# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_complex_4 _audit_creation_date 2013-10-23T08:54:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C25 H22 Au Cl N2' _chemical_formula_moiety 'C25 H22 Au Cl N2' _chemical_formula_weight 582.86 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system Monoclinic _space_group_name_H-M_alt 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 27.8036(11) _cell_length_b 8.4332(3) _cell_length_c 18.9780(7) _cell_angle_alpha 90 _cell_angle_beta 102.5720(10) _cell_angle_gamma 90 _cell_volume 4343.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_theta_min 1.80 _cell_measurement_reflns_used 9999 _cell_measurement_theta_max 36.29 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_absorpt_coefficient_mu 6.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; 'SADABS, Sheldrick, Bruker, 2000' ; _exptl_absorpt_correction_T_min 0.5561 _exptl_absorpt_correction_T_max 0.7462 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'Incoatec I\mS Microsource ' _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_unetI/netI 0.0281 _diffrn_reflns_number 44515 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.2 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4447 _reflns_number_gt 4117 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0345P)^2^+19.4974P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 4447 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.89 _refine_diff_density_min -1.649 _refine_diff_density_rms 0.174 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.37576(14) 0.5367(5) 0.0984(2) 0.0113(8) Uani 1 1 d . . . C3 C 0.36322(16) 0.4467(5) 0.2039(2) 0.0163(9) Uani 1 1 d . . . H3 H 0.3483 0.397 0.2374 0.02 Uiso 1 1 calc R . . C2 C 0.40720(16) 0.5191(5) 0.2177(2) 0.0180(9) Uani 1 1 d . . . H2 H 0.4285 0.5302 0.2626 0.022 Uiso 1 1 calc R . . C21 C 0.29694(15) 0.3909(5) 0.0915(2) 0.0128(8) Uani 1 1 d . . . H21 H 0.2848 0.4504 0.0468 0.015 Uiso 1 1 calc R . . C33 C 0.25778(15) 0.3907(5) 0.1366(2) 0.0125(8) Uani 1 1 d . . . C32 C 0.23873(16) 0.5183(5) 0.1682(2) 0.0171(9) Uani 1 1 d . . . H32 H 0.2504 0.6207 0.1646 0.021 Uiso 1 1 calc R . . C31 C 0.20175(16) 0.4882(6) 0.2051(2) 0.0206(9) Uani 1 1 d . . . H31 H 0.1886 0.5715 0.227 0.025 Uiso 1 1 calc R . . C30 C 0.18428(16) 0.3359(6) 0.2099(2) 0.0211(9) Uani 1 1 d . . . H30 H 0.1594 0.3184 0.2348 0.025 Uiso 1 1 calc R . . C29 C 0.20302(16) 0.2087(6) 0.1781(2) 0.0188(9) Uani 1 1 d . . . H29 H 0.1908 0.1069 0.1811 0.023 Uiso 1 1 calc R . . C28 C 0.24047(15) 0.2364(5) 0.1418(2) 0.0130(8) Uani 1 1 d . . . C27 C 0.26735(15) 0.1281(5) 0.1033(2) 0.0127(8) Uani 1 1 d . . . C26 C 0.26334(16) -0.0345(5) 0.0930(2) 0.0171(9) Uani 1 1 d . . . H26 H 0.2414 -0.0937 0.1128 0.021 Uiso 1 1 calc R . . C25 C 0.29308(16) -0.1062(5) 0.0523(3) 0.0193(10) Uani 1 1 d . . . H25 H 0.2912 -0.2154 0.0452 0.023 Uiso 1 1 calc R . . C24 C 0.32604(16) -0.0171(5) 0.0214(2) 0.0201(9) Uani 1 1 d . . . H24 H 0.3451 -0.0672 -0.0066 0.024 Uiso 1 1 calc R . . C23 C 0.33002(15) 0.1451(5) 0.0327(2) 0.0161(8) Uani 1 1 d . . . H23 H 0.352 0.2049 0.0131 0.019 Uiso 1 1 calc R . . C22 C 0.30059(14) 0.2164(5) 0.0739(2) 0.0129(8) Uani 1 1 d . . . C11 C 0.45665(15) 0.6626(5) 0.1400(2) 0.0151(8) Uani 1 1 d . . . C12 C 0.49276(16) 0.5812(5) 0.1137(2) 0.0189(9) Uani 1 1 d . . . C13 C 0.53063(16) 0.6702(6) 0.0958(2) 0.0215(10) Uani 1 1 d . . . H13 H 0.5556 0.6183 0.0793 0.026 Uiso 1 1 calc R . . C14 C 0.53215(16) 0.8336(6) 0.1019(2) 0.0229(10) Uani 1 1 d . . . C15 C 0.49628(17) 0.9095(5) 0.1306(3) 0.0216(10) Uani 1 1 d . . . H15 H 0.498 1.019 0.1366 0.026 Uiso 1 1 calc R . . C16 C 0.45819(16) 0.8277(6) 0.1506(2) 0.0190(9) Uani 