# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jones, William' _publ_contact_author_email jones@chem.rochester.edu _publ_section_title ; Synthesis, structure, and reductive elimination in the series Tp'Rh(PR3)(ArF)H; Determination of rhodium carbon bond energies of fluoroaryl substituents ; loop_ _publ_author_name T.Tanabe W.Brennessel E.Clot O.Eisenstein W.Jones data_jontt01_cmpd1 _database_code_depnum_ccdc_archive 'CCDC 770109' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt01 _chemical_melting_point ? _chemical_formula_moiety 'C18 H33 B N6 P Rh' _chemical_formula_sum 'C18 H33 B N6 P Rh' _chemical_formula_weight 478.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0429(15) _cell_length_b 11.5505(18) _cell_length_c 11.6084(18) _cell_angle_alpha 62.668(2) _cell_angle_beta 80.643(3) _cell_angle_gamma 66.913(3) _cell_volume 1100.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3951 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 37.83 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7577 _exptl_absorpt_correction_T_max 0.9341 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24361 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 35.63 _reflns_number_total 9947 _reflns_number_gt 8530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The positions and isotropic displacement parameters of the hydride ligands were refined independently from those of all other atoms. ; _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^)+(0.0352P)^2^+0.2436P] 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 9947 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.795272(11) 0.049282(11) 0.235506(10) 0.01563(3) Uani 1 1 d . . . H1 H 0.746(2) -0.057(2) 0.2449(19) 0.024(5) Uiso 1 1 d . . . H2 H 0.843(2) 0.047(2) 0.106(2) 0.026(5) Uiso 1 1 d . . . P1 P 1.00045(4) -0.13215(4) 0.31082(4) 0.01760(7) Uani 1 1 d . . . N1 N 0.86124(13) 0.22604(13) 0.19641(12) 0.0183(2) Uani 1 1 d . . . N2 N 0.77394(13) 0.31743(12) 0.24584(11) 0.0177(2) Uani 1 1 d . . . N3 N 0.59384(12) 0.20963(12) 0.15726(11) 0.01583(19) Uani 1 1 d . . . N4 N 0.54118(12) 0.31770(12) 0.19140(11) 0.0169(2) Uani 1 1 d . . . N5 N 0.70392(13) 0.05388(12) 0.42032(11) 0.0174(2) Uani 1 1 d . . . N6 N 0.63574(13) 0.18227(13) 0.42069(11) 0.0177(2) Uani 1 1 d . . . B1 B 0.62295(17) 0.31521(17) 0.29520(15) 0.0179(3) Uani 1 1 d . . . H1B H 0.5675 0.3991 0.3118 0.022 Uiso 1 1 calc R . . C1 C 0.97306(16) 0.26749(16) 0.14276(14) 0.0218(3) Uani 1 1 d . . . C2 C 0.96031(16) 0.38248(16) 0.16225(15) 0.0230(3) Uani 1 1 d . . . H2A H 1.0261 0.4304 0.1360 0.028 Uiso 1 1 calc R . . C3 C 0.83292(16) 0.41181(15) 0.22721(14) 0.0204(2) Uani 1 1 d . . . C4 C 0.49693(15) 0.23179(15) 0.07575(13) 0.0178(2) Uani 1 1 d . . . C5 C 0.38001(15) 0.35591(15) 0.05734(13) 0.0198(2) Uani 1 1 d . . . H5A H 0.2959 0.3963 0.0046 0.024 Uiso 1 1 calc R . . C6 C 0.41176(15) 0.40769(15) 0.13136(13) 0.0184(2) Uani 1 1 d . . . C7 C 0.68350(15) -0.03991(15) 0.53769(13) 0.0199(2) Uani 1 1 d . . . C8 C 0.60457(17) 0.02760(18) 0.61425(14) 0.0241(3) Uani 1 1 d . . . H8A H 0.5768 -0.0146 0.7015 0.029 Uiso 1 1 calc R . . C9 C 0.57529(16) 0.16803(17) 0.53715(14) 0.0220(3) Uani 1 1 d . . . C10 C 1.08574(19) 0.20191(19) 0.0687(2) 0.0335(4) Uani 1 1 d . . . H10A H 1.0532 0.1429 0.0494 0.050 Uiso 1 1 calc R . . H10B H 1.1759 0.1445 0.1204 0.050 Uiso 1 1 calc R . . H10C H 1.1025 0.2750 -0.0126 0.050 Uiso 1 1 calc R . . C11 C 0.7634(2) 0.52519(17) 0.27046(16) 0.0271(3) Uani 1 1 d . . . H11A H 0.7480 0.4839 0.3641 0.041 Uiso 1 1 calc R . . H11B H 0.6701 0.5878 0.2248 0.041 Uiso 1 1 calc R . . H11C H 0.8265 0.5784 0.2509 0.041 Uiso 1 1 calc R . . C12 C 0.52033(17) 0.13385(17) 0.01812(15) 0.0235(3) Uani 1 1 d . . . H12A H 0.5763 0.0385 0.0794 0.035 Uiso 1 1 calc R . . H12B H 0.5736 0.1609 -0.0626 0.035 Uiso 1 1 calc R . . H12C H 0.4265 0.1377 -0.0004 0.035 Uiso 1 1 calc R . . C13 C 0.32358(17) 0.53686(16) 0.14836(16) 0.0239(3) Uani 1 1 d . . . H13A H 0.3844 0.5906 0.1350 0.036 Uiso 1 1 calc R . . H13B H 0.2854 0.5110 0.2363 0.036 Uiso 1 1 calc R . . H13C H 0.2430 0.5939 0.0850 0.036 Uiso 1 1 calc R . . C14 C 0.73343(18) -0.19237(16) 0.57321(15) 0.0257(3) Uani 1 1 d . . . H14A H 0.7343 -0.2052 0.4953 0.039 Uiso 1 1 calc R . . H14B H 0.6674 -0.2325 0.6362 0.039 Uiso 1 1 calc R . . H14C H 0.8313 -0.2395 0.6115 0.039 Uiso 1 1 calc R . . C15 C 0.4911(2) 0.2887(2) 0.56853(17) 0.0308(3) Uani 1 1 d . . . H15A H 0.4091 0.3525 0.5073 0.046 Uiso 1 1 calc R . . H15B H 0.5539 0.3385 0.5618 0.046 Uiso 1 1 calc R . . H15C H 0.4553 0.2543 0.6570 0.046 Uiso 1 1 calc R . . C16 C 0.9949(2) -0.30394(17) 0.35551(19) 0.0309(3) Uani 1 1 d . . . H16A H 1.0882 -0.3765 0.3948 0.046 Uiso 1 1 calc R . . H16B H 0.9756 -0.3083 0.2778 0.046 Uiso 1 1 calc R . . H16C H 0.9179 -0.3190 0.4179 0.046 Uiso 1 1 calc R . . C17 C 1.07629(17) -0.15301(17) 0.45364(15) 0.0241(3) Uani 1 1 d . . . H17A H 1.1627 -0.2385 0.4839 0.036 Uiso 1 1 calc R . . H17B H 1.0045 -0.1596 0.5222 0.036 Uiso 1 1 calc R . . H17C H 1.1027 -0.0723 0.4320 0.036 Uiso 1 1 calc R . . C18 C 1.16042(18) -0.14560(18) 0.21007(16) 0.0296(3) Uani 1 1 d . . . H18A H 1.2360 -0.2375 0.2539 0.044 Uiso 1 1 calc R . . H18B H 1.1961 -0.0724 0.1957 0.044 Uiso 1 1 calc R . . H18C H 1.1350 -0.1341 0.1265 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01548(5) 0.01790(5) 0.01327(5) -0.00556(3) -0.00086(3) -0.00684(3) P1 0.01750(15) 0.01792(15) 0.01720(15) -0.00754(12) -0.00106(12) -0.00582(12) N1 0.0159(5) 0.0197(5) 0.0179(5) -0.0068(4) 0.0001(4) -0.0067(4) N2 0.0191(5) 0.0202(5) 0.0156(5) -0.0066(4) 0.0003(4) -0.0103(4) N3 0.0148(5) 0.0187(5) 0.0133(4) -0.0056(4) -0.0007(4) -0.0067(4) N4 0.0158(5) 0.0185(5) 0.0155(5) -0.0059(4) -0.0005(4) -0.0069(4) N5 0.0169(5) 0.0202(5) 0.0144(5) -0.0049(4) -0.0005(4) -0.0089(4) N6 0.0177(5) 0.0227(5) 0.0146(5) -0.0078(4) 0.0011(4) -0.0098(4) B1 0.0174(6) 0.0199(6) 0.0181(6) -0.0086(5) 0.0021(5) -0.0085(5) C1 0.0180(6) 0.0218(6) 0.0199(6) -0.0029(5) 0.0000(5) -0.0092(5) C2 0.0211(6) 0.0234(6) 0.0226(6) -0.0040(5) -0.0017(5) -0.0126(5) C3 0.0234(6) 0.0217(6) 0.0172(6) -0.0049(5) -0.0026(5) -0.0124(5) C4 0.0166(5) 0.0230(6) 0.0136(5) -0.0061(5) -0.0003(4) -0.0092(5) C5 0.0155(5) 0.0241(6) 0.0161(5) -0.0056(5) -0.0019(4) -0.0066(5) C6 0.0164(5) 0.0194(6) 0.0154(5) -0.0042(4) 0.0002(4) -0.0067(5) C7 0.0179(6) 0.0245(6) 0.0149(5) -0.0032(5) -0.0007(4) -0.0113(5) C8 0.0217(6) 0.0340(8) 0.0149(6) -0.0068(5) 0.0032(5) -0.0142(6) C9 0.0196(6) 0.0325(7) 0.0158(6) -0.0111(5) 0.0030(5) -0.0118(5) C10 0.0254(8) 0.0290(8) 0.0427(10) -0.0137(7) 0.0134(7) -0.0140(6) C11 0.0366(8) 0.0262(7) 0.0252(7) -0.0120(6) 0.0006(6) -0.0168(6) C12 0.0218(6) 0.0309(7) 0.0217(6) -0.0141(6) -0.0008(5) -0.0097(6) C13 0.0209(6) 0.0207(6) 0.0246(7) -0.0073(5) 0.0006(5) -0.0053(5) C14 0.0242(7) 0.0250(7) 0.0221(7) -0.0018(5) 0.0000(5) -0.0132(6) C15 0.0304(8) 0.0406(9) 0.0258(7) -0.0202(7) 0.0075(6) -0.0126(7) C16 0.0302(8) 0.0225(7) 0.0418(9) -0.0146(7) -0.0028(7) -0.0092(6) C17 0.0210(6) 0.0281(7) 0.0226(7) -0.0105(6) -0.0055(5) -0.0067(5) C18 0.0245(7) 0.0297(8) 0.0247(7) -0.0103(6) 0.0042(6) -0.0036(6) _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 N3 2.1124(11) . ? Rh1 N5 2.2076(12) . ? Rh1 P1 2.2178(5) . ? Rh1 N1 2.2193(13) . ? Rh1 H1 1.455(19) . ? Rh1 H2 1.51(2) . ? P1 C17 1.8129(15) . ? P1 C18 1.8257(17) . ? P1 C16 1.8280(17) . ? N1 C1 1.3411(19) . ? N1 N2 1.3708(17) . ? N2 C3 1.3544(18) . ? N2 B1 1.537(2) . ? N3 C4 1.3379(17) . ? N3 N4 1.3651(16) . ? N4 C6 1.3511(17) . ? N4 B1 1.5487(19) . ? N5 C7 1.3417(18) . ? N5 N6 1.3699(17) . ? N6 C9 1.3530(18) . ? N6 B1 1.533(2) . ? B1 H1B 1.0000 . ? C1 C2 1.402(2) . ? C1 C10 1.484(2) . ? C2 C3 1.379(2) . ? C2 H2A 0.9500 . ? C3 C11 1.492(2) . ? C4 C5 1.400(2) . ? C4 C12 1.489(2) . ? C5 C6 1.381(2) . ? C5 H5A 0.9500 . ? C6 C13 1.492(2) . ? C7 C8 1.396(2) . ? C7 C14 1.493(2) . ? C8 C9 1.377(2) . ? C8 H8A 0.9500 . ? C9 C15 1.494(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Rh1 N5 83.48(4) . . ? N3 Rh1 P1 174.03(3) . . ? N5 Rh1 P1 99.21(3) . . ? N3 Rh1 N1 83.52(5) . . ? N5 Rh1 N1 88.77(4) . . ? P1 Rh1 N1 101.80(3) . . ? N3 Rh1 H1 92.2(8) . . ? N5 Rh1 H1 96.2(8) . . ? P1 Rh1 H1 82.3(8) . . ? N1 Rh1 H1 173.1(8) . . ? N3 Rh1 H2 92.3(8) . . ? N5 Rh1 H2 174.2(8) . . ? P1 Rh1 H2 84.6(8) . . ? N1 Rh1 H2 94.8(8) . . ? H1 Rh1 H2 79.9(11) . . ? C17 P1 C18 100.04(8) . . ? C17 P1 C16 104.15(8) . . ? C18 P1 C16 97.93(9) . . ? C17 P1 Rh1 114.62(5) . . ? C18 P1 Rh1 120.70(6) . . ? C16 P1 Rh1 116.51(6) . . ? C1 N1 N2 106.38(12) . . ? C1 N1 Rh1 137.49(10) . . ? N2 N1 Rh1 115.94(9) . . ? C3 N2 N1 110.37(12) . . ? C3 N2 B1 128.86(13) . . ? N1 N2 B1 120.21(11) . . ? C4 N3 N4 107.44(11) . . ? C4 N3 Rh1 133.24(10) . . ? N4 N3 Rh1 119.31(8) . . ? C6 N4 N3 109.73(11) . . ? C6 N4 B1 130.22(12) . . ? N3 N4 B1 119.78(11) . . ? C7 N5 N6 106.27(12) . . ? C7 N5 Rh1 136.00(10) . . ? N6 N5 Rh1 117.36(8) . . ? C9 N6 N5 110.14(12) . . ? C9 N6 B1 129.63(13) . . ? N5 N6 B1 119.86(11) . . ? N6 B1 N2 110.44(12) . . ? N6 B1 N4 108.67(12) . . ? N2 B1 N4 109.32(11) . . ? N6 B1 H1B 109.5 . . ? N2 B1 H1B 109.5 . . ? N4 B1 H1B 109.5 . . ? N1 C1 C2 109.79(14) . . ? N1 C1 C10 122.81(15) . . ? C2 C1 C10 127.32(14) . . ? C3 C2 C1 106.02(13) . . ? C3 C2 H2A 127.0 . . ? C1 C2 H2A 127.0 . . ? N2 C3 C2 107.40(13) . . ? N2 C3 C11 123.16(14) . . ? C2 C3 C11 129.43(14) . . ? N3 C4 C5 109.11(12) . . ? N3 C4 C12 121.89(13) . . ? C5 C4 C12 128.99(13) . . ? C6 C5 C4 106.07(12) . . ? C6 C5 H5A 127.0 . . ? C4 C5 H5A 127.0 . . ? N4 C6 C5 107.64(12) . . ? N4 C6 C13 123.69(13) . . ? C5 C6 C13 128.66(13) . . ? N5 C7 C8 110.09(13) . . ? N5 C7 C14 122.81(14) . . ? C8 C7 C14 127.02(13) . . ? C9 C8 C7 105.78(13) . . ? C9 C8 H8A 127.1 . . ? C7 C8 H8A 127.1 . . ? N6 C9 C8 107.72(14) . . ? N6 C9 C15 123.48(14) . . ? C8 C9 C15 128.80(14) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P1 C16 H16A 109.5 . . ? P1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P1 C17 H17A 109.5 . . ? P1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P1 C18 H18A 109.5 . . ? P1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Rh1 P1 C17 -148.8(3) . . . . ? N5 Rh1 P1 C17 -32.28(7) . . . . ? N1 Rh1 P1 C17 58.39(7) . . . . ? N3 Rh1 P1 C18 91.6(3) . . . . ? N5 Rh1 P1 C18 -151.96(8) . . . . ? N1 Rh1 P1 C18 -61.28(8) . . . . ? N3 Rh1 P1 C16 -26.8(3) . . . . ? N5 Rh1 P1 C16 89.66(8) . . . . ? N1 Rh1 P1 C16 -179.67(8) . . . . ? N3 Rh1 N1 C1 -133.51(15) . . . . ? N5 Rh1 N1 C1 142.91(14) . . . . ? P1 Rh1 N1 C1 43.75(15) . . . . ? N3 Rh1 N1 N2 52.39(9) . . . . ? N5 Rh1 N1 N2 -31.19(9) . . . . ? P1 Rh1 N1 N2 -130.35(9) . . . . ? C1 N1 N2 C3 -2.04(15) . . . . ? Rh1 N1 N2 C3 173.80(9) . . . . ? C1 N1 N2 B1 170.14(12) . . . . ? Rh1 N1 N2 B1 -14.01(15) . . . . ? N5 Rh1 N3 C4 -132.17(13) . . . . ? P1 Rh1 N3 C4 -15.0(4) . . . . ? N1 Rh1 N3 C4 138.33(13) . . . . ? N5 Rh1 N3 N4 47.32(9) . . . . ? P1 Rh1 N3 N4 164.5(3) . . . . ? N1 Rh1 N3 N4 -42.18(9) . . . . ? C4 N3 N4 C6 -0.14(15) . . . . ? Rh1 N3 N4 C6 -179.74(9) . . . . ? C4 N3 N4 B1 174.54(12) . . . . ? Rh1 N3 N4 B1 -5.07(15) . . . . ? N3 Rh1 N5 C7 126.28(14) . . . . ? P1 Rh1 N5 C7 -48.34(13) . . . . ? N1 Rh1 N5 C7 -150.10(13) . . . . ? N3 Rh1 N5 N6 -45.55(9) . . . . ? P1 Rh1 N5 N6 139.83(9) . . . . ? N1 Rh1 N5 N6 38.07(9) . . . . ? C7 N5 N6 C9 0.65(15) . . . . ? Rh1 N5 N6 C9 174.75(9) . . . . ? C7 N5 N6 B1 -172.95(12) . . . . ? Rh1 N5 N6 B1 1.15(15) . . . . ? C9 N6 B1 N2 126.42(15) . . . . ? N5 N6 B1 N2 -61.39(16) . . . . ? C9 N6 B1 N4 -113.68(15) . . . . ? N5 N6 B1 N4 58.51(16) . . . . ? C3 N2 B1 N6 -119.36(15) . . . . ? N1 N2 B1 N6 70.06(16) . . . . ? C3 N2 B1 N4 121.13(14) . . . . ? N1 N2 B1 N4 -49.45(16) . . . . ? C6 N4 B1 N6 115.77(15) . . . . ? N3 N4 B1 N6 -57.66(16) . . . . ? C6 N4 B1 N2 -123.63(15) . . . . ? N3 N4 B1 N2 62.95(15) . . . . ? N2 N1 C1 C2 2.28(16) . . . . ? Rh1 N1 C1 C2 -172.19(11) . . . . ? N2 N1 C1 C10 -174.67(14) . . . . ? Rh1 N1 C1 C10 10.9(2) . . . . ? N1 C1 C2 C3 -1.69(17) . . . . ? C10 C1 C2 C3 175.08(16) . . . . ? N1 N2 C3 C2 1.00(16) . . . . ? B1 N2 C3 C2 -170.32(13) . . . . ? N1 N2 C3 C11 -179.98(13) . . . . ? B1 N2 C3 C11 8.7(2) . . . . ? C1 C2 C3 N2 0.40(16) . . . . ? C1 C2 C3 C11 -178.54(15) . . . . ? N4 N3 C4 C5 -0.10(15) . . . . ? Rh1 N3 C4 C5 179.43(10) . . . . ? N4 N3 C4 C12 179.55(12) . . . . ? Rh1 N3 C4 C12 -0.9(2) . . . . ? N3 C4 C5 C6 0.29(16) . . . . ? C12 C4 C5 C6 -179.33(14) . . . . ? N3 N4 C6 C5 0.32(15) . . . . ? B1 N4 C6 C5 -173.62(13) . . . . ? N3 N4 C6 C13 179.38(12) . . . . ? B1 N4 C6 C13 5.4(2) . . . . ? C4 C5 C6 N4 -0.37(16) . . . . ? C4 C5 C6 C13 -179.36(14) . . . . ? N6 N5 C7 C8 -1.03(15) . . . . ? Rh1 N5 C7 C8 -173.48(10) . . . . ? N6 N5 C7 C14 175.88(13) . . . . ? Rh1 N5 C7 C14 3.4(2) . . . . ? N5 C7 C8 C9 1.02(17) . . . . ? C14 C7 C8 C9 -175.73(14) . . . . ? N5 N6 C9 C8 -0.02(16) . . . . ? B1 N6 C9 C8 172.77(14) . . . . ? N5 N6 C9 C15 -179.15(14) . . . . ? B1 N6 C9 C15 -6.4(2) . . . . ? C7 C8 C9 N6 -0.59(16) . . . . ? C7 C8 C9 C15 178.48(15) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 35.63 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.228 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.096 #===end data_jontt06_cmpd2-d6 _database_code_depnum_ccdc_archive 'CCDC 770110' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _vrf_PLAT041_jontt06 ; PROBLEM: _C Calc. and Reported SumFormula Strings Differ ? RESPONSE: The scattering factor for hydrogen was used for the geometrically placed deuterium atoms on the phenyl ligand. ; _vrf_PLAT042_jontt06 ; PROBLEM: _C Calc. and Reported MoietyFormula Strings Differ ? RESPONSE: See above. ; _vrf_FORMU01_jontt06 ; PROBLEM: _G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. RESPONSE: See above. ; _vrf_CELLZ01_jontt06 ; PROBLEM: _G Difference between formula and atom_site contents detected. RESPONSE: See above. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt06 _chemical_melting_point ? _chemical_formula_moiety 'C24 H31 B D6 N6 P Rh' _chemical_formula_sum 'C24 H31 B D6 N6 P Rh' _chemical_formula_weight 560.32 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' D D 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.8303(11) _cell_length_b 15.7867(13) _cell_length_c 14.1339(17) _cell_angle_alpha 90.00 _cell_angle_beta 111.057(1) _cell_angle_gamma 90.00 _cell_volume 2671.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3884 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 37.93 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8458 _exptl_absorpt_correction_T_max 0.8932 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32307 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 37.78 _reflns_number_total 14040 _reflns_number_gt 13027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The boron hydride atom and the deuteride ligand were found from the difference Fourier map and refined independently from their respective bound heavier atoms. Both were refined with individual isotropic displacement parameters. ; _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^)+(0.0251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 6917 Friedel pairs, Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(11) _refine_ls_number_reflns 14040 _refine_ls_number_parameters 315 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.004 _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 0.727862(7) 0.877429(5) 0.227462(7) 0.01256(2) Uani 1 1 d . . . D1 D 0.7570(16) 0.9659(13) 0.2423(15) 0.026(5) Uiso 1 1 d . . . P1 P 0.65081(3) 0.91844(2) 0.06436(3) 0.01715(6) Uani 1 1 d . . . N1 N 0.69187(10) 0.73812(7) 0.21085(8) 0.01513(19) Uani 1 1 d . . . N2 N 0.67449(9) 0.70134(7) 0.29180(9) 0.01517(19) Uani 1 1 d . . . N3 N 0.80725(10) 0.85844(8) 0.38503(9) 0.01481(19) Uani 1 1 d . . . N4 N 0.76254(9) 0.80251(7) 0.43373(8) 0.01442(18) Uani 1 1 d . . . N5 N 0.57752(11) 0.88767(8) 0.26855(10) 0.0159(2) Uani 1 1 d . . . N6 N 0.56115(9) 0.82165(7) 0.32499(9) 0.01498(19) Uani 1 1 d . . . B1 B 0.65376(13) 0.75586(10) 0.37318(11) 0.0150(2) Uani 1 1 d . . . H1B H 0.6286(16) 0.7162(13) 0.4232(14) 0.020(5) Uiso 1 1 d . . . C1 C 0.71483(11) 0.67479(9) 0.15828(10) 0.0161(2) Uani 1 1 d . . . C2 C 0.71449(12) 0.59748(9) 0.20650(10) 0.0178(3) Uani 1 1 d . . . H2 H 0.7289 0.5430 0.1855 0.021 Uiso 1 1 calc R . . C3 C 0.68879(12) 0.61683(8) 0.29108(11) 0.0167(2) Uani 1 1 d . . . C4 C 0.89986(13) 0.89045(9) 0.45479(11) 0.0163(2) Uani 1 1 d . . . C5 C 0.91576(12) 0.85360(10) 0.54934(10) 0.0184(2) Uani 1 1 d . . . H5 H 0.9752 0.8642 0.6117 0.022 Uiso 1 1 calc R . . C6 C 0.82728(11) 0.79880(9) 0.53303(10) 0.0165(2) Uani 1 1 d . . . C7 C 0.49592(12) 0.94324(10) 0.25737(11) 0.0178(2) Uani 1 1 d . . . C8 C 0.42406(13) 0.91307(12) 0.30463(12) 0.0194(3) Uani 1 1 d . . . H8 H 0.3587 0.9398 0.3069 0.023 Uiso 1 1 calc R . . C9 C 0.46832(11) 0.83607(9) 0.34726(10) 0.0168(2) Uani 1 1 d . . . C10 C 0.73616(14) 0.68702(10) 0.06271(12) 0.0232(3) Uani 1 1 d . . . H10A H 0.7920 0.7318 0.0722 0.035 Uiso 1 1 calc R . . H10B H 0.6666 0.7033 0.0084 0.035 Uiso 1 1 calc R . . H10C H 0.7640 0.6341 0.0444 0.035 Uiso 1 1 calc R . . C11 C 0.67984(14) 0.55926(10) 0.37199(12) 0.0233(3) Uani 1 1 d . . . H11A H 0.6081 0.5685 0.3802 0.035 Uiso 1 1 calc R . . H11B H 0.7408 0.5713 0.4361 0.035 Uiso 1 1 calc R . . H11C H 0.6848 0.5002 0.3526 0.035 Uiso 1 1 calc R . . C12 C 0.97077(13) 0.95541(11) 0.43074(12) 0.0233(3) Uani 1 1 d . . . H12A H 0.9230 0.9968 0.3831 0.035 Uiso 1 1 calc R . . H12B H 1.0194 0.9278 0.4001 0.035 Uiso 1 1 calc R . . H12C H 1.0166 0.9843 0.4932 0.035 Uiso 1 1 calc R . . C13 C 0.80031(15) 0.74474(11) 0.60758(12) 0.0261(3) Uani 1 1 d . . . H13A H 0.7927 0.6857 0.5848 0.039 Uiso 1 1 calc R . . H13B H 0.7300 0.7638 0.6130 0.039 Uiso 1 1 calc R . . H13C H 0.8605 0.7492 0.6740 0.039 Uiso 1 1 calc R . . C14 C 0.48991(13) 1.02707(10) 0.20593(13) 0.0235(3) Uani 1 1 d . . . H14A H 0.5657 1.0472 0.2171 0.035 Uiso 1 1 calc R . . H14B H 0.4515 1.0681 0.2340 0.035 Uiso 1 1 calc R . . H14C H 0.4486 1.0207 0.1330 0.035 Uiso 1 1 calc R . . C15 C 0.42661(13) 0.77667(11) 0.40785(12) 0.0243(3) Uani 1 1 d . . . H15A H 0.4792 0.7757 0.4781 0.037 Uiso 1 1 calc R . . H15B H 0.4200 0.7196 0.3789 0.037 Uiso 1 1 calc R . . H15C H 0.3533 0.7957 0.4062 0.037 Uiso 1 1 calc R . . C16 C 0.87812(12) 0.86303(9) 0.21397(11) 0.0150(2) Uani 1 1 d . . . C17 C 0.94033(12) 0.78930(9) 0.25574(11) 0.0194(2) Uani 1 1 d . . . D17 H 0.9076 0.7469 0.2838 0.023 Uiso 1 1 calc R . . C18 C 1.04883(13) 0.77723(11) 0.25683(13) 0.0245(3) Uani 1 1 d . . . D18 H 1.0885 0.7271 0.2856 0.029 Uiso 1 1 calc R . . C19 C 1.09894(13) 0.83792(12) 0.21626(13) 0.0263(3) Uani 1 1 d . . . D19 H 1.1726 0.8299 0.2169 0.032 Uiso 1 1 calc R . . C20 C 1.03944(15) 0.91041(14) 0.17488(13) 0.0258(4) Uani 1 1 d . . . D20 H 1.0725 0.9523 0.1465 0.031 Uiso 1 1 calc R . . C21 C 0.93147(13) 0.92286(11) 0.17424(11) 0.0200(3) Uani 1 1 d . . . D21 H 0.8931 0.9736 0.1459 0.024 Uiso 1 1 calc R . . C22 C 0.71032(16) 0.88918(11) -0.03119(12) 0.0266(3) Uani 1 1 d . . . H22A H 0.6770 0.9244 -0.0917 0.040 Uiso 1 1 calc R . . H22B H 0.6945 0.8294 -0.0493 0.040 Uiso 1 1 calc R . . H22C H 0.7913 0.8981 -0.0036 0.040 Uiso 1 1 calc R . . C23 C 0.64676(14) 1.03276(10) 0.04469(12) 0.0244(3) Uani 1 1 d . . . H23A H 0.6080 1.0452 -0.0274 0.037 Uiso 1 1 calc R . . H23B H 0.7232 1.0549 0.0666 0.037 Uiso 1 1 calc R . . H23C H 0.6069 1.0596 0.0843 0.037 Uiso 1 1 calc R . . C24 C 0.50687(16) 0.88386(11) 0.00302(13) 0.0267(3) Uani 1 1 d . . . H24A H 0.4748 0.9106 -0.0638 0.040 Uiso 1 1 calc R . . H24B H 0.4634 0.9002 0.0447 0.040 Uiso 1 1 calc R . . H24C H 0.5049 0.8221 -0.0049 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01214(3) 0.01310(3) 0.01202(3) 0.00224(4) 0.00381(2) -0.00038(4) P1 0.01696(15) 0.01845(16) 0.01372(14) 0.00431(12) 0.00268(12) -0.00140(12) N1 0.0161(4) 0.0161(5) 0.0143(5) 0.0015(4) 0.0068(4) -0.0011(4) N2 0.0159(5) 0.0140(5) 0.0166(5) 0.0013(4) 0.0070(4) -0.0017(4) N3 0.0137(4) 0.0179(5) 0.0128(4) 0.0017(4) 0.0046(4) -0.0023(4) N4 0.0144(4) 0.0161(5) 0.0125(4) 0.0020(4) 0.0045(4) -0.0002(4) N5 0.0145(5) 0.0174(5) 0.0155(5) 0.0007(4) 0.0051(4) 0.0007(4) N6 0.0128(4) 0.0178(5) 0.0150(5) 0.0002(4) 0.0059(4) -0.0008(4) B1 0.0156(6) 0.0157(6) 0.0150(6) 0.0018(5) 0.0070(5) -0.0007(5) C1 0.0156(5) 0.0165(5) 0.0172(5) -0.0008(4) 0.0070(4) -0.0013(4) C2 0.0171(6) 0.0148(5) 0.0222(7) -0.0002(4) 0.0080(6) 0.0004(4) C3 0.0153(5) 0.0144(5) 0.0210(6) 0.0020(4) 0.0071(5) -0.0016(4) C4 0.0139(5) 0.0202(6) 0.0149(5) -0.0006(4) 0.0051(4) -0.0017(4) C5 0.0160(5) 0.0235(6) 0.0136(5) 0.0008(5) 0.0029(4) 0.0001(5) C6 0.0173(5) 0.0191(6) 0.0128(5) 0.0027(4) 0.0050(4) 0.0022(4) C7 0.0149(6) 0.0200(6) 0.0163(6) -0.0022(5) 0.0028(5) 0.0014(5) C8 0.0143(6) 0.0250(7) 0.0186(6) -0.0038(6) 0.0054(5) 0.0020(5) C9 0.0133(5) 0.0227(6) 0.0153(5) -0.0039(5) 0.0061(4) -0.0025(4) C10 0.0300(7) 0.0229(7) 0.0198(6) -0.0019(5) 0.0128(6) -0.0005(6) C11 0.0308(7) 0.0164(6) 0.0263(7) 0.0038(5) 0.0146(6) -0.0024(5) C12 0.0208(6) 0.0282(7) 0.0194(6) -0.0006(5) 0.0053(5) -0.0098(5) C13 0.0300(8) 0.0316(8) 0.0157(6) 0.0081(6) 0.0069(6) -0.0018(6) C14 0.0211(6) 0.0215(7) 0.0262(7) 0.0031(5) 0.0065(6) 0.0061(5) C15 0.0202(6) 0.0325(8) 0.0249(7) 0.0015(6) 0.0136(6) -0.0009(6) C16 0.0149(5) 0.0176(6) 0.0128(6) 0.0003(5) 0.0053(5) -0.0013(4) C17 0.0170(6) 0.0194(6) 0.0205(6) 0.0008(5) 0.0053(5) -0.0002(5) C18 0.0166(6) 0.0264(7) 0.0289(7) -0.0032(6) 0.0061(5) 0.0034(5) C19 0.0170(6) 0.0387(9) 0.0254(7) -0.0089(7) 0.0101(6) -0.0029(6) C20 0.0210(7) 0.0365(10) 0.0219(8) 0.0000(7) 0.0100(6) -0.0100(7) C21 0.0188(6) 0.0251(7) 0.0159(6) 0.0029(5) 0.0062(5) -0.0032(5) C22 0.0319(8) 0.0318(8) 0.0161(6) 0.0038(6) 0.0086(6) -0.0012(6) C23 0.0255(7) 0.0211(7) 0.0237(7) 0.0097(5) 0.0054(6) 0.0006(5) C24 0.0200(7) 0.0335(9) 0.0206(7) 0.0057(6) 0.0002(6) -0.0051(6) _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 D1 1.44(2) . ? Rh1 C16 2.0171(15) . ? Rh1 N3 2.1112(12) . ? Rh1 N5 2.2112(13) . ? Rh1 N1 2.2421(12) . ? Rh1 P1 2.2524(4) . ? P1 C24 1.8194(18) . ? P1 C23 1.8239(16) . ? P1 C22 1.8333(17) . ? N1 C1 1.3402(18) . ? N1 N2 1.3708(16) . ? N2 C3 1.3473(17) . ? N2 B1 1.5344(19) . ? N3 C4 1.3407(19) . ? N3 N4 1.3660(16) . ? N4 C6 1.3511(17) . ? N4 B1 1.5377(19) . ? N5 C7 1.331(2) . ? N5 N6 1.3737(17) . ? N6 C9 1.3559(17) . ? N6 B1 1.5404(19) . ? B1 H1B 1.077(19) . ? C1 C2 1.399(2) . ? C1 C10 1.484(2) . ? C2 C3 1.384(2) . ? C2 H2 0.9500 . ? C3 C11 1.497(2) . ? C4 C5 1.403(2) . ? C4 C12 1.489(2) . ? C5 C6 1.379(2) . ? C5 H5 0.9500 . ? C6 C13 1.490(2) . ? C7 C8 1.402(2) . ? C7 C14 1.499(2) . ? C8 C9 1.385(2) . ? C8 H8 0.9500 . ? C9 C15 1.493(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.397(2) . ? C16 C17 1.415(2) . ? C17 C18 1.400(2) . ? C17 D17 0.9500 . ? C18 C19 1.387(2) . ? C18 D18 0.9500 . ? C19 C20 1.383(3) . ? C19 D19 0.9500 . ? C20 C21 1.396(2) . ? C20 D20 0.9500 . ? C21 D21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 D1 Rh1 C16 85.2(8) . . ? D1 Rh1 N3 89.0(8) . . ? C16 Rh1 N3 88.19(5) . . ? D1 Rh1 N5 95.5(8) . . ? C16 Rh1 N5 170.63(5) . . ? N3 Rh1 N5 82.48(5) . . ? D1 Rh1 N1 176.8(8) . . ? C16 Rh1 N1 92.72(5) . . ? N3 Rh1 N1 88.53(4) . . ? N5 Rh1 N1 86.15(4) . . ? D1 Rh1 P1 82.3(8) . . ? C16 Rh1 P1 91.06(4) . . ? N3 Rh1 P1 171.29(3) . . ? N5 Rh1 P1 98.30(4) . . ? N1 Rh1 P1 100.17(3) . . ? C24 P1 C23 104.82(8) . . ? C24 P1 C22 101.16(9) . . ? C23 P1 C22 97.69(8) . . ? C24 P1 Rh1 113.49(6) . . ? C23 P1 Rh1 114.73(5) . . ? C22 P1 Rh1 122.39(6) . . ? C1 N1 N2 106.31(11) . . ? C1 N1 Rh1 135.38(9) . . ? N2 N1 Rh1 114.66(8) . . ? C3 N2 N1 110.47(11) . . ? C3 N2 B1 128.45(12) . . ? N1 N2 B1 120.80(11) . . ? C4 N3 N4 107.14(11) . . ? C4 N3 Rh1 133.35(9) . . ? N4 N3 Rh1 119.51(8) . . ? C6 N4 N3 109.80(11) . . ? C6 N4 B1 130.82(12) . . ? N3 N4 B1 119.39(11) . . ? C7 N5 N6 106.93(12) . . ? C7 N5 Rh1 137.74(10) . . ? N6 N5 Rh1 115.27(9) . . ? C9 N6 N5 109.73(11) . . ? C9 N6 B1 127.80(12) . . ? N5 N6 B1 120.92(11) . . ? N2 B1 N4 108.58(11) . . ? N2 B1 N6 111.14(11) . . ? N4 B1 N6 108.95(11) . . ? N2 B1 H1B 109.8(11) . . ? N4 B1 H1B 109.8(10) . . ? N6 B1 H1B 108.5(11) . . ? N1 C1 C2 109.94(12) . . ? N1 C1 C10 123.83(13) . . ? C2 C1 C10 126.23(13) . . ? C3 C2 C1 105.77(12) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N2 C3 C2 107.49(12) . . ? N2 C3 C11 123.19(13) . . ? C2 C3 C11 129.30(13) . . ? N3 C4 C5 109.34(12) . . ? N3 C4 C12 122.99(13) . . ? C5 C4 C12 127.67(13) . . ? C6 C5 C4 105.75(12) . . ? C6 C5 H5 127.1 . . ? C4 C5 H5 127.1 . . ? N4 C6 C5 107.96(12) . . ? N4 C6 C13 123.17(13) . . ? C5 C6 C13 128.86(13) . . ? N5 C7 C8 110.08(14) . . ? N5 C7 C14 122.74(14) . . ? C8 C7 C14 127.09(14) . . ? C9 C8 C7 105.57(13) . . ? C9 C8 H8 127.2 . . ? C7 C8 H8 127.2 . . ? N6 C9 C8 107.67(12) . . ? N6 C9 C15 123.61(13) . . ? C8 C9 C15 128.72(13) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 116.07(13) . . ? C21 C16 Rh1 125.78(12) . . ? C17 C16 Rh1 117.93(11) . . ? C18 C17 C16 121.76(14) . . ? C18 C17 D17 119.1 . . ? C16 C17 D17 119.1 . . ? C19 C18 C17 120.55(15) . . ? C19 C18 D18 119.7 . . ? C17 C18 D18 119.7 . . ? C20 C19 C18 118.60(14) . . ? C20 C19 D19 120.7 . . ? C18 C19 D19 120.7 . . ? C19 C20 C21 120.98(16) . . ? C19 C20 D20 119.5 . . ? C21 C20 D20 119.5 . . ? C20 C21 C16 122.04(16) . . ? C20 C21 D21 119.0 . . ? C16 C21 D21 119.0 . . ? P1 C22 H22A 109.5 . . ? P1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P1 C24 H24A 109.5 . . ? P1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag D1 Rh1 P1 C24 -129.6(8) . . . . ? C16 Rh1 P1 C24 145.39(8) . . . . ? N3 Rh1 P1 C24 -129.6(2) . . . . ? N5 Rh1 P1 C24 -35.11(8) . . . . ? N1 Rh1 P1 C24 52.44(8) . . . . ? D1 Rh1 P1 C23 -9.1(8) . . . . ? C16 Rh1 P1 C23 -94.12(7) . . . . ? N3 Rh1 P1 C23 -9.1(2) . . . . ? N5 Rh1 P1 C23 85.37(7) . . . . ? N1 Rh1 P1 C23 172.92(7) . . . . ? D1 Rh1 P1 C22 108.7(8) . . . . ? C16 Rh1 P1 C22 23.69(8) . . . . ? N3 Rh1 P1 C22 108.7(2) . . . . ? N5 Rh1 P1 C22 -156.81(8) . . . . ? N1 Rh1 P1 C22 -69.26(8) . . . . ? D1 Rh1 N1 C1 -84(15) . . . . ? C16 Rh1 N1 C1 -34.49(14) . . . . ? N3 Rh1 N1 C1 -122.61(13) . . . . ? N5 Rh1 N1 C1 154.83(14) . . . . ? P1 Rh1 N1 C1 57.08(13) . . . . ? D1 Rh1 N1 N2 71(15) . . . . ? C16 Rh1 N1 N2 120.37(9) . . . . ? N3 Rh1 N1 N2 32.25(9) . . . . ? N5 Rh1 N1 N2 -50.31(9) . . . . ? P1 Rh1 N1 N2 -148.06(8) . . . . ? C1 N1 N2 C3 1.36(15) . . . . ? Rh1 N1 N2 C3 -160.53(9) . . . . ? C1 N1 N2 B1 175.82(11) . . . . ? Rh1 N1 N2 B1 13.93(14) . . . . ? D1 Rh1 N3 C4 -37.7(8) . . . . ? C16 Rh1 N3 C4 47.52(14) . . . . ? N5 Rh1 N3 C4 -133.40(14) . . . . ? N1 Rh1 N3 C4 140.29(14) . . . . ? P1 Rh1 N3 C4 -37.7(3) . . . . ? D1 Rh1 N3 N4 143.0(8) . . . . ? C16 Rh1 N3 N4 -131.73(10) . . . . ? N5 Rh1 N3 N4 47.36(10) . . . . ? N1 Rh1 N3 N4 -38.96(10) . . . . ? P1 Rh1 N3 N4 143.06(18) . . . . ? C4 N3 N4 C6 -0.67(15) . . . . ? Rh1 N3 N4 C6 178.76(9) . . . . ? C4 N3 N4 B1 179.27(12) . . . . ? Rh1 N3 N4 B1 -1.31(15) . . . . ? D1 Rh1 N5 C7 36.1(8) . . . . ? C16 Rh1 N5 C7 130.0(3) . . . . ? N3 Rh1 N5 C7 124.39(16) . . . . ? N1 Rh1 N5 C7 -146.59(16) . . . . ? P1 Rh1 N5 C7 -46.85(16) . . . . ? D1 Rh1 N5 N6 -140.6(8) . . . . ? C16 Rh1 N5 N6 -46.7(4) . . . . ? N3 Rh1 N5 N6 -52.33(10) . . . . ? N1 Rh1 N5 N6 36.69(10) . . . . ? P1 Rh1 N5 N6 136.43(10) . . . . ? C7 N5 N6 C9 0.91(16) . . . . ? Rh1 N5 N6 C9 178.61(9) . . . . ? C7 N5 N6 B1 -165.92(12) . . . . ? Rh1 N5 N6 B1 11.77(16) . . . . ? C3 N2 B1 N4 104.15(15) . . . . ? N1 N2 B1 N4 -69.21(15) . . . . ? C3 N2 B1 N6 -136.02(14) . . . . ? N1 N2 B1 N6 50.61(16) . . . . ? C6 N4 B1 N2 -118.17(15) . . . . ? N3 N4 B1 N2 61.91(15) . . . . ? C6 N4 B1 N6 120.65(15) . . . . ? N3 N4 B1 N6 -59.27(15) . . . . ? C9 N6 B1 N2 127.67(14) . . . . ? N5 N6 B1 N2 -68.07(16) . . . . ? C9 N6 B1 N4 -112.72(14) . . . . ? N5 N6 B1 N4 51.54(16) . . . . ? N2 N1 C1 C2 -1.21(15) . . . . ? Rh1 N1 C1 C2 155.07(10) . . . . ? N2 N1 C1 C10 178.33(13) . . . . ? Rh1 N1 C1 C10 -25.4(2) . . . . ? N1 C1 C2 C3 0.65(16) . . . . ? C10 C1 C2 C3 -178.88(14) . . . . ? N1 N2 C3 C2 -0.96(16) . . . . ? B1 N2 C3 C2 -174.89(13) . . . . ? N1 N2 C3 C11 177.59(13) . . . . ? B1 N2 C3 C11 3.7(2) . . . . ? C1 C2 C3 N2 0.20(15) . . . . ? C1 C2 C3 C11 -178.24(15) . . . . ? N4 N3 C4 C5 0.91(16) . . . . ? Rh1 N3 C4 C5 -178.41(10) . . . . ? N4 N3 C4 C12 -178.72(14) . . . . ? Rh1 N3 C4 C12 2.0(2) . . . . ? N3 C4 C5 C6 -0.81(17) . . . . ? C12 C4 C5 C6 178.80(15) . . . . ? N3 N4 C6 C5 0.16(16) . . . . ? B1 N4 C6 C5 -179.76(13) . . . . ? N3 N4 C6 C13 178.82(13) . . . . ? B1 N4 C6 C13 -1.1(2) . . . . ? C4 C5 C6 N4 0.38(16) . . . . ? C4 C5 C6 C13 -178.18(15) . . . . ? N6 N5 C7 C8 -1.27(17) . . . . ? Rh1 N5 C7 C8 -178.17(12) . . . . ? N6 N5 C7 C14 175.62(13) . . . . ? Rh1 N5 C7 C14 -1.3(2) . . . . ? N5 C7 C8 C9 1.15(18) . . . . ? C14 C7 C8 C9 -175.57(15) . . . . ? N5 N6 C9 C8 -0.20(16) . . . . ? B1 N6 C9 C8 165.49(13) . . . . ? N5 N6 C9 C15 -179.94(13) . . . . ? B1 N6 C9 C15 -14.3(2) . . . . ? C7 C8 C9 N6 -0.56(17) . . . . ? C7 C8 C9 C15 179.17(14) . . . . ? D1 Rh1 C16 C21 -31.9(8) . . . . ? N3 Rh1 C16 C21 -121.03(13) . . . . ? N5 Rh1 C16 C21 -126.6(3) . . . . ? N1 Rh1 C16 C21 150.53(13) . . . . ? P1 Rh1 C16 C21 50.29(13) . . . . ? D1 Rh1 C16 C17 142.4(8) . . . . ? N3 Rh1 C16 C17 53.26(11) . . . . ? N5 Rh1 C16 C17 47.7(4) . . . . ? N1 Rh1 C16 C17 -35.18(11) . . . . ? P1 Rh1 C16 C17 -135.42(11) . . . . ? C21 C16 C17 C18 -0.1(2) . . . . ? Rh1 C16 C17 C18 -174.97(12) . . . . ? C16 C17 C18 C19 -0.1(2) . . . . ? C17 C18 C19 C20 0.0(2) . . . . ? C18 C19 C20 C21 0.4(3) . . . . ? C19 C20 C21 C16 -0.7(3) . . . . ? C17 C16 C21 C20 0.5(2) . . . . ? Rh1 C16 C21 C20 174.92(13) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 37.78 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.073 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.075 #===end data_jontt02_cmpd3a _database_code_depnum_ccdc_archive 'CCDC 770111' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt02 _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 B F5 N6 P Rh, 0.5(C6 H14)' _chemical_formula_sum 'C27 H39 B F5 N6 P Rh' _chemical_formula_weight 687.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6504(13) _cell_length_b 33.930(5) _cell_length_c 20.878(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.671(2) _cell_angle_gamma 90.00 _cell_volume 6021.8(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3865 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 23.89 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8760 _exptl_absorpt_correction_T_max 0.9604 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74170 _diffrn_reflns_av_R_equivalents 0.1197 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12307 _reflns_number_gt 7797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The rhodium and boron hydride atoms were found from the difference Fourier map and their positions were refined independently from their respective bonded heavier atoms. They were given relative isotropic displacement parameters, Uiso[H] = 2*Ueq[Rh] and Uiso[H] = 1.2*Ueq[B]. ; _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^)+(0.0667P)^2^+31.6948P] 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 12307 _refine_ls_number_parameters 787 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.1300 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.1985 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _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 0.85876(7) 0.398198(17) 0.16340(3) 0.03623(17) Uani 1 1 d . . . H1 H 0.717(10) 0.357(3) 0.143(4) 0.072 Uiso 1 1 d . . . N1 N 1.0274(7) 0.44624(18) 0.1922(3) 0.0404(15) Uani 1 1 d . . . N2 N 1.1182(7) 0.44240(18) 0.2533(3) 0.0424(15) Uani 1 1 d . . . N3 N 0.7897(7) 0.40554(17) 0.2539(3) 0.0385(14) Uani 1 1 d . . . N4 N 0.9077(7) 0.41148(18) 0.3062(3) 0.0404(15) Uani 1 1 d . . . N5 N 1.0108(7) 0.35539(18) 0.2172(3) 0.0389(15) Uani 1 1 d . . . N6 N 1.1112(7) 0.36893(18) 0.2720(3) 0.0390(14) Uani 1 1 d . . . B1 B 1.0819(11) 0.4099(3) 0.2993(5) 0.045(2) Uani 1 1 d . . . H1B H 1.161(9) 0.411(2) 0.347(4) 0.054 Uiso 1 1 d . . . C1 C 1.0704(10) 0.4802(2) 0.1682(4) 0.0444(19) Uani 1 1 d . . . C2 C 1.1932(10) 0.4973(3) 0.2118(5) 0.055(2) Uani 1 1 d . . . H2A H 1.2489 0.5207 0.2056 0.066 Uiso 1 1 calc R . . C3 C 1.2171(9) 0.4733(2) 0.2654(4) 0.047(2) Uani 1 1 d . . . C4 C 0.6523(10) 0.4058(2) 0.2751(4) 0.0440(19) Uani 1 1 d . . . C5 C 0.6844(10) 0.4119(2) 0.3420(4) 0.0454(19) Uani 1 1 d . . . H5A H 0.6093 0.4132 0.3699 0.054 Uiso 1 1 calc R . . C6 C 0.8427(10) 0.4155(2) 0.3602(4) 0.0449(19) Uani 1 1 d . . . C7 C 1.0365(10) 0.3168(2) 0.2133(4) 0.0449(19) Uani 1 1 d . . . C8 C 1.1557(9) 0.3059(2) 0.2654(4) 0.047(2) Uani 1 1 d . . . H8A H 1.1987 0.2803 0.2738 0.057 Uiso 1 1 calc R . . C9 C 1.1982(9) 0.3384(2) 0.3012(4) 0.0440(19) Uani 1 1 d . . . C10 C 0.9861(11) 0.4983(3) 0.1064(4) 0.058(2) Uani 1 1 d . . . H10A H 0.9061 0.4800 0.0844 0.088 Uiso 1 1 calc R . . H10B H 1.0614 0.5041 0.0779 0.088 Uiso 1 1 calc R . . H10C H 0.9353 0.5228 0.1164 0.088 Uiso 1 1 calc R . . C11 C 1.3304(12) 0.4783(3) 0.3278(5) 0.068(3) Uani 1 1 d . . . H11A H 1.3896 0.4537 0.3384 0.102 Uiso 1 1 calc R . . H11B H 1.2728 0.4845 0.3628 0.102 Uiso 1 1 calc R . . H11C H 1.4034 0.4997 0.3234 0.102 Uiso 1 1 calc R . . C12 C 0.5010(9) 0.3996(3) 0.2297(4) 0.050(2) Uani 1 1 d . . . H12A H 0.5199 0.3854 0.1911 0.074 Uiso 1 1 calc R . . H12B H 0.4528 0.4252 0.2166 0.074 Uiso 1 1 calc R . . H12C H 0.4302 0.3842 0.2515 0.074 Uiso 1 1 calc R . . C13 C 0.9402(11) 0.4214(3) 0.4260(4) 0.057(2) Uani 1 1 d . . . H13A H 1.0176 0.4001 0.4352 0.086 Uiso 1 1 calc R . . H13B H 0.8724 0.4212 0.4587 0.086 Uiso 1 1 calc R . . H13C H 0.9949 0.4467 0.4274 0.086 Uiso 1 1 calc R . . C14 C 0.9439(12) 0.2896(3) 0.1643(4) 0.063(3) Uani 1 1 d . . . H14A H 0.8429 0.3019 0.1458 0.095 Uiso 1 1 calc R . . H14B H 0.9251 0.2648 0.1855 0.095 Uiso 1 1 calc R . . H14C H 1.0029 0.2844 0.1294 0.095 Uiso 1 1 calc R . . C15 C 1.3149(10) 0.3433(3) 0.3632(4) 0.055(2) Uani 1 1 d . . . H15A H 1.3798 0.3195 0.3714 0.082 Uiso 1 1 calc R . . H15B H 1.2590 0.3475 0.3994 0.082 Uiso 1 1 calc R . . H15C H 1.3823 0.3660 0.3594 0.082 Uiso 1 1 calc R . . C16 C 0.6884(9) 0.4372(2) 0.1225(4) 0.0379(17) Uani 1 1 d . . . C17 C 0.5787(9) 0.4309(2) 0.0673(4) 0.0448(19) Uani 1 1 d . . . F1 F 0.5886(6) 0.39793(14) 0.0311(2) 0.0578(13) Uani 1 1 d . . . C18 C 0.4573(10) 0.4556(3) 0.0437(4) 0.054(2) Uani 1 1 d . . . F2 F 0.3556(6) 0.44662(16) -0.0119(3) 0.0716(16) Uani 1 1 d . . . C19 C 0.4389(10) 0.4897(3) 0.0763(5) 0.053(2) Uani 1 1 d . . . F3 F 0.3187(6) 0.51485(16) 0.0528(3) 0.0734(16) Uani 1 1 d . . . C20 C 0.5423(10) 0.4978(2) 0.1305(4) 0.046(2) Uani 1 1 d . . . F4 F 0.5233(6) 0.53176(14) 0.1644(3) 0.0669(15) Uani 1 1 d . . . C21 C 0.6637(9) 0.4726(2) 0.1547(4) 0.0451(19) Uani 1 1 d . . . F5 F 0.7555(5) 0.48379(13) 0.2097(2) 0.0506(11) Uani 1 1 d . . . P1 P 0.9542(3) 0.38530(6) 0.07159(10) 0.0426(5) Uani 1 1 d . . . C22 C 1.1660(11) 0.3771(3) 0.0926(5) 0.072(3) Uani 1 1 d . . . H22A H 1.2087 0.3738 0.0526 0.108 Uiso 1 1 calc R . . H22B H 1.1868 0.3533 0.1194 0.108 Uiso 1 1 calc R . . H22C H 1.2162 0.3998 0.1170 0.108 Uiso 1 1 calc R . . C23 C 0.8829(13) 0.3437(3) 0.0224(4) 0.068(3) Uani 1 1 d . . . H23A H 0.9525 0.3385 -0.0087 0.102 Uiso 1 1 calc R . . H23B H 0.7764 0.3492 -0.0014 0.102 Uiso 1 1 calc R . . H23C H 0.8805 0.3206 0.0504 0.102 Uiso 1 1 calc R . . C24 C 0.9507(12) 0.4214(3) 0.0082(4) 0.058(2) Uani 1 1 d . . . H24A H 0.9977 0.4101 -0.0269 0.087 Uiso 1 1 calc R . . H24B H 1.0108 0.4446 0.0261 0.087 Uiso 1 1 calc R . . H24C H 0.8416 0.4290 -0.0090 0.087 Uiso 1 1 calc R . . Rh2 Rh 0.38183(7) 0.192684(18) 0.27248(3) 0.04144(18) Uani 1 1 d . . . H2 H 0.217(11) 0.208(3) 0.230(4) 0.083 Uiso 1 1 d . . . N7 N 0.5056(7) 0.24628(19) 0.2742(3) 0.0417(15) Uani 1 1 d . . . N8 N 0.6056(7) 0.25591(18) 0.3312(3) 0.0426(15) Uani 1 1 d . . . N9 N 0.5944(7) 0.16711(18) 0.3384(3) 0.0412(15) Uani 1 1 d . . . N10 N 0.6575(7) 0.19094(18) 0.3896(3) 0.0415(15) Uani 1 1 d . . . N11 N 0.3105(7) 0.21670(19) 0.3569(3) 0.0432(16) Uani 1 1 d . . . N12 N 0.4280(8) 0.23252(18) 0.4044(3) 0.0440(16) Uani 1 1 d . . . B2 B 0.5999(11) 0.2331(3) 0.3943(5) 0.045(2) Uani 1 1 d . . . H2B H 0.678(9) 0.247(2) 0.438(4) 0.053 Uiso 1 1 d . . . C25 C 0.5234(10) 0.2729(2) 0.2305(4) 0.046(2) Uani 1 1 d . . . C26 C 0.6381(11) 0.3003(2) 0.2574(4) 0.053(2) Uani 1 1 d . . . H26A H 0.6755 0.3221 0.2363 0.064 Uiso 1 1 calc R . . C27 C 0.6851(10) 0.2887(2) 0.3213(4) 0.048(2) Uani 1 1 d . . . C28 C 0.6756(9) 0.1339(2) 0.3459(4) 0.0431(19) Uani 1 1 d . . . C29 C 0.7892(9) 0.1357(2) 0.4024(4) 0.0436(19) Uani 1 1 d . . . H29A H 0.8620 0.1156 0.4192 0.052 Uiso 1 1 calc R . . C30 C 0.7757(9) 0.1716(2) 0.4287(4) 0.0428(19) Uani 1 1 d . . . C31 C 0.1756(10) 0.2278(2) 0.3736(4) 0.046(2) Uani 1 1 d . . . C32 C 0.2032(10) 0.2486(2) 0.4319(4) 0.0465(19) Uani 1 1 d . . . H32A H 0.1270 0.2588 0.4549 0.056 Uiso 1 1 calc R . . C33 C 0.3646(10) 0.2513(2) 0.4494(4) 0.0456(19) Uani 1 1 d . . . C34 C 0.4309(11) 0.2736(3) 0.1624(4) 0.057(2) Uani 1 1 d . . . H34A H 0.3274 0.2617 0.1618 0.086 Uiso 1 1 calc R . . H34B H 0.4871 0.2587 0.1337 0.086 Uiso 1 1 calc R . . H34C H 0.4176 0.3010 0.1472 0.086 Uiso 1 1 calc R . . C35 C 0.8034(10) 0.3084(3) 0.3735(4) 0.056(2) Uani 1 1 d . . . H35A H 0.8602 0.2884 0.4025 0.084 Uiso 1 1 calc R . . H35B H 0.7488 0.3263 0.3987 0.084 Uiso 1 1 calc R . . H35C H 0.8781 0.3235 0.3531 0.084 Uiso 1 1 calc R . . C36 C 0.6521(10) 0.1008(3) 0.2981(4) 0.056(2) Uani 1 1 d . . . H36A H 0.6261 0.1115 0.2538 0.084 Uiso 1 1 calc R . . H36B H 0.5658 0.0840 0.3064 0.084 Uiso 1 1 calc R . . H36C H 0.7488 0.0853 0.3026 0.084 Uiso 1 1 calc R . . C37 C 0.8690(9) 0.1902(3) 0.4888(4) 0.052(2) Uani 1 1 d . . . H37A H 0.7980 0.1982 0.5179 0.077 Uiso 1 1 calc R . . H37B H 0.9244 0.2134 0.4765 0.077 Uiso 1 1 calc R . . H37C H 0.9457 0.1711 0.5111 0.077 Uiso 1 1 calc R . . C38 C 0.0204(10) 0.2187(3) 0.3319(4) 0.057(2) Uani 1 1 d . . . H38A H 0.0350 0.2132 0.2873 0.085 Uiso 1 1 calc R . . H38B H -0.0503 0.2413 0.3316 0.085 Uiso 1 1 calc R . . H38C H -0.0255 0.1955 0.3493 0.085 Uiso 1 1 calc R . . C39 C 0.4605(11) 0.2713(3) 0.5065(4) 0.055(2) Uani 1 1 d . . . H39A H 0.5363 0.2526 0.5304 0.083 Uiso 1 1 calc R . . H39B H 0.3914 0.2810 0.5354 0.083 Uiso 1 1 calc R . . H39C H 0.5170 0.2935 0.4916 0.083 Uiso 1 1 calc R . . C40 C 0.4533(10) 0.1796(2) 0.1860(4) 0.047(2) Uani 1 1 d . . . C41 C 0.3467(11) 0.1723(3) 0.1292(4) 0.053(2) Uani 1 1 d . . . F6 F 0.1861(6) 0.17058(16) 0.1278(2) 0.0603(13) Uani 1 1 d . . . C42 C 0.3918(12) 0.1677(3) 0.0700(4) 0.059(2) Uani 1 1 d . . . F7 F 0.2818(7) 0.1594(2) 0.0155(3) 0.0886(19) Uani 1 1 d . . . C43 C 0.5455(12) 0.1700(3) 0.0654(4) 0.061(2) Uani 1 1 d . . . F8 F 0.5914(8) 0.1661(2) 0.0077(3) 0.0878(19) Uani 1 1 d . . . C44 C 0.6515(12) 0.1781(3) 0.1212(5) 0.063(3) Uani 1 1 d . . . F9 F 0.8054(7) 0.18156(19) 0.1177(3) 0.0794(17) Uani 1 1 d . . . C45 C 0.5990(11) 0.1823(2) 0.1781(4) 0.046(2) Uani 1 1 d . . . F10 F 0.7189(6) 0.19075(15) 0.2306(2) 0.0605(13) Uani 1 1 d . . . P2 P 0.2377(3) 0.13644(7) 0.26828(11) 0.0498(5) Uani 1 1 d . . . C46 C 0.2614(13) 0.1136(3) 0.3469(5) 0.069(3) Uani 1 1 d . . . H46A H 0.1890 0.0912 0.3449 0.104 Uiso 1 1 calc R . . H46B H 0.2381 0.1328 0.3788 0.104 Uiso 1 1 calc R . . H46C H 0.3699 0.1043 0.3598 0.104 Uiso 1 1 calc R . . C47 C 0.0265(11) 0.1367(3) 0.2436(5) 0.071(3) Uani 1 1 d . . . H47A H -0.0117 0.1096 0.2365 0.106 Uiso 1 1 calc R . . H47B H -0.0025 0.1517 0.2030 0.106 Uiso 1 1 calc R . . H47C H -0.0211 0.1490 0.2778 0.106 Uiso 1 1 calc R . . C48 C 0.2763(11) 0.0974(3) 0.2124(5) 0.065(3) Uani 1 1 d . . . H48A H 0.2214 0.0733 0.2211 0.098 Uiso 1 1 calc R . . H48B H 0.3896 0.0923 0.2189 0.098 Uiso 1 1 calc R . . H48C H 0.2384 0.1058 0.1673 0.098 Uiso 1 1 calc R . . C49 C 0.931(8) 0.528(3) 0.346(4) 0.138(9) Uani 0.50 1 d PDU A 1 H49A H 0.9635 0.5385 0.3069 0.207 Uiso 0.50 1 calc PR A 1 H49B H 0.8996 0.5005 0.3391 0.207 Uiso 0.50 1 calc PR A 1 H49C H 1.0181 0.5302 0.3832 0.207 Uiso 0.50 1 calc PR A 1 C50 C 0.805(5) 0.5498(12) 0.3588(18) 0.145(9) Uani 0.50 1 d PDU A 1 H50A H 0.7160 0.5471 0.3215 0.174 Uiso 0.50 1 calc PR A 1 H50B H 0.8345 0.5780 0.3626 0.174 Uiso 0.50 1 calc PR A 1 C51 C 0.752(5) 0.5375(12) 0.4185(18) 0.168(10) Uani 0.50 1 d PDU A 1 H51A H 0.8395 0.5373 0.4563 0.202 Uiso 0.50 1 calc PR A 1 H51B H 0.7019 0.5111 0.4136 0.202 Uiso 0.50 1 calc PR A 1 C52 C 0.628(6) 0.5708(14) 0.425(3) 0.169(10) Uani 0.50 1 d PDU A 1 H52A H 0.6778 0.5965 0.4380 0.203 Uiso 0.50 1 calc PR A 1 H52B H 0.5464 0.5737 0.3853 0.203 Uiso 0.50 1 calc PR A 1 C53 C 0.569(5) 0.5510(13) 0.4789(17) 0.173(10) Uani 0.50 1 d PDU A 1 H53A H 0.5755 0.5221 0.4731 0.207 Uiso 0.50 1 calc PR A 1 H53B H 0.6380 0.5579 0.5206 0.207 Uiso 0.50 1 calc PR A 1 C54 C 0.418(5) 0.560(3) 0.483(3) 0.23(4) Uani 0.50 1 d PD A 1 H54A H 0.3899 0.5475 0.5217 0.349 Uiso 0.50 1 calc PR A 1 H54B H 0.3462 0.5512 0.4440 0.349 Uiso 0.50 1 calc PR A 1 H54C H 0.4080 0.5890 0.4872 0.349 Uiso 0.50 1 calc PR A 1 C49' C 0.947(8) 0.524(3) 0.356(4) 0.138(9) Uani 0.50 1 d PD B 5 H49D H 0.9525 0.4991 0.3336 0.207 Uiso 0.50 1 calc PR B 5 H49E H 1.0337 0.5261 0.3933 0.207 Uiso 0.50 1 calc PR B 5 H49F H 0.9547 0.5460 0.3257 0.207 Uiso 0.50 1 calc PR B 5 C50' C 0.806(5) 0.5268(9) 0.377(2) 0.145(9) Uani 0.50 1 d PD B 5 H50C H 0.8036 