# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Masahiro Ebihara' _publ_contact_author_email ebihara@gifu-u.ac.jp loop_ _publ_author_name 'Y. Fuma' 'O. Miyashita' 'T. Kawamura' 'M. Ebihara' data_[{Rh2(acam)4}3Br2].10H2O_(2.10H2O) _database_code_depnum_ccdc_archive 'CCDC 775018' #TrackingRef 'web_deposit_cif_file_0_MasahiroEbihara_1272351332.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 Br2 N12 O12 Rh6, 10(H2 O)' _chemical_formula_sum 'C24 H68 Br2 N12 O22 Rh6' _chemical_formula_weight 1654.11 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' Br Br -0.2901 2.4595 '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 trigonal _symmetry_space_group_name_H-M 'R -3 ' _symmetry_Int_Tables_number 148 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 13.1978(11) _cell_length_b 13.1978(11) _cell_length_c 25.081(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3783.4(6) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3468 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2436 _exptl_absorpt_coefficient_mu 3.585 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.780 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 10338 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1930 _reflns_number_gt 1742 _reflns_threshold_expression ' I>2\s(I)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+43.8669P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00017(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1930 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_restrained_S_all 1.242 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.11371(3) 0.22957(3) 0.322686(14) 0.01278(13) Uani 1 1 d . . . Br1 Br 0.0000 0.0000 0.29815(3) 0.01336(19) Uani 1 3 d S . . N1 N 0.2504(4) 0.2245(4) 0.35310(16) 0.0199(9) Uani 1 1 d . . . H1 H 0.2477 0.1565 0.3539 0.024 Uiso 1 1 calc R . . O1 O 0.3535(3) 0.4175(3) 0.37453(14) 0.0210(8) Uani 1 1 d . . . O2A O 0.2967(4) 0.4662(3) 0.27106(14) 0.0254(9) Uani 0.67 1 d P . 1 N2A N 0.1944(4) 0.2715(4) 0.25120(15) 0.0238(10) Uani 0.67 1 d P . 1 H2A H 0.1777 0.2158 0.2277 0.029 Uiso 0.67 1 calc PR . 1 O2B O 0.1944(4) 0.2715(4) 0.25120(15) 0.0238(10) Uani 0.33 1 d P . 2 N2B N 0.2967(4) 0.4662(3) 0.27106(14) 0.0254(9) Uani 0.33 1 d P . 2 H2B H 0.3479 0.5378 0.2610 0.030 Uiso 0.33 1 calc PR . 2 C1 C 0.3432(4) 0.3150(5) 0.37175(18) 0.0182(11) Uani 1 1 d . . . C2 C 0.4456(5) 0.3059(5) 0.3921(2) 0.0246(12) Uani 1 1 d . . . H4 H 0.4663 0.3394 0.4280 0.037 Uiso 1 1 calc R . . H5 H 0.5126 0.3488 0.3682 0.037 Uiso 1 1 calc R . . H3 H 0.4247 0.2234 0.3933 0.037 Uiso 1 1 calc R . . C3 C 0.2701(5) 0.3783(5) 0.2393(2) 0.0245(12) Uani 1 1 d . . . C4 C 0.3334(6) 0.4044(6) 0.1868(2) 0.0438(18) Uani 1 1 d . . . H7 H 0.3358 0.4730 0.1706 0.066 Uiso 1 1 calc R . . H8 H 0.2923 0.3369 0.1630 0.066 Uiso 1 1 calc R . . H6 H 0.4134 0.4202 0.1927 0.066 Uiso 1 1 calc R . . O4 O 0.2238(4) 0.0983(4) 0.19125(17) 0.0427(12) Uani 1 1 d . . . O5 O 0.0000 0.0000 0.1459(3) 0.0409(19) Uani 1 3 d S . . O3 O 0.0000 0.0000 0.4465(3) 0.047(2) Uani 1 3 d S . . 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 0.0125(2) 0.0095(2) 0.01517(19) -0.00068(14) -0.00091(14) 0.00458(17) Br1 0.0109(3) 0.0109(3) 0.0183(4) 0.000 0.000 0.00544(14) N1 0.019(2) 0.014(2) 0.029(2) -0.0011(18) -0.0055(18) 0.010(2) O1 0.020(2) 0.0127(19) 0.032(2) -0.0027(15) -0.0076(15) 0.0097(17) O2A 0.031(2) 0.017(2) 0.023(2) 0.0012(16) 0.0053(17) 0.0072(19) N2A 0.031(3) 0.017(2) 0.022(2) -0.0003(16) 0.0059(18) 0.011(2) O2B 0.031(3) 0.017(2) 0.022(2) -0.0003(16) 0.0059(18) 0.011(2) N2B 0.031(2) 0.017(2) 0.023(2) 0.0012(16) 0.0053(17) 0.0072(19) C1 0.017(3) 0.021(3) 0.017(2) 0.0020(19) 0.0029(19) 0.009(2) C2 0.021(3) 0.024(3) 0.032(3) -0.003(2) -0.005(2) 0.013(3) C3 0.027(3) 0.024(3) 0.021(3) 0.002(2) 0.001(2) 0.011(3) C4 0.054(5) 0.037(4) 0.029(3) 0.002(3) 0.018(3) 0.015(4) O4 0.039(3) 0.053(3) 0.048(3) 0.024(2) 0.017(2) 0.032(3) O5 0.044(3) 0.044(3) 0.035(4) 0.000 0.000 0.0219(16) O3 0.053(3) 0.053(3) 0.033(4) 0.000 0.000 0.0267(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 N1 1.990(4) . ? Rh1 N2A 2.016(4) . ? Rh1 N2B 2.034(4) 16 ? Rh1 O2A 2.034(4) 16 ? Rh1 O1 2.057(3) 16 ? Rh1 Rh1 2.4315(8) 16 ? Rh1 Br1 2.6952(5) . ? N1 C1 1.297(6) . ? N1 H1 0.8800 . ? O1 C1 1.292(6) . ? O2A C3 1.303(7) . ? N2A C3 1.291(7) . ? N2A H2A 0.8800 . ? C1 C2 1.506(7) . ? C2 H4 0.9800 . ? C2 H5 0.9800 . ? C2 H3 0.9800 . ? C3 C4 1.503(7) . ? C4 H7 0.9800 . ? C4 H8 0.9800 . ? C4 H6 0.9800 . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O4 O1 2.907(5) 18_545 ? O4 O5 2.805(5) . ? O4 O4 2.815(9) 13 ? O3 O3 2.684(15) 10_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2A 89.23(17) . . ? N1 Rh1 N2B 91.46(17) . 16 ? N2A Rh1 N2B 175.63(16) . 16 ? N1 Rh1 O2A 91.46(17) . 16 ? N2A Rh1 O2A 175.63(16) . 16 ? N2B Rh1 O2A 0.0(4) 16 16 ? N1 Rh1 O1 175.38(16) . 16 ? N2A Rh1 O1 90.20(16) . 16 ? N2B Rh1 O1 88.76(16) 16 16 ? O2A Rh1 O1 88.76(16) 16 16 ? N1 Rh1 Rh1 86.18(13) . 16 ? N2A Rh1 Rh1 87.66(12) . 16 ? N2B Rh1 Rh1 88.08(11) 16 16 ? O2A Rh1 Rh1 88.08(11) 16 16 ? O1 Rh1 Rh1 89.22(10) 16 16 ? N1 Rh1 Br1 93.12(12) . . ? N2A Rh1 Br1 91.49(12) . . ? N2B Rh1 Br1 92.78(11) 16 . ? O2A Rh1 Br1 92.78(11) 16 . ? O1 Rh1 Br1 91.48(10) 16 . ? Rh1 Rh1 Br1 178.91(3) 16 . ? Rh1 Br1 Rh1 114.948(13) 2 . ? Rh1 Br1 Rh1 114.947(13) 2 3 ? Rh1 Br1 Rh1 114.948(13) . 3 ? C1 N1 Rh1 124.2(4) . . ? C1 N1 H1 117.9 . . ? Rh1 N1 H1 117.9 . . ? C1 O1 Rh1 117.6(3) . 16 ? C3 O2A Rh1 119.7(3) . 16 ? C3 N2A Rh1 121.3(4) . . ? C3 N2A H2A 119.3 . . ? Rh1 N2A H2A 119.3 . . ? O1 C1 N1 122.7(5) . . ? O1 C1 C2 115.9(4) . . ? N1 C1 C2 121.4(5) . . ? C1 C2 H4 109.5 . . ? C1 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? C1 C2 H3 109.5 . . ? H4 C2 H3 109.5 . . ? H5 C2 H3 109.5 . . ? N2A C3 O2A 123.2(5) . . ? N2A C3 C4 119.4(5) . . ? O2A C3 C4 117.4(5) . . ? C3 C4 H7 109.5 . . ? C3 C4 H8 109.5 . . ? H7 C4 H8 109.5 . . ? C3 C4 H6 109.5 . . ? H7 C4 H6 109.5 . . ? H8 C4 H6 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 Br1 Rh1 135.99(12) . . . 2 ? N2A Rh1 Br1 Rh1 -134.69(13) . . . 2 ? N2B Rh1 Br1 Rh1 44.38(12) 16 . . 2 ? O2A Rh1 Br1 Rh1 44.38(12) 16 . . 2 ? O1 Rh1 Br1 Rh1 -44.45(11) 16 . . 2 ? N1 Rh1 Br1 Rh1 -0.85(12) . . . 3 ? N2A Rh1 Br1 Rh1 88.46(13) . . . 3 ? N2B Rh1 Br1 Rh1 -92.46(12) 16 . . 3 ? O2A Rh1 Br1 Rh1 -92.46(12) 16 . . 3 ? O1 Rh1 Br1 Rh1 178.71(10) 16 . . 3 ? N2A Rh1 N1 C1 86.5(4) . . . . ? N2B Rh1 N1 C1 -89.2(4) 16 . . . ? O2A Rh1 N1 C1 -89.2(4) 16 . . . ? Rh1 Rh1 N1 C1 -1.2(4) 16 . . . ? Br1 Rh1 N1 C1 178.0(4) . . . . ? N1 Rh1 N2A C3 -84.2(4) . . . . ? O1 Rh1 N2A C3 91.2(4) 16 . . . ? Rh1 Rh1 N2A C3 2.0(4) 16 . . . ? Br1 Rh1 N2A C3 -177.3(4) . . . . ? Rh1 O1 C1 N1 -3.5(6) 16 . . . ? Rh1 O1 C1 C2 177.1(3) 16 . . . ? Rh1 N1 C1 O1 3.2(7) . . . . ? Rh1 N1 C1 C2 -177.4(3) . . . . ? Rh1 N2A C3 O2A -2.4(8) . . . . ? Rh1 N2A C3 C4 176.3(4) . . . . ? Rh1 O2A C3 N2A 1.2(7) 16 . . . ? Rh1 O2A C3 C4 -177.5(4) 16 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2A 0.88 2.45 3.222(6) 147.0 18_545 N1 H1 O1 0.88 2.50 3.217(6) 139.3 18_545 N2A H2A O4 0.88 2.13 2.919(6) 148.3 . N2B H2B O3 0.88 2.08 2.754(5) 133.3 18 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.712 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.136 #===END data_[{Rh2(acam)4}3I2].10H2O_(3.10H2O) _database_code_depnum_ccdc_archive 'CCDC 775019' #TrackingRef 'web_deposit_cif_file_0_MasahiroEbihara_1272351332.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 I2 N12 O12 Rh6, 10(H2 O)' _chemical_formula_sum 'C24 H68 I2 N12 O22 Rh6' _chemical_formula_weight 1748.16 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' I I -0.4742 1.8119 '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 trigonal _symmetry_space_group_name_H-M 'R -3 ' _symmetry_Int_Tables_number 148 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 13.4834(13) _cell_length_b 13.4834(13) _cell_length_c 24.801(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3904.9(8) _cell_formula_units_Z 3 _cell_measurement_temperature 118(2) _cell_measurement_reflns_used 2629 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 3.124 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_max 0.8562 _exptl_absorpt_correction_T_min 0.7787 _exptl_special_details ; ? ; _diffrn_ambient_temperature 118(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 10695 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1997 _reflns_number_gt 1583 _reflns_threshold_expression ' I>2\s(I)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+37.4995P] 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 1997 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _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 0.11494(5) 0.23189(4) 0.321708(19) 0.01669(15) Uani 1 1 d . . . I1 I 0.0000 0.0000 0.29271(3) 0.01591(19) Uani 1 3 d S . . N1 N 0.2483(5) 0.2263(5) 0.3529(2) 0.0239(13) Uani 1 1 d . . . H1 H 0.2459 0.1599 0.3533 0.029 Uiso 1 1 calc R . . O1 O 0.3489(4) 0.4141(4) 0.37557(18) 0.0250(11) Uani 1 1 d . . . O2A O 0.2975(5) 0.4662(4) 0.27196(19) 0.0269(12) Uani 0.67 1 d P . 1 N2A N 0.1966(5) 0.2750(5) 0.2502(2) 0.0248(13) Uani 0.67 1 d P . 1 H2A H 0.1813 0.2217 0.2258 0.030 Uiso 0.67 1 calc PR . 1 O2B O 0.1966(5) 0.2750(5) 0.2502(2) 0.0248(13) Uani 0.33 1 d P . 2 N2B N 0.2975(5) 0.4662(4) 0.27196(19) 0.0269(12) Uani 0.33 1 d P . 