# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Samaresh Bhattacharya' _publ_contact_author_email 'samaresh b@yahoo.com' _publ_section_title ; Formation of organorhodium complexes via C-H bond activation of 1,3-di(phenylazo)benzene. Structural diversity and catalytic potential ; _publ_author_name S.Bhattacharya # Attachment '- 186sb-su-7(MGBD-amide)_c1.cif' data_sb-su-7 _database_code_depnum_ccdc_archive 'CCDC 810560' #TrackingRef '- 186sb-su-7(MGBD-amide)_c1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 Cl2 N5 O Rh ' _chemical_formula_weight 580.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 12.1868(11) _cell_length_b 12.0880(5) _cell_length_c 15.7543(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.597(6) _cell_angle_gamma 90.00 _cell_volume 2318.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 0.980 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10559 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.1216 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6266 _reflns_number_gt 3907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6266 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 0.006 _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 C11 C 0.2116(4) -0.0929(4) 0.7940(3) 0.0225(10) Uani 1 1 d . . . C12 C 0.3119(4) -0.1046(4) 0.7564(3) 0.0260(10) Uani 1 1 d . . . H12 H 0.3545 -0.0427 0.7458 0.031 Uiso 1 1 calc R . . C13 C 0.3477(4) -0.2081(5) 0.7350(3) 0.0300(11) Uani 1 1 d . . . H13 H 0.4148 -0.2163 0.7098 0.036 Uiso 1 1 calc R . . C14 C 0.2843(4) -0.3006(4) 0.7507(3) 0.0294(11) Uani 1 1 d . . . H14 H 0.3092 -0.3708 0.7369 0.035 Uiso 1 1 calc R . . C15 C 0.1839(5) -0.2879(5) 0.7871(3) 0.0325(12) Uani 1 1 d . . . H15 H 0.1405 -0.3497 0.7959 0.039 Uiso 1 1 calc R . . C16 C 0.1477(4) -0.1860(4) 0.8103(3) 0.0283(11) Uani 1 1 d . . . H16 H 0.0813 -0.1785 0.8366 0.034 Uiso 1 1 calc R . . C22 C 0.0718(4) 0.1300(4) 0.8884(3) 0.0237(10) Uani 1 1 d . . . C23 C -0.0017(4) 0.1619(5) 0.9489(3) 0.0290(11) Uani 1 1 d . . . H23 H -0.0294 0.1103 0.9862 0.035 Uiso 1 1 calc R . . C24 C -0.0327(4) 0.2723(4) 0.9525(3) 0.0259(10) Uani 1 1 d . . . H24 H -0.0816 0.2941 0.9929 0.031 Uiso 1 1 calc R . . C25 C 0.0072(4) 0.3514(4) 0.8975(3) 0.0286(11) Uani 1 1 d . . . H25 H -0.0161 0.4245 0.9002 0.034 Uiso 1 1 calc R . . C26 C 0.0834(4) 0.3189(4) 0.8380(3) 0.0252(10) Uani 1 1 d . . . C31 C 0.2621(4) 0.3999(4) 0.6789(3) 0.0244(10) Uani 1 1 d . . . C32 C 0.3762(4) 0.3946(4) 0.6812(3) 0.0271(11) Uani 1 1 d . . . H32 H 0.4143 0.3501 0.7206 0.033 Uiso 1 1 calc R . . C33 C 0.4317(5) 0.4570(5) 0.6232(3) 0.0328(12) Uani 1 1 d . . . H33 H 0.5080 0.4565 0.6250 0.039 Uiso 1 1 calc R . . C34 C 0.3755(5) 0.5192(5) 0.5634(3) 0.0344(12) Uani 1 1 d . . . H34 H 0.4140 0.5598 0.5243 0.041 Uiso 1 1 calc R . . C35 C 0.2622(5) 0.5227(4) 0.5603(3) 0.0319(12) Uani 1 1 d . . . H35 H 0.2246 0.5643 0.5187 0.038 Uiso 1 1 calc R . . C36 C 0.2045(4) 0.4637(4) 0.6195(3) 0.0299(11) Uani 1 1 d . . . H36 H 0.1282 0.4671 0.6190 0.036 Uiso 1 1 calc R . . C41 C 0.4980(5) 0.1250(5) 0.5768(3) 0.0390(14) Uani 1 1 d . . . C42 C 0.5491(6) 0.0364(6) 0.6096(3) 0.0439(15) Uani 1 1 d . . . H42 H 0.5150 -0.0064 0.6498 0.053 Uiso 1 1 calc R . . C43 C 0.6502(6) 0.0081(6) 0.5850(4) 0.0532(18) Uani 1 1 d . . . H43 H 0.6851 -0.0540 0.6082 0.064 Uiso 1 1 calc R . . C44 C 0.7022(5) 0.0720(6) 0.5249(5) 0.0546(18) Uani 1 1 d . . . H44 H 0.7703 0.0507 0.5062 0.066 Uiso 1 1 calc R . . C45 C 0.6518(5) 0.1675(5) 0.4932(3) 0.0367(13) Uani 1 1 d . . . H45 H 0.6870 0.2138 0.4560 0.044 Uiso 1 1 calc R . . C46 C 0.5483(5) 0.1911(5) 0.5188(3) 0.0383(14) Uani 1 1 d . . . H46 H 0.5114 0.2527 0.4966 0.046 Uiso 1 1 calc R . . N1 N 0.1776(3) 0.0167(3) 0.8156(2) 0.0244(9) Uani 1 1 d . . . N2 N 0.1081(3) 0.0213(3) 0.8738(2) 0.0243(9) Uani 1 1 d . . . N3 N 0.1354(3) 0.3887(3) 0.7810(3) 0.0240(8) Uani 1 1 d . . . N4 N 0.2065(3) 0.3358(3) 0.7399(2) 0.0237(8) Uani 1 1 d . . . C4 C 0.3830(6) 0.1500(5) 0.6045(4) 0.0451(16) Uani 1 1 d . . . N5 N 0.3073(5) 0.2016(5) 0.5477(3) 0.0542(15) Uani 1 1 d . . . H5A H 0.2420 0.2157 0.5630 0.065 Uiso 1 1 calc R . . H5B H 0.3263 0.2191 0.4975 0.065 Uiso 1 1 calc R . . O1 O 0.3553(3) 0.1259(3) 0.6747(2) 0.0305(8) Uani 1 1 d . . . C21 C 0.1141(4) 0.2099(4) 0.8360(3) 0.0212(9) Uani 1 1 d . . . Cl1 Cl 0.08902(11) 0.14041(11) 0.64943(7) 0.0295(3) Uani 1 1 d . . . Cl2 Cl 0.36162(10) 0.19149(11) 0.86285(7) 0.0287(3) Uani 1 1 d . . . Rh1 Rh 0.22025(3) 0.16760(3) 0.75957(2) 0.02066(12) 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 C11 0.028(2) 0.020(3) 0.0191(19) 0.0055(18) 0.0005(18) 0.005(2) C12 0.023(2) 0.022(3) 0.034(2) -0.004(2) 0.0095(19) -0.004(2) C13 0.027(3) 0.027(3) 0.037(3) -0.003(2) 0.006(2) 0.005(2) C14 0.033(3) 0.018(3) 0.037(3) 0.001(2) -0.002(2) 0.007(2) C15 0.037(3) 0.019(3) 0.041(3) 0.004(2) 0.005(2) -0.001(2) C16 0.031(3) 0.020(3) 0.035(2) 0.002(2) 0.006(2) -0.007(2) C22 0.021(2) 0.022(3) 0.028(2) 0.0032(19) 0.0047(18) 0.000(2) C23 0.026(2) 0.034(3) 0.028(2) 0.002(2) 0.0127(19) -0.005(2) C24 0.023(2) 0.025(3) 0.031(2) -0.002(2) 0.0107(19) 0.001(2) C25 0.033(3) 0.018(3) 0.035(2) -0.0022(19) 0.002(2) 0.006(2) C26 0.021(2) 0.026(3) 0.028(2) 0.0040(19) 0.0001(18) -0.003(2) C31 0.030(3) 0.017(3) 0.027(2) -0.0006(18) 0.0077(19) -0.006(2) C32 0.025(2) 0.028(3) 0.030(2) 0.002(2) 0.0076(19) 0.004(2) C33 0.034(3) 0.028(3) 0.037(3) 0.000(2) 0.008(2) -0.003(2) C34 0.046(3) 0.026(3) 0.032(2) 0.006(2) 0.011(2) 0.005(3) C35 0.041(3) 0.023(3) 0.032(2) 0.009(2) 0.009(2) 0.008(2) C36 0.028(3) 0.026(3) 0.036(3) 0.002(2) 0.000(2) -0.002(2) C41 0.058(4) 0.035(3) 0.024(2) -0.003(2) 0.013(2) -0.021(3) C42 0.052(4) 0.048(4) 0.031(3) -0.002(3) 0.001(3) -0.017(3) C43 0.061(5) 0.030(4) 0.067(4) 0.010(3) -0.022(4) 0.008(3) C44 0.032(3) 0.057(5) 0.075(5) -0.003(4) 0.002(3) 0.002(3) C45 0.031(3) 0.041(4) 0.038(3) 0.003(3) 0.002(2) -0.017(3) C46 0.040(3) 0.039(4) 0.038(3) 0.002(2) 0.016(2) -0.006(3) N1 0.026(2) 0.020(2) 0.0274(18) 0.0017(16) 0.0031(16) 0.0016(18) N2 0.030(2) 0.020(2) 0.0235(17) 0.0042(16) 0.0090(16) 0.0027(18) N3 0.023(2) 0.016(2) 0.034(2) 0.0001(16) 0.0062(17) -0.0013(17) N4 0.027(2) 0.014(2) 0.0306(19) 0.0040(16) 0.0047(16) 0.0009(17) C4 0.063(4) 0.033(4) 0.041(3) -0.014(3) 0.025(3) -0.018(3) N5 0.051(3) 0.074(4) 0.038(3) 0.010(3) 0.014(2) 0.007(3) O1 0.038(2) 0.029(2) 0.0255(16) 0.0021(14) 0.0130(15) 0.0023(17) C21 0.016(2) 0.021(3) 0.026(2) -0.0025(18) 0.0039(17) 0.0018(19) Cl1 0.0301(6) 0.0298(7) 0.0283(5) -0.0009(5) -0.0011(5) -0.0025(5) Cl2 0.0285(6) 0.0309(7) 0.0267(5) -0.0011(5) 0.0021(5) 0.0021(5) Rh1 0.02337(19) 0.0175(2) 0.02153(17) 0.00112(14) 0.00569(12) -0.00013(16) _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 C11 C12 1.390(6) . ? C11 C16 1.398(7) . ? C11 N1 1.435(6) . ? C12 C13 1.371(7) . ? C13 C14 1.388(8) . ? C14 C15 1.382(8) . ? C15 C16 1.364(8) . ? C22 C21 1.385(7) . ? C22 C23 1.391(6) . ? C22 N2 1.408(6) . ? C23 C24 1.389(7) . ? C24 C25 1.393(7) . ? C25 C26 1.405(7) . ? C26 C21 1.371(7) . ? C26 N3 1.404(6) . ? C31 C36 1.380(7) . ? C31 C32 1.391(7) . ? C31 N4 1.428(6) . ? C32 C33 1.385(7) . ? C33 C34 1.366(7) . ? C34 C35 1.380(8) . ? C35 C36 1.391(7) . ? C41 C42 1.332(9) . ? C41 C46 1.378(7) . ? C41 C4 1.516(9) . ? C42 C43 1.351(10) . ? C43 C44 1.397(10) . ? C44 C45 1.390(9) . ? C45 C46 1.371(8) . ? N1 N2 1.276(5) . ? N1 Rh1 2.102(4) . ? N3 N4 1.277(5) . ? N4 Rh1 2.062(4) . ? C4 O1 1.206(6) . ? C4 N5 1.402(9) . ? O1 Rh1 2.226(3) . ? C21 Rh1 1.878(4) . ? Cl1 Rh1 2.3291(13) . ? Cl2 Rh1 2.3334(13) . ? 