0.5065 0.4110 0.174 Uiso 0.50 1 calc PR B 5 H50D H 0.7193 0.5211 0.3403 0.174 Uiso 0.50 1 calc PR B 5 C51' C 0.778(5) 0.5661(11) 0.405(2) 0.168(10) Uani 0.50 1 d PD B 5 H51C H 0.7544 0.5866 0.3705 0.202 Uiso 0.50 1 calc PR B 5 H51D H 0.8671 0.5747 0.4387 0.202 Uiso 0.50 1 calc PR B 5 C52' C 0.629(6) 0.5543(13) 0.434(3) 0.169(10) Uani 0.50 1 d PD B 5 H52C H 0.5399 0.5468 0.3988 0.203 Uiso 0.50 1 calc PR B 5 H52D H 0.6527 0.5324 0.4652 0.203 Uiso 0.50 1 calc PR B 5 C53' C 0.599(5) 0.5911(11) 0.4654(19) 0.173(10) Uani 0.50 1 d PD B 5 H53C H 0.6920 0.5980 0.4985 0.207 Uiso 0.50 1 calc PR B 5 H53D H 0.5816 0.6125 0.4326 0.207 Uiso 0.50 1 calc PR B 5 C54' C 0.470(5) 0.589(3) 0.495(3) 0.23(4) Uani 0.50 1 d PD B 5 H54D H 0.4415 0.6150 0.5080 0.349 Uiso 0.50 1 calc PR B 5 H54E H 0.4942 0.5717 0.5335 0.349 Uiso 0.50 1 calc PR B 5 H54F H 0.3810 0.5774 0.4643 0.349 Uiso 0.50 1 calc PR B 5 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 0.0387(3) 0.0323(3) 0.0364(3) 0.0038(3) 0.0039(2) 0.0036(3) N1 0.043(4) 0.034(3) 0.047(4) 0.002(3) 0.015(3) 0.001(3) N2 0.039(4) 0.039(4) 0.047(4) 0.005(3) 0.003(3) -0.003(3) N3 0.037(4) 0.036(3) 0.039(3) 0.005(3) -0.001(3) 0.001(3) N4 0.041(4) 0.041(4) 0.039(4) 0.004(3) 0.004(3) -0.001(3) N5 0.047(4) 0.035(3) 0.034(3) 0.006(3) 0.007(3) 0.008(3) N6 0.032(3) 0.042(4) 0.044(4) 0.004(3) 0.009(3) 0.006(3) B1 0.035(5) 0.052(6) 0.044(5) 0.002(4) 0.000(4) 0.005(4) C1 0.052(5) 0.034(4) 0.052(5) 0.001(4) 0.019(4) -0.001(4) C2 0.045(5) 0.046(5) 0.078(7) -0.008(5) 0.020(5) -0.009(4) C3 0.042(5) 0.038(4) 0.061(5) 0.000(4) 0.009(4) 0.008(4) C4 0.049(5) 0.034(4) 0.048(5) -0.001(3) 0.007(4) 0.007(3) C5 0.052(5) 0.045(5) 0.039(4) 0.006(4) 0.007(4) 0.005(4) C6 0.048(5) 0.040(4) 0.046(5) 0.007(4) 0.005(4) 0.007(4) C7 0.053(5) 0.040(4) 0.042(5) 0.007(4) 0.010(4) 0.013(4) C8 0.049(5) 0.043(5) 0.052(5) 0.011(4) 0.017(4) 0.011(4) C9 0.043(5) 0.044(5) 0.044(5) 0.016(4) 0.008(4) 0.009(4) C10 0.082(7) 0.044(5) 0.051(5) 0.011(4) 0.018(5) -0.007(5) C11 0.067(6) 0.049(5) 0.085(7) -0.015(5) 0.005(5) -0.014(5) C12 0.039(5) 0.054(5) 0.054(5) 0.014(4) 0.006(4) 0.003(4) C13 0.070(6) 0.062(6) 0.036(5) 0.003(4) 0.001(4) 0.002(5) C14 0.082(7) 0.045(5) 0.058(6) -0.004(4) 0.001(5) 0.013(5) C15 0.050(5) 0.052(5) 0.059(6) 0.020(4) 0.001(4) 0.002(4) C16 0.042(4) 0.031(4) 0.040(4) 0.006(3) 0.007(3) 0.006(3) C17 0.044(5) 0.043(5) 0.045(5) 0.006(4) 0.002(4) 0.001(4) F1 0.058(3) 0.055(3) 0.053(3) 0.000(2) -0.011(2) -0.003(2) C18 0.049(5) 0.059(6) 0.052(5) 0.014(4) -0.001(4) -0.009(4) F2 0.060(3) 0.074(4) 0.069(4) 0.015(3) -0.018(3) -0.002(3) C19 0.040(5) 0.053(5) 0.068(6) 0.015(5) 0.009(4) 0.009(4) F3 0.050(3) 0.073(4) 0.093(4) 0.031(3) 0.004(3) 0.017(3) C20 0.047(5) 0.030(4) 0.062(5) 0.005(4) 0.013(4) -0.005(3) F4 0.061(3) 0.043(3) 0.097(4) 0.004(3) 0.015(3) 0.016(2) C21 0.038(4) 0.042(5) 0.055(5) 0.014(4) 0.007(4) 0.002(3) F5 0.051(3) 0.039(2) 0.058(3) -0.005(2) 0.002(2) 0.008(2) P1 0.0503(13) 0.0395(11) 0.0367(11) 0.0034(9) 0.0052(9) 0.0083(9) C22 0.063(6) 0.101(8) 0.053(6) 0.008(5) 0.012(5) 0.035(6) C23 0.113(9) 0.045(5) 0.047(5) -0.003(4) 0.019(5) 0.000(5) C24 0.080(7) 0.054(5) 0.042(5) 0.004(4) 0.011(5) 0.010(5) Rh2 0.0396(4) 0.0400(3) 0.0400(3) 0.0019(3) -0.0048(3) 0.0007(3) N7 0.036(4) 0.044(4) 0.040(4) 0.002(3) -0.005(3) 0.000(3) N8 0.045(4) 0.036(3) 0.044(4) 0.003(3) 0.000(3) -0.002(3) N9 0.040(4) 0.039(4) 0.042(4) -0.001(3) 0.000(3) 0.001(3) N10 0.038(4) 0.042(4) 0.038(4) 0.006(3) -0.009(3) -0.004(3) N11 0.039(4) 0.043(4) 0.042(4) 0.004(3) -0.005(3) -0.008(3) N12 0.048(4) 0.035(3) 0.045(4) 0.006(3) -0.001(3) -0.002(3) B2 0.047(6) 0.044(5) 0.039(5) -0.001(4) -0.002(4) 0.000(4) C25 0.052(5) 0.043(5) 0.044(5) 0.005(4) 0.010(4) 0.005(4) C26 0.065(6) 0.037(5) 0.058(5) 0.014(4) 0.012(4) 0.000(4) C27 0.049(5) 0.047(5) 0.049(5) 0.009(4) 0.010(4) 0.005(4) C28 0.043(5) 0.037(4) 0.048(5) 0.009(4) 0.007(4) 0.004(3) C29 0.043(5) 0.041(4) 0.044(5) 0.009(4) -0.001(4) 0.003(3) C30 0.035(4) 0.051(5) 0.039(4) 0.012(4) -0.003(3) -0.002(3) C31 0.043(5) 0.032(4) 0.060(5) 0.007(4) 0.002(4) 0.001(3) C32 0.043(5) 0.040(4) 0.056(5) 0.006(4) 0.008(4) -0.002(4) C33 0.051(5) 0.031(4) 0.053(5) 0.003(4) 0.007(4) 0.000(4) C34 0.071(6) 0.059(6) 0.042(5) 0.015(4) 0.008(4) 0.014(5) C35 0.061(6) 0.043(5) 0.062(6) 0.003(4) 0.005(4) -0.006(4) C36 0.054(5) 0.047(5) 0.061(6) 0.001(4) -0.004(4) 0.004(4) C37 0.038(5) 0.066(6) 0.046(5) 0.002(4) -0.005(4) -0.005(4) C38 0.057(6) 0.061(6) 0.049(5) -0.001(4) 0.002(4) -0.007(4) C39 0.063(6) 0.053(5) 0.045(5) -0.006(4) -0.001(4) 0.004(4) C40 0.051(5) 0.036(4) 0.045(5) 0.012(4) -0.017(4) -0.006(4) C41 0.056(6) 0.055(5) 0.045(5) 0.003(4) 0.000(4) 0.000(4) F6 0.050(3) 0.080(4) 0.044(3) 0.004(2) -0.010(2) -0.004(3) C42 0.065(6) 0.081(7) 0.027(4) -0.003(4) -0.005(4) 0.000(5) F7 0.093(5) 0.123(5) 0.043(3) -0.010(3) -0.005(3) 0.003(4) C43 0.070(7) 0.074(7) 0.040(5) -0.002(4) 0.010(5) 0.006(5) F8 0.102(5) 0.114(5) 0.050(3) -0.002(3) 0.020(3) 0.007(4) C44 0.061(6) 0.070(6) 0.061(6) 0.003(5) 0.015(5) 0.000(5) F9 0.061(4) 0.109(5) 0.072(4) 0.010(3) 0.024(3) 0.006(3) C45 0.062(6) 0.042(5) 0.037(4) 0.004(3) 0.013(4) 0.002(4) F10 0.047(3) 0.072(3) 0.059(3) 0.003(3) 0.000(2) -0.003(2) P2 0.0496(13) 0.0451(12) 0.0515(13) 0.0005(10) 0.0013(10) -0.0061(10) C46 0.087(8) 0.056(6) 0.064(6) 0.009(5) 0.010(5) -0.022(5) C47 0.061(6) 0.066(6) 0.082(7) -0.010(5) 0.007(5) -0.014(5) C48 0.064(6) 0.052(5) 0.072(6) -0.005(5) -0.005(5) -0.009(5) C49 0.176(19) 0.111(18) 0.13(2) 0.035(16) 0.036(16) 0.016(13) C50 0.17(2) 0.13(2) 0.13(2) 0.032(17) 0.037(17) 0.024(19) C51 0.198(19) 0.21(3) 0.095(14) -0.032(18) 0.024(12) 0.00(2) C52 0.204(18) 0.21(3) 0.091(13) -0.033(17) 0.022(11) -0.006(19) C53 0.202(19) 0.21(3) 0.101(14) -0.020(18) 0.021(13) -0.01(2) C54 0.17(3) 0.43(13) 0.09(2) -0.06(4) 0.01(3) 0.02(4) C49' 0.176(19) 0.111(18) 0.13(2) 0.035(16) 0.036(16) 0.016(13) C50' 0.17(2) 0.13(2) 0.13(2) 0.032(17) 0.037(17) 0.024(19) C51' 0.198(19) 0.21(3) 0.095(14) -0.032(18) 0.024(12) 0.00(2) C52' 0.204(18) 0.21(3) 0.091(13) -0.033(17) 0.022(11) -0.006(19) C53' 0.202(19) 0.21(3) 0.101(14) -0.020(18) 0.021(13) -0.01(2) C54' 0.17(3) 0.43(13) 0.09(2) -0.06(4) 0.01(3) 0.02(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 C16 2.046(7) . ? Rh1 N3 2.099(6) . ? Rh1 N5 2.134(6) . ? Rh1 N1 2.196(6) . ? Rh1 P1 2.266(2) . ? Rh1 H1 1.87(9) . ? N1 C1 1.336(9) . ? N1 N2 1.374(8) . ? N2 C3 1.347(10) . ? N2 B1 1.533(11) . ? N3 C4 1.343(10) . ? N3 N4 1.365(8) . ? N4 C6 1.356(10) . ? N4 B1 1.540(11) . ? N5 C7 1.332(9) . ? N5 N6 1.382(8) . ? N6 C9 1.357(9) . ? N6 B1 1.541(11) . ? B1 H1B 1.10(8) . ? C1 C2 1.391(12) . ? C1 C10 1.492(11) . ? C2 C3 1.368(12) . ? C2 H2A 0.9500 . ? C3 C11 1.488(12) . ? C4 C5 1.389(11) . ? C4 C12 1.481(11) . ? C5 C6 1.357(11) . ? C5 H5A 0.9500 . ? C6 C13 1.486(11) . ? C7 C8 1.402(11) . ? C7 C14 1.497(12) . ? C8 C9 1.343(11) . ? C8 H8A 0.9500 . ? C9 C15 1.497(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.368(10) . ? C16 C21 1.413(11) . ? C17 F1 1.359(9) . ? C17 C18 1.363(11) . ? C18 F2 1.357(10) . ? C18 C19 1.365(13) . ? C19 C20 1.335(12) . ? C19 F3 1.364(9) . ? C20 C21 1.374(11) . ? C20 F4 1.379(9) . ? C21 F5 1.324(9) . ? P1 C23 1.788(9) . ? P1 C24 1.798(8) . ? P1 C22 1.824(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Rh2 C40 2.062(9) . ? Rh2 N7 2.107(6) . ? Rh2 N11 2.133(7) . ? Rh2 N9 2.256(6) . ? Rh2 P2 2.273(2) . ? Rh2 H2 1.61(9) . ? N7 C25 1.314(10) . ? N7 N8 1.375(8) . ? N8 C27 1.343(10) . ? N8 B2 1.536(11) . ? N9 C28 1.320(9) . ? N9 N10 1.371(8) . ? N10 C30 1.353(9) . ? N10 B2 1.524(11) . ? N11 C31 1.333(10) . ? N11 N12 1.390(8) . ? N12 C33 1.335(10) . ? N12 B2 1.541(12) . ? B2 H2B 1.14(8) . ? C25 C26 1.398(12) . ? C25 C34 1.496(11) . ? C26 C27 1.378(11) . ? C26 H26A 0.9500 . ? C27 C35 1.506(12) . ? C28 C29 1.390(10) . ? C28 C36 1.492(11) . ? C29 C30 1.350(11) . ? C29 H29A 0.9500 . ? C30 C37 1.498(11) . ? C31 C32 1.389(11) . ? C31 C38 1.492(11) . ? C32 C33 1.379(11) . ? C32 H32A 0.9500 . ? C33 C39 1.484(11) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.305(12) . ? C40 C41 1.384(11) . ? C41 C42 1.372(12) . ? C41 F6 1.385(10) . ? C42 C43 1.353(13) . ? C42 F7 1.370(9) . ? C43 F8 1.342(10) . ? C43 C44 1.371(13) . ? C44 F9 1.352(11) . ? C44 C45 1.355(12) . ? C45 F10 1.392(9) . ? P2 C46 1.791(9) . ? P2 C47 1.804(10) . ? P2 C48 1.837(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.38(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.47(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.58(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.48(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.36(3) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C49' C50' 1.38(3) . ? C49' H49D 0.9800 . ? C49' H49E 0.9800 . ? C49' H49F 0.9800 . ? C50' C51' 1.49(3) . ? C50' H50C 0.9900 . ? C50' H50D 0.9900 . ? C51' C52' 1.57(4) . ? C51' H51C 0.9900 . ? C51' H51D 0.9900 . ? C52' C53' 1.46(3) . ? C52' H52C 0.9900 . ? C52' H52D 0.9900 . ? C53' C54' 1.37(3) . ? C53' H53C 0.9900 . ? C53' H53D 0.9900 . ? C54' H54D 0.9800 . ? C54' H54E 0.9800 . ? C54' H54F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N3 89.8(3) . . ? C16 Rh1 N5 170.4(3) . . ? N3 Rh1 N5 81.8(2) . . ? C16 Rh1 N1 91.4(3) . . ? N3 Rh1 N1 87.2(2) . . ? N5 Rh1 N1 92.7(2) . . ? C16 Rh1 P1 96.8(2) . . ? N3 Rh1 P1 173.40(17) . . ? N5 Rh1 P1 91.59(17) . . ? N1 Rh1 P1 92.73(17) . . ? C16 Rh1 H1 90(3) . . ? N3 Rh1 H1 91(3) . . ? N5 Rh1 H1 86(3) . . ? N1 Rh1 H1 178(3) . . ? P1 Rh1 H1 89(3) . . ? C1 N1 N2 106.2(6) . . ? C1 N1 Rh1 138.9(6) . . ? N2 N1 Rh1 114.9(4) . . ? C3 N2 N1 109.5(6) . . ? C3 N2 B1 129.7(7) . . ? N1 N2 B1 120.1(6) . . ? C4 N3 N4 108.2(6) . . ? C4 N3 Rh1 135.5(5) . . ? N4 N3 Rh1 116.3(5) . . ? C6 N4 N3 108.4(6) . . ? C6 N4 B1 130.1(7) . . ? N3 N4 B1 121.3(6) . . ? C7 N5 N6 106.9(6) . . ? C7 N5 Rh1 136.9(5) . . ? N6 N5 Rh1 116.2(4) . . ? C9 N6 N5 109.2(6) . . ? C9 N6 B1 129.7(7) . . ? N5 N6 B1 119.0(6) . . ? N2 B1 N4 110.6(7) . . ? N2 B1 N6 110.5(7) . . ? N4 B1 N6 107.3(7) . . ? N2 B1 H1B 113(4) . . ? N4 B1 H1B 112(4) . . ? N6 B1 H1B 104(4) . . ? N1 C1 C2 110.2(8) . . ? N1 C1 C10 123.7(8) . . ? C2 C1 C10 125.8(8) . . ? C3 C2 C1 105.6(8) . . ? C3 C2 H2A 127.2 . . ? C1 C2 H2A 127.2 . . ? N2 C3 C2 108.3(8) . . ? N2 C3 C11 123.0(8) . . ? C2 C3 C11 128.7(8) . . ? N3 C4 C5 108.0(7) . . ? N3 C4 C12 121.3(7) . . ? C5 C4 C12 130.7(8) . . ? C6 C5 C4 107.3(8) . . ? C6 C5 H5A 126.3 . . ? C4 C5 H5A 126.3 . . ? N4 C6 C5 108.1(7) . . ? N4 C6 C13 122.0(7) . . ? C5 C6 C13 129.9(8) . . ? N5 C7 C8 108.6(7) . . ? N5 C7 C14 124.9(7) . . ? C8 C7 C14 126.3(7) . . ? C9 C8 C7 107.6(7) . . ? C9 C8 H8A 126.2 . . ? C7 C8 H8A 126.2 . . ? C8 C9 N6 107.7(7) . . ? C8 C9 C15 130.1(7) . . ? N6 C9 C15 122.2(7) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 113.1(7) . . ? C17 C16 Rh1 125.7(6) . . ? C21 C16 Rh1 120.8(6) . . ? F1 C17 C18 115.5(7) . . ? F1 C17 C16 119.5(7) . . ? C18 C17 C16 125.0(8) . . ? F2 C18 C17 120.2(8) . . ? F2 C18 C19 120.0(8) . . ? C17 C18 C19 119.7(8) . . ? C20 C19 F3 121.5(8) . . ? C20 C19 C18 118.3(8) . . ? F3 C19 C18 120.1(8) . . ? C19 C20 C21 122.0(8) . . ? C19 C20 F4 118.8(7) . . ? C21 C20 F4 119.1(8) . . ? F5 C21 C20 115.8(7) . . ? F5 C21 C16 122.4(7) . . ? C20 C21 C16 121.7(8) . . ? C23 P1 C24 99.1(4) . . ? C23 P1 C22 104.0(5) . . ? C24 P1 C22 99.2(5) . . ? C23 P1 Rh1 119.8(3) . . ? C24 P1 Rh1 122.1(3) . . ? C22 P1 Rh1 109.5(3) . . ? P1 C22 H22A 109.5 . . ? P1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P1 C24 H24A 109.5 . . ? P1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C40 Rh2 N7 88.1(3) . . ? C40 Rh2 N11 170.0(3) . . ? N7 Rh2 N11 83.1(2) . . ? C40 Rh2 N9 96.2(3) . . ? N7 Rh2 N9 88.1(2) . . ? N11 Rh2 N9 88.3(2) . . ? C40 Rh2 P2 92.1(2) . . ? N7 Rh2 P2 177.23(18) . . ? N11 Rh2 P2 96.44(18) . . ? N9 Rh2 P2 94.59(17) . . ? C40 Rh2 H2 88(3) . . ? N7 Rh2 H2 98(3) . . ? N11 Rh2 H2 88(3) . . ? N9 Rh2 H2 173(3) . . ? P2 Rh2 H2 80(3) . . ? C25 N7 N8 107.6(6) . . ? C25 N7 Rh2 134.9(5) . . ? N8 N7 Rh2 117.1(5) . . ? C27 N8 N7 108.8(6) . . ? C27 N8 B2 130.3(7) . . ? N7 N8 B2 120.5(6) . . ? C28 N9 N10 106.5(6) . . ? C28 N9 Rh2 139.1(5) . . ? N10 N9 Rh2 114.3(4) . . ? C30 N10 N9 109.4(6) . . ? C30 N10 B2 129.4(7) . . ? N9 N10 B2 121.1(6) . . ? C31 N11 N12 105.3(6) . . ? C31 N11 Rh2 136.5(5) . . ? N12 N11 Rh2 116.9(5) . . ? C33 N12 N11 110.3(7) . . ? C33 N12 B2 128.5(7) . . ? N11 N12 B2 120.2(7) . . ? N10 B2 N8 110.8(7) . . ? N10 B2 N12 109.4(7) . . ? N8 B2 N12 108.0(7) . . ? N10 B2 H2B 107(4) . . ? N8 B2 H2B 112(4) . . ? N12 B2 H2B 110(4) . . ? N7 C25 C26 110.0(7) . . ? N7 C25 C34 124.0(8) . . ? C26 C25 C34 125.9(8) . . ? C27 C26 C25 105.1(7) . . ? C27 C26 H26A 127.4 . . ? C25 C26 H26A 127.4 . . ? N8 C27 C26 108.5(7) . . ? N8 C27 C35 123.8(7) . . ? C26 C27 C35 127.7(8) . . ? N9 C28 C29 110.0(7) . . ? N9 C28 C36 123.9(7) . . ? C29 C28 C36 126.0(7) . . ? C30 C29 C28 106.5(7) . . ? C30 C29 H29A 126.8 . . ? C28 C29 H29A 126.8 . . ? C29 C30 N10 107.7(7) . . ? C29 C30 C37 130.2(7) . . ? N10 C30 C37 122.1(7) . . ? N11 C31 C32 110.9(7) . . ? N11 C31 C38 121.7(8) . . ? C32 C31 C38 127.4(8) . . ? C33 C32 C31 105.5(8) . . ? C33 C32 H32A 127.2 . . ? C31 C32 H32A 127.2 . . ? N12 C33 C32 108.0(7) . . ? N12 C33 C39 122.9(8) . . ? C32 C33 C39 129.1(8) . . ? C25 C34 H34A 109.5 . . ? C25 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C25 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C27 C35 H35A 109.5 . . ? C27 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C27 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C28 C36 H36A 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C28 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C31 C38 H38A 109.5 . . ? C31 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C31 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 114.2(9) . . ? C45 C40 Rh2 123.3(6) . . ? C41 C40 Rh2 122.0(7) . . ? C42 C41 C40 122.5(9) . . ? C42 C41 F6 115.4(7) . . ? C40 C41 F6 122.1(8) . . ? C43 C42 F7 119.5(8) . . ? C43 C42 C41 120.3(8) . . ? F7 C42 C41 120.1(9) . . ? F8 C43 C42 121.1(8) . . ? F8 C43 C44 121.3(9) . . ? C42 C43 C44 117.5(9) . . ? F9 C44 C45 122.2(9) . . ? F9 C44 C43 118.7(9) . . ? C45 C44 C43 119.1(9) . . ? C40 C45 C44 126.3(9) . . ? C40 C45 F10 120.8(7) . . ? C44 C45 F10 112.9(8) . . ? C46 P2 C47 101.7(5) . . ? C46 P2 C48 105.5(5) . . ? C47 P2 C48 96.6(5) . . ? C46 P2 Rh2 111.0(3) . . ? C47 P2 Rh2 121.7(3) . . ? C48 P2 Rh2 117.9(3) . . ? P2 C46 H46A 109.5 . . ? P2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? P2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? P2 C47 H47A 109.5 . . ? P2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? P2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? P2 C48 H48A 109.5 . . ? P2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? P2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C49 C50 C51 113(4) . . ? C49 C50 H50A 108.9 . . ? C51 C50 H50A 108.9 . . ? C49 C50 H50B 108.9 . . ? C51 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C50 C51 C52 101(3) . . ? C50 C51 H51A 111.5 . . ? C52 C51 H51A 111.5 . . ? C50 C51 H51B 111.5 . . ? C52 C51 H51B 111.5 . . ? H51A C51 H51B 109.3 . . ? C53 C52 C51 94(3) . . ? C53 C52 H52A 112.8 . . ? C51 C52 H52A 112.8 . . ? C53 C52 H52B 112.8 . . ? C51 C52 H52B 112.8 . . ? H52A C52 H52B 110.3 . . ? C54 C53 C52 115(4) . . ? C54 C53 H53A 108.6 . . ? C52 C53 H53A 108.6 . . ? C54 C53 H53B 108.6 . . ? C52 C53 H53B 108.6 . . ? H53A C53 H53B 107.6 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C50' C49' H49D 109.5 . . ? C50' C49' H49E 109.5 . . ? H49D C49' H49E 109.5 . . ? C50' C49' H49F 109.5 . . ? H49D C49' H49F 109.5 . . ? H49E C49' H49F 109.5 . . ? C49' C50' C51' 113(4) . . ? C49' C50' H50C 108.9 . . ? C51' C50' H50C 108.9 . . ? C49' C50' H50D 108.9 . . ? C51' C50' H50D 108.9 . . ? H50C C50' H50D 107.7 . . ? C50' C51' C52' 97(3) . . ? C50' C51' H51C 112.4 . . ? C52' C51' H51C 112.4 . . ? C50' C51' H51D 112.4 . . ? C52' C51' H51D 112.4 . . ? H51C C51' H51D 109.9 . . ? C53' C52' C51' 101(3) . . ? C53' C52' H52C 111.6 . . ? C51' C52' H52C 111.6 . . ? C53' C52' H52D 111.6 . . ? C51' C52' H52D 111.6 . . ? H52C C52' H52D 109.4 . . ? C54' C53' C52' 113(4) . . ? C54' C53' H53C 109.1 . . ? C52' C53' H53C 109.1 . . ? C54' C53' H53D 109.1 . . ? C52' C53' H53D 109.1 . . ? H53C C53' H53D 107.8 . . ? C53' C54' H54D 109.5 . . ? C53' C54' H54E 109.5 . . ? H54D C54' H54E 109.5 . . ? C53' C54' H54F 109.5 . . ? H54D C54' H54F 109.5 . . ? H54E C54' H54F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 N1 C1 -39.9(8) . . . . ? N3 Rh1 N1 C1 -129.6(8) . . . . ? N5 Rh1 N1 C1 148.7(8) . . . . ? P1 Rh1 N1 C1 57.0(8) . . . . ? C16 Rh1 N1 N2 138.8(5) . . . . ? N3 Rh1 N1 N2 49.0(5) . . . . ? N5 Rh1 N1 N2 -32.6(5) . . . . ? P1 Rh1 N1 N2 -124.4(5) . . . . ? C1 N1 N2 C3 -1.2(8) . . . . ? Rh1 N1 N2 C3 179.7(5) . . . . ? C1 N1 N2 B1 170.3(7) . . . . ? Rh1 N1 N2 B1 -8.7(8) . . . . ? C16 Rh1 N3 C4 47.1(7) . . . . ? N5 Rh1 N3 C4 -128.3(7) . . . . ? N1 Rh1 N3 C4 138.5(7) . . . . ? P1 Rh1 N3 C4 -132.3(13) . . . . ? C16 Rh1 N3 N4 -133.2(5) . . . . ? N5 Rh1 N3 N4 51.3(5) . . . . ? N1 Rh1 N3 N4 -41.8(5) . . . . ? P1 Rh1 N3 N4 47.4(18) . . . . ? C4 N3 N4 C6 -0.1(8) . . . . ? Rh1 N3 N4 C6 -179.9(5) . . . . ? C4 N3 N4 B1 175.6(7) . . . . ? Rh1 N3 N4 B1 -4.1(8) . . . . ? C16 Rh1 N5 C7 92.6(18) . . . . ? N3 Rh1 N5 C7 121.5(8) . . . . ? N1 Rh1 N5 C7 -151.8(8) . . . . ? P1 Rh1 N5 C7 -59.0(8) . . . . ? C16 Rh1 N5 N6 -85.9(17) . . . . ? N3 Rh1 N5 N6 -57.0(5) . . . . ? N1 Rh1 N5 N6 29.7(5) . . . . ? P1 Rh1 N5 N6 122.5(5) . . . . ? C7 N5 N6 C9 0.3(8) . . . . ? Rh1 N5 N6 C9 179.2(5) . . . . ? C7 N5 N6 B1 -165.0(7) . . . . ? Rh1 N5 N6 B1 14.0(8) . . . . ? C3 N2 B1 N4 117.2(9) . . . . ? N1 N2 B1 N4 -52.5(9) . . . . ? C3 N2 B1 N6 -124.3(8) . . . . ? N1 N2 B1 N6 66.1(9) . . . . ? C6 N4 B1 N2 -122.7(8) . . . . ? N3 N4 B1 N2 62.6(9) . . . . ? C6 N4 B1 N6 116.8(8) . . . . ? N3 N4 B1 N6 -57.9(9) . . . . ? C9 N6 B1 N2 128.2(8) . . . . ? N5 N6 B1 N2 -70.0(8) . . . . ? C9 N6 B1 N4 -111.2(8) . . . . ? N5 N6 B1 N4 50.6(9) . . . . ? N2 N1 C1 C2 2.9(9) . . . . ? Rh1 N1 C1 C2 -178.3(6) . . . . ? N2 N1 C1 C10 -171.5(7) . . . . ? Rh1 N1 C1 C10 7.2(13) . . . . ? N1 C1 C2 C3 -3.5(9) . . . . ? C10 C1 C2 C3 170.8(8) . . . . ? N1 N2 C3 C2 -1.0(9) . . . . ? B1 N2 C3 C2 -171.5(8) . . . . ? N1 N2 C3 C11 179.3(8) . . . . ? B1 N2 C3 C11 8.9(13) . . . . ? C1 C2 C3 N2 2.7(9) . . . . ? C1 C2 C3 C11 -177.7(9) . . . . ? N4 N3 C4 C5 -0.2(8) . . . . ? Rh1 N3 C4 C5 179.5(5) . . . . ? N4 N3 C4 C12 -179.3(7) . . . . ? Rh1 N3 C4 C12 0.4(11) . . . . ? N3 C4 C5 C6 0.5(9) . . . . ? C12 C4 C5 C6 179.5(8) . . . . ? N3 N4 C6 C5 0.4(8) . . . . ? B1 N4 C6 C5 -174.8(7) . . . . ? N3 N4 C6 C13 178.4(7) . . . . ? B1 N4 C6 C13 3.2(13) . . . . ? C4 C5 C6 N4 -0.5(9) . . . . ? C4 C5 C6 C13 -178.4(8) . . . . ? N6 N5 C7 C8 -1.1(9) . . . . ? Rh1 N5 C7 C8 -179.6(6) . . . . ? N6 N5 C7 C14 174.7(8) . . . . ? Rh1 N5 C7 C14 -3.9(14) . . . . ? N5 C7 C8 C9 1.4(10) . . . . ? C14 C7 C8 C9 -174.3(8) . . . . ? C7 C8 C9 N6 -1.2(9) . . . . ? C7 C8 C9 C15 177.3(8) . . . . ? N5 N6 C9 C8 0.6(9) . . . . ? B1 N6 C9 C8 163.8(8) . . . . ? N5 N6 C9 C15 -178.1(7) . . . . ? B1 N6 C9 C15 -14.9(12) . . . . ? N3 Rh1 C16 C17 -129.0(7) . . . . ? N5 Rh1 C16 C17 -100.4(17) . . . . ? N1 Rh1 C16 C17 143.9(7) . . . . ? P1 Rh1 C16 C17 51.0(7) . . . . ? N3 Rh1 C16 C21 43.7(6) . . . . ? N5 Rh1 C16 C21 72.2(18) . . . . ? N1 Rh1 C16 C21 -43.5(6) . . . . ? P1 Rh1 C16 C21 -136.4(6) . . . . ? C21 C16 C17 F1 179.7(7) . . . . ? Rh1 C16 C17 F1 -7.2(11) . . . . ? C21 C16 C17 C18 0.7(12) . . . . ? Rh1 C16 C17 C18 173.9(7) . . . . ? F1 C17 C18 F2 0.5(12) . . . . ? C16 C17 C18 F2 179.5(8) . . . . ? F1 C17 C18 C19 -179.2(7) . . . . ? C16 C17 C18 C19 -0.2(14) . . . . ? F2 C18 C19 C20 -179.3(8) . . . . ? C17 C18 C19 C20 0.4(13) . . . . ? F2 C18 C19 F3 -0.3(13) . . . . ? C17 C18 C19 F3 179.4(8) . . . . ? F3 C19 C20 C21 179.9(7) . . . . ? C18 C19 C20 C21 -1.2(13) . . . . ? F3 C19 C20 F4 2.2(12) . . . . ? C18 C19 C20 F4 -178.9(7) . . . . ? C19 C20 C21 F5 -178.5(7) . . . . ? F4 C20 C21 F5 -0.8(11) . . . . ? C19 C20 C21 C16 1.8(13) . . . . ? F4 C20 C21 C16 179.5(7) . . . . ? C17 C16 C21 F5 178.8(7) . . . . ? Rh1 C16 C21 F5 5.3(10) . . . . ? C17 C16 C21 C20 -1.4(11) . . . . ? Rh1 C16 C21 C20 -175.0(6) . . . . ? C16 Rh1 P1 C23 -94.5(5) . . . . ? N3 Rh1 P1 C23 84.9(16) . . . . ? N5 Rh1 P1 C23 81.0(4) . . . . ? N1 Rh1 P1 C23 173.8(4) . . . . ? C16 Rh1 P1 C24 30.7(4) . . . . ? N3 Rh1 P1 C24 -150.0(16) . . . . ? N5 Rh1 P1 C24 -153.9(4) . . . . ? N1 Rh1 P1 C24 -61.1(4) . . . . ? C16 Rh1 P1 C22 145.7(5) . . . . ? N3 Rh1 P1 C22 -35.0(16) . . . . ? N5 Rh1 P1 C22 -38.9(4) . . . . ? N1 Rh1 P1 C22 53.9(4) . . . . ? C40 Rh2 N7 C25 41.5(8) . . . . ? N11 Rh2 N7 C25 -133.6(8) . . . . ? N9 Rh2 N7 C25 137.8(8) . . . . ? P2 Rh2 N7 C25 -53(4) . . . . ? C40 Rh2 N7 N8 -130.8(5) . . . . ? N11 Rh2 N7 N8 54.0(5) . . . . ? N9 Rh2 N7 N8 -34.5(5) . . . . ? P2 Rh2 N7 N8 135(4) . . . . ? C25 N7 N8 C27 -0.3(9) . . . . ? Rh2 N7 N8 C27 174.0(5) . . . . ? C25 N7 N8 B2 173.1(7) . . . . ? Rh2 N7 N8 B2 -12.6(9) . . . . ? C40 Rh2 N9 C28 -52.1(9) . . . . ? N7 Rh2 N9 C28 -140.0(8) . . . . ? N11 Rh2 N9 C28 136.8(8) . . . . ? P2 Rh2 N9 C28 40.5(8) . . . . ? C40 Rh2 N9 N10 133.6(5) . . . . ? N7 Rh2 N9 N10 45.7(5) . . . . ? N11 Rh2 N9 N10 -37.5(5) . . . . ? P2 Rh2 N9 N10 -133.8(5) . . . . ? C28 N9 N10 C30 -1.0(8) . . . . ? Rh2 N9 N10 C30 175.1(5) . . . . ? C28 N9 N10 B2 175.7(7) . . . . ? Rh2 N9 N10 B2 -8.2(9) . . . . ? C40 Rh2 N11 C31 87.5(17) . . . . ? N7 Rh2 N11 C31 116.5(8) . . . . ? N9 Rh2 N11 C31 -155.2(8) . . . . ? P2 Rh2 N11 C31 -60.8(7) . . . . ? C40 Rh2 N11 N12 -77.0(17) . . . . ? N7 Rh2 N11 N12 -48.0(5) . . . . ? N9 Rh2 N11 N12 40.3(5) . . . . ? P2 Rh2 N11 N12 134.8(5) . . . . ? C31 N11 N12 C33 2.2(8) . . . . ? Rh2 N11 N12 C33 171.1(5) . . . . ? C31 N11 N12 B2 -167.5(7) . . . . ? Rh2 N11 N12 B2 1.5(8) . . . . ? C30 N10 B2 N8 123.2(8) . . . . ? N9 N10 B2 N8 -52.8(10) . . . . ? C30 N10 B2 N12 -117.8(8) . . . . ? N9 N10 B2 N12 66.1(9) . . . . ? C27 N8 B2 N10 -119.9(9) . . . . ? N7 N8 B2 N10 68.3(9) . . . . ? C27 N8 B2 N12 120.3(9) . . . . ? N7 N8 B2 N12 -51.5(9) . . . . ? C33 N12 B2 N10 129.5(8) . . . . ? N11 N12 B2 N10 -62.9(9) . . . . ? C33 N12 B2 N8 -109.9(8) . . . . ? N11 N12 B2 N8 57.7(9) . . . . ? N8 N7 C25 C26 1.2(9) . . . . ? Rh2 N7 C25 C26 -171.7(6) . . . . ? N8 N7 C25 C34 -177.8(7) . . . . ? Rh2 N7 C25 C34 9.4(13) . . . . ? N7 C25 C26 C27 -1.5(10) . . . . ? C34 C25 C26 C27 177.4(8) . . . . ? N7 N8 C27 C26 -0.6(9) . . . . ? B2 N8 C27 C26 -173.2(8) . . . . ? N7 N8 C27 C35 178.8(7) . . . . ? B2 N8 C27 C35 6.2(14) . . . . ? C25 C26 C27 N8 1.3(10) . . . . ? C25 C26 C27 C35 -178.1(8) . . . . ? N10 N9 C28 C29 1.1(9) . . . . ? Rh2 N9 C28 C29 -173.4(6) . . . . ? N10 N9 C28 C36 -175.7(7) . . . . ? Rh2 N9 C28 C36 9.7(13) . . . . ? N9 C28 C29 C30 -0.8(9) . . . . ? C36 C28 C29 C30 175.9(8) . . . . ? C28 C29 C30 N10 0.2(9) . . . . ? C28 C29 C30 C37 -178.6(8) . . . . ? N9 N10 C30 C29 0.5(9) . . . . ? B2 N10 C30 C29 -175.9(8) . . . . ? N9 N10 C30 C37 179.4(7) . . . . ? B2 N10 C30 C37 3.0(13) . . . . ? N12 N11 C31 C32 -2.9(8) . . . . ? Rh2 N11 C31 C32 -168.5(6) . . . . ? N12 N11 C31 C38 176.1(7) . . . . ? Rh2 N11 C31 C38 10.5(12) . . . . ? N11 C31 C32 C33 2.6(9) . . . . ? C38 C31 C32 C33 -176.4(8) . . . . ? N11 N12 C33 C32 -0.6(8) . . . . ? B2 N12 C33 C32 168.0(7) . . . . ? N11 N12 C33 C39 180.0(7) . . . . ? B2 N12 C33 C39 -11.5(12) . . . . ? C31 C32 C33 N12 -1.1(9) . . . . ? C31 C32 C33 C39 178.2(8) . . . . ? N7 Rh2 C40 C45 49.6(7) . . . . ? N11 Rh2 C40 C45 78.4(18) . . . . ? N9 Rh2 C40 C45 -38.3(7) . . . . ? P2 Rh2 C40 C45 -133.1(7) . . . . ? N7 Rh2 C40 C41 -121.4(7) . . . . ? N11 Rh2 C40 C41 -92.6(17) . . . . ? N9 Rh2 C40 C41 150.7(7) . . . . ? P2 Rh2 C40 C41 55.8(7) . . . . ? C45 C40 C41 C42 1.1(13) . . . . ? Rh2 C40 C41 C42 172.9(7) . . . . ? C45 C40 C41 F6 -176.5(7) . . . . ? Rh2 C40 C41 F6 -4.7(11) . . . . ? C40 C41 C42 C43 0.3(15) . . . . ? F6 C41 C42 C43 178.0(9) . . . . ? C40 C41 C42 F7 178.2(8) . . . . ? F6 C41 C42 F7 -4.1(13) . . . . ? F7 C42 C43 F8 2.9(15) . . . . ? C41 C42 C43 F8 -179.1(9) . . . . ? F7 C42 C43 C44 -179.5(9) . . . . ? C41 C42 C43 C44 -1.6(15) . . . . ? F8 C43 C44 F9 -0.8(15) . . . . ? C42 C43 C44 F9 -178.4(9) . . . . ? F8 C43 C44 C45 179.0(9) . . . . ? C42 C43 C44 C45 1.5(15) . . . . ? C41 C40 C45 C44 -1.2(13) . . . . ? Rh2 C40 C45 C44 -172.9(7) . . . . ? C41 C40 C45 F10 178.1(7) . . . . ? Rh2 C40 C45 F10 6.4(11) . . . . ? F9 C44 C45 C40 179.8(8) . . . . ? C43 C44 C45 C40 -0.1(15) . . . . ? F9 C44 C45 F10 0.4(13) . . . . ? C43 C44 C45 F10 -179.4(8) . . . . ? C40 Rh2 P2 C46 138.0(5) . . . . ? N7 Rh2 P2 C46 -128(4) . . . . ? N11 Rh2 P2 C46 -47.2(4) . . . . ? N9 Rh2 P2 C46 41.6(4) . . . . ? C40 Rh2 P2 C47 -102.4(5) . . . . ? N7 Rh2 P2 C47 -8(4) . . . . ? N11 Rh2 P2 C47 72.3(5) . . . . ? N9 Rh2 P2 C47 161.1(5) . . . . ? C40 Rh2 P2 C48 16.3(4) . . . . ? N7 Rh2 P2 C48 111(4) . . . . ? N11 Rh2 P2 C48 -169.0(4) . . . . ? N9 Rh2 P2 C48 -80.1(4) . . . . ? C49 C50 C51 C52 172(6) . . . . ? C50 C51 C52 C53 171(4) . . . . ? C51 C52 C53 C54 -154(5) . . . . ? C49' C50' C51' C52' -170(5) . . . . ? C50' C51' C52' C53' 177(4) . . . . ? C51' C52' C53' C54' 179(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.058 _refine_diff_density_min -1.204 _refine_diff_density_rms 0.122 #===end data_jontt05_cmpd3b _database_code_depnum_ccdc_archive 'CCDC 770112' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt05 _chemical_melting_point ? _chemical_formula_moiety 'C24 H33 B F4 N6 P Rh' _chemical_formula_sum 'C24 H33 B F4 N6 P Rh' _chemical_formula_weight 626.25 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 29.063(3) _cell_length_b 10.5847(12) _cell_length_c 17.7982(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5475.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 4013 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 32.80 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8551 _exptl_absorpt_correction_T_max 0.9170 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 117833 _diffrn_reflns_av_R_equivalents 0.1168 _diffrn_reflns_av_sigmaI/netI 0.1054 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 36.32 _reflns_number_total 26396 _reflns_number_gt 16014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The structure refined as an merohedral (inversion) twin with a final refined mass ratio of 52:48. The hydride ligands of both molecules could not be found from the difference Fourier map, likely due to the disorder (see below). There are two molecules in the asymmetric unit, both which are modeled as disordered over two positions. Initially each molecular disorder was refined independently, but it was found that the 85:15 component ratio resulted for both. Upon further examination, it was plain that the disorders had to be refined together to avoid close intermolecular contacts. The two positions of molecule one (Rh1) had only the rhodium atom in common, whereas the all atoms of molecule two (Rh2, Rh2') were in different positions. In both cases, the two components were related by a pseudo-mirror (the disorder ratio of 85:15 disallows the refinement in a centrosymmetric space group). The corresponding atoms of each disorder were constrained to have identical anistropic displacement parameters. The corresponding bond lengths and angles of each disorder were restrained to be similar. Additionally, the planar moieties of the minor components of the disorders were restrained to be flat. ; _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^)+(0.0494P)^2^+3.1635P] 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), 15833 Friedel pairs, Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(9) _refine_ls_number_reflns 26396 _refine_ls_number_parameters 906 _refine_ls_number_restraints 329 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.011 _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 0.468028(10) 0.50339(3) 0.61181(3) 0.01626(6) Uani 1 1 d D . . N1 N 0.44970(14) 0.3616(4) 0.5210(2) 0.0171(8) Uani 0.8546(9) 1 d PD A 1 N2 N 0.41681(13) 0.4019(4) 0.4711(2) 0.0167(8) Uani 0.8546(9) 1 d PD A 1 N3 N 0.4655(2) 0.6434(5) 0.5269(3) 0.0205(9) Uani 0.8546(9) 1 d PD A 1 N4 N 0.43245(17) 0.6352(4) 0.4726(3) 0.0179(9) Uani 0.8546(9) 1 d PD A 1 N5 N 0.39623(13) 0.5498(4) 0.6202(3) 0.0179(7) Uani 0.8546(9) 1 d PD A 1 N6 N 0.37083(13) 0.5482(4) 0.5546(2) 0.0191(8) Uani 0.8546(9) 1 d PD A 1 B1 B 0.39534(18) 0.5327(4) 0.4786(3) 0.0200(11) Uani 0.8546(9) 1 d PD A 1 H1 H 0.3725 0.5449 0.4373 0.024 Uiso 0.8546(9) 1 calc PR A 1 C1 C 0.46646(18) 0.2536(5) 0.4940(3) 0.0240(10) Uani 0.8546(9) 1 d PD A 1 C2 C 0.44446(19) 0.2227(5) 0.4270(3) 0.0251(11) Uani 0.8546(9) 1 d PD A 1 H2 H 0.4496 0.1499 0.3970 0.030 Uiso 0.8546(9) 1 calc PR A 1 C3 C 0.41403(17) 0.3181(5) 0.4132(3) 0.0226(10) Uani 0.8546(9) 1 d PD A 1 C4 C 0.49157(17) 0.7438(5) 0.5103(3) 0.0237(11) Uani 0.8546(9) 1 d PD A 1 C5 C 0.47406(18) 0.8016(5) 0.4452(3) 0.0264(12) Uani 0.8546(9) 1 d PD A 1 H5 H 0.4857 0.8751 0.4212 0.032 Uiso 0.8546(9) 1 calc PR A 1 C6 C 0.43718(17) 0.7320(5) 0.4233(3) 0.0220(10) Uani 0.8546(9) 1 d PD A 1 C7 C 0.36752(16) 0.5947(4) 0.6734(3) 0.0231(9) Uani 0.8546(9) 1 d PD A 1 C8 C 0.32440(17) 0.6177(5) 0.6430(3) 0.0248(11) Uani 0.8546(9) 1 d PD A 1 H8 H 0.2979 0.6474 0.6688 0.030 Uiso 0.8546(9) 1 calc PR A 1 C9 C 0.32782(15) 0.5889(5) 0.5683(3) 0.0213(10) Uani 0.8546(9) 1 d PD A 1 C10 C 0.50374(18) 0.1777(5) 0.5299(3) 0.0282(11) Uani 0.8546(9) 1 d PD A 1 H10A H 0.5200 0.2300 0.5668 0.042 Uiso 0.8546(9) 1 calc PR A 1 H10B H 0.5254 0.1490 0.4914 0.042 Uiso 0.8546(9) 1 calc PR A 1 H10C H 0.4902 0.1043 0.5552 0.042 Uiso 0.8546(9) 1 calc PR A 1 C11 C 0.38066(18) 0.3371(6) 0.3502(3) 0.0288(11) Uani 0.8546(9) 1 d PD A 1 H11A H 0.3883 0.2796 0.3089 0.043 Uiso 0.8546(9) 1 calc PR A 1 H11B H 0.3824 0.4246 0.3326 0.043 Uiso 0.8546(9) 1 calc PR A 1 H11C H 0.3494 0.3194 0.3680 0.043 Uiso 0.8546(9) 1 calc PR A 1 C12 C 0.53091(17) 0.7857(5) 0.5582(3) 0.0281(12) Uani 0.8546(9) 1 d PD A 1 H12A H 0.5256 0.7592 0.6102 0.042 Uiso 0.8546(9) 1 calc PR A 1 H12B H 0.5335 0.8779 0.5561 0.042 Uiso 0.8546(9) 1 calc PR A 1 H12C H 0.5594 0.7474 0.5397 0.042 Uiso 0.8546(9) 1 calc PR A 1 C13 C 0.4037(2) 0.7490(6) 0.3601(3) 0.0337(13) Uani 0.8546(9) 1 d PD A 1 H13A H 0.3995 0.6684 0.3339 0.051 Uiso 0.8546(9) 1 calc PR A 1 H13B H 0.4157 0.8121 0.3248 0.051 Uiso 0.8546(9) 1 calc PR A 1 H13C H 0.3741 0.7777 0.3801 0.051 Uiso 0.8546(9) 1 calc PR A 1 C14 C 0.3830(2) 0.6182(6) 0.7520(3) 0.0300(12) Uani 0.8546(9) 1 d PD A 1 H14A H 0.3766 0.5435 0.7828 0.045 Uiso 0.8546(9) 1 calc PR A 1 H14B H 0.3664 0.6910 0.7726 0.045 Uiso 0.8546(9) 1 calc PR A 1 H14C H 0.4161 0.6357 0.7523 0.045 Uiso 0.8546(9) 1 calc PR A 1 C15 C 0.29211(18) 0.6019(6) 0.5085(3) 0.0339(13) Uani 0.8546(9) 1 d PD A 1 H15A H 0.3002 0.6722 0.4752 0.051 Uiso 0.8546(9) 1 calc PR A 1 H15B H 0.2621 0.6185 0.5318 0.051 Uiso 0.8546(9) 1 calc PR A 1 H15C H 0.2905 0.5235 0.4793 0.051 Uiso 0.8546(9) 1 calc PR A 1 C16 C 0.53662(18) 0.4850(4) 0.5934(3) 0.0153(10) Uani 0.8546(9) 1 d PD A 1 C17 C 0.5712(3) 0.4992(6) 0.6432(4) 0.0228(10) Uani 0.8546(9) 1 d PD A 1 F1 F 0.5613(4) 0.5130(6) 0.7182(4) 0.0341(10) Uani 0.8546(9) 1 d PD A 1 C18 C 0.6174(2) 0.4989(6) 0.6263(4) 0.0259(12) Uani 0.8546(9) 1 d PD A 1 F2 F 0.6497(2) 0.5148(4) 0.6799(4) 0.0331(11) Uani 0.8546(9) 1 d PD A 1 C19 C 0.6307(2) 0.4868(6) 0.5525(4) 0.0231(10) Uani 0.8546(9) 1 d PD A 1 F3 F 0.6760(2) 0.4898(6) 0.5337(6) 0.0301(9) Uani 0.8546(9) 1 d PD A 1 C20 C 0.59719(18) 0.4741(5) 0.4991(3) 0.0201(10) Uani 0.8546(9) 1 d PD A 1 F4 F 0.61043(13) 0.4657(3) 0.4265(2) 0.0289(8) Uani 0.8546(9) 1 d PD A 1 C21 C 0.55130(18) 0.4722(5) 0.5183(3) 0.0208(10) Uani 0.8546(9) 1 d PD A 1 H21 H 0.5289 0.4619 0.4799 0.025 Uiso 0.8546(9) 1 calc PR A 1 P1 P 0.46807(5) 0.37215(14) 0.71163(9) 0.0202(3) Uani 0.8546(9) 1 d PD A 1 C22 C 0.41453(18) 0.2853(5) 0.7198(3) 0.0261(11) Uani 0.8546(9) 1 d PD A 1 H22A H 0.4152 0.2333 0.7653 0.039 Uiso 0.8546(9) 1 calc PR A 1 H22B H 0.4107 0.2307 0.6758 0.039 Uiso 0.8546(9) 1 calc PR A 1 H22C H 0.3888 0.3448 0.7227 0.039 Uiso 0.8546(9) 1 calc PR A 1 C23 C 0.50943(19) 0.2410(5) 0.7149(4) 0.0285(12) Uani 0.8546(9) 1 d PD A 1 H23A H 0.5100 0.2051 0.7657 0.043 Uiso 0.8546(9) 1 calc PR A 1 H23B H 0.5402 0.2723 0.7019 0.043 Uiso 0.8546(9) 1 calc PR A 1 H23C H 0.5002 0.1757 0.6789 0.043 Uiso 0.8546(9) 1 calc PR A 1 C24 C 0.47638(19) 0.4411(6) 0.8051(3) 0.0272(11) Uani 0.8546(9) 1 d PD A 1 H24A H 0.4541 0.5094 0.8128 0.041 Uiso 0.8546(9) 1 calc PR A 1 H24B H 0.5077 0.4748 0.8091 0.041 Uiso 0.8546(9) 1 calc PR A 1 H24C H 0.4718 0.3758 0.8434 0.041 Uiso 0.8546(9) 1 calc PR A 1 B1' B 0.3982(7) 0.4795(17) 0.4770(14) 0.0200(11) Uani 0.1454(9) 1 d PD A 5 H1' H 0.3762 0.4716 0.4341 0.024 Uiso 0.1454(9) 1 calc PR A 5 N1' N 0.4605(10) 0.643(2) 0.5163(12) 0.0205(9) Uani 0.1454(9) 1 d PD A 5 N2' N 0.4264(10) 0.601(2) 0.4684(16) 0.0179(9) Uani 0.1454(9) 1 d PD A 5 C3' C 0.4182(7) 0.697(2) 0.4197(11) 0.0220(10) Uani 0.1454(9) 1 d PD A 5 C2' C 0.4456(8) 0.796(2) 0.4358(13) 0.0264(12) Uani 0.1454(9) 1 d PD A 5 H2' H 0.4467 0.8754 0.4105 0.032 Uiso 0.1454(9) 1 calc PR A 5 C1' C 0.4721(6) 0.759(2) 0.4976(12) 0.0237(11) Uani 0.1454(9) 1 d PD A 5 N3' N 0.4685(6) 0.3658(16) 0.5251(9) 0.0171(8) Uani 0.1454(9) 1 d PD A 5 N4' N 0.4354(6) 0.3773(18) 0.4707(11) 0.0167(8) Uani 0.1454(9) 1 d PD A 5 C6' C 0.4405(7) 0.280(2) 0.4204(10) 0.0226(10) Uani 0.1454(9) 1 d PD A 5 C5' C 0.4765(8) 0.2076(19) 0.4428(12) 0.0251(11) Uani 0.1454(9) 1 d PD A 5 H5' H 0.4878 0.1339 0.4185 0.030 Uiso 0.1454(9) 1 calc PR A 5 C4' C 0.4941(6) 0.2628(18) 0.5092(11) 0.0240(10) Uani 0.1454(9) 1 d PD A 5 N5' N 0.3965(2) 0.4554(16) 0.6197(11) 0.0179(7) Uani 0.1454(9) 1 d PD A 5 N6' N 0.3728(6) 0.4573(17) 0.5514(10) 0.0191(8) Uani 0.1454(9) 1 d PD A 5 C9' C 0.3302(6) 0.4166(16) 0.5628(11) 0.0213(10) Uani 0.1454(9) 1 d PD A 5 C8' C 0.3259(7) 0.3886(19) 0.6376(12) 0.0248(11) Uani 0.1454(9) 1 d PD A 5 H8' H 0.2989 0.3577 0.6617 0.030 Uiso 0.1454(9) 1 calc PR A 5 C7' C 0.3670(6) 0.4129(14) 0.6714(11) 0.0231(9) Uani 0.1454(9) 1 d PD A 5 C10' C 0.5080(8) 0.834(3) 0.5375(18) 0.0281(12) Uani 0.1454(9) 1 d PD A 5 H10D H 0.5176 0.7890 0.5830 0.042 Uiso 0.1454(9) 1 calc PR A 5 H10E H 0.4954 0.9166 0.5512 0.042 Uiso 0.1454(9) 1 calc PR A 5 H10F H 0.5346 0.8457 0.5044 0.042 Uiso 0.1454(9) 1 calc PR A 5 C11' C 0.3834(9) 0.691(4) 0.3579(15) 0.0337(13) Uani 0.1454(9) 1 d PD A 5 H11D H 0.3660 0.6118 0.3619 0.051 Uiso 0.1454(9) 1 calc PR A 5 H11E H 0.3992 0.6937 0.3092 0.051 Uiso 0.1454(9) 1 calc PR A 5 H11F H 0.3623 0.7626 0.3620 0.051 Uiso 0.1454(9) 1 calc PR A 5 C12' C 0.5332(8) 0.225(3) 0.5586(16) 0.0282(11) Uani 0.1454(9) 1 d PD A 5 H12D H 0.5357 0.2844 0.6006 0.042 Uiso 0.1454(9) 1 calc PR A 5 H12E H 0.5618 0.2256 0.5296 0.042 Uiso 0.1454(9) 1 calc PR A 5 H12F H 0.5277 0.1396 0.5782 0.042 Uiso 0.1454(9) 1 calc PR A 5 C13' C 0.4064(9) 0.281(3) 0.3576(14) 0.0288(11) Uani 0.1454(9) 1 d PD A 5 H13D H 0.3857 0.3531 0.3630 0.043 Uiso 0.1454(9) 1 calc PR A 5 H13E H 0.3884 0.2023 0.3589 0.043 Uiso 0.1454(9) 1 calc PR A 5 H13F H 0.4227 0.2864 0.3095 0.043 Uiso 0.1454(9) 1 calc PR A 5 C14' C 0.3829(11) 0.400(3) 0.7508(12) 0.0300(12) Uani 0.1454(9) 1 d PD A 5 H14D H 0.4151 0.4270 0.7545 0.045 Uiso 0.1454(9) 1 calc PR A 5 H14E H 0.3801 0.3121 0.7668 0.045 Uiso 0.1454(9) 1 calc PR A 5 H14F H 0.3638 0.4538 0.7833 0.045 Uiso 0.1454(9) 1 calc PR A 5 C15' C 0.2964(10) 0.408(3) 0.5000(16) 0.0339(13) Uani 0.1454(9) 1 d PD A 5 H15D H 0.3107 0.4379 0.4535 0.051 Uiso 0.1454(9) 1 calc PR A 5 H15E H 0.2694 0.4599 0.5116 0.051 Uiso 0.1454(9) 1 calc PR A 5 H15F H 0.2868 0.3196 0.4937 0.051 Uiso 0.1454(9) 1 calc PR A 5 C16' C 0.5387(10) 0.524(2) 0.5957(15) 0.0153(10) Uani 0.1454(9) 1 d PD A 5 C17' C 0.5728(12) 0.507(2) 0.6463(16) 0.0228(10) Uani 0.1454(9) 1 d PD A 5 F1' F 0.562(2) 0.501(3) 0.7213(18) 0.0341(10) Uani 0.1454(9) 1 d PD A 5 C18' C 0.6188(12) 0.495(2) 0.6296(17) 0.0259(12) Uani 0.1454(9) 1 d PD A 5 F2' F 0.6505(13) 0.479(3) 0.684(2) 0.0331(11) Uani 0.1454(9) 1 d PD A 5 C19' C 0.6327(10) 0.500(2) 0.5559(17) 0.0231(10) Uani 0.1454(9) 1 d PD A 5 F3' F 0.6779(11) 0.488(3) 0.538(4) 0.0301(9) Uani 0.1454(9) 1 d PD A 5 C20' C 0.5998(9) 0.5168(15) 0.5019(13) 0.0201(10) Uani 0.1454(9) 1 d PD A 5 F4' F 0.6132(9) 0.5218(19) 0.4296(13) 0.0289(8) Uani 0.1454(9) 1 d PD A 5 C21' C 0.5542(8) 0.5287(18) 0.5210(14) 0.0208(10) Uani 0.1454(9) 1 d PD A 5 H21' H 0.5322 0.5404 0.4821 0.025 Uiso 0.1454(9) 1 calc PR A 5 P1' P 0.4715(3) 0.6283(7) 0.7143(4) 0.0202(3) Uani 0.1454(9) 1 d PD A 5 C22' C 0.4193(7) 0.720(3) 0.7217(18) 0.0261(11) Uani 0.1454(9) 1 d PD A 5 H22D H 0.3926 0.6636 0.7192 0.039 Uiso 0.1454(9) 1 calc PR A 5 H22E H 0.4178 0.7809 0.6803 0.039 Uiso 0.1454(9) 1 calc PR A 5 H22F H 0.4190 0.7655 0.7697 0.039 Uiso 0.1454(9) 1 calc PR A 5 C23' C 0.5136(8) 0.756(2) 0.720(2) 0.0285(12) Uani 0.1454(9) 1 d PD A 5 H23D H 0.5446 0.7209 0.7135 0.043 Uiso 0.1454(9) 1 calc PR A 5 H23E H 0.5113 0.7969 0.7691 0.043 Uiso 0.1454(9) 1 calc PR A 5 H23F H 0.5075 0.8175 0.6802 0.043 Uiso 0.1454(9) 1 calc PR A 5 C24' C 0.4796(10) 0.557(3) 0.8087(13) 0.0272(11) Uani 0.1454(9) 1 d PD A 5 H24D H 0.5077 0.5061 0.8090 0.041 Uiso 0.1454(9) 1 calc PR A 5 H24E H 0.4531 0.5037 0.8208 0.041 Uiso 0.1454(9) 1 calc PR A 5 H24F H 0.4822 0.6246 0.8463 0.041 Uiso 0.1454(9) 1 calc PR A 5 Rh2 Rh 0.27807(2) 0.02321(4) 0.67796(6) 0.01676(9) Uani 0.8546(9) 1 d PD A 1 N7 N 0.29336(14) 0.1651(4) 0.7685(3) 0.0161(8) Uani 0.8546(9) 1 d PD A 1 N8 N 0.32736(14) 0.1309(4) 0.8192(3) 0.0184(9) Uani 0.8546(9) 1 d PD A 1 N9 N 0.27812(14) -0.1132(4) 0.7638(3) 0.0182(8) Uani 0.8546(9) 1 d PD A 1 N10 N 0.31060(14) -0.1021(4) 0.8203(3) 0.0196(8) Uani 0.8546(9) 1 d PD A 1 N11 N 0.35043(13) -0.0209(4) 0.6723(3) 0.0207(8) Uani 0.8546(9) 1 d PD A 1 N12 N 0.37428(14) -0.0193(4) 0.7401(3) 0.0185(9) Uani 0.8546(9) 1 d PD A 1 B2 B 0.34823(18) -0.0010(5) 0.8139(4) 0.0225(11) Uani 0.8546(9) 1 d PD A 1 H2A H 0.3703 -0.0123 0.8565 0.027 Uiso 0.8546(9) 1 calc PR A 1 C25 C 0.28034(15) 0.2806(4) 0.7895(3) 0.0182(8) Uani 0.8546(9) 1 d PD A 1 C26 C 0.30437(18) 0.3203(5) 0.8527(3) 0.0236(10) Uani 0.8546(9) 1 d PD A 1 H26 H 0.3014 0.3987 0.8782 0.028 Uiso 0.8546(9) 1 calc PR A 1 C27 C 0.33313(16) 0.2228(5) 0.8704(3) 0.0189(9) Uani 0.8546(9) 1 d PD A 1 C28 C 0.25296(18) -0.2168(5) 0.7792(3) 0.0271(11) Uani 0.8546(9) 1 d PD A 1 C29 C 0.2679(2) -0.2686(5) 0.8454(4) 0.0302(12) Uani 0.8546(9) 1 d PD A 1 H29 H 0.2556 -0.3410 0.8696 0.036 Uiso 0.8546(9) 1 calc PR A 1 C30 C 0.3043(2) -0.1961(5) 0.8706(3) 0.0276(12) Uani 0.8546(9) 1 d PD A 1 C31 C 0.37989(16) -0.0641(5) 0.6219(3) 0.0213(10) Uani 0.8546(9) 1 d PD A 1 C32 C 0.42242(18) -0.0883(5) 0.6551(3) 0.0296(12) Uani 0.8546(9) 1 d PD A 1 H32 H 0.4494 -0.1184 0.6308 0.035 Uiso 0.8546(9) 1 calc PR A 1 C33 C 0.41760(16) -0.0600(5) 0.7296(3) 0.0245(10) Uani 0.8546(9) 1 d PD A 1 C34 C 0.24353(18) 0.3546(5) 0.7499(3) 0.0273(11) Uani 0.8546(9) 1 d PD A 1 H34A H 0.2234 0.2965 0.7225 0.041 Uiso 0.8546(9) 1 calc PR A 1 H34B H 0.2578 0.4137 0.7145 0.041 Uiso 0.8546(9) 1 calc PR A 1 H34C H 0.2254 0.4017 0.7869 0.041 Uiso 0.8546(9) 1 calc PR A 1 C35 C 0.36748(19) 0.2108(6) 0.9328(3) 0.0304(12) Uani 0.8546(9) 1 d PD A 1 H35A H 0.3611 0.1341 0.9617 0.046 Uiso 0.8546(9) 1 calc PR A 1 H35B H 0.3653 0.2847 0.9658 0.046 Uiso 0.8546(9) 1 calc PR A 1 H35C H 0.3986 0.2058 0.9116 0.046 Uiso 0.8546(9) 1 calc PR A 1 C36 C 0.21430(17) -0.2599(5) 0.7299(4) 0.0306(13) Uani 0.8546(9) 1 d PD A 1 H36A H 0.1857 -0.2187 0.7456 0.046 Uiso 0.8546(9) 1 calc PR A 1 H36B H 0.2109 -0.3517 0.7341 0.046 Uiso 0.8546(9) 1 calc PR A 1 H36C H 0.2210 -0.2375 0.6776 0.046 Uiso 0.8546(9) 1 calc PR A 1 C37 C 0.3348(2) -0.2087(6) 0.9385(3) 0.0415(17) Uani 0.8546(9) 1 d PD A 1 H37A H 0.3660 -0.2319 0.9225 0.062 Uiso 0.8546(9) 1 calc PR A 1 H37B H 0.3225 -0.2744 0.9717 0.062 Uiso 0.8546(9) 1 calc PR A 1 H37C H 0.3358 -0.1281 0.9654 0.062 Uiso 0.8546(9) 1 calc PR A 1 C38 C 0.3660(2) -0.0912(6) 0.5425(3) 0.0333(13) Uani 0.8546(9) 1 d PD A 1 H38A H 0.3333 -0.1131 0.5409 0.050 Uiso 0.8546(9) 1 calc PR A 1 H38B H 0.3842 -0.1621 0.5231 0.050 Uiso 0.8546(9) 1 calc PR A 1 H38C H 0.3715 -0.0163 0.5114 0.050 Uiso 0.8546(9) 1 calc PR A 1 C39 C 0.45250(18) -0.0728(6) 0.7914(4) 0.0361(14) Uani 0.8546(9) 1 d PD A 1 H39A H 0.4560 0.0084 0.8172 0.054 Uiso 0.8546(9) 1 calc PR A 1 H39B H 0.4821 -0.0985 0.7700 0.054 Uiso 0.8546(9) 1 calc PR A 1 H39C H 0.4421 -0.1369 0.8274 0.054 Uiso 0.8546(9) 1 calc PR A 1 C40 C 0.20933(17) 0.0368(5) 0.6949(3) 0.0207(11) Uani 0.8546(9) 1 d PD A 1 C41 C 0.1749(2) 0.0170(6) 0.6416(4) 0.0235(12) Uani 0.8546(9) 1 d PD A 1 F5 F 0.1847(3) 0.0004(6) 0.5677(3) 0.0356(12) Uani 0.8546(9) 1 d PD A 1 C42 C 0.1284(2) 0.0089(6) 0.6595(4) 0.0268(13) Uani 0.8546(9) 1 d PD A 1 F6 F 0.0970(2) -0.0145(6) 0.6051(5) 0.0384(12) Uani 0.8546(9) 1 d PD A 1 C43 C 0.11485(19) 0.0217(5) 0.7325(4) 0.0259(12) Uani 0.8546(9) 1 d PD A 1 F7 F 0.06957(16) 0.0156(4) 0.7506(5) 0.0349(11) Uani 0.8546(9) 1 d PD A 1 C44 C 0.14768(17) 0.0409(5) 0.7869(3) 0.0225(10) Uani 0.8546(9) 1 d PD A 1 F8 F 0.13394(11) 0.0490(3) 0.8601(2) 0.0304(7) Uani 0.8546(9) 1 d PD A 1 C45 C 0.19374(16) 0.0488(5) 0.7696(3) 0.0191(9) Uani 0.8546(9) 1 d PD A 1 H45 H 0.2154 0.0626 0.8086 0.023 