# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 871906' #TrackingRef 'Laurila.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 N2 O2 Rh, C2 Cl2 O2 Rh' _chemical_formula_sum 'C14 H8 Cl2 N2 O4 Rh2' _chemical_formula_weight 544.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4' _symmetry_space_group_name_Hall 'I -4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 22.1438(8) _cell_length_b 22.1438(8) _cell_length_c 6.7080(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3289.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3740 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 33.77 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 2.352 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6648 _exptl_absorpt_correction_T_max 0.8776 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'flat graphite crystal' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on three-circle goniostat' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_measurement_method '\f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9669 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3785 _reflns_number_gt 3504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2e (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.59(3) _chemical_absolute_configuration unk _refine_ls_number_reflns 3785 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0522 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.207829(12) 0.489708(12) 0.63516(4) 0.01273(7) Uani 1 1 d . . . Rh2 Rh 0.217737(12) 0.482910(13) 0.14220(5) 0.01492(7) Uani 1 1 d . . . Cl1 Cl 0.32197(4) 0.50117(4) 0.20209(14) 0.0196(2) Uani 1 1 d . . . Cl2 Cl 0.19804(4) 0.58758(4) 0.12619(17) 0.0211(2) Uani 1 1 d . . . O1 O 0.07874(11) 0.45093(13) 0.5906(5) 0.0286(8) Uani 1 1 d . . . O2 O 0.16333(12) 0.61734(11) 0.6119(4) 0.0232(6) Uani 1 1 d . . . O3 O 0.24766(13) 0.35202(11) 0.1259(5) 0.0296(7) Uani 1 1 d . . . O4 O 0.08627(13) 0.45877(13) 0.0906(5) 0.0306(8) Uani 1 1 d . . . N1 N 0.29745(13) 0.51090(13) 0.6935(4) 0.0149(7) Uani 1 1 d . . . N2 N 0.24720(12) 0.40490(13) 0.6339(6) 0.0135(6) Uani 1 1 d . . . C1 C 0.12776(17) 0.46503(16) 0.6007(6) 0.0180(9) Uani 1 1 d . . . C2 C 0.18007(16) 0.56928(16) 0.6227(8) 0.0179(8) Uani 1 1 d . . . C3 C 0.23544(17) 0.40197(17) 0.1369(7) 0.0200(9) Uani 1 1 d . . . C4 C 0.13662(19) 0.46794(17) 0.1064(6) 0.0211(9) Uani 1 1 d . . . C10 C 0.31880(17) 0.56689(17) 0.7239(6) 0.0211(9) Uani 1 1 d . . . H10 H 0.2912 0.5998 0.7245 0.025 Uiso 1 1 calc R . . C11 C 0.37922(17) 0.57836(18) 0.7543(6) 0.0243(9) Uani 1 1 d . . . H11 H 0.3935 0.6185 0.7715 0.029 Uiso 1 1 calc R . . C12 C 0.41857(17) 0.52964(19) 0.7591(6) 0.0254(9) Uani 1 1 d . . . H12 H 0.4605 0.5362 0.7796 0.030 Uiso 1 1 calc R . . C13 C 0.39689(17) 0.47180(18) 0.7341(7) 0.0219(9) Uani 1 1 d . . . H13 H 0.4235 0.4382 0.7392 0.026 Uiso 1 1 calc R . . C14 C 0.33540(16) 0.46337(16) 0.7013(6) 0.0158(8) Uani 1 1 d . . . C15 C 0.30752(15) 0.40409(15) 0.6732(5) 0.0134(7) Uani 1 1 d . . . C16 C 0.33864(16) 0.34948(16) 0.6864(6) 0.0188(8) Uani 1 1 d . . . H16 H 0.3804 0.3490 0.7189 0.023 Uiso 1 1 calc R . . C17 C 0.30798(16) 0.29569(15) 0.6515(6) 0.0206(8) Uani 1 1 d . . . H17 H 0.3285 0.2581 0.6612 0.025 Uiso 1 1 calc R . . C18 C 0.24723(16) 0.29750(16) 0.6026(6) 0.0199(8) Uani 1 1 d . . . H18 H 0.2256 0.2615 0.5735 0.024 Uiso 1 1 calc R . . C19 C 0.21901(16) 0.35294(16) 0.5972(6) 0.0167(8) Uani 1 1 d . . . H19 H 0.1772 0.3542 0.5655 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01069(13) 0.01128(14) 0.01622(15) -0.00065(13) -0.00017(13) 0.00034(11) Rh2 0.02145(15) 0.00995(14) 0.01337(14) 0.00049(14) -0.00180(14) 0.00159(11) Cl1 0.0220(5) 0.0177(4) 0.0193(5) -0.0003(4) -0.0012(4) 0.0039(4) Cl2 0.0291(5) 0.0116(4) 0.0227(5) 0.0001(4) -0.0068(5) 0.0036(4) O1 0.0111(13) 0.0282(16) 0.046(2) -0.0028(14) -0.0026(14) 0.0000(11) O2 0.0334(14) 0.0177(13) 0.0185(15) -0.0008(12) -0.0010(14) 0.0064(11) O3 0.0455(17) 0.0123(12) 0.0310(17) 0.0005(14) 0.0028(17) 0.0059(12) O4 0.0297(16) 0.0260(16) 0.036(2) -0.0009(14) -0.0044(15) -0.0025(13) N1 0.0174(15) 0.0164(15) 0.0109(15) 0.0005(13) -0.0028(13) -0.0031(12) N2 0.0120(13) 0.0143(14) 0.0143(16) 0.0001(15) -0.0020(15) -0.0007(11) C1 0.0214(19) 0.0112(17) 0.021(2) 0.0022(16) -0.0005(18) 0.0053(16) C2 0.0187(17) 