Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Andrew Burrows' 'Ross Harrington' 'M. Mahon' 'M. T. Palmer' 'Francesco Senia' 'Maurizio Varrone' _publ_contact_author_name 'Dr Andrew Burrows' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email A.D.BURROWS@BATH.AC.UK _publ_section_title ; Synthesis and reactivity of rhodium(I) complexes containing keto-functionalised N-pyrrolyl phosphine ligands ; data_2 _database_code_CSD 184445 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.50 H21 Cl2 O P2 Rh' _chemical_formula_weight 579.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.394(2) _cell_length_b 9.683(2) _cell_length_c 17.287(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.93(2) _cell_angle_gamma 90.00 _cell_volume 2406.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4536 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4227 _reflns_number_gt 3181 _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^)+(0.0952P)^2^+2.2197P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_number_reflns 4227 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 0.870 _refine_ls_restrained_S_all 0.870 _refine_ls_shift/su_max 2.272 _refine_ls_shift/su_mean 0.007 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.58958(2) 0.00714(4) 0.04012(2) 0.01453(15) Uani 1 1 d . . . P1 P 0.65006(8) 0.12700(12) -0.05995(7) 0.0136(3) Uani 1 1 d . . . P2 P 0.46897(8) 0.10531(13) -0.14413(7) 0.0150(3) Uani 1 1 d . . . Cl1 Cl 0.7349(3) -0.1021(3) 0.06375(17) 0.0206(6) Uani 0.50 1 d P . . Cl2 Cl 0.4902(2) 0.2115(4) 0.05565(18) 0.0246(6) Uani 0.50 1 d P . . Cl3 Cl 1.0205(3) 0.1920(6) 0.0632(3) 0.0729(13) Uani 0.50 1 d P . . Cl4 Cl 0.9761(5) -0.0524(7) -0.0318(4) 0.0912(19) Uani 0.50 1 d P . . O1 O 0.7673(7) -0.1385(11) 0.0705(6) 0.029(3) Uiso 0.50 1 d P . . O2 O 0.4821(7) 0.2609(12) 0.0752(6) 0.035(3) Uiso 0.50 1 d P . . O3 O 0.5708(2) 0.1794(3) -0.12453(18) 0.0173(7) Uani 1 1 d . . . C1 C 0.7051(3) 0.2900(5) -0.0331(3) 0.0153(10) Uani 1 1 d . . . C2 C 0.7879(4) 0.2856(5) 0.0111(3) 0.0212(11) Uani 1 1 d . . . H2 H 0.8142 0.2007 0.0245 0.025 Uiso 1 1 calc R . . C3 C 0.8321(4) 0.4065(6) 0.0357(3) 0.0278(12) Uani 1 1 d . . . H3 H 0.8881 0.4025 0.0649 0.033 Uiso 1 1 calc R . . C4 C 0.7920(4) 0.5342(6) 0.0165(3) 0.0301(13) Uani 1 1 d . . . H4 H 0.8203 0.6156 0.0338 0.036 Uiso 1 1 calc R . . C5 C 0.7096(4) 0.5385(5) -0.0287(3) 0.0269(12) Uani 1 1 d . . . H5 H 0.6837 0.6235 -0.0427 0.032 Uiso 1 1 calc R . . C6 C 0.6648(4) 0.4169(5) -0.0535(3) 0.0225(11) Uani 1 1 d . . . H6 H 0.6091 0.4205 -0.0832 0.027 Uiso 1 1 calc R . . C7 C 0.7324(3) 0.0454(5) -0.1216(3) 0.0177(10) Uani 1 1 d . . . C8 C 0.7914(4) 0.1228(6) -0.1654(3) 0.0245(12) Uani 1 1 d . . . H8 H 0.7933 0.2183 -0.1600 0.029 Uiso 1 1 calc R . . C9 C 0.8472(4) 0.0584(7) -0.2167(3) 0.0359(14) Uani 1 1 d . . . H9 H 0.8862 0.1110 -0.2463 0.043 Uiso 1 1 calc R . . C10 C 0.8460(5) -0.0840(6) -0.2249(4) 0.0405(16) Uani 1 1 d . . . H10 H 0.8838 -0.1271 -0.2596 0.049 Uiso 1 1 calc R . . C11 C 0.7871(4) -0.1616(6) -0.1804(4) 0.0372(15) Uani 1 1 d . . . H11 H 0.7865 -0.2573 -0.1850 0.045 Uiso 1 1 calc R . . C12 C 0.7299(4) -0.0985(5) -0.1296(3) 0.0272(12) Uani 1 1 d . . . H12 H 0.6899 -0.1509 -0.1009 0.033 Uiso 1 1 calc R . . C13 C 0.4110(3) 0.2578(5) -0.1834(3) 0.0185(10) Uani 1 1 d . . . C14 C 0.4060(3) 0.3743(5) -0.1376(3) 0.0220(11) Uani 1 1 d . . . H14 H 0.4313 0.3721 -0.0870 0.026 Uiso 1 1 calc R . . C15 C 0.3637(4) 0.4948(6) -0.1656(3) 0.0292(12) Uani 1 1 d . . . H15 H 0.3628 0.5737 -0.1349 0.035 Uiso 1 1 calc R . . C16 C 0.3230(4) 0.4951(6) -0.2401(3) 0.0315(13) Uani 1 1 d . . . H16 H 0.2936 0.5745 -0.2594 0.038 Uiso 1 1 calc R . . C17 C 0.3257(4) 0.3791(6) -0.2856(3) 0.0311(13) Uani 1 1 d . . . H17 H 0.2983 0.3808 -0.3355 0.037 Uiso 1 1 calc R . . C18 C 0.3684(4) 0.2601(6) -0.2582(3) 0.0250(12) Uani 1 1 d . . . H18 H 0.3690 0.1816 -0.2891 0.030 Uiso 1 1 calc R . . C19 C 0.4893(3) 0.0012(5) -0.2281(3) 0.0184(10) Uani 1 1 d . . . C20 C 0.5586(4) 0.0342(6) -0.2775(3) 0.0280(13) Uani 1 1 d . . . H20 H 0.5980 0.1081 -0.2655 0.034 Uiso 1 1 calc R . . C21 C 0.5703(4) -0.0406(7) -0.3441(3) 0.0329(14) Uani 1 1 d . . . H21 H 0.6180 -0.0181 -0.3762 0.040 Uiso 1 1 calc R . . C22 C 0.5111(4) -0.1490(6) -0.3631(3) 0.0309(13) Uani 1 1 d . . . H22 H 0.5178 -0.1983 -0.4086 0.037 Uiso 1 1 calc R . . C23 C 0.4423(4) -0.1835(6) -0.3144(3) 0.0328(14) Uani 1 1 d . . . H23 H 0.4024 -0.2564 -0.3274 0.039 Uiso 1 1 calc R . . C24 C 0.4314(4) -0.1113(6) -0.2463(3) 0.0273(12) Uani 1 1 d . . . H24 H 0.3860 -0.1375 -0.2128 0.033 Uiso 1 1 calc R . . C25 C 0.9962(16) 0.017(2) 0.0525(13) 0.058(6) Uiso 0.50 1 d P . . C26 C 0.6990(10) -0.0863(16) 0.0571(8) 0.020(4) Uiso 0.50 1 d P . . C27 C 0.5144(10) 0.1571(17) 0.0552(8) 0.028(4) Uiso 0.50 1 d P . . 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 0.0170(2) 0.0106(2) 0.0164(2) 0.00406(15) 0.00387(14) 0.00047(16) P1 0.0189(6) 0.0069(6) 0.0155(6) 0.0012(5) 0.0041(5) -0.0018(5) P2 0.0187(6) 0.0119(6) 0.0145(6) 0.0032(5) 0.0020(5) -0.0009(5) Cl1 0.0183(19) 0.0195(16) 0.0239(15) 0.0066(11) 0.0007(14) 0.0024(16) Cl2 0.0294(17) 0.0200(18) 0.0252(16) 0.0028(14) 0.0103(12) 0.0049(15) Cl3 0.063(3) 0.087(3) 0.067(3) 0.012(2) -0.012(2) 0.022(2) Cl4 0.105(5) 0.084(4) 0.081(4) 0.005(3) -0.035(4) -0.011(4) O3 0.0194(17) 0.0136(17) 0.0190(17) 0.0024(14) 0.0012(14) -0.0026(14) C1 0.024(3) 0.009(2) 0.014(2) -0.0012(18) 0.0056(19) -0.005(2) C2 0.028(3) 0.016(3) 0.020(2) 0.002(2) 0.004(2) -0.002(2) C3 0.031(3) 0.030(3) 0.022(3) -0.005(2) 0.002(2) -0.008(3) C4 0.042(3) 0.020(3) 0.029(3) -0.008(2) 0.012(3) -0.013(3) C5 0.037(3) 0.008(2) 0.037(3) -0.004(2) 0.011(3) 0.000(2) C6 0.024(3) 0.019(3) 0.026(3) 0.001(2) 0.006(2) 0.003(2) C7 0.023(3) 0.011(2) 0.020(2) -0.003(2) 0.008(2) -0.001(2) C8 0.034(3) 0.013(3) 0.027(3) -0.001(2) 0.013(2) -0.002(2) C9 0.043(4) 0.029(3) 0.039(3) -0.003(3) 0.024(3) -0.003(3) C10 0.055(4) 0.030(3) 0.039(3) -0.013(3) 0.029(3) 0.004(3) C11 0.056(4) 0.013(3) 0.044(3) -0.010(3) 0.016(3) 0.002(3) C12 0.037(3) 0.014(3) 0.031(3) -0.006(2) 0.011(2) -0.003(2) C13 0.021(2) 0.016(3) 0.018(2) 0.007(2) 0.006(2) -0.006(2) C14 0.027(3) 0.019(3) 0.020(2) 0.002(2) 0.006(2) 0.001(2) C15 0.031(3) 0.020(3) 0.037(3) -0.001(2) 0.007(2) 0.003(2) C16 0.035(3) 0.021(3) 0.039(3) 0.012(3) 0.009(3) 0.012(3) C17 0.037(3) 0.035(3) 0.022(3) 0.009(3) -0.003(2) 0.009(3) C18 0.031(3) 0.020(3) 0.024(3) 0.006(2) 0.001(2) 0.001(2) C19 0.022(2) 0.013(2) 0.020(2) 0.001(2) 0.0019(19) 0.004(2) C20 0.031(3) 0.025(3) 0.029(3) -0.003(2) 0.008(2) -0.009(2) C21 0.034(3) 0.042(4) 0.023(3) -0.006(3) 0.007(2) -0.004(3) C22 0.041(3) 0.026(3) 0.026(3) -0.008(2) 0.003(2) 0.004(3) C23 0.052(4) 0.017(3) 0.029(3) -0.011(2) -0.002(3) -0.008(3) C24 0.036(3) 0.020(3) 0.025(3) 0.002(2) 0.003(2) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C26 1.828(15) . ? Rh1 C27 1.837(17) . ? Rh1 P1 2.2917(13) . ? Rh1 P2 2.2986(13) 3_655 ? Rh1 Cl1 2.361(5) . ? Rh1 Cl2 2.464(5) . ? Rh1 Rh1 2.8683(9) 3_655 ? P1 O3 1.636(3) . ? P1 C1 1.815(5) . ? P1 C7 1.815(5) . ? P2 O3 1.651(3) . ? P2 C19 1.804(5) . ? P2 C13 1.811(5) . ? P2 Rh1 2.2986(13) 3_655 ? Cl1 C26 0.545(12) . ? Cl1 O1 0.592(8) . ? Cl2 O2 0.601(9) . ? Cl2 C27 0.631(14) . ? Cl3 Cl4 1.459(8) 3_755 ? Cl3 C25 1.74(2) . ? Cl4 C25 0.648(19) 3_755 ? Cl4 Cl3 1.459(8) 3_755 ? Cl4 C25 1.62(2) . ? Cl4 Cl4 1.624(12) 3_755 ? O1 C26 1.118(15) . ? O2 C27 1.167(17) . ? C1 C2 1.383(7) . ? C1 C6 1.396(7) . ? C2 C3 1.388(7) . ? C3 C4 1.398(8) . ? C4 C5 1.388(8) . ? C5 C6 1.399(7) . ? C7 C8 1.386(7) . ? C7 C12 1.400(7) . ? C8 C9 1.377(7) . ? C9 C10 1.386(9) . ? C10 C11 1.393(8) . ? C11 C12 1.377(8) . ? C13 C14 1.382(7) . ? C13 C18 1.402(7) . ? C14 C15 1.392(7) . ? C15 C16 1.388(9) . ? C16 C17 1.373(8) . ? C17 C18 1.379(8) . ? C19 C20 1.382(7) . ? C19 C24 1.397(7) . ? C20 C21 1.379(8) . ? C21 C22 1.380(8) . ? C22 C23 1.374(8) . ? C23 C24 1.385(8) . ? C25 Cl4 0.648(19) 3_755 ? C25 C25 1.85(5) 3_755 ? 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 C26 Rh1 C27 151.3(6) . . ? C26 Rh1 P1 90.8(4) . . ? C27 Rh1 P1 87.5(4) . . ? C26 Rh1 P2 89.3(4) . 3_655 ? C27 Rh1 P2 91.2(4) . 3_655 ? P1 Rh1 P2 177.46(5) . 3_655 ? C26 Rh1 Cl1 3.1(5) . . ? C27 Rh1 Cl1 148.5(4) . . ? P1 Rh1 Cl1 89.43(7) . . ? P2 Rh1 Cl1 90.55(7) 3_655 . ? C26 Rh1 Cl2 151.7(4) . . ? C27 Rh1 Cl2 2.1(4) . . ? P1 Rh1 Cl2 85.45(7) . . ? P2 Rh1 Cl2 93.27(7) 3_655 . ? Cl1 Rh1 Cl2 148.74(11) . . ? C26 Rh1 Rh1 143.2(4) . 3_655 ? C27 Rh1 Rh1 65.5(4) . 3_655 ? P1 Rh1 Rh1 91.50(4) . 3_655 ? P2 Rh1 Rh1 89.94(4) 3_655 3_655 ? Cl1 Rh1 Rh1 145.98(7) . 3_655 ? Cl2 Rh1 Rh1 65.10(8) . 3_655 ? O3 P1 C1 100.6(2) . . ? O3 P1 C7 100.8(2) . . ? C1 P1 C7 103.8(2) . . ? O3 P1 Rh1 113.17(13) . . ? C1 P1 Rh1 115.17(15) . . ? C7 P1 Rh1 120.49(17) . . ? O3 P2 C19 103.3(2) . . ? O3 P2 C13 96.3(2) . . ? C19 P2 C13 104.1(2) . . ? O3 P2 Rh1 113.73(12) . 3_655 ? C19 P2 Rh1 116.49(17) . 3_655 ? C13 P2 Rh1 119.94(16) . 