####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_One _database_code_depnum_ccdc_archive 'CCDC 273861' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Rh2(hpp)4Br _chemical_melting_point ? _chemical_formula_moiety 'C28 H48 Br N12 Rh2' _chemical_formula_sum 'C28 H48 Br N12 Rh2' _chemical_formula_weight 838.51 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/n m m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z' '-y, -x, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z' 'y, x, z' _cell_length_a 13.976(7) _cell_length_b 13.976(7) _cell_length_c 8.139(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1590(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2925 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 27.42 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 2.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7208 _exptl_absorpt_correction_T_max 0.8726 _exptl_absorpt_process_details SADABS _exptl_special_details ; The disordered Rh~2~(hpp)~4~Br molecule resides on a special position with crystallographic C~4v~ symmetry. ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9001 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1042 _reflns_number_gt 857 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+6.0973P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1042 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.7500 0.7500 0.44001(9) 0.0203(2) Uani 1 8 d S . . Rh2 Rh 0.7500 0.7500 0.73860(9) 0.0206(2) Uani 1 8 d S . . Br1 Br 0.7500 0.7500 0.09556(16) 0.0422(4) Uani 1 8 d S . . N1 N 0.6226(5) 0.8184(5) 0.4563(7) 0.0291(14) Uani 0.50 1 d P . . N2 N 0.6059(4) 0.764(2) 0.7240(7) 0.031(5) Uani 0.50 1 d P . . N3 N 0.4727(5) 0.8318(6) 0.5881(8) 0.0376(17) Uani 0.50 1 d P . . C1 C 0.5677(6) 0.8041(5) 0.5892(9) 0.0262(15) Uani 0.50 1 d P . . C2 C 0.5818(6) 0.8787(6) 0.3268(9) 0.036(2) Uani 0.50 1 d P . . H2A H 0.6228 0.8764 0.2292 0.044 Uiso 1 2 calc SR . . H2B H 0.5788 0.9452 0.3647 0.044 Uiso 0.50 1 calc PR . . C3 C 0.4823(7) 0.8442(8) 0.2834(10) 0.043(2) Uani 0.50 1 d P . . H3A H 0.4850 0.7778 0.2445 0.052 Uiso 0.50 1 calc PR . . H3B H 0.4554 0.8839 0.1956 0.052 Uiso 0.50 1 calc PR . . C4 C 0.4201(7) 0.8507(7) 0.4361(9) 0.041(2) Uani 0.50 1 d P . . H4A H 0.3920 0.9148 0.4421 0.049 Uiso 0.50 1 calc PR . . H4B H 0.3676 0.8046 0.4266 0.049 Uiso 0.50 1 calc PR . . C5 C 0.4137(7) 0.8330(8) 0.7359(9) 0.040(2) Uani 0.50 1 d P . . H5A H 0.3622 0.7859 0.7242 0.048 Uiso 0.50 1 calc PR . . H5B H 0.3842 0.8962 0.7475 0.048 Uiso 0.50 1 calc PR . . C6 C 0.4698(7) 0.8110(8) 0.8872(10) 0.045(2) Uani 0.50 1 d P . . H6A H 0.4264 0.7907 0.9751 0.054 Uiso 0.50 1 calc PR . . H6B H 0.5035 0.8686 0.9242 0.054 Uiso 0.50 1 calc PR . . C7 C 0.5408(6) 0.7332(11) 0.8530(9) 0.034(4) Uani 0.50 1 d P . . H7A H 0.5770 0.7185 0.9530 0.041 Uiso 0.50 1 calc PR . . H7B H 0.5072 0.6750 0.8184 0.041 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0219(3) 0.0219(3) 0.0172(4) 0.000 0.000 0.000 Rh2 0.0219(3) 0.0219(3) 0.0182(4) 0.000 0.000 0.000 Br1 0.0485(5) 0.0485(5) 0.0296(6) 0.000 0.000 0.000 N1 0.032(3) 0.031(3) 0.024(3) 0.006(3) 0.000(3) 0.001(3) N2 0.024(3) 0.043(17) 0.026(2) 0.001(4) 0.002(2) 0.000(4) N3 0.027(4) 0.059(5) 0.027(3) -0.001(3) 0.000(3) 0.015(3) C1 0.027(4) 0.025(4) 0.027(3) -0.006(3) -0.002(3) 0.002(3) C2 0.044(5) 0.035(5) 0.030(3) 0.005(3) -0.001(3) 0.008(4) C3 0.045(5) 0.056(6) 0.030(4) 0.000(4) -0.004(4) 0.011(5) C4 0.034(5) 0.055(6) 0.033(4) 0.002(4) -0.006(3) 0.010(4) C5 0.031(5) 0.056(6) 0.033(4) 0.000(4) 0.006(3) 0.013(4) C6 0.040(5) 0.063(6) 0.033(4) 0.004(4) 0.008(4) 0.015(5) C7 0.033(4) 0.038(13) 0.030(3) 0.007(4) 0.003(3) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.025(7) . y Rh1 N1 2.025(7) 4_565 ? Rh1 N1 2.025(7) 3_655 ? Rh1 N1 2.025(7) 2_665 ? Rh1 Rh2 2.430(3) . y Rh1 Br1 2.803(3) . y Rh2 N2 2.026(7) 4_565 ? Rh2 N2 2.026(7) . ? Rh2 N2 2.026(7) 2_665 ? Rh2 N2 2.026(7) 3_655 ? Rh2 Br1 2.905(3) 1_556 ? Br1 Rh2 2.905(3) 1_554 y N1 C1 1.341(9) . ? N1 C2 1.465(9) . ? N2 C1 1.343(15) . ? N2 C7 1.455(13) . ? N3 C1 1.382(10) . ? N3 C5 1.459(10) . ? N3 C4 1.463(9) . ? C2 C3 1.514(13) . ? C3 C4 1.520(11) . ? C5 C6 1.492(11) . ? C6 C7 1.498(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N1 89.75(2) . 4_565 y N1 Rh1 N1 89.75(2) . 3_655 y N1 Rh1 N1 172.5(3) 4_565 3_655 y N1 Rh1 N1 172.5(3) . 2_665 y N1 Rh1 N1 89.75(2) 4_565 2_665 ? N1 Rh1 N1 89.75(2) 3_655 2_665 ? N1 Rh1 Rh2 86.24(17) . . ? N1 Rh1 Rh2 86.24(17) 4_565 . ? N1 Rh1 Rh2 86.24(17) 3_655 . ? N1 Rh1 Rh2 86.24(17) 2_665 . ? N1 Rh1 Br1 93.76(17) . . y N1 Rh1 Br1 93.76(17) 4_565 . ? N1 Rh1 Br1 93.76(17) 3_655 . ? N1 Rh1 Br1 93.76(17) 2_665 . ? Rh2 Rh1 Br1 180.0 . . y N2 Rh2 N2 89.80(2) 4_565 . y N2 Rh2 N2 89.80(2) 4_565 2_665 ? N2 Rh2 N2 173.3(3) . 2_665 y N2 Rh2 N2 89.80(2) . 3_655 y N2 Rh2 N2 89.80(2) 2_665 3_655 ? N2 Rh2 Rh1 86.63(16) 4_565 . ? N2 Rh2 Rh1 86.64(16) . . ? N2 Rh2 Rh1 86.63(16) 2_665 . ? N2 Rh2 Rh1 86.63(16) 3_655 . ? N2 Rh2 Br1 93.37(16) 4_565 1_556 ? N2 Rh2 Br1 93.36(16) . 1_556 ? N2 Rh2 Br1 93.36(16) 2_665 1_556 ? N2 Rh2 Br1 93.36(16) 3_655 1_556 ? Rh1 Rh2 Br1 180.0 . 1_556 ? Rh1 Br1 Rh2 180.0 . 