# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Satoshi Takamizawa' 'Takamasa Akatsuka' M.Kohbara 'Ryosuke Miyake' _publ_contact_author_name 'Satoshi Takamizawa' _publ_contact_author_address ; Yokohama City University Yokohama 236-0027 JAPAN ; _publ_contact_author_email STAKA@YOKOHAMA-CU.AC.JP _publ_section_title ; Gas-Adsorbing Ability of tris-Ethylenediamine Metal Complexes (M = Cr(III), Rh (III), Ir(III)) as Transformable Ionic-Single Crystal Hosts ; # Attachment 'B806467A_cif.txt' data_51030a1 _database_code_depnum_ccdc_archive 'CCDC 697678' # Validation Reply Form _vrf_PLAT306_ALERT_2_A ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O2S RESPONSE: Hydrogens of waters not located. PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O3S RESPONSE: Hydrogens of waters not located. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H24 Cr N6, 3Cl, 3.72(H2 O)' _chemical_formula_sum 'C6 H31.44 Cl3 Cr N6 O3.72' _chemical_formula_weight 405.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P -3 c 1' _symmetry\space\group\name\Hall '-P 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 11.4609(3) _cell_length_b 11.4609(3) _cell_length_c 15.4443(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1756.86(12) _cell_formula_units_Z 4 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.126 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7288 _exptl_absorpt_correction_T_max 0.8230 _exptl_absorpt_process_details ; 'SADABS; Sheldrick 1996' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12196 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1467 _reflns_number_gt 1347 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0708P)^2^+1.5619P] 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 1467 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _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 C1 C 0.3812(3) 0.2113(3) 0.07543(14) 0.0286(5) Uani 1 1 d . . . H1A H 0.2974 0.1290 0.0578 0.027(7) Uiso 1 1 calc R . . H1B H 0.3809 0.2903 0.0497 0.035(8) Uiso 1 1 calc R . . C2 C 0.3885(3) 0.2231(3) 0.17311(14) 0.0290(5) Uani 1 1 d . . . H2A H 0.3146 0.2358 0.1954 0.041(9) Uiso 1 1 calc R . . H2B H 0.3802 0.1405 0.1993 0.038(8) Uiso 1 1 calc R . . Cl1 Cl 0.49205(6) 0.10140(6) 0.37658(3) 0.0286(2) Uani 1 1 d . . . N1 N 0.5010(2) 0.2046(2) 0.04467(12) 0.0253(4) Uani 1 1 d . . . H1C H 0.5175 0.2297 -0.0126 0.039(9) Uiso 1 1 calc R . . H1D H 0.4851 0.1178 0.0494 0.032(8) Uiso 1 1 calc R . . N2 N 0.5211(2) 0.3415(2) 0.19484(12) 0.0265(4) Uani 1 1 d . . . H2C H 0.5397 0.3400 0.2526 0.033(8) Uiso 1 1 calc R . . H2D H 0.5200 0.4199 0.1838 0.029(8) Uiso 1 1 calc R . . O1S O 0.1063(3) 0.2171(4) 0.12549(19) 0.0688(14) Uani 0.907(12) 1 d P . . O2S O 0.0000 0.0000 0.0000 0.176(7) Uani 1 6 d S . . O3S O 0.0000 0.0000 0.2500 0.142(5) Uani 1 6 d S . . Cr1 