0.0193(19) 0.016(2) 0.0008(19) 0.0002(19) 0.0036(15) C3 0.0287(19) 0.0225(19) 0.0087(19) 0.0062(19) 0.005(2) -0.0008(16) C4 0.030(2) 0.0162(18) 0.017(2) -0.0002(17) -0.0019(19) 0.0044(17) C10 0.024(2) 0.0154(18) 0.024(2) 0.0004(16) 0.0014(17) -0.0059(16) C11 0.024(2) 0.024(2) 0.025(2) 0.0013(17) -0.0038(18) -0.0128(18) C12 0.0136(18) 0.034(2) 0.029(2) 0.0003(19) -0.0008(16) -0.0083(18) C13 0.0153(18) 0.027(2) 0.024(2) 0.0003(17) -0.0012(16) -0.0001(16) C14 0.0169(18) 0.0184(18) 0.0122(18) -0.0005(15) 0.0032(14) -0.0050(15) C15 0.0119(15) 0.0162(16) 0.0120(19) -0.0015(15) 0.0029(14) 0.0021(13) C16 0.0152(17) 0.0225(19) 0.019(2) 0.0009(16) -0.0008(15) 0.0031(15) C17 0.0230(18) 0.0177(17) 0.021(2) 0.0025(18) 0.0032(18) 0.0047(14) C18 0.0234(18) 0.0118(16) 0.025(2) 0.0012(15) -0.0008(17) -0.0036(14) C19 0.0184(17) 0.0144(17) 0.017(2) 0.0008(15) 0.0015(16) -0.0005(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 Rh1 C2 1.868(3) . yes Rh1 C1 1.870(4) . yes Rh1 N2 2.070(3) . yes Rh1 N1 2.077(3) . yes Rh1 Rh2 3.3174(5) . yes Rh1 Rh2 3.4116(5) 1_556 yes Rh2 C3 1.835(4) . yes Rh2 C4 1.842(4) . yes Rh2 Cl2 2.3608(9) . yes Rh2 Cl1 2.3774(10) . yes O1 C1 1.132(4) . ? O2 C2 1.129(4) . ? O3 C3 1.141(4) . ? O4 C4 1.138(5) . ? N1 C10 1.342(5) . ? N1 C14 1.348(5) . ? N2 C19 1.332(4) . ? N2 C15 1.362(4) . ? C10 C11 1.377(5) . ? C10 H10 0.9500 . ? C11 C12 1.387(6) . ? C11 H11 0.9500 . ? C12 C13 1.378(5) . ? C12 H12 0.9500 . ? C13 C14 1.392(5) . ? C13 H13 0.9500 . ? C14 C15 1.463(5) . ? C15 C16 1.395(5) . ? C16 C17 1.391(5) . ? C16 H16 0.9500 . ? C17 C18 1.385(5) . ? C17 H17 0.9500 . ? C18 C19 1.378(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Rh1 C1 87.59(15) . . yes C2 Rh1 N2 173.68(14) . . ? C1 Rh1 N2 97.69(13) . . ? C2 Rh1 N1 96.31(14) . . ? C1 Rh1 N1 174.66(14) . . ? N2 Rh1 N1 78.65(11) . . yes C2 Rh1 Rh2 91.14(16) . . ? C1 Rh1 Rh2 85.77(13) . . ? N2 Rh1 Rh2 85.82(11) . . ? N1 Rh1 Rh2 97.75(8) . . ? C2 Rh1 Rh2 96.17(16) . 1_556 ? C1 Rh1 Rh2 99.86(13) . 1_556 ? N2 Rh1 Rh2 86.38(11) . 1_556 ? N1 Rh1 Rh2 76.15(8) . 1_556 ? Rh2 Rh1 Rh2 170.927(11) . 1_556 yes C3 Rh2 C4 91.72(17) . . yes C3 Rh2 Cl2 175.92(14) . . ? C4 Rh2 Cl2 89.46(12) . . ? C3 Rh2 Cl1 87.82(12) . . ? C4 Rh2 Cl1 177.71(14) . . ? Cl2 Rh2 Cl1 91.15(3) . . yes C3 Rh2 Rh1 94.46(15) . . ? C4 Rh2 Rh1 94.22(13) . . ? Cl2 Rh2 Rh1 89.35(3) . . ? Cl1 Rh2 Rh1 83.57(2) . . ? C10 N1 C14 119.7(3) . . ? C10 N1 Rh1 125.0(3) . . ? C14 N1 Rh1 115.3(2) . . ? C19 N2 C15 119.0(3) . . ? C19 N2 Rh1 125.9(2) . . ? C15 N2 Rh1 115.1(2) . . ? O1 C1 Rh1 176.2(4) . . ? O2 C2 Rh1 178.9(5) . . ? O3 C3 Rh2 177.1(4) . . ? O4 C4 Rh2 177.8(4) . . ? N1 C10 C11 122.4(4) . . ? N1 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C12 118.0(4) . . ? C10 C11 H11 121.0 . . ? C12 C11 H11 121.0 . . ? C13 C12 C11 120.1(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.0(4) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? N1 C14 C13 120.8(3) . . ? N1 C14 C15 115.6(3) . . ? C13 C14 C15 123.6(3) . . ? N2 C15 C16 120.6(3) . . ? N2 C15 C14 115.3(3) . . ? C16 C15 C14 124.1(3) . . ? C17 C16 C15 119.4(3) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 119.3(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 118.2(4) . . ? C19 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? N2 C19 C18 123.5(3) . . ? N2 C19 H19 118.2 . . ? C18 C19 H19 118.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.150 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.089 data_2 _database_code_depnum_ccdc_archive 'CCDC 871907' #TrackingRef 'Laurila.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H8 N2 O2 Rh, C2 Cl2 O2 Rh' _chemical_formula_sum 'C16 H8 Cl2 N2 O4 Rh2' _chemical_formula_weight 568.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 6.56520(10) _cell_length_b 16.7058(4) _cell_length_c 16.9994(4) _cell_angle_alpha 72.6080(10) _cell_angle_beta 80.9340(10) _cell_angle_gamma 86.5110(10) _cell_volume 1756.79(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5709 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 30.16 _exptl_crystal_description needle _exptl_crystal_colour 'red, lustrous' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 2.