2 H2B H 0.3482 0.5365 0.2624 0.032 Uiso 0.33 1 calc PR . 2 C1 C 0.3385(6) 0.3145(6) 0.3726(2) 0.0169(14) Uani 1 1 d . . . C2 C 0.4398(6) 0.3041(7) 0.3917(3) 0.0302(17) Uani 1 1 d . . . H4 H 0.5032 0.3429 0.3661 0.045 Uiso 1 1 calc R . . H5 H 0.4175 0.2230 0.3940 0.045 Uiso 1 1 calc R . . H6 H 0.4641 0.3396 0.4273 0.045 Uiso 1 1 calc R . . C3 C 0.2720(7) 0.3813(7) 0.2398(3) 0.0303(18) Uani 1 1 d . . . C4 C 0.3371(8) 0.4081(7) 0.1869(3) 0.043(2) Uani 1 1 d . . . H7 H 0.3372 0.4734 0.1696 0.064 Uiso 1 1 calc R . . H8 H 0.3001 0.3412 0.1631 0.064 Uiso 1 1 calc R . . H9 H 0.4162 0.4269 0.1939 0.064 Uiso 1 1 calc R . . O4 O 0.2251(5) 0.1019(5) 0.1897(2) 0.0506(17) Uani 1 1 d . . . O5 O 0.0000 0.0000 0.1419(4) 0.059(3) Uani 1 3 d S . . O3 O 0.0000 0.0000 0.4460(4) 0.048(3) Uani 1 3 d S . . 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 0.0160(3) 0.0139(3) 0.0192(3) -0.0001(2) 0.0000(2) 0.0068(2) I1 0.0137(3) 0.0137(3) 0.0204(4) 0.000 0.000 0.00684(13) N1 0.026(3) 0.018(3) 0.032(3) 0.000(3) -0.007(3) 0.015(3) O1 0.023(3) 0.017(3) 0.036(3) -0.002(2) -0.006(2) 0.011(2) O2A 0.030(3) 0.020(3) 0.027(3) -0.001(2) 0.006(2) 0.010(3) N2A 0.030(3) 0.019(3) 0.024(3) 0.003(2) 0.007(2) 0.011(3) O2B 0.030(3) 0.019(3) 0.024(3) 0.003(2) 0.007(2) 0.011(3) N2B 0.030(3) 0.020(3) 0.027(3) -0.001(2) 0.006(2) 0.010(3) C1 0.018(4) 0.018(4) 0.012(3) -0.003(2) -0.001(2) 0.007(3) C2 0.025(4) 0.028(4) 0.040(4) -0.001(3) -0.007(3) 0.015(4) C3 0.037(5) 0.026(4) 0.027(4) 0.000(3) 0.002(3) 0.015(4) C4 0.051(6) 0.034(5) 0.033(4) 0.000(4) 0.013(4) 0.014(4) O4 0.045(4) 0.054(4) 0.066(4) 0.025(3) 0.026(3) 0.034(4) O5 0.070(5) 0.070(5) 0.037(6) 0.000 0.000 0.035(3) O3 0.055(4) 0.055(4) 0.035(5) 0.000 0.000 0.027(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 N1 1.994(5) . ? Rh1 N2A 2.014(5) . ? Rh1 N2B 2.035(5) 16 ? Rh1 O2A 2.035(5) 16 ? Rh1 O1 2.060(5) 16 ? Rh1 Rh1 2.4384(11) 16 ? Rh1 I1 2.8017(6) . ? N1 C1 1.298(8) . ? N1 H1 0.8800 . ? O1 C1 1.281(8) . ? O2A C3 1.293(8) . ? N2A C3 1.303(9) . ? N2A H2A 0.8800 . ? C1 C2 1.516(9) . ? C2 H4 0.9800 . ? C2 H5 0.9800 . ? C2 H6 0.9800 . ? C3 C4 1.519(9) . ? C4 H7 0.9800 . ? C4 H8 0.9800 . ? C4 H9 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2A 88.8(2) . . ? N1 Rh1 N2B 92.0(2) . 16 ? N2A Rh1 N2B 175.9(2) . 16 ? N1 Rh1 O2A 92.0(2) . 16 ? N2A Rh1 O2A 175.9(2) . 16 ? N2B Rh1 O2A 0.0(6) 16 16 ? N1 Rh1 O1 175.0(2) . 16 ? N2A Rh1 O1 91.0(2) . 16 ? N2B Rh1 O1 87.8(2) 16 16 ? O2A Rh1 O1 87.8(2) 16 16 ? N1 Rh1 Rh1 85.98(17) . 16 ? N2A Rh1 Rh1 87.77(16) . 16 ? N2B Rh1 Rh1 88.26(15) 16 16 ? O2A Rh1 Rh1 88.26(15) 16 16 ? O1 Rh1 Rh1 89.07(14) 16 16 ? N1 Rh1 I1 93.64(17) . . ? N2A Rh1 I1 90.76(16) . . ? N2B Rh1 I1 93.21(15) 16 . ? O2A Rh1 I1 93.21(15) 16 . ? O1 Rh1 I1 91.32(13) 16 . ? Rh1 Rh1 I1 178.49(4) 16 . ? Rh1 I1 Rh1 113.649(14) 2 3 ? Rh1 I1 Rh1 113.650(14) 2 . ? Rh1 I1 Rh1 113.649(14) 3 . ? C1 N1 Rh1 124.1(5) . . ? C1 N1 H1 117.9 . . ? Rh1 N1 H1 117.9 . . ? C1 O1 Rh1 117.9(4) . 16 ? C3 O2A Rh1 119.0(5) . 16 ? C3 N2A Rh1 120.3(5) . . ? C3 N2A H2A 119.8 . . ? Rh1 N2A H2A 119.8 . . ? O1 C1 N1 122.9(6) . . ? O1 C1 C2 116.6(6) . . ? N1 C1 C2 120.5(6) . . ? C1 C2 H4 109.5 . . ? C1 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? C1 C2 H6 109.5 . . ? H4 C2 H6 109.5 . . ? H5 C2 H6 109.5 . . ? O2A C3 N2A 124.6(7) . . ? O2A C3 C4 117.1(7) . . ? N2A C3 C4 118.2(7) . . ? C3 C4 H7 109.5 . . ? C3 C4 H8 109.5 . . ? H7 C4 H8 109.5 . . ? C3 C4 H9 109.5 . . ? H7 C4 H9 109.5 . . ? H8 C4 H9 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 I1 Rh1 133.36(16) . . . 2 ? N2A Rh1 I1 Rh1 -137.78(16) . . . 2 ? N2B Rh1 I1 Rh1 41.12(15) 16 . . 2 ? O2A Rh1 I1 Rh1 41.12(15) 16 . . 2 ? O1 Rh1 I1 Rh1 -46.78(13) 16 . . 2 ? N1 Rh1 I1 Rh1 1.31(16) . . . 3 ? N2A Rh1 I1 Rh1 90.16(16) . . . 3 ? N2B Rh1 I1 Rh1 -90.93(15) 16 . . 3 ? O2A Rh1 I1 Rh1 -90.93(15) 16 . . 3 ? O1 Rh1 I1 Rh1 -178.83(13) 16 . . 3 ? N2A Rh1 N1 C1 86.7(5) . . . . ? N2B Rh1 N1 C1 -89.3(5) 16 . . . ? O2A Rh1 N1 C1 -89.3(5) 16 . . . ? Rh1 Rh1 N1 C1 -1.2(5) 16 . . . ? I1 Rh1 N1 C1 177.4(5) . . . . ? N1 Rh1 N2A C3 -83.8(6) . . . . ? O1 Rh1 N2A C3 91.3(6) 16 . . . ? Rh1 Rh1 N2A C3 2.2(6) 16 . . . ? I1 Rh1 N2A C3 -177.4(6) . . . . ? Rh1 O1 C1 N1 -2.3(8) 16 . . . ? Rh1 O1 C1 C2 175.6(4) 16 . . . ? Rh1 N1 C1 O1 2.5(9) . . . . ? Rh1 N1 C1 C2 -175.4(5) . . . . ? Rh1 O2A C3 N2A 1.3(10) 16 . . . ? Rh1 O2A C3 C4 -177.2(5) 16 . . . ? Rh1 N2A C3 O2A -2.7(11) . . . . ? Rh1 N2A C3 C4 175.8(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2A 0.88 2.52 3.295(8) 148.0 18_545 N1 H1 O1 0.88 2.62 3.354(7) 142.2 18_545 N2A H2A O4 0.88 2.17 2.957(8) 148.2 . N2B H2B O3 0.88 2.13 2.802(7) 132.5 18 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O4 O1 2.948(8) 18_545 ? O4 O4 2.789(11) 13 ? O4 O5 2.887(7) . ? O3 O3 2.679(18) 10_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.310 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.186 #===END data_[{Rh2(pram)4}3Cl2].6H2O_(4.6H2O) _database_code_depnum_ccdc_archive 'CCDC 775020' #TrackingRef 'web_deposit_cif_file_0_MasahiroEbihara_1272351332.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H72 Cl2 N12 O12 Rh6, 6(H2 O)' _chemical_formula_sum 'C36 H84 Cl2 N12 O18 Rh6' _chemical_formula_weight 1661.52 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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.474(3) _cell_length_b 12.670(4) _cell_length_c 12.966(3) _cell_angle_alpha 117.033(9) _cell_angle_beta 92.940(10) _cell_angle_gamma 114.824(9) _cell_volume 1453.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 118(2) _cell_measurement_reflns_used 4658 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Platelet _exptl_crystal_colour Brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 1.828 _exptl_absorpt_correction_T_max 0.9511 _exptl_absorpt_correction_T_min 0.6749 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 118(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 12023 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6607 _reflns_number_gt 5600 _reflns_threshold_expression ' I>2\s(I)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6607 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.04396(2) 0.06252(2) 0.44981(2) 0.00721(6) Uani 1 1 d . . . Rh2 Rh 0.04136(2) 0.06004(2) 0.10978(2) 0.00766(6) Uani 1 1 d . . . Rh3 Rh 0.38425(2) 0.40648(2) 0.45113(2) 0.00698(6) Uani 1 1 d . . . Cl1 Cl 0.13655(7) 0.19442(7) 0.34266(6) 0.00858(15) Uani 1 1 d . . . N1 N -0.0834(3) -0.1085(3) 0.2976(2) 0.0110(6) Uani 1 1 d . . . H1 H -0.0881 -0.1075 0.2301 0.013 Uiso 1 1 calc R . . O1 O -0.1656(2) -0.2315(2) 0.38639(19) 0.0122(5) Uani 1 1 d . . . N2 N 0.1791(3) 0.0017(3) 0.4344(2) 0.0116(6) Uani 1 1 d . . . H2 H 0.2425 0.0324 0.4035 0.014 Uiso 1 1 calc R . . O2 O 0.0972(2) -0.1207(2) 0.52435(19) 0.0128(5) Uani 1 1 d . . . N3 N 0.2214(3) 0.1520(2) 0.0951(2) 0.0100(6) Uani 1 1 d . . . H3 H 0.2902 0.2094 0.1617 0.012 Uiso 1 1 calc R . . O3 O 0.1491(2) 0.0483(2) -0.10966(19) 0.0112(5) Uani 1 1 d . . . N4 N 0.0024(3) 0.1994(3) 0.1121(2) 0.0108(6) Uani 1 1 d . C . H4 H 0.0188 0.2701 0.1829 0.013 Uiso 1 1 calc R . . O4 O -0.0727(2) 0.0932(2) -0.09348(19) 0.0152(5) Uani 1 1 d . . . N5 N 0.3352(3) 0.5311(3) 0.5802(2) 0.0100(5) Uani 1 1 d . . . H5 H 0.2503 0.4992 0.5790 0.012 Uiso 1 1 calc R . . O5 O 0.5501(2) 0.7065(2) 0.67829(19) 0.0109(5) Uani 1 1 d . . . N6 N 0.4292(3) 0.3480(3) 0.5596(2) 0.0105(6) Uani 1 1 d . . . H6 H 0.3651 0.2739 0.5534 0.013 Uiso 1 1 calc R . . O6 O 0.6471(2) 0.5189(2) 0.65515(19) 0.0110(5) Uani 1 1 d . . . C1 C -0.1609(3) -0.2226(3) 0.2909(3) 0.0117(7) Uani 1 1 d . A . C2 C -0.2501(4) -0.3518(3) 0.1722(3) 0.0179(8) Uani 1 1 d . . . H7B H -0.3382 -0.3574 0.1547 0.021 Uiso 0.41(4) 1 calc PR A 2 H8B H -0.2100 -0.3461 0.1078 0.021 Uiso 0.41(4) 1 calc PR A 2 H7A H -0.2264 -0.3393 0.1047 0.021 Uiso 0.59(4) 1 calc PR A 1 H8A H -0.3451 -0.3746 0.1647 0.021 Uiso 0.59(4) 1 calc PR A 1 C3A C -0.2325(17) -0.4724(8) 0.1646(7) 0.025(2) Uiso 0.59(4) 1 d P A 1 H9A H -0.2936 -0.5576 0.0881 0.038 Uiso 0.59(4) 1 calc PR A 1 H10A H -0.2536 -0.4827 0.2329 0.038 Uiso 0.59(4) 1 calc PR A 1 H11A H -0.1394 -0.4514 0.1680 0.038 Uiso 0.59(4) 1 calc PR A 1 C3B C -0.2737(18) -0.4776(9) 0.1646(8) 0.009(3) Uiso 0.41(4) 1 d P A 2 H9B H -0.3175 -0.4873 0.2252 0.013 Uiso 0.41(4) 1 calc PR A 2 H10B H -0.1876 -0.4747 0.1802 0.013 Uiso 0.41(4) 1 calc PR A 2 H11B H -0.3319 -0.5556 0.0833 0.013 Uiso 0.41(4) 1 calc PR A 2 C4 C 0.1790(3) -0.0816(3) 0.4676(3) 0.0125(7) Uani 1 1 d . . . C5 C 0.2725(4) -0.1379(4) 0.4402(3) 0.0174(7) Uani 1 1 d . . . H12 H 0.3284 -0.1020 0.3958 0.021 Uiso 1 1 calc R . . H13 H 0.2191 -0.2386 0.3868 0.021 Uiso 1 1 calc R . . C6 C 0.3641(4) -0.1005(4) 0.5549(3) 0.0279(9) Uani 1 1 d . . . H14 H 0.3091 -0.1341 0.6001 0.042 Uiso 1 1 calc R . . H15 H 0.4212 -0.0010 0.6057 0.042 Uiso 1 1 calc R . . H16 H 0.4209 -0.1425 0.5328 0.042 Uiso 1 1 calc R . . C7 C 0.2443(3) 0.1324(3) -0.0079(3) 0.0105(7) Uani 1 1 d . B . C8 C 0.3830(3) 0.2062(3) -0.0140(3) 0.0148(7) Uani 1 1 d . . . H17A H 0.4463 0.2732 0.0692 0.018 Uiso 0.74(3) 1 calc PR B 1 H18A H 0.3831 0.2568 -0.0540 0.018 Uiso 0.74(3) 1 calc PR B 1 H17B H 0.3890 0.2804 -0.0253 0.018 Uiso 0.26(3) 1 calc PR B 2 H18B H 0.4475 0.2502 0.0658 0.018 Uiso 0.26(3) 1 calc PR B 2 C9A C 0.4296(6) 0.1026(7) -0.0865(6) 