Cr 0.6667 0.3333 0.11945(3) 0.0212(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 C1 0.0304(12) 0.0422(14) 0.0144(10) -0.0024(9) -0.0010(9) 0.0191(11) C2 0.0327(12) 0.0405(13) 0.0130(10) -0.0008(9) 0.0027(9) 0.0177(11) Cl1 0.0421(4) 0.0289(3) 0.0118(3) -0.00140(18) 0.0011(2) 0.0155(3) N1 0.0328(11) 0.0332(11) 0.0102(8) -0.0009(7) -0.0001(7) 0.0167(9) N2 0.0348(11) 0.0355(11) 0.0102(8) -0.0024(7) 0.0002(7) 0.0183(9) O1S 0.070(2) 0.110(3) 0.052(2) 0.0091(18) 0.0011(15) 0.064(2) O2S 0.256(11) 0.256(11) 0.016(3) 0.000 0.000 0.128(5) O3S 0.203(8) 0.203(8) 0.020(3) 0.000 0.000 0.102(4) Cr1 0.0284(3) 0.0284(3) 0.0067(3) 0.000 0.000 0.01420(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.491(3) . ? C1 C2 1.513(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.483(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 Cr1 2.077(2) . ? N1 H1C 0.9200 . ? N1 H1D 0.9200 . ? N2 Cr1 2.075(2) . ? N2 H2C 0.9200 . ? N2 H2D 0.9200 . ? Cr1 N2 2.075(2) 2_655 ? Cr1 N2 2.075(2) 3_665 ? Cr1 N1 2.077(2) 2_655 ? Cr1 N1 2.077(2) 3_665 ? 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 C1 C2 108.13(19) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 107.0(2) . . ? N2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? C1 N1 Cr1 108.93(14) . . ? C1 N1 H1C 109.9 . . ? Cr1 N1 H1C 109.9 . . ? C1 N1 H1D 109.9 . . ? Cr1 N1 H1D 109.9 . . ? H1C N1 H1D 108.3 . . ? C2 N2 Cr1 108.09(14) . . ? C2 N2 H2C 110.1 . . ? Cr1 N2 H2C 110.1 . . ? C2 N2 H2D 110.1 . . ? Cr1 N2 H2D 110.1 . . ? H2C N2 H2D 108.4 . . ? N2 Cr1 N2 91.59(8) 2_655 3_665 ? N2 Cr1 N2 91.59(8) 2_655 . ? N2 Cr1 N2 91.59(8) 3_665 . ? N2 Cr1 N1 82.76(8) 2_655 2_655 ? N2 Cr1 N1 94.10(8) 3_665 2_655 ? N2 Cr1 N1 172.08(8) . 2_655 ? N2 Cr1 N1 94.10(8) 2_655 . ? N2 Cr1 N1 172.08(8) 3_665 . ? N2 Cr1 N1 82.76(8) . . ? N1 Cr1 N1 92.08(7) 2_655 . ? N2 Cr1 N1 172.08(8) 2_655 3_665 ? N2 Cr1 N1 82.76(8) 3_665 3_665 ? N2 Cr1 N1 94.10(8) . 3_665 ? N1 Cr1 N1 92.08(7) 2_655 3_665 ? N1 Cr1 N1 92.08(7) . 3_665 ? 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 C1 C2 N2 55.1(3) . . . . ? C2 C1 N1 Cr1 -37.9(2) . . . . ? C1 C2 N2 Cr1 -44.8(2) . . . . ? C2 N2 Cr1 N2 -74.78(19) . . . 2_655 ? C2 N2 Cr1 N2 -166.41(15) . . . 3_665 ? C2 N2 Cr1 N1 -30.5(6) . . . 2_655 ? C2 N2 Cr1 N1 19.15(15) . . . . ? C2 N2 Cr1 N1 110.73(16) . . . 3_665 ? C1 N1 Cr1 N2 101.62(16) . . . 2_655 ? C1 N1 Cr1 N2 -34.2(6) . . . 3_665 ? C1 N1 Cr1 N2 10.54(16) . . . . ? C1 N1 Cr1 N1 -175.49(16) . . . 2_655 ? C1 N1 Cr1 N1 -83.33(19) . . . 3_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.585 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.218 #===END data_51108a1 _database_code_depnum_ccdc_archive 'CCDC 697679' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H24 Cl3 Cr N6' _chemical_formula_weight 338.