# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'AUFFRANT, Audrey' _publ_contact_author_email audrey.auffrant@polytechnique.edu _publ_section_title ; Iminophosphorane based [P2N2] rhodium complexes: synthesis, reactivity, and application in catalysed transfer hydrogenation of polar bonds ; loop_ _publ_author_name A.AUFFRANT E.PAYET A.BUCHARD 'X.Le Goff' 'P.Le Floch' # Attachment '- 2010_buchard_njc.cif' #=============================================================================== data_ab982 _database_code_depnum_ccdc_archive 'CCDC 772851' #TrackingRef '- 2010_buchard_njc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 N2 P4 Rh, 4(C H2 Cl2), Cl' _chemical_formula_sum 'C56 H56 Cl9 N2 P4 Rh' _chemical_formula_weight 1302.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.715(1) _cell_length_b 21.218(1) _cell_length_c 23.598(1) _cell_angle_alpha 90.00 _cell_angle_beta 91.563(1) _cell_angle_gamma 90.00 _cell_volume 5863.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 12206 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8352 _exptl_absorpt_correction_T_max 0.9832 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 13346 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.46 _reflns_number_total 13346 _reflns_number_gt 10863 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 0.500 273 59 ' ' 2 0.000 0.500 0.000 273 59 ' ' 3 0.041 0.569 0.375 9 0 ' ' 4 0.041 0.931 0.875 9 1 ' ' 5 0.108 0.668 0.396 11 1 ' ' 6 0.108 0.832 0.896 10 0 ' ' 7 0.894 0.164 0.105 11 1 ' ' 8 0.894 0.336 0.605 11 0 ' ' 9 0.961 0.065 0.126 8 0 ' ' 10 0.961 0.435 0.626 9 0 ' ' _platon_squeeze_details ; An highly disordered CH2Cl2 molecule was accounted for using the Platon SQUEEZE function. ; _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^)+(0.0402P)^2^+7.7966P] 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 13346 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.467523(16) 0.061353(8) 0.261064(8) 0.01796(6) Uani 1 1 d . . . P1 P 0.34362(5) 0.19381(3) 0.26499(3) 0.02054(13) Uani 1 1 d . . . P2 P 0.56375(5) 0.14131(3) 0.22786(3) 0.01914(13) Uani 1 1 d . . . P3 P 0.40484(6) -0.07224(3) 0.31049(3) 0.02143(13) Uani 1 1 d . . . P4 P 0.57767(5) -0.01692(3) 0.23670(3) 0.01964(13) Uani 1 1 d . . . N1 N 0.34514(18) 0.12345(9) 0.28983(9) 0.0220(4) Uani 1 1 d . . . N2 N 0.35755(19) -0.00246(9) 0.29852(9) 0.0240(4) Uani 1 1 d . . . C1 C 0.2422(2) 0.09115(12) 0.30973(12) 0.0269(6) Uani 1 1 d . . . H1A H 0.1884 0.0832 0.2774 0.032 Uiso 1 1 calc R . . H1B H 0.2032 0.1178 0.3377 0.032 Uiso 1 1 calc R . . C2 C 0.2786(2) 0.02926(12) 0.33686(12) 0.0288(6) Uani 1 1 d . . . H2A H 0.3170 0.0372 0.3741 0.035 Uiso 1 1 calc R . . H2B H 0.2109 0.0024 0.3429 0.035 Uiso 1 1 calc R . . C3 C 0.2779(2) 0.25002(11) 0.31145(11) 0.0248(5) Uani 1 1 d . . . C4 C 0.3423(3) 0.28081(13) 0.35398(12) 0.0317(6) Uani 1 1 d . . . H4 H 0.4228 0.2758 0.3567 0.038 Uiso 1 1 calc R . . C5 C 0.2856(3) 0.31916(14) 0.39235(14) 0.0410(7) Uani 1 1 d . . . H5 H 0.3282 0.3404 0.4214 0.049 Uiso 1 1 calc R . . C6 C 0.1689(3) 0.32660(14) 0.38858(14) 0.0424(8) Uani 1 1 d . . . H6 H 0.1316 0.3523 0.4154 0.051 Uiso 1 1 calc R . . C7 C 0.1058(3) 0.29707(14) 0.34630(14) 0.0392(7) Uani 1 1 d . . . H7 H 0.0253 0.3026 0.3438 0.047 Uiso 1 1 calc R . . C8 C 0.1603(2) 0.25912(12) 0.30733(13) 0.0309(6) Uani 1 1 d . . . H8 H 0.1171 0.2393 0.2777 0.037 Uiso 1 1 calc R . . C9 C 0.2681(2) 0.20452(12) 0.19762(11) 0.0248(5) Uani 1 1 d . . . C10 C 0.2578(2) 0.26428(13) 0.17373(12) 0.0316(6) Uani 1 1 d . . . H10 H 0.2907 0.2995 0.1929 0.038 Uiso 1 1 calc R . . C11 C 0.2000(3) 0.27282(15) 0.12232(13) 0.0392(7) Uani 1 1 d . . . H11 H 0.1942 0.3137 0.1061 0.047 Uiso 1 1 calc R . . C12 C 0.1509(3) 0.22183(16) 0.09463(13) 0.0420(7) Uani 1 1 d . . . H12 H 0.1111 0.2276 0.0594 0.050 Uiso 1 1 calc R . . C13 C 0.1597(3) 0.16255(16) 0.11821(14) 0.0441(8) Uani 1 1 d . . . H13 H 0.1252 0.1276 0.0994 0.053 Uiso 1 1 calc R . . C14 C 0.2188(3) 0.15379(14) 0.16942(13) 0.0347(7) Uani 1 1 d . . . H14 H 0.2254 0.1127 0.1852 0.042 Uiso 1 1 calc R . . C15 C 0.4917(2) 0.21351(11) 0.25523(11) 0.0219(5) Uani 1 1 d . . . H15A H 0.5279 0.2268 0.2917 0.026 Uiso 1 1 calc R . . H15B H 0.4979 0.2485 0.2278 0.026 Uiso 1 1 calc R . . C16 C 0.7127(2) 0.15155(11) 0.25048(11) 0.0229(5) Uani 1 1 d . . . C17 C 0.7414(2) 0.17498(13) 0.30420(12) 0.0293(6) Uani 1 1 d . . . H17 H 0.6840 0.1930 0.3268 0.035 Uiso 1 1 calc R . . C18 C 0.8542(3) 0.17215(14) 0.32503(14) 0.0372(7) Uani 1 1 d . . . H18 H 0.8733 0.1885 0.3615 0.045 Uiso 1 1 calc R . . C19 C 0.9370(3) 0.14589(14) 0.29297(16) 0.0413(8) Uani 1 1 d . . . H19 H 1.0130 0.1427 0.3078 0.050 Uiso 1 1 calc R . . C20 C 0.9112(3) 0.12396(14) 0.23927(16) 0.0408(7) Uani 1 1 d . . . H20 H 0.9698 0.1069 0.2168 0.049 Uiso 1 1 calc R . . C21 C 0.7993(2) 0.12674(12) 0.21772(13) 0.0311(6) Uani 1 1 d . . . H21 H 0.7819 0.1117 0.1806 0.037 Uiso 1 1 calc R . . C22 C 0.5635(2) 0.15677(11) 0.15151(10) 0.0231(5) Uani 1 1 d . . . C23 C 0.6349(2) 0.20102(12) 0.12719(11) 0.0284(6) Uani 1 1 d . . . H23 H 0.6870 0.2245 0.1504 0.034 Uiso 1 1 calc R . . C24 C 0.6301(3) 0.21104(13) 0.06889(12) 0.0357(7) Uani 1 1 d . . . H24 H 0.6807 0.2404 0.0524 0.043 Uiso 1 1 calc R . . C25 C 0.5522(3) 0.17856(14) 0.03484(12) 0.0394(7) Uani 1 1 d . . . H25 H 0.5495 0.1853 -0.0050 0.047 Uiso 1 1 calc R . . C26 C 0.4777(3) 0.13583(14) 0.05942(12) 0.0376(7) Uani 1 1 d . . . H26 H 0.4220 0.1147 0.0365 0.045 Uiso 1 1 calc R . . C27 C 0.4847(3) 0.12413(12) 0.11704(11) 0.0296(6) Uani 1 1 d . . . H27 H 0.4357 0.0938 0.1333 0.035 Uiso 1 1 calc R . . C28 C 0.4917(2) -0.08266(12) 0.37450(11) 0.0249(5) Uani 1 1 d . . . C29 C 0.5304(2) -0.03045(14) 0.40455(12) 0.0313(6) Uani 1 1 d . . . H29 H 0.5124 0.0108 0.3914 0.038 Uiso 1 1 calc R . . C30 C 0.5962(3) -0.03872(16) 0.45430(13) 0.0412(7) Uani 1 1 d . . . H30 H 0.6231 -0.0030 0.4750 0.049 Uiso 1 1 calc R . . C31 C 0.6222(3) -0.09844(17) 0.47349(13) 0.0439(8) Uani 1 1 d . . . H31 H 0.6662 -0.1037 0.5076 0.053 Uiso 1 1 calc R . . C32 C 0.5847(3) -0.15071(15) 0.44347(13) 0.0382(7) Uani 1 1 d . . . H32 H 0.6039 -0.1918 0.4566 0.046 Uiso 1 1 calc R . . C33 C 0.5189(2) -0.14310(13) 0.39407(12) 0.0310(6) Uani 1 1 d . . . H33 H 0.4923 -0.1790 0.3736 0.037 Uiso 1 1 calc R . . C34 C 0.2910(2) -0.12896(11) 0.31760(11) 0.0229(5) Uani 1 1 d . . . C35 C 0.2388(2) -0.13341(12) 0.37024(12) 0.0279(6) Uani 1 1 d . . . H35 H 0.2679 -0.1097 0.4016 0.033 Uiso 1 1 calc R . . C36 C 0.1449(3) -0.17234(13) 0.37671(13) 0.0342(6) Uani 1 1 d . . . H36 H 0.1094 -0.1750 0.4124 0.041 Uiso 1 1 calc R . . C37 C 0.1029(2) -0.20725(13) 0.33139(14) 0.0354(7) Uani 1 1 d . . . H37 H 0.0389 -0.2341 0.3359 0.042 Uiso 1 1 calc R . . C38 C 0.1544(2) -0.20306(12) 0.27939(13) 0.0323(6) Uani 1 1 d . . . H38 H 0.1254 -0.2273 0.2483 0.039 Uiso 1 1 calc R . . C39 C 0.2478(2) -0.16391(12) 0.27211(12) 0.0266(5) Uani 1 1 d . . . H39 H 0.2820 -0.1610 0.2362 0.032 Uiso 1 1 calc R . . C40 C 0.4931(2) -0.09015(11) 0.25105(10) 0.0218(5) Uani 1 1 d . . . H40A H 0.4451 -0.1016 0.2174 0.026 Uiso 1 1 calc R . . H40B H 0.5448 -0.1258 0.2603 0.026 Uiso 1 1 calc R . . C41 C 0.7117(2) -0.03237(12) 0.27556(11) 0.0240(5) Uani 1 1 d . . . C42 C 0.7823(2) -0.08278(13) 0.26150(13) 0.0307(6) Uani 1 1 d . . . H42 H 0.7605 -0.1104 0.2314 0.037 Uiso 1 1 calc R . . C43 C 0.8840(3) -0.09256(14) 0.29137(14) 0.0379(7) Uani 1 1 d . . . H43 H 0.9319 -0.1268 0.2816 0.045 Uiso 1 1 calc R . . C44 C 0.9163(3) -0.05293(15) 0.33532(14) 0.0396(7) Uani 1 1 d . . . H44 H 0.9864 -0.0598 0.3555 0.048 Uiso 1 1 calc R . . C45 C 0.8471(3) -0.00339(14) 0.34990(13) 0.0366(7) Uani 1 1 d . . . H45 H 0.8693 0.0237 0.3803 0.044 Uiso 1 1 calc R . . C46 C 0.7445(2) 0.00696(12) 0.32007(11) 0.0276(6) Uani 1 1 d . . . H46 H 0.6968 0.0411 0.3303 0.033 Uiso 1 1 calc R . . C47 C 0.6168(2) -0.02567(11) 0.16266(11) 0.0245(5) Uani 1 1 d . . . C48 C 0.5329(3) -0.03905(12) 0.12194(11) 0.0298(6) Uani 1 1 d . . . H48 H 0.4583 -0.0500 0.1333 0.036 Uiso 1 1 calc R . . C49 C 0.5567(3) -0.03662(14) 0.06497(12) 0.0395(7) Uani 1 1 d . . . H49 H 0.4984 -0.0463 0.0376 0.047 Uiso 1 1 calc R . . C50 C 0.6643(3) -0.02033(14) 0.04730(13) 0.0437(8) Uani 1 1 d . . . H50 H 0.6796 -0.0178 0.0080 0.052 Uiso 1 1 calc R . . C51 C 0.7497(3) -0.00773(14) 0.08763(14) 0.0416(8) Uani 1 1 d . . . H51 H 0.8242 0.0029 0.0759 0.050 Uiso 1 1 calc R . . C52 C 0.7268(3) -0.01062(12) 0.14521(12) 0.0311(6) Uani 1 1 d . . . H52 H 0.7858 -0.0024 0.1726 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.64871(6) 0.32063(3) 0.37265(3) 0.02566(13) Uani 1 1 d . . . Cl2 Cl 0.51924(8) 0.14631(4) 0.40215(3) 0.04280(19) Uani 1 1 d . . . Cl3 Cl 0.73185(9) 0.12502(4) 0.46752(4) 0.0564(2) Uani 1 1 d . . . C53 C 0.6205(3) 0.17888(14) 0.45063(13) 0.0419(7) Uani 1 1 d . . . H53A H 0.5818 0.1910 0.4858 0.050 Uiso 1 1 calc R . . H53B H 0.6534 0.2175 0.4341 0.050 Uiso 1 1 calc R . . Cl4 Cl 0.92289(11) 0.46593(7) 0.30475(6) 0.0888(4) Uani 1 1 d . . . Cl5 Cl 0.78042(9) 0.50042(4) 0.39931(4) 0.0540(2) Uani 1 1 d . . . C54 C 0.7869(3) 0.46318(16) 0.33246(14) 0.0439(8) Uani 1 1 d . . . H54A H 0.7633 0.4186 0.3363 0.053 Uiso 1 1 calc R . . H54B H 0.7323 0.4840 0.3057 0.053 Uiso 1 1 calc R . . Cl6 Cl 0.89846(9) 0.27872(4) 0.48099(4) 0.0590(2) Uani 1 1 d . . . Cl7 Cl 0.96585(8) 0.41001(5) 0.49969(4) 0.0585(2) Uani 1 1 d . . . C55 C 0.8536(4) 0.35801(18) 0.4803(2) 0.0694(13) Uani 1 1 d . . . H55A H 0.7905 0.3632 0.5070 0.083 Uiso 1 1 calc R . . H55B H 0.8240 0.3690 0.4419 0.083 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 0.01630(10) 0.01486(9) 0.02284(10) 0.00029(7) 0.00277(7) 0.00035(7) P1 0.0174(3) 0.0164(3) 0.0278(3) -0.0015(2) 0.0010(2) 0.0011(2) P2 0.0168(3) 0.0160(3) 0.0247(3) 0.0001(2) 0.0027(2) -0.0012(2) P3 0.0216(3) 0.0177(3) 0.0253(3) 0.0007(2) 0.0042(3) -0.0015(2) P4 0.0183(3) 0.0163(3) 0.0245(3) 0.0003(2) 0.0042(2) 0.0007(2) N1 0.0168(10) 0.0192(10) 0.0304(11) -0.0006(8) 0.0061(8) 0.0035(8) N2 0.0220(11) 0.0185(10) 0.0320(11) 0.0030(8) 0.0090(9) -0.0009(8) C1 0.0182(13) 0.0242(13) 0.0386(15) -0.0005(11) 0.0069(11) 0.0005(10) C2 0.0272(15) 0.0242(13) 0.0356(14) 0.0019(11) 0.0127(12) 0.0018(11) C3 0.0271(14) 0.0170(12) 0.0306(13) -0.0001(10) 0.0071(11) 0.0017(10) C4 0.0263(15) 0.0285(14) 0.0404(16) -0.0071(11) 0.0033(12) 0.0022(11) C5 0.046(2) 0.0341(16) 0.0435(17) -0.0136(13) 0.0069(14) -0.0023(14) C6 0.045(2) 0.0324(16) 0.0513(19) -0.0107(14) 0.0224(15) 0.0012(14) C7 0.0262(16) 0.0319(15) 0.060(2) -0.0067(14) 0.0160(14) 0.0018(12) C8 0.0247(14) 0.0228(13) 0.0456(16) -0.0040(11) 