1_554 y C1 N1 C2 116.3(7) . . ? C1 N1 Rh1 119.1(5) . . ? C2 N1 Rh1 124.5(5) . . ? C1 N2 C7 117.6(7) . . ? C1 N2 Rh2 118.9(7) . . ? C7 N2 Rh2 123.4(9) . . ? C1 N3 C5 122.7(7) . . ? C1 N3 C4 122.6(7) . . ? C5 N3 C4 114.3(7) . . ? N1 C1 N2 119.5(7) . . ? N1 C1 N3 120.2(7) . . ? N2 C1 N3 120.3(7) . . ? N1 C2 C3 110.0(7) . . ? C2 C3 C4 108.4(7) . . ? N3 C4 C3 113.1(7) . . ? N3 C5 C6 112.4(7) . . ? C5 C6 C7 110.1(7) . . ? N2 C7 C6 109.5(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 Rh2 N2 22.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.063 _refine_diff_density_min -2.239 _refine_diff_density_rms 0.119 data_TwoH2O _database_code_depnum_ccdc_archive 'CCDC 273862' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Rh2(hpp)(OAc)3{(OAc)(H2hpp)}2], H2O' _chemical_melting_point ? _chemical_formula_moiety 'C17 H27 N3 O10 Rh2, 2(C7 H14 N3), H2 O' _chemical_formula_sum 'C31 H57 N9 O11 Rh2' _chemical_formula_weight 937.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.272(3) _cell_length_b 11.400(3) _cell_length_c 15.856(4) _cell_angle_alpha 80.768(5) _cell_angle_beta 78.128(5) _cell_angle_gamma 87.688(5) _cell_volume 1968.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4632 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9070 _exptl_absorpt_correction_T_max 0.9604 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11314 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.11 _reflns_number_total 6911 _reflns_number_gt 5002 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+2.2900P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6911 _refine_ls_number_parameters 501 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _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 0.23818(3) 0.78075(3) 0.32525(2) 0.02179(12) Uani 1 1 d . . . Rh2 Rh 0.20746(3) 0.74328(3) 0.18711(2) 0.02337(12) Uani 1 1 d . . . N1 N 0.3413(4) 0.6337(3) 0.3312(3) 0.0283(10) Uani 1 1 d . . . N2 N 0.4700(4) 0.4970(4) 0.2613(3) 0.0436(12) Uani 1 1 d . . . N3 N 0.3460(4) 0.6270(4) 0.1865(3) 0.0302(10) Uani 1 1 d . . . N4 N 0.5006(4) 0.8638(4) 0.5828(3) 0.0313(11) Uani 1 1 d . . . H4 H 0.438(5) 0.862(5) 0.581(4) 0.038 Uiso 1 1 d . . . N5 N 0.6981(4) 0.8502(4) 0.5077(3) 0.0330(10) Uani 1 1 d . . . N6 N 0.5366(4) 0.8221(4) 0.4439(3) 0.0291(10) Uani 1 1 d . . . H6 H 0.465(5) 0.827(5) 0.447(4) 0.035 Uiso 1 1 d . . . N7 N 0.1626(4) 0.4447(4) 0.0549(3) 0.0339(11) Uani 1 1 d . . . H7 H 0.161(5) 0.514(5) 0.048(4) 0.041 Uiso 1 1 d . . . N8 N 0.1764(4) 0.2971(4) -0.0323(3) 0.0343(11) Uani 1 1 d . . . N9 N 0.1428(4) 0.4935(4) -0.0863(3) 0.0334(11) Uani 1 1 d . . . H9 H 0.125(5) 0.556(5) -0.082(4) 0.040 Uiso 1 1 d . . . O1 O 0.3824(3) 0.8826(3) 0.2584(2) 0.0281(8) Uani 1 1 d . . . O1W O 0.2698(5) 0.7648(6) -0.2367(3) 0.094(2) Uani 1 1 d D . . H1W H 0.205(6) 0.769(8) -0.193(5) 0.112 Uiso 1 1 d D . . H2W H 0.234(8) 0.750(8) -0.280(5) 0.112 Uiso 1 1 d D . . O2 O 0.3324(3) 0.8736(3) 0.1299(2) 0.0317(8) Uani 1 1 d . . . O3 O 0.1267(3) 0.9305(3) 0.3102(2) 0.0297(8) Uani 1 1 d . . . O4 O 0.0687(3) 0.8711(3) 0.1957(2) 0.0303(8) Uani 1 1 d . . . O5 O 0.0928(3) 0.6724(3) 0.3825(2) 0.0292(8) Uani 1 1 d . . . O6 O 0.0888(3) 0.6145(3) 0.2540(2) 0.0312(8) Uani 1 1 d . . . O7 O 0.2827(3) 0.8261(3) 0.4524(2) 0.0262(8) Uani 1 1 d . . . O8 O 0.2538(3) 0.8511(4) 0.5908(2) 0.0460(11) Uani 1 1 d . . . O9 O 0.1628(3) 0.6968(3) 0.0589(2) 0.0294(8) Uani 1 1 d . . . O10 O 0.1131(3) 0.7287(3) -0.0711(2) 0.0369(9) Uani 1 1 d . . . C1 C 0.3566(5) 0.5754(4) 0.4176(3) 0.0338(12) Uani 1 1 d . . . H1A H 0.2780 0.5728 0.4581 0.041 Uiso 1 1 calc R . . H1B H 0.4116 0.6226 0.4389 0.041 Uiso 1 1 calc R . . C2 C 0.4064(5) 0.4506(4) 0.4172(4) 0.0385(14) Uani 1 1 d . . . H2A H 0.4333 0.4221 0.4719 0.046 Uiso 1 1 calc R . . H2B H 0.3434 0.3972 0.4118 0.046 Uiso 1 1 calc R . . C3 C 0.5114(5) 0.4517(5) 0.3414(4) 0.0424(14) Uani 1 1 d . . . H3A H 0.5759 0.5024 0.3482 0.051 Uiso 1 1 calc R . . H3B H 0.5441 0.3711 0.3391 0.051 Uiso 1 1 calc R . . C4 C 0.3857(5) 0.5871(4) 0.2598(3) 0.0284(11) Uani 1 1 d . . . C5 C 0.5247(6) 0.4503(5) 0.1827(4) 0.0490(16) Uani 1 1 d . . . H5A H 0.4760 0.3846 0.1757 0.059 Uiso 1 1 calc R . . H5B H 0.6061 0.4196 0.1870 0.059 Uiso 1 1 calc R . . C6 C 0.5328(5) 0.5466(6) 0.1047(4) 0.0535(17) Uani 1 1 d . . . H6A H 0.5894 0.6078 0.1081 0.064 Uiso 1 1 calc R . . H6B H 0.5634 0.5130 0.0511 0.064 Uiso 1 1 calc R . . C7 C 0.4109(5) 0.6006(5) 0.1023(4) 0.0397(14) Uani 1 1 d . . . H7A H 0.4201 0.6743 0.0602 0.048 Uiso 1 1 calc R . . H7B H 0.3622 0.5461 0.0816 0.048 Uiso 1 1 calc R . . C8 C 0.3982(5) 0.9072(5) 0.1764(3) 0.0322(12) Uani 1 1 d . . . C9 C 0.5026(6) 0.9865(6) 0.1299(4) 0.0523(17) Uani 1 1 d . . . H9A H 0.5219 1.0365 0.1693 0.078 Uiso 1 1 calc R . . H9B H 0.4804 1.0361 0.0797 0.078 Uiso 1 1 calc R . . H9C H 0.5727 0.9382 0.1107 0.078 Uiso 1 1 calc R . . C10 C 0.0652(4) 0.9410(4) 0.2505(3) 0.0277(11) Uani 1 1 d . . . C11 C -0.0173(5) 1.0480(5) 0.2436(3) 0.0368(13) Uani 1 1 d . . . H11A H -0.0509 1.0523 0.1915 0.055 Uiso 1 1 calc R . . H11B H 0.0284 1.1194 0.2402 0.055 Uiso 1 1 calc R . . H11C H -0.0826 1.0410 0.2945 0.055 Uiso 1 1 calc R . . C12 C 0.0563(5) 