data_rhbpycor _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C20 N4 Rh, Cl O4, 2(C2 N)' _chemical_formula_structural '2(C10 N2) Rh, Cl O4, 2(C2 N)' _chemical_formula_analytical ? _chemical_formula_sum 'C24 H22 Cl N6 O4 Rh' _chemical_formula_weight 596.83 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x-1/2, y-1/2, -z' _cell_length_a 24.929(2) _cell_length_b 7.279(2) _cell_length_c 28.863(2) _cell_angle_alpha 90.00(2) _cell_angle_beta 115.82(2) _cell_angle_gamma 90.00(3) _cell_volume 4714.6(14) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description neeedles _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method none _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.88 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Data were collected at beamline X7B at the Brookhaven National Laboratory NSLS, using the rotation method. Data were recorded on image plates. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.95600 _diffrn_radiation_type synchrotron _diffrn_radiation_source ; National Synchrotron Light Source beamline x7b ; _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device 'Huber' _diffrn_measurement_method 'Fuji image plates' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5030 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 6.24 _diffrn_reflns_theta_max 34.23 _reflns_number_total 5030 _reflns_number_observed 2585 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; see M.J. Gray etal for a description of data collection at beamline x7b ; _computing_cell_refinement ; average of cell contants determined on each image plate ; _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.2255P)^2^+205.8863P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 5030 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2280 _refine_ls_R_factor_obs 0.1566 _refine_ls_wR_factor_all 0.4822 _refine_ls_wR_factor_obs 0.4335 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_obs 1.343 _refine_ls_restrained_S_all 1.065 _refine_ls_restrained_S_obs 1.343 _refine_ls_shift/esd_max 0.013 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh1 Rh 0.25054(8) 0.2097(3) -0.00047(8) 0.0320(8) Uani 1 d . . N111 N 0.1827(11) 0.1659(37) -0.0681(10) 0.060(7) Uiso 1 d . . C112 C 0.1260(21) 0.1738(63) -0.0729(18) 0.098(13) Uiso 1 d . . C113 C 0.0761(12) 0.1282(41) -0.1131(11) 0.044(7) Uiso 1 d . . C114 C 0.0784(14) 0.0502(46) -0.1582(13) 0.058(9) Uiso 1 d . . C115 C 0.1339(15) 0.0421(46) -0.1563(13) 0.060(9) Uiso 1 d . . C116 