# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_paper _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- rhodiuminsertion.cif' _publ_contact_author ; Prof Mir Wais Hosseini Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, 4 rue Blaise Pascal, CS 90032 F-67000 Strasbourg, France ; _publ_contact_author_email hosseini@unistra.fr _publ_contact_author_fax '33 3 68 85 13 23' _publ_contact_author_phone '33 3 68 85 13 25' _publ_requested_category FM loop_ _publ_author_name _publ_author_address D.Pogozhev ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, F-67000 Strasbourg, France ; S.A.Baudron ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, F-67000 Strasbourg, France ; M.W.Hosseini ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, F-67000 Strasbourg, France ; _publ_section_title ; From insertion of rhodium acetate paddlewheelss into 7-azaindole hydrogen bonded dimers to infinite architectures ; _publ_contact_author_name 'Prof Mir Wais Hosseini' ###Material relevant to compound 1 at 173K ######## data_compound_1_173 _database_code_depnum_ccdc_archive 'CCDC 815819' #TrackingRef '- rhodiuminsertion.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H9 N3' _chemical_formula_sum 'C14 H9 N3' _chemical_formula_weight 219.24 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4831(15) _cell_length_b 14.485(2) _cell_length_c 7.2366(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.049(4) _cell_angle_gamma 90.00 _cell_volume 1066.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1490 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 24.09 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9130 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0811 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 30.07 _reflns_number_total 3027 _reflns_number_gt 1591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0876P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3027 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1641 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _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 0.29210(18) 0.02370(13) 0.2574(2) 0.0317(4) Uani 1 1 d . . . H1 H 0.2119 -0.0071 0.2261 0.038 Uiso 1 1 calc R . . C2 C 0.32886(18) 0.08533(12) 0.4060(2) 0.0290(4) Uani 1 1 d . . . C3 C 0.45874(18) 0.11571(12) 0.4024(2) 0.0287(4) Uani 1 1 d . . . C4 C 0.49143(18) 0.07002(12) 0.2473(2) 0.0282(4) Uani 1 1 d . . . C5 C 0.55281(19) 0.17695(12) 0.5038(3) 0.0324(5) Uani 1 1 d . . . H5 H 0.5375 0.2107 0.6056 0.039 Uiso 1 1 calc R . . C6 C 0.6691(2) 0.18597(13) 0.4484(3) 0.0350(5) Uani 1 1 d . . . H6 H 0.7342 0.2253 0.5156 0.042 Uiso 1 1 calc R . . C7 C 0.6903(2) 0.13683(13) 0.2928(3) 0.0339(5) Uani 1 1 d . . . H7 H 0.7702 0.1445 0.2603 0.041 Uiso 1 1 calc R . . C8 C 0.24873(18) 0.10982(12) 0.5388(2) 0.0286(4) Uani 1 1 d . . . C9 C 0.30380(19) 0.14111(12) 0.7243(3) 0.0307(4) Uani 1 1 d . . . H9 H 0.3942 0.1501 0.7636 0.037 Uiso 1 1 calc R . . C10 C 0.2263(2) 0.15886(12) 0.8497(3) 0.0329(5) Uani 1 1 d . . . H10 H 0.2646 0.1808 0.9713 0.040 Uiso 1 1 calc R . . C11 C 0.09235(19) 0.14415(12) 0.7952(3) 0.0313(4) Uani 1 1 d . . . C12 C 0.0345(2) 0.11515(14) 0.6088(3) 0.0357(5) Uani 1 1 d . . . H12 H -0.0560 0.1065 0.5698 0.043 Uiso 1 1 calc R . . C13 C 0.11232(19) 0.09957(13) 0.4842(3) 0.0344(5) Uani 1 1 d . . . H13 H 0.0730 0.0817 0.3599 0.041 Uiso 1 1 calc R . . C14 C 0.0098(2) 0.15541(14) 0.9255(3) 0.0367(5) Uani 1 1 d . . . N1 N 0.38856(14) 0.01395(10) 0.1626(2) 0.0316(4) Uani 1 1 d . . . H1A H 0.3855 -0.0213 0.0660 0.038 Uiso 1 1 calc R . . N2 N 0.60176(15) 0.07923(10) 0.1880(2) 0.0307(4) Uani 1 1 d . . . N3 N -0.06040(19) 0.16037(13) 1.0253(3) 0.0501(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0324(12) 0.0312(10) 0.0325(10) -0.0006(8) 0.0100(9) -0.0026(8) C2 0.0329(12) 0.0273(10) 0.0275(9) 0.0016(7) 0.0084(8) 0.0018(8) C3 0.0353(12) 0.0238(9) 0.0274(9) 0.0010(7) 0.0084(8) 0.0029(7) C4 0.0319(11) 0.0245(9) 0.0287(9) 0.0037(7) 0.0085(8) 0.0022(8) C5 0.0390(13) 0.0272(10) 0.0324(10) -0.0027(7) 0.0113(9) -0.0015(8) C6 0.0406(12) 0.0300(10) 0.0351(10) -0.0026(8) 0.0104(9) -0.0040(8) C7 0.0335(12) 0.0328(11) 0.0362(10) 0.0037(8) 0.0098(9) -0.0007(8) C8 0.0344(12) 0.0212(9) 0.0318(9) 0.0032(7) 0.0111(8) 0.0003(7) C9 0.0318(11) 0.0269(10) 0.0339(10) -0.0002(7) 0.0090(8) -0.0013(8) C10 0.0414(13) 0.0262(10) 0.0317(10) -0.0024(8) 0.0099(9) 0.0002(8) C11 0.0345(12) 0.0258(10) 0.0366(10) 0.0023(8) 0.0145(9) 0.0048(8) C12 0.0304(12) 0.0394(12) 0.0379(10) -0.0001(9) 0.0096(9) 0.0019(8) C13 0.0368(13) 0.0357(11) 0.0304(10) -0.0020(8) 0.0074(9) 0.0002(8) C14 0.0382(13) 0.0342(11) 0.0396(11) -0.0004(8) 0.0129(10) 0.0026(9) N1 0.0368(10) 0.0282(8) 0.0308(8) -0.0057(6) 0.0101(7) -0.0018(7) N2 0.0353(10) 0.0270(8) 0.0311(8) 0.0016(6) 0.0103(7) 0.0033(7) N3 0.0476(12) 0.0592(13) 0.0483(11) -0.0011(9) 0.0211(10) 0.0053(9) _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 1.360(2) . ? C1 C2 1.379(2) . ? C1 H1 0.9300 . ? C2 C3 1.437(2) . ? C2 C8 1.466(2) . ? C3 C5 1.395(3) . ? C3 C4 1.415(2) . ? C4 N2 1.334(2) . ? C4 N1 1.370(2) . ? C5 C6 1.379(3) . ? C5 H5 0.9300 . ? C6 C7 1.395(3) . ? C6 H6 0.9300 . ? C7 N2 1.339(2) . ? C7 H7 0.9300 . ? C8 C13 1.396(2) . ? C8 C9 1.401(2) . ? C9 C10 1.381(3) . ? C9 H9 0.9300 . ? C10 C11 1.380(3) . ? C10 H10 0.9300 . ? C11 C12 1.402(3) . ? C11 C14 1.436(3) . ? C12 C13 1.374(2) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 N3 1.152(2) . ? N1 H1A 0.8600 . ? 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 111.06(16) . . ? N1 C1 H1 124.5 . . ? C2 C1 H1 124.5 . . ? C1 C2 C3 105.74(16) . . ? C1 C2 C8 124.90(17) . . ? C3 C2 C8 129.34(16) . . ? C5 C3 C4 115.98(17) . . ? C5 C3 C2 137.51(17) . . ? C4 C3 C2 106.49(16) . . ? N2 C4 N1 124.40(16) . . ? N2 C4 C3 127.16(17) . . ? N1 C4 C3 108.44(16) . . ? C6 C5 C3 118.01(17) . . ? C6 C5 H5 121.0 . . ? C3 C5 H5 121.0 . . ? C5 C6 C7 120.78(18) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? N2 C7 C6 123.44(19) . . ? N2 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? C13 C8 C9 117.48(17) . . ? C13 C8 C2 119.94(16) . . ? C9 C8 C2 122.55(17) . . ? C10 C9 C8 121.22(17) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 120.23(17) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.59(17) . . ? C10 C11 C14 121.91(17) . . ? C12 C11 C14 118.48(17) . . ? C13 C12 C11 119.56(18) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C8 121.83(17) . . ? C12 C13 H13 119.1 . . ? C8 C13 H13 119.1 . . ? N3 C14 C11 176.2(2) . . ? C1 N1 C4 108.28(15) . . ? C1 N1 H1A 125.9 . . ? C4 N1 H1A 125.9 . . ? C4 N2 C7 114.59(16) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.268 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.060 #===END ###Material relevant to compound 2 at 173K ## data_compound_2_173 _database_code_depnum_ccdc_archive 'CCDC 815820' #TrackingRef '- rhodiuminsertion.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H5 N5' _chemical_formula_sum 'C12 H5 N5' _chemical_formula_weight 219.21 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9962(4) _cell_length_b 5.4962(3) _cell_length_c 20.0699(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.713(2) _cell_angle_gamma 90.00 _cell_volume 978.13(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1768 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.50 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9582 _exptl_absorpt_correction_T_max 0.9971 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6991 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.45 _reflns_number_total 2212 _reflns_number_gt 1767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0721P)^2^+0.0121P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2212 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 0.11165(15) 1.1111(3) 0.11756(7) 0.0200(3) Uani 1 1 d . . . H1A H 0.0769 1.1183 0.1586 0.024 Uiso 1 1 calc R . . C2 C 0.21225(15) 0.9372(3) 0.10102(7) 0.0175(3) Uani 1 1 d . . . C3 C 0.23398(15) 0.9948(3) 0.03255(7) 0.0172(3) Uani 1 1 d . . . C4 C 0.31514(15) 0.9028(3) -0.01526(7) 0.0201(3) Uani 1 1 d . . . H4 H 0.3752 0.7649 -0.0064 0.024 Uiso 1 1 calc R . . C5 C 0.30287(17) 1.0240(3) -0.07612(7) 0.0241(4) Uani 1 1 d . . . H5 H 0.3558 0.9674 -0.1090 0.029 Uiso 1 1 calc R . . C6 C 0.21237(16) 1.2301(3) -0.08914(7) 0.0243(4) Uani 1 1 d . . . H6 H 0.2083 1.3076 -0.1306 0.029 Uiso 1 1 calc R . . C7 C 0.14461(15) 1.2018(3) 0.01337(7) 0.0177(3) Uani 1 1 d . . . C8 C 0.27743(15) 0.7400(3) 0.14225(7) 0.0179(3) Uani 1 1 d . . . C9 C 0.25480(15) 0.6734(3) 0.20581(7) 0.0198(3) Uani 1 1 d . . . C10 C 0.37992(15) 0.5808(3) 0.11388(7) 0.0198(3) Uani 1 1 d . . . C11 C 