Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Hughes, Russell P.' ; Department of Chemistry 6128 Burke Laboratory Hanover, New Hampshire 03755-3564 USA ; 'Bowden, Allen A.' ; Department of Chemistry 6128 Burke Laboratory Hanover, New Hampshire 03755-3564 USA ; 'Lindner, Danielle C.' ; Department of Chemistry 6128 Burke Laboratory Hanover, New Hampshire 03755-3564 USA ; 'Liable-Sands, Louise M.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Rheingold, Arnold L.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Incarvito, Christopher ' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; _publ_contact_author_name 'Prof Russell P Hughes' _publ_contact_author_address ; Department of Chemistry Dartmouth College 6128 Burke Laboratory Hanover NH 03755-3564 UNITED STATES OF AMERICA ; _publ_contact_author_phone '+603 646 2763' _publ_contact_author_fax '+603 646 3946' _publ_contact_author_email rph@dartmouth.edu _publ_requested_journal 'J Chem Soc Dalton Trans' _publ_section_title ; Synthesis and Stuctural Studies of Perfluoroalkyl-Rhodium and Iridium (III) Compounds Containing Tris(pyrazolyl)borate Ligands ; data_rph31a _database_code_CSD 186264 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H10 B F7 I Ir N6 O' _chemical_formula_weight 777.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.276(2) _cell_length_b 20.276(2) _cell_length_c 11.6460(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.580(10) _cell_angle_gamma 90.00 _cell_volume 2188.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 7.595 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min 0.1707 _exptl_absorpt_correction_T_max 0.5172 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(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 P4' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1% _diffrn_reflns_number 3289 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 21.49 _reflns_number_total 2508 _reflns_number_gt 1946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0300P)^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 2508 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.209 _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 Ir Ir 0.32601(6) 0.61384(3) 0.72931(5) 0.0485(2) Uani 1 1 d . . . I I 0.15077(11) 0.63330(5) 0.90204(8) 0.0659(3) Uani 1 1 d . . . F11 F 0.3943(10) 0.7349(4) 0.6237(7) 0.076(2) Uani 1 1 d . . . F12 F 0.2248(10) 0.6839(4) 0.5283(7) 0.078(3) Uani 1 1 d . . . F31 F 0.3293(11) 0.8254(4) 0.7575(8) 0.086(3) Uani 1 1 d . . . F41 F 0.1279(15) 0.9058(5) 0.8236(9) 0.125(4) Uani 1 1 d . . . F51 F -0.1538(15) 0.8750(7) 0.7937(10) 0.159(6) Uani 1 1 d . . . F61 F -0.2306(12) 0.7605(8) 0.6845(9) 0.140(5) Uani 1 1 d . . . F71 F -0.0299(10) 0.6774(5) 0.6153(9) 0.099(3) Uani 1 1 d . . . O21 O 0.0885(12) 0.5402(6) 0.6062(10) 0.080(3) Uani 1 1 d . . . B B 0.6518(19) 0.5686(8) 0.7638(15) 0.064(5) Uani 1 1 d . . . H10A H 0.7538 0.5545 0.7737 0.077 Uiso 1 1 calc R . . N5 N 0.4728(13) 0.5936(5) 0.5998(11) 0.058(3) Uani 1 1 d . . . N6 N 0.6097(13) 0.5778(5) 0.6372(10) 0.056(3) Uani 1 1 d . . . N1 N 0.4083(13) 0.5276(5) 0.8139(9) 0.058(3) Uani 1 1 d . . . N2 N 0.5520(13) 0.5177(5) 0.8158(10) 0.056(3) Uani 1 1 d . . . N3 N 0.4919(12) 0.6609(5) 0.8225(9) 0.053(3) Uani 1 1 d . . . N4 N 0.6283(13) 0.6337(6) 0.8258(10) 0.067(3) Uani 1 1 d . . . C21 C 0.1744(18) 0.5673(8) 0.6499(13) 0.062(4) Uani 1 1 d . . . C1 C 0.2667(16) 0.7025(7) 0.6382(11) 0.055(4) Uani 1 1 d . . . C3 C 0.1893(19) 0.8059(8) 0.7382(14) 0.074(5) Uani 1 1 d . . . C4 C 0.091(2) 0.8480(9) 0.7717(15) 0.082(5) Uani 1 1 d . . . C5 C -0.050(3) 0.8365(13) 0.7608(17) 0.105(8) Uani 1 1 d . . . C6 C -0.092(2) 0.7795(15) 0.7050(17) 0.104(7) Uani 1 1 d . . . C7 C 0.013(2) 0.7354(9) 0.6698(15) 0.078(5) Uani 1 1 d . . . C2 C 0.1589(17) 0.7460(7) 0.6799(13) 0.062(4) Uani 1 1 d . . . C17 C 0.6865(17) 0.5679(7) 0.5441(14) 0.064(4) Uani 1 1 d . . . H17A H 0.7848 0.5565 0.5442 0.076 Uiso 1 1 calc R . . C18 C 0.5978(18) 0.5771(7) 0.4495(14) 0.066(4) Uani 1 1 d . . . H18A H 0.6233 0.5731 0.3726 0.079 Uiso 1 1 calc R . . C19 C 0.4592(18) 0.5940(6) 0.4882(12) 0.056(4) Uani 1 1 d . . . H19A H 0.3755 0.6035 0.4427 0.067 Uiso 1 1 calc R . . C11 C 0.582(2) 0.4580(7) 0.8664(12) 0.069(4) Uani 1 1 d . . . H11A H 0.6750 0.4398 0.8788 0.083 Uiso 1 1 calc R . . C12 C 0.456(2) 0.4293(8) 0.8960(13) 0.079(5) Uani 1 1 d . . . H12A H 0.4442 0.3879 0.9307 0.094 Uiso 1 1 calc R . . C13 C 0.3484(18) 0.4741(7) 0.8641(12) 0.067(4) Uani 1 1 d . . . H13A H 0.2495 