C 0.1821(11) 0.1034(39) -0.1132(10) 0.041(7) Uiso 1 d . . N121 N 0.1811(8) 0.2492(28) 0.0172(8) 0.032(5) Uiso 1 d . . C122 C 0.1251(11) 0.2410(37) -0.0236(10) 0.035(6) Uiso 1 d . . C123 C 0.0729(13) 0.2843(44) -0.0190(12) 0.054(8) Uiso 1 d . . C124 C 0.0779(14) 0.3605(47) 0.0278(12) 0.060(9) Uiso 1 d . . C125 C 0.1348(12) 0.3598(40) 0.0693(11) 0.043(7) Uiso 1 d . . C126 C 0.1817(20) 0.2884(60) 0.0608(18) 0.096(13) Uiso 1 d . . N131 N 0.3196(8) 0.2632(27) -0.0179(7) 0.027(4) Uiso 1 d . . C132 C 0.3749(10) 0.2472(34) 0.0219(9) 0.026(5) Uiso 1 d . . C133 C 0.4269(11) 0.2940(39) 0.0162(10) 0.041(7) Uiso 1 d . . C134 C 0.4213(12) 0.3734(42) -0.0298(11) 0.048(7) Uiso 1 d . . C135 C 0.3644(12) 0.3785(40) -0.0704(10) 0.042(7) Uiso 1 d . . C136 C 0.3178(19) 0.3014(58) -0.0620(17) 0.090(12) Uiso 1 d . . N141 N 0.3196(10) 0.1709(32) 0.0682(9) 0.045(6) Uiso 1 d . . C142 C 0.3750(18) 0.1721(57) 0.0702(16) 0.085(11) Uiso 1 d . . C143 C 0.4256(12) 0.1240(41) 0.1098(11) 0.044(7) Uiso 1 d . . C144 C 0.4228(13) 0.0393(41) 0.1532(12) 0.045(7) Uiso 1 d . . C145 C 0.3702(14) 0.0381(43) 0.1565(12) 0.052(8) Uiso 1 d . . C146 C 0.3200(11) 0.1084(39) 0.1134(10) 0.040(7) Uiso 1 d . . Rh2 Rh 0.24944(9) 0.2549(3) 0.49949(8) 0.0433(9) Uani 1 d . . N211 N 0.1621(8) 0.2346(27) 0.4805(7) 0.026(4) Uiso 1 d . . C212 C 0.1451(10) 0.2368(33) 0.5208(9) 0.026(5) Uiso 1 d . . C213 C 0.0890(14) 0.2029(48) 0.5128(13) 0.063(9) Uiso 1 d . . C214 C 0.0490(13) 0.1198(44) 0.4680(12) 0.052(8) Uiso 1 d . . C215 C 0.0659(15) 0.1104(48) 0.4264(13) 0.064(9) Uiso 1 d . . C216 C 0.1221(16) 0.1573(52) 0.4376(14) 0.070(10) Uiso 1 d . . N221 N 0.2487(17) 0.2952(49) 0.5688(14) 0.104(11) Uiso 1 d . . C222 C 0.1930(17) 0.2978(53) 0.5699(15) 0.076(10) Uiso 1 d . . C223 C 0.1833(14) 0.3720(46) 0.6111(13) 0.058(8) Uiso 1 d . . C224 C 0.2301(17) 0.4248(54) 0.6536(15) 0.077(11) Uiso 1 d . . C225 C 0.2866(16) 0.4555(49) 0.6557(14) 0.068(10) Uiso 1 d . . C226 C 0.2942(12) 0.3673(43) 0.6142(11) 0.048(7) Uiso 1 d . . N231 N 0.3366(9) 0.2462(29) 0.5173(8) 0.032(5) Uiso 1 d . . C232 C 0.3517(10) 0.2421(33) 0.4765(9) 0.026(5) Uiso 1 d . . C233 C 0.4079(15) 0.2078(48) 0.4834(13) 0.065(9) Uiso 1 d . . C234 C 0.4532(13) 0.1274(46) 0.5279(12) 0.056(8) Uiso 1 d . . C235 C 0.4353(13) 0.1242(44) 0.5724(12) 0.054(8) Uiso 1 d . . C236 C 0.3767(16) 0.1742(52) 0.5616(14) 0.072(10) Uiso 1 d . . N241 N 0.2512(15) 0.3043(46) 0.4317(13) 0.091(10) Uiso 1 d . . C242 C 0.3032(19) 0.2930(57) 0.4275(17) 0.088(12) Uiso 1 d . . C243 C 