0.32634(16) 0.4609(3) 0.23812(7) 0.0223(3) Uani 1 1 d . . . C12 C 0.15865(16) 0.7998(3) 0.24423(7) 0.0227(3) Uani 1 1 d . . . N1 N 0.07197(13) 1.2661(2) 0.06620(6) 0.0196(3) Uani 1 1 d . . . H1 H 0.0110 1.3866 0.0661 0.023 Uiso 1 1 calc R . . N2 N 0.13073(13) 1.3228(2) -0.04505(6) 0.0212(3) Uani 1 1 d . . . N3 N 0.45910(15) 0.4524(3) 0.09190(7) 0.0289(3) Uani 1 1 d . . . N4 N 0.37939(16) 0.2894(3) 0.26432(7) 0.0325(4) Uani 1 1 d . . . N5 N 0.08283(15) 0.8895(3) 0.27723(7) 0.0305(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0212(7) 0.0218(8) 0.0179(7) -0.0016(6) 0.0055(5) -0.0020(6) C2 0.0171(6) 0.0168(8) 0.0186(7) -0.0013(6) 0.0030(5) -0.0011(6) C3 0.0154(7) 0.0173(8) 0.0187(7) -0.0010(6) 0.0021(5) -0.0016(6) C4 0.0188(7) 0.0211(8) 0.0209(7) -0.0003(6) 0.0048(5) 0.0015(6) C5 0.0242(7) 0.0279(9) 0.0223(8) -0.0005(7) 0.0097(6) 0.0033(7) C6 0.0247(8) 0.0293(10) 0.0199(7) 0.0047(6) 0.0067(6) 0.0027(7) C7 0.0160(6) 0.0188(8) 0.0183(7) -0.0021(6) 0.0029(5) -0.0017(6) C8 0.0162(7) 0.0182(8) 0.0193(7) -0.0032(6) 0.0031(5) -0.0024(6) C9 0.0195(7) 0.0196(8) 0.0204(7) -0.0015(6) 0.0040(5) -0.0009(6) C10 0.0205(7) 0.0208(8) 0.0181(7) 0.0013(6) 0.0033(6) -0.0019(6) C11 0.0236(7) 0.0246(9) 0.0195(7) 0.0002(6) 0.0062(6) -0.0012(7) C12 0.0261(8) 0.0211(8) 0.0216(7) 0.0022(6) 0.0062(6) -0.0023(6) N1 0.0194(6) 0.0193(7) 0.0205(6) -0.0013(5) 0.0049(5) 0.0050(5) N2 0.0206(6) 0.0228(7) 0.0201(6) 0.0018(5) 0.0037(5) 0.0016(5) N3 0.0297(7) 0.0266(8) 0.0320(7) -0.0016(6) 0.0095(6) 0.0034(6) N4 0.0347(8) 0.0321(9) 0.0315(8) 0.0086(7) 0.0076(6) 0.0052(6) N5 0.0386(8) 0.0270(8) 0.0293(7) 0.0000(6) 0.0160(6) 0.0009(6) _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 1.3386(19) . ? C1 C2 1.394(2) . ? C1 H1A 0.9300 . ? C2 C8 1.428(2) . ? C2 C3 1.4551(19) . ? C3 C4 1.3952(18) . ? C3 C7 1.409(2) . ? C4 C5 1.379(2) . ? C4 H4 0.9300 . ? C5 C6 1.394(2) . ? C5 H5 0.9300 . ? C6 N2 1.3421(17) . ? C6 H6 0.9300 . ? C7 N2 1.3352(18) . ? C7 N1 1.3820(16) . ? C8 C9 1.3750(19) . ? C8 C10 1.4549(19) . ? C9 C12 1.4320(19) . ? C9 C11 1.434(2) . ? C10 N3 1.1429(18) . ? C11 N4 1.144(2) . ? C12 N5 1.1399(18) . ? N1 H1 0.8600 . ? 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 110.64(12) . . ? N1 C1 H1A 124.7 . . ? C2 C1 H1A 124.7 . . ? C1 C2 C8 127.00(13) . . ? C1 C2 C3 105.76(12) . . ? C8 C2 C3 127.22(13) . . ? C4 C3 C7 116.46(13) . . ? C4 C3 C2 137.72(14) . . ? C7 C3 C2 105.81(12) . . ? C5 C4 C3 117.44(14) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? C4 C5 C6 121.05(13) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? N2 C6 C5 123.51(13) . . ? N2 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? N2 C7 N1 124.05(14) . . ? N2 C7 C3 127.35(13) . . ? N1 C7 C3 108.59(12) . . ? C9 C8 C2 128.98(13) . . ? C9 C8 C10 113.95(13) . . ? C2 C8 C10 117.06(12) . . ? C8 C9 C12 124.60(14) . . ? C8 C9 C11 120.72(13) . . ? C12 C9 C11 114.67(12) . . ? N3 C10 C8 178.81(16) . . ? N4 C11 C9 177.99(15) . . ? N5 C12 C9 176.13(16) . . ? C1 N1 C7 109.20(12) . . ? C1 N1 H1 125.4 . . ? C7 N1 H1 125.4 . . ? C7 N2 C6 114.17(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.239 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.070 #===END ###Material relevant to compound 10 at 173K ## data_compound_10_173 _database_code_depnum_ccdc_archive 'CCDC 815821' #TrackingRef '- rhodiuminsertion.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 N6 O8 Rh2, 2(C3 H7 N O)' _chemical_formula_sum 'C42 H44 N8 O10 Rh2' _chemical_formula_weight 1026.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1180 0.9190 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0638(2) _cell_length_b 11.2180(3) _cell_length_c 12.0060(3) _cell_angle_alpha 78.2360(10) _cell_angle_beta 84.2670(10) _cell_angle_gamma 85.0210(10) _cell_volume 1055.47(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4101 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.30 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8285 _exptl_absorpt_correction_T_max 0.9274 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13745 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.60 _reflns_number_total 4812 _reflns_number_gt 4216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0532P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4812 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _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 0.3124(4) 0.4408(3) -0.2400(3) 0.0221(7) Uani 1 1 d . . . H1 H 0.3479 0.4487 -0.3172 0.027 Uiso 1 1 calc R . . C2 C 0.3353(4) 0.5251(3) -0.1746(3) 0.0187(7) Uani 1 1 d . . . C3 C 0.2624(4) 0.4751(3) -0.0618(3) 0.0169(6) Uani 1 1 d . . . C4 C 0.2363(4) 0.5092(3) 0.0458(3) 0.0247(7) Uani 1 1 d . . . H4 H 0.2710 0.5827 0.0566 0.030 Uiso 1 1 calc R . . C5 C 0.1576(4) 0.4298(3) 0.1342(3) 0.0255(7) Uani 1 1 d . . . H5 H 0.1384 0.4503 0.2059 0.031 Uiso 1 1 calc R . . C6 C 0.1067(4) 0.3198(3) 0.1180(3) 0.0214(7) Uani 1 1 d . . . H6 H 0.0548 0.2687 0.1801 0.026 Uiso 1 1 calc R . . C7 C 0.2019(3) 0.3619(3) -0.0677(3) 0.0162(6) Uani 1 1 d . . . C8 C 0.4192(4) 0.6380(3) -0.2170(3) 0.0198(7) Uani 1 1 d . . . C9 C 0.4156(4) 0.7281(3) -0.1532(3) 0.0298(8) Uani 1 1 d . . . H9 H 0.3548 0.7183 -0.0823 0.036 Uiso 1 1 calc R . . C10 C 0.5011(5) 0.8331(3) -0.1929(3) 0.0320(9) Uani 1 1 d . . . H10 H 0.4998 0.8914 -0.1476 0.038 Uiso 1 1 calc R . . C11 C 0.5880(4) 0.8509(3) -0.2997(3) 0.0253(7) Uani 1 1 d . . . C12 C 0.5914(4) 0.7625(3) -0.3660(3) 0.0278(8) Uani 1 1 d . . . H12 H 0.6485 0.7740 -0.4382 0.033 Uiso 1 1 calc R . . C13 C 0.5097(4) 0.6578(3) -0.3239(3) 0.0266(8) Uani 1 1 d . . . H13 H 0.5150 0.5982 -0.3681 0.032 Uiso 1 1 calc R . . C14 C 0.6749(5) 0.9599(4) -0.3428(4) 0.0441(7) Uani 1 1 d . . . C15 C 0.1234(4) 0.0187(3) -0.2129(3) 0.0191(6) Uani 1 1 d . . . C16 C 0.1851(4) 0.0334(3) -0.3374(3) 0.0301(8) Uani 1 1 d . . . H16A H 0.2277 -0.0445 -0.3536 0.045 Uiso 1 1 calc R . . H16B H 0.2723 0.0890 -0.3545 0.045 Uiso 1 1 calc R . . H16C H 0.0945 0.0649 -0.3836 0.045 Uiso 1 1 calc R . . C17 C 0.2789(4) -0.1060(3) 0.0784(3) 0.0189(6) Uani 1 1 d . . . C18 C 0.4375(4) -0.1665(3) 0.1245(3) 0.0250(7) Uani 1 1 d . . . H18A H 0.4411 -0.1550 0.2012 0.037 Uiso 1 1 calc R . . H18B H 0.5313 -0.1312 0.0777 0.037 Uiso 1 1 calc R . . H18C H 0.4417 -0.2523 0.1242 0.037 Uiso 1 1 calc R . . N1 N 0.1283(3) 0.2835(2) 0.0176(2) 0.0145(5) Uani 1 1 d . . . N2 N 0.2313(3) 0.3449(2) -0.1771(2) 0.0203(6) Uani 1 1 d . . . H2 H 0.2032 0.2837 -0.2023 0.024 Uiso 1 1 calc R . . N3 N 0.7440(4) 1.0461(3) -0.3788(3) 0.0441(7) Uani 1 1 d . . . O1 O -0.0561(3) 0.0782(2) 0.16613(18) 0.0204(5) Uani 1 1 d . . . O2 O 0.1430(3) 0.10651(19) -0.16346(18) 0.0192(5) Uani 1 1 d . . . O3 O 0.2621(2) 0.00956(19) 0.06153(19) 0.0193(5) Uani 1 1 d . . . O4 O -0.1730(3) 0.17505(19) -0.05895(19) 0.0192(5) Uani 1 1 d . . . Rh1 Rh 0.04642(3) 0.09846(2) 0.002575(19) 0.01466(10) Uani 1 1 d . . . C19 C 0.0253(6) 0.3607(4) 0.5941(3) 0.0434(10) Uani 1 1 d . . . H19 H -0.0011 0.3899 0.6613 0.052 Uiso 1 1 calc R . . C20 C -0.0725(5) 0.2951(4) 0.4341(3) 0.0409(10) Uani 1 1 d . . . H20A H 0.0454 0.2849 0.4143 0.061 Uiso 1 1 calc R . . H20B H -0.1228 0.3538 0.3751 0.061 Uiso 1 1 calc R . . H20C H -0.1213 0.2184 0.4421 0.061 Uiso 1 1 calc R . . C21 C -0.2740(5) 0.3609(4) 0.5839(4) 0.0478(11) Uani 1 1 d . . . H21A H -0.2779 0.3769 0.6597 0.072 Uiso 1 1 calc R . . H21B H -0.3348 0.2907 0.5852 0.072 Uiso 1 1 calc R . . H21C H -0.3235 0.4303 0.5345 0.072 Uiso 1 1 calc R . . N4 N -0.1013(4) 0.3379(3) 0.5418(3) 0.0331(7) Uani 1 1 d . . . O5 O 0.1740(4) 0.3473(3) 0.5633(3) 0.0494(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0280(17) 0.0184(17) 0.0189(16) 0.0000(13) -0.0013(13) -0.0053(13) C2 0.0199(15) 0.0154(16) 0.0214(16) -0.0035(13) -0.0023(13) -0.0035(12) C3 0.0176(14) 0.0122(15) 0.0216(16) -0.0033(13) -0.0033(12) -0.0032(12) C4 0.0348(18) 0.0202(17) 0.0221(17) -0.0089(14) -0.0009(14) -0.0084(14) C5 0.0337(18) 0.0238(18) 0.0209(17) -0.0083(14) 0.0035(14) -0.0096(15) C6 0.0255(16) 0.0159(16) 0.0216(17) -0.0012(13) 0.0028(13) -0.0073(13) C7 0.0156(14) 0.0136(15) 0.0198(16) -0.0034(13) -0.0032(12) -0.0016(12) C8 0.0197(15) 0.0145(16) 0.0250(17) -0.0030(13) -0.0021(13) -0.0026(12) C9 0.038(2) 0.0227(18) 0.0271(19) -0.0055(15) 0.0136(16) -0.0105(16) C10 0.048(2) 0.0194(18) 0.029(2) -0.0080(15) 0.0088(17) -0.0140(16) C11 0.0279(17) 0.0170(17) 0.0290(19) 0.0001(14) 0.0030(15) -0.0085(14) C12 0.0328(18) 0.0265(19) 0.0234(18) -0.0048(15) 0.0061(15) -0.0093(15) C13 0.0354(19) 0.0240(18) 0.0231(18) -0.0102(15) 0.0030(15) -0.0097(15) C14 0.0547(17) 0.0362(15) 0.0414(16) -0.0095(13) 0.0136(13) -0.0196(12) C15 0.0212(15) 0.0172(16) 