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 C12 C11 C16 120.3(5) . . ? C12 C11 N1 117.7(4) . . ? C16 C11 N1 122.0(4) . . ? C13 C12 C11 119.5(5) . . ? C12 C13 C14 120.4(5) . . ? C15 C14 C13 119.6(5) . . ? C16 C15 C14 121.0(5) . . ? C15 C16 C11 119.2(5) . . ? C21 C22 C23 119.0(5) . . ? C21 C22 N2 115.1(4) . . ? C23 C22 N2 125.9(4) . . ? C24 C23 C22 118.6(5) . . ? C23 C24 C25 122.1(4) . . ? C24 C25 C26 118.9(5) . . ? C21 C26 N3 115.6(4) . . ? C21 C26 C25 118.2(5) . . ? N3 C26 C25 126.2(5) . . ? C36 C31 C32 121.4(5) . . ? C36 C31 N4 121.2(5) . . ? C32 C31 N4 117.5(4) . . ? C33 C32 C31 118.4(5) . . ? C34 C33 C32 120.7(5) . . ? C33 C34 C35 120.7(5) . . ? C34 C35 C36 119.8(5) . . ? C31 C36 C35 119.0(5) . . ? C42 C41 C46 120.5(6) . . ? C42 C41 C4 118.1(5) . . ? C46 C41 C4 121.3(6) . . ? C41 C42 C43 120.6(6) . . ? C42 C43 C44 120.1(6) . . ? C45 C44 C43 119.7(6) . . ? C46 C45 C44 117.7(6) . . ? C45 C46 C41 121.2(6) . . ? N2 N1 C11 114.8(4) . . ? N2 N1 Rh1 116.6(3) . . ? C11 N1 Rh1 128.5(3) . . ? N1 N2 C22 112.5(4) . . ? N4 N3 C26 111.1(4) . . ? N3 N4 C31 114.9(4) . . ? N3 N4 Rh1 118.0(3) . . ? C31 N4 Rh1 126.8(3) . . ? O1 C4 N5 119.3(6) . . ? O1 C4 C41 121.1(6) . . ? N5 C4 C41 119.7(5) . . ? C4 O1 Rh1 137.9(5) . . ? C26 C21 C22 123.2(4) . . ? C26 C21 Rh1 118.2(4) . . ? C22 C21 Rh1 118.6(4) . . ? C21 Rh1 N4 76.98(19) . . ? C21 Rh1 N1 77.04(19) . . ? N4 Rh1 N1 153.98(16) . . ? C21 Rh1 O1 175.54(17) . . ? N4 Rh1 O1 100.96(15) . . ? N1 Rh1 O1 105.06(15) . . ? C21 Rh1 Cl1 92.66(14) . . ? N4 Rh1 Cl1 88.79(12) . . ? N1 Rh1 Cl1 90.91(11) . . ? O1 Rh1 Cl1 91.25(10) . . ? C21 Rh1 Cl2 91.58(14) . . ? N4 Rh1 Cl2 92.01(12) . . ? N1 Rh1 Cl2 90.19(11) . . ? O1 Rh1 Cl2 84.51(10) . . ? Cl1 Rh1 Cl2 175.76(5) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.275 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.128 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END # Attachment '- SBSH1_c2.CIF' data_sbsh1 _database_code_depnum_ccdc_archive 'CCDC 810561' #TrackingRef '- SBSH1_c2.CIF' _refine_special_details ; Minor disorder in C1--C6 ring modelled by high U values. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.195 -0.250 0.380 430.7 65.2 2 0.805 0.250 0.619 430.8 64.5 _platon_squeeze_details ; Solvent region treated using PLATON SQUEEZE: gave 130 electrons/cell corresponding to six molecules of MeCN per unit cell. These MeCN are included in the formula and in the calculation of density, etc. The void volume in the cell was 865 cubic Angstroms. Details below. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H26 Cl2 N8 Rh2' _chemical_formula_sum 'C36 H26 Cl2 N8 Rh2' _chemical_formula_weight 847.37 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' _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 15.3407(15) _cell_length_b 13.3922(13) _cell_length_c 19.0850(19) _cell_angle_alpha 90.00 _cell_angle_beta 103.245(2) _cell_angle_gamma 90.00 _cell_volume 3816.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5571 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.7 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 1.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.598 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_process_details '(Bruker SHELXTL; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART1000 CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23798 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8634 _reflns_number_gt 5507 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ' ?' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8634 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.84 _refine_ls_restrained_S_all 0.84 _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 0.283778(19) 0.36972(2) 0.356989(15) 0.02902(8) Uani 1 1 d . . . Rh2 Rh 0.304277(18) 0.17877(2) 0.322149(14) 0.02699(8) Uani 1 1 d . . . Cl1 Cl 0.25411(6) 0.53375(7) 0.38914(5) 0.0414(2) Uani 1 1 d . . . Cl2 Cl 0.31052(7) 0.00958(7) 0.29245(5) 0.0414(2) Uani 1 1 d . . . C1 C 0.1357(3) 0.4256(4) 0.2212(2) 0.0499(12) Uani 1 1 d . . . C2 C 0.1918(3) 0.4982(4) 0.2078(2) 0.0586(14) Uani 1 1 d . . . H2A H 0.2472 0.5102 0.2410 0.070 Uiso 1 1 calc R . . C3 C 0.1675(4) 0.5548(4) 0.1449(3) 0.0710(16) Uani 1 1 d . . . H3A H 0.2062 0.6059 0.1354 0.085 Uiso 1 1 calc R . . C4 C 0.0882(5) 0.5368(5) 0.0972(3) 0.095(2) Uani 1 1 d . . . H4A H 0.0717 0.5751 0.0543 0.114 Uiso 1 1 calc R . . C5 C 0.0320(5) 0.4629(6) 0.1113(3) 0.102(3) Uani 1 1 d . . . H5A H -0.0236 0.4510 0.0783 0.122 Uiso 1 1 calc R . . C6 C 0.0556(3) 0.4063(4) 0.1727(2) 0.0678(15) Uani 1 1 d . . . H6A H 0.0173 0.3545 0.1817 0.081 Uiso 1 1 calc R . . N7 N 0.1625(2) 0.3702(2) 0.28750(16) 0.0390(8) Uani 1 1 d . . . N8 N 0.0997(2) 0.3203(3) 0.30512(18) 0.0454(9) Uani 1 1 d . . . C9 C 0.1333(3) 0.2625(3) 0.3666(2) 0.0400(10) Uani 1 1 d . . . C10 C 0.0733(3) 0.2302(4) 0.4071(2) 0.0534(12) Uani 1 1 d . . . H10A H 0.0108 0.2412 0.3902 0.064 Uiso 1 1 calc R . . C11 C 0.1057(3) 0.1824(4) 0.4719(2) 0.0539(12) Uani 1 1 d . . . H11A H 0.0654 0.1626 0.5005 0.065 Uiso 1 1 calc R . . C12 C 0.1955(3) 0.1630(3) 0.4955(2) 0.0442(10) Uani 1 1 d . . . H12A H 0.2169 0.1319 0.5410 0.053 Uiso 1 1 calc R . . C13 C 0.2561(2) 0.1882(3) 0.45368(19) 0.0326(9) Uani 1 1 d . . . C14 C 0.2269(2) 0.2416(3) 0.38707(18) 0.0333(9) Uani 1 1 d . . . N15 N 0.3432(2) 0.1567(2) 0.47504(15) 0.0308(7) Uani 1 1 d . . . N16 N 0.38144(19) 0.1526(2) 0.42220(15) 0.0286(7) Uani 1 1 d . . . C17 C 0.4751(2) 0.1298(2) 0.43858(19) 0.0287(8) Uani 1 1 d . . . C18 C 0.5252(3) 0.1293(3) 0.5097(2) 0.0388(9) Uani 1 1 d . . . H18A H 0.4973 0.1439 0.5481 0.047 Uiso 