Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Bunz, Uwe H. F.' 'Fiscus, Jeffrey E.' 'Layland, Ralph C.' 'Shotwell, Sandra' 'Smith, Mark D.' 'zur Loye, Hans-Conrad' _publ_contact_author_name 'Dr Uwe H. F. Bunz' _publ_contact_author_address ; Department of Chemistry and Biochemistry The University of South Carolina Columbia South Carolina 29208 UNITED STATES OF AMERICA ; _publ_contact_author_email 'BUNZ:MAIL.CHEM.SC.EDU' _publ_section_title ; Three unique coordination geometries involving 1,2-dimethoxy-4,5-bis(2-pyridylethynyl)benzene ; data_cocls2s _database_code_CSD 173558 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H32 Cl4 Co2 N4 O4' _chemical_formula_weight 940.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' 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 8.5272(6) _cell_length_b 18.3653(13) _cell_length_c 13.3493(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.574(2) _cell_angle_gamma 90.00 _cell_volume 2032.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 6955 _cell_measurement_theta_min 2.216 _cell_measurement_theta_max 26.366 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7094 _exptl_absorpt_correction_T_max 0.9350 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13541 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.41 _reflns_number_total 4165 _reflns_number_gt 3405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.624 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _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^)+(0.0667P)^2^+0.0069P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4165 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Co Co 0.18219(4) 0.313080(19) 0.57175(3) 0.02386(13) Uani 1 1 d . . . Cl1 Cl -0.07870(8) 0.28491(4) 0.51887(6) 0.03551(19) Uani 1 1 d . . . Cl2 Cl 0.31565(9) 0.23850(4) 0.69571(5) 0.03561(19) Uani 1 1 d . . . C1 C 0.1973(3) 0.47645(15) 0.5903(2) 0.0268(6) Uani 1 1 d . . . C2 C 0.1957(4) 0.54269(16) 0.6415(2) 0.0355(7) Uani 1 1 d . . . H2 H 0.1984 0.5874 0.6062 0.043 Uiso 1 1 calc R . . C3 C 0.1904(4) 0.54234(17) 0.7434(2) 0.0397(7) Uani 1 1 d . . . H3 H 0.1934 0.5869 0.7800 0.048 Uiso 1 1 calc R . . C4 C 0.1806(4) 0.47747(17) 0.7922(2) 0.0389(7) Uani 1 1 d . . . H4 H 0.1750 0.4763 0.8624 0.047 Uiso 1 1 calc R . . C5 C 0.1791(4) 0.41421(16) 0.7374(2) 0.0334(7) Uani 1 1 d . . . H5 H 0.1704 0.3693 0.7710 0.040 Uiso 1 1 calc R . . C6 C 0.2109(3) 0.47658(15) 0.4857(2) 0.0292(6) Uani 1 1 d . . . C7 C 0.2294(3) 0.48553(14) 0.4004(2) 0.0285(6) Uani 1 1 d . . . C8 C 0.2611(3) 0.50032(14) 0.30253(19) 0.0264(6) Uani 1 1 d . . . C9 C 0.1989(4) 0.45616(15) 0.2164(2) 0.0300(6) Uani 1 1 d . . . H9 H 0.1370 0.4144 0.2239 0.036 Uiso 1 1 calc R . . C10 C 0.2264(4) 0.47266(15) 0.1214(2) 0.0299(6) Uani 1 1 d . . . C11 C 0.3236(4) 0.53394(14) 0.1111(2) 0.0285(6) Uani 1 1 d . . . C12 C 0.3886(3) 0.57613(14) 0.1961(2) 0.0263(6) Uani 1 1 d . . . H12 H 0.4561 0.6162 0.1897 0.032 Uiso 1 1 calc R . . C13 C 0.3561(3) 0.56047(14) 0.29159(19) 0.0251(6) Uani 1 1 d . . . C14 C 0.0634(5) 0.37481(19) 0.0372(3) 0.0536(10) Uani 1 1 d . . . H14A H 0.1273 0.3344 0.0737 0.080 Uiso 1 1 calc R . . H14B H 0.0115 0.3596 -0.0331 0.080 Uiso 1 1 calc R . . H14C H -0.0193 0.3888 0.0736 0.080 Uiso 1 1 calc R . . C15 C 0.4407(4) 0.60504(16) 0.0002(2) 0.0378(7) Uani 1 1 d . . . H15A H 0.3897 0.6503 0.0153 0.057 Uiso 1 1 calc R . . H15B H 0.4509 0.6058 -0.0714 0.057 Uiso 1 1 calc R . . H15C H 0.5479 0.6006 0.0466 0.057 Uiso 1 1 calc R . . C16 C 0.4227(3) 0.60536(14) 0.3797(2) 0.0251(6) Uani 1 1 d . . . C17 C 0.4799(3) 0.64153(14) 0.4530(2) 