0.6073(5) 0.3359(4) 0.0324(12) Uani 1 1 d . . . C13 C -0.0343(6) 0.5129(6) 0.3820(4) 0.0581(19) Uani 1 1 d . . . H13A H -0.0560 0.4693 0.3397 0.087 Uiso 1 1 calc R . . H13B H -0.1063 0.5499 0.4120 0.087 Uiso 1 1 calc R . . H13C H 0.0010 0.4587 0.4240 0.087 Uiso 1 1 calc R . . C14 C 0.2150(5) 0.8360(4) 0.5246(3) 0.0291(12) Uani 1 1 d . . . C15 C 0.0800(5) 0.8320(5) 0.5329(4) 0.0394(14) Uani 1 1 d . . . H15A H 0.0563 0.8878 0.4863 0.059 Uiso 1 1 calc R . . H15B H 0.0401 0.8532 0.5888 0.059 Uiso 1 1 calc R . . H15C H 0.0565 0.7524 0.5291 0.059 Uiso 1 1 calc R . . C16 C 0.1482(5) 0.7644(4) -0.0091(3) 0.0298(12) Uani 1 1 d . . . C17 C 0.1709(6) 0.8959(5) -0.0180(4) 0.0456(15) Uani 1 1 d . . . H17A H 0.2524 0.9080 -0.0102 0.068 Uiso 1 1 calc R . . H17B H 0.1128 0.9295 0.0261 0.068 Uiso 1 1 calc R . . H17C H 0.1621 0.9346 -0.0755 0.068 Uiso 1 1 calc R . . C18 C 0.5369(5) 0.8964(5) 0.6586(4) 0.0374(13) Uani 1 1 d . . . H18A H 0.4750 0.8713 0.7110 0.045 Uiso 1 1 calc R . . H18B H 0.5452 0.9829 0.6515 0.045 Uiso 1 1 calc R . . C19 C 0.6565(5) 0.8366(5) 0.6681(4) 0.0410(14) Uani 1 1 d . . . H19A H 0.6450 0.7505 0.6837 0.049 Uiso 1 1 calc R . . H19B H 0.6862 0.8650 0.7151 0.049 Uiso 1 1 calc R . . C20 C 0.7486(5) 0.8635(5) 0.5838(4) 0.0405(14) Uani 1 1 d . . . H20A H 0.7774 0.9450 0.5774 0.049 Uiso 1 1 calc R . . H20B H 0.8183 0.8097 0.5862 0.049 Uiso 1 1 calc R . . C21 C 0.5777(5) 0.8461(4) 0.5120(3) 0.0259(11) Uani 1 1 d . . . C22 C 0.7869(5) 0.8436(5) 0.4275(4) 0.0400(14) Uani 1 1 d . . . H22A H 0.8239 0.7642 0.4305 0.048 Uiso 1 1 calc R . . H22B H 0.8512 0.9014 0.4219 0.048 Uiso 1 1 calc R . . C23 C 0.7291(5) 0.8689(5) 0.3481(4) 0.0422(14) Uani 1 1 d . . . H23A H 0.7094 0.9537 0.3365 0.051 Uiso 1 1 calc R . . H23B H 0.7859 0.8482 0.2969 0.051 Uiso 1 1 calc R . . C24 C 0.6152(5) 0.7967(5) 0.3642(4) 0.0374(13) Uani 1 1 d . . . H24A H 0.5738 0.8172 0.3151 0.045 Uiso 1 1 calc R . . H24B H 0.6356 0.7118 0.3697 0.045 Uiso 1 1 calc R . . C25 C 0.1678(6) 0.3608(5) 0.1329(4) 0.0449(15) Uani 1 1 d . . . H25A H 0.0856 0.3372 0.1636 0.054 Uiso 1 1 calc R . . H25B H 0.2061 0.3978 0.1722 0.054 Uiso 1 1 calc R . . C26 C 0.2395(6) 0.2540(5) 0.1080(4) 0.0488(16) Uani 1 1 d . . . H26A H 0.2361 0.1932 0.1597 0.059 Uiso 1 1 calc R . . H26B H 0.3245 0.2760 0.0850 0.059 Uiso 1 1 calc R . . C27 C 0.1894(6) 0.2043(5) 0.0400(4) 0.0465(15) Uani 1 1 d . . . H27A H 0.2440 0.1420 0.0180 0.056 Uiso 1 1 calc R . . H27B H 0.1103 0.1685 0.0665 0.056 Uiso 1 1 calc R . . C28 C 0.1592(4) 0.4115(4) -0.0213(4) 0.0298(12) Uani 1 1 d . . . C29 C 0.1576(5) 0.2593(5) -0.1132(4) 0.0441(15) Uani 1 1 d . . . H29A H 0.0722 0.2391 -0.1066 0.053 Uiso 1 1 calc R . . H29B H 0.2063 0.1878 -0.1232 0.053 Uiso 1 1 calc R . . C30 C 0.1922(6) 0.3546(5) -0.1900(4) 0.0438(15) Uani 1 1 d . . . H30A H 0.1693 0.3309 -0.2412 0.053 Uiso 1 1 calc R . . H30B H 0.2802 0.3654 -0.2029 0.053 Uiso 1 1 calc R . . C31 C 0.1298(6) 0.4699(5) -0.1719(4) 0.0425(14) Uani 1 1 d . . . H31A H 0.1656 0.5350 -0.2171 0.051 Uiso 1 1 calc R . . H31B H 0.0436 0.4653 -0.1734 0.051 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 0.0233(2) 0.0250(2) 0.0206(2) -0.00859(16) -0.00881(16) 0.00041(16) Rh2 0.0268(2) 0.0266(2) 0.0205(2) -0.00856(17) -0.00960(17) -0.00080(17) N1 0.035(2) 0.029(2) 0.023(2) -0.0086(18) -0.0088(19) 0.0027(19) N2 0.049(3) 0.047(3) 0.038(3) -0.016(2) -0.015(2) 0.025(2) N3 0.028(2) 0.040(3) 0.026(2) -0.014(2) -0.0086(19) 0.009(2) N4 0.027(2) 0.036(2) 0.036(3) -0.014(2) -0.012(2) 0.000(2) N5 0.026(2) 0.035(2) 0.039(3) -0.006(2) -0.011(2) -0.0048(19) N6 0.022(2) 0.037(2) 0.028(2) -0.007(2) -0.006(2) 0.002(2) N7 0.039(3) 0.033(2) 0.032(3) -0.010(2) -0.007(2) -0.002(2) N8 0.034(3) 0.032(2) 0.039(3) -0.009(2) -0.008(2) -0.002(2) N9 0.040(3) 0.029(2) 0.039(3) -0.017(2) -0.017(2) 0.001(2) O1 0.0289(19) 0.0332(19) 0.025(2) -0.0070(15) -0.0089(15) -0.0074(15) O1W 0.062(4) 0.144(6) 0.053(4) 0.017(4) 0.004(3) 0.052(4) O2 0.036(2) 0.036(2) 0.026(2) -0.0070(16) -0.0097(16) -0.0097(16) O3 0.031(2) 0.035(2) 0.028(2) -0.0111(16) -0.0133(16) 0.0079(16) O4 0.032(2) 0.036(2) 0.029(2) -0.0106(16) -0.0170(16) 0.0041(16) O5 0.032(2) 0.0345(19) 0.0236(19) -0.0078(16) -0.0085(16) -0.0093(16) O6 0.037(2) 0.035(2) 0.026(2) -0.0080(16) -0.0124(17) -0.0072(16) O7 0.0247(18) 0.037(2) 0.0197(19) -0.0117(15) -0.0065(15) 0.0007(15) O8 0.031(2) 0.089(3) 0.025(2) -0.022(2) -0.0083(17) -0.005(2) O9 0.042(2) 0.0286(19) 0.0222(19) -0.0051(15) -0.0150(16) -0.0040(16) O10 0.055(3) 0.036(2) 0.026(2) -0.0088(16) -0.0194(18) -0.0021(18) C1 0.043(3) 0.031(3) 0.029(3) -0.005(2) -0.012(3) -0.003(2) C2 0.050(4) 0.026(3) 0.042(3) -0.002(2) -0.019(3) 0.001(3) C3 0.045(3) 0.033(3) 0.054(4) -0.013(3) -0.020(3) 0.013(3) C4 0.028(3) 0.029(3) 0.029(3) -0.007(2) -0.007(2) 0.004(2) C5 0.043(4) 0.049(4) 0.060(4) -0.027(3) -0.010(3) 0.016(3) C6 0.033(3) 0.089(5) 0.042(4) -0.024(4) -0.005(3) 0.004(3) C7 0.034(3) 0.057(4) 0.034(3) -0.026(3) -0.006(3) 0.005(3) C8 0.036(3) 0.039(3) 0.021(3) -0.004(2) -0.003(2) -0.002(2) C9 0.056(4) 0.072(4) 0.030(3) -0.005(3) -0.006(3) -0.033(3) C10 0.024(3) 0.030(3) 0.027(3) -0.003(2) -0.003(2) -0.004(2) C11 0.037(3) 