3_655 ? C26 Cl1 O1 160(2) . . ? C26 Cl1 Rh1 10.5(16) . . ? O1 Cl1 Rh1 169.6(11) . . ? O2 Cl2 C27 142.6(18) . . ? O2 Cl2 Rh1 146.2(12) . . ? C27 Cl2 Rh1 6.0(13) . . ? Cl4 Cl3 C25 21.1(8) 3_755 . ? C25 Cl4 Cl3 105(3) 3_755 3_755 ? C25 Cl4 C25 101(2) 3_755 . ? Cl3 Cl4 C25 135.4(9) 3_755 . ? C25 Cl4 Cl4 78(2) 3_755 3_755 ? Cl3 Cl4 Cl4 144.1(7) 3_755 3_755 ? C25 Cl4 Cl4 23.1(7) . 3_755 ? Cl1 O1 C26 9.8(9) . . ? Cl2 O2 C27 19.2(10) . . ? P1 O3 P2 125.9(2) . . ? C2 C1 C6 120.1(4) . . ? C2 C1 P1 117.8(4) . . ? C6 C1 P1 122.1(4) . . ? C1 C2 C3 120.8(5) . . ? C2 C3 C4 119.7(5) . . ? C5 C4 C3 119.4(5) . . ? C4 C5 C6 120.9(5) . . ? C1 C6 C5 119.0(5) . . ? C8 C7 C12 119.9(5) . . ? C8 C7 P1 121.4(4) . . ? C12 C7 P1 118.5(4) . . ? C9 C8 C7 120.0(5) . . ? C8 C9 C10 120.8(6) . . ? C9 C10 C11 119.0(5) . . ? C12 C11 C10 120.9(5) . . ? C11 C12 C7 119.4(5) . . ? C14 C13 C18 118.8(5) . . ? C14 C13 P2 119.2(4) . . ? C18 C13 P2 122.0(4) . . ? C13 C14 C15 121.3(5) . . ? C16 C15 C14 118.7(5) . . ? C17 C16 C15 120.4(5) . . ? C16 C17 C18 120.8(5) . . ? C17 C18 C13 119.8(5) . . ? C20 C19 C24 118.8(5) . . ? C20 C19 P2 121.3(4) . . ? C24 C19 P2 119.8(4) . . ? C21 C20 C19 121.2(5) . . ? C20 C21 C22 119.8(5) . . ? C23 C22 C21 119.7(5) . . ? C22 C23 C24 120.9(5) . . ? C23 C24 C19 119.5(5) . . ? Cl4 C25 Cl4 79(2) 3_755 . ? Cl4 C25 Cl3 54(2) 3_755 . ? Cl4 C25 Cl3 121.8(14) . . ? Cl4 C25 C25 59(2) 3_755 3_755 ? Cl4 C25 C25 20.1(7) . 3_755 ? Cl3 C25 C25 104.8(17) . 3_755 ? Cl1 C26 O1 10.7(11) . . ? Cl1 C26 Rh1 166(2) . . ? O1 C26 Rh1 176.3(14) . . ? Cl2 C27 O2 18.2(9) . . ? Cl2 C27 Rh1 171.9(17) . . ? O2 C27 Rh1 165.7(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.451 _refine_diff_density_min -2.003 _refine_diff_density_rms 0.132 #===END data_compound4 _database_code_CSD 184446 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H40 Cl2 N8 O4 P4 Rh2' _chemical_formula_weight 1109.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.8250(2) _cell_length_b 11.8230(2) _cell_length_c 20.9580(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.9461(7) _cell_angle_gamma 90.00 _cell_volume 4587.74(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26407 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5218 _reflns_number_gt 4606 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+7.8998P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00131(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5218 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.185730(8) 0.194939(13) -0.058394(8) 0.01917(8) Uani 1 1 d . . . Cl1 Cl 0.19946(3) 0.07717(4) 0.03706(3) 0.02544(13) Uani 1 1 d . . . P1 P 0.11259(3) 0.31420(4) -0.02843(3) 0.01993(13) Uani 1 1 d . . . P2 P 0.23466(3) 0.41492(4) 0.08500(3) 0.01994(13) Uani 1 1 d . . . O1 O 0.14805(12) 0.31387(17) -0.19216(10) 0.0469(5) Uani 1 1 d . . . O2 O 0.15143(7) 0.40159(13) 0.03319(7) 0.0227(3) Uani 1 1 d . . . N1 N 0.06312(9) 0.41219(15) -0.08479(10) 0.0239(4) Uani 1 1 d . . . N2 N 0.05036(10) 0.25555(16) -0.00195(10) 0.0268(4) Uani 1 1 d . . . N3 N 0.21990(10) 0.39697(16) 0.15918(9) 0.0260(4) Uani 1 1 d . . . N4 N 0.24481(10) 0.55506(15) 0.08293(10) 0.0245(4) Uani 1 1 d . . . C1 C 0.09199(13) 0.5037(2) -0.10766(13) 0.0307(5) Uani 1 1 d . . . H3 H 0.1397 0.5280 -0.0895 0.037 Uiso 1 1 calc R . . C2 C 0.03864(15) 0.5519(2) -0.16109(13) 0.0367(6) Uani 1 1 d . . . H4 H 0.0432 0.6151 -0.1857 0.044 Uiso 1 1 calc R . . C3 C -0.02523(14) 0.4882(2) -0.17252(14) 0.0403(6) Uani 1 1 d . . . H5 H -0.0700 0.5024 -0.2061 0.048 Uiso 1 1 calc R . . C4 C -0.00976(12) 0.4033(2) -0.12626(12) 0.0311(5) Uani 1 1 d . . . H6 H -0.0419 0.3486 -0.1227 0.037 Uiso 1 1 calc R . . C5 C 0.01291(13) 0.3064(2) 0.03537(14) 0.0310(5) Uani 1 1 d . . . H7 H 0.0234 0.3761 0.0574 0.037 Uiso 1 1 calc R . . C6 C -0.04154(13) 0.2359(2) 0.03378(15) 0.0377(6) Uani 1 1 d . . . H8 H -0.0744 0.2482 0.0555 0.045 Uiso 1 1 calc R . . C7 C -0.04003(13) 0.1402(2) -0.00661(16) 0.0415(6) Uani 1 1 d . . . H9 H -0.0720 0.0796 -0.0167 0.050 Uiso 1 1 calc R . . C8 C 0.01633(13) 0.1532(2) -0.02778(14) 0.0336(5) Uani 1 1 d . . . H10 H 0.0301 0.1028 -0.0549 0.040 Uiso 1 1 calc R . . C9 C 0.19437(16) 0.2970(2) 0.17737(14) 0.0361(6) Uani 1 1 d . . . H11 H 0.1791 0.2335 0.1498 0.043 Uiso 1 1 calc R . . C10 C 0.19561(16) 0.3084(2) 0.24206(14) 0.0390(6) Uani 1 1 d . . . H12 H 0.1814 0.2541 0.2668 0.047 Uiso 1 1 calc R . . C11 C 0.22240(18) 0.4176(3) 0.26511(14) 0.0470(7) Uani 1 1 d . . . H13 H 0.2288 0.4479 0.3078 0.056 Uiso 1 1 calc R . . C12 C 0.23720(15) 0.4703(2) 0.21438(12) 0.0373(6) Uani 1 1 d . . . H14 H 0.2557 0.5430 0.2162 0.045 Uiso 1 1 calc R . . C13 C 0.19238(12) 0.6380(2) 0.07375(12) 0.0294(5) Uani 1 1 d . . . H15 H 0.1434 0.6255 0.0639 0.035 Uiso 1 1 calc R . . C14 C 0.22533(14) 0.7404(2) 0.08177(13) 0.0328(5) Uani 1 1 d . . . H16 H 0.2029 0.8104 0.0778 0.039 Uiso 1 1 calc R . . C15 C 0.29998(15) 0.7215(2) 0.09728(13) 0.0342(5) Uani 1 1 d . . . H15A H 0.3352 0.7772 0.1056 0.041 Uiso 1 1 calc R . . C16 C 0.31153(13) 0.6087(2) 0.09800(13) 0.0310(5) Uani 1 1 d . . . H16' H 0.3558 0.5733 0.1069 0.037 Uiso 1 1 calc R . . C17 C 0.16352(13) 0.2699(2) -0.14025(13) 0.0306(5) Uani 1 1 d . . . C18 C 0.0218(5) -0.0796(5) 0.2289(3) 0.162(5) Uani 1 1 d . . . H18 H 0.0368 -0.1467 0.2151 0.195 Uiso 1 1 calc R . . C19 C 0.0403(4) 0.0240(5) 0.2097(3) 0.115(2) Uani 1 1 d . . . C20 C 0.0197(3) 0.1231(5) 0.2306(4) 0.126(3) Uani 1 1 d . . . H20 H 0.0337 0.1914 0.2173 0.152 Uiso 1 1 calc R . . C21 C 0.0783(5) 0.0294(10) 0.1714(6) 0.092(3) Uani 0.50 1 d P . . H21A H 0.0486 0.0549 0.1267 0.137 Uiso 0.50 1 calc PR . . H21B H 0.0973 -0.0442 0.1681 0.137 Uiso 0.50 1 calc PR . . H21C H 0.1175 0.0815 0.1908 0.137 Uiso 0.50 1 calc PR . . 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 0.01624(11) 0.01831(11) 0.02274(11) -0.00010(6) 0.00668(7) -0.00023(5) Cl1 0.0255(3) 0.0232(3) 0.0285(3) 0.0028(2) 0.0107(2) -0.00129(19) P1 0.0151(3) 0.0183(3) 0.0268(3) 0.0007(2) 0.0079(2) -0.00012(18) P2 0.0189(3) 0.0185(3) 0.0232(3) -0.0008(2) 0.0086(2) -0.00085(19) O1 0.0571(13) 0.0527(13) 0.0326(10) 0.0170(9) 0.0180(9) 0.0176(9) O2 0.0176(7) 0.0241(8) 0.0260(7) -0.0013(6) 0.0072(6) 0.0007(6) N1 0.0182(8) 0.0210(9) 0.0293(9) 0.0021(7) 0.0048(7) 0.0023(7) N2 0.0211(9) 0.0210(9) 0.0415(11) 0.0020(8) 0.0152(8) -0.0011(7) N3 0.0288(10) 0.0268(10) 0.0238(9) -0.0008(7) 0.0110(7) -0.0021(7) N4 0.0237(9) 0.0210(9) 0.0311(10) -0.0030(7) 0.0125(7) -0.0029(7) C1 0.0286(11) 0.0234(11) 0.0356(12) 0.0037(9) 0.0060(9) -0.0029(9) C2 0.0456(15) 0.0261(12) 0.0321(12) 0.0055(10) 0.0061(11) 0.0033(10) C3 0.0311(13) 0.0436(15) 0.0341(13) 0.0025(11) -0.0032(10) 0.0072(11) C4 0.0190(10) 0.0349(13) 0.0341(12) -0.0019(10) 0.0033(9) 0.0008(9) C5 0.0262(12) 0.0298(12) 0.0424(14) 0.0024(10) 0.0187(10) 0.0034(9) C6 0.0276(12) 0.0345(13) 0.0596(17) 0.0095(12) 0.0262(12) 0.0040(10) C7 0.0251(12) 0.0295(13) 0.0728(19) 0.0085(13) 0.0212(12) -0.0029(10) C8 0.0265(12) 0.0200(11) 0.0567(16) -0.0028(10) 0.0179(11) -0.0033(9) C9 0.0477(16) 0.0317(13) 0.0340(13) 0.0010(10) 0.0209(12) -0.0073(11) C10 0.0470(16) 0.0435(16) 0.0330(13) 0.0101(11) 0.0220(12) 0.0066(11) C11 0.0626(18) 0.0529(17) 0.0262(12) -0.0006(12) 0.0167(12) 0.0043(14) C12 0.0468(15) 0.0365(14) 0.0270(12) -0.0062(10) 0.0113(11) -0.0018(11) C13 0.0271(11) 0.0237(11) 0.0352(12) -0.0010(9) 0.0083(9) 0.0026(9) C14 0.0437(14) 0.0204(11) 0.0332(12) -0.0018(9) 0.0124(10) 0.0030(10) C15 0.0424(14) 0.0279(12) 0.0407(14) -0.0090(10) 0.0254(12) -0.0124(10) C16 0.0283(11) 0.0286(12) 0.0431(13) -0.0095(10) 0.0212(10) -0.0075(9) C17 0.0274(12) 0.0290(12) 0.0364(13) 0.0000(10) 0.0126(10) 0.0032(9) C18 0.246(11) 0.083(4) 0.077(5) -0.002(3) -0.041(5) 0.015(5) C19 0.111(5) 0.083(4) 0.090(4) 0.002(3) -0.038(3) 0.004(3) C20 0.071(4) 0.082(3) 0.166(8) -0.016(4) -0.032(4) 0.009(3) C21 0.061(5) 0.101(8) 0.088(7) -0.006(6) -0.005(5) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C17 1.839(3) . ? Rh1 P2 2.2624(5) 7 ? Rh1 P1 2.2664(5) . ? Rh1 Cl1 2.3719(5) . ? Rh1 Rh1 3.1177(3) 7 ? P1 O2 1.6176(15) . ? P1 N2 1.6733(18) . ? P1 N1 1.6945(19) . ? P2 O2 1.6266(15) . ? P2 N4 1.6716(19) . ? P2 N3 1.6948(19) . ? P2 Rh1 2.2624(5) 7 ? O1 C17 1.144(3) . ? N1 C1 1.387(3) . ? N1 C4 1.399(3) . ? N2 C5 1.393(3) . ? N2 C8 1.397(3) . ? N3 C12 1.387(3) . ? N3 C9 1.391(3) . ? N4 C13 1.391(3) . ? N4 C16 1.398(3) . ? C1 C2 1.360(3) . ? C1 H3 0.9300 . ? C2 C3 1.418(4) . ? C2 H4 0.9300 . ? C3 C4 1.352(4) . ? C3 H5 0.9300 . ? C4 H6 0.9300 . ? C5 C6 1.355(3) . ? C5 H7 0.9300 . ? C6 C7 1.420(4) . ? C6 H8 0.9300 . ? C7 C8 1.350(3) . ? C7 H9 0.9300 . ? C8 H10 0.9300 . ? C9 C10 1.354(4) . ? C9 H11 0.9300 . ? C10 C11 1.414(4) . ? C10 H12 0.9300 . ? C11 C12 1.352(4) . ? C11 H13 0.9300 . ? C12 H14 0.9300 . ? C13 C14 1.357(3) . ? C13 H15 0.9300 . ? C14 C15 1.415(4) . ? C14 H16 0.9300 . ? C15 C16 1.352(3) . ? C15 H15A 0.9300 . ? C16 H16 0.9300 . ? C18 C19 1.378(9) . ? C18 C18 1.442(19) 2 ? C18 H18 0.9300 . ? C19 C21 1.285(12) . ? C19 C20 1.364(8) . ? C20 C20 1.313(15) 2 ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 C17 Rh1 P2 90.13(7) . 