# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Maria Garralda' 'Ricardo Hernandez' 'Elena Pinilla' 'M.Rosario Torres' 'Malkoa Zarandona' _publ_contact_author_name 'Maria Garralda' _publ_contact_author_email MARIAANGELES.GARRALDA@EHU.ES _publ_section_title ; Selective formation of cis-diacyl, cis-PPh2R rhodium(III) complexes by the reaction of rhodium(III) cis-diacyl, trans-PPh2R complexes with primary or N-substituted aliphatic diamines. ; #============================================================================ data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 738631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H40 N2 O2 P2 Rh, Cl O4' _chemical_formula_sum 'C42 H40 Cl N2 O6 P2 Rh' _chemical_formula_weight 869.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0986(7) _cell_length_b 15.6187(9) _cell_length_c 20.8399(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.8230(10) _cell_angle_gamma 90.00 _cell_volume 3880.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36545 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.1296 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 29.00 _reflns_number_total 9649 _reflns_number_gt 4706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The oxygen atoms of the ClO4 anion were refined isotropically. 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^)+(0.0820P)^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 or Fourier' _refine_ls_hydrogen_treatment 'constr or fixed' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9649 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1277 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1717 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.003 _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 N1 N 0.8172(4) 0.8955(3) 0.5954(2) 0.0468(12) Uani 1 1 d . . . N2 N 0.5786(4) 0.9172(3) 0.5608(2) 0.0415(11) Uani 1 1 d . . . H21 H 0.5675 0.9679 0.5387 0.050 Uiso 1 1 d . . . H22 H 0.5074 0.8905 0.5532 0.050 Uiso 1 1 d . . . O1 O 0.5131(3) 0.9034(2) 0.39784(19) 0.0525(11) Uani 1 1 d . . . O2 O 0.6655(3) 1.0399(2) 0.48553(19) 0.0477(10) Uani 1 1 d . . . P1 P 0.63349(11) 0.71157(8) 0.53436(7) 0.0339(3) Uani 1 1 d . . . P2 P 0.79489(11) 0.81605(9) 0.42663(7) 0.0357(3) Uani 1 1 d . . . Rh Rh 0.68579(3) 0.85552(2) 0.50216(2) 0.03136(14) Uani 1 1 d . . . C1 C 0.5493(4) 0.8440(3) 0.4327(3) 0.0360(12) Uani 1 1 d . . . C2 C 0.4828(4) 0.7620(3) 0.4277(2) 0.0333(12) Uani 1 1 d . . . C3 C 0.5146(4) 0.6941(3) 0.4691(3) 0.0365(12) Uani 1 1 d . . . C4 C 0.4511(5) 0.6194(4) 0.4625(3) 0.0490(15) Uani 1 1 d . . . H4 H 0.4701 0.5746 0.4917 0.059 Uiso 1 1 calc R . . C5 C 0.3609(5) 0.6113(4) 0.4135(3) 0.0555(16) Uani 1 1 d . . . H5 H 0.3215 0.5599 0.4082 0.067 Uiso 1 1 calc R . . C6 C 0.3281(5) 0.6780(4) 0.3720(3) 0.0579(17) Uani 1 1 d . . . H6 H 0.2660 0.6723 0.3392 0.070 Uiso 1 1 calc R . . C7 C 0.3878(4) 0.7542(4) 0.3791(3) 0.0451(14) Uani 1 1 d . . . H7 H 0.3648 0.8001 0.3517 0.054 Uiso 1 1 calc R . . C8 C 0.5648(4) 0.6901(3) 0.6050(3) 0.0389(13) Uani 1 1 d . . . C9 C 0.4625(5) 0.7302(4) 0.6073(3) 0.0532(16) Uani 1 1 d . . . H9 H 0.4347 0.7692 0.5748 0.064 Uiso 1 1 calc R . . C10 C 0.4015(5) 0.7138(4) 0.6560(3) 0.0608(18) Uani 1 1 d . . . H10 H 0.3334 0.7414 0.6560 0.073 Uiso 1 1 calc R . . C11 C 0.4410(6) 0.6570(5) 0.7043(3) 0.072(2) Uani 1 1 d . . . H11 H 0.3998 0.6452 0.7371 0.087 Uiso 1 1 calc R . . C12 C 0.5428(6) 0.6174(5) 0.7039(3) 0.079(2) Uani 1 1 d . . . H12 H 0.5709 0.5792 0.7369 0.095 Uiso 1 1 calc R . . C13 C 0.6027(5) 0.6340(4) 0.6554(3) 0.0643(19) Uani 1 1 d . . . H13 H 0.6712 0.6067 0.6563 0.077 Uiso 1 1 calc R . . C14 C 0.7264(4) 0.6187(3) 0.5323(3) 0.0381(13) Uani 1 1 d . . . C15 C 0.7139(5) 0.5626(3) 0.4796(3) 0.0493(15) Uani 1 1 d . . . H15 H 0.6558 0.5708 0.4447 0.059 Uiso 1 1 calc R . . C16 C 0.7864(6) 0.4952(4) 0.4788(4) 0.0643(19) Uani 1 1 d . . . H16 H 0.7772 0.4570 0.4441 0.077 Uiso 1 1 calc R . . C17 C 0.8743(6) 0.4853(4) 0.5310(4) 0.070(2) Uani 1 1 d . . . H17 H 0.9240 0.4400 0.5305 0.084 Uiso 1 1 calc R . . C18 C 0.8895(5) 0.5393(4) 0.5823(4) 0.0578(17) Uani 1 1 d . . . H18 H 0.9489 0.5314 0.6165 0.069 Uiso 1 1 calc R . . C19 C 0.8158(5) 0.6063(4) 0.5833(3) 0.0485(15) Uani 1 1 d . . . H19 H 0.8258 0.6439 0.6184 0.058 Uiso 1 1 calc R . . C20 C 0.6996(4) 0.9754(3) 0.4621(3) 0.0408(13) Uani 1 1 d . . . C21 C 0.7446(4) 0.9824(3) 0.3997(3) 0.0412(13) Uani 1 1 d . . . C22 C 0.7864(4) 0.9093(3) 0.3743(3) 0.0409(13) Uani 1 1 d . . . C23 C 0.8223(5) 0.9123(4) 0.3142(3) 0.0512(15) Uani 1 1 d . . . H23 H 0.8477 0.8630 0.2962 0.061 Uiso 1 1 calc R . . C24 C 0.8196(5) 0.9906(4) 0.2813(3) 0.0617(18) Uani 1 1 d . . . H24 H 0.8449 0.9942 0.2417 0.074 Uiso 1 1 calc R . . C25 C 0.7795(6) 1.0616(4) 0.3077(3) 0.068(2) Uani 1 1 d . . . H25 H 0.7777 1.1133 0.2855 0.081 Uiso 1 1 calc R . . C26 C 0.7419(5) 1.0591(4) 0.3658(3) 0.0605(18) Uani 1 1 d . . . H26 H 0.7146 1.1085 0.3825 0.073 Uiso 1 1 calc R . . C27 C 0.9439(4) 0.7994(3) 0.4555(3) 0.0414(13) Uani 1 1 d . . . C28 C 0.9760(5) 0.7465(4) 0.5088(3) 0.0506(15) Uani 1 1 d . . . H28 H 0.9213 0.7223 0.5296 0.061 Uiso 1 1 calc R . . C29 C 1.0873(5) 0.7289(4) 0.5314(3) 0.0649(18) Uani 1 1 d . . . H29 H 1.1077 0.6945 0.5679 0.078 Uiso 1 1 calc R . . C30 C 1.1683(5) 0.7626(4) 0.4997(4) 0.067(2) Uani 1 1 d . . . H30 H 1.2436 0.7507 0.5148 0.080 Uiso 1 1 calc R . . C31 C 1.1390(5) 0.8131(4) 0.4464(4) 0.070(2) Uani 1 1 d . . . H31 H 1.1940 0.8348 0.4247 0.084 Uiso 1 1 calc R . . C32 C 1.0262(5) 0.8323(4) 0.4243(4) 0.0597(18) Uani 1 1 d . . . H32 H 1.0064 0.8676 0.3882 0.072 Uiso 1 1 calc R . . C33 C 0.7584(5) 0.7264(3) 0.3715(3) 0.0413(13) Uani 1 1 d . . . C34 C 0.6561(5) 0.7234(4) 0.3317(3) 0.0561(16) Uani 1 1 d . . . H34 H 0.6077 0.7700 0.3296 0.067 Uiso 1 1 calc R . . C35 C 0.6241(6) 0.6509(5) 0.2943(3) 0.073(2) Uani 1 1 d . . . H35 H 0.5534 0.6489 0.2684 0.087 Uiso 1 1 calc R . . C36 C 0.6945(7) 0.5825(5) 0.2948(3) 0.071(2) Uani 1 1 d . . . H36 H 0.6710 0.5334 0.2712 0.085 Uiso 1 1 calc R . . C37 C 0.7997(7) 0.5873(4) 0.3305(3) 0.076(2) Uani 1 1 d . . . H37 H 0.8503 0.5430 0.3284 0.091 Uiso 1 1 calc R . . C38 C 0.8323(6) 0.6580(4) 0.3699(3) 0.0591(17) Uani 1 1 d . . . H38 H 0.9034 0.6597 0.3953 0.071 Uiso 1 1 calc R . . C39 C 0.8594(5) 0.8267(4) 0.6422(3) 0.0587(17) Uani 1 1 d . . . H39A H 0.8976 0.8517 0.6819 0.088 Uiso 1 1 calc R . . H39B H 0.9106 0.7909 0.6238 0.088 Uiso 1 1 calc R . . H39C H 0.7976 0.7929 0.6511 0.088 Uiso 1 1 calc R . . C40 C 0.9169(5) 0.9421(4) 0.5803(3) 0.0659(19) Uani 1 1 d . . . H40A H 0.8932 0.9840 0.5471 0.099 Uiso 1 1 calc R . . H40B H 0.9671 0.9022 0.5652 0.099 Uiso 1 1 calc R . . H40C H 0.9547 0.9702 0.6188 0.099 Uiso 1 1 calc R . . C41 C 0.7513(5) 0.9567(4) 0.6283(3) 0.0530(16) Uani 1 1 d . . . H41A H 0.7475 1.0114 0.6060 0.064 Uiso 1 1 calc R . . H41B H 0.7891 0.9656 0.6728 0.064 Uiso 1 1 calc R . . C42 C 0.6352(5) 0.9248(4) 0.6289(3) 0.0549(16) Uani 1 1 d . . . H42A H 0.6377 0.8695 0.6504 0.066 Uiso 1 1 calc R . . H42B H 0.5949 0.9645 0.6523 0.066 Uiso 1 1 calc R . . Cl1 Cl 0.10703(16) 0.83810(12) 0.23365(9) 0.0700(5) Uani 1 1 d . . . O3 O -0.0028(9) 0.8412(6) 0.2223(5) 0.197(4) Uiso 1 1 d . . . O4 O 0.1387(9) 0.8750(7) 0.1744(6) 0.222(4) Uiso 1 1 d . . . O5 O 0.1610(8) 0.8756(6) 0.2861(5) 0.209(4) Uiso 1 1 d . . . O6 O 0.1554(9) 0.7600(8) 0.2290(5) 0.235(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.042(3) 0.044(3) 0.049(3) -0.002(2) -0.009(2) 0.001(2) N2 0.042(3) 0.043(3) 0.040(3) -0.002(2) 0.007(2) 0.010(2) O1 0.053(3) 0.039(2) 0.058(3) 0.011(2) -0.013(2) 0.0038(19) O2 0.052(2) 0.031(2) 0.060(3) -0.0021(19) 0.011(2) 0.0050(18) P1 0.0318(8) 0.0312(7) 0.0380(8) 0.0034(6) 0.0035(6) 0.0022(6) P2 0.0318(8) 0.0343(7) 0.0417(8) 0.0034(6) 0.0082(6) 0.0019(6) Rh 0.0294(2) 0.0293(2) 0.0345(2) 0.00074(19) 0.00282(16) 0.00279(18) C1 0.037(3) 0.035(3) 0.036(3) 0.004(2) 0.006(2) 0.004(2) C2 0.031(3) 0.035(3) 0.035(3) 0.000(2) 0.007(2) 0.000(2) C3 0.033(3) 0.036(3) 0.042(3) 0.003(2) 0.009(2) 0.003(2) C4 0.050(4) 0.042(3) 0.054(4) 0.002(3) 0.004(3) -0.008(3) C5 0.048(4) 0.054(4) 0.061(4) 0.002(3) 0.002(3) -0.021(3) C6 0.044(4) 0.075(5) 0.050(4) -0.007(4) -0.006(3) -0.011(3) C7 0.036(3) 0.055(4) 0.042(3) 0.007(3) 0.001(3) 0.000(3) C8 0.037(3) 0.040(3) 0.040(3) 0.002(3) 0.006(3) 0.003(2) C9 0.044(4) 0.053(4) 0.066(4) 0.018(3) 0.016(3) 0.011(3) C10 0.050(4) 0.072(5) 0.066(5) 0.005(4) 0.025(4) 0.008(3) C11 0.071(5) 0.093(6) 0.060(5) 0.005(4) 0.035(4) -0.008(4) C12 0.091(6) 0.096(6) 0.056(4) 0.031(4) 0.027(4) 0.024(5) C13 0.062(4) 0.081(5) 0.055(4) 0.024(4) 0.021(3) 0.029(4) C14 0.034(3) 0.030(3) 0.051(3) 0.007(3) 0.007(3) 0.002(2) C15 0.056(4) 0.037(3) 0.057(4) 0.003(3) 0.015(3) 0.007(3) C16 0.079(5) 0.048(4) 0.072(5) -0.004(3) 0.032(4) 0.017(4) C17 0.061(5) 0.047(4) 0.108(6) 0.016(4) 0.032(5) 0.022(3) C18 0.040(4) 0.046(4) 0.084(5) 0.010(4) 0.002(3) 0.007(3) C19 0.039(3) 0.037(3) 0.065(4) -0.001(3) -0.001(3) -0.001(3) C20 0.035(3) 0.036(3) 0.048(3) 0.005(3) -0.001(3) 0.004(2) C21 0.038(3) 0.040(3) 0.045(3) 0.005(3) 0.004(3) -0.004(2) C22 0.036(3) 0.042(3) 0.044(3) 0.003(3) 0.005(3) -0.003(2) C23 0.051(4) 0.054(4) 0.052(4) 0.009(3) 0.017(3) 0.001(3) C24 0.067(4) 0.071(5) 0.048(4) 0.005(4) 0.012(3) -0.015(4) C25 0.091(5) 0.054(4) 0.057(4) 0.024(4) 0.010(4) -0.002(4) C26 0.078(5) 0.044(4) 0.062(4) 0.017(3) 0.021(4) 0.007(3) C27 0.034(3) 0.038(3) 0.053(4) -0.003(3) 0.009(3) 0.006(2) C28 0.038(3) 0.056(4) 0.058(4) 0.005(3) 0.009(3) 0.008(3) C29 0.061(5) 0.069(5) 0.062(4) -0.001(4) 0.003(4) 0.018(4) C30 0.027(4) 0.067(5) 0.100(6) -0.008(4) -0.006(4) 0.008(3) C31 0.031(4) 0.063(4) 0.117(7) 0.009(5) 0.014(4) 0.000(3) C32 0.040(4) 0.055(4) 0.083(5) 0.006(4) 0.008(3) -0.001(3) C33 0.046(4) 0.040(3) 0.041(3) 0.000(3) 0.015(3) -0.001(3) C34 0.056(4) 0.069(4) 0.046(4) -0.011(3) 0.015(3) 0.001(3) C35 0.078(5) 0.087(6) 0.052(4) -0.024(4) 0.010(4) -0.019(4) C36 0.103(6) 0.059(5) 0.051(4) -0.013(4) 0.016(4) -0.008(4) C37 0.123(7) 0.051(4) 0.052(4) -0.009(4) 0.014(5) 0.024(4) C38 0.074(5) 0.052(4) 0.051(4) -0.003(3) 0.009(3) 0.010(3) C39 0.065(4) 0.053(4) 0.050(4) 0.004(3) -0.013(3) 0.017(3) C40 0.048(4) 0.061(4) 0.082(5) -0.012(4) -0.009(4) -0.015(3) C41 0.068(4) 0.044(3) 0.042(3) -0.012(3) -0.006(3) 0.007(3) C42 0.068(4) 0.058(4) 0.039(3) -0.004(3) 0.008(3) 0.016(3) Cl1 0.0628(12) 0.0805(13) 0.0633(11) -0.0148(10) 0.0008(9) 0.0056(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 N1 C41 1.486(7) . ? N1 C39 1.482(7) . ? N1 C40 1.488(7) . ? N1 Rh 2.374(4) . ? N2 C42 1.472(7) . ? N2 Rh 2.155(4) . ? N2 H21 0.9148 . ? N2 H22 0.9463 . ? O1 C1 1.213(6) . ? O2 C20 1.222(6) . ? P1 C3 1.824(5) . ? P1 C14 1.840(5) . ? P1 C8 1.841(5) . ? P1 Rh 2.4597(13) . ? P2 C22 1.812(5) . ? P2 C33 1.817(6) . ? P2 C27 1.819(5) . ? P2 Rh 2.3042(14) . ? Rh C1 2.009(5) . ? Rh C20 2.068(5) . ? C1 C2 1.507(7) . ? C2 C3 1.381(7) . ? C2 C7 1.401(7) . ? C3 C4 1.390(7) . ? C4 C5 1.367(8) . ? C4 H4 0.9300 . ? C5 C6 1.369(8) . ? C5 H5 0.9300 . ? C6 C7 1.386(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.395(7) . ? C8 C13 1.384(8) . ? C9 C10 1.378(8) . ? C9 H9 0.9300 . ? C10 C11 1.366(9) . ? C10 H10 0.9300 . ? C11 C12 1.380(9) . ? C11 H11 0.9300 . ? C12 C13 1.364(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.392(8) . ? C14 C19 1.394(8) . ? C15 C16 1.372(8) . ? C15 H15 0.9300 . ? C16 C17 1.394(9) . ? C16 H16 0.9300 . ? C17 C18 1.349(9) . ? C17 H17 0.9300 . ? C18 C19 1.377(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.496(8) . ? C21 C22 1.390(7) . ? C21 C26 1.389(7) . ? C22 C23 1.395(7) . ? C23 C24 1.399(8) . ? C23 H23 0.9300 . ? C24 C25 1.364(9) . ? C24 H24 0.9300 . ? C25 C26 1.363(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.385(7) . ? C27 C32 1.379(8) . ? C28 C29 1.376(8) . ? C28 H28 0.9300 . ? C29 C30 1.377(9) . ? C29 H29 0.9300 . ? C30 C31 1.358(9) . ? C30 H30 0.9300 . ? C31 C32 1.397(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.369(8) . ? C33 C38 1.396(7) . ? C34 C35 1.392(8) . ? C34 H34 0.9300 . ? C35 C36 1.364(9) . ? C35 H35 0.9300 . ? C36 C37 1.362(10) . ? C36 H36 0.9300 . ? C37 C38 