0.4684 0.8753 0.081 Uiso 1 1 calc R . . C14 C 0.7173(17) 0.6757(8) 0.8906(13) 0.072(5) Uani 1 1 d . . . H14A H 0.8173 0.6702 0.9041 0.086 Uiso 1 1 calc R . . C15 C 0.6391(19) 0.7249(7) 0.9309(13) 0.068(4) Uani 1 1 d . . . H15A H 0.6727 0.7591 0.9796 0.082 Uiso 1 1 calc R . . C16 C 0.4968(17) 0.7161(6) 0.8868(11) 0.057(4) Uani 1 1 d . . . H16A H 0.4184 0.7440 0.9000 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.0624(4) 0.0414(3) 0.0420(4) 0.0004(3) 0.0049(2) 0.0027(3) I 0.0725(6) 0.0712(7) 0.0547(7) 0.0049(5) 0.0121(5) 0.0094(5) F11 0.096(6) 0.050(5) 0.082(6) 0.014(4) 0.030(5) -0.001(5) F12 0.124(7) 0.065(6) 0.045(6) 0.010(4) -0.007(5) 0.023(5) F31 0.110(8) 0.056(5) 0.092(7) 0.002(5) -0.005(6) 0.002(5) F41 0.206(12) 0.065(7) 0.103(8) -0.019(6) -0.005(8) 0.050(8) F51 0.187(12) 0.185(13) 0.107(9) 0.019(8) 0.030(9) 0.130(11) F61 0.084(8) 0.237(15) 0.101(9) 0.046(9) 0.000(6) 0.041(9) F71 0.087(6) 0.102(8) 0.106(8) 0.005(6) -0.016(6) -0.014(6) O21 0.070(7) 0.085(8) 0.083(9) -0.012(7) -0.011(6) -0.011(6) B 0.067(11) 0.053(11) 0.073(14) 0.000(10) 0.019(10) 0.016(9) N5 0.078(8) 0.027(6) 0.068(10) -0.010(6) -0.015(7) 0.003(6) N6 0.071(8) 0.054(7) 0.043(8) 0.003(6) 0.002(7) 0.014(6) N1 0.083(9) 0.051(8) 0.040(7) -0.005(6) 0.001(6) 0.007(7) N2 0.075(8) 0.040(7) 0.054(8) -0.001(6) 0.004(6) 0.005(6) N3 0.065(8) 0.050(7) 0.044(7) 0.008(6) 0.013(6) -0.002(6) N4 0.071(8) 0.069(9) 0.063(9) 0.007(7) 0.010(7) 0.011(7) C21 0.079(11) 0.068(11) 0.038(10) 0.019(8) -0.011(8) 0.021(9) C1 0.075(10) 0.068(10) 0.022(8) -0.007(7) 0.007(7) 0.002(9) C3 0.078(11) 0.064(11) 0.081(13) 0.023(9) 0.021(10) 0.036(10) C4 0.109(15) 0.073(14) 0.064(13) 0.008(10) -0.014(11) 0.019(13) C5 0.16(2) 0.107(18) 0.055(13) 0.014(12) 0.032(14) 0.065(19) C6 0.074(15) 0.17(2) 0.064(14) 0.038(15) 0.001(11) 0.039(16) C7 0.095(14) 0.068(12) 0.069(12) 0.037(10) -0.005(10) -0.002(11) C2 0.084(12) 0.039(9) 0.062(11) 0.005(8) 0.001(9) -0.003(8) C17 0.071(10) 0.057(10) 0.065(11) -0.017(8) 0.019(10) 0.000(8) C18 0.097(12) 0.047(9) 0.056(11) -0.013(8) 0.032(10) -0.017(9) C19 0.107(13) 0.044(9) 0.017(8) -0.006(6) -0.002(8) -0.017(8) C11 0.111(14) 0.044(10) 0.050(10) -0.006(8) -0.012(10) 0.015(10) C12 0.129(15) 0.045(10) 0.062(11) -0.007(8) 0.001(11) -0.003(11) C13 0.091(11) 0.052(10) 0.059(10) 0.006(8) 0.010(9) -0.011(9) C14 0.067(10) 0.080(12) 0.066(11) -0.022(9) -0.018(8) -0.014(10) C15 0.104(13) 0.037(9) 0.064(11) -0.012(8) 0.003(10) -0.003(9) C16 0.087(11) 0.025(8) 0.058(10) -0.014(7) 0.003(8) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir C21 1.899(19) . ? Ir N3 2.075(11) . ? Ir N5 2.116(12) . ? Ir N1 2.133(11) . ? Ir C1 2.147(14) . ? Ir I 2.6719(11) . ? F11 C1 1.370(15) . ? F12 C1 1.373(15) . ? F31 C3 1.366(19) . ? F41 C4 1.36(2) . ? F51 C5 1.31(2) . ? F61 C6 1.35(2) . ? F71 C7 1.385(19) . ? O21 C21 1.077(17) . ? B N6 1.52(2) . ? B N4 1.52(2) . ? B N2 1.530(19) . ? N5 C19 1.301(15) . ? N5 N6 1.362(15) . ? N6 C17 1.340(17) . ? N1 N2 1.347(15) . ? N1 C13 1.362(17) . ? N2 C11 1.370(17) . ? N3 C16 1.347(16) . ? N3 N4 1.379(15) . ? N4 C14 1.386(18) . ? C1 C2 1.434(19) . ? C3 C4 1.32(2) . ? C3 C2 1.41(2) . ? C4 C5 1.33(3) . ? C5 C6 1.37(3) . ? C6 C7 1.40(3) . ? C7 C2 1.37(2) . ? C17 C18 1.36(2) . ? C18 C19 1.424(19) . ? C11 C12 1.37(2) . ? C12 C13 1.39(2) . ? C14 C15 1.332(19) . ? C15 C16 1.406(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 C21 Ir N3 177.0(5) . . ? C21 Ir N5 92.4(6) . . ? N3 Ir N5 88.6(4) . . ? C21 Ir N1 93.4(5) . . ? N3 Ir N1 83.9(4) . . ? N5 Ir N1 86.7(4) . . ? C21 Ir C1 90.4(6) . . ? N3 Ir C1 92.4(5) . . ? N5 Ir C1 88.2(5) . . ? N1 Ir C1 173.7(5) . . ? C21 Ir I 88.7(5) . . ? N3 Ir I 90.0(3) . . ? N5 Ir I 176.0(3) . . ? N1 Ir I 89.5(3) . . ? C1 Ir I 95.6(4) . . ? N6 B N4 108.5(12) . . ? N6 B N2 109.5(13) . . ? N4 B N2 107.1(12) . . ? C19 N5 N6 111.5(12) . . ? C19 N5 Ir 132.4(11) . . ? N6 N5 Ir 116.0(9) . . ? C17 N6 N5 107.4(12) . . ? C17 N6 B 130.1(13) . . ? N5 N6 B 122.3(12) . . ? N2 N1 C13 107.3(12) . . ? N2 N1 Ir 117.6(9) . . ? C13 N1 Ir 135.0(11) . . ? N1 N2 C11 108.8(12) . . ? N1 N2 B 120.6(12) . . ? C11 N2 B 130.6(14) . . ? C16 N3 N4 108.0(11) . . ? C16 N3 Ir 132.7(10) . . ? N4 N3 Ir 119.3(9) . . ? N3 N4 C14 107.1(12) . . ? N3 N4 B 118.9(12) . . ? C14 N4 B 134.1(13) . . ? O21 C21 Ir 178.8(15) . . ? F11 C1 F12 103.1(10) . . ? F11 C1 C2 111.5(12) . . ? F12 C1 C2 108.2(12) . . ? F11 C1 Ir 105.0(9) . . ? F12 C1 Ir 106.7(8) . . ? C2 C1 Ir 120.9(10) . . ? C4 C3 F31 115.3(18) . . ? C4 C3 C2 124.9(18) . . ? F31 C3 C2 