0.0260(6) Uani 1 1 d . . . C18 C 0.5606(3) 0.67930(14) 0.5447(2) 0.0250(6) Uani 1 1 d . . . C19 C 0.4856(4) 0.69455(15) 0.6243(2) 0.0319(6) Uani 1 1 d . . . H19 H 0.3751 0.6829 0.6177 0.038 Uiso 1 1 calc R . . C20 C 0.5742(4) 0.72684(16) 0.7130(2) 0.0342(7) Uani 1 1 d . . . H20 H 0.5253 0.7375 0.7683 0.041 Uiso 1 1 calc R . . C21 C 0.7329(4) 0.74335(16) 0.7206(2) 0.0328(7) Uani 1 1 d . . . H21 H 0.7958 0.7648 0.7817 0.039 Uiso 1 1 calc R . . C22 C 0.8005(3) 0.72847(14) 0.6386(2) 0.0284(6) Uani 1 1 d . . . H22 H 0.9105 0.7406 0.6441 0.034 Uiso 1 1 calc R . . N1 N 0.1895(3) 0.41255(12) 0.63796(16) 0.0258(5) Uani 1 1 d . . . N2 N 0.7164(3) 0.69742(11) 0.55089(17) 0.0241(5) Uani 1 1 d . . . O1 O 0.1671(3) 0.43571(11) 0.03346(15) 0.0401(5) Uani 1 1 d . . . O2 O 0.3444(3) 0.54487(11) 0.01487(14) 0.0355(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 Co 0.0284(2) 0.0248(2) 0.0191(2) -0.00014(14) 0.00702(15) 0.00015(14) Cl1 0.0276(4) 0.0433(4) 0.0347(4) 0.0036(3) 0.0055(3) 0.0006(3) Cl2 0.0370(4) 0.0346(4) 0.0325(4) 0.0086(3) 0.0027(3) 0.0029(3) C1 0.0315(15) 0.0286(14) 0.0207(13) 0.0005(11) 0.0066(11) -0.0019(11) C2 0.0471(19) 0.0259(14) 0.0342(16) 0.0001(12) 0.0111(14) -0.0015(12) C3 0.053(2) 0.0345(16) 0.0318(16) -0.0113(13) 0.0102(14) -0.0015(14) C4 0.053(2) 0.0417(17) 0.0239(15) -0.0058(13) 0.0139(14) 0.0046(14) C5 0.0448(18) 0.0346(15) 0.0228(14) 0.0006(12) 0.0121(13) 0.0013(13) C6 0.0372(16) 0.0266(14) 0.0236(14) 0.0013(11) 0.0067(12) -0.0012(11) C7 0.0343(16) 0.0254(14) 0.0249(14) -0.0004(11) 0.0049(12) -0.0013(11) C8 0.0329(15) 0.0279(13) 0.0177(13) 0.0027(11) 0.0047(11) 0.0017(11) C9 0.0409(17) 0.0270(14) 0.0228(14) 0.0011(11) 0.0089(12) -0.0051(12) C10 0.0396(16) 0.0300(14) 0.0197(13) -0.0035(11) 0.0061(12) -0.0013(12) C11 0.0395(16) 0.0284(14) 0.0193(13) 0.0013(11) 0.0102(12) 0.0006(12) C12 0.0331(15) 0.0228(13) 0.0236(13) 0.0010(11) 0.0078(11) -0.0007(11) C13 0.0283(14) 0.0273(13) 0.0189(13) -0.0030(11) 0.0042(11) 0.0004(11) C14 0.081(3) 0.0441(19) 0.0390(19) -0.0146(15) 0.0207(18) -0.0317(18) C15 0.055(2) 0.0360(16) 0.0258(15) 0.0028(12) 0.0168(14) -0.0078(14) C16 0.0280(14) 0.0270(13) 0.0199(13) 0.0019(11) 0.0051(11) 0.0005(11) C17 0.0259(14) 0.0305(14) 0.0222(14) 0.0010(11) 0.0072(11) 0.0007(11) C18 0.0277(14) 0.0252(13) 0.0213(13) -0.0019(10) 0.0043(11) 0.0010(10) C19 0.0307(15) 0.0386(16) 0.0276(15) -0.0034(12) 0.0091(12) -0.0022(12) C20 0.0432(18) 0.0396(16) 0.0219(14) -0.0080(12) 0.0122(13) 0.0022(13) C21 0.0437(18) 0.0327(15) 0.0209(14) -0.0060(12) 0.0057(12) -0.0067(13) C22 0.0308(15) 0.0298(14) 0.0224(14) -0.0034(11) 0.0015(11) -0.0054(11) N1 0.0332(13) 0.0253(11) 0.0191(11) -0.0007(9) 0.0068(9) -0.0003(9) N2 0.0281(12) 0.0247(11) 0.0200(11) -0.0016(9) 0.0069(9) -0.0014(9) O1 0.0632(15) 0.0358(11) 0.0221(10) -0.0076(9) 0.0115(10) -0.0152(10) O2 0.0539(14) 0.0357(11) 0.0195(10) -0.0021(8) 0.0137(9) -0.0091(10) _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 Co N1 2.024(2) . ? Co N2 2.032(2) 3_666 ? Co Cl1 2.2311(8) . ? Co Cl2 2.2418(7) . ? C1 N1 1.344(3) . ? C1 C2 1.397(4) . ? C1 C6 1.428(4) . ? C2 C3 1.371(4) . ? C3 C4 1.370(4) . ? C4 C5 1.372(4) . ? C5 N1 1.351(3) . ? C6 C7 1.197(4) . ? C7 C8 1.421(4) . ? C8 C13 1.398(4) . ? C8 C9 1.405(4) . ? C9 C10 1.377(4) . ? C10 O1 1.347(3) . ? C10 C11 1.424(4) . ? C11 O2 1.352(3) . ? C11 C12 1.379(4) . ? C12 C13 1.396(4) . ? C13 C16 1.439(4) . ? C14 O1 1.434(4) . ? C15 O2 1.417(3) . ? C16 C17 1.188(4) . ? C17 C18 1.435(4) . ? C18 N2 1.353(4) . ? C18 C19 1.391(4) . ? C19 C20 1.380(4) . ? C20 C21 1.367(4) . ? C21 C22 1.380(4) . ? C22 N2 1.347(3) . ? N2 Co 2.032(2) 3_666 ? 