1 1 calc R . . C19 C 0.6156(3) 0.1076(3) 0.5238(2) 0.0479(11) Uani 1 1 d . . . H19A H 0.6499 0.1062 0.5720 0.057 Uiso 1 1 calc R . . C20 C 0.6558(3) 0.0878(3) 0.4675(2) 0.0495(11) Uani 1 1 d . . . H20A H 0.7183 0.0747 0.4772 0.059 Uiso 1 1 calc R . . C21 C 0.6064(3) 0.0870(3) 0.3978(2) 0.0489(11) Uani 1 1 d . . . H21A H 0.6344 0.0724 0.3595 0.059 Uiso 1 1 calc R . . C22 C 0.5153(3) 0.1076(3) 0.3834(2) 0.0386(9) Uani 1 1 d . . . H22A H 0.4808 0.1062 0.3352 0.046 Uiso 1 1 calc R . . C1' C 0.4242(2) 0.3819(3) 0.50445(18) 0.0298(8) Uani 1 1 d . . . C2' C 0.3528(3) 0.4018(3) 0.5354(2) 0.0355(9) Uani 1 1 d . . . H2'A H 0.2938 0.4072 0.5064 0.043 Uiso 1 1 calc R . . C3' C 0.3688(3) 0.4140(3) 0.6101(2) 0.0441(10) Uani 1 1 d . . . H3'A H 0.3208 0.4297 0.6320 0.053 Uiso 1 1 calc R . . C4' C 0.4541(3) 0.4030(3) 0.6516(2) 0.0478(11) Uani 1 1 d . . . H4'A H 0.4645 0.4085 0.7024 0.057 Uiso 1 1 calc R . . C5' C 0.5250(3) 0.3841(3) 0.6200(2) 0.0436(10) Uani 1 1 d . . . H5'A H 0.5838 0.3779 0.6493 0.052 Uiso 1 1 calc R . . C6' C 0.5113(3) 0.3741(3) 0.54633(19) 0.0371(9) Uani 1 1 d . . . H6'A H 0.5602 0.3622 0.5246 0.044 Uiso 1 1 calc R . . N7' N 0.40627(19) 0.3702(2) 0.42747(15) 0.0271(6) Uani 1 1 d . . . N8' N 0.47490(19) 0.3605(2) 0.40093(15) 0.0289(7) Uani 1 1 d . . . C9' C 0.4518(2) 0.3432(2) 0.32692(18) 0.0274(8) Uani 1 1 d . . . C10' C 0.5145(2) 0.3655(3) 0.28668(19) 0.0331(8) Uani 1 1 d . . . H10B H 0.5741 0.3820 0.3105 0.040 Uiso 1 1 calc R . . C11' C 0.4904(3) 0.3638(3) 0.2126(2) 0.0358(9) Uani 1 1 d . . . H11B H 0.5326 0.3818 0.1854 0.043 Uiso 1 1 calc R . . C12' C 0.4043(2) 0.3359(3) 0.17771(19) 0.0313(8) Uani 1 1 d . . . H12B H 0.3868 0.3383 0.1267 0.038 Uiso 1 1 calc R . . C13' C 0.3437(2) 0.3043(2) 0.21671(18) 0.0273(8) Uani 1 1 d . . . C14' C 0.3643(2) 0.3084(2) 0.29411(17) 0.0265(8) Uani 1 1 d . . . N15' N 0.26480(19) 0.2597(2) 0.17980(15) 0.0315(7) Uani 1 1 d . . . N16' N 0.23085(19) 0.2021(2) 0.21980(15) 0.0299(7) Uani 1 1 d . . . C17' C 0.1507(2) 0.1517(3) 0.1847(2) 0.0331(9) Uani 1 1 d . . . C18' C 0.1230(3) 0.1507(3) 0.1095(2) 0.0507(12) Uani 1 1 d . . . H18B H 0.1579 0.1831 0.0810 0.061 Uiso 1 1 calc R . . C19' C 0.0454(3) 0.1028(4) 0.0773(3) 0.0701(15) Uani 1 1 d . . . H19B H 0.0276 0.1013 0.0263 0.084 Uiso 1 1 calc R . . C20' C -0.0076(3) 0.0566(4) 0.1172(3) 0.0732(16) Uani 1 1 d . . . H20B H -0.0625 0.0255 0.0943 0.088 Uiso 1 1 calc R . . C21' C 0.0213(3) 0.0567(4) 0.1910(3) 0.0749(16) Uani 1 1 d . . . H21B H -0.0142 0.0252 0.2194 0.090 Uiso 1 1 calc R . . C22' C 0.1008(3) 0.1019(3) 0.2244(2) 0.0547(12) Uani 1 1 d . . . H22B H 0.1210 0.0984 0.2753 0.066 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 0.03229(17) 0.03462(17) 0.01994(15) 0.00012(12) 0.00557(12) 0.00526(13) Rh2 0.03260(16) 0.03233(16) 0.01551(14) -0.00018(12) 0.00441(11) -0.00188(13) Cl1 0.0402(6) 0.0391(6) 0.0451(6) -0.0035(4) 0.0099(5) 0.0090(4) Cl2 0.0675(7) 0.0308(5) 0.0216(5) -0.0023(4) 0.0010(5) 0.0054(5) C1 0.054(3) 0.069(3) 0.025(2) 0.002(2) 0.005(2) 0.033(2) C2 0.067(3) 0.077(3) 0.036(3) 0.022(2) 0.020(2) 0.042(3) C3 0.091(4) 0.086(4) 0.041(3) 0.026(3) 0.026(3) 0.055(3) C4 0.134(6) 0.120(6) 0.032(3) 0.018(3) 0.021(4) 0.084(5) C5 0.116(6) 0.147(7) 0.027(3) -0.004(4) -0.013(3) 0.077(5) C6 0.067(3) 0.097(4) 0.028(3) -0.010(3) -0.010(2) 0.036(3) N7 0.0397(19) 0.054(2) 0.0234(17) 0.0008(15) 0.0067(15) 0.0133(16) N8 0.0348(19) 0.068(2) 0.0312(19) -0.0098(18) 0.0030(16) 0.0087(18) C9 0.035(2) 0.054(3) 0.031(2) -0.0128(19) 0.0068(18) -0.0033(19) C10 0.037(2) 0.083(3) 0.043(3) -0.016(2) 0.014(2) -0.013(2) C11 0.044(3) 0.086(4) 0.037(3) -0.016(2) 0.019(2) -0.025(2) C12 0.055(3) 0.054(3) 0.026(2) -0.0069(19) 0.015(2) -0.021(2) C13 0.036(2) 0.040(2) 0.0222(19) -0.0065(16) 0.0064(16) -0.0104(17) C14 0.036(2) 0.044(2) 0.0204(19) -0.0051(16) 0.0077(17) -0.0043(17) N15 0.0430(19) 0.0329(18) 0.0179(15) -0.0021(12) 0.0097(14) -0.0078(14) N16 0.0379(18) 0.0286(17) 0.0185(16) 0.0001(12) 0.0045(13) -0.0023(13) C17 0.038(2) 0.0224(18) 0.0233(19) 0.0015(15) 0.0027(16) 0.0014(16) C18 0.054(3) 0.037(2) 0.024(2) 0.0044(17) 0.0056(19) -0.0050(19) C19 0.050(3) 0.053(3) 0.034(2) 0.011(2) -0.004(2) 0.003(2) C20 0.043(3) 0.048(3) 0.053(3) 0.005(2) 0.002(2) 0.009(2) C21 0.050(3) 0.058(3) 0.038(3) -0.009(2) 0.008(2) 0.015(2) C22 0.046(2) 0.044(2) 0.024(2) -0.0039(17) 0.0040(18) 0.0056(18) C1' 0.043(2) 0.029(2) 0.0171(18) -0.0041(15) 0.0060(16) -0.0070(16) C2' 0.049(2) 0.031(2) 0.028(2) -0.0026(16) 0.0108(19) -0.0038(17) C3' 0.076(3) 0.033(2) 0.029(2) -0.0019(17) 0.023(2) -0.010(2) C4' 0.085(3) 0.041(2) 0.017(2) -0.0031(17) 0.011(2) -0.019(2) C5' 0.062(3) 0.041(2) 0.022(2) 0.0009(17) -0.003(2) -0.014(2) C6' 0.050(2) 0.036(2) 0.023(2) -0.0016(17) 0.0056(18) -0.0067(18) N7' 0.0371(17) 0.0259(15) 0.0202(15) -0.0043(12) 0.0104(14) -0.0016(13) N8' 0.0357(17) 0.0296(17) 0.0204(16) -0.0002(12) 0.0045(13) -0.0006(13) C9' 0.0284(19) 0.030(2) 0.0230(19) -0.0022(15) 0.0044(15) 0.0026(15) C10' 0.035(2) 0.038(2) 0.026(2) -0.0047(16) 0.0061(17) -0.0029(17) C11' 0.043(2) 0.038(2) 0.031(2) -0.0023(17) 0.0165(19) -0.0072(18) C12' 0.042(2) 0.036(2) 0.0176(18) 0.0012(15) 0.0097(16) 0.0001(17) C13' 0.033(2) 0.0271(19) 0.0203(18) 0.0013(14) 0.0040(15) -0.0017(15) C14' 0.032(2) 0.029(2) 0.0186(18) 0.0017(14) 0.0064(15) 0.0053(15) N15' 0.0362(18) 0.0378(18) 0.0203(16) 0.0009(13) 0.0059(14) -0.0015(14) N16' 0.0311(17) 0.0369(18) 0.0219(16) -0.0006(13) 0.0065(13) -0.0018(13) C17' 0.029(2) 0.042(2) 0.027(2) -0.0007(16) 0.0042(16) -0.0037(16) C18' 0.047(3) 0.076(3) 0.026(2) -0.001(2) 0.001(2) -0.019(2) C19' 0.068(3) 0.098(4) 0.035(3) -0.005(3) -0.007(2) -0.030(3) C20' 0.057(3) 0.113(4) 0.047(3) -0.015(3) 0.005(3) -0.040(3) C21' 0.067(3) 0.114(5) 0.047(3) -0.014(3) 0.017(3) -0.049(3) C22' 0.058(3) 0.080(3) 0.028(2) -0.007(2) 0.013(2) -0.029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 Rh2 2.6789(5) . ? Rh1 Cl1 2.3531(10) . ? Rh1 N7 2.022(3) . ? Rh1 N7' 2.045(3) . ? Rh1 C14 2.065(4) . ? Rh1 C14' 2.078(3) . ? Rh2 Cl2 2.3430(9) . ? Rh2 N16 2.033(3) . ? Rh2 N16' 2.043(3) . ? Rh2 C14 2.080(3) . ? Rh2 C14' 2.091(3) . ? C1 C2 1.363(6) . ? C1 C6 1.383(6) . ? C1 N7 1.442(5) . ? C2 C3 1.396(6) . ? C2 H2A 0.9500 . ? C3 C4 1.363(8) . ? C3 H3A 0.9500 . ? C4 C5 1.380(9) . ? C4 H4A 0.9500 . ? C5 C6 1.372(7) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? N7 N8 1.278(4) . ? N8 C9 1.402(5) . ? C9 C10 1.399(5) . ? C9 C14 1.426(5) . ? C10 C11 1.381(6) . ? C10 H10A 0.9500 . ? C11 C12 1.373(6) . ? C11 H11A 0.9500 . ? C12 C13 1.398(5) . ? C12 H12A 0.9500 . ? C13 N15 1.371(4) . ? C13 