1.393(9) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.493(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? Cl1 O3 1.311(10) . ? Cl1 O5 1.311(11) . ? Cl1 O6 1.363(12) . ? Cl1 O4 1.471(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 N1 C39 108.3(5) . . ? C41 N1 C40 107.5(5) . . ? C39 N1 C40 107.0(5) . . ? C41 N1 Rh 102.2(3) . . ? C39 N1 Rh 117.1(4) . . ? C40 N1 Rh 114.2(4) . . ? C42 N2 Rh 111.0(3) . . ? C42 N2 H21 114.9 . . ? Rh N2 H21 98.8 . . ? C42 N2 H22 117.2 . . ? Rh N2 H22 109.1 . . ? H21 N2 H22 104.2 . . ? C3 P1 C14 105.7(2) . . ? C3 P1 C8 99.4(2) . . ? C14 P1 C8 103.7(2) . . ? C3 P1 Rh 98.07(17) . . ? C14 P1 Rh 121.84(17) . . ? C8 P1 Rh 123.85(18) . . ? C22 P2 C33 104.8(3) . . ? C22 P2 C27 105.4(2) . . ? C33 P2 C27 102.7(3) . . ? C22 P2 Rh 102.48(18) . . ? C33 P2 Rh 122.16(18) . . ? C27 P2 Rh 117.55(19) . . ? C1 Rh C20 84.4(2) . . ? C1 Rh N2 87.05(18) . . ? C20 Rh N2 85.6(2) . . ? C1 Rh P2 88.87(15) . . ? C20 Rh P2 82.58(16) . . ? N2 Rh P2 167.78(12) . . ? C1 Rh N1 165.01(18) . . ? C20 Rh N1 90.20(19) . . ? N2 Rh N1 78.56(16) . . ? P2 Rh N1 104.34(12) . . ? C1 Rh P1 84.08(15) . . ? C20 Rh P1 168.46(15) . . ? N2 Rh P1 92.65(12) . . ? P2 Rh P1 98.39(5) . . ? N1 Rh P1 100.64(12) . . ? O1 C1 C2 118.3(5) . . ? O1 C1 Rh 122.1(4) . . ? C2 C1 Rh 119.3(4) . . ? C3 C2 C7 119.4(5) . . ? C3 C2 C1 121.4(5) . . ? C7 C2 C1 119.2(5) . . ? C2 C3 C4 119.5(5) . . ? C2 C3 P1 116.8(4) . . ? C4 C3 P1 123.5(4) . . ? C3 C4 C5 120.6(6) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 120.6(6) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C5 119.8(6) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 120.0(5) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C9 C8 C13 116.1(5) . . ? C9 C8 P1 117.9(4) . . ? C13 C8 P1 125.9(4) . . ? C10 C9 C8 122.1(6) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C11 C10 C9 120.0(6) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.1(6) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 120.4(6) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 122.2(6) . . ? C12 C13 H13 118.9 . . ? C8 C13 H13 118.9 . . ? C15 C14 C19 118.6(5) . . ? C15 C14 P1 122.0(4) . . ? C19 C14 P1 119.3(4) . . ? C16 C15 C14 120.6(6) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 118.6(6) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C18 C17 C16 122.1(6) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 119.1(6) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C14 C19 C18 120.9(6) . . ? C14 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? O2 C20 C21 119.0(5) . . ? O2 C20 Rh 121.9(4) . . ? C21 C20 Rh 118.9(4) . . ? C22 C21 C26 119.6(5) . . ? C22 C21 C20 118.7(5) . . ? C26 C21 C20 121.7(5) . . ? C21 C22 C23 120.3(5) . . ? C21 C22 P2 114.7(4) . . ? C23 C22 P2 125.0(4) . . ? C24 C23 C22 118.9(6) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C25 C24 C23 119.5(6) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 122.1(6) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C21 C26 C25 119.6(6) . . ? C21 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C28 C27 C32 118.3(5) . . ? C28 C27 P2 118.5(4) . . ? C32 C27 P2 123.0(5) . . ? C27 C28 C29 121.1(6) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 119.6(6) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.4(6) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C32 119.9(6) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C27 C32 C31 120.5(6) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C38 118.4(6) . . ? C34 C33 P2 120.5(4) . . ? C38 C33 P2 121.1(5) . . ? C33 C34 C35 120.3(6) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 121.2(7) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C37 C36 C35 119.1(7) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C38 120.6(7) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C33 C38 C37 120.2(7) . . ? C33 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? N1 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N1 C40 H40A 109.5 . . ? N1 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N1 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N1 C41 C42 111.6(5) . . ? N1 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? N1 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? N2 C42 C41 107.6(5) . . ? N2 C42 H42A 110.2 . . ? C41 C42 H42A 110.2 . . ? N2 C42 H42B 110.2 . . ? C41 C42 H42B 110.2 . . ? H42A C42 H42B 108.5 . . ? O3 Cl1 O5 118.7(6) . . ? O3 Cl1 O6 117.0(6) . . ? O5 Cl1 O6 107.4(6) . . ? O3 Cl1 O4 103.6(6) . . ? O5 Cl1 O4 111.1(6) . . ? O6 Cl1 O4 96.6(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C42 N2 Rh C1 167.3(4) . . . . ? C42 N2 Rh C20 -108.0(4) . . . . ? C42 N2 Rh P2 -122.0(6) . . . . ? C42 N2 Rh N1 -16.9(4) . . . . ? C42 N2 Rh P1 83.4(4) . . . . ? C22 P2 Rh C1 71.3(2) . . . . ? C33 P2 Rh C1 -45.4(3) . . . . ? C27 P2 Rh C1 -173.7(2) . . . . ? C22 P2 Rh C20 -13.2(2) . . . . ? C33 P2 Rh C20 -129.9(3) . . . . ? C27 P2 Rh C20 101.8(3) . . . . ? C22 P2 Rh N2 0.8(6) . . . . ? C33 P2 Rh N2 -115.9(6) . . . . ? C27 P2 Rh N2 115.8(6) . . . . ? C22 P2 Rh N1 -101.5(2) . . . . ? C33 P2 Rh N1 141.8(2) . . . . ? C27 P2 Rh N1 13.5(2) . . . . ? C22 P2 Rh P1 155.15(18) . . . . ? C33 P2 Rh P1 38.5(2) . . . . ? C27 P2 Rh P1 -89.9(2) . . . . ? C41 N1 Rh C1 2.7(9) . . . . ? C39 N1 Rh C1 120.9(7) . . . . ? C40 N1 Rh C1 -113.0(7) . . . . ? C41 N1 Rh C20 71.5(4) . . . . ? C39 N1 Rh C20 -170.3(4) . . . . ? C40 N1 Rh C20 -44.2(4) . . . . ? C41 N1 Rh N2 -13.9(3) . . . . ? C39 N1 Rh N2 104.2(4) . . . . ? C40 N1 Rh N2 -129.6(4) . . . . ? C41 N1 Rh P2 153.9(3) . . . . ? C39 N1 Rh P2 -88.0(4) . . . . ? C40 N1 Rh P2 38.2(4) . . . . ? C41 N1 Rh P1 -104.5(3) . . . . ? C39 N1 Rh P1 13.7(4) . . . . ? C40 N1 Rh P1 139.8(4) . . . . ? C3 P1 Rh C1 3.8(2) . . . . ? C14 P1 Rh C1 118.0(3) . . . . ? C8 P1 Rh C1 -103.3(3) . . . . ? C3 P1 Rh C20 9.8(8) . . . . ? C14 P1 Rh C20 124.1(8) . . . . ? C8 P1 Rh C20 -97.3(9) . . . . ? C3 P1 Rh N2 90.6(2) . . . . ? C14 P1 Rh N2 -155.2(3) . . . . ? C8 P1 Rh N2 -16.5(2) . . . . ? C3 P1 Rh P2 -84.18(17) . . . . ? C14 P1 Rh P2 30.1(2) . . . . ? C8 P1 Rh P2 168.7(2) . . . . ? C3 P1 Rh N1 169.4(2) . . . . ? C14 P1 Rh N1 -76.3(3) . . . . ? C8 P1 Rh N1 62.3(2) . . . . ? C20 Rh C1 O1 -7.1(5) . . . . ? N2 Rh C1 O1 78.8(5) . . . . ? P2 Rh C1 O1 -89.7(4) . . . . ? N1 Rh C1 O1 62.5(9) . . . . ? P1 Rh C1 O1 171.7(5) . . . . ? C20 Rh C1 C2 178.9(4) . . . . ? N2 Rh C1 C2 -95.2(4) . . . . ? P2 Rh C1 C2 96.3(4) . . . . ? N1 Rh C1 C2 -111.5(7) . . . . ? P1 Rh C1 C2 -2.3(4) . . . . ? O1 C1 C2 C3 -175.2(5) . . . . ? Rh C1 C2 C3 -1.0(6) . . . . ? O1 C1 C2 C7 5.9(7) . . . . ? Rh C1 C2 C7 -179.9(4) . . . . ? C7 C2 C3 C4 -0.8(7) . . . . ? C1 C2 C3 C4 -179.7(5) . . . . ? C7 C2 C3 P1 -176.0(4) . . . . ? C1 C2 C3 P1 5.0(6) . . . . ? C14 P1 C3 C2 -132.0(4) . . . . ? C8 P1 C3 C2 120.8(4) . . . . ? Rh P1 C3 C2 -5.6(4) . . . . ? C14 P1 C3 C4 52.9(5) . . . . ? C8 P1 C3 C4 -54.2(5) . . . . ? Rh P1 C3 C4 179.3(4) . . . . ? C2 C3 C4 C5 3.2(8) . . . . ? P1 C3 C4 C5 178.1(5) . . . . ? C3 C4 C5 C6 -3.3(9) . . . . ? C4 C5 C6 C7 1.0(10) . . . . ? C5 C6 C7 C2 1.4(9) . . . . ? C3 C2 C7 C6 -1.5(8) . . . . ? C1 C2 C7 C6 177.4(5) . . . . ? C3 P1 C8 C9 -48.7(5) . . . . ? C14 P1 C8 C9 -157.5(5) . . . . ? Rh P1 C8 C9 57.7(5) . . . . ? C3 P1 C8 C13 128.0(6) . . . . ? C14 P1 C8 C13 19.1(6) . . . . ? Rh P1 C8 C13 -125.6(5) . . . . ? C13 C8 C9 C10 -1.2(9) . . . . ? P1 C8 C9 C10 175.7(5) . . . . ? C8 C9 C10 C11 0.3(10) . . . . ? C9 C10 C11 C12 0.7(11) . . . . ? C10 C11 C12 C13 -0.7(12) . . . . ? C11 C12 C13 C8 -0.2(12) . . . . ? C9 C8 C13 C12 1.2(10) . . . . ? P1 C8 C13 C12 -175.5(6) . . . . ? C3 P1 C14 C15 14.0(5) . . . . ? C8 P1 C14 C15 118.0(5) . . . . ? Rh P1 C14 C15 -96.3(5) . . . . ? C3 P1 C14 C19 -169.5(4) . . . . ? C8 P1 C14 C19 -65.4(5) . . . . ? Rh P1 C14 C19 80.3(5) . . . . ? C19 C14 C15 C16 1.6(8) . . . . ? P1 C14 C15 C16 178.2(5) . . . . ? C14 C15 C16 C17 -1.4(9) . . . . ? C15 C16 C17 C18 0.5(10) . . . . ? C16 C17 C18 C19 0.2(10) . . . . ? C15 C14 C19 C18 -1.0(8) . . . . ? P1 C14 C19 C18 -177.7(4) . . . . ? C17 C18 C19 C14 0.1(9) . . . . ? C1 Rh C20 O2 98.2(5) . . . . ? N2 Rh C20 O2 10.7(5) . . . . ? P2 Rh C20 O2 -172.2(5) . . . . ? N1 Rh C20 O2 -67.8(5) . . . . ? P1 Rh C20 O2 92.2(9) . . . . ? C1 Rh C20 C21 -77.0(4) . . . . ? N2 Rh C20 C21 -164.5(4) . . . . ? P2 Rh C20 C21 12.6(4) . . . . ? N1 Rh C20 C21 117.0(4) . . . . ? P1 Rh C20 C21 -83.0(9) . . . . ? O2 C20 C21 C22 178.1(5) . . . . ? Rh C20 C21 C22 -6.5(7) . . . . ? O2 C20 C21 C26 -4.2(8) . . . . ? Rh C20 C21 C26 171.1(4) . . . . ? C26 C21 C22 C23 -1.8(8) . . . . ? C20 C21 C22 C23 175.9(5) . . . . ? C26 C21 C22 P2 175.5(4) . . . . ? C20 C21 C22 P2 -6.8(7) . . . . ? C33 P2 C22 C21 143.1(4) . . . . ? C27 P2 C22 C21 -108.9(4) . . . . ? Rh P2 C22 C21 14.6(4) . . . . ? C33 P2 C22 C23 -39.7(5) . . . . ? C27 P2 C22 C23 68.2(5) . . . . ? Rh P2 C22 C23 -168.2(5) . . . . ? C21 C22 C23 C24 2.4(9) . . . . ? P2 C22 C23 C24 -174.6(4) . . . . ? C22 C23 C24 C25 -1.6(9) . . . . ? C23 C24 C25 C26 0.2(11) . . . . ? C22 C21 C26 C25 0.4(9) . . . . ? C20 C21 C26 C25 -177.2(6) . . . . ? C24 C25 C26 C21 0.4(11) . . . . ? C22 P2 C27 C28 164.1(4) . . . . ? C33 P2 C27 C28 -86.4(5) . . . . ? Rh P2 C27 C28 50.7(5) . . . . ? C22 P2 C27 C32 -20.5(6) . . . . ? C33 P2 C27 C32 89.1(5) . . . . ? Rh P2 C27 C32 -133.8(5) . . . . ? C32 C27 C28 C29 1.9(9) . . . . ? P2 C27 C28 C29 177.6(5) . . . . ? C27 C28 C29 C30 -1.7(10) . . . . ? C28 C29 C30 C31 0.2(10) . . . . ? C29 C30 C31 C32 1.2(11) . . . . ? C28 C27 C32 C31 -0.5(9) . . . . ? P2 C27 C32 C31 -176.0(5) . . . . ? C30 C31 C32 C27 -1.0(10) . . . . ? C22 P2 C33 C34 -59.7(5) . . . . ? C27 P2 C33 C34 -169.7(5) . . . . ? Rh P2 C33 C34 55.8(5) . . . . ? C22 P2 C33 C38 122.0(5) . . . . ? C27 P2 C33 C38 12.0(5) . . . . ? Rh P2 C33 C38 -122.5(4) . . . . ? C38 C33 C34 C35 4.7(9) . . . . ? P2 C33 C34 C35 -173.7(5) . . . . ? C33 C34 C35 C36 -2.0(10) . . . . ? C34 C35 C36 C37 -3.0(11) . . . . ? C35 C36 C37 C38 5.1(11) . . . . ? C34 C33 C38 C37 -2.6(9) . . . . ? P2 C33 C38 C37 175.7(5) . . . . ? C36 C37 C38 C33 -2.3(10) . . . . ? C39 N1 C41 C42 -80.6(6) . . . . ? C40 N1 C41 C42 164.1(5) . . . . ? Rh N1 C41 C42 43.6(5) . . . . ? Rh N2 C42 C41 45.7(5) . . . . ? N1 C41 C42 N2 -62.3(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H21 O2 0.91 2.08 2.793(6) 133.4 . N2 H22 O2 0.95 2.37 3.022(6) 125.4 3_676 _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 1.237 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.110 #==============================================================END data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 738632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H40 N2 O2 P2 Rh, Cl O4' _chemical_formula_sum 'C42 H40 Cl N2 O6 P2 Rh' _chemical_formula_weight 869.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.4770(9) _cell_length_b 18.9855(10) _cell_length_c 26.3711(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7748.