0.0186(16) -0.0032(13) -0.0004(13) -0.0023(13) C16 0.043(2) 0.0286(19) 0.0197(17) -0.0076(15) 0.0075(15) -0.0113(16) C17 0.0203(15) 0.0194(16) 0.0169(15) -0.0044(13) 0.0029(12) -0.0039(13) C18 0.0214(16) 0.0199(17) 0.0330(19) -0.0034(15) -0.0028(14) -0.0016(13) N1 0.0168(12) 0.0106(12) 0.0165(13) -0.0016(10) -0.0037(10) -0.0029(10) N2 0.0261(14) 0.0148(14) 0.0207(14) -0.0035(11) -0.0018(11) -0.0056(11) N3 0.0547(17) 0.0362(15) 0.0414(16) -0.0095(13) 0.0136(13) -0.0196(12) O1 0.0254(11) 0.0169(11) 0.0196(11) -0.0061(9) 0.0045(9) -0.0069(9) O2 0.0246(11) 0.0146(11) 0.0187(11) -0.0040(9) 0.0035(9) -0.0068(9) O3 0.0183(11) 0.0143(11) 0.0253(12) -0.0022(9) -0.0022(9) -0.0037(9) O4 0.0190(10) 0.0131(11) 0.0263(12) -0.0048(9) -0.0025(9) -0.0033(9) Rh1 0.01631(14) 0.01121(15) 0.01684(15) -0.00372(10) 0.00100(10) -0.00361(10) C19 0.059(3) 0.043(3) 0.034(2) -0.020(2) -0.012(2) 0.008(2) C20 0.045(2) 0.048(3) 0.033(2) -0.013(2) -0.0054(18) -0.005(2) C21 0.050(3) 0.047(3) 0.043(2) -0.007(2) 0.005(2) 0.002(2) N4 0.0401(18) 0.0294(17) 0.0289(17) -0.0054(14) -0.0030(14) 0.0007(14) O5 0.0473(17) 0.056(2) 0.054(2) -0.0332(17) -0.0131(15) 0.0045(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 N2 1.360(4) . ? C1 C2 1.381(4) . ? C1 H1 0.9300 . ? C2 C3 1.443(4) . ? C2 C8 1.462(4) . ? C3 C4 1.411(4) . ? C3 C7 1.417(4) . ? C4 C5 1.379(5) . ? C4 H4 0.9300 . ? C5 C6 1.390(4) . ? C5 H5 0.9300 . ? C6 N1 1.339(4) . ? C6 H6 0.9300 . ? C7 N1 1.333(4) . ? C7 N2 1.359(4) . ? C8 C9 1.385(4) . ? C8 C13 1.398(4) . ? C9 C10 1.391(5) . ? C9 H9 0.9300 . ? C10 C11 1.385(4) . ? C10 H10 0.9300 . ? C11 C12 1.389(5) . ? C11 C14 1.440(5) . ? C12 C13 1.376(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 N3 1.143(5) . ? C15 O1 1.259(4) 2 ? C15 O2 1.278(3) . ? C15 C16 1.509(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O3 1.268(4) . ? C17 O4 1.269(4) 2 ? C17 C18 1.497(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? N1 Rh1 2.279(2) . ? N2 H2 0.8600 . ? O1 C15 1.259(4) 2 ? O1 Rh1 2.029(2) . ? O2 Rh1 2.054(2) . ? O3 Rh1 2.044(2) . ? O4 C17 1.269(4) 2 ? O4 Rh1 2.038(2) . ? Rh1 Rh1 2.4076(4) 2 ? C19 O5 1.225(5) . ? C19 N4 1.320(5) . ? C19 H19 0.9300 . ? C20 N4 1.460(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N4 1.453(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 N2 C1 C2 111.2(3) . . ? N2 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C1 C2 C3 105.1(3) . . ? C1 C2 C8 124.5(3) . . ? C3 C2 C8 130.4(3) . . ? C4 C3 C7 115.8(3) . . ? C4 C3 C2 137.5(3) . . ? C7 C3 C2 106.7(3) . . ? C5 C4 C3 117.7(3) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? N1 C6 C5 123.5(3) . . ? N1 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? N1 C7 N2 124.6(3) . . ? N1 C7 C3 127.0(3) . . ? N2 C7 C3 108.4(3) . . ? C9 C8 C13 117.3(3) . . ? C9 C8 C2 122.0(3) . . ? C13 C8 C2 120.7(3) . . ? C8 C9 C10 121.4(3) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.6(3) . . ? C10 C11 C14 120.7(3) . . ? C12 C11 C14 119.7(3) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C8 122.2(3) . . ? C12 C13 H13 118.9 . . ? C8 C13 H13 118.9 . . ? N3 C14 C11 178.9(4) . . ? O1 C15 O2 125.2(3) 2 . ? O1 C15 C16 117.7(3) 2 . ? O2 C15 C16 117.0(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 O4 125.6(3) . 2 ? O3 C17 C18 117.4(3) . . ? O4 C17 C18 117.0(3) 2 . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 N1 C6 114.9(3) . . ? C7 N1 Rh1 124.71(19) . . ? C6 N1 Rh1 120.3(2) . . ? C7 N2 C1 108.7(3) . . ? C7 N2 H2 125.7 . . ? C1 N2 H2 125.7 . . ? C15 O1 Rh1 119.89(19) 2 . ? C15 O2 Rh1 119.1(2) . . ? C17 O3 Rh1 119.6(2) . . ? C17 O4 Rh1 119.0(2) 2 . ? O1 Rh1 O4 91.64(9) . . ? O1 Rh1 O3 89.07(9) . . ? O4 Rh1 O3 175.69(7) . . ? O1 Rh1 O2 175.62(8) . . ? O4 Rh1 O2 87.98(9) . . ? O3 Rh1 O2 90.99(9) . . ? O1 Rh1 N1 88.59(9) . . ? O4 Rh1 N1 91.84(8) . . ? O3 Rh1 N1 92.43(8) . . ? O2 Rh1 N1 95.78(8) . . ? O1 Rh1 Rh1 88.25(6) . 2 ? O4 Rh1 Rh1 88.32(6) . 2 ? O3 Rh1 Rh1 87.45(6) . 2 ? O2 Rh1 Rh1 87.38(6) . 2 ? N1 Rh1 Rh1 176.84(6) . 2 ? O5 C19 N4 126.7(3) . . ? O5 C19 H19 116.6 . . ? N4 C19 H19 116.6 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 N4 C21 122.3(3) . . ? C19 N4 C20 120.6(3) . . ? C21 N4 C20 117.0(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.836 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.223 #===END ###Material relevant to compound 11 at 173K ## data_compound_11_173 _database_code_depnum_ccdc_archive 'CCDC 815822' #TrackingRef '- rhodiuminsertion.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H22 N10 O8 Rh2, 4(C4 H8 O2)' _chemical_formula_sum 'C48 H54 N10 O16 Rh2' _chemical_formula_weight 1232.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1180 0.9190 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8730(2) _cell_length_b 10.5971(2) _cell_length_c 14.7313(3) _cell_angle_alpha 107.5620(10) _cell_angle_beta 90.5040(10) _cell_angle_gamma 101.4450(10) _cell_volume 1290.84(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8591 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 28.42 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8351 _exptl_absorpt_correction_T_max 0.9381 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28199 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 30.14 _reflns_number_total 7590 _reflns_number_gt 6571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0821P)^2^+1.9884P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7590 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 0.1074(6) 0.0308(4) 0.2023(3) 0.0395(9) Uani 1 1 d . . . H1 H 0.0890 0.0246 0.1387 0.047 Uiso 1 1 calc R . . C2 C 0.1542(5) -0.0686(4) 0.2333(3) 0.0314(7) Uani 1 1 d . . . C3 C 0.1676(4) -0.0165(3) 0.3369(3) 0.0274(6) Uani 1 1 d . . . C4 C 0.2058(4) -0.0594(3) 0.4130(3) 0.0306(7) Uani 1 1 d . . . H4 H 0.2311 -0.1434 0.4028 0.037 Uiso 1 1 calc R . . C5 C 0.2047(4) 0.0274(4) 0.5045(3) 0.0311(7) Uani 1 1 d . . . H5 H 0.2322 0.0028 0.5568 0.037 Uiso 1 1 calc R . . C6 C 0.1625(4) 0.1518(3) 0.5186(2) 0.0269(6) Uani 1 1 d . . . H6 H 0.1622 0.2078 0.5808 0.032 Uiso 1 1 calc R . . C7 C 0.1275(4) 0.1114(3) 0.3605(2) 0.0256(6) Uani 1 1 d . . . C8 C 0.1781(5) -0.1963(4) 0.1756(3) 0.0335(8) Uani 1 1 d . . . C9 C 0.1579(5) -0.2536(4) 0.0782(3) 0.0386(9) Uani 1 1 d . . . C10 C 0.2326(5) -0.2784(4) 0.2254(3) 0.0357(8) Uani 1 1 d . . . C11 C 0.1887(6) -0.3850(5) 0.0326(3) 0.0483(11) Uani 1 1 d . . . C12 C 0.1061(6) -0.1883(5) 0.0156(3) 0.0485(11) Uani 1 1 d . . . C13 C -0.0397(4) 0.4725(3) 0.3171(2) 0.0248(6) Uani 1 1 d . . . C14 C -0.0636(5) 0.4506(4) 0.2127(2) 0.0345(8) Uani 1 1 d . . . H14A H -0.1544 0.3815 0.1870 0.052 Uiso 1 1 calc R . . H14B H 0.0242 0.4227 0.1814 0.052 Uiso 1 1 calc R . . H14C H -0.0759 0.5334 0.2025 0.052 Uiso 1 1 calc R . . C15 C -0.2851(4) 0.3731(3) 0.4993(2) 0.0251(6) Uani 1 1 d . . . C16 C -0.4481(4) 0.3014(4) 0.5037(3) 0.0374(8) Uani 1 1 d . . . H16A H -0.4689 0.2138 0.4563 0.056 Uiso 1 1 calc R . . H16B H -0.5184 0.3537 0.4918 0.056 Uiso 1 1 calc R . . H16C H -0.4609 0.2910 0.5659 0.056 Uiso 1 1 calc R . . N1 N 0.1226(3) 0.1941(3) 0.44723(18) 0.0188(5) Uani 1 1 d . . . N2 N 0.0926(4) 0.1362(3) 0.2770(2) 0.0356(7) Uani 1 1 d . . . H2 H 0.0656 0.2082 0.2733 0.043 Uiso 1 1 calc R . . N3 N 0.2746(6) -0.3430(4) 0.2666(3) 0.0586(7) Uani 1 1 d . . . N4 N 0.0667(6) -0.1362(4) -0.0356(3) 0.0586(7) Uani 1 1 d . . . N5 N 0.2110(6) -0.4900(4) -0.0050(3) 0.0586(7) Uani 1 1 d . . . O1 O 0.0084(3) 0.3794(2) 0.34056(17) 0.0267(5) Uani 1 1 d . . . O2 O 0.0695(3) 0.4221(2) 0.62384(16) 0.0255(5) Uani 1 1 d . . . O3 O 0.2609(3) 0.4996(2) 0.48421(19) 0.0272(5) Uani 1 1 d . . . O4 O -0.1841(3) 0.3011(2) 0.48005(18) 0.0266(5) Uani 1 1 d . . . Rh1 Rh 0.04137(3) 0.39430(2) 0.481074(16) 0.02035(9) Uani 1 1 d . . . C17 C 0.7146(9) 1.0076(7) 0.2449(7) 0.0893(17) Uani 1 1 d . . . H17A H 0.7266 1.0894 0.2988 0.107 Uiso 1 1 calc R . . H17B H 0.7569 1.0327 0.1908 0.107 Uiso 1 1 calc R . . C18 C 0.5618(9) 0.9501(7) 0.2238(7) 0.0893(17) Uani 1 1 d . . . H18A H 0.5105 1.0138 0.2073 0.107 Uiso 1 1 calc R . . H18B H 0.5182 0.9342 0.2805 0.107 Uiso 1 1 calc R . . C19 C 0.6160(8) 0.7346(7) 0.1681(6) 0.082(2) Uani 1 1 d . . . H19A H 0.5728 0.7081 0.2215 0.098 Uiso 1 1 calc R . . H19B H 0.6063 0.6531 0.1141 0.098 Uiso 1 1 calc R . . C20 C 0.7720(10) 0.7936(8) 0.1916(6) 0.095(2) Uani 1 1 d . . . H20A H 0.8185 0.8092 0.1355 0.114 Uiso 1 1 calc R . . H20B H 0.8225 0.7309 0.2101 0.114 Uiso 1 1 calc R . . O5 O 0.7978(5) 0.9183(4) 0.2671(3) 0.0605(9) Uani 1 1 d . . . O6 O 0.5287(5) 0.8212(4) 0.1449(3) 0.0713(11) Uani 1 1 d . . . C21 C 0.5124(8) 0.2927(7) 0.2540(5) 0.0751(17) Uani 1 1 d . . . H21A H 0.5943 0.3348 0.3044 0.090 Uiso 1 1 calc R . . H21B H 0.4534 