119.7(13) . . ? C3 C4 C5 123(2) . . ? C3 C4 F41 122(2) . . ? C5 C4 F41 115(2) . . ? F51 C5 C4 127(3) . . ? F51 C5 C6 116(3) . . ? C4 C5 C6 116.7(19) . . ? F61 C6 C5 125(2) . . ? F61 C6 C7 116(2) . . ? C5 C6 C7 119(2) . . ? C2 C7 F71 115.7(16) . . ? C2 C7 C6 124.9(19) . . ? F71 C7 C6 119.4(19) . . ? C7 C2 C3 110.6(16) . . ? C7 C2 C1 125.1(15) . . ? C3 C2 C1 124.3(15) . . ? N6 C17 C18 108.1(14) . . ? C17 C18 C19 107.4(13) . . ? N5 C19 C18 105.5(14) . . ? C12 C11 N2 108.8(14) . . ? C11 C12 C13 105.5(14) . . ? N1 C13 C12 109.5(15) . . ? C15 C14 N4 109.4(14) . . ? C14 C15 C16 107.1(13) . . ? N3 C16 C15 108.5(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.516 _refine_diff_density_min -1.315 _refine_diff_density_rms 0.176 #===END data_rph32a _database_code_CSD 186265 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 B F7 I N6 P Rh' _chemical_formula_weight 735.99 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' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.885(3) _cell_length_b 16.4380(10) _cell_length_c 15.970(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.84(2) _cell_angle_gamma 90.00 _cell_volume 2556.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 2.010 _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 298(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 P4' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2% _diffrn_reflns_number 4351 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3339 _reflns_number_gt 2574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0200P)^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 SHELXL _refine_ls_extinction_coef 0.00200(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3339 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0545 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 Rh Rh 0.18052(4) 0.54178(2) 0.79408(2) 0.03074(13) Uani 1 1 d . . . I I 0.37191(4) 0.65149(2) 0.78095(2) 0.05610(15) Uani 1 1 d . . . P P 0.03479(15) 0.63394(8) 0.84075(9) 0.0449(4) Uani 1 1 d . . . F12 F 0.0740(3) 0.64490(18) 0.65223(18) 0.0695(10) Uani 1 1 d . . . F11 F -0.0408(3) 0.5336(2) 0.65243(17) 0.0640(9) Uani 1 1 d . . . F31 F 0.0871(4) 0.3968(2) 0.6307(2) 0.0820(11) Uani 1 1 d . . . F41 F 0.2051(5) 0.3281(3) 0.5128(3) 0.142(2) Uani 1 1 d . . . F51 F 0.3522(5) 0.4188(4) 0.4164(3) 0.158(2) Uani 1 1 d . . . F61 F 0.3705(5) 0.5811(4) 0.4412(3) 0.157(2) Uani 1 1 d . . . F71 F 0.2504(4) 0.6528(3) 0.5560(2) 0.1053(14) Uani 1 1 d . . . B B 0.2491(6) 0.3719(3) 0.8865(4) 0.0428(16) Uani 1 1 d . . . H10D H 0.2679 0.3189 0.9141 0.051 Uiso 1 1 calc R . . N1 N 0.2749(4) 0.5188(2) 0.9246(2) 0.0346(10) Uani 1 1 d . . . N2 N 0.2929(4) 0.4401(2) 0.9498(2) 0.0357(10) Uani 1 1 d . . . N3 N 0.3230(4) 0.4515(2) 0.7670(2) 0.0353(10) Uani 1 1 d . . . N4 N 0.3301(4) 0.3806(2) 0.8118(2) 0.0363(10) Uani 1 1 d . . . N5 N 0.0445(4) 0.4480(2) 0.8087(2) 0.0365(10) Uani 1 1 d . . . N6 N 0.0954(4) 0.3806(2) 0.8521(2) 0.0371(10) Uani 1 1 d . . . C1 C 0.0934(5) 0.5628(3) 0.6691(3) 0.0452(14) Uani 1 1 d . . . C3 C 0.1536(6) 0.4449(4) 0.5837(4) 0.0606(17) Uani 1 1 d . . . C4 C 0.2170(8) 0.4092(5) 0.5232(5) 0.086(2) Uani 1 1 d . . . C5 C 0.2908(9) 0.4562(9) 0.4757(5) 0.109(4) Uani 1 1 d . . . C6 C 0.2996(8) 0.5355(7) 0.4885(5) 0.099(3) Uani 1 1 d . . . C7 C 0.2359(7) 0.5730(5) 0.5498(4) 0.0704(19) Uani 1 1 d . . . C2 C 0.1624(5) 0.5274(4) 0.5996(3) 0.0483(14) Uani 1 1 d . . . C21 C -0.1293(6) 0.6616(4) 0.7752(3) 0.0725(19) Uani 1 1 d . . . H21A H -0.1774 0.6132 0.7538 0.109 Uiso 1 1 calc R . . H21B H -0.1128 0.6947 0.7284 0.109 Uiso 1 1 calc R . . H21C H -0.1839 0.6915 0.8089 0.109 Uiso 1 1 calc R . . C22 C 0.1034(6) 0.7327(3) 0.8739(4) 0.0728(19) Uani 1 1 d . . . H22A H 0.1372 0.7585 0.8277 0.109 Uiso 1 1 calc R . . H22B H 0.1771 0.7266 0.9212 0.109 Uiso 1 1 calc R . . H22C H 0.0324 0.7657 0.8907 0.109 Uiso 1 1 calc R . . C23 C -0.0217(5) 0.5967(3) 0.9358(3) 0.0576(16) Uani 1 1 d . . . H23A H -0.0618 0.5438 0.9251 0.086 Uiso 1 1 calc R . . H23B H -0.0888 0.6334 0.9516 0.086 Uiso 1 1 calc R . . H23C H 0.0554 0.5934 0.9812 0.086 Uiso 1 1 calc R . . C11 C 0.3521(5) 0.4384(4) 1.0312(3) 0.0485(15) Uani 1 1 d . . . H11A H 0.3763 0.3915 1.0628 0.058 Uiso 1 1 calc R . . C12 C 0.3712(5) 0.5145(4) 1.0605(3) 0.0524(16) Uani 1 1 d . . . H12A H 0.4084 0.5309 1.1154 0.063 Uiso 1 1 calc R . . C13 C 0.3236(5) 0.5632(3) 0.9917(3) 0.0437(14) Uani 1 1 d . . . H13A H 0.3256 0.6198 0.9924 0.052 Uiso 1 1 calc R . . C14 C 0.4243(5) 0.3316(3) 0.7870(3) 0.0491(15) Uani 