C14 1.438(5) . ? N15 N16 1.279(4) . ? N16 C17 1.432(4) . ? C17 C22 1.369(5) . ? C17 C18 1.399(5) . ? C18 C19 1.381(5) . ? C18 H18A 0.9500 . ? C19 C20 1.381(6) . ? C19 H19A 0.9500 . ? C20 C21 1.373(6) . ? C20 H20A 0.9500 . ? C21 C22 1.388(5) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C1' C2' 1.383(5) . ? C1' C6' 1.395(5) . ? C1' N7' 1.440(4) . ? C2' C3' 1.399(5) . ? C2' H2'A 0.9500 . ? C3' C4' 1.374(6) . ? C3' H3'A 0.9500 . ? C4' C5' 1.382(6) . ? C4' H4'A 0.9500 . ? C5' C6' 1.380(5) . ? C5' H5'A 0.9500 . ? C6' H6'A 0.9500 . ? N7' N8' 1.275(4) . ? N8' C9' 1.395(4) . ? C9' C10' 1.393(5) . ? C9' C14' 1.424(5) . ? C10' C11' 1.378(5) . ? C10' H10B 0.9500 . ? C11' C12' 1.387(5) . ? C11' H11B 0.9500 . ? C12' C13' 1.384(5) . ? C12' H12B 0.9500 . ? C13' N15' 1.388(4) . ? C13' C14' 1.439(4) . ? N15' N16' 1.277(4) . ? N16' C17' 1.428(4) . ? C17' C22' 1.368(5) . ? C17' C18' 1.401(5) . ? C18' C19' 1.368(6) . ? C18' H18B 0.9500 . ? C19' C20' 1.381(6) . ? C19' H19B 0.9500 . ? C20' C21' 1.377(6) . ? C20' H20B 0.9500 . ? C21' C22' 1.380(6) . ? C21' H21B 0.9500 . ? C22' H22B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Rh1 N7' 179.62(12) . . ? N7 Rh1 C14 78.51(14) . . ? N7' Rh1 C14 101.71(13) . . ? N7 Rh1 C14' 101.63(13) . . ? N7' Rh1 C14' 78.64(12) . . ? C14 Rh1 C14' 100.20(13) . . ? N7 Rh1 Cl1 87.95(9) . . ? N7' Rh1 Cl1 91.67(8) . . ? C14 Rh1 Cl1 125.71(10) . . ? C14' Rh1 Cl1 134.08(10) . . ? N7 Rh1 Rh2 89.02(9) . . ? N7' Rh1 Rh2 91.36(8) . . ? C14 Rh1 Rh2 49.99(10) . . ? C14' Rh1 Rh2 50.22(9) . . ? Cl1 Rh1 Rh2 175.27(3) . . ? N16 Rh2 N16' 177.54(11) . . ? N16 Rh2 C14 78.42(13) . . ? N16' Rh2 C14 104.04(13) . . ? N16 Rh2 C14' 100.81(12) . . ? N16' Rh2 C14' 78.87(12) . . ? C14 Rh2 C14' 99.28(13) . . ? N16 Rh2 Cl2 90.77(8) . . ? N16' Rh2 Cl2 87.75(8) . . ? C14 Rh2 Cl2 126.58(10) . . ? C14' Rh2 Cl2 134.11(9) . . ? N16 Rh2 Rh1 90.42(8) . . ? N16' Rh2 Rh1 91.20(8) . . ? C14 Rh2 Rh1 49.49(10) . . ? C14' Rh2 Rh1 49.81(9) . . ? Cl2 Rh2 Rh1 175.46(3) . . ? C2 C1 C6 120.7(4) . . ? C2 C1 N7 117.8(4) . . ? C6 C1 N7 121.5(5) . . ? C1 C2 C3 119.6(5) . . ? C1 C2 H2A 120.2 . . ? C3 C2 H2A 120.2 . . ? C4 C3 C2 120.0(6) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 119.9(6) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.6(6) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 C1 119.3(6) . . ? C5 C6 H6A 120.4 . . ? C1 C6 H6A 120.4 . . ? N8 N7 C1 114.7(3) . . ? N8 N7 Rh1 117.5(3) . . ? C1 N7 Rh1 127.7(3) . . ? N7 N8 C9 110.7(3) . . ? C10 C9 N8 118.1(4) . . ? C10 C9 C14 122.5(4) . . ? N8 C9 C14 119.4(3) . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C12 C11 C10 120.7(4) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 121.0(4) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? N15 C13 C12 119.1(3) . . ? N15 C13 C14 120.1(3) . . ? C12 C13 C14 120.8(4) . . ? C9 C14 C13 115.4(3) . . ? C9 C14 Rh1 103.0(3) . . ? C13 C14 Rh1 126.4(3) . . ? C9 C14 Rh2 126.3(3) . . ? C13 C14 Rh2 102.7(2) . . ? Rh1 C14 Rh2 80.52(12) . . ? N16 N15 C13 111.7(3) . . ? N15 N16 C17 117.1(3) . . ? N15 N16 Rh2 117.4(2) . . ? C17 N16 Rh2 125.5(2) . . ? C22 C17 C18 120.1(3) . . ? C22 C17 N16 119.0(3) . . ? C18 C17 N16 120.9(3) . . ? C19 C18 C17 119.5(4) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C18 C19 C20 119.8(4) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 119.9(4) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C17 C22 C21 120.1(4) . . ? C17 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C2' C1' C6' 121.2(3) . . ? C2' C1' N7' 118.2(3) . . ? C6' C1' N7' 120.7(3) . . ? C1' C2' C3' 119.1(4) . . ? C1' C2' H2'A 120.4 . . ? C3' C2' H2'A 120.4 . . ? C4' C3' C2' 119.8(4) . . ? C4' C3' H3'A 120.1 . . ? C2' C3' H3'A 120.1 . . ? C3' C4' C5' 120.6(4) . . ? C3' C4' H4'A 119.7 . . ? C5' C4' H4'A 119.7 . . ? C6' C5' C4' 120.7(4) . . ? C6' C5' H5'A 119.6 . . ? C4' C5' H5'A 119.6 . . ? C5' C6' C1' 118.6(4) . . ? C5' C6' H6'A 120.7 . . ? C1' C6' H6'A 120.7 . . ? N8' N7' C1' 115.7(3) . . ? N8' N7' Rh1 117.1(2) . . ? C1' N7' Rh1 127.1(2) . . ? N7' N8' C9' 112.2(3) . . ? C10' C9' N8' 118.4(3) . . ? C10' C9' C14' 121.9(3) . . ? N8' C9' C14' 119.7(3) . . ? C11' C10' C9' 120.4(3) . . ? C11' C10' H10B 119.8 . . ? C9' C10' H10B 119.8 . . ? C10' C11' C12' 119.9(3) . . ? C10' C11' H11B 120.0 . . ? C12' C11' H11B 120.0 . . ? C13' C12' C11' 120.5(3) . . ? C13' C12' H12B 119.7 . . ? C11' C12' H12B 119.7 . . ? C12' C13' N15' 118.3(3) . . ? C12' C13' C14' 121.6(3) . . ? N15' C13' C14' 119.9(3) . . ? C9' C14' C13' 115.3(3) . . ? C9' C14' Rh1 104.0(2) . . ? C13' C14' Rh1 126.0(2) . . ? C9' C14' Rh2 125.8(2) . . ? C13' C14' Rh2 103.0(2) . . ? Rh1 C14' Rh2 79.96(12) . . ? N16' N15' C13' 112.6(3) . . ? N15' N16' C17' 115.5(3) . . ? N15' N16' Rh2 116.9(2) . . ? C17' N16' Rh2 127.1(2) . . ? C22' C17' C18' 119.2(4) . . ? C22' C17' N16' 120.1(3) . . ? C18' C17' N16' 120.7(3) . . ? C19' C18' C17' 119.5(4) . . ? C19' C18' H18B 120.3 . . ? C17' C18' H18B 120.3 . . ? C18' C19' C20' 121.7(4) . . ? C18' C19' H19B 119.2 . . ? C20' C19' H19B 119.2 . . ? C21' C20' C19' 118.1(4) . . ? C21' C20' H20B 121.0 . . ? C19' C20' H20B 121.0 . . ? C20' C21' C22' 121.1(4) . . ? C20' C21' H21B 119.4 . . ? C22' C21' H21B 119.4 . . ? C17' C22' C21' 120.3(4) . . ? C17' C22' H22B 119.8 . . ? C21' C22' H22B 119.8 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.85 _refine_diff_density_min -0.81 _refine_diff_density_rms 0.09 # Attachment '- pm9_c3.cif' data_pm9_gm _database_code_depnum_ccdc_archive 'CCDC 810562' #TrackingRef '- pm9_c3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 Cl2 N5 O0 Rh' _chemical_formula_weight 562.25 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2704(2) _cell_length_b 13.3655(2) _cell_length_c 15.7056(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.1000(10) _cell_angle_gamma 90.00 _cell_volume 2365.80(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42985 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.86 _reflns_number_total 6207 _reflns_number_gt 4740 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0239P)^2^+0.8466P] 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 6207 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0647 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 -0.282527(14) -0.314739(12) 0.263428(10) 0.04685(6) Uani 1 1 d . . . Cl1 Cl -0.12984(5) -0.26422(4) 0.35481(4) 0.05787(14) Uani 1 1 d . . . Cl2 Cl -0.42785(5) -0.36481(5) 0.16696(4) 0.07103(17) Uani 1 1 d . . . N1 N -0.38770(17) -0.11854(15) 0.28997(13) 0.0653(5) Uani 1 1 d . . . N2 N -0.31653(16) -0.16261(14) 