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71166 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 29.09 _reflns_number_total 9838 _reflns_number_gt 5640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^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 or Fourier' _refine_ls_hydrogen_treatment 'constr or fixed' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9838 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.007 _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 C1 C -0.06988(16) 0.15976(15) 0.29720(10) 0.0341(6) Uani 1 1 d . . . C2 C 0.00578(17) 0.14383(14) 0.26225(10) 0.0345(6) Uani 1 1 d . . . C3 C 0.08551(17) 0.17634(14) 0.26969(10) 0.0346(6) Uani 1 1 d . . . C4 C 0.15596(18) 0.15521(16) 0.23939(11) 0.0446(8) Uani 1 1 d . . . H4 H 0.2098 0.1760 0.2442 0.054 Uiso 1 1 calc R . . C5 C 0.1460(2) 0.10452(17) 0.20315(12) 0.0518(8) Uani 1 1 d . . . H5 H 0.1935 0.0896 0.1843 0.062 Uiso 1 1 calc R . . C6 C 0.0652(2) 0.07507(17) 0.19428(12) 0.0542(9) Uani 1 1 d . . . H6 H 0.0581 0.0420 0.1686 0.065 Uiso 1 1 calc R . . C7 C -0.0042(2) 0.09489(16) 0.22352(11) 0.0479(8) Uani 1 1 d . . . H7 H -0.0583 0.0754 0.2173 0.057 Uiso 1 1 calc R . . C8 C 0.11621(16) 0.32417(14) 0.27335(11) 0.0344(6) Uani 1 1 d . . . C9 C 0.13268(19) 0.38933(16) 0.29512(12) 0.0489(8) Uani 1 1 d . . . H9 H 0.1252 0.3951 0.3299 0.059 Uiso 1 1 calc R . . C10 C 0.1599(2) 0.44576(17) 0.26636(14) 0.0540(9) Uani 1 1 d . . . H10 H 0.1726 0.4884 0.2821 0.065 Uiso 1 1 calc R . . C11 C 0.16838(19) 0.43965(18) 0.21505(14) 0.0546(9) Uani 1 1 d . . . H11 H 0.1867 0.4779 0.1958 0.066 Uiso 1 1 calc R . . C12 C 0.1495(2) 0.37662(18) 0.19214(13) 0.0569(9) Uani 1 1 d . . . H12 H 0.1541 0.3724 0.1571 0.068 Uiso 1 1 calc R . . C13 C 0.12363(19) 0.31906(17) 0.22081(12) 0.0477(8) Uani 1 1 d . . . H13 H 0.1111 0.2766 0.2048 0.057 Uiso 1 1 calc R . . C14 C 0.18781(17) 0.23807(16) 0.35084(11) 0.0411(7) Uani 1 1 d . . . C15 C 0.2150(2) 0.29128(19) 0.38292(14) 0.0673(11) Uani 1 1 d . . . H15 H 0.1831 0.3327 0.3851 0.081 Uiso 1 1 calc R . . C16 C 0.2892(3) 0.2838(3) 0.41197(18) 0.0943(15) Uani 1 1 d . . . H16 H 0.3063 0.3199 0.4336 0.113 Uiso 1 1 calc R . . C17 C 0.3369(3) 0.2241(3) 0.4090(2) 0.107(2) Uani 1 1 d . . . H17 H 0.3872 0.2198 0.4281 0.129 Uiso 1 1 calc R . . C18 C 0.3116(3) 0.1704(3) 0.37818(18) 0.0972(16) Uani 1 1 d . . . H18 H 0.3443 0.1294 0.3765 0.117 Uiso 1 1 calc R . . C19 C 0.2371(2) 0.1769(2) 0.34926(13) 0.0626(10) Uani 1 1 d . . . H19 H 0.2199 0.1398 0.3286 0.075 Uiso 1 1 calc R . . C20 C -0.17833(17) 0.20535(15) 0.37682(11) 0.0365(7) Uani 1 1 d . . . C21 C -0.19312(16) 0.13864(15) 0.40583(10) 0.0355(6) Uani 1 1 d . . . C22 C -0.12208(17) 0.09843(15) 0.41936(10) 0.0369(7) Uani 1 1 d . . . C23 C -0.13296(19) 0.03354(17) 0.44321(11) 0.0496(8) Uani 1 1 d . . . H23 H -0.0853 0.0057 0.4510 0.060 Uiso 1 1 calc R . . C24 C -0.2157(2) 0.01090(19) 0.45526(12) 0.0601(10) Uani 1 1 d . . . H24 H -0.2235 -0.0324 0.4712 0.072 Uiso 1 1 calc R . . C25 C -0.2865(2) 0.05210(18) 0.44382(12) 0.0559(9) Uani 1 1 d . . . H25 H -0.3416 0.0373 0.4530 0.067 Uiso 1 1 calc R . . C26 C -0.27546(17) 0.11520(17) 0.41882(11) 0.0450(8) Uani 1 1 d . . . H26 H -0.3234 0.1424 0.4106 0.054 Uiso 1 1 calc R . . C27 C 0.02379(18) 0.16311(16) 0.46846(11) 0.0402(7) Uani 1 1 d . . . C28 C -0.0107(2) 0.13908(17) 0.51324(11) 0.0515(8) Uani 1 1 d . . . H28 H -0.0580 0.1089 0.5126 0.062 Uiso 1 1 calc R . . C29 C 0.0243(2) 0.1595(2) 0.55951(13) 0.0675(10) Uani 1 1 d . . . H29 H 0.0003 0.1427 0.5895 0.081 Uiso 1 1 calc R . . C30 C 0.0931(3) 0.2036(2) 0.56125(14) 0.0743(11) Uani 1 1 d . . . H30 H 0.1150 0.2185 0.5923 0.089 Uiso 1 1 calc R . . C31 C 0.1297(3) 0.2257(3) 0.51740(16) 0.1002(17) Uani 1 1 d . . . H31 H 0.1788 0.2540 0.5184 0.120 Uiso 1 1 calc R . . C32 C 0.0944(3) 0.2065(2) 0.47105(14) 0.0873(14) Uani 1 1 d . . . H32 H 0.1191 0.2233 0.4413 0.105 Uiso 1 1 calc R . . C33 C 0.04841(17) 0.06586(14) 0.38639(10) 0.0345(6) Uani 1 1 d . . . C34 C 0.12659(19) 0.04960(18) 0.40927(13) 0.0545(9) Uani 1 1 d . . . H34 H 0.1476 0.0774 0.4355 0.065 Uiso 1 1 calc R . . C35 C 0.1736(2) -0.0088(2) 0.39268(15) 0.0702(11) Uani 1 1 d . . . H35 H 0.2254 -0.0203 0.4084 0.084 Uiso 1 1 calc R . . C36 C 0.1439(2) -0.0488(2) 0.35365(14) 0.0674(10) Uani 1 1 d . . . H36 H 0.1765 -0.0868 0.3421 0.081 Uiso 1 1 calc R . . C37 C 0.0664(2) -0.03344(18) 0.33123(14) 0.0613(10) Uani 1 1 d . . . H37 H 0.0461 -0.0614 0.3048 0.074 Uiso 1 1 calc R . . C38 C 0.01867(19) 0.02272(15) 0.34748(11) 0.0444(7) Uani 1 1 d . . . H38 H -0.0343 0.0322 0.3323 0.053 Uiso 1 1 calc R . . C39 C -0.0890(3) 0.3189(2) 0.45905(14) 0.0908(14) Uani 1 1 d . . . H39A H -0.0948 0.3649 0.4738 0.136 Uiso 1 1 calc R . . H39B H -0.0478 0.2920 0.4782 0.136 Uiso 1 1 calc R . . H39C H -0.1440 0.2954 0.4596 0.136 Uiso 1 1 calc R . . C40 C -0.1138(2) 0.37846(18) 0.38039(16) 0.0743(11) Uani 1 1 d . . . H40A H -0.1737 0.3692 0.3887 0.089 Uiso 1 1 calc R . . H40B H -0.0994 0.4249 0.3932 0.089 Uiso 1 1 calc R . . C41 C -0.1036(2) 0.37822(17) 0.32456(16) 0.0646(10) Uani 1 1 d . . . H41A H -0.1438 0.4113 0.3095 0.077 Uiso 1 1 calc R . . H41B H -0.0455 0.3928 0.3157 0.077 Uiso 1 1 calc R . . C42 C -0.1193(2) 0.3036(2) 0.24956(13) 0.0704(11) Uani 1 1 d . . . H42A H -0.1593 0.3374 0.2361 0.106 Uiso 1 1 calc R . . H42B H -0.1359 0.2572 0.2389 0.106 Uiso 1 1 calc R . . H42C H -0.0622 0.3138 0.2373 0.106 Uiso 1 1 calc R . . Cl Cl 0.07931(5) 0.49600(5) 0.42728(4) 0.0595(2) Uani 1 1 d . . . N1 N -0.05879(16) 0.32572(13) 0.40574(10) 0.0519(7) Uani 1 1 d . . . N2 N -0.12002(15) 0.30725(13) 0.30455(10) 0.0499(7) Uani 1 1 d . . . O1 O -0.13842(12) 0.13019(11) 0.28884(7) 0.0468(5) Uani 1 1 d . . . O2 O -0.24055(12) 0.24193(11) 0.36606(9) 0.0542(6) Uani 1 1 d . . . O3 O 0.13619(15) 0.53489(13) 0.45826(9) 0.0720(7) Uani 1 1 d . . . O4 O -0.00655(19) 0.5164(2) 0.43529(13) 0.1401(14) Uani 1 1 d . . . O5 O 0.0997(2) 0.50842(16) 0.37521(10) 0.0967(9) Uani 1 1 d . . . O6 O 0.0914(2) 0.42264(15) 0.43644(14) 0.1213(12) Uani 1 1 d . . . P1 P 0.08797(4) 0.24853(4) 0.31428(3) 0.03359(18) Uani 1 1 d . . . P2 P -0.01899(4) 0.14010(4) 0.40613(3) 0.03254(17) Uani 1 1 d . . . Rh Rh -0.055481(12) 0.230704(11) 0.352766(8) 0.03014(7) Uani 1 1 d . . . H1 H 0.0062 0.3435 0.4111 0.050 Uiso 1 1 d . . . H2 H -0.1856 0.2962 0.3187 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0326(15) 0.0341(16) 0.0355(16) 0.0018(13) -0.0013(12) 0.0020(12) C2 0.0368(15) 0.0329(16) 0.0338(16) -0.0007(13) 0.0031(12) -0.0005(12) C3 0.0336(14) 0.0318(16) 0.0384(17) 0.0017(13) 0.0051(12) -0.0014(12) C4 0.0374(16) 0.0448(19) 0.052(2) -0.0024(16) 0.0124(14) -0.0003(14) C5 0.0509(19) 0.053(2) 0.051(2) -0.0065(17) 0.0190(16) 0.0075(16) C6 0.066(2) 0.050(2) 0.046(2) -0.0170(16) 0.0107(17) 0.0000(17) C7 0.0502(19) 0.048(2) 0.0454(19) -0.0105(16) 0.0050(15) -0.0089(15) C8 0.0271(13) 0.0344(16) 0.0418(18) -0.0003(13) 0.0019(12) 0.0001(11) C9 0.057(2) 0.0394(19) 0.050(2) -0.0028(16) 0.0013(16) 0.0000(15) C10 0.056(2) 0.0322(18) 0.073(3) -0.0016(18) -0.0070(18) -0.0027(15) C11 0.0445(18) 0.046(2) 0.074(3) 0.0180(19) 0.0062(17) 0.0026(15) C12 0.063(2) 0.059(2) 0.048(2) 0.0120(19) 0.0053(17) 0.0039(18) C13 0.0563(19) 0.0417(19) 0.045(2) -0.0003(16) 0.0006(15) -0.0019(15) C14 0.0311(14) 0.0481(18) 0.0443(18) 0.0119(16) 0.0002(13) -0.0067(13) C15 0.067(2) 0.056(2) 0.079(3) 0.014(2) -0.027(2) -0.0152(18) C16 0.083(3) 0.094(4) 0.105(4) 0.027(3) -0.049(3) -0.044(3) C17 0.062(3) 0.148(5) 0.111(4) 0.062(4) -0.039(3) -0.021(3) C18 0.067(3) 0.127(4) 0.098(4) 0.044(3) -0.010(3) 0.032(3) C19 0.058(2) 0.068(3) 0.062(2) 0.014(2) -0.0027(18) 0.0107(18) C20 0.0290(14) 0.0394(17) 0.0410(17) -0.0077(14) 0.0017(13) -0.0010(12) C21 0.0292(14) 0.0440(18) 0.0334(16) -0.0048(14) 0.0038(12) -0.0065(12) C22 0.0303(14) 0.0441(18) 0.0361(17) 0.0007(14) 0.0000(12) -0.0081(12) C23 0.0444(18) 0.051(2) 0.053(2) 0.0122(17) -0.0053(15) -0.0091(15) C24 0.057(2) 0.066(2) 0.057(2) 0.0188(19) -0.0021(17) -0.0274(18) C25 0.0407(18) 0.072(2) 0.055(2) 0.0060(19) 0.0023(15) -0.0235(17) C26 0.0315(15) 0.059(2) 0.0440(19) 0.0001(16) 0.0030(13) -0.0073(14) C27 0.0388(15) 0.0487(19) 0.0331(17) -0.0027(14) 0.0001(13) -0.0049(14) C28 0.058(2) 0.056(2) 0.0412(19) -0.0001(16) -0.0043(16) -0.0094(16) C29 0.085(3) 0.082(3) 0.036(2) 0.0047(19) -0.0035(19) -0.014(2) C30 0.078(3) 0.105(3) 0.040(2) -0.009(2) -0.016(2) -0.017(2) C31 0.089(3) 0.148(5) 0.064(3) -0.024(3) -0.004(2) -0.064(3) C32 0.096(3) 0.127(4) 0.039(2) -0.008(2) 0.003(2) -0.071(3) C33 0.0332(15) 0.0325(16) 0.0378(17) 0.0048(13) -0.0014(12) -0.0017(12) C34 0.0374(17) 0.059(2) 0.067(2) -0.0026(19) -0.0132(16) 0.0025(15) C35 0.0377(19) 0.073(3) 0.100(3) 0.000(2) -0.0121(19) 0.0176(18) C36 0.059(2) 0.059(2) 0.084(3) -0.003(2) 0.007(2) 0.0179(18) C37 0.071(3) 0.046(2) 0.067(2) -0.0114(18) -0.0051(19) 0.0114(18) C38 0.0444(17) 0.0387(18) 0.050(2) -0.0037(15) -0.0095(15) 0.0067(14) C39 0.124(4) 0.074(3) 0.075(3) -0.029(2) 0.039(3) -0.010(3) C40 0.064(2) 0.044(2) 0.115(4) -0.024(2) 0.011(2) 0.0088(18) C41 0.051(2) 0.036(2) 0.106(3) 0.010(2) 0.000(2) 0.0070(16) C42 0.073(2) 0.073(3) 0.066(3) 0.031(2) -0.012(2) 0.004(2) Cl 0.0459(5) 0.0713(7) 0.0614(6) -0.0115(5) -0.0031(4) 0.0013(4) N1 0.0494(15) 0.0425(16) 0.0637(19) -0.0164(14) 0.0096(14) -0.0032(13) N2 0.0440(15) 0.0417(16) 0.0640(19) 0.0112(14) 0.0009(13) 0.0079(12) O1 0.0329(11) 0.0565(14) 0.0508(13) -0.0134(11) -0.0026(9) -0.0084(9) O2 0.0289(11) 0.0552(14) 0.0786(16) 0.0101(12) 0.0087(11) 0.0066(10) O3 0.0802(18) 0.0758(18) 0.0599(16) -0.0115(14) -0.0171(13) -0.0078(14) O4 0.0499(18) 0.224(4) 0.146(3) -0.043(3) 0.0111(18) 0.028(2) O5 0.118(2) 0.124(3) 0.0485(16) -0.0187(17) -0.0022(16) 0.004(2) O6 0.136(3) 0.062(2) 0.167(3) 0.009(2) -0.043(2) -0.0204(19) P1 0.0271(3) 0.0349(4) 0.0387(4) -0.0022(3) 0.0036(3) -0.0031(3) P2 0.0282(3) 0.0371(4) 0.0324(4) 0.0004(3) -0.0018(3) -0.0044(3) Rh 0.02532(10) 0.02985(12) 0.03527(13) -0.00134(10) 0.00268(9) -0.00028(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 C1 O1 1.220(3) . ? C1 C2 1.520(4) . ? C1 Rh 2.003(3) . ? C2 C3 1.394(4) . ? C2 C7 1.389(4) . ? C3 C4 1.410(4) . ? C3 P1 1.806(3) . ? C4 C5 1.365(4) . ? C4 H4 0.9300 . ? C5 C6 1.390(4) . ? C5 H5 0.9300 . ? C6 C7 1.375(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.394(4) . ? C8 C9 1.387(4) . ? C8 P1 1.849(3) . ? C9 C10 1.379(4) . ? C9 H9 0.9300 . ? C10 C11 1.364(4) . ? C10 H10 0.9300 . ? C11 C12 1.372(4) . ? C11 H11 0.9300 . ? C12 C13 1.388(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.391(4) . ? C14 C15 1.383(4) . ? C14 P1 1.832(3) . ? C15 C16 1.388(5) . ? C15 H15 0.9300 . ? C16 C17 1.354(6) . ? C16 H16 0.9300 . ? C17 C18 1.362(6) . ? C17 H17 0.9300 . ? C18 C19 1.388(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 O2 1.221(3) . ? C20 C21 1.497(4) . ? C20 Rh 2.061(3) . ? C21 C22 1.385(4) . ? C21 C26 1.393(3) . ? C22 C23 1.393(4) . ? C22 P2 1.815(3) . ? C23 C24 1.387(4) . ? C23 H23 0.9300 . ? C24 C25 1.380(4) . ? C24 H24 0.9300 . ? C25 C26 1.378(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.374(4) . ? C27 C32 1.371(4) . ? C27 P2 1.825(3) . ? C28 C29 1.390(4) . ? C28 H28 0.9300 . ? C29 C30 1.355(5) . ? C29 H29 0.9300 . ? C30 C31 1.355(5) . ? C30 H30 0.9300 . ? C31 C32 1.387(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.391(4) . ? C33 C34 1.387(4) . ? C33 P2 1.829(3) . ? C34 C35 1.396(4) . ? C34 H34 0.9300 . ? C35 C36 1.359(5) . ? C35 H35 0.9300 . ? C36 C37 1.369(4) . ? C36 H36 0.9300 . ? C37 C38 1.366(4) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 N1 1.487(4) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.481(5) . ? C40 N1 1.474(4) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N2 1.469(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N2 1.452(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Cl O3 1.410(2) . ? Cl O4 1.400(3) . ? Cl O6 1.426(3) . ? Cl O5 1.428(3) . ? N1 Rh 2.282(2) . ? N1 H1 1.0703 . ? N2 Rh 2.174(2) . ? N2 H2 1.1016 . ? P1 Rh 2.4646(7) . ? P2 Rh 2.2930(8) . ? 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 O1 C1 C2 117.9(2) . . ? O1 C1 Rh 122.6(2) . . ? C2 C1 Rh 119.45(19) . . ? C3 C2 C7 119.9(2) . . ? C3 C2 C1 120.6(2) . . ? C7 C2 C1 119.5(2) . . ? C2 C3 C4 118.6(3) . . ? C2 C3 P1 116.5(2) . . ? C4 C3 P1 124.6(2) . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 120.2(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C7 C6 C5 119.9(3) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 120.5(3) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C13 C8 C9 117.3(3) . . ? C13 C8 P1 123.1(2) . . ? C9 C8 P1 119.6(2) . . ? C10 C9 C8 121.4(3) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 120.6(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.4(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C8 C13 C12 120.7(3) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C19 C14 C15 117.5(3) . . ? C19 C14 P1 122.5(3) . . ? C15 C14 P1 119.9(2) . . ? C14 C15 C16 120.9(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 120.4(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.1(4) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C14 C19 C18 120.9(4) . . ? C14 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? O2 C20 C21 118.6(2) . . ? O2 C20 Rh 121.6(2) . . ? C21 C20 Rh 119.72(19) . . ? C22 C21 C26 119.1(3) . . ? C22 C21 C20 118.5(2) . . ? C26 C21 C20 122.4(3) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 P2 125.4(2) . . ? C21 C22 P2 114.1(2) . . ? C22 C23 C24 119.3(3) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.9(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 120.6(3) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 117.8(3) . . ? C28 C27 P2 123.6(2) . . ? C32 C27 P2 118.6(2) . . ? C27 C28 C29 120.7(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 119.5(3) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 120.4(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 121.1(3) . . ? C27 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C38 C33 C34 118.6(3) . . ? C38 C33 P2 118.4(2) . . ? C34 C33 P2 123.0(2) . . ? C33 C34 C35 119.7(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 120.4(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 120.2(3) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C33 C38 C37 120.8(3) . . ? C33 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? N1 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 N1 112.8(3) . . ? C41 C40 H40A 109.0 . . ? N1 C40 H40A 109.0 . . ? C41 C40 H40B 109.0 . . ? N1 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? N2 C41 C40 110.0(3) . . ? N2 C41 H41A 109.7 . . ? C40 C41 H41A 109.7 . . ? N2 C41 H41B 109.7 . . ? C40 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? N2 C42 H42A 109.5 . . ? N2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O3 Cl O4 111.14(19) . . ? O3 Cl O6 109.33(17) . . ? O4 Cl O6 111.7(2) . . ? O3 Cl O5 109.43(17) . . ? O4 Cl O5 108.0(2) . . ? O6 Cl O5 107.2(2) . . ? C39 N1 C40 107.8(3) . . ? C39 N1 Rh 121.1(2) . . ? C40 N1 Rh 105.8(2) . . ? C39 N1 H1 101.5 . . ? C40 N1 H1 112.8 . . ? Rh N1 H1 108.0 . . ? C42 N2 C41 113.6(3) . . ? C42 N2 Rh 123.3(2) . . ? C41 N2 Rh 108.9(2) . . ? C42 N2 H2 109.7 . . ? C41 N2 H2 102.3 . . ? Rh N2 H2 95.6 . . ? C3 P1 C14 106.15(14) . . ? C3 P1 C8 102.38(13) . . ? C14 P1 C8 101.07(12) . . ? C3 P1 Rh 98.33(9) . . ? C14 P1 Rh 121.88(9) . . ? C8 P1 Rh 124.06(8) . . ? C22 P2 C33 102.72(13) . . ? C22 P2 C27 104.49(13) . . ? C33 P2 C27 103.52(13) . . ? C22 P2 Rh 103.21(10) . . ? C33 P2 Rh 122.94(9) . . ? C27 P2 Rh 117.55(10) . . ? C1 Rh C20 88.02(11) . . ? C1 Rh N2 88.31(11) . . ? C20 Rh N2 84.97(10) . . ? C1 Rh P2 88.39(8) . . ? C20 Rh P2 82.13(8) . . ? N2 Rh P2 166.79(7) . . ? C1 Rh N1 167.68(10) . . ? C20 Rh N1 88.60(10) . . ? N2 Rh N1 79.59(10) . . ? P2 Rh N1 102.87(8) . . ? C1 Rh P1 83.76(8) . . ? C20 Rh P1 171.78(8) . . ? N2 Rh P1 94.66(7) . . ? P2 Rh P1 97.70(3) . . ? N1 Rh P1 99.43(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O6 1.07 2.11 3.074(4) 148.7 . N2 H2 O2 1.10 1.83 2.766(3) 140.1 . _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.629 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.072 #==============================================================END data_compound_8a[BF4] _database_code_depnum_ccdc_archive 'CCDC 738633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H56 Cl O4 P4 Rh2, B F4, C4 H10 O' _chemical_formula_sum 'C80 H66 B Cl F4 O5 P4 Rh2' _chemical_formula_weight 1630.19 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' Cl Cl 0.1484 0.1585 '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' 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' B B 0.0013 0.0007 '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' 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 C2/c 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' '-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 17.918(2) _cell_length_b 18.406(2) _cell_length_c 20.657(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.365(3) _cell_angle_gamma 90.00 _cell_volume 6806.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25936 _diffrn_reflns_av_R_equivalents 0.1735 _diffrn_reflns_av_sigmaI/netI 0.2341 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6001 _reflns_number_gt 2267 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The BF4 anion was included with fixed isotropic contributions. The final refinement show high values of residual non-modelled electronic density.Therefore, the Squeeze program was used to calculate to solvent disordered area and to remove its contribution to the overal intensity data. 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^)+(0.1195P)^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 6001 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1841 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2442 _refine_ls_wR_factor_gt 0.2052 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.877 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0157(6) 0.6148(7) 0.8908(5) 0.049(3) Uani 1 1 d . . . C2 C 0.0771(6) 0.6107(7) 0.9439(5) 0.048(3) Uani 1 1 d . . . C3 C 0.1219(7) 0.6722(7) 0.9540(5) 0.048(3) Uani 1 1 d . . . C4 C 0.1751(7) 0.6710(7) 1.0055(6) 0.059(4) Uani 1 1 d . . . H4 H 0.2045 0.7118 1.0140 0.070 Uiso 1 1 calc R . . C5 C 0.1846(8) 0.6095(9) 1.0441(7) 0.083(5) Uani 1 1 d . . . H5 H 0.2202 0.6093 1.0782 0.100 Uiso 1 1 calc R . . C6 C 0.1407(8) 0.5482(9) 1.0314(7) 0.094(6) Uani 1 1 d . . . H6 H 0.1475 0.5069 1.0569 0.112 Uiso 1 1 calc R . . C7 C 0.0866(7) 0.5483(7) 0.9808(6) 0.063(4) Uani 1 1 d . . . H7 H 0.0576 0.5072 0.9720 0.075 Uiso 1 1 calc R . . C8 C 0.1936(6) 0.7459(7) 0.8532(5) 0.044(3) Uani 1 1 d . . . C9 C 0.2013(8) 0.7965(10) 0.8046(8) 0.103(6) Uani 1 1 d . . . H9 H 0.1661 0.8333 0.7988 0.124 Uiso 1 1 calc R . . C10 C 0.2625(10) 0.7926(14) 0.7636(11) 0.173(12) Uani 1 1 d . . . H10 H 0.2650 0.8233 0.7280 0.208 Uiso 1 1 calc R . . C11 C 0.3176(9) 0.7436(11) 0.7766(9) 0.105(6) Uani 1 1 d . . . H11 H 0.3607 0.7455 0.7531 0.126 Uiso 1 1 calc R . . C12 C 0.3117(8) 0.6926(9) 0.8225(8) 0.089(5) Uani 1 1 d . . . H12 H 0.3479 0.6568 0.8289 0.107 Uiso 1 1 calc R . . C13 C 0.2491(7) 0.6956(9) 0.8604(6) 0.074(4) Uani 1 1 d . . . H13 H 0.2449 0.6609 0.8927 0.089 Uiso 1 1 calc R . . C14 C 0.1047(6) 0.8292(6) 0.9366(6) 0.045(3) Uani 1 1 d . . . C15 C 0.0889(8) 0.8931(9) 0.8971(7) 0.081(5) Uani 1 1 d . . . H15 H 0.0842 0.8883 0.8523 0.098 Uiso 1 1 calc R . . C16 C 0.0805(8) 0.9620(9) 0.9250(9) 0.089(5) Uani 1 1 d . . . H16 H 0.0677 1.0026 0.9003 0.106 Uiso 1 1 calc R . . C17 C 0.0929(8) 0.9660(9) 0.9947(9) 0.086(5) Uani 1 1 d . . . H17 H 0.0929 1.0112 1.0149 0.103 Uiso 1 1 calc R . . C18 C 0.1039(8) 0.9083(9) 1.0297(7) 0.076(5) Uani 1 1 d . . . H18 H 0.1090 0.9127 1.0745 0.092 Uiso 1 1 calc R . . C19 C 0.1084(8) 0.8402(8) 1.0018(7) 0.073(4) Uani 1 1 d . . . H19 H 0.1141 0.8000 1.0289 0.087 Uiso 1 1 calc R . . C20 C -0.0830(6) 0.6561(6) 0.7824(5) 0.037(3) Uani 1 1 d . . . C21 C -0.1536(6) 0.6332(7) 0.8168(5) 0.051(3) Uani 1 1 d . . . C22 C -0.1631(6) 0.6657(6) 0.8779(6) 0.045(3) Uani 1 1 d . . . C23 C -0.2246(7) 0.6464(8) 0.9130(6) 0.069(4) Uani 1 1 d . . . H23 H -0.2324 0.6670 0.9532 0.083 Uiso 1 1 calc R . . C24 C -0.2744(7) 0.5949(9) 0.8860(8) 0.087(5) Uani 1 1 d . . . H24 H -0.3154 0.5811 0.9092 0.104 Uiso 1 1 calc R . . C25 C -0.2647(8) 0.5647(8) 0.8275(7) 0.080(5) Uani 1 1 d . . . H25 H -0.2988 0.5304 0.8115 0.096 Uiso 1 1 calc R . . C26 C -0.2059(7) 0.5837(7) 0.7913(6) 0.058(4) Uani 1 1 d . . . H26 H -0.2006 0.5639 0.7503 0.069 Uiso 1 1 calc R . . C27 C -0.0759(6) 0.7315(9) 0.9859(6) 0.060(4) Uani 1 1 d . . . C28 C -0.0695(8) 0.6658(8) 1.0185(6) 0.070(4) Uani 1 1 d . . . H28 H -0.0781 0.6236 0.9946 0.085 Uiso 1 1 calc R . . C29 C -0.0516(10) 0.6586(11) 1.0832(7) 0.099(6) Uani 1 1 d . . . H29 H -0.0436 0.6138 1.1030 0.119 Uiso 1 1 calc R . . C30 C -0.0462(9) 0.7242(11) 1.1170(7) 0.087(5) Uani 1 1 d . . . H30 H -0.0403 0.7226 1.1619 0.104 Uiso 1 1 calc R . . C31 C -0.0490(8) 0.7883(10) 1.0885(7) 0.079(5) Uani 1 1 d . . . H31 H -0.0395 0.8303 1.1125 0.095 Uiso 1 1 calc R . . C32 C -0.0662(8) 0.7926(7) 1.0225(6) 0.065(4) Uani 1 1 d . . . H32 H -0.0712 0.8380 1.0030 0.078 Uiso 1 1 calc R . . C33 C -0.1381(7) 0.8196(7) 0.8852(6) 0.056(4) Uani 1 1 d . . . C34 C -0.2117(8) 0.8311(9) 0.9086(7) 0.085(5) Uani 1 1 d . . . H34 H -0.2361 0.7931 0.9286 0.102 Uiso 1 1 calc R . . C35 C -0.2464(9) 0.8966(11) 0.9017(9) 0.111(6) Uani 1 1 d . . . H35 H -0.2940 0.9028 0.9172 0.133 Uiso 1 1 calc R . . C36 C -0.2113(9) 0.9549(8) 0.8717(8) 0.081(5) Uani 1 1 d . . . H36 H -0.2358 0.9994 0.8688 0.097 Uiso 1 1 calc R . . C37 C -0.1438(11) 0.9486(8) 0.8472(8) 0.092(5) Uani 1 1 d . . . H37 H -0.1223 0.9868 0.8252 0.111 Uiso 1 1 calc R . . C38 C -0.1057(8) 0.8802(8) 0.8562(6) 0.068(4) Uani 1 1 d . . . H38 H -0.0573 0.8761 0.8421 0.081 Uiso 1 1 calc R . . Cl Cl 0.0000 0.7977(2) 0.7500 0.0469(10) Uani 1 2 d S . . O1 O -0.0206(5) 0.5565(5) 0.8827(4) 0.066(3) Uani 1 1 d . . . O2 O 0.0816(4) 0.6450(4) 0.7757(3) 0.0432(19) Uani 1 1 d . . . P1 P 0.10793(16) 0.74439(17) 0.89561(14) 0.0404(8) Uani 1 1 d . . . P2 P -0.09183(17) 0.73387(18) 0.89816(14) 0.0442(8) Uani 1 1 d . . . Rh1 Rh 0.00179(5) 0.70053(5) 0.83530(4) 0.0373(3) Uani 1 1 d . . . B1 B 1.0000 0.0787 0.7500 0.206 Uiso 1 2 d S . . F1 F 1.0317 0.0870 0.6947 0.200 Uiso 1 1 d . . . F2 F 0.9459 0.0512 0.7238 0.200 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.047(8) 0.055(9) 0.044(7) 0.002(6) -0.009(6) -0.016(6) C2 0.029(7) 0.075(10) 0.041(7) 0.004(7) 0.002(5) -0.013(6) C3 0.052(8) 0.067(9) 0.024(6) 0.011(6) -0.009(6) -0.002(7) C4 0.055(8) 0.068(9) 0.051(8) 0.026(7) -0.002(7) -0.010(7) C5 0.062(10) 0.099(13) 0.086(11) 0.039(10) -0.025(8) -0.008(9) C6 0.076(11) 0.099(13) 0.104(13) 0.063(10) -0.019(10) -0.025(10) C7 0.064(9) 0.050(9) 0.073(9) 0.024(7) -0.023(7) -0.019(7) C8 0.037(7) 0.063(9) 0.032(7) 0.007(6) 0.003(5) -0.013(6) C9 0.057(10) 0.159(17) 0.096(13) 0.042(12) 0.031(9) 0.019(11) C10 0.062(12) 0.27(3) 0.19(2) 0.14(2) 0.057(14) 0.036(16) C11 0.060(11) 0.145(18) 0.111(15) 0.026(13) 0.030(10) -0.008(11) C12 0.074(11) 0.099(13) 0.096(13) 0.013(10) 0.034(10) 0.029(10) C13 0.053(9) 0.121(13) 0.050(8) 0.026(9) 0.013(7) -0.006(9) C14 0.050(8) 0.044(8) 0.040(7) -0.003(6) -0.002(6) -0.025(6) C15 0.097(12) 0.083(12) 0.065(10) -0.016(9) 0.009(9) -0.040(10) C16 0.084(12) 0.060(11) 0.121(15) -0.005(10) -0.007(10) -0.010(9) C17 0.067(10) 0.084(13) 0.106(15) -0.053(11) 0.000(10) 0.000(9) C18 0.100(12) 0.066(11) 0.062(10) -0.020(9) -0.005(9) 0.010(10) C19 0.094(11) 0.069(10) 0.054(9) -0.011(8) 0.001(8) -0.009(9) C20 0.039(7) 0.047(7) 0.024(6) 0.006(5) 0.003(5) 0.004(6) C21 0.036(7) 0.075(9) 0.041(7) 0.001(7) 0.005(6) -0.014(6) C22 0.033(7) 0.051(8) 0.050(8) -0.009(6) -0.001(6) -0.006(6) C23 0.044(8) 0.091(11) 0.073(10) -0.024(8) 0.033(7) -0.027(8) C24 0.029(8) 0.123(14) 0.110(14) -0.007(11) 0.034(8) -0.022(8) C25 0.050(9) 0.115(14) 0.075(11) -0.020(10) 0.015(8) -0.036(9) C26 0.046(8) 0.080(10) 0.047(8) -0.008(7) 0.002(6) -0.018(7) C27 0.041(8) 0.102(12) 0.036(8) 0.016(8) -0.001(6) -0.010(7) C28 0.087(11) 0.081(11) 0.044(9) -0.011(8) 0.017(8) -0.015(9) C29 0.142(16) 0.115(15) 0.041(10) 0.009(10) 0.008(10) 0.022(13) C30 0.096(13) 0.117(16) 0.047(10) 0.015(11) 0.009(9) -0.011(11) C31 0.075(10) 0.100(13) 0.063(10) -0.041(10) -0.006(8) -0.033(10) C32 0.101(11) 0.055(9) 0.038(8) -0.006(7) -0.009(7) 0.000(8) C33 0.048(8) 0.079(11) 0.039(7) 0.001(7) 0.001(6) 0.008(7) C34 0.070(11) 0.087(12) 0.101(12) 0.027(10) 0.032(9) 0.026(9) C35 0.053(11) 0.109(16) 0.174(19) 0.001(14) 0.028(11) 0.014(11) C36 0.070(11) 0.048(10) 0.123(14) -0.017(10) -0.003(10) 0.009(9) C37 0.121(16) 0.048(11) 0.109(14) -0.012(9) 0.019(12) -0.003(10) C38 0.065(10) 0.064(11) 0.076(10) -0.009(8) 0.028(8) -0.011(8) Cl 0.054(3) 0.048(2) 0.038(2) 0.000 -0.0040(19) 0.000 O1 0.077(6) 0.057(6) 0.062(6) 0.011(5) -0.022(5) -0.027(5) O2 0.035(4) 0.061(5) 0.033(5) 0.004(4) -0.007(4) 0.001(4) P1 0.0352(17) 0.050(2) 0.0353(18) 0.0035(15) -0.0026(13) -0.0056(15) P2 0.0427(19) 0.056(2) 0.0338(18) -0.0044(15) 0.0005(14) -0.0049(16) Rh1 0.0305(5) 0.0524(6) 0.0290(5) -0.0003(5) -0.0007(3) -0.0053(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.263(12) . ? C1 C2 1.523(14) . ? C1 Rh1 1.960(12) . ? C2 C3 1.399(15) . ? C2 C7 1.385(15) . ? C3 C4 1.399(15) . ? C3 P1 1.805(11) . ? C4 C5 1.391(16) . ? C4 H4 0.9300 . ? C5 C6 1.394(18) . ? C5 H5 0.9300 . ? C6 C7 1.396(16) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.363(17) . ? C8 C9 1.380(17) . ? C8 P1 1.798(11) . ? C9 C10 1.42(2) . ? C9 H9 0.9300 . ? C10 C11 1.35(2) . ? C10 H10 0.9300 . ? C11 C12 1.34(2) . ? C11 H11 0.9300 . ? C12 C13 1.395(17) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.361(15) . ? C14 C15 1.453(18) . ? C14 P1 1.778(12) . ? C15 C16 1.403(19) . ? C15 H15 0.9300 . ? C16 C17 1.45(2) . ? C16 H16 0.9300 . ? C17 C18 1.296(19) . ? C17 H17 0.9300 . ? C18 C19 1.383(18) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 O2 1.220(11) 2_556 ? C20 C21 1.534(14) . ? C20 Rh1 2.009(11) . ? C21 C22 1.413(15) . ? C21 C26 1.395(15) . ? C22 C23 1.389(15) . ? C22 P2 1.827(11) . ? C23 C24 1.401(17) . ? C23 H23 0.9300 . ? C24 C25 1.347(18) . ? C24 H24 0.9300 . ? C25 C26 1.362(16) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.363(17) . ? C27 C28 1.386(18) . ? C27 P2 1.823(12) . ? C28 C29 1.369(17) . ? C28 H28 0.9300 . ? C29 C30 1.40(2) . ? C29 H29 0.9300 . ? C30 C31 1.318(19) . ? C30 H30 0.9300 . ? C31 C32 1.387(17) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.404(16) . ? C33 C34 1.438(17) . ? C33 P2 1.798(13) . ? C34 C35 1.36(2) . ? C34 H34 0.9300 . ? C35 C36 1.40(2) . ? C35 H35 0.9300 . ? C36 C37 1.335(19) . ? C36 H36 0.9300 . ? C37 C38 1.440(19) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? Cl Rh1 2.510(3) 2_556 ? Cl Rh1 2.510(3) . ? O2 C20 1.220(11) 2_556 ? O2 Rh1 2.179(7) . ? P1 Rh1 2.372(3) . ? P2 Rh1 2.249(3) . ? B1 F2 1.2025 . ? B1 F2 1.2025 2_756 ? B1 F1 1.3055 . ? B1 F1 1.3055 2_756 ? 