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 Co N2 117.53(9) . 3_666 ? N1 Co Cl1 105.87(7) . . ? N2 Co Cl1 107.72(7) 3_666 . ? N1 Co Cl2 105.71(6) . . ? N2 Co Cl2 107.37(7) 3_666 . ? Cl1 Co Cl2 112.81(3) . . ? N1 C1 C2 121.4(2) . . ? N1 C1 C6 119.2(2) . . ? C2 C1 C6 119.3(2) . . ? C3 C2 C1 119.2(3) . . ? C4 C3 C2 119.7(3) . . ? C3 C4 C5 118.5(3) . . ? N1 C5 C4 123.3(3) . . ? C7 C6 C1 171.7(3) . . ? C6 C7 C8 175.4(3) . . ? C13 C8 C9 119.2(2) . . ? C13 C8 C7 119.2(2) . . ? C9 C8 C7 121.7(2) . . ? C10 C9 C8 120.9(3) . . ? O1 C10 C9 125.6(3) . . ? O1 C10 C11 114.9(2) . . ? C9 C10 C11 119.5(2) . . ? O2 C11 C12 125.6(2) . . ? O2 C11 C10 114.7(2) . . ? C12 C11 C10 119.7(2) . . ? C11 C12 C13 120.6(2) . . ? C12 C13 C8 120.2(2) . . ? C12 C13 C16 120.2(2) . . ? C8 C13 C16 119.6(2) . . ? C17 C16 C13 178.8(3) . . ? C16 C17 C18 174.1(3) . . ? N2 C18 C19 121.6(2) . . ? N2 C18 C17 116.0(2) . . ? C19 C18 C17 122.3(3) . . ? C20 C19 C18 119.0(3) . . ? C21 C20 C19 119.5(3) . . ? C20 C21 C22 119.2(3) . . ? N2 C22 C21 122.5(3) . . ? C1 N1 C5 117.8(2) . . ? C1 N1 Co 125.55(17) . . ? C5 N1 Co 116.56(18) . . ? C22 N2 C18 118.2(2) . . ? C22 N2 Co 119.99(19) . 3_666 ? C18 N2 Co 121.63(17) . 3_666 ? C10 O1 C14 118.1(2) . . ? C11 O2 C15 117.1(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.921 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.082 data_cuoaczs _database_code_CSD 173559 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 Cu N2 O7' _chemical_formula_weight 554.04 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2357(4) _cell_length_b 12.5088(6) _cell_length_c 13.3128(6) _cell_angle_alpha 78.3000(10) _cell_angle_beta 72.1170(10) _cell_angle_gamma 76.6810(10) _cell_volume 1257.12(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9384 _cell_measurement_theta_min 2.506 _cell_measurement_theta_max 26.351 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6112 _exptl_absorpt_correction_T_max 0.8310 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 11656 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5144 _reflns_number_gt 4398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.624 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _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^)+(0.0575P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0112(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5144 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Cu Cu 0.03344(3) 0.211563(19) 1.149076(18) 0.03285(10) Uani 1 1 d . . . C1 C 0.2555(3) -0.00079(17) 1.20017(17) 0.0402(5) Uani 1 1 d . . . H1 H 0.2310 0.0243 1.2653 0.048 Uiso 1 1 calc R . . C2 C 0.3623(3) -0.10152(18) 1.18537(18) 0.0470(5) Uani 1 1 d . . . H2 H 0.4100 -0.1430 1.2392 0.056 Uiso 1 1 calc R . . C3 C 0.3980(3) -0.14040(19) 1.08954(19) 0.0496(6) Uani 1 1 d . . . H3 H 0.4704 -0.2082 1.0775 0.060 Uiso 1 1 calc R . . C4 C 0.3238(3) -0.07634(18) 1.01172(18) 0.0448(5) Uani 1 1 d . . . H4 H 0.3437 -0.1015 0.9471 0.054 Uiso 1 1 calc R . . C5 C 0.2200(3) 0.02513(16) 1.03077(15) 0.0338(4) Uani 1 1 d . . . C6 C 0.1464(3) 0.09796(17) 0.95102(16) 0.0373(5) Uani 1 1 d . . . C7 C 0.0882(3) 0.15880(17) 0.88500(16) 0.0371(5) Uani 1 1 d . . . C8 C 0.0152(3) 0.23464(17) 0.80636(16) 0.0352(4) Uani 1 1 d . . . C9 C 0.0391(3) 0.20290(18) 0.70623(16) 0.0385(5) Uani 1 1 d . . . H9 H 0.1012 0.1330 0.6916 0.046 Uiso 1 1 calc R . . C10 C -0.0292(3) 0.27490(17) 0.62964(16) 0.0377(5) Uani 1 1 d . . . C11 C -0.1206(3) 0.38107(17) 0.65117(16) 0.0393(5) Uani 1 1 d . . . C12 C -0.1457(3) 0.41243(18) 0.74937(16) 