0.3093(16) 0.3574(51) 0.3825(14) 0.069(10) Uiso 1 d . . C244 C 0.2663(19) 0.4236(58) 0.3445(17) 0.086(12) Uiso 1 d . . C245 C 0.2098(18) 0.4588(56) 0.3432(16) 0.085(12) Uiso 1 d . . C246 C 0.2066(14) 0.3756(46) 0.3877(13) 0.058(8) Uiso 1 d . . Cl1 Cl 0.2553(3) 0.2247(15) 0.2130(3) 0.059(3) Uani 1 d . . O11 O 0.2469(9) 0.0740(33) 0.1801(10) 0.069(7) Uani 1 d . . O12 O 0.2111(10) 0.2242(34) 0.2312(9) 0.080(8) Uani 1 d . . O13 O 0.2552(14) 0.3840(32) 0.1858(10) 0.105(10) Uani 1 d . . O14 O 0.3098(9) 0.2012(39) 0.2572(9) 0.087(8) Uani 1 d . . Cl2 Cl 0.4572(3) 0.2373(12) 0.7132(3) 0.043(2) Uani 1 d . . O21 O 0.4272(10) 0.0881(27) 0.6793(9) 0.075(7) Uani 1 d . . O22 O 0.4366(11) 0.3913(33) 0.6859(10) 0.085(8) Uani 1 d . . O23 O 0.5188(8) 0.2049(31) 0.7299(9) 0.071(7) Uani 1 d . . O24 O 0.4471(11) 0.2550(37) 0.7577(9) 0.090(8) Uani 1 d . . C3A C 0.0802(15) 0.2257(49) 0.2222(14) 0.069(9) Uiso 1 d . . C2A C 0.0658(17) 0.1372(56) 0.1706(17) 0.083(12) Uiso 1 d . . N1A N 0.0520(13) 0.1057(42) 0.1299(12) 0.077(9) Uiso 1 d . . C3B C 0.1577(14) 0.7118(46) 0.2054(12) 0.062(9) Uiso 1 d . . C2B C 0.1033(16) 0.6408(50) 0.1619(14) 0.070(10) Uiso 1 d . . N1B N 0.0555(13) 0.6065(41) 0.1293(11) 0.071(8) Uiso 1 d . . C3C C 0.4544(13) 0.2466(44) 0.2962(12) 0.055(8) Uiso 1 d . . C2C C 0.4403(19) 0.1536(62) 0.3382(18) 0.098(13) Uiso 1 d . . N1C N 0.4316(13) 0.1064(44) 0.3699(12) 0.079(9) Uiso 1 d . . C3D C 0.1415(13) 0.2354(43) 0.7232(12) 0.053(8) Uiso 1 d . . C2D C 0.1048(13) 0.1425(42) 0.6716(12) 0.048(7) Uiso 1 d . . N1D N 0.0711(14) 0.1129(46) 0.6302(13) 0.086(9) Uiso 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 0.0339(11) 0.024(2) 0.0419(12) 0.0000(11) 0.0194(9) -0.0010(10) Rh2 0.0366(12) 0.060(2) 0.0342(12) -0.0013(14) 0.0160(10) 0.0026(13) Cl1 0.034(4) 0.100(8) 0.043(4) -0.007(5) 0.017(3) -0.003(4) O11 0.065(14) 0.068(18) 0.092(19) 0.035(15) 0.051(14) 0.021(12) O12 0.069(15) 0.104(21) 0.086(18) -0.058(15) 0.051(13) -0.048(14) O13 0.223(34) 0.031(18) 0.102(21) -0.019(14) 0.109(23) -0.037(18) O14 0.049(13) 0.143(25) 0.060(16) 0.000(15) 0.015(12) 0.028(14) Cl2 0.041(4) 0.051(6) 0.040(4) -0.003(4) 0.018(3) -0.004(4) O21 0.100(18) 0.002(15) 0.094(19) -0.004(13) 0.015(15) -0.008(12) O22 0.092(18) 0.040(19) 0.102(21) 0.016(16) 0.024(16) 0.027(14) O23 0.024(9) 0.089(19) 0.098(19) -0.011(14) 0.025(11) -0.002(10) O24 0.116(22) 0.125(23) 0.058(15) 0.001(14) 0.065(16) -0.013(17) _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 N111 1.97(3) . ? Rh1 N141 2.00(2) . ? Rh1 