1 1 d . . . H14A H 0.4477 0.2797 0.8076 0.059 Uiso 1 1 calc R . . C15 C 0.4799(5) 0.3715(3) 0.7260(3) 0.0519(15) Uani 1 1 d . . . H15A H 0.5474 0.3522 0.6970 0.062 Uiso 1 1 calc R . . C16 C 0.4157(5) 0.4459(3) 0.7160(3) 0.0379(12) Uani 1 1 d . . . H16A H 0.4343 0.4864 0.6789 0.045 Uiso 1 1 calc R . . C17 C -0.0070(6) 0.3297(3) 0.8587(3) 0.0506(15) Uani 1 1 d . . . H17A H 0.0025 0.2793 0.8857 0.061 Uiso 1 1 calc R . . C18 C -0.1275(6) 0.3627(4) 0.8201(4) 0.0600(17) Uani 1 1 d . . . H18A H -0.2150 0.3403 0.8153 0.072 Uiso 1 1 calc R . . C19 C -0.0921(5) 0.4358(3) 0.7899(3) 0.0504(15) Uani 1 1 d . . . H19A H -0.1541 0.4725 0.7602 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.0322(2) 0.0280(2) 0.0326(2) 0.00086(19) 0.00698(17) 0.0008(2) I 0.0614(3) 0.0434(2) 0.0663(3) 0.0060(2) 0.0187(2) -0.0137(2) P 0.0492(9) 0.0412(8) 0.0466(8) 0.0042(7) 0.0143(7) 0.0134(7) F12 0.096(3) 0.054(2) 0.058(2) 0.0164(17) 0.0110(19) 0.027(2) F11 0.0438(19) 0.098(3) 0.0472(18) 0.0054(18) -0.0022(15) 0.012(2) F31 0.092(3) 0.063(2) 0.091(3) -0.023(2) 0.016(2) -0.018(2) F41 0.152(5) 0.144(4) 0.121(4) -0.087(3) -0.002(3) 0.031(4) F51 0.110(4) 0.288(7) 0.079(3) -0.075(4) 0.027(3) 0.040(4) F61 0.121(4) 0.288(7) 0.076(3) 0.053(4) 0.059(3) 0.003(4) F71 0.131(4) 0.105(3) 0.084(3) 0.044(3) 0.033(3) -0.008(3) B 0.055(4) 0.033(3) 0.043(4) 0.015(3) 0.015(3) 0.006(3) N1 0.026(2) 0.043(3) 0.034(2) -0.001(2) 0.004(2) -0.002(2) N2 0.034(2) 0.041(3) 0.033(2) 0.011(2) 0.009(2) 0.001(2) N3 0.039(2) 0.034(2) 0.034(2) -0.003(2) 0.011(2) -0.002(2) N4 0.040(3) 0.030(2) 0.041(2) 0.003(2) 0.013(2) 0.006(2) N5 0.030(2) 0.040(3) 0.039(2) -0.005(2) 0.005(2) -0.001(2) N6 0.041(3) 0.032(2) 0.040(2) -0.004(2) 0.012(2) -0.007(2) C1 0.045(4) 0.044(3) 0.047(3) 0.004(3) 0.011(3) 0.008(3) C3 0.054(4) 0.077(5) 0.047(4) -0.014(4) -0.001(3) 0.004(4) C4 0.068(5) 0.111(7) 0.068(5) -0.048(5) -0.018(4) 0.018(5) C5 0.068(6) 0.216(12) 0.043(5) -0.030(7) 0.007(4) 0.030(8) C6 0.073(5) 0.184(10) 0.040(5) 0.010(6) 0.010(4) 0.019(7) C7 0.066(5) 0.099(6) 0.046(4) 0.019(4) 0.009(4) 0.009(4) C2 0.042(3) 0.068(4) 0.032(3) 0.001(3) -0.002(3) 0.004(3) C21 0.068(4) 0.084(5) 0.065(4) 0.017(4) 0.011(3) 0.043(4) C22 0.101(5) 0.036(3) 0.087(5) -0.005(3) 0.034(4) 0.010(4) C23 0.057(4) 0.069(4) 0.053(3) 0.004(3) 0.027(3) 0.016(3) C11 0.033(3) 0.078(5) 0.034(3) 0.017(3) 0.007(3) 0.007(3) C12 0.035(3) 0.093(5) 0.029(3) -0.004(3) 0.005(3) -0.006(3) C13 0.035(3) 0.050(3) 0.046(3) -0.012(3) 0.007(3) -0.004(3) C14 0.059(4) 0.036(3) 0.055(4) -0.001(3) 0.015(3) 0.017(3) C15 0.043(3) 0.064(4) 0.054(4) -0.008(3) 0.021(3) 0.017(3) C16 0.039(3) 0.051(3) 0.027(3) 0.003(3) 0.011(2) 0.005(3) C17 0.068(4) 0.034(3) 0.055(4) -0.013(3) 0.026(4) -0.023(3) C18 0.056(4) 0.061(4) 0.066(4) -0.024(3) 0.019(4) -0.029(4) C19 0.032(3) 0.060(4) 0.059(4) -0.014(3) 0.006(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C1 2.063(5) . ? Rh N5 2.084(4) . ? Rh N3 2.140(4) . ? Rh N1 2.166(4) . ? Rh P 2.3006(14) . ? Rh I 2.6478(7) . ? P C22 1.804(5) . ? P C23 1.812(5) . ? P C21 1.832(5) . ? F12 C1 1.383(5) . ? F11 C1 1.393(6) . ? F31 C3 1.338(6) . ? F41 C4 1.347(8) . ? F51 C5 1.356(8) . ? F61 C6 1.343(9) . ? F71 C7 1.322(7) . ? B N2 1.522(7) . ? B N6 1.531(7) . ? B N4 1.552(6) . ? N1 C13 1.317(5) . ? N1 N2 1.358(5) . ? N2 C11 1.331(6) . ? N3 C16 1.330(5) . ? N3 N4 1.363(5) . ? N4 C14 1.341(5) . ? N5 C19 1.347(6) . ? N5 N6 1.358(5) . ? N6 C17 1.333(6) . ? C1 C2 1.516(7) . ? C3 C4 1.370(8) . ? C3 C2 1.379(7) . ? C4 C5 1.376(11) . ? C5 C6 1.321(12) . ? C6 C7 1.394(10) . ? C7 C2 1.386(8) . ? C11 C12 1.338(7) . ? C12 C13 1.376(7) . ? C14 C15 1.365(6) . ? C15 C16 1.375(6) . ? C17 C18 1.358(7) . ? C18 C19 1.363(7) . ? 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 Rh N5 93.52(18) . . ? C1 Rh N3 95.80(17) . . ? N5 Rh N3 88.24(14) . . ? C1 Rh N1 179.05(17) . . ? N5 Rh N1 86.77(15) . . ? N3 Rh N1 83.30(14) . . ? C1 Rh P 91.27(14) . . ? N5 Rh P 89.94(11) . . ? N3 Rh P 172.79(10) . . ? N1 Rh P 89.63(10) . . ? C1 Rh I 89.71(15) . . ? N5 Rh I 174.72(11) . . ? N3 Rh I 87.28(10) . . ? N1 Rh I 89.93(10) . . ? P Rh I 94.16(4) . . ? C22 P C23 102.2(3) . . ? C22 P C21 101.3(3) . . ? C23 P C21 101.1(3) . . ? C22 P Rh 117.6(2) . . ? C23 P Rh 110.44(17) . . ? C21 P Rh 121.39(19) . . ? N2 B N6 108.8(4) . . ? N2 B N4 108.4(4) . . ? N6 B N4 109.0(4) . . ? C13 N1 N2 106.0(4) . . ? C13 N1 Rh 136.3(4) . . ? N2 N1 Rh 117.7(3) . . ? C11 N2 N1 108.8(4) . . ? C11 N2 B 131.4(5) . . ? N1 N2 B 119.8(4) . . ? C16 N3 N4 106.5(4) . . ? C16 