Uiso 0.8546(9) 1 calc PR A 1 P2 P 0.27720(4) 0.15093(13) 0.57581(8) 0.0198(3) Uani 0.8546(9) 1 d PD A 1 C46 C 0.32919(19) 0.2451(6) 0.5657(4) 0.0316(13) Uani 0.8546(9) 1 d PD A 1 H46A H 0.3558 0.1891 0.5596 0.047 Uiso 0.8546(9) 1 calc PR A 1 H46B H 0.3334 0.2973 0.6107 0.047 Uiso 0.8546(9) 1 calc PR A 1 H46C H 0.3264 0.2998 0.5215 0.047 Uiso 0.8546(9) 1 calc PR A 1 C47 C 0.2715(2) 0.0766(6) 0.4832(3) 0.0275(11) Uani 0.8546(9) 1 d PD A 1 H47A H 0.2669 0.1420 0.4450 0.041 Uiso 0.8546(9) 1 calc PR A 1 H47B H 0.2450 0.0193 0.4834 0.041 Uiso 0.8546(9) 1 calc PR A 1 H47C H 0.2995 0.0288 0.4717 0.041 Uiso 0.8546(9) 1 calc PR A 1 C48 C 0.23341(19) 0.2728(6) 0.5668(3) 0.0297(12) Uani 0.8546(9) 1 d PD A 1 H48A H 0.2300 0.2961 0.5138 0.045 Uiso 0.8546(9) 1 calc PR A 1 H48B H 0.2426 0.3473 0.5959 0.045 Uiso 0.8546(9) 1 calc PR A 1 H48C H 0.2040 0.2407 0.5858 0.045 Uiso 0.8546(9) 1 calc PR A 1 Rh2' Rh 0.28001(16) -0.0091(3) 0.6801(4) 0.01676(9) Uani 0.1454(9) 1 d PD A 5 B2' B 0.3561(9) 0.0121(19) 0.8167(15) 0.0225(11) Uani 0.1454(9) 1 d PD A 5 H2B H 0.3789 0.0271 0.8578 0.027 Uiso 0.1454(9) 1 calc PR A 5 N7' N 0.2977(6) -0.1611(14) 0.7792(8) 0.0182(8) Uani 0.1454(9) 1 d PD A 5 N8' N 0.3312(6) -0.1145(18) 0.8241(12) 0.0196(8) Uani 0.1454(9) 1 d PD A 5 C27' C 0.3362(7) -0.205(2) 0.8769(10) 0.0276(12) Uani 0.1454(9) 1 d PD A 5 C26' C 0.3062(8) -0.3029(19) 0.8625(13) 0.0302(12) Uani 0.1454(9) 1 d PD A 5 H26' H 0.3030 -0.3782 0.8911 0.036 Uiso 0.1454(9) 1 calc PR A 5 C25' C 0.2814(6) -0.2709(17) 0.7984(12) 0.0271(11) Uani 0.1454(9) 1 d PD A 5 N9' N 0.2839(6) 0.1130(15) 0.7559(9) 0.0161(8) Uani 0.1454(9) 1 d PD A 5 N10' N 0.3166(7) 0.107(2) 0.8172(13) 0.0184(9) Uani 0.1454(9) 1 d PD A 5 C30' C 0.3124(7) 0.1972(19) 0.8712(10) 0.0189(9) Uani 0.1454(9) 1 d PD A 5 C29' C 0.2756(7) 0.2699(18) 0.8484(12) 0.0236(10) Uani 0.1454(9) 1 d PD A 5 H29' H 0.2635 0.3414 0.8740 0.028 Uiso 0.1454(9) 1 calc PR A 5 C28' C 0.2595(5) 0.2196(16) 0.7816(10) 0.0182(8) Uani 0.1454(9) 1 d PD A 5 N11' N 0.3490(3) 0.0334(17) 0.6740(14) 0.0207(8) Uani 0.1454(9) 1 d PD A 5 N12' N 0.3767(7) 0.0277(17) 0.7383(12) 0.0185(9) Uani 0.1454(9) 1 d PD A 5 C33' C 0.4196(7) 0.0656(16) 0.7285(12) 0.0245(10) Uani 0.1454(9) 1 d PD A 5 C32' C 0.4212(7) 0.0988(19) 0.6541(14) 0.0296(12) Uani 0.1454(9) 1 d PD A 5 H32' H 0.4472 0.1306 0.6280 0.035 Uiso 0.1454(9) 1 calc PR A 5 C31' C 0.3779(7) 0.0779(15) 0.6235(11) 0.0213(10) Uani 0.1454(9) 1 d PD A 5 C34' C 0.2443(8) -0.339(3) 0.7561(18) 0.0306(13) Uani 0.1454(9) 1 d PD A 5 H34D H 0.2353 -0.2884 0.7122 0.046 Uiso 0.1454(9) 1 calc PR A 5 H34E H 0.2175 -0.3504 0.7889 0.046 Uiso 0.1454(9) 1 calc PR A 5 H34F H 0.2557 -0.4211 0.7395 0.046 Uiso 0.1454(9) 1 calc PR A 5 C35' C 0.3712(10) -0.187(3) 0.9380(14) 0.0415(17) Uani 0.1454(9) 1 d PD A 5 H35D H 0.3876 -0.1073 0.9298 0.062 Uiso 0.1454(9) 1 calc PR A 5 H35E H 0.3931 -0.2573 0.9372 0.062 Uiso 0.1454(9) 1 calc PR A 5 H35F H 0.3556 -0.1844 0.9868 0.062 Uiso 0.1454(9) 1 calc PR A 5 C36' C 0.2191(7) 0.279(3) 0.7422(17) 0.0273(11) Uani 0.1454(9) 1 d PD A 5 H36D H 0.2117 0.2294 0.6972 0.041 Uiso 0.1454(9) 1 calc PR A 5 H36E H 0.2269 0.3654 0.7277 0.041 Uiso 0.1454(9) 1 calc PR A 5 H36F H 0.1925 0.2795 0.7761 0.041 Uiso 0.1454(9) 1 calc PR A 5 C37' C 0.3355(10) 0.234(3) 0.9434(12) 0.0304(12) Uani 0.1454(9) 1 d PD A 5 H37D H 0.3608 0.1757 0.9540 0.046 Uiso 0.1454(9) 1 calc PR A 5 H37E H 0.3131 0.2314 0.9845 0.046 Uiso 0.1454(9) 1 calc PR A 5 H37F H 0.3477 0.3204 0.9388 0.046 Uiso 0.1454(9) 1 calc PR A 5 C38' C 0.3655(12) 0.103(3) 0.5430(12) 0.0333(13) Uani 0.1454(9) 1 d PD A 5 H38D H 0.3330 0.0828 0.5349 0.050 Uiso 0.1454(9) 1 calc PR A 5 H38E H 0.3846 0.0501 0.5102 0.050 Uiso 0.1454(9) 1 calc PR A 5 H38F H 0.3709 0.1921 0.5314 0.050 Uiso 0.1454(9) 1 calc PR A 5 C39' C 0.4571(9) 0.071(3) 0.7866(18) 0.0361(14) Uani 0.1454(9) 1 d PD A 5 H39D H 0.4450 0.0417 0.8350 0.054 Uiso 0.1454(9) 1 calc PR A 5 H39E H 0.4682 0.1576 0.7915 0.054 Uiso 0.1454(9) 1 calc PR A 5 H39F H 0.4826 0.0158 0.7711 0.054 Uiso 0.1454(9) 1 calc PR A 5 C40' C 0.2142(8) -0.019(2) 0.7013(14) 0.0207(11) Uani 0.1454(9) 1 d PD A 5 C41' C 0.1799(10) -0.007(2) 0.6467(15) 0.0235(12) Uani 0.1454(9) 1 d PD A 5 F5' F 0.189(2) 0.003(3) 0.5719(16) 0.0356(12) Uani 0.1454(9) 1 d PD A 5 C42' C 0.1331(10) -0.004(2) 0.6635(16) 0.0268(13) Uani 0.1454(9) 1 d PD A 5 F6' F 0.1022(15) 0.009(4) 0.607(2) 0.0384(12) Uani 0.1454(9) 1 d PD A 5 C43' C 0.1185(9) -0.0124(19) 0.7363(15) 0.0259(12) Uani 0.1454(9) 1 d PD A 5 F7' F 0.0730(9) -0.009(3) 0.751(3) 0.0349(11) Uani 0.1454(9) 1 d PD A 5 C44' C 0.1499(7) -0.0248(13) 0.7933(12) 0.0225(10) Uani 0.1454(9) 1 d PD A 5 F8' F 0.1360(7) -0.0335(18) 0.8664(11) 0.0304(7) Uani 0.1454(9) 1 d PD A 5 C45' C 0.1956(7) -0.0278(16) 0.7746(14) 0.0191(9) Uani 0.1454(9) 1 d PD A 5 H45' H 0.2170 -0.0363 0.8147 0.023 Uiso 0.1454(9) 1 calc PR A 5 P2' P 0.2797(3) -0.1409(7) 0.5800(4) 0.0198(3) Uani 0.1454(9) 1 d PD A 5 C46' C 0.3308(7) -0.233(3) 0.568(2) 0.0316(13) Uani 0.1454(9) 1 d PD A 5 H46D H 0.3379 -0.2775 0.6144 0.047 Uiso 0.1454(9) 1 calc PR A 5 H46E H 0.3565 -0.1768 0.5547 0.047 Uiso 0.1454(9) 1 calc PR A 5 H46F H 0.3260 -0.2940 0.5272 0.047 Uiso 0.1454(9) 1 calc PR A 5 C47' C 0.2732(11) -0.070(3) 0.4863(13) 0.0275(11) Uani 0.1454(9) 1 d PD A 5 H47D H 0.2451 -0.0183 0.4851 0.041 Uiso 0.1454(9) 1 calc PR A 5 H47E H 0.2711 -0.1365 0.4484 0.041 Uiso 0.1454(9) 1 calc PR A 5 H47F H 0.2999 -0.0160 0.4755 0.041 Uiso 0.1454(9) 1 calc PR A 5 C48' C 0.2344(8) -0.260(3) 0.5700(19) 0.0297(12) Uani 0.1454(9) 1 d PD A 5 H48D H 0.2043 -0.2188 0.5736 0.045 Uiso 0.1454(9) 1 calc PR A 5 H48E H 0.2374 -0.3229 0.6100 0.045 Uiso 0.1454(9) 1 calc PR A 5 H48F H 0.2373 -0.3012 0.5210 0.045 Uiso 0.1454(9) 1 calc PR A 5 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 0.01543(11) 0.01807(12) 0.01528(14) -0.00060(13) 0.00017(13) -0.00057(11) N1 0.0116(18) 0.0214(19) 0.0183(19) -0.0024(14) -0.0037(16) -0.0006(16) N2 0.0132(18) 0.025(2) 0.0119(17) -0.0012(14) -0.0038(15) -0.0001(15) N3 0.023(2) 0.025(2) 0.014(2) 0.0036(16) -0.0034(16) 0.0000(16) N4 0.024(2) 0.014(2) 0.016(2) -0.0022(17) -0.0038(15) 0.0022(17) N5 0.0191(16) 0.0202(16) 0.014(2) 0.0018(16) -0.0018(15) -0.0011(14) N6 0.0157(17) 0.022(2) 0.020(2) 0.0016(16) -0.0016(14) 0.0028(15) B1 0.019(2) 0.022(3) 0.018(3) 0.004(2) -0.0027(19) 0.004(2) C1 0.026(3) 0.024(2) 0.023(3) -0.0012(19) -0.001(2) 0.004(2) C2 0.030(3) 0.024(3) 0.021(2) -0.005(2) -0.003(2) 0.002(2) C3 0.022(2) 0.027(3) 0.018(2) -0.0031(18) -0.0039(18) -0.0006(19) C4 0.020(2) 0.017(2) 0.034(3) -0.0010(19) 0.006(2) -0.0002(19) C5 0.026(3) 0.021(2) 0.031(3) 0.004(2) 0.013(2) 0.003(2) C6 0.022(3) 0.018(2) 0.025(3) 0.0023(19) 0.002(2) 0.0030(18) C7 0.025(2) 0.020(2) 0.024(2) 0.000(2) 0.008(2) 0.0049(16) C8 0.016(2) 0.034(3) 0.025(3) 0.002(2) 0.0061(18) 0.007(2) C9 0.015(2) 0.022(2) 0.027(3) 0.0048(19) -0.0014(18) 0.0025(17) C10 0.030(3) 0.025(3) 0.029(3) -0.005(2) -0.003(2) 0.007(2) C11 0.027(3) 0.036(3) 0.024(3) -0.004(2) -0.006(2) 0.000(2) C12 0.024(3) 0.022(3) 0.038(3) -0.006(2) 0.006(2) -0.0060(19) C13 0.038(3) 0.034(3) 0.029(3) 0.010(2) -0.004(3) 0.002(2) C14 0.034(3) 0.035(3) 0.021(3) -0.007(2) 0.005(2) 0.008(2) C15 0.021(2) 0.049(4) 0.032(3) 0.004(3) -0.005(2) 0.005(2) C16 0.0188(17) 0.010(2) 0.017(2) -0.0004(16) 0.0020(15) 0.0019(19) C17 0.026(2) 0.025(2) 0.018(2) -0.0067(18) 0.0041(17) -0.0021(19) F1 0.0235(16) 0.059(3) 0.020(2) -0.0060(15) -0.0038(13) -0.0024(18) C18 0.0167(17) 0.029(2) 0.032(4) -0.0026(18) -0.0050(17) -0.0061(17) F2 0.0206(13) 0.048(3) 0.0310(19) -0.003(2) -0.0049(16) -0.002(2) C19 0.0152(19) 0.021(2) 0.033(3) 0.0011(19) 0.0012(17) 0.0008(17) F3 0.0156(13) 0.0334(16) 0.041(2) -0.0048(13) -0.0001(13) 0.0004(11) C20 0.023(2) 0.018(3) 0.019(2) -0.0019(19) 0.0011(16) 0.005(2) F4 0.0261(15) 0.042(2) 0.0189(16) 0.0029(17) 0.0078(11) 0.0102(18) C21 0.020(2) 0.017(2) 0.025(3) 0.003(2) -0.0027(18) 0.0015(19) P1 0.0182(6) 0.0224(7) 0.0199(7) 0.0014(5) -0.0019(5) 0.0003(5) C22 0.028(3) 0.028(3) 0.023(3) 0.008(2) -0.002(2) -0.006(2) C23 0.029(3) 0.024(3) 0.032(3) 0.006(2) -0.005(2) 0.007(2) C24 0.024(2) 0.039(3) 0.019(3) 0.000(2) -0.0002(19) 0.003(2) B1' 0.019(2) 0.022(3) 0.018(3) 0.004(2) -0.0027(19) 0.004(2) N1' 0.023(2) 0.025(2) 0.014(2) 0.0036(16) -0.0034(16) 0.0000(16) N2' 0.024(2) 0.014(2) 0.016(2) -0.0022(17) -0.0038(15) 0.0022(17) C3' 0.022(3) 0.018(2) 0.025(3) 0.0023(19) 0.002(2) 0.0030(18) C2' 0.026(3) 0.021(2) 0.031(3) 0.004(2) 0.013(2) 0.003(2) C1' 0.020(2) 0.017(2) 0.034(3) -0.0010(19) 0.006(2) -0.0002(19) N3' 0.0116(18) 0.0214(19) 0.0183(19) -0.0024(14) -0.0037(16) -0.0006(16) N4' 0.0132(18) 0.025(2) 0.0119(17) -0.0012(14) -0.0038(15) -0.0001(15) C6' 0.022(2) 0.027(3) 0.018(2) -0.0031(18) -0.0039(18) -0.0006(19) C5' 0.030(3) 0.024(3) 0.021(2) -0.005(2) -0.003(2) 0.002(2) C4' 0.026(3) 0.024(2) 0.023(3) -0.0012(19) -0.001(2) 0.004(2) N5' 0.0191(16) 0.0202(16) 0.014(2) 0.0018(16) -0.0018(15) -0.0011(14) N6' 0.0157(17) 0.022(2) 0.020(2) 0.0016(16) -0.0016(14) 0.0028(15) C9' 0.015(2) 0.022(2) 0.027(3) 0.0048(19) -0.0014(18) 0.0025(17) C8' 0.016(2) 0.034(3) 0.025(3) 0.002(2) 0.0061(18) 0.007(2) C7' 0.025(2) 0.020(2) 0.024(2) 0.000(2) 0.008(2) 0.0049(16) C10' 0.024(3) 0.022(3) 0.038(3) -0.006(2) 0.006(2) -0.0060(19) C11' 0.038(3) 0.034(3) 0.029(3) 0.010(2) -0.004(3) 0.002(2) C12' 0.030(3) 0.025(3) 0.029(3) -0.005(2) -0.003(2) 0.007(2) C13' 0.027(3) 0.036(3) 0.024(3) -0.004(2) -0.006(2) 0.000(2) C14' 0.034(3) 0.035(3) 0.021(3) -0.007(2) 0.005(2) 0.008(2) C15' 0.021(2) 0.049(4) 0.032(3) 0.004(3) -0.005(2) 0.005(2) C16' 0.0188(17) 0.010(2) 0.017(2) -0.0004(16) 0.0020(15) 0.0019(19) C17' 0.026(2) 0.025(2) 0.018(2) -0.0067(18) 0.0041(17) -0.0021(19) F1' 0.0235(16) 0.059(3) 0.020(2) -0.0060(15) -0.0038(13) -0.0024(18) C18' 0.0167(17) 0.029(2) 0.032(4) -0.0026(18) -0.0050(17) -0.0061(17) F2' 0.0206(13) 0.048(3) 0.0310(19) -0.003(2) -0.0049(16) -0.002(2) C19' 0.0152(19) 0.021(2) 0.033(3) 0.0011(19) 0.0012(17) 0.0008(17) F3' 0.0156(13) 0.0334(16) 0.041(2) -0.0048(13) -0.0001(13) 0.0004(11) C20' 0.023(2) 0.018(3) 0.019(2) -0.0019(19) 0.0011(16) 0.005(2) F4' 0.0261(15) 0.042(2) 0.0189(16) 0.0029(17) 0.0078(11) 0.0102(18) C21' 0.020(2) 0.017(2) 0.025(3) 0.003(2) -0.0027(18) 0.0015(19) P1' 0.0182(6) 0.0224(7) 0.0199(7) 0.0014(5) -0.0019(5) 0.0003(5) C22' 0.028(3) 0.028(3) 0.023(3) 0.008(2) -0.002(2) -0.006(2) C23' 0.029(3) 0.024(3) 0.032(3) 0.006(2) -0.005(2) 0.007(2) C24' 0.024(2) 0.039(3) 0.019(3) 0.000(2) -0.0002(19) 0.003(2) Rh2 0.01644(15) 0.0176(2) 0.01625(16) -0.0020(2) 0.00132(15) -0.0009(2) N7 0.0143(17) 0.018(2) 0.016(2) -0.0046(15) -0.0056(15) 0.0046(14) N8 0.013(2) 0.022(2) 0.019(2) -0.0031(16) -0.0041(16) -0.0028(15) N9 0.0164(19) 0.0133(19) 0.025(2) -0.0013(14) 0.0063(16) -0.0010(14) N10 0.019(2) 0.0178(18) 0.022(2) 0.0029(15) 0.0037(17) -0.0010(16) N11 0.0235(17) 0.0163(18) 0.022(2) -0.0061(18) 0.0075(17) 0.0071(15) N12 0.0162(16) 0.016(2) 0.024(2) 0.0023(17) 0.0011(14) 0.0029(16) B2 0.017(3) 0.029(3) 0.022(3) 0.002(2) -0.0027(19) 0.000(2) C25 0.014(2) 0.023(2) 0.017(2) 0.0015(16) 0.0009(16) 0.0003(17) C26 0.030(3) 0.020(2) 0.020(2) -0.0060(18) -0.002(2) -0.0002(19) C27 0.018(2) 0.023(2) 0.015(2) -0.0031(17) -0.0006(17) -0.0053(18) C28 0.032(3) 0.020(2) 0.029(3) -0.002(2) 0.014(2) 0.000(2) C29 0.035(3) 0.019(2) 0.037(3) 0.005(2) 0.016(2) 0.005(2) C30 0.044(3) 0.020(2) 0.019(2) 0.0033(18) 0.005(2) 0.010(2) C31 0.020(2) 0.025(2) 0.019(2) -0.0006(19) 0.0039(17) 0.0047(17) C32 0.018(2) 0.028(3) 0.042(3) -0.005(2) 0.008(2) 0.0079(19) C33 0.017(2) 0.028(3) 0.028(3) 0.006(2) 0.0050(18) 0.0048(19) C34 0.023(3) 0.030(3) 0.029(3) -0.003(2) -0.005(2) 0.005(2) C35 0.029(3) 0.035(3) 0.027(3) -0.006(2) -0.003(2) -0.004(2) C36 0.024(3) 0.021(2) 0.047(4) -0.007(2) 0.012(2) -0.0061(19) C37 0.068(5) 0.038(3) 0.018(3) 0.010(2) 0.006(3) 0.014(3) C38 0.027(3) 0.046(3) 0.028(3) -0.006(2) 0.008(2) 0.010(2) C39 0.019(2) 0.045(4) 0.044(4) 0.008(3) -0.006(2) 0.007(2) C40 0.0161(19) 0.018(2) 0.028(3) -0.0027(19) -0.0013(18) -0.0039(18) C41 0.023(2) 0.026(3) 0.021(3) 0.000(2) -0.0067(19) -0.001(2) F5 0.030(3) 0.056(2) 0.020(2) -0.0050(14) -0.0042(16) -0.0064(15) C42 0.022(2) 0.028(3) 0.031(3) 0.0024(18) -0.0095(19) -0.0062(19) F6 0.021(2) 0.049(3) 0.045(2) 0.001(2) -0.0204(18) -0.0024(18) C43 0.016(2) 0.026(3) 0.036(3) 0.003(2) -0.0002(19) 0.001(2) F7 0.0131(14) 0.034(3) 0.058(3) 0.006(2) 0.0065(15) -0.0005(14) C44 0.018(2) 0.021(2) 0.028(3) 0.000(2) 0.0078(18) 0.0014(19) F8 0.0258(15) 0.0360(18) 0.0292(19) 0.0004(15) 0.0115(13) 0.0033(14) C45 0.0157(19) 0.022(2) 0.019(2) -0.0055(19) 0.0011(17) 0.0006(18) P2 0.0185(6) 0.0262(6) 0.0146(6) -0.0002(5) -0.0006(4) -0.0001(5) C46 0.028(3) 0.039(3) 0.028(3) 0.009(2) 0.002(2) -0.004(2) C47 0.029(3) 0.039(3) 0.014(2) -0.004(2) -0.001(2) -0.001(2) C48 0.031(3) 0.037(3) 0.022(3) 0.000(2) -0.001(2) 0.006(2) Rh2' 0.01644(15) 0.0176(2) 0.01625(16) -0.0020(2) 0.00132(15) -0.0009(2) B2' 0.017(3) 0.029(3) 0.022(3) 0.002(2) -0.0027(19) 0.000(2) N7' 0.0164(19) 0.0133(19) 0.025(2) -0.0013(14) 0.0063(16) -0.0010(14) N8' 0.019(2) 0.0178(18) 0.022(2) 0.0029(15) 0.0037(17) -0.0010(16) C27' 0.044(3) 0.020(2) 0.019(2) 0.0033(18) 0.005(2) 0.010(2) C26' 0.035(3) 0.019(2) 0.037(3) 0.005(2) 0.016(2) 0.005(2) C25' 0.032(3) 0.020(2) 0.029(3) -0.002(2) 0.014(2) 0.000(2) N9' 0.0143(17) 0.018(2) 0.016(2) -0.0046(15) -0.0056(15) 0.0046(14) N10' 0.013(2) 0.022(2) 0.019(2) -0.0031(16) -0.0041(16) -0.0028(15) C30' 0.018(2) 0.023(2) 0.015(2) -0.0031(17) -0.0006(17) -0.0053(18) C29' 0.030(3) 0.020(2) 0.020(2) -0.0060(18) -0.002(2) -0.0002(19) C28' 0.014(2) 0.023(2) 0.017(2) 0.0015(16) 0.0009(16) 0.0003(17) N11' 0.0235(17) 0.0163(18) 0.022(2) -0.0061(18) 0.0075(17) 0.0071(15) N12' 0.0162(16) 0.016(2) 0.024(2) 0.0023(17) 0.0011(14) 0.0029(16) C33' 0.017(2) 0.028(3) 0.028(3) 0.006(2) 0.0050(18) 0.0048(19) C32' 0.018(2) 0.028(3) 0.042(3) -0.005(2) 0.008(2) 0.0079(19) C31' 0.020(2) 0.025(2) 0.019(2) -0.0006(19) 0.0039(17) 0.0047(17) C34' 0.024(3) 0.021(2) 0.047(4) -0.007(2) 0.012(2) -0.0061(19) C35' 0.068(5) 0.038(3) 0.018(3) 0.010(2) 0.006(3) 0.014(3) C36' 0.023(3) 0.030(3) 0.029(3) -0.003(2) -0.005(2) 0.005(2) C37' 0.029(3) 0.035(3) 0.027(3) -0.006(2) -0.003(2) -0.004(2) C38' 0.027(3) 0.046(3) 0.028(3) -0.006(2) 0.008(2) 0.010(2) C39' 0.019(2) 0.045(4) 0.044(4) 0.008(3) -0.006(2) 0.007(2) C40' 0.0161(19) 0.018(2) 0.028(3) -0.0027(19) -0.0013(18) -0.0039(18) C41' 0.023(2) 0.026(3) 0.021(3) 0.000(2) -0.0067(19) -0.001(2) F5' 0.030(3) 0.056(2) 0.020(2) -0.0050(14) -0.0042(16) -0.0064(15) C42' 0.022(2) 0.028(3) 0.031(3) 0.0024(18) -0.0095(19) -0.0062(19) F6' 0.021(2) 0.049(3) 0.045(2) 0.001(2) -0.0204(18) -0.0024(18) C43' 0.016(2) 0.026(3) 0.036(3) 0.003(2) -0.0002(19) 0.001(2) F7' 0.0131(14) 0.034(3) 0.058(3) 0.006(2) 0.0065(15) -0.0005(14) C44' 0.018(2) 0.021(2) 0.028(3) 0.000(2) 0.0078(18) 0.0014(19) F8' 0.0258(15) 0.0360(18) 0.0292(19) 0.0004(15) 0.0115(13) 0.0033(14) C45' 0.0157(19) 0.022(2) 0.019(2) -0.0055(19) 0.0011(17) 0.0006(18) P2' 0.0185(6) 0.0262(6) 0.0146(6) -0.0002(5) -0.0006(4) -0.0001(5) C46' 0.028(3) 0.039(3) 0.028(3) 0.009(2) 0.002(2) -0.004(2) C47' 0.029(3) 0.039(3) 0.014(2) -0.004(2) -0.001(2) -0.001(2) C48' 0.031(3) 0.037(3) 0.022(3) 0.000(2) -0.001(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C16 2.030(5) . ? Rh1 C16' 2.09(3) . ? Rh1 N3 2.117(5) . ? Rh1 N3' 2.121(7) . ? Rh1 N5' 2.145(6) . ? Rh1 N5 2.149(4) . ? Rh1 P1 2.2552(16) . ? Rh1 P1' 2.256(5) . ? Rh1 N1' 2.265(6) . ? Rh1 N1 2.268(4) . ? N1 C1 1.333(6) . ? N1 N2 1.374(5) . ? N2 C3 1.361(6) . ? N2 B1 1.525(5) . ? N3 C4 1.338(7) . ? N3 N4 1.365(6) . ? N4 C6 1.356(7) . ? N4 B1 1.534(6) . ? N5 C7 1.349(6) . ? N5 N6 1.380(6) . ? N6 C9 1.344(6) . ? N6 B1 1.538(5) . ? B1 H1 1.0000 . ? C1 C2 1.391(7) . ? C1 C10 1.493(6) . ? C2 C3 1.365(7) . ? C2 H2 0.9500 . ? C3 C11 1.496(5) . ? C4 C5 1.405(8) . ? C4 C12 1.494(6) . ? C5 C6 1.358(7) . ? C5 H5 0.9500 . ? C6 C13 1.499(6) . ? C7 C8 1.386(7) . ? C7 C14 1.491(6) . ? C8 C9 1.368(7) . ? C8 H8 0.9500 . ? C9 C15 1.493(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.351(8) . ? C16 C21 1.408(7) . ? C17 F1 1.373(7) . ? C17 C18 1.376(7) . ? C18 F2 1.349(7) . ? C18 C19 1.374(9) . ? C19 F3 1.357(6) . ? C19 C20 1.369(8) . ? C20 F4 1.350(6) . ? C20 C21 1.377(7) . ? C21 H21 0.9500 . ? P1 C22 1.813(5) . ? P1 C24 1.833(6) . ? P1 C23 1.837(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? B1' N2' 1.531(9) . ? B1' N4' 1.531(9) . ? B1' N6' 1.534(9) . ? B1' H1' 1.0000 . ? N1' C1' 1.312(18) . ? N1' N2' 1.381(19) . ? N2' C3' 1.359(19) . ? C3' C2' 1.352(19) . ? C3' C11' 1.494(8) . ? C2' C1' 1.400(19) . ? C2' H2' 0.9500 . ? C1' C10' 1.491(8) . ? N3' C4' 1.350(18) . ? N3' N4' 1.371(17) . ? N4' C6' 1.370(18) . ? C6' C5' 1.360(19) . ? C6' C13' 1.494(8) . ? C5' C4' 1.413(19) . ? C5' H5' 0.9500 . ? C4' C12' 1.492(8) . ? N5' C7' 1.336(17) . ? N5' N6' 1.397(17) . ? N6' C9' 1.328(17) . ? C9' C8' 1.370(18) . ? C9' C15' 1.491(8) . ? C8' C7' 1.361(18) . ? C8' H8' 0.9500 . ? C7' C14' 1.494(8) . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C12' H12D 0.9800 . ? C12' H12E 0.9800 . ? C12' H12F 0.9800 . ? C13' H13D 0.9800 . ? C13' H13E 0.9800 . ? C13' H13F 0.9800 . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C15' H15D 0.9800 . ? C15' H15E 0.9800 . ? C15' H15F 0.9800 . ? C16' C17' 1.351(17) . ? C16' C21' 1.404(18) . ? C17' F1' 1.373(17) . ? C17' C18' 1.375(16) . ? C18' F2' 1.348(17) . ? C18' C19' 1.375(17) . ? C19' F3' 1.356(16) . ? C19' C20' 1.369(17) . ? C20' F4' 1.345(17) . ? C20' C21' 1.374(17) . ? C21' H21' 0.9500 . ? P1' C22' 1.808(17) . ? P1' C23' 1.821(17) . ? P1' C24' 1.856(17) . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23' H23D 0.9800 . ? C23' H23E 0.9800 . ? C23' H23F 0.9800 . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? Rh2 C40 2.026(5) . ? Rh2 N9 2.102(4) . ? Rh2 N11 2.156(4) . ? Rh2 N7 2.247(4) . ? Rh2 P2 2.2658(16) . ? N7 C25 1.333(6) . ? N7 N8 1.387(6) . ? N8 C27 1.344(6) . ? N8 B2 1.524(5) . ? N9 C28 1.347(6) . ? N9 N10 1.384(6) . ? N10 C30 1.351(6) . ? N10 B2 1.534(5) . ? N11 C31 1.322(6) . ? N11 N12 1.391(7) . ? N12 C33 1.343(6) . ? N12 B2 1.529(6) . ? B2 H2A 1.0000 . ? C25 C26 1.389(7) . ? C25 C34 1.501(5) . ? C26 C27 1.365(7) . ? C26 H26 0.9500 . ? C27 C35 1.498(6) . ? C28 C29 1.370(8) . ? C28 C36 1.497(6) . ? C29 C30 1.381(8) . ? C29 H29 0.9500 . ? C30 C37 1.504(6) . ? C31 C32 1.394(7) . ? C31 C38 1.498(6) . ? C32 C33 1.366(8) . ? C32 H32 0.9500 . ? C33 C39 1.503(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.395(7) . ? C40 C45 1.409(7) . ? C41 F5 1.358(7) . ? C41 C42 1.392(8) . ? C42 F6 1.352(7) . ? C42 C43 1.365(9) . ? C43 F7 1.356(6) . ? C43 C44 1.374(8) . ? C44 F8 1.365(6) . ? C44 C45 1.376(6) . ? C45 H45 0.9500 . ? P2 C46 1.819(6) . ? P2 C48 1.819(6) . ? P2 C47 1.834(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? Rh2' N9' 1.870(9) . ? Rh2' C40' 1.95(2) . ? Rh2' N11' 2.058(8) . ? Rh2' P2' 2.263(5) . ? Rh2' N7' 2.442(8) . ? B2' N10' 1.528(8) . ? B2' N8' 1.528(9) . ? B2' N12' 1.528(8) . ? B2' H2B 1.0000 . ? N7' C25' 1.301(17) . ? N7' N8' 1.353(18) . ? N8' C27' 1.351(18) . ? C27' C26' 1.378(19) . ? C27' C35' 1.500(8) . ? C26' C25' 1.390(19) . ? C26' H26' 0.9500 . ? C25' C34' 1.499(8) . ? N9' C28' 1.408(17) . ? N9' N10' 1.449(18) . ? N10' C30' 1.357(18) . ? C30' C29' 1.378(19) . ? C30' C37' 1.503(8) . ? C29' C28' 1.385(19) . ? C29' H29' 0.9500 . ? C28' C36' 1.503(8) . ? N11' C31' 1.317(17) . ? N11' N12' 1.401(18) . ? N12' C33' 1.321(17) . ? C33' C32' 1.370(19) . ? C33' C39' 1.503(8) . ? C32' C31' 1.387(18) . ? C32' H32' 0.9500 . ? C31' C38' 1.502(8) . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C35' H35D 0.9800 . ? C35' H35E 0.9800 . ? C35' H35F 0.9800 . ? C36' H36D 0.9800 . ? C36' H36E 0.9800 . ? C36' H36F 0.9800 . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? C38' H38D 0.9800 . ? C38' H38E 0.9800 . ? C38' H38F 0.9800 . ? C39' H39D 0.9800 . ? C39' H39E 0.9800 . ? C39' H39F 0.9800 . ? C40' C41' 1.398(18) . ? C40' C45' 1.413(18) . ? C41' F5' 1.361(17) . ? C41' C42' 1.393(17) . ? C42' F6' 1.356(17) . ? C42' C43' 1.366(17) . ? C43' F7' 1.352(17) . ? C43' C44' 1.372(18) . ? C44' F8' 1.366(17) . ? C44' C45' 1.370(17) . ? C45' H45' 0.9500 . ? P2' C46' 1.787(17) . ? P2' C48' 1.830(17) . ? P2' C47' 1.841(17) . ? C46' H46D 0.9800 . ? C46' H46E 0.9800 . ? C46' H46F 0.9800 . ? C47' H47D 0.9800 . ? C47' H47E 0.9800 . ? C47' H47F 0.9800 . ? C48' H48D 0.9800 . ? C48' H48E 0.9800 . ? C48' H48F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N3 89.2(2) . . ? C16' Rh1 N3' 88.1(8) . . ? C16' Rh1 N5' 171.4(8) . . ? N3' Rh1 N5' 83.7(7) . . ? N3 Rh1 N5 81.7(2) . . ? C16 Rh1 P1 93.88(14) . . ? N3 Rh1 P1 173.28(19) . . ? N5 Rh1 P1 94.99(12) . . ? C16' Rh1 P1' 90.3(7) . . ? N3' Rh1 P1' 172.0(6) . . ? N5' Rh1 P1' 97.5(6) . . ? C16' Rh1 N1' 85.6(11) . . ? N3' Rh1 N1' 84.5(10) . . ? N5' Rh1 N1' 96.3(9) . . ? P1' Rh1 N1' 103.2(8) . . ? C16 Rh1 N1 92.97(16) . . ? N3 Rh1 N1 86.9(2) . . ? N5 Rh1 N1 88.42(15) . . ? P1 Rh1 N1 98.85(12) . . ? C1 N1 N2 106.6(4) . . ? C1 N1 Rh1 137.6(3) . . ? N2 N1 Rh1 114.8(3) . . ? C3 N2 N1 109.2(4) . . ? C3 N2 B1 129.4(4) . . ? N1 N2 B1 120.6(4) . . ? C4 N3 N4 107.0(4) . . ? C4 N3 Rh1 133.9(4) . . ? N4 N3 Rh1 119.0(4) . . ? C6 N4 N3 109.8(4) . . ? C6 N4 B1 130.6(5) . . ? N3 N4 B1 119.4(5) . . ? C7 N5 N6 105.5(4) . . ? C7 N5 Rh1 136.9(3) . . ? N6 N5 Rh1 117.3(3) . . ? C9 N6 N5 109.9(4) . . ? C9 N6 B1 128.6(4) . . ? N5 N6 B1 119.8(4) . . ? N2 B1 N4 110.4(4) . . ? N2 B1 N6 111.4(4) . . ? N4 B1 N6 108.1(4) . . ? N2 B1 H1 109.0 . . ? N4 B1 H1 109.0 . . ? N6 B1 H1 109.0 . . ? N1 C1 C2 110.1(4) . . ? N1 C1 C10 124.9(5) . . ? C2 C1 C10 125.0(5) . . ? C3 C2 C1 106.2(5) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? N2 C3 C2 107.9(4) . . ? N2 C3 C11 121.2(5) . . ? C2 C3 C11 130.9(5) . . ? N3 C4 C5 108.9(5) . . ? N3 C4 C12 122.9(5) . . ? C5 C4 C12 128.2(5) . . ? C6 C5 C4 106.6(5) . . ? C6 C5 H5 126.7 . . ? C4 C5 H5 126.7 . . ? N4 C6 C5 107.7(4) . . ? N4 C6 C13 120.8(5) . . ? C5 C6 C13 131.5(5) . . ? N5 C7 C8 110.3(5) . . ? N5 C7 C14 122.1(4) . . ? C8 C7 C14 127.5(5) . . ? C9 C8 C7 105.9(4) . . ? C9 C8 H8 127.0 . . ? C7 C8 H8 127.0 . . ? N6 C9 C8 108.3(4) . . ? N6 C9 C15 123.2(5) . . ? C8 C9 C15 128.5(5) . . ? C17 C16 C21 114.1(5) . . ? C17 C16 Rh1 127.9(4) . . ? C21 C16 Rh1 117.4(4) . . ? C16 C17 F1 119.6(6) . . ? C16 C17 C18 125.6(6) . . ? F1 C17 C18 114.8(6) . . ? F2 C18 C19 119.5(5) . . ? F2 C18 C17 121.5(6) . . ? C19 C18 C17 119.0(5) . . ? F3 C19 C20 121.3(6) . . ? F3 C19 C18 120.5(6) . . ? C20 C19 C18 118.2(5) . . ? F4 C20 C19 117.9(5) . . ? F4 C20 C21 120.9(5) . . ? C19 C20 C21 121.2(5) . . ? C20 C21 C16 121.9(5) . . ? C20 C21 H21 119.1 . . ? C16 C21 H21 119.1 . . ? C22 P1 C24 104.0(3) . . ? C22 P1 C23 100.1(3) . . ? C24 P1 C23 100.7(3) . . ? C22 P1 Rh1 112.03(18) . . ? C24 P1 Rh1 118.0(2) . . ? C23 P1 Rh1 119.4(2) . . ? N2' B1' N4' 102.0(18) . . ? N2' B1' N6' 118(2) . . ? N4' B1' N6' 107.1(16) . . ? N2' B1' H1' 109.7 . . ? N4' B1' H1' 109.7 . . ? N6' B1' H1' 109.7 . . ? C1' N1' N2' 109.4(14) . . ? C1' N1' Rh1 141(2) . . ? N2' N1' Rh1 108.6(16) . . ? C3' N2' N1' 106.1(13) . . ? C3' N2' B1' 127(2) . . ? N1' N2' B1' 127(2) . . ? C2' C3' N2' 110.1(16) . . ? C2' C3' C11' 126(2) . . ? N2' C3' C11' 124(3) . . ? C3' C2' C1' 105.7(16) . . ? C3' C2' H2' 127.2 . . ? C1' C2' H2' 127.2 . . ? N1' C1' C2' 108.8(15) . . ? N1' C1' C10' 124(3) . . ? C2' C1' C10' 127(2) . . ? C4' N3' N4' 108.0(12) . . ? C4' N3' Rh1 135.3(15) . . ? N4' N3' Rh1 116.7(13) . . ? C6' N4' N3' 108.6(13) . . ? C6' N4' B1' 130.7(19) . . ? N3' N4' B1' 120.4(19) . . ? C5' C6' N4' 108.4(15) . . ? C5' C6' C13' 137(2) . . ? N4' C6' C13' 115(2) . . ? C6' C5' C4' 106.8(15) . . ? C6' C5' H5' 126.6 . . ? C4' C5' H5' 126.6 . . ? N3' C4' C5' 108.1(14) . . ? N3' C4' C12' 121(2) . . ? C5' C4' C12' 131(2) . . ? C7' N5' N6' 106.7(11) . . ? C7' N5' Rh1 138.4(14) . . ? N6' N5' Rh1 114.6(12) . . ? C9' N6' N5' 108.8(13) . . ? C9' N6' B1' 129.1(18) . . ? N5' N6' B1' 121.1(18) . . ? N6' C9' C8' 107.7(15) . . ? N6' C9' C15' 121(2) . . ? C8' C9' C15' 131(2) . . ? C7' C8' C9' 107.9(16) . . ? C7' C8' H8' 126.0 . . ? C9' C8' H8' 126.0 . . ? N5' C7' C8' 108.9(15) . . ? N5' C7' C14' 119(2) . . ? C8' C7' C14' 132(2) . . ? C1' C10' H10D 109.5 . . ? C1' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C1' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C3' C11' H11D 109.5 . . ? C3' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C3' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C4' C12' H12D 109.5 . . ? C4' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C4' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C6' C13' H13D 109.5 . . ? C6' C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? C6' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? C7' C14' H14D 109.5 . . ? C7' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C7' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C9' C15' H15D 109.5 . . ? C9' C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C9' C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C17' C16' C21' 113.5(19) . . ? C17' C16' Rh1 128.2(18) . . ? C21' C16' Rh1 116.7(17) . . ? C16' C17' F1' 119(2) . . ? C16' C17' C18' 126(2) . . ? F1' C17' C18' 115(2) . . ? F2' C18' C19' 119(2) . . ? F2' C18' C17' 122(2) . . ? C19' C18' C17' 119.2(18) . . ? F3' C19' C20' 121(2) . . ? F3' C19' C18' 121(2) . . ? C20' C19' C18' 118.0(18) . . ? F4' C20' C19' 118(2) . . ? F4' C20' C21' 121(2) . . ? C19' C20' C21' 120.8(19) . . ? C20' C21' C16' 122.8(19) . . ? C20' C21' H21' 118.6 . . ? C16' C21' H21' 118.6 . . ? C22' P1' C23' 99.4(12) . . ? C22' P1' C24' 104.9(13) . . ? C23' P1' C24' 99.5(13) . . ? C22' P1' Rh1 109.6(11) . . ? C23' P1' Rh1 120.5(12) . . ? C24' P1' Rh1 120.0(11) . . ? P1' C22' H22D 109.5 . . ? P1' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? P1' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? P1' C23' H23D 109.5 . . ? P1' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? P1' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? P1' C24' H24D 109.5 . . ? P1' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? P1' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C40 Rh2 N9 86.61(19) . . ? C40 Rh2 N11 169.75(19) . . ? N9 Rh2 N11 83.36(17) . . ? C40 Rh2 N7 92.33(18) . . ? N9 Rh2 N7 86.43(17) . . ? N11 Rh2 N7 89.15(17) . . ? C40 Rh2 P2 93.82(16) . . ? N9 Rh2 P2 173.24(13) . . ? N11 Rh2 P2 95.90(14) . . ? N7 Rh2 P2 100.28(12) . . ? C25 N7 N8 105.0(4) . . ? C25 N7 Rh2 139.3(3) . . ? N8 N7 Rh2 115.6(3) . . ? C27 N8 N7 109.9(4) . . ? C27 N8 B2 130.9(5) . . ? N7 N8 B2 118.9(4) . . ? C28 N9 N10 107.0(4) . . ? C28 N9 Rh2 135.0(4) . . ? N10 N9 Rh2 118.0(3) . . ? C30 N10 N9 109.1(4) . . ? C30 N10 B2 131.2(5) . . ? N9 N10 B2 119.5(4) . . ? C31 N11 N12 105.7(4) . . ? C31 N11 Rh2 137.6(4) . . ? N12 N11 Rh2 116.3(3) . . ? C33 N12 N11 110.0(4) . . ? C33 N12 B2 128.6(5) . . ? N11 N12 B2 120.0(4) . . ? N8 B2 N12 111.5(4) . . ? N8 B2 N10 110.5(4) . . ? N12 B2 N10 109.1(4) . . ? N8 B2 H2A 108.5 . . ? N12 B2 H2A 108.5 . . ? N10 B2 H2A 108.5 . . ? N7 C25 C26 111.2(4) . . ? N7 C25 C34 123.3(4) . . ? C26 C25 C34 125.5(5) . . ? C27 C26 C25 105.5(4) . . ? C27 C26 H26 127.3 . . ? C25 C26 H26 127.3 . . ? N8 C27 C26 108.3(4) . . ? N8 C27 C35 121.6(5) . . ? C26 C27 C35 130.0(5) . . ? N9 C28 C29 109.1(5) . . ? N9 C28 C36 122.4(5) . . ? C29 C28 C36 128.4(5) . . ? C28 C29 C30 107.5(5) . . ? C28 C29 H29 126.3 . . ? C30 C29 H29 126.3 . . ? N10 C30 C29 107.3(5) . . ? N10 C30 C37 121.2(5) . . ? C29 C30 C37 131.4(5) . . ? N11 C31 C32 110.5(5) . . ? N11 C31 C38 122.2(5) . . ? C32 C31 C38 127.1(5) . . ? C33 C32 C31 106.3(5) . . ? C33 C32 H32 126.9 . . ? C31 C32 H32 126.9 . . ? N12 C33 C32 107.5(5) . . ? N12 C33 C39 124.0(5) . . ? C32 C33 C39 128.4(5) . . ? C41 C40 C45 115.1(5) . . ? C41 C40 Rh2 126.5(4) . . ? C45 C40 Rh2 117.7(4) . . ? F5 C41 C42 114.7(6) . . ? F5 C41 C40 121.9(6) . . ? C42 C41 C40 123.4(6) . . ? F6 C42 C43 120.4(6) . . ? F6 C42 C41 120.1(6) . . ? C43 C42 C41 119.4(5) . . ? F7 C43 C42 120.0(6) . . ? F7 C43 C44 120.9(6) . . ? C42 C43 C44 119.1(5) . . ? F8 C44 C43 118.6(5) . . ? F8 C44 C45 119.7(5) . . ? C43 C44 C45 121.8(5) . . ? C44 C45 C40 121.2(5) . . ? C44 C45 H45 119.4 . . ? C40 C45 H45 119.4 . . ? C46 P2 C48 100.6(3) . . ? C46 P2 C47 102.8(3) . . ? C48 P2 C47 99.3(3) . . ? C46 P2 Rh2 113.4(2) . . ? C48 P2 Rh2 120.1(2) . . ? C47 P2 Rh2 117.8(2) . . ? N9' Rh2' C40' 87.6(9) . . ? N9' Rh2' N11' 80.2(9) . . ? C40' Rh2' N11' 167.7(9) . . ? N9' Rh2' P2' 173.4(7) . . ? C40' Rh2' P2' 96.5(7) . . ? N11' Rh2' P2' 95.5(7) . . ? N9' Rh2' N7' 85.5(8) . . ? C40' Rh2' N7' 91.7(8) . . ? N11' Rh2' N7' 88.7(8) . . ? P2' Rh2' N7' 99.4(5) . . ? N10' B2' N8' 102.9(18) . . ? N10' B2' N12' 103.3(19) . . ? N8' B2' N12' 111.0(19) . . ? N10' B2' H2B 112.9 . . ? N8' B2' H2B 112.9 . . ? N12' B2' H2B 112.9 . . ? C25' N7' N8' 115.6(13) . . ? C25' N7' Rh2' 134.6(15) . . ? N8' N7' Rh2' 109.7(12) . . ? C27' N8' N7' 103.3(14) . . ? C27' N8' B2' 129(2) . . ? N7' N8' B2' 128(2) . . ? N8' C27' C26' 109.6(16) . . ? N8' C27' C35' 119(2) . . ? C26' C27' C35' 131(2) . . ? C27' C26' C25' 107.3(16) . . ? C27' C26' H26' 126.4 . . ? C25' C26' H26' 126.4 . . ? N7' C25' C26' 104.2(14) . . ? N7' C25' C34' 124(2) . . ? C26' C25' C34' 132(2) . . ? C28' N9' N10' 96.7(12) . . ? C28' N9' Rh2' 139.3(14) . . ? N10' N9' Rh2' 123.7(13) . . ? C30' N10' N9' 116.5(15) . . ? C30' N10' B2' 122.3(19) . . ? N9' N10' B2' 121(2) . . ? N10' C30' C29' 104.6(15) . . ? N10' C30' C37' 138(2) . . ? C29' C30' C37' 117(2) . . ? C30' C29' C28' 107.4(15) . . ? C30' C29' H29' 126.3 . . ? C28' C29' H29' 126.3 . . ? C29' C28' N9' 114.7(14) . . ? C29' C28' C36' 120(2) . . ? N9' C28' C36' 125(2) . . ? C31' N11' N12' 101.8(12) . . ? C31' N11' Rh2' 137.4(17) . . ? N12' N11' Rh2' 120.5(15) . . ? C33' N12' N11' 114.9(15) . . ? C33' N12' B2' 122(2) . . ? N11' N12' B2' 122(2) . . ? N12' C33' C32' 103.7(15) . . ? N12' C33' C39' 127(2) . . ? C32' C33' C39' 129(2) . . ? C33' C32' C31' 107.9(16) . . ? C33' C32' H32' 126.0 . . ? C31' C32' H32' 126.0 . . ? N11' C31' C32' 111.6(15) . . ? N11' C31' C38' 124(2) . . ? C32' C31' C38' 124(2) . . ? C25' C34' H34D 109.5 . . ? C25' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C25' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C27' C35' H35D 109.5 . . ? C27' C35' H35E 109.5 . . ? H35D C35' H35E 109.5 . . ? C27' C35' H35F 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C28' C36' H36D 109.5 . . ? C28' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C28' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C30' C37' H37D 109.5 . . ? C30' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C30' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C31' C38' H38D 109.5 . . ? C31' C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C31' C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C33' C39' H39D 109.5 . . ? C33' C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C33' C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C41' C40' C45' 112.1(18) . . ? C41' C40' Rh2' 123.9(17) . . ? C45' C40' Rh2' 123.7(17) . . ? F5' C41' C42' 114(2) . . ? F5' C41' C40' 123(2) . . ? C42' C41' C40' 123.2(19) . . ? F6' C42' C43' 120(2) . . ? F6' C42' C41' 119(2) . . ? C43' C42' C41' 120.3(18) . . ? F7' C43' C42' 119(2) . . ? F7' C43' C44' 120(2) . . ? C42' C43' C44' 120.1(18) . . ? F8' C44' C45' 121.2(19) . . ? F8' C44' C43' 120.9(18) . . ? C45' C44' C43' 117.8(18) . . ? C44' C45' C40' 126.3(19) . . ? C44' C45' H45' 116.8 . . ? C40' C45' H45' 116.8 . . ? C46' P2' C48' 102.2(14) . . ? C46' P2' C47' 101.4(13) . . ? C48' P2' C47' 96.8(13) . . ? C46' P2' Rh2' 115.4(12) . . ? C48' P2' Rh2' 120.2(11) . . ? C47' P2' Rh2' 117.4(11) . . ? P2' C46' H46D 109.5 . . ? P2' C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? P2' C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? P2' C47' H47D 109.5 . . ? P2' C47' H47E 109.5 . . ? H47D C47' H47E 109.5 . . ? P2' C47' H47F 109.5 . . ? H47D C47' H47F 109.5 . . ? H47E C47' H47F 109.5 . . ? P2' C48' H48D 109.5 . . ? P2' C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? P2' C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 N1 C1 36.9(6) . . . . ? N3 Rh1 N1 C1 125.9(6) . . . . ? N5 Rh1 N1 C1 -152.3(5) . . . . ? P1 Rh1 N1 C1 -57.5(5) . . . . ? C16 Rh1 N1 N2 -130.3(3) . . . . ? N3 Rh1 N1 N2 -41.3(4) . . . . ? N5 Rh1 N1 N2 40.5(3) . . . . ? P1 Rh1 N1 N2 135.3(3) . . . . ? C1 N1 N2 C3 -0.5(5) . . . . ? Rh1 N1 N2 C3 170.6(3) . . . . ? C1 N1 N2 B1 -171.1(4) . . . . ? Rh1 N1 N2 B1 -0.1(5) . . . . ? C16 Rh1 N3 C4 -45.4(7) . . . . ? N5 Rh1 N3 C4 132.8(7) . . . . ? P1 Rh1 N3 C4 72.0(17) . . . . ? N1 Rh1 N3 C4 -138.4(7) . . . . ? C16 Rh1 N3 N4 131.3(4) . . . . ? N5 Rh1 N3 N4 -50.5(4) . . . . ? P1 Rh1 N3 N4 -111.3(13) . . . . ? N1 Rh1 N3 N4 38.3(4) . . . . ? C4 N3 N4 C6 -1.5(6) . . . . ? Rh1 N3 N4 C6 -179.0(4) . . . . ? C4 N3 N4 B1 -176.7(5) . . . . ? Rh1 N3 N4 B1 5.8(6) . . . . ? C16 Rh1 N5 C7 -108.4(11) . . . . ? N3 Rh1 N5 C7 -120.0(5) . . . . ? P1 Rh1 N5 C7 54.1(5) . . . . ? N1 Rh1 N5 C7 152.9(5) . . . . ? C16 Rh1 N5 N6 63.2(12) . . . . ? N3 Rh1 N5 N6 51.6(3) . . . . ? P1 Rh1 N5 N6 -134.3(3) . . . . ? N1 Rh1 N5 N6 -35.6(3) . . . . ? C7 N5 N6 C9 -1.1(5) . . . . ? Rh1 N5 N6 C9 -175.1(3) . . . . ? C7 N5 N6 B1 165.4(4) . . . . ? Rh1 N5 N6 B1 -8.6(5) . . . . ? C3 N2 B1 N4 -108.5(6) . . . . ? N1 N2 B1 N4 60.0(6) . . . . ? C3 N2 B1 N6 131.4(5) . . . . ? N1 N2 B1 N6 -60.1(5) . . . . ? C6 N4 B1 N2 120.4(6) . . . . ? N3 N4 B1 N2 -65.5(6) . . . . ? C6 N4 B1 N6 -117.5(6) . . . . ? N3 N4 B1 N6 56.6(5) . . . . ? C9 N6 B1 N2 -129.2(5) . . . . ? N5 N6 B1 N2 67.1(5) . . . . ? C9 N6 B1 N4 109.3(6) . . . . ? N5 N6 B1 N4 -54.4(5) . . . . ? N2 N1 C1 C2 -0.5(6) . . . . ? Rh1 N1 C1 C2 -168.4(4) . . . . ? N2 N1 C1 C10 178.9(5) . . . . ? Rh1 N1 C1 C10 11.0(9) . . . . ? N1 C1 C2 C3 1.2(7) . . . . ? C10 C1 C2 C3 -178.1(5) . . . . ? N1 N2 C3 C2 1.3(6) . . . . ? B1 N2 C3 C2 170.8(5) . . . . ? N1 N2 C3 C11 179.5(5) . . . . ? B1 N2 C3 C11 -10.9(8) . . . . ? C1 C2 C3 N2 -1.5(6) . . . . ? C1 C2 C3 C11 -179.5(6) . . . . ? N4 N3 C4 C5 1.3(6) . . . . ? Rh1 N3 C4 C5 178.3(5) . . . . ? N4 N3 C4 C12 178.4(5) . . . . ? Rh1 N3 C4 C12 -4.7(10) . . . . ? N3 C4 C5 C6 -0.6(6) . . . . ? C12 C4 C5 C6 -177.5(5) . . . . ? N3 N4 C6 C5 1.1(6) . . . . ? B1 N4 C6 C5 175.7(5) . . . . ? N3 N4 C6 C13 -177.0(5) . . . . ? B1 N4 C6 C13 -2.5(9) . . . . ? C4 C5 C6 N4 -0.3(6) . . . . ? C4 C5 C6 C13 177.5(6) . . . . ? N6 N5 C7 C8 1.7(6) . . . . ? Rh1 N5 C7 C8 174.0(4) . . . . ? N6 N5 C7 C14 -176.3(4) . . . . ? Rh1 N5 C7 C14 -4.0(8) . . . . ? N5 C7 C8 C9 -1.8(6) . . . . ? C14 C7 C8 C9 176.1(5) . . . . ? N5 N6 C9 C8 0.0(6) . . . . ? B1 N6 C9 C8 -165.0(5) . . . . ? N5 N6 C9 C15 178.2(5) . . . . ? B1 N6 C9 C15 13.2(8) . . . . ? C7 C8 C9 N6 1.1(6) . . . . ? C7 C8 C9 C15 -177.0(5) . . . . ? N3 Rh1 C16 C17 122.6(5) . . . . ? N5 Rh1 C16 C17 111.1(11) . . . . ? P1 Rh1 C16 C17 -51.4(5) . . . . ? N1 Rh1 C16 C17 -150.5(5) . . . . ? N3 Rh1 C16 C21 -48.1(4) . . . . ? N5 Rh1 C16 C21 -59.6(12) . . . . ? P1 Rh1 C16 C21 137.8(3) . . . . ? N1 Rh1 C16 C21 38.7(4) . . . . ? C21 C16 C17 F1 179.8(5) . . . . ? Rh1 C16 C17 F1 8.8(8) . . . . ? C21 C16 C17 C18 -1.6(8) . . . . ? Rh1 C16 C17 C18 -172.7(4) . . . . ? C16 C17 C18 F2 179.5(6) . . . . ? F1 C17 C18 F2 -1.8(8) . . . . ? C16 C17 C18 C19 2.0(9) . . . . ? F1 C17 C18 C19 -179.4(5) . . . . ? F2 C18 C19 F3 0.5(8) . . . . ? C17 C18 C19 F3 178.1(5) . . . . ? F2 C18 C19 C20 -178.3(5) . . . . ? C17 C18 C19 C20 -0.7(8) . . . . ? F3 C19 C20 F4 -0.6(7) . . . . ? C18 C19 C20 F4 178.2(5) . . . . ? F3 C19 C20 C21 -179.4(5) . . . . ? C18 C19 C20 C21 -0.7(8) . . . . ? F4 C20 C21 C16 -177.9(4) . . . . ? C19 C20 C21 C16 1.0(8) . . . . ? C17 C16 C21 C20 0.1(7) . . . . ? Rh1 C16 C21 C20 172.2(4) . . . . ? C16 Rh1 P1 C22 -147.7(2) . . . . ? N3 Rh1 P1 C22 95.2(14) . . . . ? N5 Rh1 P1 C22 35.1(2) . . . . ? N1 Rh1 P1 C22 -54.1(2) . . . . ? C16 Rh1 P1 C24 91.6(2) . . . . ? N3 Rh1 P1 C24 -25.5(14) . . . . ? N5 Rh1 P1 C24 -85.7(2) . . . . ? N1 Rh1 P1 C24 -174.8(2) . . . . ? C16 Rh1 P1 C23 -31.2(3) . . . . ? N5 Rh1 P1 C23 151.6(3) . . . . ? N1 Rh1 P1 C23 62.4(3) . . . . ? C16' Rh1 N1' C1' -59(3) . . . . ? N3' Rh1 N1' C1' -147(3) . . . . ? N5' Rh1 N1' C1' 130(3) . . . . ? P1' Rh1 N1' C1' 31(3) . . . . ? C16' Rh1 N1' N2' 136.0(10) . . . . ? N3' Rh1 N1' N2' 47.5(9) . . . . ? N5' Rh1 N1' N2' -35.5(9) . . . . ? P1' Rh1 N1' N2' -134.8(7) . . . . ? C1' N1' N2' C3' 0.0(3) . . . . ? Rh1 N1' N2' C3' 170(2) . . . . ? C1' N1' N2' B1' -171(3) . . . . ? Rh1 N1' N2' B1' -0.3(15) . . . . ? N4' B1' N2' C3' 128(2) . . . . ? N6' B1' N2' C3' -115(3) . . . . ? N4' B1' N2' N1' -63(2) . . . . ? N6' B1' N2' N1' 54(2) . . . . ? N1' N2' C3' C2' -0.1(5) . . . . ? B1' N2' C3' C2' 171(3) . . . . ? N1' N2' C3' C11' -180.0(5) . . . . ? B1' N2' C3' C11' -9(3) . . . . ? N2' C3' C2' C1' 0.2(6) . . . . ? C11' C3' C2' C1' -180.0(5) . . . . ? N2' N1' C1' C2' 0.1(3) . . . . ? Rh1 N1' C1' C2' -165(3) . . . . ? N2' N1' C1' C10' 180.0(3) . . . . ? Rh1 N1' C1' C10' 15(3) . . . . ? C3' C2' C1' N1' -0.1(5) . . . . ? C3' C2' C1' C10' 179.9(4) . . . . ? C16' Rh1 N3' C4' 48.9(18) . . . . ? N5' Rh1 N3' C4' -128.3(18) . . . . ? P1' Rh1 N3' C4' -29(5) . . . . ? N1' Rh1 N3' C4' 134.7(18) . . . . ? C16' Rh1 N3' N4' -132.2(10) . . . . ? N5' Rh1 N3' N4' 50.6(9) . . . . ? P1' Rh1 N3' N4' 150(4) . . . . ? N1' Rh1 N3' N4' -46.4(10) . . . . ? C4' N3' N4' C6' 0.0(3) . . . . ? Rh1 N3' N4' C6' -179.2(15) . . . . ? C4' N3' N4' B1' 174.8(19) . . . . ? Rh1 N3' N4' B1' -4.3(13) . . . . ? N2' B1' N4' C6' -120(2) . . . . ? N6' B1' N4' C6' 115(2) . . . . ? N2' B1' N4' N3' 66.5(19) . . . . ? N6' B1' N4' N3' -58(2) . . . . ? N3' N4' C6' C5' 0.1(5) . . . . ? B1' N4' C6' C5' -174(2) . . . . ? N3' N4' C6' C13' 179.9(4) . . . . ? B1' N4' C6' C13' 6(2) . . . . ? N4' C6' C5' C4' -0.1(6) . . . . ? C13' C6' C5' C4' -179.9(6) . . . . ? N4' N3' C4' C5' 0.0(2) . . . . ? Rh1 N3' C4' C5' 178.9(19) . . . . ? N4' N3' C4' C12' -179.9(3) . . . . ? Rh1 N3' C4' C12' -1.0(19) . . . . ? C6' C5' C4' N3' 0.1(5) . . . . ? C6' C5' C4' C12' 180.0(4) . . . . ? C16' Rh1 N5' C7' 104(6) . . . . ? N3' Rh1 N5' C7' 122.5(17) . . . . ? P1' Rh1 N5' C7' -49.5(16) . . . . ? N1' Rh1 N5' C7' -153.8(17) . . . . ? C16' Rh1 N5' N6' -69(6) . . . . ? N3' Rh1 N5' N6' -50.5(8) . . . . ? P1' Rh1 N5' N6' 137.4(6) . . . . ? N1' Rh1 N5' N6' 33.2(11) . . . . ? C7' N5' N6' C9' 0.0(3) . . . . ? Rh1 N5' N6' C9' 175.2(13) . . . . ? C7' N5' N6' B1' -169.5(17) . . . . ? Rh1 N5' N6' B1' 5.7(13) . . . . ? N2' B1' N6' C9' 136(2) . . . . ? N4' B1' N6' C9' -110(2) . . . . ? N2' B1' N6' N5' -57(2) . . . . ? N4' B1' N6' N5' 57(2) . . . . ? N5' N6' C9' C8' 0.1(5) . . . . ? B1' N6' C9' C8' 168.5(19) . . . . ? N5' N6' C9' C15' -179.9(4) . . . . ? B1' N6' C9' C15' -12(2) . . . . ? N6' C9' C8' C7' -0.2(6) . . . . ? C15' C9' C8' C7' 179.9(5) . . . . ? N6' N5' C7' C8' -0.1(3) . . . . ? Rh1 N5' C7' C8' -173.5(17) . . . . ? N6' N5' C7' C14' 179.9(2) . . . . ? Rh1 N5' C7' C14' 6.5(18) . . . . ? C9' C8' C7' N5' 0.2(5) . . . . ? C9' C8' C7' C14' -179.8(4) . . . . ? N3' Rh1 C16' C17' -121.4(13) . . . . ? N5' Rh1 C16' C17' -103(6) . . . . ? P1' Rh1 C16' C17' 50.7(12) . . . . ? N1' Rh1 C16' C17' 154.0(14) . . . . ? N3' Rh1 C16' C21' 43.1(11) . . . . ? N5' Rh1 C16' C21' 62(7) . . . . ? P1' Rh1 C16' C21' -144.7(10) . . . . ? N1' Rh1 C16' C21' -41.5(12) . . . . ? C21' C16' C17' F1' 180.0(4) . . . . ? Rh1 C16' C17' F1' -15.1(16) . . . . ? C21' C16' C17' C18' 0.0(3) . . . . ? Rh1 C16' C17' C18' 164.9(16) . . . . ? C16' C17' C18' F2' 180.0(3) . . . . ? F1' C17' C18' F2' 0.0(5) . . . . ? C16' C17' C18' C19' 0.0(3) . . . . ? F1' C17' C18' C19' -180.0(4) . . . . ? F2' C18' C19' F3' 0.0(8) . . . . ? C17' C18' C19' F3' 180.0(5) . . . . ? F2' C18' C19' C20' 180.0(6) . . . . ? C17' C18' C19' C20' 0.0(7) . . . . ? F3' C19' C20' F4' -0.1(10) . . . . ? C18' C19' C20' F4' 179.9(6) . . . . ? F3' C19' C20' C21' -180.0(7) . . . . ? C18' C19' C20' C21' 0.1(10) . . . . ? F4' C20' C21' C16' -179.9(6) . . . . ? C19' C20' C21' C16' -0.1(10) . . . . ? C17' C16' C21' C20' 0.1(7) . . . . ? Rh1 C16' C21' C20' -166.7(15) . . . . ? C16' Rh1 P1' C22' 145.8(12) . . . . ? N3' Rh1 P1' C22' -136(4) . . . . ? N5' Rh1 P1' C22' -38.0(11) . . . . ? N1' Rh1 P1' C22' 60.3(13) . . . . ? C16' Rh1 P1' C23' 31.6(13) . . . . ? N3' Rh1 P1' C23' 110(4) . . . . ? N5' Rh1 P1' C23' -152.3(12) . . . . ? N1' Rh1 P1' C23' -54.0(14) . . . . ? C16' Rh1 P1' C24' -92.7(14) . . . . ? N3' Rh1 P1' C24' -15(4) . . . . ? N5' Rh1 P1' C24' 83.4(13) . . . . ? N1' Rh1 P1' C24' -178.3(14) . . . . ? C40 Rh2 N7 C25 -50.2(6) . . . . ? N9 Rh2 N7 C25 -136.6(5) . . . . ? N11 Rh2 N7 C25 140.0(5) . . . . ? P2 Rh2 N7 C25 44.1(5) . . . . ? C40 Rh2 N7 N8 132.3(4) . . . . ? N9 Rh2 N7 N8 45.9(4) . . . . ? N11 Rh2 N7 N8 -37.5(4) . . . . ? P2 Rh2 N7 N8 -133.4(3) . . . . ? C25 N7 N8 C27 1.9(6) . . . . ? Rh2 N7 N8 C27 -179.8(3) . . . . ? C25 N7 N8 B2 176.6(4) . . . . ? Rh2 N7 N8 B2 -5.0(6) . . . . ? C40 Rh2 N9 C28 48.6(5) . . . . ? N11 Rh2 N9 C28 -129.2(5) . . . . ? N7 Rh2 N9 C28 141.2(5) . . . . ? P2 Rh2 N9 C28 -45.2(13) . . . . ? C40 Rh2 N9 N10 -131.7(4) . . . . ? N11 Rh2 N9 N10 50.4(3) . . . . ? N7 Rh2 N9 N10 -39.2(3) . . . . ? P2 Rh2 N9 N10 134.5(9) . . . . ? C28 N9 N10 C30 -1.7(5) . . . . ? Rh2 N9 N10 