7 ? C17 Rh1 P1 89.72(7) . . ? P2 Rh1 P1 175.82(2) 7 . ? C17 Rh1 Cl1 170.64(8) . . ? P2 Rh1 Cl1 89.489(19) 7 . ? P1 Rh1 Cl1 91.340(19) . . ? C17 Rh1 Rh1 112.77(8) . 7 ? P2 Rh1 Rh1 89.245(15) 7 7 ? P1 Rh1 Rh1 86.961(15) . 7 ? Cl1 Rh1 Rh1 76.577(14) . 7 ? O2 P1 N2 101.35(9) . . ? O2 P1 N1 96.40(9) . . ? N2 P1 N1 101.71(9) . . ? O2 P1 Rh1 116.71(6) . . ? N2 P1 Rh1 117.04(7) . . ? N1 P1 Rh1 120.03(7) . . ? O2 P2 N4 100.46(9) . . ? O2 P2 N3 97.68(9) . . ? N4 P2 N3 102.11(9) . . ? O2 P2 Rh1 114.23(6) . 7 ? N4 P2 Rh1 117.49(7) . 7 ? N3 P2 Rh1 121.24(7) . 7 ? P1 O2 P2 132.42(10) . . ? C1 N1 C4 107.82(19) . . ? C1 N1 P1 124.52(16) . . ? C4 N1 P1 126.42(16) . . ? C5 N2 C8 108.13(19) . . ? C5 N2 P1 127.69(16) . . ? C8 N2 P1 122.79(17) . . ? C12 N3 C9 107.9(2) . . ? C12 N3 P2 127.92(17) . . ? C9 N3 P2 123.83(17) . . ? C13 N4 C16 108.13(19) . . ? C13 N4 P2 127.68(16) . . ? C16 N4 P2 123.86(16) . . ? C2 C1 N1 108.4(2) . . ? C2 C1 H3 125.8 . . ? N1 C1 H3 125.8 . . ? C1 C2 C3 107.5(2) . . ? C1 C2 H4 126.2 . . ? C3 C2 H4 126.2 . . ? C4 C3 C2 108.2(2) . . ? C4 C3 H5 125.9 . . ? C2 C3 H5 125.9 . . ? C3 C4 N1 108.0(2) . . ? C3 C4 H6 126.0 . . ? N1 C4 H6 126.0 . . ? C6 C5 N2 107.5(2) . . ? C6 C5 H7 126.3 . . ? N2 C5 H7 126.3 . . ? C5 C6 C7 108.6(2) . . ? C5 C6 H8 125.7 . . ? C7 C6 H8 125.7 . . ? C8 C7 C6 107.5(2) . . ? C8 C7 H9 126.2 . . ? C6 C7 H9 126.2 . . ? C7 C8 N2 108.3(2) . . ? C7 C8 H10 125.9 . . ? N2 C8 H10 125.9 . . ? C10 C9 N3 108.2(2) . . ? C10 C9 H11 125.9 . . ? N3 C9 H11 125.9 . . ? C9 C10 C11 107.6(2) . . ? C9 C10 H12 126.2 . . ? C11 C10 H12 126.2 . . ? C12 C11 C10 108.2(2) . . ? C12 C11 H13 125.9 . . ? C10 C11 H13 125.9 . . ? C11 C12 N3 108.0(2) . . ? C11 C12 H14 126.0 . . ? N3 C12 H14 126.0 . . ? C14 C13 N4 108.0(2) . . ? C14 C13 H15 126.0 . . ? N4 C13 H15 126.0 . . ? C13 C14 C15 107.8(2) . . ? C13 C14 H16 126.1 . . ? C15 C14 H16 126.1 . . ? C16 C15 C14 108.5(2) . . ? C16 C15 H15A 125.7 . . ? C14 C15 H15A 125.7 . . ? C15 C16 N4 107.6(2) . . ? C15 C16 H16 126.2 . . ? N4 C16 H16 126.2 . . ? O1 C17 Rh1 177.8(2) . . ? C19 C18 C18 117.3(5) . 2 ? C19 C18 H18 121.3 . . ? C18 C18 H18 121.3 2 . ? C21 C19 C20 117.9(8) . . ? C21 C19 C18 120.2(9) . . ? C20 C19 C18 121.9(9) . . ? C20 C20 C19 120.8(5) 2 . ? C20 C20 H20 119.6 2 . ? C19 C20 H20 119.6 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.626 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.074 #===END data_compound2_h01adb11 _database_code_CSD 211980 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 Cl N3 O2 P Rh' _chemical_formula_weight 437.62 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.2510(3) _cell_length_b 8.54700(10) _cell_length_c 17.3260(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.1430(10) _cell_angle_gamma 90.00 _cell_volume 3323.57(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Parallelepiped _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.03 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35297 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 30.04 _reflns_number_total 4856 _reflns_number_gt 4304 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+3.1808*P+(0.0339P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00234(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4856 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.823340(5) 0.139588(14) 0.585047(7) 0.02103(6) Uani 1 1 d . . . Cl1 Cl 0.753644(18) -0.01264(5) 0.62839(2) 0.02794(9) Uani 1 1 d . . . P1 P 0.888671(18) 0.26480(5) 0.54174(2) 0.02117(9) Uani 1 1 d . . . O1 O 0.79585(6) 0.02049(15) 0.47765(7) 0.0282(3) Uani 1 1 d . . . N1 N 0.87047(6) 0.27720(16) 0.43980(8) 0.0229(3) Uani 1 1 d . . . C1 C 0.76833(9) -0.0660(2) 0.34533(11) 0.0341(4) Uani 1 1 d . . . H1A H 0.7889 -0.1645 0.3517 0.051 Uiso 1 1 calc R . . H1B H 0.7669 -0.0236 0.2935 0.051 Uiso 1 1 calc R . . H1C H 0.7285 -0.0812 0.3501 0.051 Uiso 1 1 calc R . . O2 O 0.85860(9) 0.3044(2) 0.74013(9) 0.0527(4) Uani 1 1 d . . . N2 N 0.95798(6) 0.18564(18) 0.56450(9) 0.0253(3) Uani 1 1 d . . . C2 C 0.80064(7) 0.0453(2) 0.40865(10) 0.0234(3) Uani 1 1 d . . . N3 N 0.90519(6) 0.45463(17) 0.56686(9) 0.0246(3) Uani 1 1 d . . . C3 C 0.83501(7) 0.1694(2) 0.38659(9) 0.0224(3) Uani 1 1 d . . . C4 C 0.83809(8) 0.2091(2) 0.31033(10) 0.0270(3) Uani 1 1 d . . . H4 H 0.8191 0.1571 0.2634 0.032 Uiso 1 1 calc R . . C5 C 0.87473(8) 0.3409(2) 0.31596(11) 0.0290(4) Uani 1 1 d . . . H5 H 0.8843 0.3921 0.2737 0.035 Uiso 1 1 calc R . . C6 C 0.89379(8) 0.3804(2) 0.39496(11) 0.0276(3) Uani 1 1 d . . . H6 H 0.9187 0.4641 0.4153 0.033 Uiso 1 1 calc R . . C7 C 1.00493(8) 0.2173(2) 0.53114(12) 0.0320(4) Uani 1 1 d . . . H7 H 1.0028 0.2779 0.4859 0.038 Uiso 1 1 calc R . . C8 C 1.05446(9) 0.1450(2) 0.57569(14) 0.0382(5) Uani 1 1 d . . . H8 H 1.0921 0.1469 0.5664 0.046 Uiso 1 1 calc R . . C9 C 1.03856(9) 0.0661(3) 0.63890(14) 0.0429(5) Uani 1 1 d . . . H9 H 1.0639 0.0072 0.6787 0.051 Uiso 1 1 calc R . . C10 C 0.97975(8) 0.0917(2) 0.63125(12) 0.0335(4) Uani 1 1 d . . . H10 H 0.9578 0.0530 0.6649 0.040 Uiso 1 1 calc R . . C11 C 0.95552(8) 0.5083(2) 0.62393(10) 0.0280(3) Uani 1 1 d . . . H11 H 0.9899 0.4509 0.6458 0.034 Uiso 1 1 calc R . . C12 C 0.94558(10) 0.6576(2) 0.64179(12) 0.0354(4) Uani 1 1 d . . . H12 H 0.9722 0.7217 0.6774 0.042 Uiso 1 1 calc R . . C13 C 0.88728(9) 0.7002(2) 0.59690(12) 0.0351(4) Uani 1 1 d . . . H13 H 0.8691 0.7968 0.5980 0.042 Uiso 1 1 calc R . . C14 C 0.86306(8) 0.5747(2) 0.55225(12) 0.0317(4) Uani 1 1 d . . . H14 H 0.8250 0.5696 0.5179 0.038 Uiso 1 1 calc R . . C15 C 0.84530(9) 0.2404(2) 0.68047(11) 0.0320(4) 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 0.02251(8) 0.02125(9) 0.01925(8) -0.00044(4) 0.00532(5) -0.00019(4) Cl1 0.02676(19) 0.0330(2) 0.02467(19) 0.00416(15) 0.00782(15) -0.00217(15) P1 0.02080(19) 0.0215(2) 0.02018(19) -0.00090(15) 0.00351(14) -0.00079(14) O1 0.0341(6) 0.0283(7) 0.0226(6) -0.0034(5) 0.0081(5) -0.0081(5) N1 0.0234(6) 0.0231(7) 0.0211(6) 0.0004(5) 0.0040(5) -0.0012(5) C1 0.0433(11) 0.0309(10) 0.0271(9) -0.0057(7) 0.0072(7) -0.0104(8) O2 0.0794(12) 0.0479(10) 0.0303(8) -0.0136(7) 0.0132(8) -0.0106(9) N2 0.0246(7) 0.0257(7) 0.0249(7) 0.0009(6) 0.0051(5) 0.0025(5) C2 0.0219(7) 0.0242(8) 0.0229(7) -0.0013(6) 0.0040(6) 0.0011(6) N3 0.0237(7) 0.0213(7) 0.0268(7) -0.0014(5) 0.0029(5) -0.0013(5) C3 0.0227(7) 0.0229(8) 0.0205(7) -0.0011(6) 0.0037(6) 0.0021(6) C4 0.0306(8) 0.0275(9) 0.0224(8) 0.0003(6) 0.0061(6) 0.0033(6) C5 0.0311(9) 0.0315(9) 0.0251(8) 0.0055(7) 0.0084(7) 0.0016(7) C6 0.0268(8) 0.0279(9) 0.0284(9) 0.0039(6) 0.0078(7) -0.0031(6) C7 0.0284(9) 0.0360(10) 0.0339(9) 0.0020(8) 0.0121(7) 0.0029(7) C8 0.0272(9) 0.0415(12) 0.0464(12) 0.0007(8) 0.0105(8) 0.0065(7) C9 0.0332(10) 0.0483(13) 0.0440(12) 0.0088(9) 0.0044(8) 0.0141(9) C10 0.0318(9) 0.0353(10) 0.0318(9) 0.0085(8) 0.0054(7) 0.0069(7) C11 0.0252(8) 0.0305(9) 0.0259(8) -0.0020(7) 0.0024(6) -0.0041(6) C12 0.0417(11) 0.0309(10) 0.0310(10) -0.0075(7) 0.0051(8) -0.0074(8) C13 0.0430(10) 0.0255(9) 0.0368(10) -0.0039(7) 0.0104(8) 0.0020(8) C14 0.0298(9) 0.0253(9) 0.0365(9) -0.0018(7) 0.0025(7) 0.0023(7) C15 0.0407(10) 0.0285(9) 0.0276(9) -0.0010(7) 0.0100(7) -0.0018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C15 1.8152(19) . ? Rh1 O1 2.0701(12) . ? Rh1 P1 2.1474(4) . ? Rh1 Cl1 2.3492(4) . ? P1 N2 1.6965(14) . ? P1 N3 1.6977(15) . ? P1 N1 1.7085(14) . ? O1 C2 1.248(2) . ? N1 C6 1.377(2) . ? N1 C3 1.408(2) . ? C1 C2 1.497(2) . ? O2 C15 1.139(2) . ? N2 C7 1.389(2) . ? N2 C10 1.390(2) . ? C2 C3 1.438(2) . ? N3 C14 1.396(2) . ? N3 C11 1.397(2) . ? C3 C4 1.384(2) . ? C4 C5 1.400(3) . ? C5 C6 1.366(3) . ? C7 C8 1.356(3) . ? C8 C9 1.415(3) . ? C9 C10 1.356(3) . ? C11 C12 1.348(3) . ? C12 C13 1.423(3) . ? C13 C14 1.356(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 C15 Rh1 O1 177.88(7) . . ? C15 Rh1 P1 91.46(6) . . ? O1 Rh1 P1 90.66(4) . . ? C15 Rh1 Cl1 91.44(6) . . ? O1 Rh1 Cl1 86.46(4) . . ? P1 Rh1 Cl1 176.136(16) . . ? N2 P1 N3 100.60(7) . . ? N2 P1 N1 103.23(7) . . ? N3 P1 N1 100.61(7) . . ? N2 P1 Rh1 115.83(6) . . ? N3 P1 Rh1 121.34(5) . . ? N1 P1 Rh1 112.66(5) . . ? C2 O1 Rh1 133.94(11) . . ? C6 N1 C3 107.41(14) . . ? C6 N1 P1 126.55(12) . . ? C3 N1 P1 125.51(11) . . ? C7 N2 C10 107.69(15) . . ? C7 N2 P1 128.87(13) . . ? C10 N2 P1 122.76(13) . . ? O1 C2 C3 125.09(15) . . ? O1 C2 C1 116.16(15) . . ? C3 C2 C1 118.74(15) . . ? C14 N3 C11 107.78(15) . . ? C14 N3 P1 123.74(12) . . ? C11 N3 P1 125.90(12) . . ? C4 C3 N1 107.28(15) . . ? C4 C3 C2 127.26(15) . . ? N1 C3 C2 125.42(14) . . ? C3 C4 C5 108.25(16) . . ? C6 C5 C4 107.49(16) . . ? C5 C6 N1 109.56(16) . . ? C8 C7 N2 108.49(17) . . ? C7 C8 C9 107.62(18) . . ? C10 C9 C8 107.94(18) . . ? C9 C10 N2 108.25(18) . . ? C12 C11 N3 108.12(16) . . ? C11 C12 C13 108.24(17) . . ? C14 C13 C12 107.69(17) . . ? C13 C14 N3 108.13(16) . . ? O2 C15 Rh1 179.4(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.692 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.076 #===END data_compound7b_k00adb2 _database_code_CSD 211981 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 F6 N2 O2 P3 Rh' _chemical_formula_weight 834.