Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof. Helgard Raubenheimer' _publ_contact_author_address ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; _publ_contact_author_email hgr@sun.ac.za _publ_contact_author_phone '+27 21 808 3850' _publ_contact_author_fax '+27 21 808 3849' loop_ _publ_author_name _publ_author_address A.Neveling ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; H.G.Raubenheimer ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; S.Cronje ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; G.R.Julius ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; C.Esterhuysen ; Department of Chemistry University of Stellenbosch Private Bag X1 Matieland, 7602 South Africa ; _publ_section_title ; Thione complexes of Rh(I): a first comparison with the bonding and catalytic activity of related carbene and imine compounds. ; _publ_section_references ; Barbour, L. J. (1999). X-Seed. University of Stellenbosch, South Africa. Farrugia, L.J. (1997). J. Appl. Cryst. 30, 565. Nonius BV (1998) COLLECT. Data collection software. Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997) Methods Enzymol., 276, 307. Sheldrick, G.M. (1997). SHELX-97. Program for crystal structure analysis. Univ. of Gottingen, Germany. ; #========================================================================== data_1b _database_code_depnum_ccdc_archive 'CCDC 250303' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 Cl N2 Rh S' _chemical_formula_sum 'C15 H24 Cl N2 Rh S' _chemical_formula_weight 402.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 14.389(3) _cell_length_b 7.702(2) _cell_length_c 14.993(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.79(3) _cell_angle_gamma 90.00 _cell_volume 1632.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3740 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.330 _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 173(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 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 11509 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3740 _reflns_number_gt 3032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'X-Seed (Barbour, 1999)' _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^)+(0.0177P)^2^+0.3083P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 3740 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0517 _refine_ls_wR_factor_gt 0.0485 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.295901(11) 0.83556(2) 0.797247(11) 0.02047(6) Uani 1 1 d . . . Cl1 Cl 0.18845(4) 0.75334(7) 0.66341(4) 0.03009(14) Uani 1 1 d . . . S1 S 0.22325(4) 1.10870(7) 0.80426(4) 0.03145(15) Uani 1 1 d . . . N11 N 0.15619(12) 1.2197(2) 0.63009(12) 0.0242(4) Uani 1 1 d . . . N12 N 0.04839(12) 1.1006(2) 0.69172(11) 0.0200(4) Uani 1 1 d . . . C1 C 0.41697(15) 0.9233(3) 0.89009(15) 0.0280(5) Uani 1 1 d . . . C2 C 0.50679(15) 0.8271(3) 0.88136(15) 0.0306(5) Uani 1 1 d . . . H2A H 0.5255 0.7504 0.9347 0.037 Uiso 1 1 calc R . . H2B H 0.5584 0.9121 0.8811 0.037 Uiso 1 1 calc R . . C3 C 0.49436(16) 0.7179(3) 0.79461(16) 0.0342(6) Uani 1 1 d . . . H3A H 0.5117 0.7889 0.7451 0.041 Uiso 1 1 calc R . . H3B H 0.5380 0.6175 0.8049 0.041 Uiso 1 1 calc R . . C4 C 0.39445(16) 0.6526(3) 0.76555(16) 0.0270(5) Uani 1 1 d . . . C5 C 0.34032(16) 0.5729(3) 0.82164(15) 0.0286(5) Uani 1 1 d . . . C6 C 0.37731(17) 0.5334(3) 0.92096(16) 0.0375(6) Uani 1 1 d . . . H6A H 0.4464 0.5128 0.9301 0.045 Uiso 1 1 calc R . . H6B H 0.3472 0.4257 0.9377 0.045 Uiso 1 1 calc R . . C7 C 0.35786(17) 0.6807(3) 0.98353(16) 0.0383(6) Uani 1 1 d . . . H7A H 0.2981 0.6561 1.0048 0.046 Uiso 1 1 calc R . . H7B H 0.4094 0.6842 1.0374 0.046 Uiso 1 1 calc R . . C8 C 0.35035(17) 0.8563(3) 0.93773(15) 0.0309(6) Uani 1 1 d . . . C11 C 0.14122(15) 1.1395(2) 0.70580(15) 0.0230(5) Uani 1 1 d . . . C12 C 0.07189(15) 1.2325(3) 0.56776(14) 0.0241(5) Uani 1 1 d . . . C13 C 0.00402(15) 1.1583(3) 0.60657(14) 0.0219(5) Uani 1 1 d . . . C14 C 0.24807(16) 1.2780(3) 0.61396(17) 0.0386(6) Uani 1 1 d . . . H14A H 0.2967 1.2527 0.6675 0.058 Uiso 1 1 calc R . . H14B H 0.2460 1.4033 0.6025 0.058 Uiso 1 1 calc R . . H14C H 0.2633 1.2171 0.5611 0.058 Uiso 1 1 calc R . . C15 C 0.06654(18) 1.3195(3) 0.47863(16) 0.0370(6) Uani 1 1 d . . . H15A H 0.0025 1.3073 0.4429 0.055 Uiso 1 1 calc R . . H15B H 0.1120 1.2658 0.4459 0.055 Uiso 1 1 calc R . . H15C H 0.0816 1.4430 0.4882 0.055 Uiso 1 1 calc R . . C16 C -0.10000(15) 1.1422(3) 0.57511(15) 0.0306(5) Uani 1 1 d . . . H16A H -0.1328 1.2154 0.6128 0.046 Uiso 1 1 calc R . . H16B H -0.1190 1.0209 0.5801 0.046 Uiso 1 1 calc R . . H16C H -0.1168 1.1797 0.5117 0.046 Uiso 1 1 calc R . . C17 C 0.00194(16) 1.0029(3) 0.75383(15) 0.0300(5) Uani 1 1 d . . . H17A H 0.0483 0.9722 0.8081 0.045 Uiso 1 1 calc R . . H17B H -0.0256 0.8967 0.7239 0.045 Uiso 1 1 calc R . . H17C H -0.0482 1.0738 0.7714 0.045 Uiso 1 1 calc R . . H1 H 0.4190(15) 1.043(3) 0.8812(14) 0.036 Uiso 1 1 d . . . H4 H 0.3762(16) 0.638(3) 0.7014(16) 0.036 Uiso 1 1 d . . . H5 H 0.2907(15) 0.504(3) 0.7943(14) 0.036 Uiso 1 1 d . . . H8 H 0.3142(16) 0.935(3) 0.9632(15) 0.036 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01650(10) 0.02348(10) 0.02038(10) -0.00022(7) 0.00077(7) 0.00227(7) Cl1 0.0271(3) 0.0336(3) 0.0259(3) -0.0031(2) -0.0044(2) 0.0035(2) S1 0.0288(3) 0.0308(3) 0.0307(3) -0.0066(2) -0.0049(3) 0.0088(3) N11 0.0214(10) 0.0235(9) 0.0292(10) 0.0002(8) 0.0088(8) 0.0018(8) N12 0.0185(10) 0.0198(9) 0.0222(10) 0.0004(7) 0.0051(7) 0.0020(7) C1 0.0213(12) 0.0292(12) 0.0291(13) -0.0044(10) -0.0067(10) 0.0001(10) C2 0.0184(12) 0.0351(13) 0.0364(14) 0.0031(10) 0.0004(10) -0.0012(10) C3 0.0209(13) 0.0371(13) 0.0455(15) 0.0009(11) 0.0086(11) 0.0068(10) C4 0.0236(12) 0.0263(12) 0.0305(13) -0.0032(10) 0.0032(10) 0.0084(10) C5 0.0244(13) 0.0227(12) 0.0351(14) 0.0026(10) -0.0034(10) 0.0022(10) C6 0.0323(14) 0.0358(14) 0.0404(15) 0.0122(11) -0.0029(11) 0.0000(11) C7 0.0236(13) 0.0628(17) 0.0269(13) 0.0143(12) 0.0002(10) 0.0057(12) C8 0.0237(13) 0.0460(15) 0.0197(12) -0.0061(11) -0.0040(10) 0.0066(11) C11 0.0224(12) 0.0186(11) 0.0280(12) -0.0041(9) 0.0051(9) 0.0048(9) C12 0.0267(13) 0.0219(11) 0.0238(12) -0.0003(9) 0.0052(10) 0.0046(9) C13 0.0217(12) 0.0216(11) 0.0215(11) -0.0017(9) 0.0018(9) 0.0050(9) C14 0.0248(14) 0.0462(15) 0.0481(16) -0.0017(12) 0.0156(11) -0.0044(11) C15 0.0437(16) 0.0368(14) 0.0332(14) 0.0079(11) 0.0143(12) 0.0069(11) C16 0.0234(13) 0.0363(13) 0.0306(13) -0.0024(10) 0.0013(10) 0.0026(10) C17 0.0327(13) 0.0298(13) 0.0291(13) 0.0048(10) 0.0096(10) -0.0043(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 C8 2.111(2) . ? Rh1 C4 2.115(2) . ? Rh1 C1 2.126(2) . ? Rh1 C5 2.132(2) . ? Rh1 S1 2.3602(7) . ? Rh1 Cl1 2.3783(9) . ? S1 C11 1.725(2) . ? N11 C11 1.345(3) . ? N11 C12 1.389(3) . ? N11 C14 1.459(3) . ? N12 C11 1.346(3) . ? N12 C13 1.389(3) . ? N12 C17 1.454(3) . ? C1 C8 1.397(3) . ? C1 C2 1.516(3) . ? C1 H1 0.93(2) . ? C2 C3 1.531(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.508(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.391(3) . ? C4 H4 0.96(2) . ? C5 C6 1.515(3) . ? C5 H5 0.92(2) . ? C6 C7 1.531(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.511(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8 0.93(2) . ? C12 C13 1.354(3) . ? C12 C15 1.484(3) . ? C13 C16 1.488(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 C8 Rh1 C4 97.78(9) . . ? C8 Rh1 C1 38.49(9) . . ? C4 Rh1 C1 81.79(9) . . ? C8 Rh1 C5 81.80(9) . . ? C4 Rh1 C5 38.24(9) . . ? C1 Rh1 C5 90.38(9) . . ? C8 Rh1 S1 88.44(7) . . ? C4 Rh1 S1 157.65(7) . . ? C1 Rh1 S1 90.18(6) . . ? C5 Rh1 S1 163.53(7) . . ? C8 Rh1 Cl1 157.38(7) . . ? C4 Rh1 Cl1 89.44(7) . . ? C1 Rh1 Cl1 163.84(7) . . ? C5 Rh1 Cl1 91.07(6) . . ? S1 Rh1 Cl1 92.95(2) . . ? C11 S1 Rh1 108.81(7) . . ? C11 N11 C12 110.05(18) . . ? C11 N11 C14 125.08(19) . . ? C12 N11 C14 124.82(19) . . ? C11 N12 C13 110.17(17) . . ? C11 N12 C17 125.19(18) . . ? C13 N12 C17 124.54(18) . . ? C8 C1 C2 122.8(2) . . ? C8 C1 Rh1 70.18(13) . . ? C2 C1 Rh1 113.29(15) . . ? C8 C1 H1 118.7(14) . . ? C2 C1 H1 114.9(14) . . ? Rh1 C1 H1 105.3(13) . . ? C1 C2 C3 112.08(18) . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 112.45(19) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 125.7(2) . . ? C5 C4 Rh1 71.54(13) . . ? C3 C4 Rh1 110.84(14) . . ? C5 C4 H4 118.6(14) . . ? C3 C4 H4 113.4(14) . . ? Rh1 C4 H4 103.5(14) . . ? C4 C5 C6 123.3(2) . . ? C4 C5 Rh1 70.22(12) . . ? C6 C5 Rh1 113.45(15) . . ? C4 C5 H5 117.4(13) . . ? C6 C5 H5 115.0(14) . . ? Rh1 C5 H5 106.6(14) . . ? C5 C6 C7 112.48(19) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 113.0(2) . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C1 C8 C7 124.4(2) . . ? C1 C8 Rh1 71.33(13) . . ? C7 C8 Rh1 111.53(16) . . ? C1 C8 H8 117.5(15) . . ? C7 C8 H8 113.3(14) . . ? Rh1 C8 H8 109.2(14) . . ? N11 C11 N12 106.31(18) . . ? N11 C11 S1 126.41(17) . . ? N12 C11 S1 127.11(17) . . ? C13 C12 N11 106.87(18) . . ? C13 C12 C15 131.1(2) . . ? N11 C12 C15 122.0(2) . . ? C12 C13 N12 106.60(18) . . ? C12 C13 C16 131.5(2) . . ? N12 C13 C16 121.79(19) . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N12 C17 H17A 109.5 . . ? N12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.543 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.073 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 250304' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H19 Cl N Rh S' _chemical_formula_weight 335.69 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 7.26030(10) _cell_length_b 15.2871(2) _cell_length_c 11.67520(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.0180(10) _cell_angle_gamma 90.00 _cell_volume 1295.82(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5983 _cell_measurement_theta_max 29.58 _cell_measurement_theta_min 1.02 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.654 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8390 _exptl_absorpt_correction_T_max 0.8791 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 9994 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2826 _reflns_number_gt 2608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'X-Seed (Barbour, 1999)' _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^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0169(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2826 _refine_ls_number_parameters 141 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.223 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.26341(4) -0.287235(13) 0.07674(2) 0.02085(11) Uani 1 1 d . . . Cl1 Cl 0.29727(15) -0.39103(6) 0.22732(8) 0.0357(3) Uani 1 1 d . . . S1 S 0.23463(18) -0.39311(5) -0.07005(7) 0.0304(2) Uani 1 1 d . . . N11 N 0.2391(4) -0.56696(16) -0.0750(2) 0.0264(5) Uani 1 1 d . . . C1 C 0.3489(7) -0.1995(3) -0.0518(4) 0.0291(11) Uani 1 1 d . . . H1 H 0.3884 -0.2288 -0.1243 0.035 Uiso 1 1 calc R . . C2 C 0.4874(6) -0.1347(2) -0.0064(4) 0.0364(10) Uani 1 1 d . . . H2A H 0.4811 -0.0807 -0.0531 0.044 Uiso 1 1 calc R . . H2B H 0.6125 -0.1596 -0.0152 0.044 Uiso 1 1 calc R . . C3 C 0.4574(6) -0.1109(3) 0.1192(4) 0.0358(10) Uani 1 1 d . . . H3A H 0.3797 -0.0578 0.1238 0.043 Uiso 1 1 calc R . . H3B H 0.5777 -0.0972 0.1549 0.043 Uiso 1 1 calc R . . C4 C 0.3647(7) -0.1850(3) 0.1862(4) 0.0346(11) Uani 1 1 d . . . H4 H 0.4366 -0.2062 0.2538 0.041 Uiso 1 1 calc R . . C5 C 0.1756(8) -0.1923(3) 0.1981(4) 0.0384(12) Uani 1 1 d . . . H5 H 0.1372 -0.2181 0.2730 0.046 Uiso 1 1 calc R . . C6 C 0.0339(7) -0.1316(3) 0.1473(4) 0.0444(13) Uani 1 1 d . . . H6A H 0.0374 -0.0751 0.1888 0.053 Uiso 1 1 calc R . . H6B H -0.0901 -0.1572 0.1581 0.053 Uiso 1 1 calc R . . C7 C 0.0652(6) -0.1149(3) 0.0206(4) 0.0407(11) Uani 1 1 d . . . H7A H 0.1429 -0.0622 0.0115 0.049 Uiso 1 1 calc R . . H7B H -0.0548 -0.1031 -0.0166 0.049 Uiso 1 1 calc R . . C8 C 0.1588(7) -0.1925(3) -0.0403(4) 0.0280(10) Uani 1 1 d . . . H8 H 0.0868 -0.2174 -0.1056 0.034 Uiso 1 1 calc R . . C11 C 0.2494(5) -0.4953(2) -0.0159(3) 0.0272(7) Uani 1 1 d D . . H11 H 0.2668 -0.5007 0.0644 0.033 Uiso 1 1 calc RD . . C12 C 0.2528(6) -0.6530(2) -0.0200(3) 0.0376(8) Uani 1 1 d . . . H12A H 0.2535 -0.6457 0.0634 0.056 Uiso 1 1 calc R . . H12B H 0.3669 -0.6818 -0.0442 0.056 Uiso 1 1 calc R . . H12C H 0.1471 -0.6890 -0.0424 0.056 Uiso 1 1 calc R . . C13 C 0.2087(6) -0.5678(2) -0.1985(3) 0.0379(9) Uani 1 1 d . . . H13A H 0.0790 -0.5808 -0.2144 0.057 Uiso 1 1 calc R . . H13B H 0.2866 -0.6126 -0.2338 0.057 Uiso 1 1 calc R . . H13C H 0.2400 -0.5104 -0.2305 0.057 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 0.02428(16) 0.02024(15) 0.01802(15) -0.00017(8) 0.00087(16) -0.00096(10) Cl1 0.0495(7) 0.0338(4) 0.0239(4) 0.0084(4) -0.0032(4) -0.0052(4) S1 0.0477(5) 0.0200(4) 0.0233(4) -0.0018(3) -0.0041(5) 0.0013(4) N11 0.0255(13) 0.0209(11) 0.0328(14) 0.0005(10) 0.0014(17) 0.0005(11) C1 0.042(3) 0.0202(18) 0.025(3) 0.0075(15) 0.0052(18) 0.0002(15) C2 0.038(2) 0.027(2) 0.044(3) 0.0074(17) 0.0078(19) -0.0042(18) C3 0.038(2) 0.0270(18) 0.043(3) -0.0022(19) -0.0065(18) -0.0066(16) C4 0.049(3) 0.030(2) 0.025(2) -0.0072(19) -0.015(2) -0.003(2) C5 0.052(3) 0.036(2) 0.027(2) -0.0122(18) 0.011(2) -0.005(2) C6 0.038(2) 0.041(3) 0.054(3) -0.018(2) 0.007(2) 0.0101(19) C7 0.037(2) 0.0306(19) 0.055(3) -0.008(2) -0.009(2) 0.0088(18) C8 0.037(2) 0.0239(17) 0.023(2) -0.0007(15) -0.0115(16) 0.0041(16) C11 0.0272(17) 0.0281(14) 0.0264(16) 0.0004(12) 0.0007(17) 0.0019(16) C12 0.041(2) 0.0227(14) 0.049(2) 0.0061(14) 0.001(2) 0.0010(19) C13 0.047(2) 0.0324(16) 0.0340(19) -0.0079(14) -0.0062(19) 0.0013(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 2.107(4) . ? Rh1 C5 2.127(5) . ? Rh1 C8 2.131(4) . ? Rh1 C4 2.148(4) . ? Rh1 S1 2.3665(8) . ? Rh1 Cl1 2.3808(9) . ? S1 C11 1.688(3) . ? N11 C11 1.297(4) . ? N11 C13 1.459(4) . ? N11 C12 1.467(4) . ? C1 C8 1.391(6) . ? C1 C2 1.507(6) . ? C1 H1 1.0000 . ? C2 C3 1.527(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.532(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.384(7) . ? C4 H4 1.0000 . ? C5 C6 1.507(7) . ? C5 H5 1.0000 . ? C6 C7 1.518(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.540(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8 1.0000 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C5 97.4(2) . . ? C1 Rh1 C8 38.31(16) . . ? C5 Rh1 C8 81.72(16) . . ? C1 Rh1 C4 81.92(16) . . ? C5 Rh1 C4 37.78(19) . . ? C8 Rh1 C4 90.5(2) . . ? C1 Rh1 S1 86.89(12) . . ? C5 Rh1 S1 157.38(16) . . ? C8 Rh1 S1 88.25(13) . . ? C4 Rh1 S1 163.42(15) . . ? C1 Rh1 Cl1 156.94(15) . . ? C5 Rh1 Cl1 89.65(15) . . ? C8 Rh1 Cl1 164.39(15) . . ? C4 Rh1 Cl1 90.60(13) . . ? S1 Rh1 Cl1 95.05(3) . . ? C11 S1 Rh1 110.87(12) . . ? C11 N11 C13 122.8(3) . . ? C11 N11 C12 121.4(3) . . ? C13 N11 C12 115.8(3) . . ? C8 C1 C2 125.3(4) . . ? C8 C1 Rh1 71.8(3) . . ? C2 C1 Rh1 111.3(3) . . ? C8 C1 H1 113.7 . . ? C2 C1 H1 113.7 . . ? Rh1 C1 H1 113.7 . . ? C1 C2 C3 113.6(3) . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 112.1(3) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 123.1(5) . . ? C5 C4 Rh1 70.3(3) . . ? C3 C4 Rh1 112.6(3) . . ? C5 C4 H4 114.4 . . ? C3 C4 H4 114.4 . . ? Rh1 C4 H4 114.4 . . ? C4 C5 C6 126.0(5) . . ? C4 C5 Rh1 72.0(3) . . ? C6 C5 Rh1 111.3(3) . . ? C4 C5 H5 113.4 . . ? C6 C5 H5 113.4 . . ? Rh1 C5 H5 113.4 . . ? C5 C6 C7 112.6(4) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C6 C7 C8 112.8(4) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C1 C8 C7 122.8(5) . . ? C1 C8 Rh1 69.9(3) . . ? C7 C8 Rh1 112.6(3) . . ? C1 C8 H8 114.5 . . ? C7 C8 H8 114.5 . . ? Rh1 C8 H8 114.5 . . ? N11 C11 S1 125.4(2) . . ? N11 C11 H11 117.3 . . ? S1 C11 H11 117.3 . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N11 C13 H13A 109.5 . . ? N11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.234 _refine_diff_density_min -1.353 _refine_diff_density_rms 0.421 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 250305' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H36 N4 Rh1 1+, Cl 1-, C1 H2 Cl2, 0.50(H2 O1)' _chemical_formula_sum 'C23 H39 Cl3 N4 O0.50 Rh' _chemical_formula_weight 588.84 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' Rh Rh -1.1178 0.9187 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 26.8149(4) _cell_length_b 13.2815(3) _cell_length_c 18.8678(5) _cell_angle_alpha 90.00 _cell_angle_beta 126.8510(10) _cell_angle_gamma 90.00 _cell_volume 5377.