0.0401(5) Uani 1 1 d . . . H12 H -0.2078 0.4824 0.7636 0.048 Uiso 1 1 calc R . . C13 C -0.0779(3) 0.33913(17) 0.82805(15) 0.0351(4) Uani 1 1 d . . . C14 C 0.0834(4) 0.1459(2) 0.50392(19) 0.0548(6) Uani 1 1 d . . . H14A H 0.2004 0.1385 0.5071 0.082 Uiso 1 1 calc R . . H14B H 0.0839 0.1400 0.4330 0.082 Uiso 1 1 calc R . . H14C H 0.0302 0.0882 0.5533 0.082 Uiso 1 1 calc R . . C15 C -0.2539(4) 0.56021(19) 0.5849(2) 0.0584(7) Uani 1 1 d . . . H15A H -0.3596 0.5629 0.6416 0.088 Uiso 1 1 calc R . . H15B H -0.2782 0.6008 0.5202 0.088 Uiso 1 1 calc R . . H15C H -0.1734 0.5928 0.6026 0.088 Uiso 1 1 calc R . . C16 C -0.1083(3) 0.37354(17) 0.92972(16) 0.0363(4) Uani 1 1 d . . . C17 C -0.1352(3) 0.40289(17) 1.01391(16) 0.0356(4) Uani 1 1 d . . . C18 C -0.1754(2) 0.43386(16) 1.11810(15) 0.0331(4) Uani 1 1 d . . . C19 C -0.2737(3) 0.53559(18) 1.14265(18) 0.0447(5) Uani 1 1 d . . . H19 H -0.3116 0.5882 1.0905 0.054 Uiso 1 1 calc R . . C20 C -0.3145(3) 0.5577(2) 1.2455(2) 0.0546(6) Uani 1 1 d . . . H20 H -0.3820 0.6250 1.2643 0.066 Uiso 1 1 calc R . . C21 C -0.2535(3) 0.4783(2) 1.32071(18) 0.0518(6) Uani 1 1 d . . . H21 H -0.2804 0.4914 1.3908 0.062 Uiso 1 1 calc R . . C22 C -0.1533(3) 0.38041(19) 1.29087(16) 0.0425(5) Uani 1 1 d . . . H22 H -0.1109 0.3282 1.3416 0.051 Uiso 1 1 calc R . . C23 C -0.2284(3) 0.11210(17) 1.27274(17) 0.0381(5) Uani 1 1 d . . . C24 C -0.3938(3) 0.0666(2) 1.3066(2) 0.0568(6) Uani 1 1 d . . . H24A H -0.4883 0.1256 1.2975 0.085 Uiso 1 1 calc R . . H24B H -0.4155 0.0342 1.3802 0.085 Uiso 1 1 calc R . . H24C H -0.3833 0.0110 1.2636 0.085 Uiso 1 1 calc R . . C25 C 0.3005(3) 0.29115(17) 1.15401(18) 0.0400(5) Uani 1 1 d . . . C26 C 0.4598(3) 0.3436(2) 1.1193(2) 0.0572(6) Uani 1 1 d . . . H26A H 0.4998 0.3425 1.1801 0.086 Uiso 1 1 calc R . . H26B H 0.4320 0.4190 1.0871 0.086 Uiso 1 1 calc R . . H26C H 0.5492 0.3028 1.0684 0.086 Uiso 1 1 calc R . . N1 N 0.1848(2) 0.06301(13) 1.12499(12) 0.0320(4) Uani 1 1 d . . . N2 N -0.1137(2) 0.35663(14) 1.19118(12) 0.0326(4) Uani 1 1 d . . . O1 O -0.0131(2) 0.25211(13) 0.53127(11) 0.0491(4) Uani 1 1 d . . . O2 O -0.1806(2) 0.44748(12) 0.57049(12) 0.0530(4) Uani 1 1 d . . . O3 O -0.17602(18) 0.15041(12) 1.17515(11) 0.0400(3) Uani 1 1 d . . . O4 O -0.1488(2) 0.11194(14) 1.33846(13) 0.0520(4) Uani 1 1 d . . . O5 O 0.23679(19) 0.28333(12) 1.08073(12) 0.0420(3) Uani 1 1 d . . . O6 O 0.2391(2) 0.25746(16) 1.24914(14) 0.0599(5) Uani 1 1 d . . . C1S C 0.5535(4) 0.2195(3) 0.5428(3) 0.0849(10) Uani 1 1 d . . . H1S3 H 0.6088 0.2740 0.5541 0.127 Uiso 1 1 calc R . . H1S2 H 0.4441 0.2179 0.5958 0.127 Uiso 1 1 calc R . . H1S1 H 0.5348 0.2382 0.4732 0.127 Uiso 1 1 calc R . . O1S O 0.6587(3) 0.11594(18) 0.55068(16) 0.0799(6) Uani 1 1 d . . . H1S H 0.7375 0.1117 0.4749 0.120 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.03233(15) 0.03219(15) 0.03374(15) -0.00616(10) -0.00931(10) -0.00360(10) C1 0.0443(12) 0.0422(12) 0.0346(11) -0.0051(9) -0.0153(9) -0.0029(10) C2 0.0534(14) 0.0420(12) 0.0451(13) 0.0013(10) -0.0256(11) 0.0025(11) C3 0.0553(14) 0.0353(12) 0.0549(14) -0.0080(10) -0.0224(11) 0.0097(10) C4 0.0544(13) 0.0399(12) 0.0398(12) -0.0117(9) -0.0165(10) 0.0020(10) C5 0.0347(10) 0.0331(10) 0.0345(10) -0.0034(8) -0.0127(8) -0.0046(8) C6 0.0414(11) 0.0382(11) 0.0328(10) -0.0088(9) -0.0128(9) -0.0017(9) C7 0.0420(11) 0.0384(11) 0.0325(10) -0.0075(9) -0.0128(9) -0.0046(9) C8 0.0380(11) 0.0392(11) 0.0293(10) -0.0019(8) -0.0121(8) -0.0075(9) C9 0.0471(12) 0.0355(11) 0.0331(10) -0.0051(8) -0.0149(9) -0.0023(9) C10 0.0480(12) 0.0367(11) 0.0307(10) -0.0052(8) -0.0149(9) -0.0064(9) C11 