0.0053(12) -0.0018(11) C9 0.0193(13) 0.0256(13) 0.0298(13) -0.0012(10) 0.0016(10) 0.0029(10) C10 0.0282(15) 0.0280(14) 0.0387(15) 0.0023(11) 0.0001(12) -0.0001(11) C11 0.0357(17) 0.0413(17) 0.0405(17) 0.0127(13) 0.0003(13) 0.0059(13) C12 0.0350(18) 0.058(2) 0.0329(16) 0.0025(14) -0.0054(13) 0.0063(15) C13 0.045(2) 0.0423(18) 0.0443(18) -0.0092(14) -0.0141(15) 0.0028(14) C14 0.0376(17) 0.0273(14) 0.0389(16) -0.0039(12) -0.0066(13) -0.0005(12) C15 0.0200(13) 0.0183(11) 0.0276(12) -0.0009(9) 0.0014(10) 0.0005(9) C16 0.0190(13) 0.0165(11) 0.0333(14) 0.0038(9) 0.0024(10) 0.0002(9) C17 0.0243(14) 0.0289(14) 0.0346(14) 0.0020(11) -0.0004(11) -0.0025(11) C18 0.0289(16) 0.0361(16) 0.0460(17) 0.0052(13) -0.0107(13) -0.0069(12) C19 0.0179(14) 0.0305(15) 0.075(2) 0.0093(15) -0.0086(14) -0.0020(11) C20 0.0204(15) 0.0304(15) 0.072(2) 0.0027(14) 0.0095(14) 0.0043(12) C21 0.0230(14) 0.0227(13) 0.0480(17) -0.0009(11) 0.0060(12) -0.0006(11) C22 0.0252(13) 0.0201(12) 0.0240(12) -0.0005(9) 0.0027(10) 0.0024(10) C23 0.0304(15) 0.0228(13) 0.0320(14) -0.0001(10) 0.0024(11) -0.0042(11) C24 0.0482(19) 0.0289(14) 0.0303(14) 0.0071(11) 0.0083(13) -0.0032(13) C25 0.058(2) 0.0336(16) 0.0268(14) 0.0011(12) 0.0024(14) -0.0021(14) C26 0.050(2) 0.0347(15) 0.0273(14) -0.0045(11) -0.0043(13) -0.0081(14) C27 0.0334(16) 0.0254(13) 0.0301(14) -0.0015(10) 0.0027(12) -0.0066(11) C28 0.0224(13) 0.0268(13) 0.0257(13) 0.0007(10) 0.0049(10) 0.0001(10) C29 0.0301(15) 0.0320(15) 0.0319(14) -0.0039(11) 0.0038(12) -0.0052(12) C30 0.0364(18) 0.0498(19) 0.0374(16) -0.0077(14) -0.0004(14) -0.0104(14) C31 0.0325(17) 0.067(2) 0.0326(16) 0.0065(15) -0.0015(13) -0.0046(15) C32 0.0321(17) 0.0444(17) 0.0382(16) 0.0099(13) 0.0014(13) 0.0039(13) C33 0.0293(15) 0.0262(14) 0.0378(15) 0.0020(11) 0.0034(12) 0.0008(11) C34 0.0210(13) 0.0157(11) 0.0321(13) 0.0041(9) 0.0036(10) 0.0015(9) C35 0.0279(15) 0.0235(13) 0.0324(14) 0.0024(10) 0.0050(11) 0.0000(11) C36 0.0281(15) 0.0285(14) 0.0469(17) 0.0083(12) 0.0142(13) 0.0033(11) C37 0.0211(14) 0.0243(14) 0.061(2) 0.0057(13) 0.0066(13) 0.0007(11) C38 0.0243(14) 0.0224(13) 0.0501(17) -0.0026(12) -0.0036(13) 0.0020(11) C39 0.0241(14) 0.0226(12) 0.0333(14) 0.0027(10) 0.0009(11) 0.0016(10) C40 0.0226(13) 0.0177(11) 0.0253(12) -0.0003(9) 0.0037(10) 0.0005(10) C41 0.0208(13) 0.0211(12) 0.0301(13) 0.0044(10) 0.0024(10) -0.0001(10) C42 0.0258(15) 0.0248(13) 0.0416(16) -0.0003(11) 0.0042(12) 0.0030(11) C43 0.0267(16) 0.0296(15) 0.0574(19) 0.0049(13) 0.0004(14) 0.0094(12) C44 0.0261(16) 0.0413(17) 0.0511(19) 0.0088(14) -0.0069(13) 0.0022(13) C45 0.0334(16) 0.0343(15) 0.0416(17) 0.0030(12) -0.0093(13) -0.0010(12) C46 0.0243(14) 0.0235(13) 0.0351(14) 0.0016(10) 0.0027(11) 0.0011(10) C47 0.0317(15) 0.0145(11) 0.0277(13) -0.0001(9) 0.0081(11) 0.0023(10) C48 0.0352(16) 0.0258(13) 0.0286(14) 0.0005(10) 0.0047(12) 0.0040(11) C49 0.054(2) 0.0357(16) 0.0285(15) 0.0000(12) -0.0003(14) 0.0037(14) C50 0.069(2) 0.0348(16) 0.0282(15) 0.0007(12) 0.0152(15) -0.0007(16) C51 0.049(2) 0.0331(16) 0.0432(17) 0.0006(13) 0.0233(15) -0.0055(14) C52 0.0359(16) 0.0242(13) 0.0338(14) -0.0008(11) 0.0103(12) -0.0044(11) Cl1 0.0295(3) 0.0198(3) 0.0277(3) 0.0013(2) 0.0005(2) -0.0015(2) Cl2 0.0535(5) 0.0365(4) 0.0383(4) 0.0012(3) 0.0008(3) -0.0113(3) Cl3 0.0648(6) 0.0489(5) 0.0549(5) 0.0047(4) -0.0100(4) -0.0006(4) C53 0.058(2) 0.0337(16) 0.0335(16) -0.0033(12) 0.0019(15) -0.0068(14) Cl4 0.0628(7) 0.0879(8) 0.1177(10) -0.0195(7) 0.0419(7) -0.0157(6) Cl5 0.0736(7) 0.0438(5) 0.0445(5) -0.0021(3) 0.0009(4) -0.0023(4) C54 0.046(2) 0.0416(17) 0.0437(18) -0.0035(14) 0.0037(15) -0.0129(15) Cl6 0.0555(6) 0.0491(5) 0.0718(6) 0.0085(4) -0.0081(5) 0.0039(4) Cl7 0.0469(5) 0.0582(5) 0.0701(6) -0.0122(5) -0.0047(4) 0.0019(4) C55 0.048(2) 0.048(2) 0.111(4) 0.009(2) -0.024(2) -0.0023(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.075(2) . ? Rh1 N2 2.082(2) . ? Rh1 P4 2.1896(6) . ? Rh1 P2 2.1935(6) . ? P1 N1 1.604(2) . ? P1 C15 1.805(3) . ? P1 C3 1.806(3) . ? P1 C9 1.812(3) . ? P2 C16 1.824(3) . ? P2 C22 1.831(3) . ? P2 C15 1.873(2) . ? P3 N2 1.603(2) . ? P3 C40 1.805(3) . ? P3 C34 1.808(3) . ? P3 C28 1.812(3) . ? P4 C41 1.827(3) . ? P4 C47 1.828(3) . ? P4 C40 1.879(2) . ? N1 C1 1.475(3) . ? N2 C2 1.474(3) . ? C1 C2 1.517(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.392(4) . ? C3 C4 1.400(4) . ? C4 C5 1.399(4) . ? C4 H4 0.9500 . ? C5 C6 1.377(5) . ? C5 H5 0.9500 . ? C6 C7 1.376(5) . ? C6 H6 0.9500 . ? C7 C8 1.391(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.384(4) . ? C9 C10 1.391(4) . ? C10 C11 1.385(4) . ? C10 H10 0.9500 . ? C11 C12 1.381(5) . ? C11 H11 0.9500 . ? C12 C13 1.378(5) . ? C12 H12 0.9500 . ? C13 C14 1.389(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.394(4) . ? C16 C21 1.395(4) . ? C17 C18 1.399(4) . ? C17 H17 0.9500 . ? C18 C19 1.365(5) . ? C18 H18 0.9500 . ? C19 C20 1.376(5) . ? C19 H19 0.9500 . ? C20 C21 1.395(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.392(4) . ? C22 C27 1.397(4) . ? C23 C24 1.392(4) . ? C23 H23 0.9500 . ? C24 C25 1.383(4) . ? C24 H24 0.9500 . ? C25 C26 1.396(4) . ? C25 H25 0.9500 . ? C26 C27 1.382(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.385(4) . ? C28 C33 1.397(4) . ? C29 C30 1.398(4) . ? C29 H29 0.9500 . ? C30 C31 1.377(5) . ? C30 H30 0.9500 . ? C31 C32 1.381(5) . ? C31 H31 0.9500 . ? C32 C33 1.390(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.389(4) . ? C34 C35 1.403(4) . ? C35 C36 1.388(4) . ? C35 H35 0.9500 . ? C36 C37 1.380(4) . ? C36 H36 0.9500 . ? C37 C38 1.385(4) . ? C37 H37 0.9500 . ? C38 C39 1.388(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.388(4) . ? C41 C42 1.397(4) . ? C42 C43 1.383(4) . ? C42 H42 0.9500 . ? C43 C44 1.380(5) . ? C43 H43 0.9500 . ? C44 C45 1.377(4) . ? C44 H44 0.9500 . ? C45 C46 1.393(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.385(4) . ? C47 C52 1.400(4) . ? C48 C49 1.381(4) . ? C48 H48 0.9500 . ? C49 C50 1.383(5) . ? C49 H49 0.9500 . ? C50 C51 1.388(5) . ? C50 H50 0.9500 . ? C51 C52 1.394(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? Cl2 C53 1.766(3) . ? Cl3 C53 1.772(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? Cl4 C54 1.740(4) . ? Cl5 C54 1.768(3) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? Cl6 C55 1.763(4) . ? Cl7 C55 1.767(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2 80.39(8) . . ? N1 Rh1 P4 170.04(6) . . ? N2 Rh1 P4 89.66(6) . . ? N1 Rh1 P2 89.55(6) . . ? N2 Rh1 P2 169.89(6) . . ? P4 Rh1 P2 100.40(2) . . ? N1 P1 C15 105.14(11) . . ? N1 P1 C3 113.16(11) . . ? C15 P1 C3 110.56(12) . . ? N1 P1 C9 115.96(12) . . ? C15 P1 C9 107.87(12) . . ? C3 P1 C9 104.10(12) . . ? C16 P2 C22 104.04(12) . . ? C16 P2 C15 103.79(11) . . ? C22 P2 C15 101.78(11) . . ? C16 P2 Rh1 118.98(8) . . ? C22 P2 Rh1 120.19(9) . . ? C15 P2 Rh1 105.57(8) . . ? N2 P3 C40 105.06(11) . . ? N2 P3 C34 112.26(11) . . ? C40 P3 C34 111.81(12) . . ? N2 P3 C28 116.31(12) . . ? C40 P3 C28 107.56(12) . . ? C34 P3 C28 103.92(12) . . ? C41 P4 C47 103.13(12) . . ? C41 P4 C40 102.22(11) . . ? C47 P4 C40 103.63(11) . . ? C41 P4 Rh1 120.60(9) . . ? C47 P4 Rh1 119.54(8) . . ? C40 P4 Rh1 105.21(8) . . ? C1 N1 P1 123.21(17) . . ? C1 N1 Rh1 112.80(15) . . ? P1 N1 Rh1 118.18(12) . . ? C2 N2 P3 122.22(17) . . ? C2 N2 Rh1 111.69(15) . . ? P3 N2 Rh1 117.42(12) . . ? N1 C1 C2 108.3(2) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 108.1(2) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C8 C3 C4 119.9(2) . . ? C8 C3 P1 119.1(2) . . ? C4 C3 P1 120.9(2) . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C6 C5 C4 120.9(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C7 C6 C5 120.5(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 119.7(3) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C3 120.4(3) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? C14 C9 C10 118.9(2) . . ? C14 C9 P1 120.8(2) . . ? C10 C9 P1 120.3(2) . . ? C11 C10 C9 120.6(3) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 120.0(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C9 C14 C13 120.4(3) . . ? C9 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? P1 C15 P2 107.37(12) . . ? P1 C15 H15A 110.2 . . ? P2 C15 H15A 110.2 . . ? P1 C15 H15B 110.2 . . ? P2 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C17 C16 C21 118.5(2) . . ? C17 C16 P2 120.9(2) . . ? C21 C16 P2 119.8(2) . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.5(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 120.3(3) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C23 C22 C27 119.3(2) . . ? C23 C22 P2 122.8(2) . . ? C27 C22 P2 117.9(2) . . ? C22 C23 C24 120.1(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.5(3) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C22 120.3(3) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C29 C28 C33 119.8(3) . . ? C29 C28 P3 119.9(2) . . ? C33 C28 P3 120.4(2) . . ? C28 C29 C30 119.7(3) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.4(3) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 119.9(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C28 120.0(3) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C39 C34 C35 119.4(2) . . ? C39 C34 P3 122.5(2) . . ? C35 C34 P3 117.9(2) . . ? C36 C35 C34 120.2(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.0(3) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 119.9(3) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C39 120.8(3) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C38 C39 C34 119.7(3) . . ? C38 C39 H39 120.1 . . ? C34 C39 H39 120.1 . . ? P3 C40 P4 106.38(12) . . ? P3 C40 H40A 110.5 . . ? P4 C40 H40A 110.5 . . ? P3 C40 H40B 110.5 . . ? P4 C40 H40B 110.5 . . ? H40A C40 H40B 108.6 . . ? C46 C41 C42 119.1(2) . . ? C46 C41 P4 119.3(2) . . ? C42 C41 P4 121.6(2) . . ? C43 C42 C41 120.1(3) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C44 C43 C42 120.4(3) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 120.1(3) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.0(3) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 120.3(3) . . ? C41 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C48 C47 C52 118.9(2) . . ? C48 C47 P4 119.5(2) . . ? C52 C47 P4 121.0(2) . . ? C49 C48 C47 120.6(3) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 120.9(3) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C49 C50 C51 119.2(3) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? C50 C51 C52 120.4(3) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 C47 120.0(3) . . ? C51 C52 H52 120.0 . . ? C47 C52 H52 120.0 . . ? Cl2 C53 Cl3 111.76(17) . . ? Cl2 C53 H53A 109.3 . . ? Cl3 C53 H53A 109.3 . . ? Cl2 C53 H53B 109.3 . . ? Cl3 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? Cl4 C54 Cl5 112.49(19) . . ? Cl4 C54 H54A 109.1 . . ? Cl5 C54 H54A 109.1 . . ? Cl4 C54 H54B 109.1 . . ? Cl5 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? Cl6 C55 Cl7 112.0(2) . . ? Cl6 C55 H55A 109.2 . . ? Cl7 C55 H55A 109.2 . . ? Cl6 C55 H55B 109.2 . . ? Cl7 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.910 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.076 #===END #compound 2_BF4 data_ab695 _database_code_depnum_ccdc_archive 'CCDC 772852' #TrackingRef '- 2010_buchard_njc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 N2 P4 Rh, 2(C H2 Cl2), B F4' _chemical_formula_sum 'C54 H52 B Cl4 F4 N2 P4 Rh' _chemical_formula_weight 1184.