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 10.9745(16) _cell_length_b 10.9745(16) _cell_length_c 15.421(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1608.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6578 _exptl_absorpt_correction_T_max 0.7293 _exptl_absorpt_process_details ; 'SADABS; Sheldrick 1996' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10853 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.25 _reflns_number_total 1340 _reflns_number_gt 1215 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0469P)^2^+0.2209P] 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 1340 _refine_ls_number_parameters 49 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 C1 C 0.37049(15) 0.20801(15) 0.07022(8) 0.0177(3) Uani 1 1 d . . . H1A H 0.2829 0.1232 0.0513 0.021 Uiso 1 1 calc R . . H1B H 0.3739 0.2914 0.0431 0.021 Uiso 1 1 calc R . . C2 C 0.37247(15) 0.22093(15) 0.16810(8) 0.0183(3) Uani 1 1 d . . . H2A H 0.2975 0.2399 0.1874 0.022 Uiso 1 1 calc R . . H2B H 0.3560 0.1323 0.1954 0.022 Uiso 1 1 calc R . . Cl1 Cl 0.48158(4) 0.11026(3) 0.370989(19) 0.01880(12) Uani 1 1 d . . . N1 N 0.49488(12) 0.19751(12) 0.04338(7) 0.0145(2) Uani 1 1 d . . . H1C H 0.5141 0.2209 -0.0143 0.017 Uiso 1 1 calc R . . H1D H 0.4766 0.1067 0.0505 0.017 Uiso 1 1 calc R . . N2 N 0.51257(12) 0.33881(12) 0.19360(7) 0.0166(2) Uani 1 1 d . . . H2C H 0.5287 0.3310 0.2513 0.020 Uiso 1 1 calc R . . H2D H 0.5152 0.4232 0.1856 0.020 Uiso 1 1 calc R . . Cr1 Cr 0.6667 0.3333 0.11849(2) 0.01199(12) 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 C1 0.0177(6) 0.0235(7) 0.0123(6) -0.0013(5) -0.0006(5) 0.0106(6) C2 0.0189(7) 0.0219(7) 0.0127(6) -0.0012(5) 0.0026(5) 0.0091(6) Cl1 0.02417(19) 0.01738(18) 0.01051(18) -0.00055(11) 0.00197(11) 0.00713(14) N1 0.0179(5) 0.0174(5) 0.0081(5) -0.0007(4) 0.0001(4) 0.0088(5) N2 0.0204(6) 0.0201(6) 0.0091(5) -0.0014(4) 0.0003(4) 0.0100(5) Cr1 0.01506(15) 0.01506(15) 0.00584(19) 0.000 0.000 0.00753(7) _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 C1 N1 1.4851(17) . ? C1 C2 1.5153(18) . ? C2 N2 1.4843(18) . ? N1 Cr1 2.0754(11) . ? N2 Cr1 2.0754(12) . ? Cr1 N2 2.0754(12) 2_655 ? Cr1 N2 2.0754(12) 3_665 ? Cr1 N1 2.0754(11) 2_655 ? Cr1 N1 2.0754(11) 3_665 ? 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 C1 C2 108.31(11) . . ? N2 C2 C1 107.80(11) . . ? C1 N1 Cr1 109.20(8) . . ? C2 N2 Cr1 109.32(8) . . ? N2 Cr1 N2 91.87(5) 2_655 3_665 ? N2 Cr1 N2 91.87(5) 2_655 . ? N2 Cr1 N2 91.87(5) 3_665 . ? N2 Cr1 N1 82.62(4) 2_655 2_655 ? N2 Cr1 N1 94.17(5) 3_665 2_655 ? N2 Cr1 N1 171.94(4) . 2_655 ? N2 Cr1 N1 94.17(5) 2_655 . ? N2 Cr1 N1 171.94(4) 3_665 . ? N2 Cr1 N1 82.62(4) . . ? N1 Cr1 N1 91.88(4) 2_655 . ? N2 Cr1 N1 171.94(4) 2_655 3_665 ? N2 Cr1 N1 82.62(4) 3_665 3_665 ? N2 Cr1 N1 94.17(5) . 3_665 ? N1 Cr1 N1 91.88(4) 2_655 3_665 ? N1 Cr1 N1 91.88(4) . 