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 O1 C1 C2 114.0(10) . . ? O1 C1 Rh1 123.6(8) . . ? C2 C1 Rh1 122.1(9) . . ? C3 C2 C7 122.2(10) . . ? C3 C2 C1 117.4(11) . . ? C7 C2 C1 120.4(11) . . ? C2 C3 C4 118.0(11) . . ? C2 C3 P1 115.7(8) . . ? C4 C3 P1 126.2(10) . . ? C3 C4 C5 120.8(13) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.8(13) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 120.6(13) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 118.6(12) . . ? C2 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C13 C8 C9 116.3(12) . . ? C13 C8 P1 124.8(10) . . ? C9 C8 P1 118.6(10) . . ? C8 C9 C10 120.3(16) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.3(17) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 122.0(16) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C13 117.2(15) . . ? C11 C12 H12 121.4 . . ? C13 C12 H12 121.4 . . ? C8 C13 C12 124.5(13) . . ? C8 C13 H13 117.8 . . ? C12 C13 H13 117.8 . . ? C19 C14 C15 115.8(12) . . ? C19 C14 P1 126.9(11) . . ? C15 C14 P1 117.0(9) . . ? C16 C15 C14 121.5(13) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 116.1(15) . . ? C15 C16 H16 121.9 . . ? C17 C16 H16 121.9 . . ? C18 C17 C16 121.7(15) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 121.4(15) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C14 C19 C18 123.1(14) . . ? C14 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? O2 C20 C21 117.5(10) 2_556 . ? O2 C20 Rh1 123.9(8) 2_556 . ? C21 C20 Rh1 118.6(7) . . ? C22 C21 C26 120.6(10) . . ? C22 C21 C20 115.5(10) . . ? C26 C21 C20 123.9(11) . . ? C21 C22 C23 119.0(11) . . ? C21 C22 P2 112.7(8) . . ? C23 C22 P2 128.2(9) . . ? C24 C23 C22 118.1(12) . . ? C24 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C25 C24 C23 122.1(12) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C26 C25 C24 121.2(13) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C21 118.9(12) . . ? C25 C26 H26 120.5 . . ? C21 C26 H26 120.5 . . ? C32 C27 C28 116.3(12) . . ? C32 C27 P2 122.9(11) . . ? C28 C27 P2 120.7(11) . . ? C29 C28 C27 124.8(15) . . ? C29 C28 H28 117.6 . . ? C27 C28 H28 117.6 . . ? C28 C29 C30 114.4(16) . . ? C28 C29 H29 122.8 . . ? C30 C29 H29 122.8 . . ? C31 C30 C29 123.4(15) . . ? C31 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? C30 C31 C32 119.5(14) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C27 C32 C31 121.1(13) . . ? C27 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C38 C33 C34 115.3(12) . . ? C38 C33 P2 124.4(10) . . ? C34 C33 P2 120.2(11) . . ? C35 C34 C33 121.0(15) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 120.9(15) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C37 C36 C35 122.0(15) . . ? C37 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? C36 C37 C38 117.4(15) . . ? C36 C37 H37 121.3 . . ? C38 C37 H37 121.3 . . ? C33 C38 C37 123.2(13) . . ? C33 C38 H38 118.4 . . ? C37 C38 H38 118.4 . . ? Rh1 Cl Rh1 89.09(14) 2_556 . ? C20 O2 Rh1 121.3(7) 2_556 . ? C14 P1 C8 105.3(5) . . ? C14 P1 C3 109.5(6) . . ? C8 P1 C3 103.9(6) . . ? C14 P1 Rh1 120.5(4) . . ? C8 P1 Rh1 115.5(4) . . ? C3 P1 Rh1 100.8(4) . . ? C33 P2 C22 104.8(6) . . ? C33 P2 C27 102.8(6) . . ? C22 P2 C27 106.9(6) . . ? C33 P2 Rh1 120.3(4) . . ? C22 P2 Rh1 102.2(4) . . ? C27 P2 Rh1 118.5(4) . . ? C1 Rh1 C20 93.7(4) . . ? C1 Rh1 O2 83.3(4) . . ? C20 Rh1 O2 90.1(3) . . ? C1 Rh1 P2 87.8(4) . . ? C20 Rh1 P2 81.9(3) . . ? O2 Rh1 P2 167.6(2) . . ? C1 Rh1 P1 83.5(3) . . ? C20 Rh1 P1 175.2(3) . . ? O2 Rh1 P1 85.73(19) . . ? P2 Rh1 P1 101.83(11) . . ? C1 Rh1 Cl 169.1(4) . . ? C20 Rh1 Cl 85.5(3) . . ? O2 Rh1 Cl 85.8(2) . . ? P2 Rh1 Cl 102.86(10) . . ? P1 Rh1 Cl 96.48(9) . . ? F2 B1 F2 130.1 . 2_756 ? F2 B1 F1 91.6 . . ? F2 B1 F1 94.1 2_756 . ? F2 B1 F1 94.1 . 2_756 ? F2 B1 F1 91.6 2_756 2_756 ? F1 B1 F1 166.6 . 2_756 ? 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 O1 C1 C2 C3 177.3(11) . . . . ? Rh1 C1 C2 C3 2.9(15) . . . . ? O1 C1 C2 C7 -3.4(17) . . . . ? Rh1 C1 C2 C7 -177.9(9) . . . . ? C7 C2 C3 C4 -3.5(18) . . . . ? C1 C2 C3 C4 175.7(11) . . . . ? C7 C2 C3 P1 173.4(10) . . . . ? C1 C2 C3 P1 -7.4(14) . . . . ? C2 C3 C4 C5 2.0(19) . . . . ? P1 C3 C4 C5 -174.5(11) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C4 C5 C6 C7 -1(2) . . . . ? C3 C2 C7 C6 3(2) . . . . ? C1 C2 C7 C6 -176.3(13) . . . . ? C5 C6 C7 C2 -1(2) . . . . ? C13 C8 C9 C10 3(2) . . . . ? P1 C8 C9 C10 -170.4(16) . . . . ? C8 C9 C10 C11 -7(3) . . . . ? C9 C10 C11 C12 8(4) . . . . ? C10 C11 C12 C13 -5(3) . . . . ? C9 C8 C13 C12 0(2) . . . . ? P1 C8 C13 C12 172.9(12) . . . . ? C11 C12 C13 C8 1(2) . . . . ? C19 C14 C15 C16 2.0(19) . . . . ? P1 C14 C15 C16 176.0(11) . . . . ? C14 C15 C16 C17 4(2) . . . . ? C15 C16 C17 C18 -6(2) . . . . ? C16 C17 C18 C19 3(2) . . . . ? C15 C14 C19 C18 -5(2) . . . . ? P1 C14 C19 C18 -178.7(11) . . . . ? C17 C18 C19 C14 3(2) . . . . ? O2 C20 C21 C22 -161.6(10) 2_556 . . . ? Rh1 C20 C21 C22 19.4(14) . . . . ? O2 C20 C21 C26 18.8(17) 2_556 . . . ? Rh1 C20 C21 C26 -160.2(10) . . . . ? C26 C21 C22 C23 1.4(19) . . . . ? C20 C21 C22 C23 -178.2(11) . . . . ? C26 C21 C22 P2 -175.4(10) . . . . ? C20 C21 C22 P2 4.9(13) . . . . ? C21 C22 C23 C24 0(2) . . . . ? P2 C22 C23 C24 176.6(11) . . . . ? C22 C23 C24 C25 -1(2) . . . . ? C23 C24 C25 C26 -1(3) . . . . ? C24 C25 C26 C21 2(2) . . . . ? C22 C21 C26 C25 -2.7(19) . . . . ? C20 C21 C26 C25 176.9(12) . . . . ? C32 C27 C28 C29 -3(2) . . . . ? P2 C27 C28 C29 174.4(12) . . . . ? C27 C28 C29 C30 5(2) . . . . ? C28 C29 C30 C31 -8(3) . . . . ? C29 C30 C31 C32 7(3) . . . . ? C28 C27 C32 C31 2(2) . . . . ? P2 C27 C32 C31 -175.4(10) . . . . ? C30 C31 C32 C27 -4(2) . . . . ? C38 C33 C34 C35 1(2) . . . . ? P2 C33 C34 C35 177.1(14) . . . . ? C33 C34 C35 C36 0(3) . . . . ? C34 C35 C36 C37 2(3) . . . . ? C35 C36 C37 C38 -4(3) . . . . ? C34 C33 C38 C37 -3(2) . . . . ? P2 C33 C38 C37 -179.2(11) . . . . ? C36 C37 C38 C33 4(2) . . . . ? C19 C14 P1 C8 -114.1(12) . . . . ? C15 C14 P1 C8 72.8(11) . . . . ? C19 C14 P1 C3 -2.9(13) . . . . ? C15 C14 P1 C3 -176.1(10) . . . . ? C19 C14 P1 Rh1 113.1(11) . . . . ? C15 C14 P1 Rh1 -60.1(11) . . . . ? C13 C8 P1 C14 123.0(12) . . . . ? C9 C8 P1 C14 -64.4(12) . . . . ? C13 C8 P1 C3 7.9(13) . . . . ? C9 C8 P1 C3 -179.5(12) . . . . ? C13 C8 P1 Rh1 -101.4(11) . . . . ? C9 C8 P1 Rh1 71.2(12) . . . . ? C2 C3 P1 C14 135.6(9) . . . . ? C4 C3 P1 C14 -47.8(13) . . . . ? C2 C3 P1 C8 -112.3(10) . . . . ? C4 C3 P1 C8 64.3(12) . . . . ? C2 C3 P1 Rh1 7.6(10) . . . . ? C4 C3 P1 Rh1 -175.8(10) . . . . ? C38 C33 P2 C22 -139.0(11) . . . . ? C34 C33 P2 C22 44.8(12) . . . . ? C38 C33 P2 C27 109.5(11) . . . . ? C34 C33 P2 C27 -66.7(12) . . . . ? C38 C33 P2 Rh1 -24.9(13) . . . . ? C34 C33 P2 Rh1 158.9(9) . . . . ? C21 C22 P2 C33 103.8(9) . . . . ? C23 C22 P2 C33 -72.7(13) . . . . ? C21 C22 P2 C27 -147.6(9) . . . . ? C23 C22 P2 C27 35.9(14) . . . . ? C21 C22 P2 Rh1 -22.4(9) . . . . ? C23 C22 P2 Rh1 161.1(11) . . . . ? C32 C27 P2 C33 -29.3(13) . . . . ? C28 C27 P2 C33 153.9(11) . . . . ? C32 C27 P2 C22 -139.3(11) . . . . ? C28 C27 P2 C22 43.9(12) . . . . ? C32 C27 P2 Rh1 106.1(11) . . . . ? C28 C27 P2 Rh1 -70.7(11) . . . . ? O1 C1 Rh1 C20 4.0(11) . . . . ? C2 C1 Rh1 C20 177.9(9) . . . . ? O1 C1 Rh1 O2 -85.7(11) . . . . ? C2 C1 Rh1 O2 88.2(9) . . . . ? O1 C1 Rh1 P2 85.7(11) . . . . ? C2 C1 Rh1 P2 -100.4(9) . . . . ? O1 C1 Rh1 P1 -172.1(11) . . . . ? C2 C1 Rh1 P1 1.8(9) . . . . ? O1 C1 Rh1 Cl -82(2) . . . . ? C2 C1 Rh1 Cl 92.4(19) . . . . ? O2 C20 Rh1 C1 -118.8(10) 2_556 . . . ? C21 C20 Rh1 C1 60.2(9) . . . . ? O2 C20 Rh1 O2 -35.5(9) 2_556 . . . ? C21 C20 Rh1 O2 143.4(8) . . . . ? O2 C20 Rh1 P2 154.0(10) 2_556 . . . ? C21 C20 Rh1 P2 -27.1(8) . . . . ? O2 C20 Rh1 P1 -64(4) 2_556 . . . ? C21 C20 Rh1 P1 115(3) . . . . ? O2 C20 Rh1 Cl 50.3(9) 2_556 . . . ? C21 C20 Rh1 Cl -130.7(8) . . . . ? C20 O2 Rh1 C1 154.1(9) 2_556 . . . ? C20 O2 Rh1 C20 60.4(7) 2_556 . . . ? C20 O2 Rh1 P2 110.0(11) 2_556 . . . ? C20 O2 Rh1 P1 -121.9(8) 2_556 . . . ? C20 O2 Rh1 Cl -25.1(8) 2_556 . . . ? C33 P2 Rh1 C1 175.0(6) . . . . ? C22 P2 Rh1 C1 -69.6(5) . . . . ? C27 P2 Rh1 C1 47.5(7) . . . . ? C33 P2 Rh1 C20 -90.9(6) . . . . ? C22 P2 Rh1 C20 24.5(5) . . . . ? C27 P2 Rh1 C20 141.6(6) . . . . ? C33 P2 Rh1 O2 -141.2(10) . . . . ? C22 P2 Rh1 O2 -25.8(10) . . . . ? C27 P2 Rh1 O2 91.3(11) . . . . ? C33 P2 Rh1 P1 92.1(5) . . . . ? C22 P2 Rh1 P1 -152.5(4) . . . . ? C27 P2 Rh1 P1 -35.4(6) . . . . ? C33 P2 Rh1 Cl -7.5(5) . . . . ? C22 P2 Rh1 Cl 107.9(4) . . . . ? C27 P2 Rh1 Cl -135.0(6) . . . . ? C14 P1 Rh1 C1 -125.0(6) . . . . ? C8 P1 Rh1 C1 106.6(6) . . . . ? C3 P1 Rh1 C1 -4.6(5) . . . . ? C14 P1 Rh1 C20 180(100) . . . . ? C8 P1 Rh1 C20 52(4) . . . . ? C3 P1 Rh1 C20 -60(4) . . . . ? C14 P1 Rh1 O2 151.3(5) . . . . ? C8 P1 Rh1 O2 22.9(5) . . . . ? C3 P1 Rh1 O2 -88.3(4) . . . . ? C14 P1 Rh1 P2 -38.7(5) . . . . ? C8 P1 Rh1 P2 -167.0(5) . . . . ? C3 P1 Rh1 P2 81.8(4) . . . . ? C14 P1 Rh1 Cl 66.0(5) . . . . ? C8 P1 Rh1 Cl -62.4(5) . . . . ? C3 P1 Rh1 Cl -173.6(4) . . . . ? Rh1 Cl Rh1 C1 37.8(17) 2_556 . . . ? Rh1 Cl Rh1 C20 -48.5(3) 2_556 . . . ? Rh1 Cl Rh1 O2 41.93(18) 2_556 . . . ? Rh1 Cl Rh1 P2 -129.12(9) 2_556 . . . ? Rh1 Cl Rh1 P1 127.14(9) 2_556 . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.432 0.750 146 76 ' ' 2 0.000 0.568 0.250 146 74 ' ' 3 0.500 0.068 0.250 146 74 ' ' 4 0.500 0.932 0.750 146 76 ' ' _platon_squeeze_details ; The final refinement show high values of residual non-modelled electronic density.Therefore, the Squeeze program was used to calculate to solvent disordered area and to remove its contribution to the overal intensity data.An improvement was observed in all refinement parameters and residual when this procedure is applied ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.864 _refine_diff_density_min -1.276 _refine_diff_density_rms 0.164 #=======================================================================END data_compound_8b[ClO4] _database_code_depnum_ccdc_archive 'CCDC 738634' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H56 Cl O4 P4 Rh2, Cl O4' _chemical_formula_sum 'C76 H56 Cl2 O8 P4 Rh2' _chemical_formula_weight 1497.81 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.2966(12) _cell_length_b 11.8233(7) _cell_length_c 28.3790(16) _cell_angle_alpha 90.00 _cell_angle_beta 98.8240(10) _cell_angle_gamma 90.00 _cell_volume 6729.