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.299(1) _cell_length_b 19.674(1) _cell_length_c 22.075(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5341.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 8951 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8739 _exptl_absorpt_correction_T_max 0.9596 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 36847 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 30.02 _reflns_number_total 15419 _reflns_number_gt 12655 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.045(15) _refine_ls_number_reflns 15419 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.757086(13) 0.480949(7) 0.252645(6) 0.01725(4) Uani 1 1 d . . . P1 P 0.78340(5) 0.41701(3) 0.38378(2) 0.01979(12) Uani 1 1 d . . . P2 P 0.78203(5) 0.55287(3) 0.32731(2) 0.01909(13) Uani 1 1 d . . . P3 P 0.69555(5) 0.41694(3) 0.12530(2) 0.01983(12) Uani 1 1 d . . . P4 P 0.76448(6) 0.55040(3) 0.17516(2) 0.02067(12) Uani 1 1 d . . . N1 N 0.74429(19) 0.40201(8) 0.31568(7) 0.0205(4) Uani 1 1 d . . . N2 N 0.73355(17) 0.39921(9) 0.19327(7) 0.0198(4) Uani 1 1 d . . . C1 C 0.7536(2) 0.33452(10) 0.28657(9) 0.0239(5) Uani 1 1 d . . . H1A H 0.7194 0.2994 0.3124 0.029 Uiso 1 1 calc R . . H1B H 0.8311 0.3225 0.2809 0.029 Uiso 1 1 calc R . . C2 C 0.6965(2) 0.33782(11) 0.22558(10) 0.0249(5) Uani 1 1 d . . . H2A H 0.7138 0.2968 0.2015 0.030 Uiso 1 1 calc R . . H2B H 0.6167 0.3396 0.2316 0.030 Uiso 1 1 calc R . . C3 C 0.92725(19) 0.41043(12) 0.39949(10) 0.0238(5) Uani 1 1 d . . . C4 C 1.0006(2) 0.40344(13) 0.35229(12) 0.0318(6) Uani 1 1 d . . . H4 H 0.9754 0.3999 0.3117 0.038 Uiso 1 1 calc R . . C5 C 1.1120(2) 0.40162(15) 0.36480(13) 0.0415(7) Uani 1 1 d . . . H5 H 1.1627 0.3960 0.3327 0.050 Uiso 1 1 calc R . . C6 C 1.1483(2) 0.40799(14) 0.42371(14) 0.0415(7) Uani 1 1 d . . . H6 H 1.2242 0.4080 0.4318 0.050 Uiso 1 1 calc R . . C7 C 1.0758(2) 0.41436(14) 0.47098(13) 0.0407(7) Uani 1 1 d . . . H7 H 1.1012 0.4182 0.5115 0.049 Uiso 1 1 calc R . . C8 C 0.9647(2) 0.41511(13) 0.45854(11) 0.0325(6) Uani 1 1 d . . . H8 H 0.9141 0.4189 0.4909 0.039 Uiso 1 1 calc R . . C9 C 0.7212(2) 0.36083(12) 0.43892(9) 0.0249(5) Uani 1 1 d . . . C10 C 0.6260(2) 0.37826(13) 0.46939(10) 0.0285(5) Uani 1 1 d . . . H10 H 0.5947 0.4219 0.4637 0.034 Uiso 1 1 calc R . . C11 C 0.5767(2) 0.33188(14) 0.50814(10) 0.0333(6) Uani 1 1 d . . . H11 H 0.5117 0.3439 0.5289 0.040 Uiso 1 1 calc R . . C12 C 0.6221(3) 0.26837(14) 0.51652(11) 0.0377(7) Uani 1 1 d . . . H12 H 0.5880 0.2368 0.5429 0.045 Uiso 1 1 calc R . . C13 C 0.7168(3) 0.25044(13) 0.48678(11) 0.0360(7) Uani 1 1 d . . . H13 H 0.7477 0.2067 0.4928 0.043 Uiso 1 1 calc R . . C14 C 0.7666(2) 0.29672(11) 0.44809(10) 0.0292(6) Uani 1 1 d . . . H14 H 0.8318 0.2846 0.4278 0.035 Uiso 1 1 calc R . . C15 C 0.7449(2) 0.50414(11) 0.39732(8) 0.0222(5) Uani 1 1 d . . . H15A H 0.7843 0.5224 0.4329 0.027 Uiso 1 1 calc R . . H15B H 0.6658 0.5074 0.4051 0.027 Uiso 1 1 calc R . . C16 C 0.9186(2) 0.58314(12) 0.34575(10) 0.0233(5) Uani 1 1 d . . . C17 C 1.0044(2) 0.56670(13) 0.30759(12) 0.0307(6) Uani 1 1 d . . . H17 H 0.9912 0.5410 0.2719 0.037 Uiso 1 1 calc R . . C18 C 1.1094(2) 0.58761(15) 0.32126(14) 0.0426(7) Uani 1 1 d . . . H18 H 1.1677 0.5768 0.2947 0.051 Uiso 1 1 calc R . . C19 C 1.1290(3) 0.62406(15) 0.37334(14) 0.0459(8) Uani 1 1 d . . . H19 H 1.2011 0.6374 0.3831 0.055 Uiso 1 1 calc R . . C20 C 1.0437(2) 0.64142(15) 0.41170(13) 0.0414(7) Uani 1 1 d . . . H20 H 1.0574 0.6668 0.4475 0.050 Uiso 1 1 calc R . . C21 C 0.9394(2) 0.62175(13) 0.39774(11) 0.0309(6) Uani 1 1 d . . . H21 H 0.8810 0.6345 0.4235 0.037 Uiso 1 1 calc R . . C22 C 0.6999(2) 0.63032(11) 0.33328(10) 0.0220(5) Uani 1 1 d . . . C23 C 0.7449(2) 0.69327(11) 0.31897(10) 0.0275(5) Uani 1 1 d . . . H23 H 0.8205 0.6965 0.3107 0.033 Uiso 1 1 calc R . . C24 C 0.6811(2) 0.75108(13) 0.31657(12) 0.0350(6) Uani 1 1 d . . . H24 H 0.7125 0.7939 0.3070 0.042 Uiso 1 1 calc R . . C25 C 0.5702(2) 0.74588(14) 0.32831(12) 0.0366(6) Uani 1 1 d . . . H25 H 0.5256 0.7852 0.3263 0.044 Uiso 1 1 calc R . . C26 C 0.5246(2) 0.68390(14) 0.34282(11) 0.0339(6) Uani 1 1 d . . . H26 H 0.4490 0.6807 0.3510 0.041 Uiso 1 1 calc R . . C27 C 0.5888(2) 0.62658(13) 0.34539(11) 0.0289(5) Uani 1 1 d . . . H27 H 0.5570 0.5841 0.3555 0.035 Uiso 1 1 calc R . . C28 C 0.7276(2) 0.35243(11) 0.06968(9) 0.0217(5) Uani 1 1 d . . . C29 C 0.8187(2) 0.35676(13) 0.03225(10) 0.0304(6) Uani 1 1 d . . . H29 H 0.8647 0.3955 0.0343 0.036 Uiso 1 1 calc R . . C30 C 0.8424(3) 0.30460(15) -0.00796(11) 0.0394(7) Uani 1 1 d . . . H30 H 0.9045 0.3079 -0.0334 0.047 Uiso 1 1 calc R . . C31 C 0.7763(3) 0.24799(14) -0.01132(11) 0.0407(7) Uani 1 1 d . . . H31 H 0.7928 0.2125 -0.0390 0.049 Uiso 1 1 calc R . . C32 C 0.6864(3) 0.24295(14) 0.02549(12) 0.0401(7) Uani 1 1 d . . . H32 H 0.6408 0.2041 0.0233 0.048 Uiso 1 1 calc R . . C33 C 0.6626(2) 0.29497(13) 0.06597(11) 0.0322(6) Uani 1 1 d . . . H33 H 0.6007 0.2911 0.0915 0.039 Uiso 1 1 calc R . . C34 C 0.55140(19) 0.43109(11) 0.11577(10) 0.0233(5) Uani 1 1 d . . . C35 C 0.4862(2) 0.44225(13) 0.16586(11) 0.0287(6) Uani 1 1 d . . . H35 H 0.5176 0.4432 0.2052 0.034 Uiso 1 1 calc R . . C36 C 0.3753(2) 0.45204(15) 0.15901(12) 0.0386(7) Uani 1 1 d . . . H36 H 0.3311 0.4602 0.1935 0.046 Uiso 1 1 calc R . . C37 C 0.3288(2) 0.44990(14) 0.10173(11) 0.0365(6) Uani 1 1 d . . . H37 H 0.2525 0.4557 0.0974 0.044 Uiso 1 1 calc R . . C38 C 0.3924(2) 0.43943(14) 0.05113(12) 0.0366(6) Uani 1 1 d . . . H38 H 0.3605 0.4388 0.0119 0.044 Uiso 1 1 calc R . . C39 C 0.5038(2) 0.42971(13) 0.05811(11) 0.0286(6) Uani 1 1 d . . . H39 H 0.5480 0.4221 0.0235 0.034 Uiso 1 1 calc R . . C40 C 0.7667(2) 0.49413(11) 0.10626(9) 0.0227(5) Uani 1 1 d . . . H40A H 0.7305 0.5171 0.0718 0.027 Uiso 1 1 calc R . . H40B H 0.8426 0.4838 0.0945 0.027 Uiso 1 1 calc R . . C41 C 0.6514(2) 0.60679(12) 0.15771(11) 0.0271(5) Uani 1 1 d . . . C42 C 0.6526(2) 0.65015(13) 0.10725(11) 0.0345(6) Uani 1 1 d . . . H42 H 0.7148 0.6517 0.0818 0.041 Uiso 1 1 calc R . . C43 C 0.5636(3) 0.69067(15) 0.09448(12) 0.0440(8) Uani 1 1 d . . . H43 H 0.5646 0.7199 0.0602 0.053 Uiso 1 1 calc R . . C44 C 0.4730(3) 0.68858(17) 0.13165(13) 0.0521(9) Uani 1 1 d . . . H44 H 0.4119 0.7164 0.1226 0.062 Uiso 1 1 calc R . . C45 C 0.4705(3) 0.64663(17) 0.18155(12) 0.0461(8) Uani 1 1 d . . . H45 H 0.4081 0.6455 0.2069 0.055 Uiso 1 1 calc R . . C46 C 0.5597(2) 0.60609(14) 0.19452(12) 0.0339(6) Uani 1 1 d . . . H46 H 0.5582 0.5774 0.2291 0.041 Uiso 1 1 calc R . . C47 C 0.8855(2) 0.60299(12) 0.16362(10) 0.0261(5) Uani 1 1 d . . . C48 C 0.8841(3) 0.67286(13) 0.17747(11) 0.0358(6) Uani 1 1 d . . . H48 H 0.8179 0.6950 0.1877 0.043 Uiso 1 1 calc R . . C49 C 0.9818(3) 0.70912(15) 0.17594(13) 0.0485(9) Uani 1 1 d . . . H49 H 0.9814 0.7562 0.1853 0.058 Uiso 1 1 calc R . . C50 C 1.0783(3) 0.67818(17) 0.16118(13) 0.0507(9) Uani 1 1 d . . . H50 H 1.1439 0.7037 0.1609 0.061 Uiso 1 1 calc R . . C51 C 1.0799(3) 0.61032(17) 0.14685(12) 0.0467(8) Uani 1 1 d . . . H51 H 1.1462 0.5890 0.1356 0.056 Uiso 1 1 calc R . . C52 C 0.9837(2) 0.57288(14) 0.14892(11) 0.0362(6) Uani 1 1 d . . . H52 H 0.9856 0.5256 0.1400 0.043 Uiso 1 1 calc R . . Cl1 Cl 0.37027(7) 0.49732(4) 0.31701(3) 0.0526(2) Uani 1 1 d . . . Cl2 Cl 0.40864(8) 0.35154(5) 0.31662(4) 0.0661(3) Uani 1 1 d . . . C53 C 0.4517(3) 0.43106(18) 0.34347(13) 0.0510(9) Uani 1 1 d . . . H53A H 0.4503 0.4308 0.3883 0.061 Uiso 1 1 calc R . . H53B H 0.5277 0.4390 0.3305 0.061 Uiso 1 1 calc R . . Cl3 Cl -0.02113(8) 0.28421(5) 0.17267(5) 0.0714(3) Uani 1 1 d . . . Cl4 Cl 0.11292(7) 0.40092(5) 0.20513(4) 0.0620(2) Uani 1 1 d . . . C54 C 0.0021(3) 0.37121(17) 0.16403(15) 0.0534(8) Uani 1 1 d . . . H54A H 0.0141 0.3811 0.1206 0.064 Uiso 1 1 calc R . . H54B H -0.0637 0.3963 0.1770 0.064 Uiso 1 1 calc R . . F1 F 0.65678(17) 0.07333(11) 0.02515(11) 0.0826(7) Uani 1 1 d . . . F2 F 0.49041(15) 0.03190(9) 0.04264(8) 0.0566(5) Uani 1 1 d . . . F3 F 0.62385(16) -0.03677(9) 0.00870(8) 0.0576(5) Uani 1 1 d . . . F4 F 0.55072(19) 0.04273(12) -0.05248(7) 0.0748(7) Uani 1 1 d . . . B1 B 0.5802(3) 0.02834(16) 0.00601(13) 0.0309(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01914(8) 0.01536(7) 0.01726(7) 0.00082(6) -0.00062(8) -0.00061(6) P1 0.0227(3) 0.0183(3) 0.0184(3) 0.0019(2) -0.0004(2) 0.0004(2) P2 0.0206(3) 0.0166(3) 0.0201(3) -0.0002(2) -0.0005(2) 0.0002(2) P3 0.0211(3) 0.0206(3) 0.0178(3) -0.0002(2) 0.0000(2) -0.0020(2) P4 0.0248(3) 0.0178(3) 0.0194(2) 0.0022(2) -0.0010(3) -0.0012(3) N1 0.0260(10) 0.0158(8) 0.0198(8) 0.0034(6) 0.0018(10) 0.0001(9) N2 0.0226(11) 0.0179(8) 0.0189(8) -0.0028(6) -0.0008(9) -0.0029(8) C1 0.0307(13) 0.0186(10) 0.0224(10) 0.0014(8) 0.0012(11) -0.0011(11) C2 0.0306(14) 0.0187(11) 0.0253(11) 0.0006(9) -0.0021(10) -0.0051(10) C3 0.0238(12) 0.0191(11) 0.0285(12) 0.0031(9) -0.0050(10) -0.0001(10) C4 0.0253(14) 0.0334(14) 0.0367(14) 0.0062(11) -0.0044(11) -0.0023(12) C5 0.0269(15) 0.0494(18) 0.0484(17) 0.0105(14) 0.0020(13) -0.0026(14) C6 0.0267(14) 0.0323(15) 0.0655(19) 0.0093(14) -0.0124(14) -0.0015(12) C7 0.0445(18) 0.0338(15) 0.0437(16) -0.0024(13) -0.0208(14) 0.0007(14) C8 0.0368(16) 0.0322(14) 0.0285(13) -0.0046(11) -0.0051(11) 0.0052(12) C9 0.0328(15) 0.0262(12) 0.0157(10) -0.0003(8) -0.0018(10) -0.0050(11) C10 0.0310(14) 0.0311(13) 0.0233(12) 0.0026(10) 0.0002(11) -0.0025(11) C11 0.0347(15) 0.0421(16) 0.0233(12) -0.0015(11) 0.0048(11) -0.0097(13) C12 0.0558(19) 0.0340(15) 0.0234(13) 0.0000(11) 0.0004(13) -0.0217(14) C13 0.058(2) 0.0226(12) 0.0277(12) 0.0012(10) -0.0047(13) -0.0084(13) C14 0.0418(16) 0.0229(11) 0.0230(10) -0.0001(9) -0.0007(11) -0.0005(12) C15 0.0248(12) 0.0216(10) 0.0200(9) 0.0004(8) 0.0032(10) -0.0012(10) C16 0.0224(13) 0.0194(11) 0.0281(12) 