1 1 d . . . C17 C 0.49126(19) 0.4037(5) 0.1059(3) 0.0260(11) Uani 1 1 d . . . H17A H 0.4872 0.3562 0.1502 0.039 Uiso 1 1 calc R . . H17B H 0.5215 0.3672 0.0948 0.039 Uiso 1 1 calc R . . H17C H 0.4641 0.3742 0.0675 0.039 Uiso 1 1 calc R . . C18 C 0.5714(2) 0.9282(7) 0.0768(3) 0.0347(13) Uani 1 1 d . . . H18A H 0.601 0.8665 0.0832 0.052 Uiso 1 1 calc R . . H18B H 0.5779 1.024 0.1047 0.052 Uiso 1 1 calc R . . H18C H 0.5602 0.9544 0.0267 0.052 Uiso 1 1 calc R . . C19 C 0.41986(18) 0.9114(6) 0.1823(3) 0.0253(11) Uani 1 1 d . . . H19A H 0.4253 0.8882 0.233 0.038 Uiso 1 1 calc R . . H19B H 0.3876 0.8754 0.1586 0.038 Uiso 1 1 calc R . . H19C H 0.4222 1.0237 0.1756 0.038 Uiso 1 1 calc R . . N2 N 0.34412(12) 0.4598(4) 0.13040(18) 0.0123(7) Uani 1 1 d . . . N1 N 0.41486(13) 0.5742(4) 0.15235(19) 0.0154(7) Uani 1 1 d . . . Cl1 Cl 0.36739(4) 0.66172(13) -0.12173(5) 0.0181(2) Uani 1 1 d . . . Au1 Au 0.370728(5) 0.590010(17) -0.004957(7) 0.01132(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0112(19) 0.0100(19) 0.0120(19) -0.0036(15) 0.0010(15) 0.0004(16) C3 0.024(2) 0.017(2) 0.0093(19) 0.0027(16) 0.0053(17) -0.0005(18) C2 0.023(2) 0.022(2) 0.0089(19) 0.0002(17) 0.0029(17) -0.0011(19) C21 0.015(2) 0.012(2) 0.0106(19) -0.0007(15) 0.0026(16) 0.0003(16) C33 0.012(2) 0.013(2) 0.0111(19) 0.0002(15) 0.0009(16) -0.0006(15) C32 0.023(2) 0.011(2) 0.017(2) -0.0019(17) 0.0038(17) -0.0004(17) C31 0.020(2) 0.025(3) 0.018(2) -0.0035(19) 0.0061(18) 0.0035(19) C30 0.018(2) 0.029(3) 0.018(2) -0.0005(19) 0.0083(18) 0.0020(19) C29 0.018(2) 0.020(2) 0.018(2) 0.0022(18) 0.0030(17) -0.0043(18) C28 0.0150(19) 0.012(2) 0.0106(18) 0.0024(16) 0.0002(15) 0.0000(16) C27 0.014(2) 0.012(2) 0.0105(19) -0.0001(15) -0.0007(16) -0.0002(16) C26 0.016(2) 0.012(2) 0.021(2) 0.0028(17) -0.0003(17) -0.0011(17) C25 0.018(2) 0.010(2) 0.025(2) -0.0060(17) -0.0045(18) 0.0018(16) C24 0.020(2) 0.020(2) 0.020(2) -0.0060(18) 0.0030(18) 0.0042(18) C23 0.017(2) 0.018(2) 0.014(2) -0.0014(17) 0.0047(16) -0.0023(18) C22 0.0147(19) 0.013(2) 0.0101(18) -0.0002(15) 0.0014(15) -0.0009(16) C11 0.014(2) 0.022(2) 0.0097(18) -0.0001(17) 0.0032(15) -0.0013(17) C12 0.017(2) 0.026(2) 0.012(2) 0.0006(17) 0.0006(17) 0.0020(18) C13 0.020(2) 0.029(3) 0.016(2) -0.0007(19) 0.0052(18) 0.0021(19) C14 0.018(2) 0.033(3) 0.018(2) 0.003(2) 0.0020(18) -0.003(2) C15 0.024(2) 0.019(2) 0.021(2) -0.0015(18) 0.0025(19) -0.0058(19) C16 0.016(2) 0.026(2) 0.013(2) -0.0016(18) 0.0003(17) -0.0002(18) C17 0.026(3) 0.023(3) 0.030(3) -0.003(2) 0.008(2) 0.002(2) C18 0.025(3) 0.042(3) 0.041(3) 0.003(2) 0.014(2) -0.008(2) C19 0.024(2) 0.025(3) 0.026(3) -0.004(2) 0.006(2) -0.002(2) N2 0.0148(17) 0.0129(17) 0.0096(16) -0.0009(13) 0.0038(13) -0.0012(14) N1 0.0170(18) 0.0161(18) 0.0117(17) -0.0007(14) 0.0004(14) -0.0030(14) Cl1 0.0242(5) 0.0215(5) 0.0093(4) 0.0017(4) 0.0050(4) -0.0039(4) Au1 0.01351(10) 0.01284(9) 0.00811(9) -0.00037(6) 0.00346(6) -0.00156(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.340(5) . ? C1 N1 1.359(5) . ? C1 Au1 1.987(4) . ? C3 C2 1.341(6) . ? C3 N2 1.386(5) . ? C3 H3 0.93 . ? C2 N1 1.384(5) . ? C2 H2 0.93 . ? C21 N2 1.477(5) . ? C21 C22 1.517(6) . ? C21 C33 1.525(6) . ? C21 H21 0.98 . ? C33 C32 1.391(6) . ? C33 C28 1.398(6) . ? C32 C31 1.389(6) . ? C32 H32 0.93 . ? C31 C30 1.383(7) . ? C31 H31 0.93 . ? C30 C29 1.386(7) . ? C30 H30 0.93 . ? C29 C28 1.388(6) . ? C29 H29 0.93 . ? C28 C27 1.472(6) . ? C27 C26 1.386(6) . ? C27 C22 1.394(6) . ? C26 C25 1.388(7) . ? C26 H26 0.93 . ? C25 C24 1.408(7) . ? C25 H25 0.93 . ? C24 C23 1.386(7) . ? C24 H24 0.93 . ? C23 C22 1.385(6) . ? C23 H23 0.93 . ? C11 C12 1.395(6) . ? C11 C16 1.406(7) . ? C11 N1 1.442(5) . ? C12 C13 1.395(7) . ? C12 