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6641 _exptl_absorpt_correction_T_max 0.9530 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'curved graphite crystal' _diffrn_measurement_device_type 'Bruker KAPPA APEX II DUO CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15324 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.17 _reflns_number_total 10077 _reflns_number_gt 7971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2e (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10077 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0508 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 0.07716(3) 0.463557(12) 0.305024(12) 0.01515(4) Uani 1 1 d . . . Rh2 Rh 0.58720(3) 0.461659(13) 0.289042(12) 0.01635(4) Uani 1 1 d . . . Cl1 Cl 0.63530(11) 0.59337(4) 0.18461(4) 0.02465(13) Uani 1 1 d . . . Cl2 Cl 0.65528(9) 0.38474(4) 0.19087(4) 0.01847(12) Uani 1 1 d . . . O1 O 0.0555(3) 0.64602(12) 0.29517(13) 0.0300(5) Uani 1 1 d . . . O2 O -0.0344(4) 0.42244(13) 0.49009(12) 0.0341(5) Uani 1 1 d . . . O3 O 0.4779(4) 0.55615(16) 0.41329(15) 0.0441(6) Uani 1 1 d . . . O4 O 0.5240(3) 0.29461(14) 0.41551(13) 0.0338(5) Uani 1 1 d . . . N1 N 0.0923(3) 0.33940(13) 0.30344(13) 0.0161(4) Uani 1 1 d . . . N2 N 0.1500(3) 0.48113(13) 0.17759(13) 0.0164(4) Uani 1 1 d . . . C1 C 0.0645(4) 0.57712(17) 0.29852(16) 0.0199(5) Uani 1 1 d . . . C2 C 0.0087(4) 0.43846(16) 0.42015(17) 0.0207(5) Uani 1 1 d . . . C3 C 0.5224(4) 0.51942(19) 0.36693(19) 0.0274(6) Uani 1 1 d . . . C4 C 0.5483(4) 0.35921(18) 0.36854(17) 0.0226(5) Uani 1 1 d . . . C10 C 0.0628(4) 0.26928(16) 0.36748(16) 0.0187(5) Uani 1 1 d . . . H10 H 0.0319 0.2741 0.4224 0.022 Uiso 1 1 calc R . . C11 C 0.0755(4) 0.18943(17) 0.35661(17) 0.0218(5) Uani 1 1 d . . . H11 H 0.0521 0.1410 0.4034 0.026 Uiso 1 1 calc R . . C12 C 0.1222(4) 0.18163(16) 0.27771(17) 0.0210(5) Uani 1 1 d . . . H12 H 0.1339 0.1276 0.2696 0.025 Uiso 1 1 calc R . . C13 C 0.1527(4) 0.25376(16) 0.20905(16) 0.0183(5) Uani 1 1 d . . . C14 C 0.2008(4) 0.25195(18) 0.12424(17) 0.0229(5) Uani 1 1 d . . . H14 H 0.2116 0.1995 0.1126 0.028 Uiso 1 1 calc R . . C15 C 0.2312(4) 0.32402(18) 0.06029(17) 0.0229(5) Uani 1 1 d . . . H15 H 0.2634 0.3212 0.0047 0.028 Uiso 1 1 calc R . . C16 C 0.2156(4) 0.40409(17) 0.07545(16) 0.0200(5) Uani 1 1 d . . . C17 C 0.2471(4) 0.48095(17) 0.01200(16) 0.0208(5) Uani 1 1 d . . . H17 H 0.2807 0.4816 -0.0446 0.025 Uiso 1 1 calc R . . C18 C 0.2292(4) 0.55449(18) 0.03234(17) 0.0226(5) Uani 1 1 d . . . H18 H 0.2496 0.6066 -0.0100 0.027 Uiso 1 1 calc R . . C19 C 0.1804(4) 0.55257(16) 0.11633(16) 0.0198(5) Uani 1 1 d . . . H19 H 0.1686 0.6040 0.1299 0.024 Uiso 1 1 calc R . . C20 C 0.1687(4) 0.40760(16) 0.15759(15) 0.0153(5) Uani 1 1 d . . . C21 C 0.1370(3) 0.33175(16) 0.22499(15) 0.0154(5) Uani 1 1 d . . . Rh1B Rh 0.32556(3) 0.120645(12) 0.663828(12) 0.01583(4) Uani 1 1 d . . . Rh2B Rh -0.18550(3) 0.109368(12) 0.700679(12) 0.01524(4) Uani 1 1 d . . . Cl1B Cl -0.13029(10) 0.03365(4) 0.60179(4) 0.02222(13) Uani 1 1 d . . . Cl2B Cl -0.18754(9) -0.01368(4) 0.81585(4) 0.01771(11) Uani 1 1 d . . . O1B O 0.4094(3) 0.09895(14) 0.49224(12) 0.0305(5) Uani 1 1 d . . . O2B O 0.2765(3) 0.30484(13) 0.58262(13) 0.0329(5) Uani 1 1 d . . . O3B O -0.2079(3) 0.26278(13) 0.55762(13) 0.0305(5) Uani 1 1 d . . . O4B O -0.2511(3) 0.20173(12) 0.82820(12) 0.0255(4) Uani 1 1 d . . . N1B N 0.2837(3) 0.12524(13) 0.78603(12) 0.0146(4) Uani 1 1 d . . . N2B N 0.3358(3) -0.00683(13) 0.72677(13) 0.0163(4) Uani 1 1 d . . . C1B C 0.3756(4) 0.10706(17) 0.55686(16) 0.0217(5) Uani 1 1 d . . . C2B C 0.2980(4) 0.23532(18) 0.61415(16) 0.0214(5) Uani 1 1 d . . . C3B C -0.1981(4) 0.20454(17) 0.61324(16) 0.0205(5) Uani 1 1 d . . . C4B C -0.2260(4) 0.16825(16) 0.77831(16) 0.0185(5) Uani 1 1 d . . . C10B C 0.2605(4) 0.19185(16) 0.81502(16) 0.0176(5) Uani 1 1 d . . . H10B H 0.2597 0.2462 0.7762 0.021 Uiso 1 1 calc R . . C11B C 0.2377(4) 0.18513(17) 0.89939(17) 0.0220(5) Uani 1 1 d . . . H11B H 0.2206 0.2341 0.9173 0.026 Uiso 1 1 calc R . . C12B C 0.2398(4) 0.10755(18) 0.95648(17) 0.0230(5) Uani 1 1 d . . . H12B H 0.2250 0.1023 1.0143 0.028 Uiso 1 1 calc R . . C13B C 0.2641(4) 0.03544(17) 0.92884(16) 0.0190(5) Uani 1 1 d . . . C14B C 0.2677(4) -0.04862(18) 0.98382(16) 0.0226(5) Uani 1 1 d . . . H14B H 0.2548 -0.0575 1.0422 0.027 Uiso 1 1 calc R . . C15B C 0.2891(4) -0.11545(18) 0.95339(17) 0.0228(5) Uani 1 1 d . . . H15B H 0.2894 -0.1704 0.9911 