0.041(3) 0.031(3) -0.007(3) -0.007(3) 0.013(3) C12 0.031(3) 0.036(3) 0.033(3) -0.001(2) -0.015(3) -0.009(2) C13 0.079(5) 0.061(4) 0.036(4) 0.000(3) -0.012(3) -0.040(4) C14 0.027(3) 0.032(3) 0.032(3) -0.011(2) -0.009(2) 0.002(2) C15 0.025(3) 0.058(4) 0.038(3) -0.021(3) -0.003(2) -0.004(3) C16 0.027(3) 0.034(3) 0.030(3) -0.010(2) -0.005(2) -0.002(2) C17 0.066(4) 0.038(3) 0.039(3) -0.002(3) -0.025(3) -0.009(3) C18 0.044(3) 0.038(3) 0.038(3) -0.014(3) -0.018(3) 0.001(3) C19 0.046(4) 0.041(3) 0.044(4) -0.006(3) -0.027(3) -0.007(3) C20 0.032(3) 0.040(3) 0.054(4) -0.001(3) -0.023(3) -0.006(3) C21 0.027(3) 0.020(2) 0.032(3) -0.002(2) -0.011(2) 0.001(2) C22 0.024(3) 0.042(3) 0.052(4) -0.007(3) -0.004(3) -0.003(2) C23 0.040(3) 0.047(3) 0.038(3) -0.015(3) 0.002(3) -0.001(3) C24 0.036(3) 0.040(3) 0.037(3) -0.012(3) -0.005(3) -0.002(3) C25 0.046(4) 0.049(4) 0.038(4) -0.003(3) -0.008(3) 0.000(3) C26 0.052(4) 0.048(4) 0.047(4) 0.001(3) -0.016(3) -0.002(3) C27 0.052(4) 0.034(3) 0.054(4) -0.008(3) -0.012(3) -0.001(3) C28 0.025(3) 0.030(3) 0.037(3) -0.009(2) -0.007(2) -0.005(2) C29 0.038(3) 0.047(3) 0.054(4) -0.029(3) -0.008(3) -0.003(3) C30 0.048(4) 0.053(4) 0.040(4) -0.027(3) -0.017(3) 0.003(3) C31 0.052(4) 0.048(3) 0.036(3) -0.018(3) -0.018(3) 0.000(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 N1 2.002(4) . ? Rh1 O1 2.040(3) . ? Rh1 O5 2.056(3) . ? Rh1 O3 2.091(3) . ? Rh1 O7 2.314(3) . ? Rh1 Rh2 2.3927(7) . ? Rh2 N3 2.007(4) . ? Rh2 O6 2.036(3) . ? Rh2 O2 2.056(3) . ? Rh2 O4 2.093(3) . ? Rh2 O9 2.336(3) . ? N1 C4 1.325(6) . ? N1 C1 1.465(6) . ? N2 C4 1.371(6) . ? N2 C5 1.445(7) . ? N2 C3 1.453(7) . ? N3 C4 1.337(6) . ? N3 C7 1.455(6) . ? N4 C21 1.309(7) . ? N4 C18 1.451(6) . ? N5 C21 1.347(6) . ? N5 C22 1.458(7) . ? N5 C20 1.468(7) . ? N6 C21 1.329(6) . ? N6 C24 1.449(7) . ? N7 C28 1.332(7) . ? N7 C25 1.447(7) . ? N8 C28 1.345(6) . ? N8 C27 1.457(7) . ? N8 C29 1.473(7) . ? N9 C28 1.313(7) . ? N9 C31 1.463(7) . ? O1 C8 1.261(6) . ? O2 C8 1.257(6) . ? O3 C10 1.271(6) . ? O4 C10 1.264(6) . ? O5 C12 1.262(6) . ? O6 C12 1.264(6) . ? O7 C14 1.258(6) . ? O8 C14 1.254(6) . ? O9 C16 1.257(6) . ? O10 C16 1.261(6) . ? C1 C2 1.508(7) . ? C2 C3 1.502(8) . ? C5 C6 1.506(9) . ? C6 C7 1.488(8) . ? C8 C9 1.503(7) . ? C10 C11 1.507(7) . ? C12 C13 1.505(7) . ? C14 C15 1.502(7) . ? C16 C17 1.510(7) . ? C18 C19 1.510(7) . ? C19 C20 1.511(8) . ? C22 C23 1.517(8) . ? C23 C24 1.507(7) . ? C25 C26 1.495(8) . ? C26 C27 1.508(8) . ? C29 C30 1.494(8) . ? C30 C31 1.506(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 O1 91.83(16) . . ? N1 Rh1 O5 86.87(16) . . ? O1 Rh1 O5 174.88(12) . . ? N1 Rh1 O3 175.41(14) . . ? O1 Rh1 O3 88.59(14) . . ? O5 Rh1 O3 92.32(14) . . ? N1 Rh1 O7 91.80(14) . . ? O1 Rh1 O7 87.72(12) . . ? O5 Rh1 O7 97.26(12) . . ? O3 Rh1 O7 92.78(12) . . ? N1 Rh1 Rh2 88.04(11) . . ? O1 Rh1 Rh2 87.32(9) . . ? O5 Rh1 Rh2 87.68(9) . . ? O3 Rh1 Rh2 87.41(9) . . ? O7 Rh1 Rh2 175.03(9) . . ? N3 Rh2 O6 90.75(16) . . ? N3 Rh2 O2 87.87(16) . . ? O6 Rh2 O2 174.80(13) . . ? N3 Rh2 O4 175.06(14) . . ? O6 Rh2 O4 90.71(14) . . ? O2 Rh2 O4 90.27(14) . . ? N3 Rh2 O9 93.52(14) . . ? O6 Rh2 O9 87.70(12) . . ? O2 Rh2 O9 97.38(13) . . ? O4 Rh2 O9 91.25(12) . . ? N3 Rh2 Rh1 87.66(11) . . ? O6 Rh2 Rh1 87.41(9) . . ? O2 Rh2 Rh1 87.53(9) . . ? O4 Rh2 Rh1 87.70(9) . . ? O9 Rh2 Rh1 174.98(9) . . ? C4 N1 C1 121.9(4) . . ? C4 N1 Rh1 120.5(3) . . ? C1 N1 Rh1 117.5(3) . . ? C4 N2 C5 120.9(5) . . ? C4 N2 C3 120.3(4) . . ? C5 N2 C3 118.7(4) . . ? C4 N3 C7 121.4(4) . . ? C4 N3 Rh2 120.6(3) . . ? C7 N3 Rh2 117.5(3) . . ? C21 N4 C18 123.3(4) . . ? C21 N5 C22 122.8(4) . . ? C21 N5 C20 121.8(5) . . ? C22 N5 C20 115.4(4) . . ? C21 N6 C24 123.3(4) . . ? C28 N7 C25 123.0(5) . . ? C28 N8 C27 121.4(5) . . ? C28 N8 C29 120.0(4) . . ? C27 N8 C29 117.5(4) . . ? C28 N9 C31 124.7(4) . . ? C8 O1 Rh1 119.3(3) . . ? C8 O2 Rh2 117.9(3) . . ? C10 O3 Rh1 118.3(3) . . ? C10 O4 Rh2 117.7(3) . . ? C12 O5 Rh1 117.6(3) . . ? C12 O6 Rh2 119.3(3) . . ? C14 O7 Rh1 130.8(3) . . ? C16 O9 Rh2 129.7(3) . . ? N1 C1 C2 112.8(4) . . ? C3 C2 C1 108.5(5) . . ? N2 C3 C2 108.9(5) . . ? N1 C4 N3 119.4(4) . . ? N1 C4 N2 120.4(4) . . ? N3 C4 N2 120.2(4) . . ? N2 C5 C6 110.0(5) . . ? C7 C6 C5 109.8(5) . . ? N3 C7 C6 113.5(5) . . ? O2 C8 O1 125.7(5) . . ? O2 C8 C9 116.6(5) . . ? O1 C8 C9 117.6(5) . . ? O4 C10 O3 125.9(4) . . ? O4 C10 C11 117.2(4) . . ? O3 C10 C11 116.9(4) . . ? O5 C12 O6 125.8(5) . . ? O5 C12 C13 117.0(5) . . ? O6 C12 C13 117.2(5) . . ? O8 C14 O7 123.6(5) . . ? O8 C14 C15 117.4(5) . . ? O7 C14 C15 119.0(4) . . ? O9 C16 O10 123.4(5) . . ? O9 C16 C17 119.5(4) . . ? O10 C16 C17 117.2(5) . . ? N4 C18 C19 109.0(4) . . ? C18 C19 C20 110.3(5) . . ? N5 C20 C19 112.1(4) . . ? N4 C21 N6 119.5(5) . . ? N4 C21 N5 120.9(5) . . ? N6 C21 N5 119.6(5) . . ? N5 C22 C23 111.4(4) . . ? C24 C23 C22 109.4(5) . . ? N6 C24 C23 108.8(4) . . ? N7 C25 C26 109.1(5) . . ? C25 C26 C27 110.3(5) . . ? N8 C27 C26 111.0(4) . . ? N9 C28 N7 118.6(5) . . ? N9 C28 N8 120.8(5) . . ? N7 C28 N8 120.6(5) . . ? N8 C29 C30 111.5(4) . . ? C29 C30 C31 110.5(5) . . ? N9 C31 C30 110.0(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.351 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.100 data_Two3CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 273863' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Rh2(OAc)4[(OAc)(H2hpp)]2, 3CH2Cl2' _chemical_melting_point ? _chemical_formula_moiety 'C12 H18 O12 Rh2, 2(C7 H14 N3), 3(C H2 Cl2)' _chemical_formula_sum 'C29 H52 Cl6 N6 O12 Rh2' _chemical_formula_weight 1095.