C17 1.504(6) . ? C13 C14 1.383(7) . ? C13 H13 0.93 . ? C14 C15 1.392(7) . ? C14 C18 1.510(7) . ? C15 C16 1.384(6) . ? C15 H15 0.93 . ? C16 C19 1.509(6) . ? C17 H17A 0.96 . ? C17 H17B 0.96 . ? C17 H17C 0.96 . ? C18 H18A 0.96 . ? C18 H18B 0.96 . ? C18 H18C 0.96 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? Cl1 Au1 2.2794(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 105.5(3) . . ? N2 C1 Au1 130.1(3) . . ? N1 C1 Au1 124.3(3) . . ? C2 C3 N2 107.1(4) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? C3 C2 N1 106.8(4) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? N2 C21 C22 113.4(3) . . ? N2 C21 C33 112.6(3) . . ? C22 C21 C33 102.3(3) . . ? N2 C21 H21 109.4 . . ? C22 C21 H21 109.4 . . ? C33 C21 H21 109.4 . . ? C32 C33 C28 121.3(4) . . ? C32 C33 C21 128.8(4) . . ? C28 C33 C21 109.9(3) . . ? C31 C32 C33 118.0(4) . . ? C31 C32 H32 121 . . ? C33 C32 H32 121 . . ? C30 C31 C32 120.7(4) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C31 C30 C29 121.4(4) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C29 C28 118.6(4) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? C29 C28 C33 120.0(4) . . ? C29 C28 C27 131.2(4) . . ? C33 C28 C27 108.8(4) . . ? C26 C27 C22 120.8(4) . . ? C26 C27 C28 130.5(4) . . ? C22 C27 C28 108.7(4) . . ? C27 C26 C25 118.0(4) . . ? C27 C26 H26 121 . . ? C25 C26 H26 121 . . ? C26 C25 C24 121.3(4) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C23 C24 C25 120.0(4) . . ? C23 C24 H24 120 . . ? C25 C24 H24 120 . . ? C22 C23 C24 118.6(4) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C23 C22 C27 121.2(4) . . ? C23 C22 C21 128.4(4) . . ? C27 C22 C21 110.3(4) . . ? C12 C11 C16 122.5(4) . . ? C12 C11 N1 118.1(4) . . ? C16 C11 N1 119.3(4) . . ? C13 C12 C11 117.5(4) . . ? C13 C12 C17 121.2(4) . . ? C11 C12 C17 121.3(4) . . ? C14 C13 C12 121.8(4) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 118.7(4) . . ? C13 C14 C18 120.8(5) . . ? C15 C14 C18 120.6(5) . . ? C16 C15 C14 122.3(4) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C11 117.1(4) . . ? C15 C16 C19 121.7(4) . . ? C11 C16 C19 121.2(4) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C1 N2 C3 110.5(3) . . ? C1 N2 C21 124.2(3) . . ? C3 N2 C21 125.2(3) . . ? C1 N1 C2 110.1(3) . . ? C1 N1 C11 122.6(3) . . ? C2 N1 C11 127.3(3) . . ? C1 Au1 Cl1 177.17(12) . . ? 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 N2 C3 C2 N1 -0.7(5) . . . . ? N2 C21 C33 C32 58.1(6) . . . . ? C22 C21 C33 C32 -179.8(4) . . . . ? N2 C21 C33 C28 -123.7(4) . . . . ? C22 C21 C33 C28 -1.7(4) . . . . ? C28 C33 C32 C31 -0.1(6) . . . . ? C21 C33 C32 C31 177.9(4) . . . . ? C33 C32 C31 C30 -0.5(6) . . . . ? C32 C31 C30 C29 0.1(7) . . . . ? C31 C30 C29 C28 0.7(6) . . . . ? C30 C29 C28 C33 -1.3(6) . . . . ? C30 C29 C28 C27 -179.9(4) . . . . ? C32 C33 C28 C29 1.0(6) . . . . ? C21 C33 C28 C29 -177.4(4) . . . . ? C32 C33 C28 C27 179.9(4) . . . . ? C21 C33 C28 C27 1.5(5) . . . . ? C29 C28 C27 C26 -1.0(7) . . . . ? C33 C28 C27 C26 -179.7(4) . . . . ? C29 C28 C27 C22 178.0(4) . . . . ? C33 C28 C27 C22 -0.7(5) . . . . ? C22 C27 C26 C25 -0.4(6) . . . . ? C28 C27 C26 C25 178.5(4) . . . . ? C27 C26 C25 C24 -0.8(6) . . . . ? C26 C25 C24 C23 1.4(7) . . . . ? C25 C24 C23 C22 -0.9(6) . . . . ? C24 C23 C22 C27 -0.3(6) . . . . ? C24 C23 C22 C21 -177.6(4) . . . . ? C26 C27 C22 C23 1.0(6) . . . . ? C28 C27 C22 C23 -178.2(4) . . . . ? C26 C27 C22 C21 178.7(4) . . . . ? C28 C27 C22 C21 -0.4(5) . . . . ? N2 C21 C22 C23 -59.7(5) . . . . ? C33 C21 C22 C23 178.8(4) . . . . ? N2 C21 C22 C27 122.8(4) . . . . ? C33 C21 C22 C27 1.2(4) . . . . ? C16 C11 C12 C13 -1.9(6) . . . . ? N1 C11 C12 C13 174.3(4) . . . . ? C16 C11 C12 C17 