0.2126 0.2660 0.090 Uiso 1 1 calc R . . C22 C 0.4134(10) 0.3858(8) 0.2557(5) 0.087(2) Uani 1 1 d . . . H22A H 0.4736 0.4685 0.2482 0.104 Uiso 1 1 calc R . . H22B H 0.3687 0.4085 0.3169 0.104 Uiso 1 1 calc R . . C23 C 0.3585(10) 0.2875(11) 0.0917(5) 0.104(3) Uani 1 1 d . . . H23A H 0.4159 0.3681 0.0796 0.125 Uiso 1 1 calc R . . H23B H 0.2778 0.2438 0.0407 0.125 Uiso 1 1 calc R . . C24 C 0.4588(9) 0.1985(9) 0.0901(5) 0.089(2) Uani 1 1 d . . . H24A H 0.5045 0.1782 0.0291 0.106 Uiso 1 1 calc R . . H24B H 0.3997 0.1143 0.0959 0.106 Uiso 1 1 calc R . . O7 O 0.2901(5) 0.3263(5) 0.1792(4) 0.0777(13) Uani 1 1 d . . . O8 O 0.5780(5) 0.2540(5) 0.1646(4) 0.0822(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.069(3) 0.0292(18) 0.0218(16) 0.0010(14) -0.0025(17) 0.0256(18) C2 0.048(2) 0.0235(16) 0.0241(16) 0.0033(13) 0.0008(14) 0.0168(15) C3 0.0349(16) 0.0173(14) 0.0298(16) 0.0049(12) 0.0024(13) 0.0092(12) C4 0.0431(19) 0.0214(15) 0.0325(18) 0.0104(13) 0.0035(15) 0.0154(14) C5 0.0419(18) 0.0282(17) 0.0280(17) 0.0109(14) 0.0014(14) 0.0154(14) C6 0.0326(15) 0.0224(15) 0.0263(16) 0.0056(12) 0.0024(13) 0.0099(12) C7 0.0355(16) 0.0165(13) 0.0259(15) 0.0054(12) 0.0011(13) 0.0102(12) C8 0.045(2) 0.0249(16) 0.0322(18) 0.0053(14) 0.0017(15) 0.0175(15) C9 0.060(2) 0.0289(18) 0.0298(18) 0.0041(15) -0.0013(17) 0.0225(17) C10 0.049(2) 0.0254(16) 0.0322(18) 0.0025(14) 0.0012(16) 0.0168(16) C11 0.076(3) 0.039(2) 0.032(2) 0.0018(17) -0.005(2) 0.030(2) C12 0.080(3) 0.040(2) 0.0271(18) -0.0015(17) -0.002(2) 0.035(2) C13 0.0330(15) 0.0210(14) 0.0205(14) 0.0056(11) 0.0011(12) 0.0073(12) C14 0.054(2) 0.0296(17) 0.0215(15) 0.0056(13) -0.0011(15) 0.0157(16) C15 0.0267(14) 0.0250(15) 0.0237(15) 0.0071(12) -0.0011(12) 0.0064(12) C16 0.0284(16) 0.0340(19) 0.050(2) 0.0155(17) 0.0024(16) 0.0029(14) N1 0.0211(11) 0.0181(11) 0.0174(11) 0.0047(9) 0.0006(9) 0.0060(9) N2 0.063(2) 0.0249(14) 0.0228(14) 0.0052(12) 0.0010(14) 0.0218(15) N3 0.099(2) 0.0433(12) 0.0391(12) 0.0055(10) 0.0001(12) 0.0394(13) N4 0.099(2) 0.0433(12) 0.0391(12) 0.0055(10) 0.0001(12) 0.0394(13) N5 0.099(2) 0.0433(12) 0.0391(12) 0.0055(10) 0.0001(12) 0.0394(13) O1 0.0399(13) 0.0222(11) 0.0194(10) 0.0042(9) 0.0001(9) 0.0136(10) O2 0.0364(12) 0.0218(11) 0.0191(10) 0.0038(9) 0.0009(9) 0.0120(9) O3 0.0252(11) 0.0219(11) 0.0355(13) 0.0092(10) 0.0028(9) 0.0070(9) O4 0.0272(11) 0.0201(10) 0.0321(12) 0.0075(9) 0.0012(9) 0.0054(9) Rh1 0.02659(14) 0.01583(13) 0.01909(14) 0.00385(9) 0.00096(9) 0.00799(9) C17 0.092(3) 0.060(3) 0.111(4) 0.015(3) -0.026(3) 0.026(3) C18 0.092(3) 0.060(3) 0.111(4) 0.015(3) -0.026(3) 0.026(3) C19 0.071(4) 0.048(3) 0.117(6) 0.012(4) -0.004(4) 0.014(3) C20 0.107(6) 0.067(4) 0.096(6) -0.003(4) -0.006(5) 0.027(4) O5 0.077(3) 0.056(2) 0.0464(19) 0.0067(16) -0.0094(18) 0.0246(19) O6 0.057(2) 0.062(2) 0.092(3) 0.027(2) -0.016(2) 0.0023(19) C21 0.084(4) 0.080(4) 0.063(4) 0.017(3) 0.000(3) 0.029(4) C22 0.114(6) 0.084(5) 0.067(4) 0.009(4) 0.004(4) 0.051(5) C23 0.098(6) 0.165(9) 0.063(4) 0.036(5) 0.015(4) 0.058(6) C24 0.082(5) 0.125(7) 0.058(4) 0.014(4) -0.003(3) 0.042(5) O7 0.078(3) 0.092(3) 0.082(3) 0.037(3) 0.018(2) 0.044(3) O8 0.060(2) 0.103(4) 0.081(3) 0.015(3) 0.011(2) 0.031(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 C1 N2 1.339(4) . ? C1 C2 1.397(5) . ? C1 H1 0.9300 . ? C2 C8 1.422(5) . ? C2 C3 1.452(5) . ? C3 C4 1.393(5) . ? C3 C7 1.412(4) . ? C4 C5 1.385(5) . ? C4 H4 0.9300 . ? C5 C6 1.398(5) . ? C5 H5 0.9300 . ? C6 N1 1.331(4) . ? C6 H6 0.9300 . ? C7 N1 1.320(4) . ? C7 N2 1.378(4) . ? C8 C9 1.373(5) . ? C8 C10 1.440(5) . ? C9 C12 1.430(6) . ? C9 C11 1.433(5) . ? C10 N3 1.150(5) . ? C11 N5 1.141(6) . ? C12 N4 1.148(6) . ? C13 O2 1.269(4) 2_566 ? C13 O1 1.282(4) . ? C13 C14 1.491(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O4 1.269(4) . ? C15 O3 1.270(4) 2_566 ? C15 C16 1.506(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 Rh1 2.290(2) . ? N2 H2 0.8600 . ? O1 Rh1 2.042(2) . ? O2 C13 1.269(4) 2_566 ? O2 Rh1 2.040(2) . ? O3 C15 1.270(4) 2_566 ? O3 Rh1 2.036(2) . ? O4 Rh1 2.046(2) . ? Rh1 Rh1 2.4031(4) 2_566 ? C17 C18 1.362(10) . ? C17 O5 1.416(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O6 1.476(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.394(10) . ? C19 O6 1.423(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O5 1.424(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O8 1.422(8) . ? C21 C22 1.440(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O7 1.464(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O7 1.411(8) . ? C23 C24 1.415(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O8 1.419(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? 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 N2 C1 C2 110.5(3) . . ? N2 C1 H1 124.7 . . ? C2 C1 H1 124.7 . . ? C1 C2 C8 127.1(3) . . ? C1 C2 C3 105.6(3) . . ? C8 C2 C3 127.2(3) . . ? C4 C3 C7 116.5(3) . . ? C4 C3 C2 137.5(3) . . ? C7 C3 C2 106.0(3) . . ? C5 C4 C3 117.7(3) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? N1 C6 C5 123.2(3) . . ? N1 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? N1 C7 N2 125.1(3) . . ? N1 C7 C3 126.6(3) . . ? N2 C7 C3 108.3(3) . . ? C9 C8 C2 129.5(4) . . ? C9 C8 C10 114.4(3) . . ? C2 C8 C10 116.1(3) . . ? C8 C9 C12 123.3(3) . . ? C8 C9 C11 121.2(4) . . ? C12 C9 C11 115.5(3) . . ? N3 C10 C8 178.7(4) . . ? N5 C11 C9 178.6(5) . . ? N4 C12 C9 178.8(5) . . ? O2 C13 O1 124.4(3) 2_566 . ? O2 C13 C14 119.4(3) 2_566 . ? O1 C13 C14 116.1(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C15 O3 125.8(3) . 2_566 ? O4 C15 C16 117.2(3) . . ? O3 C15 C16 117.0(3) 2_566 . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C7 N1 C6 115.7(3) . . ? C7 N1 Rh1 124.9(2) . . ? C6 N1 Rh1 119.4(2) . . ? C1 N2 C7 109.4(3) . . ? C1 N2 H2 125.3 . . ? C7 N2 H2 125.3 . . ? C13 O1 Rh1 120.3(2) . . ? C13 O2 Rh1 119.4(2) 2_566 . ? C15 O3 Rh1 119.2(2) 2_566 . ? C15 O4 Rh1 118.9(2) . . ? O3 Rh1 O2 90.07(10) . . ? O3 Rh1 O1 89.74(11) . . ? O2 Rh1 O1 175.90(8) . . ? O3 Rh1 O4 175.98(8) . . ? O2 Rh1 O4 89.88(10) . . ? O1 Rh1 O4 90.02(10) . . ? O3 Rh1 N1 91.46(9) . . ? O2 Rh1 N1 90.63(9) . . ? O1 Rh1 N1 93.46(9) . . ? O4 Rh1 N1 92.55(9) . . ? O3 Rh1 Rh1 88.09(7) . 2_566 ? O2 Rh1 Rh1 88.58(6) . 2_566 ? O1 Rh1 Rh1 87.32(7) . 2_566 ? O4 Rh1 Rh1 87.90(7) . 2_566 ? N1 Rh1 Rh1 179.09(7) . 2_566 ? C18 C17 O5 111.7(6) . . ? C18 C17 H17A 109.3 . . ? O5 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? O5 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C17 C18 O6 114.4(7) . . ? C17 C18 H18A 108.7 . . ? O6 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? O6 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 O6 113.7(6) . . ? C20 C19 H19A 108.8 . . ? O6 C19 H19A 108.8 . . ? C20 C19 H19B 108.8 . . ? O6 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C19 C20 O5 113.0(7) . . ? C19 C20 H20A 109.0 . . ? O5 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? O5 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C17 O5 C20 110.0(6) . . ? C19 O6 C18 107.0(5) . . ? O8 C21 C22 111.5(6) . . ? O8 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? O8 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C21 C22 O7 110.7(6) . . ? C21 C22 H22A 109.5 . . ? O7 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? O7 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? O7 C23 C24 113.2(7) . . ? O7 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? O7 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.8 . . ? C23 C24 O8 112.4(7) . . ? C23 C24 H24A 109.1 . . ? O8 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? O8 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C23 O7 C22 108.1(6) . . ? C24 O8 C21 109.6(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.14 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.008 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.195 #===END ###Material relevant to compound 12 at 173K ## data_compound_12_173 _database_code_depnum_ccdc_archive 'CCDC 815823' #TrackingRef '- rhodiuminsertion.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 N8 O8 Rh2, 4(C4 H8 O2)' _chemical_formula_sum 'C68 H76 N8 O16 Rh2' _chemical_formula_weight 1467.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1180 0.9190 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7968(4) _cell_length_b 36.9943(15) _cell_length_c 10.2665(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.402(2) _cell_angle_gamma 90.00 _cell_volume 3286.