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.76700(10) _cell_length_b 20.3440(3) _cell_length_c 17.9680(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.8440(9) _cell_angle_gamma 90.00 _cell_volume 3451.09(8) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.8438 _exptl_absorpt_correction_T_max 0.8868 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42796 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7921 _reflns_number_gt 7055 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0953P)^2^+0.4084P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7921 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.471520(14) 0.290714(7) 0.092547(8) 0.01887(8) Uani 1 1 d . . . P1 P 0.61508(5) 0.36779(2) 0.14795(3) 0.01942(12) Uani 1 1 d . . . P2 P 0.56911(5) 0.26714(3) 0.00008(3) 0.01957(12) Uani 1 1 d . . . P3 P 0.92148(6) 0.06112(3) 0.15970(4) 0.03810(16) Uani 1 1 d . . . O1 O 0.34446(15) 0.30745(8) 0.16806(9) 0.0270(3) Uani 1 1 d . . . O2 O 0.33197(16) 0.21203(7) 0.05994(9) 0.0266(3) Uani 1 1 d . . . N1 N 0.52174(17) 0.42717(8) 0.18676(10) 0.0233(3) Uani 1 1 d . . . N2 N 0.55861(17) 0.18219(8) -0.01660(10) 0.0234(3) Uani 1 1 d . . . F1 F 0.9269(2) 0.05232(12) 0.24810(11) 0.0775(6) Uani 1 1 d . . . F2 F 0.9146(2) 0.07240(15) 0.07207(12) 0.0906(8) Uani 1 1 d . . . F3 F 0.97948(19) 0.13433(8) 0.17739(13) 0.0704(6) Uani 1 1 d . . . F4 F 0.76332(17) 0.08749(10) 0.14540(12) 0.0672(5) Uani 1 1 d . . . F5 F 0.8622(2) -0.01164(9) 0.14374(13) 0.0720(6) Uani 1 1 d . . . F6 F 1.08017(17) 0.03556(9) 0.17522(14) 0.0724(6) Uani 1 1 d . . . C1 C 0.7481(2) 0.34091(10) 0.23303(11) 0.0237(4) Uani 1 1 d . . . C2 C 0.7888(2) 0.27474(12) 0.23769(13) 0.0304(5) Uani 1 1 d . . . H2 H 0.7431 0.2449 0.1985 0.036 Uiso 1 1 calc R . . C3 C 0.8958(2) 0.25265(13) 0.29945(14) 0.0394(6) Uani 1 1 d . . . H3 H 0.9243 0.2079 0.3022 0.047 Uiso 1 1 calc R . . C4 C 0.9608(3) 0.29618(14) 0.35705(15) 0.0420(6) Uani 1 1 d . . . H4 H 1.0343 0.2811 0.3991 0.050 Uiso 1 1 calc R . . C5 C 0.9200(3) 0.36119(14) 0.35392(13) 0.0400(6) Uani 1 1 d . . . H5 H 0.9646 0.3905 0.3939 0.048 Uiso 1 1 calc R . . C6 C 0.8137(2) 0.38378(12) 0.29241(12) 0.0304(5) Uani 1 1 d . . . H6 H 0.7853 0.4285 0.2906 0.037 Uiso 1 1 calc R . . C7 C 0.7079(2) 0.42269(10) 0.09738(11) 0.0221(4) Uani 1 1 d . . . C8 C 0.6335(2) 0.44453(10) 0.02491(12) 0.0243(4) Uani 1 1 d . . . H8 H 0.5405 0.4286 0.0029 0.029 Uiso 1 1 calc R . . C9 C 0.6940(2) 0.48925(11) -0.01542(13) 0.0290(4) Uani 1 1 d . . . H9 H 0.6424 0.5042 -0.0647 0.035 Uiso 1 1 calc R . . C10 C 0.8298(2) 0.51207(11) 0.01631(13) 0.0305(5) Uani 1 1 d . . . H10 H 0.8709 0.5430 -0.0111 0.037 Uiso 1 1 calc R . . C11 C 0.9060(2) 0.49008(12) 0.08771(13) 0.0321(5) Uani 1 1 d . . . H11 H 0.9995 0.5057 0.1090 0.039 Uiso 1 1 calc R . . C12 C 0.8455(2) 0.44482(11) 0.12860(12) 0.0274(4) Uani 1 1 d . . . H12 H 0.8981 0.4293 0.1774 0.033 Uiso 1 1 calc R . . C13 C 0.5616(2) 0.49099(10) 0.20392(13) 0.0300(4) Uani 1 1 d . . . H13 H 0.6402 0.5119 0.1918 0.036 Uiso 1 1 calc R . . C14 C 0.4714(3) 0.52049(12) 0.24120(14) 0.0369(5) Uani 1 1 d . . . H14 H 0.4754 0.5647 0.2586 0.044 Uiso 1 1 calc R . . C15 C 0.3728(2) 0.47293(11) 0.24844(14) 0.0339(5) Uani 1 1 d . . . H15 H 0.2974 0.4792 0.2722 0.041 Uiso 1 1 calc R . . C16 C 0.4027(2) 0.41550(10) 0.21546(12) 0.0253(4) Uani 1 1 d . . . C17 C 0.3258(2) 0.35486(11) 0.20804(12) 0.0252(4) Uani 1 1 d . . . C18 C 0.2140(3) 0.34705(13) 0.25187(16) 0.0404(6) Uani 1 1 d . . . H18A H 0.1287 0.3276 0.2181 0.061 Uiso 1 1 calc R . . H18B H 0.1908 0.3902 0.2696 0.061 Uiso 1 1 calc R . . H18C H 0.2498 0.3183 0.2964 0.061 Uiso 1 1 calc R . . C19 C 0.4698(2) 0.29821(9) -0.09319(12) 0.0223(4) Uani 1 1 d . . . C20 C 0.3454(2) 0.33346(11) -0.09786(12) 0.0277(4) Uani 1 1 d . . . H20 H 0.3164 0.3426 -0.0523 0.033 Uiso 1 1 calc R . . C21 C 0.2635(2) 0.35529(12) -0.16844(14) 0.0349(5) Uani 1 1 d . . . H21 H 0.1783 0.3788 -0.1713 0.042 Uiso 1 1 calc R . . C22 C 0.3066(3) 0.34271(12) -0.23446(14) 0.0383(5) Uani 1 1 d . . . H22 H 0.2506 0.3575 -0.2829 0.046 Uiso 1 1 calc R . . C23 C 0.4308(3) 0.30873(12) -0.23040(13) 0.0333(5) Uani 1 1 d . . . H23 H 0.4610 0.3014 -0.2759 0.040 Uiso 1 1 calc R . . C24 C 0.5112(3) 0.28540(10) -0.16100(13) 0.0281(5) Uani 1 1 d . . . H24 H 0.5945 0.2607 -0.1590 0.034 Uiso 1 1 calc R . . C25 C 0.7546(2) 0.28201(10) 0.00480(12) 0.0223(4) Uani 1 1 d . . . C26 C 0.8568(2) 0.24799(11) 0.05910(12) 0.0261(4) Uani 1 1 d . . . H26 H 0.8290 0.2150 0.0896 0.031 Uiso 1 1 calc R . . C27 C 1.0000(2) 0.26208(12) 0.06896(13) 0.0311(5) Uani 1 1 d . . . H27 H 1.0697 0.2384 0.1058 0.037 Uiso 1 1 calc R . . C28 C 1.0402(2) 0.31069(12) 0.02495(14) 0.0324(5) Uani 1 1 d . . . H28 H 1.1376 0.3211 0.0325 0.039 Uiso 1 1 calc R . . C29 C 0.9390(2) 0.34425(11) -0.02999(13) 0.0300(5) Uani 1 1 d . . . H29 H 0.9675 0.3770 -0.0606 0.036 Uiso 1 1 calc R . . C30 C 0.7958(2) 0.33032(10) -0.04058(12) 0.0242(4) Uani 1 1 d . . . H30 H 0.7265 0.3534 -0.0783 0.029 Uiso 1 1 calc R . . C31 C 0.6390(2) 0.14753(11) -0.05553(14) 0.0316(5) Uani 1 1 d . . . H31 H 0.7214 0.1637 -0.0682 0.038 Uiso 1 1 calc R . . C32 C 0.5825(2) 0.08595(11) -0.07341(14) 0.0348(5) Uani 1 1 d . . . H32 H 0.6187 0.0524 -0.0999 0.042 Uiso 1 1 calc R . . C33 C 0.4623(2) 0.08198(11) -0.04541(13) 0.0326(5) Uani 1 1 d . . . H33 H 0.4015 0.0450 -0.0497 0.039 Uiso 1 1 calc R . . C34 C 0.4465(2) 0.14108(10) -0.01033(12) 0.0247(4) Uani 1 1 d . . . C35 C 0.3394(2) 0.15811(10) 0.02789(12) 0.0249(4) Uani 1 1 d . . . C36 C 0.2296(2) 0.10707(12) 0.03253(15) 0.0372(5) Uani 1 1 d . . . H36A H 0.2672 0.0781 0.0766 0.056 Uiso 1 1 calc R . . H36B H 0.2062 0.0811 -0.0150 0.056 Uiso 1 1 calc R . . H36C H 0.1440 0.1290 0.0390 0.056 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 0.01734(12) 0.02065(12) 0.02055(12) -0.00027(5) 0.00840(8) -0.00155(5) P1 0.0182(2) 0.0210(3) 0.0207(2) 0.00018(18) 0.00799(19) -0.00121(18) P2 0.0179(2) 0.0208(3) 0.0219(3) -0.00030(19) 0.00845(19) -0.00029(19) P3 0.0305(3) 0.0397(4) 0.0426(4) 0.0097(3) 0.0065(3) -0.0079(2) O1 0.0248(7) 0.0301(8) 0.0309(8) -0.0034(6) 0.0158(6) -0.0046(6) O2 0.0224(7) 0.0274(8) 0.0326(8) -0.0045(6) 0.0118(6) -0.0058(5) N1 0.0221(8) 0.0244(8) 0.0261(9) -0.0022(7) 0.0108(7) -0.0013(6) N2 0.0238(8) 0.0213(8) 0.0273(9) -0.0027(7) 0.0104(7) -0.0014(7) F1 0.0802(13) 0.1041(16) 0.0420(10) 0.0180(10) 0.0043(9) -0.0158(12) F2 0.0771(14) 0.149(2) 0.0504(11) 0.0147(13) 0.0252(10) -0.0265(14) F3 0.0537(10) 0.0371(9) 0.1081(16) 0.0171(9) -0.0019(10) -0.0062(8) F4 0.0342(8) 0.0838(14) 0.0798(13) 0.0173(11) 0.0077(8) 0.0032(8) F5 0.0613(11) 0.0517(11) 0.1129(17) -0.0189(11) 0.0406(11) -0.0268(9) F6 0.0375(8) 0.0443(10) 0.1357(19) 0.0195(11) 0.0227(10) 0.0021(7) C1 0.0189(8) 0.0311(11) 0.0232(9) 0.0033(8) 0.0091(7) -0.0022(8) C2 0.0287(11) 0.0358(11) 0.0289(11) 0.0066(9) 0.0115(9) 0.0024(9) C3 0.0358(12) 0.0458(14) 0.0390(13) 0.0171(11) 0.0139(10) 0.0094(11) C4 0.0280(12) 0.0663(19) 0.0304(13) 0.0196(11) 0.0052(10) 0.0008(11) C5 0.0339(12) 0.0607(17) 0.0242(11) 0.0048(11) 0.0053(9) -0.0140(11) C6 0.0281(10) 0.0380(12) 0.0255(10) 0.0013(9) 0.0072(9) -0.0071(9) C7 0.0228(9) 0.0218(9) 0.0241(9) 0.0000(7) 0.0106(8) -0.0010(7) C8 0.0225(9) 0.0228(10) 0.0292(10) -0.0010(8) 0.0096(8) -0.0011(7) C9 0.0330(11) 0.0277(11) 0.0287(11) 0.0048(8) 0.0122(9) 0.0036(8) C10 0.0370(11) 0.0252(11) 0.0352(12) 0.0011(9) 0.0201(10) -0.0048(9) C11 0.0265(10) 0.0397(13) 0.0336(11) -0.0014(10) 0.0139(9) -0.0100(9) C12 0.0259(10) 0.0321(11) 0.0267(10) 0.0001(9) 0.0113(8) -0.0062(8) C13 0.0333(11) 0.0240(10) 0.0358(12) -0.0028(9) 0.0145(9) -0.0037(8) C14 0.0451(13) 0.0270(11) 0.0442(13) -0.0074(10) 0.0219(11) -0.0007(10) C15 0.0364(11) 0.0339(12) 0.0377(12) -0.0047(10) 0.0207(10) 0.0019(9) C16 0.0225(9) 0.0291(11) 0.0269(10) 0.0010(8) 0.0112(8) 0.0023(8) C17 0.0207(9) 0.0315(11) 0.0252(10) 0.0015(8) 0.0092(8) 0.0018(8) C18 0.0396(13) 0.0430(14) 0.0497(15) -0.0087(11) 0.0317(12) -0.0064(11) C19 0.0228(10) 0.0221(9) 0.0215(10) 0.0004(7) 0.0046(8) -0.0041(7) C20 0.0256(10) 0.0287(11) 0.0298(11) 0.0007(8) 0.0087(9) -0.0013(8) C21 0.0264(10) 0.0354(12) 0.0398(13) 0.0058(10) 0.0030(10) 0.0007(9) C22 0.0426(13) 0.0394(13) 0.0266(11) 0.0068(10) -0.0030(10) -0.0078(10) C23 0.0437(13) 0.0351(12) 0.0219(10) -0.0039(9) 0.0098(10) -0.0069(10) C24 0.0317(11) 0.0312(12) 0.0228(11) -0.0043(8) 0.0096(9) -0.0020(8) C25 0.0195(9) 0.0238(10) 0.0259(10) -0.0023(8) 0.0098(8) -0.0006(7) C26 0.0240(9) 0.0278(10) 0.0290(10) 0.0008(8) 0.0110(8) 0.0024(8) C27 0.0217(10) 0.0364(13) 0.0350(12) -0.0031(9) 0.0069(9) 0.0030(9) C28 0.0203(9) 0.0394(12) 0.0409(13) -0.0073(10) 0.0140(9) -0.0049(9) C29 0.0309(11) 0.0276(11) 0.0359(12) -0.0046(9) 0.0164(9) -0.0077(8) C30 0.0257(10) 0.0222(10) 0.0275(10) -0.0028(8) 0.0121(8) -0.0019(8) C31 0.0315(11) 0.0280(11) 0.0402(12) -0.0068(9) 0.0180(10) 0.0013(9) C32 0.0371(12) 0.0257(11) 0.0439(13) -0.0110(10) 0.0147(11) 0.0020(9) C33 0.0357(11) 0.0250(11) 0.0377(12) -0.0054(9) 0.0103(10) -0.0050(9) C34 0.0255(10) 