0.027 Uiso 1 1 calc R . . C16B C 0.3114(4) -0.10513(16) 0.86579(16) 0.0190(5) Uani 1 1 d . . . C17B C 0.3336(4) -0.17166(17) 0.83039(18) 0.0229(5) Uani 1 1 d . . . H17B H 0.3319 -0.2281 0.8651 0.028 Uiso 1 1 calc R . . C18B C 0.3578(4) -0.15465(17) 0.74506(18) 0.0239(6) Uani 1 1 d . . . H18B H 0.3737 -0.1992 0.7204 0.029 Uiso 1 1 calc R . . C19B C 0.3586(4) -0.07161(17) 0.69515(17) 0.0224(5) Uani 1 1 d . . . H19B H 0.3762 -0.0606 0.6364 0.027 Uiso 1 1 calc R . . C20B C 0.3120(3) -0.02323(16) 0.81096(15) 0.0154(5) Uani 1 1 d . . . C21B C 0.2853(3) 0.04720(16) 0.84292(15) 0.0153(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 Rh1 0.01786(9) 0.01301(9) 0.01477(9) -0.00475(7) -0.00172(7) 0.00001(7) Rh2 0.01470(9) 0.01780(10) 0.01662(9) -0.00490(7) -0.00253(7) -0.00101(7) Cl1 0.0299(3) 0.0169(3) 0.0258(3) -0.0032(2) -0.0055(3) -0.0014(2) Cl2 0.0183(3) 0.0185(3) 0.0188(3) -0.0056(2) -0.0032(2) -0.0002(2) O1 0.0425(12) 0.0172(10) 0.0283(11) -0.0063(8) 0.0001(9) -0.0007(9) O2 0.0621(15) 0.0200(10) 0.0185(10) -0.0059(8) 0.0026(9) -0.0089(10) O3 0.0456(14) 0.0537(16) 0.0437(14) -0.0334(13) 0.0004(11) -0.0043(12) O4 0.0397(12) 0.0321(12) 0.0234(11) 0.0038(9) -0.0070(9) -0.0068(10) N1 0.0161(10) 0.0161(10) 0.0163(10) -0.0049(8) -0.0030(8) 0.0006(8) N2 0.0147(10) 0.0173(10) 0.0175(10) -0.0054(8) -0.0028(8) 0.0006(8) C1 0.0218(13) 0.0194(13) 0.0175(12) -0.0057(10) 0.0000(9) 0.0001(10) C2 0.0256(13) 0.0110(11) 0.0256(14) -0.0052(10) -0.0040(10) -0.0015(10) C3 0.0235(14) 0.0299(15) 0.0300(15) -0.0107(12) -0.0027(11) -0.0040(12) C4 0.0189(12) 0.0301(15) 0.0197(13) -0.0080(11) -0.0030(10) -0.0021(11) C10 0.0217(12) 0.0176(12) 0.0166(12) -0.0048(9) -0.0030(9) -0.0004(10) C11 0.0246(13) 0.0171(12) 0.0230(13) -0.0028(10) -0.0067(10) -0.0020(10) C12 0.0212(13) 0.0149(12) 0.0286(14) -0.0078(10) -0.0065(10) 0.0017(10) C13 0.0157(11) 0.0193(12) 0.0222(12) -0.0090(10) -0.0045(9) 0.0013(9) C14 0.0238(13) 0.0236(14) 0.0265(14) -0.0146(11) -0.0054(11) 0.0019(11) C15 0.0254(13) 0.0268(14) 0.0186(12) -0.0102(11) -0.0030(10) 0.0007(11) C16 0.0158(12) 0.0263(14) 0.0191(12) -0.0080(10) -0.0036(9) -0.0006(10) C17 0.0154(11) 0.0292(15) 0.0175(12) -0.0066(10) -0.0024(9) 0.0002(10) C18 0.0213(13) 0.0234(13) 0.0195(12) -0.0005(10) -0.0033(10) -0.0013(10) C19 0.0192(12) 0.0177(12) 0.0209(12) -0.0038(10) -0.0022(9) -0.0004(10) C20 0.0129(11) 0.0181(12) 0.0160(11) -0.0058(9) -0.0034(8) 0.0000(9) C21 0.0099(10) 0.0193(12) 0.0175(11) -0.0058(9) -0.0031(8) 0.0005(9) Rh1B 0.01800(9) 0.01667(10) 0.01284(9) -0.00477(7) -0.00120(7) -0.00088(7) Rh2B 0.01376(9) 0.01580(9) 0.01587(9) -0.00433(7) -0.00158(7) -0.00107(7) Cl1B 0.0265(3) 0.0221(3) 0.0196(3) -0.0087(2) -0.0025(2) -0.0006(2) Cl2B 0.0176(3) 0.0175(3) 0.0174(3) -0.0039(2) -0.0028(2) -0.0004(2) O1B 0.0380(12) 0.0374(12) 0.0170(10) -0.0098(9) -0.0030(8) -0.0009(9) O2B 0.0395(12) 0.0239(11) 0.0299(11) -0.0025(9) -0.0010(9) 0.0033(9) O3B 0.0352(11) 0.0258(11) 0.0255(11) 0.0003(9) -0.0034(9) -0.0048(9) O4B 0.0312(11) 0.0224(10) 0.0228(10) -0.0078(8) -0.0009(8) -0.0026(8) N1B 0.0127(9) 0.0163(10) 0.0146(9) -0.0040(8) -0.0019(7) -0.0016(8) N2B 0.0162(10) 0.0163(10) 0.0174(10) -0.0070(8) -0.0009(8) -0.0005(8) C1B 0.0237(13) 0.0206(13) 0.0193(13) -0.0041(10) -0.0023(10) -0.0007(10) C2B 0.0196(12) 0.0264(14) 0.0173(12) -0.0064(10) 0.0004(9) -0.0022(10) C3B 0.0200(12) 0.0231(13) 0.0196(12) -0.0083(10) -0.0004(9) -0.0048(10) C4B 0.0163(11) 0.0163(12) 0.0208(12) -0.0024(10) -0.0019(9) -0.0023(9) C10B 0.0168(11) 0.0178(12) 0.0184(12) -0.0062(10) -0.0013(9) -0.0007(9) C11B 0.0229(13) 0.0242(14) 0.0233(13) -0.0135(11) -0.0027(10) -0.0019(11) C12B 0.0212(13) 0.0329(15) 0.0177(12) -0.0117(11) -0.0018(10) -0.0025(11) C13B 0.0165(11) 0.0228(13) 0.0182(12) -0.0063(10) -0.0034(9) -0.0012(10) C14B 0.0240(13) 0.0265(14) 0.0153(12) -0.0016(10) -0.0043(10) -0.0033(11) C15B 0.0194(12) 0.0232(14) 0.0207(13) 0.0021(10) -0.0035(10) -0.0024(10) C16B 0.0124(11) 0.0197(13) 0.0225(13) -0.0025(10) -0.0016(9) -0.0021(9) C17B 0.0179(12) 0.0173(13) 0.0319(15) -0.0039(11) -0.0040(10) -0.0034(10) C18B 0.0213(13) 0.0196(13) 0.0334(15) -0.0122(11) -0.0020(11) -0.0017(10) C19B 0.0243(13) 0.0208(13) 0.0234(13) -0.0101(11) -0.0007(10) 0.0000(10) C20B 0.0099(10) 0.0187(12) 0.0173(12) -0.0043(9) -0.0019(8) -0.0020(9) C21B 0.0098(10) 