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M '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 17.368(8) _cell_length_b 14.227(6) _cell_length_c 20.933(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.792(7) _cell_angle_gamma 90.00 _cell_volume 4925(4) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5313 _cell_measurement_theta_min 5 _cell_measurement_theta_max 45 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8220 _exptl_absorpt_correction_T_max 0.9023 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11103 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3215 _reflns_number_gt 2588 _reflns_threshold_expression I>2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1054P)^2^+50.9944P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3215 _refine_ls_number_parameters 300 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.2021 _refine_ls_wR_factor_gt 0.1901 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.04740(4) 0.43241(5) 0.30547(3) 0.0536(3) Uani 1 1 d . . . O1 O 0.0442(4) 0.5749(4) 0.3017(3) 0.0670(18) Uani 1 1 d . . . O2 O -0.1381(3) 0.4317(4) 0.2379(3) 0.0606(16) Uani 1 1 d . . . O3 O 0.0457(3) 0.2892(5) 0.3020(3) 0.0632(16) Uani 1 1 d . . . O4 O 0.1430(3) 0.4256(4) 0.4090(3) 0.0511(14) Uani 1 1 d . . . O5 O 0.2114(4) 0.4599(5) 0.5123(3) 0.081(2) Uani 1 1 d . . . O6 O -0.0492(3) 0.4292(5) 0.3423(3) 0.0628(17) Uani 1 1 d . . . N3 N 0.2613(4) 0.2914(5) 0.3955(3) 0.062(2) Uani 1 1 d . . . H3A H 0.2223 0.3291 0.3965 0.075 Uiso 1 1 calc R A 1 N4 N 0.3903(4) 0.2356(6) 0.4466(4) 0.067(2) Uani 1 1 d . . . N5 N 0.3313(4) 0.3416(5) 0.5001(3) 0.0611(19) Uani 1 1 d . . . H5A H 0.2903 0.3781 0.4976 0.073 Uiso 1 1 calc R B . C5 C 0.0000 0.6154(11) 0.2500 0.070(4) Uani 1 2 d S . . C6 C 0.0000 0.7202(11) 0.2500 0.095(5) Uani 1 2 d S . . H6A H 0.0362 0.7429 0.2922 0.142 Uiso 0.50 1 calc PR . . H6B H -0.0543 0.7429 0.2445 0.142 Uiso 0.50 1 calc PR . . H6C H 0.0181 0.7429 0.2133 0.142 Uiso 0.50 1 calc PR . . C7 C -0.1195(5) 0.4264(7) 0.3018(5) 0.061(2) Uani 1 1 d . . . C8 C -0.1875(6) 0.4145(9) 0.3310(5) 0.079(3) Uani 1 1 d . . . H8A H -0.1661 0.4120 0.3795 0.119 Uiso 1 1 calc R . . H8B H -0.2162 0.3566 0.3145 0.119 Uiso 1 1 calc R . . H8C H -0.2245 0.4672 0.3179 0.119 Uiso 1 1 calc R . . C9 C 0.0000 0.2497(10) 0.2500 0.063(3) Uani 1 2 d S . . C10 C 0.0000 0.1430(11) 0.2500 0.088(5) Uani 1 2 d S . . H10A H -0.0366 0.1203 0.2080 0.132 Uiso 0.50 1 calc PR . . H10B H -0.0175 0.1203 0.2870 0.132 Uiso 0.50 1 calc PR . . H10C H 0.0542 0.1203 0.2550 0.132 Uiso 0.50 1 calc PR . . C11 C 0.1539(5) 0.4703(7) 0.4620(4) 0.053(2) Uani 1 1 d . . . C12 C 0.0910(6) 0.5447(7) 0.4626(5) 0.072(3) Uani 1 1 d . . . H12A H 0.1062 0.5758 0.5059 0.108 Uiso 1 1 calc R . . H12B H 0.0386 0.5149 0.4547 0.108 Uiso 1 1 calc R . . H12C H 0.0880 0.5905 0.4277 0.108 Uiso 1 1 calc R . . C13 C 0.2508(6) 0.2328(11) 0.3363(6) 0.103(4) Uani 0.60 1 d PD B 1 H13A H 0.2174 0.2661 0.2965 0.123 Uiso 0.60 1 calc PR B 1 H13B H 0.2227 0.1747 0.3410 0.123 Uiso 0.60 1 calc PR B 1 C14 C 0.3305(8) 0.2092(17) 0.3273(9) 0.085(6) Uani 0.60 1 d PD B 1 H14A H 0.3539 0.2657 0.3138 0.102 Uiso 0.60 1 calc PR B 1 H14B H 0.3229 0.1623 0.2916 0.102 Uiso 0.60 1 calc PR B 1 C15 C 0.3873(7) 0.1715(8) 0.3910(5) 0.086(3) Uani 0.60 1 d PD B 1 H15A H 0.3690 0.1093 0.4005 0.103 Uiso 0.60 1 calc PR B 1 H15B H 0.4415 0.1647 0.3864 0.103 Uiso 0.60 1 calc PR B 1 C13' C 0.2508(6) 0.2328(11) 0.3363(6) 0.103(4) Uani 0.40 1 d P B 2 H13C H 0.1959 0.2068 0.3223 0.123 Uiso 0.40 1 calc PR B 2 H13D H 0.2569 0.2717 0.2995 0.123 Uiso 0.40 1 calc PR B 2 C14' C 0.3070(11) 0.158(2) 0.3481(15) 0.114(15) Uani 0.40 1 d PD B 2 H14C H 0.3108 0.1382 0.3044 0.137 Uiso 0.40 1 calc PR B 2 H14D H 0.2838 0.1058 0.3662 0.137 Uiso 0.40 1 calc PR B 2 C15' C 0.3873(7) 0.1715(8) 0.3910(5) 0.086(3) Uani 0.40 1 d P B 2 H15C H 0.4207 0.1968 0.3649 0.103 Uiso 0.40 1 calc PR B 2 H15D H 0.4099 0.1105 0.4093 0.103 Uiso 0.40 1 calc PR B 2 C16 C 0.3278(5) 0.2898(6) 0.4477(4) 0.051(2) Uani 1 1 d . B . C17 C 0.4636(6) 0.2309(8) 0.5049(6) 0.081(3) Uani 1 1 d . B . H17A H 0.5110 0.2227 0.4893 0.097 Uiso 1 1 calc R . . H17B H 0.4602 0.1764 0.5325 0.097 Uiso 1 1 calc R . . C18 C 0.4736(6) 0.3178(9) 0.5461(6) 0.091(3) Uani 1 1 d . . . H18A H 0.4891 0.3698 0.5219 0.109 Uiso 1 1 calc R B . H18B H 0.5173 0.3084 0.5882 0.109 Uiso 1 1 calc R . . C19 C 0.3977(6) 0.3432(8) 0.5617(5) 0.085(3) Uani 1 1 d . B . H19A H 0.3878 0.2982 0.5938 0.102 Uiso 1 1 calc R . . H19B H 0.4029 0.4061 0.5818 0.102 Uiso 1 1 calc R . . C1S C 0.7030(10) 0.4701(12) 0.6329(7) 0.136(6) Uani 1 1 d . . . H1SA H 0.6990 0.4747 0.5853 0.164 Uiso 1 1 calc R . . H1SB H 0.7521 0.5029 0.6592 0.164 Uiso 1 1 calc R . . Cl1 Cl 0.7067(5) 0.3541(5) 0.6568(4) 0.250(4) Uani 1 1 d . . . Cl2 Cl 0.6175(4) 0.5210(5) 0.6471(4) 0.203(3) Uani 1 1 d . . . C2S C 0.6686(9) 0.3777(15) 0.4039(7) 0.073(9) Uani 0.34 1 d PD C 1 H2SA H 0.6908 0.3179 0.3945 0.088 Uiso 0.34 1 calc PR C 1 H2SB H 0.7132 0.4194 0.4275 0.088 Uiso 0.34 1 calc PR C 1 Cl3 Cl 0.6007(12) 0.3603(13) 0.4512(10) 0.188(8) Uani 0.34 1 d PD C 1 Cl4 Cl 0.6060(4) 0.4309(5) 0.3288(4) 0.076(2) Uani 0.34 1 d PD C 1 C2S' C 0.664(3) 0.327(5) 0.4138(16) 0.08(2) Uani 0.16 1 d PDU D 2 H2SC H 0.6531 0.2665 0.3901 0.097 Uiso 0.16 1 calc PR D 2 H2SD H 0.7090 0.3578 0.4037 0.097 Uiso 0.16 1 calc PR D 2 Cl3' Cl 0.6850(13) 0.3101(15) 0.5025(14) 0.118(8) Uani 0.16 1 d PD D 2 Cl4' Cl 0.5751(17) 0.4001(14) 0.3902(14) 0.126(9) Uani 0.16 1 d PD D 2 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 0.0380(5) 0.0786(6) 0.0387(5) -0.0025(3) 0.0035(3) 0.0029(3) O1 0.074(5) 0.053(4) 0.063(4) -0.010(3) 0.006(4) 0.000(3) O2 0.037(3) 0.094(5) 0.046(4) -0.001(3) 0.005(3) -0.003(3) O3 0.067(4) 0.076(4) 0.039(3) 0.001(3) 0.005(3) 0.001(3) O4 0.034(3) 0.072(4) 0.040(3) -0.004(3) 0.001(2) 0.013(2) O5 0.060(4) 0.117(6) 0.048(4) -0.019(4) -0.007(3) 0.039(4) O6 0.040(3) 0.103(5) 0.041(3) -0.005(3) 0.006(3) 0.002(3) N3 0.054(4) 0.080(5) 0.050(4) -0.004(4) 0.011(4) 0.021(4) N4 0.062(5) 0.070(5) 0.065(5) 0.000(4) 0.015(4) 0.020(4) N5 0.056(4) 0.070(5) 0.051(4) -0.002(4) 0.007(4) 0.021(4) C5 0.060(8) 0.093(11) 0.048(8) 0.000 0.003(7) 0.000 C6 0.120(13) 0.075(11) 0.081(11) 0.000 0.020(10) 0.000 C7 0.046(5) 0.081(6) 0.050(6) -0.009(4) 0.007(4) 0.000(4) C8 0.057(6) 0.119(9) 0.063(6) -0.010(6) 0.020(5) -0.009(6) C9 0.067(8) 0.075(9) 0.045(8) 0.000 0.016(7) 0.000 C10 0.117(13) 0.079(11) 0.057(9) 0.000 0.010(8) 0.000 C11 0.040(5) 0.078(6) 0.035(5) -0.013(4) 0.000(4) 0.010(4) C12 0.058(6) 0.090(7) 0.058(6) -0.014(5) 0.005(5) 0.028(5) C13 0.072(7) 0.156(12) 0.070(7) -0.050(8) 0.008(6) 0.008(7) C14 0.114(15) 0.072(14) 0.068(12) 0.021(10) 0.024(11) 0.032(11) C15 0.081(7) 0.095(8) 0.077(7) -0.011(6) 0.017(6) 0.033(6) C13' 0.072(7) 0.156(12) 0.070(7) -0.050(8) 0.008(6) 0.008(7) C14' 0.22(4) 0.044(17) 0.054(18) -0.002(14) 0.00(2) 0.08(2) C15' 0.081(7) 0.095(8) 0.077(7) -0.011(6) 0.017(6) 0.033(6) C16 0.046(5) 0.058(5) 0.049(5) 0.005(4) 0.012(4) 0.004(4) C17 0.052(5) 0.084(7) 0.092(8) 0.002(6) 0.000(5) 0.019(5) C18 0.059(6) 0.107(9) 0.089(8) -0.017(7) -0.001(6) 0.007(6) C19 0.072(7) 0.096(8) 0.068(7) -0.009(6) -0.006(5) 0.031(6) C1S 0.123(12) 0.179(16) 0.087(9) 0.035(10) 0.001(9) -0.061(11) Cl1 0.249(7) 0.165(5) 0.233(7) 0.074(5) -0.080(6) -0.058(5) Cl2 0.207(6) 0.208(6) 0.226(7) -0.046(5) 0.115(5) -0.107(5) C2S 0.09(2) 0.031(14) 0.13(3) -0.027(15) 0.07(2) -0.048(14) Cl3 0.236(18) 0.196(15) 0.216(17) -0.067(13) 0.192(16) -0.103(14) Cl4 0.063(4) 0.060(4) 0.094(6) -0.016(4) 0.008(4) -0.008(3) C2S' 0.07(2) 0.09(2) 0.08(2) 0.000(10) 0.033(12) -0.013(10) Cl3' 0.074(12) 0.087(14) 0.19(3) 0.004(14) 0.039(14) -0.023(10) Cl4' 0.17(2) 0.062(11) 0.12(2) -0.037(12) 0.018(18) -0.045(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O1 2.029(6) . ? Rh1 O3 2.039(7) . ? Rh1 O2 2.044(6) 2 ? Rh1 O6 2.050(6) . ? Rh1 O4 2.294(5) . ? Rh1 Rh1 2.4017(15) 2 ? O1 C5 1.259(9) . ? O2 C7 1.278(11) . ? O2 Rh1 2.044(6) 2 ? O3 C9 1.266(8) . ? O4 C11 1.242(10) . ? O5 C11 1.218(10) . ? O6 C7 1.256(10) . ? N3 C16 1.325(10) . ? N3 C13 1.458(12) . ? N4 C16 1.337(11) . ? N4 C15 1.467(13) . ? N4 C17 1.471(12) . ? N5 C16 1.308(11) . ? N5 C19 1.444(12) . ? C5 O1 1.259(9) 2 ? C5 C6 1.49(2) . ? C7 C8 1.496(13) . ? C9 O3 1.266(8) 2 ? C9 C10 1.52(2) . ? C11 C12 1.524(12) . ? C13 C14 1.492(15) . ? C14 C15 1.495(14) . ? C17 C18 1.487(15) . ? C18 C19 1.496(15) . ? C1S Cl1 1.720(17) . ? C1S Cl2 1.757(19) . ? C2S Cl3 1.773(8) . ? C2S Cl4 1.784(8) . ? C2S' Cl3' 1.796(9) . ? C2S' Cl4' 1.799(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Rh1 O3 175.8(2) . . ? O1 Rh1 O2 90.2(3) . 2 ? O3 Rh1 O2 89.1(2) . 2 ? O1 Rh1 O6 91.2(3) . . ? O3 Rh1 O6 89.2(2) . . ? O2 Rh1 O6 175.6(2) 2 . ? O1 Rh1 O4 94.7(2) . . ? O3 Rh1 O4 89.4(2) . . ? O2 Rh1 O4 89.2(2) 2 . ? O6 Rh1 O4 94.8(2) . . ? O1 Rh1 Rh1 87.71(17) . 2 ? O3 Rh1 Rh1 88.14(15) . 2 ? O2 Rh1 Rh1 87.92(16) 2 2 ? O6 Rh1 Rh1 88.02(16) . 2 ? O4 Rh1 Rh1 176.28(13) . 2 ? C5 O1 Rh1 119.5(8) . . ? C7 O2 Rh1 118.9(5) . 2 ? C9 O3 Rh1 118.2(7) . . ? C11 O4 Rh1 133.8(5) . . ? C7 O6 Rh1 119.1(6) . . ? C16 N3 C13 122.8(7) . . ? C16 N4 C15 122.7(8) . . ? C16 N4 C17 120.9(8) . . ? C15 N4 C17 116.2(7) . . ? C16 N5 C19 125.4(7) . . ? O1 C5 O1 125.6(14) . 2 ? O1 C5 C6 117.2(7) . . ? O1 C5 C6 117.2(7) 2 . ? O6 C7 O2 125.9(8) . . ? O6 C7 C8 117.0(8) . . ? O2 C7 C8 117.1(8) . . ? O3 C9 O3 127.3(13) . 2 ? O3 C9 C10 116.3(6) . . ? O3 C9 C10 116.3(6) 2 . ? O5 C11 O4 124.8(8) . . ? O5 C11 C12 118.5(7) . . ? O4 C11 C12 116.6(7) . . ? N3 C13 C14 110.8(11) . . ? C13 C14 C15 110.7(15) . . ? N4 C15 C14 109.7(10) . . ? N5 C16 N3 119.2(7) . . ? N5 C16 N4 120.6(7) . . ? N3 C16 N4 120.2(8) . . ? N4 C17 C18 111.2(8) . . ? C17 C18 C19 112.0(9) . . ? N5 C19 C18 108.5(9) . . ? Cl1 C1S Cl2 107.7(9) . . ? Cl3 C2S Cl4 102.8(11) . . ? Cl3' C2S' Cl4' 104(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.763 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.128 data_Three2CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 273864' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Rh2(hpp)(OAc)3(Hhpp)2, 2CH2Cl2' _chemical_melting_point ? _chemical_formula_moiety 'C27 H47 N9 O6 Rh2, 2(C H2 Cl2)' _chemical_formula_sum 'C29 H51 Cl4 N9 O6 Rh2' _chemical_formula_weight 969.