3_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.523 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.079 #===END data_60113k1 _database_code_depnum_ccdc_archive 'CCDC 697680' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H24 Cl3 N6 Rh' _chemical_formula_weight 389.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 10.9593(5) _cell_length_b 10.9593(5) _cell_length_c 15.3981(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1601.63(18) _cell_formula_units_Z 4 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.555 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7260 _exptl_absorpt_correction_T_max 0.8600 _exptl_absorpt_process_details ; SADABS; sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10901 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1338 _reflns_number_gt 1263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0340P)^2^+22.6487P] 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 1338 _refine_ls_number_parameters 49 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 1.379 _refine_ls_restrained_S_all 1.379 _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 C1 C 0.3721(8) 0.2079(7) 0.0704(4) 0.0118(13) Uani 1 1 d . . . H1A H 0.2837 0.1227 0.0527 0.014 Uiso 1 1 calc R . . H1B H 0.3759 0.2908 0.0419 0.014 Uiso 1 1 calc R . . C2 C 0.3759(7) 0.2246(8) 0.1678(4) 0.0138(14) Uani 1 1 d . . . H2A H 0.3003 0.2431 0.1867 0.017 Uiso 1 1 calc R . . H2B H 0.3606 0.1371 0.1963 0.017 Uiso 1 1 calc R . . Cl1 Cl 0.47982(19) 0.11339(18) 0.37054(10) 0.0147(4) Uani 1 1 d . . . N1 N 0.4957(6) 0.1950(6) 0.0437(3) 0.0107(11) Uani 1 1 d . . . H1C H 0.5146 0.2165 -0.0143 0.013 Uiso 1 1 calc R . . H1D H 0.4770 0.1042 0.0523 0.013 Uiso 1 1 calc R . . N2 N 0.5143(6) 0.3431(6) 0.1924(4) 0.0125(11) Uani 1 1 d . . . H2C H 0.5308 0.3376 0.2505 0.015 Uiso 1 1 calc R . . H2D H 0.5166 0.4271 0.1828 0.015 Uiso 1 1 calc R . . Rh1 Rh 0.6667 0.3333 0.11805(5) 0.0090(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 C1 0.018(3) 0.008(3) 0.014(3) -0.004(2) -0.001(3) 0.010(3) C2 0.013(3) 0.018(3) 0.009(3) -0.002(2) 0.001(2) 0.007(3) Cl1 0.0202(8) 0.0135(8) 0.0076(7) 0.0000(6) 0.0014(6) 0.0061(7) N1 0.011(3) 0.013(3) 0.005(2) 0.001(2) 0.002(2) 0.004(2) N2 0.015(3) 0.013(3) 0.008(2) -0.001(2) 0.002(2) 0.006(2) Rh1 0.0122(3) 0.0122(3) 0.0024(4) 0.000 0.000 0.00612(15) _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 C1 N1 1.488(8) . ? C1 C2 1.510(9) . ? C2 N2 1.470(9) . ? N1 Rh1 2.069(5) . ? N2 Rh1 2.072(6) . ? Rh1 N1 2.069(5) 2_655 ? Rh1 N1 2.069(5) 3_665 ? Rh1 N2 2.072(6) 3_665 ? Rh1 N2 2.072(6) 2_655 ? 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 C1 C2 108.3(5) . . ? N2 C2 C1 108.5(6) . . ? C1 N1 Rh1 108.2(4) . . ? C2 N2 Rh1 108.3(4) . . ? N1 Rh1 N1 92.3(2) 2_655 . ? N1 Rh1 N1 92.3(2) 2_655 3_665 ? N1 Rh1 N1 92.3(2) . 3_665 ? N1 Rh1 N2 92.2(2) 2_655 3_665 ? N1 Rh1 N2 173.9(2) . 