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5231 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.02 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 0.953 _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 173(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 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 11822 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5296 _reflns_number_gt 3625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'X-Seed (Barbour, 1999)' _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^)+(0.0490P)^2^+1.2941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5296 _refine_ls_number_parameters 315 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.164960(12) 0.25681(2) 0.10926(2) 0.02171(11) Uani 1 1 d . . . Cl1 Cl 0.0000 0.01414(14) 0.7500 0.0531(5) Uani 1 2 d S A 1 O1 O 0.0482(4) 0.2197(6) 0.2837(6) 0.073(2) Uani 0.50 1 d PD . . H1A H 0.037(5) 0.284(3) 0.285(8) 0.087 Uiso 0.50 1 d PD . . H1B H 0.016(3) 0.178(7) 0.248(6) 0.087 Uiso 0.50 1 d PD . . C1 C 0.19840(17) 0.3949(3) 0.0888(3) 0.0292(10) Uani 1 1 d . . . H1 H 0.1648 0.4372 0.0387 0.035 Uiso 1 1 calc R . . Cl2 Cl 0.0000 0.44729(13) 0.2500 0.0646(6) Uani 1 2 d S B 2 C2 C 0.24994(19) 0.3671(3) 0.0819(3) 0.0401(11) Uani 1 1 d . . . H2A H 0.2755 0.4277 0.0943 0.048 Uiso 1 1 calc R . . H2B H 0.2311 0.3458 0.0204 0.048 Uiso 1 1 calc R . . Cl3 Cl 0.19222(7) 0.44993(12) 0.37236(10) 0.0807(5) Uani 1 1 d . C . C3 C 0.29252(18) 0.2831(3) 0.1449(3) 0.0379(11) Uani 1 1 d . . . H3A H 0.3114 0.2486 0.1198 0.045 Uiso 1 1 calc R . . H3B H 0.3267 0.3133 0.2022 0.045 Uiso 1 1 calc R . . Cl4 Cl 0.20933(9) 0.35131(13) 0.52105(13) 0.0717(7) Uani 0.807(4) 1 d P C 3 C4 C 0.25902(16) 0.2058(3) 0.1617(3) 0.0316(10) Uani 1 1 d . . . H4 H 0.2604 0.1360 0.1431 0.038 Uiso 1 1 calc R . . Cl5 Cl 0.1611(7) 0.2474(6) 0.3836(8) 0.116(5) Uani 0.193(4) 1 d P C 4 C5 C 0.25351(17) 0.2090(3) 0.2295(3) 0.0319(10) Uani 1 1 d . . . H5 H 0.2524 0.1414 0.2519 0.038 Uiso 1 1 calc R . . C6 C 0.27811(19) 0.2928(3) 0.2972(3) 0.0397(11) Uani 1 1 d . . . H6A H 0.3236 0.2837 0.3421 0.048 Uiso 1 1 calc R . . H6B H 0.2586 0.2870 0.3280 0.048 Uiso 1 1 calc R . . C7 C 0.26601(18) 0.3985(3) 0.2581(3) 0.0326(10) Uani 1 1 d . . . H7A H 0.2658 0.4470 0.2979 0.039 Uiso 1 1 calc R . . H7B H 0.3004 0.4175 0.2551 0.039 Uiso 1 1 calc R . . C8 C 0.20451(17) 0.4062(3) 0.1661(3) 0.0284(9) Uani 1 1 d . . . H8 H 0.1742 0.4546 0.1617 0.034 Uiso 1 1 calc R . . N11 N 0.03762(13) 0.3167(2) -0.0627(2) 0.0237(7) Uani 1 1 d . . . C11 C 0.07490(16) 0.3096(3) 0.0264(3) 0.0215(9) Uani 1 1 d . . . N12 N 0.03846(13) 0.3422(2) 0.0497(2) 0.0227(7) Uani 1 1 d . . . C12 C -0.02166(16) 0.3528(3) -0.0951(3) 0.0276(9) Uani 1 1 d . . . C13 C -0.02083(16) 0.3689(3) -0.0240(3) 0.0245(9) Uani 1 1 d . . . C14 C 0.05649(19) 0.2920(3) -0.1188(3) 0.0348(10) Uani 1 1 d . . . H14A H 0.1015 0.2795 -0.0817 0.052 Uiso 1 1 calc R . . H14B H 0.0464 0.3484 -0.1589 0.052 Uiso 1 1 calc R . . H14C H 0.0343 0.2316 -0.1536 0.052 Uiso 1 1 calc R . . C15 C -0.07152(18) 0.3655(3) -0.1918(3) 0.0382(11) Uani 1 1 d . . . H15A H -0.1103 0.3862 -0.2015 0.057 Uiso 1 1 calc R . . H15B H -0.0782 0.3015 -0.2222 0.057 Uiso 1 1 calc R . . H15C H -0.0589 0.4171 -0.2153 0.057 Uiso 1 1 calc R . . C16 C -0.06985(18) 0.4060(3) -0.0162(3) 0.0391(11) Uani 1 1 d . . . H16A H -0.0595 0.4743 0.0082 0.059 Uiso 1 1 calc R . . H16B H -0.0720 0.3613 0.0232 0.059 Uiso 1 1 calc R . . H16C H -0.1102 0.4065 -0.0749 0.059 Uiso 1 1 calc R . . C17 C 0.05893(19) 0.3537(3) 0.1407(3) 0.0347(10) Uani 1 1 d . . . H17A H 0.0339 0.3100 0.1501 0.052 Uiso 1 1 calc R . . H17B H 0.0536 0.4240 0.1509 0.052 Uiso 1 1 calc R . . H17C H 0.1030 0.3349 0.1821 0.052 Uiso 1 1 calc R . . N21 N 0.12165(13) 0.0466(2) 0.0265(2) 0.0273(8) Uani 1 1 d . . . C21 C 0.12966(16) 0.1136(3) 0.0860(3) 0.0251(9) Uani 1 1 d . . . N22 N 0.10557(14) 0.0661(2) 0.1233(2) 0.0278(8) Uani 1 1 d . . . C22 C 0.09192(17) -0.0410(3) 0.0247(3) 0.0318(10) Uani 1 1 d . . . C23 C 0.08187(18) -0.0289(3) 0.0858(3) 0.0334(10) Uani 1 1 d . . . C24 C 0.14137(19) 0.0615(3) -0.0303(3) 0.0368(11) Uani 1 1 d . . . H24A H 0.1598 0.1287 -0.0198 0.055 Uiso 1 1 calc R . . H24B H 0.1052 0.0555 -0.0926 0.055 Uiso 1 1 calc R . . H24C H 0.1723 0.0104 -0.0166 0.055 Uiso 1 1 calc R . . C25 C 0.0775(2) -0.1269(3) -0.0352(3) 0.0523(13) Uani 1 1 d . . . H25A H 0.0535 -0.1775 -0.0297 0.078 Uiso 1 1 calc R . . H25B H 0.1165 -0.1569 -0.0190 0.078 Uiso 1 1 calc R . . H25C H 0.0531 -0.1028 -0.0965 0.078 Uiso 1 1 calc R . . C26 C 0.05152(19) -0.0948(3) 0.1135(3) 0.0461(13) Uani 1 1 d . . . H26A H 0.0329 -0.1531 0.0738 0.069 Uiso 1 1 calc R . . H26B H 0.0190 -0.0568 0.1105 0.069 Uiso 1 1 calc R . . H26C H 0.0827 -0.1179 0.1743 0.069 Uiso 1 1 calc R . . C27 C 0.1089(2) 0.1049(3) 0.1979(3) 0.0469(13) Uani 1 1 d . . . H27A H 0.1288 0.1713 0.2145 0.070 Uiso 1 1 calc R . . H27B H 0.1334 0.0587 0.2483 0.070 Uiso 1 1 calc R . . H27C H 0.0667 0.1109 0.1815 0.070 Uiso 1 1 calc R . . C31 C 0.1604(3) 0.3681(4) 0.4074(4) 0.0737(17) Uani 1 1 d . . . H51A H 0.1200 0.3952 0.3896 0.088 Uiso 1 1 calc R C 3 H51B H 0.1524 0.3021 0.3779 0.088 Uiso 1 1 calc R C 3 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 0.01537(16) 0.01967(18) 0.02280(19) 0.00015(13) 0.00754(14) 0.00006(13) Cl1 0.0469(10) 0.0653(12) 0.0303(10) 0.000 0.0141(9) 0.000 O1 0.081(6) 0.058(5) 0.075(6) 0.014(5) 0.044(5) 0.000(4) C1 0.019(2) 0.023(2) 0.036(3) 0.0065(18) 0.011(2) -0.0007(17) Cl2 0.0999(15) 0.0438(10) 0.1041(17) 0.000 0.0901(15) 0.000 C2 0.036(3) 0.041(3) 0.046(3) 0.001(2) 0.026(2) -0.004(2) Cl3 0.0695(10) 0.1014(12) 0.0632(10) 0.0044(8) 0.0355(9) -0.0325(9) C3 0.021(2) 0.048(3) 0.040(3) -0.003(2) 0.016(2) -0.0007(19) Cl4 0.0944(15) 0.0654(12) 0.0770(15) 0.0192(10) 0.0630(13) 0.0202(10) C4 0.013(2) 0.030(2) 0.036(3) -0.0024(19) 0.006(2) 0.0064(17) Cl5 0.195(13) 0.069(6) 0.103(8) 0.001(5) 0.100(9) -0.021(6) C5 0.020(2) 0.025(2) 0.029(3) 0.0067(19) 0.003(2) 0.0036(17) C6 0.029(2) 0.041(3) 0.030(3) -0.002(2) 0.008(2) -0.003(2) C7 0.027(2) 0.029(2) 0.030(3) -0.0031(18) 0.011(2) -0.0031(18) C8 0.024(2) 0.019(2) 0.033(3) -0.0037(18) 0.012(2) -0.0018(16) N11 0.0218(17) 0.0249(18) 0.021(2) 0.0020(14) 0.0109(16) -0.0004(14) C11 0.020(2) 0.016(2) 0.030(3) -0.0016(17) 0.015(2) -0.0023(16) N12 0.0211(17) 0.0189(17) 0.025(2) 0.0016(14) 0.0125(16) 0.0006(13) C12 0.0135(19) 0.022(2) 0.034(3) 0.0022(18) 0.0077(19) -0.0015(16) C13 0.017(2) 0.017(2) 0.032(3) 0.0029(17) 0.011(2) -0.0013(15) C14 0.035(2) 0.038(2) 0.030(3) 0.004(2) 0.018(2) 0.005(2) C15 0.029(2) 0.033(2) 0.030(3) 0.003(2) 0.006(2) -0.0059(19) C16 0.025(2) 0.031(2) 0.065(3) 0.007(2) 0.029(2) 0.0022(19) C17 0.039(3) 0.034(2) 0.035(3) 0.001(2) 0.025(2) 0.005(2) N21 0.0214(17) 0.0231(18) 0.025(2) -0.0004(15) 0.0071(16) -0.0017(14) C21 0.020(2) 0.021(2) 0.026(2) 0.0013(18) 0.0092(19) 0.0027(16) N22 0.0237(18) 0.0237(18) 0.032(2) 0.0037(15) 0.0148(17) 0.0035(14) C22 0.021(2) 0.018(2) 0.034(3) 0.0026(18) 0.004(2) -0.0011(17) C23 0.021(2) 0.021(2) 0.042(3) 0.007(2) 0.010(2) 0.0013(17) C24 0.038(3) 0.034(2) 0.035(3) -0.007(2) 0.020(2) -0.003(2) C25 0.056(3) 0.036(3) 0.035(3) -0.005(2) 0.012(3) -0.011(2) C26 0.031(3) 0.031(3) 0.064(4) 0.019(2) 0.022(3) 0.002(2) C27 0.064(3) 0.033(3) 0.064(4) 0.006(2) 0.049(3) 0.006(2) C31 0.076(4) 0.075(4) 0.074(5) 0.000(3) 0.047(4) -0.018(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 C21 2.051(4) . ? Rh1 C11 2.059(3) . ? Rh1 C5 2.174(4) . ? Rh1 C1 2.175(4) . ? Rh1 C4 2.192(3) . ? Rh1 C8 2.202(4) . ? O1 H1A 0.91(2) . ? O1 H1B 0.90(2) . ? C1 C8 1.375(5) . ? C1 C2 1.510(5) . ? C1 H1 1.0000 . ? C2 C3 1.527(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? Cl3 C31 1.740(5) . ? C3 C4 1.518(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? Cl4 C31 1.730(6) . ? C4 C5 1.374(6) . ? C4 H4 1.0000 . ? Cl5 C31 1.668(10) . ? C5 C6 1.516(6) . ? C5 H5 1.0000 . ? C6 C7 1.528(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.520(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8 1.0000 . ? N11 C11 1.349(4) . ? N11 C12 1.402(4) . ? N11 C14 1.458(5) . ? C11 N12 1.361(4) . ? N12 C13 1.392(4) . ? N12 C17 1.464(5) . ? C12 C13 1.344(5) . ? C12 C15 1.489(5) . ? C13 C16 1.491(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N21 C21 1.346(5) . ? N21 C22 1.399(5) . ? N21 C24 1.466(5) . ? C21 N22 1.362(4) . ? N22 C23 1.399(5) . ? N22 C27 1.451(5) . ? C22 C23 1.340(6) . ? C22 C25 1.485(6) . ? C23 C26 1.488(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 H51A 0.9900 . ? C31 H51B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Rh1 C11 88.44(13) . . ? C21 Rh1 C5 91.58(15) . . ? C11 Rh1 C5 160.29(16) . . ? C21 Rh1 C1 158.49(16) . . ? C11 Rh1 C1 89.92(14) . . ? C5 Rh1 C1 97.06(15) . . ? C21 Rh1 C4 93.93(15) . . ? C11 Rh1 C4 162.93(15) . . ? C5 Rh1 C4 36.67(15) . . ? C1 Rh1 C4 81.70(15) . . ? C21 Rh1 C8 164.88(15) . . ? C11 Rh1 C8 93.77(14) . . ? C5 Rh1 C8 81.34(15) . . ? C1 Rh1 C8 36.60(14) . . ? C4 Rh1 C8 88.34(15) . . ? H1A O1 H1B 114(10) . . ? C8 C1 C2 125.8(4) . . ? C8 C1 Rh1 72.8(2) . . ? C2 C1 Rh1 107.8(2) . . ? C8 C1 H1 114.1 . . ? C2 C1 H1 114.1 . . ? Rh1 C1 H1 114.1 . . ? C1 C2 C3 114.0(3) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 113.4(3) . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 125.5(4) . . ? C5 C4 Rh1 70.9(2) . . ? C3 C4 Rh1 111.2(3) . . ? C5 C4 H4 113.8 . . ? C3 C4 H4 113.8 . . ? Rh1 C4 H4 113.8 . . ? C4 C5 C6 125.0(4) . . ? C4 C5 Rh1 72.4(2) . . ? C6 C5 Rh1 108.4(3) . . ? C4 C5 H5 114.3 . . ? C6 C5 H5 114.3 . . ? Rh1 C5 H5 114.3 . . ? C5 C6 C7 114.1(4) . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C6 112.6(3) . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C1 C8 C7 124.2(4) . . ? C1 C8 Rh1 70.6(2) . . ? C7 C8 Rh1 111.8(2) . . ? C1 C8 H8 114.1 . . ? C7 C8 H8 114.1 . . ? Rh1 C8 H8 114.1 . . ? C11 N11 C12 111.4(3) . . ? C11 N11 C14 124.7(3) . . ? C12 N11 C14 123.9(3) . . ? N11 C11 N12 104.0(3) . . ? N11 C11 Rh1 128.7(2) . . ? N12 C11 Rh1 127.3(3) . . ? C11 N12 C13 111.6(3) . . ? C11 N12 C17 125.2(3) . . ? C13 N12 C17 123.1(3) . . ? C13 C12 N11 106.5(3) . . ? C13 C12 C15 132.0(4) . . ? N11 C12 C15 121.5(4) . . ? C12 C13 N12 106.4(3) . . ? C12 C13 C16 131.5(4) . . ? N12 C13 C16 122.1(4) . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N12 C17 H17A 109.5 . . ? N12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 N21 C22 111.9(3) . . ? C21 N21 C24 125.0(3) . . ? C22 N21 C24 123.0(3) . . ? N21 C21 N22 103.7(3) . . ? N21 C21 Rh1 127.9(3) . . ? N22 C21 Rh1 128.4(3) . . ? C21 N22 C23 111.6(3) . . ? C21 N22 C27 124.3(3) . . ? C23 N22 C27 123.8(3) . . ? C23 C22 N21 106.5(3) . . ? C23 C22 C25 130.7(4) . . ? N21 C22 C25 122.7(4) . . ? C22 C23 N22 106.2(3) . . ? C22 C23 C26 131.7(4) . . ? N22 C23 C26 122.1(4) . . ? N21 C24 H24A 109.5 . . ? N21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N22 C27 H27A 109.5 . . ? N22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Cl5 C31 Cl4 95.0(5) . . ? Cl5 C31 Cl3 114.2(5) . . ? Cl4 C31 Cl3 111.8(3) . . ? Cl5 C31 H51A 116.5 . . ? Cl4 C31 H51A 109.3 . . ? Cl3 C31 H51A 109.3 . . ? Cl5 C31 H51B 14.5 . . ? Cl4 C31 H51B 109.3 . . ? Cl3 C31 H51B 109.3 . . ? H51A C31 H51B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.180 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.095 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 250306' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C19 H28 N4 Rh1), C1 H2 Cl2, 2(P1 F6)' _chemical_formula_sum 'C39 H58 Cl2 F12 N8 P2 Rh2' _chemical_formula_weight 1205.59 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.8475(2) _cell_length_b 17.4778(2) _cell_length_c 17.5446(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4859.49(10) _cell_formula_units_Z 4 _cell_measurement_temperature 203 _cell_measurement_reflns_used 22001 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.02 _exptl_crystal_description prism _exptl_crystal_colour orange?? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 0.940 _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 203(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 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 35432 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9504 _reflns_number_gt 6859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'X-Seed (Barbour, 1999)' _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^)+(0.0281P)^2^+1.5609P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00099(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.24(3) _chemical_absolute_configuration unk _refine_ls_number_reflns 9504 _refine_ls_number_parameters 641 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.003 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 1.036489(16) 0.99918(2) 0.207485(14) 0.02798(9) Uani 1 1 d . . . Rh2 Rh 0.530215(17) 0.50289(2) 0.212488(15) 0.03082(9) Uani 1 1 d . . . Cl1 Cl 0.17961(9) 0.81954(9) 0.47955(9) 0.0850(5) Uani 1 1 d . . . Cl2 Cl 0.18931(10) 0.98272(9) 0.50636(10) 0.0987(5) Uani 1 1 d . . . P1 P 0.87183(6) 0.87740(5) 0.49403(7) 0.0336(2) Uani 1 1 d . . . P2 P 0.71178(7) 0.19791(7) 0.49304(8) 0.0503(3) Uani 1 1 d . . . F11 F 0.8622(2) 0.88781(17) 0.40445(15) 0.0743(9) Uani 1 1 d . . . F12 F 0.79843(16) 0.93687(16) 0.5052(2) 0.0784(8) Uani 1 1 d . . . F13 F 0.80703(17) 0.80867(16) 0.4905(2) 0.0870(10) Uani 1 1 d . . . F14 F 0.8812(2) 0.8656(2) 0.58243(16) 0.0943(12) Uani 1 1 d . . . F15 F 0.94603(16) 0.81780(14) 0.48123(16) 0.0678(8) Uani 1 1 d . . . F16 F 0.93706(16) 0.94546(14) 0.4973(2) 0.0803(9) Uani 1 1 d . . . F21 F 0.7276(2) 0.1827(3) 0.57966(18) 0.1361(19) Uani 1 1 d . . . F22 F 0.7154(18) 0.1147(5) 0.4859(12) 0.170(9) Uani 0.54(3) 1 d P . . F23 F 0.6946(2) 0.2142(3) 0.40683(18) 0.1110(14) Uani 1 1 d . . . F24 F 0.668(2) 0.124(2) 0.460(3) 0.134(19) Uani 0.23(3) 1 d P . . F25 F 0.6178(4) 0.2138(11) 0.5162(4) 0.099(4) Uani 0.80(4) 1 d P . . F26 F 0.6978(18) 0.2898(12) 0.4947(12) 0.101(9) Uani 0.36(3) 1 d P . . F27 F 0.8080(4) 0.2091(13) 0.4742(6) 0.102(6) Uani 0.61(3) 1 d P . . F28 F 0.7416(19) 0.2762(14) 0.5121(11) 0.165(11) Uani 0.60(4) 1 d P . . F29 F 0.785(2) 0.142(3) 0.4759(9) 0.157(17) Uani 0.48(3) 1 d P . . F210 F 0.641(3) 0.251(3) 0.505(2) 0.036(13) Uiso 0.11(3) 1 d P . . F211 F 0.636(2) 0.136(3) 0.4950(17) 0.13(2) Uani 0.27(3) 1 d P . . N11 N 0.8746(2) 1.0813(2) 0.1581(2) 0.0451(10) Uani 1 1 d . . . N12 N 0.8869(2) 1.08138(18) 0.27903(19) 0.0381(8) Uani 1 1 d . . . N21 N 1.1089(2) 1.15819(19) 0.17122(19) 0.0382(8) Uani 1 1 d . . . N22 N 1.0939(2) 1.14183(18) 0.2914(2) 0.0379(8) Uani 1 1 d . . . N41 N 0.5523(2) 0.39258(19) 0.34589(18) 0.0347(8) Uani 1 1 d . . . N42 N 0.4247(2) 0.4303(2) 0.33889(19) 0.0360(9) Uani 1 1 d . . . N51 N 0.5164(2) 0.3503(2) 0.12558(18) 0.0391(9) Uani 1 1 d . . . N52 N 0.3956(2) 0.4004(2) 0.14612(19) 0.0417(9) Uani 1 1 d . . . C1 C 0.9860(3) 0.8841(2) 0.2347(3) 0.0423(11) Uani 1 1 d . . . H1 H 0.9412 0.9066 0.2607 0.051 Uiso 1 1 calc R . . C2 C 1.0501(3) 0.8430(3) 0.2813(3) 0.0563(13) Uani 1 1 d . . . H2A H 1.0415 0.7885 0.2742 0.068 Uiso 1 1 calc R . . H2B H 1.0391 0.8542 0.3345 0.068 Uiso 1 1 calc R . . C3 C 1.1413(3) 0.8601(3) 0.2656(3) 0.0583(13) Uani 1 1 d . . . H3A H 1.1631 0.8222 0.2304 0.070 Uiso 1 1 calc R . . H3B H 1.1728 0.8555 0.3128 0.070 Uiso 1 1 calc R . . C4 C 1.1565(2) 0.9398(2) 0.2322(2) 0.0398(10) Uani 1 1 d . . . H4 H 1.1689 0.9793 0.2659 0.048 Uiso 1 1 calc R . . C5 C 1.1529(3) 0.9571(2) 0.1564(2) 0.0376(10) Uani 1 1 d . . . H5 H 1.1655 1.0072 0.1428 0.045 Uiso 1 1 calc R . . C6 C 1.1311(3) 0.9038(3) 0.0935(3) 0.0618(14) Uani 1 1 d . . . H6A H 1.1785 0.8697 0.0851 0.074 Uiso 1 1 calc R . . H6B H 1.1232 0.9334 0.0472 0.074 Uiso 1 1 calc R . . C7 C 1.0538(4) 0.8563(3) 0.1062(3) 0.0638(15) Uani 1 1 d . . . H7A H 1.0709 0.8079 0.1283 0.077 Uiso 1 1 calc R . . H7B H 1.0285 0.8453 0.0570 0.077 Uiso 1 1 calc R . . C8 C 0.9871(3) 0.8918(2) 0.1570(3) 0.0453(11) Uani 1 1 d . . . H58 H 0.9446 0.9204 0.1342 0.054 Uiso 1 1 calc R . . C11 C 0.9233(2) 1.0541(2) 0.2149(2) 0.0364(9) Uani 1 1 d . . . C12 C 0.8088(3) 1.1252(3) 0.1872(3) 0.0590(13) Uani 1 1 d . . . H12 H 0.7675 1.1503 0.1591 0.071 Uiso 1 1 calc R . . C13 C 0.8159(3) 1.1246(3) 