0.0201(16) Uiso 0.74(3) 1 d P B 1 H19A H 0.5203 0.1516 -0.0901 0.030 Uiso 0.74(3) 1 calc PR B 1 H20A H 0.3674 0.0371 -0.1690 0.030 Uiso 0.74(3) 1 calc PR B 1 H21A H 0.4305 0.0536 -0.0461 0.030 Uiso 0.74(3) 1 calc PR B 1 C9B C 0.4275(16) 0.129(2) -0.1056(16) 0.019(5) Uiso 0.26(3) 1 d P B 2 H19B H 0.3607 0.0772 -0.1850 0.028 Uiso 0.26(3) 1 calc PR B 2 H20B H 0.4384 0.0659 -0.0878 0.028 Uiso 0.26(3) 1 calc PR B 2 H21B H 0.5139 0.1915 -0.1066 0.028 Uiso 0.26(3) 1 calc PR B 2 C10 C -0.0463(3) 0.1919(3) 0.0142(3) 0.0143(7) Uani 1 1 d . . . C11A C -0.0939(9) 0.2895(7) 0.0220(5) 0.0145(15) Uiso 0.621(16) 1 d P C 1 H22A H -0.0442 0.3759 0.1017 0.017 Uiso 0.621(16) 1 calc PR C 1 H23A H -0.1908 0.2490 0.0159 0.017 Uiso 0.621(16) 1 calc PR C 1 C12A C -0.0721(9) 0.3204(7) -0.0806(5) 0.0220(18) Uiso 0.621(16) 1 d P C 1 H24A H -0.1240 0.2354 -0.1596 0.033 Uiso 0.621(16) 1 calc PR C 1 H25A H 0.0237 0.3603 -0.0748 0.033 Uiso 0.621(16) 1 calc PR C 1 H26A H -0.1021 0.3851 -0.0720 0.033 Uiso 0.621(16) 1 calc PR C 1 C11B C -0.0399(14) 0.3228(11) 0.0280(8) 0.012(2) Uiso 0.379(16) 1 d P C 2 H22B H -0.0626 0.3685 0.1025 0.015 Uiso 0.379(16) 1 calc PR C 2 H23B H 0.0532 0.3866 0.0377 0.015 Uiso 0.379(16) 1 calc PR C 2 C12B C -0.1337(17) 0.2937(13) -0.0780(10) 0.033(3) Uiso 0.379(16) 1 d P C 2 H24B H -0.2259 0.2287 -0.0896 0.049 Uiso 0.379(16) 1 calc PR C 2 H25B H -0.1077 0.2547 -0.1512 0.049 Uiso 0.379(16) 1 calc PR C 2 H26B H -0.1289 0.3789 -0.0627 0.049 Uiso 0.379(16) 1 calc PR C 2 C13 C 0.4210(3) 0.6548(3) 0.6644(3) 0.0095(6) Uani 1 1 d . . . C14 C 0.3827(3) 0.7517(3) 0.7551(3) 0.0128(7) Uani 1 1 d . . . H27 H 0.4318 0.8405 0.7604 0.015 Uiso 1 1 calc R . . H28 H 0.4153 0.7672 0.8356 0.015 Uiso 1 1 calc R . . C15 C 0.2344(3) 0.7090(3) 0.7308(3) 0.0195(8) Uani 1 1 d . . . H29 H 0.1852 0.6269 0.7346 0.029 Uiso 1 1 calc R . . H30 H 0.1989 0.6894 0.6500 0.029 Uiso 1 1 calc R . . H31 H 0.2234 0.7830 0.7920 0.029 Uiso 1 1 calc R . . C16 C 0.5446(3) 0.4099(3) 0.6381(3) 0.0097(6) Uani 1 1 d . . . C17 C 0.5688(3) 0.3552(3) 0.7144(3) 0.0149(7) Uani 1 1 d . . . H32 H 0.4811 0.2857 0.7083 0.018 Uiso 1 1 calc R . . H33 H 0.6215 0.3094 0.6811 0.018 Uiso 1 1 calc R . . C18 C 0.6432(4) 0.4650(4) 0.8467(3) 0.0287(9) Uani 1 1 d . . . H34 H 0.5869 0.5032 0.8830 0.043 Uiso 1 1 calc R . . H35 H 0.7272 0.5376 0.8532 0.043 Uiso 1 1 calc R . . H36 H 0.6636 0.4252 0.8897 0.043 Uiso 1 1 calc R . . O7 O 0.3272(3) 0.0245(3) 0.2646(2) 0.0185(5) Uani 1 1 d . . . H37 H 0.255(4) -0.014(4) 0.212(4) 0.028 Uiso 1 1 d . . . H38 H 0.363(4) 0.101(4) 0.283(4) 0.028 Uiso 1 1 d . . . O8 O 0.0997(3) 0.4585(3) 0.3491(2) 0.0179(6) Uani 1 1 d . . . H39 H 0.079(4) 0.436(4) 0.388(4) 0.027 Uiso 1 1 d . . . H40 H 0.182(4) 0.482(4) 0.357(3) 0.027 Uiso 1 1 d . . . O9 O 0.0240(3) 0.3898(3) 0.5231(2) 0.0206(6) Uani 1 1 d . . . H41 H -0.014(4) 0.305(4) 0.503(4) 0.031 Uiso 1 1 d . . . H42 H -0.010(4) 0.420(4) 0.564(4) 0.031 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.00740(13) 0.00733(12) 0.00676(12) 0.00417(10) 0.00303(10) 0.00293(10) Rh2 0.00816(13) 0.00763(12) 0.00536(12) 0.00313(11) 0.00128(10) 0.00288(10) Rh3 0.00514(13) 0.00730(12) 0.00635(12) 0.00292(11) 0.00161(10) 0.00213(10) Cl1 0.0080(4) 0.0086(3) 0.0063(3) 0.0038(3) 0.0019(3) 0.0019(3) N1 0.0131(15) 0.0110(13) 0.0078(13) 0.0065(12) 0.0022(11) 0.0035(12) O1 0.0139(13) 0.0113(11) 0.0098(11) 0.0067(10) 0.0037(10) 0.0037(10) N2 0.0138(15) 0.0142(14) 0.0133(14) 0.0102(13) 0.0071(12) 0.0085(12) O2 0.0132(13) 0.0152(12) 0.0168(12) 0.0111(11) 0.0084(10) 0.0091(10) N3 0.0079(14) 0.0089(13) 0.0064(13) 0.0019(12) -0.0016(11) 0.0014(11) O3 0.0113(12) 0.0130(11) 0.0070(11) 0.0048(10) 0.0022(10) 0.0048(10) N4 0.0150(15) 0.0085(13) 0.0084(13) 0.0033(12) 0.0028(12) 0.0067(12) O4 0.0215(14) 0.0155(12) 0.0089(11) 0.0054(11) 0.0023(10) 0.0110(11) N5 0.0062(14) 0.0105(13) 0.0098(14) 0.0037(12) 0.0039(11) 0.0030(11) O5 0.0085(12) 0.0095(11) 0.0104(11) 0.0030(10) 0.0031(9) 0.0035(9) N6 0.0083(14) 0.0096(13) 0.0116(14) 0.0067(12) 0.0023(12) 0.0017(11) O6 0.0087(12) 0.0123(11) 0.0107(11) 0.0065(10) 0.0009(9) 0.0039(10) C1 0.0121(18) 0.0123(16) 0.0080(16) 0.0038(14) 0.0015(14) 0.0057(14) C2 0.022(2) 0.0136(17) 0.0117(17) 0.0072(16) 0.0037(15) 0.0032(15) C4 0.0117(18) 0.0154(17) 0.0120(17) 0.0075(15) 0.0053(14) 0.0075(14) C5 0.018(2) 0.0222(19) 0.0184(18) 0.0124(17) 0.0102(16) 0.0131(16) C6 0.025(2) 0.047(3) 0.025(2) 0.020(2) 0.0107(18) 0.027(2) C7 0.0100(17) 0.0121(16) 0.0105(16) 0.0064(14) 0.0011(14) 0.0060(14) C8 0.0106(18) 0.0173(17) 0.0145(17) 0.0089(16) 0.0039(14) 0.0048(14) C10 0.0180(19) 0.0116(16) 0.0129(17) 0.0055(15) 0.0048(15) 0.0080(15) C13 0.0092(17) 0.0119(16) 0.0073(15) 0.0054(14) 0.0028(13) 0.0046(13) C14 0.0110(18) 0.0122(16) 0.0103(16) 0.0022(14) 0.0035(14) 0.0060(14) C15 0.017(2) 0.0161(18) 0.023(2) 0.0060(17) 0.0086(16) 0.0099(16) C16 0.0134(18) 0.0114(16) 0.0087(15) 0.0056(14) 0.0064(14) 0.0089(14) C17 0.0173(19) 0.0157(17) 0.0149(17) 0.0096(16) 0.0048(15) 0.0090(15) C18 0.038(3) 0.027(2) 0.018(2) 0.0147(19) 0.0003(18) 0.0119(19) O7 0.0152(14) 0.0152(13) 0.0212(14) 0.0098(12) 0.0017(11) 0.0046(11) O8 0.0141(14) 0.0194(13) 0.0188(14) 0.0090(12) 0.0054(12) 0.0083(12) O9 0.0241(16) 0.0146(13) 0.0254(15) 0.0098(13) 0.0131(12) 0.0116(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 1.971(3) . ? Rh1 N2 1.983(3) . ? Rh1 O1 2.024(2) 2_556 ? Rh1 O2 2.028(2) 2_556 ? Rh1 Rh1 2.4266(6) 2_556 ? Rh1 Cl1 2.5735(8) . ? Rh2 N3 1.970(3) . ? Rh2 N4 1.983(2) . ? Rh2 O3 2.034(2) 2 ? Rh2 O4 2.041(2) 2 ? Rh2 Rh2 2.4276(8) 2 ? Rh2 Cl1 2.5761(10) . ? Rh3 N6 1.997(2) . ? Rh3 N5 2.013(3) . ? Rh3 O5 2.070(2) 2_666 ? Rh3 O6 2.0837(19) 2_666 ? Rh3 Rh3 2.4325(8) 2_666 ? Rh3 Cl1 2.6491(11) . ? N1 C1 1.300(4) . ? N1 H1 0.8800 . ? O1 C1 1.295(3) . ? N2 C4 1.308(4) . ? N2 H2 0.8800 . ? O2 C4 1.296(3) . ? N3 C7 1.306(4) . ? N3 H3 0.8800 . ? O3 C7 1.291(4) . ? N4 C10 1.306(4) . ? N4 H4 0.8800 . ? O4 C10 1.287(4) . ? N5 C13 1.287(4) . ? N5 H5 0.8800 . ? O5 C13 1.307(4) . ? N6 C16 1.292(4) . ? N6 H6 0.8800 . ? O6 C16 1.292(4) . ? C1 C2 1.496(4) . ? C2 C3B 1.455(9) . ? C2 C3A 1.583(10) . ? C2 H7B 0.9900 . ? C2 H8B 0.9900 . ? C2 H7A 0.9900 . ? C2 H8A 0.9900 . ? C3A H9A 0.9800 . ? C3A H10A 0.9800 . ? C3A H11A 0.9800 . ? C3B H9B 0.9800 . ? C3B H10B 0.9800 . ? C3B H11B 0.9800 . ? C4 C5 1.496(4) . ? C5 C6 1.525(5) . ? C5 H12 0.9900 . ? C5 H13 0.9900 . ? C6 H14 0.9800 . ? C6 H15 0.9800 . ? C6 H16 0.9800 . ? C7 C8 1.499(4) . ? C8 C9B 1.432(15) . ? C8 C9A 1.554(7) . ? C8 H17A 0.9900 . ? C8 H18A 0.9900 . ? C8 H17B 0.9900 . ? C8 H18B 0.9900 . ? C9A H19A 0.9800 . ? C9A H20A 0.9800 . ? C9A H21A 0.9800 . ? C9B H19B 0.9800 . ? C9B H20B 0.9800 . ? C9B H21B 0.9800 . ? C10 C11A 1.516(6) . ? C10 C11B 1.554(9) . ? C11A C12A 1.552(9) . ? C11A H22A 0.9900 . ? C11A H23A 0.9900 . ? C12A H24A 0.9800 . ? C12A H25A 0.9800 . ? C12A H26A 0.9800 . ? C11B C12B 1.496(15) . ? C11B H22B 0.9900 . ? C11B H23B 0.9900 . ? C12B H24B 0.9800 . ? C12B H25B 0.9800 . ? C12B H26B 0.9800 . ? C13 C14 1.509(5) . ? C14 C15 1.518(5) . ? C14 H27 0.9900 . ? C14 H28 0.9900 . ? C15 H29 0.9800 . ? C15 H30 0.9800 . ? C15 H31 0.9800 . ? C16 C17 1.515(4) . ? C17 C18 1.514(5) . ? C17 H32 0.9900 . ? C17 H33 0.9900 . ? C18 H34 0.9800 . ? C18 H35 0.9800 . ? C18 H36 0.9800 . ? O7 H37 0.83(4) . ? O7 H38 0.79(4) . ? O8 H39 0.68(3) . ? O8 H40 0.85(4) . ? O9 H41 0.87(4) . ? O9 H42 0.73(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2 90.17(11) . . ? N1 Rh1 O1 175.23(9) . 2_556 ? N2 Rh1 O1 90.99(10) . 2_556 ? N1 Rh1 O2 90.86(10) . 2_556 ? N2 Rh1 O2 175.47(8) . 2_556 ? O1 Rh1 O2 87.64(9) 2_556 2_556 ? N1 Rh1 Rh1 86.37(7) . 2_556 ? N2 Rh1 Rh1 86.44(7) . 2_556 ? O1 Rh1 Rh1 89.08(6) 2_556 2_556 ? O2 Rh1 Rh1 89.22(5) 2_556 2_556 ? N1 Rh1 Cl1 93.43(7) . . ? N2 Rh1 Cl1 93.60(7) . . ? O1 Rh1 Cl1 91.11(6) 2_556 . ? O2 Rh1 Cl1 90.75(6) 2_556 . ? Rh1 Rh1 Cl1 179.80(3) 2_556 . ? N3 Rh2 N4 90.81(10) . . ? N3 Rh2 O3 174.98(9) . 2 ? N4 Rh2 O3 90.89(10) . 2 ? N3 Rh2 O4 90.02(10) . 2 ? N4 Rh2 O4 175.52(9) . 2 ? O3 Rh2 O4 87.93(9) 2 2 ? N3 Rh2 Rh2 86.88(8) . 2 ? N4 Rh2 Rh2 86.28(8) . 2 ? O3 Rh2 Rh2 88.52(6) 2 2 ? O4 Rh2 Rh2 89.37(6) 2 2 ? N3 Rh2 Cl1 91.20(8) . . ? N4 Rh2 Cl1 92.93(8) . . ? O3 Rh2 Cl1 93.43(6) 2 . ? O4 Rh2 Cl1 91.46(6) 2 . ? Rh2 Rh2 Cl1 177.91(2) 2 . ? N6 Rh3 N5 91.04(10) . . ? N6 Rh3 O5 90.36(9) . 2_666 ? N5 Rh3 O5 175.00(9) . 2_666 ? N6 Rh3 O6 175.40(9) . 2_666 ? N5 Rh3 O6 88.48(9) . 2_666 ? O5 Rh3 O6 89.74(8) 2_666 2_666 ? N6 Rh3 Rh3 85.32(8) . 2_666 ? N5 Rh3 Rh3 86.92(8) . 2_666 ? O5 Rh3 Rh3 88.41(6) 2_666 2_666 ? O6 Rh3 Rh3 90.08(6) 2_666 2_666 ? N6 Rh3 Cl1 92.91(8) . . ? N5 Rh3 Cl1 95.28(8) . . ? O5 Rh3 Cl1 89.45(7) 2_666 . ? O6 Rh3 Cl1 91.69(7) 2_666 . ? Rh3 Rh3 Cl1 177.21(2) 2_666 . ? Rh1 Cl1 Rh2 117.10(3) . . ? Rh1 Cl1 Rh3 117.21(3) . . ? Rh2 Cl1 Rh3 119.57(3) . . ? C1 N1 Rh1 123.9(2) . . ? C1 N1 H1 118.1 . . ? Rh1 N1 H1 118.1 . . ? C1 O1 Rh1 118.46(19) . 2_556 ? C4 N2 Rh1 123.5(2) . . ? C4 N2 H2 118.3 . . ? Rh1 N2 H2 118.3 . . ? C4 O2 Rh1 118.66(18) . 2_556 ? C7 N3 Rh2 123.6(2) . . ? C7 N3 H3 118.2 . . ? Rh2 N3 H3 118.2 . . ? C7 O3 Rh2 118.98(19) . 2 ? C10 N4 Rh2 123.6(2) . . ? C10 N4 H4 118.2 . . ? Rh2 N4 H4 118.2 . . ? C10 O4 Rh2 117.82(18) . 2 ? C13 N5 Rh3 123.7(2) . . ? C13 N5 H5 118.2 . . ? Rh3 N5 H5 118.2 . . ? C13 O5 Rh3 118.64(19) . 