0.0222(10) 0.0258(10) 0.0017(8) 0.0054(8) -0.0021(8) C35 0.0235(9) 0.0258(10) 0.0250(10) 0.0014(8) 0.0054(8) -0.0052(8) C36 0.0346(12) 0.0344(13) 0.0457(14) -0.0062(10) 0.0163(11) -0.0165(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O2 2.0867(14) . ? Rh1 O1 2.0880(13) . ? Rh1 P1 2.1680(5) . ? Rh1 P2 2.1704(5) . ? P1 N1 1.7615(16) . ? P1 C1 1.818(2) . ? P1 C7 1.8214(19) . ? P2 N2 1.7525(17) . ? P2 C25 1.817(2) . ? P2 C19 1.821(2) . ? P3 F2 1.576(2) . ? P3 F1 1.5859(19) . ? P3 F5 1.5886(18) . ? P3 F6 1.5902(17) . ? P3 F4 1.5927(17) . ? P3 F3 1.5962(18) . ? O1 C17 1.243(3) . ? O2 C35 1.250(2) . ? N1 C13 1.368(3) . ? N1 C16 1.408(2) . ? N2 C31 1.372(3) . ? N2 C34 1.405(2) . ? C1 C2 1.400(3) . ? C1 C6 1.400(3) . ? C2 C3 1.390(3) . ? C3 C4 1.386(4) . ? C4 C5 1.378(4) . ? C5 C6 1.386(3) . ? C7 C12 1.392(3) . ? C7 C8 1.391(3) . ? C8 C9 1.386(3) . ? C9 C10 1.383(3) . ? C10 C11 1.382(3) . ? C11 C12 1.400(3) . ? C13 C14 1.374(3) . ? C14 C15 1.395(3) . ? C15 C16 1.375(3) . ? C16 C17 1.432(3) . ? C17 C18 1.510(3) . ? C19 C20 1.395(3) . ? C19 C24 1.403(3) . ? C20 C21 1.387(3) . ? C21 C22 1.380(3) . ? C22 C23 1.382(4) . ? C23 C24 1.377(3) . ? C25 C26 1.389(3) . ? C25 C30 1.400(3) . ? C26 C27 1.393(3) . ? C27 C28 1.384(3) . ? C28 C29 1.385(3) . ? C29 C30 1.392(3) . ? C31 C32 1.373(3) . ? C32 C33 1.393(3) . ? C33 C34 1.384(3) . ? C34 C35 1.433(3) . ? C35 C36 1.511(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 O2 Rh1 O1 81.57(6) . . ? O2 Rh1 P1 169.36(5) . . ? O1 Rh1 P1 90.34(4) . . ? O2 Rh1 P2 89.93(4) . . ? O1 Rh1 P2 169.80(4) . . ? P1 Rh1 P2 98.748(18) . . ? N1 P1 C1 101.78(9) . . ? N1 P1 C7 98.70(8) . . ? C1 P1 C7 105.30(9) . . ? N1 P1 Rh1 109.78(6) . . ? C1 P1 Rh1 114.04(7) . . ? C7 P1 Rh1 124.10(7) . . ? N2 P2 C25 100.73(8) . . ? N2 P2 C19 101.01(9) . . ? C25 P2 C19 105.94(9) . . ? N2 P2 Rh1 109.32(6) . . ? C25 P2 Rh1 123.75(7) . . ? C19 P2 Rh1 113.14(7) . . ? F2 P3 F1 178.04(15) . . ? F2 P3 F5 92.02(14) . . ? F1 P3 F5 89.58(12) . . ? F2 P3 F6 90.74(12) . . ? F1 P3 F6 90.37(12) . . ? F5 P3 F6 91.20(10) . . ? F2 P3 F4 89.92(12) . . ? F1 P3 F4 88.95(11) . . ? F5 P3 F4 89.48(11) . . ? F6 P3 F4 179.04(13) . . ? F2 P3 F3 89.15(13) . . ? F1 P3 F3 89.24(12) . . ? F5 P3 F3 178.67(12) . . ? F6 P3 F3 89.42(10) . . ? F4 P3 F3 89.88(10) . . ? C17 O1 Rh1 134.52(13) . . ? C35 O2 Rh1 133.76(13) . . ? C13 N1 C16 106.96(16) . . ? C13 N1 P1 126.43(14) . . ? C16 N1 P1 126.11(14) . . ? C31 N2 C34 107.10(17) . . ? C31 N2 P2 125.29(14) . . ? C34 N2 P2 125.88(13) . . ? C2 C1 C6 119.1(2) . . ? C2 C1 P1 118.04(16) . . ? C6 C1 P1 122.85(17) . . ? C3 C2 C1 120.2(2) . . ? C4 C3 C2 119.8(2) . . ? C5 C4 C3 120.7(2) . . ? C4 C5 C6 120.0(2) . . ? C5 C6 C1 120.3(2) . . ? C12 C7 C8 119.51(18) . . ? C12 C7 P1 123.37(16) . . ? C8 C7 P1 117.08(14) . . ? C9 C8 C7 120.57(19) . . ? C10 C9 C8 119.8(2) . . ? C9 C10 C11 120.37(19) . . ? C10 C11 C12 120.0(2) . . ? C7 C12 C11 119.7(2) . . ? N1 C13 C14 110.08(19) . . ? C13 C14 C15 106.7(2) . . ? C16 C15 C14 108.76(18) . . ? C15 C16 N1 107.52(18) . . ? C15 C16 C17 127.46(18) . . ? N1 C16 C17 124.98(17) . . ? O1 C17 C16 124.83(17) . . ? O1 C17 C18 116.88(19) . . ? C16 C17 C18 118.29(18) . . ? C20 C19 C24 118.9(2) . . ? C20 C19 P2 118.96(16) . . ? C24 C19 P2 122.07(17) . . ? C21 C20 C19 120.6(2) . . ? C22 C21 C20 119.7(2) . . ? C23 C22 C21 120.3(2) . . ? C24 C23 C22 120.6(2) . . ? C23 C24 C19 119.9(2) . . ? C26 C25 C30 119.77(18) . . ? C26 C25 P2 118.59(15) . . ? C30 C25 P2 121.44(16) . . ? C25 C26 C27 120.28(19) . . ? C28 C27 C26 119.8(2) . . ? C29 C28 C27 120.30(19) . . ? C28 C29 C30 120.4(2) . . ? C29 C30 C25 119.5(2) . . ? C32 C31 N2 109.90(18) . . ? C31 C32 C33 107.05(19) . . ? C34 C33 C32 108.45(19) . . ? C33 C34 N2 107.49(17) . . ? C33 C34 C35 127.46(19) . . ? N2 C34 C35 125.02(18) . . ? O2 C35 C34 124.68(18) . . ? O2 C35 C36 116.84(18) . . ? C34 C35 C36 118.45(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.669 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.073 #===END data_compound8_k00adb5 _database_code_CSD 211982 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 F6 N6 O2 P3 Rh' _chemical_formula_weight 790.38 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.02300(10) _cell_length_b 20.4470(2) _cell_length_c 17.3330(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.5720(6) _cell_angle_gamma 90.00 _cell_volume 3132.82(6) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74888 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7159 _reflns_number_gt 6508 _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^)+(0.0493P)^2^+4.5232P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7159 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.925285(18) 0.283099(8) 0.910511(10) 0.01760(7) Uani 1 1 d . . . P1 P 1.01524(6) 0.36706(3) 0.86207(3) 0.01738(12) Uani 1 1 d . . . P2 P 1.10512(6) 0.26634(3) 1.00962(3) 0.01773(12) Uani 1 1 d . . . P3 P 1.21271(11) 0.06939(4) 0.83627(5) 0.0434(2) Uani 1 1 d . . . F1 F 1.2446(4) 0.14353(12) 0.82120(17) 0.0993(10) Uani 1 1 d . . . F2 F 1.2771(4) 0.07642(16) 0.92732(13) 0.0895(9) Uani 1 1 d . . . F3 F 1.1885(3) -0.00722(11) 0.84628(18) 0.0780(7) Uani 1 1 d . . . F4 F 1.1468(3) 0.06225(14) 0.74466(12) 0.0782(8) Uani 1 1 d . . . F5 F 1.3795(3) 0.05415(13) 0.82175(15) 0.0740(7) Uani 1 1 d . . . F6 F 1.0453(3) 0.07955(19) 0.84940(16) 0.0997(10) Uani 1 1 d . . . O1 O 0.72845(18) 0.29523(8) 0.82455(10) 0.0245(3) Uani 1 1 d . . . O2 O 0.81404(18) 0.19868(8) 0.93276(10) 0.0259(3) Uani 1 1 d . . . N1 N 0.8742(2) 0.42398(9) 0.83078(11) 0.0215(4) Uani 1 1 d . . . N2 N 1.1529(2) 0.41770(9) 0.90869(11) 0.0207(4) Uani 1 1 d . . . N3 N 1.0715(2) 0.34879(10) 0.77731(11) 0.0223(4) Uani 1 1 d . . . N4 N 1.1164(2) 0.18488(9) 1.03590(11) 0.0207(4) Uani 1 1 d . . . N5 N 1.2905(2) 0.28057(9) 1.01136(12) 0.0225(4) Uani 1 1 d . . . N6 N 1.0811(2) 0.30532(10) 1.09242(11) 0.0230(4) Uani 1 1 d . . . C1 C 0.6567(2) 0.34545(12) 0.79773(13) 0.0222(4) Uani 1 1 d . . . C2 C 0.4948(3) 0.33614(14) 0.75701(17) 0.0329(6) Uani 1 1 d . . . H2A H 0.4897 0.3040 0.7146 0.049 Uiso 1 1 calc R . . H2B H 0.4532 0.3779 0.7349 0.049 Uiso 1 1 calc R . . H2C H 0.4359 0.3203 0.7950 0.049 Uiso 1 1 calc R . . C3 C 0.7199(2) 0.40978(12) 0.80324(13) 0.0229(4) Uani 1 1 d . . . C4 C 0.6476(3) 0.46834(12) 0.77994(15) 0.0296(5) Uani 1 1 d . . . H4 H 0.5426 0.4737 0.7592 0.036 Uiso 1 1 calc R . . C5 C 0.7555(3) 0.51827(13) 0.79215(16) 0.0335(6) Uani 1 1 d . . . H5 H 0.7370 0.5634 0.7812 0.040 Uiso 1 1 calc R . . C6 C 0.8929(3) 0.49040(11) 0.82272(15) 0.0281(5) Uani 1 1 d . . . H6 H 0.9862 0.5132 0.8362 0.034 Uiso 1 1 calc R . . C7 C 1.1450(3) 0.44881(11) 0.97938(14) 0.0241(5) Uani 1 1 d . . . H7 H 1.0761 0.4385 1.0125 0.029 Uiso 1 1 calc R . . C8 C 1.2522(3) 0.49621(12) 0.99279(15) 0.0289(5) Uani 1 1 d . . . H8 H 1.2718 0.5248 1.0368 0.035 Uiso 1 1 calc R . . C9 C 1.3298(3) 0.49541(13) 0.92934(16) 0.0320(5) Uani 1 1 d . . . H9 H 1.4112 0.5233 0.9236 0.038 Uiso 1 1 calc R . . C10 C 1.2675(3) 0.44787(12) 0.87806(15) 0.0264(5) Uani 1 1 d . . . H10 H 1.2967 0.4371 0.8299 0.032 Uiso 1 1 calc R . . C11 C 1.0846(3) 0.38988(13) 0.71408(14) 0.0284(5) Uani 1 1 d . . . H11 H 1.0698 0.4359 0.7119 0.034 Uiso 1 1 calc R . . C12 C 1.1221(3) 0.35205(16) 0.65687(15) 0.0357(6) Uani 1 1 d . . . H12 H 1.1394 0.3672 0.6076 0.043 Uiso 1 1 calc R . . C13 C 1.1315(3) 0.28636(15) 0.68251(17) 0.0360(6) Uani 1 1 d . . . H13 H 1.1555 0.2498 0.6535 0.043 Uiso 1 1 calc R . . C14 C 1.1000(3) 0.28471(12) 0.75584(16) 0.0276(5) Uani 1 1 d . . . H14 H 1.0978 0.2467 0.7871 0.033 Uiso 1 1 calc R . . C15 C 0.8555(3) 0.14706(11) 0.96974(14) 0.0235(4) Uani 1 1 d . . . C16 C 0.7466(3) 0.09092(13) 0.95558(17) 0.0346(6) Uani 1 1 d . . . H16A H 0.6432 0.1077 0.9402 0.052 Uiso 1 1 calc R . . H16B H 0.7556 0.0651 1.0039 0.052 Uiso 1 1 calc R . . H16C H 0.7698 0.0632 0.9134 0.052 Uiso 1 1 calc R . . C17 C 0.9990(3) 0.13821(11) 1.02137(13) 0.0223(4) Uani 1 1 d . . . C18 C 1.0520(3) 0.08214(12) 1.06274(14) 0.0274(5) Uani 1 1 d . . . H18 H 0.9967 0.0428 1.0643 0.033 Uiso 1 1 calc R . . C19 C 1.2015(3) 0.09359(12) 1.10201(14) 0.0295(5) Uani 1 1 d . . . H19 H 1.2660 0.0632 1.1341 0.035 Uiso 1 1 calc R . . C20 C 1.2376(3) 0.15635(12) 1.08579(14) 0.0257(5) Uani 1 1 d . . . H20 H 1.3316 0.1771 1.1058 0.031 Uiso 1 1 calc R . . C21 C 1.3686(3) 0.24839(14) 0.96086(15) 0.0318(5) Uani 1 1 d . . . H21 H 1.3330 0.2118 0.9287 0.038 Uiso 1 1 calc R . . C22 C 1.5039(3) 0.27841(15) 0.96553(19) 0.0395(7) Uani 1 1 d . . . H22 H 1.5807 0.2661 0.9380 0.047 Uiso 1 1 calc R . . C23 C 1.5104(3) 0.33120(14) 1.0186(2) 0.0413(7) Uani 1 1 d . . . H23 H 1.5924 0.3609 1.0328 0.050 Uiso 1 1 calc R . . C24 C 1.3797(3) 0.33236(12) 1.04593(17) 0.0309(5) Uani 1 1 d . . . H24 H 1.3537 0.3630 1.0822 0.037 Uiso 1 1 calc R . . C25 C 0.9463(3) 0.33776(12) 1.09607(16) 0.0285(5) Uani 1 1 d . . . H25 H 0.8678 0.3479 1.0524 0.034 Uiso 1 1 calc R . . C26 C 0.9461(3) 0.35239(14) 1.17254(17) 0.0373(6) Uani 1 1 d . . . H26 H 0.8687 0.3749 1.1917 0.045 Uiso 1 1 calc R . . C27 C 1.0825(4) 0.32795(13) 1.21836(16) 0.0399(7) Uani 1 1 d . . . H27 H 1.1125 0.3312 1.2740 0.048 Uiso 1 1 calc R . . C28 C 1.1632(3) 0.29904(13) 1.16961(14) 0.0324(6) Uani 1 1 d . . . H28 H 1.2586 0.2782 1.1852 0.039 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 0.01556(10) 0.01752(10) 0.01910(10) 0.00085(6) 0.00201(7) -0.00160(6) P1 0.0171(2) 0.0168(2) 0.0180(3) -0.00052(19) 0.00285(19) -0.00121(19) P2 0.0161(2) 0.0182(3) 0.0186(3) 0.0006(2) 0.0029(2) -0.0006(2) P3 0.0651(5) 0.0374(4) 0.0304(4) -0.0069(3) 0.0163(3) -0.0129(4) F1 0.161(3) 0.0395(12) 0.0839(19) -0.0058(12) -0.0076(19) -0.0168(15) F2 0.117(2) 0.118(2) 0.0308(11) -0.0062(12) 0.0086(12) 0.0096(18) F3 0.0786(16) 0.0476(13) 0.114(2) 0.0075(13) 0.0332(15) -0.0154(11) F4 0.0875(17) 0.110(2) 0.0373(11) -0.0126(12) 0.0140(11) -0.0499(16) F5 0.0585(13) 0.0892(18) 0.0792(16) 0.0051(13) 0.0257(12) -0.0183(12) F6 0.0836(18) 0.154(3) 0.0690(16) -0.0093(18) 0.0334(14) 0.0475(19) O1 0.0203(8) 0.0248(8) 0.0258(8) 0.0014(6) -0.0015(6) -0.0020(6) O2 0.0202(8) 0.0228(8) 0.0335(9) 0.0051(7) 0.0024(7) -0.0047(6) N1 0.0205(9) 0.0190(9) 0.0241(9) -0.0003(7) 0.0028(7) 0.0003(7) N2 0.0201(9) 0.0210(9) 0.0204(9) -0.0025(7) 0.0029(7) -0.0028(7) N3 0.0234(9) 0.0233(9) 0.0204(9) -0.0019(7) 0.0051(7) -0.0020(7) N4 0.0197(9) 0.0191(9) 0.0231(9) 0.0024(7) 0.0039(7) 0.0014(7) N5 0.0183(9) 0.0253(10) 0.0234(9) -0.0001(7) 0.0028(7) -0.0024(7) N6 0.0264(10) 0.0217(10) 0.0208(9) -0.0010(7) 0.0044(8) 0.0011(7) C1 0.0196(10) 0.0286(11) 0.0181(10) -0.0015(8) 0.0029(8) 0.0010(9) C2 0.0202(11) 0.0357(14) 0.0386(14) -0.0010(11) -0.0040(10) 0.0005(10) C3 0.0198(10) 0.0270(12) 0.0209(10) -0.0011(8) 0.0020(8) 0.0030(8) C4 0.0289(12) 0.0290(12) 0.0295(12) 0.0000(10) 0.0023(10) 0.0073(10) C5 0.0386(14) 0.0215(12) 0.0383(14) 0.0020(10) 0.0027(11) 0.0069(10) C6 0.0326(13) 0.0192(11) 0.0315(12) 0.0007(9) 0.0041(10) -0.0008(9) C7 0.0272(11) 0.0223(11) 0.0225(11) -0.0012(8) 0.0045(9) -0.0002(9) C8 0.0332(13) 0.0227(11) 0.0282(12) -0.0062(9) 0.0002(10) -0.0030(9) C9 0.0280(12) 0.0298(13) 0.0368(14) -0.0031(10) 0.0032(10) -0.0103(10) C10 0.0217(11) 0.0294(12) 0.0292(12) -0.0034(9) 0.0075(9) -0.0067(9) C11 0.0258(11) 0.0351(13) 0.0238(11) 0.0043(10) 0.0039(9) -0.0058(10) C12 0.0273(12) 0.0601(18) 0.0205(11) -0.0027(11) 0.0067(10) -0.0067(12) C13 0.0271(13) 0.0490(17) 0.0324(14) -0.0172(12) 0.0069(11) -0.0031(11) C14 0.0234(11) 0.0276(12) 0.0317(13) -0.0083(9) 0.0049(10) -0.0016(9) C15 0.0255(11) 0.0218(11) 0.0250(11) -0.0004(9) 0.0093(9) -0.0036(9) C16 0.0341(13) 0.0260(13) 0.0423(15) 0.0034(11) 0.0043(11) -0.0108(10) C17 0.0256(11) 0.0209(10) 0.0220(10) -0.0007(8) 0.0083(9) -0.0025(9) C18 0.0370(13) 0.0212(11) 0.0253(11) 0.0028(9) 0.0093(10) -0.0005(10) C19 0.0377(13) 0.0250(12) 0.0251(11) 0.0048(9) 0.0047(10) 0.0063(10) C20 0.0262(11) 0.0262(11) 0.0232(11) 0.0027(9) 0.0012(9) 0.0049(9) C21 0.0248(12) 0.0433(15) 0.0286(12) -0.0023(11) 0.0085(10) 0.0015(11) C22 0.0245(13) 0.0478(17) 0.0495(17) 0.0162(13) 0.0156(12) 0.0051(11) C23 0.0207(12) 0.0340(14) 0.068(2) 0.0125(13) 0.0048(12) -0.0034(10) C24 0.0215(11) 0.0216(11) 0.0460(15) 0.0025(10) -0.0017(10) -0.0020(9) C25 0.0279(12) 0.0266(12) 0.0340(13) -0.0032(10) 0.0133(10) 0.0003(9) C26 0.0491(16) 0.0301(13) 0.0397(15) -0.0067(11) 0.0254(13) -0.0027(12) C27 0.070(2) 0.0277(13) 0.0234(12) -0.0030(10) 0.0127(13) -0.0057(13) C28 0.0473(15) 0.0258(12) 0.0208(11) 0.0007(9) -0.0007(11) 0.0008(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O2 2.0716(16) . ? Rh1 O1 2.0914(16) . ? Rh1 P2 2.1409(6) . ? Rh1 P1 2.1411(6) . ? P1 N3 1.690(2) . ? P1 N2 1.6930(19) . ? P1 N1 1.7297(19) . ? P2 N5 1.692(2) . ? P2 N6 1.693(2) . ? P2 N4 1.7243(19) . ? P3 F1 1.575(3) . ? P3 F2 1.575(2) . ? P3 F6 1.585(3) . ? P3 F4 1.587(2) . ? P3 F3 1.596(2) . ? P3 F5 1.605(3) . ? O1 C1 1.253(3) . ? O2 C15 1.252(3) . ? N1 C6 1.379(3) . ? N1 C3 1.408(3) . ? N2 C7 1.395(3) . ? N2 C10 1.397(3) . ? N3 C14 1.400(3) . ? N3 C11 1.405(3) . ? N4 C20 1.380(3) . ? N4 C17 1.410(3) . ? N5 C24 1.391(3) . ? N5 C21 1.394(3) . ? N6 C25 1.399(3) . ? N6 C28 1.399(3) . ? C1 C3 1.429(3) . ? C1 C2 1.501(3) . ? C3 C4 1.384(3) . ? C4 C5 1.397(4) . ? C5 C6 1.371(4) . ? C7 C8 1.356(3) . ? C8 C9 1.417(4) . ? C9 C10 1.360(3) . ? C11 C12 1.353(4) . ? C12 C13 1.412(4) . ? C13 C14 1.357(4) . ? C15 C17 1.430(3) . ? C15 C16 1.499(3) . ? C17 C18 1.386(3) . ? C18 C19 1.403(4) . ? C19 C20 1.367(4) . ? C21 C22 1.355(4) . ? C22 C23 1.412(5) . ? C23 C24 1.357(4) . ? C25 C26 1.359(4) . ? C26 C27 1.415(5) . ? C27 C28 1.357(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Rh1 O1 81.81(7) . . ? O2 Rh1 P2 91.99(5) . . ? O1 Rh1 P2 171.60(5) . . ? O2 Rh1 P1 167.71(5) . . ? O1 Rh1 P1 87.71(5) . . ? P2 Rh1 P1 99.04(2) . . ? N3 P1 N2 103.33(10) . . ? N3 P1 N1 101.93(10) . . ? N2 P1 N1 99.30(9) . . ? N3 P1 Rh1 111.55(7) . . ? N2 P1 Rh1 127.08(7) . . ? N1 P1 Rh1 110.45(7) . . ? N5 P2 N6 101.42(10) . . ? N5 P2 N4 98.96(9) . . ? N6 P2 N4 103.98(10) . . ? N5 P2 Rh1 125.04(7) . . ? N6 P2 Rh1 113.56(7) . . ? N4 P2 Rh1 111.20(7) . . ? F1 P3 F2 92.03(17) . . ? F1 P3 F6 96.2(2) . . ? F2 P3 F6 90.83(16) . . ? F1 P3 F4 88.10(15) . . ? F2 P3 F4 179.62(17) . . ? F6 P3 F4 88.80(15) . . ? F1 P3 F3 175.28(18) . . ? F2 P3 F3 90.66(17) . . ? F6 P3 F3 87.59(18) . . ? F4 P3 F3 89.23(16) . . ? F1 P3 F5 87.28(18) . . ? F2 P3 F5 90.34(16) . . ? F6 P3 F5 176.24(18) . . ? F4 P3 F5 90.02(14) . . ? F3 P3 F5 88.82(14) . . ? C1 O1 Rh1 131.57(15) . . ? C15 O2 Rh1 133.74(15) . . ? C6 N1 C3 107.53(19) . . ? C6 N1 P1 126.67(17) . . ? C3 N1 P1 125.65(16) . . ? C7 N2 C10 107.74(19) . . ? C7 N2 P1 122.40(16) . . ? C10 N2 P1 128.10(16) . . ? C14 N3 C11 107.7(2) . . ? C14 N3 P1 122.78(17) . . ? C11 N3 P1 129.29(17) . . ? C20 N4 C17 107.35(19) . . ? C20 N4 P2 124.83(17) . . ? C17 N4 P2 127.16(16) . . ? C24 N5 C21 107.9(2) . . ? C24 N5 P2 128.54(18) . . ? C21 N5 P2 122.02(17) . . ? C25 N6 C28 107.4(2) . . ? C25 N6 P2 121.46(16) . . ? C28 N6 P2 129.37(18) . . ? O1 C1 C3 124.1(2) . . ? O1 C1 C2 116.9(2) . . ? C3 C1 C2 119.1(2) . . ? C4 C3 N1 107.2(2) . . ? C4 C3 C1 128.2(2) . . ? N1 C3 C1 124.5(2) . . ? C3 C4 C5 108.3(2) . . ? C6 C5 C4 107.7(2) . . ? C5 C6 N1 109.2(2) . . ? C8 C7 N2 108.4(2) . . ? C7 C8 C9 107.8(2) . . ? C10 C9 C8 108.2(2) . . ? C9 C10 N2 107.9(2) . . ? C12 C11 N3 107.6(2) . . ? C11 C12 C13 108.7(2) . . ? C14 C13 C12 107.9(2) . . ? C13 C14 N3 108.0(2) . . ? O2 C15 C17 124.5(2) . . ? O2 C15 C16 116.3(2) . . ? C17 C15 C16 119.2(2) . . ? C18 C17 N4 107.4(2) . . ? C18 C17 C15 127.1(2) . . ? N4 C17 C15 125.4(2) . . ? C17 C18 C19 108.1(2) . . ? C20 C19 C18 107.6(2) . . ? C19 C20 N4 109.5(2) . . ? C22 C21 N5 108.2(3) . . ? C21 C22 C23 107.7(3) . . ? C24 C23 C22 108.4(2) . . ? C23 C24 N5 107.7(3) . . ? C26 C25 N6 108.6(2) . . ? C25 C26 C27 107.4(2) . . ? C28 C27 C26 108.6(2) . . ? C27 C28 N6 108.0(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.178 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.077 #===END data_compound11_k00adb12 _database_code_CSD 211983 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H56 Cl2 N12 O4 P4 Rh2' _chemical_formula_weight 1361.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.408(4) _cell_length_b 9.2298(18) _cell_length_c 33.971(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.13(3) _cell_angle_gamma 90.00 _cell_volume 5739(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type multiscan #_exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_max 1.060 _exptl_absorpt_correction_T_min 0.954 _exptl_absorpt_process_details ; Sortav Blessing (1995) multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26128 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.72 _reflns_number_total 9154 _reflns_number_gt 6289 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1192P)^2^+8.3627P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9154 _refine_ls_number_parameters 725 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1733 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _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 0.06395(3) 0.97815(5) 0.221161(12) 0.02526(17) Uani 1 1 d . . . Rh2 Rh 0.34924(3) 0.78511(5) 0.031095(12) 0.02422(17) Uani 1 1 d . . . Cl1 Cl 0.15944(11) 0.89155(17) 0.26707(4) 0.0337(5) Uani 1 1 d . . . Cl2 Cl 0.38333(13) 0.87737(19) 0.09459(4) 0.0418(5) Uani 1 1 d . . . P1 P 0.23859(12) 0.76861(16) 0.04649(4) 0.0243(5) Uani 1 1 d . . . P2 P 0.33662(12) 0.70628(16) -0.02834(4) 0.0248(5) Uani 1 1 d . . . P3 P -0.00768(12) 1.08831(16) 0.17755(4) 0.0252(5) Uani 1 1 d . . . P4 P -0.01930(12) 0.88706(16) 0.25489(4) 0.0254(5) Uani 1 1 d . . . O1 O 0.2976(3) 0.4806(4) 0.06327(11) 0.0291(13) Uani 1 1 d . . . O2 O 0.4583(3) 0.8350(5) 0.02137(12) 0.0341(14) Uani 1 1 d . . . O3 O 0.1516(3) 1.0439(5) 0.19091(11) 0.0331(13) Uani 1 1 d . . . O4 O 0.0426(3) 0.6587(5) 0.21022(12) 0.0356(14) Uani 1 1 d . . . N1 N 0.2275(4) 0.7176(5) 0.09465(13) 0.0267(15) Uani 1 1 d . . . N2 N 0.1689(3) 0.6727(5) 0.02142(13) 0.0228(14) Uani 1 1 d . . . N3 N 0.1953(4) 0.9327(5) 