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50730 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11825 _reflns_number_gt 6562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Due to a non-resolvable positional disorder, the carbon atoms of one phenyl ring were refined with restrained C-C distances. Two carbon atoms in this phenyl ring and the oxygen atoms of the ClO4--- group were refined isotropically. 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^)+(0.0756P)^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 11825 _refine_ls_number_parameters 799 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1514 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.49966(2) 0.26189(4) 0.223067(16) 0.02465(14) Uani 1 1 d . . . Rh2 Rh 0.57839(2) 0.24813(4) 0.344865(15) 0.02418(14) Uani 1 1 d . . . P1 P 0.43802(8) 0.42459(14) 0.19214(6) 0.0308(4) Uani 1 1 d . . . P2 P 0.45249(8) 0.12975(14) 0.17063(6) 0.0296(4) Uani 1 1 d . . . P3 P 0.69676(8) 0.23146(13) 0.36353(5) 0.0271(4) Uani 1 1 d . . . P4 P 0.55529(8) 0.35928(14) 0.40478(6) 0.0300(4) Uani 1 1 d . . . O1 O 0.6087(2) 0.2467(4) 0.17234(15) 0.0434(12) Uani 1 1 d . . . O2 O 0.58422(19) 0.1231(3) 0.29093(14) 0.0299(10) Uani 1 1 d . . . O3 O 0.5283(2) 0.0587(4) 0.38940(17) 0.0487(13) Uani 1 1 d . . . O4 O 0.44623(19) 0.2409(3) 0.28805(14) 0.0306(10) Uani 1 1 d . . . Cl1 Cl 0.57257(8) 0.38668(12) 0.27714(5) 0.0301(4) Uani 1 1 d . . . C1 C 0.5563(3) 0.2967(5) 0.1735(2) 0.0294(15) Uani 1 1 d . . . C2 C 0.5356(3) 0.3902(5) 0.1380(2) 0.0315(15) Uani 1 1 d . . . C3 C 0.4809(3) 0.4599(5) 0.1423(2) 0.0318(16) Uani 1 1 d . . . C4 C 0.4649(4) 0.5462(6) 0.1099(3) 0.050(2) Uani 1 1 d . . . H4 H 0.4304 0.5956 0.1136 0.060 Uiso 1 1 calc R . . C5 C 0.4996(4) 0.5601(7) 0.0721(3) 0.059(2) Uani 1 1 d . . . H5 H 0.4870 0.6166 0.0498 0.071 Uiso 1 1 calc R . . C6 C 0.5534(4) 0.4902(7) 0.0672(3) 0.054(2) Uani 1 1 d . . . H6 H 0.5770 0.5003 0.0419 0.064 Uiso 1 1 calc R . . C7 C 0.5713(3) 0.4062(6) 0.1003(2) 0.0404(17) Uani 1 1 d . . . H7 H 0.6074 0.3597 0.0975 0.049 Uiso 1 1 calc R . . C8 C 0.4365(3) 0.5487(5) 0.2282(2) 0.0424(18) Uani 1 1 d D . . C11 C 0.4263(5) 0.7363(7) 0.2878(4) 0.097(4) Uani 1 1 d D . . H11 H 0.4180 0.8005 0.3049 0.117 Uiso 1 1 calc R . . C13 C 0.4096(4) 0.5397(6) 0.2700(2) 0.076(3) Uani 1 1 d D . . H13 H 0.3947 0.4694 0.2785 0.091 Uiso 1 1 calc R . . C12 C 0.4040(4) 0.6313(6) 0.2996(3) 0.082(3) Uani 1 1 d D . . H12 H 0.3853 0.6220 0.3273 0.099 Uiso 1 1 calc R . . C14 C 0.3486(3) 0.4071(5) 0.1712(2) 0.0340(16) Uani 1 1 d . . . C15 C 0.3123(4) 0.4658(6) 0.1345(3) 0.057(2) Uani 1 1 d . . . H15 H 0.3339 0.5161 0.1167 0.068 Uiso 1 1 calc R . . C16 C 0.2440(4) 0.4514(7) 0.1233(3) 0.060(2) Uani 1 1 d . . . H16 H 0.2198 0.4922 0.0985 0.072 Uiso 1 1 calc R . . C17 C 0.2127(4) 0.3778(7) 0.1488(3) 0.060(2) Uani 1 1 d . . . H17 H 0.1669 0.3679 0.1411 0.072 Uiso 1 1 calc R . . C18 C 0.2476(4) 0.3173(7) 0.1859(3) 0.057(2) Uani 1 1 d . . . H18 H 0.2258 0.2666 0.2032 0.068 Uiso 1 1 calc R . . C19 C 0.3151(3) 0.3333(6) 0.1967(2) 0.0431(18) Uani 1 1 d . . . H19 H 0.3389 0.2932 0.2219 0.052 Uiso 1 1 calc R . . C20 C 0.5556(3) 0.1267(5) 0.2489(2) 0.0290(15) Uani 1 1 d . . . C21 C 0.5601(3) 0.0251(5) 0.2195(2) 0.0292(15) Uani 1 1 d . . . C22 C 0.5122(3) 0.0145(5) 0.1786(2) 0.0318(16) Uani 1 1 d . . . C23 C 0.5111(3) -0.0796(6) 0.1499(2) 0.0448(19) Uani 1 1 d . . . H23 H 0.4791 -0.0865 0.1229 0.054 Uiso 1 1 calc R . . C24 C 0.5576(4) -0.1631(6) 0.1615(3) 0.051(2) Uani 1 1 d . . . H24 H 0.5571 -0.2265 0.1421 0.061 Uiso 1 1 calc R . . C25 C 0.6054(4) -0.1542(6) 0.2019(3) 0.0487(19) Uani 1 1 d . . . H25 H 0.6372 -0.2108 0.2090 0.058 Uiso 1 1 calc R . . C26 C 0.6059(3) -0.0619(5) 0.2315(2) 0.0403(17) Uani 1 1 d . . . H26 H 0.6366 -0.0576 0.2594 0.048 Uiso 1 1 calc R . . C27 C 0.3752(3) 0.0625(5) 0.1791(2) 0.0328(16) Uani 1 1 d . . . C28 C 0.3351(4) 0.0067(6) 0.1420(2) 0.051(2) Uani 1 1 d . . . H28 H 0.3472 0.0064 0.1117 0.061 Uiso 1 1 calc R . . C29 C 0.2781(4) -0.0475(7) 0.1496(3) 0.073(3) Uani 1 1 d . . . H29 H 0.2517 -0.0841 0.1245 0.087 Uiso 1 1 calc R . . C30 C 0.2600(4) -0.0479(7) 0.1941(3) 0.076(3) Uani 1 1 d . . . H30 H 0.2221 -0.0874 0.1993 0.091 Uiso 1 1 calc R . . C31 C 0.2965(5) 0.0085(7) 0.2308(3) 0.077(3) Uani 1 1 d . . . H31 H 0.2822 0.0124 0.2604 0.093 Uiso 1 1 calc R . . C32 C 0.3565(4) 0.0615(6) 0.2235(2) 0.054(2) Uani 1 1 d . . . H32 H 0.3835 0.0958 0.2489 0.065 Uiso 1 1 calc R . . C33 C 0.4408(3) 0.1642(5) 0.1075(2) 0.0337(16) Uani 1 1 d . . . C34 C 0.4898(4) 0.1413(6) 0.0795(2) 0.049(2) Uani 1 1 d . . . H34 H 0.5286 0.1039 0.0928 0.059 Uiso 1 1 calc R . . C35 C 0.4816(5) 0.1735(8) 0.0321(3) 0.071(3) Uani 1 1 d . . . H35 H 0.5143 0.1574 0.0134 0.085 Uiso 1 1 calc R . . C36 C 0.4243(5) 0.2296(7) 0.0130(3) 0.070(3) Uani 1 1 d . . . H36 H 0.4188 0.2512 -0.0189 0.084 Uiso 1 1 calc R . . C37 C 0.3759(4) 0.2545(7) 0.0392(3) 0.063(2) Uani 1 1 d . . . H37 H 0.3378 0.2934 0.0257 0.076 Uiso 1 1 calc R . . C38 C 0.3840(4) 0.2208(6) 0.0871(2) 0.0461(19) Uani 1 1 d . . . H38 H 0.3508 0.2367 0.1053 0.055 Uiso 1 1 calc R . . C39 C 0.5779(3) 0.1132(5) 0.3880(2) 0.0328(16) Uani 1 1 d . . . C40 C 0.6449(3) 0.0743(5) 0.4161(2) 0.0316(15) Uani 1 1 d . . . C41 C 0.7044(3) 0.1255(5) 0.4098(2) 0.0300(15) Uani 1 1 d . . . C42 C 0.7635(3) 0.0903(5) 0.4376(2) 0.0410(18) Uani 1 1 d . . . H42 H 0.8037 0.1245 0.4341 0.049 Uiso 1 1 calc R . . C43 C 0.7619(4) 0.0047(6) 0.4704(3) 0.056(2) Uani 1 1 d . . . H43 H 0.8014 -0.0189 0.4887 0.067 Uiso 1 1 calc R . . C44 C 0.7031(4) -0.0465(6) 0.4763(3) 0.056(2) Uani 1 1 d . . . H44 H 0.7031 -0.1049 0.4983 0.067 Uiso 1 1 calc R . . C45 C 0.6440(4) -0.0114(6) 0.4498(2) 0.0478(19) Uani 1 1 d . . . H45 H 0.6039 -0.0446 0.4543 0.057 Uiso 1 1 calc R . . C46 C 0.7512(3) 0.3481(5) 0.3865(2) 0.0314(15) Uani 1 1 d . . . C47 C 0.7675(3) 0.3669(6) 0.4351(2) 0.0425(18) Uani 1 1 d . . . H47 H 0.7532 0.3164 0.4565 0.051 Uiso 1 1 calc R . . C48 C 0.8050(4) 0.4608(7) 0.4517(3) 0.058(2) Uani 1 1 d . . . H48 H 0.8164 0.4724 0.4844 0.070 Uiso 1 1 calc R . . C49 C 0.8253(4) 0.5366(6) 0.4204(3) 0.055(2) Uani 1 1 d . . . H49 H 0.8498 0.6002 0.4315 0.066 Uiso 1 1 calc R . . C50 C 0.8094(4) 0.5175(6) 0.3727(3) 0.057(2) Uani 1 1 d . . . H50 H 0.8235 0.5680 0.3512 0.069 Uiso 1 1 calc R . . C51 C 0.7725(3) 0.4242(6) 0.3560(2) 0.0466(19) Uani 1 1 d . . . H51 H 0.7619 0.4128 0.3233 0.056 Uiso 1 1 calc R . . C52 C 0.7376(3) 0.1726(5) 0.3160(2) 0.0289(15) Uani 1 1 d . . . C53 C 0.7844(3) 0.0851(6) 0.3236(2) 0.0468(19) Uani 1 1 d . . . H53 H 0.7945 0.0518 0.3535 0.056 Uiso 1 1 calc R . . C54 C 0.8156(4) 0.0483(6) 0.2861(3) 0.058(2) Uani 1 1 d . . . H54 H 0.8463 -0.0104 0.2912 0.070 Uiso 1 1 calc R . . C55 C 0.8022(4) 0.0962(7) 0.2421(3) 0.056(2) Uani 1 1 d . . . H55 H 0.8245 0.0725 0.2176 0.067 Uiso 1 1 calc R . . C56 C 0.7547(3) 0.1805(7) 0.2346(2) 0.049(2) Uani 1 1 d . . . H56 H 0.7440 0.2127 0.2045 0.059 Uiso 1 1 calc R . . C57 C 0.7234(3) 0.2170(6) 0.2711(2) 0.0386(17) Uani 1 1 d . . . H57 H 0.6915 0.2738 0.2652 0.046 Uiso 1 1 calc R . . C58 C 0.4769(3) 0.2495(5) 0.3292(2) 0.0291(14) Uani 1 1 d . . . C59 C 0.4375(3) 0.2644(5) 0.3694(2) 0.0292(15) Uani 1 1 d . . . C60 C 0.4706(3) 0.3186(5) 0.4102(2) 0.0315(15) Uani 1 1 d . . . C61 C 0.4378(3) 0.3331(6) 0.4493(2) 0.0425(18) Uani 1 1 d . . . H61 H 0.4592 0.3686 0.4767 0.051 Uiso 1 1 calc R . . C62 C 0.3739(4) 0.2949(6) 0.4472(3) 0.049(2) Uani 1 1 d . . . H62 H 0.3522 0.3034 0.4736 0.058 Uiso 1 1 calc R . . C63 C 0.3411(4) 0.2438(6) 0.4067(3) 0.0472(19) Uani 1 1 d . . . H63 H 0.2974 0.2192 0.4059 0.057 Uiso 1 1 calc R . . C64 C 0.3719(3) 0.2289(5) 0.3675(2) 0.0385(17) Uani 1 1 d . . . H64 H 0.3493 0.1955 0.3401 0.046 Uiso 1 1 calc R . . C65 C 0.6008(3) 0.3489(5) 0.4653(2) 0.0347(16) Uani 1 1 d . . . C66 C 0.5958(4) 0.2486(6) 0.4908(2) 0.0459(18) Uani 1 1 d . . . H66 H 0.5679 0.1905 0.4778 0.055 Uiso 1 1 calc R . . C67 C 0.6335(4) 0.2368(7) 0.5362(3) 0.060(2) Uani 1 1 d . . . H67 H 0.6305 0.1705 0.5534 0.072 Uiso 1 1 calc R . . C68 C 0.6750(4) 0.3225(8) 0.5556(3) 0.065(2) Uani 1 1 d . . . H68 H 0.7006 0.3135 0.5855 0.078 Uiso 1 1 calc R . . C69 C 0.6784(4) 0.4209(7) 0.5307(3) 0.062(2) Uani 1 1 d . . . H69 H 0.7055 0.4794 0.5444 0.074 Uiso 1 1 calc R . . C70 C 0.6424(3) 0.4352(6) 0.4857(2) 0.0457(19) Uani 1 1 d . . . H70 H 0.6460 0.5021 0.4691 0.055 Uiso 1 1 calc R . . C71 C 0.5548(3) 0.5112(5) 0.3943(2) 0.0355(16) Uani 1 1 d . . . C72 C 0.6068(4) 0.5565(6) 0.3742(2) 0.051(2) Uani 1 1 d . . . H72 H 0.6386 0.5095 0.3641 0.061 Uiso 1 1 calc R . . C73 C 0.6111(5) 0.6740(7) 0.3694(3) 0.072(3) Uani 1 1 d . . . H73 H 0.6451 0.7051 0.3550 0.086 Uiso 1 1 calc R . . C74 C 0.5665(6) 0.7419(7) 0.3853(3) 0.079(3) Uani 1 1 d . . . H74 H 0.5701 0.8199 0.3820 0.095 Uiso 1 1 calc R . . C75 C 0.5155(5) 0.6978(7) 0.4063(3) 0.075(3) Uani 1 1 d . . . H75 H 0.4850 0.7458 0.4176 0.090 Uiso 1 1 calc R . . C76 C 0.5097(4) 0.5840(6) 0.4106(2) 0.052(2) Uani 1 1 d . . . H76 H 0.4750 0.5544 0.4248 0.062 Uiso 1 1 calc R . . Cl2 Cl 0.34016(11) 0.77113(17) 0.03901(8) 0.0580(5) Uani 1 1 d . . . O5 O 0.3913(5) 0.8402(8) 0.0564(3) 0.177(4) Uiso 1 1 d . . . O6 O 0.2824(4) 0.8375(7) 0.0283(3) 0.123(3) Uiso 1 1 d . . . O7 O 0.3222(4) 0.6853(7) 0.0666(3) 0.128(3) Uiso 1 1 d . . . O8 O 0.3590(4) 0.7192(6) -0.0020(3) 0.117(3) Uiso 1 1 d . . . C9 C 0.4618(5) 0.6523(6) 0.2186(4) 0.110(4) Uiso 1 1 d D . . H9 H 0.4797 0.6623 0.1906 0.132 Uiso 1 1 calc R . . C10 C 0.4611(6) 0.7429(9) 0.2499(4) 0.129(4) Uiso 1 1 d D . . H10 H 0.4845 0.8086 0.2452 0.154 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 0.0242(3) 0.0267(3) 0.0221(3) 0.0006(2) 0.0004(2) 0.0006(2) Rh2 0.0235(3) 0.0275(3) 0.0208(3) -0.0008(2) 0.0011(2) 0.0003(2) P1 0.0287(10) 0.0301(10) 0.0331(10) 0.0041(8) 0.0039(8) 0.0045(8) P2 0.0297(10) 0.0329(10) 0.0244(9) -0.0009(7) -0.0013(7) -0.0017(8) P3 0.0244(9) 0.0311(10) 0.0246(8) -0.0005(7) 0.0004(7) 0.0015(8) P4 0.0317(10) 0.0320(10) 0.0259(9) -0.0030(7) 0.0035(8) 0.0013(8) O1 0.036(3) 0.053(3) 0.042(3) 0.006(2) 0.009(2) 0.009(3) O2 0.032(3) 0.029(2) 0.029(2) 0.0005(19) 0.005(2) 0.002(2) O3 0.039(3) 0.042(3) 0.063(3) 0.012(3) 0.002(3) -0.008(3) O4 0.024(2) 0.041(3) 0.026(2) -0.001(2) -0.0008(19) 0.000(2) Cl1 0.0312(9) 0.0287(8) 0.0295(8) -0.0007(7) 0.0020(7) -0.0044(7) C1 0.031(4) 0.033(4) 0.024(3) -0.004(3) 0.001(3) -0.004(3) C2 0.028(4) 0.035(4) 0.031(4) -0.001(3) 0.002(3) -0.003(3) C3 0.031(4) 0.030(4) 0.035(4) 0.004(3) 0.005(3) -0.004(3) C4 0.049(5) 0.046(5) 0.057(5) 0.014(4) 0.013(4) -0.001(4) C5 0.061(6) 0.065(6) 0.050(5) 0.029(4) 0.000(4) -0.014(5) C6 0.049(5) 0.067(6) 0.046(5) 0.012(4) 0.013(4) -0.008(4) C7 0.034(4) 0.053(5) 0.036(4) -0.001(4) 0.009(3) -0.005(4) C8 0.037(4) 0.039(4) 0.054(5) -0.005(4) 0.014(4) -0.005(3) C11 0.099(8) 0.058(6) 0.143(10) -0.048(6) 0.049(7) -0.016(6) C13 0.113(8) 0.055(6) 0.060(6) -0.014(5) 0.017(6) 0.008(5) C12 0.089(7) 0.087(7) 0.073(6) -0.027(6) 0.021(5) 0.010(6) C14 0.034(4) 0.029(4) 0.039(4) 0.001(3) 0.005(3) -0.003(3) C15 0.047(5) 0.051(5) 0.068(6) 0.016(4) -0.009(4) -0.010(4) C16 0.049(6) 0.062(6) 0.062(6) 0.007(4) -0.013(4) 0.007(4) C17 0.034(5) 0.084(6) 0.057(5) -0.008(5) -0.003(4) -0.001(5) C18 0.048(5) 0.072(6) 0.054(5) -0.004(4) 0.019(4) -0.016(5) C19 0.033(4) 0.053(5) 0.042(4) 0.001(4) 0.003(3) 0.002(4) C20 0.026(4) 0.034(4) 0.026(4) 0.004(3) 0.000(3) 0.000(3) C21 0.029(4) 0.027(4) 0.030(4) -0.001(3) 0.000(3) 0.001(3) C22 0.034(4) 0.036(4) 0.025(4) -0.005(3) 0.002(3) 0.001(3) C23 0.046(5) 0.046(5) 0.038(4) -0.012(4) -0.008(4) 0.005(4) C24 0.058(5) 0.038(4) 0.057(5) -0.024(4) 0.013(4) -0.002(4) C25 0.046(5) 0.038(4) 0.059(5) -0.010(4) 0.000(4) 0.013(4) C26 0.037(4) 0.041(4) 0.041(4) -0.001(3) -0.002(3) 0.005(3) C27 0.033(4) 0.031(4) 0.033(4) 0.001(3) 0.003(3) -0.004(3) C28 0.055(5) 0.059(5) 0.038(4) -0.007(4) 0.003(4) -0.026(4) C29 0.064(6) 0.096(7) 0.056(6) -0.010(5) 0.003(5) -0.037(5) C30 0.067(6) 0.079(7) 0.084(7) 0.001(5) 0.015(5) -0.043(5) C31 0.098(7) 0.082(7) 0.060(6) -0.013(5) 0.039(5) -0.047(6) C32 0.061(5) 0.060(5) 0.038(4) -0.001(4) 0.000(4) -0.023(4) C33 0.039(4) 0.036(4) 0.023(4) -0.004(3) -0.003(3) -0.007(3) C34 0.041(5) 0.066(5) 0.037(4) -0.003(4) -0.007(4) -0.003(4) C35 0.074(7) 