2_666 ? C16 N6 Rh3 125.4(2) . . ? C16 N6 H6 117.3 . . ? Rh3 N6 H6 117.3 . . ? C16 O6 Rh3 115.91(19) . 2_666 ? O1 C1 N1 122.1(3) . . ? O1 C1 C2 116.0(3) . . ? N1 C1 C2 121.9(3) . . ? C3B C2 C1 115.9(5) . . ? C1 C2 C3A 109.7(4) . . ? C3B C2 H7B 108.3 . . ? C1 C2 H7B 108.3 . . ? C3B C2 H8B 108.3 . . ? C1 C2 H8B 108.3 . . ? C3A C2 H8B 97.7 . . ? H7B C2 H8B 107.4 . . ? C1 C2 H7A 109.7 . . ? C3A C2 H7A 109.7 . . ? C1 C2 H8A 109.7 . . ? C3A C2 H8A 109.7 . . ? H7A C2 H8A 108.2 . . ? C2 C3A H9A 109.5 . . ? C2 C3A H10A 109.5 . . ? C2 C3A H11A 109.5 . . ? C2 C3B H9B 109.5 . . ? C2 C3B H10B 109.5 . . ? H9B C3B H10B 109.5 . . ? C2 C3B H11B 109.5 . . ? H9B C3B H11B 109.5 . . ? H10B C3B H11B 109.5 . . ? O2 C4 N2 121.9(3) . . ? O2 C4 C5 116.8(2) . . ? N2 C4 C5 121.3(3) . . ? C4 C5 C6 112.1(3) . . ? C4 C5 H12 109.2 . . ? C6 C5 H12 109.2 . . ? C4 C5 H13 109.2 . . ? C6 C5 H13 109.2 . . ? H12 C5 H13 107.9 . . ? C5 C6 H14 109.5 . . ? C5 C6 H15 109.5 . . ? H14 C6 H15 109.5 . . ? C5 C6 H16 109.5 . . ? H14 C6 H16 109.5 . . ? H15 C6 H16 109.5 . . ? O3 C7 N3 121.9(3) . . ? O3 C7 C8 116.5(3) . . ? N3 C7 C8 121.5(3) . . ? C9B C8 C7 118.2(8) . . ? C7 C8 C9A 110.0(3) . . ? C7 C8 H17A 109.7 . . ? C9A C8 H17A 109.7 . . ? C7 C8 H18A 109.7 . . ? C9A C8 H18A 109.7 . . ? H17A C8 H18A 108.2 . . ? C9B C8 H17B 107.8 . . ? C7 C8 H17B 107.8 . . ? C9B C8 H18B 107.8 . . ? C7 C8 H18B 107.8 . . ? H17B C8 H18B 107.1 . . ? C8 C9A H19A 109.5 . . ? C8 C9A H20A 109.5 . . ? C8 C9A H21A 109.5 . . ? C8 C9B H19B 109.5 . . ? C8 C9B H20B 109.5 . . ? H19B C9B H20B 109.5 . . ? C8 C9B H21B 109.5 . . ? H19B C9B H21B 109.5 . . ? H20B C9B H21B 109.5 . . ? O4 C10 N4 122.9(3) . . ? O4 C10 C11A 115.7(3) . . ? N4 C10 C11A 120.8(3) . . ? O4 C10 C11B 117.9(4) . . ? N4 C10 C11B 117.6(4) . . ? C10 C11A C12A 111.5(5) . . ? C10 C11A H22A 109.3 . . ? C12A C11A H22A 109.3 . . ? C10 C11A H23A 109.3 . . ? C12A C11A H23A 109.3 . . ? H22A C11A H23A 108.0 . . ? C12B C11B C10 112.9(9) . . ? C12B C11B H22B 109.0 . . ? C10 C11B H22B 109.0 . . ? C12B C11B H23B 109.0 . . ? C10 C11B H23B 109.0 . . ? H22B C11B H23B 107.8 . . ? C11B C12B H24B 109.5 . . ? C11B C12B H25B 109.5 . . ? H24B C12B H25B 109.5 . . ? C11B C12B H26B 109.5 . . ? H24B C12B H26B 109.5 . . ? H25B C12B H26B 109.5 . . ? N5 C13 O5 122.0(3) . . ? N5 C13 C14 123.6(3) . . ? O5 C13 C14 114.4(3) . . ? C13 C14 C15 117.3(3) . . ? C13 C14 H27 108.0 . . ? C15 C14 H27 108.0 . . ? C13 C14 H28 108.0 . . ? C15 C14 H28 108.0 . . ? H27 C14 H28 107.2 . . ? C14 C15 H29 109.5 . . ? C14 C15 H30 109.5 . . ? H29 C15 H30 109.5 . . ? C14 C15 H31 109.5 . . ? H29 C15 H31 109.5 . . ? H30 C15 H31 109.5 . . ? N6 C16 O6 123.3(2) . . ? N6 C16 C17 121.1(3) . . ? O6 C16 C17 115.6(3) . . ? C18 C17 C16 113.2(3) . . ? C18 C17 H32 108.9 . . ? C16 C17 H32 108.9 . . ? C18 C17 H33 108.9 . . ? C16 C17 H33 108.9 . . ? H32 C17 H33 107.7 . . ? C17 C18 H34 109.5 . . ? C17 C18 H35 109.5 . . ? H34 C18 H35 109.5 . . ? C17 C18 H36 109.5 . . ? H34 C18 H36 109.5 . . ? H35 C18 H36 109.5 . . ? H37 O7 H38 105(4) . . ? H39 O8 H40 109(4) . . ? H41 O9 H42 106(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 Cl1 Rh2 -2.15(8) . . . . ? N2 Rh1 Cl1 Rh2 88.23(8) . . . . ? O1 Rh1 Cl1 Rh2 179.29(7) 2_556 . . . ? O2 Rh1 Cl1 Rh2 -93.06(7) 2_556 . . . ? N1 Rh1 Cl1 Rh3 -154.57(8) . . . . ? N2 Rh1 Cl1 Rh3 -64.18(8) . . . . ? O1 Rh1 Cl1 Rh3 26.87(7) 2_556 . . . ? O2 Rh1 Cl1 Rh3 114.53(7) 2_556 . . . ? N3 Rh2 Cl1 Rh1 -139.40(7) . . . . ? N4 Rh2 Cl1 Rh1 129.73(8) . . . . ? O3 Rh2 Cl1 Rh1 38.67(6) 2 . . . ? O4 Rh2 Cl1 Rh1 -49.34(7) 2 . . . ? N3 Rh2 Cl1 Rh3 12.35(7) . . . . ? N4 Rh2 Cl1 Rh3 -78.52(8) . . . . ? O3 Rh2 Cl1 Rh3 -169.59(6) 2 . . . ? O4 Rh2 Cl1 Rh3 102.40(7) 2 . . . ? N6 Rh3 Cl1 Rh1 16.70(8) . . . . ? N5 Rh3 Cl1 Rh1 -74.61(7) . . . . ? O5 Rh3 Cl1 Rh1 107.04(6) 2_666 . . . ? O6 Rh3 Cl1 Rh1 -163.24(7) 2_666 . . . ? N6 Rh3 Cl1 Rh2 -135.01(8) . . . . ? N5 Rh3 Cl1 Rh2 133.68(7) . . . . ? O5 Rh3 Cl1 Rh2 -44.67(6) 2_666 . . . ? O6 Rh3 Cl1 Rh2 45.05(7) 2_666 . . . ? N2 Rh1 N1 C1 83.4(3) . . . . ? O2 Rh1 N1 C1 -92.2(3) 2_556 . . . ? Rh1 Rh1 N1 C1 -3.1(3) 2_556 . . . ? Cl1 Rh1 N1 C1 177.0(3) . . . . ? N1 Rh1 N2 C4 -81.9(3) . . . . ? O1 Rh1 N2 C4 93.4(3) 2_556 . . . ? Rh1 Rh1 N2 C4 4.4(3) 2_556 . . . ? Cl1 Rh1 N2 C4 -175.4(3) . . . . ? N4 Rh2 N3 C7 -83.9(2) . . . . ? O4 Rh2 N3 C7 91.7(2) 2 . . . ? Rh2 Rh2 N3 C7 2.3(2) 2 . . . ? Cl1 Rh2 N3 C7 -176.9(2) . . . . ? N3 Rh2 N4 C10 86.1(3) . . . . ? O3 Rh2 N4 C10 -89.2(3) 2 . . . ? Rh2 Rh2 N4 C10 -0.7(3) 2 . . . ? Cl1 Rh2 N4 C10 177.3(3) . . . . ? N6 Rh3 N5 C13 86.3(2) . . . . ? O6 Rh3 N5 C13 -89.1(2) 2_666 . . . ? Rh3 Rh3 N5 C13 1.0(2) 2_666 . . . ? Cl1 Rh3 N5 C13 179.3(2) . . . . ? N5 Rh3 N6 C16 -86.8(3) . . . . ? O5 Rh3 N6 C16 88.4(3) 2_666 . . . ? Rh3 Rh3 N6 C16 0.1(3) 2_666 . . . ? Cl1 Rh3 N6 C16 177.9(3) . . . . ? Rh1 O1 C1 N1 -1.7(4) 2_556 . . . ? Rh1 O1 C1 C2 178.3(2) 2_556 . . . ? Rh1 N1 C1 O1 3.7(5) . . . . ? Rh1 N1 C1 C2 -176.3(2) . . . . ? O1 C1 C2 C3B -31.9(9) . . . . ? N1 C1 C2 C3B 148.1(9) . . . . ? O1 C1 C2 C3A -48.2(7) . . . . ? N1 C1 C2 C3A 131.8(7) . . . . ? Rh1 O2 C4 N2 4.8(4) 2_556 . . . ? Rh1 O2 C4 C5 -174.3(2) 2_556 . . . ? Rh1 N2 C4 O2 -6.7(4) . . . . ? Rh1 N2 C4 C5 172.3(2) . . . . ? O2 C4 C5 C6 -59.8(4) . . . . ? N2 C4 C5 C6 121.0(3) . . . . ? Rh2 O3 C7 N3 -1.5(4) 2 . . . ? Rh2 O3 C7 C8 178.28(19) 2 . . . ? Rh2 N3 C7 O3 -1.0(4) . . . . ? Rh2 N3 C7 C8 179.2(2) . . . . ? O3 C7 C8 C9B -45.2(13) . . . . ? N3 C7 C8 C9B 134.6(13) . . . . ? O3 C7 C8 C9A -64.0(5) . . . . ? N3 C7 C8 C9A 115.8(5) . . . . ? Rh2 O4 C10 N4 1.8(4) 2 . . . ? Rh2 O4 C10 C11A -169.6(4) 2 . . . ? Rh2 O4 C10 C11B 167.0(6) 2 . . . ? Rh2 N4 C10 O4 -0.5(5) . . . . ? Rh2 N4 C10 C11A 170.4(4) . . . . ? Rh2 N4 C10 C11B -165.8(6) . . . . ? O4 C10 C11A C12A -40.1(9) . . . . ? N4 C10 C11A C12A 148.3(6) . . . . ? C11B C10 C11A C12A 61.0(12) . . . . ? O4 C10 C11B C12B 31.9(15) . . . . ? N4 C10 C11B C12B -162.1(11) . . . . ? C11A C10 C11B C12B -57.7(15) . . . . ? Rh3 N5 C13 O5 -5.4(4) . . . . ? Rh3 N5 C13 C14 175.0(2) . . . . ? Rh3 O5 C13 N5 7.4(3) 2_666 . . . ? Rh3 O5 C13 C14 -173.00(17) 2_666 . . . ? N5 C13 C14 C15 -11.6(4) . . . . ? O5 C13 C14 C15 168.8(2) . . . . ? Rh3 N6 C16 O6 -0.6(5) . . . . ? Rh3 N6 C16 C17 -178.8(2) . . . . ? Rh3 O6 C16 N6 0.8(4) 2_666 . . . ? Rh3 O6 C16 C17 179.1(2) 2_666 . . . ? N6 C16 C17 C18 -135.6(3) . . . . ? O6 C16 C17 C18 46.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O3 0.88 2.21 3.011(3) 151.3 2 N2 H2 O7 0.88 2.07 2.893(4) 154.6 . N3 H3 O5 0.88 2.18 3.032(3) 162.4 2_666 N4 H4 O8 0.88 2.11 2.978(4) 167.8 . N5 H5 O9 0.88 2.25 3.108(4) 164.9 . N6 H6 O1 0.88 2.38 3.037(3) 131.6 2_556 O7 H37 O4 0.83(4) 2.06(4) 2.889(3) 174(4) 2 O7 H38 O5 0.79(4) 1.99(4) 2.778(3) 178(4) 2_666 O8 H40 O6 0.85(4) 1.97(4) 2.803(4) 164(4) 2_666 O8 H39 O9 0.68(3) 2.14(4) 2.820(3) 174(5) . O9 H41 O2 0.87(4) 1.95(4) 2.821(3) 174(4) 2_556 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.951 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.114 #===END data_[{Rh2(pram)4}3Br2].6H2O_(5.6H2O) _database_code_depnum_ccdc_archive 'CCDC 775021' #TrackingRef 'web_deposit_cif_file_0_MasahiroEbihara_1272351332.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H72 Br2 N12 O12 Rh6, 6(H2 O)' _chemical_formula_sum 'C36 H84 Br2 N12 O18 Rh6' _chemical_formula_weight 1750.44 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.446(3) _cell_length_b 12.754(4) _cell_length_c 13.172(4) _cell_angle_alpha 117.150(10) _cell_angle_beta 93.74(2) _cell_angle_gamma 113.690(10) _cell_volume 1492.1(8) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4272 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Platelet _exptl_crystal_colour Brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 3.031 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.906 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 12344 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6793 _reflns_number_gt 5815 _reflns_threshold_expression ' I>2\s(I)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0089P)^2^+5.4497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00094(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6793 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.04286(4) 0.06193(4) 0.45126(4) 0.00735(10) Uani 1 1 d . . . Rh2 Rh 0.04074(4) 0.05970(4) 0.10840(4) 0.00767(10) Uani 1 1 d . . . Rh3 Rh 0.38499(4) 0.40844(4) 0.45266(4) 0.00717(10) Uani 1 1 d . . . Br1 Br 0.13325(4) 0.19835(5) 0.34528(4) 0.00781(11) Uani 1 1 d . . . N1 N -0.0866(4) -0.1051(5) 0.3003(4) 0.0117(9) Uani 1 1 d . . . H1 H -0.0917 -0.1038 0.2340 0.014 Uiso 1 1 calc R . . O1 O -0.1675(3) -0.2268(4) 0.3867(3) 0.0121(8) Uani 1 1 d . . . N2 N 0.1754(4) -0.0031(5) 0.4324(4) 0.0133(9) Uani 1 1 d . . . H2 H 0.2370 0.0247 0.4004 0.016 Uiso 1 1 calc R . . O2 O 0.0962(3) -0.1251(4) 0.5194(3) 0.0110(7) Uani 1 1 d . . . N3 N 0.2204(4) 0.1509(4) 0.0959(4) 0.0100(9) Uani 1 1 d . . . H3 H 0.2886 0.2076 0.1621 0.012 Uiso 1 1 calc R . . O3 O 0.1484(3) 0.0491(4) -0.1068(3) 0.0122(8) Uani 1 1 d . . . N4 N -0.0023(4) 0.1951(4) 0.1082(4) 0.0100(9) Uani 1 1 d . . . H4 H 0.0136 0.2653 0.1779 0.012 Uiso 1 1 calc R . . O4 O -0.0772(3) 0.0896(4) -0.0938(3) 0.0126(8) Uani 1 1 d . . . N5 N 0.3366(4) 0.5347(4) 0.5794(4) 0.0107(9) Uani 1 1 d . . . H5 H 0.2522 0.5048 0.5780 0.013 Uiso 1 1 calc R . . O5 O 0.5510(3) 0.7073(4) 