0.04314(14) 0.0267(15) Uani 1 1 d . . . N4 N 0.2758(4) 0.5836(5) -0.04867(13) 0.0264(15) Uani 1 1 d . . . N5 N 0.3309(4) 0.8347(5) -0.06476(13) 0.0273(15) Uani 1 1 d . . . N6 N 0.4157(4) 0.6221(5) -0.03886(13) 0.0259(15) Uani 1 1 d . . . N7 N 0.0358(4) 1.2377(5) 0.15908(14) 0.0300(16) Uani 1 1 d . . . N8 N -0.0345(4) 0.9990(5) 0.13453(14) 0.0293(16) Uani 1 1 d . . . N9 N -0.0865(4) 1.1730(5) 0.18637(14) 0.0296(16) Uani 1 1 d . . . N10 N -0.1029(4) 0.8239(5) 0.23461(14) 0.0278(15) Uani 1 1 d . . . N11 N -0.0488(4) 1.0067(5) 0.28814(14) 0.0271(15) Uani 1 1 d . . . N12 N 0.0062(4) 0.7434(5) 0.28567(13) 0.0259(15) Uani 1 1 d . . . C1 C 0.1914(5) 0.7991(7) 0.12091(18) 0.041(2) Uani 1 1 d . . . H1 H 0.1589 0.8771 0.1139 0.049 Uiso 1 1 calc R . . C2 C 0.2102(6) 0.7486(8) 0.15876(18) 0.053(3) Uani 1 1 d . . . H2 H 0.1930 0.7848 0.1822 0.063 Uiso 1 1 calc R . . C3 C 0.2593(5) 0.6347(7) 0.15638(17) 0.033(2) Uani 1 1 d . . . H3 H 0.2813 0.5792 0.1780 0.040 Uiso 1 1 calc R . . C4 C 0.2705(4) 0.6165(6) 0.11696(16) 0.0259(17) Uani 1 1 d . . . C5 C 0.3087(4) 0.5034(6) 0.09901(16) 0.0259(17) Uani 1 1 d . . . C6 C 0.3647(5) 0.4179(7) 0.12477(18) 0.0346(19) Uani 1 1 d . . . H6A H 0.3715 0.3232 0.1126 0.052 Uiso 1 1 calc R . . H6B H 0.3480 0.4042 0.1509 0.052 Uiso 1 1 calc R . . H6C H 0.4112 0.4705 0.1275 0.052 Uiso 1 1 calc R . . C7 C 0.1351(4) 0.5490(6) 0.03310(18) 0.0297(19) Uani 1 1 d . . . H7 H 0.1441 0.5042 0.0583 0.036 Uiso 1 1 calc R . . C8 C 0.0875(5) 0.5018(7) 0.0030(2) 0.034(2) Uani 1 1 d . . . H8 H 0.0580 0.4175 0.0032 0.040 Uiso 1 1 calc R . . C9 C 0.0892(4) 0.5995(7) -0.02877(19) 0.0309(19) Uani 1 1 d . . . H9 H 0.0605 0.5938 -0.0537 0.037 Uiso 1 1 calc R . . C10 C 0.1389(4) 0.7024(6) -0.01737(17) 0.0278(18) Uani 1 1 d . . . H10 H 0.1515 0.7819 -0.0330 0.033 Uiso 1 1 calc R . . C11 C 0.2324(5) 1.0633(6) 0.04246(16) 0.0311(19) Uani 1 1 d . . . H11 H 0.2837 1.0748 0.0427 0.037 Uiso 1 1 calc R . . C12 C 0.1830(5) 1.1706(7) 0.04146(19) 0.036(2) Uani 1 1 d . . . H12 H 0.1931 1.2714 0.0407 0.043 Uiso 1 1 calc R . . C13 C 0.1135(5) 1.1075(7) 0.04166(18) 0.036(2) Uani 1 1 d . . . H13 H 0.0684 1.1581 0.0410 0.044 Uiso 1 1 calc R . . C14 C 0.1221(5) 0.9628(7) 0.04288(17) 0.034(2) Uani 1 1 d . . . H14 H 0.0841 0.8934 0.0435 0.040 Uiso 1 1 calc R . . C15 C 0.2460(4) 0.5708(7) -0.08799(16) 0.0327(19) Uani 1 1 d . . . H15 H 0.2483 0.6425 -0.1079 0.039 Uiso 1 1 calc R . . C16 C 0.2136(5) 0.4404(7) -0.09316(18) 0.036(2) Uani 1 1 d . . . H16 H 0.1890 0.4037 -0.1171 0.043 Uiso 1 1 calc R . . C17 C 0.2229(5) 0.3677(7) -0.05588(18) 0.034(2) Uani 1 1 d . . . H17 H 0.2051 0.2739 -0.0506 0.041 Uiso 1 1 calc R . . C18 C 0.2615(5) 0.4553(6) -0.02941(18) 0.033(2) Uani 1 1 d . . . H18 H 0.2762 0.4332 -0.0024 0.040 Uiso 1 1 calc R . . C19 C 0.3660(5) 0.8405(7) -0.09893(17) 0.035(2) Uani 1 1 d . . . H19 H 0.4012 0.7734 -0.1064 0.042 Uiso 1 1 calc R . . C20 C 0.3412(5) 0.9584(8) -0.11972(18) 0.042(2) Uani 1 1 d . . . H20 H 0.3559 0.9889 -0.1444 0.050 Uiso 1 1 calc R . . C21 C 0.2902(5) 1.0275(7) -0.09873(18) 0.039(2) Uani 1 1 d . . . H21 H 0.2643 1.1135 -0.1067 0.047 Uiso 1 1 calc R . . C22 C 0.2837(4) 0.9528(6) -0.06542(17) 0.0295(18) Uani 1 1 d . . . H22 H 0.2525 0.9763 -0.0458 0.035 Uiso 1 1 calc R . . C23 C 0.4208(5) 0.5075(7) -0.06457(17) 0.034(2) Uani 1 1 d . . . H23 H 0.3806 0.4566 -0.0779 0.041 Uiso 1 1 calc R . . C24 C 0.4923(5) 0.4791(7) -0.06784(18) 0.034(2) Uani 1 1 d . . . H24 H 0.5101 0.4043 -0.0834 0.041 Uiso 1 1 calc R . . C25 C 0.5352(5) 0.5779(7) -0.04450(18) 0.036(2) Uani 1 1 d . . . H25 H 0.5870 0.5835 -0.0415 0.043 Uiso 1 1 calc R . . C26 C 0.4879(5) 0.6653(7) -0.02671(17) 0.0296(18) Uani 1 1 d . . . C27 C 0.5036(5) 0.7798(7) 0.00192(19) 0.032(2) Uani 1 1 d . . . C28 C 0.5814(5) 0.8348(7) 0.0083(2) 0.041(2) Uani 1 1 d . . . H28A H 0.5908 0.8986 -0.0137 0.061 Uiso 1 1 calc R . . H28B H 0.6152 0.7525 0.0094 0.061 Uiso 1 1 calc R . . H28C H 0.5887 0.8888 0.0332 0.061 Uiso 1 1 calc R . . C29 C 0.0015(5) 1.3591(7) 0.14324(17) 0.037(2) Uani 1 1 d . . . H29 H -0.0486 1.3822 0.1439 0.045 Uiso 1 1 calc R . . C30 C 0.0514(5) 1.4417(8) 0.12629(19) 0.041(2) Uani 1 1 d . . . H30 H 0.0424 1.5325 0.1135 0.049 Uiso 1 1 calc R . . C31 C 0.1185(5) 1.3681(7) 0.13122(17) 0.039(2) Uani 1 1 d . . . H31 H 0.1629 1.3992 0.1220 0.047 Uiso 1 1 calc R . . C32 C 0.1085(5) 1.2445(7) 0.15151(16) 0.0292(19) Uani 1 1 d . . . C33 C 0.1636(5) 1.1407(7) 0.16700(17) 0.033(2) Uani 1 1 d . . . C34 C 0.2387(5) 1.1546(8) 0.15541(18) 0.044(2) Uani 1 1 d . . . H34A H 0.2666 1.2227 0.1733 0.066 Uiso 1 1 calc R . . H34B H 0.2365 1.1906 0.1282 0.066 Uiso 1 1 calc R . . H34C H 0.2627 1.0597 0.1571 0.066 Uiso 1 1 calc R . . C35 C -0.0359(5) 0.8508(7) 0.13209(18) 0.036(2) Uani 1 1 d . . . H35 H -0.0232 0.7858 0.1534 0.044 Uiso 1 1 calc R . . C36 C -0.0582(5) 0.8123(7) 0.09429(18) 0.043(2) Uani 1 1 d . . . H36 H -0.0645 0.7162 0.0845 0.052 Uiso 1 1 calc R . . C37 C -0.0706(5) 0.9425(7) 0.07176(17) 0.037(2) Uani 1 1 d . . . H37 H -0.0864 0.9493 0.0443 0.044 Uiso 1 1 calc R . . C38 C -0.0555(5) 1.0530(7) 0.09682(17) 0.036(2) Uani 1 1 d . . . H38 H -0.0587 1.1527 0.0899 0.043 Uiso 1 1 calc R . . C39 C -0.1548(5) 1.1747(7) 0.16456(18) 0.0331(19) Uani 1 1 d . . . H39 H -0.1675 1.1279 0.1399 0.040 Uiso 1 1 calc R . . C40 C -0.1997(5) 1.2547(7) 0.1847(2) 0.039(2) Uani 1 1 d . . . H40 H -0.2498 1.2737 0.1766 0.047 Uiso 1 1 calc R . . C41 C -0.1597(5) 1.3065(7) 0.22040(18) 0.037(2) Uani 1 1 d . . . H41 H -0.1780 1.3655 0.2400 0.044 Uiso 1 1 calc R . . C42 C -0.0915(5) 1.2558(7) 0.22077(17) 0.036(2) Uani 1 1 d . . . H42 H -0.0527 1.2730 0.2410 0.043 Uiso 1 1 calc R . . C43 C -0.1626(4) 0.9079(7) 0.21955(17) 0.0304(19) Uani 1 1 d . . . H43 H -0.1658 1.0104 0.2215 0.036 Uiso 1 1 calc R . . C44 C -0.2150(5) 0.8207(7) 0.20174(18) 0.038(2) Uani 1 1 d . . . H44 H -0.2613 0.8493 0.1892 0.045 Uiso 1 1 calc R . . C45 C -0.1870(5) 0.6775(7) 0.2056(2) 0.038(2) Uani 1 1 d . . . H45 H -0.2118 0.5923 0.1959 0.046 Uiso 1 1 calc R . . C46 C -0.1200(5) 0.6819(7) 0.22502(19) 0.034(2) Uani 1 1 d . . . H46 H -0.0892 0.6007 0.2312 0.041 Uiso 1 1 calc R . . C47 C -0.0030(5) 1.1126(7) 0.30606(16) 0.0306(19) Uani 1 1 d . . . H47 H 0.0453 1.1333 0.3002 0.037 Uiso 1 1 calc R . . C48 C -0.0392(5) 1.1813(8) 0.33327(18) 0.038(2) Uani 1 1 d . . . H48 H -0.0208 1.2595 0.3496 0.046 Uiso 1 1 calc R . . C49 C -0.1075(5) 1.1182(8) 0.33328(17) 0.040(2) Uani 1 1 d . . . H49 H -0.1440 1.1454 0.3497 0.048 Uiso 1 1 calc R . . C50 C -0.1134(5) 1.0103(7) 0.30565(17) 0.0293(19) Uani 1 1 d . . . H50 H -0.1544 0.9486 0.2995 0.035 Uiso 1 1 calc R . . C51 C 0.0229(5) 0.6125(7) 0.34131(19) 0.036(2) Uani 1 1 d . . . H51 H 0.0203 0.5792 0.3676 0.044 Uiso 1 1 calc R . . C52 C 0.0603(5) 0.5466(7) 0.31261(18) 0.037(2) Uani 1 1 d . . . H52 H 0.0887 0.4608 0.3162 0.045 Uiso 1 1 calc R . . C53 C 0.0493(5) 0.6251(6) 0.27856(17) 0.0294(19) Uani 1 1 d . . . C54 C 0.0720(5) 0.5960(7) 0.23926(18) 0.034(2) Uani 1 1 d . . . C55 C 0.1321(5) 0.4892(8) 0.2364(2) 0.049(3) Uani 1 1 d . . . H55A H 0.1372 0.4697 0.2084 0.073 Uiso 1 1 calc R . . H55B H 0.1206 0.3989 0.2495 0.073 Uiso 1 1 calc R . . H55C H 0.1780 0.5290 0.2492 0.073 Uiso 1 1 calc R . . C56 C -0.0093(5) 0.7344(7) 0.32451(17) 0.036(2) Uani 1 1 d . . . H56 H -0.0378 0.8018 0.3374 0.043 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 0.0303(5) 0.0242(3) 0.0204(2) 0.00124(17) -0.0012(2) -0.0006(2) Rh2 0.0281(5) 0.0217(3) 0.0216(2) -0.00121(17) -0.0032(2) -0.0010(2) Cl1 0.0321(16) 0.0390(9) 0.0279(7) 0.0023(6) -0.0059(7) -0.0003(8) Cl2 0.0444(18) 0.0485(10) 0.0301(8) -0.0127(7) -0.0066(7) -0.0114(9) P1 0.0315(16) 0.0201(7) 0.0207(7) 0.0009(6) 0.0004(7) 0.0012(8) P2 0.0258(15) 0.0258(8) 0.0215(7) 0.0011(6) -0.0028(6) 0.0020(8) P3 0.0285(16) 0.0241(8) 0.0218(7) 0.0026(6) -0.0020(7) -0.0018(8) P4 0.0310(16) 0.0233(8) 0.0205(7) 0.0035(6) -0.0042(7) -0.0001(8) O1 0.033(4) 0.030(2) 0.023(2) -0.0010(16) -0.0017(19) 0.000(2) O2 0.031(5) 0.031(2) 0.039(2) -0.004(2) 0.001(2) -0.003(2) O3 0.031(4) 0.039(3) 0.029(2) 0.0024(19) 0.001(2) -0.007(2) O4 0.048(5) 0.029(2) 0.028(2) -0.0006(18) -0.003(2) -0.003(2) N1 0.035(5) 0.026(3) 0.019(2) -0.0036(19) 0.001(2) 0.005(3) N2 0.017(5) 0.023(2) 0.027(2) 0.0020(19) -0.003(2) -0.003(2) N3 0.030(5) 0.020(3) 0.031(3) 0.0030(19) 0.004(2) 0.005(3) N4 0.033(5) 0.027(3) 0.019(2) 0.0009(19) -0.002(2) 0.000(3) N5 0.029(5) 0.027(3) 0.025(2) 0.004(2) -0.001(2) -0.002(3) N6 0.022(5) 0.030(3) 0.025(2) 0.003(2) -0.003(2) 0.000(3) N7 0.039(6) 0.024(3) 0.027(3) 0.003(2) 0.000(2) -0.009(3) N8 0.040(5) 0.024(3) 0.023(2) -0.002(2) 0.001(2) -0.001(3) N9 0.033(6) 0.029(3) 0.026(3) 0.006(2) 0.001(2) 0.003(3) N10 0.031(5) 0.024(3) 0.026(2) 0.003(2) -0.007(2) -0.003(3) N11 0.028(5) 0.028(3) 0.024(2) 0.002(2) -0.003(2) 0.001(3) N12 0.030(5) 0.027(3) 0.021(2) 0.0040(19) 0.001(2) -0.001(3) C1 0.052(8) 0.037(4) 0.034(3) 0.002(3) 0.011(3) 0.009(4) C2 0.097(10) 0.042(4) 0.022(3) -0.001(3) 0.019(4) 0.018(5) C3 0.040(7) 0.034(4) 0.027(3) -0.001(3) 0.007(3) 0.006(4) C4 0.025(6) 