3_665 ? N1 Rh1 N2 83.4(2) 3_665 3_665 ? N1 Rh1 N2 83.4(2) 2_655 2_655 ? N1 Rh1 N2 92.2(2) . 2_655 ? N1 Rh1 N2 173.9(2) 3_665 2_655 ? N2 Rh1 N2 92.4(2) 3_665 2_655 ? N1 Rh1 N2 173.9(2) 2_655 . ? N1 Rh1 N2 83.4(2) . . ? N1 Rh1 N2 92.2(2) 3_665 . ? N2 Rh1 N2 92.4(2) 3_665 . ? N2 Rh1 N2 92.4(2) 2_655 . ? 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 C1 C2 N2 53.9(7) . . . . ? C2 C1 N1 Rh1 -39.4(6) . . . . ? C1 C2 N2 Rh1 -40.8(6) . . . . ? C1 N1 Rh1 N1 -170.7(4) . . . 2_655 ? C1 N1 Rh1 N1 -78.3(5) . . . 3_665 ? C1 N1 Rh1 N2 -33(2) . . . 3_665 ? C1 N1 Rh1 N2 105.8(4) . . . 2_655 ? C1 N1 Rh1 N2 13.6(4) . . . . ? C2 N2 Rh1 N1 -31(2) . . . 2_655 ? C2 N2 Rh1 N1 15.1(4) . . . . ? C2 N2 Rh1 N1 107.2(4) . . . 3_665 ? C2 N2 Rh1 N2 -169.3(4) . . . 3_665 ? C2 N2 Rh1 N2 -76.8(5) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.368 _refine_diff_density_min -2.418 _refine_diff_density_rms 0.201 #===END data_60112k1 _database_code_depnum_ccdc_archive 'CCDC 697681' # Validation Reply Form _vrf_PLAT306_ALERT_2_A ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O2S RESPONSE: Hydrogens of waters not located. PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O3S RESPONSE: Hydrogens of waters not located. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H24 N6 Rh, 3Cl, 3.37(H2 O)' _chemical_formula_sum 'C6 H30.74 Cl3 N6 O3.37 Rh' _chemical_formula_weight 450.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 11.4083(6) _cell_length_b 11.4083(6) _cell_length_c 15.3968(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1735.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7393 _exptl_absorpt_correction_T_max 0.8676 _exptl_absorpt_process_details ; 'SADABS; Sheldrick 1996' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11878 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.31 _reflns_number_total 1456 _reflns_number_gt 1112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0546P)^2^+2.7380P] 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 1456 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 C1 C 0.3820(5) 0.2110(5) 0.0738(3) 0.0318(10) Uani 1 1 d . . . H1A H 0.2972 0.1287 0.0565 0.013(10) Uiso 1 1 calc R . . H1B H 0.3837 0.2904 0.0466 0.030(12) Uiso 1 1 calc R . . C2 C 0.3888(5) 0.2256(5) 0.1719(3) 0.0329(10) Uani 1 1 d . . . H2A H 0.3146 0.2393 0.1932 0.021(11) Uiso 1 1 calc R . . H2B H 0.3799 0.1431 0.1994 0.030(12) Uiso 1 1 calc R . . Cl1 Cl 0.49076(12) 0.10507(11) 0.37547(6) 0.0329(3) Uani 1 1 d . . . N1 N 0.5010(4) 0.2009(4) 0.0449(2) 0.0283(8) Uani 1 1 d . . . H1C H 0.5179 0.2231 -0.0129 0.053(16) Uiso 1 1 calc R . . H1D H 0.4842 0.1138 0.0521 0.044(15) Uiso 1 1 calc R . . N2 N 0.5219(4) 0.3447(4) 0.1935(2) 0.0309(8) Uani 1 1 d . . . H2C H 0.5405 0.3441 0.2516 0.064(17) Uiso 1 1 calc R . . H2D H 0.5214 