177.4(4) . . . . ? N1 C11 C12 C17 -6.4(6) . . . . ? C11 C12 C13 C14 -1.5(6) . . . . ? C17 C12 C13 C14 179.2(4) . . . . ? C12 C13 C14 C15 3.7(7) . . . . ? C12 C13 C14 C18 -175.3(4) . . . . ? C13 C14 C15 C16 -2.6(7) . . . . ? C18 C14 C15 C16 176.5(4) . . . . ? C14 C15 C16 C11 -0.6(7) . . . . ? C14 C15 C16 C19 179.4(4) . . . . ? C12 C11 C16 C15 2.9(6) . . . . ? N1 C11 C16 C15 -173.2(4) . . . . ? C12 C11 C16 C19 -177.1(4) . . . . ? N1 C11 C16 C19 6.8(6) . . . . ? N1 C1 N2 C3 -0.8(5) . . . . ? Au1 C1 N2 C3 178.9(3) . . . . ? N1 C1 N2 C21 -177.4(3) . . . . ? Au1 C1 N2 C21 2.3(6) . . . . ? C2 C3 N2 C1 0.9(5) . . . . ? C2 C3 N2 C21 177.5(4) . . . . ? C22 C21 N2 C1 94.8(5) . . . . ? C33 C21 N2 C1 -149.6(4) . . . . ? C22 C21 N2 C3 -81.3(5) . . . . ? C33 C21 N2 C3 34.2(5) . . . . ? N2 C1 N1 C2 0.4(5) . . . . ? Au1 C1 N1 C2 -179.4(3) . . . . ? N2 C1 N1 C11 -178.2(4) . . . . ? Au1 C1 N1 C11 2.1(6) . . . . ? C3 C2 N1 C1 0.2(5) . . . . ? C3 C2 N1 C11 178.7(4) . . . . ? C12 C11 N1 C1 -80.9(5) . . . . ? C16 C11 N1 C1 95.4(5) . . . . ? C12 C11 N1 C2 100.9(5) . . . . ? C16 C11 N1 C2 -82.9(5) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 969666' ####################################################################### # # 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_complex_5 _audit_creation_date 2008-07-16T15:57:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C34 H35 Cl4 N2 Rh' _chemical_formula_moiety 'C33 H34 Cl N2 Rh, C H Cl3' _chemical_formula_weight 716.35 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 12.688(3) _cell_length_b 16.274(3) _cell_length_c 16.218(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.45(3) _cell_angle_gamma 90.00 _cell_volume 3211.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 35.11 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Siemens Industrial Automation, Inc.: Madison, WI.. ; _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.890 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 116702 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _reflns_number_total 6543 _reflns_number_gt 5590 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0526P)^2^+5.1701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6543 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.704 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.101 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1734(2) 0.38998(17) 0.29699(18) 0.0205(6) Uani 1 1 d . . . C2 C 0.1693(3) 0.25075(19) 0.2893(2) 0.0267(6) Uani 1 1 d . . . H2 H 0.1762 0.1959 0.3061 0.032 Uiso 1 1 calc R . . C3 C 0.1360(3) 0.27905(18) 0.2089(2) 0.0256(6) Uani 1 1 d . . . H3 H 0.1150 0.2479 0.1588 0.031 Uiso 1 1 calc R . . C41 C 0.1067(3) 0.49340(18) 0.4318(2) 0.0254(6) Uani 1 1 d . . . H41 H 0.1053 0.4366 0.4515 0.030 Uiso 1 1 calc R . . C48 C 0.0317(3) 0.50944(18) 0.3508(2) 0.0246(6) Uani 1 1 d . . . H48 H -0.0124 0.4618 0.3248 0.030 Uiso 1 1 calc R . . C47 C -0.0242(3) 0.5908(2) 0.3243(2) 0.0325(7) Uani 1 1 d . . . H47A H -0.0814 0.5978 0.3526 0.039 Uiso 1 1 calc R . . H47B H -0.0590 0.5900 0.2628 0.039 Uiso 1 1 calc R . . C46 C 0.0541(3) 0.6642(2) 0.3459(2) 0.0374(8) Uani 1 1 d . . . H46A H 0.0263 0.7076 0.3045 0.045 Uiso 1 1 calc R . . H46B H 0.0555 0.6849 0.4023 0.045 Uiso 1 1 calc R . . C45 C 0.1702(3) 0.64275(19) 0.3454(2) 0.0320(7) Uani 1 1 d . . . H45 H 0.1963 0.6741 0.3034 0.038 Uiso 1 1 calc R . . C44 C 0.2524(3) 0.6184(2) 0.4162(2) 0.0323(7) Uani 1 1 d . . . H44 H 0.3260 0.6359 0.4154 0.039 Uiso 1 1 calc R . . C43 C 0.2413(3) 0.6036(2) 0.5052(2) 0.0414(9) Uani 1 1 d . . . H43A H 0.2407 0.6560 0.5335 0.050 Uiso 1 1 calc R . . H43B H 0.3046 0.5729 0.5385 0.050 Uiso 1 1 calc R . . C42 C 0.1368(3) 