N3 Rh 135.9(3) . . ? N4 N3 Rh 117.6(3) . . ? C14 N4 N3 109.5(4) . . ? C14 N4 B 130.4(4) . . ? N3 N4 B 119.7(4) . . ? C19 N5 N6 105.2(4) . . ? C19 N5 Rh 136.6(4) . . ? N6 N5 Rh 118.1(3) . . ? C17 N6 N5 109.5(4) . . ? C17 N6 B 129.3(5) . . ? N5 N6 B 121.2(4) . . ? F12 C1 F11 101.7(4) . . ? F12 C1 C2 107.3(4) . . ? F11 C1 C2 105.1(4) . . ? F12 C1 Rh 111.9(3) . . ? F11 C1 Rh 110.7(3) . . ? C2 C1 Rh 118.6(3) . . ? F31 C3 C4 118.1(7) . . ? F31 C3 C2 119.9(5) . . ? C4 C3 C2 121.9(7) . . ? F41 C4 C3 118.0(8) . . ? F41 C4 C5 122.1(9) . . ? C3 C4 C5 119.9(8) . . ? C6 C5 F51 122.1(11) . . ? C6 C5 C4 119.7(9) . . ? F51 C5 C4 118.2(11) . . ? C5 C6 F61 119.3(10) . . ? C5 C6 C7 121.3(9) . . ? F61 C6 C7 119.4(10) . . ? F71 C7 C2 123.7(6) . . ? F71 C7 C6 115.8(7) . . ? C2 C7 C6 120.5(7) . . ? C3 C2 C7 116.7(6) . . ? C3 C2 C1 119.4(5) . . ? C7 C2 C1 123.9(6) . . ? N2 C11 C12 109.5(5) . . ? C11 C12 C13 104.8(5) . . ? N1 C13 C12 110.8(5) . . ? N4 C14 C15 107.9(5) . . ? C14 C15 C16 106.0(4) . . ? N3 C16 C15 110.0(4) . . ? N6 C17 C18 109.4(5) . . ? C17 C18 C19 104.7(5) . . ? N5 C19 C18 111.2(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.387 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.069 #===END data_rph178a _database_code_CSD 186266 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H19 B F7 I N6 P Rh' _chemical_formula_weight 687.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4007(12) _cell_length_b 13.4025(15) _cell_length_c 16.4201(19) _cell_angle_alpha 87.188(2) _cell_angle_beta 76.796(2) _cell_angle_gamma 85.574(2) _cell_volume 2220.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(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 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 2.306 _exptl_absorpt_correction_type 'Empirical from SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 P4 '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_% 1% _diffrn_reflns_number 25831 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.33 _reflns_number_total 10328 _reflns_number_gt 7263 _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^)+(0.1000P)^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 10328 _refine_ls_number_parameters 585 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1056 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1591 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 0.26842(6) 0.34866(5) 0.20804(4) 0.01734(16) Uani 1 1 d . . . Rh1' Rh 0.77265(6) 0.84433(5) 0.27081(4) 0.01808(16) Uani 1 1 d . . . I1 I 0.26835(6) 0.53223(4) 0.14104(4) 0.02663(16) Uani 1 1 d . . . I1' I 0.81392(7) 1.02821(5) 0.30673(4) 0.03214(17) Uani 1 1 d . . . P1 P 0.2157(2) 0.29663(18) 0.08936(14) 0.0243(5) Uani 1 1 d . . . P1' P 0.8928(2) 0.77342(18) 0.36295(14) 0.0238(5) Uani 1 1 d . . . B1 B 0.4948(10) 0.2487(8) 0.2941(6) 0.021(2) Uani 1 1 d . . . H1 H 0.564(10) 0.211(7) 0.322(6) 0.03(3) Uiso 1 1 d . . . B1' B 0.4886(11) 0.7789(9) 0.2637(7) 0.029(2) Uani 1 1 d . . . H1' H 0.396(7) 0.750(5) 0.250(4) 0.001(18) Uiso 1 1 d . . . F11 F 0.0042(5) 0.2799(4) 0.2465(3) 0.0339(13) Uani 1 1 d . . . F12 F 0.0004(5) 0.4422(4) 0.2327(3) 0.0328(13) Uani 1 1 d . . . F21 F 0.0374(6) 0.4645(4) 0.3787(4) 0.0370(14) Uani 1 1 d . . . F22 F 0.1005(5) 0.3081(4) 0.3976(3) 0.0349(13) Uani 1 1 d . . . F31 F -0.1353(7) 0.2507(5) 0.3981(4) 0.0516(17) Uani 1 1 d . . . F32 F -0.2047(6) 0.3982(6) 0.3617(4) 0.0546(19) Uani 1 1 d . . . F33 F -0.1477(6) 0.3728(5) 0.4792(4) 0.0498(17) Uani 1 1 d . . . F12' F 0.9981(6) 0.7402(4) 0.1666(4) 0.0359(14) Uani 1 1 d . . . F11' F 0.8702(5) 0.8235(5) 0.0979(3) 0.0363(14) Uani 1 1 d . . . F22' F 0.9768(6) 0.9918(4) 0.1128(4) 0.0354(13) Uani 1 1 d . . . F21' F 1.0915(5) 0.9212(4) 0.1998(3) 0.0324(13) Uani 1 1 d . . . F31' F 1.2215(6) 0.9486(5) 0.0376(4) 0.0432(15) Uani 1 1 d . . . F32' F 1.2235(6) 0.7974(4) 0.0842(4) 0.0374(14) Uani 1 1 d . . . F33' F 1.1012(6) 0.8452(5) -0.0019(4) 0.0424(15) Uani 1 1 d . . . N1 N 0.4782(7) 0.3314(5) 0.1562(4) 0.0186(14) Uani 1 1 d . . . N2 N 0.5551(7) 0.2806(5) 0.2036(4) 0.0211(15) Uani 1 1 d . . . N3 N 0.3359(7) 0.4011(5) 0.3108(4) 0.0197(15) Uani 1 1 d . . . N4 N 0.4305(7) 0.3433(5) 0.3398(4) 0.0200(15) Uani 1 1 d . . . N5 N 0.2783(7) 0.2043(5) 0.2630(4) 0.0220(15) Uani 1 1 d . . . N6 N 0.3870(8) 0.1767(6) 0.2957(5) 0.0261(17) Uani 1 1 d . . . N5' N 0.7248(7) 0.7046(6) 0.2427(5) 0.0241(16) Uani 1 1 d . . . N6' N 0.5953(8) 0.6911(6) 0.2415(5) 0.0302(18) Uani 1 1 d . . . N1' N 0.5952(7) 0.8491(6) 0.3689(5) 0.0267(17) Uani 1 