0.0190(12) 0.0175(11) -0.0056(9) -0.0017(8) -0.0039(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 Rh1 C2 1.861(3) . yes Rh1 C1 1.865(3) . yes Rh1 N2 2.078(2) . yes Rh1 N1 2.078(2) . yes Rh1 Rh2 3.2734(3) 1_455 yes Rh1 Rh2 3.3155(3) . yes Rh2 C4 1.839(3) . yes Rh2 C3 1.844(3) . yes Rh2 Cl2 2.3692(6) . yes Rh2 Cl1 2.3803(7) . yes O1 C1 1.134(3) . ? O2 C2 1.131(3) . ? O3 C3 1.130(4) . ? O4 C4 1.137(3) . ? N1 C10 1.339(3) . ? N1 C21 1.362(3) . ? N2 C19 1.330(3) . ? N2 C20 1.363(3) . ? C10 C11 1.396(4) . ? C10 H10 0.9500 . ? C11 C12 1.371(4) . ? C11 H11 0.9500 . ? C12 C13 1.403(4) . ? C12 H12 0.9500 . ? C13 C21 1.402(3) . ? C13 C14 1.436(4) . ? C14 C15 1.360(4) . ? C14 H14 0.9500 . ? C15 C16 1.431(4) . ? C15 H15 0.9500 . ? C16 C20 1.400(3) . ? C16 C17 1.410(4) . ? C17 C18 1.366(4) . ? C17 H17 0.9500 . ? C18 C19 1.404(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.432(3) . ? Rh1B C2B 1.859(3) . yes Rh1B C1B 1.875(3) . yes Rh1B N1B 2.076(2) . yes Rh1B N2B 2.080(2) . yes Rh1B Rh2B 3.3211(3) . yes Rh1B Rh2B 3.3498(3) 1_655 yes Rh2B C3B 1.831(3) . yes Rh2B C4B 1.848(3) . yes Rh2B Cl1B 2.3624(7) . yes Rh2B Cl2B 2.3766(6) . yes O1B C1B 1.133(3) . ? O2B C2B 1.135(3) . ? O3B C3B 1.143(3) . ? O4B C4B 1.135(3) . ? N1B C10B 1.337(3) . ? N1B C21B 1.372(3) . ? N2B C19B 1.336(3) . ? N2B C20B 1.359(3) . ? C10B C11B 1.389(4) . ? C10B H10B 0.9500 . ? C11B C12B 1.368(4) . ? C11B H11B 0.9500 . ? C12B C13B 1.410(4) . ? C12B H12B 0.9500 . ? C13B C21B 1.400(3) . ? C13B C14B 1.437(4) . ? C14B C15B 1.355(4) . ? C14B H14B 0.9500 . ? C15B C16B 1.432(4) . ? C15B H15B 0.9500 . ? C16B C17B 1.404(4) . ? C16B C20B 1.406(3) . ? C17B C18B 1.377(4) . ? C17B H17B 0.9500 . ? C18B C19B 1.393(4) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? C20B C21B 1.427(3) . ? 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 C2 Rh1 C1 88.65(11) . . yes C2 Rh1 N2 175.24(10) . . ? C1 Rh1 N2 96.04(10) . . ? C2 Rh1 N1 95.20(10) . . ? C1 Rh1 N1 176.07(10) . . ? N2 Rh1 N1 80.10(8) . . yes C2 Rh1 Rh2 89.50(8) . 1_455 ? C1 Rh1 Rh2 92.14(8) . 1_455 ? N2 Rh1 Rh2 89.52(5) . 1_455 ? N1 Rh1 Rh2 87.16(6) . 1_455 ? C2 Rh1 Rh2 99.71(8) . . ? C1 Rh1 Rh2 91.20(8) . . ? N2 Rh1 Rh2 81.04(5) . . ? N1 Rh1 Rh2 88.89(6) . . ? Rh2 Rh1 Rh2 170.275(9) 1_455 . yes C4 Rh2 C3 92.63(13) . . yes C4 Rh2 Cl2 86.05(9) . . ? C3 Rh2 Cl2 177.38(9) . . ? C4 Rh2 Cl1 179.06(9) . . ? C3 Rh2 Cl1 88.13(10) . . ? Cl2 Rh2 Cl1 93.18(2) . . yes C4 Rh2 Rh1 83.72(8) . . ? C3 Rh2 Rh1 80.66(9) . . ? Cl2 Rh2 Rh1 96.936(16) . . ? Cl1 Rh2 Rh1 95.860(18) . . ? C10 N1 C21 118.2(2) . . ? C10 N1 Rh1 128.97(17) . . ? C21 N1 Rh1 112.83(16) . . ? C19 N2 C20 118.4(2) . . ? C19 N2 Rh1 128.73(18) . . ? C20 N2 Rh1 112.83(16) . . ? O1 C1 Rh1 179.4(3) . . ? O2 C2 Rh1 179.1(3) . . ? O3 C3 Rh2 177.8(3) . . ? O4 C4 Rh2 177.6(3) . . ? N1 C10 C11 122.5(2) . . ? N1 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C12 C11 C10 119.3(2) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 119.7(2) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C21 C13 C12 117.6(2) . . ? C21 C13 C14 118.6(2) . . ? C12 C13 C14 123.8(2) . . ? C15 C14 C13 121.1(2) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 121.0(2) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C20 C16 C17 117.2(2) . . ? C20 C16 C15 119.0(2) . . ? C17 C16 C15 123.7(2) . . ? C18 C17 C16 119.7(2) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.5(2) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? N2 C19 C18 122.2(2) . . ? N2 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? N2 C20 C16 122.9(2) . . ? N2 C20 C21 117.1(2) . . ? C16 C20 C21 120.0(2) . . ? N1 C21 C13 122.6(2) . . ? N1 C21 C20 117.1(2) . . ? C13 C21 C20 120.2(2) . . ? C2B Rh1B C1B 88.25(11) . . yes C2B Rh1B N1B 96.59(10) . . ? C1B Rh1B N1B 174.79(10) . . ? C2B Rh1B N2B 175.26(10) . . ? C1B Rh1B N2B 95.34(10) . . ? N1B Rh1B N2B 79.94(8) . . yes C2B Rh1B Rh2B 88.49(8) . . ? C1B Rh1B Rh2B 100.20(8) . . ? N1B Rh1B Rh2B 81.92(5) . . ? N2B Rh1B Rh2B 87.83(6) . . ? C2B Rh1B Rh2B 100.49(8) . 1_655 ? C1B Rh1B Rh2B 98.40(8) . 1_655 ? N1B Rh1B Rh2B 78.86(5) . 1_655 ? N2B Rh1B Rh2B 82.09(6) . 1_655 ? Rh2B Rh1B Rh2B 159.573(9) . 