0.105(8) 0.037(5) -0.001(5) 0.017(5) -0.040(6) C36 0.085(7) 0.094(7) 0.026(4) 0.010(5) -0.007(5) -0.023(6) C37 0.069(6) 0.069(6) 0.045(5) 0.014(5) -0.012(4) 0.004(5) C38 0.049(5) 0.047(5) 0.039(4) 0.000(3) -0.001(4) 0.002(4) C39 0.042(4) 0.031(4) 0.025(4) -0.001(3) 0.004(3) -0.003(3) C40 0.044(4) 0.025(3) 0.024(3) -0.002(3) -0.001(3) 0.005(3) C41 0.027(4) 0.029(4) 0.032(4) 0.000(3) 0.000(3) 0.002(3) C42 0.038(4) 0.038(4) 0.045(4) 0.011(3) -0.001(3) 0.005(3) C43 0.053(5) 0.055(5) 0.054(5) 0.011(4) -0.010(4) 0.007(4) C44 0.066(6) 0.049(5) 0.047(5) 0.016(4) -0.008(4) 0.002(4) C45 0.064(6) 0.038(4) 0.043(4) 0.006(4) 0.014(4) -0.001(4) C46 0.024(4) 0.035(4) 0.035(4) -0.001(3) 0.004(3) 0.002(3) C47 0.056(5) 0.036(4) 0.034(4) -0.008(3) 0.003(4) -0.004(4) C48 0.061(6) 0.059(5) 0.050(5) -0.013(4) -0.009(4) -0.004(5) C49 0.049(5) 0.045(5) 0.068(6) -0.014(4) -0.001(4) -0.010(4) C50 0.054(5) 0.041(5) 0.079(6) -0.007(4) 0.019(5) -0.019(4) C51 0.056(5) 0.042(4) 0.042(4) -0.004(4) 0.008(4) -0.006(4) C52 0.023(4) 0.033(4) 0.029(4) -0.002(3) 0.001(3) 0.001(3) C53 0.049(5) 0.046(4) 0.047(4) -0.004(4) 0.010(4) 0.014(4) C54 0.058(5) 0.060(5) 0.058(5) -0.011(4) 0.014(4) 0.019(4) C55 0.049(5) 0.076(6) 0.045(5) -0.024(4) 0.014(4) 0.001(5) C56 0.039(5) 0.076(6) 0.031(4) -0.008(4) 0.004(4) 0.014(4) C57 0.026(4) 0.051(4) 0.037(4) -0.008(3) 0.000(3) 0.006(3) C58 0.029(4) 0.023(3) 0.034(4) 0.003(3) 0.001(3) 0.002(3) C59 0.033(4) 0.025(3) 0.031(3) 0.007(3) 0.008(3) 0.004(3) C60 0.031(4) 0.029(4) 0.035(4) 0.005(3) 0.003(3) 0.005(3) C61 0.040(5) 0.056(5) 0.034(4) -0.003(3) 0.015(3) -0.004(4) C62 0.051(5) 0.050(5) 0.050(5) 0.000(4) 0.027(4) 0.004(4) C63 0.032(4) 0.051(5) 0.063(5) 0.000(4) 0.018(4) 0.004(4) C64 0.026(4) 0.045(4) 0.043(4) 0.002(3) 0.000(3) 0.000(3) C65 0.040(4) 0.040(4) 0.023(3) -0.007(3) 0.002(3) 0.005(3) C66 0.057(5) 0.050(5) 0.028(4) -0.003(4) -0.002(3) 0.002(4) C67 0.076(6) 0.060(6) 0.040(4) 0.010(4) -0.003(4) 0.002(5) C68 0.077(7) 0.076(6) 0.035(5) -0.009(5) -0.011(4) 0.010(5) C69 0.067(6) 0.072(6) 0.039(5) -0.015(4) -0.010(4) -0.001(5) C70 0.052(5) 0.049(5) 0.032(4) -0.010(3) -0.005(4) -0.004(4) C71 0.049(5) 0.028(4) 0.030(4) -0.006(3) 0.007(3) 0.002(3) C72 0.061(5) 0.040(5) 0.053(5) -0.007(4) 0.013(4) 0.007(4) C73 0.103(8) 0.051(6) 0.069(6) -0.006(5) 0.034(6) -0.018(5) C74 0.127(9) 0.033(5) 0.081(7) -0.007(5) 0.026(6) -0.010(6) C75 0.095(8) 0.049(6) 0.087(7) -0.003(5) 0.030(6) 0.025(5) C76 0.060(5) 0.045(5) 0.053(5) -0.001(4) 0.013(4) 0.008(4) Cl2 0.0532(13) 0.0504(12) 0.0732(14) 0.0121(11) 0.0186(11) 0.0022(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.992(6) . ? Rh1 C20 2.030(6) . ? Rh1 P2 2.2660(17) . ? Rh1 O4 2.292(4) . ? Rh1 P1 2.3873(17) . ? Rh1 Cl1 2.4544(15) . ? Rh2 C39 2.011(6) . ? Rh2 C58 2.040(6) . ? Rh2 O2 2.144(4) . ? Rh2 P4 2.2544(16) . ? Rh2 P3 2.3877(17) . ? Rh2 Cl1 2.5143(15) . ? P1 C3 1.819(6) . ? P1 C8 1.792(6) . ? P1 C14 1.833(7) . ? P2 C27 1.808(6) . ? P2 C22 1.815(6) . ? P2 C33 1.816(6) . ? P3 C41 1.804(6) . ? P3 C46 1.824(6) . ? P3 C52 1.826(6) . ? P4 C71 1.821(6) . ? P4 C60 1.814(6) . ? P4 C65 1.826(6) . ? O1 C1 1.220(7) . ? O2 C20 1.246(6) . ? O3 C39 1.201(7) . ? O4 C58 1.240(7) . ? C1 C2 1.511(8) . ? C2 C3 1.403(8) . ? C2 C7 1.395(8) . ? C3 C4 1.378(8) . ? C4 C5 1.379(9) . ? C4 H4 0.9300 . ? C5 C6 1.394(10) . ? C5 H5 0.9300 . ? C6 C7 1.377(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.372(5) . ? C8 C13 1.383(5) . ? C11 C10 1.377(5) . ? C11 C12 1.380(5) . ? C11 H11 0.9300 . ? C13 C12 1.387(5) . ? C13 H13 0.9300 . ? C12 H12 0.9300 . ? C14 C19 1.378(8) . ? C14 C15 1.369(8) . ? C15 C16 1.384(10) . ? C15 H15 0.9300 . ? C16 C17 1.351(10) . ? C16 H16 0.9300 . ? C17 C18 1.375(10) . ? C17 H17 0.9300 . ? C18 C19 1.370(9) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.472(8) . ? C21 C26 1.392(8) . ? C21 C22 1.401(8) . ? C22 C23 1.378(8) . ? C23 C24 1.370(9) . ? C23 H23 0.9300 . ? C24 C25 1.387(9) . ? C24 H24 0.9300 . ? C25 C26 1.377(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.370(9) . ? C27 C28 1.393(8) . ? C28 C29 1.367(10) . ? C28 H28 0.9300 . ? C29 C30 1.370(10) . ? C29 H29 0.9300 . ? C30 C31 1.357(10) . ? C30 H30 0.9300 . ? C31 C32 1.413(10) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.381(9) . ? C33 C34 1.393(9) . ? C34 C35 1.384(9) . ? C34 H34 0.9300 . ? C35 C36 1.376(11) . ? C35 H35 0.9300 . ? C36 C37 1.354(12) . ? C36 H36 0.9300 . ? C37 C38 1.400(10) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.538(8) . ? C40 C41 1.386(8) . ? C40 C45 1.395(8) . ? C41 C42 1.395(8) . ? C42 C43 1.378(9) . ? C42 H42 0.9300 . ? C43 C44 1.372(10) . ? C43 H43 0.9300 . ? C44 C45 1.380(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C51 1.362(8) . ? C46 C47 1.386(8) . ? C47 C48 1.388(9) . ? C47 H47 0.9300 . ? C48 C49 1.370(10) . ? C48 H48 0.9300 . ? C49 C50 1.361(10) . ? C49 H49 0.9300 . ? C50 C51 1.376(9) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C57 1.368(8) . ? C52 C53 1.399(8) . ? C53 C54 1.388(9) . ? C53 H53 0.9300 . ? C54 C55 1.359(10) . ? C54 H54 0.9300 . ? C55 C56 1.380(9) . ? C55 H55 0.9300 . ? C56 C57 1.365(8) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 C59 1.500(8) . ? C59 C64 1.388(8) . ? C59 C60 1.402(8) . ? C60 C61 1.389(8) . ? C61 C62 1.366(9) . ? C61 H61 0.9300 . ? C62 C63 1.378(9) . ? C62 H62 0.9300 . ? C63 C64 1.367(9) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 C70 1.393(8) . ? C65 C66 1.401(8) . ? C66 C67 1.401(9) . ? C66 H66 0.9300 . ? C67 C68 1.377(10) . ? C67 H67 0.9300 . ? C68 C69 1.368(10) . ? C68 H68 0.9300 . ? C69 C70 1.381(9) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 C72 1.381(9) . ? C71 C76 1.388(9) . ? C72 C73 1.400(10) . ? C72 H72 0.9300 . ? C73 C74 1.339(11) . ? C73 H73 0.9300 . ? C74 C75 1.375(12) . ? C74 H74 0.9300 . ? C75 C76 1.358(10) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? Cl2 O5 1.353(10) . ? Cl2 O7 1.365(8) . ? Cl2 O8 1.420(8) . ? Cl2 O6 1.405(8) . ? C9 C10 1.394(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C20 93.8(3) . . ? C1 Rh1 P2 84.83(17) . . ? C20 Rh1 P2 81.41(18) . . ? C1 Rh1 O4 170.6(2) . . ? C20 Rh1 O4 86.11(19) . . ? P2 Rh1 O4 104.44(11) . . ? C1 Rh1 P1 84.31(19) . . ? C20 Rh1 P1 177.63(17) . . ? P2 Rh1 P1 99.75(6) . . ? O4 Rh1 P1 95.57(11) . . ? C1 Rh1 Cl1 87.68(17) . . ? C20 Rh1 Cl1 89.86(18) . . ? P2 Rh1 Cl1 168.09(6) . . ? O4 Rh1 Cl1 82.89(10) . . ? P1 Rh1 Cl1 88.69(6) . . ? C39 Rh2 C58 92.3(3) . . ? C39 Rh2 O2 83.9(2) . . ? C58 Rh2 O2 90.8(2) . . ? C39 Rh2 P4 89.02(18) . . ? C58 Rh2 P4 80.77(18) . . ? O2 Rh2 P4 168.78(11) . . ? C39 Rh2 P3 84.2(2) . . ? C58 Rh2 P3 175.72(17) . . ? O2 Rh2 P3 86.42(11) . . ? P4 Rh2 P3 101.51(6) . . ? C39 Rh2 Cl1 167.86(17) . . ? C58 Rh2 Cl1 84.31(17) . . ? O2 Rh2 Cl1 84.53(11) . . ? P4 Rh2 Cl1 101.89(6) . . ? P3 Rh2 Cl1 98.69(5) . . ? C3 P1 C8 108.0(3) . . ? C3 P1 C14 109.9(3) . . ? C8 P1 C14 100.1(3) . . ? C3 P1 Rh1 100.6(2) . . ? C8 P1 Rh1 120.3(2) . . ? C14 P1 Rh1 117.7(2) . . ? C27 P2 C22 103.3(3) . . ? C27 P2 C33 104.2(3) . . ? C22 P2 C33 106.0(3) . . ? C27 P2 Rh1 120.3(2) . . ? C22 P2 Rh1 103.2(2) . . ? C33 P2 Rh1 118.1(2) . . ? C41 P3 C46 106.6(3) . . ? C41 P3 C52 106.0(3) . . ? C46 P3 C52 103.5(3) . . ? C41 P3 Rh2 100.9(2) . . ? C46 P3 Rh2 123.4(2) . . ? C52 P3 Rh2 115.0(2) . . ? C71 P4 C60 107.1(3) . . ? C71 P4 C65 102.1(3) . . ? C60 P4 C65 104.6(3) . . ? C71 P4 Rh2 116.6(2) . . ? C60 P4 Rh2 102.6(2) . . ? C65 P4 Rh2 122.5(2) . . ? C20 O2 Rh2 126.3(4) . . ? C58 O4 Rh1 121.2(4) . . ? Rh1 Cl1 Rh2 92.26(5) . . ? O1 C1 C2 119.5(6) . . ? O1 C1 Rh1 121.2(5) . . ? C2 C1 Rh1 119.3(5) . . ? C3 C2 C7 119.9(6) . . ? C3 C2 C1 121.1(6) . . ? C7 C2 C1 119.1(6) . . ? C2 C3 C4 119.0(6) . . ? C2 C3 P1 114.3(5) . . ? C4 C3 P1 126.7(5) . . ? C5 C4 C3 120.7(7) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 120.6(7) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 119.2(7) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C6 C7 C2 120.5(7) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C9 C8 C13 116.6(7) . . ? C9 C8 P1 125.3(6) . . ? C13 C8 P1 118.0(5) . . ? C10 C11 C12 117.9(9) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? C8 C13 C12 122.7(7) . . ? C8 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C11 C12 C13 119.7(8) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C19 C14 C15 118.0(6) . . ? C19 C14 P1 116.4(5) . . ? C15 C14 P1 125.5(5) . . ? C14 C15 C16 120.9(7) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 119.6(7) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 121.0(7) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 118.7(7) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C14 C19 C18 121.8(7) . . ? C14 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? O2 C20 C21 117.0(5) . . ? O2 C20 Rh1 121.7(4) . . ? C21 C20 Rh1 121.2(4) . . ? C26 C21 C22 119.2(6) . . ? C26 C21 C20 124.2(6) . . ? C22 C21 C20 116.5(5) . . ? C23 C22 C21 120.6(6) . . ? C23 C22 P2 125.6(5) . . ? C21 C22 P2 113.7(4) . . ? C24 C23 C22 119.4(6) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 120.9(6) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 120.1(7) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 119.7(6) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C32 C27 C28 118.6(6) . . ? C32 C27 P2 119.6(5) . . ? C28 C27 P2 121.8(5) . . ? C27 C28 C29 120.9(7) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C28 120.0(8) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.9(8) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 119.1(8) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C27 C32 C31 120.3(7) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C38 C33 C34 118.5(6) . . ? C38 C33 P2 119.9(5) . . ? C34 C33 P2 121.5(5) . . ? C33 C34 C35 120.8(7) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 119.0(8) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C37 122.0(8) . . ? C35 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C36 C37 C38 118.9(8) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C33 C38 C37 120.9(7) . . ? C33 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? O3 C39 C40 120.1(6) . . ? O3 C39 Rh2 121.9(5) . . ? C40 C39 Rh2 117.8(5) . . ? C41 C40 C45 120.7(6) . . ? C41 C40 C39 121.3(5) . . ? C45 C40 C39 118.0(6) . . ? C40 C41 C42 119.1(6) . . ? C40 C41 P3 114.8(5) . . ? C42 C41 P3 126.1(5) . . ? C43 C42 C41 119.6(7) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 121.2(7) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 120.0(7) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C40 119.4(7) . . ? C44 C45 H45 120.3 . . ? C40 C45 H45 120.3 . . ? C51 C46 C47 118.4(6) . . ? C51 C46 P3 120.4(5) . . ? C47 C46 P3 121.0(5) . . ? C46 C47 C48 120.1(7) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 120.4(7) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C50 C49 C48 119.2(7) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? C49 C50 C51 120.5(7) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C46 C51 C50 121.3(7) . . ? C46 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C57 C52 C53 118.0(6) . . ? C57 C52 P3 119.2(5) . . ? C53 C52 P3 122.8(5) . . ? C54 C53 C52 119.4(7) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C55 C54 C53 121.5(7) . . ? C55 C54 H54 119.2 . . ? C53 C54 H54 119.2 . . ? C54 C55 C56 118.7(7) . . ? C54 C55 H55 120.7 . . ? C56 C55 H55 120.7 . . ? C57 C56 C55 120.4(7) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C52 C57 C56 122.0(6) . . ? C52 C57 H57 119.0 . . ? C56 C57 H57 119.0 . . ? O4 C58 C59 118.5(5) . . ? O4 C58 Rh2 123.2(4) . . ? C59 C58 Rh2 118.3(4) . . ? C64 C59 C60 120.3(6) . . ? C64 C59 C58 123.8(6) . . ? C60 C59 C58 115.9(5) . . ? C61 C60 C59 119.2(6) . . ? C61 C60 P4 127.7(5) . . ? C59 C60 P4 113.1(5) . . ? C60 C61 C62 119.5(6) . . ? C60 C61 H61 120.2 . . ? C62 C61 H61 120.2 . . ? C63 C62 C61 121.0(7) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C62 C63 C64 120.8(7) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.6 . . ? C63 C64 C59 119.1(6) . . ? C63 C64 H64 120.4 . . ? C59 C64 H64 120.4 . . ? C70 C65 C66 119.5(6) . . ? C70 C65 P4 121.9(5) . . ? C66 C65 P4 118.5(5) . . ? C65 