0.2615(3) 0.0596(14) Uani 1 1 d . . . H13 H 0.7801 1.1485 0.2961 0.071 Uiso 1 1 calc R . . C14 C 0.8880(3) 1.0660(3) 0.0772(3) 0.0722(16) Uani 1 1 d . . . H14A H 0.9347 1.0316 0.0712 0.108 Uiso 1 1 calc R . . H14B H 0.9000 1.1131 0.0512 0.108 Uiso 1 1 calc R . . H14C H 0.8381 1.0433 0.0559 0.108 Uiso 1 1 calc R . . C15 C 0.9163(3) 1.0638(3) 0.3557(3) 0.0562(14) Uani 1 1 d . . . H15A H 0.9413 1.0131 0.3551 0.067 Uiso 1 1 calc R . . H15B H 0.8676 1.0618 0.3892 0.067 Uiso 1 1 calc R . . C21 C 1.0845(2) 1.1051(2) 0.2233(2) 0.0319(9) Uani 1 1 d . . . C22 C 1.1330(3) 1.2258(2) 0.2074(3) 0.0485(11) Uani 1 1 d . . . H22 H 1.1522 1.2701 0.1838 0.058 Uiso 1 1 calc R . . C23 C 1.1237(3) 1.2152(2) 0.2808(3) 0.0498(12) Uani 1 1 d . . . H23 H 1.1351 1.2507 0.3189 0.060 Uiso 1 1 calc R . . C24 C 1.1052(3) 1.1456(3) 0.0895(3) 0.0593(15) Uani 1 1 d . . . H24A H 1.0964 1.0922 0.0796 0.089 Uiso 1 1 calc R . . H24B H 1.1573 1.1617 0.0667 0.089 Uiso 1 1 calc R . . H24C H 1.0594 1.1746 0.0683 0.089 Uiso 1 1 calc R . . C25 C 1.0722(3) 1.1087(3) 0.3652(2) 0.0462(12) Uani 1 1 d . . . H25A H 1.1084 1.1312 0.4036 0.055 Uiso 1 1 calc R . . H25B H 1.0844 1.0543 0.3636 0.055 Uiso 1 1 calc R . . C26 C 0.9803(3) 1.1192(3) 0.3900(2) 0.0543(13) Uani 1 1 d . . . H26A H 0.9777 1.1146 0.4450 0.065 Uiso 1 1 calc R . . H26B H 0.9631 1.1709 0.3770 0.065 Uiso 1 1 calc R . . C31 C 0.5308(3) 0.6110(3) 0.2771(3) 0.0511(12) Uani 1 1 d . . . H31 H 0.4974 0.5896 0.3151 0.061 Uiso 1 1 calc R . . C32 C 0.4906(3) 0.6706(3) 0.2266(3) 0.0706(16) Uani 1 1 d . . . H32A H 0.5073 0.7208 0.2446 0.085 Uiso 1 1 calc R . . H32B H 0.4298 0.6669 0.2317 0.085 Uiso 1 1 calc R . . C33 C 0.5134(4) 0.6641(3) 0.1417(3) 0.0759(19) Uani 1 1 d . . . H33A H 0.4692 0.6879 0.1117 0.091 Uiso 1 1 calc R . . H33B H 0.5652 0.6922 0.1325 0.091 Uiso 1 1 calc R . . C34 C 0.5249(4) 0.5830(3) 0.1153(3) 0.0603(15) Uani 1 1 d . . . H34 H 0.4774 0.5562 0.0990 0.072 Uiso 1 1 calc R . . C35 C 0.6005(3) 0.5465(3) 0.1137(2) 0.0526(12) Uani 1 1 d . . . H35 H 0.6008 0.4974 0.0931 0.063 Uiso 1 1 calc R . . C36 C 0.6827(3) 0.5765(3) 0.1412(3) 0.0664(15) Uani 1 1 d . . . H36A H 0.7052 0.6111 0.1030 0.080 Uiso 1 1 calc R . . H36B H 0.7218 0.5342 0.1462 0.080 Uiso 1 1 calc R . . C37 C 0.6781(3) 0.6184(3) 0.2166(3) 0.0578(13) Uani 1 1 d . . . H37A H 0.7333 0.6170 0.2405 0.069 Uiso 1 1 calc R . . H37B H 0.6641 0.6715 0.2071 0.069 Uiso 1 1 calc R . . C38 C 0.6140(3) 0.5853(3) 0.2714(2) 0.0473(12) Uani 1 1 d . . . H38 H 0.6310 0.5456 0.3032 0.057 Uiso 1 1 calc R . . C41 C 0.5007(2) 0.4403(2) 0.3061(2) 0.0311(9) Uani 1 1 d . . . C42 C 0.5082(3) 0.3548(3) 0.4017(2) 0.0463(12) Uani 1 1 d . . . H42 H 0.5299 0.3197 0.4365 0.056 Uiso 1 1 calc R . . C43 C 0.4296(3) 0.3777(3) 0.3966(3) 0.0537(13) Uani 1 1 d . . . H43 H 0.3850 0.3611 0.4268 0.064 Uiso 1 1 calc R . . C44 C 0.6412(3) 0.3812(3) 0.3305(2) 0.0467(11) Uani 1 1 d . . . H44A H 0.6729 0.3888 0.3765 0.070 Uiso 1 1 calc R . . H44B H 0.6595 0.4171 0.2926 0.070 Uiso 1 1 calc R . . H44C H 0.6501 0.3300 0.3123 0.070 Uiso 1 1 calc R . . C45 C 0.3480(3) 0.4713(3) 0.3174(3) 0.0512(13) Uani 1 1 d . . . H45A H 0.3635 0.5229 0.3026 0.061 Uiso 1 1 calc R . . H45B H 0.3120 0.4752 0.3620 0.061 Uiso 1 1 calc R . . C51 C 0.4794(2) 0.4134(2) 0.1554(2) 0.0343(10) Uani 1 1 d . . . C52 C 0.4570(3) 0.2997(3) 0.0983(2) 0.0503(12) Uani 1 1 d . . . H52 H 0.4675 0.2525 0.0757 0.060 Uiso 1 1 calc R . . C53 C 0.3817(3) 0.3310(3) 0.1105(2) 0.0474(12) Uani 1 1 d . . . H53 H 0.3296 0.3102 0.0976 0.057 Uiso 1 1 calc R . . C54 C 0.6074(3) 0.3357(3) 0.1251(3) 0.0529(13) Uani 1 1 d . . . H54A H 0.6356 0.3743 0.1545 0.079 Uiso 1 1 calc R . . H54B H 0.6278 0.3369 0.0736 0.079 Uiso 1 1 calc R . . H54C H 0.6184 0.2863 0.1469 0.079 Uiso 1 1 calc R . . C55 C 0.3289(3) 0.4513(3) 0.1730(3) 0.0524(13) Uani 1 1 d . . . H55A H 0.2818 0.4481 0.1379 0.063 Uiso 1 1 calc R . . H55B H 0.3499 0.5034 0.1715 0.063 Uiso 1 1 calc R . . C56 C 0.2968(3) 0.4352(3) 0.2524(3) 0.0506(12) Uani 1 1 d . . . H56A H 0.2957 0.3802 0.2598 0.061 Uiso 1 1 calc R . . H56B H 0.2391 0.4534 0.2559 0.061 Uiso 1 1 calc R . . C61 C 0.1257(3) 0.9037(3) 0.5032(5) 0.0906(18) Uani 1 1 d . . . H1A H 0.0814 0.9123 0.4659 0.109 Uiso 1 1 calc R . . H1B H 0.0990 0.8971 0.5525 0.109 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 0.02630(16) 0.03005(18) 0.02760(15) 0.00031(19) -0.00066(11) -0.00216(19) Rh2 0.02894(17) 0.03230(18) 0.03123(16) 0.00192(19) -0.00391(12) -0.0015(2) Cl1 0.0666(9) 0.0816(10) 0.1067(14) 0.0262(9) 0.0073(8) 0.0061(8) Cl2 0.1024(11) 0.0905(11) 0.1031(12) 0.0124(11) -0.0288(10) -0.0210(9) P1 0.0306(5) 0.0333(5) 0.0370(6) -0.0001(5) -0.0022(5) 0.0025(4) P2 0.0430(7) 0.0644(8) 0.0434(7) 0.0067(7) 0.0016(6) 0.0170(6) F11 0.112(3) 0.071(2) 0.0404(16) 0.0042(14) -0.0046(15) 0.013(2) F12 0.0588(17) 0.0808(19) 0.096(2) -0.017(2) 0.0074(19) 0.0362(15) F13 0.0578(17) 0.0635(18) 0.140(3) 0.015(2) -0.017(2) -0.0275(14) F14 0.145(3) 0.099(3) 0.0388(18) 0.0082(16) -0.0146(18) 0.024(3) F15 0.0540(16) 0.0492(15) 0.100(2) -0.0030(15) -0.0032(15) 0.0236(13) F16 0.0576(16) 0.0468(15) 0.137(3) 0.012(2) -0.028(2) -0.0133(13) F21 0.096(3) 0.261(6) 0.051(2) 0.027(3) 0.0028(18) 0.083(3) F22 0.21(2) 0.041(5) 0.261(18) 0.061(8) 0.075(16) 0.029(7) F23 0.107(3) 0.173(4) 0.053(2) 0.026(2) 0.0007(18) 0.043(3) F24 0.11(2) 0.09(2) 0.21(4) -0.12(2) -0.10(2) 0.035(16) F25 0.039(3) 0.141(13) 0.116(5) 0.035(5) 0.016(2) -0.006(4) F26 0.134(19) 0.074(10) 0.094(10) 0.025(8) 0.013(10) 0.071(15) F27 0.037(4) 0.186(14) 0.083(6) 0.051(6) 0.018(3) 0.016(5) F28 0.19(2) 0.139(13) 0.169(13) -0.070(10) 0.052(12) -0.118(13) F29 0.136(18) 0.28(4) 0.058(8) -0.049(12) -0.026(8) 0.16(2) F211 0.09(2) 0.21(6) 0.079(15) 0.05(2) -0.024(13) -0.10(3) N11 0.032(2) 0.051(2) 0.053(2) 0.0077(18) -0.0062(17) 0.0019(19) N12 0.034(2) 0.036(2) 0.044(2) -0.0004(16) 0.0075(16) 0.0038(16) N21 0.0304(19) 0.033(2) 0.051(2) 0.0080(17) 0.0057(16) 0.0027(16) N22 0.0339(19) 0.034(2) 0.046(2) -0.0069(17) -0.0116(17) 0.0048(15) N41 0.038(2) 0.035(2) 0.0307(19) 0.0004(15) 0.0003(15) -0.0010(17) N42 0.028(2) 0.036(2) 0.045(2) -0.0055(17) 0.0028(16) -0.0028(17) N51 0.041(2) 0.039(2) 0.0368(19) -0.0074(16) 0.0053(16) 0.0010(18) N52 0.041(2) 0.041(2) 0.043(2) -0.0086(17) -0.0070(17) -0.0006(18) C1 0.038(3) 0.031(3) 0.058(3) 0.002(2) 0.000(2) -0.011(2) C2 0.061(3) 0.044(3) 0.064(3) 0.012(2) -0.008(3) -0.001(2) C3 0.047(3) 0.059(3) 0.069(3) 0.028(3) -0.008(2) 0.004(3) C4 0.031(2) 0.040(3) 0.048(3) -0.003(2) -0.0016(19) -0.0001(19) C5 0.037(3) 0.037(3) 0.039(3) -0.0055(19) 0.0045(18) 0.008(2) C6 0.055(3) 0.077(4) 0.053(3) -0.021(3) -0.003(2) 0.007(3) C7 0.079(4) 0.058(3) 0.055(3) -0.026(3) 0.002(3) -0.011(3) C8 0.044(3) 0.037(3) 0.055(3) -0.004(2) -0.013(2) -0.012(2) C11 0.031(2) 0.035(2) 0.043(3) 0.006(2) 0.0001(19) -0.0047(18) C12 0.038(3) 0.057(3) 0.082(4) 0.012(3) -0.008(2) 0.010(2) C13 0.040(3) 0.051(3) 0.087(4) 0.006(3) 0.016(3) 0.005(2) C14 0.065(4) 0.102(5) 0.050(3) 0.017(3) -0.019(3) 0.007(3) C15 0.064(4) 0.065(4) 0.040(3) 0.006(2) 0.020(2) 0.007(3) C21 0.023(2) 0.036(2) 0.037(2) 0.0028(18) -0.0004(17) 0.0048(17) C22 0.045(3) 0.024(2) 0.076(4) 0.002(2) 0.005(2) -0.003(2) C23 0.044(3) 0.028(2) 0.077(4) -0.012(2) -0.011(2) 0.005(2) C24 0.070(4) 0.054(3) 0.054(3) 0.018(2) 0.017(3) 0.002(3) C25 0.060(3) 0.042(3) 0.036(3) -0.007(2) -0.014(2) 0.006(2) C26 0.077(4) 0.056(3) 0.030(3) -0.007(2) 0.003(2) 0.007(3) C31 0.054(3) 0.033(3) 0.066(3) -0.009(2) -0.002(3) -0.010(2) C32 0.068(4) 0.035(3) 0.108(5) -0.009(3) -0.023(3) 0.011(3) C33 0.083(5) 0.041(3) 0.104(5) 0.016(3) -0.046(4) -0.001(3) C34 0.067(4) 0.048(3) 0.065(3) 0.024(2) -0.024(3) -0.014(3) C35 0.061(3) 0.053(3) 0.044(3) 0.020(2) 0.001(2) -0.008(3) C36 0.055(3) 0.075(4) 0.069(4) 0.033(3) 0.008(3) -0.010(3) C37 0.045(3) 0.052(3) 0.076(4) 0.020(3) -0.021(3) -0.016(2) C38 0.046(3) 0.041(3) 0.055(3) 0.002(2) -0.017(2) -0.008(2) C41 0.028(2) 0.036(2) 0.028(2) -0.0050(17) 0.0009(17) -0.0055(18) C42 0.060(3) 0.045(3) 0.034(2) 0.004(2) 0.003(2) -0.007(3) C43 0.065(4) 0.057(3) 0.039(3) -0.005(2) 0.017(2) -0.020(3) C44 0.034(3) 0.058(3) 0.047(3) 0.003(2) -0.004(2) 0.005(2) C45 