0.6755(3) 0.0108(7) Uani 1 1 d . . . N6 N 0.4317(4) 0.3526(4) 0.5619(4) 0.0112(9) Uani 1 1 d . . . H6 H 0.3684 0.2812 0.5576 0.013 Uiso 1 1 calc R . . O6 O 0.6485(3) 0.5197(4) 0.6537(3) 0.0122(8) Uani 1 1 d . . . C1 C -0.1653(4) -0.2175(5) 0.2936(5) 0.0100(10) Uani 1 1 d . A . C2 C -0.2561(5) -0.3457(5) 0.1750(5) 0.0160(12) Uani 1 1 d . . . H7A H -0.3446 -0.3510 0.1595 0.019 Uiso 0.57(7) 1 calc PR A 1 H8A H -0.2186 -0.3398 0.1110 0.019 Uiso 0.57(7) 1 calc PR A 1 H7B H -0.2329 -0.3347 0.1081 0.019 Uiso 0.43(7) 1 calc PR A 2 H8B H -0.3506 -0.3667 0.1675 0.019 Uiso 0.43(7) 1 calc PR A 2 C3A C -0.276(3) -0.4723(12) 0.1660(11) 0.016(4) Uiso 0.57(7) 1 d P A 1 H9A H -0.3130 -0.4796 0.2291 0.023 Uiso 0.57(7) 1 calc PR A 1 H10A H -0.1905 -0.4717 0.1754 0.023 Uiso 0.57(7) 1 calc PR A 1 H11A H -0.3392 -0.5495 0.0875 0.023 Uiso 0.57(7) 1 calc PR A 1 C3B C -0.237(3) -0.4646(17) 0.1700(15) 0.016(5) Uiso 0.43(7) 1 d P A 2 H9B H -0.2863 -0.5460 0.0900 0.024 Uiso 0.43(7) 1 calc PR A 2 H10B H -0.2712 -0.4827 0.2298 0.024 Uiso 0.43(7) 1 calc PR A 2 H11B H -0.1415 -0.4383 0.1872 0.024 Uiso 0.43(7) 1 calc PR A 2 C4 C 0.1756(5) -0.0847(5) 0.4651(5) 0.0113(11) Uani 1 1 d . . . C5 C 0.2719(5) -0.1419(6) 0.4389(5) 0.0171(12) Uani 1 1 d . . . H12 H 0.2197 -0.2414 0.3877 0.021 Uiso 1 1 calc R . . H13 H 0.3263 -0.1084 0.3942 0.021 Uiso 1 1 calc R . . C6 C 0.3639(6) -0.1025(8) 0.5524(6) 0.0314(16) Uani 1 1 d . . . H14 H 0.3104 -0.1363 0.5965 0.047 Uiso 1 1 calc R . . H15 H 0.4176 -0.0041 0.6024 0.047 Uiso 1 1 calc R . . H16 H 0.4234 -0.1416 0.5320 0.047 Uiso 1 1 calc R . . C7 C 0.2431(5) 0.1315(5) -0.0047(5) 0.0105(11) Uani 1 1 d . B . C8 C 0.3810(5) 0.2038(6) -0.0113(5) 0.0139(11) Uani 1 1 d . . . H17A H 0.4447 0.2691 0.0706 0.017 Uiso 0.74(5) 1 calc PR B 1 H18A H 0.3795 0.2545 -0.0497 0.017 Uiso 0.74(5) 1 calc PR B 1 H17B H 0.3868 0.2785 -0.0203 0.017 Uiso 0.26(5) 1 calc PR B 2 H18B H 0.4470 0.2446 0.0661 0.017 Uiso 0.26(5) 1 calc PR B 2 C9A C 0.4287(9) 0.1018(11) -0.0845(10) 0.017(3) Uiso 0.74(5) 1 d P B 1 H19A H 0.5169 0.1502 -0.0905 0.025 Uiso 0.74(5) 1 calc PR B 1 H20A H 0.3645 0.0359 -0.1651 0.025 Uiso 0.74(5) 1 calc PR B 1 H21A H 0.4348 0.0550 -0.0442 0.025 Uiso 0.74(5) 1 calc PR B 1 C9B C 0.419(3) 0.126(4) -0.103(3) 0.028(9) Uiso 0.26(5) 1 d P B 2 H19B H 0.3624 0.0947 -0.1808 0.043 Uiso 0.26(5) 1 calc PR B 2 H20B H 0.4092 0.0486 -0.0987 0.043 Uiso 0.26(5) 1 calc PR B 2 H21B H 0.5131 0.1813 -0.0940 0.043 Uiso 0.26(5) 1 calc PR B 2 C10 C -0.0524(5) 0.1876(5) 0.0125(5) 0.0131(11) Uani 1 1 d . C . C11 C -0.0899(7) 0.2908(7) 0.0188(6) 0.0292(15) Uani 1 1 d . . . H22A H -0.1854 0.2586 0.0152 0.035 Uiso 0.79(3) 1 calc PR C 1 H23A H -0.0362 0.3760 0.0971 0.035 Uiso 0.79(3) 1 calc PR C 1 H22B H -0.1606 0.2860 0.0586 0.035 Uiso 0.21(3) 1 calc PR C 2 H23B H -0.0105 0.3805 0.0734 0.035 Uiso 0.21(3) 1 calc PR C 2 C12A C -0.0691(13) 0.3198(10) -0.0788(8) 0.028(3) Uiso 0.79(3) 1 d P C 1 H24A H -0.1069 0.3775 -0.0753 0.042 Uiso 0.79(3) 1 calc PR C 1 H25A H -0.1137 0.2349 -0.1568 0.042 Uiso 0.79(3) 1 calc PR C 1 H26A H 0.0271 0.3658 -0.0682 0.042 Uiso 0.79(3) 1 calc PR C 1 C12B C -0.133(4) 0.289(3) -0.081(3) 0.022(10) Uiso 0.21(3) 1 d P C 2 H24B H -0.2229 0.2117 -0.1285 0.033 Uiso 0.21(3) 1 calc PR C 2 H25B H -0.0714 0.2823 -0.1283 0.033 Uiso 0.21(3) 1 calc PR C 2 H26B H -0.1365 0.3727 -0.0568 0.033 Uiso 0.21(3) 1 calc PR C 2 C13 C 0.4231(5) 0.6573(5) 0.6626(5) 0.0099(10) Uani 1 1 d . . . C14 C 0.3850(5) 0.7547(6) 0.7527(5) 0.0137(11) Uani 1 1 d . . . H27 H 0.4227 0.7744 0.8330 0.016 Uiso 1 1 calc R . . H28 H 0.4286 0.8404 0.7544 0.016 Uiso 1 1 calc R . . C15 C 0.2367(5) 0.7096(6) 0.7316(5) 0.0205(13) Uani 1 1 d . . . H29 H 0.1935 0.6315 0.7400 0.031 Uiso 1 1 calc R . . H30 H 0.1962 0.6846 0.6506 0.031 Uiso 1 1 calc R . . H31 H 0.2245 0.7834 0.7904 0.031 Uiso 1 1 calc R . . C16 C 0.5490(5) 0.4144(5) 0.6390(4) 0.0096(10) Uani 1 1 d . . . C17 C 0.5746(5) 0.3614(6) 0.7154(5) 0.0151(11) Uani 1 1 d . . . H32 H 0.6298 0.3179 0.6849 0.018 Uiso 1 1 calc R . . H33 H 0.4880 0.2919 0.7080 0.018 Uiso 1 1 calc R . . C18 C 0.6458(6) 0.4718(7) 0.8472(5) 0.0275(14) Uani 1 1 d . . . H34 H 0.5902 0.5132 0.8787 0.041 Uiso 1 1 calc R . . H35 H 0.7320 0.5405 0.8553 0.041 Uiso 1 1 calc R . . H36 H 0.6608 0.4326 0.8923 0.041 Uiso 1 1 calc R . . O7 O 0.3273(4) 0.0250(4) 0.2684(4) 0.0165(9) Uani 1 1 d . . . H37 H 0.254(6) -0.012(7) 0.217(6) 0.025 Uiso 1 1 d . . . H38 H 0.363(6) 0.096(7) 0.293(6) 0.025 Uiso 1 1 d . . . O8 O 0.0950(4) 0.4540(4) 0.3465(4) 0.0162(8) Uani 1 1 d . . . H39 H 0.170(6) 0.461(6) 0.349(6) 0.024 Uiso 1 1 d . . . H40 H 0.073(6) 0.423(7) 0.393(6) 0.024 Uiso 1 1 d . . . O9 O 0.0251(4) 0.3937(4) 0.5256(4) 0.0195(9) Uani 1 1 d . . . H41 H -0.008(6) 0.314(7) 0.507(6) 0.029 Uiso 1 1 d . . . H42 H -0.021(6) 0.421(7) 0.563(6) 0.029 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.00766(18) 0.0075(2) 0.0070(2) 0.00439(17) 0.00296(14) 0.00303(15) Rh2 0.00784(18) 0.0072(2) 0.0053(2) 0.00260(17) 0.00076(14) 0.00243(15) Rh3 0.00508(18) 0.0074(2) 0.0067(2) 0.00288(17) 0.00148(14) 0.00208(15) Br1 0.0073(2) 0.0071(3) 0.0057(2) 0.0029(2) 0.00104(18) 0.00130(18) N1 0.014(2) 0.016(3) 0.007(2) 0.008(2) 0.0034(17) 0.0067(18) O1 0.0156(18) 0.0096(19) 0.0075(19) 0.0046(16) 0.0035(14) 0.0031(15) N2 0.010(2) 0.013(2) 0.013(2) 0.006(2) 0.0061(17) 0.0037(18) O2 0.0106(16) 0.014(2) 0.0123(19) 0.0088(17) 0.0063(14) 0.0064(15) N3 0.0067(19) 0.010(2) 0.007(2) 0.0023(19) -0.0009(16) 0.0020(17) O3 0.0127(17) 0.011(2) 0.0089(19) 0.0042(17) 0.0031(14) 0.0039(15) N4 0.015(2) 0.010(2) 0.005(2) 0.0022(19) 0.0034(17) 0.0075(18) O4 0.0155(17) 0.0088(19) 0.0092(19) 0.0028(16) 0.0010(14) 0.0050(15) N5 0.0057(18) 0.016(2) 0.009(2) 0.006(2) 0.0020(16) 0.0048(17) O5 0.0065(16) 0.0079(19) 0.0109(19) 0.0023(16) 0.0018(13) 0.0007(14) N6 0.011(2) 0.011(2) 0.011(2) 0.006(2) 0.0040(17) 0.0047(18) O6 0.0093(16) 0.011(2) 0.0100(19) 0.0041(17) 0.0006(14) 0.0023(14) C1 0.004(2) 0.010(3) 0.007(3) 0.001(2) -0.0023(18) 0.0001(19) C2 0.020(3) 0.007(3) 0.011(3) 0.003(2) 0.003(2) 0.002(2) C4 0.007(2) 0.012(3) 0.014(3) 0.007(2) 0.0020(19) 0.003(2) C5 0.017(3) 0.025(3) 0.016(3) 0.012(3) 0.010(2) 0.014(2) C6 0.027(3) 0.053(5) 0.030(4) 0.026(4) 0.013(3) 0.028(3) C7 0.005(2) 0.017(3) 0.009(3) 0.007(2) 0.0007(19) 0.006(2) C8 0.014(2) 0.014(3) 0.009(3) 0.005(2) 0.002(2) 0.006(2) C10 0.016(2) 0.011(3) 0.012(3) 0.006(2) 0.003(2) 0.007(2) C11 0.056(4) 0.027(4) 0.014(3) 0.009(3) 0.009(3) 0.031(3) C13 0.009(2) 0.011(3) 0.008(3) 0.006(2) 0.0014(19) 0.003(2) C14 0.011(2) 0.015(3) 0.011(3) 0.003(2) 0.004(2) 0.007(2) C15 0.012(3) 0.023(3) 0.027(3) 0.010(3) 0.011(2) 0.012(2) C16 0.015(2) 0.012(3) 0.006(2) 0.005(2) 0.0072(19) 0.010(2) C17 0.017(3) 0.019(3) 0.013(3) 0.009(3) 0.006(2) 0.012(2) C18 0.034(3) 0.025(4) 0.018(3) 0.012(3) 0.001(3) 0.009(3) O7 0.0107(19) 0.016(2) 0.019(2) 0.010(2) 0.0031(16) 0.0017(16) O8 0.0166(19) 0.018(2) 0.017(2) 0.0086(19) 0.0063(16) 0.0119(17) O9 0.022(2) 0.016(2) 0.024(2) 0.010(2) 0.0128(18) 0.0115(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 1.975(4) . ? Rh1 N2 1.981(4) . ? Rh1 O1 2.027(4) 2_556 ? Rh1 O2 2.039(3) 2_556 ? Rh1 Rh1 2.4242(10) 2_556 ? Rh1 Br1 2.6467(9) . ? Rh2 N3 1.976(4) . ? Rh2 N4 1.979(4) . ? Rh2 O4 2.038(4) 2 ? Rh2 O3 2.041(3) 2 ? Rh2 Rh2 2.4261(12) 2 ? Rh2 Br1 2.6481(12) . ? Rh3 N6 2.001(4) . ? Rh3 N5 2.017(4) . ? Rh3 O5 2.079(3) 2_666 ? Rh3 O6 2.082(4) 2_666 ? Rh3 Rh3 2.4318(11) 2_666 ? Rh3 Br1 2.6996(11) . ? N1 C1 1.307(7) . ? N1 H1 0.8800 . ? O1 C1 1.286(6) . ? N2 C4 1.296(7) . ? N2 H2 0.8800 . ? O2 C4 1.284(6) . ? N3 C7 1.297(6) . ? N3 H3 0.8800 . ? O3 C7 1.301(6) . ? N4 C10 1.296(6) . ? N4 H4 0.8800 . ? O4 C10 1.292(6) . ? N5 C13 1.295(7) . ? N5 H5 0.8800 . ? O5 C13 1.303(6) . ? N6 C16 1.302(6) . ? N6 H6 0.8800 . ? O6 C16 1.282(6) . ? C1 C2 1.511(7) . ? C2 C3A 1.481(13) . ? C2 C3B 1.59(2) . ? C2 H7A 0.9900 . ? C2 H8A 0.9900 . ? C2 H7B 0.9900 . ? C2 H8B 0.9900 . ? C3A H9A 0.9800 . ? C3A H10A 0.9800 . ? C3A H11A 0.9800 . ? C3B H9B 0.9800 . ? C3B H10B 0.9800 . ? C3B H11B 0.9800 . ? C4 C5 1.526(7) . ? C5 C6 1.510(8) . ? C5 H12 0.9900 . ? C5 H13 0.9900 . ? C6 H14 0.9800 . ? C6 H15 0.9800 . ? C6 H16 0.9800 . ? C7 C8 1.508(7) . ? C8 C9B 1.40(3) . ? C8 C9A 1.553(12) . ? C8 H17A 0.9900 . ? C8 H18A 0.9900 . ? C8 H17B 0.9900 . ? C8 H18B 0.9900 . ? C9A H19A 0.9800 . ? C9A H20A 0.9800 . ? C9A H21A 0.9800 . ? C9B H19B 0.9800 . ? C9B H20B 0.9800 . ? C9B H21B 0.9800 . ? C10 C11 1.511(8) . ? C11 C12B 1.36(3) . ? C11 C12A 1.499(11) . ? C11 H22A 0.9900 . ? C11 H23A 0.9900 . ? C11 H22B 0.9900 . ? C11 H23B 0.9900 . ? C12A H24A 0.9800 . ? C12A H25A 0.9800 . ? C12A H26A 0.9800 . ? C12B H24B 0.9800 . ? C12B H25B 0.9800 . ? C12B H26B 0.9800 . ? C13 C14 1.517(7) . ? C14 C15 1.515(6) . ? C14 H27 0.9900 . ? C14 H28 0.9900 . ? C15 H29 0.9800 . ? C15 H30 0.9800 . ? C15 H31 0.9800 . ? C16 C17 1.516(7) . ? C17 C18 1.524(8) . ? C17 H32 0.9900 . ? C17 H33 0.9900 . ? C18 H34 0.9800 . ? C18 H35 0.9800 . ? C18 H36 0.9800 . ? O7 H37 0.84(6) . ? O7 H38 0.72(7) . ? O8 H39 0.82(6) . ? O8 H40 0.87(7) . ? O9 H41 0.83(7) . ? O9 H42 0.82(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2 90.06(17) . . ? N1 Rh1 O1 175.36(16) . 2_556 ? N2 Rh1 O1 90.82(16) . 2_556 ? N1 Rh1 O2 91.00(16) . 2_556 ? N2 Rh1 O2 175.51(17) . 2_556 ? O1 Rh1 O2 87.77(14) 2_556 2_556 ? N1 Rh1 Rh1 86.42(13) . 