) 0.0345(19) Uani 1 1 d . . . N4 N 0.0727(4) -0.0006(6) 0.9320(3) 0.0363(18) Uani 1 1 d . . . N5 N 0.1139(4) 0.0285(7) 0.8158(3) 0.0363(17) Uani 1 1 d . . . N3 N 0.0568(4) -0.1041(6) 0.9040(3) 0.0336(17) Uani 1 1 d . . . C15 C -0.1537(4) 0.0946(9) 0.8227(4) 0.042(2) Uani 1 1 d . . . H15A H -0.1431 0.0815 0.7852 0.063 Uiso 1 1 calc R . . H15B H -0.1920 0.1515 0.8258 0.063 Uiso 1 1 calc R . . H15C H -0.1671 0.0192 0.8391 0.063 Uiso 1 1 calc R . . C18 C 0.0944(5) -0.1470(8) 0.9870(4) 0.038(2) Uani 1 1 d . . . H18 H 0.1073 -0.1924 1.0171 0.045 Uiso 1 1 calc R . . C17 C 0.0962(5) -0.0263(9) 0.9832(3) 0.037(2) Uani 1 1 d . . . C19 C 0.0700(5) -0.1929(8) 0.9382(3) 0.035(2) Uani 1 1 d . . . C16 C 0.1148(5) 0.0716(9) 1.0224(4) 0.046(2) Uani 1 1 d . . . H16A H 0.1245 0.0362 1.0571 0.069 Uiso 1 1 calc R . . H16B H 0.0759 0.1272 1.0256 0.069 Uiso 1 1 calc R . . H16C H 0.1559 0.1142 1.0099 0.069 Uiso 1 1 calc R . . C14 C -0.0895(5) 0.1443(8) 0.8507(3) 0.035(2) Uani 1 1 d . . . C8 C 0.0809(5) 0.1124(8) 0.9028(3) 0.035(2) Uani 1 1 d . . . H1 H 0.1001 0.1723 0.9281 0.042 Uiso 1 1 calc R . . C13 C -0.0826(5) 0.2566(8) 0.8761(3) 0.038(2) Uani 1 1 d . . . H13 H -0.1173 0.3163 0.8780 0.045 Uiso 1 1 calc R . . C20 C 0.0612(6) -0.3260(9) 0.9252(4) 0.052(3) Uani 1 1 d . . . H20A H 0.0121 -0.3432 0.9188 0.078 Uiso 1 1 calc R . . H20B H 0.0778 -0.3738 0.9550 0.078 Uiso 1 1 calc R . . H20C H 0.0882 -0.3454 0.8935 0.078 Uiso 1 1 calc R . . C11 C 0.0193(5) 0.3606(8) 0.9288(4) 0.046(2) Uani 1 1 d . . . H11A H -0.0117 0.4290 0.9327 0.069 Uiso 1 1 calc R . . H11B H 0.0615 0.3853 0.9102 0.069 Uiso 1 1 calc R . . H11C H 0.0316 0.3299 0.9639 0.069 Uiso 1 1 calc R . . P1 P 0.18133(14) 0.0668(2) 0.55613(11) 0.0488(7) Uani 1 1 d D . . C7 C -0.0082(5) -0.0910(8) 0.7399(3) 0.038(2) Uani 1 1 d . . . H7A H 0.0224 -0.0387 0.7179 0.045 Uiso 1 1 calc R . . C24 C 0.1734(5) 0.0247(9) 0.7864(4) 0.042(2) Uani 1 1 d . . . C1 C -0.0825(5) -0.0862(9) 0.7221(4) 0.042(2) Uani 1 1 d . . . C5 C 0.0032(5) -0.2644(9) 0.8009(4) 0.045(3) Uani 1 1 d . . . H5A H 0.0323 -0.3284 0.8170 0.054 Uiso 1 1 calc R . . C4 C -0.0590(5) -0.2208(8) 0.8278(4) 0.044(2) Uani 1 1 d . . . H4A H -0.0651 -0.2537 0.8643 0.052 Uiso 1 1 calc R . . C23 C 0.2271(5) 0.0898(11) 0.8118(4) 0.055(3) Uani 1 1 d . . . H23 H 0.2732 0.0996 0.7995 0.066 Uiso 1 1 calc R . . C22 C 0.1993(6) 0.1363(10) 