0.4234 0.1815 0.036(14) Uiso 1 1 calc R . . O1S O 0.0967(8) 0.2095(8) 0.1302(6) 0.124(5) Uani 0.79(2) 1 d P . . O2S O 0.0000 0.0000 0.0000 0.148(7) Uani 1 6 d S . . O3S O 0.0000 0.0000 0.2500 0.213(13) Uani 1 6 d S . . Rh1 Rh 0.6667 0.3333 0.11903(3) 0.02375(18) 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 C1 0.037(2) 0.044(3) 0.0158(18) -0.0028(17) 0.0000(17) 0.021(2) C2 0.034(2) 0.045(3) 0.0169(19) -0.0050(17) 0.0007(17) 0.018(2) Cl1 0.0499(7) 0.0341(6) 0.0106(4) -0.0016(4) 0.0005(4) 0.0179(5) N1 0.035(2) 0.038(2) 0.0110(15) -0.0017(14) -0.0019(14) 0.0175(17) N2 0.041(2) 0.042(2) 0.0106(15) -0.0019(14) 0.0017(14) 0.0216(19) O1S 0.111(7) 0.130(8) 0.168(10) -0.028(6) -0.053(6) 0.088(6) O2S 0.182(12) 0.182(12) 0.080(12) 0.000 0.000 0.091(6) O3S 0.30(2) 0.30(2) 0.040(9) 0.000 0.000 0.149(10) Rh1 0.0325(2) 0.0325(2) 0.0062(2) 0.000 0.000 0.01626(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 C1 N1 1.486(6) . ? C1 C2 1.517(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.483(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 Rh1 2.074(3) . ? N1 H1C 0.9200 . ? N1 H1D 0.9200 . ? N2 Rh1 2.067(3) . ? N2 H2C 0.9200 . ? N2 H2D 0.9200 . ? Rh1 N2 2.067(3) 2_655 ? Rh1 N2 2.067(3) 3_665 ? Rh1 N1 2.074(3) 2_655 ? Rh1 N1 2.074(3) 3_665 ? 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 C1 C2 107.9(3) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 107.3(3) . . ? N2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C1 N1 Rh1 108.3(3) . . ? C1 N1 H1C 110.0 . . ? Rh1 N1 H1C 110.0 . . ? C1 N1 H1D 110.0 . . ? Rh1 N1 H1D 110.0 . . ? H1C N1 H1D 108.4 . . ? C2 N2 Rh1 107.6(2) . . ? C2 N2 H2C 110.2 . . ? Rh1 N2 H2C 110.2 . . ? C2 N2 H2D 110.2 . . ? Rh1 N2 H2D 110.2 . . ? H2C N2 H2D 108.5 . . ? N2 Rh1 N2 92.18(13) 2_655 3_665 ? N2 Rh1 N2 92.18(13) 2_655 . ? N2 Rh1 N2 92.18(13) 3_665 . ? N2 Rh1 N1 83.42(13) 2_655 2_655 ? N2 Rh1 N1 92.06(15) 3_665 2_655 ? N2 Rh1 N1 174.00(14) . 2_655 ? N2 Rh1 N1 92.06(15) 2_655 . ? N2 Rh1 N1 174.00(14) 3_665 . ? N2 Rh1 N1 83.42(13) . . ? N1 Rh1 N1 92.64(13) 2_655 . ? N2 Rh1 N1 174.00(14) 2_655 3_665 ? N2 Rh1 N1 83.42(13) 3_665 3_665 ? N2 Rh1 N1 92.06(14) . 3_665 ? N1 Rh1 N1 92.64(13) 2_655 3_665 ? N1 Rh1 N1 92.64(13) . 3_665 ? 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 C1 C2 N2 55.9(5) . . . . ? C2 C1 N1 Rh1 -39.0(4) . . . . ? C1 C2 N2 Rh1 -44.4(4) . . . . ? C2 N2 Rh1 N2 -73.5(3) . . . 2_655 ? C2 N2 Rh1 N2 -165.8(3) . . . 3_665 ? C2 N2 Rh1 N1 -30.9(14) . . . 2_655 ? C2 N2 Rh1 N1 18.3(3) . . . . ? C2 N2 Rh1 N1 110.7(3) . . . 3_665 ? C1 N1 Rh1 N2 103.6(3) . . . 2_655 ? C1 N1 Rh1 N2 -31.3(14) . . . 3_665 ? C1 N1 Rh1 N2 11.6(3) . . . . ? C1 N1 Rh1 N1 -172.9(3) . . . 2_655 ? C1 N1 Rh1 N1 -80.1(3) . . . 3_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.926 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.140