2_556 ? N2 Rh1 Rh1 86.39(14) . 2_556 ? O1 Rh1 Rh1 89.09(11) 2_556 2_556 ? O2 Rh1 Rh1 89.33(10) 2_556 2_556 ? N1 Rh1 Br1 93.54(13) . . ? N2 Rh1 Br1 94.58(13) . . ? O1 Rh1 Br1 90.93(11) 2_556 . ? O2 Rh1 Br1 89.71(10) 2_556 . ? Rh1 Rh1 Br1 179.03(3) 2_556 . ? N3 Rh2 N4 91.10(17) . . ? N3 Rh2 O4 89.40(16) . 2 ? N4 Rh2 O4 175.29(16) . 2 ? N3 Rh2 O3 174.88(16) . 2 ? N4 Rh2 O3 91.26(16) . 2 ? O4 Rh2 O3 87.88(14) 2 2 ? N3 Rh2 Rh2 87.02(13) . 2 ? N4 Rh2 Rh2 85.95(12) . 2 ? O4 Rh2 Rh2 89.40(10) 2 2 ? O3 Rh2 Rh2 88.61(11) 2 2 ? N3 Rh2 Br1 91.81(13) . . ? N4 Rh2 Br1 92.37(12) . . ? O4 Rh2 Br1 92.30(10) 2 . ? O3 Rh2 Br1 92.63(11) 2 . ? Rh2 Rh2 Br1 177.93(3) 2 . ? N6 Rh3 N5 90.93(17) . . ? N6 Rh3 O5 90.69(16) . 2_666 ? N5 Rh3 O5 175.16(16) . 2_666 ? N6 Rh3 O6 175.39(16) . 2_666 ? N5 Rh3 O6 88.29(16) . 2_666 ? O5 Rh3 O6 89.74(14) 2_666 2_666 ? N6 Rh3 Rh3 85.62(12) . 2_666 ? N5 Rh3 Rh3 86.92(12) . 2_666 ? O5 Rh3 Rh3 88.66(10) 2_666 2_666 ? O6 Rh3 Rh3 89.80(10) 2_666 2_666 ? N6 Rh3 Br1 93.16(12) . . ? N5 Rh3 Br1 94.94(12) . . ? O5 Rh3 Br1 89.53(9) 2_666 . ? O6 Rh3 Br1 91.44(10) 2_666 . ? Rh3 Rh3 Br1 177.80(3) 2_666 . ? Rh1 Br1 Rh2 116.47(3) . . ? Rh1 Br1 Rh3 117.43(3) . . ? Rh2 Br1 Rh3 118.17(3) . . ? C1 N1 Rh1 123.6(4) . . ? C1 N1 H1 118.2 . . ? Rh1 N1 H1 118.2 . . ? C1 O1 Rh1 118.7(3) . 2_556 ? C4 N2 Rh1 123.0(4) . . ? C4 N2 H2 118.5 . . ? Rh1 N2 H2 118.5 . . ? C4 O2 Rh1 117.3(3) . 2_556 ? C7 N3 Rh2 123.4(3) . . ? C7 N3 H3 118.3 . . ? Rh2 N3 H3 118.3 . . ? C7 O3 Rh2 118.4(3) . 2 ? C10 N4 Rh2 124.5(4) . . ? C10 N4 H4 117.8 . . ? Rh2 N4 H4 117.8 . . ? C10 O4 Rh2 117.9(3) . 2 ? C13 N5 Rh3 123.5(3) . . ? C13 N5 H5 118.2 . . ? Rh3 N5 H5 118.2 . . ? C13 O5 Rh3 118.3(3) . 2_666 ? C16 N6 Rh3 124.7(4) . . ? C16 N6 H6 117.6 . . ? Rh3 N6 H6 117.6 . . ? C16 O6 Rh3 116.6(3) . 2_666 ? O1 C1 N1 122.2(5) . . ? O1 C1 C2 115.9(5) . . ? N1 C1 C2 121.9(5) . . ? C3A C2 C1 115.7(8) . . ? C1 C2 C3B 108.3(9) . . ? C3A C2 H7A 108.4 . . ? C1 C2 H7A 108.4 . . ? C3A C2 H8A 108.4 . . ? C1 C2 H8A 108.4 . . ? H7A C2 H8A 107.4 . . ? C1 C2 H7B 110.0 . . ? C3B C2 H7B 110.0 . . ? C3A C2 H8B 95.0 . . ? C1 C2 H8B 110.0 . . ? C3B C2 H8B 110.0 . . ? H7B C2 H8B 108.4 . . ? C2 C3A H9A 109.5 . . ? C2 C3A H10A 109.5 . . ? C2 C3A H11A 109.5 . . ? C2 C3B H9B 109.5 . . ? C2 C3B H10B 109.5 . . ? H9B C3B H10B 109.5 . . ? C2 C3B H11B 109.5 . . ? H9B C3B H11B 109.5 . . ? H10B C3B H11B 109.5 . . ? O2 C4 N2 123.9(5) . . ? O2 C4 C5 114.9(5) . . ? N2 C4 C5 121.2(5) . . ? C6 C5 C4 111.9(5) . . ? C6 C5 H12 109.2 . . ? C4 C5 H12 109.2 . . ? C6 C5 H13 109.2 . . ? C4 C5 H13 109.2 . . ? H12 C5 H13 107.9 . . ? C5 C6 H14 109.5 . . ? C5 C6 H15 109.5 . . ? H14 C6 H15 109.5 . . ? C5 C6 H16 109.5 . . ? H14 C6 H16 109.5 . . ? H15 C6 H16 109.5 . . ? N3 C7 O3 122.4(4) . . ? N3 C7 C8 122.3(4) . . ? O3 C7 C8 115.3(4) . . ? C9B C8 C7 116.7(14) . . ? C7 C8 C9A 110.7(5) . . ? C7 C8 H17A 109.5 . . ? C9A C8 H17A 109.5 . . ? C7 C8 H18A 109.5 . . ? C9A C8 H18A 109.5 . . ? H17A C8 H18A 108.1 . . ? C9B C8 H17B 108.1 . . ? C7 C8 H17B 108.1 . . ? C9B C8 H18B 108.1 . . ? C7 C8 H18B 108.1 . . ? H17B C8 H18B 107.3 . . ? C8 C9A H19A 109.5 . . ? C8 C9A H20A 109.5 . . ? C8 C9A H21A 109.5 . . ? C8 C9B H19B 109.5 . . ? C8 C9B H20B 109.5 . . ? H19B C9B H20B 109.5 . . ? C8 C9B H21B 109.5 . . ? H19B C9B H21B 109.5 . . ? H20B C9B H21B 109.5 . . ? O4 C10 N4 122.3(5) . . ? O4 C10 C11 115.9(5) . . ? N4 C10 C11 121.7(5) . . ? C12B C11 C10 122.1(14) . . ? C12A C11 C10 114.4(6) . . ? C12B C11 H22A 82.3 . . ? C12A C11 H22A 108.7 . . ? C10 C11 H22A 108.7 . . ? C12B C11 H23A 122.0 . . ? C12A C11 H23A 108.7 . . ? C10 C11 H23A 108.7 . . ? H22A C11 H23A 107.6 . . ? C12B C11 H22B 106.8 . . ? C10 C11 H22B 106.8 . . ? C12B C11 H23B 106.8 . . ? C10 C11 H23B 106.8 . . ? H22B C11 H23B 106.7 . . ? C11 C12A H24A 109.5 . . ? C11 C12A H25A 109.5 . . ? C11 C12A H26A 109.5 . . ? C11 C12B H24B 109.5 . . ? C11 C12B H25B 109.5 . . ? H24B C12B H25B 109.5 . . ? C11 C12B H26B 109.5 . . ? H24B C12B H26B 109.5 . . ? H25B C12B H26B 109.5 . . ? N5 C13 O5 122.4(5) . . ? N5 C13 C14 123.3(4) . . ? O5 C13 C14 114.3(4) . . ? C15 C14 C13 116.7(4) . . ? C15 C14 H27 108.1 . . ? C13 C14 H27 108.1 . . ? C15 C14 H28 108.1 . . ? C13 C14 H28 108.1 . . ? H27 C14 H28 107.3 . . ? C14 C15 H29 109.5 . . ? C14 C15 H30 109.5 . . ? H29 C15 H30 109.5 . . ? C14 C15 H31 109.5 . . ? H29 C15 H31 109.5 . . ? H30 C15 H31 109.5 . . ? O6 C16 N6 123.2(5) . . ? O6 C16 C17 116.4(4) . . ? N6 C16 C17 120.4(5) . . ? C16 C17 C18 112.7(5) . . ? C16 C17 H32 109.0 . . ? C18 C17 H32 109.0 . . ? C16 C17 H33 109.0 . . ? C18 C17 H33 109.0 . . ? H32 C17 H33 107.8 . . ? C17 C18 H34 109.5 . . ? C17 C18 H35 109.5 . . ? H34 C18 H35 109.5 . . ? C17 C18 H36 109.5 . . ? H34 C18 H36 109.5 . . ? H35 C18 H36 109.5 . . ? H37 O7 H38 112(7) . . ? H39 O8 H40 101(6) . . ? H41 O9 H42 104(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 Br1 Rh2 -5.95(12) . . . . ? N2 Rh1 Br1 Rh2 84.40(13) . . . . ? O1 Rh1 Br1 Rh2 175.30(10) 2_556 . . . ? O2 Rh1 Br1 Rh2 -96.93(11) 2_556 . . . ? N1 Rh1 Br1 Rh3 -154.44(12) . . . . ? N2 Rh1 Br1 Rh3 -64.09(13) . . . . ? O1 Rh1 Br1 Rh3 26.81(10) 2_556 . . . ? O2 Rh1 Br1 Rh3 114.58(10) 2_556 . . . ? N3 Rh2 Br1 Rh1 -137.61(12) . . . . ? N4 Rh2 Br1 Rh1 131.21(12) . . . . ? O4 Rh2 Br1 Rh1 -48.13(10) 2 . . . ? O3 Rh2 Br1 Rh1 39.85(10) 2 . . . ? N3 Rh2 Br1 Rh3 10.64(13) . . . . ? N4 Rh2 Br1 Rh3 -80.54(12) . . . . ? O4 Rh2 Br1 Rh3 100.12(10) 2 . . . ? O3 Rh2 Br1 Rh3 -171.90(10) 2 . . . ? N6 Rh3 Br1 Rh1 14.16(12) . . . . ? N5 Rh3 Br1 Rh1 -77.04(12) . . . . ? O5 Rh3 Br1 Rh1 104.82(10) 2_666 . . . ? O6 Rh3 Br1 Rh1 -165.45(10) 2_666 . . . ? N6 Rh3 Br1 Rh2 -133.79(12) . . . . ? N5 Rh3 Br1 Rh2 135.01(12) . . . . ? O5 Rh3 Br1 Rh2 -43.13(10) 2_666 . . . ? O6 Rh3 Br1 Rh2 46.60(10) 2_666 . . . ? N2 Rh1 N1 C1 84.2(4) . . . . ? O2 Rh1 N1 C1 -91.5(4) 2_556 . . . ? Rh1 Rh1 N1 C1 -2.2(4) 2_556 . . . ? Br1 Rh1 N1 C1 178.8(4) . . . . ? N1 Rh1 N2 C4 -83.1(4) . . . . ? O1 Rh1 N2 C4 92.4(4) 2_556 . . . ? Rh1 Rh1 N2 C4 3.3(4) 2_556 . . . ? Br1 Rh1 N2 C4 -176.6(4) . . . . ? N4 Rh2 N3 C7 -83.3(4) . . . . ? O4 Rh2 N3 C7 92.0(4) 2 . . . ? Rh2 Rh2 N3 C7 2.6(4) 2 . . . ? Br1 Rh2 N3 C7 -175.7(4) . . . . ? N3 Rh2 N4 C10 86.8(4) . . . . ? O3 Rh2 N4 C10 -88.6(4) 2 . . . ? Rh2 Rh2 N4 C10 -0.1(4) 2 . . . ? Br1 Rh2 N4 C10 178.7(4) . . . . ? N6 Rh3 N5 C13 85.7(4) . . . . ? O6 Rh3 N5 C13 -89.8(4) 2_666 . . . ? Rh3 Rh3 N5 C13 0.1(4) 2_666 . . . ? Br1 Rh3 N5 C13 178.9(4) . . . . ? N5 Rh3 N6 C16 -87.5(4) . . . . ? O5 Rh3 N6 C16 87.9(4) 2_666 . . . ? Rh3 Rh3 N6 C16 -0.7(4) 2_666 . . . ? Br1 Rh3 N6 C16 177.5(4) . . . . ? Rh1 O1 C1 N1 -0.8(6) 2_556 . . . ? Rh1 O1 C1 C2 177.3(3) 2_556 . . . ? Rh1 N1 C1 O1 2.4(7) . . . . ? Rh1 N1 C1 C2 -175.7(3) . . . . ? O1 C1 C2 C3A -32.7(13) . . . . ? N1 C1 C2 C3A 145.5(12) . . . . ? O1 C1 C2 C3B -46.8(13) . . . . ? N1 C1 C2 C3B 131.4(12) . . . . ? Rh1 O2 C4 N2 2.7(7) 2_556 . . . ? Rh1 O2 C4 C5 -176.5(3) 2_556 . . . ? Rh1 N2 C4 O2 -4.5(7) . . . . ? Rh1 N2 C4 C5 174.6(4) . . . . ? O2 C4 C5 C6 -61.2(7) . . . . ? N2 C4 C5 C6 119.6(6) . . . . ? Rh2 N3 C7 O3 -0.3(7) . . . . ? Rh2 N3 C7 C8 179.3(4) . . . . ? Rh2 O3 C7 N3 -2.9(7) 2 . . . ? Rh2 O3 C7 C8 177.4(3) 2 . . . ? N3 C7 C8 C9B 137(3) . . . . ? O3 C7 C8 C9B -44(3) . . . . ? N3 C7 C8 C9A 116.8(8) . . . . ? O3 C7 C8 C9A -63.6(8) . . . . ? Rh2 O4 C10 N4 2.0(6) 2 . . . ? Rh2 O4 C10 C11 -176.0(4) 2 . . . ? Rh2 N4 C10 O4 -1.2(7) . . . . ? Rh2 N4 C10 C11 176.7(4) . . . . ? O4 C10 C11 C12B -7(2) . . . . ? N4 C10 C11 C12B 175(2) . . . . ? O4 C10 C11 C12A -35.9(9) . . . . ? N4 C10 C11 C12A 146.1(7) . . . . ? Rh3 N5 C13 O5 -3.9(7) . . . . ? Rh3 N5 C13 C14 175.8(4) . . . . ? Rh3 O5 C13 N5 6.1(6) 2_666 . . . ? Rh3 O5 C13 C14 -173.6(3) 2_666 . . . ? N5 C13 C14 C15 -8.3(8) . . . . ? O5 C13 C14 C15 171.5(5) . . . . ? Rh3 O6 C16 N6 0.3(6) 2_666 . . . ? Rh3 O6 C16 C17 179.2(3) 2_666 . . . ? Rh3 N6 C16 O6 0.4(7) . . . . ? Rh3 N6 C16 C17 -178.5(4) . . . . ? O6 C16 C17 C18 48.1(6) . . . . ? N6 C16 C17 C18 -133.0(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O3 0.88 2.24 3.056(6) 154.8 2 N2 H2 O7 0.88 2.08 2.918(6) 158.6 . N3 H3 O5 0.88 2.21 3.063(5) 162.6 2_666 N4 H4 O8 0.88 2.15 3.020(6) 167.9 . N5 H5 O9 0.88 2.27 3.131(6) 165.9 . N6 H6 O1 0.88 2.39 3.088(5) 136.5 2_556 O7 H37 O4 0.84(6) 2.05(6) 2.886(5) 176(6) 2 O7 H38 O5 0.72(7) 2.11(7) 2.808(6) 166(8) 2_666 O8 H39 O6 0.82(6) 2.00(6) 2.817(5) 176(6) 2_666 O8 H40 O9 0.87(7) 2.01(7) 2.865(6) 166(6) . O9 H41 O2 0.83(7) 2.05(7) 2.869(6) 173(7) 2_556 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.263 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.161 #===END data_[{Rh2(pram)4}3I2].6H2O_(6.6H2O) _database_code_depnum_ccdc_archive 'CCDC 775022' #TrackingRef 'web_deposit_cif_file_0_MasahiroEbihara_1272351332.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H72 I2 N12 O12 Rh6, 6(H2 O)' _chemical_formula_sum 'C18 H42 I N6 O9 Rh3' _chemical_formula_weight 922.21 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.272(2) _cell_length_b 12.031(2) _cell_length_c 13.355(2) _cell_angle_alpha 114.544(4) _cell_angle_beta 97.115(4) _cell_angle_gamma 109.390(3) _cell_volume 1479.