0.5564(2) 0.5039(2) 0.0367(8) Uani 1 1 d . . . H42A H 0.1473 0.5286 0.5586 0.044 Uiso 1 1 calc R . . H42B H 0.0766 0.5949 0.4970 0.044 Uiso 1 1 calc R . . C11 C 0.2290(3) 0.31064(18) 0.43548(19) 0.0258(6) Uani 1 1 d . . . C12 C 0.3371(3) 0.3293(2) 0.4793(2) 0.0342(7) Uani 1 1 d . . . C13 C 0.3688(3) 0.3186(3) 0.5684(2) 0.0460(10) Uani 1 1 d . . . H13 H 0.4400 0.3326 0.5996 0.055 Uiso 1 1 calc R . . C14 C 0.2978(4) 0.2880(3) 0.6117(2) 0.0463(10) Uani 1 1 d . . . C15 C 0.1908(3) 0.2700(2) 0.5650(2) 0.0392(9) Uani 1 1 d . . . H15 H 0.1422 0.2501 0.5938 0.047 Uiso 1 1 calc R . . C16 C 0.1541(3) 0.28081(19) 0.4768(2) 0.0295(7) Uani 1 1 d . . . C17 C 0.4194(3) 0.3572(3) 0.4335(3) 0.0514(10) Uani 1 1 d . . . H17A H 0.4029 0.3316 0.3779 0.077 Uiso 1 1 calc R . . H17B H 0.4921 0.3418 0.4667 0.077 Uiso 1 1 calc R . . H17C H 0.4155 0.4158 0.4268 0.077 Uiso 1 1 calc R . . C18 C 0.3372(5) 0.2718(4) 0.7070(3) 0.0727(16) Uani 1 1 d . . . H18A H 0.4011 0.3047 0.7322 0.109 Uiso 1 1 calc R . . H18B H 0.3556 0.2147 0.7168 0.109 Uiso 1 1 calc R . . H18C H 0.2802 0.2857 0.7328 0.109 Uiso 1 1 calc R . . C19 C 0.0376(3) 0.2610(2) 0.4284(2) 0.0378(8) Uani 1 1 d . . . H19A H 0.0092 0.3030 0.3864 0.057 Uiso 1 1 calc R . . H19B H -0.0063 0.2582 0.4678 0.057 Uiso 1 1 calc R . . H19C H 0.0352 0.2090 0.4000 0.057 Uiso 1 1 calc R . . C21 C 0.1093(2) 0.41672(17) 0.13806(18) 0.0222(6) Uani 1 1 d . . . H21 H 0.1303 0.4736 0.1549 0.027 Uiso 1 1 calc R . . C22 C -0.0114(2) 0.41383(17) 0.08775(19) 0.0236(6) Uani 1 1 d . . . C23 C -0.1022(3) 0.4339(2) 0.1142(2) 0.0288(6) Uani 1 1 d . . . H23 H -0.0948 0.4490 0.1709 0.035 Uiso 1 1 calc R . . C24 C -0.2058(3) 0.4312(2) 0.0541(2) 0.0361(8) Uani 1 1 d . . . H24 H -0.2679 0.4444 0.0710 0.043 Uiso 1 1 calc R . . C25 C -0.2167(3) 0.4091(2) -0.0301(2) 0.0370(8) Uani 1 1 d . . . H25 H -0.2860 0.4086 -0.0695 0.044 Uiso 1 1 calc R . . C26 C -0.1255(3) 0.3878(2) -0.0568(2) 0.0341(7) Uani 1 1 d . . . H26 H -0.1332 0.3723 -0.1134 0.041 Uiso 1 1 calc R . . C27 C -0.0225(3) 0.39005(18) 0.00292(19) 0.0263(6) Uani 1 1 d . . . C28 C 0.0876(3) 0.37348(19) -0.00673(19) 0.0280(7) Uani 1 1 d . . . C29 C 0.1209(3) 0.3468(2) -0.0769(2) 0.0390(8) Uani 1 1 d . . . H29 H 0.0696 0.3355 -0.1292 0.047 Uiso 1 1 calc R . . C30 C 0.2328(4) 0.3376(2) -0.0670(3) 0.0456(10) Uani 1 1 d . . . H30 H 0.2566 0.3205 -0.1134 0.055 Uiso 1 1 calc R . . C31 C 0.3091(3) 0.3536(2) 0.0108(3) 0.0430(9) Uani 1 1 d . . . H31 H 0.3835 0.3471 0.0160 0.052 Uiso 1 1 calc R . . C32 C 0.2765(3) 0.3791(2) 0.0814(2) 0.0342(7) Uani 1 1 d . . . H32 H 0.3280 0.3893 0.1339 0.041 Uiso 1 1 calc R . . C33 C 0.1656(3) 0.38893(18) 0.0718(2) 0.0261(6) Uani 1 1 d . . . C100 C 0.4243(3) 0.5244(3) -0.2235(3) 0.0454(9) Uani 1 1 d . . . H100 H 0.4703 0.5016 -0.2573 0.054 Uiso 1 1 calc R . . N1 N 0.1919(2) 0.31873(15) 0.34299(15) 0.0226(5) Uani 1 1 d . . . N2 N 0.1386(2) 0.36409(15) 0.21453(15) 0.0207(5) Uani 1 1 d . . . Cl1 Cl 0.33680(6) 0.52934(5) 0.26932(5) 0.02396(16) Uani 1 1 d . . . Cl2 Cl 0.28781(13) 0.49188(10) -0.26864(11) 0.0853(5) Uani 1 1 d . . . Cl3 Cl 0.47151(11) 0.48819(10) -0.11825(9) 0.0699(4) Uani 1 1 d . . . Cl4 Cl 0.42931(13) 0.63083(8) -0.22710(13) 0.0915(5) Uani 1 1 d . . . Rh1 Rh 0.192197(18) 0.509163(13) 0.338219(14) 0.01997(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0176(13) 0.0222(14) 0.0235(14) -0.0009(11) 0.0090(11) 0.0023(11) C2 0.0341(16) 0.0186(14) 0.0306(16) 0.0001(11) 0.0142(13) 0.0052(12) C3 0.0328(16) 0.0190(14) 0.0263(15) -0.0036(11) 0.0105(13) 0.0018(12) C41 0.0313(16) 0.0230(14) 0.0283(16) -0.0003(12) 0.0189(13) -0.0013(12) C48 0.0249(15) 0.0238(15) 0.0295(16) -0.0035(12) 0.0148(13) -0.0025(11) C47 0.0280(16) 