1_655 yes C3B Rh2B C4B 92.89(11) . . yes C3B Rh2B Cl1B 87.36(8) . . ? C4B Rh2B Cl1B 179.41(8) . . ? C3B Rh2B Cl2B 177.11(8) . . ? C4B Rh2B Cl2B 86.38(8) . . ? Cl1B Rh2B Cl2B 93.39(2) . . yes C3B Rh2B Rh1B 88.89(8) . . ? C4B Rh2B Rh1B 96.76(8) . . ? Cl1B Rh2B Rh1B 82.718(17) . . ? Cl2B Rh2B Rh1B 93.974(16) . . ? C10B N1B C21B 117.8(2) . . ? C10B N1B Rh1B 129.42(17) . . ? C21B N1B Rh1B 112.76(16) . . ? C19B N2B C20B 118.3(2) . . ? C19B N2B Rh1B 128.52(18) . . ? C20B N2B Rh1B 113.19(16) . . ? O1B C1B Rh1B 178.8(2) . . ? O2B C2B Rh1B 177.9(2) . . ? O3B C3B Rh2B 178.3(2) . . ? O4B C4B Rh2B 177.5(2) . . ? N1B C10B C11B 122.9(2) . . ? N1B C10B H10B 118.5 . . ? C11B C10B H10B 118.5 . . ? C12B C11B C10B 119.6(2) . . ? C12B C11B H11B 120.2 . . ? C10B C11B H11B 120.2 . . ? C11B C12B C13B 119.5(2) . . ? C11B C12B H12B 120.3 . . ? C13B C12B H12B 120.3 . . ? C21B C13B C12B 117.6(2) . . ? C21B C13B C14B 118.7(2) . . ? C12B C13B C14B 123.7(2) . . ? C15B C14B C13B 120.8(2) . . ? C15B C14B H14B 119.6 . . ? C13B C14B H14B 119.6 . . ? C14B C15B C16B 121.5(2) . . ? C14B C15B H15B 119.2 . . ? C16B C15B H15B 119.2 . . ? C17B C16B C20B 117.3(2) . . ? C17B C16B C15B 124.3(2) . . ? C20B C16B C15B 118.4(2) . . ? C18B C17B C16B 119.6(2) . . ? C18B C17B H17B 120.2 . . ? C16B C17B H17B 120.2 . . ? C17B C18B C19B 119.4(3) . . ? C17B C18B H18B 120.3 . . ? C19B C18B H18B 120.3 . . ? N2B C19B C18B 122.5(3) . . ? N2B C19B H19B 118.7 . . ? C18B C19B H19B 118.7 . . ? N2B C20B C16B 122.9(2) . . ? N2B C20B C21B 117.0(2) . . ? C16B C20B C21B 120.2(2) . . ? N1B C21B C13B 122.5(2) . . ? N1B C21B C20B 117.1(2) . . ? C13B C21B C20B 120.3(2) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 30.17 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.734 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.107 data_3 _database_code_depnum_ccdc_archive 'CCDC 871908' #TrackingRef 'Laurila.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Cl2 N4 Rh, C2 Cl2 O2 Rh' _chemical_formula_sum 'C26 H16 Cl4 N4 O2 Rh2' _chemical_formula_weight 764.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 8.7104(11) _cell_length_b 11.2066(14) _cell_length_c 14.5161(19) _cell_angle_alpha 96.101(3) _cell_angle_beta 90.288(3) _cell_angle_gamma 107.315(2) _cell_volume 1344.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3751 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 29.92 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7773 _exptl_absorpt_correction_T_max 0.8517 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_measurement_device '62mm x 62mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 16 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12064 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6107 _reflns_number_gt 4821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT (Bruker AXS, 2009)' _computing_data_reduction 'SAINT (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.2e (Brandenburg, 2010)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0325P)^2^+0.3550P] 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 6107 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.73057(3) -0.34009(2) 0.80520(2) 0.01460(9) Uani 1 1 d . . . Rh2 Rh 0.65616(4) 0.10409(3) 0.69281(2) 0.02363(10) Uani 1 1 d . . . Cl1 Cl 0.92126(13) 0.23941(11) 0.69152(8) 0.0358(3) Uani 1 1 d . . . Cl2 Cl 0.62899(12) 0.19273(9) 0.84381(8) 0.0294(2) Uani 1 1 d . . . Cl3 Cl 0.64029(10) -0.34592(8) 0.95678(7) 0.0178(2) Uani 1 1 d . . . Cl4 Cl 0.52627(10) -0.26650(8) 0.75117(7) 0.0208(2) Uani 1 1 d . . . O3 O 0.7097(5) -0.0117(3) 0.5083(3) 0.0563(11) Uani 1 1 d . . . O4 O 0.3180(4) -0.0632(3) 0.6939(2) 0.0429(9) Uani 1 1 d . . . N1 N 0.8108(3) -0.3500(3) 0.6746(2) 0.0195(7) Uani 1 1 d . . . N2 N 0.5830(3) -0.5144(3) 0.7553(2) 0.0155(7) Uani 1 1 d . . . N3 N 0.9221(3) -0.3902(3) 0.8504(2) 0.0170(7) Uani 1 1 d . . . N4 N 0.8817(3) -0.1646(3) 0.8453(2) 0.0165(7) Uani 1 1 d . . . C3 C 0.6862(6) 0.0325(4) 0.5783(4) 0.0378(12) Uani 1 1 d . . . C4 C 0.4469(5) -0.0002(4) 0.6942(3) 0.0280(10) Uani 1 1 d . . . C10 C 0.9295(5) -0.2653(4) 0.6366(3) 0.0261(9) Uani 1 1 d . . . H10 H 0.9879 -0.1902 0.6735 0.031 Uiso 1 1 calc R . . C11 C 0.9692(5) -0.2845(4) 0.5447(3) 0.0332(11) Uani 1 1 d . . . H11 H 1.0552 -0.2236 0.5203 0.040 Uiso 1 1 calc R . . C12 C 0.8845(5) -0.3914(4) 0.4890(3) 0.0288(10) Uani 1 1 d . . . H12 H 0.9112 -0.4047 0.4261 0.035 Uiso 1 1 calc R . . C13 C 0.7578(5) -0.4807(4) 0.5265(3) 0.0240(9) Uani 