1 d . . . N2' N 0.4876(7) 0.8114(6) 0.3517(5) 0.0280(17) Uani 1 1 d . . . N3' N 0.6432(7) 0.9086(6) 0.1974(5) 0.0245(16) Uani 1 1 d . . . N4' N 0.5276(8) 0.8662(7) 0.2028(5) 0.0309(18) Uani 1 1 d . . . C11 C 0.6828(8) 0.2783(7) 0.1612(6) 0.027(2) Uani 1 1 d . . . H11 H 0.7552 0.2443 0.1794 0.032 Uiso 1 1 calc R . . C12 C 0.6907(9) 0.3320(7) 0.0893(6) 0.0250(19) Uani 1 1 d . . . H12 H 0.7685 0.3456 0.0483 0.030 Uiso 1 1 calc R . . C13 C 0.5604(9) 0.3635(7) 0.0875(5) 0.0233(18) Uani 1 1 d . . . H13 H 0.5343 0.4024 0.0433 0.028 Uiso 1 1 calc R . . C14 C 0.4690(9) 0.3923(8) 0.3983(6) 0.029(2) Uani 1 1 d . . . H14 H 0.5349 0.3681 0.4274 0.034 Uiso 1 1 calc R . . C15 C 0.3983(9) 0.4824(7) 0.4092(6) 0.028(2) Uani 1 1 d . . . H15 H 0.4039 0.5327 0.4469 0.034 Uiso 1 1 calc R . . C16 C 0.3166(9) 0.4846(7) 0.3536(5) 0.0242(19) Uani 1 1 d . . . H16 H 0.2548 0.5386 0.3468 0.029 Uiso 1 1 calc R . . C17 C 0.3756(10) 0.0858(7) 0.3313(6) 0.030(2) Uani 1 1 d . . . H17 H 0.4381 0.0501 0.3579 0.036 Uiso 1 1 calc R . . C18 C 0.2559(11) 0.0515(7) 0.3229(6) 0.036(2) Uani 1 1 d . . . H18 H 0.2216 -0.0113 0.3417 0.043 Uiso 1 1 calc R . . C19 C 0.1978(10) 0.1282(6) 0.2816(6) 0.027(2) Uani 1 1 d . . . H19 H 0.1138 0.1274 0.2682 0.032 Uiso 1 1 calc R . . C21 C 0.0700(10) 0.3577(8) 0.0596(6) 0.037(2) Uani 1 1 d . . . H21A H 0.0587 0.3288 0.0082 0.056 Uiso 1 1 calc R . . H21B H 0.0813 0.4295 0.0499 0.056 Uiso 1 1 calc R . . H21C H -0.0083 0.3475 0.1045 0.056 Uiso 1 1 calc R . . C22 C 0.1886(11) 0.1659(7) 0.0911(7) 0.038(3) Uani 1 1 d . . . H22A H 0.1666 0.1496 0.0385 0.058 Uiso 1 1 calc R . . H22B H 0.1153 0.1505 0.1381 0.058 Uiso 1 1 calc R . . H22C H 0.2691 0.1263 0.0975 0.058 Uiso 1 1 calc R . . C23 C 0.3393(10) 0.3086(8) -0.0068(6) 0.035(2) Uani 1 1 d . . . H23A H 0.3064 0.2843 -0.0530 0.053 Uiso 1 1 calc R . . H23B H 0.4205 0.2689 -0.0017 0.053 Uiso 1 1 calc R . . H23C H 0.3583 0.3791 -0.0178 0.053 Uiso 1 1 calc R . . C1 C 0.0699(8) 0.3629(7) 0.2622(6) 0.0242(19) Uani 1 1 d . . . C2 C 0.0236(9) 0.3692(7) 0.3578(5) 0.0247(19) Uani 1 1 d . . . C3 C -0.1197(10) 0.3467(8) 0.3995(7) 0.037(2) Uani 1 1 d . . . C17' C 0.5849(11) 0.5983(8) 0.2228(6) 0.034(2) Uani 1 1 d . . . H17' H 0.5053 0.5710 0.2183 0.041 Uiso 1 1 calc R . . C18' C 0.7045(12) 0.5476(7) 0.2111(6) 0.039(3) Uani 1 1 d . . . H18' H 0.7261 0.4795 0.1967 0.047 Uiso 1 1 calc R . . C19' C 0.7891(11) 0.6173(7) 0.2247(6) 0.035(2) Uani 1 1 d . . . H19' H 0.8811 0.6037 0.2215 0.042 Uiso 1 1 calc R . . C11' C 0.3886(10) 0.8169(8) 0.4198(7) 0.036(2) Uani 1 1 d . . . H11' H 0.3029 0.7942 0.4242 0.044 Uiso 1 1 calc R . . C12' C 0.4294(11) 0.8600(8) 0.4815(6) 0.041(3) Uani 1 1 d . . . H12' H 0.3792 0.8742 0.5362 0.049 Uiso 1 1 calc R . . C13' C 0.5603(10) 0.8790(7) 0.4477(6) 0.029(2) Uani 1 1 d . . . H13' H 0.6167 0.9088 0.4763 0.035 Uiso 1 1 calc R . . C14' C 0.4624(10) 0.9188(9) 0.1516(6) 0.038(3) Uani 1 1 d . . . H14' H 0.3786 0.9043 0.1431 0.046 Uiso 1 1 calc R . . C15' C 0.5330(9) 0.9954(9) 0.1137(6) 0.037(3) Uani 1 1 d . . . H15' H 0.5091 1.0442 0.0748 0.044 Uiso 1 1 calc R . . C16' C 0.6476(10) 0.9876(8) 0.1437(5) 0.033(2) Uani 1 1 d . . . H16' H 0.7177 1.0311 0.1287 0.039 Uiso 1 1 calc R . . C21' C 0.9272(12) 0.8532(8) 0.4396(6) 0.041(3) Uani 1 1 d . . . H21D H 0.9787 0.8143 0.4748 0.061 Uiso 1 1 calc R . . H21E H 0.8437 0.8802 0.4747 0.061 Uiso 1 1 calc R . . H21F H 0.9779 0.9085 0.4110 0.061 Uiso 1 1 calc R . . C22' C 0.8052(11) 0.6741(8) 0.4244(6) 0.036(2) Uani 1 1 d . . . H22D H 0.8570 0.6443 0.4635 0.054 Uiso 1 1 calc R . . H22E H 0.7920 0.6227 0.3872 0.054 Uiso 1 1 calc R . . H22F H 0.7190 0.7013 0.4559 0.054 Uiso 1 1 calc R . . C23' C 1.0561(10) 0.7147(9) 0.3249(7) 0.043(3) Uani 1 1 d . . . H23D H 1.0925 0.6888 0.3724 0.065 Uiso 1 1 calc R . . H23E H 1.1137 0.7640 0.2924 0.065 Uiso 1 1 calc R . . H23F H 1.0508 0.6594 0.2891 0.065 Uiso 1 1 calc R . . C1' C 0.9278(10) 0.8315(7) 0.1658(5) 0.027(2) Uani 1 1 d . . . C2' C 1.0307(9) 0.9041(7) 0.1368(6) 0.028(2) Uani 1 1 d . . . C3' C 1.1444(10) 0.8721(7) 0.0636(6) 0.030(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 0.0193(3) 0.0176(3) 0.0155(3) -0.0001(2) -0.0052(3) 0.0001(3) Rh1' 0.0189(3) 0.0199(3) 0.0156(3) -0.0005(2) -0.0044(3) -0.0006(3) I1 0.0315(3) 0.0216(3) 0.0272(3) 0.0035(2) -0.0086(3) -0.0008(2) I1' 0.0373(4) 0.0273(3) 0.0301(3) -0.0050(3) -0.0042(3) 0.0013(3) P1 0.0284(13) 0.0272(12) 0.0196(11) -0.0018(9) -0.0104(10) -0.0010(10) P1' 0.0261(12) 0.0255(12) 0.0210(11) 0.0006(9) -0.0079(9) -0.0016(10) B1 