0.0490(12) 0.0368(11) 0.0341(11) -0.0012(9) -0.0194(9) -0.0040(9) C12 0.0479(12) 0.0359(11) 0.0372(11) -0.0072(9) -0.0164(9) -0.0004(9) C13 0.0379(11) 0.0393(11) 0.0288(10) -0.0039(8) -0.0110(8) -0.0066(9) C14 0.0798(18) 0.0460(13) 0.0404(12) -0.0153(10) -0.0248(12) 0.0047(13) C15 0.0863(19) 0.0393(13) 0.0500(14) -0.0040(11) -0.0347(14) 0.0076(13) C16 0.0375(11) 0.0371(11) 0.0336(11) -0.0016(9) -0.0122(9) -0.0051(9) C17 0.0368(11) 0.0359(11) 0.0331(10) -0.0029(8) -0.0110(8) -0.0042(9) C18 0.0327(10) 0.0353(10) 0.0317(10) -0.0062(8) -0.0067(8) -0.0087(8) C19 0.0513(13) 0.0361(11) 0.0435(12) -0.0062(9) -0.0131(10) -0.0009(10) C20 0.0649(16) 0.0426(13) 0.0539(14) -0.0225(11) -0.0107(12) 0.0013(12) C21 0.0664(16) 0.0525(14) 0.0383(12) -0.0196(11) -0.0119(11) -0.0063(12) C22 0.0496(13) 0.0470(12) 0.0329(11) -0.0074(9) -0.0142(9) -0.0071(10) C23 0.0372(11) 0.0311(10) 0.0444(12) -0.0057(9) -0.0116(9) -0.0021(9) C24 0.0462(14) 0.0615(16) 0.0614(16) -0.0002(12) -0.0114(12) -0.0191(12) C25 0.0330(11) 0.0328(11) 0.0521(13) -0.0095(9) -0.0110(10) 0.0001(9) C26 0.0428(13) 0.0529(15) 0.0808(18) -0.0181(13) -0.0157(12) -0.0123(11) N1 0.0322(8) 0.0330(9) 0.0304(8) -0.0031(7) -0.0106(7) -0.0033(7) N2 0.0340(9) 0.0356(9) 0.0290(8) -0.0071(7) -0.0084(7) -0.0058(7) O1 0.0769(11) 0.0395(8) 0.0343(8) -0.0076(6) -0.0272(8) 0.0012(8) O2 0.0844(12) 0.0380(8) 0.0412(9) -0.0056(7) -0.0355(9) 0.0047(8) O3 0.0373(8) 0.0427(8) 0.0411(8) -0.0058(6) -0.0105(6) -0.0098(6) O4 0.0511(9) 0.0610(10) 0.0463(9) -0.0017(8) -0.0194(8) -0.0118(8) O5 0.0388(8) 0.0416(8) 0.0467(8) -0.0079(7) -0.0106(7) -0.0093(7) O6 0.0529(10) 0.0759(12) 0.0500(10) -0.0050(9) -0.0154(8) -0.0113(9) C1S 0.083(2) 0.085(2) 0.070(2) -0.0094(17) -0.0134(17) 0.0044(19) O1S 0.0895(15) 0.0834(15) 0.0549(12) 0.0032(10) -0.0122(10) -0.0139(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O3 1.9529(14) . ? Cu O5 1.9657(14) . ? Cu N1 2.0095(16) . ? Cu N2 2.0145(16) . ? Cu O6 2.6676(18) . ? Cu O4 2.7251(16) . ? C1 N1 1.341(3) . ? C1 C2 1.373(3) . ? C2 C3 1.381(3) . ? C3 C4 1.384(3) . ? C4 C5 1.380(3) . ? C5 N1 1.355(2) . ? C5 C6 1.440(3) . ? C6 C7 1.184(3) . ? C7 C8 1.442(3) . ? C8 C13 1.391(3) . ? C8 C9 1.411(3) . ? C9 C10 1.383(3) . ? C10 O1 1.357(2) . ? C10 C11 1.405(3) . ? C11 O2 1.365(2) . ? C11 C12 1.382(3) . ? C12 C13 1.409(3) . ? C13 C16 1.435(3) . ? C14 O1 1.435(3) . ? C15 O2 1.427(3) . ? C16 C17 1.190(3) . ? C17 C18 1.435(3) . ? C18 N2 1.354(2) . ? C18 C19 1.383(3) . ? C19 C20 1.376(3) . ? C20 C21 1.384(3) . ? C21 C22 1.367(3) . ? C22 N2 1.344(2) . ? C23 O4 1.243(2) . ? C23 O3 1.266(3) . ? C23 C24 1.503(3) . ? C25 O6 1.235(3) . ? C25 O5 1.270(3) . ? C25 C26 1.505(3) . ? C1S O1S 1.387(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu O5 163.38(6) . . ? O3 Cu N1 91.45(6) . . ? O5 Cu N1 89.67(6) . . ? O3 Cu N2 89.93(6) . . ? O5 Cu N2 90.98(6) . . ? N1 Cu N2 172.98(6) . . ? O3 Cu O6 142.19(6) . . ? O5 Cu O6 54.30(6) . . ? N1 Cu O6 91.49(6) . . ? N2 Cu O6 83.22(6) . . ? O3 Cu O4 52.99(5) . . ? O5 Cu O4 143.62(6) . . ? N1 Cu O4 88.28(6) . . ? N2 Cu O4 87.06(6) . . ? O6 Cu O4 89.45(5) . . ? N1 C1 C2 122.97(19) . . ? C1 C2 C3 119.1(2) . . ? C2 C3 C4 118.6(2) . . ? C5 C4 C3 119.5(2) . . ? N1 C5 C4 121.78(18) . . ? N1 C5 C6 116.17(17) . . ? C4 C5 C6 122.03(18) . . ? C7 C6 C5 178.9(2) . . ? C6 C7 C8 178.7(2) . . ? C13 C8 C9 119.64(17) . . ? C13 C8 C7 120.61(17) . . ? C9 C8 C7 119.75(19) . . ? C10 C9 C8 120.50(19) . . ? O1 C10 C9 124.85(18) . . ? O1 C10 C11 115.44(17) . . ? C9 C10 C11 119.70(18) . . ? O2 C11 C12 124.03(19) . . ? O2 C11 C10 115.84(17) . . ? C12 C11 