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5202 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.41 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8835 _exptl_absorpt_correction_T_max 0.9885 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18888 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7311 _reflns_number_gt 5704 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0152P)^2^+7.7926P] 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 7311 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 0.1410(8) 0.38007(15) 0.2959(7) 0.0592(17) Uani 1 1 d . . . H1 H 0.1426 0.4032 0.3316 0.071 Uiso 1 1 calc R . . C2 C 0.2780(8) 0.35956(16) 0.2940(7) 0.0649(19) Uani 1 1 d . . . H2A H 0.3797 0.3665 0.3253 0.078 Uiso 1 1 calc R . . C3 C 0.2275(7) 0.32788(15) 0.2367(6) 0.0535(16) Uani 1 1 d . . . H3A H 0.2889 0.3084 0.2214 0.064 Uiso 1 1 calc R . . C4 C 0.0640(6) 0.32959(13) 0.2043(5) 0.0404(13) Uani 1 1 d . . . C5 C -0.0372(6) 0.30337(13) 0.1469(5) 0.0395(13) Uani 1 1 d . . . C6 C -0.2005(6) 0.30839(14) 0.1084(5) 0.0402(13) Uani 1 1 d . . . C7 C -0.3159(7) 0.28330(17) 0.0738(6) 0.0552(16) Uani 1 1 d . . . H7 H -0.3023 0.2585 0.0656 0.066 Uiso 1 1 calc R . . C8 C -0.4564(8) 0.3015(2) 0.0531(7) 0.071(2) Uani 1 1 d . . . H8 H -0.5535 0.2911 0.0277 0.085 Uiso 1 1 calc R . . C9 C -0.4265(8) 0.33726(19) 0.0767(6) 0.0622(19) Uani 1 1 d . . . H9 H -0.4996 0.3556 0.0711 0.075 Uiso 1 1 calc R . . C10 C 0.0236(6) 0.26677(13) 0.1217(5) 0.0399(12) Uani 1 1 d . . . C11 C -0.0002(7) 0.25145(13) -0.0033(5) 0.0421(13) Uani 1 1 d . . . H11 H -0.0561 0.2641 -0.0743 0.051 Uiso 1 1 calc R . . C12 C 0.0574(6) 0.21766(13) -0.0245(5) 0.0413(13) Uani 1 1 d . . . H12 H 0.0413 0.2081 -0.1097 0.050 Uiso 1 1 calc R . . C13 C 0.1389(6) 0.19782(12) 0.0796(5) 0.0323(11) Uani 1 1 d . . . C14 C 0.1614(7) 0.21285(14) 0.2045(5) 0.0438(14) Uani 1 1 d . . . H14 H 0.2155 0.1999 0.2757 0.053 Uiso 1 1 calc R . . C15 C 0.1046(7) 0.24700(13) 0.2257(5) 0.0444(14) Uani 1 1 d . . . H15 H 0.1214 0.2566 0.3108 0.053 Uiso 1 1 calc R . . C16 C 0.2515(6) 0.14968(13) -0.0507(5) 0.0385(12) Uani 1 1 d . . . H16 H 0.2518 0.1634 -0.1265 0.046 Uiso 1 1 calc R . . C17 C 0.1988(6) 0.16136(12) 0.0585(5) 0.0312(11) Uani 1 1 d . . . C18 C 0.2224(5) 0.13190(12) 0.1515(5) 0.0286(10) Uani 1 1 d . . . C19 C 0.1949(6) 0.12516(13) 0.2771(5) 0.0381(12) Uani 1 1 d . . . H19 H 0.1481 0.1425 0.3222 0.046 Uiso 1 1 calc R . . C20 C 0.2380(6) 0.09218(13) 0.3347(5) 0.0381(12) Uani 1 1 d . . . H20 H 0.2214 0.0872 0.4197 0.046 Uiso 1 1 calc R . . C21 C 0.3066(5) 0.06642(12) 0.2650(5) 0.0322(11) Uani 1 1 d . . . H21 H 0.3360 0.0445 0.3066 0.039 Uiso 1 1 calc R . . C22 C 0.2895(5) 0.10343(11) 0.0889(5) 0.0272(10) Uani 1 1 d . . . C23 C 0.4409(5) 0.03019(12) -0.2344(5) 0.0280(10) Uani 1 1 d . . . C24 C 0.4056(6) 0.04628(13) -0.3696(5) 0.0362(11) Uani 1 1 d . . . H24A H 0.3569 0.0694 -0.3654 0.054 Uiso 1 1 calc R . . H24B H 0.3375 0.0305 -0.4272 0.054 Uiso 1 1 calc R . . H24C H 0.4998 0.0493 -0.4031 0.054 Uiso 1 1 calc R . . C25 C 0.7677(5) 0.03246(12) 0.0464(5) 0.0282(10) Uani 1 1 d . . . N1 N 0.0135(6) 0.36364(11) 0.2433(5) 0.0464(12) Uani 1 1 d . . . N2 N -0.2728(6) 0.34129(12) 0.1096(4) 0.0474(12) Uani 1 1 d . . . H2 H -0.2262 0.3616 0.1286 0.057 Uiso 1 1 calc R . . N3 N 0.3044(5) 0.11470(10) -0.0334(4) 0.0373(10) Uani 1 1 d . . . H3 H 0.3410 0.1021 -0.0910 0.045 Uiso 1 1 calc R . . N4 N 0.3327(4) 0.07125(9) 0.1425(4) 0.0246(8) Uani 1 1 d . . . O1 O 0.4016(4) 0.04783(8) -0.1399(3) 0.0284(7) Uani 1 1 d . . . O2 O 0.4941(4) 0.00043(8) 0.2242(3) 0.0303(7) Uani 1 1 d . . . O3 O 0.6549(3) 0.04932(8) 0.0788(3) 0.0320(8) Uani 1 1 d . . . O4 O 0.2367(3) -0.00138(8) 0.0047(3) 0.0300(7) Uani 1 1 d . . . Rh1 Rh 0.44259(4) 0.025435(9) 0.04554(4) 0.02320(10) Uani 1 1 d . . . C26 C 0.9205(6) 0.05174(14) 0.0707(6) 0.0463(14) Uani 1 1 d . . . H26A H 0.9088 0.0749 0.1096 0.069 Uiso 1 1 calc R . . H26B H 0.9556 0.0549 -0.0118 0.069 Uiso 1 1 calc R . . H26C H 0.9947 0.0377 0.1297 0.069 Uiso 1 1 calc R . . C27 C 0.4273(9) 0.4381(2) 0.9730(8) 0.089(3) Uani 1 1 d . . . H27A H 0.4150 0.4181 0.9108 0.106 Uiso 1 1 calc R . . H27B H 0.4887 0.4565 0.9395 0.106 Uiso 1 1 calc R . . C28 C 0.2780(9) 0.4528(2) 0.9795(7) 0.081(2) Uani 1 1 d . . . H28A H 0.2318 0.4619 0.8928 0.097 Uiso 1 1 calc R . . H28B H 0.2123 0.4336 1.0021 0.097 Uiso 1 1 calc R . . C29 C 0.3582(9) 0.4686(2) 1.1965(7) 0.076(2) Uani 1 1 d . . . H29A H 0.2952 0.4502 1.2281 0.091 Uiso 1 1 calc R . . H29B H 0.3683 0.4886 1.2587 0.091 Uiso 1 1 calc R . . C30 C 0.5104(8) 0.4538(2) 1.1934(8) 0.081(2) Uani 1 1 d . . . H30A H 0.5774 0.4731 1.1737 0.097 Uiso 1 1 calc R . . H30B H 0.5535 0.4444 1.2805 0.097 Uiso 1 1 calc R . . O5 O 0.5087(5) 0.42567(12) 1.0982(5) 0.0692(13) Uani 1 1 d . . . O6 O 0.2833(6) 0.48077(12) 1.0727(5) 0.0727(14) Uani 1 1 d . . . C31 C 0.1535(17) 0.3568(5) 0.8332(16) 0.184(7) Uani 1 1 d . . . H31A H 0.1645 0.3636 0.9256 0.221 Uiso 1 1 calc R . . H31B H 0.0701 0.3708 0.7826 0.221 Uiso 1 1 calc R . . C32 C 0.122(2) 0.3214(6) 0.8190(19) 0.313(18) Uani 1 1 d . . . H32A H 0.0421 0.3146 0.8683 0.375 Uiso 1 1 calc R . . H32B H 0.2136 0.3071 0.8501 0.375 Uiso 1 1 calc R . . C33 C 0.2039(15) 0.3206(4) 0.6258(12) 0.147(5) Uani 1 1 d . . . H33A H 0.2837 0.3037 0.6643 0.176 Uiso 1 1 calc R . . H33B H 0.1797 0.3166 0.5310 0.176 Uiso 1 1 calc R . . C34 C 0.2524(17) 0.3561(3) 0.6535(12) 0.160(6) Uani 1 1 d . . . H34A H 0.3417 0.3608 0.6127 0.192 Uiso 1 1 calc R . . H34B H 0.1707 0.3724 0.6138 0.192 Uiso 1 1 calc R . . O7 O 0.2908(12) 0.3635(2) 0.7876(12) 0.165(4) Uani 1 1 d . . . O8 O 0.0708(11) 0.3164(3) 0.6830(17) 0.232(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.071(4) 0.031(3) 0.079(5) -0.009(3) 0.024(4) -0.002(3) C2 0.053(4) 0.046(4) 0.097(6) -0.010(4) 0.017(4) 0.004(3) C3 0.050(3) 0.042(3) 0.072(4) -0.005(3) 0.021(3) 0.015(3) C4 0.057(3) 0.026(3) 0.042(3) -0.001(2) 0.018(3) 0.014(2) C5 0.060(3) 0.032(3) 0.029(3) 0.005(2) 0.015(2) 0.018(2) C6 0.056(3) 0.035(3) 0.031(3) 0.001(2) 0.010(2) 0.018(2) C7 0.060(4) 0.050(4) 0.053(4) -0.014(3) 0.004(3) 0.013(3) C8 0.054(4) 0.087(5) 0.070(5) -0.018(4) 0.006(4) 0.012(4) C9 0.067(4) 0.072(5) 0.050(4) 0.001(3) 0.014(3) 0.039(4) C10 0.055(3) 0.027(3) 0.038(3) 0.001(2) 0.010(3) 0.012(2) C11 0.061(3) 0.033(3) 0.029(3) 0.005(2) 0.000(3) 0.018(2) C12 0.057(3) 0.033(3) 0.033(3) -0.002(2) 0.002(3) 0.016(2) C13 0.041(3) 0.025(2) 0.031(3) -0.003(2) 0.007(2) 0.010(2) C14 0.064(4) 0.033(3) 0.030(3) 0.005(2) -0.001(3) 0.020(2) C15 0.068(4) 0.030(3) 0.033(3) -0.006(2) 0.003(3) 0.016(3) C16 0.053(3) 0.031(3) 0.032(3) 0.007(2) 0.010(2) 0.013(2) C17 0.045(3) 0.026(2) 0.023(2) -0.0005(19) 0.004(2) 0.009(2) C18 0.033(2) 0.024(2) 0.029(3) -0.0019(19) 0.007(2) 0.0043(18) C19 0.051(3) 0.033(3) 0.031(3) -0.005(2) 0.011(2) 0.012(2) C20 0.052(3) 0.038(3) 0.027(3) 0.003(2) 0.012(2) 0.013(2) C21 0.040(3) 0.025(2) 0.033(3) 0.002(2) 0.009(2) 0.007(2) C22 0.032(2) 0.023(2) 0.027(2) -0.0029(18) 0.006(2) 0.0017(18) C23 0.026(2) 0.023(2) 0.034(3) 0.0081(19) 0.0015(19) 0.0004(17) C24 0.043(3) 0.034(3) 0.031(3) 0.007(2) 0.005(2) 0.005(2) C25 0.025(2) 0.029(3) 0.031(2) 0.0055(19) 0.0038(19) -0.0013(18) N1 0.060(3) 0.023(2) 0.058(3) -0.002(2) 0.019(3) 0.008(2) N2 0.065(3) 0.040(3) 0.038(3) 0.009(2) 0.013(2) 0.026(2) N3 0.055(3) 0.032(2) 0.028(2) 0.0021(17) 0.017(2) 0.0179(19) N4 0.0257(18) 0.0228(19) 0.0243(19) -0.0017(15) 0.0020(15) 0.0029(15) O1 0.0366(17) 0.0219(16) 0.0276(17) 0.0037(13) 0.0083(14) 0.0086(13) O2 0.0382(18) 0.0236(16) 0.0288(18) 0.0027(13) 0.0053(14) 0.0084(13) O3 0.0262(16) 0.0251(17) 0.045(2) -0.0064(15) 0.0063(15) -0.0054(13) O4 0.0258(16) 0.0261(16) 0.039(2) -0.0035(14) 0.0085(14) -0.0009(13) Rh1 0.02456(17) 0.01821(16) 0.02651(18) 0.00034(15) 0.00373(13) 0.00313(14) C26 0.033(3) 0.043(3) 0.063(4) -0.006(3) 0.009(3) -0.008(2) C27 0.084(6) 0.100(7) 0.084(6) -0.017(5) 0.023(5) 0.016(5) C28 0.080(5) 0.101(6) 0.060(5) 0.002(4) 0.009(4) 0.023(5) C29 0.085(5) 0.079(5) 0.067(5) -0.002(4) 0.026(4) 0.014(4) C30 0.059(4) 0.106(6) 0.077(5) -0.023(5) 0.008(4) 0.022(4) O5 0.063(3) 0.064(3) 0.083(4) -0.009(3) 0.018(3) 0.019(2) O6 0.089(3) 0.067(3) 0.064(3) 0.004(3) 0.019(3) 0.030(3) C31 0.111(11) 0.29(2) 0.164(15) -0.058(15) 0.054(11) 0.019(13) C32 0.30(3) 0.41(3) 0.191(19) 0.20(2) -0.061(17) -0.23(2) C33 0.134(11) 0.161(12) 0.147(11) -0.079(9) 0.028(9) -0.033(9) C34 0.231(16) 0.143(11) 0.098(9) -0.005(8) 0.011(10) -0.081(10) O7 0.161(8) 0.133(7) 0.183(10) -0.023(6) -0.023(8) -0.011(6) O8 0.122(7) 0.194(10) 0.339(17) 0.077(11) -0.072(9) -0.080(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 1.304(7) . ? C1 C2 1.427(8) . ? C1 H1 0.9300 . ? C2 C3 1.350(8) . ? C2 H2A 0.9300 . ? C3 C4 1.418(8) . ? C3 H3A 0.9300 . ? C4 C5 1.375(7) . ? C4 N1 1.417(6) . ? C5 C6 1.432(7) . ? C5 C10 1.495(6) . ? C6 C7 1.374(8) . ? C6 N2 1.374(6) . ? C7 C8 1.389(8) . ? C7 H7 0.9300 . ? C8 C9 1.363(9) . ? C8 H8 0.9300 . ? C9 N2 1.341(8) . ? C9 H9 0.9300 . ? C10 C15 1.382(7) . ? C10 C11 1.383(7) . ? C11 C12 1.381(6) . ? C11 H11 0.9300 . ? C12 C13 1.385(6) . ? C12 H12 0.9300 . ? C13 C14 1.378(7) . ? C13 C17 1.479(6) . ? C14 C15 1.390(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.358(7) . ? C16 N3 1.376(6) . ? C16 H16 0.9300 . ? C17 C18 1.439(6) . ? C18 C19 1.376(7) . ? C18 C22 1.417(6) . ? C19 C20 1.379(6) . ? C19 H19 0.9300 . ? C20 C21 1.393(6) . ? C20 H20 0.9300 . ? C21 N4 1.330(6) . ? C21 H21 0.9300 . ? C22 N4 1.337(5) . ? C22 N3 1.352(6) . ? C23 O2 1.265(5) 3_655 ? C23 O1 1.268(5) . ? C23 C24 1.490(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O4 1.262(5) 3_655 ? C25 O3 1.266(5) . ? C25 C26 1.502(6) . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 Rh1 2.268(3) . ? O1 Rh1 2.048(3) . ? O2 C23 1.265(5) 3_655 ? O2 Rh1 2.031(3) . ? O3 Rh1 2.038(3) . ? O4 C25 1.262(5) 3_655 ? O4 Rh1 2.041(3) . ? Rh1 Rh1 2.4036(7) 3_655 ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O5 1.429(9) . ? C27 C28 1.433(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O6 1.405(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O6 1.396(8) . ? C29 C30 1.453(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O5 1.426(8) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.34(2) . ? C31 O7 1.394(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O8 1.40(2) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.392(13) . ? C33 O8 1.410(15) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O7 1.385(12) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? 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 114.3(5) . . ? N1 C1 H1 122.8 . . ? C2 C1 H1 122.8 . . ? C3 C2 C1 104.8(6) . . ? C3 C2 H2A 127.6 . . ? C1 C2 H2A 127.6 . . ? C2 C3 C4 107.7(5) . . ? C2 C3 H3A 126.2 . . ? C4 C3 H3A 126.2 . . ? C5 C4 N1 122.5(5) . . ? C5 C4 C3 128.3(5) . . ? N1 C4 C3 109.2(5) . . ? C4 C5 C6 124.5(5) . . ? C4 C5 C10 119.3(5) . . ? C6 C5 C10 116.2(5) . . ? C7 C6 N2 106.2(5) . . ? C7 C6 C5 129.9(5) . . ? N2 C6 C5 123.7(5) . . ? C6 C7 C8 108.0(6) . . ? C6 C7 H7 126.0 . . ? C8 C7 H7 126.0 . . ? C9 C8 C7 107.7(6) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? N2 C9 C8 107.8(5) . . ? N2 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? C15 C10 C11 118.1(4) . . ? C15 C10 C5 119.8(5) . . ? C11 C10 C5 122.2(4) . . ? C12 C11 C10 121.3(5) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 120.7(5) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 118.1(4) . . ? C14 C13 C17 120.6(4) . . ? C12 C13 C17 121.2(4) . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C10 C15 C14 120.6(5) . . ? C10 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 N3 110.5(4) . . ? C17 C16 H16 124.7 . . ? N3 C16 H16 124.7 . . ? C16 C17 C18 106.1(4) . . ? C16 C17 C13 126.5(4) . . ? C18 C17 C13 127.3(4) . . ? C19 C18 C22 116.6(4) . . ? C19 C18 C17 136.9(4) . . ? C22 C18 C17 106.5(4) . . ? C18 C19 C20 118.7(4) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C19 C20 C21 119.8(5) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? N4 C21 C20 123.9(4) . . ? N4 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? N4 C22 N3 126.0(4) . . ? N4 C22 C18 125.8(4) . . ? N3 C22 C18 108.1(4) . . ? O2 C23 O1 125.4(4) 3_655 . ? O2 C23 C24 116.8(4) 3_655 . ? O1 C23 C24 117.9(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 O3 126.3(4) 3_655 . ? O4 C25 C26 117.5(4) 3_655 . ? O3 C25 C26 116.3(4) . . ? C1 N1 C4 104.0(5) . . ? C9 N2 C6 110.3(5) . . ? C9 N2 H2 124.9 . . ? C6 N2 H2 124.9 . . ? C22 N3 C16 108.8(4) . . ? C22 N3 H3 125.6 . . ? C16 N3 H3 125.6 . . ? C21 N4 C22 115.1(4) . . ? C21 N4 Rh1 118.3(3) . . ? C22 N4 Rh1 126.6(3) . . ? C23 O1 Rh1 118.5(3) . . ? C23 O2 Rh1 120.5(3) 3_655 . ? C25 O3 Rh1 118.7(3) . . ? C25 O4 Rh1 119.2(3) 3_655 . ? O2 Rh1 O3 89.87(13) . . ? O2 Rh1 O4 90.54(13) . . ? O3 Rh1 O4 175.78(13) . . ? O2 Rh1 O1 175.56(12) . . ? O3 Rh1 O1 88.99(13) . . ? O4 Rh1 O1 90.28(13) . . ? O2 Rh1 N4 89.29(13) . . ? O3 Rh1 N4 93.04(13) . . ? O4 Rh1 N4 91.17(12) . . ? O1 Rh1 N4 95.06(12) . . ? O2 Rh1 Rh1 87.35(9) . 3_655 ? O3 Rh1 Rh1 88.15(9) . 3_655 ? O4 Rh1 Rh1 87.67(9) . 3_655 ? O1 Rh1 Rh1 88.32(8) . 3_655 ? N4 Rh1 Rh1 176.43(10) . 3_655 ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O5 C27 C28 113.2(7) . . ? O5 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? O5 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? O6 C28 C27 113.1(7) . . ? O6 C28 H28A 109.0 . . ? C27 C28 H28A 109.0 . . ? O6 C28 H28B 109.0 . . ? C27 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? O6 C29 C30 112.8(7) . . ? O6 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? O6 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? O5 C30 C29 113.3(6) . . ? O5 C30 H30A 108.9 . . ? C29 C30 H30A 108.9 . . ? O5 C30 H30B 108.9 . . ? C29 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C30 O5 C27 108.9(6) . . ? C29 O6 C28 109.5(5) . . ? C32 C31 O7 108.3(15) . . ? C32 C31 H31A 110.0 . . ? O7 C31 H31A 110.0 . . ? C32 C31 H31B 110.0 . . ? O7 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? C31 C32 O8 105.1(14) . . ? C31 C32 H32A 110.7 . . ? O8 C32 H32A 110.7 . . ? C31 C32 H32B 110.7 . . ? O8 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C34 C33 O8 105.5(11) . . ? C34 C33 H33A 110.6 . . ? O8 C33 H33A 110.6 . . ? C34 C33 H33B 110.6 . . ? O8 C33 H33B 110.6 . . ? H33A C33 H33B 108.8 . . ? O7 C34 C33 113.6(11) . . ? O7 C34 H34A 108.9 . . ? C33 C34 H34A 108.9 . . ? O7 C34 H34B 108.9 . . ? C33 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C34 O7 C31 103.2(11) . . ? C32 O8 C33 105.0(11) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.771 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.112 #===END ###Material relevant to compound 13 at 173K ## data_compound_13_173 _database_code_depnum_ccdc_archive 'CCDC 815824' #TrackingRef '- rhodiuminsertion.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H32 N4 O12 Rh2' _chemical_formula_sum 'C36 H32 N4 O12 Rh2' _chemical_formula_weight 918.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7872(2) _cell_length_b 11.7497(3) _cell_length_c 13.7757(4) _cell_angle_alpha 110.5140(10) _cell_angle_beta 96.1150(10) _cell_angle_gamma 96.0720(10) _cell_volume 1159.85(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6509 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 27.37 _exptl_crystal_description plate _exptl_crystal_colour pink-red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9273 _exptl_absorpt_correction_T_max 0.9555 _exptl_absorpt_process_details sadabs _exptl_special_details ; The squeeze command was apllied owing to the solvent disorder ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18223 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5262 _reflns_number_gt 4437 _reflns_threshold_expression >2sigma(I) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.021 -0.002 0.000 364.5 179.6 _platon_squeeze_details ; ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0590P)^2^+0.1072P] 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 5262 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.5350(4) 0.1735(2) 0.4294(2) 0.0311(6) Uani 1 1 d . . . H1 H 0.6484 0.2008 0.4655 0.037 Uiso 1 1 calc R . . C2 C 0.4737(3) 0.0555(2) 0.3609(2) 0.0282(6) Uani 1 1 d . . . C3 C 0.2943(3) 0.0543(2) 0.3226(2) 0.0266(5) Uani 1 1 d . . . C4 C 0.1563(4) -0.0321(2) 0.2569(2) 0.0318(6) Uani 1 1 d . . . H4 H 0.1712 -0.1131 0.2224 0.038 Uiso 1 1 calc R . . C5 C -0.0051(4) 0.0056(2) 0.2441(2) 0.0352(6) Uani 1 1 d . . . H5 H -0.0991 -0.0499 0.1990 0.042 Uiso 1 1 calc R . . C6 C -0.0255(4) 0.1263(2) 0.2989(2) 0.0319(6) Uani 1 1 d . . . H6 H -0.1358 0.1483 0.2902 0.038 Uiso 1 1 calc R . . C7 C 0.2569(3) 0.1749(2) 0.3733(2) 0.0255(5) Uani 1 1 d . . . C8 C 0.5739(4) -0.0489(2) 0.3378(2) 0.0300(6) Uani 1 1 d . . . C9 C 0.7087(4) -0.0504(3) 0.4129(2) 0.0347(6) Uani 1 1 d . . . H9 H 0.7379 0.0159 0.4764 0.042 Uiso 1 1 calc R . . C10 C 0.7994(4) -0.1500(3) 0.3936(2) 0.0400(7) Uani 1 1 d . . . H10 H 0.8908 -0.1490 0.4433 0.048 Uiso 1 1 calc R . . C11 C 0.7538(4) -0.2505(3) 0.3008(2) 0.0361(7) Uani 1 1 d . . . H11 H 0.8117 -0.3182 0.2893 0.043 Uiso 1 1 calc R . . C12 C 0.6218(4) -0.2502(3) 0.2247(2) 0.0336(6) Uani 1 1 d . . . C13 C 0.5341(4) -0.1487(2) 0.2428(2) 0.0303(6) Uani 1 1 d . . . H13 H 0.4482 -0.1476 0.1910 0.036 Uiso 1 1 calc R . . C14 C 0.5691(4) -0.3588(3) 0.1263(2) 0.0384(7) Uani 1 1 d . . . C15 C 0.1380(3) 0.5912(2) 0.3731(2) 0.0298(6) Uani 1 1 d . . . C16 C 0.2174(4) 0.6441(3) 0.3004(3) 0.0468(8) Uani 1 1 d . . . H16A H 0.3255 0.6139 0.2864 