C30 178.6(3) . . . . ? C28 N9 N10 B2 173.1(4) . . . . ? Rh2 N9 N10 B2 -6.6(5) . . . . ? C40 Rh2 N11 C31 108.6(12) . . . . ? N9 Rh2 N11 C31 120.6(5) . . . . ? N7 Rh2 N11 C31 -152.9(5) . . . . ? P2 Rh2 N11 C31 -52.7(5) . . . . ? C40 Rh2 N11 N12 -62.0(12) . . . . ? N9 Rh2 N11 N12 -50.1(3) . . . . ? N7 Rh2 N11 N12 36.4(3) . . . . ? P2 Rh2 N11 N12 136.7(3) . . . . ? C31 N11 N12 C33 0.7(5) . . . . ? Rh2 N11 N12 C33 174.1(3) . . . . ? C31 N11 N12 B2 -167.2(4) . . . . ? Rh2 N11 N12 B2 6.3(5) . . . . ? C27 N8 B2 N12 -122.0(6) . . . . ? N7 N8 B2 N12 64.5(6) . . . . ? C27 N8 B2 N10 116.4(6) . . . . ? N7 N8 B2 N10 -57.0(6) . . . . ? C33 N12 B2 N8 127.8(5) . . . . ? N11 N12 B2 N8 -66.8(5) . . . . ? C33 N12 B2 N10 -109.8(6) . . . . ? N11 N12 B2 N10 55.5(6) . . . . ? C30 N10 B2 N8 -119.7(6) . . . . ? N9 N10 B2 N8 66.8(6) . . . . ? C30 N10 B2 N12 117.3(6) . . . . ? N9 N10 B2 N12 -56.1(6) . . . . ? N8 N7 C25 C26 -1.0(6) . . . . ? Rh2 N7 C25 C26 -178.7(4) . . . . ? N8 N7 C25 C34 -179.6(5) . . . . ? Rh2 N7 C25 C34 2.7(8) . . . . ? N7 C25 C26 C27 -0.2(6) . . . . ? C34 C25 C26 C27 178.3(5) . . . . ? N7 N8 C27 C26 -2.1(6) . . . . ? B2 N8 C27 C26 -176.0(5) . . . . ? N7 N8 C27 C35 179.4(5) . . . . ? B2 N8 C27 C35 5.5(8) . . . . ? C25 C26 C27 N8 1.4(6) . . . . ? C25 C26 C27 C35 179.7(5) . . . . ? N10 N9 C28 C29 2.0(6) . . . . ? Rh2 N9 C28 C29 -178.3(4) . . . . ? N10 N9 C28 C36 -179.7(5) . . . . ? Rh2 N9 C28 C36 0.0(8) . . . . ? N9 C28 C29 C30 -1.6(6) . . . . ? C36 C28 C29 C30 -179.8(5) . . . . ? N9 N10 C30 C29 0.7(6) . . . . ? B2 N10 C30 C29 -173.3(5) . . . . ? N9 N10 C30 C37 179.9(5) . . . . ? B2 N10 C30 C37 5.9(8) . . . . ? C28 C29 C30 N10 0.5(6) . . . . ? C28 C29 C30 C37 -178.5(6) . . . . ? N12 N11 C31 C32 -1.1(6) . . . . ? Rh2 N11 C31 C32 -172.4(4) . . . . ? N12 N11 C31 C38 174.3(5) . . . . ? Rh2 N11 C31 C38 3.0(8) . . . . ? N11 C31 C32 C33 1.1(7) . . . . ? C38 C31 C32 C33 -174.0(6) . . . . ? N11 N12 C33 C32 0.0(6) . . . . ? B2 N12 C33 C32 166.5(5) . . . . ? N11 N12 C33 C39 -178.6(5) . . . . ? B2 N12 C33 C39 -12.1(9) . . . . ? C31 C32 C33 N12 -0.7(6) . . . . ? C31 C32 C33 C39 177.9(5) . . . . ? N9 Rh2 C40 C41 -122.2(5) . . . . ? N11 Rh2 C40 C41 -110.3(12) . . . . ? N7 Rh2 C40 C41 151.5(5) . . . . ? P2 Rh2 C40 C41 51.0(5) . . . . ? N9 Rh2 C40 C45 47.7(4) . . . . ? N11 Rh2 C40 C45 59.5(13) . . . . ? N7 Rh2 C40 C45 -38.6(4) . . . . ? P2 Rh2 C40 C45 -139.1(4) . . . . ? C45 C40 C41 F5 -178.3(5) . . . . ? Rh2 C40 C41 F5 -8.2(8) . . . . ? C45 C40 C41 C42 -0.2(8) . . . . ? Rh2 C40 C41 C42 169.8(4) . . . . ? F5 C41 C42 F6 0.3(8) . . . . ? C40 C41 C42 F6 -177.8(5) . . . . ? F5 C41 C42 C43 178.7(5) . . . . ? C40 C41 C42 C43 0.6(9) . . . . ? F6 C42 C43 F7 -2.4(8) . . . . ? C41 C42 C43 F7 179.2(5) . . . . ? F6 C42 C43 C44 177.6(5) . . . . ? C41 C42 C43 C44 -0.8(8) . . . . ? F7 C43 C44 F8 2.4(8) . . . . ? C42 C43 C44 F8 -177.6(5) . . . . ? F7 C43 C44 C45 -179.2(5) . . . . ? C42 C43 C44 C45 0.7(8) . . . . ? F8 C44 C45 C40 177.9(5) . . . . ? C43 C44 C45 C40 -0.4(8) . . . . ? C41 C40 C45 C44 0.2(8) . . . . ? Rh2 C40 C45 C44 -170.9(4) . . . . ? C40 Rh2 P2 C46 147.1(3) . . . . ? N9 Rh2 P2 C46 -119.5(10) . . . . ? N11 Rh2 P2 C46 -36.2(3) . . . . ? N7 Rh2 P2 C46 54.0(3) . . . . ? C40 Rh2 P2 C48 28.2(3) . . . . ? N9 Rh2 P2 C48 121.6(10) . . . . ? N11 Rh2 P2 C48 -155.0(3) . . . . ? N7 Rh2 P2 C48 -64.8(3) . . . . ? C40 Rh2 P2 C47 -92.9(3) . . . . ? N9 Rh2 P2 C47 0.5(10) . . . . ? N11 Rh2 P2 C47 83.9(2) . . . . ? N7 Rh2 P2 C47 174.1(2) . . . . ? N9' Rh2' N7' C25' 135.2(15) . . . . ? C40' Rh2' N7' C25' 47.7(16) . . . . ? N11' Rh2' N7' C25' -144.6(15) . . . . ? P2' Rh2' N7' C25' -49.2(15) . . . . ? N9' Rh2' N7' N8' -42.3(8) . . . . ? C40' Rh2' N7' N8' -129.7(9) . . . . ? N11' Rh2' N7' N8' 38.0(8) . . . . ? P2' Rh2' N7' N8' 133.4(6) . . . . ? C25' N7' N8' C27' -0.1(3) . . . . ? Rh2' N7' N8' C27' 177.9(12) . . . . ? C25' N7' N8' B2' -179(2) . . . . ? Rh2' N7' N8' B2' -0.7(15) . . . . ? N10' B2' N8' C27' -122(2) . . . . ? N12' B2' N8' C27' 128(2) . . . . ? N10' B2' N8' N7' 56(2) . . . . ? N12' B2' N8' N7' -54(2) . . . . ? N7' N8' C27' C26' 0.3(5) . . . . ? B2' N8' C27' C26' 179(2) . . . . ? N7' N8' C27' C35' 179.9(5) . . . . ? B2' N8' C27' C35' -2(2) . . . . ? N8' C27' C26' C25' -0.4(6) . . . . ? C35' C27' C26' C25' -179.9(6) . . . . ? N8' N7' C25' C26' -0.2(3) . . . . ? Rh2' N7' C25' C26' -177.5(16) . . . . ? N8' N7' C25' C34' 180.0(3) . . . . ? Rh2' N7' C25' C34' 2.7(16) . . . . ? C27' C26' C25' N7' 0.3(5) . . . . ? C27' C26' C25' C34' -179.9(4) . . . . ? C40' Rh2' N9' C28' -43(2) . . . . ? N11' Rh2' N9' C28' 136(2) . . . . ? P2' Rh2' N9' C28' 87(6) . . . . ? N7' Rh2' N9' C28' -135(2) . . . . ? C40' Rh2' N9' N10' 128.6(11) . . . . ? N11' Rh2' N9' N10' -52.8(10) . . . . ? P2' Rh2' N9' N10' -102(6) . . . . ? N7' Rh2' N9' N10' 36.6(9) . . . . ? C28' N9' N10' C30' -0.1(2) . . . . ? Rh2' N9' N10' C30' -174.4(16) . . . . ? C28' N9' N10' B2' -174.9(19) . . . . ? Rh2' N9' N10' B2' 10.7(14) . . . . ? N8' B2' N10' C30' 118(2) . . . . ? N12' B2' N10' C30' -126.0(19) . . . . ? N8' B2' N10' N9' -67.1(19) . . . . ? N12' B2' N10' N9' 48.5(19) . . . . ? N9' N10' C30' C29' 0.0(4) . . . . ? B2' N10' C30' C29' 174.8(19) . . . . ? N9' N10' C30' C37' 179.8(5) . . . . ? B2' N10' C30' C37' -5(2) . . . . ? N10' C30' C29' C28' 0.0(5) . . . . ? C37' C30' C29' C28' -179.8(4) . . . . ? C30' C29' C28' N9' -0.1(4) . . . . ? C30' C29' C28' C36' -180.0(3) . . . . ? N10' N9' C28' C29' 0.1(2) . . . . ? Rh2' N9' C28' C29' 173(2) . . . . ? N10' N9' C28' C36' 180.0(2) . . . . ? Rh2' N9' C28' C36' -7(2) . . . . ? N9' Rh2' N11' C31' -119.8(17) . . . . ? C40' Rh2' N11' C31' -113(5) . . . . ? P2' Rh2' N11' C31' 55.2(16) . . . . ? N7' Rh2' N11' C31' 154.5(17) . . . . ? N9' Rh2' N11' N12' 53.3(10) . . . . ? C40' Rh2' N11' N12' 60(5) . . . . ? P2' Rh2' N11' N12' -131.6(8) . . . . ? N7' Rh2' N11' N12' -32.4(9) . . . . ? C31' N11' N12' C33' -0.1(3) . . . . ? Rh2' N11' N12' C33' -175.4(14) . . . . ? C31' N11' N12' B2' 164.8(18) . . . . ? Rh2' N11' N12' B2' -10.4(14) . . . . ? N10' B2' N12' C33' 117.9(19) . . . . ? N8' B2' N12' C33' -132.4(18) . . . . ? N10' B2' N12' N11' -46(2) . . . . ? N8' B2' N12' N11' 64(2) . . . . ? N11' N12' C33' C32' 0.1(5) . . . . ? B2' N12' C33' C32' -164.8(18) . . . . ? N11' N12' C33' C39' 179.8(4) . . . . ? B2' N12' C33' C39' 14.9(19) . . . . ? N12' C33' C32' C31' 0.0(5) . . . . ? C39' C33' C32' C31' -179.8(5) . . . . ? N12' N11' C31' C32' 0.1(2) . . . . ? Rh2' N11' C31' C32' 174.0(17) . . . . ? N12' N11' C31' C38' -179.9(3) . . . . ? Rh2' N11' C31' C38' -5.9(18) . . . . ? C33' C32' C31' N11' 0.0(5) . . . . ? C33' C32' C31' C38' 179.9(4) . . . . ? N9' Rh2' C40' C41' 127.3(12) . . . . ? N11' Rh2' C40' C41' 121(5) . . . . ? P2' Rh2' C40' C41' -47.6(11) . . . . ? N7' Rh2' C40' C41' -147.2(11) . . . . ? N9' Rh2' C40' C45' -46.2(11) . . . . ? N11' Rh2' C40' C45' -52(5) . . . . ? P2' Rh2' C40' C45' 138.9(9) . . . . ? N7' Rh2' C40' C45' 39.3(11) . . . . ? C45' C40' C41' F5' -180.0(4) . . . . ? Rh2' C40' C41' F5' 5.8(14) . . . . ? C45' C40' C41' C42' 0.0(3) . . . . ? Rh2' C40' C41' C42' -174.2(13) . . . . ? F5' C41' C42' F6' -0.1(4) . . . . ? C40' C41' C42' F6' 179.9(3) . . . . ? F5' C41' C42' C43' -180.0(4) . . . . ? C40' C41' C42' C43' 0.0(3) . . . . ? F6' C42' C43' F7' 0.2(7) . . . . ? C41' C42' C43' F7' -179.9(4) . . . . ? F6' C42' C43' C44' -180.0(5) . . . . ? C41' C42' C43' C44' -0.1(7) . . . . ? F7' C43' C44' F8' -0.2(10) . . . . ? C42' C43' C44' F8' 179.9(5) . . . . ? F7' C43' C44' C45' 179.9(6) . . . . ? C42' C43' C44' C45' 0.1(9) . . . . ? F8' C44' C45' C40' -179.9(5) . . . . ? C43' C44' C45' C40' -0.1(9) . . . . ? C41' C40' C45' C44' 0.0(7) . . . . ? Rh2' C40' C45' C44' 174.2(14) . . . . ? N9' Rh2' P2' C46' 83(6) . . . . ? C40' Rh2' P2' C46' -147.6(13) . . . . ? N11' Rh2' P2' C46' 34.8(13) . . . . ? N7' Rh2' P2' C46' -54.8(12) . . . . ? N9' Rh2' P2' C48' -153(6) . . . . ? C40' Rh2' P2' C48' -24.4(14) . . . . ? N11' Rh2' P2' C48' 158.1(13) . . . . ? N7' Rh2' P2' C48' 68.5(13) . . . . ? N9' Rh2' P2' C47' -36(6) . . . . ? C40' Rh2' P2' C47' 92.9(13) . . . . ? N11' Rh2' P2' C47' -84.7(13) . . . . ? N7' Rh2' P2' C47' -174.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 36.32 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.091 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.132 #===end data_jontt04_cmpd3d _database_code_depnum_ccdc_archive 'CCDC 770113' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt04 _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 B F3 N6 P Rh, 0.5(C4 H10 O)' _chemical_formula_sum 'C26 H39 B F3 N6 O0.5 P Rh' _chemical_formula_weight 645.32 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' 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 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.612(10) _cell_length_b 33.54(4) _cell_length_c 20.40(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.62(2) _cell_angle_gamma 90.00 _cell_volume 5809(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 845 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 16.76 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7695 _exptl_absorpt_correction_T_max 0.9863 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21541 _diffrn_reflns_av_R_equivalents 0.3773 _diffrn_reflns_av_sigmaI/netI 0.2323 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 18.00 _reflns_number_total 3999 _reflns_number_gt 1935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The intensity data were extremely weak due to the small crystal mass. The data were cut at a resolution of 1.15 \%A since no intensities above the background were present beyond that. In the event that future crystallizations are unable to produce better samples, this structure may be used solely as supplemental confirmation of formulation for independent characterization techniques that agree with it unambiguously. Only the rhodium and phosphorus atoms were refined with anisotropic displacement parameters. The phenyl rings were given a rigid body model (idealized benzene) to minimize large variations in C--C bond lengths. The hydride ligands could not be located in the difference Fourier map, but were included in the molecular formula. ; _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^)+(0.1297P)^2^+29.0596P] 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 3999 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2150 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.2957 _refine_ls_wR_factor_gt 0.2330 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.1542(3) 0.10075(8) 0.33271(11) 0.0279(9) Uani 1 1 d . . . F1 F 0.4085(18) 0.1062(5) 0.4697(8) 0.047(5) Uiso 1 1 d . . . F2 F 0.706(2) -0.0080(6) 0.4594(10) 0.083(7) Uiso 1 1 d . . . F3 F 0.2758(19) 0.0155(5) 0.2952(9) 0.053(5) Uiso 1 1 d . . . N1 N -0.009(3) 0.0511(7) 0.3039(11) 0.026(7) Uiso 1 1 d . . . N2 N -0.096(2) 0.0541(7) 0.2395(10) 0.019(6) Uiso 1 1 d . . . N3 N 0.001(2) 0.1439(6) 0.2751(10) 0.014(6) Uiso 1 1 d . . . N4 N -0.096(2) 0.1275(7) 0.2215(11) 0.023(6) Uiso 1 1 d . . . N5 N 0.234(3) 0.0920(6) 0.2417(11) 0.024(7) Uiso 1 1 d . . . N6 N 0.112(3) 0.0866(7) 0.1861(12) 0.030(7) Uiso 1 1 d . . . B1 B -0.066(4) 0.0868(10) 0.1927(17) 0.021(10) Uiso 1 1 d . . . H1B H -0.1339 0.0832 0.1482 0.025 Uiso 1 1 calc R . . C1 C -0.058(4) 0.0154(10) 0.3266(16) 0.042(10) Uiso 1 1 d . . . C2 C -0.170(3) -0.0023(10) 0.2804(15) 0.037(9) Uiso 1 1 d . . . H2A H -0.2212 -0.0271 0.2841 0.045 Uiso 1 1 calc R . . C3 C -0.190(3) 0.0227(9) 0.2293(14) 0.022(8) Uiso 1 1 d . . . C4 C -0.033(3) 0.1823(9) 0.2780(13) 0.021(8) Uiso 1 1 d . . . C5 C -0.148(3) 0.1937(9) 0.2275(12) 0.016(8) Uiso 1 1 d . . . H5A H -0.1936 0.2192 0.2180 0.019 Uiso 1 1 calc R . . C6 C -0.180(3) 0.1592(10) 0.1948(15) 0.036(9) Uiso 1 1 d . . . C7 C 0.367(3) 0.0899(8) 0.2223(14) 0.028(9) Uiso 1 1 d . . . C8 C 0.339(3) 0.0846(7) 0.1522(12) 0.005(7) Uiso 1 1 d . . . H8A H 0.4166 0.0836 0.1243 0.006 Uiso 1 1 calc R . . C9 C 0.189(3) 0.0814(9) 0.1332(15) 0.029(9) Uiso 1 1 d . . . C10 C 0.030(3) -0.0004(8) 0.3910(13) 0.027(8) Uiso 1 1 d . . . H10A H 0.1329 0.0127 0.4012 0.040 Uiso 1 1 calc R . . H10B H 0.0443 -0.0292 0.3873 0.040 Uiso 1 1 calc R . . H10C H -0.0305 0.0052 0.4267 0.040 Uiso 1 1 calc R . . C11 C -0.300(4) 0.0162(11) 0.1632(17) 0.067(12) Uiso 1 1 d . . . H11A H -0.3694 0.0394 0.1533 0.101 Uiso 1 1 calc R . . H11B H -0.3636 -0.0077 0.1661 0.101 Uiso 1 1 calc R . . H11C H -0.2372 0.0128 0.1277 0.101 Uiso 1 1 calc R . . C12 C 0.064(4) 0.2096(9) 0.3279(15) 0.045(10) Uiso 1 1 d . . . H12A H 0.1561 0.1951 0.3511 0.067 Uiso 1 1 calc R . . H12B H 0.0002 0.2189 0.3603 0.067 Uiso 1 1 calc R . . H12C H 0.0999 0.2326 0.3048 0.067 Uiso 1 1 calc R . . C13 C -0.300(4) 0.1534(10) 0.1306(16) 0.051(10) Uiso 1 1 d . . . H13A H -0.3697 0.1310 0.1362 0.077 Uiso 1 1 calc R . . H13B H -0.2445 0.1480 0.0935 0.077 Uiso 1 1 calc R . . H13C H -0.3635 0.1777 0.1213 0.077 Uiso 1 1 calc R . . C14 C 0.522(3) 0.0969(9) 0.2647(14) 0.030(8) Uiso 1 1 d . . . H14A H 0.5066 0.1051 0.3092 0.045 Uiso 1 1 calc R . . H14B H 0.5788 0.1179 0.2449 0.045 Uiso 1 1 calc R . . H14C H 0.5842 0.0722 0.2680 0.045 Uiso 1 1 calc R . . C15 C 0.092(4) 0.0728(10) 0.0659(16) 0.055(11) Uiso 1 1 d . . . H15A H 0.1613 0.0652 0.0346 0.082 Uiso 1 1 calc R . . H15B H 0.0319 0.0966 0.0494 0.082 Uiso 1 1 calc R . . H15C H 0.0183 0.0509 0.0699 0.082 Uiso 1 1 calc R . . C16 C 0.3302(19) 0.0620(6) 0.3781(10) 0.029(9) Uiso 1 1 d G . . C17 C 0.428(2) 0.0743(5) 0.4358(10) 0.032(9) Uiso 1 1 d G . . C18 C 0.555(2) 0.0508(6) 0.4635(8) 0.052(10) Uiso 1 1 d G . . H18A H 0.6215 0.0591 0.5030 0.062 Uiso 1 1 calc R . . C19 C 0.584(2) 0.0150(6) 0.4335(10) 0.042(10) Uiso 1 1 d G . . C20 C 0.487(2) 0.0027(5) 0.3757(10) 0.045(10) Uiso 1 1 d G . . H20A H 0.5067 -0.0217 0.3552 0.054 Uiso 1 1 calc R . . C21 C 0.360(2) 0.0262(6) 0.3480(8) 0.039(10) Uiso 1 1 d G . . P1 P 0.0518(10) 0.1147(3) 0.4248(4) 0.035(3) Uani 1 1 d . . . C22 C 0.051(3) 0.0790(8) 0.4889(13) 0.028(9) Uiso 1 1 d . . . H22A H 0.0028 0.0907 0.5247 0.043 Uiso 1 1 calc R . . H22B H 0.1589 0.0709 0.5064 0.043 Uiso 1 1 calc R . . H22C H -0.0105 0.0556 0.4709 0.043 Uiso 1 1 calc R . . C23 C 0.113(4) 0.1566(9) 0.4762(16) 0.052(10) Uiso 1 1 d . . . H23A H 0.0566 0.1568 0.5141 0.078 Uiso 1 1 calc R . . H23B H 0.0893 0.1812 0.4504 0.078 Uiso 1 1 calc R . . H23C H 0.2265 0.1550 0.4923 0.078 Uiso 1 1 calc R . . C24 C -0.154(3) 0.1217(9) 0.4023(15) 0.041(10) Uiso 1 1 d . . . H24A H -0.2007 0.1258 0.4424 0.062 Uiso 1 1 calc R . . H24B H -0.2013 0.0981 0.3784 0.062 Uiso 1 1 calc R . . H24C H -0.1745 0.1452 0.3735 0.062 Uiso 1 1 calc R . . Rh2 Rh 0.6229(3) 0.30455(8) 0.22664(12) 0.0324(9) Uani 1 1 d . . . F4 F 0.816(2) 0.3230(5) 0.3739(9) 0.060(6) Uiso 1 1 d . . . F5 F 0.398(2) 0.3364(6) 0.4923(10) 0.078(7) Uiso 1 1 d . . . F6 F 0.2839(19) 0.3086(5) 0.2667(8) 0.054(5) Uiso 1 1 d . . . N7 N 0.414(3) 0.3323(7) 0.1602(11) 0.030(7) Uiso 1 1 d . . . N8 N 0.350(3) 0.3082(7) 0.1065(11) 0.025(7) Uiso 1 1 d . . . N9 N 0.504(2) 0.2524(7) 0.2240(11) 0.022(6) Uiso 1 1 d . . . N10 N 0.393(2) 0.2419(7) 0.1637(11) 0.021(6) Uiso 1 1 d . . . N11 N 0.697(3) 0.2816(6) 0.1380(11) 0.021(6) Uiso 1 1 d . . . N12 N 0.581(3) 0.2654(7) 0.0910(11) 0.027(7) Uiso 1 1 d . . . B2 B 0.412(4) 0.2656(11) 0.1023(18) 0.030(11) Uiso 1 1 d . . . H2B H 0.3467 0.2524 0.0631 0.036 Uiso 1 1 calc R . . C25 C 0.331(3) 0.3653(9) 0.1551(14) 0.024(8) Uiso 1 1 d . . . C26 C 0.219(3) 0.3618(9) 0.0945(13) 0.023(8) Uiso 1 1 d . . . H26A H 0.1435 0.3814 0.0768 0.028 Uiso 1 1 calc R . . C27 C 0.239(3) 0.3256(8) 0.0674(14) 0.018(8) Uiso 1 1 d . . . C28 C 0.473(3) 0.2239(9) 0.2625(14) 0.025(8) Uiso 1 1 d . . . C29 C 0.367(3) 0.1946(9) 0.2354(14) 0.027(8) Uiso 1 1 d . . . H29A H 0.3353 0.1712 0.2561 0.032 Uiso 1 1 calc R . . C30 C 0.318(4) 0.2079(10) 0.1698(17) 0.046(10) Uiso 1 1 d . . . C31 C 0.836(3) 0.2727(8) 0.1208(14) 0.023(8) Uiso 1 1 d . . . C32 C 0.801(3) 0.2507(8) 0.0605(14) 0.028(9) Uiso 1 1 d . . . H32A H 0.8765 0.2404 0.0356 0.033 Uiso 1 1 calc R . . C33 C 0.647(3) 0.2470(9) 0.0450(14) 0.025(8) Uiso 1 1 d . . . C34 C 0.351(3) 0.3993(8) 0.1996(14) 0.029(8) Uiso 1 1 d . . . H34A H 0.3740 0.3900 0.2458 0.044 Uiso 1 1 calc R . . H34B H 0.2546 0.4153 0.1931 0.044 Uiso 1 1 calc R . . H34C H 0.4391 0.4157 0.1901 0.044 Uiso 1 1 calc R . . C35 C 0.146(3) 0.3090(9) 0.0079(13) 0.028(8) Uiso 1 1 d . . . H35A H 0.2168 0.3000 -0.0221 0.041 Uiso 1 1 calc R . . H35B H 0.0749 0.3295 -0.0143 0.041 Uiso 1 1 calc R . . H35C H 0.0848 0.2864 0.0199 0.041 Uiso 1 1 calc R . . C36 C 0.563(3) 0.2222(9) 0.3346(14) 0.044(10) Uiso 1 1 d . . . H36A H 0.6715 0.2316 0.3356 0.066 Uiso 1 1 calc R . . H36B H 0.5649 0.1947 0.3508 0.066 Uiso 1 1 calc R . . H36C H 0.5105 0.2393 0.3630 0.066 Uiso 1 1 calc R . . C37 C 0.208(3) 0.1870(9) 0.1160(14) 0.040(9) Uiso 1 1 d . . . H37A H 0.1401 0.2066 0.0895 0.060 Uiso 1 1 calc R . . H37B H 0.1426 0.1681 0.1360 0.060 Uiso 1 1 calc R . . H37C H 0.2691 0.1725 0.0872 0.060 Uiso 1 1 calc R . . C38 C 0.988(3) 0.2820(9) 0.1639(15) 0.042(10) Uiso 1 1 d . . . H38A H 0.9738 0.2823 0.2105 0.063 Uiso 1 1 calc R . . H38B H 1.0251 0.3083 0.1519 0.063 Uiso 1 1 calc R . . H38C H 1.0663 0.2617 0.1577 0.063 Uiso 1 1 calc R . . C39 C 0.556(3) 0.2261(8) -0.0144(12) 0.020(8) Uiso 1 1 d . . . H39A H 0.4753 0.2440 -0.0375 0.030 Uiso 1 1 calc R . . H39B H 0.5065 0.2022 0.0002 0.030 Uiso 1 1 calc R . . H39C H 0.6286 0.2185 -0.0446 0.030 Uiso 1 1 calc R . . C40 C 0.551(2) 0.3179(6) 0.3151(8) 0.016(8) Uiso 1 1 d G . . C41 C 0.6594(18) 0.3236(7) 0.3731(11) 0.048(10) Uiso 1 1 d G . . C42 C 0.607(2) 0.3287(7) 0.4334(8) 0.050(10) Uiso 1 1 d G . . H42A H 0.6807 0.3326 0.4730 0.060 Uiso 1 1 calc R . . C43 C 0.447(3) 0.3282(7) 0.4357(9) 0.054(11) Uiso 1 1 d G . . C44 C 0.3386(19) 0.3225(7) 0.3777(12) 0.082(13) Uiso 1 1 d G . . H44A H 0.2290 0.3221 0.3793 0.099 Uiso 1 1 calc R . . C45 C 0.391(2) 0.3173(7) 0.3174(9) 0.061(11) Uiso 1 1 d G . . P2 P 0.7708(11) 0.3598(3) 0.2341(4) 0.048(3) Uani 1 1 d . . . C46 C 0.727(4) 0.3984(10) 0.2900(17) 0.069(12) Uiso 1 1 d . . . H46A H 0.7786 0.4233 0.2802 0.103 Uiso 1 1 calc R . . H46B H 0.7662 0.3904 0.3360 0.103 Uiso 1 1 calc R . . H46C H 0.6130 0.4025 0.2841 0.103 Uiso 1 1 calc R . . C47 C 0.977(3) 0.3597(10) 0.2620(16) 0.052(11) Uiso 1 1 d . . . H47A H 1.0044 0.3814 0.2940 0.077 Uiso 1 1 calc R . . H47B H 1.0313 0.3635 0.2241 0.077 Uiso 1 1 calc R . . H47C H 1.0082 0.3342 0.2835 0.077 Uiso 1 1 calc R . . C48 C 0.765(4) 0.3843(10) 0.1582(17) 0.066(12) Uiso 1 1 d . . . H48A H 0.8030 0.4117 0.1662 0.099 Uiso 1 1 calc R . . H48B H 0.6561 0.3848 0.1343 0.099 Uiso 1 1 calc R . . H48C H 0.8316 0.3702 0.1314 0.099 Uiso 1 1 calc R . . C49 C 0.001(9) 0.422(2) 0.477(4) 0.23(4) Uiso 1 1 d . . . H49A H 0.0419 0.4317 0.5225 0.338 Uiso 1 1 calc R . . H49B H -0.0470 0.3961 0.4794 0.338 Uiso 1 1 calc R . . H49C H -0.0776 0.4413 0.4555 0.338 Uiso 1 1 calc R . . C50 C 0.101(9) 0.420(2) 0.448(4) 0.19(3) Uiso 1 1 d . . . H50A H 0.0586 0.4027 0.4105 0.234 Uiso 1 1 calc R . . H50B H 0.1806 0.4040 0.4772 0.234 Uiso 1 1 calc R . . O1 O 0.190(6) 0.4484(15) 0.420(3) 0.192(18) Uiso 1 1 d . . . C51 C 0.306(13) 0.450(3) 0.384(6) 0.33(6) Uiso 1 1 d . . . H51A H 0.3893 0.4357 0.4143 0.399 Uiso 1 1 calc R . . H51B H 0.2664 0.4305 0.3494 0.399 Uiso 1 1 calc R . . C52 C 0.381(6) 0.4689(17) 0.357(3) 0.14(2) Uiso 1 1 d . . . H52A H 0.4920 0.4631 0.3727 0.213 Uiso 1 1 calc R . . H52B H 0.3601 0.4972 0.3638 0.213 Uiso 1 1 calc R . . H52C H 0.3553 0.4628 0.3090 0.213 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0392(17) 0.0357(19) 0.0088(15) 0.0020(13) 0.0038(12) 0.0023(16) P1 0.050(6) 0.045(7) 0.010(5) 0.000(4) 0.007(5) 0.000(5) Rh2 0.0432(18) 0.039(2) 0.0108(16) -0.0006(14) -0.0068(13) 0.0033(16) P2 0.050(7) 0.072(8) 0.023(6) -0.004(5) 0.010(5) 0.004(6) _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 C16 2.090(14) . ? Rh1 N5 2.10(2) . ? Rh1 N3 2.17(2) . ? Rh1 N1 2.19(2) . ? Rh1 P1 2.252(9) . ? F1 C17 1.30(2) . ? F2 C19 1.34(2) . ? F3 C21 1.25(2) . ? N1 C1 1.37(3) . ? N1 N2 1.40(3) . ? N2 C3 1.32(3) . ? N2 B1 1.51(4) . ? N3 C4 1.32(3) . ? N3 N4 1.37(3) . ? N4 C6 1.35(3) . ? N4 B1 1.52(4) . ? N5 C7 1.28(3) . ? N5 N6 1.42(3) . ? N6 C9 1.37(3) . ? N6 B1 1.57(4) . ? B1 H1B 1.0000 . ? C1 C2 1.37(4) . ? C1 C10 1.50(4) . ? C2 C3 1.33(4) . ? C2 H2A 0.9500 . ? C3 C11 1.53(4) . ? C4 C5 1.36(3) . ? C4 C12 1.52(4) . ? C5 C6 1.34(4) . ? C5 H5A 0.9500 . ? C6 C13 1.54(4) . ? C7 C8 1.42(3) . ? C7 C14 1.48(4) . ? C8 C9 1.29(3) . ? C8 H8A 0.9500 . ? C9 C15 1.51(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C18 H18A 0.9500 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C20 H20A 0.9500 . ? P1 C24 1.77(3) . ? P1 C22 1.77(3) . ? P1 C23 1.78(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Rh2 N9 2.02(2) . ? Rh2 C40 2.051(16) . ? Rh2 N11 2.16(2) . ? Rh2 P2 2.239(11) . ? Rh2 N7 2.26(2) . ? F4 C41 1.35(2) . ? F5 C43 1.32(2) . ? F6 C45 1.30(2) . ? N7 C25 1.31(3) . ? N7 N8 1.40(3) . ? N8 C27 1.28(3) . ? N8 B2 1.53(4) . ? N9 C28 1.29(3) . ? N9 N10 1.47(3) . ? N10 C30 1.33(3) . ? N10 B2 1.52(4) . ? N11 C31 1.34(3) . ? N11 N12 1.38(3) . ? N12 C33 1.33(3) . ? N12 B2 1.51(4) . ? B2 H2B 1.0000 . ? C25 C26 1.44(4) . ? C25 C34 1.45(4) . ? C26 C27 1.36(3) . ? C26 H26A 0.9500 . ? C27 C35 1.45(3) . ? C28 C29 1.39(4) . ? C28 C36 1.54(4) . ? C29 C30 1.41(4) . ? C29 H29A 0.9500 . ? C30 C37 1.50(4) . ? C31 C32 1.42(4) . ? C31 C38 1.48(4) . ? C32 C33 1.32(3) . ? C32 H32A 0.9500 . ? C33 C39 1.50(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C42 H42A 0.9500 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C44 H44A 0.9500 . ? P2 C48 1.75(3) . ? P2 C47 1.77(3) . ? P2 C46 1.81(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.12(8) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 O1 1.40(7) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? O1 C51 1.33(10) . ? C51 C52 1.12(11) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N5 89.1(8) . . ? C16 Rh1 N3 170.2(8) . . ? N5 Rh1 N3 82.8(8) . . ? C16 Rh1 N1 91.8(8) . . ? N5 Rh1 N1 86.9(8) . . ? N3 Rh1 N1 93.3(8) . . ? C16 Rh1 P1 96.6(6) . . ? N5 Rh1 P1 174.2(7) . . ? N3 Rh1 P1 91.5(6) . . ? N1 Rh1 P1 93.4(6) . . ? C1 N1 N2 103(2) . . ? C1 N1 Rh1 142(2) . . ? N2 N1 Rh1 114.5(17) . . ? C3 N2 N1 108(2) . . ? C3 N2 B1 130(2) . . ? N1 N2 B1 122(2) . . ? C4 N3 N4 109(2) . . ? C4 N3 Rh1 138.0(18) . . ? N4 N3 Rh1 113.3(16) . . ? C6 N4 N3 103(2) . . ? C6 N4 B1 131(2) . . ? N3 N4 B1 123(2) . . ? C7 N5 N6 109(2) . . ? C7 N5 Rh1 136(2) . . ? N6 N5 Rh1 114.7(16) . . ? C9 N6 N5 105(2) . . ? C9 N6 B1 133(2) . . ? N5 N6 B1 122(2) . . ? N2 B1 N4 111(2) . . ? N2 B1 N6 109(2) . . ? N4 B1 N6 105(2) . . ? N2 B1 H1B 110.6 . . ? N4 B1 H1B 110.6 . . ? N6 B1 H1B 110.6 . . ? C2 C1 N1 112(3) . . ? C2 C1 C10 130(3) . . ? N1 C1 C10 118(3) . . ? C3 C2 C1 105(3) . . ? C3 C2 H2A 127.7 . . ? C1 C2 H2A 127.7 . . ? N2 C3 C2 112(3) . . ? N2 C3 C11 122(3) . . ? C2 C3 C11 126(3) . . ? N3 C4 C5 112(3) . . ? N3 C4 C12 121(2) . . ? C5 C4 C12 126(3) . . ? C6 C5 C4 102(3) . . ? C6 C5 H5A 129.2 . . ? C4 C5 H5A 129.2 . . ? C5 C6 N4 115(3) . . ? C5 C6 C13 126(3) . . ? N4 C6 C13 119(3) . . ? N5 C7 C8 108(2) . . ? N5 C7 C14 125(3) . . ? C8 C7 C14 126(3) . . ? C9 C8 C7 108(2) . . ? C9 C8 H8A 126.0 . . ? C7 C8 H8A 126.0 . . ? C8 C9 N6 110(3) . . ? C8 C9 C15 132(3) . . ? N6 C9 C15 118(3) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 120.0 . . ? C17 C16 Rh1 118.8(11) . . ? C21 C16 Rh1 120.9(11) . . ? F1 C17 C18 114.4(17) . . ? F1 C17 C16 125.6(17) . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? F2 C19 C20 119.3(18) . . ? F2 C19 C18 120.7(18) . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? F3 C21 C20 119.3(17) . . ? F3 C21 C16 120.7(18) . . ? C20 C21 C16 120.0 . . ? C24 P1 C22 98.8(14) . . ? C24 P1 C23 103.3(15) . . ? C22 P1 C23 97.9(15) . . ? C24 P1 Rh1 109.0(11) . . ? C22 P1 Rh1 121.7(10) . . ? C23 P1 Rh1 122.4(11) . . ? P1 C22 H22A 109.5 . . ? P1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P1 C24 H24A 109.5 . . ? P1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N9 Rh2 C40 89.3(9) . . ? N9 Rh2 N11 83.6(9) . . ? C40 Rh2 N11 171.7(8) . . ? N9 Rh2 P2 175.4(7) . . ? C40 Rh2 P2 90.6(6) . . ? N11 Rh2 P2 96.1(6) . . ? N9 Rh2 N7 89.6(9) . . ? C40 Rh2 N7 96.5(8) . . ? N11 Rh2 N7 87.8(8) . . ? P2 Rh2 N7 95.0(6) . . ? C25 N7 N8 107(2) . . ? C25 N7 Rh2 139.6(19) . . ? N8 N7 Rh2 113.7(17) . . ? C27 N8 N7 112(2) . . ? C27 N8 B2 128(3) . . ? N7 N8 B2 119(2) . . ? C28 N9 N10 99(2) . . ? C28 N9 Rh2 141(2) . . ? N10 N9 Rh2 119.1(16) . . ? C30 N10 N9 113(2) . . ? C30 N10 B2 131(3) . . ? N9 N10 B2 115(2) . . ? C31 N11 N12 108(2) . . ? C31 N11 Rh2 134.6(18) . . ? N12 N11 Rh2 116.2(16) . . ? C33 N12 N11 109(2) . . ? C33 N12 B2 130(3) . . ? N11 N12 B2 120(2) . . ? N12 B2 N10 112(3) . . ? N12 B2 N8 111(3) . . ? N10 B2 N8 111(2) . . ? N12 B2 H2B 107.7 . . ? N10 B2 H2B 107.7 . . ? N8 B2 H2B 107.7 . . ? N7 C25 C26 106(2) . . ? N7 C25 C34 127(3) . . ? C26 C25 C34 126(3) . . ? C27 C26 C25 108(3) . . ? C27 C26 H26A 126.0 . . ? C25 C26 H26A 126.0 . . ? N8 C27 C26 107(3) . . ? N8 C27 C35 127(3) . . ? C26 C27 C35 127(3) . . ? N9 C28 C29 118(3) . . ? N9 C28 C36 119(3) . . ? C29 C28 C36 123(3) . . ? C28 C29 C30 103(3) . . ? C28 C29 H29A 128.5 . . ? C30 C29 H29A 128.5 . . ? N10 C30 C29 107(3) . . ? N10 C30 C37 126(3) . . ? C29 C30 C37 127(3) . . ? N11 C31 C32 106(2) . . ? N11 C31 C38 123(3) . . ? C32 C31 C38 131(3) . . ? C33 C32 C31 108(3) . . ? C33 C32 H32A 126.0 . . ? C31 C32 H32A 126.0 . . ? C32 C33 N12 109(3) . . ? C32 C33 C39 127(3) . . ? N12 C33 C39 124(2) . . ? C25 C34 H34A 109.5 . . ? C25 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C25 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C27 C35 H35A 109.5 . . ? C27 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C27 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C28 C36 H36A 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C28 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C31 C38 H38A 109.5 . . ? C31 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C31 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 120.0 . . ? C41 C40 Rh2 121.5(12) . . ? C45 C40 Rh2 118.2(12) . . ? F4 C41 C40 122.3(17) . . ? F4 C41 C42 117.7(17) . . ? C40 C41 C42 120.0 . . ? C43 C42 C41 120.0 . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? F5 C43 C44 120.5(19) . . ? F5 C43 C42 119.3(19) . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? F6 C45 C44 116.1(18) . . ? F6 C45 C40 123.6(18) . . ? C44 C45 C40 120.0 . . ? C48 P2 C47 99.6(16) . . ? C48 P2 C46 104.1(17) . . ? C47 P2 C46 95.8(16) . . ? C48 P2 Rh2 113.4(12) . . ? C47 P2 Rh2 123.3(12) . . ? C46 P2 Rh2 117.4(12) . . ? P2 C46 H46A 109.5 . . ? P2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? P2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? P2 C47 H47A 109.5 . . ? P2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? P2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? P2 C48 H48A 109.5 . . ? P2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? P2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C49 C50 O1 134(9) . . ? C49 C50 H50A 103.7 . . ? O1 C50 H50A 103.7 . . ? C49 C50 H50B 103.7 . . ? O1 C50 H50B 103.7 . . ? H50A C50 H50B 105.3 . . ? C51 O1 C50 140(8) . . ? C52 C51 O1 148(10) . . ? C52 C51 H51A 99.7 . . ? O1 C51 H51A 99.7 . . ? C52 C51 H51B 99.7 . . ? O1 C51 H51B 99.7 . . ? H51A C51 H51B 104.1 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 N1 C1 39(3) . . . . ? N5 Rh1 N1 C1 128(3) . . . . ? N3 Rh1 N1 C1 -149(3) . . . . ? P1 Rh1 N1 C1 -57(3) . . . . ? C16 Rh1 N1 N2 -138.5(17) . . . . ? N5 Rh1 N1 N2 -49.5(17) . . . . ? N3 Rh1 N1 N2 33.1(17) . . . . ? P1 Rh1 N1 N2 124.7(16) . . . . ? C1 N1 N2 C3 2(3) . . . . ? Rh1 N1 N2 C3 -179.1(16) . . . . ? C1 N1 N2 B1 -173(2) . . . . ? Rh1 N1 N2 B1 6(3) . . . . ? C16 Rh1 N3 C4 -90(5) . . . . ? N5 Rh1 N3 C4 -124(3) . . . . ? N1 Rh1 N3 C4 149(3) . . . . ? P1 Rh1 N3 C4 56(3) . . . . ? C16 Rh1 N3 N4 94(5) . . . . ? N5 Rh1 N3 N4 59.2(16) . . . . ? N1 Rh1 N3 N4 -27.2(16) . . . . ? P1 Rh1 N3 N4 -120.7(15) . . . . ? C4 N3 N4 C6 1(3) . . . . ? Rh1 N3 N4 C6 178.9(17) . . . . ? C4 N3 N4 B1 165(2) . . . . ? Rh1 N3 N4 B1 -17(3) . . . . ? C16 Rh1 N5 C7 -43(3) . . . . ? N3 Rh1 N5 C7 132(3) . . . . ? N1 Rh1 N5 C7 -134(3) . . . . ? P1 Rh1 N5 C7 133(6) . . . . ? C16 Rh1 N5 N6 136.9(17) . . . . ? N3 Rh1 N5 N6 -48.6(17) . . . . ? N1 Rh1 N5 N6 45.1(17) . . . . ? P1 Rh1 N5 N6 -47(8) . . . . ? C7 N5 N6 C9 0(3) . . . . ? Rh1 N5 N6 C9 -179.9(17) . . . . ? C7 N5 N6 B1 179(2) . . . . ? Rh1 N5 N6 B1 -1(3) . . . . ? C3 N2 B1 N4 125(3) . . . . ? N1 N2 B1 N4 -61(3) . . . . ? C3 N2 B1 N6 -120(3) . . . . ? N1 N2 B1 N6 54(3) . . . . ? C6 N4 B1 N2 -131(3) . . . . ? N3 N4 B1 N2 71(3) . . . . ? C6 N4 B1 N6 111(3) . . . . ? N3 N4 B1 N6 -47(3) . . . . ? C9 N6 B1 N2 120(3) . . . . ? N5 N6 B1 N2 -59(3) . . . . ? C9 N6 B1 N4 -122(3) . . . . ? N5 N6 B1 N4 59(3) . . . . ? N2 N1 C1 C2 -1(3) . . . . ? Rh1 N1 C1 C2 -179(2) . . . . ? N2 N1 C1 C10 171(2) . . . . ? Rh1 N1 C1 C10 -7(5) . . . . ? N1 C1 C2 C3 0(3) . . . . ? C10 C1 C2 C3 -171(3) . . . . ? N1 N2 C3 C2 -3(3) . . . . ? B1 N2 C3 C2 172(3) . . . . ? N1 N2 C3 C11 -179(2) . . . . ? B1 N2 C3 C11 -4(4) . . . . ? C1 C2 C3 N2 2(3) . . . . ? C1 C2 C3 C11 178(3) . . . . ? N4 N3 C4 C5 -1(3) . . . . ? Rh1 N3 C4 C5 -177.6(18) . . . . ? N4 N3 C4 C12 -174(2) . . . . ? Rh1 N3 C4 C12 9(4) . . . . ? N3 C4 C5 C6 0(3) . . . . ? C12 C4 C5 C6 173(3) . . . . ? C4 C5 C6 N4 1(3) . . . . ? C4 C5 C6 C13 -178(3) . . . . ? N3 N4 C6 C5 -1(3) . . . . ? B1 N4 C6 C5 -163(3) . . . . ? N3 N4 C6 C13 178(2) . . . . ? B1 N4 C6 C13 16(4) . . . . ? N6 N5 C7 C8 2(3) . . . . ? Rh1 N5 C7 C8 -178.1(19) . . . . ? N6 N5 C7 C14 175(3) . . . . ? Rh1 N5 C7 C14 -5(5) . . . . ? N5 C7 C8 C9 -4(3) . . . . ? C14 C7 C8 C9 -177(3) . . . . ? C7 C8 C9 N6 4(3) . . . . ? C7 C8 C9 C15 -175(3) . . . . ? N5 N6 C9 C8 -2(3) . . . . ? B1 N6 C9 C8 179(3) . . . . ? N5 N6 C9 C15 177(3) . . . . ? B1 N6 C9 C15 -2(5) . . . . ? N5 Rh1 C16 C17 129.5(11) . . . . ? N3 Rh1 C16 C17 95(5) . . . . ? N1 Rh1 C16 C17 -143.7(11) . . . . ? P1 Rh1 C16 C17 -50.1(10) . . . . ? N5 Rh1 C16 C21 -44.5(11) . . . . ? N3 Rh1 C16 C21 -79(5) . . . . ? N1 Rh1 C16 C21 42.3(11) . . . . ? P1 Rh1 C16 C21 135.9(10) . . . . ? C21 C16 C17 F1 -177(2) . . . . ? Rh1 C16 C17 F1 9.0(19) . . . . ? C21 C16 C17 C18 0.0 . . . . ? Rh1 C16 C17 C18 -174.0(13) . . . . ? F1 C17 C18 C19 177.3(19) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 F2 180(2) . . . . ? C17 C18 C19 C20 0.0 . . . . ? F2 C19 C20 C21 -180(2) . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 F3 178(2) . . . . ? C19 C20 C21 C16 0.0 . . . . ? C17 C16 C21 F3 -178(2) . . . . ? Rh1 C16 C21 F3 -4.0(19) . . . . ? C17 C16 C21 C20 0.0 . . . . ? Rh1 C16 C21 C20 173.9(14) . . . . ? C16 Rh1 P1 C24 -146.2(12) . . . . ? N5 Rh1 P1 C24 38(7) . . . . ? N3 Rh1 P1 C24 39.3(13) . . . . ? N1 Rh1 P1 C24 -54.0(13) . . . . ? C16 Rh1 P1 C22 -32.5(13) . . . . ? N5 Rh1 P1 C22 152(7) . . . . ? N3 Rh1 P1 C22 153.1(13) . . . . ? N1 Rh1 P1 C22 59.7(13) . . . . ? C16 Rh1 P1 C23 93.2(14) . . . . ? N5 Rh1 P1 C23 -83(7) . . . . ? N3 Rh1 P1 C23 -81.2(14) . . . . ? N1 Rh1 P1 C23 -174.6(14) . . . . ? N9 Rh2 N7 C25 136(3) . . . . ? C40 Rh2 N7 C25 47(3) . . . . ? N11 Rh2 N7 C25 -140(3) . . . . ? P2 Rh2 N7 C25 -44(3) . . . . ? N9 Rh2 N7 N8 -45.0(17) . . . . ? C40 Rh2 N7 N8 -134.2(17) . . . . ? N11 Rh2 N7 N8 38.6(17) . . . . ? P2 Rh2 N7 N8 134.6(16) . . . . ? C25 N7 N8 C27 3(3) . . . . ? Rh2 N7 N8 C27 -176.0(17) . . . . ? C25 N7 N8 B2 -174(2) . . . . ? Rh2 N7 N8 B2 7(3) . . . . ? C40 Rh2 N9 C28 -39(3) . . . . ? N11 Rh2 N9 C28 137(3) . . . . ? P2 Rh2 N9 C28 50(10) . . . . ? N7 Rh2 N9 C28 -136(3) . . . . ? C40 Rh2 N9 N10 128.4(17) . . . . ? N11 Rh2 N9 N10 -55.9(16) . . . . ? P2 Rh2 N9 N10 -143(8) . . . . ? N7 Rh2 N9 N10 31.9(17) . . . . ? C28 N9 N10 C30 -5(3) . . . . ? Rh2 N9 N10 C30 -177(2) . . . . ? C28 N9 N10 B2 -171(2) . . . . ? Rh2 N9 N10 B2 17(3) . . . . ? N9 Rh2 N11 C31 -119(3) . . . . ? C40 Rh2 N11 C31 -88(6) . . . . ? P2 Rh2 N11 C31 56(3) . . . . ? N7 Rh2 N11 C31 151(3) . . . . ? N9 Rh2 N11 N12 46.3(18) . . . . ? C40 Rh2 N11 N12 77(6) . . . . ? P2 Rh2 N11 N12 -138.3(17) . . . . ? N7 Rh2 N11 N12 -43.5(18) . . . . ? C31 N11 N12 C33 -1(3) . . . . ? Rh2 N11 N12 C33 -170.0(18) . . . . ? C31 N11 N12 B2 171(2) . . . . ? Rh2 N11 N12 B2 2(3) . . . . ? C33 N12 B2 N10 108(3) . . . . ? N11 N12 B2 N10 -62(3) . . . . ? C33 N12 B2 N8 -127(3) . . . . ? N11 N12 B2 N8 63(3) . . . . ? C30 N10 B2 N12 -112(3) . . . . ? N9 N10 B2 N12 51(3) . . . . ? C30 N10 B2 N8 123(3) . . . . ? N9 N10 B2 N8 -74(3) . . . . ? C27 N8 B2 N12 116(3) . . . . ? N7 N8 B2 N12 -67(3) . . . . ? C27 N8 B2 N10 -119(3) . . . . ? N7 N8 B2 N10 58(3) . . . . ? N8 N7 C25 C26 -3(3) . . . . ? Rh2 N7 C25 C26 176(2) . . . . ? N8 N7 C25 C34 179(3) . . . . ? Rh2 N7 C25 C34 -2(5) . . . . ? N7 C25 C26 C27 2(3) . . . . ? C34 C25 C26 C27 180(3) . . . . ? N7 N8 C27 C26 -2(3) . . . . ? B2 N8 C27 C26 175(3) . . . . ? N7 N8 C27 C35 -179(3) . . . . ? B2 N8 C27 C35 -2(5) . . . . ? C25 C26 C27 N8 0(3) . . . . ? C25 C26 C27 C35 177(3) . . . . ? N10 N9 C28 C29 5(3) . . . . ? Rh2 N9 C28 C29 174(2) . . . . ? N10 N9 C28 C36 -179(2) . . . . ? Rh2 N9 C28 C36 -10(5) . . . . ? N9 C28 C29 C30 -3(4) . . . . ? C36 C28 C29 C30 -179(3) . . . . ? N9 N10 C30 C29 3(3) . . . . ? B2 N10 C30 C29 167(3) . . . . ? N9 N10 C30 C37 -174(3) . . . . ? B2 N10 C30 C37 -11(5) . . . . ? C28 C29 C30 N10 0(3) . . . . ? C28 C29 C30 C37 177(3) . . . . ? N12 N11 C31 C32 1(3) . . . . ? Rh2 N11 C31 C32 167.4(19) . . . . ? N12 N11 C31 C38 -174(3) . . . . ? Rh2 N11 C31 C38 -7(4) . . . . ? N11 C31 C32 C33 -1(3) . . . . ? C38 C31 C32 C33 173(3) . . . . ? C31 C32 C33 N12 0(3) . . . . ? C31 C32 C33 C39 -180(3) . . . . ? N11 N12 C33 C32 0(3) . . . . ? B2 N12 C33 C32 -171(3) . . . . ? N11 N12 C33 C39 -180(2) . . . . ? B2 N12 C33 C39 10(5) . . . . ? N9 Rh2 C40 C41 118.8(12) . . . . ? N11 Rh2 C40 C41 88(6) . . . . ? P2 Rh2 C40 C41 -56.6(11) . . . . ? N7 Rh2 C40 C41 -151.7(12) . . . . ? N9 Rh2 C40 C45 -55.1(12) . . . . ? N11 Rh2 C40 C45 -86(6) . . . . ? P2 Rh2 C40 C45 129.5(11) . . . . ? N7 Rh2 C40 C45 34.4(13) . . . . ? C45 C40 C41 F4 178(2) . . . . ? Rh2 C40 C41 F4 4(2) . . . . ? C45 C40 C41 C42 0.0 . . . . ? Rh2 C40 C41 C42 -173.8(14) . . . . ? F4 C41 C42 C43 -178(2) . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 F5 -174(2) . . . . ? C41 C42 C43 C44 0.0 . . . . ? F5 C43 C44 C45 174(2) . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 F6 174(2) . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 F6 -174(2) . . . . ? Rh2 C40 C45 F6 0(2) . . . . ? C41 C40 C45 C44 0.0 . . . . ? Rh2 C40 C45 C44 174.0(14) . . . . ? N9 Rh2 P2 C48 131(9) . . . . ? C40 Rh2 P2 C48 -140.1(14) . . . . ? N11 Rh2 P2 C48 44.7(14) . . . . ? N7 Rh2 P2 C48 -43.6(15) . . . . ? N9 Rh2 P2 C47 11(9) . . . . ? C40 Rh2 P2 C47 99.8(15) . . . . ? N11 Rh2 P2 C47 -75.4(15) . . . . ? N7 Rh2 P2 C47 -163.6(15) . . . . ? N9 Rh2 P2 C46 -107(9) . . . . ? C40 Rh2 P2 C46 -18.6(15) . . . . ? N11 Rh2 P2 C46 166.2(15) . . . . ? N7 Rh2 P2 C46 77.9(15) . . . . ? C49 C50 O1 C51 -178(12) . . . . ? C50 O1 C51 C52 174(16) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 18.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.306 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.156 #===end data_jontt03_cmpd3g _database_code_depnum_ccdc_archive 'CCDC 770114' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt03 _chemical_melting_point ? _chemical_formula_moiety 'C24 H35 B F2 N6 P Rh' _chemical_formula_sum 'C24 H35 B F2 N6 P Rh' _chemical_formula_weight 590.27 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 10.4449(16) _cell_length_b 14.597(2) _cell_length_c 17.499(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.021(3) _cell_angle_gamma 90.00 _cell_volume 2666.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3865 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 29.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8785 _exptl_absorpt_correction_T_max 0.9433 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42567 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8144 _reflns_number_gt 4948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The rhodium and boron hydride atoms were found from the difference Fourier map and their positions were refined independently from their respective bonded heavier atoms. The former was refined with an independent isotropic displacement parameter and the latter was refined with a relative isotropic displacement parameter, Uiso[H] = 1.2*Ueq[B]. ; _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^)+(0.0438P)^2^+1.4662P] 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 8144 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.0954 _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 0.75990(3) 0.30553(2) 0.975685(15) 0.02227(8) Uani 1 1 d . . . H1 H 0.664(4) 0.283(3) 1.029(2) 0.045(13) Uiso 1 1 d . . . N1 N 0.8920(3) 0.3378(2) 0.87986(16) 0.0246(6) Uani 1 1 d . . . N2 N 0.8490(3) 0.4044(2) 0.83030(15) 0.0245(6) Uani 1 1 d . . . N3 N 0.6121(3) 0.3019(2) 0.89103(16) 0.0239(6) Uani 1 1 d . . . N4 N 0.6166(3) 0.3620(2) 0.83165(17) 0.0275(7) Uani 1 1 d . . . N5 N 0.7124(3) 0.4495(2) 0.97955(16) 0.0246(6) Uani 1 1 d . . . N6 N 0.6987(3) 0.4937(2) 0.91019(16) 0.0255(6) Uani 1 1 d . . . B1 B 0.7127(4) 0.4413(3) 0.8348(2) 0.0278(9) Uani 1 1 d . . . H1B H 0.691(4) 0.488(3) 0.789(2) 0.033 Uiso 1 1 d . . . C1 C 1.0099(3) 0.3152(3) 0.85775(19) 0.0242(7) Uani 1 1 d . . . C2 C 1.0419(4) 0.3685(3) 0.7951(2) 0.0293(8) Uani 1 1 d . . . H2 H 1.1202 0.3670 0.7691 0.035 Uiso 1 1 calc R . . C3 C 0.9381(4) 0.4235(3) 0.77852(19) 0.0273(8) Uani 1 1 d . . . C4 C 0.5104(4) 0.2472(3) 0.8780(2) 0.0313(9) Uani 1 1 d . . . C5 C 0.4502(4) 0.2727(3) 0.8092(2) 0.0336(9) Uani 1 1 d . . . H5 H 0.3757 0.2456 0.7862 0.040 Uiso 1 1 calc R . . C6 C 0.5187(4) 0.3446(3) 0.7809(2) 0.0316(9) Uani 1 1 d . . . C7 C 0.6744(3) 0.5084(3) 1.0317(2) 0.0285(8) Uani 1 1 d . . . C8 C 0.6410(4) 0.5907(3) 0.9976(2) 0.0322(9) Uani 1 1 d . . . H8 H 0.6133 0.6446 1.0226 0.039 Uiso 1 1 calc R . . C9 C 0.6557(4) 0.5796(3) 0.9215(2) 0.0292(8) Uani 1 1 d . . . C10 C 1.0878(4) 0.2418(3) 0.8948(2) 0.0325(9) Uani 1 1 d . . . H10A H 1.0319 0.2008 0.9229 0.049 Uiso 1 1 calc R . . H10B H 1.1516 0.2691 0.9303 0.049 Uiso 1 1 calc R . . H10C H 1.1314 0.2067 0.8556 0.049 Uiso 1 1 calc R . . C11 C 0.9195(4) 0.4939(3) 0.7175(2) 0.0341(9) Uani 1 1 d . . . H11A H 0.8385 0.4824 0.6892 0.051 Uiso 1 1 calc R . . H11B H 0.9904 0.4907 0.6824 0.051 Uiso 1 1 calc R . . H11C H 0.9173 0.5549 0.7408 0.051 Uiso 1 1 calc R . . C12 C 0.4723(4) 0.1737(3) 0.9317(2) 0.0371(10) Uani 1 1 d . . . H12A H 0.5040 0.1888 0.9836 0.056 Uiso 1 1 calc R . . H12B H 0.5091 0.1152 0.9160 0.056 Uiso 1 1 calc R . . H12C H 0.3787 0.1687 0.9310 0.056 Uiso 1 1 calc R . . C13 C 0.4975(4) 0.3985(3) 0.7094(2) 0.0419(11) Uani 1 1 d . . . H13A H 0.4834 0.4630 0.7223 0.063 Uiso 1 1 calc R . . H13B H 0.4221 0.3747 0.6809 0.063 Uiso 1 1 calc R . . H13C H 0.5729 0.3933 0.6779 0.063 Uiso 1 1 calc R . . C14 C 0.6668(4) 0.4855(3) 1.1142(2) 0.0328(9) Uani 1 1 d . . . H14A H 0.6433 0.4209 1.1197 0.049 Uiso 1 1 calc R . . H14B H 0.6018 0.5241 1.1373 0.049 Uiso 1 1 calc R . . H14C H 0.7502 0.4965 1.1400 0.049 Uiso 1 1 calc R . . C15 C 0.6319(4) 0.6465(3) 0.8576(2) 0.0404(10) Uani 1 1 d . . . H15A H 0.5684 0.6210 0.8209 0.061 Uiso 1 1 calc R . . H15B H 0.7121 0.6579 0.8318 0.061 Uiso 1 1 calc R . . H15C H 0.5997 0.7041 0.8782 0.061 Uiso 1 1 calc R . . C16 C 0.7757(3) 0.1692(3) 0.9616(2) 0.0262(8) Uani 1 1 d . . . C17 C 0.7650(4) 0.1018(3) 1.0164(2) 0.0311(9) Uani 1 1 d . . . F1 F 0.7536(2) 0.12851(16) 1.09184(12) 0.0411(6) Uani 1 1 d . . . C18 C 0.7599(4) 0.0095(3) 1.0042(2) 0.0388(10) Uani 1 1 d . . . H18 H 0.7532 -0.0319 1.0457 0.047 Uiso 1 1 calc R . . C19 C 0.7646(4) -0.0225(3) 0.9297(2) 0.0370(10) Uani 1 1 d . . . H19 H 0.7605 -0.0861 0.9182 0.044 Uiso 1 1 calc R . . C20 C 0.7754(4) 0.0417(3) 0.8738(2) 0.0309(8) Uani 1 1 d . . . F2 F 0.7769(2) 0.01241(16) 0.79920(13) 0.0410(6) Uani 1 1 d . . . C21 C 0.7822(3) 0.1337(3) 0.8875(2) 0.0265(8) Uani 1 1 d . . . H21 H 0.7915 0.1745 0.8458 0.032 Uiso 1 1 calc R . . P1 P 0.90445(9) 0.30736(7) 1.07473(5) 0.02468(19) Uani 1 1 d . . . C22 C 1.0020(4) 0.4098(3) 1.0753(2) 0.0329(9) Uani 1 1 d . . . H22A H 1.0637 0.4077 1.1188 0.049 Uiso 1 1 calc R . . H22B H 0.9470 0.4638 1.0800 0.049 Uiso 1 1 calc R . . H22C H 1.0481 0.4135 1.0276 0.049 Uiso 1 1 calc R . . C23 C 0.8465(4) 0.3024(3) 1.17209(19) 0.0340(9) Uani 1 1 d . . . H23A H 0.9194 0.2962 1.2085 0.051 Uiso 1 1 calc R . . H23B H 0.7893 0.2497 1.1769 0.051 Uiso 1 1 calc R . . H23C H 0.7996 0.3588 1.1830 0.051 Uiso 1 1 calc R . . C24 C 1.0265(4) 0.2190(3) 1.0829(2) 0.0370(10) Uani 1 1 d . . . H24A H 1.0670 0.2207 1.1343 0.055 Uiso 1 1 calc R . . H24B H 1.0915 0.2298 1.0448 0.055 Uiso 1 1 calc R . . H24C H 0.9871 0.1589 1.0740 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02383(13) 0.02462(14) 0.01830(12) -0.00072(13) -0.00029(9) -0.00042(13) N1 0.0261(16) 0.0279(16) 0.0196(14) 0.0012(12) -0.0033(12) 0.0025(13) N2 0.0261(15) 0.0311(17) 0.0163(13) 0.0013(12) -0.0007(11) -0.0016(13) N3 0.0235(14) 0.0240(15) 0.0241(14) -0.0035(13) -0.0015(11) -0.0013(13) N4 0.0224(16) 0.0374(19) 0.0223(15) -0.0022(14) -0.0050(12) 0.0048(13) N5 0.0260(15) 0.0287(17) 0.0189(13) -0.0006(12) -0.0037(11) 0.0016(13) N6 0.0278(16) 0.0262(16) 0.0224(14) 0.0009(12) -0.0024(12) 0.0018(13) B1 0.031(2) 0.032(2) 0.0202(19) 0.0007(17) -0.0010(16) 0.0033(18) C1 0.0209(16) 0.028(2) 0.0234(16) -0.0079(15) -0.0019(13) -0.0009(15) C2 0.029(2) 0.037(2) 0.0222(17) -0.0038(16) 0.0028(15) -0.0066(16) C3 0.030(2) 0.032(2) 0.0193(16) -0.0020(15) -0.0019(14) -0.0064(16) C4 0.0257(19) 0.034(2) 0.034(2) -0.0115(17) -0.0007(16) 0.0022(16) C5 0.0252(19) 0.042(2) 0.033(2) -0.0140(18) -0.0037(16) -0.0010(17) C6 0.0261(19) 0.043(2) 0.0246(18) -0.0087(17) -0.0064(15) 0.0090(17) C7 0.0236(19) 0.031(2) 0.0305(19) -0.0046(16) -0.0006(15) 0.0018(15) C8 0.032(2) 0.029(2) 0.035(2) -0.0077(17) -0.0005(16) 0.0066(17) C9 0.0265(19) 0.031(2) 0.0302(19) 0.0033(16) -0.0019(15) 0.0016(16) C10 0.030(2) 0.037(2) 0.031(2) 0.0034(17) 0.0028(16) 0.0067(17) C11 0.039(2) 0.042(2) 0.0204(17) 0.0049(17) -0.0011(16) -0.0056(19) C12 0.028(2) 0.031(2) 0.052(3) -0.0053(19) 0.0009(18) -0.0028(16) C13 0.039(2) 0.059(3) 0.026(2) -0.008(2) -0.0064(17) 0.011(2) C14 0.032(2) 0.037(2) 0.0291(19) -0.0060(17) 0.0013(16) 0.0067(17) C15 0.046(3) 0.034(2) 0.041(2) 0.0060(19) -0.002(2) 0.010(2) C16 0.0220(18) 0.028(2) 0.0283(19) 0.0010(14) -0.0013(14) -0.0033(14) C17 0.036(2) 0.031(2) 0.0269(19) -0.0002(16) -0.0023(16) -0.0009(17) F1 0.0591(16) 0.0381(14) 0.0262(12) 0.0038(10) 0.0013(11) -0.0076(12) C18 0.049(3) 0.031(2) 0.035(2) 0.0070(18) -0.0106(19) -0.0029(19) C19 0.040(2) 0.025(2) 0.044(2) -0.0057(18) -0.0078(19) -0.0029(18) C20 0.027(2) 0.034(2) 0.0314(19) -0.0122(17) -0.0014(15) 0.0003(16) F2 0.0450(14) 0.0421(14) 0.0358(13) -0.0184(11) 0.0017(11) -0.0016(11) C21 0.0214(18) 0.0268(19) 0.0313(19) -0.0012(16) -0.0002(15) -0.0016(15) P1 0.0270(5) 0.0272(5) 0.0196(4) -0.0005(4) -0.0025(3) 0.0007(4) C22 0.032(2) 0.038(2) 0.0288(19) -0.0010(17) -0.0046(16) -0.0056(18) C23 0.041(2) 0.041(2) 0.0197(16) 0.0017(18) -0.0029(15) 0.004(2) C24 0.039(2) 0.044(3) 0.0283(19) 0.0012(18) -0.0033(17) 0.0081(19) _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 C16 2.013(4) . ? Rh1 N3 2.102(3) . ? Rh1 N5 2.161(3) . ? Rh1 P1 2.2582(9) . ? Rh1 N1 2.258(3) . ? Rh1 H1 1.44(4) . ? N1 C1 1.345(4) . ? N1 N2 1.369(4) . ? N2 C3 1.350(4) . ? N2 B1 1.527(5) . ? N3 C4 1.342(5) . ? N3 N4 1.363(4) . ? N4 C6 1.355(5) . ? N4 B1 1.531(5) . ? N5 C7 1.325(5) . ? N5 N6 1.378(4) . ? N6 C9 1.349(5) . ? N6 B1 1.537(5) . ? B1 H1B 1.07(4) . ? C1 C2 1.394(5) . ? C1 C10 1.481(5) . ? C2 C3 1.372(5) . ? C2 H2 0.9500 . ? C3 C11 1.489(5) . ? C4 C5 1.388(5) . ? C4 C12 1.490(6) . ? C5 C6 1.372(6) . ? C5 H5 0.9500 . ? C6 C13 1.488(5) . ? C7 C8 1.381(5) . ? C7 C14 1.486(5) . ? C8 C9 1.357(5) . ? C8 H8 0.9500 . ? C9 C15 1.498(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.381(5) . ? C16 C21 1.400(5) . ? C17 C18 1.365(6) . ? C17 F1 1.387(4) . ? C18 C19 1.386(6) . ? C18 H18 0.9500 . ? C19 C20 1.363(6) . ? C19 H19 0.9500 . ? C20 C21 1.365(5) . ? C20 F2 1.374(4) . ? C21 H21 0.9500 . ? P1 C22 1.809(4) . ? P1 C24 1.816(4) . ? P1 C23 1.830(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 C16 Rh1 N3 87.11(13) . . ? C16 Rh1 N5 170.15(13) . . ? N3 Rh1 N5 83.29(11) . . ? C16 Rh1 P1 92.88(11) . . ? N3 Rh1 P1 174.65(8) . . ? N5 Rh1 P1 96.47(8) . . ? C16 Rh1 N1 93.46(13) . . ? N3 Rh1 N1 86.25(11) . . ? N5 Rh1 N1 88.15(11) . . ? P1 Rh1 N1 99.09(8) . . ? C16 Rh1 H1 85.3(17) . . ? N3 Rh1 H1 86.9(17) . . ? N5 Rh1 H1 92.0(16) . . ? P1 Rh1 H1 87.8(17) . . ? N1 Rh1 H1 173.0(17) . . ? C1 N1 N2 105.9(3) . . ? C1 N1 Rh1 138.8(2) . . ? N2 N1 Rh1 115.1(2) . . ? C3 N2 N1 110.7(3) . . ? C3 N2 B1 128.9(3) . . ? N1 N2 B1 120.2(3) . . ? C4 N3 N4 107.6(3) . . ? C4 N3 Rh1 133.8(3) . . ? N4 N3 Rh1 118.5(2) . . ? C6 N4 N3 109.5(3) . . ? C6 N4 B1 130.1(3) . . ? N3 N4 B1 120.0(3) . . ? C7 N5 N6 106.2(3) . . ? C7 N5 Rh1 136.6(3) . . ? N6 N5 Rh1 116.4(2) . . ? C9 N6 N5 109.3(3) . . ? C9 N6 B1 129.1(3) . . ? N5 N6 B1 120.9(3) . . ? N2 B1 N4 110.1(3) . . ? N2 B1 N6 109.7(3) . . ? N4 B1 N6 109.0(3) . . ? N2 B1 H1B 111(2) . . ? N4 B1 H1B 110(2) . . ? N6 B1 H1B 107(2) . . ? N1 C1 C2 109.7(3) . . ? N1 C1 C10 123.1(3) . . ? C2 C1 C10 127.2(3) . . ? C3 C2 C1 106.4(3) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? N2 C3 C2 107.2(3) . . ? N2 C3 C11 123.2(3) . . ? C2 C3 C11 129.6(3) . . ? N3 C4 C5 108.6(4) . . ? N3 C4 C12 123.2(4) . . ? C5 C4 C12 128.1(4) . . ? C6 C5 C4 107.0(3) . . ? C6 C5 H5 126.5 . . ? C4 C5 H5 126.5 . . ? N4 C6 C5 107.3(3) . . ? N4 C6 C13 122.6(4) . . ? C5 C6 C13 130.1(4) . . ? N5 C7 C8 110.1(3) . . ? N5 C7 C14 123.5(3) . . ? C8 C7 C14 126.4(4) . . ? C9 C8 C7 106.6(3) . . ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? N6 C9 C8 107.7(3) . . ? N6 C9 C15 122.9(3) . . ? C8 C9 C15 129.4(4) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 112.8(3) . . ? C17 C16 Rh1 127.6(3) . . ? C21 C16 Rh1 119.1(3) . . ? C18 C17 C16 126.8(4) . . ? C18 C17 F1 115.0(3) . . ? C16 C17 F1 118.2(3) . . ? C17 C18 C19 118.5(4) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C20 C19 C18 116.7(4) . . ? C20 C19 H19 121.6 . . ? C18 C19 H19 121.6 . . ? C19 C20 C21 123.8(4) . . ? C19 C20 F2 118.1(3) . . ? C21 C20 F2 118.1(4) . . ? C20 C21 C16 121.5(4) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? C22 P1 C24 101.1(2) . . ? C22 P1 C23 103.40(19) . . ? C24 P1 C23 98.83(19) . . ? C22 P1 Rh1 112.05(13) . . ? C24 P1 Rh1 120.05(14) . . ? C23 P1 Rh1 118.67(13) . . ? P1 C22 H22A 109.5 . . ? P1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P1 C24 H24A 109.5 . . ? P1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 N1 C1 -52.3(4) . . . . ? N3 Rh1 N1 C1 -139.2(4) . . . . ? N5 Rh1 N1 C1 137.5(4) . . . . ? P1 Rh1 N1 C1 41.2(4) . . . . ? C16 Rh1 N1 N2 133.8(2) . . . . ? N3 Rh1 N1 N2 47.0(2) . . . . ? N5 Rh1 N1 N2 -36.4(2) . . . . ? P1 Rh1 N1 N2 -132.7(2) . . . . ? C1 N1 N2 C3 -0.2(4) . . . . ? Rh1 N1 N2 C3 175.6(2) . . . . ? C1 N1 N2 B1 175.3(3) . . . . ? Rh1 N1 N2 B1 -8.9(4) . . . . ? C16 Rh1 N3 C4 45.4(3) . . . . ? N5 Rh1 N3 C4 -132.4(3) . . . . ? P1 Rh1 N3 C4 -44.7(12) . . . . ? N1 Rh1 N3 C4 139.0(3) . . . . ? C16 Rh1 N3 N4 -129.9(3) . . . . ? N5 Rh1 N3 N4 52.3(2) . . . . ? P1 Rh1 N3 N4 140.0(9) . . . . ? N1 Rh1 N3 N4 -36.2(2) . . . . ? C4 N3 N4 C6 -0.7(4) . . . . ? Rh1 N3 N4 C6 175.7(2) . . . . ? C4 N3 N4 B1 172.4(3) . . . . ? Rh1 N3 N4 B1 -11.1(4) . . . . ? C16 Rh1 N5 C7 108.4(8) . . . . ? N3 Rh1 N5 C7 121.6(4) . . . . ? P1 Rh1 N5 C7 -53.0(4) . . . . ? N1 Rh1 N5 C7 -152.0(4) . . . . ? C16 Rh1 N5 N6 -60.1(8) . . . . ? N3 Rh1 N5 N6 -46.9(2) . . . . ? P1 Rh1 N5 N6 138.5(2) . . . . ? N1 Rh1 N5 N6 39.5(2) . . . . ? C7 N5 N6 C9 1.6(4) . . . . ? Rh1 N5 N6 C9 173.4(2) . . . . ? C7 N5 N6 B1 -169.9(3) . . . . ? Rh1 N5 N6 B1 1.9(4) . . . . ? C3 N2 B1 N4 121.5(4) . . . . ? N1 N2 B1 N4 -53.1(4) . . . . ? C3 N2 B1 N6 -118.6(4) . . . . ? N1 N2 B1 N6 66.8(4) . . . . ? C6 N4 B1 N2 -120.3(4) . . . . ? N3 N4 B1 N2 68.2(4) . . . . ? C6 N4 B1 N6 119.4(4) . . . . ? N3 N4 B1 N6 -52.2(4) . . . . ? C9 N6 B1 N2 126.9(4) . . . . ? N5 N6 B1 N2 -63.5(4) . . . . ? C9 N6 B1 N4 -112.5(4) . . . . ? N5 N6 B1 N4 57.1(4) . . . . ? N2 N1 C1 C2 0.9(4) . . . . ? Rh1 N1 C1 C2 -173.4(3) . . . . ? N2 N1 C1 C10 -177.1(3) . . . . ? Rh1 N1 C1 C10 8.7(6) . . . . ? N1 C1 C2 C3 -1.2(4) . . . . ? C10 C1 C2 C3 176.7(4) . . . . ? N1 N2 C3 C2 -0.5(4) . . . . ? B1 N2 C3 C2 -175.5(3) . . . . ? N1 N2 C3 C11 -179.4(3) . . . . ? B1 N2 C3 C11 5.6(6) . . . . ? C1 C2 C3 N2 1.0(4) . . . . ? C1 C2 C3 C11 179.8(4) . . . . ? N4 N3 C4 C5 0.4(4) . . . . ? Rh1 N3 C4 C5 -175.2(3) . . . . ? N4 N3 C4 C12 -178.5(3) . . . . ? Rh1 N3 C4 C12 5.9(6) . . . . ? N3 C4 C5 C6 0.1(4) . . . . ? C12 C4 C5 C6 178.9(4) . . . . ? N3 N4 C6 C5 0.8(4) . . . . ? B1 N4 C6 C5 -171.5(4) . . . . ? N3 N4 C6 C13 -179.8(3) . . . . ? B1 N4 C6 C13 8.0(6) . . . . ? C4 C5 C6 N4 -0.5(4) . . . . ? C4 C5 C6 C13 -179.9(4) . . . . ? N6 N5 C7 C8 -2.2(4) . . . . ? Rh1 N5 C7 C8 -171.5(3) . . . . ? N6 N5 C7 C14 176.2(3) . . . . ? Rh1 N5 C7 C14 7.0(6) . . . . ? N5 C7 C8 C9 2.0(5) . . . . ? C14 C7 C8 C9 -176.4(4) . . . . ? N5 N6 C9 C8 -0.3(4) . . . . ? B1 N6 C9 C8 170.2(4) . . . . ? N5 N6 C9 C15 179.3(3) . . . . ? B1 N6 C9 C15 -10.1(6) . . . . ? C7 C8 C9 N6 -1.0(4) . . . . ? C7 C8 C9 C15 179.4(4) . . . . ? N3 Rh1 C16 C17 -122.7(3) . . . . ? N5 Rh1 C16 C17 -109.6(8) . . . . ? P1 Rh1 C16 C17 52.0(3) . . . . ? N1 Rh1 C16 C17 151.3(3) . . . . ? N3 Rh1 C16 C21 48.4(3) . . . . ? N5 Rh1 C16 C21 61.5(9) . . . . ? P1 Rh1 C16 C21 -136.9(3) . . . . ? N1 Rh1 C16 C21 -37.6(3) . . . . ? C21 C16 C17 C18 -0.5(6) . . . . ? Rh1 C16 C17 C18 171.1(3) . . . . ? C21 C16 C17 F1 -177.9(3) . . . . ? Rh1 C16 C17 F1 -6.4(5) . . . . ? C16 C17 C18 C19 -0.5(7) . . . . ? F1 C17 C18 C19 177.0(4) . . . . ? C17 C18 C19 C20 0.6(6) . . . . ? C18 C19 C20 C21 0.3(6) . . . . ? C18 C19 C20 F2 -178.3(3) . . . . ? C19 C20 C21 C16 -1.4(6) . . . . ? F2 C20 C21 C16 177.2(3) . . . . ? C17 C16 C21 C20 1.4(5) . . . . ? Rh1 C16 C21 C20 -171.0(3) . . . . ? C16 Rh1 P1 C22 144.18(18) . . . . ? N3 Rh1 P1 C22 -126.0(10) . . . . ? N5 Rh1 P1 C22 -38.94(17) . . . . ? N1 Rh1 P1 C22 50.21(17) . . . . ? C16 Rh1 P1 C24 25.8(2) . . . . ? N3 Rh1 P1 C24 115.7(10) . . . . ? N5 Rh1 P1 C24 -157.28(19) . . . . ? N1 Rh1 P1 C24 -68.12(19) . . . . ? C16 Rh1 P1 C23 -95.39(19) . . . . ? N3 Rh1 P1 C23 -5.6(10) . . . . ? N5 Rh1 P1 C23 81.49(18) . . . . ? N1 Rh1 P1 C23 170.64(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.270 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.117 #===end data_jontt09_cmpd5 _database_code_depnum_ccdc_archive 'CCDC 770115' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt09 _chemical_melting_point ? _chemical_formula_moiety 'C23 H35 B N6 P Rh' _chemical_formula_sum 'C23 H35 B N6 P Rh' _chemical_formula_weight 540.26 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' 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 'P 1 21/c 1' 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 11.4148(12) _cell_length_b 15.6111(16) _cell_length_c 14.8282(15) _cell_angle_alpha 90.00 _cell_angle_beta 107.784(2) _cell_angle_gamma 90.00 _cell_volume 2516.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 4002 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 32.63 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8746 _exptl_absorpt_correction_T_max 0.9555 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60723 _diffrn_reflns_av_R_equivalents 0.0989 _diffrn_reflns_av_sigmaI/netI 0.0888 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 37.78 _reflns_number_total 13296 _reflns_number_gt 8337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The hydride ligands were found from the difference Fourier map and refined independently from the rhodium atom with individual isotropic displacement parameters. ; _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^)+(0.0408P)^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 13296 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 0.871611(15) 0.228065(10) 0.678030(11) 0.01492(4) Uani 1 1 d . . . H1 H 0.845(3) 0.2586(18) 0.578(2) 0.035(8) Uiso 1 1 d . . . H2 H 0.814(3) 0.1470(18) 0.630(2) 0.036(8) Uiso 1 1 d . . . P1 P 0.67353(5) 0.26059(4) 0.64545(4) 0.02023(11) Uani 1 1 d . . . N1 N 0.93016(16) 0.17805(11) 0.82628(13) 0.0176(3) Uani 1 1 d . . . N2 N 1.04823(16) 0.19664(12) 0.88087(13) 0.0179(3) Uani 1 1 d . . . N3 N 1.04510(16) 0.18491(11) 0.67536(12) 0.0171(3) Uani 1 1 d . . . N4 N 1.14712(16) 0.19563(12) 0.75222(13) 0.0184(3) Uani 1 1 d . . . N5 N 0.96869(17) 0.34476(11) 0.74062(13) 0.0183(3) Uani 1 1 d . . . N6 N 1.08214(17) 0.33527(11) 0.80617(13) 0.0185(3) Uani 1 1 d . . . B1 B 1.1349(2) 0.24561(16) 0.83850(18) 0.0196(5) Uani 1 1 d . . . H1B H 1.2176 0.2513 0.8869 0.024 Uiso 1 1 calc R . . C1 C 0.8819(2) 0.12771(15) 0.87925(16) 0.0218(4) Uani 1 1 d . . . C2 C 0.9682(2) 0.11434(15) 0.96770(16) 0.0249(5) Uani 1 1 d . . . H2A H 0.9575 0.0814 1.0185 0.030 Uiso 1 1 calc R . . C3 C 1.0725(2) 0.15872(14) 0.96658(16) 0.0222(4) Uani 1 1 d . . . C4 C 1.0795(2) 0.13797(14) 0.61229(15) 0.0186(4) Uani 1 1 d . . . C5 C 1.2041(2) 0.11705(15) 0.64951(16) 0.0233(4) Uani 1 1 d . . . H5A H 1.2515 0.0835 0.6200 0.028 Uiso 1 1 calc R . . C6 C 1.2443(2) 0.15495(15) 0.73766(17) 0.0218(4) Uani 1 1 d . . . C7 C 0.9512(2) 0.42902(14) 0.72591(16) 0.0212(4) Uani 1 1 d . . . C8 C 1.0533(2) 0.47397(15) 0.78142(18) 0.0251(5) Uani 1 1 d . . . H8A H 1.0645 0.5343 0.7843 0.030 Uiso 1 1 calc R . . C9 C 1.1344(2) 0.41310(15) 0.83110(16) 0.0224(4) Uani 1 1 d . . . C10 C 0.7556(2) 0.09273(17) 0.84297(18) 0.0303(5) Uani 1 1 d . . . H10A H 0.7432 0.0679 0.7800 0.045 Uiso 1 1 calc R . . H10B H 0.6959 0.1389 0.8387 0.045 Uiso 1 1 calc R . . H10C H 0.7442 0.0483 0.8862 0.045 Uiso 1 1 calc R . . C11 C 1.1926(2) 0.16437(17) 1.04235(17) 0.0299(5) Uani 1 1 d . . . H11A H 1.2163 0.2246 1.0542 0.045 Uiso 1 1 calc R . . H11B H 1.2555 0.1339 1.0223 0.045 Uiso 1 1 calc R . . H11C H 1.1852 0.1383 1.1005 0.045 Uiso 1 1 calc R . . C12 C 0.9906(2) 0.11545(15) 0.51889(16) 0.0236(5) Uani 1 1 d . . . H12A H 0.9471 0.1672 0.4891 0.035 Uiso 1 1 calc R . . H12B H 0.9311 0.0737 0.5280 0.035 Uiso 1 1 calc R . . H12C H 1.0351 0.0907 0.4781 0.035 Uiso 1 1 calc R . . C13 C 1.3688(2) 0.15266(18) 0.80898(18) 0.0303(5) Uani 1 1 d . . . H13A H 1.4015 0.2110 0.8209 0.045 Uiso 1 1 calc R . . H13B H 1.4239 0.1176 0.7848 0.045 Uiso 1 1 calc R . . H13C H 1.3629 0.1278 0.8681 0.045 Uiso 1 1 calc R . . C14 C 0.8370(2) 0.46543(15) 0.65861(18) 0.0277(5) Uani 1 1 d . . . H14A H 0.8130 0.4312 0.6004 0.042 Uiso 1 1 calc R . . H14B H 0.8522 0.5247 0.6434 0.042 Uiso 1 1 calc R . . H14C H 0.7707 0.4643 0.6878 0.042 Uiso 1 1 calc R . . C15 C 1.2575(2) 0.42504(17) 0.90312(19) 0.0310(6) Uani 1 1 d . . . H15A H 1.3187 0.3903 0.8857 0.046 Uiso 1 1 calc R . . H15B H 1.2534 0.4071 0.9654 0.046 Uiso 1 1 calc R . . H15C H 1.2810 0.4856 0.9054 0.046 Uiso 1 1 calc R . . C16 C 0.7040(2) 0.33603(15) 0.82118(16) 0.0233(5) Uani 1 1 d . . . H16A H 0.7821 0.3087 0.8389 0.028 Uiso 1 1 calc R . . C17 C 0.6700(2) 0.38526(17) 0.88727(18) 0.0279(5) Uani 1 1 d . . . H17A H 0.7242 0.3905 0.9500 0.033 Uiso 1 1 calc R . . C18 C 0.5578(2) 0.42639(17) 0.86206(19) 0.0294(5) Uani 1 1 d . . . H18A H 0.5349 0.4608 0.9068 0.035 Uiso 1 1 calc R . . C19 C 0.4791(3) 0.4172(2) 0.7713(2) 0.0454(8) Uani 1 1 d . . . H19A H 0.4017 0.4454 0.7534 0.054 Uiso 1 1 calc R . . C20 C 0.5123(3) 0.3671(2) 0.70617(19) 0.0419(8) Uani 1 1 d . . . H20A H 0.4566 0.3604 0.6442 0.050 Uiso 1 1 calc R . . C21 C 0.6256(2) 0.32633(15) 0.73002(16) 0.0218(4) Uani 1 1 d . . . C22 C 0.6050(2) 0.31560(19) 0.53264(17) 0.0323(6) Uani 1 1 d . . . H22A H 0.5162 0.3218 0.5214 0.049 Uiso 1 1 calc R . . H22B H 0.6197 0.2821 0.4812 0.049 Uiso 1 1 calc R . . H22C H 0.6424 0.3724 0.5349 0.049 Uiso 1 1 calc R . . C23 C 0.5633(2) 0.17170(18) 0.6243(2) 0.0328(6) Uani 1 1 d . . . H23A H 0.4794 0.1946 0.6063 0.049 Uiso 1 1 calc R . . H23B H 0.5785 0.1375 0.6822 0.049 Uiso 1 1 calc R . . H23C H 0.5731 0.1355 0.5731 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01522(7) 0.01418(6) 0.01542(7) -0.00003(6) 0.00475(5) 0.00071(6) P1 0.0163(2) 0.0257(3) 0.0172(3) -0.0012(2) 0.0029(2) 0.0027(2) N1 0.0182(8) 0.0161(8) 0.0185(8) -0.0011(6) 0.0056(7) -0.0006(6) N2 0.0173(8) 0.0180(8) 0.0180(8) -0.0003(6) 0.0046(7) 0.0009(6) N3 0.0171(8) 0.0173(8) 0.0168(8) -0.0003(6) 0.0049(7) -0.0001(6) N4 0.0165(8) 0.0201(8) 0.0185(8) -0.0006(7) 0.0051(7) 0.0010(6) N5 0.0201(9) 0.0169(8) 0.0185(9) -0.0003(6) 0.0069(7) 0.0000(6) N6 0.0192(8) 0.0179(8) 0.0192(9) -0.0019(7) 0.0070(7) -0.0024(7) B1 0.0194(11) 0.0186(10) 0.0200(12) -0.0033(8) 0.0048(9) -0.0004(8) C1 0.0259(11) 0.0209(10) 0.0210(11) 0.0002(8) 0.0107(9) -0.0016(8) C2 0.0331(13) 0.0242(11) 0.0194(11) 0.0041(8) 0.0110(10) 0.0027(9) C3 0.0286(12) 0.0200(10) 0.0175(10) 0.0002(8) 0.0061(9) 0.0063(8) C4 0.0222(10) 0.0179(9) 0.0172(10) 0.0015(7) 0.0082(8) 0.0019(8) C5 0.0250(11) 0.0246(11) 0.0230(11) 0.0009(9) 0.0112(9) 0.0066(8) C6 0.0176(10) 0.0243(11) 0.0247(11) 0.0027(9) 0.0080(9) 0.0034(8) C7 0.0281(11) 0.0166(9) 0.0234(11) 0.0009(8) 0.0146(9) 0.0003(8) C8 0.0353(13) 0.0176(10) 0.0278(12) -0.0036(8) 0.0176(11) -0.0055(9) C9 0.0248(11) 0.0228(10) 0.0237(11) -0.0063(8) 0.0133(9) -0.0082(9) C10 0.0309(13) 0.0319(13) 0.0313(13) 0.0012(10) 0.0143(11) -0.0090(10) C11 0.0323(13) 0.0313(13) 0.0196(11) 0.0022(9) -0.0018(10) 0.0064(10) C12 0.0239(11) 0.0268(12) 0.0206(11) -0.0043(9) 0.0076(9) 0.0016(9) C13 0.0197(11) 0.0428(15) 0.0276(13) -0.0008(11) 0.0060(10) 0.0058(10) C14 0.0338(13) 0.0191(10) 0.0324(13) 0.0011(9) 0.0134(11) 0.0049(9) C15 0.0314(13) 0.0316(13) 0.0322(14) -0.0108(10) 0.0129(11) -0.0146(10) C16 0.0169(10) 0.0287(12) 0.0234(11) -0.0029(9) 0.0050(8) 0.0050(8) C17 0.0212(11) 0.0365(14) 0.0254(12) -0.0064(10) 0.0063(9) 0.0012(9) C18 0.0313(13) 0.0307(13) 0.0303(13) -0.0004(10) 0.0154(11) 0.0075(10) C19 0.0376(16) 0.068(2) 0.0292(14) 0.0041(14) 0.0084(12) 0.0351(15) C20 0.0307(14) 0.069(2) 0.0208(12) -0.0033(12) 0.0002(11) 0.0279(14) C21 0.0192(10) 0.0251(11) 0.0214(10) 0.0024(8) 0.0066(8) 0.0056(8) C22 0.0288(13) 0.0464(16) 0.0177(11) 0.0019(10) 0.0010(9) 0.0113(11) C23 0.0207(12) 0.0406(15) 0.0347(14) -0.0054(11) 0.0049(10) -0.0058(10) _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 N3 2.1036(18) . ? Rh1 N5 2.1863(18) . ? Rh1 P1 2.2218(6) . ? Rh1 N1 2.2341(18) . ? Rh1 H1 1.49(3) . ? Rh1 H2 1.50(3) . ? P1 C21 1.829(2) . ? P1 C22 1.830(2) . ? P1 C23 1.835(3) . ? N1 C1 1.342(3) . ? N1 N2 1.375(2) . ? N2 C3 1.352(3) . ? N2 B1 1.529(3) . ? N3 C4 1.338(3) . ? N3 N4 1.368(2) . ? N4 C6 1.352(3) . ? N4 B1 1.541(3) . ? N5 C7 1.338(3) . ? N5 N6 1.369(3) . ? N6 C9 1.354(3) . ? N6 B1 1.541(3) . ? B1 H1B 1.0000 . ? C1 C2 1.395(3) . ? C1 C10 1.481(3) . ? C2 C3 1.382(3) . ? C2 H2A 0.9500 . ? C3 C11 1.486(3) . ? C4 C5 1.398(3) . ? C4 C12 1.488(3) . ? C5 C6 1.379(3) . ? C5 H5A 0.9500 . ? C6 C13 1.490(3) . ? C7 C8 1.394(3) . ? C7 C14 1.491(3) . ? C8 C9 1.373(3) . ? C8 H8A 0.9500 . ? C9 C15 1.494(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.383(3) . ? C16 C17 1.391(3) . ? C16 H16A 0.9500 . ? C17 C18 1.378(3) . ? C17 H17A 0.9500 . ? C18 C19 1.378(4) . ? C18 H18A 0.9500 . ? C19 C20 1.383(4) . ? C19 H19A 0.9500 . ? C20 C21 1.387(3) . ? C20 H20A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Rh1 N5 85.23(7) . . ? N3 Rh1 P1 166.04(5) . . ? N5 Rh1 P1 104.60(5) . . ? N3 Rh1 N1 84.62(7) . . ? N5 Rh1 N1 85.01(7) . . ? P1 Rh1 N1 105.82(5) . . ? N3 Rh1 H1 89.7(11) . . ? N5 Rh1 H1 94.5(11) . . ? P1 Rh1 H1 79.8(11) . . ? N1 Rh1 H1 174.3(11) . . ? N3 Rh1 H2 90.1(11) . . ? N5 Rh1 H2 174.5(11) . . ? P1 Rh1 H2 79.6(11) . . ? N1 Rh1 H2 97.5(11) . . ? H1 Rh1 H2 82.5(15) . . ? C21 P1 C22 103.28(11) . . ? C21 P1 C23 102.03(12) . . ? C22 P1 C23 96.86(13) . . ? C21 P1 Rh1 118.48(8) . . ? C22 P1 Rh1 115.38(9) . . ? C23 P1 Rh1 117.62(9) . . ? C1 N1 N2 106.42(18) . . ? C1 N1 Rh1 136.68(15) . . ? N2 N1 Rh1 116.77(13) . . ? C3 N2 N1 110.11(18) . . ? C3 N2 B1 129.24(19) . . ? N1 N2 B1 120.32(17) . . ? C4 N3 N4 106.99(17) . . ? C4 N3 Rh1 131.89(15) . . ? N4 N3 Rh1 120.77(13) . . ? C6 N4 N3 109.92(18) . . ? C6 N4 B1 131.08(19) . . ? N3 N4 B1 118.95(17) . . ? C7 N5 N6 106.47(17) . . ? C7 N5 Rh1 135.96(16) . . ? N6 N5 Rh1 117.26(13) . . ? C9 N6 N5 109.81(18) . . ? C9 N6 B1 129.2(2) . . ? N5 N6 B1 120.95(17) . . ? N2 B1 N4 108.78(18) . . ? N2 B1 N6 109.94(18) . . ? N4 B1 N6 109.12(18) . . ? N2 B1 H1B 109.7 . . ? N4 B1 H1B 109.7 . . ? N6 B1 H1B 109.7 . . ? N1 C1 C2 109.9(2) . . ? N1 C1 C10 122.1(2) . . ? C2 C1 C10 128.0(2) . . ? C3 C2 C1 106.1(2) . . ? C3 C2 H2A 126.9 . . ? C1 C2 H2A 126.9 . . ? N2 C3 C2 107.5(2) . . ? N2 C3 C11 124.2(2) . . ? C2 C3 C11 128.3(2) . . ? N3 C4 C5 109.43(19) . . ? N3 C4 C12 121.16(19) . . ? C5 C4 C12 129.4(2) . . ? C6 C5 C4 106.1(2) . . ? C6 C5 H5A 126.9 . . ? C4 C5 H5A 126.9 . . ? N4 C6 C5 107.5(2) . . ? N4 C6 C13 123.3(2) . . ? C5 C6 C13 129.2(2) . . ? N5 C7 C8 110.0(2) . . ? N5 C7 C14 122.7(2) . . ? C8 C7 C14 127.3(2) . . ? C9 C8 C7 105.9(2) . . ? C9 C8 H8A 127.1 . . ? C7 C8 H8A 127.1 . . ? N6 C9 C8 107.8(2) . . ? N6 C9 C15 123.1(2) . . ? C8 C9 C15 129.0(2) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 120.8(2) . . ? C21 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 120.2(2) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C19 C18 C17 119.4(2) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C20 120.4(2) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C21 121.0(2) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C16 C21 C20 118.3(2) . . ? C16 C21 P1 119.47(17) . . ? C20 C21 P1 122.24(19) . . ? P1 C22 H22A 109.5 . . ? P1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Rh1 P1 C21 -172.9(2) . . . . ? N5 Rh1 P1 C21 -39.12(10) . . . . ? N1 Rh1 P1 C21 49.75(10) . . . . ? N3 Rh1 P1 C22 -49.8(2) . . . . ? N5 Rh1 P1 C22 84.01(12) . . . . ? N1 Rh1 P1 C22 172.88(11) . . . . ? N3 Rh1 P1 C23 63.6(2) . . . . ? N5 Rh1 P1 C23 -162.58(11) . . . . ? N1 Rh1 P1 C23 -73.71(11) . . . . ? N3 Rh1 N1 C1 -131.0(2) . . . . ? N5 Rh1 N1 C1 143.3(2) . . . . ? P1 Rh1 N1 C1 39.5(2) . . . . ? N3 Rh1 N1 N2 44.09(14) . . . . ? N5 Rh1 N1 N2 -41.57(14) . . . . ? P1 Rh1 N1 N2 -145.36(13) . . . . ? C1 N1 N2 C3 -0.3(2) . . . . ? Rh1 N1 N2 C3 -176.83(14) . . . . ? C1 N1 N2 B1 173.67(19) . . . . ? Rh1 N1 N2 B1 -2.8(2) . . . . ? N5 Rh1 N3 C4 -142.6(2) . . . . ? P1 Rh1 N3 C4 -7.1(4) . . . . ? N1 Rh1 N3 C4 132.0(2) . . . . ? N5 Rh1 N3 N4 45.04(15) . . . . ? P1 Rh1 N3 N4 -179.49(14) . . . . ? N1 Rh1 N3 N4 -40.39(15) . . . . ? C4 N3 N4 C6 -0.6(2) . . . . ? Rh1 N3 N4 C6 173.44(14) . . . . ? C4 N3 N4 B1 -178.36(19) . . . . ? Rh1 N3 N4 B1 -4.3(2) . . . . ? N3 Rh1 N5 C7 132.2(2) . . . . ? P1 Rh1 N5 C7 -37.7(2) . . . . ? N1 Rh1 N5 C7 -142.8(2) . . . . ? N3 Rh1 N5 N6 -40.38(14) . . . . ? P1 Rh1 N5 N6 149.69(13) . . . . ? N1 Rh1 N5 N6 44.62(14) . . . . ? C7 N5 N6 C9 -0.4(2) . . . . ? Rh1 N5 N6 C9 174.24(14) . . . . ? C7 N5 N6 B1 -178.29(19) . . . . ? Rh1 N5 N6 B1 -3.6(2) . . . . ? C3 N2 B1 N4 115.1(2) . . . . ? N1 N2 B1 N4 -57.6(2) . . . . ? C3 N2 B1 N6 -125.5(2) . . . . ? N1 N2 B1 N6 61.8(2) . . . . ? C6 N4 B1 N2 -113.6(3) . . . . ? N3 N4 B1 N2 63.7(2) . . . . ? C6 N4 B1 N6 126.5(2) . . . . ? N3 N4 B1 N6 -56.3(2) . . . . ? C9 N6 B1 N2 124.0(2) . . . . ? N5 N6 B1 N2 -58.6(2) . . . . ? C9 N6 B1 N4 -116.8(2) . . . . ? N5 N6 B1 N4 60.6(2) . . . . ? N2 N1 C1 C2 0.3(2) . . . . ? Rh1 N1 C1 C2 175.80(16) . . . . ? N2 N1 C1 C10 -178.5(2) . . . . ? Rh1 N1 C1 C10 -3.1(4) . . . . ? N1 C1 C2 C3 -0.2(3) . . . . ? C10 C1 C2 C3 178.5(2) . . . . ? N1 N2 C3 C2 0.2(2) . . . . ? B1 N2 C3 C2 -173.1(2) . . . . ? N1 N2 C3 C11 178.9(2) . . . . ? B1 N2 C3 C11 5.6(4) . . . . ? C1 C2 C3 N2 0.0(3) . . . . ? C1 C2 C3 C11 -178.6(2) . . . . ? N4 N3 C4 C5 1.0(2) . . . . ? Rh1 N3 C4 C5 -172.08(16) . . . . ? N4 N3 C4 C12 -178.93(19) . . . . ? Rh1 N3 C4 C12 7.9(3) . . . . ? N3 C4 C5 C6 -1.1(3) . . . . ? C12 C4 C5 C6 178.9(2) . . . . ? N3 N4 C6 C5 -0.1(3) . . . . ? B1 N4 C6 C5 177.3(2) . . . . ? N3 N4 C6 C13 -178.6(2) . . . . ? B1 N4 C6 C13 -1.2(4) . . . . ? C4 C5 C6 N4 0.7(3) . . . . ? C4 C5 C6 C13 179.1(2) . . . . ? N6 N5 C7 C8 0.3(2) . . . . ? Rh1 N5 C7 C8 -172.87(16) . . . . ? N6 N5 C7 C14 -179.9(2) . . . . ? Rh1 N5 C7 C14 7.0(3) . . . . ? N5 C7 C8 C9 -0.1(3) . . . . ? C14 C7 C8 C9 -179.9(2) . . . . ? N5 N6 C9 C8 0.4(2) . . . . ? B1 N6 C9 C8 178.0(2) . . . . ? N5 N6 C9 C15 178.6(2) . . . . ? B1 N6 C9 C15 -3.8(4) . . . . ? C7 C8 C9 N6 -0.2(3) . . . . ? C7 C8 C9 C15 -178.2(2) . . . . ? C21 C16 C17 C18 -1.1(4) . . . . ? C16 C17 C18 C19 1.0(4) . . . . ? C17 C18 C19 C20 0.1(5) . . . . ? C18 C19 C20 C21 -1.1(5) . . . . ? C17 C16 C21 C20 0.1(4) . . . . ? C17 C16 C21 P1 -179.7(2) . . . . ? C19 C20 C21 C16 1.0(5) . . . . ? C19 C20 C21 P1 -179.2(3) . . . . ? C22 P1 C21 C16 -145.4(2) . . . . ? C23 P1 C21 C16 114.5(2) . . . . ? Rh1 P1 C21 C16 -16.4(2) . . . . ? C22 P1 C21 C20 34.8(3) . . . . ? C23 P1 C21 C20 -65.3(3) . . . . ? Rh1 P1 C21 C20 163.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 37.78 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.210 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.140 #===end data_jontt08_cmpd7 _database_code_depnum_ccdc_archive 'CCDC 770116' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt08 _chemical_melting_point ? _chemical_formula_moiety 'C23 H33 B N6 P Rh' _chemical_formula_sum 'C23 H33 B N6 P Rh' _chemical_formula_weight 538.24 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' 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 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.600(4) _cell_length_b 12.888(4) _cell_length_c 14.424(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.895(4) _cell_angle_gamma 90.00 _cell_volume 2454.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 4081 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 32.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.9399 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42160 _diffrn_reflns_av_R_equivalents 0.1047 _diffrn_reflns_av_sigmaI/netI 0.0911 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 32.57 _reflns_number_total 8821 _reflns_number_gt 5887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The hydride ligand was found from the difference Fourier map, and its position and isotropic displacement parameter were refined independently from those of all other atoms. ; _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^)+(0.0560P)^2^+14.3847P] 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 8821 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.1888 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 0.73923(3) 0.39285(3) 1.01298(3) 0.01735(10) Uani 1 1 d . . . H1 H 0.820(5) 0.398(5) 1.113(5) 0.033(18) Uiso 1 1 d . . . P1 P 0.64049(10) 0.36236(10) 1.11453(10) 0.0184(3) Uani 1 1 d . . . N1 N 0.6291(3) 0.3825(3) 0.8711(3) 0.0187(8) Uani 1 1 d . . . N2 N 0.6435(3) 0.4531(3) 0.8040(3) 0.0200(8) Uani 1 1 d . . . N3 N 0.8506(3) 0.3939(3) 0.9343(3) 0.0192(8) Uani 1 1 d . . . N4 N 0.8355(3) 0.4562(3) 0.8539(3) 0.0201(8) Uani 1 1 d . . . N5 N 0.7359(3) 0.5585(3) 0.9935(3) 0.0183(8) Uani 1 1 d . . . N6 N 0.7360(3) 0.5984(3) 0.9059(3) 0.0198(8) Uani 1 1 d . . . B1 B 0.7389(4) 0.5228(4) 0.8238(4) 0.0196(11) Uani 1 1 d . . . H1B H 0.7407 0.5630 0.7649 0.029 Uiso 1 1 calc R . . C1 C 0.5438(4) 0.3308(4) 0.8311(4) 0.0211(10) Uani 1 1 d . . . C2 C 0.5012(4) 0.3706(4) 0.7398(4) 0.0226(10) Uani 1 1 d . . . H2 H 0.4402 0.3488 0.6969 0.027 Uiso 1 1 calc R . . C3 C 0.5660(4) 0.4477(4) 0.7251(4) 0.0214(10) Uani 1 1 d . . . C4 C 0.9447(4) 0.3577(4) 0.9496(4) 0.0233(10) Uani 1 1 d . . . C5 C 0.9925(4) 0.3978(5) 0.8813(4) 0.0268(11) Uani 1 1 d . . . H5 H 1.0597 0.3845 0.8761 0.032 Uiso 1 1 calc R . . C6 C 0.9218(4) 0.4605(4) 0.8233(4) 0.0226(10) Uani 1 1 d . . . C7 C 0.7341(4) 0.6389(4) 1.0522(4) 0.0213(10) Uani 1 1 d . . . C8 C 0.7339(4) 0.7318(4) 1.0015(4) 0.0249(11) Uani 1 1 d . . . H8 H 0.7337 0.8003 1.0259 0.030 Uiso 1 1 calc R . . C9 C 0.7343(4) 0.7039(4) 0.9086(4) 0.0219(10) Uani 1 1 d . . . C10 C 0.5024(4) 0.2420(4) 0.8779(4) 0.0237(11) Uani 1 1 d . . . H10A H 0.5576 0.1943 0.9064 0.036 Uiso 1 1 calc R . . H10B H 0.4512 0.2049 0.8300 0.036 Uiso 1 1 calc R . . H10C H 0.4716 0.2688 0.9279 0.036 Uiso 1 1 calc R . . C11 C 0.5579(5) 0.5153(5) 0.6391(4) 0.0298(12) Uani 1 1 d . . . H11A H 0.4936 0.5015 0.5929 0.045 Uiso 1 1 calc R . . H11B H 0.6142 0.5002 0.6097 0.045 Uiso 1 1 calc R . . H11C H 0.5606 0.5884 0.6584 0.045 Uiso 1 1 calc R . . C12 C 0.9894(5) 0.2906(5) 1.0339(5) 0.0301(12) Uani 1 1 d . . . H12A H 0.9394 0.2800 1.0719 0.045 Uiso 1 1 calc R . . H12B H 1.0496 0.3245 1.0733 0.045 Uiso 1 1 calc R . . H12C H 1.0085 0.2234 1.0118 0.045 Uiso 1 1 calc R . . C13 C 0.9338(5) 0.5254(5) 0.7406(4) 0.0286(12) Uani 1 1 d . . . H13A H 1.0046 0.5234 0.7362 0.043 Uiso 1 1 calc R . . H13B H 0.9145 0.5972 0.7499 0.043 Uiso 1 1 calc R . . H13C H 0.8902 0.4980 0.6814 0.043 Uiso 1 1 calc R . . C14 C 0.7328(5) 0.6229(4) 1.1539(4) 0.0260(11) Uani 1 1 d . . . H14A H 0.7774 0.5648 1.1800 0.039 Uiso 1 1 calc R . . H14B H 0.6636 0.6074 1.1584 0.039 Uiso 1 1 calc R . . H14C H 0.7567 0.6860 1.1903 0.039 Uiso 1 1 calc R . . C15 C 0.7354(5) 0.7702(4) 0.8234(5) 0.0303(13) Uani 1 1 d . . . H15A H 0.7421 0.8433 0.8427 0.045 Uiso 1 1 calc R . . H15B H 0.6720 0.7604 0.7747 0.045 Uiso 1 1 calc R . . H15C H 0.7927 0.7503 0.7971 0.045 Uiso 1 1 calc R . . C16 C 0.7286(4) 0.2387(4) 1.0349(4) 0.0204(10) Uani 1 1 d . . . C17 C 0.7619(4) 0.1486(4) 0.9972(4) 0.0253(11) Uani 1 1 d . . . H17 H 0.8100 0.1531 0.9592 0.030 Uiso 1 1 calc R . . C18 C 0.7240(5) 0.0523(4) 1.0158(4) 0.0276(12) Uani 1 1 d . . . H18 H 0.7473 -0.0087 0.9909 0.033 Uiso 1 1 calc R . . C19 C 0.6520(5) 0.0438(4) 1.0707(4) 0.0290(12) Uani 1 1 d . . . H19 H 0.6260 -0.0225 1.0811 0.035 Uiso 1 1 calc R . . C20 C 0.6185(5) 0.1320(4) 1.1100(4) 0.0254(11) Uani 1 1 d . . . H20 H 0.5701 0.1273 1.1477 0.031 Uiso 1 1 calc R . . C21 C 0.6585(4) 0.2272(4) 1.0920(4) 0.0196(10) Uani 1 1 d . . . C22 C 0.6837(5) 0.3831(4) 1.2433(4) 0.0258(11) Uani 1 1 d . . . H22A H 0.6446 0.3389 1.2766 0.039 Uiso 1 1 calc R . . H22B H 0.6740 0.4560 1.2580 0.039 Uiso 1 1 calc R . . H22C H 0.7557 0.3654 1.2643 0.039 Uiso 1 1 calc R . . C23 C 0.5084(4) 0.3966(5) 1.0943(4) 0.0277(11) Uani 1 1 d . . . H23A H 0.4754 0.3508 1.1319 0.041 Uiso 1 1 calc R . . H23B H 0.4756 0.3889 1.0264 0.041 Uiso 1 1 calc R . . H23C H 0.5025 0.4688 1.1138 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01807(17) 0.01434(16) 0.01951(18) 0.00134(16) 0.00428(12) 0.00085(15) P1 0.0211(6) 0.0145(5) 0.0195(6) -0.0001(5) 0.0046(5) 0.0016(4) N1 0.022(2) 0.0142(19) 0.021(2) 0.0022(16) 0.0067(16) 0.0017(15) N2 0.022(2) 0.0160(19) 0.020(2) 0.0008(16) 0.0033(17) -0.0014(16) N3 0.0182(18) 0.0183(18) 0.0185(19) 0.0017(17) -0.0009(15) -0.0013(17) N4 0.022(2) 0.0169(19) 0.022(2) 0.0025(16) 0.0064(17) 0.0034(16) N5 0.019(2) 0.0153(19) 0.021(2) 0.0020(15) 0.0055(17) 0.0013(15) N6 0.022(2) 0.0148(19) 0.022(2) 0.0004(17) 0.0044(16) -0.0002(16) B1 0.022(3) 0.017(2) 0.020(3) 0.003(2) 0.006(2) 0.001(2) C1 0.022(2) 0.019(2) 0.023(2) -0.0039(19) 0.0061(19) 0.0026(18) C2 0.023(2) 0.023(3) 0.021(2) -0.0035(19) 0.0029(19) -0.0016(18) C3 0.022(2) 0.023(2) 0.019(2) -0.0004(19) 0.0046(19) 0.0020(19) C4 0.019(2) 0.025(2) 0.025(3) 0.000(2) 0.005(2) 0.0010(19) C5 0.019(2) 0.029(3) 0.033(3) 0.004(2) 0.007(2) 0.001(2) C6 0.025(3) 0.016(2) 0.029(3) -0.002(2) 0.010(2) 0.0006(19) C7 0.019(2) 0.019(2) 0.025(3) -0.0020(19) 0.0030(19) 0.0003(18) C8 0.028(3) 0.017(2) 0.029(3) -0.001(2) 0.006(2) -0.001(2) C9 0.021(2) 0.016(2) 0.028(3) 0.0013(19) 0.005(2) -0.0005(18) C10 0.024(3) 0.017(2) 0.029(3) -0.003(2) 0.004(2) -0.0014(19) C11 0.030(3) 0.035(3) 0.021(3) 0.007(2) -0.001(2) -0.002(2) C12 0.025(3) 0.030(3) 0.034(3) 0.006(2) 0.005(2) 0.006(2) C13 0.030(3) 0.027(3) 0.032(3) 0.006(2) 0.014(2) 0.000(2) C14 0.033(3) 0.018(3) 0.027(3) -0.004(2) 0.006(2) -0.002(2) C15 0.037(3) 0.015(2) 0.039(3) 0.008(2) 0.009(3) 0.003(2) C16 0.023(2) 0.014(2) 0.022(2) 0.0027(18) 0.0024(19) 0.0035(18) C17 0.026(3) 0.017(2) 0.033(3) 0.005(2) 0.009(2) 0.006(2) C18 0.035(3) 0.016(2) 0.031(3) -0.001(2) 0.007(2) 0.002(2) C19 0.040(3) 0.015(2) 0.029(3) 0.003(2) 0.002(2) -0.002(2) C20 0.032(3) 0.018(2) 0.026(3) 0.003(2) 0.007(2) -0.004(2) C21 0.023(2) 0.015(2) 0.020(2) 0.0019(18) 0.0028(19) 0.0006(18) C22 0.036(3) 0.019(2) 0.022(2) 0.002(2) 0.004(2) 0.003(2) C23 0.024(3) 0.024(3) 0.034(3) -0.002(2) 0.006(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C16 2.022(5) . ? Rh1 N3 2.099(4) . ? Rh1 N5 2.152(4) . ? Rh1 N1 2.231(4) . ? Rh1 P1 2.2468(15) . ? Rh1 H1 1.59(7) . ? P1 C21 1.799(5) . ? P1 C23 1.804(6) . ? P1 C22 1.828(6) . ? N1 C1 1.342(7) . ? N1 N2 1.376(6) . ? N2 C3 1.354(7) . ? N2 B1 1.548(7) . ? N3 C4 1.330(7) . ? N3 N4 1.385(6) . ? N4 C6 1.351(7) . ? N4 B1 1.542(7) . ? N5 C7 1.342(7) . ? N5 N6 1.365(6) . ? N6 C9 1.360(6) . ? N6 B1 1.542(7) . ? B1 H1B 1.0000 . ? C1 C2 1.403(7) . ? C1 C10 1.505(8) . ? C2 C3 1.378(8) . ? C2 H2 0.9500 . ? C3 C11 1.498(8) . ? C4 C5 1.404(8) . ? C4 C12 1.497(8) . ? C5 C6 1.375(8) . ? C5 H5 0.9500 . ? C6 C13 1.498(8) . ? C7 C8 1.403(8) . ? C7 C14 1.485(8) . ? C8 C9 1.389(8) . ? C8 H8 0.9500 . ? C9 C15 1.500(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.403(7) . ? C16 C21 1.409(8) . ? C17 C18 1.394(8) . ? C17 H17 0.9500 . ? C18 C19 1.403(9) . ? C18 H18 0.9500 . ? C19 C20 1.395(8) . ? C19 H19 0.9500 . ? C20 C21 1.393(7) . ? C20 H20 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N3 100.3(2) . . ? C16 Rh1 N5 174.12(19) . . ? N3 Rh1 N5 85.33(17) . . ? C16 Rh1 N1 91.54(18) . . ? N3 Rh1 N1 85.23(16) . . ? N5 Rh1 N1 87.22(16) . . ? C16 Rh1 P1 69.52(16) . . ? N3 Rh1 P1 167.24(12) . . ? N5 Rh1 P1 105.13(12) . . ? N1 Rh1 P1 102.30(12) . . ? C16 Rh1 H1 88(2) . . ? N3 Rh1 H1 93(2) . . ? N5 Rh1 H1 94(2) . . ? N1 Rh1 H1 178(2) . . ? P1 Rh1 H1 79(2) . . ? C21 P1 C23 112.4(3) . . ? C21 P1 C22 107.5(2) . . ? C23 P1 C22 101.1(3) . . ? C21 P1 Rh1 85.55(18) . . ? C23 P1 Rh1 125.4(2) . . ? C22 P1 Rh1 122.7(2) . . ? C1 N1 N2 106.3(4) . . ? C1 N1 Rh1 138.1(4) . . ? N2 N1 Rh1 115.4(3) . . ? C3 N2 N1 110.1(4) . . ? C3 N2 B1 129.3(5) . . ? N1 N2 B1 120.6(4) . . ? C4 N3 N4 106.6(4) . . ? C4 N3 Rh1 134.3(4) . . ? N4 N3 Rh1 118.4(3) . . ? C6 N4 N3 109.4(4) . . ? C6 N4 B1 129.3(5) . . ? N3 N4 B1 120.2(4) . . ? C7 N5 N6 107.3(4) . . ? C7 N5 Rh1 133.4(4) . . ? N6 N5 Rh1 119.3(3) . . ? C9 N6 N5 110.3(4) . . ? C9 N6 B1 131.1(5) . . ? N5 N6 B1 118.7(4) . . ? N6 B1 N4 108.2(4) . . ? N6 B1 N2 109.5(4) . . ? N4 B1 N2 110.4(4) . . ? N6 B1 H1B 109.6 . . ? N4 B1 H1B 109.6 . . ? N2 B1 H1B 109.6 . . ? N1 C1 C2 110.0(5) . . ? N1 C1 C10 124.3(5) . . ? C2 C1 C10 125.8(5) . . ? C3 C2 C1 105.8(5) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N2 C3 C2 107.7(5) . . ? N2 C3 C11 123.6(5) . . ? C2 C3 C11 128.6(5) . . ? N3 C4 C5 110.1(5) . . ? N3 C4 C12 121.6(5) . . ? C5 C4 C12 128.1(5) . . ? C6 C5 C4 105.6(5) . . ? C6 C5 H5 127.2 . . ? C4 C5 H5 127.2 . . ? N4 C6 C5 108.2(5) . . ? N4 C6 C13 123.6(5) . . ? C5 C6 C13 128.2(5) . . ? N5 C7 C8 109.2(5) . . ? N5 C7 C14 121.4(5) . . ? C8 C7 C14 129.4(5) . . ? C9 C8 C7 106.4(5) . . ? C9 C8 H8 126.8 . . ? C7 C8 H8 126.8 . . ? N6 C9 C8 106.9(5) . . ? N6 C9 C15 122.9(5) . . ? C8 C9 C15 130.2(5) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 117.8(5) . . ? C17 C16 Rh1 135.3(4) . . ? C21 C16 Rh1 106.1(3) . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 121.3(5) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 120.4(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 117.5(5) . . ? C21 C20 H20 121.3 . . ? C19 C20 H20 121.3 . . ? C20 C21 C16 123.5(5) . . ? C20 C21 P1 138.0(4) . . ? C16 C21 P1 98.3(3) . . ? P1 C22 H22A 109.5 . . ? P1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 P1 C21 -3.9(2) . . . . ? N3 Rh1 P1 C21 -42.2(6) . . . . ? N5 Rh1 P1 C21 173.5(2) . . . . ? N1 Rh1 P1 C21 83.1(2) . . . . ? C16 Rh1 P1 C23 -118.4(3) . . . . ? N3 Rh1 P1 C23 -156.6(6) . . . . ? N5 Rh1 P1 C23 59.1(3) . . . . ? N1 Rh1 P1 C23 -31.4(3) . . . . ? C16 Rh1 P1 C22 104.0(3) . . . . ? N3 Rh1 P1 C22 65.8(6) . . . . ? N5 Rh1 P1 C22 -78.5(2) . . . . ? N1 Rh1 P1 C22 -168.9(2) . . . . ? C16 Rh1 N1 C1 37.8(5) . . . . ? N3 Rh1 N1 C1 138.0(5) . . . . ? N5 Rh1 N1 C1 -136.4(5) . . . . ? P1 Rh1 N1 C1 -31.5(5) . . . . ? C16 Rh1 N1 N2 -149.2(4) . . . . ? N3 Rh1 N1 N2 -48.9(3) . . . . ? N5 Rh1 N1 N2 36.6(3) . . . . ? P1 Rh1 N1 N2 141.5(3) . . . . ? C1 N1 N2 C3 2.3(6) . . . . ? Rh1 N1 N2 C3 -172.9(3) . . . . ? C1 N1 N2 B1 -176.6(4) . . . . ? Rh1 N1 N2 B1 8.2(6) . . . . ? C16 Rh1 N3 C4 -56.0(6) . . . . ? N5 Rh1 N3 C4 125.7(5) . . . . ? N1 Rh1 N3 C4 -146.7(5) . . . . ? P1 Rh1 N3 C4 -19.9(10) . . . . ? C16 Rh1 N3 N4 135.1(4) . . . . ? N5 Rh1 N3 N4 -43.2(4) . . . . ? N1 Rh1 N3 N4 44.4(4) . . . . ? P1 Rh1 N3 N4 171.3(4) . . . . ? C4 N3 N4 C6 -2.4(6) . . . . ? Rh1 N3 N4 C6 169.3(3) . . . . ? C4 N3 N4 B1 -171.7(5) . . . . ? Rh1 N3 N4 B1 0.0(6) . . . . ? C16 Rh1 N5 C7 61(2) . . . . ? N3 Rh1 N5 C7 -135.5(5) . . . . ? N1 Rh1 N5 C7 139.1(5) . . . . ? P1 Rh1 N5 C7 37.1(5) . . . . ? C16 Rh1 N5 N6 -119.4(19) . . . . ? N3 Rh1 N5 N6 44.0(4) . . . . ? N1 Rh1 N5 N6 -41.4(4) . . . . ? P1 Rh1 N5 N6 -143.4(3) . . . . ? C7 N5 N6 C9 0.0(6) . . . . ? Rh1 N5 N6 C9 -179.6(3) . . . . ? C7 N5 N6 B1 179.5(4) . . . . ? Rh1 N5 N6 B1 -0.2(6) . . . . ? C9 N6 B1 N4 120.3(6) . . . . ? N5 N6 B1 N4 -59.0(6) . . . . ? C9 N6 B1 N2 -119.3(6) . . . . ? N5 N6 B1 N2 61.4(6) . . . . ? C6 N4 B1 N6 -106.8(6) . . . . ? N3 N4 B1 N6 60.2(6) . . . . ? C6 N4 B1 N2 133.4(5) . . . . ? N3 N4 B1 N2 -59.6(6) . . . . ? C3 N2 B1 N6 115.0(6) . . . . ? N1 N2 B1 N6 -66.3(6) . . . . ? C3 N2 B1 N4 -126.0(5) . . . . ? N1 N2 B1 N4 52.7(6) . . . . ? N2 N1 C1 C2 -2.1(6) . . . . ? Rh1 N1 C1 C2 171.3(4) . . . . ? N2 N1 C1 C10 176.7(5) . . . . ? Rh1 N1 C1 C10 -9.9(8) . . . . ? N1 C1 C2 C3 1.2(6) . . . . ? C10 C1 C2 C3 -177.5(5) . . . . ? N1 N2 C3 C2 -1.5(6) . . . . ? B1 N2 C3 C2 177.3(5) . . . . ? N1 N2 C3 C11 179.2(5) . . . . ? B1 N2 C3 C11 -2.0(9) . . . . ? C1 C2 C3 N2 0.2(6) . . . . ? C1 C2 C3 C11 179.4(6) . . . . ? N4 N3 C4 C5 1.5(6) . . . . ? Rh1 N3 C4 C5 -168.3(4) . . . . ? N4 N3 C4 C12 177.3(5) . . . . ? Rh1 N3 C4 C12 7.5(9) . . . . ? N3 C4 C5 C6 -0.2(7) . . . . ? C12 C4 C5 C6 -175.6(6) . . . . ? N3 N4 C6 C5 2.3(6) . . . . ? B1 N4 C6 C5 170.3(5) . . . . ? N3 N4 C6 C13 -176.8(5) . . . . ? B1 N4 C6 C13 -8.8(9) . . . . ? C4 C5 C6 N4 -1.3(6) . . . . ? C4 C5 C6 C13 177.8(6) . . . . ? N6 N5 C7 C8 -0.5(6) . . . . ? Rh1 N5 C7 C8 179.0(4) . . . . ? N6 N5 C7 C14 179.6(5) . . . . ? Rh1 N5 C7 C14 -0.8(8) . . . . ? N5 C7 C8 C9 0.8(6) . . . . ? C14 C7 C8 C9 -179.4(6) . . . . ? N5 N6 C9 C8 0.5(6) . . . . ? B1 N6 C9 C8 -178.9(5) . . . . ? N5 N6 C9 C15 179.2(5) . . . . ? B1 N6 C9 C15 -0.2(9) . . . . ? C7 C8 C9 N6 -0.8(6) . . . . ? C7 C8 C9 C15 -179.3(6) . . . . ? N3 Rh1 C16 C17 -13.4(6) . . . . ? N5 Rh1 C16 C17 149.8(17) . . . . ? N1 Rh1 C16 C17 72.1(6) . . . . ? P1 Rh1 C16 C17 174.6(6) . . . . ? N3 Rh1 C16 C21 177.2(3) . . . . ? N5 Rh1 C16 C21 -20(2) . . . . ? N1 Rh1 C16 C21 -97.4(4) . . . . ? P1 Rh1 C16 C21 5.2(3) . . . . ? C21 C16 C17 C18 1.0(8) . . . . ? Rh1 C16 C17 C18 -167.5(5) . . . . ? C16 C17 C18 C19 0.8(9) . . . . ? C17 C18 C19 C20 -1.6(9) . . . . ? C18 C19 C20 C21 0.4(9) . . . . ? C19 C20 C21 C16 1.5(8) . . . . ? C19 C20 C21 P1 174.9(5) . . . . ? C17 C16 C21 C20 -2.2(8) . . . . ? Rh1 C16 C21 C20 169.4(5) . . . . ? C17 C16 C21 P1 -177.8(4) . . . . ? Rh1 C16 C21 P1 -6.1(4) . . . . ? C23 P1 C21 C20 -42.5(7) . . . . ? C22 P1 C21 C20 68.0(7) . . . . ? Rh1 P1 C21 C20 -169.1(6) . . . . ? C23 P1 C21 C16 132.0(4) . . . . ? C22 P1 C21 C16 -117.6(4) . . . . ? Rh1 P1 C21 C16 5.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 32.57 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.200 _refine_diff_density_min -1.330 _refine_diff_density_rms 0.178 #===end data_jontt11_cmpd9a _database_code_depnum_ccdc_archive 'CCDC 770117' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _vrf_CHEMW03_jontt11 ; PROBLEM: _A ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 RESPONSE: See response to alert PLAT602. ; _vrf_PLAT602_jontt11 ; PROBLEM: _A VERY LARGE Solvent Accessible VOID(S) in Structure! RESPONSE: Highly disordered co-crystallized n-hexane solvent molecules (two per unit cell) were found in channels parallel to the a-axis. The reflection contributions from this solvent were removed using program PLATON, function SQUEEZE (Spek, 2003), which determined there to be 99 electrons in 394 A**3 removed per unit cell. Since the solvent could be identified, it was included in the molecular formula, but not in the atom list. ; _vrf_PLAT043_jontt11 ; PROBLEM: _A Check Reported Molecular Weight ................ 792.48 RESPONSE: See above. ; _vrf_PLAT041_jontt11 ; PROBLEM: _C Calc. and Reported SumFormula Strings Differ ? RESPONSE: See above. ; _vrf_PLAT068_jontt11 ; PROBLEM: _C Reported F000 Differs from Calcd (or Missing) ... ? RESPONSE: See above. ; _vrf_FORMU01_jontt11 ; PROBLEM: _G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. RESPONSE: See above. ; _vrf_CELLZ01_jontt11 ; PROBLEM: _G Difference between formula and atom_site contents detected. RESPONSE: See above. ; _chemical_name_common jontt11 _chemical_melting_point ? _chemical_formula_moiety 'C29 H34 B F5 N6 P Rh, C6 H14' _chemical_formula_sum 'C35 H48 B F5 N6 P Rh' _chemical_formula_weight 792.48 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' _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 10.2069(10) _cell_length_b 13.0730(13) _cell_length_c 15.3042(15) _cell_angle_alpha 105.613(2) _cell_angle_beta 108.235(2) _cell_angle_gamma 101.547(2) _cell_volume 1775.