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3485 _cell_measurement_theta_min 3.0312 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Platelet _exptl_crystal_colour Brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.749 _exptl_absorpt_correction_T_min 0.8026 _exptl_absorpt_correction_T_max 0.9488 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 12182 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6747 _reflns_number_gt 5244 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+6.2085P] 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 6747 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.03646(6) 0.06761(6) 0.45317(5) 0.00901(13) Uani 1 1 d . . . Rh2 Rh 0.03620(6) 0.06519(6) 0.10520(4) 0.00904(13) Uani 1 1 d . . . Rh3 Rh 0.38504(6) 0.41705(6) 0.45137(5) 0.00912(13) Uani 1 1 d . . . I1 I 0.11603(5) 0.22639(5) 0.34655(4) 0.00892(11) Uani 1 1 d . . . N1 N -0.0839(7) -0.0948(7) 0.3076(5) 0.0210(16) Uani 1 1 d . . . H1 H -0.0922 -0.0885 0.2440 0.025 Uiso 1 1 calc R . . O1 O -0.1496(6) -0.2284(5) 0.3896(4) 0.0191(13) Uani 1 1 d . . . N2 N 0.1791(7) 0.0064(7) 0.4388(6) 0.0215(16) Uani 1 1 d . . . H2 H 0.2398 0.0402 0.4111 0.026 Uiso 1 1 calc R . . O2 O 0.1100(6) -0.1286(6) 0.5204(5) 0.0239(14) Uani 1 1 d . . . N3 N 0.2128(6) 0.1551(6) 0.0950(5) 0.0147(14) Uani 1 1 d . . . H3 H 0.2778 0.2149 0.1595 0.018 Uiso 1 1 calc R . . O3 O 0.1488(5) 0.0420(5) -0.1015(4) 0.0130(11) Uani 1 1 d . . . N4 N -0.0184(6) 0.1976(6) 0.0854(5) 0.0110(13) Uani 1 1 d . B . H4 H -0.0070 0.2707 0.1479 0.013 Uiso 1 1 calc R . . O4 O -0.0872(5) 0.0795(5) -0.1106(4) 0.0156(12) Uani 1 1 d . . . N5 N 0.3394(6) 0.5506(6) 0.5727(5) 0.0138(14) Uani 1 1 d . . . H5 H 0.2554 0.5297 0.5670 0.017 Uiso 1 1 calc R . . O5 O 0.5514(5) 0.7054(5) 0.6717(4) 0.0140(12) Uani 1 1 d . . . N6 N 0.4207(6) 0.3466(6) 0.5587(5) 0.0122(13) Uani 1 1 d . . . H6 H 0.3561 0.2754 0.5516 0.015 Uiso 1 1 calc R . . O6 O 0.6360(5) 0.4986(5) 0.6541(4) 0.0145(12) Uani 1 1 d . . . C1 C -0.1528(8) -0.2123(8) 0.2993(6) 0.0194(18) Uani 1 1 d . . . C2 C -0.2414(9) -0.3346(8) 0.1836(6) 0.0217(19) Uani 1 1 d . . . H7 H -0.3301 -0.3359 0.1683 0.026 Uiso 1 1 calc R . . H8 H -0.2049 -0.3272 0.1218 0.026 Uiso 1 1 calc R . . C3 C -0.2540(10) -0.4641(8) 0.1800(6) 0.028(2) Uani 1 1 d . . . H9 H -0.2931 -0.4736 0.2391 0.042 Uiso 1 1 calc R . . H10 H -0.1663 -0.4636 0.1948 0.042 Uiso 1 1 calc R . . H11 H -0.3106 -0.5400 0.1036 0.042 Uiso 1 1 calc R . . C4 C 0.1870(9) -0.0819(9) 0.4687(7) 0.023(2) Uani 1 1 d . . . C5 C 0.2862(9) -0.1413(10) 0.4408(7) 0.028(2) Uani 1 1 d . . . H12 H 0.2383 -0.2403 0.3904 0.033 Uiso 1 1 calc R . . H13 H 0.3365 -0.1036 0.3979 0.033 Uiso 1 1 calc R . . C6 C 0.3805(10) -0.1110(12) 0.5481(8) 0.046(3) Uani 1 1 d . . . H14 H 0.3333 -0.1619 0.5831 0.069 Uiso 1 1 calc R . . H15 H 0.4183 -0.0142 0.6030 0.069 Uiso 1 1 calc R . . H16 H 0.4514 -0.1373 0.5281 0.069 Uiso 1 1 calc R . . C7 C 0.2370(8) 0.1291(8) -0.0039(6) 0.0136(17) Uani 1 1 d . A . C8 C 0.3723(8) 0.2038(8) -0.0071(6) 0.0177(18) Uani 1 1 d . . . H17A H 0.4354 0.2506 0.0714 0.021 Uiso 0.41(7) 1 calc PR A 1 H18A H 0.3699 0.2737 -0.0271 0.021 Uiso 0.41(7) 1 calc PR A 1 H17B H 0.4315 0.2687 0.0729 0.021 Uiso 0.59(7) 1 calc PR A 2 H18B H 0.3662 0.2554 -0.0475 0.021 Uiso 0.59(7) 1 calc PR A 2 C9A C 0.424(2) 0.117(2) -0.091(2) 0.031(6) Uiso 0.59(7) 1 d P A 1 H19A H 0.3614 0.0686 -0.1692 0.046 Uiso 0.59(7) 1 calc PR A 1 H20A H 0.4331 0.0516 -0.0688 0.046 Uiso 0.59(7) 1 calc PR A 1 H21A H 0.5097 0.1740 -0.0901 0.046 Uiso 0.59(7) 1 calc PR A 1 C9B C 0.431(3) 0.104(3) -0.070(3) 0.016(6) Uiso 0.41(7) 1 d P A 2 H19B H 0.3793 0.0477 -0.1522 0.024 Uiso 0.41(7) 1 calc PR A 2 H20B H 0.4286 0.0463 -0.0352 0.024 Uiso 0.41(7) 1 calc PR A 2 H21B H 0.5229 0.1551 -0.0632 0.024 Uiso 0.41(7) 1 calc PR A 2 C10 C -0.0702(8) 0.1823(8) -0.0148(6) 0.0160(17) Uani 1 1 d . . . C11A C -0.1139(12) 0.2859(12) -0.0226(9) 0.022(3) Uiso 0.883(18) 1 d P B 1 H22A H -0.2108 0.2510 -0.0376 0.026 Uiso 0.883(18) 1 calc PR B 1 H23A H -0.0727 0.3696 0.0532 0.026 Uiso 0.883(18) 1 calc PR B 1 C12A C -0.0810(12) 0.3206(11) -0.1130(8) 0.033(3) Uiso 0.883(18) 1 d P B 1 H24A H -0.1100 0.2376 -0.1867 0.050 Uiso 0.883(18) 1 calc PR B 1 H25A H 0.0147 0.3723 -0.0908 0.050 Uiso 0.883(18) 1 calc PR B 1 H26A H -0.1258 0.3750 -0.1212 0.050 Uiso 0.883(18) 1 calc PR B 1 C11B C -0.155(8) 0.252(8) -0.024(6) 0.010(16) Uiso 0.117(18) 1 d P B 2 H22B H -0.1121 0.3408 0.0470 0.012 Uiso 0.117(18) 1 calc PR B 2 H23B H -0.2382 0.2014 -0.0147 0.012 Uiso 0.117(18) 1 calc PR B 2 C12B C -0.200(7) 0.283(7) -0.125(5) 0.019(19) Uiso 0.117(18) 1 d P B 2 H24B H -0.1760 0.2334 -0.1928 0.028 Uiso 0.117(18) 1 calc PR B 2 H25B H -0.1554 0.3797 -0.0977 0.028 Uiso 0.117(18) 1 calc PR B 2 H26B H -0.2957 0.2534 -0.1464 0.028 Uiso 0.117(18) 1 calc PR B 2 C13 C 0.4251(8) 0.6646(8) 0.6581(6) 0.0129(16) Uani 1 1 d . . . C14 C 0.3878(7) 0.7614(8) 0.7495(6) 0.0139(16) Uani 1 1 d . . . H27 H 0.4239 0.7681 0.8243 0.017 Uiso 1 1 calc R . . H28 H 0.4325 0.8518 0.7569 0.017 Uiso 1 1 calc R . . C15 C 0.2426(8) 0.7281(8) 0.7306(7) 0.024(2) Uani 1 1 d . . . H29 H 0.1967 0.6401 0.7255 0.036 Uiso 1 1 calc R . . H30 H 0.2056 0.7249 0.6586 0.036 Uiso 1 1 calc R . . H31 H 0.2315 0.7976 0.7955 0.036 Uiso 1 1 calc R . . C16 C 0.5327(8) 0.3986(8) 0.6384(6) 0.0131(16) Uani 1 1 d . . . C17 C 0.5473(8) 0.3407(8) 0.7189(6) 0.0170(17) Uani 1 1 d . . . H32 H 0.4594 0.2742 0.7075 0.020 Uiso 1 1 calc R . . H33 H 0.6041 0.2925 0.6983 0.020 Uiso 1 1 calc R . . C18 C 0.6068(9) 0.4485(9) 0.8457(6) 0.028(2) Uani 1 1 d . . . H34 H 0.5496 0.4947 0.8674 0.042 Uiso 1 1 calc R . . H35 H 0.6945 0.5140 0.8579 0.042 Uiso 1 1 calc R . . H36 H 0.6147 0.4061 0.8934 0.042 Uiso 1 1 calc R . . O7 O 0.3282(6) 0.0283(6) 0.2805(5) 0.0231(14) Uani 1 1 d . . . H37 H 0.376(9) 0.127(10) 0.325(7) 0.035 Uiso 1 1 d . . . H38 H 0.250(10) -0.010(9) 0.226(7) 0.035 Uiso 1 1 d . . . O8 O 0.1120(7) 0.4841(7) 0.2585(5) 0.0248(15) Uani 1 1 d . . . H39 H 0.086(10) 0.495(10) 0.307(8) 0.037 Uiso 1 1 d . . . H40 H 0.184(10) 0.486(10) 0.276(8) 0.037 Uiso 1 1 d . . . O9A O -0.0156(19) 0.4247(16) 0.5510(16) 0.032(5) Uiso 0.59(7) 1 d P . 1 O9B O 0.009(2) 0.409(2) 0.573(2) 0.025(7) Uiso 0.41(7) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0090(3) 0.0091(3) 0.0089(3) 0.0048(2) 0.0036(2) 0.0029(3) Rh2 0.0101(3) 0.0080(3) 0.0065(3) 0.0030(2) 0.0014(2) 0.0022(3) Rh3 0.0079(3) 0.0080(3) 0.0081(3) 0.0026(2) 0.0019(2) 0.0016(3) I1 0.0091(3) 0.0082(2) 0.0066(2) 0.00326(18) 0.00181(18) 0.0012(2) N1 0.026(4) 0.021(4) 0.010(3) 0.008(3) 0.001(3) 0.003(3) O1 0.027(4) 0.009(3) 0.012(2) 0.005(2) 0.001(2) -0.003(3) N2 0.018(4) 0.035(5) 0.038(4) 0.031(4) 0.022(3) 0.020(4) O2 0.021(4) 0.031(4) 0.037(3) 0.025(3) 0.018(3) 0.016(3) N3 0.014(4) 0.016(4) 0.006(3) 0.003(3) 0.000(3) 0.002(3) O3 0.013(3) 0.012(3) 0.013(2) 0.006(2) 0.005(2) 0.003(2) N4 0.017(4) 0.008(3) 0.008(3) 0.003(2) 0.003(2) 0.005(3) O4 0.017(3) 0.011(3) 0.014(2) 0.003(2) 0.000(2) 0.005(3) N5 0.005(3) 0.018(4) 0.013(3) 0.004(3) 0.003(3) 0.005(3) O5 0.012(3) 0.011(3) 0.012(2) 0.000(2) 0.002(2) 0.004(2) N6 0.012(4) 0.008(3) 0.020(3) 0.009(3) 0.005(3) 0.004(3) O6 0.011(3) 0.016(3) 0.014(2) 0.009(2) 0.002(2) 0.002(2) C1 0.013(4) 0.021(5) 0.019(4) 0.007(4) 0.005(3) 0.006(4) C2 0.023(5) 0.020(5) 0.012(4) 0.008(3) -0.003(3) 0.001(4) C3 0.040(6) 0.014(5) 0.014(4) 0.004(3) -0.001(4) 0.002(4) C4 0.021(5) 0.037(6) 0.027(4) 0.022(4) 0.014(4) 0.020(5) C5 0.022(5) 0.034(6) 0.040(5) 0.025(5) 0.014(4) 0.016(5) C6 0.027(6) 0.092(10) 0.049(6) 0.049(7) 0.018(5) 0.038(7) C7 0.013(4) 0.007(4) 0.014(4) 0.003(3) 0.002(3) 0.001(3) C8 0.022(5) 0.011(4) 0.017(4) 0.004(3) 0.007(3) 0.007(4) C10 0.021(5) 0.010(4) 0.013(4) 0.003(3) 0.003(3) 0.006(4) C13 0.017(4) 0.013(4) 0.014(4) 0.008(3) 0.009(3) 0.010(4) C14 0.010(4) 0.014(4) 0.014(4) 0.002(3) 0.004(3) 0.008(3) C15 0.014(5) 0.019(5) 0.029(4) 0.000(4) 0.013(4) 0.007(4) C16 0.010(4) 0.018(4) 0.014(4) 0.009(3) 0.005(3) 0.009(4) C17 0.017(5) 0.015(4) 0.018(4) 0.009(3) 0.004(3) 0.005(4) C18 0.030(6) 0.040(6) 0.014(4) 0.019(4) 0.000(4) 0.009(5) O7 0.016(4) 0.016(3) 0.023(3) 0.004(3) -0.001(2) 0.000(3) O8 0.029(4) 0.028(4) 0.024(3) 0.013(3) 0.012(3) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 1.967(6) . ? Rh1 N2 1.977(7) . ? Rh1 O1 2.025(5) 2_556 ? Rh1 O2 2.030(6) 2_556 ? Rh1 Rh1 2.4381(11) 2_556 ? Rh1 I1 2.8141(8) . ? Rh2 N3 1.978(6) . ? Rh2 N4 1.987(6) . ? Rh2 O4 2.031(5) 2 ? Rh2 O3 2.037(5) 2 ? Rh2 Rh2 2.4376(11) 2 ? Rh2 I1 2.8089(8) . ? Rh3 N6 2.007(6) . ? Rh3 N5 2.016(6) . ? Rh3 O6 2.081(5) 2_666 ? Rh3 O5 2.090(5) 2_666 ? Rh3 Rh3 2.4424(12) 2_666 ? Rh3 I1 2.8423(9) . ? N1 C1 1.317(10) . ? N1 H1 0.8800 . ? O1 C1 1.296(9) . ? N2 C4 1.306(10) . ? N2 H2 0.8800 . ? O2 C4 1.301(9) . ? N3 C7 1.312(8) . ? N3 H3 0.8800 . ? O3 C7 1.280(8) . ? N4 C10 1.302(9) . ? N4 H4 0.8800 . ? O4 C10 1.293(8) . ? N5 C13 1.289(9) . ? N5 H5 0.8800 . ? O5 C13 1.303(9) . ? N6 C16 1.306(9) . ? N6 H6 0.8800 . ? O6 C16 1.284(9) . ? C1 C2 1.517(10) . ? C2 C3 1.496(11) . ? C2 H7 0.9900 . ? C2 H8 0.9900 . ? C3 H9 0.9800 . ? C3 H10 0.9800 . ? C3 H11 0.9800 . ? C4 C5 1.520(11) . ? C5 C6 1.499(12) . ? C5 H12 0.9900 . ? C5 H13 0.9900 . ? C6 H14 0.9800 . ? C6 H15 0.9800 . ? C6 H16 0.9800 . ? C7 C8 1.507(10) . ? C8 C9A 1.51(2) . ? C8 C9B 1.56(3) . ? C8 H17A 0.9900 . ? C8 H18A 0.9900 . ? C8 H17B 0.9900 . ? C8 H18B 0.9900 . ? C9A H19A 0.9800 . ? C9A H20A 0.9800 . ? C9A H21A 0.9800 . ? C9B H19B 0.9800 . ? C9B H20B 0.9800 . ? C9B H21B 0.9800 . ? C10 C11B 1.48(7) . ? C10 C11A 1.521(13) . ? C11A C12A 1.481(13) . ? C11A H22A 0.9900 . ? C11A H23A 0.9900 . ? C12A H24A 0.9800 . ? C12A H25A 0.9800 . ? C12A H26A 0.9800 . ? C11B C12B 1.61(9) . ? C11B H22B 0.9900 . ? C11B H23B 0.9900 . ? C12B H24B 0.9800 . ? C12B H25B 0.9800 . ? C12B H26B 0.9800 . ? C13 C14 1.514(9) . ? C14 C15 1.510(10) . ? C14 H27 0.9900 . ? C14 H28 0.9900 . ? C15 H29 0.9800 . ? C15 H30 0.9800 . ? C15 H31 0.9800 . ? C16 C17 1.524(10) . ? C17 C18 1.521(10) . ? C17 H32 0.9900 . ? C17 H33 0.9900 . ? C18 H34 0.9800 . ? C18 H35 0.9800 . ? C18 H36 0.9800 . ? O7 H37 0.98(9) . ? O7 H38 0.90(9) . ? O8 H39 0.72(9) . ? O8 H40 0.81(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N2 90.8(3) . . ? N1 Rh1 O1 174.8(2) . 