1 1 d . . . C14 C 0.6539(5) -0.5928(4) 0.4740(3) 0.0275(10) Uani 1 1 d . . . H14 H 0.6744 -0.6121 0.4108 0.033 Uiso 1 1 calc R . . C15 C 0.5290(5) -0.6701(4) 0.5129(3) 0.0285(10) Uani 1 1 d . . . H15 H 0.4600 -0.7409 0.4759 0.034 Uiso 1 1 calc R . . C16 C 0.4969(4) -0.6482(3) 0.6097(3) 0.0207(9) Uani 1 1 d . . . C17 C 0.3657(4) -0.7224(4) 0.6550(3) 0.0244(9) Uani 1 1 d . . . H17 H 0.2894 -0.7927 0.6215 0.029 Uiso 1 1 calc R . . C18 C 0.3491(4) -0.6925(4) 0.7474(3) 0.0241(9) Uani 1 1 d . . . H18 H 0.2610 -0.7422 0.7783 0.029 Uiso 1 1 calc R . . C19 C 0.4618(4) -0.5888(3) 0.7968(3) 0.0192(8) Uani 1 1 d . . . H19 H 0.4511 -0.5712 0.8615 0.023 Uiso 1 1 calc R . . C20 C 0.6006(4) -0.5425(3) 0.6634(3) 0.0178(8) Uani 1 1 d . . . C21 C 0.7268(4) -0.4573(3) 0.6203(3) 0.0185(8) Uani 1 1 d . . . C22 C 0.9345(4) -0.5050(4) 0.8550(3) 0.0224(9) Uani 1 1 d . . . H22 H 0.8460 -0.5764 0.8348 0.027 Uiso 1 1 calc R . . C23 C 1.0764(5) -0.5219(4) 0.8895(3) 0.0283(10) Uani 1 1 d . . . H23 H 1.0817 -0.6044 0.8942 0.034 Uiso 1 1 calc R . . C24 C 1.2070(4) -0.4205(4) 0.9163(3) 0.0243(9) Uani 1 1 d . . . H24 H 1.3034 -0.4325 0.9387 0.029 Uiso 1 1 calc R . . C25 C 1.1976(4) -0.2976(4) 0.9105(3) 0.0204(9) Uani 1 1 d . . . C26 C 1.3273(4) -0.1838(4) 0.9348(3) 0.0226(9) Uani 1 1 d . . . H26 H 1.4293 -0.1892 0.9540 0.027 Uiso 1 1 calc R . . C27 C 1.3072(4) -0.0696(4) 0.9309(3) 0.0222(9) Uani 1 1 d . . . H27 H 1.3952 0.0039 0.9471 0.027 Uiso 1 1 calc R . . C28 C 1.1559(4) -0.0573(3) 0.9028(3) 0.0191(8) Uani 1 1 d . . . C29 C 1.1235(5) 0.0585(4) 0.9018(3) 0.0240(9) Uani 1 1 d . . . H29 H 1.2053 0.1352 0.9202 0.029 Uiso 1 1 calc R . . C30 C 0.9726(5) 0.0598(4) 0.8738(3) 0.0258(9) Uani 1 1 d . . . H30 H 0.9495 0.1375 0.8737 0.031 Uiso 1 1 calc R . . C31 C 0.8526(4) -0.0544(3) 0.8454(3) 0.0208(9) Uani 1 1 d . . . H31 H 0.7489 -0.0528 0.8260 0.025 Uiso 1 1 calc R . . C32 C 1.0299(4) -0.1671(3) 0.8750(3) 0.0162(8) Uani 1 1 d . . . C33 C 1.0517(4) -0.2878(3) 0.8786(3) 0.0170(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 Rh1 0.00883(13) 0.01448(14) 0.01785(17) -0.00116(11) -0.00185(11) 0.00055(10) Rh2 0.02149(17) 0.02134(17) 0.0247(2) 0.00298(13) -0.00244(13) 0.00119(12) Cl1 0.0281(5) 0.0396(6) 0.0276(6) 0.0013(5) 0.0016(5) -0.0076(4) Cl2 0.0277(5) 0.0275(5) 0.0298(6) 0.0006(4) 0.0009(4) 0.0042(4) Cl3 0.0133(4) 0.0203(4) 0.0180(5) -0.0003(4) -0.0007(3) 0.0031(3) Cl4 0.0160(4) 0.0227(5) 0.0234(5) 0.0000(4) -0.0059(4) 0.0061(3) O3 0.062(2) 0.045(2) 0.043(3) -0.0092(18) 0.010(2) -0.0081(18) O4 0.0266(17) 0.047(2) 0.047(2) 0.0095(17) -0.0032(15) -0.0018(15) N1 0.0109(14) 0.0233(17) 0.0206(19) 0.0010(14) -0.0002(13) 0.0002(12) N2 0.0112(14) 0.0120(14) 0.0219(19) 0.0007(12) -0.0012(13) 0.0017(11) N3 0.0084(14) 0.0185(15) 0.0208(18) -0.0017(13) -0.0014(12) 0.0004(11) N4 0.0153(15) 0.0134(14) 0.0175(18) 0.0004(12) -0.0035(13) 0.0000(12) C3 0.035(3) 0.029(2) 0.039(3) 0.003(2) -0.001(2) -0.0057(19) C4 0.025(2) 0.026(2) 0.029(3) 0.0050(18) -0.0003(18) 0.0030(17) C10 0.0186(19) 0.028(2) 0.027(3) 0.0015(18) 0.0033(17) 0.0013(16) C11 0.026(2) 0.040(3) 0.028(3) 0.007(2) 0.0062(19) -0.0004(19) C12 0.027(2) 0.037(2) 0.021(2) 0.0049(19) 0.0050(18) 0.0068(18) C13 0.0195(19) 0.033(2) 0.019(2) -0.0035(17) -0.0008(16) 0.0094(16) C14 0.026(2) 0.030(2) 0.025(3) -0.0041(18) -0.0018(18) 0.0094(18) C15 0.028(2) 0.026(2) 0.029(3) -0.0110(18) -0.0090(19) 0.0071(17) C16 0.0167(18) 0.0188(19) 0.025(2) -0.0020(16) -0.0029(16) 0.0045(15) C17 0.0174(19) 0.0195(19) 0.032(3) -0.0025(17) -0.0073(17) 0.0007(15) C18 0.0165(18) 0.021(2) 0.031(3) 0.0031(17) 0.0007(17) -0.0007(15) C19 0.0127(17) 0.0191(18) 0.025(2) 0.0021(16) 0.0021(15) 0.0032(14) C20 0.0120(16) 0.0196(18) 0.020(2) -0.0015(15) -0.0024(15) 0.0041(14) C21 0.0137(17) 0.0208(19) 0.020(2) 0.0018(16) -0.0006(15) 0.0041(14) C22 0.0164(18) 0.0197(19) 0.030(2) -0.0031(17) -0.0035(17) 0.0055(15) C23 0.021(2) 0.022(2) 0.043(3) -0.0017(19) -0.0010(19) 0.0103(16) C24 0.0140(18) 0.026(2) 0.034(3) -0.0015(18) -0.0037(17) 0.0091(15) C25 0.0089(16) 0.027(2) 0.023(2) -0.0019(17) 0.0034(15) 0.0033(14) C26 0.0107(17) 0.030(2) 0.024(2) -0.0028(17) -0.0014(16) 0.0028(15) C27 0.0118(17) 0.026(2) 0.022(2) 0.0004(17) -0.0045(15) -0.0042(15) C28 0.0166(18) 0.0207(19) 0.016(2) -0.0027(15) -0.0010(15) 0.0013(15) C29 0.028(2) 