0.8583(4) 0.049(3) Uani 1 1 d . . . C6 C 0.0274(5) -0.1982(9) 0.7571(4) 0.046(3) Uani 1 1 d . . . H6A H 0.0747 -0.2152 0.7428 0.055 Uiso 1 1 calc R . . C3 C -0.1253(6) -0.2110(9) 0.7975(4) 0.053(3) Uani 1 1 d . . . H3A H -0.1650 -0.2455 0.8134 0.063 Uiso 1 1 calc R . . C25 C 0.1789(5) -0.0395(11) 0.7335(4) 0.059(3) Uani 1 1 d . . . H25A H 0.1841 -0.1250 0.7397 0.089 Uiso 1 1 calc R . . H25B H 0.2194 -0.0099 0.7141 0.089 Uiso 1 1 calc R . . H25C H 0.1369 -0.0250 0.7127 0.089 Uiso 1 1 calc R . . O1 O -0.0994(4) -0.0190(7) 0.6847(3) 0.0586(19) Uani 1 1 d . . . C2 C -0.1355(6) -0.1579(10) 0.7493(4) 0.054(3) Uani 1 1 d . . . H2A H -0.1791 -0.1679 0.7325 0.065 Uiso 1 1 calc R . . C21 C 0.2322(6) 0.2150(13) 0.9014(5) 0.084(4) Uani 1 1 d . . . H21A H 0.2032 0.2853 0.9071 0.125 Uiso 1 1 calc R . . H21B H 0.2786 0.2400 0.8899 0.125 Uiso 1 1 calc R . . H21C H 0.2359 0.1699 0.9344 0.125 Uiso 1 1 calc R . . F1 F 0.1283(10) 0.1486(14) 0.5257(8) 0.109(6) Uani 0.630(18) 1 d PD A 1 F2 F 0.2368(8) 0.0743(15) 0.5111(6) 0.097(6) Uani 0.630(18) 1 d PD A 1 F3 F 0.2066(10) 0.1826(12) 0.5862(6) 0.091(7) Uani 0.630(18) 1 d PD A 1 F4 F 0.1255(7) 0.0470(10) 0.6040(5) 0.071(4) Uani 0.630(18) 1 d PD A 1 F5 F 0.1489(10) -0.0510(14) 0.5305(5) 0.075(6) Uani 0.630(18) 1 d PD A 1 F6 F 0.211(3) -0.010(2) 0.6028(13) 0.28(3) Uani 0.630(18) 1 d PD A 1 F1' F 0.184(2) 0.137(3) 0.5011(8) 0.118(12) Uani 0.370(18) 1 d PD A 2 F2' F 0.1013(8) 0.069(5) 0.5468(15) 0.20(3) Uani 0.370(18) 1 d PD A 2 F3' F 0.174(4) 0.174(5) 0.595(3) 0.38(6) Uani 0.370(18) 1 d PD A 2 F4' F 0.2612(8) 0.093(3) 0.5584(13) 0.130(13) Uani 0.370(18) 1 d PD A 2 F5' F 0.190(4) -0.047(3) 0.5209(19) 0.23(3) Uani 0.370(18) 1 d PD A 2 F6' F 0.2295(11) -0.026(2) 0.5860(9) 0.068(9) Uani 0.370(18) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0446(4) 0.0248(3) 0.0259(3) -0.0023(3) -0.0004(3) -0.0020(3) N1 0.032(4) 0.032(4) 0.027(3) -0.005(3) 0.001(3) -0.002(4) N6 0.037(4) 0.032(4) 0.039(4) -0.003(3) -0.001(3) -0.002(4) N2 0.038(4) 0.029(4) 0.030(4) -0.002(3) -0.006(4) 0.000(4) C12 0.053(6) 0.024(5) 0.027(4) 0.002(3) 0.001(4) -0.003(4) N4 0.049(5) 0.029(4) 0.031(4) -0.003(3) -0.003(3) -0.003(3) N5 0.043(5) 0.033(4) 0.033(4) 0.000(3) 0.001(4) 0.004(3) N3 0.041(4) 0.026(4) 0.034(4) 0.000(3) 0.002(3) -0.005(3) C15 0.036(5) 0.052(6) 0.038(5) 0.000(5) -0.002(4) 0.000(4) C18 0.045(6) 0.035(6) 