0.23848(12) 0.0561(4) Uani 1 1 d . . . N3 N -0.38611(15) -0.44981(15) 0.38732(12) 0.0578(5) Uani 1 1 d . . . N4 N -0.30849(14) -0.44837(13) 0.32818(11) 0.0494(4) Uani 1 1 d . . . N5 N -0.14067(16) -0.35536(14) 0.17261(11) 0.0550(4) Uani 1 1 d . . . C1 C -0.39625(18) -0.28141(18) 0.34541(14) 0.0536(5) Uani 1 1 d . . . C2 C -0.4337(2) -0.18361(19) 0.35058(16) 0.0628(6) Uani 1 1 d . . . C3 C -0.5113(2) -0.1570(2) 0.41584(18) 0.0792(8) Uani 1 1 d . . . H3 H -0.5368 -0.0912 0.4218 0.095 Uiso 1 1 calc R . . C4 C -0.5495(2) -0.2299(3) 0.47138(18) 0.0846(9) Uani 1 1 d . . . H4 H -0.6010 -0.2119 0.5150 0.101 Uiso 1 1 calc R . . C5 C -0.5145(2) -0.3289(2) 0.46498(16) 0.0731(7) Uani 1 1 d . . . H5 H -0.5432 -0.3769 0.5026 0.088 Uiso 1 1 calc R . . C6 C -0.43477(19) -0.35500(19) 0.40038(14) 0.0592(6) Uani 1 1 d . . . C7 C -0.2661(2) -0.09825(17) 0.17535(14) 0.0583(5) Uani 1 1 d . . . C8 C -0.2575(3) 0.0034(2) 0.18815(18) 0.0919(10) Uani 1 1 d . . . H8 H -0.2852 0.0318 0.2384 0.110 Uiso 1 1 calc R . . C9 C -0.2078(4) 0.0624(2) 0.1263(2) 0.1119(13) Uani 1 1 d . . . H9 H -0.2021 0.1311 0.1347 0.134 Uiso 1 1 calc R . . C10 C -0.1663(3) 0.0210(2) 0.05223(19) 0.0911(9) Uani 1 1 d . . . H10 H -0.1315 0.0613 0.0110 0.109 Uiso 1 1 calc R . . C11 C -0.1761(3) -0.0791(2) 0.03937(17) 0.0773(7) Uani 1 1 d . . . H11 H -0.1486 -0.1070 -0.0111 0.093 Uiso 1 1 calc R . . C12 C -0.2263(2) -0.13975(19) 0.10046(15) 0.0654(6) Uani 1 1 d . . . H12 H -0.2331 -0.2082 0.0911 0.078 Uiso 1 1 calc R . . C13 C -0.25663(18) -0.54407(16) 0.31028(12) 0.0479(5) Uani 1 1 d . . . C14 C -0.13562(19) -0.54843(17) 0.29865(13) 0.0548(5) Uani 1 1 d . . . H14 H -0.0895 -0.4909 0.3015 0.066 Uiso 1 1 calc R . . C15 C -0.0844(2) -0.64066(19) 0.28257(15) 0.0632(6) Uani 1 1 d . . . H15 H -0.0027 -0.6455 0.2754 0.076 Uiso 1 1 calc R . . C16 C -0.1536(2) -0.72510(19) 0.27712(16) 0.0682(6) Uani 1 1 d . . . H16 H -0.1188 -0.7866 0.2653 0.082 Uiso 1 1 calc R . . C17 C -0.2738(3) -0.7189(2) 0.28906(17) 0.0722(7) Uani 1 1 d . . . H17 H -0.3201 -0.7764 0.2853 0.087 Uiso 1 1 calc R . . C18 C -0.3268(2) -0.62822(18) 0.30654(15) 0.0608(6) Uani 1 1 d . . . H18 H -0.4081 -0.6240 0.3156 0.073 Uiso 1 1 calc R . . C19 C -0.06085(19) -0.37555(16) 0.13169(13) 0.0499(5) Uani 1 1 d . . . C20 C 0.03908(17) -0.40159(16) 0.07964(12) 0.0469(4) Uani 1 1 d . . . C21 C 0.0687(2) -0.34279(19) 0.01019(15) 0.0642(6) Uani 1 1 d . . . H21 H 0.0276 -0.2839 -0.0012 0.077 Uiso 1 1 calc R . . C22 C 0.1606(2) -0.3736(2) -0.04173(16) 0.0788(8) Uani 1 1 d . . . H22 H 0.1815 -0.3352 -0.0887 0.095 Uiso 1 1 calc R . . C23 C 0.2212(2) -0.4600(2) -0.02464(19) 0.0772(8) Uani 1 1 d . . . H23 H 0.2821 -0.4804 -0.0605 0.093 Uiso 1 1 calc R . . C24 C 0.1928(2) -0.5158(2) 0.04416(19) 0.0738(7) Uani 1 1 d . . . H24 H 0.2355 -0.5738 0.0558 0.089 Uiso 1 1 calc R . . C25 C 0.1019(2) -0.48803(18) 0.09706(15) 0.0591(5) Uani 1 1 d . . . H25 H 0.0827 -0.5270 0.1441 0.071 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 0.04330(9) 0.04574(10) 0.05152(9) -0.00718(7) 0.00594(6) 0.00665(7) Cl1 0.0545(3) 0.0578(3) 0.0613(3) -0.0035(3) -0.0015(2) -0.0053(2) Cl2 0.0610(3) 0.0803(4) 0.0718(4) -0.0162(3) -0.0111(3) 0.0041(3) N1 0.0628(12) 0.0605(12) 0.0727(13) -0.0137(10) 0.0005(10) 0.0230(10) N2 0.0571(10) 0.0514(11) 0.0599(10) -0.0085(9) -0.0040(8) 0.0138(8) N3 0.0463(10) 0.0681(12) 0.0590(10) -0.0026(9) 0.0095(8) 0.0005(9) N4 0.0420(9) 0.0526(10) 0.0536(9) -0.0044(8) 0.0060(7) 0.0019(8) N5 0.0572(11) 0.0493(10) 0.0584(10) -0.0051(8) 0.0094(9) 0.0045(9) C1 0.0410(10) 0.0628(14) 0.0570(12) -0.0129(10) 0.0036(9) 0.0105(10) C2 0.0530(12) 0.0682(15) 0.0674(14) -0.0130(12) 0.0026(10) 0.0198(12) C3 0.0633(15) 0.090(2) 0.0842(18) -0.0206(16) 0.0113(14) 0.0300(14) C4 0.0622(16) 0.117(3) 0.0742(17) -0.0210(17) 0.0176(13) 0.0275(16) C5 0.0541(13) 0.100(2) 0.0651(14) -0.0034(14) 0.0158(11) 0.0122(13) C6 0.0455(11) 0.0721(15) 0.0602(13) -0.0082(12) 0.0091(10) 0.0082(11) C7 0.0676(14) 0.0483(12) 0.0588(13) -0.0014(10) -0.0100(10) 0.0092(11) C8 0.159(3) 0.0508(15) 0.0663(16) -0.0097(13) -0.0011(18) 0.0081(17) C9 0.206(4) 0.0531(17) 0.077(2) 0.0008(15) 0.000(2) -0.015(2) C10 0.134(3) 0.072(2) 0.0672(17) 0.0105(15) -0.0070(17) -0.0111(18) C11 0.098(2) 0.0734(19) 0.0605(15) -0.0005(13) 0.0011(13) 0.0098(15) C12 0.0779(16) 0.0543(14) 0.0638(14) -0.0059(12) -0.0028(12) 0.0081(12) C13 0.0485(11) 0.0481(12) 0.0470(10) -0.0010(9) 0.0026(8) 0.0038(9) C14 0.0512(12) 0.0529(13) 0.0604(12) 0.0000(10) 0.0048(10) 0.0029(10) C15 0.0565(13) 0.0658(15) 0.0673(14) 0.0050(12) 0.0028(11) 0.0152(12) C16 0.0850(18) 0.0518(14) 0.0677(15) 0.0014(12) -0.0037(13) 0.0187(13) C17 0.0869(19) 0.0489(14) 0.0808(17) -0.0023(12) -0.0036(14) -0.0071(13) C18 0.0548(13) 0.0591(14) 0.0684(14) -0.0047(11) 0.0011(10) -0.0048(11) C19 0.0527(12) 0.0470(12) 0.0500(11) -0.0051(9) 0.0031(9) 0.0000(9) C20 0.0437(10) 0.0495(12) 0.0476(10) -0.0056(9) 0.0044(8) -0.0024(9) C21 0.0616(14) 0.0659(15) 0.0652(14) 0.0084(12) 0.0043(11) -0.0039(12) C22 0.0735(17) 0.101(2) 0.0619(15) 0.0028(15) 0.0171(13) -0.0304(17) C23 0.0491(13) 0.088(2) 0.0942(19) -0.0295(16) 0.0253(13) -0.0177(14) C24 0.0487(13) 0.0703(17) 0.102(2) -0.0111(15) 0.0117(13) 0.0048(12) C25 0.0552(13) 0.0585(14) 0.0637(13) 0.0025(11) 0.0071(10) 0.0019(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.872(2) . ? Rh1 N4 2.0763(18) . ? Rh1 N2 2.1058(18) . ? Rh1 N5 2.2121(17) . ? Rh1 Cl2 2.3276(6) . ? Rh1 Cl1 2.3385(6) . ? N1 N2 1.283(2) . ? N1 C2 1.390(3) . ? N2 C7 1.431(3) . ? N3 N4 1.277(2) . ? N3 C6 1.396(3) . ? N4 C13 1.434(3) . ? N5 C19 1.139(2) . ? C1 C2 1.376(3) . ? C1 C6 1.379(3) . ? C2 C3 1.395(3) . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.385(4) . ? C4 H4 0.9300 . ? C5 C6 1.401(3) . ? C5 H5 0.9300 . ? C7 C8 1.376(3) . ? C7 C12 1.377(3) . ? C8 C9 1.372(4) . ? C8 H8 0.9300 . ? C9 C10 1.371(4) . ? C9 H9 0.9300 . ? C10 C11 1.357(4) . ? C10 H10 0.9300 . ? C11 C12 1.378(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.376(3) . ? C13 C14 1.377(3) . ? C14 C15 1.384(3) . ? C14 H14 0.9300 . ? C15 C16 1.374(4) . ? C15 H15 0.9300 . ? C16 C17 1.371(4) . ? C16 H16 0.9300 . ? C17 C18 1.379(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.436(3) . ? C20 C25 1.382(3) . ? C20 C21 1.386(3) . ? C21 C22 1.382(4) . ? C21 H21 0.9300 . ? C22 C23 1.368(4) . ? C22 H22 0.9300 . ? C23 C24 1.352(4) . ? C23 H23 0.9300 . ? C24 C25 1.372(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? 