0.0338(17) 0.0377(18) 0.0009(14) 0.0126(14) 0.0066(13) C46 0.045(2) 0.0242(16) 0.049(2) 0.0021(14) 0.0235(17) 0.0066(14) C45 0.0426(19) 0.0166(14) 0.0439(19) -0.0024(13) 0.0238(16) -0.0066(13) C44 0.0377(18) 0.0267(16) 0.0360(18) -0.0106(13) 0.0164(15) -0.0131(14) C43 0.050(2) 0.042(2) 0.0337(18) -0.0136(15) 0.0134(16) -0.0143(17) C42 0.049(2) 0.0366(18) 0.0297(17) -0.0047(14) 0.0201(15) -0.0048(16) C11 0.0351(17) 0.0216(14) 0.0213(14) 0.0017(11) 0.0090(12) 0.0082(12) C12 0.0331(17) 0.0359(18) 0.0320(17) 0.0017(14) 0.0065(14) 0.0109(14) C13 0.045(2) 0.052(2) 0.0326(19) -0.0020(16) -0.0028(16) 0.0178(18) C14 0.067(3) 0.048(2) 0.0223(17) 0.0028(15) 0.0103(17) 0.025(2) C15 0.066(3) 0.0324(18) 0.0269(17) 0.0068(14) 0.0247(17) 0.0169(17) C16 0.0433(19) 0.0215(14) 0.0279(16) 0.0017(12) 0.0171(14) 0.0090(13) C17 0.0293(19) 0.069(3) 0.053(2) 0.010(2) 0.0067(17) 0.0039(18) C18 0.101(4) 0.086(4) 0.025(2) 0.007(2) 0.009(2) 0.035(3) C19 0.048(2) 0.0335(18) 0.0396(19) -0.0014(15) 0.0247(17) -0.0043(15) C21 0.0293(15) 0.0190(13) 0.0198(14) 0.0011(10) 0.0093(12) 0.0018(11) C22 0.0292(15) 0.0172(13) 0.0238(14) 0.0029(11) 0.0066(12) -0.0013(11) C23 0.0300(16) 0.0263(15) 0.0297(16) 0.0022(12) 0.0078(13) 0.0016(13) C24 0.0289(17) 0.0316(17) 0.047(2) 0.0055(15) 0.0101(15) 0.0015(14) C25 0.0320(18) 0.0270(16) 0.043(2) 0.0055(14) -0.0036(15) -0.0024(13) C26 0.044(2) 0.0246(16) 0.0270(16) 0.0014(13) -0.0003(14) -0.0050(14) C27 0.0360(17) 0.0174(13) 0.0237(15) 0.0017(11) 0.0057(13) -0.0021(12) C28 0.0421(18) 0.0209(14) 0.0239(15) 0.0020(11) 0.0137(13) -0.0012(13) C29 0.064(2) 0.0323(18) 0.0235(16) 0.0000(13) 0.0166(16) -0.0013(17) C30 0.073(3) 0.0363(19) 0.042(2) 0.0003(16) 0.039(2) 0.0065(19) C31 0.047(2) 0.040(2) 0.052(2) 0.0056(17) 0.0311(19) 0.0088(17) C32 0.0346(18) 0.0344(18) 0.0378(18) 0.0020(14) 0.0173(15) 0.0033(14) C33 0.0364(17) 0.0194(14) 0.0267(15) 0.0031(11) 0.0154(13) 0.0014(12) C100 0.036(2) 0.047(2) 0.056(2) -0.0066(19) 0.0174(18) -0.0029(17) N1 0.0264(13) 0.0203(12) 0.0227(12) 0.0013(9) 0.0095(10) 0.0048(9) N2 0.0237(12) 0.0192(12) 0.0206(12) 0.0021(9) 0.0085(10) 0.0028(9) Cl1 0.0229(3) 0.0278(4) 0.0274(4) 0.0005(3) 0.0172(3) -0.0014(3) Cl2 0.0609(8) 0.0959(11) 0.0831(10) -0.0067(8) -0.0056(7) -0.0288(7) Cl3 0.0472(6) 0.1008(10) 0.0612(7) 0.0133(7) 0.0143(5) 0.0063(6) Cl4 0.0808(9) 0.0421(7) 0.1403(15) -0.0023(8) 0.0130(9) -0.0026(6) Rh1 0.02122(14) 0.01889(13) 0.02227(14) -0.00142(8) 0.01018(9) -0.00159(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.352(4) . ? C1 N1 1.363(4) . ? C1 Rh1 2.043(3) . ? C2 C3 1.334(4) . ? C2 N1 1.387(4) . ? C2 H2 0.9300 . ? C3 N2 1.387(4) . ? C3 H3 0.9300 . ? C41 C48 1.411(5) . ? C41 C42 1.520(4) . ? C41 Rh1 2.116(3) . ? C41 H41 0.9800 . ? C48 C47 1.506(4) . ? C48 Rh1 2.104(3) . ? C48 H48 0.9800 . ? C47 C46 1.529(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C46 C45 1.517(5) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C45 C44 1.373(5) . ? C45 Rh1 2.199(3) . ? C45 H45 0.9800 . ? C44 C43 1.509(5) . ? C44 Rh1 2.190(3) . ? C44 H44 0.9800 . ? C43 C42 1.527(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C11 C12 1.387(5) . ? C11 C16 1.396(5) . ? C11 N1 1.446(4) . ? C12 C13 1.397(5) . ? C12 C17 1.512(5) . ? C13 C14 1.383(6) . ? C13 H13 0.9300 . ? C14 C15 1.386(6) . ? C14 C18 1.507(5) . ? C15 C16 1.385(5) . ? C15 H15 0.9300 . ? C16 C19 1.500(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C21 N2 1.466(4) . ? C21 C33 1.517(4) . ? C21 C22 1.518(4) . ? C21 H21 0.9800 . ? C22 C23 1.378(4) . ? C22 C27 1.397(4) . ? C23 C24 1.397(5) . ? C23 H23 0.9300 . ? C24 C25 1.381(5) . ? C24 H24 0.9300 . ? C25 C26 1.389(5) . ? C25 H25 0.9300 . ? C26 C27 1.390(5) . ? C26 