0.027(3) 0.024(3) 0.003(2) -0.003(3) 0.001(3) C5 0.029(6) 0.026(3) 0.021(3) 0.004(2) -0.002(3) -0.003(3) C6 0.028(7) 0.042(4) 0.034(3) 0.010(3) 0.001(3) 0.005(4) C7 0.029(7) 0.025(3) 0.035(3) 0.003(3) 0.002(3) 0.002(3) C8 0.022(7) 0.024(3) 0.053(4) 0.008(3) -0.003(3) 0.000(3) C9 0.021(6) 0.029(3) 0.040(3) -0.002(3) -0.008(3) 0.000(3) C10 0.029(6) 0.028(3) 0.027(3) 0.004(2) 0.005(3) 0.003(3) C11 0.041(7) 0.026(3) 0.028(3) -0.001(2) 0.009(3) -0.002(3) C12 0.046(8) 0.021(3) 0.043(4) -0.006(3) 0.012(4) 0.008(4) C13 0.042(7) 0.031(4) 0.036(3) 0.006(3) 0.004(3) 0.014(4) C14 0.038(7) 0.031(4) 0.032(3) 0.002(3) 0.004(3) 0.000(4) C15 0.033(6) 0.045(4) 0.017(3) 0.001(2) -0.008(3) 0.000(4) C16 0.036(7) 0.040(4) 0.030(3) -0.009(3) -0.006(3) -0.002(4) C17 0.033(7) 0.031(3) 0.037(3) -0.002(3) -0.002(3) -0.002(3) C18 0.043(7) 0.025(3) 0.030(3) 0.000(2) -0.004(3) 0.006(3) C19 0.039(7) 0.042(4) 0.026(3) 0.002(3) 0.010(3) 0.001(4) C20 0.046(8) 0.051(4) 0.027(3) 0.015(3) 0.004(3) -0.002(4) C21 0.054(8) 0.027(3) 0.035(3) 0.003(3) 0.004(3) 0.003(4) C22 0.030(6) 0.026(3) 0.030(3) 0.002(2) -0.006(3) 0.002(3) C23 0.047(7) 0.032(3) 0.022(3) 0.002(2) -0.001(3) 0.013(4) C24 0.033(7) 0.039(4) 0.030(3) 0.003(3) 0.000(3) 0.007(4) C25 0.032(7) 0.040(4) 0.034(3) 0.009(3) 0.001(3) 0.008(4) C26 0.029(6) 0.035(3) 0.025(3) 0.006(3) 0.002(3) 0.005(3) C27 0.028(7) 0.023(3) 0.041(4) 0.009(3) -0.008(3) -0.004(3) C28 0.020(7) 0.033(4) 0.069(5) 0.003(3) 0.001(4) -0.004(4) C29 0.050(7) 0.031(4) 0.031(3) 0.002(3) -0.001(3) -0.004(4) C30 0.053(8) 0.033(4) 0.034(3) 0.012(3) -0.002(3) -0.004(4) C31 0.052(8) 0.041(4) 0.024(3) 0.007(3) -0.005(3) -0.020(4) C32 0.032(7) 0.032(3) 0.023(3) -0.002(2) -0.001(3) -0.009(3) C33 0.045(7) 0.029(3) 0.024(3) -0.001(3) 0.000(3) -0.017(4) C34 0.047(8) 0.056(4) 0.030(3) 0.003(3) 0.003(3) -0.020(4) C35 0.046(7) 0.027(3) 0.034(3) 0.001(3) -0.008(3) 0.002(3) C36 0.065(8) 0.031(4) 0.031(3) -0.006(3) -0.007(3) -0.004(4) C37 0.042(7) 0.045(4) 0.021(3) 0.000(3) -0.008(3) 0.002(4) C38 0.045(7) 0.037(4) 0.024(3) 0.006(3) -0.002(3) 0.004(4) C39 0.027(7) 0.042(4) 0.029(3) 0.010(3) -0.004(3) 0.005(4) C40 0.029(7) 0.043(4) 0.045(4) 0.012(3) 0.004(4) 0.017(4) C41 0.043(8) 0.038(4) 0.029(3) 0.008(3) 0.003(3) 0.009(4) C42 0.055(8) 0.025(3) 0.026(3) 0.007(2) 0.001(3) -0.004(4) C43 0.026(6) 0.032(3) 0.032(3) 0.014(3) -0.003(3) -0.003(3) C44 0.030(7) 0.043(4) 0.038(4) 0.012(3) -0.011(3) -0.010(4) C45 0.029(7) 0.034(4) 0.049(4) -0.001(3) -0.009(3) -0.012(4) C46 0.031(7) 0.024(3) 0.045(4) 0.000(3) -0.007(3) -0.005(3) C47 0.032(6) 0.036(4) 0.021(3) 0.000(3) -0.005(3) -0.006(3) C48 0.045(8) 0.039(4) 0.028(3) -0.003(3) -0.003(3) 0.007(4) C49 0.046(8) 0.051(4) 0.023(3) 0.002(3) 0.007(3) 0.017(4) C50 0.025(6) 0.036(3) 0.026(3) 0.008(3) 0.002(3) 0.005(3) C51 0.037(7) 0.035(4) 0.036(3) 0.010(3) -0.001(3) -0.003(4) C52 0.045(7) 0.030(3) 0.035(3) 0.006(3) -0.003(3) 0.005(4) C53 0.032(6) 0.022(3) 0.033(3) 0.003(2) -0.002(3) -0.006(3) C54 0.046(7) 0.026(3) 0.030(3) 0.002(3) 0.002(3) -0.002(3) C55 0.057(8) 0.046(4) 0.042(4) -0.004(3) 0.000(4) 0.021(4) C56 0.046(7) 0.037(4) 0.025(3) 0.006(3) 0.003(3) -0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O3 2.093(5) . ? Rh1 P3 2.1332(18) . ? Rh1 P4 2.178(2) . ? Rh1 Cl1 2.3614(19) . ? Rh2 O2 2.120(6) . ? Rh2 P2 2.1353(15) . ? Rh2 P1 2.162(2) . ? Rh2 Cl2 2.3416(16) . ? P1 N2 1.710(6) . ? P1 N3 1.710(5) . ? P1 N1 1.735(5) . ? P2 N4 1.687(6) . ? P2 N5 1.708(5) . ? P2 N6 1.721(6) . ? P3 N9 1.703(7) . ? P3 N8 1.705(5) . ? P3 N7 1.745(6) . ? P4 N11 1.709(5) . ? P4 N10 1.720(6) . ? P4 N12 1.723(5) . ? O1 C5 1.228(7) . ? O2 C27 1.227(9) . ? O3 C33 1.243(7) . ? O4 C54 1.219(8) . ? N1 C1 1.389(8) . ? N1 C4 1.394(8) . ? N2 C7 1.378(8) . ? N2 C10 1.400(7) . ? N3 C14 1.375(10) . ? N3 C11 1.387(9) . ? N4 C18 1.391(8) . ? N4 C15 1.394(7) . ? N5 C19 1.389(8) . ? N5 C22 1.392(9) . ? N6 C23 1.381(8) . ? N6 C26 1.407(9) . ? N7 C29 1.368(9) . ? N7 C32 1.390(9) . ? N8 C35 1.370(8) . ? N8 C38 1.390(7) . ? N9 C39 1.388(9) . ? N9 C42 1.408(8) . ? N10 C46 1.378(8) . ? N10 C43 1.396(9) . ? N11 C50 1.385(9) . ? N11 C47 1.389(8) . ? N12 C56 1.382(8) . ? N12 C53 1.385(9) . ? C1 C2 1.377(9) . ? C2 C3 1.394(10) . ? C3 C4 1.387(8) . ? C4 C5 1.432(9) . ? C5 C6 1.503(9) . ? C7 C8 1.345(9) . ? C8 C9 1.410(9) . ? C9 C10 1.347(9) . ? C11 C12 1.343(10) . ? C12 C13 1.406(11) . ? C13 C14 1.345(9) . ? C15 C16 1.347(9) . ? C16 C17 1.427(9) . ? C17 C18 1.353(9) . ? C19 C20 1.350(9) . ? C20 C21 1.393(11) . ? C21 C22 1.341(9) . ? C23 C24 1.358(11) . ? C24 C25 1.397(10) . ? C25 C26 1.373(10) . ? C26 C27 1.444(9) . ? C27 C28 1.514(11) . ? C29 C30 1.368(11) . ? C30 C31 1.404(11) . ? C31 C32 1.356(9) . ? C32 C33 1.453(10) . ? C33 C34 1.483(11) . ? C35 C36 1.354(9) . ? C36 C37 1.430(9) . ? C37 C38 1.338(9) . ? C39 C40 1.349(10) . ? C40 C41 1.431(10) . ? C41 C42 1.339(11) . ? C43 C44 1.349(10) . ? C44 C45 1.420(10) . ? C45 C46 1.336(10) . ? C47 C48 1.353(10) . ? C48 C49 1.387(11) . ? C49 C50 1.365(9) . ? C51 C56 1.368(10) . ? C51 C52 1.392(10) . ? C52 C53 1.362(8) . ? C53 C54 1.465(9) . ? C54 C55 1.494(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Rh1 P3 88.42(14) . . ? O3 Rh1 P4 173.11(14) . . ? P3 Rh1 P4 97.58(7) . . ? O3 Rh1 Cl1 82.19(14) . . ? P3 Rh1 Cl1 168.95(7) . . ? P4 Rh1 Cl1 92.17(7) . . ? O2 Rh2 P2 86.33(13) . . ? O2 Rh2 P1 170.25(13) . . ? P2 Rh2 P1 101.22(8) . . ? O2 Rh2 Cl2 84.23(13) . . ? P2 Rh2 Cl2 170.52(9) . . ? P1 Rh2 Cl2 88.25(7) . . ? N2 P1 N3 96.1(3) . . ? N2 P1 N1 99.9(3) . . ? N3 P1 N1 101.7(2) . . ? N2 P1 Rh2 126.3(2) . . ? N3 P1 Rh2 111.5(2) . . ? N1 P1 Rh2 117.1(2) . . ? N4 P2 N5 100.5(3) . . ? N4 P2 N6 98.7(3) . . ? N5 P2 N6 98.7(3) . . ? N4 P2 Rh2 128.03(19) . . ? N5 P2 Rh2 116.14(18) . . ? N6 P2 Rh2 109.95(19) . . ? N9 P3 N8 101.4(3) . . ? N9 P3 N7 97.6(3) . . ? N8 P3 N7 100.1(2) . . ? N9 P3 Rh1 124.89(18) . . ? N8 P3 Rh1 117.8(2) . . ? N7 P3 Rh1 110.7(2) . . ? N11 P4 N10 98.6(3) . . ? N11 P4 N12 100.5(2) . . ? N10 P4 N12 99.0(3) . . ? N11 P4 Rh1 112.9(2) . . ? N10 P4 Rh1 124.75(18) . . ? N12 P4 Rh1 117.1(2) . . ? C27 O2 Rh2 134.6(5) . . ? C33 O3 Rh1 136.8(6) . . ? C1 N1 C4 107.2(5) . . ? C1 N1 P1 124.8(4) . . ? C4 N1 P1 125.2(5) . . ? C7 N2 C10 106.8(5) . . ? C7 N2 P1 128.5(4) . . ? C10 N2 P1 124.5(4) . . ? C14 N3 C11 107.9(6) . . ? C14 N3 P1 129.0(5) . . ? C11 N3 P1 123.0(6) . . ? C18 N4 C15 107.7(5) . . ? C18 N4 P2 122.0(4) . . ? C15 N4 P2 128.7(4) . . ? C19 N5 C22 107.5(5) . . ? C19 N5 P2 129.3(5) . . ? C22 N5 P2 123.1(5) . . ? C23 N6 C26 106.1(7) . . ? C23 N6 P2 126.4(6) . . ? C26 N6 P2 127.2(4) . . ? C29 N7 C32 107.7(6) . . ? C29 N7 P3 125.4(6) . . ? C32 N7 P3 126.1(5) . . ? C35 N8 C38 107.5(5) . . ? C35 N8 P3 122.4(4) . . ? C38 N8 P3 130.0(4) . . ? C39 N9 C42 107.6(7) . . ? C39 N9 P3 130.6(5) . . ? C42 N9 P3 121.8(6) . . ? C46 N10 C43 106.9(6) . . ? C46 N10 P4 126.0(5) . . ? C43 N10 P4 126.4(4) . . ? C50 N11 C47 107.7(6) . . ? C50 N11 P4 130.3(5) . . ? C47 N11 P4 121.6(5) . . ? C56 N12 C53 107.4(5) . . ? C56 N12 P4 123.7(5) . . ? C53 N12 P4 128.7(4) . . ? C2 C1 N1 109.1(6) . . ? C1 C2 C3 107.5(6) . . ? C4 C3 C2 108.1(6) . . ? C3 C4 N1 108.1(6) . . ? C3 C4 C5 129.0(6) . . ? N1 C4 C5 122.2(5) . . ? O1 C5 C4 120.6(6) . . ? O1 C5 C6 121.1(6) . . ? C4 C5 C6 118.2(5) . . ? C8 C7 N2 109.1(5) . . ? C7 C8 C9 108.0(6) . . ? C10 C9 C8 107.4(6) . . ? C9 C10 N2 108.7(5) . . ? C12 C11 N3 108.0(7) . . ? C11 C12 C13 108.0(6) . . ? C14 C13 C12 107.9(8) . . ? C13 C14 N3 108.2(7) . . ? C16 C15 N4 108.9(5) . . ? C15 C16 C17 107.1(6) . . ? C18 C17 C16 108.3(6) . . ? C17 C18 N4 108.0(5) . . ? C20 C19 N5 107.9(7) . . ? C19 C20 C21 108.1(6) . . ? C22 C21 C20 108.8(6) . . ? C21 C22 N5 107.8(7) . . ? C24 C23 N6 109.4(7) . . ? C23 C24 C25 108.8(7) . . ? C26 C25 C24 106.6(8) . . ? C25 C26 N6 109.1(6) . . ? C25 C26 C27 129.5(8) . . ? N6 C26 C27 121.3(7) . . ? O2 C27 C26 124.6(8) . . ? O2 C27 C28 118.1(6) . . ? C26 C27 C28 117.3(7) . . ? C30 C29 N7 108.6(8) . . ? C29 C30 C31 107.6(7) . . ? C32 C31 C30 107.6(8) . . ? C31 C32 N7 108.5(7) . . ? C31 C32 C33 127.7(8) . . ? N7 C32 C33 123.5(6) . . ? O3 C33 C32 123.0(8) . . ? O3 C33 C34 118.1(7) . . ? C32 C33 C34 118.8(6) . . ? C36 C35 N8 108.7(6) . . ? C35 C36 C37 107.6(6) . . ? C38 C37 C36 106.8(5) . . ? C37 C38 N8 109.3(6) . . ? C40 C39 N9 107.7(6) . . ? C39 C40 C41 109.0(8) . . ? C42 C41 C40 106.8(7) . . ? C41 C42 N9 109.0(7) . . ? C44 C43 N10 109.2(6) . . ? C43 C44 C45 106.2(7) . . ? C46 C45 C44 108.9(6) . . ? C45 C46 N10 108.7(7) . . ? C48 C47 N11 108.0(7) . . ? C47 C48 C49 108.5(7) . . ? C50 C49 C48 108.1(7) . . ? C49 C50 N11 107.7(7) . . ? C56 C51 C52 107.0(6) . . ? C53 C52 C51 108.8(6) . . ? C52 C53 N12 107.9(6) . . ? C52 C53 C54 130.2(7) . . ? N12 C53 C54 121.8(5) . . ? O4 C54 C53 120.3(7) . . ? O4 C54 C55 121.9(6) . . ? C53 C54 C55 117.8(6) . . ? C51 C56 N12 108.8(6) . . ? _diffrn_measured_fraction_theta_max 0.680 _diffrn_reflns_theta_full 27.72 _diffrn_measured_fraction_theta_full 0.680 _refine_diff_density_max 0.983 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.103