0.031(2) 0.063(3) 0.059(3) -0.020(2) 0.008(2) 0.003(2) C51 0.032(2) 0.043(3) 0.028(2) 0.0021(18) -0.0052(17) 0.001(2) C52 0.062(3) 0.046(3) 0.042(3) -0.019(2) -0.004(2) 0.000(3) C53 0.041(3) 0.050(3) 0.051(3) -0.017(2) -0.011(2) -0.010(2) C54 0.046(3) 0.059(3) 0.054(3) -0.007(2) 0.009(2) 0.008(2) C55 0.034(3) 0.054(3) 0.069(3) -0.013(2) -0.021(2) 0.006(2) C56 0.028(2) 0.053(3) 0.071(3) -0.022(2) 0.005(2) 0.004(2) C61 0.049(3) 0.110(5) 0.113(5) -0.021(5) 0.000(4) -0.007(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 C21 2.020(4) . ? Rh1 C11 2.038(4) . ? Rh1 C5 2.180(4) . ? Rh1 C4 2.209(4) . ? Rh1 C1 2.217(4) . ? Rh1 C8 2.218(4) . ? Rh2 C51 2.023(4) . ? Rh2 C41 2.028(4) . ? Rh2 C35 2.197(4) . ? Rh2 C31 2.203(4) . ? Rh2 C34 2.208(4) . ? Rh2 C38 2.215(4) . ? Cl1 C61 1.752(6) . ? Cl2 C61 1.710(5) . ? P1 F14 1.572(3) . ? P1 F12 1.572(2) . ? P1 F16 1.577(3) . ? P1 F13 1.582(3) . ? P1 F15 1.587(2) . ? P1 F11 1.589(3) . ? P2 F22 1.461(9) . ? P2 F210 1.48(3) . ? P2 F28 1.485(12) . ? P2 F29 1.549(10) . ? P2 F23 1.563(3) . ? P2 F21 1.563(3) . ? P2 F25 1.569(4) . ? P2 F27 1.573(7) . ? P2 F24 1.58(3) . ? P2 F211 1.62(2) . ? P2 F26 1.621(19) . ? F22 F24 0.90(3) . ? F22 F29 1.22(5) . ? F22 F211 1.32(6) . ? F24 F211 0.82(4) . ? F25 F210 0.77(5) . ? F25 F211 1.44(7) . ? F26 F28 0.79(3) . ? F26 F210 1.14(6) . ? F27 F29 1.23(4) . ? F27 F28 1.71(4) . ? F28 F210 1.66(6) . ? N11 C11 1.347(5) . ? N11 C12 1.391(6) . ? N11 C14 1.461(6) . ? N12 C11 1.352(5) . ? N12 C13 1.389(6) . ? N12 C15 1.457(5) . ? N21 C21 1.359(5) . ? N21 C22 1.394(5) . ? N21 C24 1.451(5) . ? N22 C21 1.364(5) . ? N22 C23 1.379(5) . ? N22 C25 1.460(5) . ? N41 C41 1.360(5) . ? N41 C42 1.372(5) . ? N41 C44 1.448(5) . ? N42 C41 1.347(5) . ? N42 C43 1.369(5) . ? N42 C45 1.460(5) . ? N51 C51 1.355(5) . ? N51 C52 1.377(5) . ? N51 C54 1.464(6) . ? N52 C51 1.358(5) . ? N52 C53 1.382(5) . ? N52 C55 1.460(5) . ? C1 C8 1.371(6) . ? C1 C2 1.489(6) . ? C1 H1 0.9300 . ? C2 C3 1.501(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.530(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.365(5) . ? C4 H4 0.9300 . ? C5 C6 1.486(6) . ? C5 H5 0.9300 . ? C6 C7 1.496(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.516(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H58 0.9300 . ? C12 C13 1.309(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C26 1.526(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C22 C23 1.310(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.531(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C31 C38 1.397(6) . ? C31 C32 1.508(6) . ? C31 H31 0.9300 . ? C32 C33 1.537(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.503(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.358(7) . ? C34 H34 0.9300 . ? C35 C36 1.485(7) . ? C35 H35 0.9300 . ? C36 C37 1.514(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.514(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38 0.9300 . ? C42 C43 1.312(7) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C56 1.537(6) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C52 C53 1.330(6) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.509(6) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C61 H1A 0.9700 . ? C61 H1B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Rh1 C11 83.77(15) . . ? C21 Rh1 C5 92.69(15) . . ? C11 Rh1 C5 158.47(16) . . ? C21 Rh1 C4 94.53(15) . . ? C11 Rh1 C4 165.01(16) . . ? C5 Rh1 C4 36.24(14) . . ? C21 Rh1 C1 159.62(16) . . ? C11 Rh1 C1 95.49(16) . . ? C5 Rh1 C1 95.05(16) . . ? C4 Rh1 C1 80.92(16) . . ? C21 Rh1 C8 164.37(16) . . ? C11 Rh1 C8 96.51(17) . . ? C5 Rh1 C8 81.30(17) . . ? C4 Rh1 C8 89.11(16) . . ? C1 Rh1 C8 36.01(15) . . ? C51 Rh2 C41 83.79(15) . . ? C51 Rh2 C35 94.53(17) . . ? C41 Rh2 C35 160.56(17) . . ? C51 Rh2 C31 156.73(17) . . ? C41 Rh2 C31 92.72(16) . . ? C35 Rh2 C31 96.11(19) . . ? C51 Rh2 C34 95.30(16) . . ? C41 Rh2 C34 163.5(2) . . ? C35 Rh2 C34 35.90(18) . . ? C31 Rh2 C34 81.58(19) . . ? C51 Rh2 C38 166.37(17) . . ? C41 Rh2 C38 96.37(15) . . ? C35 Rh2 C38 80.76(18) . . ? C31 Rh2 C38 36.85(16) . . ? C34 Rh2 C38 88.37(17) . . ? F14 P1 F12 91.94(19) . . ? F14 P1 F16 90.1(2) . . ? F12 P1 F16 88.96(15) . . ? F14 P1 F13 90.0(2) . . ? F12 P1 F13 91.52(16) . . ? F16 P1 F13 179.51(19) . . ? F14 P1 F15 89.03(17) . . ? F12 P1 F15 179.01(19) . . ? F16 P1 F15 90.84(15) . . ? F13 P1 F15 88.68(16) . . ? F14 P1 F11 179.00(18) . . ? F12 P1 F11 88.67(18) . . ? F16 P1 F11 90.71(19) . . ? F13 P1 F11 89.2(2) . . ? F15 P1 F11 90.37(17) . . ? F22 P2 F210 132(3) . . ? F22 P2 F28 157(2) . . ? F210 P2 F28 68(2) . . ? F22 P2 F29 48(2) . . ? F210 P2 F29 177.1(14) . . ? F28 P2 F29 113(2) . . ? F22 P2 F23 96.1(10) . . ? F210 P2 F23 83.7(15) . . ? F28 P2 F23 96.1(11) . . ? F29 P2 F23 93.4(7) . . ? F22 P2 F21 84.7(9) . . ? F210 P2 F21 95.2(15) . . ? F28 P2 F21 83.5(11) . . ? F29 P2 F21 87.7(7) . . ? F23 P2 F21 178.9(2) . . ? F22 P2 F25 103.7(11) . . ? F210 P2 F25 29(2) . . ? F28 P2 F25 94.6(12) . . ? F29 P2 F25 151(2) . . ? F23 P2 F25 93.0(3) . . ? F21 P2 F25 86.1(3) . . ? F22 P2 F27 93.9(12) . . ? F210 P2 F27 134(3) . . ? F28 P2 F27 67.9(15) . . ? F29 P2 F27 46.3(15) . . ? F23 P2 F27 86.8(3) . . ? F21 P2 F27 94.0(3) . . ? F25 P2 F27 162.4(12) . . ? F22 P2 F24 34.0(11) . . ? F210 P2 F24 103(2) . . ? F28 P2 F24 168(2) . . ? F29 P2 F24 75(2) . . ? F23 P2 F24 74(2) . . ? F21 P2 F24 107(2) . . ? F25 P2 F24 79.6(16) . . ? F27 P2 F24 117.0(18) . . ? F22 P2 F211 51(3) . . ? F210 P2 F211 82(4) . . ? F28 P2 F211 148(3) . . ? F29 P2 F211 98(3) . . ? F23 P2 F211 90.8(8) . . ? F21 P2 F211 89.1(8) . . ? F25 P2 F211 54(2) . . ? F27 P2 F211 144(3) . . ? F24 P2 F211 29.6(16) . . ? F22 P2 F26 173.2(16) . . ? F210 P2 F26 43(2) . . ? F28 P2 F26 29.2(10) . . ? F29 P2 F26 137(2) . . ? F23 P2 F26 79.2(8) . . ? F21 P2 F26 100.0(8) . . ? F25 P2 F26 72.0(11) . . ? F27 P2 F26 90.7(14) . . ? F24 P2 F26 139.3(17) . . ? F211 P2 F26 124(3) . . ? F24 F22 F29 129(4) . . ? F24 F22 F211 38(3) . . ? F29 F22 F211 140(3) . . ? F24 F22 P2 80.6(19) . . ? F29 F22 P2 70.0(15) . . ? F211 F22 P2 71(2) . . ? F211 F24 F22 100(6) . . ? F211 F24 P2 77(3) . . ? F22 F24 P2 65.4(17) . . ? F210 F25 F211 130(3) . . ? F210 F25 P2 69(2) . . ? F211 F25 P2 64.8(10) . . ? F28 F26 F210 117(3) . . ? F28 F26 P2 65.9(19) . . ? F210 F26 P2 61.9(16) . . ? F29 F27 P2 65.8(8) . . ? F29 F27 F28 117.7(13) . . ? P2 F27 F28 53.6(6) . . ? F26 F28 P2 85(2) . . ? F26 F28 F210 38(2) . . ? P2 F28 F210 55.8(11) . . ? F26 F28 F27 126(2) . . ? P2 F28 F27 58.5(10) . . ? F210 F28 F27 112.7(12) . . ? F22 F29 F27 130.2(12) . . ? F22 F29 P2 62.4(8) . . ? F27 F29 P2 67.9(10) . . ? F25 F210 F26 155(3) . . ? F25 F210 P2 81.7(19) . . ? F26 F210 P2 75(3) . . ? F25 F210 F28 131(3) . . ? F26 F210 F28 25.2(15) . . ? P2 F210 F28 56.0(17) . . ? F24 F211 F22 42(4) . . ? F24 F211 F25 124(6) . . ? F22 F211 F25 119.3(19) . . ? F24 F211 P2 73(3) . . ? F22 F211 P2 58.7(10) . . ? F25 F211 P2 61.5(17) . . ? C11 N11 C12 110.7(4) . . ? C11 N11 C14 124.8(4) . . ? C12 N11 C14 124.5(4) . . ? C11 N12 C13 110.7(4) . . ? C11 N12 C15 123.9(3) . . ? C13 N12 C15 125.3(4) . . ? C21 N21 C22 110.5(4) . . ? C21 N21 C24 123.3(4) . . ? C22 N21 C24 126.1(4) . . ? C21 N22 C23 111.0(4) . . ? C21 N22 C25 124.3(3) . . ? C23 N22 C25 124.7(4) . . ? C41 N41 C42 110.9(4) . . ? C41 N41 C44 124.9(3) . . ? C42 N41 C44 124.2(4) . . ? C41 N42 C43 110.6(4) . . ? C41 N42 C45 124.8(4) . . ? C43 N42 C45 124.6(4) . . ? C51 N51 C52 111.2(4) . . ? C51 N51 C54 124.8(4) . . ? C52 N51 C54 124.0(4) . . ? C51 N52 C53 111.0(4) . . ? C51 N52 C55 124.5(4) . . ? C53 N52 C55 124.5(4) . . ? C8 C1 C2 125.7(4) . . ? C8 C1 Rh1 72.1(2) . . ? C2 C1 Rh1 108.1(3) . . ? C8 C1 H1 117.1 . . ? C2 C1 H1 117.1 . . ? Rh1 C1 H1 89.9 . . ? C1 C2 C3 117.4(4) . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? C3 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? C2 C3 C4 113.8(4) . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 124.6(4) . . ? C5 C4 Rh1 70.7(2) . . ? C3 C4 Rh1 111.6(3) . . ? C5 C4 H4 117.7 . . ? C3 C4 H4 117.7 . . ? Rh1 C4 H4 87.7 . . ? C4 C5 C6 126.5(4) . . ? C4 C5 Rh1 73.0(2) . . ? C6 C5 Rh1 108.7(3) . . ? C4 C5 H5 116.7 . . ? C6 C5 H5 116.7 . . ? Rh1 C5 H5 88.2 . . ? C5 C6 C7 115.4(4) . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6B 108.4 . . ? C7 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C6 C7 C8 115.5(4) . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C1 C8 C7 123.7(4) . . ? C1 C8 Rh1 71.9(2) . . ? C7 C8 Rh1 109.6(3) . . ? C1 C8 H58 118.2 . . ? C7 C8 H58 118.2 . . ? Rh1 C8 H58 88.5 . . ? N11 C11 N12 104.2(3) . . ? N11 C11 Rh1 128.6(3) . . ? N12 C11 Rh1 126.5(3) . . ? C13 C12 N11 107.2(4) . . ? C13 C12 H12 126.4 . . ? N11 C12 H12 126.4 . . ? C12 C13 N12 107.1(4) . . ? C12 C13 H13 126.4 . . ? N12 C13 H13 126.4 . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N12 C15 C26 116.2(4) . . ? N12 C15 H15A 108.2 . . ? C26 C15 H15A 108.2 . . ? N12 C15 H15B 108.2 . . ? C26 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? N21 C21 N22 103.6(3) . . ? N21 C21 Rh1 129.8(3) . . ? N22 C21 Rh1 126.4(3) . . ? C23 C22 N21 107.3(4) . . ? C23 C22 H22 126.4 . . ? N21 C22 H22 126.4 . . ? C22 C23 N22 107.6(4) . . ? C22 C23 H23 126.2 . . ? N22 C23 H23 126.2 . . ? N21 C24 H24A 109.5 . . ? N21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N22 C25 C26 115.4(4) . . ? N22 C25 H25A 108.4 . . ? C26 C25 H25A 108.4 . . ? N22 C25 H25B 108.4 . . ? C26 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C15 C26 C25 116.3(4) . . ? C15 C26 H26A 108.2 . . ? C25 C26 H26A 108.2 . . ? C15 C26 H26B 108.2 . . ? C25 C26 H26B 108.2 . . ? H26A C26 H26B 107.4 . . ? C38 C31 C32 125.4(5) . . ? C38 C31 Rh2 72.0(3) . . ? C32 C31 Rh2 106.8(3) . . ? C38 C31 H31 117.3 . . ? C32 C31 H31 117.3 . . ? Rh2 C31 H31 91.2 . . ? C31 C32 C33 114.7(4) . . ? C31 C32 H32A 108.6 . . ? C33 C32 H32A 108.6 . . ? C31 C32 H32B 108.6 . . ? C33 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? C34 C33 C32 113.4(4) . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C35 C34 C33 123.8(5) . . ? C35 C34 Rh2 71.6(3) . . ? C33 C34 Rh2 111.3(4) . . ? C35 C34 H34 118.1 . . ? C33 C34 H34 118.1 . . ? Rh2 C34 H34 87.1 . . ? C34 C35 C36 126.9(5) . . ? C34 C35 Rh2 72.5(3) . . ? C36 C35 Rh2 108.1(3) . . ? C34 C35 H35 116.5 . . ? C36 C35 H35 116.5 . . ? Rh2 C35 H35 89.4 . . ? C35 C36 C37 114.4(4) . . ? C35 C36 H36A 108.7 . . ? C37 C36 H36A 108.7 . . ? C35 C36 H36B 108.7 . . ? C37 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C38 C37 C36 113.8(4) . . ? C38 C37 H37A 108.8 . . ? C36 C37 H37A 108.8 . . ? C38 C37 H37B 108.8 . . ? C36 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C31 C38 C37 123.8(4) . . ? C31 C38 Rh2 71.1(2) . . ? C37 C38 Rh2 110.7(3) . . ? C31 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? Rh2 C38 H38 88.2 . . ? N42 C41 N41 103.8(3) . . ? N42 C41 Rh2 128.5(3) . . ? N41 C41 Rh2 127.5(3) . . ? C43 C42 N41 106.7(4) . . ? C43 C42 H42 126.7 . . ? N41 C42 H42 126.7 . . ? C42 C43 N42 108.1(4) . . ? C42 C43 H43 126.0 . . ? N42 C43 H43 126.0 . . ? N41 C44 H44A 109.5 . . ? N41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N42 C45 C56 115.5(4) . . ? N42 C45 H45A 108.4 . . ? C56 C45 H45A 108.4 . . ? N42 C45 H45B 108.4 . . ? C56 C45 H45B 108.4 . . ? H45A C45 H45B 107.5 . . ? N51 C51 N52 103.9(3) . . ? N51 C51 Rh2 130.4(3) . . ? N52 C51 Rh2 125.3(3) . . ? C53 C52 N51 107.1(4) . . ? C53 C52 H52 126.5 . . ? N51 C52 H52 126.5 . . ? C52 C53 N52 106.9(4) . . ? C52 C53 H53 126.6 . . ? N52 C53 H53 126.6 . . ? N51 C54 H54A 109.5 . . ? N51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N52 C55 C56 115.4(4) . . ? N52 C55 H55A 108.4 . . ? C56 C55 H55A 108.4 . . ? N52 C55 H55B 108.4 . . ? C56 C55 H55B 108.4 . . ? H55A C55 H55B 107.5 . . ? C55 C56 C45 115.5(4) . . ? C55 C56 H56A 108.4 . . ? C45 C56 H56A 108.4 . . ? C55 C56 H56B 108.4 . . ? C45 C56 H56B 108.4 . . ? H56A C56 H56B 107.5 . . ? Cl2 C61 Cl1 113.5(3) . . ? Cl2 C61 H1A 108.9 . . ? Cl1 C61 H1A 108.9 . . ? Cl2 C61 H1B 108.9 . . ? Cl1 C61 H1B 108.9 . . ? H1A C61 H1B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.316 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.065 #===END data_19 _database_code_depnum_ccdc_archive 'CCDC 250307' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H35 Cl N2 O P Rh S' _chemical_formula_weight 640.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.04670(10) _cell_length_b 10.58750(10) _cell_length_c 30.4334(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.147(1) _cell_angle_gamma 90.00 _cell_volume 2907.34(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7915 _cell_measurement_theta_max 28.7 _cell_measurement_theta_min 1.02 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.832 _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 173(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 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_reflns_number 12308 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6329 _reflns_number_gt 5053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia,1997)' _computing_publication_material 'X-Seed (Barbour, 1999)' _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^)+(0.0305P)^2^+0.8904P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6329 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.307016(17) 0.926122(15) 0.601524(5) 0.02312(6) Uani 1 1 d . . . Cl1 Cl 0.44174(7) 0.83313(6) 0.662922(18) 0.03925(15) Uani 1 1 d . . . S1 S 0.22484(7) 1.09230(5) 0.647904(19) 0.03464(14) Uani 1 1 d . . . P1 P 0.38199(6) 0.76861(5) 0.557925(17) 0.02212(12) Uani 1 1 d . . . O1 O 0.1520(2) 1.07106(17) 0.52934(6) 0.0492(5) Uani 1 1 d . . . N11 N 0.13744(18) 0.94410(16) 0.71545(6) 0.0260(4) Uani 1 1 d . . . N12 N 0.31544(19) 1.07418(17) 0.73592(6) 0.0302(4) Uani 1 1 d . . . C1 C 0.2115(2) 1.0105(2) 0.55642(7) 0.0306(5) Uani 1 1 d . . . C11 C 0.2294(2) 1.0325(2) 0.70063(7) 0.0268(5) Uani 1 1 d . . . C12 C 0.1648(2) 0.9316(2) 0.76100(7) 0.0281(5) Uani 1 1 d . . . C13 C 0.2758(2) 1.0119(2) 0.77350(7) 0.0303(5) Uani 1 1 d . . . C14 C 0.0279(2) 0.8752(2) 0.68579(7) 0.0336(5) Uani 1 1 d . . . H14 H 0.0601 0.8849 0.6552 0.040 Uiso 1 1 calc R . . C15 C 0.0786(3) 0.8496(3) 0.78974(8) 0.0407(6) Uani 1 1 d . . . H15A H 0.1021 0.7608 0.7844 0.061 Uiso 1 1 calc R . . H15B H -0.0276 0.8638 0.7830 0.061 Uiso 1 1 calc R . . H15C H 0.1048 0.8703 0.8207 0.061 Uiso 1 1 calc R . . C16 C 0.3462(3) 1.0371(3) 0.81856(8) 0.0456(6) Uani 1 1 d . . . H16A H 0.2964 0.9869 0.8402 0.068 Uiso 1 1 calc R . . H16B H 0.3372 1.1271 0.8255 0.068 Uiso 1 1 calc R . . H16C H 0.4513 1.0138 0.8196 0.068 Uiso 1 1 calc R . . C17 C 0.4360(3) 1.1697(2) 0.73676(9) 0.0419(6) Uani 1 1 d . . . H17 H 0.4733 1.1754 0.7684 0.050 Uiso 1 1 calc R . . C18 C 0.0261(3) 0.7350(2) 0.69542(9) 0.0460(6) Uani 1 1 d . . . H18A H 0.1280 0.7047 0.7012 0.069 Uiso 1 1 calc R . . H18B H -0.0212 0.6901 0.6700 0.069 Uiso 1 1 calc R . . H18C H -0.0296 0.7196 0.7213 0.069 Uiso 1 1 calc R . . C19 C -0.1222(3) 0.9392(3) 0.68654(9) 0.0515(7) Uani 1 1 d . . . H19A H -0.1519 0.9418 0.7169 0.077 Uiso 1 1 calc R . . H19B H -0.1958 0.8917 0.6680 0.077 Uiso 1 1 calc R . . H19C H -0.1155 1.0255 0.6752 0.077 Uiso 1 1 calc R . . C21 C 0.5801(2) 0.7356(2) 0.56621(7) 0.0264(5) Uani 1 1 d . . . C22 C 0.6770(2) 0.8378(2) 0.56816(8) 0.0361(5) Uani 1 1 d . . . H22 H 0.6390 0.9214 0.5665 0.043 Uiso 1 1 calc R . . C23 C 0.8288(3) 0.8180(3) 0.57254(8) 0.0470(7) Uani 1 1 d . . . H23 H 0.8946 0.8880 0.5731 0.056 Uiso 1 1 calc R . . C24 C 0.8844(3) 0.6973(3) 0.57604(8) 0.0488(7) Uani 1 1 d . . . H24 H 0.9885 0.6841 0.5794 0.059 Uiso 1 1 calc R . . C25 C 0.7898(3) 0.5955(3) 0.57471(8) 0.0432(6) Uani 1 1 d . . . H25 H 0.8288 0.5123 0.5772 0.052 Uiso 1 1 calc R . . C26 C 0.6375(2) 0.6137(2) 0.56966(7) 0.0321(5) Uani 1 1 d . . . H26 H 0.5725 0.5431 0.5686 0.039 Uiso 1 1 calc R . . C31 C 0.3530(2) 0.78535(19) 0.49799(7) 0.0243(4) Uani 1 1 d . . . C32 C 0.4679(2) 0.7709(2) 0.47042(7) 0.0332(5) Uani 1 1 d . . . H32 H 0.5654 0.7541 0.4827 0.040 Uiso 1 1 calc R . . C33 C 0.4411(3) 0.7810(3) 0.42502(8) 0.0432(6) Uani 1 1 d . . . H33 H 0.5202 0.7704 0.4065 0.052 Uiso 1 1 calc R . . C34 C 0.3004(3) 0.8063(2) 0.40681(8) 0.0411(6) Uani 1 1 d . . . H34 H 0.2826 0.8136 0.3758 0.049 Uiso 1 1 calc R . . C35 C 0.1857(3) 0.8210(2) 