0.033(5) 0.007(4) -0.006(4) -0.002(4) C17 0.042(6) 0.037(6) 0.032(5) -0.002(4) -0.002(4) 0.005(4) C19 0.033(5) 0.043(6) 0.029(5) 0.002(4) -0.001(4) -0.001(4) C16 0.067(7) 0.036(6) 0.034(5) -0.006(5) -0.009(4) 0.004(5) C14 0.050(6) 0.031(5) 0.023(4) 0.000(4) 0.001(4) -0.001(4) C8 0.044(6) 0.030(5) 0.031(5) -0.011(4) 0.000(4) -0.013(4) C13 0.052(6) 0.027(5) 0.034(5) -0.003(4) 0.001(4) 0.007(4) C20 0.079(8) 0.036(6) 0.041(6) 0.005(5) -0.009(5) 0.002(5) C11 0.061(6) 0.034(5) 0.043(5) -0.008(4) -0.004(5) -0.003(5) P1 0.0506(16) 0.0411(16) 0.0546(16) 0.0082(13) -0.0101(13) -0.0007(13) C7 0.047(6) 0.033(5) 0.033(4) -0.001(4) 0.005(4) 0.004(5) C24 0.048(6) 0.044(6) 0.035(5) 0.004(5) 0.008(5) 0.007(5) C1 0.059(6) 0.034(5) 0.034(5) -0.009(5) -0.001(4) 0.000(5) C5 0.067(7) 0.033(5) 0.034(5) -0.009(4) -0.018(5) -0.001(5) C4 0.064(7) 0.031(5) 0.036(5) 0.002(4) -0.003(5) -0.008(5) C23 0.036(6) 0.071(7) 0.060(7) -0.010(6) 0.005(5) -0.006(6) C22 0.052(7) 0.048(6) 0.048(6) 0.000(5) -0.002(5) -0.006(5) C6 0.062(7) 0.045(6) 0.032(5) -0.015(4) -0.011(5) 0.007(5) C3 0.067(7) 0.042(6) 0.048(6) -0.005(5) -0.003(5) -0.018(5) C25 0.050(7) 0.082(9) 0.046(6) -0.005(6) 0.012(5) 0.000(6) O1 0.079(5) 0.055(4) 0.043(4) 0.012(4) -0.009(4) -0.001(4) C2 0.062(7) 0.051(7) 0.049(6) -0.010(5) -0.017(5) -0.010(5) C21 0.062(8) 0.109(12) 0.080(9) -0.032(8) 0.012(7) -0.033(7) F1 0.095(13) 0.096(11) 0.135(15) 0.054(11) -0.030(12) 0.031(10) F2 0.077(10) 0.114(13) 0.100(12) 0.045(10) 0.030(9) 0.004(9) F3 0.126(14) 0.057(9) 0.090(11) -0.019(8) 0.008(9) -0.060(10) F4 0.109(10) 0.038(7) 0.065(8) -0.016(5) 0.029(7) -0.004(6) F5 0.119(13) 0.067(10) 0.039(6) -0.009(6) -0.002(7) -0.040(9) F6 0.55(7) 0.17(3) 0.111(18) 0.097(17) -0.19(3) -0.19(4) F1' 0.14(3) 0.16(3) 0.056(14) 0.057(16) -0.012(16) -0.01(2) F2' 0.052(16) 0.39(8) 0.14(3) 0.08(4) -0.017(16) -0.10(3) F3' 0.47(11) 0.49(12) 0.18(5) -0.24(7) -0.07(6) 0.33(9) F4' 0.050(14) 0.23(4) 0.11(2) -0.02(3) -0.017(13) -0.008(18) F5' 0.41(8) 0.04(2) 0.23(5) -0.08(3) -0.11(5) 0.09(3) F6' 0.044(11) 0.087(17) 0.073(16) 0.019(12) 0.000(10) 0.068(13) _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 C6 2.086(9) . ? Rh1 C5 2.105(9) . ? Rh1 C4 2.110(9) . ? Rh1 C7 2.117(8) . ? Rh1 N3 2.153(7) . ? Rh1 N1 2.178(7) . ? Rh1 N5 2.199(8) . ? N1 C14 1.321(11) . ? N1 N2 1.371(9) . ? N6 C22 1.350(12) . ? N6 N5 1.373(10) . ? N6 