C10 120.13(18) . . ? C11 C12 C13 120.44(19) . . ? C8 C13 C12 119.58(17) . . ? C8 C13 C16 121.31(17) . . ? C12 C13 C16 119.10(18) . . ? C17 C16 C13 179.3(2) . . ? C16 C17 C18 176.5(2) . . ? N2 C18 C19 122.16(17) . . ? N2 C18 C17 115.89(17) . . ? C19 C18 C17 121.94(18) . . ? C20 C19 C18 118.9(2) . . ? C19 C20 C21 119.1(2) . . ? C22 C21 C20 119.3(2) . . ? N2 C22 C21 122.6(2) . . ? O4 C23 O3 122.4(2) . . ? O4 C23 C24 120.9(2) . . ? O3 C23 C24 116.72(19) . . ? O6 C25 O5 123.3(2) . . ? O6 C25 C26 120.4(2) . . ? O5 C25 C26 116.4(2) . . ? C1 N1 C5 118.03(17) . . ? C1 N1 Cu 121.55(14) . . ? C5 N1 Cu 120.42(13) . . ? C22 N2 C18 117.99(17) . . ? C22 N2 Cu 121.93(14) . . ? C18 N2 Cu 120.08(12) . . ? C10 O1 C14 117.77(16) . . ? C11 O2 C15 116.97(16) . . ? C23 O3 Cu 110.33(13) . . ? C23 O4 Cu 74.26(12) . . ? C25 O5 Cu 107.24(14) . . ? C25 O6 Cu 75.20(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1S H1S O4 1.02 1.77 2.787(3) 173.0 1_654 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.437 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.058 data_rhzlig _database_code_CSD 173560 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H30 Cl2 N2 O10 Rh2' _chemical_formula_weight 867.29 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.5985(13) _cell_length_b 20.2480(12) _cell_length_c 8.0207(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.2650(10) _cell_angle_gamma 90.00 _cell_volume 3414.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 7157 _cell_measurement_theta_min 2.758 _cell_measurement_theta_max 25.055 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 1.180 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7982 _exptl_absorpt_correction_T_max 0.9654 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15208 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.39 _reflns_number_total 3504 _reflns_number_gt 3000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.624 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _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^)+(0.0672P)^2^+2.4149P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3504 _refine_ls_number_parameters 225 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.221555(17) 0.205224(18) 0.04622(4) 0.02362(14) Uani 1 1 d . . . C1 C 0.2048(3) 0.0631(3) 0.1640(6) 0.0373(13) Uani 1 1 d . . . H1 H 0.2425 0.0602 0.1224 0.045 Uiso 1 1 calc R . . C2 C 0.1857(3) 0.0071(3) 0.2399(7) 0.0481(15) Uani 1 1 d . . . H2 H 0.2101 -0.0324 0.2521 0.058 Uiso 1 1 calc R . . C3 C 0.1304(3) 0.0109(3) 0.2964(8) 0.0562(19) Uani 1 1 d . . . H3 H 0.1154 -0.0265 0.3468 0.067 Uiso 1 1 calc R . . C4 C 0.0973(3) 0.0689(3) 0.2795(8) 0.0553(18) Uani 1 1 d . . . H4 H 0.0587 0.0718 0.3170 0.066 Uiso 1 1 calc R . . C5 C 0.1200(2) 0.1240(3) 0.2070(7) 0.0352(12) Uani 1 1 d . . . C6 C 0.0888(3) 0.1858(3) 0.1989(7) 0.0404(14) Uani 1 1 d . . . C7 C 0.0598(2) 0.2363(3) 0.2042(7) 0.0414(14) Uani 1 1 d . . . C8 C 0.0290(3) 0.2970(3) 0.2231(7) 0.0401(13) Uani 1 1 d . . . C9 C 0.0559(3) 0.3572(3) 0.1937(8) 0.0496(15) Uani 1 1 d . . . H9 H 0.0943 0.3573 0.1550 0.060 Uiso 1 1 calc R . . C10 C 0.0283(3) 0.4167(3) 0.2191(8) 0.0563(17) Uani 1 1 d . . . C11 C 0.1042(5) 0.4795(4) 0.1171(12) 0.091(3) Uani 1 1 d . . . H11A H 0.1402 0.4567 0.1916 0.136 Uiso 1 1 calc R . . H11B H 0.1158 0.5256 0.1028 0.136 Uiso 1 1 calc R . . H11C H 0.0936 0.4577 0.0050 0.136 Uiso 1 1 calc R . . C12 C 0.2407(2) 0.3188(3) 0.2680(6) 0.0308(11) Uani 1 1 d . . . C13 C 0.2392(3) 0.3544(3) 0.4321(6) 0.0434(14) Uani 1 1 d . . . H13A H 0.2581 0.3262 0.5299 0.065 Uiso 1 1 calc R . . H13B