0.070 Uiso 1 1 calc R . . H16B H 0.2391 0.7321 0.3326 0.070 Uiso 1 1 calc R . . H16C H 0.1383 0.6200 0.2358 0.070 Uiso 1 1 calc R . . C17 C -0.2962(3) 0.4376(2) 0.3700(2) 0.0268(5) Uani 1 1 d . . . C18 C -0.4571(4) 0.4041(3) 0.2901(2) 0.0364(6) Uani 1 1 d . . . H18A H -0.4413 0.4451 0.2417 0.055 Uiso 1 1 calc R . . H18B H -0.5553 0.4289 0.3245 0.055 Uiso 1 1 calc R . . H18C H -0.4781 0.3167 0.2527 0.055 Uiso 1 1 calc R . . N1 N 0.1032(3) 0.2130(2) 0.36331(17) 0.0261(5) Uani 1 1 d . . . N2 N 0.4058(3) 0.2454(2) 0.43687(18) 0.0301(5) Uani 1 1 d . . . H2 H 0.4166 0.3222 0.4752 0.036 Uiso 1 1 calc R . . O1 O 0.6459(3) -0.4508(2) 0.11302(18) 0.0553(7) Uani 1 1 d . . . O2 O 0.4479(4) -0.3530(2) 0.05915(19) 0.0619(7) Uani 1 1 d . . . H2A H 0.4301 -0.4172 0.0077 0.093 Uiso 1 1 calc R . . O3 O 0.1476(2) 0.47983(17) 0.35766(15) 0.0312(4) Uani 1 1 d . . . O4 O -0.0695(2) 0.33678(16) 0.55491(14) 0.0287(4) Uani 1 1 d . . . O5 O -0.1905(2) 0.36064(16) 0.35696(14) 0.0286(4) Uani 1 1 d . . . O6 O 0.2734(2) 0.45856(16) 0.55508(14) 0.0291(4) Uani 1 1 d . . . Rh1 Rh 0.04201(2) 0.402165(16) 0.453261(15) 0.02277(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0207(13) 0.0280(14) 0.0416(15) 0.0082(12) 0.0025(11) 0.0084(11) C2 0.0242(14) 0.0256(14) 0.0364(14) 0.0108(11) 0.0082(11) 0.0091(11) C3 0.0259(14) 0.0208(12) 0.0333(13) 0.0077(10) 0.0077(11) 0.0088(10) C4 0.0293(15) 0.0209(13) 0.0420(15) 0.0058(11) 0.0075(12) 0.0084(11) C5 0.0279(15) 0.0257(14) 0.0457(16) 0.0062(12) 0.0023(12) 0.0048(11) C6 0.0218(14) 0.0271(14) 0.0446(16) 0.0092(12) 0.0035(11) 0.0096(11) C7 0.0233(13) 0.0231(13) 0.0322(13) 0.0104(11) 0.0068(10) 0.0084(10) C8 0.0229(14) 0.0261(14) 0.0458(16) 0.0153(12) 0.0122(12) 0.0096(11) C9 0.0297(15) 0.0349(15) 0.0413(16) 0.0135(13) 0.0068(12) 0.0130(12) C10 0.0338(17) 0.0487(18) 0.0485(17) 0.0269(15) 0.0085(13) 0.0199(14) C11 0.0327(16) 0.0324(15) 0.0503(17) 0.0187(13) 0.0124(13) 0.0166(12) C12 0.0305(15) 0.0279(14) 0.0470(16) 0.0143(12) 0.0150(13) 0.0129(12) C13 0.0298(15) 0.0242(13) 0.0397(15) 0.0123(11) 0.0091(12) 0.0095(11) C14 0.0413(18) 0.0267(15) 0.0498(18) 0.0121(13) 0.0145(14) 0.0147(13) C15 0.0210(13) 0.0316(14) 0.0398(15) 0.0153(12) 0.0055(11) 0.0077(11) C16 0.046(2) 0.0458(19) 0.062(2) 0.0296(16) 0.0248(16) 0.0152(15) C17 0.0192(13) 0.0242(13) 0.0376(14) 0.0113(11) 0.0050(10) 0.0056(10) C18 0.0262(15) 0.0352(16) 0.0453(16) 0.0111(13) 0.0011(12) 0.0112(12) N1 0.0231(12) 0.0226(11) 0.0324(11) 0.0085(9) 0.0051(9) 0.0077(9) N2 0.0225(12) 0.0211(11) 0.0417(13) 0.0047(9) 0.0036(9) 0.0075(9) O1 0.0749(18) 0.0338(12) 0.0564(14) 0.0083(10) 0.0111(12) 0.0326(12) O2 0.0609(17) 0.0420(14) 0.0621(15) -0.0061(11) -0.0086(13) 0.0258(12) O3 0.0290(10) 0.0280(10) 0.0407(10) 0.0132(8) 0.0127(8) 0.0114(8) O4 0.0249(10) 0.0230(9) 0.0401(10) 0.0125(8) 0.0068(8) 0.0075(7) O5 0.0218(9) 0.0238(9) 0.0367(10) 0.0061(8) 0.0005(7) 0.0096(7) O6 0.0199(9) 0.0242(9) 0.0399(10) 0.0063(8) 0.0027(8) 0.0101(7) Rh1 0.01595(12) 0.01744(12) 0.03385(13) 0.00662(8) 0.00404(8) 0.00749(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 N2 1.371(3) . ? C1 C2 1.373(4) . ? C1 H1 0.9300 . ? C2 C3 1.436(4) . ? C2 C8 1.483(3) . ? C3 C4 1.386(4) . ? C3 C7 1.420(3) . ? C4 C5 1.389(4) . ? C4 H4 0.9300 . ? C5 C6 1.389(4) . ? C5 H5 0.9300 . ? C6 N1 1.339(3) . ? C6 H6 0.9300 . ? C7 N1 1.331(3) . ? C7 N2 1.368(3) . ? C8 C13 1.393(4) . ? C8 C9 1.399(4) . ? C9 C10 1.392(4) . ? C9 H9 0.9300 . ? C10 C11 1.382(4) . ? C10 H10 0.9300 . ? C11 C12 1.389(4) . ? C11 H11 0.9300 . ? C12 C13 1.397(4) . ? C12 C14 1.480(4) . ? C13 H13 0.9300 . ? C14 O1 1.258(3) . ? C14 O2 1.274(4) . ? C15 O3 1.261(3) . ? C15 O4 1.267(3) 2_566 ? C15 C16 1.502(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O5 1.266(3) . ? C17 O6 1.272(3) 2_566 ? C17 C18 1.495(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? N1 Rh1 2.263(2) . ? N2 H2 0.8600 . ? O2 H2A 0.8200 . ? O3 Rh1 2.0389(18) . ? O4 C15 1.267(3) 2_566 ? O4 Rh1 2.0439(18) . ? O5 Rh1 2.0309(18) . ? O6 C17 1.272(3) 2_566 ? O6 Rh1 2.0521(18) . ? Rh1 Rh1 2.4072(3) 2_566 ? 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 N2 C1 C2 110.5(2) . . ? N2 C1 H1 124.7 . . ? C2 C1 H1 124.7 . . ? C1 C2 C3 106.2(2) . . ? C1 C2 C8 125.5(3) . . ? C3 C2 C8 128.2(2) . . ? C4 C3 C7 116.4(2) . . ? C4 C3 C2 136.9(2) . . ? C7 C3 C2 106.5(2) . . ? C3 C4 C5 118.3(2) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? N1 C6 C5 124.2(2) . . ? N1 C6 H6 117.9 . . ? C5 C6 H6 117.9 . . ? N1 C7 N2 125.4(2) . . ? N1 C7 C3 126.5(2) . . ? N2 C7 C3 108.1(2) . . ? C13 C8 C9 118.5(2) . . ? C13 C8 C2 121.4(3) . . ? C9 C8 C2 120.1(3) . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 119.7(3) . . ? C11 C12 C14 120.4(2) . . ? C13 C12 C14 119.9(3) . . ? C8 C13 C12 120.8(3) . . ? C8 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? O1 C14 O2 123.6(3) . . ? O1 C14 C12 118.8(3) . . ? O2 C14 C12 117.6(2) . . ? O3 C15 O4 126.0(2) . 2_566 ? O3 C15 C16 117.2(2) . . ? O4 C15 C16 116.8(2) 2_566 . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 O6 124.6(2) . 2_566 ? O5 C17 C18 117.1(2) . . ? O6 C17 C18 118.2(2) 2_566 . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 N1 C6 114.7(2) . . ? C7 N1 Rh1 125.84(17) . . ? C6 N1 Rh1 119.26(16) . . ? C7 N2 C1 108.7(2) . . ? C7 N2 H2 125.7 . . ? C1 N2 H2 125.7 . . ? C14 O2 H2A 109.5 . . ? C15 O3 Rh1 119.17(17) . . ? C15 O4 Rh1 119.10(17) 2_566 . ? C17 O5 Rh1 120.65(17) . . ? C17 O6 Rh1 119.04(15) 2_566 . ? O5 Rh1 O3 88.73(8) . . ? O5 Rh1 O4 91.00(7) . . ? O3 Rh1 O4 175.68(6) . . ? O5 Rh1 O6 175.38(6) . . ? O3 Rh1 O6 90.08(8) . . ? O4 Rh1 O6 89.86(7) . . ? O5 Rh1 N1 89.41(7) . . ? O3 Rh1 N1 93.86(7) . . ? O4 Rh1 N1 90.45(7) . . ? O6 Rh1 N1 95.12(7) . . ? O5 Rh1 Rh1 87.58(5) . 2_566 ? O3 Rh1 Rh1 87.99(5) . 2_566 ? O4 Rh1 Rh1 87.69(5) . 2_566 ? O6 Rh1 Rh1 87.91(5) . 2_566 ? N1 Rh1 Rh1 176.44(6) . 2_566 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.410 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.118 #===END ###Material relevant to compound 14 at 173K ## data_compound_14_173 _database_code_depnum_ccdc_archive 'CCDC 815825' #TrackingRef '- rhodiuminsertion.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H32 N4 O12 Rh2, 2(C5 H11 N O)' _chemical_formula_sum 'C46 H54 N6 O14 Rh2' _chemical_formula_weight 1120.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1180 0.9190 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4005(2) _cell_length_b 10.4754(3) _cell_length_c 13.6491(4) _cell_angle_alpha 77.8610(10) _cell_angle_beta 88.822(2) _cell_angle_gamma 88.1780(10) _cell_volume 1173.53(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5426 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.51 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8539 _exptl_absorpt_correction_T_max 0.9846 _exptl_absorpt_process_details sadabs _exptl_special_details ; The oxygen atom of the DEF molecule is disordered over two positions. Therefore the hydrogen atom on the carbon atom of this carbonyl function has not been introduced although it is taken into account in the formula of the compound. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17206 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5351 _reflns_number_gt 4719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0419P)^2^+0.0859P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5351 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _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 0.3019(3) 0.3150(3) 0.2461(2) 0.0247(6) Uani 1 1 d . . . H1 H 0.3274 0.2789 0.3123 0.030 Uiso 1 1 calc R . . C2 C 0.3364(3) 0.4395(3) 0.1977(2) 0.0221(6) Uani 1 1 d . . . C3 C 0.2765(3) 0.4537(2) 0.0979(2) 0.0208(6) Uani 1 1 d . . . C4 C 0.2597(3) 0.5543(3) 0.0124(2) 0.0248(6) Uani 1 1 d . . . H4 H 0.2972 0.6372 0.0112 0.030 Uiso 1 1 calc R . . C5 C 0.1865(3) 0.5270(3) -0.0690(2) 0.0251(6) Uani 1 1 d . . . H5 H 0.1749 0.5919 -0.1267 0.030 Uiso 1 1 calc R . . C6 C 0.1289(3) 0.4023(3) -0.0667(2) 0.0228(6) Uani 1 1 d . . . H6 H 0.0813 0.3867 -0.1238 0.027 Uiso 1 1 calc R . . C7 C 0.2093(3) 0.3329(2) 0.0926(2) 0.0186(5) Uani 1 1 d . . . C8 C 0.4219(3) 0.5341(3) 0.2405(2) 0.0237(6) Uani 1 1 d . . . C9 C 0.4198(3) 0.5275(3) 0.3440(2) 0.0261(6) Uani 1 1 d . . . H9 H 0.3573 0.4664 0.3857 0.031 Uiso 1 1 calc R . . C10 C 0.5095(3) 0.6107(3) 0.3850(2) 0.0272(6) Uani 1 1 d . . . H10 H 0.5081 0.6038 0.4540 0.033 Uiso 1 1 calc R . . C11 C 0.6019(3) 0.7046(3) 0.3248(2) 0.0253(6) Uani 1 1 d . . . C12 C 0.6002(3) 0.7160(3) 0.2218(2) 0.0273(6) Uani 1 1 d . . . H12 H 0.6578 0.7810 0.1804 0.033 Uiso 1 1 calc R . . C13 C 0.5134(3) 0.6313(3) 0.1802(2) 0.0262(6) Uani 1 1 d . . . H13 H 0.5155 0.6388 