C8 1.438(11) . ? N2 C12 1.369(11) . ? N2 C8 1.407(11) . ? C12 C13 1.348(12) . ? C12 C11 1.493(12) . ? N4 N3 1.368(9) . ? N4 C17 1.371(11) . ? N4 C8 1.449(11) . ? N5 C24 1.340(11) . ? N3 C19 1.317(11) . ? C15 C14 1.501(12) . ? C18 C17 1.334(13) . ? C18 C19 1.388(12) . ? C17 C16 1.495(13) . ? C19 C20 1.512(13) . ? C14 C13 1.394(12) . ? P1 F3' 1.523(17) . ? P1 F2' 1.530(15) . ? P1 F2 1.532(10) . ? P1 F6 1.534(14) . ? P1 F5' 1.536(16) . ? P1 F4' 1.536(14) . ? P1 F1 1.544(10) . ? P1 F3 1.553(10) . ? P1 F6' 1.558(12) . ? P1 F1' 1.568(14) . ? P1 F5 1.570(11) . ? P1 F4 1.601(9) . ? C7 C6 1.425(13) . ? C7 C1 1.473(12) . ? C24 C23 1.394(14) . ? C24 C25 1.492(13) . ? C1 O1 1.229(11) . ? C1 C2 1.443(14) . ? C5 C6 1.385(14) . ? C5 C4 1.434(14) . ? C4 C3 1.466(14) . ? C23 C22 1.365(14) . ? C22 C21 1.509(15) . ? C3 C2 1.341(14) . ? F4 F6 1.73(5) . ? F4' F6' 1.59(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Rh1 C5 38.6(4) . . ? C6 Rh1 C4 70.0(4) . . ? C5 Rh1 C4 39.8(4) . . ? C6 Rh1 C7 39.6(4) . . ? C5 Rh1 C7 70.8(4) . . ? C4 Rh1 C7 82.2(4) . . ? C6 Rh1 N3 128.8(3) . . ? C5 Rh1 N3 100.2(3) . . ? C4 Rh1 N3 95.8(3) . . ? C7 Rh1 N3 168.2(3) . . ? C6 Rh1 N1 146.9(3) . . ? C5 Rh1 N1 147.8(3) . . ? C4 Rh1 N1 108.3(3) . . ? C7 Rh1 N1 107.5(3) . . ? N3 Rh1 N1 84.2(3) . . ? C6 Rh1 N5 101.6(3) . . ? C5 Rh1 N5 127.8(3) . . ? C4 Rh1 N5 166.8(3) . . ? C7 Rh1 N5 97.8(3) . . ? N3 Rh1 N5 81.5(3) . . ? N1 Rh1 N5 84.4(3) . . ? C14 N1 N2 106.3(7) . . ? C14 N1 Rh1 137.8(6) . . ? N2 N1 Rh1 115.5(5) . . ? C22 N6 N5 112.5(7) . . ? C22 N6 C8 128.1(8) . . ? N5 N6 C8 119.1(7) . . ? C12 N2 N1 110.4(7) . . ? C12 N2 C8 128.0(7) . . ? N1 N2 C8 120.8(7) . . ? C13 C12 N2 105.8(7) . . ? C13 C12 C11 132.0(9) . . ? N2 C12 C11 122.2(8) . . ? N3 N4 C17 111.5(7) . . ? N3 N4 C8 119.2(7) . . ? C17 N4 C8 127.2(7) . . ? C24 N5 N6 104.2(7) . . ? C24 N5 Rh1 136.3(7) . . ? N6 N5 Rh1 116.4(5) . . ? C19 N3 N4 104.7(7) . . ? C19 N3 Rh1 138.5(6) . . ? N4 N3 Rh1 116.8(5) . . ? C17 C18 C19 108.1(8) . . ? C18 C17 N4 105.3(8) . . ? C18 C17 C16 132.8(9) . . ? N4 C17 C16 121.8(8) . . ? N3 C19 C18 110.5(8) . . ? N3 C19 C20 124.3(8) . . ? C18 C19 C20 125.2(8) . . ? N1 C14 C13 109.3(8) . . ? N1 C14 C15 123.3(8) . . ? C13 C14 C15 127.4(9) . . ? N2 C8 N6 112.0(7) . . ? N2 C8 N4 111.9(7) . . ? N6 C8 N4 110.3(7) . . ? C12 C13 C14 108.2(8) . . ? F3' P1 F2' 89(3) . . ? F3' P1 