0.0056(9) -0.0036(10) -0.0012(10) C17 0.0279(14) 0.0283(13) 0.0359(14) 0.0031(11) -0.0035(11) 0.0018(11) C18 0.0247(14) 0.0501(18) 0.0531(18) 0.0089(15) 0.0002(14) -0.0021(14) C19 0.0313(16) 0.0513(19) 0.0550(18) 0.0135(15) -0.0144(15) -0.0126(14) C20 0.0447(18) 0.0404(17) 0.0390(15) 0.0021(12) -0.0162(14) -0.0127(14) C21 0.0356(16) 0.0278(13) 0.0293(13) 0.0000(10) -0.0075(11) -0.0026(11) C22 0.0247(12) 0.0207(11) 0.0205(11) -0.0034(9) -0.0012(10) 0.0042(10) C23 0.0254(13) 0.0252(11) 0.0318(11) 0.0032(9) 0.0012(12) 0.0008(11) C24 0.0386(16) 0.0246(13) 0.0418(15) 0.0036(11) -0.0008(13) 0.0051(12) C25 0.0434(17) 0.0291(14) 0.0374(14) 0.0025(11) -0.0021(13) 0.0134(13) C26 0.0265(14) 0.0351(15) 0.0400(15) -0.0027(12) 0.0022(12) 0.0074(12) C27 0.0273(14) 0.0276(13) 0.0319(13) -0.0018(10) 0.0007(11) -0.0017(11) C28 0.0230(13) 0.0238(11) 0.0183(10) -0.0013(8) -0.0015(9) -0.0004(10) C29 0.0341(15) 0.0312(13) 0.0258(12) -0.0026(10) 0.0009(11) 0.0032(12) C30 0.0453(18) 0.0476(18) 0.0253(13) -0.0004(12) 0.0075(12) 0.0139(15) C31 0.064(2) 0.0340(14) 0.0245(12) -0.0075(10) -0.0059(14) 0.0173(15) C32 0.057(2) 0.0248(13) 0.0380(15) -0.0064(11) -0.0017(15) -0.0042(13) C33 0.0403(16) 0.0281(13) 0.0283(13) -0.0028(10) 0.0041(12) -0.0039(12) C34 0.0227(12) 0.0208(11) 0.0266(12) 0.0030(9) -0.0011(10) -0.0042(9) C35 0.0245(13) 0.0387(14) 0.0228(12) -0.0033(11) -0.0020(10) 0.0001(12) C36 0.0284(15) 0.0525(18) 0.0350(14) -0.0040(13) 0.0041(12) 0.0010(13) C37 0.0225(13) 0.0450(16) 0.0420(15) 0.0016(13) -0.0038(12) 0.0016(13) C38 0.0326(15) 0.0435(16) 0.0339(14) 0.0040(12) -0.0101(12) -0.0018(13) C39 0.0269(13) 0.0358(14) 0.0231(12) 0.0016(10) -0.0008(10) 0.0016(11) C40 0.0246(13) 0.0243(11) 0.0193(10) -0.0005(8) -0.0002(9) -0.0044(10) C41 0.0335(15) 0.0226(12) 0.0250(12) -0.0005(10) -0.0042(11) 0.0015(11) C42 0.0430(17) 0.0358(14) 0.0249(12) 0.0043(11) -0.0007(12) 0.0093(13) C43 0.058(2) 0.0419(17) 0.0320(14) 0.0061(12) -0.0053(14) 0.0216(16) C44 0.054(2) 0.063(2) 0.0389(16) -0.0033(15) -0.0049(15) 0.0372(17) C45 0.0383(17) 0.065(2) 0.0350(15) -0.0043(14) -0.0007(13) 0.0220(16) C46 0.0377(16) 0.0367(15) 0.0274(13) 0.0012(11) -0.0015(12) 0.0067(13) C47 0.0343(15) 0.0246(12) 0.0193(11) 0.0059(9) -0.0034(11) -0.0052(11) C48 0.0501(18) 0.0251(13) 0.0323(14) 0.0009(11) -0.0067(13) -0.0098(13) C49 0.075(3) 0.0297(15) 0.0406(17) 0.0046(13) -0.0116(17) -0.0250(16) C50 0.058(2) 0.054(2) 0.0405(16) 0.0098(15) -0.0085(16) -0.0371(18) C51 0.0371(18) 0.059(2) 0.0443(16) 0.0071(14) -0.0005(14) -0.0206(15) C52 0.0361(16) 0.0336(15) 0.0388(15) 0.0042(12) 0.0014(13) -0.0117(13) Cl1 0.0484(5) 0.0539(5) 0.0553(4) -0.0069(4) -0.0051(4) -0.0017(4) Cl2 0.0662(6) 0.0520(5) 0.0801(6) -0.0046(5) 0.0162(5) 0.0025(5) C53 0.0373(18) 0.074(2) 0.0421(16) -0.0190(16) -0.0058(14) 0.0076(17) Cl3 0.0649(6) 0.0473(5) 0.1020(7) -0.0006(5) 0.0062(6) 0.0148(5) Cl4 0.0403(5) 0.0915(7) 0.0543(5) -0.0052(4) 0.0057(4) -0.0006(5) C54 0.0404(19) 0.059(2) 0.061(2) 0.0190(17) -0.0003(16) 0.0022(17) F1 0.0560(14) 0.0637(14) 0.1281(18) -0.0189(13) -0.0004(13) -0.0246(11) F2 0.0481(11) 0.0565(12) 0.0653(11) 0.0086(9) 0.0315(9) 0.0038(9) F3 0.0575(12) 0.0501(12) 0.0651(11) 0.0027(9) -0.0034(10) 0.0224(10) F4 0.0913(16) 0.1012(17) 0.0319(9) 0.0094(9) -0.0041(10) 0.0439(14) B1 0.0290(16) 0.0327(16) 0.0311(15) 0.0013(12) 0.0026(13) -0.0008(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.0912(16) . ? Rh1 N2 2.0947(16) . ? Rh1 P4 2.1911(5) . ? Rh1 P2 2.1937(6) . ? P1 N1 1.6057(18) . ? P1 C15 1.803(2) . ? P1 C3 1.808(2) . ? P1 C9 1.813(2) . ? P2 C16 1.829(2) . ? P2 C22 1.833(2) . ? P2 C15 1.875(2) . ? P3 N2 1.6099(18) . ? P3 C40 1.802(2) . ? P3 C34 1.807(2) . ? P3 C28 1.809(2) . ? P4 C41 1.820(3) . ? P4 C47 1.830(3) . ? P4 C40 1.882(2) . ? N1 C1 1.480(3) . ? N2 C2 1.475(3) . ? C1 C2 1.520(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.385(3) . ? C3 C8 1.385(3) . ? C4 C5 1.398(4) . ? C4 H4 0.9500 . ? C5 C6 1.381(4) . ? C5 H5 0.9500 . ? C6 C7 1.378(4) . ? C6 H6 0.9500 . ? C7 C8 1.394(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.394(3) . ? C9 C14 1.394(3) . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 C13 1.383(4) . ? C12 H12 0.9500 . ? C13 C14 1.391(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.388(3) . ? C16 C21 1.400(3) . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 C19 1.376(4) . ? C18 H18 0.9500 . ? C19 C20 1.391(4) . ? C19 H19 0.9500 . ? C20 C21 1.374(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.393(3) . ? C22 C27 1.394(3) . ? C23 C24 1.383(3) . ? C23 H23 0.9500 . ? C24 C25 1.392(4) . ? C24 H24 0.9500 . ? C25 C26 1.380(4) . ? C25 H25 0.9500 . ? C26 C27 1.378(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.387(3) . ? C28 C29 1.395(3) . ? C29 C30 1.388(4) . ? C29 H29 0.9500 . ? C30 C31 1.381(4) . ? C30 H30 0.9500 . ? C31 C32 1.375(4) . ? C31 H31 0.9500 . ? C32 C33 1.390(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.384(3) . ? C34 C39 1.401(3) . ? C35 C36 1.385(4) . ? C35 H35 0.9500 . ? C36 C37 1.389(4) . ? C36 H36 0.9500 . ? C37 C38 1.379(4) . ? C37 H37 0.9500 . ? C38 C39 1.392(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.390(4) . ? C41 C42 1.403(3) . ? C42 C43 1.384(4) . ? C42 H42 0.9500 . ? C43 C44 1.384(4) . ? C43 H43 0.9500 . ? C44 C45 1.377(4) . ? C44 H44 0.9500 . ? C45 C46 1.387(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.384(4) . ? C47 C48 1.408(3) . ? C48 C49 1.398(4) . ? C48 H48 0.9500 . ? C49 C50 1.373(5) . ? C49 H49 0.9500 . ? C50 C51 1.372(4) . ? C50 H50 0.9500 . ? C51 C52 1.395(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? Cl1 C53 1.745(3) . ? Cl2 C53 1.755(3) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? Cl3 C54 1.746(3) . ? Cl4 C54 1.739(3) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? F1 B1 1.360(4) . ? F2 B1 1.370(3) . ? F3 B1 1.390(4) . ? F4 B1 1.371(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2 80.55(7) . . ? N1 Rh1 P4 170.30(5) . . ? N2 Rh1 P4 89.78(5) . . ? N1 Rh1 P2 89.41(5) . . ? N2 Rh1 P2 169.92(5) . . ? P4 Rh1 P2 100.28(2) . . ? N1 P1 C15 104.56(9) . . ? N1 P1 C3 117.37(11) . . ? C15 P1 C3 107.04(11) . . ? N1 P1 C9 112.97(10) . . ? C15 P1 C9 110.95(11) . . ? C3 P1 C9 103.90(11) . . ? C16 P2 C22 102.70(11) . . ? C16 P2 C15 101.92(10) . . ? C22 P2 C15 103.39(10) . . ? C16 P2 Rh1 120.39(8) . . ? C22 P2 Rh1 120.87(7) . . ? C15 P2 Rh1 104.80(7) . . ? N2 P3 C40 105.01(10) . . ? N2 P3 C34 115.26(11) . . ? C40 P3 C34 108.62(11) . . ? N2 P3 C28 114.66(10) . . ? C40 P3 C28 109.09(10) . . ? C34 P3 C28 104.05(11) . . ? C41 P4 C47 104.30(11) . . ? C41 P4 C40 101.45(11) . . ? C47 P4 C40 102.03(11) . . ? C41 P4 Rh1 120.91(9) . . ? C47 P4 Rh1 119.67(8) . . ? C40 P4 Rh1 105.35(7) . . ? C1 N1 P1 123.26(14) . . ? C1 N1 Rh1 111.81(12) . . ? P1 N1 Rh1 117.64(10) . . ? C2 N2 P3 122.58(15) . . ? C2 N2 Rh1 111.64(12) . . ? P3 N2 Rh1 117.19(10) . . ? N1 C1 C2 108.10(17) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 108.69(18) . . ? N2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C4 C3 C8 119.8(2) . . ? C4 C3 P1 120.02(18) . . ? C8 C3 P1 120.08(19) . . ? C3 C4 C5 119.5(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C7 C6 C5 120.8(3) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 119.1(3) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C3 C8 C7 120.7(3) . . ? C3 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C14 119.3(2) . . ? C10 C9 P1 121.90(19) . . ? C14 C9 P1 118.72(19) . . ? C11 C10 C9 120.2(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 120.0(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.5(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 119.7(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C9 120.4(3) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? P1 C15 P2 106.59(10) . . ? P1 C15 H15A 110.4 . . ? P2 C15 H15A 110.4 . . ? P1 C15 H15B 110.4 . . ? P2 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? C17 C16 C21 119.0(2) . . ? C17 C16 P2 119.16(18) . . ? C21 C16 P2 121.8(2) . . ? C16 C17 C18 120.4(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.3(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C16 120.4(3) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C23 C22 C27 118.7(2) . . ? C23 C22 P2 120.24(19) . . ? C27 C22 P2 120.68(18) . . ? C24 C23 C22 120.9(2) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 119.2(3) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 120.4(2) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C25 120.0(3) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 120.7(2) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? C33 C28 C29 118.5(2) . . ? C33 C28 P3 119.09(18) . . ? C29 C28 P3 122.29(18) . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.5(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 119.7(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C28 C33 C32 121.1(3) . . ? C28 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C35 C34 C39 119.1(2) . . ? C35 C34 P3 120.02(18) . . ? C39 C34 P3 120.84(19) . . ? C34 C35 C36 120.4(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 120.0(3) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.6(3) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 119.3(2) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C38 C39 C34 120.6(2) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? P3 C40 P4 107.47(10) . . ? P3 C40 H40A 110.2 . . ? P4 C40 H40A 110.2 . . ? P3 C40 H40B 110.2 . . ? P4 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? C46 C41 C42 118.6(2) . . ? C46 C41 P4 119.34(18) . . ? C42 C41 P4 122.1(2) . . ? C43 C42 C41 120.2(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.9(3) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.7(3) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 119.5(3) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C45 C46 C41 121.1(2) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? C52 C47 C48 118.6(3) . . ? C52 C47 P4 120.02(19) . . ? C48 C47 P4 120.8(2) . . ? C49 C48 C47 118.8(3) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C50 C49 C48 121.5(3) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C51 C50 C49 119.9(3) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C50 C51 C52 119.6(3) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C47 C52 C51 121.5(3) . . ? C47 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? Cl1 C53 Cl2 112.32(17) . . ? Cl1 C53 H53A 109.1 . . ? Cl2 C53 H53A 109.1 . . ? Cl1 C53 H53B 109.1 . . ? Cl2 C53 H53B 109.1 . . ? H53A C53 H53B 107.9 . . ? Cl4 C54 Cl3 113.63(18) . . ? Cl4 C54 H54A 108.8 . . ? Cl3 C54 H54A 108.8 . . ? Cl4 C54 H54B 108.8 . . ? Cl3 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? F1 B1 F2 110.0(2) . . ? F1 B1 F4 110.0(3) . . ? F2 B1 F4 109.4(2) . . ? F1 B1 F3 108.6(3) . . ? F2 B1 F3 109.5(2) . . ? F4 B1 F3 109.