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.952(3) _cell_length_b 13.2172(19) _cell_length_c 14.875(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.844(2) _cell_angle_gamma 90.00 _cell_volume 3898.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7575 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7581 _exptl_absorpt_correction_T_max 0.9018 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12802 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4420 _reflns_number_gt 3754 _reflns_threshold_expression I>2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+7.4775P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4420 _refine_ls_number_parameters 249 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.440172(8) 0.633459(14) 0.239818(12) 0.02703(7) Uani 1 1 d . . . N1 N 0.44166(9) 0.48180(16) 0.22627(14) 0.0307(4) Uani 1 1 d . . . N2 N 0.5000 0.3261(2) 0.2500 0.0349(6) Uani 1 2 d S . . N3 N 0.32704(10) 0.64764(16) 0.22098(15) 0.0327(5) Uani 1 1 d . . . N4 N 0.22472(11) 0.60311(18) 0.24602(17) 0.0389(5) Uani 1 1 d . . . N5 N 0.32862(11) 0.5602(2) 0.35414(16) 0.0405(5) Uani 1 1 d . . . H5 H 0.3686(16) 0.559(2) 0.367(2) 0.049 Uiso 1 1 d . . . O1 O 0.44609(9) 0.79127(14) 0.24950(13) 0.0387(4) Uani 1 1 d . . . O2 O 0.42185(8) 0.64423(13) 0.09603(12) 0.0344(4) Uani 1 1 d . . . O3 O 0.53251(8) 0.62534(13) 0.11464(12) 0.0318(4) Uani 1 1 d . . . C1 C 0.37827(12) 0.4271(2) 0.18958(19) 0.0368(6) Uani 1 1 d . . . H1A H 0.3443 0.4711 0.1466 0.044 Uiso 1 1 calc R . . H1B H 0.3623 0.4083 0.2424 0.044 Uiso 1 1 calc R . . C2 C 0.38650(13) 0.3327(2) 0.1368(2) 0.0430(6) Uani 1 1 d . . . H2A H 0.3437 0.2956 0.1146 0.052 Uiso 1 1 calc R . . H2B H 0.3997 0.3510 0.0815 0.052 Uiso 1 1 calc R . . C3 C 0.44021(14) 0.2673(2) 0.2038(2) 0.0447(6) Uani 1 1 d . . . H3A H 0.4229 0.2380 0.2518 0.054 Uiso 1 1 calc R . . H3B H 0.4517 0.2117 0.1682 0.054 Uiso 1 1 calc R . . C4 C 0.5000 0.4314(3) 0.2500 0.0284(7) Uani 1 2 d S . . C5 C 0.47090(12) 0.63632(19) 0.06481(18) 0.0318(5) Uani 1 1 d . B . C6 C 0.45625(14) 0.6417(2) -0.04116(19) 0.0412(6) Uani 1 1 d . . . H6A H 0.4980 0.6345 -0.0556 0.062 Uiso 0.50 1 calc PR A 1 H6B H 0.4358 0.7065 -0.0645 0.062 Uiso 0.50 1 calc PR A 1 H6C H 0.4256 0.5876 -0.0716 0.062 Uiso 0.50 1 calc PR A 1 H6D H 0.4713 0.5798 -0.0631 0.062 Uiso 0.50 1 calc PR A 2 H6E H 0.4799 0.6989 -0.0563 0.062 Uiso 0.50 1 calc PR A 2 H6F H 0.4081 0.6498 -0.0723 0.062 Uiso 0.50 1 calc PR A 2 C7 C 0.5000 0.8348(3) 0.2500 0.0407(8) Uani 1 2 d S . . C8 C 0.5000 0.9491(3) 0.2500 0.0680(15) Uani 1 2 d S . . H8A H 0.5437 0.9735 0.2502 0.102 Uiso 0.50 1 calc PR B . H8B H 0.4909 0.9735 0.3061 0.102 Uiso 0.50 1 calc PR . . H8C H 0.4654 0.9735 0.1936 0.102 Uiso 0.50 1 calc PR . . C9A C 0.28912(14) 0.7005(3) 0.1331(2) 0.0511(8) Uani 0.55 1 d PD B 1 H9AA H 0.2914 0.6597 0.0792 0.061 Uiso 0.55 1 calc PR B 1 H9AB H 0.3120 0.7647 0.1310 0.061 Uiso 0.55 1 calc PR B 1 C10A C 0.2178(2) 0.7225(5) 0.1194(5) 0.0460(13) Uani 0.55 1 d PD B 1 H10A H 0.2149 0.7873 0.1499 0.055 Uiso 0.55 1 calc PR B 1 H10B H 0.1939 0.7300 0.0513 0.055 Uiso 0.55 1 calc PR B 1 C11A C 0.18429(16) 0.6466(3) 0.1569(3) 0.0732(13) Uani 0.55 1 d PD B 1 H11A H 0.1695 0.5922 0.1100 0.088 Uiso 0.55 1 calc PR B 1 H11B H 0.1439 0.6766 0.1654 0.088 Uiso 0.55 1 calc PR B 1 C9B C 0.28912(14) 0.7005(3) 0.1331(2) 0.0511(8) Uani 0.45 1 d PD B 2 H9BA H 0.2899 0.7733 0.1459 0.061 Uiso 0.45 1 calc PR B 2 H9BB H 0.3116 0.6895 0.0855 0.061 Uiso 0.45 1 calc PR B 2 C10B C 0.2206(3) 0.6680(7) 0.0949(5) 0.056(2) Uani 0.45 1 d PD B 2 H10C H 0.1959 0.7204 0.0508 0.067 Uiso 0.45 1 calc PR B 2 H10D H 0.2200 0.6070 0.0572 0.067 Uiso 0.45 1 calc PR B 2 C11B C 0.18429(16) 0.6466(3) 0.1569(3) 0.0732(13) Uani 0.45 1 d PD B 2 H11C H 0.1477 0.5996 0.1255 0.088 Uiso 0.45 1 calc PR B 2 H11D H 0.1638 0.7093 0.1697 0.088 Uiso 0.45 1 calc PR B 2 C12 C 0.29360(12) 0.60619(18) 0.27092(17) 0.0300(5) Uani 1 1 d . B . C13A C 0.18981(15) 0.5559(3) 0.3043(3) 0.0711(12) Uani 0.48 1 d PD B 1 H13A H 0.1532 0.6006 0.3073 0.085 Uiso 0.48 1 calc PR B 1 H13B H 0.1694 0.4927 0.2739 0.085 Uiso 0.48 1 calc PR B 1 C13B C 0.18981(15) 0.5559(3) 0.3043(3) 0.0711(12) Uani 0.52 1 d PD B 2 H13C H 0.1522 0.5167 0.2624 0.085 Uiso 0.52 1 calc PR B 2 H13D H 0.1703 0.6097 0.3326 0.085 Uiso 0.52 1 calc PR B 2 C14A C 0.2314(3) 0.5342(7) 0.3977(7) 0.059(3) Uani 0.48 1 d PD B 1 H14A H 0.2292 0.5927 0.4372 0.070 Uiso 0.48 1 calc PR B 1 H14B H 0.2110 0.4771 0.4205 0.070 Uiso 0.48 1 calc PR B 1 C14B C 0.2281(3) 0.4896(6) 0.3802(7) 0.060(3) Uani 0.52 1 d PD B 2 H14C H 0.2097 0.4944 0.4328 0.072 Uiso 0.52 1 calc PR B 2 H14D H 0.2221 0.4197 0.3571 0.072 Uiso 0.52 1 calc PR B 2 C15A C 0.29897(16) 0.5115(4) 0.4159(3) 0.0755(13) Uani 0.48 1 d PD B 1 H15A H 0.3036 0.4381 0.4106 0.091 Uiso 0.48 1 calc PR B 1 H15B