H 0.1951 0.3646 0.4345 0.065 Uiso 1 1 calc R . . H13C H 0.2636 0.3955 0.4384 0.065 Uiso 1 1 calc R . . C14 C 0.3560(2) 0.2028(3) 0.1867(6) 0.0353(12) Uani 1 1 d . . . C15 C 0.4167(3) 0.1783(4) 0.3022(8) 0.0574(19) Uani 1 1 d . . . H15A H 0.4402 0.1515 0.2356 0.086 Uiso 1 1 calc R . . H15B H 0.4066 0.1513 0.3938 0.086 Uiso 1 1 calc R . . H15C H 0.4428 0.2160 0.3524 0.086 Uiso 1 1 calc R . . N1 N 0.17390(19) 0.1201(2) 0.1461(5) 0.0271(9) Uani 1 1 d . . . O1 O 0.0509(3) 0.4773(2) 0.1920(6) 0.0727(14) Uani 1 1 d . . . O2 O 0.21556(16) 0.26233(17) 0.2506(4) 0.0299(8) Uani 1 1 d . . . O3 O 0.26750(18) 0.34747(17) 0.1630(4) 0.0340(8) Uani 1 1 d . . . O4 O 0.30618(16) 0.16966(17) 0.1845(4) 0.0328(8) Uani 1 1 d . . . O5 O 0.35952(16) 0.25449(18) 0.1024(4) 0.0348(8) Uani 1 1 d . . . C1SA C 0.0000 0.1669(5) 0.7500 0.089(4) Uani 0.50 2 d SPD . 1 H1SA H -0.0282 0.1969 0.6691 0.106 Uiso 0.25 1 d PR . 1 H1SB H 0.0282 0.1969 0.8309 0.106 Uiso 0.25 1 d PR . 1 C1SB C 0.0000 0.1669(5) 0.7500 0.089(4) Uani 0.50 2 d SPD . 2 H1SC H -0.0384 0.1933 0.7008 0.106 Uiso 0.25 1 d PR . 2 H1SD H 0.0384 0.1933 0.7992 0.106 Uiso 0.25 1 d PR . 2 Cl1 Cl 0.0570(2) 0.1402(3) 0.6113(6) 0.0891(14) Uani 0.50 1 d PD . . Cl2 Cl 0.0105(3) 0.0927(3) 0.6482(7) 0.1047(17) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0253(2) 0.0283(2) 0.0177(2) 0.00098(15) 0.00575(14) -0.00720(16) C1 0.055(3) 0.032(3) 0.026(3) -0.005(2) 0.012(2) -0.005(2) C2 0.077(5) 0.027(3) 0.035(3) 0.000(2) 0.002(3) -0.006(3) C3 0.062(4) 0.054(4) 0.042(3) 0.021(3) -0.009(3) -0.031(3) C4 0.034(3) 0.071(5) 0.056(4) 0.028(3) 0.001(3) -0.019(3) C5 0.029(3) 0.041(3) 0.032(3) 0.009(2) 0.000(2) -0.012(2) C6 0.026(3) 0.066(4) 0.031(3) 0.018(3) 0.011(2) 0.001(3) C7 0.023(3) 0.069(4) 0.031(3) 0.011(3) 0.005(2) -0.007(3) C8 0.035(3) 0.058(4) 0.024(3) 0.002(2) 0.000(2) 0.001(3) C9 0.049(4) 0.062(4) 0.035(3) 0.009(3) 0.004(3) -0.006(3) C10 0.067(4) 0.061(4) 0.034(3) 0.006(3) 0.000(3) -0.007(4) C11 0.114(8) 0.066(5) 0.094(7) 0.027(5) 0.028(6) -0.022(5) C12 0.030(3) 0.035(3) 0.028(3) 0.000(2) 0.007(2) -0.002(2) C13 0.067(4) 0.041(3) 0.025(3) -0.005(2) 0.015(3) -0.012(3) C14 0.031(3) 0.053(3) 0.023(2) 0.003(2) 0.009(2) -0.001(2) C15 0.033(3) 0.078(5) 0.056(4) 0.035(4) 0.001(3) -0.006(3) N1 0.031(2) 0.029(2) 0.0197(19) -0.0013(16) 0.0018(16) -0.0063(17) O1 0.098(4) 0.057(3) 0.061(3) 0.009(2) 0.012(3) -0.014(3) O2 0.0361(19) 0.0342(19) 0.0219(17) -0.0055(14) 0.0117(14) -0.0089(16) O3 0.046(2) 0.0308(19) 0.0289(18) -0.0026(15) 0.0160(16) -0.0096(16) O4 0.0305(19) 0.036(2) 0.0331(19) 0.0087(16) 0.0093(15) 0.0012(16) O5 0.0300(18) 0.045(2) 0.0289(18) 0.0108(16) 0.0053(15) -0.0063(16) C1SA 0.137(12) 0.068(7) 0.052(6) 0.000 0.003(7) 0.000 C1SB 0.137(12) 0.068(7) 0.052(6) 0.000 0.003(7) 0.000 Cl1 0.090(3) 0.098(3) 0.076(3) -0.004(2) 0.012(2) 0.029(3) Cl2 0.109(4) 0.107(4) 0.099(4) 0.016(3) 0.026(3) 0.047(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O2 2.035(3) . ? Rh1 O4 2.039(3) . ? Rh1 O3 2.048(3) 7 ? Rh1 O5 2.048(3) 7 ? Rh1 N1 2.247(4) . ? Rh1 Rh1 2.4011(7) 7 ? C1 N1 1.325(7) . ? C1 C2 1.394(8) . ? C2 C3 1.372(9) . ? C3 C4 1.366(10) . ? C4 C5 1.399(7) . ? C5 N1 1.363(6) . ? C5 C6 1.416(8) . ? C6 C7 1.205(9) . ? C7 C8 1.421(9) . ? C8 C9 1.394(8) . ? C8 C8 1.416(11) 2 ? C9 C10 1.380(9) . ? C10 O1 1.356(8) . ? C10 C10 1.422(14) 2 ? C11 O1 1.416(10) . ? C12 O2 1.259(6) . ? C12 O3 1.267(6) . ? C12 C13 1.507(7) . ? C14 O5 1.258(6) . ? C14 O4 1.265(6) . ? C14 C15 1.505(7) . ? O3 Rh1 2.048(3) 7 ? O5 Rh1 2.048(3) 7 ? C1SA Cl2 1.749(9) . ? C1SA Cl2 1.749(9) 2_556 ? C1SA Cl1 1.916(6) . ? C1SA Cl1 1.916(6) 2_556 ? Cl1 Cl2 1.470(7) . ? Cl2 Cl2 1.791(11) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Rh1 O4 88.69(14) . . ? O2 Rh1 O3 175.78(13) . 