0.024(5) 0.024(5) 0.017(4) 0.008(4) -0.010(4) 0.005(4) B1' 0.028(6) 0.037(6) 0.024(5) -0.001(5) -0.009(5) -0.004(5) F11 0.029(3) 0.043(3) 0.031(3) -0.006(3) -0.008(2) -0.005(3) F12 0.028(3) 0.033(3) 0.037(3) 0.006(2) -0.011(2) 0.005(2) F21 0.037(3) 0.029(3) 0.042(3) -0.016(3) -0.002(3) 0.002(3) F22 0.033(3) 0.047(4) 0.021(3) 0.005(2) -0.002(2) 0.008(3) F31 0.052(4) 0.051(4) 0.046(4) 0.003(3) 0.005(3) -0.023(3) F32 0.020(3) 0.086(5) 0.054(4) 0.018(4) -0.004(3) -0.001(3) F33 0.044(4) 0.069(5) 0.028(3) -0.002(3) 0.009(3) -0.004(3) F12' 0.035(3) 0.024(3) 0.044(3) -0.005(3) 0.001(3) 0.003(2) F11' 0.033(3) 0.058(4) 0.020(3) -0.012(3) -0.006(2) -0.011(3) F22' 0.038(3) 0.027(3) 0.038(3) 0.007(2) -0.004(3) 0.001(2) F21' 0.030(3) 0.035(3) 0.036(3) -0.006(2) -0.013(3) -0.008(2) F31' 0.042(4) 0.042(4) 0.041(3) 0.002(3) 0.004(3) -0.010(3) F32' 0.031(3) 0.037(3) 0.039(3) -0.003(3) -0.001(3) 0.007(3) F33' 0.042(4) 0.053(4) 0.030(3) -0.010(3) 0.001(3) -0.007(3) N1 0.020(4) 0.021(4) 0.014(3) 0.002(3) -0.004(3) -0.001(3) N2 0.017(4) 0.025(4) 0.020(4) -0.002(3) -0.006(3) 0.006(3) N3 0.019(4) 0.026(4) 0.014(3) 0.001(3) -0.005(3) 0.000(3) N4 0.017(4) 0.026(4) 0.015(3) -0.001(3) -0.001(3) -0.001(3) N5 0.024(4) 0.020(4) 0.022(4) 0.004(3) -0.007(3) -0.001(3) N6 0.028(4) 0.024(4) 0.025(4) -0.003(3) -0.006(3) 0.003(3) N5' 0.023(4) 0.024(4) 0.025(4) 0.000(3) -0.005(3) -0.006(3) N6' 0.023(4) 0.041(5) 0.028(4) -0.003(4) -0.006(3) -0.010(4) N1' 0.025(4) 0.032(4) 0.022(4) 0.004(3) -0.003(3) 0.002(3) N2' 0.022(4) 0.037(5) 0.023(4) 0.003(3) -0.002(3) -0.003(3) N3' 0.020(4) 0.031(4) 0.022(4) -0.001(3) -0.006(3) 0.001(3) N4' 0.025(4) 0.045(5) 0.024(4) -0.002(4) -0.009(3) -0.003(4) C11 0.011(4) 0.028(5) 0.043(6) -0.013(4) -0.010(4) 0.002(4) C12 0.017(4) 0.028(5) 0.029(5) -0.009(4) -0.002(4) 0.003(4) C13 0.024(5) 0.026(5) 0.021(4) -0.005(4) -0.007(4) 0.000(4) C14 0.015(4) 0.046(6) 0.026(5) -0.004(4) -0.006(4) -0.007(4) C15 0.031(5) 0.028(5) 0.026(5) -0.008(4) -0.005(4) -0.003(4) C16 0.025(5) 0.022(4) 0.024(4) -0.013(4) 0.001(4) -0.003(4) C17 0.039(6) 0.028(5) 0.023(5) 0.000(4) -0.009(4) 0.005(4) C18 0.049(7) 0.025(5) 0.032(5) 0.008(4) -0.008(5) 0.001(5) C19 0.038(5) 0.017(4) 0.027(5) 0.000(4) -0.009(4) -0.001(4) C21 0.041(6) 0.044(6) 0.034(5) -0.001(5) -0.024(5) 0.004(5) C22 0.051(7) 0.027(5) 0.043(6) -0.012(5) -0.023(5) 0.003(5) C23 0.038(6) 0.052(7) 0.017(4) -0.003(4) -0.008(4) -0.005(5) C1 0.013(4) 0.022(4) 0.038(5) 0.006(4) -0.009(4) -0.004(3) C2 0.023(5) 0.032(5) 0.021(4) -0.003(4) -0.008(4) 0.004(4) C3 0.033(6) 0.043(6) 0.035(6) 0.004(5) -0.006(5) -0.010(5) C17' 0.040(6) 0.041(6) 0.027(5) 0.000(4) -0.013(4) -0.017(5) C18' 0.068(8) 0.022(5) 0.028(5) -0.002(4) -0.010(5) -0.014(5) C19' 0.042(6) 0.029(5) 0.034(5) -0.005(4) -0.008(5) -0.008(5) C11' 0.029(5) 0.039(6) 0.038(6) 0.010(5) -0.004(5) -0.005(5) C12' 0.049(7) 0.048(7) 0.021(5) 0.002(5) -0.002(5) -0.001(5) C13' 0.031(5) 0.033(5) 0.019(4) -0.003(4) 0.001(4) 0.006(4) C14' 0.028(5) 0.064(8) 0.029(5) 0.007(5) -0.018(4) -0.013(5) C15' 0.020(5) 0.064(8) 0.025(5) 0.010(5) -0.007(4) 0.002(5) C16' 0.034(5) 0.045(6) 0.017(4) 0.007(4) -0.006(4) 0.009(5) C21' 0.053(7) 0.049(7) 0.027(5) -0.009(5) -0.017(5) -0.012(5) C22' 0.042(6) 0.035(6) 0.032(5) 0.006(4) -0.006(5) -0.013(5) C23' 0.035(6) 0.048(7) 0.048(7) 0.002(5) -0.017(5) 0.006(5) C1' 0.039(5) 0.024(5) 0.021(4) 0.000(4) -0.015(4) 0.010(4) C2' 0.025(5) 0.026(5) 0.030(5) 0.000(4) -0.005(4) 0.001(4) C3' 0.037(6) 0.022(5) 0.028(5) 0.002(4) -0.005(4) -0.003(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 2.052(9) . ? Rh1 N5 2.099(7) . ? Rh1 N3 2.138(7) . ? Rh1 N1 2.153(7) . ? Rh1 P1 2.295(2) . ? Rh1 I1 2.6454(9) . ? Rh1' N5' 2.074(7) . ? Rh1' C1' 2.078(10) . ? Rh1' N3' 2.113(7) . ? Rh1' N1' 2.154(7) . ? Rh1' P1' 2.301(2) . ? Rh1' I1' 2.6509(10) . ? P1 C22 1.794(10) . ? P1 C23 1.803(10) . ? P1 C21 1.820(10) . ? P1' C23' 1.803(11) . ? P1' C21' 1.804(10) . ? P1' C22' 1.805(10) . ? B1 N6 1.530(13) . ? B1 N2 1.530(12) . ? B1 N4 1.533(12) . ? B1' N4' 1.518(14) . ? B1' N2' 1.526(13) . ? B1' N6' 1.551(14) . ? F11 C1 1.413(10) . ? F12 C1 1.370(10) . ? F21 C2 1.365(10) . ? F22 C2 1.350(10) . ? F31 C3 1.311(12) . ? F32 C3 1.326(12) . ? F33 C3 1.332(12) . ? F12' C1' 1.378(10) . ? F11' C1' 1.394(10) . ? F22' C2' 1.344(10) . ? F21' C2' 1.366(10) . ? F31' C3' 1.344(11) . ? F32' C3' 1.327(11) . ? F33' C3' 1.332(11) . ? N1 C13 1.325(11) . ? N1 N2 1.362(9) . ? N2 C11 1.350(11) . ? N3 C16 1.328(11) . ? N3 N4 1.362(9) . ? N4 C14 1.338(11) . ? N5 C19 1.349(11) . ? N5 N6 1.378(10) . ? N6 C17 1.327(12) . ? N5' C19' 1.313(12) . ? N5' N6' 1.378(10) . ? N6' C17' 1.314(13) . ? N1' C13' 1.334(11) . ? N1' N2' 1.355(11) . ? N2' C11' 1.336(12) . ? N3' C16' 1.341(12) . ? N3' N4' 1.353(11) . ? N4' C14' 1.339(12) . ? C11 C12 1.342(13) . ? C12 C13 1.394(12) . ? C14 C15 1.363(13) . ? C15 C16 1.380(13) . ? C17 C18 1.397(14) . ? C18 C19 1.379(12) . ? C1 C2 1.537(13) . ? C2 C3 1.538(14) . ? C17' C18' 1.348(15) . ? C18' C19' 1.392(14) . ? C11' C12' 1.355(15) . ? C12' C13' 1.386(15) . ? C14' C15' 1.351(15) . ? C15' C16' 1.385(13) . ? C1' C2' 1.484(14) . ? C2' C3' 1.533(13) . ? 