H 0.3240 0.5308 0.4815 0.091 Uiso 0.48 1 calc PR B 1 C15B C 0.29897(16) 0.5115(4) 0.4159(3) 0.0755(13) Uani 0.52 1 d PD B 2 H15C H 0.3072 0.5538 0.4726 0.091 Uiso 0.52 1 calc PR B 2 H15D H 0.3229 0.4475 0.4364 0.091 Uiso 0.52 1 calc PR B 2 C1S C 0.12384(16) 0.3194(3) 0.0961(3) 0.0578(8) Uani 1 1 d . . . H1SA H 0.1185 0.3197 0.1592 0.069 Uiso 1 1 calc R . . H1SB H 0.1127 0.2514 0.0694 0.069 Uiso 1 1 calc R . . Cl1 Cl 0.06731(6) 0.40573(10) 0.02357(9) 0.0909(3) Uani 1 1 d . . . Cl2 Cl 0.20738(5) 0.34552(10) 0.10791(11) 0.0952(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02457(10) 0.03496(11) 0.02590(10) 0.00143(7) 0.01416(7) 0.00139(7) N1 0.0245(10) 0.0367(11) 0.0320(11) -0.0015(8) 0.0107(8) -0.0007(8) N2 0.0303(14) 0.0350(15) 0.0390(17) 0.000 0.0108(13) 0.000 N3 0.0300(10) 0.0416(12) 0.0315(11) 0.0073(9) 0.0167(9) 0.0069(8) N4 0.0304(10) 0.0465(12) 0.0436(13) 0.0110(10) 0.0171(9) 0.0027(9) N5 0.0310(11) 0.0603(15) 0.0343(12) 0.0118(10) 0.0163(10) 0.0008(10) O1 0.0391(10) 0.0362(9) 0.0510(11) 0.0021(8) 0.0286(9) 0.0020(7) O2 0.0287(8) 0.0500(11) 0.0287(9) 0.0039(7) 0.0149(7) 0.0041(7) O3 0.0272(8) 0.0447(10) 0.0275(8) 0.0006(7) 0.0143(7) 0.0018(7) C1 0.0272(11) 0.0477(15) 0.0375(14) -0.0082(11) 0.0134(10) -0.0033(10) C2 0.0339(13) 0.0512(16) 0.0428(15) -0.0139(13) 0.0111(12) -0.0051(12) C3 0.0428(15) 0.0405(15) 0.0525(17) -0.0076(13) 0.0178(13) -0.0067(12) C4 0.0278(15) 0.0371(17) 0.0231(15) 0.000 0.0122(13) 0.000 C5 0.0321(12) 0.0386(13) 0.0288(12) 0.0021(10) 0.0156(10) 0.0012(10) C6 0.0357(13) 0.0637(18) 0.0278(13) 0.0044(12) 0.0154(11) 0.0052(12) C7 0.045(2) 0.0372(19) 0.050(2) 0.000 0.0293(18) 0.000 C8 0.060(3) 0.040(2) 0.123(5) 0.000 0.055(3) 0.000 C9A 0.0381(15) 0.066(2) 0.0563(19) 0.0288(16) 0.0245(14) 0.0140(13) C10A 0.032(3) 0.065(4) 0.042(3) 0.015(3) 0.013(2) 0.011(3) C11A 0.0313(15) 0.111(3) 0.073(2) 0.052(2) 0.0100(15) 0.0033(17) C9B 0.0381(15) 0.066(2) 0.0563(19) 0.0288(16) 0.0245(14) 0.0140(13) C10B 0.069(5) 0.071(5) 0.030(4) 0.011(4) 0.020(3) 0.026(5) C11B 0.0313(15) 0.111(3) 0.073(2) 0.052(2) 0.0100(15) 0.0033(17) C12 0.0304(11) 0.0315(12) 0.0327(12) -0.0010(10) 0.0165(10) 0.0022(9) C13A 0.0353(15) 0.105(3) 0.078(3) 0.046(2) 0.0261(16) -0.0010(17) C13B 0.0353(15) 0.105(3) 0.078(3) 0.046(2) 0.0261(16) -0.0010(17) C14A 0.064(5) 0.055(6) 0.080(6) 0.032(5) 0.056(5) 0.010(4) C14B 0.043(3) 0.048(5) 0.091(7) 0.048(5) 0.024(4) 0.002(3) C15A 0.0420(17) 0.131(4) 0.052(2) 0.044(2) 0.0123(15) -0.017(2) C15B 0.0420(17) 0.131(4) 0.052(2) 0.044(2) 0.0123(15) -0.017(2) C1S 0.0503(18) 0.064(2) 0.066(2) 0.0108(17) 0.0290(16) -0.0015(15) Cl1 0.0820(7) 0.0860(7) 0.0896(8) 0.0145(6) 0.0066(6) 0.0205(6) Cl2 0.0553(5) 0.1031(8) 0.1401(11) 0.0399(8) 0.0494(7) -0.0027(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.016(2) . ? Rh1 O2 2.0523(18) . ? Rh1 O3 2.0557(17) 2_655 ? Rh1 O1 2.0917(19) . ? Rh1 N3 2.303(2) . ? Rh1 Rh1 2.4262(5) 2_655 ? N1 C4 1.335(3) . ? N1 C1 1.455(3) . ? N2 C4 1.392(5) . ? N2 C3 1.445(3) . ? N2 C3 1.445(3) 2_655 ? N3 C12 1.296(3) . ? N3 C9A 1.469(3) . ? N4 C12 1.370(3) . ? N4 C11A 1.442(4) . ? N4 C13A 1.445(4) . ? N5 C12 1.361(3) . ? N5 C15A 1.419(4) . ? O1 C7 1.266(2) . ? O2 C5 1.261(3) . ? O3 C5 1.272(3) . ? O3 Rh1 2.0557(17) 2_655 ? C1 C2 1.513(4) . ? C2 C3 1.510(4) . ? C4 N1 1.336(3) 2_655 ? C5 C6 1.507(3) . ? C7 O1 1.265(2) 2_655 ? C7 C8 1.510(6) . ? C9A C10A 1.471(5) . ? C10A C11A 1.436(6) . ? C13A C14A 1.411(8) . ? C14A C15A 1.386(7) . ? C1S Cl2 1.736(3) . ? C1S Cl1 1.744(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 O2 88.20(7) . . ? N1 Rh1 O3 92.60(7) . 2_655 ? O2 Rh1 O3 174.83(6) . 2_655 ? N1 Rh1 O1 174.86(7) . . ? O2 Rh1 O1 89.40(7) . . ? O3 Rh1 O1 89.39(7) 2_655 . ? N1 Rh1 N3 96.74(7) . . ? O2 Rh1 N3 91.65(7) . . ? O3 Rh1 N3 93.32(7) 2_655 . ? O1 Rh1 N3 87.88(7) . . ? N1 Rh1 Rh1 87.92(5) . 2_655 ? O2 Rh1 Rh1 88.17(5) . 2_655 ? O3 Rh1 Rh1 86.76(5) 2_655 2_655 ? O1 Rh1 Rh1 87.45(5) . 2_655 ? N3 Rh1 Rh1 175.33(5) . 2_655 ? C4 N1 C1 119.9(2) . . ? C4 N1 Rh1 120.78(18) . . ? C1 N1 Rh1 119.35(15) . . ? C4 N2 C3 122.51(16) . . ? C4 N2 C3 122.51(16) . 2_655 ? C3 N2 C3 115.0(3) . 2_655 ? C12 N3 C9A 118.3(2) . . ? C12 N3 Rh1 128.44(17) . . ? C9A N3 Rh1 112.75(15) . . ? C12 N4 C11A 119.4(2) . . ? C12 N4 C13A 123.0(2) . . ? C11A N4 C13A 117.6(2) . . ? C12 N5 C15A 124.8(2) . . ? C7 O1 Rh1 119.12(19) . . ? C5 O2 Rh1 118.53(16) . . ? C5 O3 Rh1 119.52(15) . 2_655 ? N1 C1 C2 111.2(2) . . ? C3 C2 C1 108.4(2) . . ? N2 C3 C2 110.7(2) . . ? N1 C4 N1 120.2(3) . 2_655 ? N1 C4 N2 119.91(15) . . ? N1 C4 N2 119.91(15) 2_655 . ? O2 C5 O3 126.1(2) . . ? O2 C5 C6 117.8(2) . . ? O3 C5 C6 116.1(2) . . ? O1 C7 O1 125.9(4) 2_655 . ? O1 C7 C8 117.04(18) 2_655 . ? O1 C7 C8 117.04(18) . . ? N3 C9A C10A 116.8(3) . . ? C11A C10A C9A 114.2(4) . . ? C10A C11A N4 114.8(3) . . ? N3 C12 N5 118.5(2) . . ? N3 C12 N4 125.1(2) . . ? N5 C12 N4 116.4(2) . . ? C14A C13A N4 114.1(4) . . ? C15A C14A C13A 120.2(8) . . ? C14A C15A N5 114.1(4) . . ? Cl2 C1S Cl1 113.17(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.743 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.071 #===END CIF for 3.2CH2Cl2 ========================