7 ? O4 Rh1 O3 90.25(14) . 7 ? O2 Rh1 O5 92.22(14) . 7 ? O4 Rh1 O5 175.59(13) . 7 ? O3 Rh1 O5 88.54(15) 7 7 ? O2 Rh1 N1 91.69(13) . . ? O4 Rh1 N1 87.82(14) . . ? O3 Rh1 N1 92.35(13) 7 . ? O5 Rh1 N1 96.46(14) 7 . ? O2 Rh1 Rh1 87.21(9) . 7 ? O4 Rh1 Rh1 88.64(10) . 7 ? O3 Rh1 Rh1 88.68(9) 7 7 ? O5 Rh1 Rh1 87.09(10) 7 7 ? N1 Rh1 Rh1 176.32(10) . 7 ? N1 C1 C2 124.3(5) . . ? C3 C2 C1 117.8(6) . . ? C4 C3 C2 119.4(5) . . ? C3 C4 C5 120.1(6) . . ? N1 C5 C4 120.9(5) . . ? N1 C5 C6 118.2(4) . . ? C4 C5 C6 121.0(5) . . ? C7 C6 C5 173.9(5) . . ? C6 C7 C8 175.5(6) . . ? C9 C8 C8 118.9(4) . 2 ? C9 C8 C7 121.0(5) . . ? C8 C8 C7 120.0(3) 2 . ? C10 C9 C8 121.9(6) . . ? O1 C10 C9 125.7(6) . . ? O1 C10 C10 115.2(4) . 2 ? C9 C10 C10 119.1(4) . 2 ? O2 C12 O3 126.4(5) . . ? O2 C12 C13 115.9(4) . . ? O3 C12 C13 117.7(5) . . ? O5 C14 O4 126.1(5) . . ? O5 C14 C15 117.0(5) . . ? O4 C14 C15 116.8(5) . . ? C1 N1 C5 117.5(4) . . ? C1 N1 Rh1 116.5(3) . . ? C5 N1 Rh1 125.6(3) . . ? C10 O1 C11 117.0(6) . . ? C12 O2 Rh1 120.0(3) . . ? C12 O3 Rh1 117.5(3) . 7 ? C14 O4 Rh1 118.3(3) . . ? C14 O5 Rh1 119.7(3) . 7 ? Cl2 C1SA Cl2 61.6(5) . 2_556 ? Cl2 C1SA Cl1 47.0(3) . . ? Cl2 C1SA Cl1 101.4(5) 2_556 . ? Cl2 C1SA Cl1 101.4(5) . 2_556 ? Cl2 C1SA Cl1 47.0(3) 2_556 2_556 ? Cl1 C1SA Cl1 147.3(7) . 2_556 ? Cl2 Cl1 C1SA 60.5(3) . . ? Cl1 Cl2 C1SA 72.5(3) . . ? Cl1 Cl2 Cl2 120.7(4) . 2_556 ? C1SA Cl2 Cl2 59.2(3) . 2_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.5(8) . . . . ? C1 C2 C3 C4 -1.2(9) . . . . ? C2 C3 C4 C5 -0.8(9) . . . . ? C3 C4 C5 N1 2.7(9) . . . . ? C3 C4 C5 C6 -175.7(6) . . . . ? N1 C5 C6 C7 -156(6) . . . . ? C4 C5 C6 C7 22(6) . . . . ? C5 C6 C7 C8 70(11) . . . . ? C6 C7 C8 C9 76(8) . . . . ? C6 C7 C8 C8 -103(7) . . . 2 ? C8 C8 C9 C10 1.5(10) 2 . . . ? C7 C8 C9 C10 -176.9(6) . . . . ? C8 C9 C10 O1 -179.3(6) . . . . ? C8 C9 C10 C10 1.5(11) . . . 2 ? C2 C1 N1 C5 0.4(7) . . . . ? C2 C1 N1 Rh1 173.3(4) . . . . ? C4 C5 N1 C1 -2.4(7) . . . . ? C6 C5 N1 C1 176.0(5) . . . . ? C4 C5 N1 Rh1 -174.6(4) . . . . ? C6 C5 N1 Rh1 3.8(6) . . . . ? O2 Rh1 N1 C1 -125.4(3) . . . . ? O4 Rh1 N1 C1 -36.8(3) . . . . ? O3 Rh1 N1 C1 53.4(4) 7 . . . ? O5 Rh1 N1 C1 142.2(3) 7 . . . ? Rh1 Rh1 N1 C1 -52.8(18) 7 . . . ? O2 Rh1 N1 C5 46.9(4) . . . . ? O4 Rh1 N1 C5 135.5(4) . . . . ? O3 Rh1 N1 C5 -134.4(4) 7 . . . ? O5 Rh1 N1 C5 -45.6(4) 7 . . . ? Rh1 Rh1 N1 C5 119.4(15) 7 . . . ? C9 C10 O1 C11 5.9(10) . . . . ? C10 C10 O1 C11 -174.9(7) 2 . . . ? O3 C12 O2 Rh1 4.6(7) . . . . ? C13 C12 O2 Rh1 -174.2(4) . . . . ? O4 Rh1 O2 C12 87.5(4) . . . . ? O3 Rh1 O2 C12 12(2) 7 . . . ? O5 Rh1 O2 C12 -88.2(4) 7 . . . ? N1 Rh1 O2 C12 175.3(4) . . . . ? Rh1 Rh1 O2 C12 -1.2(4) 7 . . . ? O2 C12 O3 Rh1 -5.6(7) . . . 7 ? C13 C12 O3 Rh1 173.1(4) . . . 7 ? O5 C14 O4 Rh1 -4.6(7) . . . . ? C15 C14 O4 Rh1 174.8(4) . . . . ? O2 Rh1 O4 C14 -84.1(4) . . . . ? O3 Rh1 O4 C14 91.8(4) 7 . . . ? O5 Rh1 O4 C14 18(2) 7 . . . ? N1 Rh1 O4 C14 -175.9(4) . . . . ? Rh1 Rh1 O4 C14 3.1(4) 7 . . . ? O4 C14 O5 Rh1 3.3(7) . . . 7 ? C15 C14 O5 Rh1 -176.1(4) . . . 7 ? Cl2 C1SA Cl1 Cl2 31.6(5) 2_556 . . . ? Cl1 C1SA Cl1 Cl2 18.2(3) 2_556 . . . ? C1SA Cl1 Cl2 Cl2 -35.7(4) . . . 2_556 ? Cl2 C1SA Cl2 Cl1 -144.3(5) 2_556 . . . ? Cl1 C1SA Cl2 Cl1 -170.1(2) 2_556 . . . ? Cl1 C1SA Cl2 Cl2 144.3(5) . . . 2_556 ? Cl1 C1SA Cl2 Cl2 -25.8(4) 2_556 . . 2_556 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.404 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.121