C66 C67 119.1(7) . . ? C65 C66 H66 120.4 . . ? C67 C66 H66 120.4 . . ? C68 C67 C66 120.5(7) . . ? C68 C67 H67 119.7 . . ? C66 C67 H67 119.7 . . ? C69 C68 C67 119.8(7) . . ? C69 C68 H68 120.1 . . ? C67 C68 H68 120.1 . . ? C68 C69 C70 121.3(8) . . ? C68 C69 H69 119.4 . . ? C70 C69 H69 119.4 . . ? C65 C70 C69 119.8(7) . . ? C65 C70 H70 120.1 . . ? C69 C70 H70 120.1 . . ? C72 C71 C76 118.9(6) . . ? C72 C71 P4 117.7(5) . . ? C76 C71 P4 122.9(5) . . ? C71 C72 C73 119.2(7) . . ? C71 C72 H72 120.4 . . ? C73 C72 H72 120.4 . . ? C74 C73 C72 120.5(8) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C73 C74 C75 120.8(8) . . ? C73 C74 H74 119.6 . . ? C75 C74 H74 119.6 . . ? C76 C75 C74 119.7(8) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C75 C76 C71 120.9(8) . . ? C75 C76 H76 119.6 . . ? C71 C76 H76 119.6 . . ? O5 Cl2 O7 119.7(6) . . ? O5 Cl2 O8 105.9(5) . . ? O7 Cl2 O8 106.2(5) . . ? O5 Cl2 O6 108.0(5) . . ? O7 Cl2 O6 104.6(5) . . ? O8 Cl2 O6 112.7(4) . . ? C8 C9 C10 121.2(9) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 120.7(10) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 P1 C3 4.4(3) . . . . ? C20 Rh1 P1 C3 40(4) . . . . ? P2 Rh1 P1 C3 -79.3(2) . . . . ? O4 Rh1 P1 C3 175.0(2) . . . . ? Cl1 Rh1 P1 C3 92.2(2) . . . . ? C1 Rh1 P1 C8 -113.8(3) . . . . ? C20 Rh1 P1 C8 -78(4) . . . . ? P2 Rh1 P1 C8 162.4(2) . . . . ? O4 Rh1 P1 C8 56.7(3) . . . . ? Cl1 Rh1 P1 C8 -26.0(2) . . . . ? C1 Rh1 P1 C14 123.8(3) . . . . ? C20 Rh1 P1 C14 159(4) . . . . ? P2 Rh1 P1 C14 40.1(2) . . . . ? O4 Rh1 P1 C14 -65.7(3) . . . . ? Cl1 Rh1 P1 C14 -148.4(2) . . . . ? C1 Rh1 P2 C27 -166.7(3) . . . . ? C20 Rh1 P2 C27 98.7(3) . . . . ? O4 Rh1 P2 C27 15.0(3) . . . . ? P1 Rh1 P2 C27 -83.3(2) . . . . ? Cl1 Rh1 P2 C27 142.1(3) . . . . ? C1 Rh1 P2 C22 79.1(3) . . . . ? C20 Rh1 P2 C22 -15.5(3) . . . . ? O4 Rh1 P2 C22 -99.2(2) . . . . ? P1 Rh1 P2 C22 162.4(2) . . . . ? Cl1 Rh1 P2 C22 27.8(4) . . . . ? C1 Rh1 P2 C33 -37.4(3) . . . . ? C20 Rh1 P2 C33 -132.0(3) . . . . ? O4 Rh1 P2 C33 144.3(3) . . . . ? P1 Rh1 P2 C33 45.9(3) . . . . ? Cl1 Rh1 P2 C33 -88.7(4) . . . . ? C39 Rh2 P3 C41 -8.4(3) . . . . ? C58 Rh2 P3 C41 -42(2) . . . . ? O2 Rh2 P3 C41 -92.6(2) . . . . ? P4 Rh2 P3 C41 79.4(2) . . . . ? Cl1 Rh2 P3 C41 -176.5(2) . . . . ? C39 Rh2 P3 C46 -126.9(3) . . . . ? C58 Rh2 P3 C46 -161(2) . . . . ? O2 Rh2 P3 C46 148.9(3) . . . . ? P4 Rh2 P3 C46 -39.1(3) . . . . ? Cl1 Rh2 P3 C46 65.0(2) . . . . ? C39 Rh2 P3 C52 105.1(3) . . . . ? C58 Rh2 P3 C52 71(2) . . . . ? O2 Rh2 P3 C52 20.9(2) . . . . ? P4 Rh2 P3 C52 -167.1(2) . . . . ? Cl1 Rh2 P3 C52 -63.0(2) . . . . ? C39 Rh2 P4 C71 174.4(3) . . . . ? C58 Rh2 P4 C71 -93.2(3) . . . . ? O2 Rh2 P4 C71 -135.1(6) . . . . ? P3 Rh2 P4 C71 90.5(3) . . . . ? Cl1 Rh2 P4 C71 -11.0(3) . . . . ? C39 Rh2 P4 C60 -68.9(3) . . . . ? C58 Rh2 P4 C60 23.6(3) . . . . ? O2 Rh2 P4 C60 -18.4(6) . . . . ? P3 Rh2 P4 C60 -152.7(2) . . . . ? Cl1 Rh2 P4 C60 105.7(2) . . . . ? C39 Rh2 P4 C65 47.7(3) . . . . ? C58 Rh2 P4 C65 140.2(3) . . . . ? O2 Rh2 P4 C65 98.2(6) . . . . ? P3 Rh2 P4 C65 -36.1(3) . . . . ? Cl1 Rh2 P4 C65 -137.7(3) . . . . ? C39 Rh2 O2 C20 141.6(5) . . . . ? C58 Rh2 O2 C20 49.4(5) . . . . ? P4 Rh2 O2 C20 90.7(7) . . . . ? P3 Rh2 O2 C20 -133.9(5) . . . . ? Cl1 Rh2 O2 C20 -34.8(5) . . . . ? C1 Rh1 O4 C58 -28.4(15) . . . . ? C20 Rh1 O4 C58 61.2(5) . . . . ? P2 Rh1 O4 C58 141.3(4) . . . . ? P1 Rh1 O4 C58 -117.2(4) . . . . ? Cl1 Rh1 O4 C58 -29.2(4) . . . . ? C1 Rh1 Cl1 Rh2 -135.45(19) . . . . ? C20 Rh1 Cl1 Rh2 -41.68(17) . . . . ? P2 Rh1 Cl1 Rh2 -84.4(3) . . . . ? O4 Rh1 Cl1 Rh2 44.42(10) . . . . ? P1 Rh1 Cl1 Rh2 140.20(6) . . . . ? C39 Rh2 Cl1 Rh1 22.7(9) . . . . ? C58 Rh2 Cl1 Rh1 -51.48(17) . . . . ? O2 Rh2 Cl1 Rh1 39.91(11) . . . . ? P4 Rh2 Cl1 Rh1 -130.78(6) . . . . ? P3 Rh2 Cl1 Rh1 125.43(5) . . . . ? C20 Rh1 C1 O1 -7.5(5) . . . . ? P2 Rh1 C1 O1 -88.5(5) . . . . ? O4 Rh1 C1 O1 81.4(14) . . . . ? P1 Rh1 C1 O1 171.2(5) . . . . ? Cl1 Rh1 C1 O1 82.2(5) . . . . ? C20 Rh1 C1 C2 175.3(5) . . . . ? P2 Rh1 C1 C2 94.3(4) . . . . ? O4 Rh1 C1 C2 -95.8(13) . . . . ? P1 Rh1 C1 C2 -6.1(4) . . . . ? Cl1 Rh1 C1 C2 -95.0(4) . . . . ? O1 C1 C2 C3 -171.0(6) . . . . ? Rh1 C1 C2 C3 6.3(8) . . . . ? O1 C1 C2 C7 9.5(9) . . . . ? Rh1 C1 C2 C7 -173.1(5) . . . . ? C7 C2 C3 C4 -2.4(9) . . . . ? C1 C2 C3 C4 178.1(6) . . . . ? C7 C2 C3 P1 177.9(5) . . . . ? C1 C2 C3 P1 -1.6(8) . . . . ? C8 P1 C3 C2 124.2(5) . . . . ? C14 P1 C3 C2 -127.6(5) . . . . ? Rh1 P1 C3 C2 -2.7(5) . . . . ? C8 P1 C3 C4 -55.5(7) . . . . ? C14 P1 C3 C4 52.8(7) . . . . ? Rh1 P1 C3 C4 177.7(6) . . . . ? C2 C3 C4 C5 3.7(10) . . . . ? P1 C3 C4 C5 -176.6(5) . . . . ? C3 C4 C5 C6 -2.9(11) . . . . ? C4 C5 C6 C7 0.6(12) . . . . ? C5 C6 C7 C2 0.7(11) . . . . ? C3 C2 C7 C6 0.2(10) . . . . ? C1 C2 C7 C6 179.7(6) . . . . ? C3 P1 C8 C9 1.7(8) . . . . ? C14 P1 C8 C9 -113.3(8) . . . . ? Rh1 P1 C8 C9 116.1(7) . . . . ? C3 P1 C8 C13 -176.2(6) . . . . ? C14 P1 C8 C13 68.9(7) . . . . ? Rh1 P1 C8 C13 -61.7(7) . . . . ? C9 C8 C13 C12 4.1(13) . . . . ? P1 C8 C13 C12 -177.8(7) . . . . ? C10 C11 C12 C13 -8.1(16) . . . . ? C8 C13 C12 C11 -0.5(15) . . . . ? C3 P1 C14 C19 150.9(5) . . . . ? C8 P1 C14 C19 -95.7(5) . . . . ? Rh1 P1 C14 C19 36.5(6) . . . . ? C3 P1 C14 C15 -33.2(7) . . . . ? C8 P1 C14 C15 80.2(7) . . . . ? Rh1 P1 C14 C15 -147.6(6) . . . . ? C19 C14 C15 C16 0.0(11) . . . . ? P1 C14 C15 C16 -175.8(6) . . . . ? C14 C15 C16 C17 -0.5(12) . . . . ? C15 C16 C17 C18 0.4(12) . . . . ? C16 C17 C18 C19 0.1(12) . . . . ? C15 C14 C19 C18 0.6(10) . . . . ? P1 C14 C19 C18 176.8(6) . . . . ? C17 C18 C19 C14 -0.6(11) . . . . ? Rh2 O2 C20 C21 -172.7(4) . . . . ? Rh2 O2 C20 Rh1 2.9(7) . . . . ? C1 Rh1 C20 O2 119.2(5) . . . . ? P2 Rh1 C20 O2 -156.6(5) . . . . ? O4 Rh1 C20 O2 -51.3(5) . . . . ? P1 Rh1 C20 O2 84(4) . . . . ? Cl1 Rh1 C20 O2 31.6(5) . . . . ? C1 Rh1 C20 C21 -65.2(5) . . . . ? P2 Rh1 C20 C21 18.9(4) . . . . ? O4 Rh1 C20 C21 124.2(5) . . . . ? P1 Rh1 C20 C21 -101(4) . . . . ? Cl1 Rh1 C20 C21 -152.9(5) . . . . ? O2 C20 C21 C26 -15.8(9) . . . . ? Rh1 C20 C21 C26 168.4(5) . . . . ? O2 C20 C21 C22 160.4(6) . . . . ? Rh1 C20 C21 C22 -15.3(8) . . . . ? C26 C21 C22 C23 -1.3(10) . . . . ? C20 C21 C22 C23 -177.8(6) . . . . ? C26 C21 C22 P2 175.4(5) . . . . ? C20 C21 C22 P2 -1.0(7) . . . . ? C27 P2 C22 C23 64.0(6) . . . . ? C33 P2 C22 C23 -45.3(7) . . . . ? Rh1 P2 C22 C23 -170.0(5) . . . . ? C27 P2 C22 C21 -112.6(5) . . . . ? C33 P2 C22 C21 138.2(5) . . . . ? Rh1 P2 C22 C21 13.4(5) . . . . ? C21 C22 C23 C24 -0.4(10) . . . . ? P2 C22 C23 C24 -176.7(5) . . . . ? C22 C23 C24 C25 0.4(11) . . . . ? C23 C24 C25 C26 1.4(11) . . . . ? C24 C25 C26 C21 -3.0(11) . . . . ? C22 C21 C26 C25 3.0(10) . . . . ? C20 C21 C26 C25 179.1(6) . . . . ? C22 P2 C27 C32 92.6(6) . . . . ? C33 P2 C27 C32 -156.8(6) . . . . ? Rh1 P2 C27 C32 -21.6(6) . . . . ? C22 P2 C27 C28 -84.4(6) . . . . ? C33 P2 C27 C28 26.1(6) . . . . ? Rh1 P2 C27 C28 161.3(5) . . . . ? C32 C27 C28 C29 0.3(11) . . . . ? P2 C27 C28 C29 177.4(6) . . . . ? C27 C28 C29 C30 -0.3(13) . . . . ? C28 C29 C30 C31 2.5(15) . . . . ? C29 C30 C31 C32 -4.6(14) . . . . ? C28 C27 C32 C31 -2.4(11) . . . . ? P2 C27 C32 C31 -179.5(6) . . . . ? C30 C31 C32 C27 4.5(13) . . . . ? C27 P2 C33 C38 50.2(6) . . . . ? C22 P2 C33 C38 158.8(5) . . . . ? Rh1 P2 C33 C38 -86.2(5) . . . . ? C27 P2 C33 C34 -133.9(6) . . . . ? C22 P2 C33 C34 -25.3(6) . . . . ? Rh1 P2 C33 C34 89.7(6) . . . . ? C38 C33 C34 C35 -0.6(11) . . . . ? P2 C33 C34 C35 -176.6(6) . . . . ? C33 C34 C35 C36 0.6(12) . . . . ? C34 C35 C36 C37 0.1(13) . . . . ? C35 C36 C37 C38 -0.8(13) . . . . ? C34 C33 C38 C37 -0.1(10) . . . . ? P2 C33 C38 C37 176.0(5) . . . . ? C36 C37 C38 C33 0.8(11) . . . . ? C58 Rh2 C39 O3 10.9(6) . . . . ? O2 Rh2 C39 O3 -79.7(5) . . . . ? P4 Rh2 C39 O3 91.6(5) . . . . ? P3 Rh2 C39 O3 -166.7(6) . . . . ? Cl1 Rh2 C39 O3 -62.5(12) . . . . ? C58 Rh2 C39 C40 -174.6(4) . . . . ? O2 Rh2 C39 C40 94.8(4) . . . . ? P4 Rh2 C39 C40 -93.9(4) . . . . ? P3 Rh2 C39 C40 7.8(4) . . . . ? Cl1 Rh2 C39 C40 112.0(9) . . . . ? O3 C39 C40 C41 170.4(6) . . . . ? Rh2 C39 C40 C41 -4.2(8) . . . . ? O3 C39 C40 C45 -12.1(9) . . . . ? Rh2 C39 C40 C45 173.3(4) . . . . ? C45 C40 C41 C42 -0.1(9) . . . . ? C39 C40 C41 C42 177.3(5) . . . . ? C45 C40 C41 P3 178.2(5) . . . . ? C39 C40 C41 P3 -4.4(8) . . . . ? C46 P3 C41 C40 138.9(5) . . . . ? C52 P3 C41 C40 -111.3(5) . . . . ? Rh2 P3 C41 C40 8.9(5) . . . . ? C46 P3 C41 C42 -42.9(6) . . . . ? C52 P3 C41 C42 66.8(6) . . . . ? Rh2 P3 C41 C42 -172.9(5) . . . . ? C40 C41 C42 C43 0.9(10) . . . . ? P3 C41 C42 C43 -177.2(5) . . . . ? C41 C42 C43 C44 -0.4(11) . . . . ? C42 C43 C44 C45 -0.9(12) . . . . ? C43 C44 C45 C40 1.6(11) . . . . ? C41 C40 C45 C44 -1.1(10) . . . . ? C39 C40 C45 C44 -178.6(6) . . . . ? C41 P3 C46 C51 159.7(5) . . . . ? C52 P3 C46 C51 48.2(6) . . . . ? Rh2 P3 C46 C51 -84.6(6) . . . . ? C41 P3 C46 C47 -25.5(6) . . . . ? C52 P3 C46 C47 -137.0(5) . . . . ? Rh2 P3 C46 C47 90.2(5) . . . . ? C51 C46 C47 C48 -0.5(10) . . . . ? P3 C46 C47 C48 -175.4(5) . . . . ? C46 C47 C48 C49 1.0(11) . . . . ? C47 C48 C49 C50 -1.2(12) . . . . ? C48 C49 C50 C51 0.9(12) . . . . ? C47 C46 C51 C50 0.1(10) . . . . ? P3 C46 C51 C50 175.0(5) . . . . ? C49 C50 C51 C46 -0.3(11) . . . . ? C41 P3 C52 C57 160.8(5) . . . . ? C46 P3 C52 C57 -87.2(5) . . . . ? Rh2 P3 C52 C57 50.3(6) . . . . ? C41 P3 C52 C53 -20.7(6) . . . . ? C46 P3 C52 C53 91.3(6) . . . . ? Rh2 P3 C52 C53 -131.2(5) . . . . ? C57 C52 C53 C54 1.4(10) . . . . ? P3 C52 C53 C54 -177.1(5) . . . . ? C52 C53 C54 C55 0.6(12) . . . . ? C53 C54 C55 C56 -2.2(12) . . . . ? C54 C55 C56 C57 1.9(11) . . . . ? C53 C52 C57 C56 -1.8(10) . . . . ? P3 C52 C57 C56 176.8(5) . . . . ? C55 C56 C57 C52 0.2(11) . . . . ? Rh1 O4 C58 C59 164.7(4) . . . . ? Rh1 O4 C58 Rh2 -13.8(6) . . . . ? C39 Rh2 C58 O4 -121.5(5) . . . . ? O2 Rh2 C58 O4 -37.6(5) . . . . ? P4 Rh2 C58 O4 149.8(5) . . . . ? P3 Rh2 C58 O4 -88(2) . . . . ? Cl1 Rh2 C58 O4 46.8(5) . . . . ? C39 Rh2 C58 C59 59.9(5) . . . . ? O2 Rh2 C58 C59 143.8(4) . . . . ? P4 Rh2 C58 C59 -28.7(4) . . . . ? P3 Rh2 C58 C59 94(2) . . . . ? Cl1 Rh2 C58 C59 -131.8(4) . . . . ? O4 C58 C59 C64 24.7(9) . . . . ? Rh2 C58 C59 C64 -156.7(5) . . . . ? O4 C58 C59 C60 -154.7(5) . . . . ? Rh2 C58 C59 C60 23.9(7) . . . . ? C64 C59 C60 C61 2.1(9) . . . . ? C58 C59 C60 C61 -178.5(6) . . . . ? C64 C59 C60 P4 -179.3(5) . . . . ? C58 C59 C60 P4 0.1(7) . . . . ? C71 P4 C60 C61 -77.7(6) . . . . ? C65 P4 C60 C61 30.2(7) . . . . ? Rh2 P4 C60 C61 159.0(6) . . . . ? C71 P4 C60 C59 103.9(5) . . . . ? C65 P4 C60 C59 -148.3(4) . . . . ? Rh2 P4 C60 C59 -19.5(5) . . . . ? C59 C60 C61 C62 -0.3(10) . . . . ? P4 C60 C61 C62 -178.7(5) . . . . ? C60 C61 C62 C63 -1.1(11) . . . . ? C61 C62 C63 C64 0.8(11) . . . . ? C62 C63 C64 C59 1.0(10) . . . . ? C60 C59 C64 C63 -2.4(9) . . . . ? C58 C59 C64 C63 178.3(6) . . . . ? C71 P4 C65 C70 -20.4(6) . . . . ? C60 P4 C65 C70 -131.9(6) . . . . ? Rh2 P4 C65 C70 112.4(5) . . . . ? C71 P4 C65 C66 162.8(5) . . . . ? C60 P4 C65 C66 51.3(6) . . . . ? Rh2 P4 C65 C66 -64.4(6) . . . . ? C70 C65 C66 C67 -0.7(10) . . . . ? P4 C65 C66 C67 176.2(6) . . . . ? C65 C66 C67 C68 -0.1(12) . . . . ? C66 C67 C68 C69 1.3(13) . . . . ? C67 C68 C69 C70 -1.9(13) . . . . ? C66 C65 C70 C69 0.1(10) . . . . ? P4 C65 C70 C69 -176.7(6) . . . . ? C68 C69 C70 C65 1.2(12) . . . . ? C60 P4 C71 C72 -159.9(5) . . . . ? C65 P4 C71 C72 90.6(6) . . . . ? Rh2 P4 C71 C72 -45.6(6) . . . . ? C60 P4 C71 C76 28.2(7) . . . . ? C65 P4 C71 C76 -81.4(6) . . . . ? Rh2 P4 C71 C76 142.4(5) . . . . ? C76 C71 C72 C73 -2.4(11) . . . . ? P4 C71 C72 C73 -174.6(6) . . . . ? C71 C72 C73 C74 2.0(13) . . . . ? C72 C73 C74 C75 -0.5(15) . . . . ? C73 C74 C75 C76 -0.7(15) . . . . ? C74 C75 C76 C71 0.3(13) . . . . ? C72 C71 C76 C75 1.3(11) . . . . ? P4 C71 C76 C75 173.1(6) . . . . ? C13 C8 C9 C10 1.0(15) . . . . ? P1 C8 C9 C10 -176.9(8) . . . . ? C12 C11 C10 C9 13.2(18) . . . . ? C8 C9 C10 C11 -9.8(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.426 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.106 #=======================================================================END