2_556 ? N2 Rh1 O1 91.3(3) . 2_556 ? N1 Rh1 O2 91.1(3) . 2_556 ? N2 Rh1 O2 175.3(2) . 2_556 ? O1 Rh1 O2 86.4(2) 2_556 2_556 ? N1 Rh1 Rh1 86.31(19) . 2_556 ? N2 Rh1 Rh1 86.58(18) . 2_556 ? O1 Rh1 Rh1 89.08(14) 2_556 2_556 ? O2 Rh1 Rh1 89.27(15) 2_556 2_556 ? N1 Rh1 I1 93.88(19) . . ? N2 Rh1 I1 94.84(18) . . ? O1 Rh1 I1 90.68(14) 2_556 . ? O2 Rh1 I1 89.29(15) 2_556 . ? Rh1 Rh1 I1 178.56(4) 2_556 . ? N3 Rh2 N4 90.5(3) . . ? N3 Rh2 O4 89.2(2) . 2 ? N4 Rh2 O4 175.2(2) . 2 ? N3 Rh2 O3 174.8(2) . 2 ? N4 Rh2 O3 91.4(2) . 2 ? O4 Rh2 O3 88.5(2) 2 2 ? N3 Rh2 Rh2 87.11(16) . 2 ? N4 Rh2 Rh2 86.42(16) . 2 ? O4 Rh2 Rh2 88.74(13) 2 2 ? O3 Rh2 Rh2 88.15(13) 2 2 ? N3 Rh2 I1 92.80(16) . . ? N4 Rh2 I1 90.41(16) . . ? O4 Rh2 I1 94.44(13) 2 . ? O3 Rh2 I1 92.05(13) 2 . ? Rh2 Rh2 I1 176.82(4) 2 . ? N6 Rh3 N5 89.7(2) . . ? N6 Rh3 O6 175.4(2) . 2_666 ? N5 Rh3 O6 90.2(2) . 2_666 ? N6 Rh3 O5 92.3(2) . 2_666 ? N5 Rh3 O5 174.4(2) . 2_666 ? O6 Rh3 O5 87.4(2) 2_666 2_666 ? N6 Rh3 Rh3 85.10(18) . 2_666 ? N5 Rh3 Rh3 86.63(18) . 2_666 ? O6 Rh3 Rh3 90.27(15) 2_666 2_666 ? O5 Rh3 Rh3 88.38(15) 2_666 2_666 ? N6 Rh3 I1 93.49(18) . . ? N5 Rh3 I1 91.71(18) . . ? O6 Rh3 I1 91.15(15) 2_666 . ? O5 Rh3 I1 93.34(14) 2_666 . ? Rh3 Rh3 I1 177.82(4) 2_666 . ? Rh2 I1 Rh1 111.02(3) . . ? Rh2 I1 Rh3 115.89(2) . . ? Rh1 I1 Rh3 113.02(3) . . ? C1 N1 Rh1 124.1(5) . . ? C1 N1 H1 117.9 . . ? Rh1 N1 H1 117.9 . . ? C1 O1 Rh1 118.8(5) . 2_556 ? C4 N2 Rh1 122.8(5) . . ? C4 N2 H2 118.6 . . ? Rh1 N2 H2 118.6 . . ? C4 O2 Rh1 117.5(5) . 2_556 ? C7 N3 Rh2 122.7(5) . . ? C7 N3 H3 118.7 . . ? Rh2 N3 H3 118.7 . . ? C7 O3 Rh2 119.3(4) . 2 ? C10 N4 Rh2 123.7(5) . . ? C10 N4 H4 118.2 . . ? Rh2 N4 H4 118.2 . . ? C10 O4 Rh2 119.2(5) . 2 ? C13 N5 Rh3 124.4(5) . . ? C13 N5 H5 117.8 . . ? Rh3 N5 H5 117.8 . . ? C13 O5 Rh3 118.5(4) . 2_666 ? C16 N6 Rh3 124.9(5) . . ? C16 N6 H6 117.6 . . ? Rh3 N6 H6 117.6 . . ? C16 O6 Rh3 116.2(5) . 2_666 ? O1 C1 N1 121.6(7) . . ? O1 C1 C2 116.9(7) . . ? N1 C1 C2 121.5(7) . . ? C3 C2 C1 112.3(7) . . ? C3 C2 H7 109.1 . . ? C1 C2 H7 109.1 . . ? C3 C2 H8 109.1 . . ? C1 C2 H8 109.1 . . ? H7 C2 H8 107.9 . . ? C2 C3 H9 109.5 . . ? C2 C3 H10 109.5 . . ? H9 C3 H10 109.5 . . ? C2 C3 H11 109.5 . . ? H9 C3 H11 109.5 . . ? H10 C3 H11 109.5 . . ? O2 C4 N2 123.6(8) . . ? O2 C4 C5 115.2(7) . . ? N2 C4 C5 121.2(7) . . ? C6 C5 C4 111.7(7) . . ? C6 C5 H12 109.3 . . ? C4 C5 H12 109.3 . . ? C6 C5 H13 109.3 . . ? C4 C5 H13 109.3 . . ? H12 C5 H13 107.9 . . ? C5 C6 H14 109.5 . . ? C5 C6 H15 109.5 . . ? H14 C6 H15 109.5 . . ? C5 C6 H16 109.5 . . ? H14 C6 H16 109.5 . . ? H15 C6 H16 109.5 . . ? O3 C7 N3 122.7(7) . . ? O3 C7 C8 116.7(6) . . ? N3 C7 C8 120.6(7) . . ? C7 C8 C9A 115.1(10) . . ? C7 C8 C9B 110.9(12) . . ? C7 C8 H17A 108.5 . . ? C9A C8 H17A 108.5 . . ? C7 C8 H18A 108.5 . . ? C9A C8 H18A 108.5 . . ? H17A C8 H18A 107.5 . . ? C7 C8 H17B 109.5 . . ? C9B C8 H17B 109.5 . . ? C7 C8 H18B 109.5 . . ? C9B C8 H18B 109.5 . . ? H17B C8 H18B 108.0 . . ? C8 C9A H19A 109.5 . . ? C8 C9A H20A 109.5 . . ? C8 C9A H21A 109.5 . . ? C8 C9B H19B 109.5 . . ? C8 C9B H20B 109.5 . . ? H19B C9B H20B 109.5 . . ? C8 C9B H21B 109.5 . . ? H19B C9B H21B 109.5 . . ? H20B C9B H21B 109.5 . . ? O4 C10 N4 122.0(7) . . ? O4 C10 C11B 115(3) . . ? N4 C10 C11B 120(3) . . ? O4 C10 C11A 117.5(7) . . ? N4 C10 C11A 120.5(7) . . ? C12A C11A C10 115.0(8) . . ? C12A C11A H22A 108.5 . . ? C10 C11A H22A 108.5 . . ? C12A C11A H23A 108.5 . . ? C10 C11A H23A 108.5 . . ? H22A C11A H23A 107.5 . . ? C10 C11B C12B 130(5) . . ? C10 C11B H22B 104.8 . . ? C12B C11B H22B 104.8 . . ? C10 C11B H23B 104.8 . . ? C12B C11B H23B 104.8 . . ? H22B C11B H23B 105.8 . . ? C11B C12B H24B 109.5 . . ? C11B C12B H25B 109.5 . . ? H24B C12B H25B 109.5 . . ? C11B C12B H26B 109.5 . . ? H24B C12B H26B 109.5 . . ? H25B C12B H26B 109.5 . . ? N5 C13 O5 122.0(6) . . ? N5 C13 C14 123.2(7) . . ? O5 C13 C14 114.8(6) . . ? C15 C14 C13 117.3(6) . . ? C15 C14 H27 108.0 . . ? C13 C14 H27 108.0 . . ? C15 C14 H28 108.0 . . ? C13 C14 H28 108.0 . . ? H27 C14 H28 107.2 . . ? C14 C15 H29 109.5 . . ? C14 C15 H30 109.5 . . ? H29 C15 H30 109.5 . . ? C14 C15 H31 109.5 . . ? H29 C15 H31 109.5 . . ? H30 C15 H31 109.5 . . ? O6 C16 N6 123.5(7) . . ? O6 C16 C17 115.9(7) . . ? N6 C16 C17 120.6(7) . . ? C18 C17 C16 112.8(7) . . ? C18 C17 H32 109.0 . . ? C16 C17 H32 109.0 . . ? C18 C17 H33 109.0 . . ? C16 C17 H33 109.0 . . ? H32 C17 H33 107.8 . . ? C17 C18 H34 109.5 . . ? C17 C18 H35 109.5 . . ? H34 C18 H35 109.5 . . ? C17 C18 H36 109.5 . . ? H34 C18 H36 109.5 . . ? H35 C18 H36 109.5 . . ? H37 O7 H38 120(8) . . ? H39 O8 H40 109(10) . . ? 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 N3 Rh2 I1 Rh1 -132.07(19) . . . . ? N4 Rh2 I1 Rh1 137.40(18) . . . . ? O4 Rh2 I1 Rh1 -42.68(15) 2 . . . ? O3 Rh2 I1 Rh1 45.97(15) 2 . . . ? N3 Rh2 I1 Rh3 -1.36(19) . . . . ? N4 Rh2 I1 Rh3 -91.89(18) . . . . ? O4 Rh2 I1 Rh3 88.03(15) 2 . . . ? O3 Rh2 I1 Rh3 176.68(15) 2 . . . ? N1 Rh1 I1 Rh2 -13.0(2) . . . . ? N2 Rh1 I1 Rh2 78.1(2) . . . . ? O1 Rh1 I1 Rh2 169.47(17) 2_556 . . . ? O2 Rh1 I1 Rh2 -104.10(17) 2_556 . . . ? N1 Rh1 I1 Rh3 -145.2(2) . . . . ? N2 Rh1 I1 Rh3 -54.1(2) . . . . ? O1 Rh1 I1 Rh3 37.28(17) 2_556 . . . ? O2 Rh1 I1 Rh3 123.72(17) 2_556 . . . ? N6 Rh3 I1 Rh2 -124.17(16) . . . . ? N5 Rh3 I1 Rh2 146.01(17) . . . . ? O6 Rh3 I1 Rh2 55.77(14) 2_666 . . . ? O5 Rh3 I1 Rh2 -31.66(14) 2_666 . . . ? N6 Rh3 I1 Rh1 5.58(16) . . . . ? N5 Rh3 I1 Rh1 -84.24(17) . . . . ? O6 Rh3 I1 Rh1 -174.48(14) 2_666 . . . ? O5 Rh3 I1 Rh1 98.09(14) 2_666 . . . ? N2 Rh1 N1 C1 83.2(7) . . . . ? O2 Rh1 N1 C1 -92.5(7) 2_556 . . . ? Rh1 Rh1 N1 C1 -3.3(7) 2_556 . . . ? I1 Rh1 N1 C1 178.1(7) . . . . ? N1 Rh1 N2 C4 -81.1(7) . . . . ? O1 Rh1 N2 C4 94.1(7) 2_556 . . . ? Rh1 Rh1 N2 C4 5.1(7) 2_556 . . . ? I1 Rh1 N2 C4 -175.1(7) . . . . ? N4 Rh2 N3 C7 -83.8(6) . . . . ? O4 Rh2 N3 C7 91.3(6) 2 . . . ? Rh2 Rh2 N3 C7 2.6(6) 2 . . . ? I1 Rh2 N3 C7 -174.3(6) . . . . ? N3 Rh2 N4 C10 88.0(6) . . . . ? O3 Rh2 N4 C10 -87.2(6) 2 . . . ? Rh2 Rh2 N4 C10 0.9(6) 2 . . . ? I1 Rh2 N4 C10 -179.2(6) . . . . ? N6 Rh3 N5 C13 81.9(6) . . . . ? O6 Rh3 N5 C13 -93.4(6) 2_666 . . . ? Rh3 Rh3 N5 C13 -3.2(6) 2_666 . . . ? I1 Rh3 N5 C13 175.4(6) . . . . ? N5 Rh3 N6 C16 -85.0(6) . . . . ? O5 Rh3 N6 C16 89.8(6) 2_666 . . . ? Rh3 Rh3 N6 C16 1.6(6) 2_666 . . . ? I1 Rh3 N6 C16 -176.7(6) . . . . ? Rh1 O1 C1 N1 0.5(10) 2_556 . . . ? Rh1 O1 C1 C2 -178.6(5) 2_556 . . . ? Rh1 N1 C1 O1 2.5(11) . . . . ? Rh1 N1 C1 C2 -178.5(6) . . . . ? O1 C1 C2 C3 -30.5(11) . . . . ? N1 C1 C2 C3 150.5(8) . . . . ? Rh1 O2 C4 N2 3.7(11) 2_556 . . . ? Rh1 O2 C4 C5 -174.3(6) 2_556 . . . ? Rh1 N2 C4 O2 -6.7(12) . . . . ? Rh1 N2 C4 C5 171.2(6) . . . . ? O2 C4 C5 C6 -62.1(11) . . . . ? N2 C4 C5 C6 119.8(10) . . . . ? Rh2 O3 C7 N3 -1.6(10) 2 . . . ? Rh2 O3 C7 C8 179.3(5) 2 . . . ? Rh2 N3 C7 O3 -1.2(11) . . . . ? Rh2 N3 C7 C8 177.9(5) . . . . ? O3 C7 C8 C9A -44.9(16) . . . . ? N3 C7 C8 C9A 136.0(15) . . . . ? O3 C7 C8 C9B -59.8(16) . . . . ? N3 C7 C8 C9B 121.1(16) . . . . ? Rh2 O4 C10 N4 1.5(10) 2 . . . ? Rh2 O4 C10 C11B -157(3) 2 . . . ? Rh2 O4 C10 C11A -178.0(7) 2 . . . ? Rh2 N4 C10 O4 -1.7(11) . . . . ? Rh2 N4 C10 C11B 156(4) . . . . ? Rh2 N4 C10 C11A 177.8(7) . . . . ? O4 C10 C11A C12A -42.1(13) . . . . ? N4 C10 C11A C12A 138.3(9) . . . . ? C11B C10 C11A C12A -129(9) . . . . ? O4 C10 C11B C12B -38(8) . . . . ? N4 C10 C11B C12B 162(6) . . . . ? C11A C10 C11B C12B 64(8) . . . . ? Rh3 N5 C13 O5 1.9(10) . . . . ? Rh3 N5 C13 C14 -178.6(5) . . . . ? Rh3 O5 C13 N5 1.2(9) 2_666 . . . ? Rh3 O5 C13 C14 -178.4(5) 2_666 . . . ? N5 C13 C14 C15 -7.0(11) . . . . ? O5 C13 C14 C15 172.6(7) . . . . ? Rh3 O6 C16 N6 2.6(9) 2_666 . . . ? Rh3 O6 C16 C17 -177.8(5) 2_666 . . . ? Rh3 N6 C16 O6 -3.1(10) . . . . ? Rh3 N6 C16 C17 177.3(5) . . . . ? O6 C16 C17 C18 50.2(9) . . . . ? N6 C16 C17 C18 -130.2(8) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O9A O9A 2.65(5) 2_566 ? O9A O2 3.02(2) 2_556 ? O9B O2 2.80(2) 2_556 ? O9B O9A 3.07(6) 2_566 ? O9B O9B 3.52(7) 2_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O3 0.88 2.27 3.126(8) 163.8 2 N2 H2 O7 0.88 2.09 2.901(8) 152.6 . N3 H3 O5 0.88 2.37 3.198(8) 157.1 2_666 N4 H4 O8 0.88 2.15 2.925(9) 145.9 . N6 H6 O1 0.88 2.51 3.208(8) 136.7 2_556 O7 H38 O4 0.90(9) 1.91(10) 2.811(8) 176(9) 2 O7 H37 O5 0.98(9) 1.89(9) 2.777(8) 149(7) 2_666 O8 H39 O9A 0.72(9) 2.13(9) 2.830(13) 165(11) 2_566 O8 H39 O9B 0.72(9) 2.19(9) 2.846(18) 153(11) 2_566 O8 H40 O6 0.81(10) 2.04(10) 2.840(8) 171(9) 2_666 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.985 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.221 #===END