H26 0.9300 . ? C27 C28 1.474(4) . ? C28 C29 1.390(5) . ? C28 C33 1.397(4) . ? C29 C30 1.391(6) . ? C29 H29 0.9300 . ? C30 C31 1.380(6) . ? C30 H30 0.9300 . ? C31 C32 1.387(5) . ? C31 H31 0.9300 . ? C32 C33 1.380(5) . ? C32 H32 0.9300 . ? C100 Cl4 1.734(4) . ? C100 Cl3 1.744(5) . ? C100 Cl2 1.760(4) . ? C100 H100 0.9800 . ? Cl1 Rh1 2.4256(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 103.5(2) . . ? N2 C1 Rh1 126.5(2) . . ? N1 C1 Rh1 130.0(2) . . ? C3 C2 N1 106.9(3) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C2 C3 N2 106.6(3) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? C48 C41 C42 123.2(3) . . ? C48 C41 Rh1 69.98(17) . . ? C42 C41 Rh1 113.7(2) . . ? C48 C41 H41 114.1 . . ? C42 C41 H41 114.1 . . ? Rh1 C41 H41 114.1 . . ? C41 C48 C47 124.6(3) . . ? C41 C48 Rh1 70.96(18) . . ? C47 C48 Rh1 111.4(2) . . ? C41 C48 H48 114.0 . . ? C47 C48 H48 114.0 . . ? Rh1 C48 H48 114.0 . . ? C48 C47 C46 113.5(3) . . ? C48 C47 H47A 108.9 . . ? C46 C47 H47A 108.9 . . ? C48 C47 H47B 108.9 . . ? C46 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? C45 C46 C47 112.8(3) . . ? C45 C46 H46A 109.0 . . ? C47 C46 H46A 109.0 . . ? C45 C46 H46B 109.0 . . ? C47 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C44 C45 C46 124.8(3) . . ? C44 C45 Rh1 71.39(19) . . ? C46 C45 Rh1 111.4(2) . . ? C44 C45 H45 113.9 . . ? C46 C45 H45 113.9 . . ? Rh1 C45 H45 113.9 . . ? C45 C44 C43 126.3(3) . . ? C45 C44 Rh1 72.14(18) . . ? C43 C44 Rh1 108.1(2) . . ? C45 C44 H44 114.0 . . ? C43 C44 H44 114.0 . . ? Rh1 C44 H44 114.0 . . ? C44 C43 C42 112.5(3) . . ? C44 C43 H43A 109.1 . . ? C42 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? C42 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? C41 C42 C43 112.2(3) . . ? C41 C42 H42A 109.2 . . ? C43 C42 H42A 109.2 . . ? C41 C42 H42B 109.2 . . ? C43 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C12 C11 C16 122.6(3) . . ? C12 C11 N1 119.7(3) . . ? C16 C11 N1 117.6(3) . . ? C11 C12 C13 117.1(3) . . ? C11 C12 C17 122.3(3) . . ? C13 C12 C17 120.6(3) . . ? C14 C13 C12 122.1(4) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 118.5(3) . . ? C13 C14 C18 120.6(4) . . ? C15 C14 C18 120.9(4) . . ? C16 C15 C14 121.9(4) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C11 117.7(3) . . ? C15 C16 C19 120.4(3) . . ? C11 C16 C19 121.9(3) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C21 C33 111.6(2) . . ? N2 C21 C22 114.3(2) . . ? C33 C21 C22 102.4(2) . . ? N2 C21 H21 109.4 . . ? C33 C21 H21 109.4 . . ? C22 C21 H21 109.4 . . ? C23 C22 C27 120.8(3) . . ? C23 C22 C21 129.1(3) . . ? C27 C22 C21 110.0(3) . . ? C22 C23 C24 118.6(3) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C25 C24 C23 120.6(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.9(3) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C27 118.6(3) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C26 C27 C22 120.4(3) . . ? C26 C27 C28 130.8(3) . . ? C22 C27 C28 108.7(3) . . ? C29 C28 C33 120.1(3) . . ? C29 C28 C27 131.4(3) . . ? C33 C28 C27 108.5(3) . . ? C28 C29 C30 118.5(3) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C31 C30 C29 120.9(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 121.1(4) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C33 C32 C31 118.3(3) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C32 C33 C28 121.2(3) . . ? C32 C33 C21 128.6(3) . . ? C28 C33 C21 110.2(3) . . ? Cl4 C100 Cl3 111.4(2) . . ? Cl4 C100 Cl2 109.1(2) . . ? Cl3 C100 Cl2 109.3(2) . . ? Cl4 C100 H100 109.0 . . ? Cl3 C100 H100 109.0 . . ? Cl2 C100 H100 109.0 . . ? C1 N1 C2 111.2(2) . . ? C1 N1 C11 126.9(2) . . ? C2 N1 C11 121.9(2) . . ? C1 N2 C3 111.8(2) . . ? C1 N2 C21 126.1(2) . . ? C3 