0.43374(8) 0.0371(6) Uani 1 1 d . . . H35 H 0.0886 0.8383 0.4212 0.045 Uiso 1 1 calc R . . C36 C 0.2110(2) 0.8109(2) 0.47900(7) 0.0306(5) Uani 1 1 d . . . H36 H 0.1312 0.8214 0.4973 0.037 Uiso 1 1 calc R . . C41 C 0.2935(2) 0.6164(2) 0.56771(7) 0.0260(5) Uani 1 1 d . . . C42 C 0.2475(3) 0.5344(2) 0.53354(8) 0.0407(6) Uani 1 1 d . . . H42 H 0.2624 0.5568 0.5040 0.049 Uiso 1 1 calc R . . C43 C 0.1803(3) 0.4206(2) 0.54239(10) 0.0499(7) Uani 1 1 d . . . H43 H 0.1489 0.3658 0.5188 0.060 Uiso 1 1 calc R . . C44 C 0.1589(3) 0.3869(2) 0.58460(10) 0.0478(7) Uani 1 1 d . . . H44 H 0.1136 0.3083 0.5904 0.057 Uiso 1 1 calc R . . C45 C 0.2029(3) 0.4665(3) 0.61904(9) 0.0466(7) Uani 1 1 d . . . H45 H 0.1878 0.4425 0.6485 0.056 Uiso 1 1 calc R . . C46 C 0.2690(3) 0.5814(2) 0.61065(8) 0.0365(5) Uani 1 1 d . . . H46 H 0.2977 0.6366 0.6344 0.044 Uiso 1 1 calc R . . C110 C 0.5652(3) 1.1275(3) 0.71365(12) 0.0607(9) Uani 1 1 d . . . H11D H 0.5970 1.0441 0.7246 0.091 Uiso 1 1 calc R . . H11E H 0.6466 1.1879 0.7190 0.091 Uiso 1 1 calc R . . H11F H 0.5379 1.1223 0.6819 0.091 Uiso 1 1 calc R . . C111 C 0.3801(3) 1.2987(2) 0.72544(11) 0.0538(7) Uani 1 1 d . . . H11G H 0.3500 1.3028 0.6939 0.081 Uiso 1 1 calc R . . H11H H 0.4587 1.3606 0.7326 0.081 Uiso 1 1 calc R . . H11I H 0.2947 1.3176 0.7424 0.081 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 0.02417(9) 0.02459(9) 0.02076(9) 0.00040(7) 0.00284(6) 0.00254(7) Cl1 0.0477(4) 0.0428(3) 0.0259(3) -0.0034(2) -0.0069(2) 0.0149(3) S1 0.0498(4) 0.0281(3) 0.0273(3) 0.0013(2) 0.0117(3) 0.0077(3) P1 0.0199(3) 0.0252(3) 0.0214(3) 0.0004(2) 0.0023(2) 0.0016(2) O1 0.0627(12) 0.0473(11) 0.0365(10) 0.0073(8) -0.0045(9) 0.0189(9) N11 0.0228(9) 0.0325(10) 0.0229(9) -0.0020(7) 0.0031(7) -0.0018(7) N12 0.0255(10) 0.0324(10) 0.0331(10) -0.0072(8) 0.0052(8) -0.0041(8) C1 0.0328(12) 0.0296(12) 0.0300(12) -0.0031(10) 0.0065(10) 0.0029(10) C11 0.0274(11) 0.0269(11) 0.0273(11) -0.0030(9) 0.0092(9) 0.0036(9) C12 0.0248(11) 0.0371(13) 0.0228(10) -0.0022(9) 0.0051(8) 0.0029(10) C13 0.0281(12) 0.0373(13) 0.0257(11) -0.0056(10) 0.0033(9) 0.0018(10) C14 0.0295(12) 0.0418(14) 0.0289(12) -0.0059(10) -0.0015(9) -0.0053(10) C15 0.0350(13) 0.0551(16) 0.0330(13) 0.0073(12) 0.0092(10) -0.0041(12) C16 0.0480(15) 0.0561(17) 0.0319(13) -0.0098(12) -0.0024(11) -0.0044(13) C17 0.0341(13) 0.0366(14) 0.0553(16) -0.0068(12) 0.0047(11) -0.0096(11) C18 0.0499(16) 0.0404(15) 0.0470(16) -0.0071(12) -0.0019(12) -0.0127(12) C19 0.0321(14) 0.070(2) 0.0512(17) -0.0070(14) -0.0065(12) 0.0061(13) C21 0.0215(11) 0.0374(13) 0.0204(10) 0.0003(9) 0.0024(8) 0.0035(9) C22 0.0288(12) 0.0423(14) 0.0369(13) -0.0019(11) 0.0003(10) -0.0024(11) C23 0.0266(13) 0.072(2) 0.0421(15) -0.0001(13) -0.0015(11) -0.0094(13) C24 0.0221(12) 0.092(2) 0.0325(13) 0.0035(14) 0.0017(10) 0.0128(14) C25 0.0380(14) 0.0592(18) 0.0325(13) 0.0049(12) 0.0036(11) 0.0231(13) C26 0.0305(12) 0.0396(13) 0.0266(11) 0.0013(10) 0.0041(9) 0.0087(10) C31 0.0257(11) 0.0238(11) 0.0231(10) 0.0005(8) 0.0010(8) -0.0020(9) C32 0.0266(12) 0.0476(14) 0.0257(11) 0.0016(10) 0.0036(9) 0.0000(10) C33 0.0420(15) 0.0613(17) 0.0274(12) 0.0020(12) 0.0103(11) -0.0032(13) C34 0.0526(16) 0.0489(16) 0.0209(11) 0.0030(10) -0.0038(11) -0.0083(12) C35 0.0314(13) 0.0420(14) 0.0362(13) 0.0004(11) -0.0097(10) -0.0037(10) C36 0.0275(12) 0.0355(13) 0.0287(12) -0.0016(9) 0.0005(9) -0.0023(9) C41 0.0214(11) 0.0260(11) 0.0309(11) 0.0029(9) 0.0034(9) 0.0033(8) C42 0.0540(16) 0.0333(13) 0.0357(13) -0.0021(10) 0.0100(12) -0.0077(11) C43 0.0616(18) 0.0336(14) 0.0541(17) -0.0046(13) 0.0014(14) -0.0114(13) C44 0.0414(15) 0.0313(14) 0.070(2) 0.0161(13) -0.0027(13) -0.0070(11) C45 0.0464(15) 0.0505(16) 0.0426(15) 0.0219(13) 0.0018(12) -0.0067(13) C46 0.0369(13) 0.0399(14) 0.0323(12) 0.0052(10) 0.0002(10) -0.0046(11) C110 0.0333(15) 0.0434(16) 0.108(3) -0.0019(17) 0.0230(16) -0.0061(12) C111 0.0440(16) 0.0348(15) 0.082(2) -0.0097(14) 0.0007(14) -0.0018(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.805(2) . ? Rh1 P1 2.2654(5) . ? Rh1 Cl1 2.3700(6) . ? Rh1 S1 2.4067(6) . ? S1 C11 1.723(2) . ? P1 C21 1.826(2) . ? P1 C31 1.832(2) . ? P1 C41 1.833(2) . ? O1 C1 1.147(3) . ? N11 C11 1.352(3) . ? N11 C12 1.397(3) . ? N11 C14 1.483(3) . ? N12 C11 1.354(3) . ? N12 C13 1.389(3) . ? N12 C17 1.487(3) . ? C12 C13 1.350(3) . ? C12 C15 1.492(3) . ? C13 C16 1.494(3) . ? C14 C18 1.512(3) . ? C14 C19 1.519(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C110 1.477(4) . ? C17 C111 1.488(4) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.391(3) . ? C21 C26 1.392(3) . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 C24 1.374(4) . ? C23 H23 0.9500 . ? C24 C25 1.375(4) . ? C24 H24 0.9500 . ? C25 C26 1.389(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.391(3) . ? C31 C36 1.396(3) . ? C32 C33 1.389(3) . ? C32 H32 0.9500 . ? C33 C34 1.377(3) . ? C33 H33 0.9500 . ? C34 C35 1.377(3) . ? C34 H34 0.9500 . ? C35 C36 1.384(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C46 1.391(3) . ? C41 C42 1.395(3) . ? C42 C43 1.384(3) . ? C42 H42 0.9500 . ? C43 C44 1.361(4) . ? C43 H43 0.9500 . ? C44 C45 1.381(4) . ? C44 H44 0.9500 . ? C45 C46 1.388(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C110 H11D 0.9800 . ? C110 H11E 0.9800 . ? C110 H11F 0.9800 . ? C111 H11G 0.9800 . ? C111 H11H 0.9800 . ? C111 H11I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 P1 93.79(7) . . ? C1 Rh1 Cl1 174.81(7) . . ? P1 Rh1 Cl1 89.84(2) . . ? C1 Rh1 S1 86.16(7) . . ? P1 Rh1 S1 179.38(2) . . ? Cl1 Rh1 S1 90.25(2) . . ? C11 S1 Rh1 106.86(7) . . ? C21 P1 C31 102.96(9) . . ? C21 P1 C41 104.18(10) . . ? C31 P1 C41 102.36(10) . . ? C21 P1 Rh1 113.12(7) . . ? C31 P1 Rh1 118.98(7) . . ? C41 P1 Rh1 113.53(7) . . ? C11 N11 C12 109.14(18) . . ? C11 N11 C14 122.55(18) . . ? C12 N11 C14 128.31(18) . . ? C11 N12 C13 109.31(18) . . ? C11 N12 C17 127.9(2) . . ? C13 N12 C17 122.78(19) . . ? O1 C1 Rh1 175.6(2) . . ? N11 C11 N12 107.06(18) . . ? N11 C11 S1 126.26(17) . . ? N12 C11 S1 126.37(17) . . ? C13 C12 N11 107.14(19) . . ? C13 C12 C15 127.7(2) . . ? N11 C12 C15 125.1(2) . . ? C12 C13 N12 107.34(18) . . ? C12 C13 C16 129.1(2) . . ? N12 C13 C16 123.6(2) . . ? N11 C14 C18 112.38(19) . . ? N11 C14 C19 109.24(19) . . ? C18 C14 C19 114.4(2) . . ? N11 C14 H14 106.8 . . ? C18 C14 H14 106.8 . . ? C19 C14 H14 106.8 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C110 C17 N12 113.0(2) . . ? C110 C17 C111 115.8(2) . . ? N12 C17 C111 112.6(2) . . ? C110 C17 H17 104.7 . . ? N12 C17 H17 104.7 . . ? C111 C17 H17 104.7 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C26 119.2(2) . . ? C22 C21 P1 117.78(17) . . ? C26 C21 P1 123.01(17) . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.2(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.4(2) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 119.9(2) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C32 C31 C36 118.46(19) . . ? C32 C31 P1 122.05(16) . . ? C36 C31 P1 119.47(16) . . ? C33 C32 C31 120.5(2) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.3(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.8(2) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 120.4(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.6(2) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C46 C41 C42 118.4(2) . . ? C46 C41 P1 119.18(17) . . ? C42 C41 P1 122.44(17) . . ? C43 C42 C41 120.5(2) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C44 C43 C42 120.4(3) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 120.3(2) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C46 120.0(2) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 120.4(2) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C17 C110 H11D 109.5 . . ? C17 C110 H11E 109.5 . . ? H11D C110 H11E 109.5 . . ? C17 C110 H11F 109.5 . . ? H11D C110 H11F 109.5 . . ? H11E C110 H11F 109.5 . . ? C17 C111 H11G 109.5 . . ? C17 C111 H11H 109.5 . . ? H11G C111 H11H 109.5 . . ? C17 C111 H11I 109.5 . . ? H11G C111 H11I 109.5 . . ? H11H C111 H11I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.838 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.061 #===END