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 N4 76.73(9) . . ? C1 Rh1 N2 76.92(9) . . ? N4 Rh1 N2 153.64(7) . . ? C1 Rh1 N5 176.68(8) . . ? N4 Rh1 N5 101.97(6) . . ? N2 Rh1 N5 104.39(7) . . ? C1 Rh1 Cl2 91.97(7) . . ? N4 Rh1 Cl2 88.39(5) . . ? N2 Rh1 Cl2 91.66(5) . . ? N5 Rh1 Cl2 91.05(5) . . ? C1 Rh1 Cl1 90.75(7) . . ? N4 Rh1 Cl1 92.98(5) . . ? N2 Rh1 Cl1 88.22(5) . . ? N5 Rh1 Cl1 86.26(5) . . ? Cl2 Rh1 Cl1 177.18(2) . . ? N2 N1 C2 112.24(19) . . ? N1 N2 C7 114.21(19) . . ? N1 N2 Rh1 116.09(16) . . ? C7 N2 Rh1 129.57(14) . . ? N4 N3 C6 111.28(18) . . ? N3 N4 C13 114.14(17) . . ? N3 N4 Rh1 117.81(14) . . ? C13 N4 Rh1 127.82(12) . . ? C19 N5 Rh1 173.97(18) . . ? C2 C1 C6 122.9(2) . . ? C2 C1 Rh1 118.48(18) . . ? C6 C1 Rh1 118.52(17) . . ? C1 C2 C3 118.6(3) . . ? C1 C2 N1 116.1(2) . . ? C3 C2 N1 125.4(2) . . ? C4 C3 C2 118.9(3) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 122.7(2) . . ? C3 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? C4 C5 C6 118.3(3) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C1 C6 N3 115.53(18) . . ? C1 C6 C5 118.6(2) . . ? N3 C6 C5 125.8(2) . . ? C8 C7 C12 120.0(2) . . ? C8 C7 N2 121.3(2) . . ? C12 C7 N2 118.7(2) . . ? C7 C8 C9 119.5(3) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 119.7(3) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C7 C12 C11 119.5(2) . . ? C7 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C18 C13 C14 121.9(2) . . ? C18 C13 N4 120.20(18) . . ? C14 C13 N4 117.88(19) . . ? C13 C14 C15 118.3(2) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 120.4(2) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.2(2) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 118.6(2) . . ? C13 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? N5 C19 C20 179.5(3) . . ? C25 C20 C21 120.4(2) . . ? C25 C20 C19 119.48(19) . . ? C21 C20 C19 120.1(2) . . ? C22 C21 C20 118.5(2) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C23 C22 C21 120.6(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 120.3(2) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C20 119.3(2) . . ? C24 C25 H25 120.3 . . ? C20 C25 H25 120.3 . . ? 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 C2 N1 N2 C7 -179.47(19) . . . . ? C2 N1 N2 Rh1 -3.2(2) . . . . ? C1 Rh1 N2 N1 4.09(16) . . . . ? N4 Rh1 N2 N1 6.0(3) . . . . ? N5 Rh1 N2 N1 -172.77(16) . . . . ? Cl2 Rh1 N2 N1 95.72(16) . . . . ? Cl1 Rh1 N2 N1 -87.10(16) . . . . ? C1 Rh1 N2 C7 179.6(2) . . . . ? N4 Rh1 N2 C7 -178.46(16) . . . . ? N5 Rh1 N2 C7 2.8(2) . . . . ? Cl2 Rh1 N2 C7 -88.75(18) . . . . ? Cl1 Rh1 N2 C7 88.43(18) . . . . ? C6 N3 N4 C13 -178.78(17) . . . . ? C6 N3 N4 Rh1 -3.8(2) . . . . ? C1 Rh1 N4 N3 2.40(15) . . . . ? N2 Rh1 N4 N3 0.5(3) . . . . ? N5 Rh1 N4 N3 179.27(15) . . . . ? Cl2 Rh1 N4 N3 -90.00(15) . . . . ? Cl1 Rh1 N4 N3 92.47(15) . . . . ? C1 Rh1 N4 C13 176.57(18) . . . . ? N2 Rh1 N4 C13 174.65(16) . . . . ? N5 Rh1 N4 C13 -6.56(17) . . . . ? Cl2 Rh1 N4 C13 84.17(16) . . . . ? Cl1 Rh1 N4 C13 -93.36(16) . . . . ? C1 Rh1 N5 C19 -11(3) . . . . ? N4 Rh1 N5 C19 -77.9(17) . . . . ? N2 Rh1 N5 C19 101.5(17) . . . . ? Cl2 Rh1 N5 C19 -166.5(17) . . . . ? Cl1 Rh1 N5 C19 14.3(17) . . . . ? N4 Rh1 C1 C2 176.9(2) . . . . ? N2 Rh1 C1 C2 -3.96(18) . . . . ? N5 Rh1 C1 C2 109.6(15) . . . . ? Cl2 Rh1 C1 C2 -95.20(18) . . . . ? Cl1 Rh1 C1 C2 84.04(18) . . . . ? N4 Rh1 C1 C6 -0.23(17) . . . . ? N2 Rh1 C1 C6 178.90(19) . . . . ? N5 Rh1 C1 C6 -67.5(16) . . . . ? Cl2 Rh1 C1 C6 87.66(18) . . . . ? Cl1 Rh1 C1 C6 -93.11(18) . . . . ? C6 C1 C2 C3 2.0(4) . . . . ? Rh1 C1 C2 C3 -175.03(19) . . . . ? C6 C1 C2 N1 -179.3(2) . . . . ? Rh1 C1 C2 N1 3.7(3) . . . . ? N2 N1 C2 C1 0.0(3) . . . . ? N2 N1 C2 C3 178.6(2) . . . . ? C1 C2 C3 C4 -1.4(4) . . . . ? N1 C2 C3 C4 -180.0(2) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C3 C4 C5 C6 1.5(4) . . . . ? C2 C1 C6 N3 -178.7(2) . . . . ? Rh1 C1 C6 N3 -1.7(3) . . . . ? C2 C1 C6 C5 -0.7(4) . . . . ? Rh1 C1 C6 C5 176.27(18) . . . . ? N4 N3 C6 C1 3.6(3) . . . . ? N4 N3 C6 C5 -174.3(2) . . . . ? C4 C5 C6 C1 -1.0(4) . . . . ? C4 C5 C6 N3 176.8(2) . . . . ? N1 N2 C7 C8 23.5(3) . . . . ? Rh1 N2 C7 C8 -152.1(2) . . . . ? N1 N2 C7 C12 -156.2(2) . . . . ? Rh1 N2 C7 C12 28.2(3) . . . . ? C12 C7 C8 C9 -0.8(5) . . . . ? N2 C7 C8 C9 179.5(3) . . . . ? C7 C8 C9 C10 -0.3(6) . . . . ? C8 C9 C10 C11 1.0(6) . . . . ? C9 C10 C11 C12 -0.7(5) . . . . ? C8 C7 C12 C11 1.1(4) . . . . ? N2 C7 C12 C11 -179.2(2) . . . . ? C10 C11 C12 C7 -0.4(4) . . . . ? N3 N4 C13 C18 42.5(3) . . . . ? Rh1 N4 C13 C18 -131.82(18) . . . . ? N3 N4 C13 C14 -136.4(2) . . . . ? Rh1 N4 C13 C14 49.3(3) . . . . ? C18 C13 C14 C15 0.2(3) . . . . ? N4 C13 C14 C15 179.07(19) . . . . ? C13 C14 C15 C16 1.0(3) . . . . ? C14 C15 C16 C17 -1.1(4) . . . . ? C15 C16 C17 C18 0.1(4) . . . . ? C14 C13 C18 C17 -1.2(3) . . . . ? N4 C13 C18 C17 179.9(2) . . . . ? C16 C17 C18 C13 1.1(4) . . . . ? Rh1 N5 C19 C20 148(31) . . . . ? N5 C19 C20 C25 -84(33) . . . . ? N5 C19 C20 C21 93(33) . . . . ? C25 C20 C21 C22 1.1(3) . . . . ? C19 C20 C21 C22 -175.9(2) . . . . ? C20 C21 C22 C23 -0.2(4) . . . . ? C21 C22 C23 C24 -0.9(4) . . . . ? C22 C23 C24 C25 1.2(4) . . . . ? C23 C24 C25 C20 -0.2(4) . . . . ? C21 C20 C25 C24 -0.9(3) . . . . ? C19 C20 C25 C24 176.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.86 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.321 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.049 #===END of CIF # Attachment '- pm10_c4.cif' data_pm10mc _database_code_depnum_ccdc_archive 'CCDC 810563' #TrackingRef '- pm10_c4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H13 Cl2 N4 O Rh' _chemical_formula_weight 475.13 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' 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.488(5) _cell_length_b 12.271(2) _cell_length_c 7.9630(16) _cell_angle_alpha 90.00 _cell_angle_beta 106.575(16) _cell_angle_gamma 90.00 _cell_volume 1825.