N121 2.03(2) . ? Rh1 N131 2.03(2) . ? N111 C112 1.36(5) . ? N111 C116 1.37(3) . ? C112 C113 1.32(5) . ? C112 C122 1.52(5) . ? C113 C114 1.45(4) . ? C114 C115 1.36(4) . ? C115 C116 1.37(4) . ? N121 C126 1.28(5) . ? N121 C122 1.38(3) . ? C122 C123 1.40(4) . ? C123 C124 1.41(4) . ? C124 C125 1.40(4) . ? C125 C126 1.40(5) . ? N131 C136 1.29(4) . ? N131 C132 1.36(3) . ? C132 C133 1.42(3) . ? C132 C142 1.50(4) . ? C133 C134 1.40(4) . ? C134 C135 1.39(4) . ? C135 C136 1.40(5) . ? N141 C142 1.36(4) . ? N141 C146 1.38(3) . ? C142 C143 1.33(4) . ? C143 C144 1.43(4) . ? C144 C145 1.35(4) . ? C145 C146 1.42(4) . ? Rh2 N231 2.00(2) . ? Rh2 N211 2.01(2) . ? Rh2 N241 2.01(3) . ? Rh2 N221 2.03(4) . ? N211 C216 1.33(4) . ? N211 C212 1.40(3) . ? C212 C213 1.34(4) . ? C212 C222 1.47(4) . ? C213 C214 1.38(4) . ? C214 C215 1.44(4) . ? C215 C216 1.34(4) . ? N221 C222 1.40(5) . ? N221 C226 1.41(4) . ? C222 C223 1.42(5) . ? C223 C224 1.33(4) . ? C224 C225 1.40(4) . ? C225 C226 1.44(4) . ? N231 C236 1.34(4) . ? N231 C232 1.38(3) . ? C232 C233 1.35(4) . ? C232 C242 1.45(5) . ? C233 C234 1.42(4) . ? C234 C235 1.53(4) . ? C235 C236 1.40(4) . ? N241 C242 1.36(5) . ? N241 C246 1.38(4) . ? C242 C243 1.45(5) . ? C243 C244 1.25(5) . ? C244 C245 1.42(5) . ? C245 C246 1.46(5) . ? Cl1 O13 1.40(2) . ? Cl1 O11 1.41(3) . ? Cl1 O12 1.41(2) . ? Cl1 O14 1.41(2) . ? Cl2 O22 1.34(2) . ? Cl2 O23 1.42(2) . ? Cl2 O24 1.42(2) . ? Cl2 O21 1.44(2) . ? C3A C2A 1.52(5) . ? C2A N1A 1.10(4) . ? C3B C2B 1.48(4) . ? C2B N1B 1.18(4) . ? C3C C2C 1.56(5) . ? C2C N1C 1.08(5) . ? C3D C2D 1.52(4) . ? C2D N1D 1.14(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 N111 Rh1 N141 162.6(11) . . ? N111 Rh1 N121 79.3(9) . . ? N141 Rh1 N121 103.4(8) . . ? N111 Rh1 N131 103.9(9) . . ? N141 Rh1 N131 79.3(8) . . ? N121 Rh1 N131 160.8(8) . . ? C112 N111 C116 109.6(31) . . ? C112 N111 Rh1 119.9(27) . . ? C116 N111 Rh1 129.9(21) . . ? C113 C112 N111 128.3(41) . . ? C113 C112 C122 120.8(38) . . ? N111 C112 C122 110.9(36) . . ? C112 C113 C114 119.8(33) . . ? C115 C114 C113 114.8(31) . . ? C114 C115 C116 119.8(32) . . ? N111 C116 C115 127.5(28) . . ? C126 N121 C122 114.9(28) . . ? C126 N121 Rh1 129.1(26) . . ? C122 N121 Rh1 115.9(16) . . ? N121 C122 C123 123.1(25) . . ? N121 C122 C112 113.1(27) . . ? C123 C122 C112 123.8(29) . . ? C122 C123 C124 118.7(28) . . ? C125 C124 C123 116.8(29) . . ? C126 C125 C124 117.6(31) . . ? N121 C126 C125 127.0(40) . . ? C136 N131 C132 116.2(26) . . ? C136 N131 Rh1 128.2(24) . . ? C132 N131 