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3787 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 37.89 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8528 _exptl_absorpt_correction_T_max 0.9436 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41158 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 36.32 _reflns_number_total 16867 _reflns_number_gt 14559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The hydride ligand atom was found from the difference Fourier map, and its position and isotropic displacement parameter were refined independently from those of all other atoms. ; _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^)+(0.0379P)^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 16867 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.677154(8) 0.247319(6) 0.369760(5) 0.01331(2) Uani 1 1 d . . . H1 H 0.8316(18) 0.3098(13) 0.4291(12) 0.030(4) Uiso 1 1 d . . . P1 P 0.62466(3) 0.30298(2) 0.505766(19) 0.01464(5) Uani 1 1 d . . . N1 N 0.44233(10) 0.15490(8) 0.26693(6) 0.01820(16) Uani 1 1 d . . . N2 N 0.39629(10) 0.18039(7) 0.18361(6) 0.01752(15) Uani 1 1 d . . . N3 N 0.72782(10) 0.19942(7) 0.24489(6) 0.01633(15) Uani 1 1 d . . . N4 N 0.62986(10) 0.19429(7) 0.15746(6) 0.01783(16) Uani 1 1 d . . . N5 N 0.65563(9) 0.38962(7) 0.32797(6) 0.01560(15) Uani 1 1 d . . . N6 N 0.57518(10) 0.36795(8) 0.23035(6) 0.01879(16) Uani 1 1 d . . . B1 B 0.50798(13) 0.24769(10) 0.15586(9) 0.0189(2) Uani 1 1 d . . . H1B H 0.4591 0.2486 0.0884 0.023 Uiso 1 1 calc R . . C1 C 0.32610(12) 0.08267(9) 0.26366(8) 0.02037(19) Uani 1 1 d . . . C2 C 0.20458(12) 0.06343(10) 0.17919(8) 0.0224(2) Uani 1 1 d . . . H2 H 0.1088 0.0163 0.1597 0.027 Uiso 1 1 calc R . . C3 C 0.25303(12) 0.12699(9) 0.13042(8) 0.01971(19) Uani 1 1 d . . . C4 C 0.82977(12) 0.15887(9) 0.22560(8) 0.01932(18) Uani 1 1 d . . . C5 C 0.79644(13) 0.12554(9) 0.12440(8) 0.0229(2) Uani 1 1 d . . . H5 H 0.8503 0.0933 0.0905 0.028 Uiso 1 1 calc R . . C6 C 0.66978(13) 0.14867(9) 0.08331(8) 0.0213(2) Uani 1 1 d . . . C7 C 0.71936(11) 0.50083(8) 0.36946(8) 0.01631(17) Uani 1 1 d . . . C8 C 0.67717(13) 0.55045(9) 0.29943(8) 0.02094(19) Uani 1 1 d . . . H8 H 0.7051 0.6279 0.3097 0.025 Uiso 1 1 calc R . . C9 C 0.58699(13) 0.46457(9) 0.21254(8) 0.0219(2) Uani 1 1 d . . . C10 C 0.32960(14) 0.03050(11) 0.33930(9) 0.0276(2) Uani 1 1 d . . . H10A H 0.2591 -0.0446 0.3082 0.041 Uiso 1 1 calc R . . H10B H 0.3049 0.0762 0.3902 0.041 Uiso 1 1 calc R . . H10C H 0.4271 0.0256 0.3693 0.041 Uiso 1 1 calc R . . C11 C 0.17111(13) 0.14150(10) 0.03693(8) 0.0257(2) Uani 1 1 d . . . H11A H 0.1841 0.2211 0.0490 0.039 Uiso 1 1 calc R . . H11B H 0.0677 0.1011 0.0138 0.039 Uiso 1 1 calc R . . H11C H 0.2079 0.1118 -0.0133 0.039 Uiso 1 1 calc R . . C12 C 0.95831(13) 0.15553(10) 0.30399(9) 0.0241(2) Uani 1 1 d . . . H12A H 0.9724 0.2081 0.3679 0.036 Uiso 1 1 calc R . . H12B H 1.0449 0.1765 0.2897 0.036 Uiso 1 1 calc R . . H12C H 0.9420 0.0798 0.3058 0.036 Uiso 1 1 calc R . . C13 C 0.58432(15) 0.12739(12) -0.02225(8) 0.0300(3) Uani 1 1 d . . . H13A H 0.4866 0.0767 -0.0427 0.045 Uiso 1 1 calc R . . H13B H 0.6327 0.0933 -0.0629 0.045 Uiso 1 1 calc R . . H13C H 0.5776 0.1982 -0.0305 0.045 Uiso 1 1 calc R . . C14 C 0.82388(12) 0.55959(9) 0.47335(8) 0.01886(18) Uani 1 1 d . . . H14A H 0.8903 0.5168 0.4905 0.028 Uiso 1 1 calc R . . H14B H 0.7707 0.5665 0.5169 0.028 Uiso 1 1 calc R . . H14C H 0.8795 0.6342 0.4812 0.028 Uiso 1 1 calc R . . C15 C 0.51257(17) 0.46960(12) 0.11352(10) 0.0347(3) Uani 1 1 d . . . H15A H 0.5338 0.5477 0.1179 0.052 Uiso 1 1 calc R . . H15B H 0.4076 0.4358 0.0911 0.052 Uiso 1 1 calc R . . H15C H 0.5475 0.4286 0.0666 0.052 Uiso 1 1 calc R . . C16 C 0.71997(11) 0.11211(8) 0.40036(7) 0.01612(17) Uani 1 1 d . . . C17 C 0.82139(11) 0.11764(9) 0.48862(8) 0.01716(17) Uani 1 1 d . . . F1 F 0.90117(7) 0.21759(6) 0.56152(5) 0.02142(13) Uani 1 1 d . . . C18 C 0.84988(12) 0.02667(9) 0.51074(8) 0.01977(19) Uani 1 1 d . . . F2 F 0.94804(8) 0.04080(6) 0.59925(6) 0.02581(14) Uani 1 1 d . . . C19 C 0.77743(13) -0.07909(9) 0.44170(9) 0.0230(2) Uani 1 1 d . . . F3 F 0.80281(9) -0.16888(6) 0.46146(7) 0.03350(18) Uani 1 1 d . . . C20 C 0.67905(14) -0.09048(9) 0.35142(9) 0.0233(2) Uani 1 1 d . . . F4 F 0.60671(10) -0.19325(6) 0.28261(6) 0.03502(18) Uani 1 1 d . . . C21 C 0.65469(12) 0.00290(9) 0.33225(8) 0.01920(18) Uani 1 1 d . . . F5 F 0.55882(9) -0.01836(6) 0.24087(5) 0.02634(15) Uani 1 1 d . . . C22 C 0.74566(12) 0.42675(9) 0.61382(7) 0.01730(17) Uani 1 1 d . . . C23 C 0.68767(13) 0.49222(10) 0.66985(8) 0.0227(2) Uani 1 1 d . . . H23 H 0.5855 0.4735 0.6510 0.027 Uiso 1 1 calc R . . C24 C 0.77891(16) 0.58515(11) 0.75350(9) 0.0294(3) Uani 1 1 d . . . H24 H 0.7385 0.6299 0.7908 0.035 Uiso 1 1 calc R . . C25 C 0.92761(15) 0.61248(10) 0.78234(9) 0.0289(3) Uani 1 1 d . . . H25 H 0.9894 0.6761 0.8392 0.035 Uiso 1 1 calc R . . C26 C 0.98660(14) 0.54691(10) 0.72817(9) 0.0260(2) Uani 1 1 d . . . H26 H 1.0890 0.5654 0.7482 0.031 Uiso 1 1 calc R . . C27 C 0.89679(12) 0.45427(9) 0.64471(8) 0.02076(19) Uani 1 1 d . . . H27 H 0.9381 0.4093 0.6084 0.025 Uiso 1 1 calc R . . C28 C 0.59752(13) 0.20744(9) 0.57113(8) 0.02079(19) Uani 1 1 d . . . H28A H 0.5519 0.2357 0.6161 0.031 Uiso 1 1 calc R . . H28B H 0.6915 0.2021 0.6088 0.031 Uiso 1 1 calc R . . H28C H 0.5346 0.1333 0.5235 0.031 Uiso 1 1 calc R . . C29 C 0.45267(12) 0.33268(10) 0.47056(9) 0.0226(2) Uani 1 1 d . . . H29A H 0.4192 0.3418 0.5248 0.034 Uiso 1 1 calc R . . H29B H 0.3804 0.2706 0.4120 0.034 Uiso 1 1 calc R . . H29C H 0.4658 0.4016 0.4559 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01548(4) 0.01193(3) 0.01194(3) 0.00481(2) 0.00431(2) 0.00393(2) P1 0.01580(11) 0.01459(11) 0.01348(10) 0.00538(8) 0.00527(9) 0.00476(9) N1 0.0187(4) 0.0178(4) 0.0157(4) 0.0070(3) 0.0046(3) 0.0029(3) N2 0.0189(4) 0.0162(4) 0.0139(3) 0.0054(3) 0.0029(3) 0.0038(3) N3 0.0194(4) 0.0149(4) 0.0144(3) 0.0057(3) 0.0062(3) 0.0049(3) N4 0.0221(4) 0.0164(4) 0.0133(3) 0.0054(3) 0.0063(3) 0.0032(3) N5 0.0171(4) 0.0134(3) 0.0147(3) 0.0055(3) 0.0041(3) 0.0042(3) N6 0.0226(4) 0.0159(4) 0.0155(4) 0.0077(3) 0.0034(3) 0.0046(3) B1 0.0219(5) 0.0173(5) 0.0146(4) 0.0069(4) 0.0041(4) 0.0037(4) C1 0.0189(4) 0.0211(5) 0.0181(4) 0.0068(4) 0.0062(4) 0.0016(4) C2 0.0178(4) 0.0232(5) 0.0190(5) 0.0043(4) 0.0036(4) 0.0015(4) C3 0.0188(4) 0.0180(4) 0.0152(4) 0.0020(3) 0.0017(3) 0.0040(4) C4 0.0231(5) 0.0150(4) 0.0210(5) 0.0055(4) 0.0110(4) 0.0055(4) C5 0.0279(5) 0.0190(5) 0.0202(5) 0.0024(4) 0.0130(4) 0.0043(4) C6 0.0266(5) 0.0175(4) 0.0158(4) 0.0034(3) 0.0094(4) 0.0006(4) C7 0.0180(4) 0.0144(4) 0.0181(4) 0.0068(3) 0.0079(3) 0.0055(3) C8 0.0262(5) 0.0152(4) 0.0225(5) 0.0098(4) 0.0081(4) 0.0066(4) C9 0.0257(5) 0.0185(5) 0.0217(5) 0.0118(4) 0.0061(4) 0.0060(4) C10 0.0230(5) 0.0307(6) 0.0233(5) 0.0130(5) 0.0056(4) -0.0026(4) C11 0.0241(5) 0.0250(5) 0.0180(5) 0.0057(4) -0.0014(4) 0.0052(4) C12 0.0257(5) 0.0259(5) 0.0253(5) 0.0101(4) 0.0121(4) 0.0126(4) C13 0.0353(6) 0.0320(6) 0.0151(5) 0.0040(4) 0.0090(5) 0.0020(5) C14 0.0203(4) 0.0148(4) 0.0188(4) 0.0045(3) 0.0067(4) 0.0036(3) C15 0.0453(8) 0.0257(6) 0.0252(6) 0.0162(5) 0.0011(5) 0.0052(5) C16 0.0196(4) 0.0139(4) 0.0153(4) 0.0056(3) 0.0069(3) 0.0055(3) C17 0.0185(4) 0.0160(4) 0.0178(4) 0.0071(3) 0.0068(3) 0.0061(3) F1 0.0225(3) 0.0182(3) 0.0181(3) 0.0061(2) 0.0019(2) 0.0051(2) C18 0.0201(4) 0.0225(5) 0.0231(5) 0.0136(4) 0.0095(4) 0.0104(4) F2 0.0240(3) 0.0314(4) 0.0286(3) 0.0194(3) 0.0082(3) 0.0134(3) C19 0.0282(5) 0.0175(5) 0.0317(6) 0.0141(4) 0.0152(5) 0.0114(4) F3 0.0424(4) 0.0212(3) 0.0471(5) 0.0211(3) 0.0183(4) 0.0172(3) C20 0.0308(6) 0.0132(4) 0.0263(5) 0.0061(4) 0.0125(5) 0.0066(4) F4 0.0486(5) 0.0126(3) 0.0350(4) 0.0033(3) 0.0116(4) 0.0059(3) C21 0.0240(5) 0.0152(4) 0.0175(4) 0.0059(3) 0.0073(4) 0.0055(4) F5 0.0352(4) 0.0182(3) 0.0161(3) 0.0028(2) 0.0031(3) 0.0043(3) C22 0.0216(4) 0.0153(4) 0.0145(4) 0.0050(3) 0.0070(3) 0.0049(3) C23 0.0264(5) 0.0210(5) 0.0202(5) 0.0047(4) 0.0111(4) 0.0062(4) C24 0.0383(7) 0.0221(5) 0.0227(5) -0.0001(4) 0.0138(5) 0.0066(5) C25 0.0355(6) 0.0199(5) 0.0209(5) 0.0011(4) 0.0084(5) -0.0004(5) C26 0.0249(5) 0.0228(5) 0.0213(5) 0.0048(4) 0.0049(4) -0.0007(4) C27 0.0215(5) 0.0191(5) 0.0182(4) 0.0047(4) 0.0065(4) 0.0037(4) C28 0.0236(5) 0.0202(5) 0.0192(4) 0.0090(4) 0.0089(4) 0.0043(4) C29 0.0204(5) 0.0256(5) 0.0220(5) 0.0072(4) 0.0075(4) 0.0107(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 C16 2.0400(10) . ? Rh1 N3 2.1013(9) . ? Rh1 N5 2.1527(9) . ? Rh1 N1 2.2667(9) . ? Rh1 P1 2.2777(3) . ? Rh1 H1 1.472(16) . ? P1 C29 1.8210(11) . ? P1 C28 1.8290(11) . ? P1 C22 1.8329(11) . ? N1 C1 1.3380(14) . ? N1 N2 1.3691(12) . ? N2 C3 1.3523(14) . ? N2 B1 1.5351(15) . ? N3 C4 1.3341(14) . ? N3 N4 1.3720(12) . ? N4 C6 1.3534(14) . ? N4 B1 1.5406(16) . ? N5 C7 1.3438(13) . ? N5 N6 1.3777(12) . ? N6 C9 1.3526(14) . ? N6 B1 1.5349(15) . ? B1 H1B 1.0000 . ? C1 C2 1.4033(16) . ? C1 C10 1.4885(16) . ? C2 C3 1.3757(16) . ? C2 H2 0.9500 . ? C3 C11 1.4978(15) . ? C4 C5 1.3971(15) . ? C4 C12 1.4929(17) . ? C5 C6 1.3814(18) . ? C5 H5 0.9500 . ? C6 C13 1.4924(16) . ? C7 C8 1.3972(15) . ? C7 C14 1.4863(15) . ? C8 C9 1.3758(16) . ? C8 H8 0.9500 . ? C9 C15 1.4936(16) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.3941(14) . ? C16 C21 1.3973(14) . ? C17 F1 1.3549(12) . ? C17 C18 1.3810(15) . ? C18 F2 1.3470(13) . ? C18 C19 1.3749(17) . ? C19 F3 1.3418(13) . ? C19 C20 1.3787(17) . ? C20 F4 1.3468(13) . ? C20 C21 1.3808(15) . ? C21 F5 1.3476(13) . ? C22 C23 1.3941(15) . ? C22 C27 1.4008(16) . ? C23 C24 1.3950(17) . ? C23 H23 0.9500 . ? C24 C25 1.380(2) . ? C24 H24 0.9500 . ? C25 C26 1.3860(19) . ? C25 H25 0.9500 . ? C26 C27 1.3888(16) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N3 89.58(4) . . ? C16 Rh1 N5 171.51(4) . . ? N3 Rh1 N5 83.09(3) . . ? C16 Rh1 N1 95.23(4) . . ? N3 Rh1 N1 86.58(3) . . ? N5 Rh1 N1 88.63(3) . . ? C16 Rh1 P1 91.31(3) . . ? N3 Rh1 P1 178.82(2) . . ? N5 Rh1 P1 95.96(2) . . ? N1 Rh1 P1 94.10(3) . . ? C16 Rh1 H1 87.5(6) . . ? N3 Rh1 H1 89.1(6) . . ? N5 Rh1 H1 88.1(6) . . ? N1 Rh1 H1 174.8(6) . . ? P1 Rh1 H1 90.2(6) . . ? C29 P1 C28 102.80(6) . . ? C29 P1 C22 103.51(5) . . ? C28 P1 C22 97.43(5) . . ? C29 P1 Rh1 108.85(4) . . ? C28 P1 Rh1 119.96(4) . . ? C22 P1 Rh1 121.70(4) . . ? C1 N1 N2 105.95(9) . . ? C1 N1 Rh1 138.89(7) . . ? N2 N1 Rh1 115.08(6) . . ? C3 N2 N1 110.71(9) . . ? C3 N2 B1 129.11(9) . . ? N1 N2 B1 119.61(8) . . ? C4 N3 N4 107.64(8) . . ? C4 N3 Rh1 134.57(7) . . ? N4 N3 Rh1 117.30(7) . . ? C6 N4 N3 109.42(9) . . ? C6 N4 B1 129.64(9) . . ? N3 N4 B1 120.58(8) . . ? C7 N5 N6 106.27(8) . . ? C7 N5 Rh1 136.07(7) . . ? N6 N5 Rh1 116.74(6) . . ? C9 N6 N5 110.03(9) . . ? C9 N6 B1 128.41(9) . . ? N5 N6 B1 120.77(8) . . ? N6 B1 N2 109.73(9) . . ? N6 B1 N4 108.67(9) . . ? N2 B1 N4 109.89(9) . . ? N6 B1 H1B 109.5 . . ? N2 B1 H1B 109.5 . . ? N4 B1 H1B 109.5 . . ? N1 C1 C2 110.20(10) . . ? N1 C1 C10 123.66(10) . . ? C2 C1 C10 126.14(10) . . ? C3 C2 C1 105.70(10) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N2 C3 C2 107.42(9) . . ? N2 C3 C11 122.85(10) . . ? C2 C3 C11 129.72(10) . . ? N3 C4 C5 108.98(10) . . ? N3 C4 C12 122.86(10) . . ? C5 C4 C12 128.13(10) . . ? C6 C5 C4 106.51(10) . . ? C6 C5 H5 126.7 . . ? C4 C5 H5 126.7 . . ? N4 C6 C5 107.43(10) . . ? N4 C6 C13 123.48(11) . . ? C5 C6 C13 129.07(11) . . ? N5 C7 C8 109.79(9) . . ? N5 C7 C14 124.14(9) . . ? C8 C7 C14 126.02(10) . . ? C9 C8 C7 106.21(9) . . ? C9 C8 H8 126.9 . . ? C7 C8 H8 126.9 . . ? N6 C9 C8 107.69(9) . . ? N6 C9 C15 123.24(10) . . ? C8 C9 C15 129.07(10) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 112.23(9) . . ? C17 C16 Rh1 124.58(7) . . ? C21 C16 Rh1 123.12(8) . . ? F1 C17 C18 114.35(9) . . ? F1 C17 C16 120.53(9) . . ? C18 C17 C16 125.12(10) . . ? F2 C18 C19 119.85(10) . . ? F2 C18 C17 120.54(10) . . ? C19 C18 C17 119.61(10) . . ? F3 C19 C18 120.78(11) . . ? F3 C19 C20 120.86(11) . . ? C18 C19 C20 118.36(10) . . ? F4 C20 C19 119.43(10) . . ? F4 C20 C21 120.50(11) . . ? C19 C20 C21 120.06(10) . . ? F5 C21 C20 114.73(9) . . ? F5 C21 C16 120.79(9) . . ? C20 C21 C16 124.48(10) . . ? C23 C22 C27 118.76(10) . . ? C23 C22 P1 119.87(8) . . ? C27 C22 P1 121.29(8) . . ? C22 C23 C24 120.35(11) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 120.35(12) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.82(11) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C27 120.32(12) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 120.37(11) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? P1 C28 H28A 109.5 . . ? P1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P1 C29 H29A 109.5 . . ? P1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 P1 C29 -131.04(5) . . . . ? N3 Rh1 P1 C29 89.5(12) . . . . ? N5 Rh1 P1 C29 53.34(5) . . . . ? N1 Rh1 P1 C29 -35.70(5) . . . . ? C16 Rh1 P1 C28 -13.21(5) . . . . ? N3 Rh1 P1 C28 -152.7(12) . . . . ? N5 Rh1 P1 C28 171.17(5) . . . . ? N1 Rh1 P1 C28 82.13(5) . . . . ? C16 Rh1 P1 C22 108.89(5) . . . . ? N3 Rh1 P1 C22 -30.6(12) . . . . ? N5 Rh1 P1 C22 -66.73(5) . . . . ? N1 Rh1 P1 C22 -155.77(5) . . . . ? C16 Rh1 N1 C1 45.48(12) . . . . ? N3 Rh1 N1 C1 134.75(12) . . . . ? N5 Rh1 N1 C1 -142.10(12) . . . . ? P1 Rh1 N1 C1 -46.22(12) . . . . ? C16 Rh1 N1 N2 -138.43(7) . . . . ? N3 Rh1 N1 N2 -49.16(7) . . . . ? N5 Rh1 N1 N2 34.00(7) . . . . ? P1 Rh1 N1 N2 129.87(7) . . . . ? C1 N1 N2 C3 1.40(12) . . . . ? Rh1 N1 N2 C3 -175.94(7) . . . . ? C1 N1 N2 B1 -170.68(10) . . . . ? Rh1 N1 N2 B1 11.99(12) . . . . ? C16 Rh1 N3 C4 -40.77(10) . . . . ? N5 Rh1 N3 C4 134.94(10) . . . . ? N1 Rh1 N3 C4 -136.03(10) . . . . ? P1 Rh1 N3 C4 98.7(12) . . . . ? C16 Rh1 N3 N4 130.07(7) . . . . ? N5 Rh1 N3 N4 -54.22(7) . . . . ? N1 Rh1 N3 N4 34.81(7) . . . . ? P1 Rh1 N3 N4 -90.4(12) . . . . ? C4 N3 N4 C6 1.01(12) . . . . ? Rh1 N3 N4 C6 -172.16(7) . . . . ? C4 N3 N4 B1 -172.76(9) . . . . ? Rh1 N3 N4 B1 14.07(12) . . . . ? C16 Rh1 N5 C7 -89.1(3) . . . . ? N3 Rh1 N5 C7 -119.58(10) . . . . ? N1 Rh1 N5 C7 153.69(10) . . . . ? P1 Rh1 N5 C7 59.72(10) . . . . ? C16 Rh1 N5 N6 78.1(3) . . . . ? N3 Rh1 N5 N6 47.60(7) . . . . ? N1 Rh1 N5 N6 -39.13(7) . . . . ? P1 Rh1 N5 N6 -133.10(7) . . . . ? C7 N5 N6 C9 -1.18(12) . . . . ? Rh1 N5 N6 C9 -171.96(7) . . . . ? C7 N5 N6 B1 169.47(9) . . . . ? Rh1 N5 N6 B1 -1.30(12) . . . . ? C9 N6 B1 N2 -127.95(12) . . . . ? N5 N6 B1 N2 63.28(13) . . . . ? C9 N6 B1 N4 111.87(12) . . . . ? N5 N6 B1 N4 -56.91(12) . . . . ? C3 N2 B1 N6 120.76(11) . . . . ? N1 N2 B1 N6 -68.80(12) . . . . ? C3 N2 B1 N4 -119.79(11) . . . . ? N1 N2 B1 N4 50.64(12) . . . . ? C6 N4 B1 N6 -122.42(11) . . . . ? N3 N4 B1 N6 49.95(12) . . . . ? C6 N4 B1 N2 117.49(11) . . . . ? N3 N4 B1 N2 -70.14(12) . . . . ? N2 N1 C1 C2 -1.18(13) . . . . ? Rh1 N1 C1 C2 175.14(9) . . . . ? N2 N1 C1 C10 177.99(11) . . . . ? Rh1 N1 C1 C10 -5.7(2) . . . . ? N1 C1 C2 C3 0.56(14) . . . . ? C10 C1 C2 C3 -178.58(12) . . . . ? N1 N2 C3 C2 -1.06(13) . . . . ? B1 N2 C3 C2 170.05(11) . . . . ? N1 N2 C3 C11 178.04(10) . . . . ? B1 N2 C3 C11 -10.84(18) . . . . ? C1 C2 C3 N2 0.31(13) . . . . ? C1 C2 C3 C11 -178.71(12) . . . . ? N4 N3 C4 C5 -0.89(12) . . . . ? Rh1 N3 C4 C5 170.58(8) . . . . ? N4 N3 C4 C12 177.46(10) . . . . ? Rh1 N3 C4 C12 -11.08(17) . . . . ? N3 C4 C5 C6 0.45(13) . . . . ? C12 C4 C5 C6 -177.78(11) . . . . ? N3 N4 C6 C5 -0.72(12) . . . . ? B1 N4 C6 C5 172.32(10) . . . . ? N3 N4 C6 C13 177.95(10) . . . . ? B1 N4 C6 C13 -9.01(18) . . . . ? C4 C5 C6 N4 0.17(12) . . . . ? C4 C5 C6 C13 -178.41(12) . . . . ? N6 N5 C7 C8 1.45(12) . . . . ? Rh1 N5 C7 C8 169.54(8) . . . . ? N6 N5 C7 C14 -176.02(10) . . . . ? Rh1 N5 C7 C14 -7.94(16) . . . . ? N5 C7 C8 C9 -1.20(13) . . . . ? C14 C7 C8 C9 176.22(11) . . . . ? N5 N6 C9 C8 0.45(13) . . . . ? B1 N6 C9 C8 -169.29(11) . . . . ? N5 N6 C9 C15 179.97(12) . . . . ? B1 N6 C9 C15 10.2(2) . . . . ? C7 C8 C9 N6 0.44(13) . . . . ? C7 C8 C9 C15 -179.04(13) . . . . ? N3 Rh1 C16 C17 123.06(9) . . . . ? N5 Rh1 C16 C17 92.8(2) . . . . ? N1 Rh1 C16 C17 -150.41(9) . . . . ? P1 Rh1 C16 C17 -56.17(9) . . . . ? N3 Rh1 C16 C21 -53.74(9) . . . . ? N5 Rh1 C16 C21 -84.0(3) . . . . ? N1 Rh1 C16 C21 32.79(9) . . . . ? P1 Rh1 C16 C21 127.02(9) . . . . ? C21 C16 C17 F1 176.50(9) . . . . ? Rh1 C16 C17 F1 -0.61(14) . . . . ? C21 C16 C17 C18 -3.86(16) . . . . ? Rh1 C16 C17 C18 179.03(8) . . . . ? F1 C17 C18 F2 1.14(15) . . . . ? C16 C17 C18 F2 -178.52(10) . . . . ? F1 C17 C18 C19 -178.80(10) . . . . ? C16 C17 C18 C19 1.54(17) . . . . ? F2 C18 C19 F3 0.27(17) . . . . ? C17 C18 C19 F3 -179.80(10) . . . . ? F2 C18 C19 C20 -179.18(10) . . . . ? C17 C18 C19 C20 0.75(17) . . . . ? F3 C19 C20 F4 0.58(18) . . . . ? C18 C19 C20 F4 -179.97(11) . . . . ? F3 C19 C20 C21 -179.77(11) . . . . ? C18 C19 C20 C21 -0.32(18) . . . . ? F4 C20 C21 F5 -1.82(16) . . . . ? C19 C20 C21 F5 178.53(11) . . . . ? F4 C20 C21 C16 177.20(11) . . . . ? C19 C20 C21 C16 -2.45(18) . . . . ? C17 C16 C21 F5 -176.74(10) . . . . ? Rh1 C16 C21 F5 0.41(15) . . . . ? C17 C16 C21 C20 4.30(16) . . . . ? Rh1 C16 C21 C20 -178.55(9) . . . . ? C29 P1 C22 C23 23.89(10) . . . . ? C28 P1 C22 C23 -81.24(10) . . . . ? Rh1 P1 C22 C23 146.50(8) . . . . ? C29 P1 C22 C27 -159.42(9) . . . . ? C28 P1 C22 C27 95.44(10) . . . . ? Rh1 P1 C22 C27 -36.81(10) . . . . ? C27 C22 C23 C24 1.78(17) . . . . ? P1 C22 C23 C24 178.54(10) . . . . ? C22 C23 C24 C25 -0.8(2) . . . . ? C23 C24 C25 C26 -0.3(2) . . . . ? C24 C25 C26 C27 0.4(2) . . . . ? C25 C26 C27 C22 0.65(18) . . . . ? C23 C22 C27 C26 -1.71(17) . . . . ? P1 C22 C27 C26 -178.43(9) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 36.32 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.104 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.078 #===end data_jontt16_cmpd9b _database_code_depnum_ccdc_archive 'CCDC 770118' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt16 _chemical_melting_point ? _chemical_formula_moiety 'C29 H35 B F4 N6 P Rh, C6 H14' _chemical_formula_sum 'C35 H49 B F4 N6 P Rh' _chemical_formula_weight 774.49 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' _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 10.2654(11) _cell_length_b 13.2828(14) _cell_length_c 15.0471(16) _cell_angle_alpha 106.173(2) _cell_angle_beta 107.854(2) _cell_angle_gamma 101.522(2) _cell_volume 1782.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3982 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 38.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8734 _exptl_absorpt_correction_T_max 0.9443 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64752 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 37.41 _reflns_number_total 18391 _reflns_number_gt 15601 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The hydride ligand atom was found from the difference Fourier map and its position and isotropic displacement parameter were refined independently from those of all other atoms. ; _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^)+(0.0413P)^2^+0.5145P] 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 18391 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.172425(9) 0.746438(7) 0.865878(6) 0.01213(2) Uani 1 1 d . . . H1 H 0.328(2) 0.8060(15) 0.9263(14) 0.022(4) Uiso 1 1 d . . . P1 P 0.12576(3) 0.80325(2) 1.00613(2) 0.01320(5) Uani 1 1 d . . . N1 N -0.06149(11) 0.65368(8) 0.76188(7) 0.01577(16) Uani 1 1 d . . . N2 N -0.10745(11) 0.67750(8) 0.67688(7) 0.01585(16) Uani 1 1 d . . . N3 N 0.21999(11) 0.69566(8) 0.73690(7) 0.01513(16) Uani 1 1 d . . . N4 N 0.12322(11) 0.69028(8) 0.64825(7) 0.01626(17) Uani 1 1 d . . . N5 N 0.15108(11) 0.88617(8) 0.82269(7) 0.01443(16) Uani 1 1 d . . . N6 N 0.06901(11) 0.86290(8) 0.72351(7) 0.01645(17) Uani 1 1 d . . . B1 B 0.00272(15) 0.74345(11) 0.64771(10) 0.0171(2) Uani 1 1 d . . . H1B H -0.0464 0.7434 0.5791 0.020 Uiso 1 1 calc R . . C1 C -0.17873(12) 0.58689(10) 0.76181(9) 0.01691(19) Uani 1 1 d . . . C2 C -0.29982(13) 0.56917(11) 0.67714(9) 0.0191(2) Uani 1 1 d . . . H2 H -0.3959 0.5255 0.6592 0.023 Uiso 1 1 calc R . . C3 C -0.25062(13) 0.62834(10) 0.62534(9) 0.0178(2) Uani 1 1 d . . . C4 C 0.32087(13) 0.65460(10) 0.71711(9) 0.0179(2) Uani 1 1 d . . . C5 C 0.28771(15) 0.62065(11) 0.61371(10) 0.0214(2) Uani 1 1 d . . . H5 H 0.3407 0.5880 0.5788 0.026 Uiso 1 1 calc R . . C6 C 0.16269(14) 0.64412(10) 0.57249(9) 0.0193(2) Uani 1 1 d . . . C7 C 0.21211(12) 0.99616(9) 0.86416(9) 0.01493(18) Uani 1 1 d . . . C8 C 0.16652(14) 1.04372(10) 0.79295(10) 0.0191(2) Uani 1 1 d . . . H8 H 0.1920 1.1200 0.8031 0.023 Uiso 1 1 calc R . . C9 C 0.07700(14) 0.95723(10) 0.70495(9) 0.0188(2) Uani 1 1 d . . . C10 C -0.17707(14) 0.54033(12) 0.84143(10) 0.0223(2) Uani 1 1 d . . . H10A H -0.0820 0.5326 0.8711 0.034 Uiso 1 1 calc R . . H10B H -0.2506 0.4678 0.8120 0.034 Uiso 1 1 calc R . . H10C H -0.1974 0.5900 0.8935 0.034 Uiso 1 1 calc R . . C11 C -0.33312(15) 0.64236(12) 0.53120(10) 0.0234(2) Uani 1 1 d . . . H11A H -0.3184 0.7210 0.5437 0.035 Uiso 1 1 calc R . . H11B H -0.4359 0.6039 0.5094 0.035 Uiso 1 1 calc R . . H11C H -0.2991 0.6113 0.4787 0.035 Uiso 1 1 calc R . . C12 C 0.44710(15) 0.65104(12) 0.79686(11) 0.0236(2) Uani 1 1 d . . . H12A H 0.4629 0.7052 0.8617 0.035 Uiso 1 1 calc R . . H12B H 0.5330 0.6685 0.7813 0.035 Uiso 1 1 calc R . . H12C H 0.4284 0.5771 0.8000 0.035 Uiso 1 1 calc R . . C13 C 0.07742(16) 0.62125(13) 0.46467(10) 0.0263(3) Uani 1 1 d . . . H13A H 0.0691 0.6905 0.4560 0.039 Uiso 1 1 calc R . . H13B H -0.0190 0.5703 0.4441 0.039 Uiso 1 1 calc R . . H13C H 0.1262 0.5880 0.4233 0.039 Uiso 1 1 calc R . . C14 C 0.31790(13) 1.05598(10) 0.96945(9) 0.0182(2) Uani 1 1 d . . . H14A H 0.3859 1.0152 0.9857 0.027 Uiso 1 1 calc R . . H14B H 0.2668 1.0621 1.0151 0.027 Uiso 1 1 calc R . . H14C H 0.3706 1.1299 0.9768 0.027 Uiso 1 1 calc R . . C15 C 0.00006(18) 0.96030(13) 0.60449(11) 0.0296(3) Uani 1 1 d . . . H15A H -0.1038 0.9263 0.5832 0.044 Uiso 1 1 calc R . . H15B H 0.0339 0.9196 0.5558 0.044 Uiso 1 1 calc R . . H15C H 0.0196 1.0371 0.6085 0.044 Uiso 1 1 calc R . . C16 C 0.20703(12) 0.61103(9) 0.89252(8) 0.01462(17) Uani 1 1 d . . . C17 C 0.31185(12) 0.61059(10) 0.97662(9) 0.01554(18) Uani 1 1 d . . . F1 F 0.40361(8) 0.70599(6) 1.05176(6) 0.02015(14) Uani 1 1 d . . . C18 C 0.33116(13) 0.51539(10) 0.99129(9) 0.01715(19) Uani 1 1 d . . . F2 F 0.43378(9) 0.52126(7) 1.07530(6) 0.02240(15) Uani 1 1 d . . . C19 C 0.24602(14) 0.41358(10) 0.91912(10) 0.0198(2) Uani 1 1 d . . . F3 F 0.26368(11) 0.32075(7) 0.93324(7) 0.02813(18) Uani 1 1 d . . . C20 C 0.14334(14) 0.41053(10) 0.83288(10) 0.0195(2) Uani 1 1 d . . . F4 F 0.05876(10) 0.31070(7) 0.76193(7) 0.02713(17) Uani 1 1 d . . . C21 C 0.12517(13) 0.50581(10) 0.81914(9) 0.01717(19) Uani 1 1 d . . . H21 H 0.0551 0.5003 0.7581 0.021 Uiso 1 1 calc R . . C22 C 0.39918(14) 0.94819(11) 1.14340(9) 0.0195(2) Uani 1 1 d . . . H22 H 0.4364 0.8995 1.1064 0.023 Uiso 1 1 calc R . . C23 C 0.49327(15) 1.04084(12) 1.22638(10) 0.0242(2) Uani 1 1 d . . . H23 H 0.5944 1.0553 1.2457 0.029 Uiso 1 1 calc R . . C24 C 0.43955(17) 1.11216(12) 1.28100(11) 0.0273(3) Uani 1 1 d . . . H24 H 0.5038 1.1761 1.3369 0.033 Uiso 1 1 calc R . . C25 C 0.29218(17) 1.08984(12) 1.25374(11) 0.0281(3) Uani 1 1 d . . . H25 H 0.2555 1.1382 1.2916 0.034 Uiso 1 1 calc R . . C26 C 0.19758(15) 0.99699(11) 1.17119(10) 0.0223(2) Uani 1 1 d . . . H26 H 0.0966 0.9817 1.1536 0.027 Uiso 1 1 calc R . . C27 C 0.25004(13) 0.92622(10) 1.11408(8) 0.01620(18) Uani 1 1 d . . . C28 C 0.10362(14) 0.71060(10) 1.07393(9) 0.0185(2) Uani 1 1 d . . . H28A H 0.0645 0.7408 1.1235 0.028 Uiso 1 1 calc R . . H28B H 0.1973 0.7033 1.1081 0.028 Uiso 1 1 calc R . . H28C H 0.0372 0.6379 1.0265 0.028 Uiso 1 1 calc R . . C29 C -0.04384(14) 0.83417(11) 0.97480(10) 0.0206(2) Uani 1 1 d . . . H29A H -0.0735 0.8450 1.0319 0.031 Uiso 1 1 calc R . . H29B H -0.1179 0.7726 0.9164 0.031 Uiso 1 1 calc R . . H29C H -0.0314 0.9015 0.9593 0.031 Uiso 1 1 calc R . . C30 C 0.2963(2) 0.26294(18) 0.68258(16) 0.0443(4) Uani 1 1 d . . . H30A H 0.1936 0.2206 0.6499 0.067 Uiso 1 1 calc R . . H30B H 0.3125 0.3301 0.6670 0.067 Uiso 1 1 calc R . . H30C H 0.3270 0.2829 0.7553 0.067 Uiso 1 1 calc R . . C31 C 0.3820(2) 0.19389(15) 0.64500(14) 0.0360(3) Uani 1 1 d . . . H31A H 0.3682 0.1274 0.6630 0.043 Uiso 1 1 calc R . . H31B H 0.3461 0.1694 0.5710 0.043 Uiso 1 1 calc R . . C32 C 0.5400(2) 0.25781(17) 0.68922(13) 0.0393(4) Uani 1 1 d . . . H32A H 0.5739 0.2839 0.7632 0.047 Uiso 1 1 calc R . . H32B H 0.5524 0.3237 0.6703 0.047 Uiso 1 1 calc R . . C33 C 0.6360(2) 0.1918(2) 0.65577(15) 0.0439(4) Uani 1 1 d . . . H33A H 0.7381 0.2339 0.6994 0.053 Uiso 1 1 calc R . . H33B H 0.6139 0.1211 0.6664 0.053 Uiso 1 1 calc R . . C34 C 0.6190(2) 0.16756(17) 0.54930(14) 0.0378(4) Uani 1 1 d . . . H34A H 0.6379 0.2377 0.5374 0.045 Uiso 1 1 calc R . . H34B H 0.5183 0.1223 0.5050 0.045 Uiso 1 1 calc R . . C35 C 0.7192(2) 0.10737(19) 0.5225(2) 0.0505(5) Uani 1 1 d . . . H35A H 0.7085 0.0973 0.4533 0.076 Uiso 1 1 calc R . . H35B H 0.6955 0.0351 0.5287 0.076 Uiso 1 1 calc R . . H35C H 0.8188 0.1505 0.5680 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01349(4) 0.01220(4) 0.01070(4) 0.00449(3) 0.00420(3) 0.00425(3) P1 0.01418(11) 0.01391(12) 0.01157(11) 0.00467(9) 0.00475(9) 0.00479(9) N1 0.0153(4) 0.0177(4) 0.0131(4) 0.0069(3) 0.0037(3) 0.0035(3) N2 0.0158(4) 0.0164(4) 0.0128(4) 0.0053(3) 0.0027(3) 0.0039(3) N3 0.0173(4) 0.0147(4) 0.0145(4) 0.0061(3) 0.0068(3) 0.0051(3) N4 0.0195(4) 0.0163(4) 0.0117(4) 0.0049(3) 0.0060(3) 0.0034(3) N5 0.0160(4) 0.0139(4) 0.0125(4) 0.0051(3) 0.0041(3) 0.0047(3) N6 0.0193(4) 0.0160(4) 0.0137(4) 0.0072(3) 0.0043(3) 0.0053(3) B1 0.0197(5) 0.0163(5) 0.0136(5) 0.0065(4) 0.0044(4) 0.0038(4) C1 0.0158(4) 0.0176(5) 0.0151(4) 0.0051(4) 0.0056(4) 0.0022(4) C2 0.0151(5) 0.0201(5) 0.0164(5) 0.0033(4) 0.0036(4) 0.0022(4) C3 0.0166(5) 0.0173(5) 0.0141(4) 0.0026(4) 0.0020(4) 0.0046(4) C4 0.0209(5) 0.0160(5) 0.0188(5) 0.0058(4) 0.0107(4) 0.0059(4) C5 0.0255(6) 0.0192(5) 0.0195(5) 0.0033(4) 0.0138(5) 0.0046(4) C6 0.0236(5) 0.0166(5) 0.0139(4) 0.0026(4) 0.0086(4) 0.0002(4) C7 0.0165(4) 0.0142(4) 0.0157(4) 0.0062(4) 0.0073(4) 0.0055(3) C8 0.0229(5) 0.0152(5) 0.0200(5) 0.0082(4) 0.0077(4) 0.0060(4) C9 0.0225(5) 0.0175(5) 0.0179(5) 0.0099(4) 0.0062(4) 0.0068(4) C10 0.0205(5) 0.0246(6) 0.0193(5) 0.0096(5) 0.0067(4) 0.0010(4) C11 0.0217(5) 0.0230(6) 0.0170(5) 0.0049(4) -0.0008(4) 0.0055(4) C12 0.0230(6) 0.0281(6) 0.0243(6) 0.0098(5) 0.0116(5) 0.0131(5) C13 0.0294(6) 0.0297(7) 0.0142(5) 0.0049(5) 0.0084(5) 0.0017(5) C14 0.0191(5) 0.0156(5) 0.0170(5) 0.0046(4) 0.0059(4) 0.0032(4) C15 0.0387(8) 0.0252(7) 0.0218(6) 0.0148(5) 0.0030(5) 0.0087(6) C16 0.0167(4) 0.0138(4) 0.0141(4) 0.0056(4) 0.0060(4) 0.0054(3) C17 0.0164(4) 0.0156(5) 0.0150(4) 0.0056(4) 0.0059(4) 0.0060(4) F1 0.0197(3) 0.0178(3) 0.0170(3) 0.0049(3) 0.0013(3) 0.0049(3) C18 0.0186(5) 0.0205(5) 0.0184(5) 0.0113(4) 0.0088(4) 0.0101(4) F2 0.0224(4) 0.0291(4) 0.0227(4) 0.0158(3) 0.0082(3) 0.0143(3) C19 0.0259(6) 0.0162(5) 0.0249(6) 0.0111(4) 0.0138(5) 0.0107(4) F3 0.0393(5) 0.0191(4) 0.0353(5) 0.0160(4) 0.0169(4) 0.0157(3) C20 0.0247(5) 0.0135(5) 0.0197(5) 0.0043(4) 0.0100(4) 0.0052(4) F4 0.0344(4) 0.0134(3) 0.0268(4) 0.0025(3) 0.0098(4) 0.0037(3) C21 0.0194(5) 0.0156(5) 0.0158(4) 0.0054(4) 0.0064(4) 0.0052(4) C22 0.0198(5) 0.0187(5) 0.0164(5) 0.0043(4) 0.0055(4) 0.0040(4) C23 0.0222(6) 0.0236(6) 0.0192(5) 0.0049(5) 0.0047(4) 0.0003(5) C24 0.0325(7) 0.0201(6) 0.0185(5) 0.0007(5) 0.0076(5) -0.0018(5) C25 0.0344(7) 0.0215(6) 0.0217(6) -0.0015(5) 0.0127(5) 0.0049(5) C26 0.0241(6) 0.0210(6) 0.0195(5) 0.0028(4) 0.0104(4) 0.0059(4) C27 0.0196(5) 0.0151(5) 0.0132(4) 0.0046(4) 0.0068(4) 0.0042(4) C28 0.0209(5) 0.0195(5) 0.0153(5) 0.0078(4) 0.0073(4) 0.0045(4) C29 0.0179(5) 0.0245(6) 0.0193(5) 0.0067(5) 0.0059(4) 0.0104(4) C30 0.0521(11) 0.0461(11) 0.0403(10) 0.0155(9) 0.0236(9) 0.0178(9) C31 0.0379(8) 0.0325(8) 0.0344(8) 0.0105(7) 0.0138(7) 0.0070(7) C32 0.0386(9) 0.0429(10) 0.0265(7) 0.0071(7) 0.0085(6) 0.0064(7) C33 0.0362(9) 0.0648(13) 0.0359(9) 0.0265(9) 0.0114(7) 0.0186(9) C34 0.0336(8) 0.0428(10) 0.0325(8) 0.0129(7) 0.0105(7) 0.0076(7) C35 0.0446(11) 0.0421(11) 0.0624(14) 0.0127(10) 0.0245(10) 0.0112(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 C16 2.0228(11) . ? Rh1 N3 2.1078(10) . ? Rh1 N5 2.1592(10) . ? Rh1 P1 2.2649(4) . ? Rh1 N1 2.2744(10) . ? Rh1 H1 1.486(19) . ? P1 C29 1.8199(13) . ? P1 C28 1.8267(12) . ? P1 C27 1.8311(12) . ? N1 C1 1.3444(15) . ? N1 N2 1.3689(14) . ? N2 C3 1.3504(15) . ? N2 B1 1.5368(17) . ? N3 C4 1.3353(16) . ? N3 N4 1.3702(14) . ? N4 C6 1.3538(16) . ? N4 B1 1.5411(18) . ? N5 C7 1.3428(15) . ? N5 N6 1.3786(14) . ? N6 C9 1.3500(15) . ? N6 B1 1.5382(17) . ? B1 H1B 1.0000 . ? C1 C2 1.4031(17) . ? C1 C10 1.4908(17) . ? C2 C3 1.3801(18) . ? C2 H2 0.9500 . ? C3 C11 1.4942(17) . ? C4 C5 1.4010(18) . ? C4 C12 1.4913(19) . ? C5 C6 1.381(2) . ? C5 H5 0.9500 . ? C6 C13 1.4963(18) . ? C7 C8 1.3978(16) . ? C7 C14 1.4899(17) . ? C8 C9 1.3793(18) . ? C8 H8 0.9500 . ? C9 C15 1.4919(18) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.3896(16) . ? C16 C21 1.4074(16) . ? C17 F1 1.3577(14) . ? C17 C18 1.3842(17) . ? C18 F2 1.3452(14) . ? C18 C19 1.3783(18) . ? C19 F3 1.3454(14) . ? C19 C20 1.3826(19) . ? C20 F4 1.3546(15) . ? C20 C21 1.3768(17) . ? C21 H21 0.9500 . ? C22 C23 1.3915(18) . ? C22 C27 1.3997(17) . ? C22 H22 0.9500 . ? C23 C24 1.389(2) . ? C23 H23 0.9500 . ? C24 C25 1.385(2) . ? C24 H24 0.9500 . ? C25 C26 1.391(2) . ? C25 H25 0.9500 . ? C26 C27 1.3958(18) . ? C26 H26 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.508(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.506(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.549(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.490(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.505(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N3 88.84(4) . . ? C16 Rh1 N5 171.73(4) . . ? N3 Rh1 N5 83.18(4) . . ? C16 Rh1 P1 91.32(3) . . ? N3 Rh1 P1 178.89(3) . . ? N5 Rh1 P1 96.61(3) . . ? C16 Rh1 N1 92.74(4) . . ? N3 Rh1 N1 85.96(4) . . ? N5 Rh1 N1 88.89(4) . . ? P1 Rh1 N1 95.13(3) . . ? C16 Rh1 H1 88.1(7) . . ? N3 Rh1 H1 89.4(7) . . ? N5 Rh1 H1 89.6(7) . . ? P1 Rh1 H1 89.5(7) . . ? N1 Rh1 H1 175.3(7) . . ? C29 P1 C28 103.33(6) . . ? C29 P1 C27 103.41(6) . . ? C28 P1 C27 97.71(6) . . ? C29 P1 Rh1 109.35(4) . . ? C28 P1 Rh1 119.79(4) . . ? C27 P1 Rh1 120.82(4) . . ? C1 N1 N2 106.00(9) . . ? C1 N1 Rh1 138.72(8) . . ? N2 N1 Rh1 114.90(7) . . ? C3 N2 N1 110.83(10) . . ? C3 N2 B1 129.09(10) . . ? N1 N2 B1 119.85(9) . . ? C4 N3 N4 107.88(10) . . ? C4 N3 Rh1 133.97(8) . . ? N4 N3 Rh1 117.75(7) . . ? C6 N4 N3 109.34(10) . . ? C6 N4 B1 130.04(10) . . ? N3 N4 B1 120.30(9) . . ? C7 N5 N6 106.22(9) . . ? C7 N5 Rh1 136.67(8) . . ? N6 N5 Rh1 116.48(7) . . ? C9 N6 N5 110.06(10) . . ? C9 N6 B1 128.19(10) . . ? N5 N6 B1 121.03(9) . . ? N2 B1 N6 109.61(10) . . ? N2 B1 N4 109.62(10) . . ? N6 B1 N4 109.19(10) . . ? N2 B1 H1B 109.5 . . ? N6 B1 H1B 109.5 . . ? N4 B1 H1B 109.5 . . ? N1 C1 C2 109.96(10) . . ? N1 C1 C10 123.94(11) . . ? C2 C1 C10 126.09(11) . . ? C3 C2 C1 105.80(11) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N2 C3 C2 107.41(10) . . ? N2 C3 C11 123.33(11) . . ? C2 C3 C11 129.24(12) . . ? N3 C4 C5 108.77(11) . . ? N3 C4 C12 122.74(11) . . ? C5 C4 C12 128.47(12) . . ? C6 C5 C4 106.43(11) . . ? C6 C5 H5 126.8 . . ? C4 C5 H5 126.8 . . ? N4 C6 C5 107.58(11) . . ? N4 C6 C13 123.59(13) . . ? C5 C6 C13 128.80(12) . . ? N5 C7 C8 109.94(10) . . ? N5 C7 C14 124.00(10) . . ? C8 C7 C14 126.00(11) . . ? C9 C8 C7 105.95(11) . . ? C9 C8 H8 127.0 . . ? C7 C8 H8 127.0 . . ? N6 C9 C8 107.79(10) . . ? N6 C9 C15 123.33(12) . . ? C8 C9 C15 128.88(12) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 114.56(10) . . ? C17 C16 Rh1 125.99(9) . . ? C21 C16 Rh1 119.37(8) . . ? F1 C17 C18 114.88(10) . . ? F1 C17 C16 121.38(10) . . ? C18 C17 C16 123.74(11) . . ? F2 C18 C19 119.45(11) . . ? F2 C18 C17 120.48(11) . . ? C19 C18 C17 120.06(11) . . ? F3 C19 C18 120.33(12) . . ? F3 C19 C20 121.71(12) . . ? C18 C19 C20 117.97(11) . . ? F4 C20 C21 120.32(12) . . ? F4 C20 C19 118.24(11) . . ? C21 C20 C19 121.43(12) . . ? C20 C21 C16 122.14(11) . . ? C20 C21 H21 118.9 . . ? C16 C21 H21 118.9 . . ? C23 C22 C27 120.44(12) . . ? C23 C22 H22 119.8 . . ? C27 C22 H22 119.8 . . ? C24 C23 C22 120.07(13) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 119.87(13) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.31(13) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 120.41(13) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 118.86(11) . . ? C26 C27 P1 120.47(10) . . ? C22 C27 P1 120.61(9) . . ? P1 C28 H28A 109.5 . . ? P1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P1 C29 H29A 109.5 . . ? P1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C30 111.32(16) . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C33 114.51(17) . . ? C31 C32 H32A 108.6 . . ? C33 C32 H32A 108.6 . . ? C31 C32 H32B 108.6 . . ? C33 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? C34 C33 C32 114.84(16) . . ? C34 C33 H33A 108.6 . . ? C32 C33 H33A 108.6 . . ? C34 C33 H33B 108.6 . . ? C32 C33 H33B 108.6 . . ? H33A C33 H33B 107.5 . . ? C33 C34 C35 112.34(18) . . ? C33 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? C33 C34 H34B 109.1 . . ? C35 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 P1 C29 -129.09(6) . . . . ? N3 Rh1 P1 C29 132.8(15) . . . . ? N5 Rh1 P1 C29 53.26(6) . . . . ? N1 Rh1 P1 C29 -36.21(6) . . . . ? C16 Rh1 P1 C28 -10.23(6) . . . . ? N3 Rh1 P1 C28 -108.3(15) . . . . ? N5 Rh1 P1 C28 172.12(6) . . . . ? N1 Rh1 P1 C28 82.64(6) . . . . ? C16 Rh1 P1 C27 111.19(6) . . . . ? N3 Rh1 P1 C27 13.1(15) . . . . ? N5 Rh1 P1 C27 -66.45(5) . . . . ? N1 Rh1 P1 C27 -155.93(5) . . . . ? C16 Rh1 N1 C1 50.40(13) . . . . ? N3 Rh1 N1 C1 139.04(13) . . . . ? N5 Rh1 N1 C1 -137.72(13) . . . . ? P1 Rh1 N1 C1 -41.17(13) . . . . ? C16 Rh1 N1 N2 -138.01(8) . . . . ? N3 Rh1 N1 N2 -49.36(8) . . . . ? N5 Rh1 N1 N2 33.88(8) . . . . ? P1 Rh1 N1 N2 130.42(8) . . . . ? C1 N1 N2 C3 0.97(13) . . . . ? Rh1 N1 N2 C3 -173.28(8) . . . . ? C1 N1 N2 B1 -173.95(11) . . . . ? Rh1 N1 N2 B1 11.81(13) . . . . ? C16 Rh1 N3 C4 -43.09(12) . . . . ? N5 Rh1 N3 C4 134.71(12) . . . . ? P1 Rh1 N3 C4 55.0(15) . . . . ? N1 Rh1 N3 C4 -135.93(12) . . . . ? C16 Rh1 N3 N4 128.60(8) . . . . ? N5 Rh1 N3 N4 -53.60(8) . . . . ? P1 Rh1 N3 N4 -133.3(14) . . . . ? N1 Rh1 N3 N4 35.77(8) . . . . ? C4 N3 N4 C6 0.90(13) . . . . ? Rh1 N3 N4 C6 -172.83(8) . . . . ? C4 N3 N4 B1 -173.20(10) . . . . ? Rh1 N3 N4 B1 13.08(13) . . . . ? C16 Rh1 N5 C7 -106.0(3) . . . . ? N3 Rh1 N5 C7 -121.46(12) . . . . ? P1 Rh1 N5 C7 57.43(12) . . . . ? N1 Rh1 N5 C7 152.47(12) . . . . ? C16 Rh1 N5 N6 63.4(3) . . . . ? N3 Rh1 N5 N6 47.92(8) . . . . ? P1 Rh1 N5 N6 -133.18(8) . . . . ? N1 Rh1 N5 N6 -38.15(8) . . . . ? C7 N5 N6 C9 -1.33(13) . . . . ? Rh1 N5 N6 C9 -173.76(8) . . . . ? C7 N5 N6 B1 169.75(10) . . . . ? Rh1 N5 N6 B1 -2.68(14) . . . . ? C3 N2 B1 N6 117.48(13) . . . . ? N1 N2 B1 N6 -68.65(14) . . . . ? C3 N2 B1 N4 -122.70(13) . . . . ? N1 N2 B1 N4 51.17(14) . . . . ? C9 N6 B1 N2 -126.53(13) . . . . ? N5 N6 B1 N2 64.15(14) . . . . ? C9 N6 B1 N4 113.39(13) . . . . ? N5 N6 B1 N4 -55.93(14) . . . . ? C6 N4 B1 N2 117.49(13) . . . . ? N3 N4 B1 N2 -69.79(13) . . . . ? C6 N4 B1 N6 -122.43(13) . . . . ? N3 N4 B1 N6 50.30(13) . . . . ? N2 N1 C1 C2 -0.65(14) . . . . ? Rh1 N1 C1 C2 171.43(10) . . . . ? N2 N1 C1 C10 179.69(12) . . . . ? Rh1 N1 C1 C10 -8.2(2) . . . . ? N1 C1 C2 C3 0.12(15) . . . . ? C10 C1 C2 C3 179.77(13) . . . . ? N1 N2 C3 C2 -0.91(14) . . . . ? B1 N2 C3 C2 173.41(12) . . . . ? N1 N2 C3 C11 177.65(12) . . . . ? B1 N2 C3 C11 -8.0(2) . . . . ? C1 C2 C3 N2 0.47(14) . . . . ? C1 C2 C3 C11 -177.96(13) . . . . ? N4 N3 C4 C5 -0.84(13) . . . . ? Rh1 N3 C4 C5 171.44(9) . . . . ? N4 N3 C4 C12 177.79(11) . . . . ? Rh1 N3 C4 C12 -9.93(19) . . . . ? N3 C4 C5 C6 0.47(14) . . . . ? C12 C4 C5 C6 -178.06(13) . . . . ? N3 N4 C6 C5 -0.60(13) . . . . ? B1 N4 C6 C5 172.74(12) . . . . ? N3 N4 C6 C13 177.31(11) . . . . ? B1 N4 C6 C13 -9.3(2) . . . . ? C4 C5 C6 N4 0.09(14) . . . . ? C4 C5 C6 C13 -177.68(13) . . . . ? N6 N5 C7 C8 1.65(13) . . . . ? Rh1 N5 C7 C8 171.76(9) . . . . ? N6 N5 C7 C14 -175.70(11) . . . . ? Rh1 N5 C7 C14 -5.59(18) . . . . ? N5 C7 C8 C9 -1.37(14) . . . . ? C14 C7 C8 C9 175.91(12) . . . . ? N5 N6 C9 C8 0.49(14) . . . . ? B1 N6 C9 C8 -169.78(12) . . . . ? N5 N6 C9 C15 -179.95(13) . . . . ? B1 N6 C9 C15 9.8(2) . . . . ? C7 C8 C9 N6 0.51(14) . . . . ? C7 C8 C9 C15 -179.01(14) . . . . ? N3 Rh1 C16 C17 118.50(10) . . . . ? N5 Rh1 C16 C17 103.1(3) . . . . ? P1 Rh1 C16 C17 -60.40(10) . . . . ? N1 Rh1 C16 C17 -155.60(10) . . . . ? N3 Rh1 C16 C21 -57.96(9) . . . . ? N5 Rh1 C16 C21 -73.3(3) . . . . ? P1 Rh1 C16 C21 123.14(9) . . . . ? N1 Rh1 C16 C21 27.94(9) . . . . ? C21 C16 C17 F1 177.01(10) . . . . ? Rh1 C16 C17 F1 0.40(16) . . . . ? C21 C16 C17 C18 -3.37(17) . . . . ? Rh1 C16 C17 C18 -179.98(9) . . . . ? F1 C17 C18 F2 0.53(16) . . . . ? C16 C17 C18 F2 -179.11(11) . . . . ? F1 C17 C18 C19 -178.77(11) . . . . ? C16 C17 C18 C19 1.59(18) . . . . ? F2 C18 C19 F3 1.12(18) . . . . ? C17 C18 C19 F3 -179.57(11) . . . . ? F2 C18 C19 C20 -178.84(11) . . . . ? C17 C18 C19 C20 0.47(18) . . . . ? F3 C19 C20 F4 0.43(19) . . . . ? C18 C19 C20 F4 -179.61(11) . . . . ? F3 C19 C20 C21 179.58(11) . . . . ? C18 C19 C20 C21 -0.47(19) . . . . ? F4 C20 C21 C16 177.58(11) . . . . ? C19 C20 C21 C16 -1.55(19) . . . . ? C17 C16 C21 C20 3.32(17) . . . . ? Rh1 C16 C21 C20 -179.83(9) . . . . ? C27 C22 C23 C24 0.2(2) . . . . ? C22 C23 C24 C25 1.1(2) . . . . ? C23 C24 C25 C26 -0.8(2) . . . . ? C24 C25 C26 C27 -0.9(2) . . . . ? C25 C26 C27 C22 2.2(2) . . . . ? C25 C26 C27 P1 179.41(11) . . . . ? C23 C22 C27 C26 -1.86(19) . . . . ? C23 C22 C27 P1 -179.03(10) . . . . ? C29 P1 C27 C26 20.53(12) . . . . ? C28 P1 C27 C26 -85.22(11) . . . . ? Rh1 P1 C27 C26 143.14(9) . . . . ? C29 P1 C27 C22 -162.34(10) . . . . ? C28 P1 C27 C22 91.91(11) . . . . ? Rh1 P1 C27 C22 -39.73(11) . . . . ? C30 C31 C32 C33 178.92(16) . . . . ? C31 C32 C33 C34 70.8(2) . . . . ? C32 C33 C34 C35 177.69(17) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 37.41 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.183 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.092 #===end data_jontt14_cmpd9c _database_code_depnum_ccdc_archive 'CCDC 770119' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt14 _chemical_melting_point ? _chemical_formula_moiety 'C29 H35 B F4 N6 P Rh' _chemical_formula_sum 'C29 H35 B F4 N6 P Rh' _chemical_formula_weight 688.32 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9400(8) _cell_length_b 18.7449(13) _cell_length_c 14.5298(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.712(1) _cell_angle_gamma 90.00 _cell_volume 3061.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 3862 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 33.