F2 119(3) . . ? F2' P1 F2 124.4(15) . . ? F3' P1 F6 89(3) . . ? F2' P1 F6 118(2) . . ? F2 P1 F6 109(2) . . ? F3' P1 F5' 176(4) . . ? F2' P1 F5' 92(3) . . ? F2 P1 F5' 64(3) . . ? F6 P1 F5' 86(2) . . ? F3' P1 F4' 86(3) . . ? F2' P1 F4' 167(2) . . ? F2 P1 F4' 49.1(11) . . ? F6 P1 F4' 74(2) . . ? F5' P1 F4' 94(3) . . ? F3' P1 F1 78(3) . . ? F2' P1 F1 43.7(15) . . ? F2 P1 F1 93.3(10) . . ? F6 P1 F1 157(2) . . ? F5' P1 F1 106(2) . . ? F4' P1 F1 123.2(16) . . ? F3' P1 F3 25(3) . . ? F2' P1 F3 111(2) . . ? F2 P1 F3 95.4(9) . . ? F6 P1 F3 89.0(13) . . ? F5' P1 F3 156(3) . . ? F4' P1 F3 61.8(13) . . ? F1 P1 F3 87.4(10) . . ? F3' P1 F6' 105(3) . . ? F2' P1 F6' 131(2) . . ? F2 P1 F6' 88.9(10) . . ? F6 P1 F6' 21(2) . . ? F5' P1 F6' 71(2) . . ? F4' P1 F6' 62.0(16) . . ? F1 P1 F6' 174.2(14) . . ? F3 P1 F6' 97.7(13) . . ? F3' P1 F1' 99(3) . . ? F2' P1 F1' 83.6(17) . . ? F2 P1 F1' 47.4(14) . . ? F6 P1 F1' 156(3) . . ? F5' P1 F1' 85(2) . . ? F4' P1 F1' 85.0(18) . . ? F1 P1 F1' 46.0(12) . . ? F3 P1 F1' 90.0(13) . . ? F6' P1 F1' 136.2(18) . . ? F3' P1 F5 149(3) . . ? F2' P1 F5 64(2) . . ? F2 P1 F5 91.0(9) . . ? F6 P1 F5 89.3(12) . . ? F5' P1 F5 30(3) . . ? F4' P1 F5 123.5(15) . . ? F1 P1 F5 91.9(10) . . ? F3 P1 F5 173.6(9) . . ? F6' P1 F5 82.8(13) . . ? F1' P1 F5 94.0(12) . . ? F3' P1 F4 65(3) . . ? F2' P1 F4 57.5(13) . . ? F2 P1 F4 175.0(8) . . ? F6 P1 F4 67(2) . . ? F5' P1 F4 112(3) . . ? F4' P1 F4 130.1(13) . . ? F1 P1 F4 90.7(11) . . ? F3 P1 F4 87.7(7) . . ? F6' P1 F4 86.8(9) . . ? F1' P1 F4 136.7(17) . . ? F5 P1 F4 85.9(7) . . ? C6 C7 C1 124.6(9) . . ? C6 C7 Rh1 69.0(5) . . ? C1 C7 Rh1 120.3(6) . . ? N5 C24 C23 110.5(9) . . ? N5 C24 C25 123.4(9) . . ? C23 C24 C25 126.1(9) . . ? O1 C1 C2 120.1(9) . . ? O1 C1 C7 119.6(9) . . ? C2 C1 C7 120.3(9) . . ? C6 C5 C4 117.3(9) . . ? C6 C5 Rh1 70.0(5) . . ? C4 C5 Rh1 70.3(5) . . ? C5 C4 C3 119.2(9) . . ? C5 C4 Rh1 69.9(5) . . ? C3 C4 Rh1 120.1(7) . . ? C22 C23 C24 107.1(9) . . ? N6 C22 C23 105.8(9) . . ? N6 C22 C21 123.5(9) . . ? C23 C22 C21 130.7(10) . . ? C5 C6 C7 121.0(9) . . ? C5 C6 Rh1 71.4(5) . . ? C7 C6 Rh1 71.3(5) . . ? C2 C3 C4 127.6(10) . . ? C3 C2 C1 123.6(10) . . ? P1 F4 F6 54.8(9) . . ? P1 F6 F4 58.5(13) . . ? P1 F4' F6' 59.7(10) . . ? P1 F6' F4' 58.3(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.714 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.125