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 N5 89.3(3) . . ? C1 Rh1 N3 96.8(3) . . ? N5 Rh1 N3 87.6(3) . . ? C1 Rh1 N1 177.6(3) . . ? N5 Rh1 N1 89.0(3) . . ? N3 Rh1 N1 81.3(3) . . ? C1 Rh1 P1 88.4(3) . . ? N5 Rh1 P1 94.7(2) . . ? N3 Rh1 P1 174.3(2) . . ? N1 Rh1 P1 93.44(19) . . ? C1 Rh1 I1 93.0(2) . . ? N5 Rh1 I1 176.9(2) . . ? N3 Rh1 I1 90.06(19) . . ? N1 Rh1 I1 88.59(18) . . ? P1 Rh1 I1 87.49(7) . . ? N5' Rh1' C1' 86.3(3) . . ? N5' Rh1' N3' 88.1(3) . . ? C1' Rh1' N3' 91.2(3) . . ? N5' Rh1' N1' 87.7(3) . . ? C1' Rh1' N1' 171.9(3) . . ? N3' Rh1' N1' 83.1(3) . . ? N5' Rh1' P1' 91.3(2) . . ? C1' Rh1' P1' 95.2(2) . . ? N3' Rh1' P1' 173.5(2) . . ? N1' Rh1' P1' 90.4(2) . . ? N5' Rh1' I1' 175.4(2) . . ? C1' Rh1' I1' 96.4(3) . . ? N3' Rh1' I1' 88.1(2) . . ? N1' Rh1' I1' 89.3(2) . . ? P1' Rh1' I1' 92.21(7) . . ? C22 P1 C23 101.0(5) . . ? C22 P1 C21 103.6(5) . . ? C23 P1 C21 101.4(5) . . ? C22 P1 Rh1 114.4(4) . . ? C23 P1 Rh1 116.5(3) . . ? C21 P1 Rh1 117.6(3) . . ? C23' P1' C21' 99.7(5) . . ? C23' P1' C22' 102.9(5) . . ? C21' P1' C22' 104.2(5) . . ? C23' P1' Rh1' 120.5(4) . . ? C21' P1' Rh1' 117.5(4) . . ? C22' P1' Rh1' 110.0(4) . . ? N6 B1 N2 109.5(7) . . ? N6 B1 N4 108.5(7) . . ? N2 B1 N4 107.3(7) . . ? N4' B1' N2' 108.3(8) . . ? N4' B1' N6' 108.5(8) . . ? N2' B1' N6' 108.1(8) . . ? C13 N1 N2 106.3(7) . . ? C13 N1 Rh1 135.9(6) . . ? N2 N1 Rh1 117.7(5) . . ? C11 N2 N1 109.1(7) . . ? C11 N2 B1 130.2(8) . . ? N1 N2 B1 120.2(7) . . ? C16 N3 N4 106.0(7) . . ? C16 N3 Rh1 135.7(6) . . ? N4 N3 Rh1 118.0(5) . . ? C14 N4 N3 109.4(7) . . ? C14 N4 B1 129.2(7) . . ? N3 N4 B1 120.2(7) . . ? C19 N5 N6 106.4(7) . . ? C19 N5 Rh1 136.1(6) . . ? N6 N5 Rh1 117.2(5) . . ? C17 N6 N5 109.9(8) . . ? C17 N6 B1 128.4(8) . . ? N5 N6 B1 121.6(7) . . ? C19' N5' N6' 105.3(8) . . ? C19' N5' Rh1' 136.0(7) . . ? N6' N5' Rh1' 118.7(6) . . ? C17' N6' N5' 109.6(8) . . ? C17' N6' B1' 130.8(9) . . ? N5' N6' B1' 119.6(8) . . ? C13' N1' N2' 107.0(8) . . ? C13' N1' Rh1' 136.3(7) . . ? N2' N1' Rh1' 116.7(6) . . ? C11' N2' N1' 108.8(8) . . ? C11' N2' B1' 130.0(9) . . ? N1' N2' B1' 121.0(8) . . ? C16' N3' N4' 108.1(8) . . ? C16' N3' Rh1' 133.9(7) . . ? N4' N3' Rh1' 118.0(6) . . ? C14' N4' N3' 107.6(8) . . ? C14' N4' B1' 131.4(9) . . ? N3' N4' B1' 120.8(8) . . ? C12 C11 N2 108.9(8) . . ? C11 C12 C13 105.3(8) . . ? N1 C13 C12 110.3(8) . . ? N4 C14 C15 108.9(8) . . ? C14 C15 C16 104.8(8) . . ? N3 C16 C15 110.9(8) . . ? N6 C17 C18 108.3(9) . . ? C19 C18 C17 105.5(9) . . ? N5 C19 C18 109.9(9) . . ? F12 C1 F11 102.7(6) . . ? F12 C1 C2 103.6(7) . . ? F11 C1 C2 101.6(7) . . ? F12 C1 Rh1 115.4(6) . . ? F11 C1 Rh1 111.6(6) . . ? C2 C1 Rh1 119.8(6) . . ? F22 C2 F21 106.6(7) . . ? F22 C2 C1 111.6(7) . . ? F21 C2 C1 107.9(7) . . ? F22 C2 C3 105.5(8) . . ? F21 C2 C3 105.7(7) . . ? C1 C2 C3 118.8(8) . . ? F31 C3 F32 109.6(9) . . ? F31 C3 F33 108.0(8) . . ? F32 C3 F33 107.9(9) . . ? F31 C3 C2 110.4(9) . . ? F32 C3 C2 111.0(8) . . ? F33 C3 C2 109.8(8) . . ? N6' C17' C18' 109.7(9) . . ? C17' C18' C19' 104.4(9) . . ? N5' C19' C18' 111.0(10) . . ? N2' C11' C12' 109.4(9) . . ? C11' C12' C13' 105.1(9) . . ? N1' C13' C12' 109.6(9) . . ? N4' C14' C15' 110.3(9) . . ? C14' C15' C16' 105.2(9) . . ? N3' C16' C15' 108.9(10) . . ? F12' C1' F11' 101.7(7) . . ? F12' C1' C2' 104.4(8) . . ? F11' C1' C2' 104.7(7) . . ? F12' C1' Rh1' 111.0(6) . . ? F11' C1' Rh1' 106.3(6) . . ? C2' C1' Rh1' 126.0(6) . . ? F22' C2' F21' 108.4(7) . . ? F22' C2' C1' 110.7(8) . . ? F21' C2' C1' 110.3(7) . . ? F22' C2' C3' 106.4(7) . . ? F21' C2' C3' 104.5(7) . . ? C1' C2' C3' 116.2(8) . . ? F32' C3' F33' 108.2(8) . . ? F32' C3' F31' 105.9(8) . . ? F33' C3' F31' 107.1(7) . . ? F32' C3' C2' 113.0(8) . . ? F33' C3' C2' 112.3(8) . . ? F31' C3' C2' 109.9(8) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 1.155 _refine_diff_density_min -1.868 _refine_diff_density_rms 0.180 #===END