0.1111 0.031 Uiso 1 1 calc R . . C14 C 0.7038(3) 0.7885(3) 0.3703(2) 0.0278(6) Uani 1 1 d . . . C15 C -0.1036(3) 0.1071(2) -0.1791(2) 0.0209(6) Uani 1 1 d . . . C16 C -0.1689(4) 0.1692(3) -0.2804(2) 0.0317(7) Uani 1 1 d . . . H16A H -0.2773 0.1978 -0.2729 0.048 Uiso 1 1 calc R . . H16B H -0.1648 0.1065 -0.3226 0.048 Uiso 1 1 calc R . . H16C H -0.1062 0.2427 -0.3102 0.048 Uiso 1 1 calc R . . C17 C -0.2766(3) 0.0580(3) 0.0737(2) 0.0209(6) Uani 1 1 d . . . C18 C -0.4372(3) 0.0906(3) 0.1133(2) 0.0302(7) Uani 1 1 d . . . H18A H -0.4339 0.1730 0.1334 0.045 Uiso 1 1 calc R . . H18B H -0.4655 0.0238 0.1700 0.045 Uiso 1 1 calc R . . H18C H -0.5150 0.0960 0.0619 0.045 Uiso 1 1 calc R . . N1 N 0.1393(2) 0.3043(2) 0.01414(16) 0.0178(4) Uani 1 1 d . . . N2 N 0.2251(3) 0.2508(2) 0.18425(17) 0.0227(5) Uani 1 1 d . . . H2 H 0.1923 0.1721 0.2003 0.027 Uiso 1 1 calc R . . O1 O 0.7206(3) 0.7550(3) 0.46594(18) 0.0456(6) Uani 1 1 d . . . H1A H 0.7844 0.8026 0.4840 0.068 Uiso 1 1 calc R . . O2 O 0.7700(3) 0.8849(2) 0.31584(19) 0.0450(6) Uani 1 1 d . . . O3 O -0.0356(2) 0.17964(17) -0.13111(14) 0.0234(4) Uani 1 1 d . . . O4 O 0.1226(2) 0.01489(17) 0.14890(14) 0.0230(4) Uani 1 1 d . . . O5 O 0.2600(2) 0.05128(17) -0.04829(14) 0.0221(4) Uani 1 1 d . . . O6 O -0.1695(2) 0.14142(17) 0.06789(14) 0.0227(4) Uani 1 1 d . . . Rh1 Rh 0.04760(2) 0.104151(18) 0.008504(15) 0.01722(8) Uani 1 1 d . . . C19 C 0.9893(4) 0.1270(3) 0.3946(3) 0.0361(8) Uani 1 1 d . . . C20 C 0.7230(4) 0.2010(3) 0.3441(3) 0.0449(9) Uani 1 1 d . . . H20A H 0.7418 0.1534 0.2910 0.054 Uiso 1 1 calc R A . H20B H 0.6756 0.2857 0.3146 0.054 Uiso 1 1 calc R . . C21 C 0.6088(4) 0.1268(4) 0.4209(4) 0.0613(12) Uani 1 1 d . A . H21A H 0.6589 0.0461 0.4541 0.092 Uiso 1 1 calc R . . H21B H 0.5147 0.1088 0.3880 0.092 Uiso 1 1 calc R . . H21C H 0.5802 0.1784 0.4693 0.092 Uiso 1 1 calc R . . C22 C 0.8917(4) 0.3331(3) 0.4340(3) 0.0430(8) Uani 1 1 d . . . H22A H 0.9770 0.3155 0.4822 0.052 Uiso 1 1 calc R A . H22B H 0.7939 0.3468 0.4699 0.052 Uiso 1 1 calc R . . C23 C 0.9267(5) 0.4564(3) 0.3577(3) 0.0526(10) Uani 1 1 d . A . H23A H 1.0218 0.4428 0.3206 0.079 Uiso 1 1 calc R . . H23B H 0.9415 0.5267 0.3915 0.079 Uiso 1 1 calc R . . H23C H 0.8391 0.4780 0.3126 0.079 Uiso 1 1 calc R . . N3 N 0.8753(3) 0.2193(3) 0.3893(2) 0.0329(6) Uani 1 1 d . A . O7A O 1.1223(4) 0.1214(3) 0.4273(3) 0.0326(10) Uani 0.609(5) 1 d P A 1 O7B O 0.9744(6) 0.0328(5) 0.3745(4) 0.0295(15) Uani 0.391(5) 1 d P A 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 C1 0.0292(14) 0.0220(14) 0.0232(15) -0.0048(11) -0.0066(11) -0.0018(11) C2 0.0227(13) 0.0185(13) 0.0274(15) -0.0093(11) -0.0032(11) -0.0019(10) C3 0.0221(13) 0.0159(12) 0.0256(15) -0.0068(11) -0.0010(11) -0.0021(10) C4 0.0291(14) 0.0162(13) 0.0276(15) -0.0003(11) 0.0004(12) -0.0046(11) C5 0.0309(15) 0.0177(13) 0.0247(15) 0.0009(11) -0.0014(12) -0.0040(11) C6 0.0255(14) 0.0202(13) 0.0235(14) -0.0052(11) -0.0030(11) -0.0044(11) C7 0.0178(12) 0.0140(12) 0.0242(14) -0.0039(10) -0.0025(10) -0.0006(10) C8 0.0248(14) 0.0183(13) 0.0293(16) -0.0075(11) -0.0053(12) 0.0008(11) C9 0.0306(15) 0.0210(14) 0.0259(15) -0.0024(11) -0.0034(12) -0.0039(11) C10 0.0334(16) 0.0257(15) 0.0231(15) -0.0060(12) -0.0054(12) -0.0024(12) C11 0.0256(14) 0.0216(14) 0.0308(16) -0.0099(12) -0.0064(12) -0.0008(11) C12 0.0300(15) 0.0216(14) 0.0314(16) -0.0076(12) 0.0032(12) -0.0057(11) C13 0.0288(15) 0.0242(14) 0.0268(15) -0.0078(12) 0.0011(12) -0.0032(12) C14 0.0280(15) 0.0247(15) 0.0334(17) -0.0117(12) -0.0019(12) -0.0024(12) C15 0.0224(13) 0.0193(13) 0.0199(14) -0.0016(10) -0.0027(10) -0.0003(10) C16 0.0381(17) 0.0233(15) 0.0311(17) 0.0011(12) -0.0122(13) -0.0001(12) C17 0.0227(13) 0.0194(13) 0.0198(14) -0.0019(10) -0.0054(10) -0.0003(10) C18 0.0221(14) 0.0324(16) 0.0379(18) -0.0117(13) 0.0007(12) -0.0004(12) N1 0.0167(10) 0.0149(10) 0.0206(12) -0.0011(9) -0.0006(8) -0.0002(8) N2 0.0272(12) 0.0150(11) 0.0256(13) -0.0026(9) -0.0046(10) -0.0034(9) O1 0.0433(14) 0.0573(16) 0.0416(14) -0.0205(12) -0.0159(11) -0.0080(12) O2 0.0461(14) 0.0412(14) 0.0534(16) -0.0203(12) 0.0015(12) -0.0211(11) O3 0.0301(10) 0.0157(9) 0.0231(10) -0.0003(8) -0.0072(8) -0.0021(8) O4 0.0282(10) 0.0152(9) 0.0250(10) -0.0016(8) -0.0072(8) -0.0040(8) O5 0.0194(9) 0.0188(9) 0.0278(11) -0.0035(8) 0.0013(8) -0.0040(7) O6 0.0217(9) 0.0170(9) 0.0301(11) -0.0065(8) 0.0001(8) -0.0017(7) Rh1 0.01864(12) 0.01194(11) 0.02051(13) -0.00149(8) -0.00260(8) -0.00297(8) C19 0.0321(17) 0.0283(17) 0.044(2) 0.0019(14) -0.0059(14) -0.0089(13) C20 0.0356(18) 0.041(2) 0.055(2) -0.0022(17) -0.0123(16) -0.0028(15) C21 0.037(2) 0.042(2) 0.099(4) -0.003(2) 0.007(2) -0.0003(16) C22 0.047(2) 0.047(2) 0.037(2) -0.0155(16) -0.0096(16) 0.0068(16) C23 0.052(2) 0.036(2) 0.073(3) -0.0181(19) 0.000(2) -0.0018(17) N3 0.0310(14) 0.0325(14) 0.0330(15) -0.0012(11) -0.0066(11) -0.0030(11) O7A 0.032(2) 0.032(2) 0.035(2) -0.0083(15) -0.0090(15) -0.0058(15) O7B 0.030(3) 0.021(3) 0.042(3) -0.018(2) -0.004(2) -0.001(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 C1 N2 1.368(3) . ? C1 C2 1.369(4) . ? C1 H1 0.9300 . ? C2 C3 1.438(4) . ? C2 C8 1.465(4) . ? C3 C4 1.405(4) . ? C3 C7 1.419(4) . ? C4 C5 1.366(4) . ? C4 H4 0.9300 . ? C5 C6 1.401(4) . ? C5 H5 0.9300 . ? C6 N1 1.341(3) . ? C6 H6 0.9300 . ? C7 N1 1.324(3) . ? C7 N2 1.367(3) . ? C8 C9 1.400(4) . ? C8 C13 1.406(4) . ? C9 C10 1.380(4) . ? C9 H9 0.9300 . ? C10 C11 1.388(4) . ? C10 H10 0.9300 . ? C11 C12 1.386(4) . ? C11 C14 1.480(4) . ? C12 C13 1.382(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O2 1.259(3) . ? C14 O1 1.289(4) . ? C15 O3 1.259(3) . ? C15 O4 1.272(3) 2 ? C15 C16 1.505(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O6 1.264(3) . ? C17 O5 1.267(3) 2 ? C17 C18 1.499(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? N1 Rh1 2.274(2) . ? N2 H2 0.8600 . ? O1 H1A 0.8200 . ? O3 Rh1 2.0325(18) . ? O4 C15 1.272(3) 2 ? O4 Rh1 2.0498(18) . ? O5 C17 1.267(3) 2 ? O5 Rh1 2.0380(18) . ? O6 Rh1 2.0402(18) . ? Rh1 Rh1 2.4055(4) 2 ? C19 O7B 1.090(6) . ? C19 O7A 1.206(4) . ? C19 N3 1.331(4) . ? C20 N3 1.467(4) . ? C20 C21 1.512(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N3 1.459(4) . ? C22 C23 1.511(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? 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 N2 C1 C2 111.1(2) . . ? N2 C1 H1 124.5 . . ? C2 C1 H1 124.5 . . ? C1 C2 C3 105.8(2) . . ? C1 C2 C8 125.7(3) . . ? C3 C2 C8 128.6(2) . . ? C4 C3 C7 116.0(2) . . ? C4 C3 C2 137.1(2) . . ? C7 C3 C2 106.7(2) . . ? C5 C4 C3 118.1(2) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? N1 C6 C5 123.0(3) . . ? N1 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? N1 C7 N2 125.4(2) . . ? N1 C7 C3 126.6(2) . . ? N2 C7 C3 108.0(2) . . ? C9 C8 C13 117.6(3) . . ? C9 C8 C2 120.8(2) . . ? C13 C8 C2 121.6(3) . . ? C10 C9 C8 120.7(3) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 121.1(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 118.9(3) . . ? C12 C11 C14 120.7(3) . . ? C10 C11 C14 120.4(3) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 121.2(3) . . ? C12 C13 H13 119.4 . . ? C8 C13 H13 119.4 . . ? O2 C14 O1 123.8(3) . . ? O2 C14 C11 120.1(3) . . ? O1 C14 C11 116.1(3) . . ? O3 C15 O4 125.3(2) . 2 ? O3 C15 C16 117.7(2) . . ? O4 C15 C16 116.9(2) 2 . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 125.4(2) . 2 ? O6 C17 C18 117.6(2) . . ? O5 C17 C18 116.9(2) 2 . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 N1 C6 115.4(2) . . ? C7 N1 Rh1 124.44(16) . . ? C6 N1 Rh1 120.13(18) . . ? C7 N2 C1 108.5(2) . . ? C7 N2 H2 125.8 . . ? C1 N2 H2 125.8 . . ? C14 O1 H1A 109.5 . . ? C15 O3 Rh1 119.94(16) . . ? C15 O4 Rh1 119.10(17) 2 . ? C17 O5 Rh1 120.13(16) 2 . ? C17 O6 Rh1 118.81(17) . . ? O3 Rh1 O5 91.61(8) . . ? O3 Rh1 O6 89.69(8) . . ? O5 Rh1 O6 175.35(6) . . ? O3 Rh1 O4 175.53(6) . . ? O5 Rh1 O4 88.88(8) . . ? O6 Rh1 O4 89.47(8) . . ? O3 Rh1 N1 88.91(7) . . ? O5 Rh1 N1 91.26(7) . . ? O6 Rh1 N1 93.23(7) . . ? O4 Rh1 N1 95.52(7) . . ? O3 Rh1 Rh1 87.96(5) . 2 ? O5 Rh1 Rh1 87.21(5) . 2 ? O6 Rh1 Rh1 88.37(5) . 2 ? O4 Rh1 Rh1 87.63(5) . 2 ? N1 Rh1 Rh1 176.47(6) . 2 ? O7B C19 O7A 104.8(4) . . ? O7B C19 N3 124.6(4) . . ? O7A C19 N3 130.4(4) . . ? N3 C20 C21 111.5(3) . . ? N3 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? N3 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C23 113.1(3) . . ? N3 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? N3 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 N3 C22 122.3(3) . . ? C19 N3 C20 118.9(3) . . ? C22 N3 C20 118.6(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.579 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.161 #===END