Rh1 115.5(15) . . ? N131 C132 C133 121.5(22) . . ? N131 C132 C142 114.1(24) . . ? C133 C132 C142 124.4(26) . . ? C134 C133 C132 119.4(25) . . ? C135 C134 C133 117.0(26) . . ? C134 C135 C136 117.5(29) . . ? N131 C136 C135 125.6(37) . . ? C142 N141 C146 111.9(28) . . ? C142 N141 Rh1 117.6(24) . . ? C146 N141 Rh1 129.3(18) . . ? C143 C142 N141 127.2(37) . . ? C143 C142 C132 120.9(34) . . ? N141 C142 C132 111.9(33) . . ? C142 C143 C144 118.5(31) . . ? C145 C144 C143 118.9(29) . . ? C144 C145 C146 116.6(29) . . ? N141 C146 C145 126.0(26) . . ? N231 Rh2 N211 173.9(8) . . ? N231 Rh2 N241 77.0(11) . . ? N211 Rh2 N241 103.2(11) . . ? N231 Rh2 N221 103.0(12) . . ? N211 Rh2 N221 78.8(12) . . ? N241 Rh2 N221 161.4(15) . . ? C216 N211 C212 113.8(23) . . ? C216 N211 Rh2 124.8(19) . . ? C212 N211 Rh2 117.1(15) . . ? C213 C212 N211 121.7(25) . . ? C213 C212 C222 124.8(27) . . ? N211 C212 C222 113.2(24) . . ? C212 C213 C214 121.0(30) . . ? C213 C214 C215 116.7(30) . . ? C216 C215 C214 116.2(32) . . ? N211 C216 C215 128.0(32) . . ? C222 N221 C226 112.3(34) . . ? C222 N221 Rh2 117.2(29) . . ? C226 N221 Rh2 128.4(27) . . ? N221 C222 C223 123.7(37) . . ? N221 C222 C212 111.8(33) . . ? C223 C222 C212 124.1(33) . . ? C224 C223 C222 118.8(35) . . ? C223 C224 C225 123.3(38) . . ? C224 C225 C226 112.7(34) . . ? N221 C226 C225 126.5(31) . . ? C236 N231 C232 115.8(24) . . ? C236 N231 Rh2 122.2(20) . . ? C232 N231 Rh2 116.6(16) . . ? C233 C232 N231 121.9(26) . . ? C233 C232 C242 124.0(29) . . ? N231 C232 C242 113.9(26) . . ? C232 C233 C234 125.1(31) . . ? C233 C234 C235 111.1(28) . . ? C236 C235 C234 117.6(29) . . ? N231 C236 C235 126.0(31) . . ? C242 N241 C246 111.1(35) . . ? C242 N241 Rh2 120.3(30) . . ? C246 N241 Rh2 128.0(26) . . ? N241 C242 C232 110.4(36) . . ? N241 C242 C243 122.6(40) . . ? C232 C242 C243 126.0(36) . . ? C244 C243 C242 121.7(40) . . ? C243 C244 C245 123.9(44) . . ? C244 C245 C246 109.8(37) . . ? N241 C246 C245 129.7(34) . . ? O13 Cl1 O11 107.7(14) . . ? O13 Cl1 O12 113.6(18) . . ? O11 Cl1 O12 109.8(13) . . ? O13 Cl1 O14 111.8(19) . . ? O11 Cl1 O14 108.4(15) . . ? O12 Cl1 O14 105.4(15) . . ? O22 Cl2 O23 114.9(15) . . ? O22 Cl2 O24 106.5(17) . . ? O23 Cl2 O24 107.6(16) . . ? O22 Cl2 O21 106.2(15) . . ? O23 Cl2 O21 105.8(14) . . ? O24 Cl2 O21 116.2(16) . . ? N1A C2A C3A 166.6(45) . . ? N1B C2B C3B 169.4(38) . . ? N1C C2C C3C 172.5(47) . . ? N1D C2D C3D 163.8(34) . . ? _refine_diff_density_max 1.806 _refine_diff_density_min -1.930 _refine_diff_density_rms 0.220