0.0173(19) 0.020(2) -0.0012(16) -0.0042(17) -0.0022(16) C30 0.033(2) 0.0151(18) 0.027(2) -0.0003(16) -0.0076(18) 0.0046(16) C31 0.0198(18) 0.0177(18) 0.024(2) 0.0041(16) -0.0054(16) 0.0041(15) C32 0.0104(16) 0.0153(17) 0.019(2) -0.0007(15) 0.0004(14) -0.0017(13) C33 0.0122(17) 0.0169(18) 0.017(2) -0.0033(15) 0.0009(14) -0.0013(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.027(3) . yes Rh1 N4 2.037(3) . yes Rh1 N3 2.038(3) . yes Rh1 N2 2.046(3) . yes Rh1 Cl4 2.3364(9) . yes Rh1 Cl3 2.3413(11) . yes Rh2 C3 1.823(5) . yes Rh2 C4 1.851(4) . yes Rh2 Cl2 2.3515(12) . yes Rh2 Cl1 2.3567(11) . yes O3 C3 1.129(6) . ? O4 C4 1.135(5) . ? N1 C10 1.345(5) . ? N1 C21 1.368(4) . ? N2 C19 1.327(5) . ? N2 C20 1.358(5) . ? N3 C22 1.331(5) . ? N3 C33 1.372(4) . ? N4 C31 1.332(5) . ? N4 C32 1.368(4) . ? C10 C11 1.390(6) . ? C10 H10 0.9500 . ? C11 C12 1.377(6) . ? C11 H11 0.9500 . ? C12 C13 1.407(6) . ? C12 H12 0.9500 . ? C13 C21 1.401(6) . ? C13 C14 1.446(5) . ? C14 C15 1.343(6) . ? C14 H14 0.9500 . ? C15 C16 1.444(6) . ? C15 H15 0.9500 . ? C16 C20 1.409(5) . ? C16 C17 1.409(6) . ? C17 C18 1.368(6) . ? C17 H17 0.9500 . ? C18 C19 1.402(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.422(5) . ? C22 C23 1.402(5) . ? C22 H22 0.9500 . ? C23 C24 1.367(5) . ? C23 H23 0.9500 . ? C24 C25 1.415(6) . ? C24 H24 0.9500 . ? C25 C33 1.389(5) . ? C25 C26 1.439(5) . ? C26 C27 1.350(6) . ? C26 H26 0.9500 . ? C27 C28 1.427(5) . ? C27 H27 0.9500 . ? C28 C32 1.403(5) . ? C28 C29 1.409(5) . ? C29 C30 1.379(5) . ? C29 H29 0.9500 . ? C30 C31 1.411(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.426(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N4 94.91(12) . . ? N1 Rh1 N3 89.10(13) . . ? N4 Rh1 N3 81.62(12) . . yes N1 Rh1 N2 81.08(12) . . yes N4 Rh1 N2 175.88(13) . . ? N3 Rh1 N2 99.14(11) . . ? N1 Rh1 Cl4 89.23(9) . . ? N4 Rh1 Cl4 94.03(9) . . ? N3 Rh1 Cl4 175.19(9) . . ? N2 Rh1 Cl4 85.04(9) . . ? N1 Rh1 Cl3 175.04(9) . . ? N4 Rh1 Cl3 88.39(10) . . ? N3 Rh1 Cl3 87.73(10) . . ? N2 Rh1 Cl3 95.67(10) . . ? Cl4 Rh1 Cl3 94.23(4) . . yes C3 Rh2 C4 92.33(19) . . yes C3 Rh2 Cl2 176.82(16) . . ? C4 Rh2 Cl2 89.18(14) . . ? C3 Rh2 Cl1 88.17(14) . . ? C4 Rh2 Cl1 179.17(14) . . ? Cl2 Rh2 Cl1 90.35(4) . . yes C10 N1 C21 118.4(4) . . ? C10 N1 Rh1 128.5(3) . . ? C21 N1 Rh1 113.1(3) . . ? C19 N2 C20 118.8(3) . . ? C19 N2 Rh1 128.1(3) . . ? C20 N2 Rh1 112.1(2) . . ? C22 N3 C33 119.0(3) . . ? C22 N3 Rh1 128.7(2) . . ? C33 N3 Rh1 112.3(2) . . ? C31 N4 C32 119.4(3) . . ? C31 N4 Rh1 128.4(2) . . ? C32 N4 Rh1 112.2(2) . . ? O3 C3 Rh2 177.7(5) . . ? O4 C4 Rh2 178.9(4) . . ? N1 C10 C11 121.9(4) . . ? N1 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 120.3(4) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.0(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C21 C13 C12 117.8(3) . . ? C21 C13 C14 117.8(4) . . ? C12 C13 C14 124.3(4) . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 121.6(3) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C20 C16 C17 116.7(4) . . ? C20 C16 C15 118.3(4) . . ? C17 C16 C15 125.0(3) . . ? C18 C17 C16 119.5(3) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? N2 C19 C18 121.6(4) . . ? N2 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? N2 C20 C16 123.1(4) . . ? N2 C20 C21 117.3(3) . . ? C16 C20 C21 119.6(4) . . ? N1 C21 C13 122.5(4) . . ? N1 C21 C20 116.1(3) . . ? C13 C21 C20 121.3(3) . . ? N3 C22 C23 120.9(3) . . ? N3 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 120.6(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C33 C25 C24 116.8(3) . . ? C33 C25 C26 118.4(4) . . ? C24 C25 C26 124.8(3) . . ? C27 C26 C25 121.3(3) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 121.1(3) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C32 C28 C29 117.4(3) . . ? C32 C28 C27 118.4(4) . . ? C29 C28 C27 124.3(3) . . ? C30 C29 C28 119.6(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 119.8(4) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? N4 C31 C30 121.3(3) . . ? N4 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? N4 C32 C28 122.5(3) . . ? N4 C32 C33 117.1(3) . . ? C28 C32 C33 120.4(3) . . ? N3 C33 C25 123.2(3) . . ? N3 C33 C32 116.6(3) . . ? C25 C33 C32 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.845 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.130