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8462 _exptl_absorpt_correction_T_max 0.8898 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; The crystals encounter a phase change at 150 K. Below this temperature they irreversibly shatter and lose their single crystallinity. ; _diffrn_ambient_temperature 173(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74523 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 37.78 _reflns_number_total 16316 _reflns_number_gt 9949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The hydride ligand atom was found from the difference Fourier map, and its position and isotropic displacement parameter were refined independently from all other atoms. ; _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^)+(0.0574P)^2^+0.3760P] 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 16316 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.344700(11) 0.364525(7) 0.614981(9) 0.03488(4) Uani 1 1 d . . . H1 H 0.3311(15) 0.4453(10) 0.6191(13) 0.034(5) Uiso 1 1 d . . . P1 P 0.45511(5) 0.37078(2) 0.77568(4) 0.04326(11) Uani 1 1 d . . . N1 N 0.36552(13) 0.24556(8) 0.60069(11) 0.0394(3) Uani 1 1 d . . . N2 N 0.39215(14) 0.22517(9) 0.52002(11) 0.0449(3) Uani 1 1 d . . . N3 N 0.24887(13) 0.36425(7) 0.46403(10) 0.0354(3) Uani 1 1 d . . . N4 N 0.29440(13) 0.32566(8) 0.40471(10) 0.0395(3) Uani 1 1 d . . . N5 N 0.49571(14) 0.38019(10) 0.56755(12) 0.0454(3) Uani 1 1 d . . . N6 N 0.51063(14) 0.33118(10) 0.50234(12) 0.0489(4) Uani 1 1 d . . . B1 B 0.40866(19) 0.28057(13) 0.44886(15) 0.0462(5) Uani 1 1 d . . . H1B H 0.4278 0.2559 0.3950 0.055 Uiso 1 1 calc R . . C1 C 0.35248(16) 0.18516(10) 0.64546(13) 0.0416(4) Uani 1 1 d . . . C2 C 0.3723(2) 0.12643(10) 0.59383(15) 0.0490(4) Uani 1 1 d . . . H2 H 0.3695 0.0775 0.6101 0.059 Uiso 1 1 calc R . . C3 C 0.3965(2) 0.15313(12) 0.51573(15) 0.0522(5) Uani 1 1 d . . . C4 C 0.15531(14) 0.40046(9) 0.40621(13) 0.0389(3) Uani 1 1 d . . . C5 C 0.14061(17) 0.38577(11) 0.30954(14) 0.0440(4) Uani 1 1 d . . . H5 H 0.0808 0.4044 0.2535 0.053 Uiso 1 1 calc R . . C6 C 0.22963(16) 0.33877(10) 0.31030(13) 0.0417(4) Uani 1 1 d . . . C7 C 0.58467(17) 0.42775(13) 0.58387(16) 0.0553(5) Uani 1 1 d . . . C8 C 0.65735(19) 0.40675(17) 0.53025(19) 0.0697(7) Uani 1 1 d . . . H8 H 0.7278 0.4299 0.5296 0.084 Uiso 1 1 calc R . . C9 C 0.60837(18) 0.34750(16) 0.47981(17) 0.0612(6) Uani 1 1 d . . . C10 C 0.08292(17) 0.44872(11) 0.44592(15) 0.0492(4) Uani 1 1 d . . . H10A H 0.1343 0.4705 0.5068 0.074 Uiso 1 1 calc R . . H10B H 0.0202 0.4211 0.4589 0.074 Uiso 1 1 calc R . . H10C H 0.0468 0.4862 0.3981 0.074 Uiso 1 1 calc R . . C11 C 0.2563(2) 0.30688(14) 0.22578(15) 0.0578(5) Uani 1 1 d . . . H11A H 0.1917 0.3183 0.1650 0.087 Uiso 1 1 calc R . . H11B H 0.2633 0.2550 0.2338 0.087 Uiso 1 1 calc R . . H11C H 0.3312 0.3265 0.2231 0.087 Uiso 1 1 calc R . . C12 C 0.3188(2) 0.18218(11) 0.73469(16) 0.0518(5) Uani 1 1 d . . . H12A H 0.2677 0.2229 0.7354 0.078 Uiso 1 1 calc R . . H12B H 0.3908 0.1839 0.7927 0.078 Uiso 1 1 calc R . . H12C H 0.2758 0.1377 0.7350 0.078 Uiso 1 1 calc R . . C13 C 0.4275(3) 0.11398(15) 0.43703(19) 0.0790(8) Uani 1 1 d . . . H13A H 0.5042 0.1311 0.4352 0.118 Uiso 1 1 calc R . . H13B H 0.3657 0.1227 0.3736 0.118 Uiso 1 1 calc R . . H13C H 0.4326 0.0627 0.4511 0.118 Uiso 1 1 calc R . . C14 C 0.5964(2) 0.49273(15) 0.64374(18) 0.0696(7) Uani 1 1 d . . . H14A H 0.5172 0.5095 0.6400 0.104 Uiso 1 1 calc R . . H14B H 0.6365 0.5300 0.6191 0.104 Uiso 1 1 calc R . . H14C H 0.6432 0.4819 0.7119 0.104 Uiso 1 1 calc R . . C15 C 0.6491(2) 0.3034(2) 0.4102(2) 0.0863(10) Uani 1 1 d . . . H15A H 0.7255 0.3216 0.4090 0.129 Uiso 1 1 calc R . . H15B H 0.5898 0.3063 0.3445 0.129 Uiso 1 1 calc R . . H15C H 0.6583 0.2536 0.4320 0.129 Uiso 1 1 calc R . . C16 C 0.18994(16) 0.35668(8) 0.64456(13) 0.0363(3) Uani 1 1 d . . . C17 C 0.15412(18) 0.40369(9) 0.70396(13) 0.0419(4) Uani 1 1 d . . . F1 F 0.22615(12) 0.45810(6) 0.74975(10) 0.0585(3) Uani 1 1 d . . . C18 C 0.04679(19) 0.40069(9) 0.71921(14) 0.0444(4) Uani 1 1 d . . . F2 F 0.02322(13) 0.45019(6) 0.77834(10) 0.0634(4) Uani 1 1 d . . . C19 C -0.03662(19) 0.35044(10) 0.67533(16) 0.0473(4) Uani 1 1 d . . . H19 H -0.1110 0.3481 0.6856 0.057 Uiso 1 1 calc R . . C20 C -0.00596(16) 0.30332(9) 0.61516(15) 0.0432(4) Uani 1 1 d . . . F3 F -0.08527(11) 0.25275(7) 0.56791(10) 0.0601(3) Uani 1 1 d . . . C21 C 0.10225(15) 0.30666(9) 0.60077(13) 0.0381(3) Uani 1 1 d . . . F4 F 0.11811(10) 0.25737(6) 0.53781(9) 0.0492(3) Uani 1 1 d . . . C22 C 0.4608(2) 0.52104(11) 0.79903(18) 0.0566(5) Uani 1 1 d . . . H22 H 0.3895 0.5224 0.7442 0.068 Uiso 1 1 calc R . . C23 C 0.5102(2) 0.58397(11) 0.84534(19) 0.0625(6) Uani 1 1 d . . . H23 H 0.4718 0.6281 0.8225 0.075 Uiso 1 1 calc R . . C24 C 0.6129(3) 0.58303(12) 0.92285(18) 0.0720(7) Uani 1 1 d . . . H24 H 0.6483 0.6265 0.9521 0.086 Uiso 1 1 calc R . . C25 C 0.6650(3) 0.51945(14) 0.9587(2) 0.0956(12) Uani 1 1 d . . . H25 H 0.7359 0.5186 1.0139 0.115 Uiso 1 1 calc R . . C26 C 0.6145(3) 0.45607(13) 0.91453(18) 0.0827(9) Uani 1 1 d . . . H26 H 0.6495 0.4120 0.9417 0.099 Uiso 1 1 calc R . . C27 C 0.5152(2) 0.45585(10) 0.83262(14) 0.0515(5) Uani 1 1 d . . . C28 C 0.3928(3) 0.33867(14) 0.86685(17) 0.0723(7) Uani 1 1 d . . . H28A H 0.4573 0.3303 0.9288 0.109 Uiso 1 1 calc R . . H28B H 0.3497 0.2940 0.8441 0.109 Uiso 1 1 calc R . . H28C H 0.3381 0.3745 0.8766 0.109 Uiso 1 1 calc R . . C29 C 0.5861(2) 0.31557(12) 0.79766(17) 0.0594(6) Uani 1 1 d . . . H29A H 0.6301 0.3135 0.8680 0.089 Uiso 1 1 calc R . . H29B H 0.6370 0.3360 0.7638 0.089 Uiso 1 1 calc R . . H29C H 0.5620 0.2673 0.7730 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.03607(7) 0.03660(7) 0.03424(7) 0.00324(5) 0.01485(5) 0.00535(5) P1 0.0564(3) 0.0355(2) 0.0354(2) 0.00125(17) 0.01212(19) 0.00668(19) N1 0.0413(7) 0.0415(7) 0.0371(7) 0.0020(6) 0.0153(6) 0.0094(6) N2 0.0510(9) 0.0480(8) 0.0388(7) 0.0026(6) 0.0192(6) 0.0177(7) N3 0.0347(6) 0.0385(7) 0.0358(6) 0.0042(5) 0.0157(5) 0.0068(5) N4 0.0388(7) 0.0477(8) 0.0364(7) 0.0043(6) 0.0184(6) 0.0069(6) N5 0.0351(7) 0.0600(9) 0.0419(8) 0.0067(7) 0.0142(6) 0.0040(6) N6 0.0374(7) 0.0690(11) 0.0444(8) 0.0080(8) 0.0190(6) 0.0134(7) B1 0.0470(11) 0.0576(12) 0.0391(9) 0.0038(9) 0.0213(8) 0.0161(9) C1 0.0422(9) 0.0404(9) 0.0387(8) 0.0031(7) 0.0092(7) 0.0073(7) C2 0.0552(11) 0.0400(9) 0.0437(9) 0.0007(7) 0.0059(8) 0.0124(8) C3 0.0598(12) 0.0515(10) 0.0426(9) -0.0013(8) 0.0138(9) 0.0222(9) C4 0.0354(8) 0.0393(8) 0.0422(8) 0.0076(7) 0.0134(6) 0.0030(6) C5 0.0383(8) 0.0494(9) 0.0413(9) 0.0096(7) 0.0096(7) 0.0002(7) C6 0.0405(8) 0.0493(9) 0.0365(8) 0.0048(7) 0.0146(7) -0.0043(7) C7 0.0368(9) 0.0775(14) 0.0482(10) 0.0107(10) 0.0099(8) -0.0048(9) C8 0.0339(9) 0.116(2) 0.0620(13) 0.0187(14) 0.0195(9) -0.0011(12) C9 0.0350(9) 0.1010(18) 0.0513(11) 0.0143(12) 0.0195(8) 0.0134(10) C10 0.0450(10) 0.0472(10) 0.0562(11) 0.0094(8) 0.0180(8) 0.0138(8) C11 0.0616(12) 0.0771(15) 0.0405(10) 0.0010(10) 0.0248(9) -0.0001(11) C12 0.0636(12) 0.0447(10) 0.0511(11) 0.0079(8) 0.0246(9) 0.0022(9) C13 0.115(2) 0.0675(15) 0.0591(14) -0.0050(12) 0.0350(15) 0.0402(16) C14 0.0568(13) 0.0879(18) 0.0608(13) 0.0009(13) 0.0154(11) -0.0251(12) C15 0.0518(13) 0.149(3) 0.0700(16) 0.0017(18) 0.0360(12) 0.0194(16) C16 0.0413(8) 0.0344(7) 0.0372(8) 0.0041(6) 0.0185(6) 0.0053(6) C17 0.0549(10) 0.0336(8) 0.0453(9) 0.0018(7) 0.0275(8) 0.0032(7) F1 0.0715(8) 0.0467(6) 0.0704(8) -0.0175(6) 0.0409(7) -0.0091(6) C18 0.0625(11) 0.0333(8) 0.0509(10) 0.0056(7) 0.0368(9) 0.0083(7) F2 0.0898(9) 0.0472(6) 0.0790(9) -0.0062(6) 0.0623(8) 0.0048(6) C19 0.0531(10) 0.0396(9) 0.0620(12) 0.0111(8) 0.0363(9) 0.0082(7) C20 0.0433(9) 0.0366(8) 0.0537(10) 0.0061(7) 0.0217(8) 0.0025(7) F3 0.0483(6) 0.0530(7) 0.0826(9) -0.0088(6) 0.0267(6) -0.0071(5) C21 0.0438(8) 0.0346(7) 0.0396(8) 0.0026(6) 0.0190(7) 0.0073(6) F4 0.0458(6) 0.0490(6) 0.0547(6) -0.0140(5) 0.0195(5) 0.0024(5) C22 0.0597(12) 0.0429(10) 0.0661(13) 0.0002(9) 0.0195(10) 0.0033(9) C23 0.0774(16) 0.0389(10) 0.0734(15) -0.0018(10) 0.0284(13) 0.0051(10) C24 0.114(2) 0.0438(11) 0.0514(12) -0.0109(9) 0.0193(13) 0.0011(12) C25 0.135(3) 0.0549(14) 0.0550(14) -0.0139(11) -0.0230(16) 0.0112(15) C26 0.115(2) 0.0481(12) 0.0518(12) -0.0082(10) -0.0157(13) 0.0168(13) C27 0.0720(13) 0.0389(9) 0.0395(9) -0.0017(7) 0.0132(9) 0.0056(9) C28 0.116(2) 0.0626(14) 0.0416(11) 0.0044(10) 0.0302(13) -0.0040(14) C29 0.0638(13) 0.0443(10) 0.0553(12) -0.0048(9) 0.0004(10) 0.0154(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 C16 2.0388(17) . ? Rh1 N3 2.1040(15) . ? Rh1 N5 2.1565(16) . ? Rh1 N1 2.2611(15) . ? Rh1 P1 2.2643(5) . ? Rh1 H1 1.53(2) . ? P1 C29 1.812(2) . ? P1 C28 1.826(3) . ? P1 C27 1.828(2) . ? N1 C1 1.341(2) . ? N1 N2 1.368(2) . ? N2 C3 1.354(3) . ? N2 B1 1.524(3) . ? N3 C4 1.335(2) . ? N3 N4 1.3704(19) . ? N4 C6 1.351(2) . ? N4 B1 1.548(2) . ? N5 C7 1.345(3) . ? N5 N6 1.374(2) . ? N6 C9 1.349(3) . ? N6 B1 1.532(3) . ? B1 H1B 1.0000 . ? C1 C2 1.397(3) . ? C1 C12 1.482(3) . ? C2 C3 1.357(3) . ? C2 H2 0.9500 . ? C3 C13 1.506(3) . ? C4 C5 1.383(3) . ? C4 C10 1.495(3) . ? C5 C6 1.378(3) . ? C5 H5 0.9500 . ? C6 C11 1.493(3) . ? C7 C8 1.404(3) . ? C7 C14 1.476(4) . ? C8 C9 1.350(4) . ? C8 H8 0.9500 . ? C9 C15 1.508(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.390(2) . ? C16 C17 1.398(2) . ? C17 F1 1.355(2) . ? C17 C18 1.373(3) . ? C18 F2 1.357(2) . ? C18 C19 1.363(3) . ? C19 C20 1.376(3) . ? C19 H19 0.9500 . ? C20 F3 1.352(2) . ? C20 C21 1.378(2) . ? C21 F4 1.3575(19) . ? C22 C23 1.387(3) . ? C22 C27 1.393(3) . ? C22 H22 0.9500 . ? C23 C24 1.356(4) . ? C23 H23 0.9500 . ? C24 C25 1.364(4) . ? C24 H24 0.9500 . ? C25 C26 1.388(4) . ? C25 H25 0.9500 . ? C26 C27 1.368(3) . ? C26 H26 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N3 90.38(6) . . ? C16 Rh1 N5 172.81(6) . . ? N3 Rh1 N5 83.49(6) . . ? C16 Rh1 N1 94.81(6) . . ? N3 Rh1 N1 86.55(5) . . ? N5 Rh1 N1 88.58(6) . . ? C16 Rh1 P1 92.30(5) . . ? N3 Rh1 P1 176.23(4) . . ? N5 Rh1 P1 93.66(5) . . ? N1 Rh1 P1 95.85(4) . . ? C16 Rh1 H1 87.0(7) . . ? N3 Rh1 H1 90.9(7) . . ? N5 Rh1 H1 89.4(7) . . ? N1 Rh1 H1 176.9(7) . . ? P1 Rh1 H1 86.6(7) . . ? C29 P1 C28 102.85(13) . . ? C29 P1 C27 103.60(11) . . ? C28 P1 C27 98.78(11) . . ? C29 P1 Rh1 108.66(8) . . ? C28 P1 Rh1 119.54(10) . . ? C27 P1 Rh1 120.99(7) . . ? C1 N1 N2 106.16(15) . . ? C1 N1 Rh1 138.93(12) . . ? N2 N1 Rh1 114.75(11) . . ? C3 N2 N1 109.97(16) . . ? C3 N2 B1 129.25(16) . . ? N1 N2 B1 120.75(15) . . ? C4 N3 N4 107.34(14) . . ? C4 N3 Rh1 134.46(12) . . ? N4 N3 Rh1 117.73(10) . . ? C6 N4 N3 109.27(14) . . ? C6 N4 B1 130.00(15) . . ? N3 N4 B1 120.58(14) . . ? C7 N5 N6 106.64(16) . . ? C7 N5 Rh1 136.85(15) . . ? N6 N5 Rh1 116.50(12) . . ? C9 N6 N5 109.86(19) . . ? C9 N6 B1 128.44(19) . . ? N5 N6 B1 119.87(14) . . ? N2 B1 N6 109.89(16) . . ? N2 B1 N4 110.82(15) . . ? N6 B1 N4 108.10(16) . . ? N2 B1 H1B 109.3 . . ? N6 B1 H1B 109.3 . . ? N4 B1 H1B 109.3 . . ? N1 C1 C2 109.66(18) . . ? N1 C1 C12 124.49(17) . . ? C2 C1 C12 125.83(18) . . ? C3 C2 C1 106.31(18) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? N2 C3 C2 107.89(17) . . ? N2 C3 C13 123.0(2) . . ? C2 C3 C13 129.1(2) . . ? N3 C4 C5 109.30(16) . . ? N3 C4 C10 122.34(16) . . ? C5 C4 C10 128.36(16) . . ? C6 C5 C4 106.61(16) . . ? C6 C5 H5 126.7 . . ? C4 C5 H5 126.7 . . ? N4 C6 C5 107.48(16) . . ? N4 C6 C11 123.68(18) . . ? C5 C6 C11 128.83(18) . . ? N5 C7 C8 108.4(2) . . ? N5 C7 C14 124.3(2) . . ? C8 C7 C14 127.2(2) . . ? C9 C8 C7 107.2(2) . . ? C9 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? N6 C9 C8 107.8(2) . . ? N6 C9 C15 122.6(3) . . ? C8 C9 C15 129.5(2) . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 111.60(15) . . ? C21 C16 Rh1 123.27(12) . . ? C17 C16 Rh1 124.93(13) . . ? F1 C17 C18 115.08(15) . . ? F1 C17 C16 120.13(16) . . ? C18 C17 C16 124.77(18) . . ? F2 C18 C19 119.60(17) . . ? F2 C18 C17 118.57(18) . . ? C19 C18 C17 121.83(16) . . ? C18 C19 C20 115.57(17) . . ? C18 C19 H19 122.2 . . ? C20 C19 H19 122.2 . . ? F3 C20 C19 118.79(16) . . ? F3 C20 C21 119.12(16) . . ? C19 C20 C21 122.08(18) . . ? F4 C21 C20 114.98(16) . . ? F4 C21 C16 120.87(15) . . ? C20 C21 C16 124.14(16) . . ? C23 C22 C27 120.3(2) . . ? C23 C22 H22 119.9 . . ? C27 C22 H22 119.9 . . ? C24 C23 C22 120.6(2) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.8(2) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.0(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 121.3(2) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C22 117.9(2) . . ? C26 C27 P1 119.27(16) . . ? C22 C27 P1 122.79(17) . . ? P1 C28 H28A 109.5 . . ? P1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P1 C29 H29A 109.5 . . ? P1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 P1 C29 137.57(10) . . . . ? N3 Rh1 P1 C29 -87.0(6) . . . . ? N5 Rh1 P1 C29 -46.45(10) . . . . ? N1 Rh1 P1 C29 42.49(10) . . . . ? C16 Rh1 P1 C28 20.10(12) . . . . ? N3 Rh1 P1 C28 155.5(6) . . . . ? N5 Rh1 P1 C28 -163.93(12) . . . . ? N1 Rh1 P1 C28 -74.98(11) . . . . ? C16 Rh1 P1 C27 -102.94(10) . . . . ? N3 Rh1 P1 C27 32.5(6) . . . . ? N5 Rh1 P1 C27 73.04(10) . . . . ? N1 Rh1 P1 C27 161.99(10) . . . . ? C16 Rh1 N1 C1 -41.78(19) . . . . ? N3 Rh1 N1 C1 -131.88(19) . . . . ? N5 Rh1 N1 C1 144.57(19) . . . . ? P1 Rh1 N1 C1 51.04(19) . . . . ? C16 Rh1 N1 N2 132.75(12) . . . . ? N3 Rh1 N1 N2 42.66(12) . . . . ? N5 Rh1 N1 N2 -40.90(12) . . . . ? P1 Rh1 N1 N2 -134.43(11) . . . . ? C1 N1 N2 C3 -0.5(2) . . . . ? Rh1 N1 N2 C3 -176.80(13) . . . . ? C1 N1 N2 B1 177.72(16) . . . . ? Rh1 N1 N2 B1 1.4(2) . . . . ? C16 Rh1 N3 C4 49.77(17) . . . . ? N5 Rh1 N3 C4 -126.47(17) . . . . ? N1 Rh1 N3 C4 144.56(17) . . . . ? P1 Rh1 N3 C4 -85.7(6) . . . . ? C16 Rh1 N3 N4 -139.35(12) . . . . ? N5 Rh1 N3 N4 44.41(12) . . . . ? N1 Rh1 N3 N4 -44.56(12) . . . . ? P1 Rh1 N3 N4 85.2(6) . . . . ? C4 N3 N4 C6 0.69(19) . . . . ? Rh1 N3 N4 C6 -172.50(11) . . . . ? C4 N3 N4 B1 176.62(16) . . . . ? Rh1 N3 N4 B1 3.4(2) . . . . ? C16 Rh1 N5 C7 93.2(6) . . . . ? N3 Rh1 N5 C7 124.8(2) . . . . ? N1 Rh1 N5 C7 -148.5(2) . . . . ? P1 Rh1 N5 C7 -52.8(2) . . . . ? C16 Rh1 N5 N6 -85.9(6) . . . . ? N3 Rh1 N5 N6 -54.33(13) . . . . ? N1 Rh1 N5 N6 32.36(13) . . . . ? P1 Rh1 N5 N6 128.13(12) . . . . ? C7 N5 N6 C9 0.9(2) . . . . ? Rh1 N5 N6 C9 -179.70(13) . . . . ? C7 N5 N6 B1 -164.92(17) . . . . ? Rh1 N5 N6 B1 14.4(2) . . . . ? C3 N2 B1 N6 -122.3(2) . . . . ? N1 N2 B1 N6 59.8(2) . . . . ? C3 N2 B1 N4 118.3(2) . . . . ? N1 N2 B1 N4 -59.6(2) . . . . ? C9 N6 B1 N2 125.5(2) . . . . ? N5 N6 B1 N2 -71.5(2) . . . . ? C9 N6 B1 N4 -113.4(2) . . . . ? N5 N6 B1 N4 49.5(2) . . . . ? C6 N4 B1 N2 -126.27(19) . . . . ? N3 N4 B1 N2 58.8(2) . . . . ? C6 N4 B1 N6 113.3(2) . . . . ? N3 N4 B1 N6 -61.7(2) . . . . ? N2 N1 C1 C2 0.7(2) . . . . ? Rh1 N1 C1 C2 175.58(14) . . . . ? N2 N1 C1 C12 -177.73(17) . . . . ? Rh1 N1 C1 C12 -2.9(3) . . . . ? N1 C1 C2 C3 -0.7(2) . . . . ? C12 C1 C2 C3 177.77(19) . . . . ? N1 N2 C3 C2 0.1(2) . . . . ? B1 N2 C3 C2 -177.94(19) . . . . ? N1 N2 C3 C13 -178.1(2) . . . . ? B1 N2 C3 C13 3.9(4) . . . . ? C1 C2 C3 N2 0.3(2) . . . . ? C1 C2 C3 C13 178.4(2) . . . . ? N4 N3 C4 C5 -0.4(2) . . . . ? Rh1 N3 C4 C5 171.17(12) . . . . ? N4 N3 C4 C10 180.00(16) . . . . ? Rh1 N3 C4 C10 -8.5(3) . . . . ? N3 C4 C5 C6 -0.1(2) . . . . ? C10 C4 C5 C6 179.53(18) . . . . ? N3 N4 C6 C5 -0.7(2) . . . . ? B1 N4 C6 C5 -176.15(19) . . . . ? N3 N4 C6 C11 178.48(18) . . . . ? B1 N4 C6 C11 3.1(3) . . . . ? C4 C5 C6 N4 0.5(2) . . . . ? C4 C5 C6 C11 -178.7(2) . . . . ? N6 N5 C7 C8 -1.7(2) . . . . ? Rh1 N5 C7 C8 179.17(16) . . . . ? N6 N5 C7 C14 174.9(2) . . . . ? Rh1 N5 C7 C14 -4.2(3) . . . . ? N5 C7 C8 C9 1.8(3) . . . . ? C14 C7 C8 C9 -174.7(2) . . . . ? N5 N6 C9 C8 0.2(2) . . . . ? B1 N6 C9 C8 164.5(2) . . . . ? N5 N6 C9 C15 179.7(2) . . . . ? B1 N6 C9 C15 -16.0(4) . . . . ? C7 C8 C9 N6 -1.2(3) . . . . ? C7 C8 C9 C15 179.4(2) . . . . ? N3 Rh1 C16 C21 49.45(14) . . . . ? N5 Rh1 C16 C21 80.8(6) . . . . ? N1 Rh1 C16 C21 -37.12(14) . . . . ? P1 Rh1 C16 C21 -133.19(14) . . . . ? N3 Rh1 C16 C17 -124.93(15) . . . . ? N5 Rh1 C16 C17 -93.6(6) . . . . ? N1 Rh1 C16 C17 148.50(15) . . . . ? P1 Rh1 C16 C17 52.43(15) . . . . ? C21 C16 C17 F1 -177.33(16) . . . . ? Rh1 C16 C17 F1 -2.4(2) . . . . ? C21 C16 C17 C18 1.1(3) . . . . ? Rh1 C16 C17 C18 176.03(14) . . . . ? F1 C17 C18 F2 -1.1(3) . . . . ? C16 C17 C18 F2 -179.53(17) . . . . ? F1 C17 C18 C19 177.72(18) . . . . ? C16 C17 C18 C19 -0.8(3) . . . . ? F2 C18 C19 C20 178.76(17) . . . . ? C17 C18 C19 C20 0.0(3) . . . . ? C18 C19 C20 F3 -178.91(17) . . . . ? C18 C19 C20 C21 0.3(3) . . . . ? F3 C20 C21 F4 0.5(2) . . . . ? C19 C20 C21 F4 -178.73(16) . . . . ? F3 C20 C21 C16 179.33(16) . . . . ? C19 C20 C21 C16 0.1(3) . . . . ? C17 C16 C21 F4 178.02(15) . . . . ? Rh1 C16 C21 F4 3.0(2) . . . . ? C17 C16 C21 C20 -0.8(2) . . . . ? Rh1 C16 C21 C20 -175.81(14) . . . . ? C27 C22 C23 C24 1.0(4) . . . . ? C22 C23 C24 C25 -3.2(4) . . . . ? C23 C24 C25 C26 1.4(5) . . . . ? C24 C25 C26 C27 2.7(6) . . . . ? C25 C26 C27 C22 -4.8(5) . . . . ? C25 C26 C27 P1 178.3(3) . . . . ? C23 C22 C27 C26 3.0(4) . . . . ? C23 C22 C27 P1 179.82(19) . . . . ? C29 P1 C27 C26 -33.1(3) . . . . ? C28 P1 C27 C26 72.5(3) . . . . ? Rh1 P1 C27 C26 -155.1(2) . . . . ? C29 P1 C27 C22 150.1(2) . . . . ? C28 P1 C27 C22 -104.3(2) . . . . ? Rh1 P1 C27 C22 28.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 37.78 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.953 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.083 #===end data_jontt13_cmpd9d _database_code_depnum_ccdc_archive 'CCDC 770120' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt13 _chemical_melting_point ? _chemical_formula_moiety 'C29 H36 B F3 N6 P Rh' _chemical_formula_sum 'C29 H36 B F3 N6 P Rh' _chemical_formula_weight 670.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.2916(14) _cell_length_b 11.5263(16) _cell_length_c 12.4406(17) _cell_angle_alpha 90.743(2) _cell_angle_beta 93.433(2) _cell_angle_gamma 92.065(2) _cell_volume 1472.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3974 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 37.98 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8530 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34212 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 36.32 _reflns_number_total 13969 _reflns_number_gt 11895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The hydride ligand was found from the difference Fourier map and its position and isotropic displacement parameter were refined independently from those of all other atoms. ; _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^)+(0.0394P)^2^+0.1081P] 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 13969 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.261894(10) 0.167331(8) 0.170181(8) 0.00998(3) Uani 1 1 d . . . H1 H 0.3664(18) 0.2381(17) 0.1252(15) 0.017(5) Uiso 1 1 d . . . P1 P 0.13029(3) 0.25573(3) 0.04605(3) 0.01216(6) Uani 1 1 d . . . N1 N 0.10798(11) 0.05272(10) 0.24190(9) 0.01310(19) Uani 1 1 d . . . N2 N 0.15065(11) -0.05368(10) 0.27359(9) 0.01305(19) Uani 1 1 d . . . N3 N 0.40235(11) 0.09308(9) 0.27578(9) 0.01178(18) Uani 1 1 d . . . N4 N 0.39364(11) -0.02320(10) 0.29463(9) 0.01216(19) Uani 1 1 d . . . N5 N 0.29515(11) 0.02018(9) 0.06864(9) 0.01186(18) Uani 1 1 d . . . N6 N 0.28952(11) -0.08676(9) 0.11642(9) 0.01211(19) Uani 1 1 d . . . B1 B 0.28050(15) -0.09710(13) 0.23928(12) 0.0125(2) Uani 1 1 d . . . H1B H 0.2889 -0.1801 0.2602 0.015 Uiso 1 1 calc R . . C1 C -0.00510(14) 0.06590(13) 0.28838(12) 0.0165(2) Uani 1 1 d . . . C2 C -0.03485(15) -0.03132(14) 0.34916(13) 0.0201(3) Uani 1 1 d . . . H2 H -0.1097 -0.0441 0.3891 0.024 Uiso 1 1 calc R . . C3 C 0.06619(14) -0.10483(13) 0.33949(12) 0.0169(2) Uani 1 1 d . . . C4 C 0.51341(13) 0.13453(12) 0.32688(11) 0.0133(2) Uani 1 1 d . . . C5 C 0.57578(14) 0.04339(13) 0.37928(11) 0.0158(2) Uani 1 1 d . . . H5 H 0.6556 0.0483 0.4218 0.019 Uiso 1 1 calc R . . C6 C 0.49808(13) -0.05532(12) 0.35680(10) 0.0134(2) Uani 1 1 d . . . C7 C 0.32817(13) 0.00144(11) -0.03266(10) 0.0127(2) Uani 1 1 d . . . C8 C 0.34109(14) -0.11772(12) -0.05076(11) 0.0155(2) Uani 1 1 d . . . H8 H 0.3622 -0.1546 -0.1159 0.019 Uiso 1 1 calc R . . C9 C 0.31692(13) -0.17051(11) 0.04491(11) 0.0139(2) Uani 1 1 d . . . C10 C -0.08221(16) 0.17265(15) 0.27945(14) 0.0238(3) Uani 1 1 d . . . H10A H -0.0253 0.2409 0.2979 0.036 Uiso 1 1 calc R . . H10B H -0.1526 0.1681 0.3291 0.036 Uiso 1 1 calc R . . H10C H -0.1194 0.1792 0.2055 0.036 Uiso 1 1 calc R . . C11 C 0.08878(17) -0.21835(14) 0.39227(14) 0.0236(3) Uani 1 1 d . . . H11A H 0.1734 -0.2147 0.4329 0.035 Uiso 1 1 calc R . . H11B H 0.0881 -0.2799 0.3372 0.035 Uiso 1 1 calc R . . H11C H 0.0197 -0.2350 0.4414 0.035 Uiso 1 1 calc R . . C12 C 0.55708(14) 0.25926(12) 0.32499(12) 0.0176(2) Uani 1 1 d . . . H12A H 0.5397 0.2895 0.2525 0.026 Uiso 1 1 calc R . . H12B H 0.6507 0.2666 0.3447 0.026 Uiso 1 1 calc R . . H12C H 0.5095 0.3036 0.3766 0.026 Uiso 1 1 calc R . . C13 C 0.52000(16) -0.17771(13) 0.38840(12) 0.0196(3) Uani 1 1 d . . . H13A H 0.4412 -0.2108 0.4184 0.029 Uiso 1 1 calc R . . H13B H 0.5929 -0.1794 0.4427 0.029 Uiso 1 1 calc R . . H13C H 0.5403 -0.2233 0.3249 0.029 Uiso 1 1 calc R . . C14 C 0.35115(15) 0.09564(13) -0.11066(11) 0.0177(2) Uani 1 1 d . . . H14A H 0.3892 0.1646 -0.0720 0.027 Uiso 1 1 calc R . . H14B H 0.2683 0.1149 -0.1479 0.027 Uiso 1 1 calc R . . H14C H 0.4112 0.0695 -0.1635 0.027 Uiso 1 1 calc R . . C15 C 0.32059(16) -0.29606(12) 0.07216(13) 0.0202(3) Uani 1 1 d . . . H15A H 0.2368 -0.3217 0.0989 0.030 Uiso 1 1 calc R . . H15B H 0.3902 -0.3075 0.1279 0.030 Uiso 1 1 calc R . . H15C H 0.3372 -0.3415 0.0076 0.030 Uiso 1 1 calc R . . C16 C 0.24950(13) 0.29913(11) 0.28026(10) 0.0126(2) Uani 1 1 d . . . C17 C 0.27342(15) 0.41672(12) 0.26207(11) 0.0164(2) Uani 1 1 d . . . F1 F 0.30046(11) 0.45017(8) 0.16052(7) 0.02324(19) Uani 1 1 d . . . C18 C 0.27426(17) 0.50786(13) 0.33609(12) 0.0218(3) Uani 1 1 d . . . H18 H 0.2909 0.5861 0.3163 0.026 Uiso 1 1 calc R . . C19 C 0.24947(18) 0.47816(13) 0.44025(12) 0.0230(3) Uani 1 1 d . . . F2 F 0.24747(14) 0.56380(9) 0.51595(8) 0.0371(3) Uani 1 1 d . . . C20 C 0.22734(16) 0.36517(13) 0.46962(12) 0.0200(3) Uani 1 1 d . . . H20 H 0.2115 0.3456 0.5417 0.024 Uiso 1 1 calc R . . C21 C 0.22909(14) 0.28058(12) 0.38890(11) 0.0144(2) Uani 1 1 d . . . F3 F 0.21054(9) 0.17044(7) 0.42417(7) 0.01817(17) Uani 1 1 d . . . C22 C 0.11800(15) 0.36325(13) -0.15459(12) 0.0185(3) Uani 1 1 d . . . H22 H 0.0302 0.3343 -0.1590 0.022 Uiso 1 1 calc R . . C23 C 0.16325(17) 0.42985(14) -0.23820(12) 0.0219(3) Uani 1 1 d . . . H23 H 0.1066 0.4460 -0.2988 0.026 Uiso 1 1 calc R . . C24 C 0.29092(17) 0.47241(13) -0.23275(12) 0.0223(3) Uani 1 1 d . . . H24 H 0.3226 0.5171 -0.2899 0.027 Uiso 1 1 calc R . . C25 C 0.37231(16) 0.44945(13) -0.14325(12) 0.0203(3) Uani 1 1 d . . . H25 H 0.4596 0.4796 -0.1388 0.024 Uiso 1 1 calc R . . C26 C 0.32713(15) 0.38257(12) -0.05981(12) 0.0167(2) Uani 1 1 d . . . H26 H 0.3842 0.3671 0.0008 0.020 Uiso 1 1 calc R . . C27 C 0.19913(14) 0.33811(11) -0.06425(11) 0.0141(2) Uani 1 1 d . . . C28 C 0.01983(14) 0.14968(13) -0.02404(12) 0.0183(3) Uani 1 1 d . . . H28A H -0.0397 0.1895 -0.0743 0.027 Uiso 1 1 calc R . . H28B H -0.0304 0.1075 0.0284 0.027 Uiso 1 1 calc R . . H28C H 0.0701 0.0948 -0.0640 0.027 Uiso 1 1 calc R . . C29 C 0.01927(17) 0.36505(14) 0.08987(13) 0.0238(3) Uani 1 1 d . . . H29A H -0.0397 0.3858 0.0289 0.036 Uiso 1 1 calc R . . H29B H 0.0697 0.4344 0.1165 0.036 Uiso 1 1 calc R . . H29C H -0.0316 0.3335 0.1476 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01126(5) 0.00921(4) 0.00957(4) 0.00067(3) 0.00120(3) 0.00064(3) P1 0.01300(15) 0.01149(14) 0.01216(14) 0.00179(11) 0.00113(11) 0.00153(11) N1 0.0122(5) 0.0130(5) 0.0142(5) 0.0012(4) 0.0011(4) 0.0011(4) N2 0.0125(5) 0.0136(5) 0.0131(5) 0.0017(4) 0.0019(4) -0.0003(4) N3 0.0123(5) 0.0112(4) 0.0118(4) 0.0007(3) 0.0005(4) 0.0006(3) N4 0.0129(5) 0.0112(4) 0.0124(5) 0.0010(3) 0.0004(4) 0.0010(4) N5 0.0133(5) 0.0112(4) 0.0112(4) 0.0010(3) 0.0015(4) 0.0008(4) N6 0.0136(5) 0.0105(4) 0.0122(5) 0.0004(3) 0.0011(4) 0.0008(4) B1 0.0142(6) 0.0117(6) 0.0117(6) 0.0005(4) 0.0013(5) 0.0005(5) C1 0.0135(6) 0.0184(6) 0.0180(6) 0.0019(5) 0.0032(5) 0.0018(5) C2 0.0153(6) 0.0235(7) 0.0223(7) 0.0054(5) 0.0074(5) 0.0005(5) C3 0.0158(6) 0.0180(6) 0.0171(6) 0.0037(5) 0.0037(5) -0.0020(5) C4 0.0118(5) 0.0146(5) 0.0135(5) -0.0011(4) 0.0015(4) 0.0000(4) C5 0.0140(6) 0.0190(6) 0.0142(6) 0.0003(4) -0.0019(4) 0.0017(4) C6 0.0148(6) 0.0146(5) 0.0110(5) 0.0002(4) 0.0004(4) 0.0029(4) C7 0.0130(5) 0.0142(5) 0.0108(5) -0.0006(4) 0.0013(4) 0.0015(4) C8 0.0165(6) 0.0162(6) 0.0140(5) -0.0028(4) 0.0017(4) 0.0029(4) C9 0.0136(6) 0.0124(5) 0.0155(6) -0.0018(4) 0.0009(4) 0.0016(4) C10 0.0175(7) 0.0258(7) 0.0296(8) 0.0063(6) 0.0083(6) 0.0075(6) C11 0.0239(7) 0.0211(7) 0.0268(8) 0.0103(6) 0.0072(6) -0.0003(6) C12 0.0153(6) 0.0149(6) 0.0223(7) -0.0011(5) 0.0000(5) -0.0025(5) C13 0.0234(7) 0.0164(6) 0.0189(6) 0.0024(5) -0.0034(5) 0.0058(5) C14 0.0212(7) 0.0193(6) 0.0133(6) 0.0023(5) 0.0054(5) 0.0023(5) C15 0.0253(7) 0.0125(6) 0.0230(7) -0.0019(5) 0.0017(6) 0.0025(5) C16 0.0139(5) 0.0119(5) 0.0123(5) 0.0002(4) 0.0011(4) 0.0015(4) C17 0.0223(7) 0.0134(5) 0.0135(6) 0.0008(4) 0.0010(5) 0.0003(5) F1 0.0393(6) 0.0141(4) 0.0166(4) 0.0019(3) 0.0065(4) -0.0027(4) C18 0.0336(8) 0.0124(6) 0.0189(7) -0.0016(5) -0.0012(6) 0.0013(5) C19 0.0371(9) 0.0157(6) 0.0159(6) -0.0063(5) -0.0032(6) 0.0057(6) F2 0.0727(9) 0.0191(5) 0.0191(5) -0.0082(4) -0.0032(5) 0.0077(5) C20 0.0280(8) 0.0193(6) 0.0126(6) -0.0013(5) 0.0004(5) 0.0038(5) C21 0.0162(6) 0.0132(5) 0.0139(5) -0.0002(4) 0.0000(4) 0.0016(4) F3 0.0257(5) 0.0147(4) 0.0141(4) 0.0023(3) 0.0019(3) -0.0008(3) C22 0.0186(6) 0.0210(6) 0.0160(6) 0.0038(5) 0.0006(5) 0.0010(5) C23 0.0304(8) 0.0215(7) 0.0138(6) 0.0053(5) 0.0002(5) 0.0018(6) C24 0.0327(8) 0.0180(6) 0.0165(6) 0.0040(5) 0.0047(6) -0.0014(6) C25 0.0242(7) 0.0170(6) 0.0199(7) 0.0015(5) 0.0053(5) -0.0036(5) C26 0.0196(6) 0.0148(6) 0.0156(6) 0.0016(4) 0.0016(5) -0.0016(5) C27 0.0171(6) 0.0130(5) 0.0123(5) 0.0012(4) 0.0014(4) 0.0012(4) C28 0.0152(6) 0.0175(6) 0.0217(7) 0.0025(5) -0.0026(5) -0.0025(5) C29 0.0289(8) 0.0226(7) 0.0217(7) 0.0066(5) 0.0078(6) 0.0130(6) _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 C16 2.0446(13) . ? Rh1 N3 2.1068(11) . ? Rh1 N5 2.1513(11) . ? Rh1 N1 2.2582(12) . ? Rh1 P1 2.2688(4) . ? Rh1 H1 1.469(19) . ? P1 C28 1.8167(15) . ? P1 C29 1.8305(16) . ? P1 C27 1.8407(14) . ? N1 C1 1.3427(18) . ? N1 N2 1.3723(16) . ? N2 C3 1.3550(18) . ? N2 B1 1.5262(19) . ? N3 C4 1.3433(17) . ? N3 N4 1.3643(15) . ? N4 C6 1.3518(17) . ? N4 B1 1.5403(19) . ? N5 C7 1.3416(17) . ? N5 N6 1.3762(15) . ? N6 C9 1.3529(17) . ? N6 B1 1.5428(18) . ? B1 H1B 1.0000 . ? C1 C2 1.395(2) . ? C1 C10 1.490(2) . ? C2 C3 1.375(2) . ? C2 H2 0.9500 . ? C3 C11 1.491(2) . ? C4 C5 1.3988(19) . ? C4 C12 1.4917(19) . ? C5 C6 1.383(2) . ? C5 H5 0.9500 . ? C6 C13 1.4907(19) . ? C7 C8 1.4012(19) . ? C7 C14 1.4875(19) . ? C8 C9 1.375(2) . ? C8 H8 0.9500 . ? C9 C15 1.492(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.3926(19) . ? C16 C21 1.3982(19) . ? C17 F1 1.3671(16) . ? C17 C18 1.387(2) . ? C18 C19 1.381(2) . ? C18 H18 0.9500 . ? C19 F2 1.3569(17) . ? C19 C20 1.372(2) . ? C20 C21 1.392(2) . ? C20 H20 0.9500 . ? C21 F3 1.3592(16) . ? C22 C23 1.393(2) . ? C22 C27 1.399(2) . ? C22 H22 0.9500 . ? C23 C24 1.383(2) . ? C23 H23 0.9500 . ? C24 C25 1.387(2) . ? C24 H24 0.9500 . ? C25 C26 1.393(2) . ? C25 H25 0.9500 . ? C26 C27 1.394(2) . ? C26 H26 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N3 88.51(5) . . ? C16 Rh1 N5 172.37(5) . . ? N3 Rh1 N5 83.88(4) . . ? C16 Rh1 N1 94.47(5) . . ? N3 Rh1 N1 88.64(4) . . ? N5 Rh1 N1 85.86(4) . . ? C16 Rh1 P1 92.51(4) . . ? N3 Rh1 P1 173.35(3) . . ? N5 Rh1 P1 94.99(3) . . ? N1 Rh1 P1 97.82(3) . . ? C16 Rh1 H1 86.5(8) . . ? N3 Rh1 H1 89.0(7) . . ? N5 Rh1 H1 92.9(8) . . ? N1 Rh1 H1 177.4(7) . . ? P1 Rh1 H1 84.5(7) . . ? C28 P1 C29 102.42(8) . . ? C28 P1 C27 103.26(7) . . ? C29 P1 C27 97.77(7) . . ? C28 P1 Rh1 110.36(5) . . ? C29 P1 Rh1 119.58(6) . . ? C27 P1 Rh1 120.80(5) . . ? C1 N1 N2 105.83(11) . . ? C1 N1 Rh1 137.55(10) . . ? N2 N1 Rh1 114.03(8) . . ? C3 N2 N1 110.47(11) . . ? C3 N2 B1 128.57(12) . . ? N1 N2 B1 120.87(11) . . ? C4 N3 N4 107.14(10) . . ? C4 N3 Rh1 133.35(9) . . ? N4 N3 Rh1 119.25(8) . . ? C6 N4 N3 110.16(11) . . ? C6 N4 B1 130.34(11) . . ? N3 N4 B1 119.31(10) . . ? C7 N5 N6 106.45(10) . . ? C7 N5 Rh1 137.22(9) . . ? N6 N5 Rh1 116.22(8) . . ? C9 N6 N5 109.96(11) . . ? C9 N6 B1 128.03(11) . . ? N5 N6 B1 120.90(10) . . ? N2 B1 N4 109.89(11) . . ? N2 B1 N6 110.59(11) . . ? N4 B1 N6 107.94(11) . . ? N2 B1 H1B 109.5 . . ? N4 B1 H1B 109.5 . . ? N6 B1 H1B 109.5 . . ? N1 C1 C2 110.25(13) . . ? N1 C1 C10 123.80(13) . . ? C2 C1 C10 125.88(13) . . ? C3 C2 C1 106.04(13) . . ? C3 C2 H2 127.0 . . ? C1 C2 H2 127.0 . . ? N2 C3 C2 107.39(12) . . ? N2 C3 C11 123.43(13) . . ? C2 C3 C11 129.13(13) . . ? N3 C4 C5 109.07(12) . . ? N3 C4 C12 123.00(12) . . ? C5 C4 C12 127.92(13) . . ? C6 C5 C4 106.32(12) . . ? C6 C5 H5 126.8 . . ? C4 C5 H5 126.8 . . ? N4 C6 C5 107.31(12) . . ? N4 C6 C13 123.31(12) . . ? C5 C6 C13 129.34(13) . . ? N5 C7 C8 109.74(12) . . ? N5 C7 C14 123.79(12) . . ? C8 C7 C14 126.44(12) . . ? C9 C8 C7 106.02(12) . . ? C9 C8 H8 127.0 . . ? C7 C8 H8 127.0 . . ? N6 C9 C8 107.82(12) . . ? N6 C9 C15 123.23(12) . . ? C8 C9 C15 128.95(13) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 110.51(12) . . ? C17 C16 Rh1 125.89(10) . . ? C21 C16 Rh1 123.26(9) . . ? F1 C17 C18 113.91(12) . . ? F1 C17 C16 118.40(12) . . ? C18 C17 C16 127.69(13) . . ? C19 C18 C17 116.05(14) . . ? C19 C18 H18 122.0 . . ? C17 C18 H18 122.0 . . ? F2 C19 C20 119.08(14) . . ? F2 C19 C18 118.72(14) . . ? C20 C19 C18 122.20(14) . . ? C19 C20 C21 116.94(13) . . ? C19 C20 H20 121.5 . . ? C21 C20 H20 121.5 . . ? F3 C21 C20 113.85(12) . . ? F3 C21 C16 119.57(12) . . ? C20 C21 C16 126.57(13) . . ? C23 C22 C27 121.38(14) . . ? C23 C22 H22 119.3 . . ? C27 C22 H22 119.3 . . ? C24 C23 C22 119.85(14) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 119.55(14) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C26 120.58(15) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 120.71(14) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C22 117.92(13) . . ? C26 C27 P1 123.08(10) . . ? C22 C27 P1 118.91(11) . . ? P1 C28 H28A 109.5 . . ? P1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P1 C29 H29A 109.5 . . ? P1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 P1 C28 -140.06(7) . . . . ? N3 Rh1 P1 C28 121.2(3) . . . . ? N5 Rh1 P1 C28 41.30(6) . . . . ? N1 Rh1 P1 C28 -45.20(6) . . . . ? C16 Rh1 P1 C29 -21.75(8) . . . . ? N3 Rh1 P1 C29 -120.5(3) . . . . ? N5 Rh1 P1 C29 159.61(7) . . . . ? N1 Rh1 P1 C29 73.12(8) . . . . ? C16 Rh1 P1 C27 99.54(6) . . . . ? N3 Rh1 P1 C27 0.8(3) . . . . ? N5 Rh1 P1 C27 -79.11(6) . . . . ? N1 Rh1 P1 C27 -165.60(6) . . . . ? C16 Rh1 N1 C1 36.81(15) . . . . ? N3 Rh1 N1 C1 125.21(14) . . . . ? N5 Rh1 N1 C1 -150.83(14) . . . . ? P1 Rh1 N1 C1 -56.35(14) . . . . ? C16 Rh1 N1 N2 -121.61(9) . . . . ? N3 Rh1 N1 N2 -33.22(9) . . . . ? N5 Rh1 N1 N2 50.75(9) . . . . ? P1 Rh1 N1 N2 145.23(8) . . . . ? C1 N1 N2 C3 -0.69(15) . . . . ? Rh1 N1 N2 C3 164.36(9) . . . . ? C1 N1 N2 B1 -177.77(12) . . . . ? Rh1 N1 N2 B1 -12.73(15) . . . . ? C16 Rh1 N3 C4 -51.94(13) . . . . ? N5 Rh1 N3 C4 127.58(13) . . . . ? N1 Rh1 N3 C4 -146.44(13) . . . . ? P1 Rh1 N3 C4 47.0(4) . . . . ? C16 Rh1 N3 N4 134.73(10) . . . . ? N5 Rh1 N3 N4 -45.76(9) . . . . ? N1 Rh1 N3 N4 40.22(9) . . . . ? P1 Rh1 N3 N4 -126.3(2) . . . . ? C4 N3 N4 C6 -0.12(14) . . . . ? Rh1 N3 N4 C6 174.82(9) . . . . ? C4 N3 N4 B1 -175.63(11) . . . . ? Rh1 N3 N4 B1 -0.70(15) . . . . ? C16 Rh1 N5 C7 -121.8(3) . . . . ? N3 Rh1 N5 C7 -125.45(14) . . . . ? N1 Rh1 N5 C7 145.48(14) . . . . ? P1 Rh1 N5 C7 47.97(13) . . . . ? C16 Rh1 N5 N6 53.8(4) . . . . ? N3 Rh1 N5 N6 50.11(9) . . . . ? N1 Rh1 N5 N6 -38.96(9) . . . . ? P1 Rh1 N5 N6 -136.47(9) . . . . ? C7 N5 N6 C9 -0.86(14) . . . . ? Rh1 N5 N6 C9 -177.71(9) . . . . ? C7 N5 N6 B1 168.02(12) . . . . ? Rh1 N5 N6 B1 -8.84(15) . . . . ? C3 N2 B1 N4 -108.25(15) . . . . ? N1 N2 B1 N4 68.26(15) . . . . ? C3 N2 B1 N6 132.67(14) . . . . ? N1 N2 B1 N6 -50.82(16) . . . . ? C6 N4 B1 N2 124.76(14) . . . . ? N3 N4 B1 N2 -60.77(15) . . . . ? C6 N4 B1 N6 -114.56(14) . . . . ? N3 N4 B1 N6 59.91(15) . . . . ? C9 N6 B1 N2 -126.76(14) . . . . ? N5 N6 B1 N2 66.55(15) . . . . ? C9 N6 B1 N4 113.00(14) . . . . ? N5 N6 B1 N4 -53.69(15) . . . . ? N2 N1 C1 C2 -0.13(16) . . . . ? Rh1 N1 C1 C2 -159.69(11) . . . . ? N2 N1 C1 C10 176.99(14) . . . . ? Rh1 N1 C1 C10 17.4(2) . . . . ? N1 C1 C2 C3 0.86(18) . . . . ? C10 C1 C2 C3 -176.18(15) . . . . ? N1 N2 C3 C2 1.23(16) . . . . ? B1 N2 C3 C2 178.03(13) . . . . ? N1 N2 C3 C11 -176.57(14) . . . . ? B1 N2 C3 C11 0.2(2) . . . . ? C1 C2 C3 N2 -1.25(17) . . . . ? C1 C2 C3 C11 176.38(16) . . . . ? N4 N3 C4 C5 -0.27(15) . . . . ? Rh1 N3 C4 C5 -174.18(10) . . . . ? N4 N3 C4 C12 179.98(12) . . . . ? Rh1 N3 C4 C12 6.1(2) . . . . ? N3 C4 C5 C6 0.54(16) . . . . ? C12 C4 C5 C6 -179.72(14) . . . . ? N3 N4 C6 C5 0.45(15) . . . . ? B1 N4 C6 C5 175.32(13) . . . . ? N3 N4 C6 C13 -177.67(13) . . . . ? B1 N4 C6 C13 -2.8(2) . . . . ? C4 C5 C6 N4 -0.60(15) . . . . ? C4 C5 C6 C13 177.37(14) . . . . ? N6 N5 C7 C8 1.23(15) . . . . ? Rh1 N5 C7 C8 177.08(10) . . . . ? N6 N5 C7 C14 -176.88(12) . . . . ? Rh1 N5 C7 C14 -1.0(2) . . . . ? N5 C7 C8 C9 -1.16(16) . . . . ? C14 C7 C8 C9 176.90(13) . . . . ? N5 N6 C9 C8 0.14(15) . . . . ? B1 N6 C9 C8 -167.73(13) . . . . ? N5 N6 C9 C15 179.16(13) . . . . ? B1 N6 C9 C15 11.3(2) . . . . ? C7 C8 C9 N6 0.60(16) . . . . ? C7 C8 C9 C15 -178.35(14) . . . . ? N3 Rh1 C16 C17 121.30(13) . . . . ? N5 Rh1 C16 C17 117.6(3) . . . . ? N1 Rh1 C16 C17 -150.18(12) . . . . ? P1 Rh1 C16 C17 -52.13(12) . . . . ? N3 Rh1 C16 C21 -51.41(12) . . . . ? N5 Rh1 C16 C21 -55.1(4) . . . . ? N1 Rh1 C16 C21 37.11(12) . . . . ? P1 Rh1 C16 C21 135.16(11) . . . . ? C21 C16 C17 F1 177.57(13) . . . . ? Rh1 C16 C17 F1 4.1(2) . . . . ? C21 C16 C17 C18 -2.0(2) . . . . ? Rh1 C16 C17 C18 -175.51(13) . . . . ? F1 C17 C18 C19 -179.02(14) . . . . ? C16 C17 C18 C19 0.6(3) . . . . ? C17 C18 C19 F2 -179.22(15) . . . . ? C17 C18 C19 C20 1.0(3) . . . . ? F2 C19 C20 C21 179.37(15) . . . . ? C18 C19 C20 C21 -0.9(3) . . . . ? C19 C20 C21 F3 178.05(14) . . . . ? C19 C20 C21 C16 -0.9(2) . . . . ? C17 C16 C21 F3 -176.73(12) . . . . ? Rh1 C16 C21 F3 -3.03(18) . . . . ? C17 C16 C21 C20 2.2(2) . . . . ? Rh1 C16 C21 C20 175.87(12) . . . . ? C27 C22 C23 C24 0.1(2) . . . . ? C22 C23 C24 C25 -0.8(2) . . . . ? C23 C24 C25 C26 1.0(2) . . . . ? C24 C25 C26 C27 -0.4(2) . . . . ? C25 C26 C27 C22 -0.3(2) . . . . ? C25 C26 C27 P1 -176.65(11) . . . . ? C23 C22 C27 C26 0.5(2) . . . . ? C23 C22 C27 P1 177.00(12) . . . . ? C28 P1 C27 C26 -145.25(12) . . . . ? C29 P1 C27 C26 109.97(13) . . . . ? Rh1 P1 C27 C26 -21.42(14) . . . . ? C28 P1 C27 C22 38.41(13) . . . . ? C29 P1 C27 C22 -66.37(13) . . . . ? Rh1 P1 C27 C22 162.23(10) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 36.32 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.079 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.106 #===end data_jontt15_cmpd9e _database_code_depnum_ccdc_archive 'CCDC 770121' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt15 _chemical_melting_point ? _chemical_formula_moiety 'C29 H37 B F2 N6 P Rh' _chemical_formula_sum 'C29 H37 B F2 N6 P Rh' _chemical_formula_weight 652.34 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' _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 10.2523(9) _cell_length_b 11.6983(10) _cell_length_c 12.3627(11) _cell_angle_alpha 92.716(2) _cell_angle_beta 95.959(2) _cell_angle_gamma 92.041(2) _cell_volume 1471.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 4048 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 30.59 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8878 _exptl_absorpt_correction_T_max 0.9605 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26065 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.1238 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 31.50 _reflns_number_total 9759 _reflns_number_gt 6497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The hydride ligand atom was found from the difference Fourier map and its position and isotropic thermal parameter were refined independently from those of all other atoms. ; _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^)+(0.0467P)^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 9759 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 0.26887(3) 0.67001(2) 0.67250(2) 0.01322(7) Uani 1 1 d . . . H1 H 0.379(4) 0.733(3) 0.635(3) 0.024(11) Uiso 1 1 d . . . P1 P 0.13246(9) 0.75446(8) 0.54838(7) 0.01561(18) Uani 1 1 d . . . N1 N 0.1193(3) 0.5584(2) 0.7452(2) 0.0165(6) Uani 1 1 d . . . N2 N 0.1651(3) 0.4543(2) 0.7765(2) 0.0159(6) Uani 1 1 d . . . N3 N 0.2996(3) 0.5200(2) 0.5700(2) 0.0165(6) Uani 1 1 d . . . N4 N 0.2967(3) 0.4164(2) 0.6181(2) 0.0147(6) Uani 1 1 d . . . N5 N 0.4149(3) 0.6019(2) 0.7820(2) 0.0153(6) Uani 1 1 d . . . N6 N 0.4103(3) 0.4871(2) 0.7988(2) 0.0144(6) Uani 1 1 d . . . B1 B 0.2946(4) 0.4111(3) 0.7422(3) 0.0170(8) Uani 1 1 d . . . H1B H 0.3050 0.3303 0.7635 0.020 Uiso 1 1 calc R . . C1 C 0.0046(3) 0.5693(3) 0.7873(3) 0.0201(7) Uani 1 1 d . . . C2 C -0.0227(4) 0.4738(3) 0.8452(3) 0.0229(8) Uani 1 1 d . . . H2 H -0.0977 0.4601 0.8826 0.027 Uiso 1 1 calc R . . C3 C 0.0801(4) 0.4034(3) 0.8376(3) 0.0200(7) Uani 1 1 d . . . C4 C 0.3270(3) 0.4971(3) 0.4677(3) 0.0168(7) Uani 1 1 d . . . C5 C 0.3411(3) 0.3802(3) 0.4502(3) 0.0190(7) Uani 1 1 d . . . H5 H 0.3600 0.3418 0.3846 0.023 Uiso 1 1 calc R . . C6 C 0.3224(3) 0.3311(3) 0.5462(3) 0.0183(7) Uani 1 1 d . . . C7 C 0.5273(3) 0.6455(3) 0.8356(3) 0.0164(7) Uani 1 1 d . . . C8 C 0.5949(3) 0.5575(3) 0.8860(3) 0.0184(7) Uani 1 1 d . . . H8 H 0.6774 0.5644 0.9290 0.022 Uiso 1 1 calc R . . C9 C 0.5187(3) 0.4591(3) 0.8609(3) 0.0153(7) Uani 1 1 d . . . C10 C -0.0770(4) 0.6707(4) 0.7743(3) 0.0286(9) Uani 1 1 d . . . H10A H -0.0245 0.7399 0.8012 0.043 Uiso 1 1 calc R . . H10B H -0.1526 0.6625 0.8161 0.043 Uiso 1 1 calc R . . H10C H -0.1077 0.6769 0.6972 0.043 Uiso 1 1 calc R . . C11 C 0.1044(4) 0.2904(3) 0.8877(3) 0.0276(9) Uani 1 1 d . . . H11A H 0.1866 0.2964 0.9361 0.041 Uiso 1 1 calc R . . H11B H 0.1106 0.2310 0.8301 0.041 Uiso 1 1 calc R . . H11C H 0.0317 0.2701 0.9297 0.041 Uiso 1 1 calc R . . C12 C 0.3445(4) 0.5875(3) 0.3892(3) 0.0208(8) Uani 1 1 d . . . H12A H 0.3807 0.6580 0.4289 0.031 Uiso 1 1 calc R . . H12B H 0.2594 0.6022 0.3496 0.031 Uiso 1 1 calc R . . H12C H 0.4049 0.5619 0.3375 0.031 Uiso 1 1 calc R . . C13 C 0.3277(4) 0.2089(3) 0.5753(3) 0.0242(8) Uani 1 1 d . . . H13A H 0.2475 0.1867 0.6072 0.036 Uiso 1 1 calc R . . H13B H 0.4041 0.1996 0.6282 0.036 Uiso 1 1 calc R . . H13C H 0.3348 0.1603 0.5096 0.036 Uiso 1 1 calc R . . C14 C 0.5682(4) 0.7689(3) 0.8375(3) 0.0228(8) Uani 1 1 d . . . H14A H 0.5465 0.7981 0.7651 0.034 Uiso 1 1 calc R . . H14B H 0.6631 0.7780 0.8579 0.034 Uiso 1 1 calc R . . H14C H 0.5220 0.8119 0.8907 0.034 Uiso 1 1 calc R . . C15 C 0.5473(4) 0.3391(3) 0.8888(3) 0.0231(8) Uani 1 1 d . . . H15A H 0.4682 0.3013 0.9110 0.035 Uiso 1 1 calc R . . H15B H 0.6179 0.3402 0.9488 0.035 Uiso 1 1 calc R . . H15C H 0.5746 0.2971 0.8250 0.035 Uiso 1 1 calc R . . C16 C 0.2573(3) 0.8003(3) 0.7848(3) 0.0171(7) Uani 1 1 d . . . C17 C 0.2902(4) 0.9141(3) 0.7738(3) 0.0222(8) Uani 1 1 d . . . F1 F 0.3233(2) 0.95169(19) 0.67779(19) 0.0307(5) Uani 1 1 d . . . C18 C 0.2918(4) 0.9971(3) 0.8578(3) 0.0284(9) Uani 1 1 d . . . F2 F 0.3284(3) 1.1063(2) 0.8378(2) 0.0433(7) Uani 1 1 d . . . C19 C 0.2616(5) 0.9714(4) 0.9586(4) 0.0336(10) Uani 1 1 d . . . H19 H 0.2633 1.0287 1.0160 0.040 Uiso 1 1 calc R . . C20 C 0.2284(4) 0.8583(4) 0.9739(3) 0.0290(9) Uani 1 1 d . . . H20 H 0.2066 0.8370 1.0432 0.035 Uiso 1 1 calc R . . C21 C 0.2265(4) 0.7750(3) 0.8895(3) 0.0209(8) Uani 1 1 d . . . H21 H 0.2034 0.6981 0.9032 0.025 Uiso 1 1 calc R . . C22 C 0.3253(4) 0.8779(3) 0.4460(3) 0.0217(8) Uani 1 1 d . . . H22A H 0.3847 0.8635 0.5076 0.026 Uiso 1 1 calc R . . C23 C 0.3681(4) 0.9434(3) 0.3648(3) 0.0256(8) Uani 1 1 d . . . H23 H 0.4564 0.9726 0.3706 0.031 Uiso 1 1 calc R . . C24 C 0.2828(4) 0.9660(3) 0.2759(3) 0.0282(9) Uani 1 1 d . . . H24 H 0.3120 1.0110 0.2205 0.034 Uiso 1 1 calc R . . C25 C 0.1549(4) 0.9234(4) 0.2670(3) 0.0273(9) Uani 1 1 d . . . H25 H 0.0960 0.9391 0.2055 0.033 Uiso 1 1 calc R . . C26 C 0.1122(4) 0.8575(3) 0.3480(3) 0.0253(8) Uani 1 1 d . . . H26 H 0.0238 0.8286 0.3417 0.030 Uiso 1 1 calc R . . C27 C 0.1977(4) 0.8334(3) 0.4387(3) 0.0185(7) Uani 1 1 d . . . C28 C 0.0283(4) 0.8661(3) 0.5947(3) 0.0251(8) Uani 1 1 d . . . H28A H -0.0427 0.8780 0.5374 0.038 Uiso 1 1 calc R . . H28B H 0.0808 0.9376 0.6113 0.038 Uiso 1 1 calc R . . H28C H -0.0092 0.8427 0.6604 0.038 Uiso 1 1 calc R . . C29 C 0.0164(4) 0.6500(3) 0.4753(3) 0.0221(8) Uani 1 1 d . . . H29A H -0.0479 0.6895 0.4278 0.033 Uiso 1 1 calc R . . H29B H -0.0290 0.6072 0.5275 0.033 Uiso 1 1 calc R . . H29C H 0.0635 0.5969 0.4311 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01406(13) 0.01300(13) 0.01277(12) 0.00121(9) 0.00184(9) 0.00090(9) P1 0.0160(4) 0.0151(4) 0.0160(4) 0.0028(3) 0.0020(3) 0.0012(3) N1 0.0183(15) 0.0172(15) 0.0142(14) 0.0008(11) 0.0025(11) 0.0001(12) N2 0.0141(14) 0.0163(15) 0.0173(14) 0.0037(12) 0.0010(11) -0.0028(11) N3 0.0202(15) 0.0160(15) 0.0134(14) 0.0017(11) 0.0008(11) 0.0020(12) N4 0.0149(14) 0.0154(14) 0.0136(14) 0.0014(11) 0.0004(11) 0.0003(11) N5 0.0163(14) 0.0142(14) 0.0158(14) 0.0027(11) 0.0026(11) 0.0023(11) N6 0.0142(14) 0.0140(14) 0.0157(14) 0.0015(11) 0.0037(11) 0.0011(11) B1 0.0193(19) 0.0148(19) 0.0171(19) 0.0037(15) 0.0013(15) 0.0025(15) C1 0.0160(17) 0.027(2) 0.0172(17) -0.0006(15) 0.0029(13) 0.0008(15) C2 0.0170(18) 0.031(2) 0.0221(19) 0.0044(16) 0.0091(14) 0.0003(15) C3 0.0184(17) 0.0223(19) 0.0196(18) 0.0011(14) 0.0057(14) -0.0073(14) C4 0.0143(16) 0.0218(18) 0.0139(16) 0.0003(14) 0.0005(13) 0.0001(13) C5 0.0173(17) 0.0229(19) 0.0167(17) -0.0052(14) 0.0029(13) 0.0030(14) C6 0.0159(17) 0.0185(18) 0.0199(18) -0.0032(14) 0.0005(13) 0.0015(14) C7 0.0188(17) 0.0175(17) 0.0135(16) -0.0006(13) 0.0052(13) 0.0002(13) C8 0.0169(17) 0.0233(19) 0.0146(17) -0.0012(14) -0.0002(13) 0.0031(14) C9 0.0147(16) 0.0191(17) 0.0122(15) 0.0005(13) 0.0018(12) 0.0018(13) C10 0.022(2) 0.036(2) 0.029(2) 0.0060(18) 0.0092(16) 0.0074(17) C11 0.027(2) 0.026(2) 0.030(2) 0.0086(17) 0.0037(17) -0.0053(17) C12 0.0216(18) 0.025(2) 0.0162(17) 0.0013(15) 0.0031(14) 0.0033(15) C13 0.027(2) 0.0197(19) 0.025(2) -0.0034(15) 0.0000(16) 0.0051(15) C14 0.0198(18) 0.0217(19) 0.026(2) -0.0014(15) 0.0020(15) -0.0010(15) C15 0.029(2) 0.0198(19) 0.0207(19) 0.0032(15) -0.0001(15) 0.0033(16) C16 0.0158(17) 0.0140(17) 0.0217(18) 0.0018(14) 0.0015(13) 0.0019(13) C17 0.028(2) 0.0195(19) 0.0192(18) 0.0008(15) 0.0032(15) 0.0041(16) F1 0.0444(15) 0.0221(12) 0.0262(13) 0.0038(10) 0.0078(11) -0.0036(11) C18 0.037(2) 0.0148(19) 0.032(2) -0.0025(16) -0.0008(18) 0.0016(16) F2 0.074(2) 0.0161(12) 0.0389(16) -0.0028(11) 0.0056(14) -0.0037(12) C19 0.049(3) 0.024(2) 0.027(2) -0.0069(17) 0.0009(19) 0.008(2) C20 0.038(2) 0.029(2) 0.0195(19) -0.0018(16) 0.0032(17) 0.0049(18) C21 0.0244(19) 0.0191(19) 0.0195(18) 0.0000(14) 0.0040(15) 0.0023(15) C22 0.027(2) 0.0189(18) 0.0195(18) 0.0039(14) 0.0017(15) -0.0014(15) C23 0.029(2) 0.020(2) 0.029(2) 0.0050(16) 0.0086(17) -0.0033(16) C24 0.043(3) 0.020(2) 0.023(2) 0.0056(16) 0.0080(18) -0.0006(18) C25 0.035(2) 0.030(2) 0.0166(18) 0.0073(16) -0.0027(16) 0.0011(17) C26 0.027(2) 0.026(2) 0.0226(19) 0.0049(16) -0.0014(16) -0.0015(16) C27 0.0249(19) 0.0163(17) 0.0149(16) 0.0046(13) 0.0031(14) 0.0014(14) C28 0.027(2) 0.026(2) 0.024(2) 0.0067(16) 0.0040(16) 0.0075(16) C29 0.0196(18) 0.0210(19) 0.026(2) 0.0051(15) -0.0002(15) -0.0006(15) _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 C16 2.028(4) . ? Rh1 N5 2.115(3) . ? Rh1 N3 2.167(3) . ? Rh1 P1 2.2545(10) . ? Rh1 N1 2.263(3) . ? Rh1 H1 1.45(4) . ? P1 C29 1.815(4) . ? P1 C28 1.825(4) . ? P1 C27 1.844(4) . ? N1 C1 1.342(4) . ? N1 N2 1.378(4) . ? N2 C3 1.351(4) . ? N2 B1 1.531(5) . ? N3 C4 1.341(4) . ? N3 N4 1.376(4) . ? N4 C6 1.355(4) . ? N4 B1 1.541(5) . ? N5 C7 1.340(4) . ? N5 N6 1.369(4) . ? N6 C9 1.343(4) . ? N6 B1 1.542(5) . ? B1 H1B 1.0000 . ? C1 C2 1.391(5) . ? C1 C10 1.481(5) . ? C2 C3 1.369(5) . ? C2 H2 0.9500 . ? C3 C11 1.504(5) . ? C4 C5 1.389(5) . ? C4 C12 1.487(5) . ? C5 C6 1.371(5) . ? C5 H5 0.9500 . ? C6 C13 1.491(5) . ? C7 C8 1.396(5) . ? C7 C14 1.487(5) . ? C8 C9 1.372(5) . ? C8 H8 0.9500 . ? C9 C15 1.494(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.378(5) . ? C16 C21 1.407(5) . ? C17 F1 1.356(4) . ? C17 C18 1.386(5) . ? C18 F2 1.359(5) . ? C18 C19 1.360(6) . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 C21 1.391(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.383(5) . ? C22 C23 1.389(5) . ? C22 H22A 0.9500 . ? C23 C24 1.373(6) . ? C23 H23 0.9500 . ? C24 C25 1.378(6) . ? C24 H24 0.9500 . ? C25 C26 1.389(5) . ? C25 H25 0.9500 . ? C26 C27 1.396(5) . ? C26 H26 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N5 87.87(13) . . ? C16 Rh1 N3 171.88(12) . . ? N5 Rh1 N3 84.06(11) . . ? C16 Rh1 P1 91.89(10) . . ? N5 Rh1 P1 173.30(8) . . ? N3 Rh1 P1 96.24(8) . . ? C16 Rh1 N1 92.88(12) . . ? N5 Rh1 N1 87.82(11) . . ? N3 Rh1 N1 85.88(11) . . ? P1 Rh1 N1 98.88(8) . . ? C16 Rh1 H1 88.0(15) . . ? N5 Rh1 H1 84.2(15) . . ? N3 Rh1 H1 92.1(15) . . ? P1 Rh1 H1 89.1(15) . . ? N1 Rh1 H1 172.0(15) . . ? C29 P1 C28 103.52(18) . . ? C29 P1 C27 103.38(17) . . ? C28 P1 C27 97.05(17) . . ? C29 P1 Rh1 110.86(12) . . ? C28 P1 Rh1 118.90(13) . . ? C27 P1 Rh1 120.65(12) . . ? C1 N1 N2 106.0(3) . . ? C1 N1 Rh1 138.5(3) . . ? N2 N1 Rh1 114.0(2) . . ? C3 N2 N1 109.8(3) . . ? C3 N2 B1 129.0(3) . . ? N1 N2 B1 121.2(3) . . ? C4 N3 N4 106.0(3) . . ? C4 N3 Rh1 137.4(2) . . ? N4 N3 Rh1 116.5(2) . . ? C6 N4 N3 110.2(3) . . ? C6 N4 B1 127.8(3) . . ? N3 N4 B1 120.7(3) . . ? C7 N5 N6 106.8(3) . . ? C7 N5 Rh1 133.5(2) . . ? N6 N5 Rh1 119.3(2) . . ? C9 N6 N5 110.1(3) . . ? C9 N6 B1 130.6(3) . . ? N5 N6 B1 119.3(3) . . ? N2 B1 N4 110.4(3) . . ? N2 B1 N6 109.8(3) . . ? N4 B1 N6 108.3(3) . . ? N2 B1 H1B 109.4 . . ? N4 B1 H1B 109.4 . . ? N6 B1 H1B 109.4 . . ? N1 C1 C2 110.0(3) . . ? N1 C1 C10 123.7(3) . . ? C2 C1 C10 126.3(3) . . ? C3 C2 C1 106.3(3) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? N2 C3 C2 107.9(3) . . ? N2 C3 C11 122.9(3) . . ? C2 C3 C11 129.2(3) . . ? N3 C4 C5 110.0(3) . . ? N3 C4 C12 123.0(3) . . ? C5 C4 C12 126.9(3) . . ? C6 C5 C4 106.6(3) . . ? C6 C5 H5 126.7 . . ? C4 C5 H5 126.7 . . ? N4 C6 C5 107.2(3) . . ? N4 C6 C13 122.6(3) . . ? C5 C6 C13 130.2(3) . . ? N5 C7 C8 109.1(3) . . ? N5 C7 C14 123.2(3) . . ? C8 C7 C14 127.7(3) . . ? C9 C8 C7 106.4(3) . . ? C9 C8 H8 126.8 . . ? C7 C8 H8 126.8 . . ? N6 C9 C8 107.7(3) . . ? N6 C9 C15 123.3(3) . . ? C8 C9 C15 128.9(3) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 114.1(3) . . ? C17 C16 Rh1 126.5(3) . . ? C21 C16 Rh1 119.1(3) . . ? F1 C17 C16 121.0(3) . . ? F1 C17 C18 115.6(3) . . ? C16 C17 C18 123.3(4) . . ? F2 C18 C19 120.1(4) . . ? F2 C18 C17 118.0(4) . . ? C19 C18 C17 121.9(4) . . ? C18 C19 C20 117.0(4) . . ? C18 C19 H19 121.5 . . ? C20 C19 H19 121.5 . . ? C19 C20 C21 121.1(4) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 122.6(4) . . ? C20 C21 H21 118.7 . . ? C16 C21 H21 118.7 . . ? C27 C22 C23 121.1(4) . . ? C27 C22 H22A 119.4 . . ? C23 C22 H22A 119.4 . . ? C24 C23 C22 120.0(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.1(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 119.9(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 120.7(4) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C22 C27 C26 118.1(3) . . ? C22 C27 P1 122.9(3) . . ? C26 C27 P1 118.7(3) . . ? P1 C28 H28A 109.5 . . ? P1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P1 C29 H29A 109.5 . . ? P1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 P1 C29 -138.35(17) . . . . ? N5 Rh1 P1 C29 133.8(7) . . . . ? N3 Rh1 P1 C29 41.64(16) . . . . ? N1 Rh1 P1 C29 -45.14(16) . . . . ? C16 Rh1 P1 C28 -18.60(19) . . . . ? N5 Rh1 P1 C28 -106.4(7) . . . . ? N3 Rh1 P1 C28 161.39(17) . . . . ? N1 Rh1 P1 C28 74.61(17) . . . . ? C16 Rh1 P1 C27 100.74(17) . . . . ? N5 Rh1 P1 C27 12.9(8) . . . . ? N3 Rh1 P1 C27 -79.26(16) . . . . ? N1 Rh1 P1 C27 -166.04(15) . . . . ? C16 Rh1 N1 C1 41.3(4) . . . . ? N5 Rh1 N1 C1 129.0(4) . . . . ? N3 Rh1 N1 C1 -146.8(4) . . . . ? P1 Rh1 N1 C1 -51.1(4) . . . . ? C16 Rh1 N1 N2 -122.2(2) . . . . ? N5 Rh1 N1 N2 -34.4(2) . . . . ? N3 Rh1 N1 N2 49.8(2) . . . . ? P1 Rh1 N1 N2 145.4(2) . . . . ? C1 N1 N2 C3 -0.6(4) . . . . ? Rh1 N1 N2 C3 168.1(2) . . . . ? C1 N1 N2 B1 179.3(3) . . . . ? Rh1 N1 N2 B1 -12.0(4) . . . . ? C16 Rh1 N3 C4 -133.7(9) . . . . ? N5 Rh1 N3 C4 -126.9(4) . . . . ? P1 Rh1 N3 C4 46.4(4) . . . . ? N1 Rh1 N3 C4 144.9(4) . . . . ? C16 Rh1 N3 N4 43.2(10) . . . . ? N5 Rh1 N3 N4 50.0(2) . . . . ? P1 Rh1 N3 N4 -136.8(2) . . . . ? N1 Rh1 N3 N4 -38.3(2) . . . . ? C4 N3 N4 C6 0.2(4) . . . . ? Rh1 N3 N4 C6 -177.6(2) . . . . ? C4 N3 N4 B1 168.0(3) . . . . ? Rh1 N3 N4 B1 -9.8(4) . . . . ? C16 Rh1 N5 C7 -52.8(3) . . . . ? N3 Rh1 N5 C7 128.2(3) . . . . ? P1 Rh1 N5 C7 35.3(10) . . . . ? N1 Rh1 N5 C7 -145.7(3) . . . . ? C16 Rh1 N5 N6 135.5(2) . . . . ? N3 Rh1 N5 N6 -43.5(2) . . . . ? P1 Rh1 N5 N6 -136.4(6) . . . . ? N1 Rh1 N5 N6 42.6(2) . . . . ? C7 N5 N6 C9 -0.6(4) . . . . ? Rh1 N5 N6 C9 173.1(2) . . . . ? C7 N5 N6 B1 -177.0(3) . . . . ? Rh1 N5 N6 B1 -3.3(4) . . . . ? C3 N2 B1 N4 128.3(4) . . . . ? N1 N2 B1 N4 -51.6(4) . . . . ? C3 N2 B1 N6 -112.3(4) . . . . ? N1 N2 B1 N6 67.8(4) . . . . ? C6 N4 B1 N2 -127.3(4) . . . . ? N3 N4 B1 N2 67.2(4) . . . . ? C6 N4 B1 N6 112.5(4) . . . . ? N3 N4 B1 N6 -53.1(4) . . . . ? C9 N6 B1 N2 125.5(4) . . . . ? N5 N6 B1 N2 -59.1(4) . . . . ? C9 N6 B1 N4 -113.9(4) . . . . ? N5 N6 B1 N4 61.6(4) . . . . ? N2 N1 C1 C2 0.3(4) . . . . ? Rh1 N1 C1 C2 -164.1(3) . . . . ? N2 N1 C1 C10 179.0(3) . . . . ? Rh1 N1 C1 C10 14.7(6) . . . . ? N1 C1 C2 C3 0.2(4) . . . . ? C10 C1 C2 C3 -178.5(4) . . . . ? N1 N2 C3 C2 0.8(4) . . . . ? B1 N2 C3 C2 -179.2(3) . . . . ? N1 N2 C3 C11 -177.7(3) . . . . ? B1 N2 C3 C11 2.4(6) . . . . ? C1 C2 C3 N2 -0.6(4) . . . . ? C1 C2 C3 C11 177.8(4) . . . . ? N4 N3 C4 C5 0.2(4) . . . . ? Rh1 N3 C4 C5 177.3(3) . . . . ? N4 N3 C4 C12 -177.4(3) . . . . ? Rh1 N3 C4 C12 -0.3(5) . . . . ? N3 C4 C5 C6 -0.5(4) . . . . ? C12 C4 C5 C6 177.0(3) . . . . ? N3 N4 C6 C5 -0.5(4) . . . . ? B1 N4 C6 C5 -167.2(3) . . . . ? N3 N4 C6 C13 179.2(3) . . . . ? B1 N4 C6 C13 12.4(5) . . . . ? C4 C5 C6 N4 0.6(4) . . . . ? C4 C5 C6 C13 -179.1(4) . . . . ? N6 N5 C7 C8 0.5(4) . . . . ? Rh1 N5 C7 C8 -171.9(2) . . . . ? N6 N5 C7 C14 -179.8(3) . . . . ? Rh1 N5 C7 C14 7.8(5) . . . . ? N5 C7 C8 C9 -0.2(4) . . . . ? C14 C7 C8 C9 -179.9(3) . . . . ? N5 N6 C9 C8 0.5(4) . . . . ? B1 N6 C9 C8 176.3(3) . . . . ? N5 N6 C9 C15 -176.4(3) . . . . ? B1 N6 C9 C15 -0.6(6) . . . . ? C7 C8 C9 N6 -0.2(4) . . . . ? C7 C8 C9 C15 176.5(3) . . . . ? N5 Rh1 C16 C17 114.8(3) . . . . ? N3 Rh1 C16 C17 121.5(9) . . . . ? P1 Rh1 C16 C17 -58.5(3) . . . . ? N1 Rh1 C16 C17 -157.5(3) . . . . ? N5 Rh1 C16 C21 -57.9(3) . . . . ? N3 Rh1 C16 C21 -51.2(11) . . . . ? P1 Rh1 C16 C21 128.8(3) . . . . ? N1 Rh1 C16 C21 29.8(3) . . . . ? C21 C16 C17 F1 179.5(3) . . . . ? Rh1 C16 C17 F1 6.5(5) . . . . ? C21 C16 C17 C18 -0.6(6) . . . . ? Rh1 C16 C17 C18 -173.6(3) . . . . ? F1 C17 C18 F2 -1.3(6) . . . . ? C16 C17 C18 F2 178.7(4) . . . . ? F1 C17 C18 C19 -179.6(4) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? F2 C18 C19 C20 -178.4(4) . . . . ? C17 C18 C19 C20 -0.3(7) . . . . ? C18 C19 C20 C21 0.1(7) . . . . ? C19 C20 C21 C16 -0.2(6) . . . . ? C17 C16 C21 C20 0.4(5) . . . . ? Rh1 C16 C21 C20 174.0(3) . . . . ? C27 C22 C23 C24 0.7(6) . . . . ? C22 C23 C24 C25 -0.2(6) . . . . ? C23 C24 C25 C26 0.0(6) . . . . ? C24 C25 C26 C27 -0.3(6) . . . . ? C23 C22 C27 C26 -1.0(6) . . . . ? C23 C22 C27 P1 -175.6(3) . . . . ? C25 C26 C27 C22 0.7(6) . . . . ? C25 C26 C27 P1 175.6(3) . . . . ? C29 P1 C27 C22 -146.9(3) . . . . ? C28 P1 C27 C22 107.3(3) . . . . ? Rh1 P1 C27 C22 -22.4(4) . . . . ? C29 P1 C27 C26 38.4(3) . . . . ? C28 P1 C27 C26 -67.3(3) . . . . ? Rh1 P1 C27 C26 162.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.058 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.151 #===end data_jontt17_cmpd9g _database_code_depnum_ccdc_archive 'CCDC 770122' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt17 _chemical_melting_point ? _chemical_formula_moiety 'C29 H37 B F2 N6 P Rh' _chemical_formula_sum 'C29 H37 B F2 N6 P Rh' _chemical_formula_weight 652.34 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' _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 10.1914(10) _cell_length_b 10.5164(11) _cell_length_c 15.794(2) _cell_angle_alpha 99.310(2) _cell_angle_beta 99.180(2) _cell_angle_gamma 115.370(2) _cell_volume 1458.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3746 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 37.79 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8424 _exptl_absorpt_correction_T_max 0.9474 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39002 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 36.32 _reflns_number_total 13918 _reflns_number_gt 11379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. The hydride ligand atom was found from the difference Fourier map, and its position and isotropic displacement parameter were refined independently from those of all other atoms. ; _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^)+(0.0545P)^2^+0.0974P] 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 13918 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.891398(13) 0.698725(13) 0.782054(8) 0.01644(4) Uani 1 1 d . . . H1 H 0.851(3) 0.657(3) 0.8634(15) 0.027(6) Uiso 1 1 d . . . P1 P 0.64023(5) 0.60187(5) 0.72407(3) 0.02106(8) Uani 1 1 d . . . N1 N 0.97632(15) 0.76945(15) 0.66605(9) 0.0184(2) Uani 1 1 d . . . N2 N 1.08196(15) 0.91306(14) 0.68552(9) 0.0170(2) Uani 1 1 d . . . N3 N 1.12058(15) 0.78638(14) 0.84881(9) 0.0161(2) Uani 1 1 d . . . N4 N 1.22078(15) 0.90720(14) 0.82955(9) 0.0166(2) Uani 1 1 d . . . N5 N 0.92888(16) 0.91721(15) 0.83613(9) 0.0189(2) Uani 1 1 d . . . N6 N 1.06039(16) 1.02958(15) 0.83206(9) 0.0185(2) Uani 1 1 d . . . B1 B 1.1646(2) 0.99864(19) 0.78220(11) 0.0176(3) Uani 1 1 d . . . H1B H 1.2521 1.0926 0.7840 0.021 Uiso 1 1 calc R . . C1 C 0.94730(19) 0.71698(19) 0.57794(11) 0.0208(3) Uani 1 1 d . . . C2 C 1.0325(2) 0.82718(19) 0.54101(11) 0.0220(3) Uani 1 1 d . . . H2 H 1.0322 0.8192 0.4802 0.026 Uiso 1 1 calc R . . C3 C 1.11719(19) 0.94976(18) 0.61068(10) 0.0195(3) Uani 1 1 d . . . C4 C 1.19980(18) 0.74056(17) 0.90049(10) 0.0181(3) Uani 1 1 d . . . C5 C 1.35272(19) 0.83177(19) 0.91296(11) 0.0212(3) Uani 1 1 d . . . H5 H 1.4340 0.8240 0.9463 0.025 Uiso 1 1 calc R . . C6 C 1.36265(18) 0.93582(18) 0.86717(10) 0.0188(3) Uani 1 1 d . . . C7 C 0.8764(2) 0.9760(2) 0.89538(11) 0.0216(3) Uani 1 1 d . . . C8 C 0.9722(2) 1.1239(2) 0.92895(11) 0.0248(3) Uani 1 1 d . . . H8 H 0.9599 1.1904 0.9712 0.030 Uiso 1 1 calc R . . C9 C 1.0891(2) 1.15529(18) 0.88873(11) 0.0213(3) Uani 1 1 d . . . C10 C 0.8413(2) 0.5625(2) 0.52999(12) 0.0285(4) Uani 1 1 d . . . H10A H 0.8150 0.5044 0.5731 0.043 Uiso 1 1 calc R . . H10B H 0.8891 0.5244 0.4910 0.043 Uiso 1 1 calc R . . H10C H 0.7500 0.5570 0.4944 0.043 Uiso 1 1 calc R . . C11 C 1.2306(2) 1.09772(19) 0.61084(12) 0.0252(3) Uani 1 1 d . . . H11A H 1.2100 1.1710 0.6443 0.038 Uiso 1 1 calc R . . H11B H 1.2252 1.1061 0.5496 0.038 Uiso 1 1 calc R . . H11C H 1.3312 1.1135 0.6387 0.038 Uiso 1 1 calc R . . C12 C 1.1276(2) 0.61171(18) 0.93655(11) 0.0224(3) Uani 1 1 d . . . H12A H 1.0266 0.5956 0.9395 0.034 Uiso 1 1 calc R . . H12B H 1.1882 0.6297 0.9962 0.034 Uiso 1 1 calc R . . H12C H 1.1209 0.5253 0.8976 0.034 Uiso 1 1 calc R . . C13 C 1.49674(19) 1.0601(2) 0.85632(12) 0.0257(3) Uani 1 1 d . . . H13A H 1.4919 1.1509 0.8760 0.039 Uiso 1 1 calc R . . H13B H 1.4984 1.0447 0.7937 0.039 Uiso 1 1 calc R . . H13C H 1.5882 1.0663 0.8922 0.039 Uiso 1 1 calc R . . C14 C 0.7367(2) 0.8881(2) 0.92059(12) 0.0268(3) Uani 1 1 d . . . H14A H 0.7400 0.8023 0.9353 0.040 Uiso 1 1 calc R . . H14B H 0.6494 0.8569 0.8708 0.040 Uiso 1 1 calc R . . H14C H 0.7288 0.9473 0.9723 0.040 Uiso 1 1 calc R . . C15 C 1.2262(2) 1.29594(19) 0.90212(13) 0.0280(4) Uani 1 1 d . . . H15A H 1.3158 1.2831 0.9187 0.042 Uiso 1 1 calc R . . H15B H 1.2282 1.3700 0.9495 0.042 Uiso 1 1 calc R . . H15C H 1.2248 1.3272 0.8469 0.042 Uiso 1 1 calc R . . C16 C 0.89172(18) 0.50408(18) 0.74753(11) 0.0196(3) Uani 1 1 d . . . C17 C 0.8048(2) 0.3749(2) 0.76769(13) 0.0256(3) Uani 1 1 d . . . F1 F 0.69167(14) 0.36633(14) 0.80682(10) 0.0385(3) Uani 1 1 d . . . C18 C 0.8228(2) 0.2509(2) 0.75327(14) 0.0299(4) Uani 1 1 d . . . H18 H 0.7569 0.1662 0.7680 0.036 Uiso 1 1 calc R . . C19 C 0.9380(2) 0.25115(19) 0.71716(13) 0.0267(3) Uani 1 1 d . . . H19 H 0.9541 0.1681 0.7065 0.032 Uiso 1 1 calc R . . C20 C 1.02790(19) 0.37790(18) 0.69747(11) 0.0207(3) Uani 1 1 d . . . F2 F 1.14605(12) 0.38356(12) 0.66464(7) 0.0257(2) Uani 1 1 d . . . C21 C 1.00777(18) 0.50039(17) 0.71099(10) 0.0190(3) Uani 1 1 d . . . H21 H 1.0735 0.5841 0.6953 0.023 Uiso 1 1 calc R . . C22 C 0.4348(2) 0.7095(2) 0.67929(14) 0.0288(4) Uani 1 1 d . . . H22 H 0.3722 0.6424 0.7071 0.035 Uiso 1 1 calc R . . C23 C 0.3833(2) 0.7924(2) 0.63848(15) 0.0314(4) Uani 1 1 d . . . H23 H 0.2858 0.7819 0.6383 0.038 Uiso 1 1 calc R . . C24 C 0.4742(2) 0.8909(2) 0.59787(12) 0.0278(3) Uani 1 1 d . . . H24 H 0.4382 0.9462 0.5685 0.033 Uiso 1 1 calc R . . C25 C 0.6164(2) 0.9082(2) 0.60018(14) 0.0304(4) Uani 1 1 d . . . H25 H 0.6795 0.9773 0.5736 0.036 Uiso 1 1 calc R . . C26 C 0.6685(2) 0.8251(2) 0.64128(13) 0.0276(4) Uani 1 1 d . . . H26 H 0.7671 0.8382 0.6428 0.033 Uiso 1 1 calc R . . C27 C 0.57710(19) 0.72303(18) 0.68024(11) 0.0211(3) Uani 1 1 d . . . C28 C 0.5190(2) 0.5343(2) 0.79765(15) 0.0319(4) Uani 1 1 d . . . H28A H 0.4157 0.4693 0.7621 0.048 Uiso 1 1 calc R . . H28B H 0.5212 0.6168 0.8382 0.048 Uiso 1 1 calc R . . H28C H 0.5550 0.4808 0.8321 0.048 Uiso 1 1 calc R . . C29 C 0.5485(2) 0.4429(2) 0.62867(15) 0.0308(4) Uani 1 1 d . . . H29A H 0.4393 0.4045 0.6166 0.046 Uiso 1 1 calc R . . H29B H 0.5753 0.3677 0.6416 0.046 Uiso 1 1 calc R . . H29C H 0.5817 0.4711 0.5766 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01440(6) 0.01828(6) 0.01961(6) 0.00807(4) 0.00562(4) 0.00872(4) P1 0.01512(18) 0.02118(19) 0.0286(2) 0.01139(16) 0.00590(15) 0.00817(15) N1 0.0174(6) 0.0193(6) 0.0187(6) 0.0059(5) 0.0037(5) 0.0089(5) N2 0.0182(6) 0.0176(6) 0.0182(5) 0.0067(4) 0.0061(4) 0.0098(5) N3 0.0163(6) 0.0152(5) 0.0187(5) 0.0059(4) 0.0042(4) 0.0086(5) N4 0.0163(6) 0.0166(5) 0.0188(5) 0.0058(4) 0.0055(4) 0.0084(5) N5 0.0193(6) 0.0230(6) 0.0205(6) 0.0091(5) 0.0078(5) 0.0131(5) N6 0.0209(6) 0.0190(6) 0.0206(6) 0.0072(5) 0.0073(5) 0.0122(5) B1 0.0189(7) 0.0176(7) 0.0190(7) 0.0056(6) 0.0061(6) 0.0101(6) C1 0.0190(7) 0.0247(7) 0.0188(6) 0.0054(6) 0.0028(5) 0.0110(6) C2 0.0246(8) 0.0251(8) 0.0180(6) 0.0070(6) 0.0064(6) 0.0124(6) C3 0.0224(7) 0.0236(7) 0.0192(6) 0.0096(5) 0.0081(5) 0.0144(6) C4 0.0207(7) 0.0200(7) 0.0171(6) 0.0053(5) 0.0052(5) 0.0122(6) C5 0.0197(7) 0.0254(7) 0.0214(7) 0.0075(6) 0.0040(5) 0.0131(6) C6 0.0174(7) 0.0205(7) 0.0189(6) 0.0049(5) 0.0046(5) 0.0092(6) C7 0.0239(7) 0.0303(8) 0.0203(7) 0.0097(6) 0.0078(6) 0.0195(7) C8 0.0323(9) 0.0301(8) 0.0228(7) 0.0073(6) 0.0099(6) 0.0230(8) C9 0.0283(8) 0.0218(7) 0.0203(7) 0.0065(5) 0.0062(6) 0.0171(6) C10 0.0272(9) 0.0271(8) 0.0214(7) 0.0028(6) 0.0007(6) 0.0071(7) C11 0.0308(9) 0.0227(8) 0.0265(8) 0.0115(6) 0.0125(7) 0.0130(7) C12 0.0260(8) 0.0217(7) 0.0231(7) 0.0105(6) 0.0067(6) 0.0126(6) C13 0.0169(7) 0.0286(8) 0.0280(8) 0.0100(7) 0.0047(6) 0.0068(6) C14 0.0250(8) 0.0389(10) 0.0256(8) 0.0117(7) 0.0114(6) 0.0200(8) C15 0.0367(10) 0.0208(8) 0.0293(8) 0.0055(6) 0.0094(7) 0.0160(7) C16 0.0183(7) 0.0193(7) 0.0236(7) 0.0096(5) 0.0058(5) 0.0093(6) C17 0.0221(8) 0.0238(8) 0.0350(9) 0.0142(7) 0.0118(7) 0.0106(7) F1 0.0338(6) 0.0326(6) 0.0657(9) 0.0289(6) 0.0310(6) 0.0186(5) C18 0.0297(9) 0.0216(8) 0.0420(10) 0.0163(7) 0.0122(8) 0.0113(7) C19 0.0301(9) 0.0199(7) 0.0326(9) 0.0090(6) 0.0070(7) 0.0135(7) C20 0.0222(7) 0.0202(7) 0.0202(7) 0.0043(5) 0.0037(6) 0.0111(6) F2 0.0271(5) 0.0238(5) 0.0302(5) 0.0053(4) 0.0093(4) 0.0152(4) C21 0.0191(7) 0.0175(6) 0.0203(6) 0.0054(5) 0.0038(5) 0.0086(6) C22 0.0164(7) 0.0279(9) 0.0425(10) 0.0147(8) 0.0054(7) 0.0095(7) C23 0.0216(8) 0.0327(9) 0.0439(11) 0.0121(8) 0.0049(7) 0.0167(8) C24 0.0322(9) 0.0312(9) 0.0280(8) 0.0097(7) 0.0053(7) 0.0221(8) C25 0.0345(10) 0.0359(10) 0.0351(9) 0.0196(8) 0.0153(8) 0.0234(8) C26 0.0248(8) 0.0343(9) 0.0349(9) 0.0188(8) 0.0125(7) 0.0188(8) C27 0.0175(7) 0.0220(7) 0.0232(7) 0.0064(6) 0.0027(5) 0.0094(6) C28 0.0207(8) 0.0383(10) 0.0447(11) 0.0246(9) 0.0134(8) 0.0144(8) C29 0.0208(8) 0.0208(8) 0.0440(11) 0.0062(7) 0.0021(7) 0.0064(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 Rh1 C16 2.0329(16) . ? Rh1 N3 2.1146(13) . ? Rh1 N5 2.1595(14) . ? Rh1 N1 2.2482(13) . ? Rh1 P1 2.2681(5) . ? Rh1 H1 1.49(2) . ? P1 C29 1.826(2) . ? P1 C28 1.8320(19) . ? P1 C27 1.8337(17) . ? N1 C1 1.345(2) . ? N1 N2 1.3730(19) . ? N2 C3 1.3563(19) . ? N2 B1 1.532(2) . ? N3 C4 1.342(2) . ? N3 N4 1.3646(18) . ? N4 C6 1.353(2) . ? N4 B1 1.542(2) . ? N5 C7 1.342(2) . ? N5 N6 1.3754(19) . ? N6 C9 1.355(2) . ? N6 B1 1.528(2) . ? B1 H1B 1.0000 . ? C1 C2 1.398(2) . ? C1 C10 1.489(3) . ? C2 C3 1.379(2) . ? C2 H2 0.9500 . ? C3 C11 1.488(2) . ? C4 C5 1.396(2) . ? C4 C12 1.494(2) . ? C5 C6 1.384(2) . ? C5 H5 0.9500 . ? C6 C13 1.490(2) . ? C7 C8 1.386(3) . ? C7 C14 1.487(2) . ? C8 C9 1.379(2) . ? C8 H8 0.9500 . ? C9 C15 1.489(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.390(2) . ? C16 C21 1.408(2) . ? C17 F1 1.369(2) . ? C17 C18 1.382(3) . ? C18 C19 1.383(3) . ? C18 H18 0.9500 . ? C19 C20 1.375(2) . ? C19 H19 0.9500 . ? C20 F2 1.368(2) . ? C20 C21 1.378(2) . ? C21 H21 0.9500 . ? C22 C23 1.385(3) . ? C22 C27 1.392(2) . ? C22 H22 0.9500 . ? C23 C24 1.387(3) . ? C23 H23 0.9500 . ? C24 C25 1.375(3) . ? C24 H24 0.9500 . ? C25 C26 1.392(3) . ? C25 H25 0.9500 . ? C26 C27 1.392(2) . ? C26 H26 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Rh1 N3 86.98(6) . . ? C16 Rh1 N5 169.58(6) . . ? N3 Rh1 N5 82.97(5) . . ? C16 Rh1 N1 92.85(6) . . ? N3 Rh1 N1 85.50(5) . . ? N5 Rh1 N1 89.14(5) . . ? C16 Rh1 P1 93.52(5) . . ? N3 Rh1 P1 174.10(4) . . ? N5 Rh1 P1 96.19(4) . . ? N1 Rh1 P1 100.34(4) . . ? C16 Rh1 H1 86.3(9) . . ? N3 Rh1 H1 88.7(9) . . ? N5 Rh1 H1 90.7(9) . . ? N1 Rh1 H1 174.2(9) . . ? P1 Rh1 H1 85.5(9) . . ? C29 P1 C28 99.65(10) . . ? C29 P1 C27 99.82(9) . . ? C28 P1 C27 103.28(8) . . ? C29 P1 Rh1 118.64(7) . . ? C28 P1 Rh1 116.98(7) . . ? C27 P1 Rh1 115.61(6) . . ? C1 N1 N2 106.13(13) . . ? C1 N1 Rh1 139.28(12) . . ? N2 N1 Rh1 114.32(9) . . ? C3 N2 N1 110.45(13) . . ? C3 N2 B1 128.19(14) . . ? N1 N2 B1 120.08(12) . . ? C4 N3 N4 107.49(13) . . ? C4 N3 Rh1 134.42(11) . . ? N4 N3 Rh1 117.47(9) . . ? C6 N4 N3 109.80(12) . . ? C6 N4 B1 129.73(14) . . ? N3 N4 B1 119.96(13) . . ? C7 N5 N6 106.01(14) . . ? C7 N5 Rh1 134.28(12) . . ? N6 N5 Rh1 116.85(9) . . ? C9 N6 N5 110.20(13) . . ? C9 N6 B1 128.34(15) . . ? N5 N6 B1 120.46(13) . . ? N6 B1 N2 111.30(13) . . ? N6 B1 N4 107.57(12) . . ? N2 B1 N4 109.12(13) . . ? N6 B1 H1B 109.6 . . ? N2 B1 H1B 109.6 . . ? N4 B1 H1B 109.6 . . ? N1 C1 C2 109.95(15) . . ? N1 C1 C10 123.30(15) . . ? C2 C1 C10 126.74(15) . . ? C3 C2 C1 106.15(14) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? N2 C3 C2 107.32(14) . . ? N2 C3 C11 122.94(15) . . ? C2 C3 C11 129.73(15) . . ? N3 C4 C5 108.92(14) . . ? N3 C4 C12 122.84(15) . . ? C5 C4 C12 128.25(15) . . ? C6 C5 C4 106.44(14) . . ? C6 C5 H5 126.8 . . ? C4 C5 H5 126.8 . . ? N4 C6 C5 107.34(14) . . ? N4 C6 C13 122.21(14) . . ? C5 C6 C13 130.45(15) . . ? N5 C7 C8 110.25(15) . . ? N5 C7 C14 122.60(16) . . ? C8 C7 C14 127.12(15) . . ? C9 C8 C7 106.34(14) . . ? C9 C8 H8 126.8 . . ? C7 C8 H8 126.8 . . ? N6 C9 C8 107.17(15) . . ? N6 C9 C15 123.28(15) . . ? C8 C9 C15 129.53(16) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 113.23(15) . . ? C17 C16 Rh1 127.97(13) . . ? C21 C16 Rh1 118.00(11) . . ? F1 C17 C18 115.20(15) . . ? F1 C17 C16 118.97(15) . . ? C18 C17 C16 125.82(17) . . ? C17 C18 C19 119.34(17) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 116.55(16) . . ? C20 C19 H19 121.7 . . ? C18 C19 H19 121.7 . . ? F2 C20 C19 118.02(15) . . ? F2 C20 C21 118.27(15) . . ? C19 C20 C21 123.69(16) . . ? C20 C21 C16 121.35(15) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? C23 C22 C27 121.05(18) . . ? C23 C22 H22 119.5 . . ? C27 C22 H22 119.5 . . ? C22 C23 C24 119.85(17) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 119.84(17) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.35(18) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 120.50(17) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 118.38(16) . . ? C26 C27 P1 119.81(13) . . ? C22 C27 P1 121.66(13) . . ? P1 C28 H28A 109.5 . . ? P1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? P1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P1 C29 H29A 109.5 . . ? P1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Rh1 P1 C29 -30.37(9) . . . . ? N3 Rh1 P1 C29 -125.1(4) . . . . ? N5 Rh1 P1 C29 153.43(9) . . . . ? N1 Rh1 P1 C29 63.18(9) . . . . ? C16 Rh1 P1 C28 89.12(9) . . . . ? N3 Rh1 P1 C28 -5.6(4) . . . . ? N5 Rh1 P1 C28 -87.08(9) . . . . ? N1 Rh1 P1 C28 -177.33(9) . . . . ? C16 Rh1 P1 C27 -148.89(8) . . . . ? N3 Rh1 P1 C27 116.4(3) . . . . ? N5 Rh1 P1 C27 34.92(7) . . . . ? N1 Rh1 P1 C27 -55.34(7) . . . . ? C16 Rh1 N1 C1 47.77(17) . . . . ? N3 Rh1 N1 C1 134.51(17) . . . . ? N5 Rh1 N1 C1 -142.47(17) . . . . ? P1 Rh1 N1 C1 -46.34(17) . . . . ? C16 Rh1 N1 N2 -139.36(11) . . . . ? N3 Rh1 N1 N2 -52.61(10) . . . . ? N5 Rh1 N1 N2 30.40(10) . . . . ? P1 Rh1 N1 N2 126.54(10) . . . . ? C1 N1 N2 C3 0.52(17) . . . . ? Rh1 N1 N2 C3 -174.65(10) . . . . ? C1 N1 N2 B1 -167.59(13) . . . . ? Rh1 N1 N2 B1 17.24(16) . . . . ? C16 Rh1 N3 C4 -41.83(15) . . . . ? N5 Rh1 N3 C4 135.38(15) . . . . ? N1 Rh1 N3 C4 -134.93(15) . . . . ? P1 Rh1 N3 C4 53.2(4) . . . . ? C16 Rh1 N3 N4 127.75(11) . . . . ? N5 Rh1 N3 N4 -55.03(10) . . . . ? N1 Rh1 N3 N4 34.65(10) . . . . ? P1 Rh1 N3 N4 -137.2(3) . . . . ? C4 N3 N4 C6 1.36(16) . . . . ? Rh1 N3 N4 C6 -170.86(10) . . . . ? C4 N3 N4 B1 -171.24(13) . . . . ? Rh1 N3 N4 B1 16.54(17) . . . . ? C16 Rh1 N5 C7 -99.3(3) . . . . ? N3 Rh1 N5 C7 -114.83(16) . . . . ? N1 Rh1 N5 C7 159.60(16) . . . . ? P1 Rh1 N5 C7 59.29(16) . . . . ? C16 Rh1 N5 N6 58.5(3) . . . . ? N3 Rh1 N5 N6 42.93(11) . . . . ? N1 Rh1 N5 N6 -42.65(11) . . . . ? P1 Rh1 N5 N6 -142.95(10) . . . . ? C7 N5 N6 C9 0.65(17) . . . . ? Rh1 N5 N6 C9 -162.97(10) . . . . ? C7 N5 N6 B1 170.14(14) . . . . ? Rh1 N5 N6 B1 6.52(18) . . . . ? C9 N6 B1 N2 -136.30(16) . . . . ? N5 N6 B1 N2 56.31(18) . . . . ? C9 N6 B1 N4 104.22(18) . . . . ? N5 N6 B1 N4 -63.18(18) . . . . ? C3 N2 B1 N6 123.07(16) . . . . ? N1 N2 B1 N6 -71.15(17) . . . . ? C3 N2 B1 N4 -118.38(16) . . . . ? N1 N2 B1 N4 47.40(18) . . . . ? C6 N4 B1 N6 -121.28(16) . . . . ? N3 N4 B1 N6 49.66(18) . . . . ? C6 N4 B1 N2 117.86(17) . . . . ? N3 N4 B1 N2 -71.20(16) . . . . ? N2 N1 C1 C2 -0.82(18) . . . . ? Rh1 N1 C1 C2 172.42(13) . . . . ? N2 N1 C1 C10 178.04(16) . . . . ? Rh1 N1 C1 C10 -8.7(3) . . . . ? N1 C1 C2 C3 0.82(19) . . . . ? C10 C1 C2 C3 -177.99(17) . . . . ? N1 N2 C3 C2 -0.02(18) . . . . ? B1 N2 C3 C2 166.87(15) . . . . ? N1 N2 C3 C11 -178.90(15) . . . . ? B1 N2 C3 C11 -12.0(2) . . . . ? C1 C2 C3 N2 -0.47(18) . . . . ? C1 C2 C3 C11 178.31(17) . . . . ? N4 N3 C4 C5 -1.16(17) . . . . ? Rh1 N3 C4 C5 169.16(11) . . . . ? N4 N3 C4 C12 178.71(14) . . . . ? Rh1 N3 C4 C12 -11.0(2) . . . . ? N3 C4 C5 C6 0.55(18) . . . . ? C12 C4 C5 C6 -179.31(15) . . . . ? N3 N4 C6 C5 -1.01(17) . . . . ? B1 N4 C6 C5 170.65(15) . . . . ? N3 N4 C6 C13 178.83(14) . . . . ? B1 N4 C6 C13 -9.5(2) . . . . ? C4 C5 C6 N4 0.28(18) . . . . ? C4 C5 C6 C13 -179.54(16) . . . . ? N6 N5 C7 C8 0.10(18) . . . . ? Rh1 N5 C7 C8 159.52(13) . . . . ? N6 N5 C7 C14 -178.27(15) . . . . ? Rh1 N5 C7 C14 -18.8(2) . . . . ? N5 C7 C8 C9 -0.78(19) . . . . ? C14 C7 C8 C9 177.49(16) . . . . ? N5 N6 C9 C8 -1.14(18) . . . . ? B1 N6 C9 C8 -169.57(15) . . . . ? N5 N6 C9 C15 177.83(15) . . . . ? B1 N6 C9 C15 9.4(3) . . . . ? C7 C8 C9 N6 1.15(19) . . . . ? C7 C8 C9 C15 -177.73(17) . . . . ? N3 Rh1 C16 C17 120.01(16) . . . . ? N5 Rh1 C16 C17 104.5(3) . . . . ? N1 Rh1 C16 C17 -154.65(16) . . . . ? P1 Rh1 C16 C17 -54.10(16) . . . . ? N3 Rh1 C16 C21 -48.93(13) . . . . ? N5 Rh1 C16 C21 -64.4(3) . . . . ? N1 Rh1 C16 C21 36.41(13) . . . . ? P1 Rh1 C16 C21 136.96(12) . . . . ? C21 C16 C17 F1 177.52(16) . . . . ? Rh1 C16 C17 F1 8.1(3) . . . . ? C21 C16 C17 C18 -1.3(3) . . . . ? Rh1 C16 C17 C18 -170.64(16) . . . . ? F1 C17 C18 C19 -177.55(18) . . . . ? C16 C17 C18 C19 1.3(3) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? C18 C19 C20 F2 177.71(16) . . . . ? C18 C19 C20 C21 -0.6(3) . . . . ? F2 C20 C21 C16 -177.74(14) . . . . ? C19 C20 C21 C16 0.6(3) . . . . ? C17 C16 C21 C20 0.3(2) . . . . ? Rh1 C16 C21 C20 170.84(12) . . . . ? C27 C22 C23 C24 -0.1(3) . . . . ? C22 C23 C24 C25 -1.6(3) . . . . ? C23 C24 C25 C26 1.5(3) . . . . ? C24 C25 C26 C27 0.3(3) . . . . ? C25 C26 C27 C22 -1.9(3) . . . . ? C25 C26 C27 P1 173.84(16) . . . . ? C23 C22 C27 C26 1.8(3) . . . . ? C23 C22 C27 P1 -173.83(16) . . . . ? C29 P1 C27 C26 -95.23(16) . . . . ? C28 P1 C27 C26 162.31(16) . . . . ? Rh1 P1 C27 C26 33.26(17) . . . . ? C29 P1 C27 C22 80.35(17) . . . . ? C28 P1 C27 C22 -22.11(18) . . . . ? Rh1 P1 C27 C22 -151.16(14) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 36.32 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.512 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.112 #===end data_jontt12_cmpdTp'RhCl2(PPhMe2) _database_code_depnum_ccdc_archive 'CCDC 770123' _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R (1999). SIR97, J. Appl. Cryst. 32, 115-119. Bruker (2007). SAINT V7.46A, Bruker AXS, Inc., Madison, WI, USA. Bruker (2007). APEX2 V2.2-0, Bruker AXS, Inc., Madison, WI, USA. Sheldrick, G. M. (2007). SADABS V2007/4, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta. Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common jontt12 _chemical_melting_point ? _chemical_formula_moiety 'C23 H33 B Cl2 N6 P Rh' _chemical_formula_sum 'C23 H33 B Cl2 N6 P Rh' _chemical_formula_weight 609.14 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' 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 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3576(19) _cell_length_b 13.122(2) _cell_length_c 18.725(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.373(3) _cell_angle_gamma 90.00 _cell_volume 2690.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 4026 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 33.23 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8524 _exptl_absorpt_correction_T_max 0.9643 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61181 _diffrn_reflns_av_R_equivalents 0.1263 _diffrn_reflns_av_sigmaI/netI 0.1086 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 36.32 _reflns_number_total 12968 _reflns_number_gt 7915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0344P)^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 12968 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 0.160952(18) 0.014453(15) 0.831671(11) 0.01171(4) Uani 1 1 d . . . Cl1 Cl 0.34679(6) 0.00103(5) 0.80017(4) 0.01842(13) Uani 1 1 d . . . Cl2 Cl 0.26557(6) 0.11845(5) 0.92921(4) 0.01880(13) Uani 1 1 d . . . P1 P 0.10409(6) 0.15858(5) 0.76313(4) 0.01462(13) Uani 1 1 d . . . N1 N 0.00477(19) 0.01402(16) 0.87075(11) 0.0141(4) Uani 1 1 d . . . N2 N -0.0687(2) -0.07099(16) 0.85042(12) 0.0145(4) Uani 1 1 d . . . N3 N 0.1996(2) -0.12312(16) 0.89483(12) 0.0137(4) Uani 1 1 d . . . N4 N 0.1069(2) -0.19325(15) 0.88015(12) 0.0132(4) Uani 1 1 d . . . N5 N 0.0839(2) -0.07727(16) 0.74011(12) 0.0138(4) Uani 1 1 d . . . N6 N 0.0037(2) -0.15136(16) 0.74903(12) 0.0140(4) Uani 1 1 d . . . B1 B -0.0167(3) -0.1680(2) 0.82514(16) 0.0148(5) Uani 1 1 d . . . H1B H -0.0749 -0.2258 0.8231 0.018 Uiso 1 1 calc R . . C1 C -0.0504(2) 0.0730(2) 0.91143(14) 0.0164(5) Uani 1 1 d . . . C2 C -0.1596(3) 0.0276(2) 0.91465(16) 0.0203(5) Uani 1 1 d . . . H2A H -0.2166 0.0536 0.9391 0.024 Uiso 1 1 calc R . . C3 C -0.1690(2) -0.0621(2) 0.87569(15) 0.0188(5) Uani 1 1 d . . . C4 C 0.2932(2) -0.1639(2) 0.94593(14) 0.0157(5) Uani 1 1 d . . . C5 C 0.2608(2) -0.26181(19) 0.96359(14) 0.0162(5) Uani 1 1 d . . . H5A H 0.3101 -0.3079 0.9980 0.019 Uiso 1 1 calc R . . C6 C 0.1433(2) -0.27802(19) 0.92119(14) 0.0150(5) Uani 1 1 d . . . C7 C 0.0920(2) -0.0850(2) 0.66973(14) 0.0158(5) Uani 1 1 d . . . C8 C 0.0173(3) -0.1636(2) 0.63489(15) 0.0191(5) Uani 1 1 d . . . H8A H 0.0057 -0.1852 0.5851 0.023 Uiso 1 1 calc R . . C9 C -0.0369(3) -0.2043(2) 0.68572(15) 0.0181(5) Uani 1 1 d . . . C10 C -0.0029(3) 0.1685(2) 0.95245(15) 0.0212(6) Uani 1 1 d . . . H10A H 0.0776 0.1844 0.9454 0.032 Uiso 1 1 calc R . . H10B H 0.0042 0.1589 1.0053 0.032 Uiso 1 1 calc R . . H10C H -0.0592 0.2248 0.9335 0.032 Uiso 1 1 calc R . . C11 C -0.2680(3) -0.1398(2) 0.86225(19) 0.0279(7) Uani 1 1 d . . . H11A H -0.2936 -0.1567 0.8094 0.042 Uiso 1 1 calc R . . H11B H -0.3378 -0.1125 0.8776 0.042 Uiso 1 1 calc R . . H11C H -0.2378 -0.2014 0.8909 0.042 Uiso 1 1 calc R . . C12 C 0.4106(2) -0.1086(2) 0.97680(15) 0.0193(5) Uani 1 1 d . . . H12A H 0.4310 -0.0687 0.9375 0.029 Uiso 1 1 calc R . . H12B H 0.4758 -0.1579 0.9967 0.029 Uiso 1 1 calc R . . H12C H 0.4019 -0.0628 1.0165 0.029 Uiso 1 1 calc R . . C13 C 0.0644(3) -0.3697(2) 0.91675(17) 0.0229(6) Uani 1 1 d . . . H13A H -0.0119 -0.3504 0.9282 0.034 Uiso 1 1 calc R . . H13B H 0.1071 -0.4208 0.9525 0.034 Uiso 1 1 calc R . . H13C H 0.0462 -0.3983 0.8666 0.034 Uiso 1 1 calc R . . C14 C 0.1724(3) -0.0234(2) 0.63494(15) 0.0193(5) Uani 1 1 d . . . H14A H 0.1998 0.0377 0.6648 0.029 Uiso 1 1 calc R . . H14B H 0.1267 -0.0033 0.5848 0.029 Uiso 1 1 calc R . . H14C H 0.2435 -0.0641 0.6323 0.029 Uiso 1 1 calc R . . C15 C -0.1216(3) -0.2935(2) 0.67777(17) 0.0292(7) Uani 1 1 d . . . H15A H -0.1875 -0.2775 0.7008 0.044 Uiso 1 1 calc R . . H15B H -0.0763 -0.3531 0.7022 0.044 Uiso 1 1 calc R . . H15C H -0.1565 -0.3084 0.6251 0.044 Uiso 1 1 calc R . . C16 C -0.1242(3) 0.0822(2) 0.69002(15) 0.0193(5) Uani 1 1 d . . . H16A H -0.1256 0.0573 0.7374 0.023 Uiso 1 1 calc R . . C17 C -0.2224(3) 0.0641(2) 0.62962(17) 0.0241(6) Uani 1 1 d . . . H17A H -0.2905 0.0263 0.6356 0.029 Uiso 1 1 calc R . . C18 C -0.2219(3) 0.1009(2) 0.56037(16) 0.0247(6) Uani 1 1 d . . . H18A H -0.2890 0.0877 0.5188 0.030 Uiso 1 1 calc R . . C19 C -0.1230(3) 0.1570(2) 0.55193(16) 0.0236(6) Uani 1 1 d . . . H19A H -0.1231 0.1838 0.5048 0.028 Uiso 1 1 calc R . . C20 C -0.0239(3) 0.1738(2) 0.61249(15) 0.0197(5) Uani 1 1 d . . . H20A H 0.0443 0.2113 0.6064 0.024 Uiso 1 1 calc R . . C21 C -0.0234(2) 0.13642(19) 0.68200(14) 0.0157(5) Uani 1 1 d . . . C22 C 0.0455(3) 0.2639(2) 0.80633(16) 0.0223(6) Uani 1 1 d . . . H22A H 0.0341 0.3235 0.7737 0.034 Uiso 1 1 calc R . . H22B H 0.1036 0.2805 0.8537 0.034 Uiso 1 1 calc R . . H22C H -0.0330 0.2446 0.8149 0.034 Uiso 1 1 calc R . . C23 C 0.2244(3) 0.2214(2) 0.73430(16) 0.0201(5) Uani 1 1 d . . . H23A H 0.1937 0.2856 0.7096 0.030 Uiso 1 1 calc R . . H23B H 0.2525 0.1774 0.6999 0.030 Uiso 1 1 calc R . . H23C H 0.2925 0.2356 0.7777 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01232(8) 0.01122(7) 0.01162(8) -0.00080(8) 0.00325(6) -0.00078(8) Cl1 0.0155(3) 0.0192(3) 0.0224(3) -0.0007(2) 0.0081(2) -0.0009(2) Cl2 0.0183(3) 0.0181(3) 0.0180(3) -0.0051(2) 0.0012(2) -0.0020(2) P1 0.0163(3) 0.0128(3) 0.0148(3) 0.0004(2) 0.0043(3) -0.0011(2) N1 0.0156(10) 0.0124(9) 0.0145(9) 0.0005(8) 0.0043(8) -0.0012(8) N2 0.0135(10) 0.0135(10) 0.0166(10) 0.0022(8) 0.0042(8) 0.0004(8) N3 0.0131(10) 0.0143(10) 0.0131(10) -0.0010(8) 0.0024(8) -0.0016(8) N4 0.0142(10) 0.0119(9) 0.0145(10) -0.0005(8) 0.0053(8) -0.0010(8) N5 0.0151(10) 0.0130(9) 0.0135(10) -0.0006(8) 0.0040(8) -0.0015(8) N6 0.0141(10) 0.0138(10) 0.0134(10) -0.0013(8) 0.0022(8) -0.0025(8) B1 0.0137(14) 0.0139(12) 0.0170(13) 0.0015(10) 0.0042(11) -0.0026(10) C1 0.0177(13) 0.0171(12) 0.0148(12) 0.0019(9) 0.0051(10) 0.0049(10) C2 0.0189(13) 0.0218(14) 0.0238(13) 0.0045(11) 0.0121(11) 0.0052(11) C3 0.0147(13) 0.0218(13) 0.0211(13) 0.0071(10) 0.0071(10) 0.0029(10) C4 0.0169(13) 0.0155(11) 0.0143(11) -0.0006(9) 0.0036(10) 0.0008(9) C5 0.0172(13) 0.0158(12) 0.0155(12) 0.0011(9) 0.0039(10) 0.0034(9) C6 0.0166(12) 0.0134(11) 0.0154(11) 0.0006(9) 0.0049(10) 0.0008(9) C7 0.0163(13) 0.0171(12) 0.0139(11) -0.0008(9) 0.0041(10) 0.0019(9) C8 0.0197(14) 0.0212(13) 0.0143(12) -0.0054(10) 0.0010(10) 0.0010(10) C9 0.0188(13) 0.0179(12) 0.0154(12) -0.0022(10) 0.0004(10) -0.0023(10) C10 0.0279(15) 0.0198(13) 0.0170(13) -0.0026(10) 0.0077(11) 0.0045(11) C11 0.0178(14) 0.0262(15) 0.0433(19) 0.0041(14) 0.0145(13) -0.0005(12) C12 0.0173(13) 0.0202(13) 0.0184(13) -0.0019(10) 0.0011(10) -0.0003(10) C13 0.0214(14) 0.0147(12) 0.0305(15) 0.0061(11) 0.0033(12) -0.0009(10) C14 0.0227(13) 0.0189(12) 0.0174(12) -0.0009(10) 0.0075(10) -0.0007(11) C15 0.0313(17) 0.0305(16) 0.0260(16) -0.0078(13) 0.0076(13) -0.0146(13) C16 0.0201(14) 0.0178(12) 0.0192(13) 0.0028(10) 0.0041(11) 0.0004(10) C17 0.0183(14) 0.0219(14) 0.0292(16) 0.0009(12) 0.0012(12) -0.0022(11) C18 0.0207(15) 0.0272(15) 0.0210(14) -0.0043(11) -0.0035(11) 0.0036(12) C19 0.0260(16) 0.0293(15) 0.0156(13) 0.0014(11) 0.0054(11) 0.0064(12) C20 0.0187(14) 0.0206(13) 0.0206(13) 0.0018(10) 0.0064(11) 0.0025(10) C21 0.0162(12) 0.0144(11) 0.0159(12) 0.0007(9) 0.0035(10) 0.0028(9) C22 0.0274(16) 0.0170(13) 0.0241(14) -0.0004(11) 0.0095(12) 0.0043(11) C23 0.0171(13) 0.0207(13) 0.0229(14) 0.0030(11) 0.0057(11) -0.0040(10) _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 N5 2.088(2) . ? Rh1 N1 2.091(2) . ? Rh1 N3 2.139(2) . ? Rh1 P1 2.2807(8) . ? Rh1 Cl2 2.3365(7) . ? Rh1 Cl1 2.3439(7) . ? P1 C23 1.797(3) . ? P1 C22 1.815(3) . ? P1 C21 1.822(3) . ? N1 C1 1.351(3) . ? N1 N2 1.384(3) . ? N2 C3 1.350(3) . ? N2 B1 1.530(4) . ? N3 C4 1.339(3) . ? N3 N4 1.370(3) . ? N4 C6 1.353(3) . ? N4 B1 1.541(4) . ? N5 C7 1.349(3) . ? N5 N6 1.373(3) . ? N6 C9 1.346(3) . ? N6 B1 1.519(4) . ? B1 H1B 1.0000 . ? C1 C2 1.391(4) . ? C1 C10 1.494(4) . ? C2 C3 1.374(4) . ? C2 H2A 0.9500 . ? C3 C11 1.489(4) . ? C4 C5 1.399(4) . ? C4 C12 1.493(4) . ? C5 C6 1.377(4) . ? C5 H5A 0.9500 . ? C6 C13 1.490(4) . ? C7 C8 1.384(4) . ? C7 C14 1.493(4) . ? C8 C9 1.372(4) . ? C8 H8A 0.9500 . ? C9 C15 1.497(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.382(4) . ? C16 C21 1.390(4) . ? C16 H16A 0.9500 . ? C17 C18 1.385(4) . ? C17 H17A 0.9500 . ? C18 C19 1.387(4) . ? C18 H18A 0.9500 . ? C19 C20 1.387(4) . ? C19 H19A 0.9500 . ? C20 C21 1.389(4) . ? C20 H20A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Rh1 N1 94.36(8) . . ? N5 Rh1 N3 86.99(8) . . ? N1 Rh1 N3 82.70(8) . . ? N5 Rh1 P1 91.22(6) . . ? N1 Rh1 P1 93.40(6) . . ? N3 Rh1 P1 175.57(6) . . ? N5 Rh1 Cl2 173.86(6) . . ? N1 Rh1 Cl2 91.77(6) . . ? N3 Rh1 Cl2 94.21(6) . . ? P1 Rh1 Cl2 88.00(3) . . ? N5 Rh1 Cl1 87.67(6) . . ? N1 Rh1 Cl1 172.81(6) . . ? N3 Rh1 Cl1 90.53(6) . . ? P1 Rh1 Cl1 93.45(3) . . ? Cl2 Rh1 Cl1 86.29(3) . . ? C23 P1 C22 100.51(14) . . ? C23 P1 C21 108.78(13) . . ? C22 P1 C21 100.89(13) . . ? C23 P1 Rh1 115.17(10) . . ? C22 P1 Rh1 117.59(10) . . ? C21 P1 Rh1 112.37(9) . . ? C1 N1 N2 106.3(2) . . ? C1 N1 Rh1 139.42(18) . . ? N2 N1 Rh1 114.29(15) . . ? C3 N2 N1 109.7(2) . . ? C3 N2 B1 127.7(2) . . ? N1 N2 B1 120.1(2) . . ? C4 N3 N4 107.3(2) . . ? C4 N3 Rh1 137.76(18) . . ? N4 N3 Rh1 114.94(15) . . ? C6 N4 N3 109.6(2) . . ? C6 N4 B1 130.1(2) . . ? N3 N4 B1 120.3(2) . . ? C7 N5 N6 106.5(2) . . ? C7 N5 Rh1 136.35(18) . . ? N6 N5 Rh1 117.11(15) . . ? C9 N6 N5 110.0(2) . . ? C9 N6 B1 130.6(2) . . ? N5 N6 B1 119.2(2) . . ? N6 B1 N2 109.7(2) . . ? N6 B1 N4 108.6(2) . . ? N2 B1 N4 109.3(2) . . ? N6 B1 H1B 109.7 . . ? N2 B1 H1B 109.7 . . ? N4 B1 H1B 109.7 . . ? N1 C1 C2 109.4(2) . . ? N1 C1 C10 127.7(2) . . ? C2 C1 C10 122.8(2) . . ? C3 C2 C1 106.8(2) . . ? C3 C2 H2A 126.6 . . ? C1 C2 H2A 126.6 . . ? N2 C3 C2 107.8(2) . . ? N2 C3 C11 123.5(3) . . ? C2 C3 C11 128.7(3) . . ? N3 C4 C5 109.1(2) . . ? N3 C4 C12 122.7(2) . . ? C5 C4 C12 128.2(2) . . ? C6 C5 C4 106.3(2) . . ? C6 C5 H5A 126.8 . . ? C4 C5 H5A 126.8 . . ? N4 C6 C5 107.7(2) . . ? N4 C6 C13 122.9(2) . . ? C5 C6 C13 129.3(2) . . ? N5 C7 C8 109.0(2) . . ? N5 C7 C14 126.4(2) . . ? C8 C7 C14 124.6(2) . . ? C9 C8 C7 107.2(2) . . ? C9 C8 H8A 126.4 . . ? C7 C8 H8A 126.4 . . ? N6 C9 C8 107.4(2) . . ? N6 C9 C15 123.5(3) . . ? C8 C9 C15 129.1(3) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 120.6(3) . . ? C17 C16 H16A 119.7 . . ? C21 C16 H16A 119.7 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C19 119.8(3) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C19 C20 C21 120.7(3) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C20 C21 C16 118.9(3) . . ? C20 C21 P1 122.0(2) . . ? C16 C21 P1 119.1(2) . . ? P1 C22 H22A 109.5 . . ? P1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Rh1 P1 C23 -102.47(12) . . . . ? N1 Rh1 P1 C23 163.08(12) . . . . ? N3 Rh1 P1 C23 -168.6(8) . . . . ? Cl2 Rh1 P1 C23 71.43(11) . . . . ? Cl1 Rh1 P1 C23 -14.73(11) . . . . ? N5 Rh1 P1 C22 139.30(13) . . . . ? N1 Rh1 P1 C22 44.86(13) . . . . ? N3 Rh1 P1 C22 73.2(8) . . . . ? Cl2 Rh1 P1 C22 -46.79(12) . . . . ? Cl1 Rh1 P1 C22 -132.96(12) . . . . ? N5 Rh1 P1 C21 22.84(11) . . . . ? N1 Rh1 P1 C21 -71.60(11) . . . . ? N3 Rh1 P1 C21 -43.3(8) . . . . ? Cl2 Rh1 P1 C21 -163.25(10) . . . . ? Cl1 Rh1 P1 C21 110.58(10) . . . . ? N5 Rh1 N1 C1 -153.3(3) . . . . ? N3 Rh1 N1 C1 120.3(3) . . . . ? P1 Rh1 N1 C1 -61.8(3) . . . . ? Cl2 Rh1 N1 C1 26.3(3) . . . . ? Cl1 Rh1 N1 C1 100.5(5) . . . . ? N5 Rh1 N1 N2 26.63(17) . . . . ? N3 Rh1 N1 N2 -59.77(16) . . . . ? P1 Rh1 N1 N2 118.12(15) . . . . ? Cl2 Rh1 N1 N2 -153.78(15) . . . . ? Cl1 Rh1 N1 N2 -79.6(5) . . . . ? C1 N1 N2 C3 2.4(3) . . . . ? Rh1 N1 N2 C3 -177.55(16) . . . . ? C1 N1 N2 B1 -161.0(2) . . . . ? Rh1 N1 N2 B1 19.1(3) . . . . ? N5 Rh1 N3 C4 135.1(3) . . . . ? N1 Rh1 N3 C4 -130.1(3) . . . . ? P1 Rh1 N3 C4 -158.6(6) . . . . ? Cl2 Rh1 N3 C4 -38.8(3) . . . . ? Cl1 Rh1 N3 C4 47.5(3) . . . . ? N5 Rh1 N3 N4 -43.00(17) . . . . ? N1 Rh1 N3 N4 51.79(17) . . . . ? P1 Rh1 N3 N4 23.3(9) . . . . ? Cl2 Rh1 N3 N4 143.04(16) . . . . ? Cl1 Rh1 N3 N4 -130.64(16) . . . . ? C4 N3 N4 C6 -0.9(3) . . . . ? Rh1 N3 N4 C6 177.79(16) . . . . ? C4 N3 N4 B1 177.8(2) . . . . ? Rh1 N3 N4 B1 -3.5(3) . . . . ? N1 Rh1 N5 C7 146.0(3) . . . . ? N3 Rh1 N5 C7 -131.6(3) . . . . ? P1 Rh1 N5 C7 52.5(3) . . . . ? Cl2 Rh1 N5 C7 -30.2(7) . . . . ? Cl1 Rh1 N5 C7 -40.9(3) . . . . ? N1 Rh1 N5 N6 -34.50(18) . . . . ? N3 Rh1 N5 N6 47.94(17) . . . . ? P1 Rh1 N5 N6 -128.01(17) . . . . ? Cl2 Rh1 N5 N6 149.3(5) . . . . ? Cl1 Rh1 N5 N6 138.59(17) . . . . ? C7 N5 N6 C9 0.2(3) . . . . ? Rh1 N5 N6 C9 -179.41(17) . . . . ? C7 N5 N6 B1 174.9(2) . . . . ? Rh1 N5 N6 B1 -4.8(3) . . . . ? C9 N6 B1 N2 -125.2(3) . . . . ? N5 N6 B1 N2 61.4(3) . . . . ? C9 N6 B1 N4 115.4(3) . . . . ? N5 N6 B1 N4 -58.0(3) . . . . ? C3 N2 B1 N6 128.4(3) . . . . ? N1 N2 B1 N6 -71.5(3) . . . . ? C3 N2 B1 N4 -112.6(3) . . . . ? N1 N2 B1 N4 47.5(3) . . . . ? C6 N4 B1 N6 -118.5(3) . . . . ? N3 N4 B1 N6 63.1(3) . . . . ? C6 N4 B1 N2 121.8(3) . . . . ? N3 N4 B1 N2 -56.6(3) . . . . ? N2 N1 C1 C2 -2.0(3) . . . . ? Rh1 N1 C1 C2 177.9(2) . . . . ? N2 N1 C1 C10 173.8(2) . . . . ? Rh1 N1 C1 C10 -6.3(4) . . . . ? N1 C1 C2 C3 1.0(3) . . . . ? C10 C1 C2 C3 -175.1(2) . . . . ? N1 N2 C3 C2 -1.8(3) . . . . ? B1 N2 C3 C2 159.9(2) . . . . ? N1 N2 C3 C11 178.9(2) . . . . ? B1 N2 C3 C11 -19.3(4) . . . . ? C1 C2 C3 N2 0.5(3) . . . . ? C1 C2 C3 C11 179.8(3) . . . . ? N4 N3 C4 C5 0.7(3) . . . . ? Rh1 N3 C4 C5 -177.48(19) . . . . ? N4 N3 C4 C12 -179.0(2) . . . . ? Rh1 N3 C4 C12 2.8(4) . . . . ? N3 C4 C5 C6 -0.3(3) . . . . ? C12 C4 C5 C6 179.3(3) . . . . ? N3 N4 C6 C5 0.7(3) . . . . ? B1 N4 C6 C5 -177.9(2) . . . . ? N3 N4 C6 C13 -178.5(2) . . . . ? B1 N4 C6 C13 2.9(4) . . . . ? C4 C5 C6 N4 -0.2(3) . . . . ? C4 C5 C6 C13 178.9(3) . . . . ? N6 N5 C7 C8 0.0(3) . . . . ? Rh1 N5 C7 C8 179.50(19) . . . . ? N6 N5 C7 C14 -177.2(2) . . . . ? Rh1 N5 C7 C14 2.4(4) . . . . ? N5 C7 C8 C9 -0.2(3) . . . . ? C14 C7 C8 C9 177.0(3) . . . . ? N5 N6 C9 C8 -0.3(3) . . . . ? B1 N6 C9 C8 -174.2(3) . . . . ? N5 N6 C9 C15 177.3(3) . . . . ? B1 N6 C9 C15 3.4(5) . . . . ? C7 C8 C9 N6 0.3(3) . . . . ? C7 C8 C9 C15 -177.1(3) . . . . ? C21 C16 C17 C18 -0.6(4) . . . . ? C16 C17 C18 C19 -0.8(5) . . . . ? C17 C18 C19 C20 1.6(4) . . . . ? C18 C19 C20 C21 -1.1(4) . . . . ? C19 C20 C21 C16 -0.3(4) . . . . ? C19 C20 C21 P1 -179.1(2) . . . . ? C17 C16 C21 C20 1.1(4) . . . . ? C17 C16 C21 P1 179.9(2) . . . . ? C23 P1 C21 C20 -5.7(3) . . . . ? C22 P1 C21 C20 99.5(2) . . . . ? Rh1 P1 C21 C20 -134.4(2) . . . . ? C23 P1 C21 C16 175.6(2) . . . . ? C22 P1 C21 C16 -79.2(2) . . . . ? Rh1 P1 C21 C16 46.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 36.32 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.743 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.161 #===end