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.680 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.066 #===END #compound 3_BF4 data_ab807 _database_code_depnum_ccdc_archive 'CCDC 772853' #TrackingRef '- 2010_buchard_njc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Cl2 N2 P4 Rh, 3(C H Cl3), B F4' _chemical_formula_sum 'C55 H51 B Cl11 F4 N2 P4 Rh' _chemical_formula_weight 1443.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 10.806(1) _cell_length_b 35.589(1) _cell_length_c 16.434(1) _cell_angle_alpha 90.00 _cell_angle_beta 100.108(1) _cell_angle_gamma 90.00 _cell_volume 6222.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 44719 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7147 _exptl_absorpt_correction_T_max 0.9315 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 40501 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 30.03 _reflns_number_total 17688 _reflns_number_gt 12337 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0791P)^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 17688 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.294774(18) 0.114745(6) 0.890380(12) 0.01891(6) Uani 1 1 d . . . Cl1 Cl 0.12214(6) 0.12626(2) 0.95767(4) 0.02322(14) Uani 1 1 d . . . Cl2 Cl 0.45998(6) 0.09572(2) 0.82276(4) 0.02373(14) Uani 1 1 d . . . P1 P 0.11933(6) 0.07330(2) 0.73714(4) 0.02286(16) Uani 1 1 d . . . P2 P 0.22777(6) 0.14962(2) 0.77329(4) 0.02085(15) Uani 1 1 d . . . P3 P 0.42791(6) 0.07947(2) 1.06532(4) 0.02241(15) Uani 1 1 d . . . P4 P 0.40489(6) 0.15526(2) 0.98660(4) 0.02107(15) Uani 1 1 d . . . N1 N 0.1917(2) 0.07053(7) 0.82996(13) 0.0226(5) Uani 1 1 d . . . N2 N 0.3493(2) 0.07215(7) 0.97584(13) 0.0221(5) Uani 1 1 d . . . C1 C 0.1865(3) 0.03842(8) 0.88519(18) 0.0292(6) Uani 1 1 d . . . H1A H 0.1663 0.0152 0.8525 0.035 Uiso 1 1 calc R . . H1B H 0.1206 0.0425 0.9192 0.035 Uiso 1 1 calc R . . C2 C 0.3156(3) 0.03481(9) 0.94081(18) 0.0291(6) Uani 1 1 d . . . H2A H 0.3120 0.0164 0.9855 0.035 Uiso 1 1 calc R . . H2B H 0.3790 0.0262 0.9082 0.035 Uiso 1 1 calc R . . C3 C 0.1404(3) 0.03055(9) 0.68313(17) 0.0266(6) Uani 1 1 d . . . C4 C 0.2627(3) 0.01748(10) 0.68775(19) 0.0344(7) Uani 1 1 d . . . H4 H 0.3309 0.0322 0.7148 0.041 Uiso 1 1 calc R . . C5 C 0.2864(3) -0.01660(11) 0.6536(2) 0.0431(9) Uani 1 1 d . . . H5 H 0.3704 -0.0251 0.6566 0.052 Uiso 1 1 calc R . . C6 C 0.1864(4) -0.03854(11) 0.6148(2) 0.0484(9) Uani 1 1 d . . . H6 H 0.2019 -0.0622 0.5917 0.058 Uiso 1 1 calc R . . C7 C 0.0665(4) -0.02592(12) 0.6102(2) 0.0551(10) Uani 1 1 d . . . H7 H -0.0013 -0.0409 0.5835 0.066 Uiso 1 1 calc R . . C8 C 0.0414(3) 0.00842(10) 0.6438(2) 0.0405(8) Uani 1 1 d . . . H8 H -0.0429 0.0168 0.6400 0.049 Uiso 1 1 calc R . . C9 C -0.0462(3) 0.08358(9) 0.72281(18) 0.0268(6) Uani 1 1 d . . . C10 C -0.1015(3) 0.08931(9) 0.79206(18) 0.0293(6) Uani 1 1 d . . . H10 H -0.0530 0.0868 0.8459 0.035 Uiso 1 1 calc R . . C11 C -0.2282(3) 0.09869(10) 0.7821(2) 0.0359(7) Uani 1 1 d . . . H11 H -0.2666 0.1025 0.8292 0.043 Uiso 1 1 calc R . . C12 C -0.2977(3) 0.10248(11) 0.7040(2) 0.0421(9) Uani 1 1 d . . . H12 H -0.3843 0.1088 0.6974 0.051 Uiso 1 1 calc R . . C13 C -0.2428(3) 0.09721(12) 0.6351(2) 0.0439(9) Uani 1 1 d . . . H13 H -0.2919 0.1000 0.5815 0.053 Uiso 1 1 calc R . . C14 C -0.1169(3) 0.08783(11) 0.64339(19) 0.0367(8) Uani 1 1 d . . . H14 H -0.0790 0.0843 0.5960 0.044 Uiso 1 1 calc R . . C15 C 0.1927(2) 0.11234(8) 0.69431(16) 0.0241(6) Uani 1 1 d . . . H15A H 0.1357 0.1222 0.6452 0.029 Uiso 1 1 calc R . . H15B H 0.2714 0.1039 0.6769 0.029 Uiso 1 1 calc R . . C16 C 0.0871(2) 0.17845(9) 0.76452(17) 0.0257(6) Uani 1 1 d . . . C17 C 0.0034(3) 0.18181(10) 0.6898(2) 0.0387(8) Uani 1 1 d . . . H17 H 0.0166 0.1680 0.6426 0.046 Uiso 1 1 calc R . . C18 C -0.1003(3) 0.20578(11) 0.6856(2) 0.0480(10) Uani 1 1 d . . . H18 H -0.1580 0.2081 0.6351 0.058 Uiso 1 1 calc R . . C19 C -0.1196(3) 0.22608(11) 0.7534(2) 0.0455(9) Uani 1 1 d . . . H19 H -0.1903 0.2422 0.7497 0.055 Uiso 1 1 calc R . . C20 C -0.0367(3) 0.22299(9) 0.8265(2) 0.0346(7) Uani 1 1 d . . . H20 H -0.0501 0.2371 0.8732 0.041 Uiso 1 1 calc R . . C21 C 0.0665(3) 0.19939(9) 0.83284(18) 0.0286(6) Uani 1 1 d . . . H21 H 0.1234 0.1974 0.8838 0.034 Uiso 1 1 calc R . . C22 C 0.3394(2) 0.18019(8) 0.73379(16) 0.0235(6) Uani 1 1 d . . . C23 C 0.4184(3) 0.16734(10) 0.6815(2) 0.0350(7) Uani 1 1 d . . . H23 H 0.4129 0.1420 0.6630 0.042 Uiso 1 1 calc R . . C24 C 0.5053(3) 0.19149(11) 0.6562(2) 0.0426(8) Uani 1 1 d . . . H24 H 0.5583 0.1826 0.6200 0.051 Uiso 1 1 calc R . . C25 C 0.5156(3) 0.22807(11) 0.6829(2) 0.0419(9) Uani 1 1 d . . . H25 H 0.5764 0.2442 0.6661 0.050 Uiso 1 1 calc R . . C26 C 0.4375(3) 0.24120(10) 0.7342(2) 0.0409(8) Uani 1 1 d . . . H26 H 0.4443 0.2665 0.7527 0.049 Uiso 1 1 calc R . . C27 C 0.3487(3) 0.21762(10) 0.75914(19) 0.0335(7) Uani 1 1 d . . . H27 H 0.2940 0.2271 0.7937 0.040 Uiso 1 1 calc R . . C28 C 0.3700(3) 0.05006(9) 1.13897(16) 0.0248(6) Uani 1 1 d . . . C29 C 0.2437(3) 0.05333(10) 1.1448(2) 0.0402(8) Uani 1 1 d . . . H29 H 0.1941 0.0725 1.1150 0.048 Uiso 1 1 calc R . . C30 C 0.1896(3) 0.02872(11) 1.1938(2) 0.0466(9) Uani 1 1 d . . . H30 H 0.1041 0.0317 1.1994 0.056 Uiso 1 1 calc R . . C31 C 0.2600(3) -0.00022(10) 1.23460(19) 0.0355(7) Uani 1 1 d . . . H31 H 0.2226 -0.0172 1.2676 0.043 Uiso 1 1 calc R . . C32 C 0.3844(3) -0.00446(9) 1.22754(19) 0.0343(7) Uani 1 1 d . . . H32 H 0.4323 -0.0246 1.2551 0.041 Uiso 1 1 calc R . . C33 C 0.4398(3) 0.02074(9) 1.18002(17) 0.0280(6) Uani 1 1 d . . . H33 H 0.5258 0.0179 1.1756 0.034 Uiso 1 1 calc R . . C34 C 0.5969(3) 0.07333(8) 1.07887(18) 0.0274(6) Uani 1 1 d . . . C35 C 0.6739(3) 0.07939(9) 1.1553(2) 0.0340(7) Uani 1 1 d . . . H35 H 0.6374 0.0847 1.2026 0.041 Uiso 1 1 calc R . . C36 C 0.8040(3) 0.07776(11) 1.1624(2) 0.0436(9) Uani 1 1 d . . . H36 H 0.8566 0.0818 1.2143 0.052 Uiso 1 1 calc R . . C37 C 0.8557(3) 0.07015(11) 1.0929(2) 0.0434(9) Uani 1 1 d . . . H37 H 0.9445 0.0691 1.0973 0.052 Uiso 1 1 calc R . . C38 C 0.7800(3) 0.06405(11) 1.0172(2) 0.0416(8) Uani 1 1 d . . . H38 H 0.8170 0.0588 0.9701 0.050 Uiso 1 1 calc R . . C39 C 0.6498(3) 0.06561(9) 1.00955(19) 0.0314(7) Uani 1 1 d . . . H39 H 0.5977 0.0614 0.9575 0.038 Uiso 1 1 calc R . . C40 C 0.4010(3) 0.12865(8) 1.08288(16) 0.0236(6) Uani 1 1 d . . . H40A H 0.4667 0.1382 1.1277 0.028 Uiso 1 1 calc R . . H40B H 0.3182 0.1319 1.1000 0.028 Uiso 1 1 calc R . . C41 C 0.5707(3) 0.16601(9) 0.98900(17) 0.0262(6) Uani 1 1 d . . . C42 C 0.6492(3) 0.17416(11) 1.06331(19) 0.0418(9) Uani 1 1 d . . . H42 H 0.6164 0.1742 1.1133 0.050 Uiso 1 1 calc R . . C43 C 0.7751(3) 0.18218(13) 1.0650(2) 0.0522(11) Uani 1 1 d . . . H43 H 0.8283 0.1873 1.1162 0.063 Uiso 1 1 calc R . . C44 C 0.8233(3) 0.18282(11) 0.9936(2) 0.0479(9) Uani 1 1 d . . . H44 H 0.9098 0.1881 0.9953 0.057 Uiso 1 1 calc R . . C45 C 0.7456(3) 0.17577(11) 0.9190(2) 0.0482(10) Uani 1 1 d . . . H45 H 0.7787 0.1767 0.8691 0.058 Uiso 1 1 calc R . . C46 C 0.6193(3) 0.16737(10) 0.9165(2) 0.0364(7) Uani 1 1 d . . . H46 H 0.5663 0.1626 0.8650 0.044 Uiso 1 1 calc R . . C47 C 0.3399(3) 0.20126(8) 1.00463(16) 0.0246(6) Uani 1 1 d . . . C48 C 0.3852(3) 0.23271(9) 0.96818(18) 0.0308(7) Uani 1 1 d . . . H48 H 0.4538 0.2303 0.9395 0.037 Uiso 1 1 calc R . . C49 C 0.3294(3) 0.26769(10) 0.9741(2) 0.0409(8) Uani 1 1 d . . . H49 H 0.3588 0.2889 0.9481 0.049 Uiso 1 1 calc R . . C50 C 0.2318(3) 0.27173(10) 1.0174(2) 0.0431(9) Uani 1 1 d . . . H50 H 0.1938 0.2956 1.0209 0.052 Uiso 1 1 calc R . . C51 C 0.1897(3) 0.24089(10) 1.0556(2) 0.0393(8) Uani 1 1 d . . . H51 H 0.1240 0.2438 1.0866 0.047 Uiso 1 1 calc R . . C52 C 0.2424(3) 0.20575(9) 1.04909(17) 0.0305(7) Uani 1 1 d . . . H52 H 0.2119 0.1847 1.0750 0.037 Uiso 1 1 calc R . . F1 F 0.0745(2) 0.09106(6) 0.50665(12) 0.0504(5) Uani 1 1 d . . . F2 F 0.1755(2) 0.13927(7) 0.45729(14) 0.0631(6) Uani 1 1 d . . . F3 F -0.0036(2) 0.15014(8) 0.50513(14) 0.0681(7) Uani 1 1 d . . . F4 F -0.0086(2) 0.11877(7) 0.38423(12) 0.0622(7) Uani 1 1 d . . . B1 B 0.0579(3) 0.12542(10) 0.4637(2) 0.0282(7) Uani 1 1 d . . . Cl3 Cl 0.32036(10) 0.15992(3) 0.27597(6) 0.0605(3) Uani 1 1 d . . . Cl4 Cl 0.09939(11) 0.20451(3) 0.27873(8) 0.0697(3) Uani 1 1 d . . . Cl5 Cl 0.08056(10) 0.13902(3) 0.17688(7) 0.0628(3) Uani 1 1 d . . . C53 C 0.1572(4) 0.15941(11) 0.2707(2) 0.0469(9) Uani 1 1 d . . . H53 H 0.1374 0.1441 0.3177 0.056 Uiso 1 1 calc R . . Cl6 Cl 0.44461(12) 0.06937(5) 0.55705(8) 0.0879(4) Uani 1 1 d . . . Cl7 Cl 0.30979(19) 0.01104(5) 0.45611(8) 0.1306(8) Uani 1 1 d . . . Cl8 Cl 0.3920(2) 0.07501(4) 0.38092(9) 0.1223(7) Uani 1 1 d . . . C54 C 0.3371(4) 0.05831(15) 0.4672(2) 0.0680(14) Uani 1 1 d . . . H54 H 0.2556 0.0711 0.4702 0.082 Uiso 1 1 calc R . . Cl9 Cl 0.71946(13) 0.22128(4) 0.42752(9) 0.0874(4) Uani 1 1 d . . . Cl10 Cl 0.62450(14) 0.14511(5) 0.42352(10) 0.1089(6) Uani 1 1 d . . . Cl11 Cl 0.72104(17) 0.17470(5) 0.28571(7) 0.1026(5) Uani 1 1 d . . . C55 C 0.7349(4) 0.17499(13) 0.3931(2) 0.0562(11) Uani 1 1 d . . . H55 H 0.8207 0.1657 0.4177 0.067 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 0.01929(10) 0.01767(11) 0.01981(10) -0.00025(8) 0.00356(7) -0.00025(8) Cl1 0.0226(3) 0.0249(4) 0.0228(3) -0.0009(3) 0.0058(2) 0.0014(3) Cl2 0.0204(3) 0.0255(4) 0.0260(3) -0.0014(3) 0.0061(2) 0.0007(3) P1 0.0201(3) 0.0246(4) 0.0239(3) -0.0029(3) 0.0038(3) -0.0031(3) P2 0.0203(3) 0.0212(4) 0.0209(3) 0.0007(3) 0.0033(3) -0.0002(3) P3 0.0225(3) 0.0207(4) 0.0237(3) 0.0030(3) 0.0034(3) 0.0015(3) P4 0.0233(3) 0.0193(4) 0.0203(3) -0.0001(3) 0.0027(3) -0.0004(3) N1 0.0226(11) 0.0200(13) 0.0246(11) -0.0017(9) 0.0020(9) -0.0059(10) N2 0.0264(11) 0.0159(12) 0.0243(11) 0.0035(9) 0.0052(9) 0.0035(9) C1 0.0352(15) 0.0194(15) 0.0329(15) -0.0011(12) 0.0055(12) -0.0073(13) C2 0.0345(15) 0.0196(15) 0.0327(15) 0.0013(12) 0.0047(12) 0.0003(13) C3 0.0282(14) 0.0258(16) 0.0252(13) -0.0020(12) 0.0028(11) -0.0031(12) C4 0.0318(15) 0.035(2) 0.0343(16) -0.0069(14) 0.0007(13) 0.0047(14) C5 0.0470(19) 0.041(2) 0.0395(18) -0.0083(16) 0.0029(15) 0.0130(17) C6 0.072(3) 0.031(2) 0.0425(19) -0.0121(16) 0.0105(18) 0.0019(19) C7 0.056(2) 0.046(3) 0.061(2) -0.023(2) 0.0030(19) -0.013(2) C8 0.0333(16) 0.039(2) 0.0485(19) -0.0157(16) 0.0040(14) -0.0076(15) C9 0.0219(12) 0.0251(16) 0.0334(15) -0.0009(12) 