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.243 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6331 _diffrn_reflns_av_R_equivalents 0.1024 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 17.51 _reflns_number_total 579 _reflns_number_gt 481 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1892P)^2^+82.7684P] 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 579 _refine_ls_number_parameters 120 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.1045 _refine_ls_wR_factor_ref 0.3063 _refine_ls_wR_factor_gt 0.2953 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.164 _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 1.0000 0.7017(2) 1.2500 0.067(2) Uani 1 2 d S . . Cl1 Cl 1.0554(5) 0.6924(6) 1.0288(11) 0.095(3) Uani 1 1 d . . . O1 O 1.0000 0.509(2) 1.2500 0.114(12) Uani 1 2 d S . . N1 N 0.9016(16) 0.740(3) 1.053(4) 0.076(8) Uani 1 1 d . . . N2 N 0.8882(13) 0.841(3) 1.029(3) 0.073(8) Uani 1 1 d . . . C1 C 0.848(2) 0.670(4) 0.953(5) 0.067(9) Uani 1 1 d . . . C2 C 0.851(2) 0.564(4) 0.976(4) 0.091(12) Uani 1 1 d . . . H2 H 0.8889 0.5331 1.0613 0.110 Uiso 1 1 calc R . . C3 C 0.797(2) 0.499(3) 0.874(6) 0.109(13) Uani 1 1 d . . . H3 H 0.7999 0.4236 0.8891 0.131 Uiso 1 1 calc R . . C4 C 0.742(2) 0.542(3) 0.756(5) 0.093(11) Uani 1 1 d . . . H4 H 0.7058 0.4971 0.6899 0.111 Uiso 1 1 calc R . . C5 C 0.738(3) 0.649(4) 0.733(6) 0.16(2) Uani 1 1 d . . . H5 H 0.6998 0.6795 0.6489 0.196 Uiso 1 1 calc R . . C6 C 0.791(3) 0.716(3) 0.831(7) 0.16(2) Uani 1 1 d . . . H6 H 0.7878 0.7914 0.8162 0.188 Uiso 1 1 calc R . . C7 C 1.0000 0.856(3) 1.2500 0.048(10) Uani 1 2 d SU . . C8 C 1.060(2) 0.905(3) 1.365(5) 0.084(11) Uani 1 1 d . . . C9 C 1.0570(14) 1.018(3) 1.365(4) 0.078(9) Uani 1 1 d . . . H9 H 1.0935 1.0574 1.4418 0.093 Uiso 1 1 calc R . . C10 C 1.0000 1.074(4) 1.2500 0.067(12) Uani 1 2 d SU . . H10 H 1.0000 1.1496 1.2500 0.080 Uiso 1 2 calc SR . . 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 0.094(4) 0.022(3) 0.069(3) 0.000 -0.003(2) 0.000 Cl1 0.137(8) 0.046(6) 0.093(7) -0.006(4) 0.020(6) 0.014(5) O1 0.14(3) 0.014(16) 0.13(3) 0.000 -0.04(2) 0.000 N1 0.09(2) 0.024(19) 0.10(2) 0.012(18) 0.002(19) 0.02(2) N2 0.08(2) 0.04(2) 0.084(19) -0.010(17) -0.011(15) -0.009(19) C1 0.05(2) 0.05(3) 0.08(2) -0.01(3) -0.01(2) -0.01(3) C2 0.11(3) 0.02(3) 0.11(3) -0.02(2) -0.02(2) 0.02(2) C3 0.12(3) 0.06(3) 0.12(3) -0.03(3) -0.02(3) -0.02(3) C4 0.11(3) 0.06(3) 0.08(2) -0.01(2) -0.02(2) -0.02(2) C5 0.18(5) 0.03(3) 0.19(5) 0.00(3) -0.08(4) -0.01(3) C6 0.17(4) 0.03(2) 0.19(5) -0.02(3) -0.08(4) -0.02(3) C7 0.051(13) 0.046(13) 0.044(13) 0.000 0.010(10) 0.000 C8 0.13(4) 0.04(3) 0.09(3) -0.02(2) 0.03(3) -0.01(2) C9 0.06(2) 0.06(3) 0.09(3) -0.006(18) -0.008(18) -0.011(17) C10 0.071(15) 0.060(15) 0.068(14) 0.000 0.018(10) 0.000 _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 C7 1.89(4) . ? Rh1 N1 2.15(3) 2_757 ? Rh1 N1 2.15(3) . ? Rh1 Cl1 2.316(9) . ? Rh1 Cl1 2.316(9) 2_757 ? Rh1 O1 2.37(2) . ? N1 N2 1.26(3) . ? N1 C1 1.41(4) . ? N2 C8 1.37(4) 2_757 ? C1 C2 1.31(4) . ? C1 C6 1.38(5) . ? C2 C3 1.39(4) . ? C2 H2 0.9300 . ? C3 C4 1.32(4) . ? C3 H3 0.9300 . ? C4 C5 1.33(4) . ? C4 H4 0.9300 . ? C5 C6 1.37(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.39(4) . ? C7 C8 1.39(4) 2_757 ? C8 C9 1.39(4) . ? C8 N2 1.37(4) 2_757 ? C9 C10 1.40(3) . ? C9 H9 0.9300 . ? C10 C9 1.40(3) 2_757 ? C10 H10 0.9300 . ? 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 C7 Rh1 N1 77.3(11) . 2_757 ? C7 Rh1 N1 77.3(11) . . ? N1 Rh1 N1 155(2) 2_757 . ? C7 Rh1 Cl1 92.82(18) . . ? N1 Rh1 Cl1 93.0(7) 2_757 . ? N1 Rh1 Cl1 88.2(7) . . ? C7 Rh1 Cl1 92.82(18) . 2_757 ? N1 Rh1 Cl1 88.2(7) 2_757 2_757 ? N1 Rh1 Cl1 93.0(7) . 2_757 ? Cl1 Rh1 Cl1 174.4(4) . 2_757 ? C7 Rh1 O1 180.000(10) . . ? N1 Rh1 O1 102.7(11) 2_757 . ? N1 Rh1 O1 102.7(11) . . ? Cl1 Rh1 O1 87.18(18) . . ? Cl1 Rh1 O1 87.18(18) 2_757 . ? N2 N1 C1 115(3) . . ? N2 N1 Rh1 115(2) . . ? C1 N1 Rh1 129(3) . . ? N1 N2 C8 112(3) . 2_757 ? C2 C1 C6 120(3) . . ? C2 C1 N1 122(4) . . ? C6 C1 N1 118(4) . . ? C1 C2 C3 120(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 121(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 121(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 119(3) . . ? C5 C6 H6 120.7 . . ? C1 C6 H6 120.7 . . ? C8 C7 C8 129(5) . 2_757 ? C8 C7 Rh1 116(2) . . ? C8 C7 Rh1 116(2) 2_757 . ? C9 C8 N2 126(3) . 2_757 ? C9 C8 C7 114(4) . . ? N2 C8 C7 119(3) 2_757 . ? C8 C9 C10 121(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C9 122(4) 2_757 . ? C9 C10 H10 119.2 2_757 . ? C9 C10 H10 119.2 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 17.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.679 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.226 # Attachment '- sb-su-6_c5.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 810564' #TrackingRef '- sb-su-6_c5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Cl2 N5 Rh' _chemical_formula_weight 500.18 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' _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 8.6950(9) _cell_length_b 9.7051(11) _cell_length_c 12.1143(15) _cell_angle_alpha 78.088(10) _cell_angle_beta 84.530(9) _cell_angle_gamma 83.077(9) _cell_volume 990.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6958 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 29.99 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 1.148 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number n/a _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 6958 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 29.99 _reflns_number_total 5524 _reflns_number_gt 4831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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. C52 was refined with ISOR constraints the residual electron density was located close to the metal atom. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+7.8354P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5524 _refine_ls_number_parameters 254 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1855 _refine_ls_wR_factor_gt 0.1817 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.176 _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 C12 C 0.3488(6) 0.3659(6) 0.0234(5) 0.0200(10) Uani 1 1 d . . . C13 C 0.3475(7) 0.4755(6) -0.0716(5) 0.0226(11) Uani 1 1 d . . . H13 H 0.4172 0.4692 -0.1340 0.027 Uiso 1 1 calc R . . C14 C 0.2391(7) 0.5956(6) -0.0715(5) 0.0246(11) Uani 1 1 d . . . H14 H 0.2383 0.6693 -0.1343 0.030 Uiso 1 1 calc R . . C15 C 0.1319(8) 0.6062(6) 0.0219(5) 0.0260(12) Uani 1 1 d . . . H15 H 0.0586 0.6846 0.0201 0.031 Uiso 1 1 calc R . . C16 C 0.1375(7) 0.4972(6) 0.1171(5) 0.0213(10) Uani 1 1 d . . . C31 C -0.0211(7) 0.3677(6) 0.3929(5) 0.0218(10) Uani 1 1 d . . . C32 C -0.1809(7) 0.4077(7) 0.3918(6) 0.0266(12) Uani 1 1 d . . . H32 H -0.2257 0.4449 0.3238 0.032 Uiso 1 1 calc R . . C33 C -0.2716(8) 0.3914(8) 0.4922(6) 0.0314(13) Uani 1 1 d . . . H33 H -0.3781 0.4177 0.4921 0.038 Uiso 1 1 calc R . . C34 C -0.2049(8) 0.3362(7) 0.5935(6) 0.0301(13) Uani 1 1 d . . . H34 H -0.2669 0.3254 0.6610 0.036 Uiso 1 1 calc R . . C35 C -0.0470(8) 0.2970(7) 0.5949(5) 0.0273(12) Uani 1 1 d . . . H35 H -0.0032 0.2600 0.6633 0.033 Uiso 1 1 calc R . . C36 C 0.0468(7) 0.3125(6) 0.4948(5) 0.0230(11) Uani 1 1 d . . . H36 H 0.1533 0.2864 0.4956 0.028 Uiso 1 1 calc R . . C41 C 0.5313(7) 0.0333(6) 0.1512(5) 0.0211(10) Uani 1 1 d . . . C42 C 0.4813(7) -0.0826(6) 0.2277(6) 0.0271(12) Uani 1 1 d . . . H42 H 0.3819 -0.0780 0.2636 0.033 Uiso 1 1 calc R . . C43 C 0.5826(8) -0.2063(7) 0.2501(6) 0.0299(13) Uani 1 1 d . . . H43 H 0.5498 -0.2854 0.3001 0.036 Uiso 1 1 calc R . . C44 C 0.7322(8) -0.2123(7) 0.1981(6) 0.0290(13) Uani 1 1 d . . . H44 H 0.8002 -0.2940 0.2155 0.035 Uiso 1 1 calc R . . C45 C 0.7802(7) -0.0963(7) 0.1200(6) 0.0288(12) Uani 1 1 d . . . H45 H 0.8792 -0.1012 0.0836 0.035 Uiso 1 1 calc R . . C46 C 0.6798(7) 0.0269(6) 0.0967(5) 0.0249(11) Uani 1 1 d . . . H46 H 0.7116 0.1049 0.0448 0.030 Uiso 1 1 calc R . . C52 C 0.2574(6) 0.0041(6) 0.4942(5) 0.0190(10) Uani 1 1 d U . . C53 C 0.2497(9) -0.0621(7) 0.6094(5) 0.0325(14) Uani 1 1 d . . . H53A H 0.2642 0.0051 0.6547 0.049 Uiso 1 1 calc R . . H53B H 0.3297 -0.1398 0.6216 0.049 Uiso 1 1 calc R . . H53C H 0.1500 -0.0966 0.6305 0.049 Uiso 1 1 calc R . . C11 C 0.2457(6) 0.3794(6) 0.1143(5) 0.0182(10) Uani 1 1 d . . . N17 N 0.4511(6) 0.2411(5) 0.0355(4) 0.0202(9) Uani 1 1 d . . . N18 N 0.4274(6) 0.1605(5) 0.1323(4) 0.0204(9) Uani 1 1 d . . . N19 N 0.0409(6) 0.4932(5) 0.2165(4) 0.0226(9) Uani 1 1 d . . . N20 N 0.0748(6) 0.3801(5) 0.2907(4) 0.0213(9) Uani 1 1 d . . . N51 N 0.2615(6) 0.0729(5) 0.4015(4) 0.0241(10) Uani 1 1 d . . . Cl1 Cl 0.43596(16) 0.34667(15) 0.31549(12) 0.0241(3) Uani 1 1 d . . . Cl2 Cl 0.07244(16) 0.11621(15) 0.17956(12) 0.0235(3) Uani 1 1 d . . . Rh1 Rh 0.25398(5) 0.23503(4) 0.24389(3) 0.01530(13) 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 C12 0.021(2) 0.022(2) 0.017(2) -0.0036(19) -0.0026(19) -0.0030(19) C13 0.024(3) 0.025(3) 0.019(3) -0.004(2) 0.001(2) -0.004(2) C14 0.031(3) 0.023(3) 0.018(3) 0.004(2) -0.004(2) -0.007(2) C15 0.034(3) 0.018(2) 0.027(3) -0.002(2) -0.011(2) -0.004(2) C16 0.023(3) 0.018(2) 0.023(3) -0.003(2) -0.002(2) -0.0016(19) C31 0.023(3) 0.020(2) 0.022(3) -0.007(2) 0.002(2) -0.001(2) C32 0.024(3) 0.025(3) 0.032(3) -0.009(2) -0.001(2) -0.002(2) C33 0.025(3) 0.038(3) 0.035(3) -0.015(3) 0.002(2) -0.005(3) C34 0.031(3) 0.035(3) 0.025(3) -0.010(3) 0.008(2) -0.008(3) C35 0.031(3) 0.028(3) 0.022(3) -0.005(2) -0.002(2) -0.002(2) C36 0.021(2) 0.022(3) 0.026(3) -0.007(2) 0.001(2) 0.000(2) C41 0.021(2) 0.021(2) 0.022(3) -0.008(2) -0.004(2) 0.0013(19) C42 0.028(3) 0.021(3) 0.031(3) -0.007(2) 0.002(2) 0.000(2) C43 0.036(3) 0.020(3) 0.033(3) -0.004(2) -0.003(3) 0.000(2) C44 0.030(3) 0.022(3) 0.035(3) -0.010(2) -0.008(3) 0.007(2) C45 0.021(3) 0.030(3) 0.034(3) -0.009(3) -0.001(2) 0.003(2) C46 0.022(3) 0.024(3) 0.028(3) -0.007(2) 0.004(2) -0.001(2) C52 0.0174(12) 0.0206(13) 0.0193(13) -0.0057(9) -0.0023(9) 0.0005(9) C53 0.047(4) 0.028(3) 0.019(3) 0.003(2) 0.003(3) -0.005(3) C11 0.016(2) 0.017(2) 0.023(3) -0.0043(19) -0.0071(19) 0.0011(18) N17 0.024(2) 0.020(2) 0.016(2) -0.0027(17) -0.0004(17) -0.0039(17) N18 0.020(2) 0.019(2) 0.020(2) -0.0017(17) 0.0029(17) -0.0012(17) N19 0.023(2) 0.021(2) 0.024(2) -0.0041(18) -0.0034(18) 0.0006(17) N20 0.025(2) 0.020(2) 0.018(2) -0.0056(17) -0.0063(18) 0.0055(17) N51 0.027(2) 0.020(2) 0.025(2) -0.0074(19) -0.0017(19) 0.0016(18) Cl1 0.0227(6) 0.0266(6) 0.0239(6) -0.0061(5) -0.0041(5) -0.0029(5) Cl2 0.0228(6) 0.0237(6) 0.0244(6) -0.0040(5) -0.0019(5) -0.0047(5) Rh1 0.01451(19) 0.0155(2) 0.0146(2) -0.00179(13) -0.00026(13) 0.00098(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C12 C11 1.370(8) . ? C12 C13 1.396(8) . ? C12 N17 1.404(7) . ? C13 C14 1.408(8) . ? C13 H13 0.9300 . ? C14 C15 1.408(9) . ? C14 H14 0.9300 . ? C15 C16 1.395(8) . ? C15 H15 0.9300 . ? C16 C11 1.394(7) . ? C16 N19 1.398(8) . ? C31 C32 1.397(8) . ? C31 C36 1.397(8) . ? C31 N20 1.417(7) . ? C32 C33 1.377(9) . ? C32 H32 0.9300 . ? C33 C34 1.385(10) . ? C33 H33 0.9300 . ? C34 C35 1.381(9) . ? C34 H34 0.9300 . ? C35 C36 1.387(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.387(8) . ? C41 C46 1.394(8) . ? C41 N18 1.430(7) . ? C42 C43 1.395(9) . ? C42 H42 0.9300 . ? C43 C44 1.390(9) . ? C43 H43 0.9300 . ? C44 C45 1.391(9) . ? C44 H44 0.9300 . ? C45 C46 1.388(8) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C52 N51 1.182(8) . ? C52 C53 1.409(8) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C11 Rh1 1.876(6) . ? N17 N18 1.283(6) . ? N18 Rh1 2.092(5) . ? N19 N20 1.291(7) . ? N20 Rh1 2.089(5) . ? N51 Rh1 2.210(5) . ? Cl1 Rh1 2.3438(14) . ? Cl2 Rh1 2.3394(14) . ? 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 C11 C12 C13 118.9(5) . . ? C11 C12 N17 115.9(5) . . ? C13 C12 N17 125.1(5) . . ? C12 C13 C14 119.0(5) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 118.9(6) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C11 C16 C15 118.5(5) . . ? C11 C16 N19 115.8(5) . . ? C15 C16 N19 125.7(5) . . ? C32 C31 C36 120.5(5) . . ? C32 C31 N20 120.8(5) . . ? C36 C31 N20 118.6(5) . . ? C33 C32 C31 119.4(6) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 120.2(6) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 120.5(6) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.3(6) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 119.0(5) . . ? C35 C36 H36 120.5 . . ? C31 C36 H36 120.5 . . ? C42 C41 C46 120.8(5) . . ? C42 C41 N18 118.0(5) . . ? C46 C41 N18 121.1(5) . . ? C41 C42 C43 119.0(6) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C44 C43 C42 120.5(6) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 120.1(6) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 119.8(6) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C41 119.8(6) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? N51 C52 C53 173.0(6) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C12 C11 C16 123.3(5) . . ? C12 C11 Rh1 118.6(4) . . ? C16 C11 Rh1 118.0(4) . . ? N18 N17 C12 111.5(5) . . ? N17 N18 C41 114.3(5) . . ? N17 N18 Rh1 117.0(4) . . ? C41 N18 Rh1 128.7(4) . . ? N20 N19 C16 111.8(5) . . ? N19 N20 C31 114.7(5) . . ? N19 N20 Rh1 117.0(4) . . ? C31 N20 Rh1 128.2(4) . . ? C52 N51 Rh1 169.3(4) . . ? C11 Rh1 N20 77.4(2) . . ? C11 Rh1 N18 76.9(2) . . ? N20 Rh1 N18 154.3(2) . . ? C11 Rh1 N51 177.2(2) . . ? N20 Rh1 N51 100.44(19) . . ? N18 Rh1 N51 105.24(18) . . ? C11 Rh1 Cl2 91.89(16) . . ? N20 Rh1 Cl2 89.87(14) . . ? N18 Rh1 Cl2 90.41(14) . . ? N51 Rh1 Cl2 89.79(14) . . ? C11 Rh1 Cl1 90.56(16) . . ? N20 Rh1 Cl1 90.55(14) . . ? N18 Rh1 Cl1 90.27(14) . . ? N51 Rh1 Cl1 87.75(14) . . ? Cl2 Rh1 Cl1 177.54(5) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 4.477 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.225 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END