0.0053(11) -0.0060(12) C10 0.0256(13) 0.0310(18) 0.0312(15) -0.0049(13) 0.0050(12) -0.0032(13) C11 0.0276(14) 0.037(2) 0.0451(18) -0.0068(15) 0.0116(13) -0.0012(14) C12 0.0214(14) 0.045(2) 0.059(2) 0.0120(18) 0.0048(14) 0.0034(14) C13 0.0276(15) 0.060(3) 0.0414(18) 0.0148(18) -0.0018(14) -0.0012(16) C14 0.0246(14) 0.051(2) 0.0341(16) 0.0077(15) 0.0040(12) -0.0028(14) C15 0.0223(12) 0.0287(16) 0.0217(12) -0.0021(11) 0.0049(10) -0.0011(12) C16 0.0221(12) 0.0256(16) 0.0293(14) 0.0058(12) 0.0045(11) 0.0006(12) C17 0.0348(16) 0.043(2) 0.0351(16) -0.0009(15) -0.0032(13) 0.0040(15) C18 0.0346(17) 0.050(3) 0.052(2) 0.0048(19) -0.0110(16) 0.0110(17) C19 0.0297(16) 0.037(2) 0.069(2) 0.0025(18) 0.0070(16) 0.0106(15) C20 0.0327(15) 0.0264(17) 0.0475(18) 0.0021(14) 0.0151(14) 0.0029(14) C21 0.0295(14) 0.0251(16) 0.0331(15) 0.0055(13) 0.0104(12) 0.0021(13) C22 0.0209(12) 0.0256(16) 0.0222(12) 0.0055(11) -0.0009(10) -0.0002(11) C23 0.0340(16) 0.0318(18) 0.0425(17) 0.0042(15) 0.0159(14) -0.0016(14) C24 0.0350(17) 0.046(2) 0.052(2) 0.0090(18) 0.0198(15) -0.0012(16) C25 0.0304(16) 0.043(2) 0.051(2) 0.0153(17) 0.0038(15) -0.0078(15) C26 0.0409(17) 0.0271(18) 0.054(2) 0.0034(16) 0.0054(16) -0.0134(15) C27 0.0335(15) 0.0324(19) 0.0344(16) -0.0001(14) 0.0056(13) -0.0067(14) C28 0.0264(13) 0.0238(15) 0.0242(13) 0.0033(11) 0.0051(11) 0.0005(12) C29 0.0259(15) 0.039(2) 0.057(2) 0.0214(17) 0.0109(14) 0.0075(14) C30 0.0293(16) 0.052(2) 0.060(2) 0.0238(19) 0.0117(15) 0.0029(16) C31 0.0388(16) 0.0326(19) 0.0366(16) 0.0075(14) 0.0105(14) -0.0068(14) C32 0.0387(16) 0.0275(18) 0.0375(16) 0.0073(14) 0.0084(14) 0.0036(14) C33 0.0293(14) 0.0265(16) 0.0292(14) 0.0037(12) 0.0076(11) 0.0046(13) C34 0.0267(13) 0.0198(15) 0.0353(15) 0.0084(12) 0.0038(12) 0.0016(12) C35 0.0320(15) 0.0325(19) 0.0355(16) 0.0043(14) 0.0000(13) -0.0025(14) C36 0.0292(16) 0.042(2) 0.054(2) 0.0110(17) -0.0077(15) -0.0039(15) C37 0.0228(14) 0.043(2) 0.062(2) 0.0120(18) 0.0020(15) 0.0031(15) C38 0.0318(16) 0.042(2) 0.054(2) 0.0110(17) 0.0160(15) 0.0106(15) C39 0.0275(14) 0.0326(18) 0.0345(15) 0.0086(13) 0.0063(12) 0.0069(13) C40 0.0281(13) 0.0203(15) 0.0230(13) 0.0020(11) 0.0066(11) 0.0025(12) C41 0.0246(13) 0.0229(15) 0.0311(14) 0.0004(12) 0.0052(11) -0.0033(12) C42 0.0333(16) 0.060(3) 0.0307(16) 0.0078(16) 0.0015(13) -0.0138(17) C43 0.0307(16) 0.074(3) 0.048(2) 0.014(2) -0.0041(15) -0.0164(18) C44 0.0262(15) 0.045(2) 0.072(3) 0.0052(19) 0.0092(16) -0.0077(16) C45 0.047(2) 0.047(2) 0.057(2) -0.0133(18) 0.0276(17) -0.0195(18) C46 0.0377(16) 0.037(2) 0.0357(16) -0.0067(14) 0.0107(13) -0.0171(15) C47 0.0317(14) 0.0180(14) 0.0217(12) -0.0023(11) -0.0021(11) 0.0004(12) C48 0.0382(16) 0.0218(16) 0.0308(15) 0.0006(12) 0.0021(13) -0.0013(13) C49 0.056(2) 0.0235(18) 0.0384(17) 0.0036(14) -0.0043(16) 0.0009(16) C50 0.057(2) 0.0235(18) 0.0420(18) -0.0044(15) -0.0089(16) 0.0127(16) C51 0.0444(18) 0.037(2) 0.0353(16) -0.0101(15) 0.0026(14) 0.0085(16) C52 0.0378(16) 0.0259(17) 0.0266(14) -0.0046(12) 0.0026(12) 0.0028(13) F1 0.0670(14) 0.0467(14) 0.0373(10) -0.0006(9) 0.0090(10) -0.0115(11) F2 0.0612(14) 0.0588(17) 0.0713(15) -0.0007(13) 0.0175(12) -0.0178(12) F3 0.0788(16) 0.0723(19) 0.0555(13) -0.0128(13) 0.0181(12) 0.0139(14) F4 0.0872(17) 0.0626(17) 0.0330(11) -0.0008(10) -0.0002(11) -0.0232(13) B1 0.0354(17) 0.0274(19) 0.0237(15) -0.0049(14) 0.0107(13) -0.0066(15) Cl3 0.0642(6) 0.0679(8) 0.0479(5) -0.0053(5) 0.0060(5) 0.0153(6) Cl4 0.0783(7) 0.0440(6) 0.0869(8) -0.0184(6) 0.0149(6) 0.0137(6) Cl5 0.0662(6) 0.0586(7) 0.0685(6) -0.0233(5) 0.0255(5) -0.0208(6) C53 0.074(3) 0.034(2) 0.0393(18) -0.0001(16) 0.0281(18) 0.0000(19) Cl6 0.0668(7) 0.1156(13) 0.0750(8) -0.0244(8) -0.0051(6) -0.0294(8) Cl7 0.1839(17) 0.1388(16) 0.0553(7) 0.0220(8) -0.0172(9) -0.1091(14) Cl8 0.236(2) 0.0624(10) 0.0716(8) -0.0010(7) 0.0361(11) -0.0499(12) C54 0.040(2) 0.107(4) 0.055(2) -0.023(3) 0.0031(18) 0.011(2) Cl9 0.0946(9) 0.0704(9) 0.0994(10) -0.0154(8) 0.0227(8) -0.0010(7) Cl10 0.0863(9) 0.1123(14) 0.1200(12) 0.0595(10) -0.0043(9) -0.0375(9) Cl11 0.1537(15) 0.1017(13) 0.0474(6) 0.0026(7) 0.0042(8) -0.0109(10) C55 0.058(2) 0.053(3) 0.053(2) 0.010(2) -0.0009(19) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.077(2) . ? Rh1 N2 2.080(2) . ? Rh1 P2 2.2974(7) . ? Rh1 P4 2.3097(7) . ? Rh1 Cl2 2.3616(7) . ? Rh1 Cl1 2.3653(7) . ? P1 N1 1.591(2) . ? P1 C3 1.796(3) . ? P1 C9 1.801(3) . ? P1 C15 1.803(3) . ? P2 C16 1.818(3) . ? P2 C22 1.826(3) . ? P2 C15 1.848(3) . ? P3 N2 1.585(2) . ? P3 C28 1.794(3) . ? P3 C40 1.806(3) . ? P3 C34 1.814(3) . ? P4 C41 1.825(3) . ? P4 C47 1.826(3) . ? P4 C40 1.851(3) . ? N1 C1 1.467(4) . ? N2 C2 1.468(4) . ? C1 C2 1.533(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.390(4) . ? C3 C8 1.393(4) . ? C4 C5 1.379(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 C7 1.361(5) . ? C6 H6 0.9500 . ? C7 C8 1.388(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.390(4) . ? C9 C14 1.400(4) . ? C10 C11 1.390(4) . ? C10 H10 0.9500 . ? C11 C12 1.376(4) . ? C11 H11 0.9500 . ? C12 C13 1.380(5) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.396(4) . ? C16 C21 1.398(4) . ? C17 C18 1.400(5) . ? C17 H17 0.9500 . ? C18 C19 1.375(5) . ? C18 H18 0.9500 . ? C19 C20 1.371(5) . ? C19 H19 0.9500 . ? C20 C21 1.385(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.390(4) . ? C22 C27 1.394(4) . ? C23 C24 1.389(4) . ? C23 H23 0.9500 . ? C24 C25 1.372(5) . ? C24 H24 0.9500 . ? C25 C26 1.375(5) . ? C25 H25 0.9500 . ? C26 C27 1.390(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.390(4) . ? C28 C33 1.390(4) . ? C29 C30 1.387(4) . ? C29 H29 0.9500 . ? C30 C31 1.382(5) . ? C30 H30 0.9500 . ? C31 C32 1.377(4) . ? C31 H31 0.9500 . ? C32 C33 1.392(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.389(4) . ? C34 C35 1.396(4) . ? C35 C36 1.391(4) . ? C35 H35 0.9500 . ? C36 C37 1.384(5) . ? C36 H36 0.9500 . ? C37 C38 1.380(5) . ? C37 H37 0.9500 . ? C38 C39 1.392(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.385(4) . ? C41 C42 1.390(4) . ? C42 C43 1.386(4) . ? C42 H42 0.9500 . ? C43 C44 1.363(5) . ? C43 H43 0.9500 . ? C44 C45 1.383(5) . ? C44 H44 0.9500 . ? C45 C46 1.391(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.393(4) . ? C47 C48 1.398(4) . ? C48 C49 1.394(5) . ? C48 H48 0.9500 . ? C49 C50 1.379(5) . ? C49 H49 0.9500 . ? C50 C51 1.381(5) . ? C50 H50 0.9500 . ? C51 C52 1.386(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? F1 B1 1.408(4) . ? F2 B1 1.384(4) . ? F3 B1 1.355(4) . ? F4 B1 1.396(4) . ? Cl3 C53 1.750(4) . ? Cl4 C53 1.736(4) . ? Cl5 C53 1.772(4) . ? C53 H53 1.0000 . ? Cl6 C54 1.756(4) . ? Cl7 C54 1.712(5) . ? Cl8 C54 1.735(5) . ? C54 H54 1.0000 . ? Cl9 C55 1.759(5) . ? Cl10 C55 1.736(4) . ? Cl11 C55 1.745(4) . ? C55 H55 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2 80.51(9) . . ? N1 Rh1 P2 86.85(7) . . ? N2 Rh1 P2 165.80(7) . . ? N1 Rh1 P4 165.65(7) . . ? N2 Rh1 P4 86.67(7) . . ? P2 Rh1 P4 106.56(3) . . ? N1 Rh1 Cl2 86.79(7) . . ? N2 Rh1 Cl2 87.76(7) . . ? P2 Rh1 Cl2 85.06(3) . . ? P4 Rh1 Cl2 99.21(3) . . ? N1 Rh1 Cl1 87.36(7) . . ? N2 Rh1 Cl1 87.91(7) . . ? P2 Rh1 Cl1 98.02(2) . . ? P4 Rh1 Cl1 85.73(3) . . ? Cl2 Rh1 Cl1 173.23(3) . . ? N1 P1 C3 109.75(13) . . ? N1 P1 C9 116.62(13) . . ? C3 P1 C9 108.46(13) . . ? N1 P1 C15 104.26(12) . . ? C3 P1 C15 110.94(13) . . ? C9 P1 C15 106.70(14) . . ? C16 P2 C22 103.33(13) . . ? C16 P2 C15 106.49(13) . . ? C22 P2 C15 104.17(13) . . ? C16 P2 Rh1 120.49(9) . . ? C22 P2 Rh1 119.26(8) . . ? C15 P2 Rh1 101.32(9) . . ? N2 P3 C28 109.65(13) . . ? N2 P3 C40 103.43(12) . . ? C28 P3 C40 111.88(14) . . ? N2 P3 C34 117.28(13) . . ? C28 P3 C34 108.04(13) . . ? C40 P3 C34 106.50(14) . . ? C41 P4 C47 102.27(14) . . ? C41 P4 C40 104.96(13) . . ? C47 P4 C40 104.65(13) . . ? C41 P4 Rh1 122.09(10) . . ? C47 P4 Rh1 120.28(9) . . ? C40 P4 Rh1 100.35(10) . . ? C1 N1 P1 125.16(19) . . ? C1 N1 Rh1 111.72(16) . . ? P1 N1 Rh1 122.94(13) . . ? C2 N2 P3 124.60(19) . . ? C2 N2 Rh1 111.93(16) . . ? P3 N2 Rh1 123.27(13) . . ? N1 C1 C2 107.7(2) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C1 107.1(2) . . ? N2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C4 C3 C8 118.8(3) . . ? C4 C3 P1 117.3(2) . . ? C8 C3 P1 123.7(2) . . ? C5 C4 C3 121.0(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 121.3(3) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C3 119.7(3) . . ? C7 C8 H8 120.2 . . ? C3 C8 H8 120.2 . . ? C10 C9 C14 120.3(3) . . ? C10 C9 P1 118.9(2) . . ? C14 C9 P1 120.7(2) . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.7(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C9 118.9(3) . . ? C13 C14 H14 120.5 . . ? C9 C14 H14 120.5 . . ? P1 C15 P2 109.21(14) . . ? P1 C15 H15A 109.8 . . ? P2 C15 H15A 109.8 . . ? P1 C15 H15B 109.8 . . ? P2 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? C17 C16 C21 119.3(3) . . ? C17 C16 P2 121.5(2) . . ? C21 C16 P2 119.1(2) . . ? C16 C17 C18 119.1(3) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 120.9(3) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C16 120.2(3) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? C23 C22 C27 118.6(3) . . ? C23 C22 P2 122.6(2) . . ? C27 C22 P2 118.7(2) . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.9(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.6(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 120.4(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 120.4(3) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C29 C28 C33 119.0(3) . . ? C29 C28 P3 117.4(2) . . ? C33 C28 P3 122.8(2) . . ? C30 C29 C28 120.4(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.0(3) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 119.9(3) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C28 C33 C32 120.4(3) . . ? C28 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C39 C34 C35 120.1(3) . . ? C39 C34 P3 118.3(2) . . ? C35 C34 P3 121.4(2) . . ? C36 C35 C34 120.2(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 119.2(3) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C38 C37 C36 120.9(3) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 120.3(3) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C34 C39 C38 119.3(3) . . ? C34 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? P3 C40 P4 109.32(14) . . ? P3 C40 H40A 109.8 . . ? P4 C40 H40A 109.8 . . ? P3 C40 H40B 109.8 . . ? P4 C40 H40B 109.8 . . ? H40A C40 H40B 108.3 . . ? C46 C41 C42 118.9(3) . . ? C46 C41 P4 120.5(2) . . ? C42 C41 P4 120.5(2) . . ? C43 C42 C41 120.4(3) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 120.6(3) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 119.7(3) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C41 C46 C45 120.1(3) . . ? C41 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C52 C47 C48 119.2(3) . . ? C52 C47 P4 122.4(2) . . ? C48 C47 P4 118.3(2) . . ? C49 C48 C47 119.8(3) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C50 C49 C48 120.6(3) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 119.6(3) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C52 120.7(3) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C51 C52 C47 120.2(3) . . ? C51 C52 H52 119.9 . . ? C47 C52 H52 119.9 . . ? F3 B1 F2 110.1(3) . . ? F3 B1 F4 111.3(3) . . ? F2 B1 F4 108.5(3) . . ? F3 B1 F1 110.0(3) . . ? F2 B1 F1 108.0(3) . . ? F4 B1 F1 108.7(3) . . ? Cl4 C53 Cl3 111.1(2) . . ? Cl4 C53 Cl5 109.0(2) . . ? Cl3 C53 Cl5 111.14(19) . . ? Cl4 C53 H53 108.5 . . ? Cl3 C53 H53 108.5 . . ? Cl5 C53 H53 108.5 . . ? Cl7 C54 Cl8 109.1(2) . . ? Cl7 C54 Cl6 112.7(3) . . ? Cl8 C54 Cl6 109.9(3) . . ? Cl7 C54 H54 108.4 . . ? Cl8 C54 H54 108.4 . . ? Cl6 C54 H54 108.4 . . ? Cl10 C55 Cl11 110.2(2) . . ? Cl10 C55 Cl9 111.9(3) . . ? Cl11 C55 Cl9 109.5(2) . . ? Cl10 C55 H55 108.4 . . ? Cl11 C55 H55 108.4 . . ? Cl9 C55 H55 108.4 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.922 _refine_diff_density_min -1.417 _refine_diff_density_rms 0.101 #===END #compound 3_Cl data_ab1009 _database_code_depnum_ccdc_archive 'CCDC 772854' #TrackingRef '- 2010_buchard_njc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Cl2 N2 P4 Rh, Cl, 3(C2 H3 N)' _chemical_formula_sum 'C58 H57 Cl6 N2 P4 Rh' _chemical_formula_weight 1221.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorombic _symmetry_space_group_name_H-M 'P21212 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 19.416(1) _cell_length_b 24.922(1) _cell_length_c 10.803(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5227.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 7935 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7841 _exptl_absorpt_correction_T_max 0.9687 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 8882 _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_sigmaI/netI 0.1842 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8882 _reflns_number_gt 5203 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.147 0.000 0.500 191 92 ' ' 2 -0.147 0.500 0.000 191 92 ' ' 3 0.417 0.000 0.000 162 85 ' ' 4 0.583 0.500 0.500 162 85 ' ' _platon_squeeze_details ; Three highly disordered CH3CN molecule were accounted by using Squeeze Platon's function. ; _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^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.10(5) _refine_ls_number_reflns 8882 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1201 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh -0.06512(3) -0.25077(3) 0.31091(5) 0.02396(17) Uani 1 1 d . . . Cl1 Cl -0.10273(10) -0.29510(9) 0.49074(18) 0.0265(5) Uani 1 1 d . . . Cl2 Cl -0.04020(10) -0.20705(9) 0.12211(18) 0.0268(5) Uani 1 1 d . . . P1 P -0.13647(11) -0.35088(10) 0.1690(2) 0.0265(6) Uani 1 1 d . . . P2 P 0.00159(12) -0.32493(9) 0.2741(2) 0.0262(6) Uani 1 1 d . . . P3 P -0.13278(11) -0.14013(10) 0.4068(2) 0.0275(6) Uani 1 1 d . . . P4 P 0.00596(11) -0.19018(10) 0.4098(2) 0.0268(6) Uani 1 1 d . . . N1 N -0.1440(3) -0.2908(3) 0.2175(6) 0.0296(19) Uani 1 1 d . . . N2 N -0.1454(3) -0.1956(3) 0.3399(6) 0.0238(18) Uani 1 1 d . . . C1 C -0.2026(4) -0.2531(4) 0.1956(7) 0.033(2) Uani 1 1 d . . . H1A H -0.1926 -0.2301 0.1231 0.040 Uiso 1 1 calc R . . H1B H -0.2451 -0.2737 0.1780 0.040 Uiso 1 1 calc R . . C2 C -0.2130(4) -0.2191(3) 0.3075(8) 0.029(2) Uani 1 1 d . . . H2A H -0.2468 -0.1903 0.2899 0.035 Uiso 1 1 calc R . . H2B H -0.2306 -0.2411 0.3769 0.035 Uiso 1 1 calc R . . C3 C -0.2111(4) -0.3908(4) 0.2074(9) 0.031(2) Uani 1 1 d . . . C4 C -0.2327(4) -0.3893(4) 0.3302(8) 0.031(2) Uani 1 1 d . . . H4 H -0.2063 -0.3703 0.3898 0.038 Uiso 1 1 calc R . . C5 C -0.2931(5) -0.4156(4) 0.3666(9) 0.048(3) Uani 1 1 d . . . H5 H -0.3078 -0.4152 0.4505 0.057 Uiso 1 1 calc R . . C6 C -0.3327(5) -0.4433(4) 0.2725(12) 0.054(3) Uani 1 1 d . . . H6 H -0.3741 -0.4611 0.2957 0.064 Uiso 1 1 calc R . . C7 C -0.3126(5) -0.4446(4) 0.1531(9) 0.040(3) Uani 1 1 d . . . H7 H -0.3388 -0.4639 0.0935 0.048 Uiso 1 1 calc R . . C8 C -0.2522(5) -0.4171(4) 0.1175(9) 0.038(2) Uani 1 1 d . . . H8 H -0.2390 -0.4162 0.0329 0.046 Uiso 1 1 calc R . . C9 C -0.1197(4) -0.3581(4) 0.0070(7) 0.024(2) Uani 1 1 d . . . C10 C -0.1078(4) -0.4107(4) -0.0424(8) 0.034(2) Uani 1 1 d . . . H10 H -0.1106 -0.4416 0.0089 0.041 Uiso 1 1 calc R . . C11 C -0.0919(4) -0.4153(4) -0.1703(8) 0.039(3) Uani 1 1 d . . . H11 H -0.0825 -0.4497 -0.2042 0.047 Uiso 1 1 calc R . . C12 C -0.0898(4) -0.3716(4) -0.2447(8) 0.037(3) Uani 1 1 d . . . H12 H -0.0820 -0.3757 -0.3310 0.044 Uiso 1 1 calc R . . C13 C -0.0992(4) -0.3210(4) -0.1946(8) 0.037(2) Uani 1 1 d . . . H13 H -0.0965 -0.2903 -0.2466 0.044 Uiso 1 1 calc R . . C14 C -0.1125(4) -0.3144(4) -0.0677(8) 0.031(2) Uani 1 1 d . . . H14 H -0.1165 -0.2794 -0.0338 0.037 Uiso 1 1 calc R . . C15 C -0.0651(4) -0.3785(4) 0.2520(7) 0.032(2) Uani 1 1 d . . . H15A H -0.0452 -0.4089 0.2050 0.038 Uiso 1 1 calc R . . H15B H -0.0807 -0.3920 0.3334 0.038 Uiso 1 1 calc R . . C16 C 0.0609(4) -0.3261(3) 0.1419(7) 0.027(2) Uani 1 1 d . . . C17 C 0.0685(5) -0.3727(4) 0.0735(7) 0.037(2) Uani 1 1 d . . . H17 H 0.0389 -0.4025 0.0870 0.045 Uiso 1 1 calc R . . C18 C 0.1205(5) -0.3753(5) -0.0158(9) 0.051(3) Uani 1 1 d . . . H18 H 0.1271 -0.4069 -0.0635 0.061 Uiso 1 1 calc R . . C19 C 0.1627(5) -0.3307(5) -0.0338(9) 0.043(3) Uani 1 1 d . . . H19 H 0.1987 -0.3319 -0.0932 0.051 Uiso 1 1 calc R . . C20 C 0.1521(5) -0.2864(4) 0.0326(8) 0.036(2) Uani 1 1 d . . . H20 H 0.1807 -0.2562 0.0176 0.043 Uiso 1 1 calc R . . C21 C 0.1014(4) -0.2823(4) 0.1224(8) 0.027(2) Uani 1 1 d . . . H21 H 0.0952 -0.2503 0.1686 0.033 Uiso 1 1 calc R . . C22 C 0.0544(4) -0.3510(4) 0.3983(8) 0.030(2) Uani 1 1 d . . . C23 C 0.1220(5) -0.3318(4) 0.4120(8) 0.035(2) Uani 1 1 d . . . H23 H 0.1403 -0.3078 0.3520 0.042 Uiso 1 1 calc R . . C24 C 0.1622(5) -0.3470(4) 0.5110(9) 0.048(3) Uani 1 1 d . . . H24 H 0.2083 -0.3348 0.5191 0.058 Uiso 1 1 calc R . . C25 C 0.1322(5) -0.3818(4) 0.6009(8) 0.040(3) Uani 1 1 d . . . H25 H 0.1586 -0.3908 0.6719 0.049 Uiso 1 1 calc R . . C26 C 0.0685(4) -0.4027(4) 0.5905(8) 0.032(2) Uani 1 1 d . . . H26 H 0.0514 -0.4277 0.6494 0.038 Uiso 1 1 calc R . . C27 C 0.0285(4) -0.3864(4) 0.4910(8) 0.032(2) Uani 1 1 d . . . H27 H -0.0175 -0.3992 0.4843 0.039 Uiso 1 1 calc R . . C28 C -0.1787(4) -0.0882(4) 0.3280(9) 0.031(2) Uani 1 1 d . . . C29 C -0.1800(5) -0.0912(4) 0.1988(9) 0.042(3) Uani 1 1 d . . . H29 H -0.1578 -0.1199 0.1570 0.050 Uiso 1 1 calc R . . C30 C -0.2148(5) -0.0508(4) 0.1311(9) 0.045(3) Uani 1 1 d . . . H30 H -0.2162 -0.0534 0.0435 0.053 Uiso 1 1 calc R . . C31 C -0.2457(5) -0.0090(4) 0.1856(10) 0.045(3) Uani 1 1 d . . . H31 H -0.2680 0.0176 0.1369 0.054 Uiso 1 1 calc R . . C32 C -0.2451(4) -0.0049(4) 0.3096(12) 0.058(3) Uani 1 1 d . . . H32 H -0.2675 0.0245 0.3486 0.070 Uiso 1 1 calc R . . C33 C -0.2095(5) -0.0460(4) 0.3863(9) 0.044(3) Uani 1 1 d . . . H33 H -0.2082 -0.0429 0.4739 0.052 Uiso 1 1 calc R . . C34 C -0.1515(4) -0.1378(4) 0.5698(7) 0.024(2) Uani 1 1 d . . . C35 C -0.1804(4) -0.1832(4) 0.6248(8) 0.030(2) Uani 1 1 d . . . H35 H -0.1924 -0.2133 0.5755 0.036 Uiso 1 1 calc R . . C36 C -0.1912(5) -0.1841(5) 0.7478(9) 0.049(3) Uani 1 1 d . . . H36 H -0.2102 -0.2152 0.7855 0.059 Uiso 1 1 calc R . . C37 C -0.1746(5) -0.1393(5) 0.8205(10) 0.056(3) Uani 1 1 d . . . H37 H -0.1835 -0.1404 0.9069 0.067 Uiso 1 1 calc R . . C38 C -0.1460(5) -0.0937(4) 0.7705(9) 0.044(3) Uani 1 1 d . . . H38 H -0.1351 -0.0635 0.8205 0.053 Uiso 1 1 calc R . . C39 C -0.1335(5) -0.0936(4) 0.6431(8) 0.041(3) Uani 1 1 d . . . H39 H -0.1125 -0.0632 0.6058 0.049 Uiso 1 1 calc R . . C40 C -0.0426(4) -0.1276(3) 0.3859(7) 0.027(2) Uani 1 1 d . . . H40A H -0.0269 -0.1001 0.4458 0.032 Uiso 1 1 calc R . . H40B H -0.0341 -0.1139 0.3013 0.032 Uiso 1 1 calc R . . C41 C 0.0223(4) -0.1955(4) 0.5754(7) 0.024(2) Uani 1 1 d . . . C42 C 0.0263(4) -0.1494(4) 0.6488(8) 0.039(3) Uani 1 1 d . . . H42 H 0.0191 -0.1151 0.6127 0.046 Uiso 1 1 calc R . . C43 C 0.0412(5) -0.1538(4) 0.7765(9) 0.043(3) Uani 1 1 d . . . H43 H 0.0429 -0.1227 0.8276 0.051 Uiso 1 1 calc R . . C44 C 0.0532(4) -0.2040(5) 0.8253(8) 0.045(3) Uani 1 1 d . . . H44 H 0.0633 -0.2073 0.9110 0.054 Uiso 1 1 calc R . . C45 C 0.0510(4) -0.2489(5) 0.7545(7) 0.035(2) Uani 1 1 d . . . H45 H 0.0607 -0.2829 0.7899 0.042 Uiso 1 1 calc R . . C46 C 0.0346(4) -0.2446(4) 0.6299(7) 0.028(2) Uani 1 1 d . . . H46 H 0.0318 -0.2763 0.5810 0.034 Uiso 1 1 calc R . . C47 C 0.0912(4) -0.1725(4) 0.3487(8) 0.032(2) Uani 1 1 d . . . C48 C 0.0959(5) -0.1438(4) 0.2369(9) 0.037(2) Uani 1 1 d . . . H48 H 0.0566 -0.1318 0.1925 0.045 Uiso 1 1 calc R . . C49 C 0.1629(5) -0.1343(4) 0.1966(10) 0.052(3) Uani 1 1 d . . . H49 H 0.1673 -0.1149 0.1213 0.062 Uiso 1 1 calc R . . C50 C 0.2201(5) -0.1487(4) 0.2491(10) 0.047(3) Uani 1 1 d . . . H50 H 0.2635 -0.1395 0.2145 0.057 Uiso 1 1 calc R . . C51 C 0.2153(5) -0.1777(4) 0.3569(9) 0.047(3) Uani 1 1 d . . . H51 H 0.2562 -0.1890 0.3974 0.056 Uiso 1 1 calc R . . C52 C 0.1515(4) -0.1908(4) 0.4081(9) 0.031(2) Uani 1 1 d . . . H52 H 0.1488 -0.2117 0.4815 0.037 Uiso 1 1 calc R . . Cl3 Cl 0.0000 -0.5000 0.1394(3) 0.0378(8) Uani 1 2 d S . . Cl4 Cl -0.5000 -0.5000 0.4561(2) 0.0183(6) Uani 1 2 d S . . 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) 0.0278(4) 0.0200(3) 0.0004(4) 0.0002(3) -0.0003(4) Cl1 0.0294(12) 0.0308(14) 0.0193(11) 0.0004(10) 0.0034(10) 0.0010(10) Cl2 0.0290(12) 0.0308(14) 0.0207(11) 0.0048(10) 0.0013(10) 0.0007(10) P1 0.0265(12) 0.0301(15) 0.0229(13) -0.0027(12) -0.0039(11) -0.0024(11) P2 0.0254(12) 0.0288(14) 0.0242(13) 0.0017(10) 0.0027(11) 0.0026(11) P3 0.0255(13) 0.0306(16) 0.0263(13) -0.0017(12) 0.0020(11) 0.0010(11) P4 0.0246(12) 0.0301(15) 0.0257(13) 0.0016(11) -0.0011(11) 0.0006(11) N1 0.028(4) 0.029(5) 0.032(5) 0.005(4) 0.003(3) 0.005(4) N2 0.024(4) 0.021(4) 0.026(4) -0.004(3) -0.006(3) 0.000(3) C1 0.031(4) 0.036(5) 0.033(5) 0.014(6) -0.010(4) 0.007(5) C2 0.030(5) 0.033(6) 0.024(5) -0.006(5) 0.004(5) 0.001(4) C3 0.019(5) 0.038(6) 0.036(6) 0.012(5) -0.002(5) -0.007(4) C4 0.020(5) 0.046(7) 0.028(6) -0.012(5) 0.007(4) -0.003(4) C5 0.060(7) 0.039(7) 0.045(6) 0.015(6) 0.029(6) -0.004(6) C6 0.038(6) 0.014(6) 0.108(11) 0.001(6) 0.001(7) -0.006(5) C7 0.035(6) 0.053(8) 0.032(6) -0.004(5) 0.006(5) -0.008(5) C8 0.035(6) 0.053(7) 0.026(5) -0.012(5) 0.002(5) -0.005(5) C9 0.026(5) 0.023(6) 0.024(5) -0.006(5) 0.008(4) 0.011(4) C10 0.029(5) 0.046(7) 0.029(5) 0.005(5) -0.001(4) 0.015(5) C11 0.042(6) 0.050(7) 0.026(6) -0.016(5) 0.002(5) 0.007(5) C12 0.030(6) 0.060(8) 0.020(5) 0.016(6) 0.000(4) 0.008(5) C13 0.047(6) 0.036(6) 0.027(5) 0.009(5) 0.007(5) 0.004(5) C14 0.044(6) 0.022(6) 0.027(5) 0.003(4) -0.005(4) 0.004(4) C15 0.028(5) 0.046(6) 0.021(4) -0.003(4) 0.005(4) 0.002(5) C16 0.027(5) 0.028(6) 0.027(5) 0.008(4) 0.009(4) 0.003(5) C17 0.038(5) 0.048(7) 0.026(5) -0.009(5) 0.010(5) -0.016(5) C18 0.068(8) 0.056(8) 0.029(6) -0.019(6) 0.010(6) -0.005(6) C19 0.039(6) 0.061(9) 0.028(6) 0.009(6) 0.009(5) -0.019(6) C20 0.040(6) 0.034(7) 0.034(6) 0.002(5) 0.005(5) -0.012(5) C21 0.024(5) 0.027(6) 0.031(5) 0.009(4) 0.011(5) -0.004(4) C22 0.020(5) 0.034(6) 0.035(5) -0.001(5) -0.003(5) 0.005(4) C23 0.037(6) 0.044(7) 0.023(5) -0.003(5) -0.002(5) 0.006(5) C24 0.043(6) 0.070(9) 0.032(6) -0.023(6) -0.005(5) 0.009(6) C25 0.056(7) 0.047(7) 0.018(5) 0.005(5) -0.025(5) -0.001(5) C26 0.019(5) 0.048(6) 0.027(5) 0.007(5) -0.010(5) -0.005(5) C27 0.036(5) 0.035(6) 0.025(5) -0.006(5) -0.012(4) 0.002(4) C28 0.030(5) 0.028(6) 0.035(6) -0.004(5) 0.003(5) 0.003(4) C29 0.064(7) 0.037(7) 0.024(6) 0.002(5) 0.009(5) 0.009(5) C30 0.053(7) 0.043(7) 0.037(6) 0.011(6) -0.007(5) 0.004(6) C31 0.047(6) 0.053(8) 0.034(6) 0.023(6) 0.003(6) 0.016(5) C32 0.034(6) 0.037(7) 0.102(10) -0.015(8) 0.033(7) 0.016(5) C33 0.046(6) 0.044(7) 0.041(6) 0.012(6) 0.007(5) -0.002(5) C34 0.020(5) 0.027(6) 0.023(5) -0.003(5) -0.004(4) 0.006(4) C35 0.025(5) 0.034(7) 0.031(6) -0.013(5) -0.004(4) 0.011(4) C36 0.066(8) 0.052(8) 0.028(6) -0.003(6) 0.010(5) -0.004(6) C37 0.080(8) 0.055(8) 0.034(6) -0.004(7) 0.014(6) -0.005(6) C38 0.056(7) 0.036(7) 0.042(7) 0.003(5) 0.012(5) -0.016(5) C39 0.041(6) 0.047(7) 0.034(6) 0.000(5) 0.022(5) 0.008(5) C40 0.034(5) 0.026(6) 0.020(5) 0.006(4) 0.000(4) 0.012(4) C41 0.009(4) 0.046(7) 0.017(5) -0.007(5) -0.004(4) 0.004(4) C42 0.043(6) 0.040(7) 0.032(6) -0.001(5) -0.016(4) -0.008(5) C43 0.044(6) 0.040(7) 0.044(7) -0.002(5) 0.003(5) 0.007(5) C44 0.038(6) 0.075(8) 0.023(5) -0.001(6) 0.007(5) 0.014(6) C45 0.042(6) 0.037(6) 0.025(4) 0.003(6) -0.004(4) 0.006(6) C46 0.032(4) 0.026(6) 0.028(5) -0.004(5) -0.007(4) -0.002(5) C47 0.028(5) 0.030(6) 0.038(6) -0.003(5) 0.010(5) 0.001(4) C48 0.033(5) 0.035(6) 0.044(6) 0.003(5) 0.008(5) -0.002(5) C49 0.057(7) 0.053(8) 0.046(7) 0.012(6) 0.014(6) -0.005(6) C50 0.023(6) 0.054(8) 0.064(8) 0.006(7) 0.008(5) 0.000(5) C51 0.046(7) 0.043(7) 0.051(7) -0.003(6) 0.001(5) 0.003(5) C52 0.033(6) 0.025(6) 0.036(6) -0.009(5) 0.011(5) 0.001(4) Cl3 0.0421(19) 0.0194(19) 0.052(2) 0.000 0.000 0.0084(16) Cl4 0.0271(15) 0.0025(15) 0.0251(16) 0.000 0.000 0.0066(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.087(7) . ? Rh1 N2 2.102(6) . ? Rh1 P2 2.291(2) . ? Rh1 P4 2.308(2) . ? Rh1 Cl1 2.351(2) . ? Rh1 Cl2 2.362(2) . ? P1 N1 1.593(8) . ? P1 C15 1.787(8) . ? P1 C9 1.790(8) . ? P1 C3 1.807(8) . ? P2 C22 1.809(8) . ? P2 C16 1.835(8) . ? P2 C15 1.875(9) . ? P3 N2 1.578(7) . ? P3 C28 1.787(9) . ? P3 C40 1.794(8) . ? P3 C34 1.799(8) . ? P4 C41 1.822(8) . ? P4 C47 1.836(8) . ? P4 C40 1.840(8) . ? N1 C1 1.496(10) . ? N2 C2 1.479(9) . ? C1 C2 1.489(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.392(12) . ? C3 C8 1.417(12) . ? C4 C5 1.400(12) . ? C4 H4 0.9500 . ? C5 C6 1.450(14) . ? C5 H5 0.9500 . ? C6 C7 1.349(14) . ? C6 H6 0.9500 . ? C7 C8 1.412(12) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.361(11) . ? C9 C10 1.435(12) . ? C10 C11 1.420(11) . ? C10 H10 0.9500 . ? C11 C12 1.354(12) . ? C11 H11 0.9500 . ? C12 C13 1.385(12) . ? C12 H12 0.9500 . ? C13 C14 1.405(12) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.362(11) . ? C16 C17 1.385(12) . ? C17 C18 1.398(12) . ? C17 H17 0.9500 . ? C18 C19 1.393(13) . ? C18 H18 0.9500 . ? C19 C20 1.332(13) . ? C19 H19 0.9500 . ? C20 C21 1.386(11) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.406(12) . ? C22 C27 1.426(12) . ? C23 C24 1.377(12) . ? C23 H23 0.9500 . ? C24 C25 1.426(13) . ? C24 H24 0.9500 . ? C25 C26 1.347(11) . ? C25 H25 0.9500 . ? C26 C27 1.387(11) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.365(12) . ? C28 C29 1.397(13) . ? C29 C30 1.416(13) . ? C29 H29 0.9500 . ? C30 C31 1.339(13) . ? C30 H30 0.9500 . ? C31 C32 1.344(14) . ? C31 H31 0.9500 . ? C32 C33 1.488(14) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.395(12) . ? C34 C39 1.402(12) . ? C35 C36 1.346(11) . ? C35 H35 0.9500 . ? C36 C37 1.403(14) . ? C36 H36 0.9500 . ? C37 C38 1.376(13) . ? C37 H37 0.9500 . ? C38 C39 1.397(12) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.379(13) . ? C41 C42 1.398(12) . ? C42 C43 1.414(12) . ? C42 H42 0.9500 . ? C43 C44 1.379(13) . ? C43 H43 0.9500 . ? C44 C45 1.355(13) . ? C44 H44 0.9500 . ? C45 C46 1.387(10) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.408(12) . ? C47 C52 1.410(11) . ? C48 C49 1.392(12) . ? C48 H48 0.9500 . ? C49 C50 1.297(13) . ? C49 H49 0.9500 . ? C50 C51 1.373(13) . ? C50 H50 0.9500 . ? C51 C52 1.396(12) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2 80.9(3) . . ? N1 Rh1 P2 86.9(2) . . ? N2 Rh1 P2 166.57(19) . . ? N1 Rh1 P4 167.2(2) . . ? N2 Rh1 P4 86.90(18) . . ? P2 Rh1 P4 105.66(8) . . ? N1 Rh1 Cl1 86.97(19) . . ? N2 Rh1 Cl1 87.37(19) . . ? P2 Rh1 Cl1 86.55(8) . . ? P4 Rh1 Cl1 96.34(8) . . ? N1 Rh1 Cl2 87.32(19) . . ? N2 Rh1 Cl2 88.78(18) . . ? P2 Rh1 Cl2 96.12(8) . . ? P4 Rh1 Cl2 88.60(8) . . ? Cl1 Rh1 Cl2 173.56(8) . . ? N1 P1 C15 105.5(4) . . ? N1 P1 C9 115.6(4) . . ? C15 P1 C9 108.1(4) . . ? N1 P1 C3 111.7(4) . . ? C15 P1 C3 107.1(4) . . ? C9 P1 C3 108.4(4) . . ? C22 P2 C16 102.5(4) . . ? C22 P2 C15 103.3(4) . . ? C16 P2 C15 108.8(4) . . ? C22 P2 Rh1 118.7(3) . . ? C16 P2 Rh1 120.2(3) . . ? C15 P2 Rh1 101.9(3) . . ? N2 P3 C28 109.7(4) . . ? N2 P3 C40 104.2(4) . . ? C28 P3 C40 107.6(4) . . ? N2 P3 C34 116.4(4) . . ? C28 P3 C34 110.0(4) . . ? C40 P3 C34 108.4(4) . . ? C41 P4 C47 102.3(4) . . ? C41 P4 C40 106.8(4) . . ? C47 P4 C40 102.0(4) . . ? C41 P4 Rh1 120.7(3) . . ? C47 P4 Rh1 122.0(3) . . ? C40 P4 Rh1 100.6(3) . . ? C1 N1 P1 127.5(6) . . ? C1 N1 Rh1 109.6(5) . . ? P1 N1 Rh1 122.8(4) . . ? C2 N2 P3 126.4(5) . . ? C2 N2 Rh1 111.3(5) . . ? P3 N2 Rh1 121.8(3) . . ? C2 C1 N1 109.4(6) . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? N1 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 107.3(6) . . ? N2 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? N2 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C4 C3 C8 119.8(8) . . ? C4 C3 P1 116.4(7) . . ? C8 C3 P1 123.3(7) . . ? C3 C4 C5 120.4(8) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 118.1(9) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C7 C6 C5 121.9(9) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C8 119.3(9) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C7 C8 C3 120.3(8) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? C14 C9 C10 119.6(8) . . ? C14 C9 P1 121.2(7) . . ? C10 C9 P1 119.0(7) . . ? C11 C10 C9 118.0(9) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? C12 C11 C10 121.3(9) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.7(9) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 120.8(9) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 120.3(9) . . ? C9 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? P1 C15 P2 109.0(5) . . ? P1 C15 H15A 109.9 . . ? P2 C15 H15A 109.9 . . ? P1 C15 H15B 109.9 . . ? P2 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C21 C16 C17 121.9(8) . . ? C21 C16 P2 118.0(7) . . ? C17 C16 P2 119.7(7) . . ? C16 C17 C18 118.9(9) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 119.0(10) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C18 119.7(9) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 123.1(9) . . ? C19 C20 H20 118.4 . . ? C21 C20 H20 118.4 . . ? C16 C21 C20 117.4(9) . . ? C16 C21 H21 121.3 . . ? C20 C21 H21 121.3 . . ? C23 C22 C27 117.8(8) . . ? C23 C22 P2 119.0(7) . . ? C27 C22 P2 122.9(6) . . ? C24 C23 C22 121.1(9) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 117.8(9) . . ? C23 C24 H24 121.1 . . ? C25 C24 H24 121.1 . . ? C26 C25 C24 123.6(8) . . ? C26 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? C25 C26 C27 117.8(9) . . ? C25 C26 H26 121.1 . . ? C27 C26 H26 121.1 . . ? C26 C27 C22 121.8(8) . . ? C26 C27 H27 119.1 . . ? C22 C27 H27 119.1 . . ? C33 C28 C29 119.6(9) . . ? C33 C28 P3 123.8(7) . . ? C29 C28 P3 116.6(7) . . ? C28 C29 C30 119.2(9) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 122.7(10) . . ? C31 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? C30 C31 C32 119.5(10) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 120.5(9) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C28 C33 C32 118.5(9) . . ? C28 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C35 C34 C39 119.8(8) . . ? C35 C34 P3 118.2(7) . . ? C39 C34 P3 121.8(7) . . ? C36 C35 C34 119.8(10) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.2(11) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 122.0(10) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C38 C39 117.3(10) . . ? C37 C38 H38 121.3 . . ? C39 C38 H38 121.3 . . ? C38 C39 C34 120.7(10) . . ? C38 C39 H39 119.6 . . ? C34 C39 H39 119.6 . . ? P3 C40 P4 109.6(4) . . ? P3 C40 H40A 109.8 . . ? P4 C40 H40A 109.8 . . ? P3 C40 H40B 109.8 . . ? P4 C40 H40B 109.8 . . ? H40A C40 H40B 108.2 . . ? C46 C41 C42 118.5(8) . . ? C46 C41 P4 120.9(7) . . ? C42 C41 P4 120.4(7) . . ? C41 C42 C43 120.1(10) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 118.5(10) . . ? C44 C43 H43 120.8 . . ? C42 C43 H43 120.8 . . ? C45 C44 C43 121.9(9) . . ? C45 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? C44 C45 C46 119.5(10) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 121.4(10) . . ? C41 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C48 C47 C52 120.1(8) . . ? C48 C47 P4 119.3(7) . . ? C52 C47 P4 120.5(7) . . ? C49 C48 C47 114.5(9) . . ? C49 C48 H48 122.7 . . ? C47 C48 H48 122.7 . . ? C50 C49 C48 128.0(11) . . ? C50 C49 H49 116.0 . . ? C48 C49 H49 116.0 . . ? C49 C50 C51 117.3(10) . . ? C49 C50 H50 121.4 . . ? C51 C50 H50 121.4 . . ? C50 C51 C52 121.3(10) . . ? C50 C51 H51 119.3 . . ? C52 C51 H51 119.3 . . ? C51 C52 C47 118.7(9) . . ? C51 C52 H52 120.7 . . ? C47 C52 H52 120.7 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.842 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.106 #===END