N2 C21 122.1(2) . . ? C1 Rh1 C48 90.42(11) . . ? C1 Rh1 C41 94.79(11) . . ? C48 Rh1 C41 39.06(13) . . ? C1 Rh1 C44 161.58(13) . . ? C48 Rh1 C44 97.54(12) . . ? C41 Rh1 C44 81.38(12) . . ? C1 Rh1 C45 161.95(12) . . ? C48 Rh1 C45 81.49(12) . . ? C41 Rh1 C45 89.06(12) . . ? C44 Rh1 C45 36.47(13) . . ? C1 Rh1 Cl1 90.65(8) . . ? C48 Rh1 Cl1 157.50(9) . . ? C41 Rh1 Cl1 162.74(10) . . ? C44 Rh1 Cl1 88.30(9) . . ? C45 Rh1 Cl1 90.81(9) . . ? _database_code_depnum_ccdc_archive 'CCDC 969667' ####################################################################### # # 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_complex_6 _audit_creation_date 2008-07-17T17:55:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C25 H22 Ag Br N2 ' _chemical_formula_moiety 'C25 H22 Ag Br N2 ' _chemical_formula_weight 538.22 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4907(13) _cell_length_b 11.3717(10) _cell_length_c 20.0840(19) _cell_angle_alpha 101.272(8) _cell_angle_beta 102.156(12) _cell_angle_gamma 93.563(9) _cell_volume 2283.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 35.11 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Siemens Industrial Automation, Inc.: Madison, WI.. ; _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.66 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_unetI/netI 0.0247 _diffrn_reflns_number 91358 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 11317 _reflns_number_gt 8760 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0833P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 11317 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.2 _refine_ls_restrained_S_all 1.2 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.648 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.115 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1A C 0.2205(4) -0.1500(3) 0.10927(19) 0.0318(7) Uani 1 1 d . . . C1B C 0.2748(3) 0.2581(3) 0.39593(17) 0.0237(6) Uani 1 1 d . . . C2A C 0.3046(4) -0.2024(3) 0.21009(19) 0.0369(9) Uani 1 1 d . . . H2A H 0.3124 -0.2394 0.2479 0.044 Uiso 1 1 calc R . . C2B C 0.1595(4) 0.1742(3) 0.28769(18) 0.0334(8) Uani 1 1 d . . . H2B H 0.0997 0.1635 0.2451 0.04 Uiso 1 1 calc R . . C3A C 0.3944(4) -0.1256(3) 0.19898(19) 0.0368(8) Uani 1 1 d . . . H3A H 0.477 -0.0983 0.2276 0.044 Uiso 1 1 calc R . . C3B C 0.2437(4) 0.0971(3) 0.30797(18) 0.0366(9) Uani 1 1 d . . . H3B H 0.2528 0.022 0.2822 0.044 Uiso 1 1 calc R . . C11A C 0.0772(5) -0.2944(3) 0.14471(19) 0.0423(10) Uani 1 1 d . . . C11B C 0.1049(3) 0.3742(3) 0.34293(17) 0.0265(7) Uani 1 1 d . . . C12A C 0.0705(6) -0.4156(4) 0.1119(2) 0.0590(14) Uani 1 1 d . . . C12B C 0.1266(3) 0.4550(3) 0.30237(18) 0.0306(7) Uani 1 1 d . . . C13A C -0.0499(7) -0.4868(4) 0.1028(3) 0.076(2) Uani 1 1 d . . . H13A H -0.0565 -0.5686 0.0829 0.091 Uiso 1 1 calc R . . C13B C 0.0496(4) 0.5503(3) 0.3017(2) 0.0425(9) Uani 1 1 d . . . H13B H 0.0612 0.6051 0.2742 0.051 Uiso 1 1 calc R . . C14A C -0.1557(7) -0.4404(5) 0.1218(3) 0.0704(17) Uani 1 1 d . . . C14B C -0.0445(4) 0.5654(4) 0.3415(2) 0.0472(11) Uani 1 1 d . . . C15A C -0.1454(5) -0.3206(5) 0.1544(2) 0.0616(14) Uani 1 1 d . . . H15A H -0.2174 -0.2891 0.1687 0.074 Uiso 1 1 calc R . . C15B C -0.0633(4) 0.4825(4) 0.3812(2) 0.0444(10) Uani 1 1 d . . . H15B H -0.1266 0.4922 0.4075 0.053 Uiso 1 1 calc R . . C16A C -0.0293(4) -0.2463(4) 0.1664(2) 0.0424(9) Uani 1 1 d . . . C16B C 0.0096(4) 0.3853(3) 0.38299(19) 0.0325(7) Uani 1 1 d . . . C17A C 0.1850(8) -0.4662(4) 0.0883(3) 0.082(2) Uani 1 1 d . . . H17A H 0.1801 -0.4601 0.0409 0.123 Uiso 1 1 calc R . . H17B H 0.1842 -0.5494 0.0915 0.123 Uiso 1 1 calc R . . H17C H 0.2647 -0.4217 0.1174 0.123 Uiso 1 1 calc R . . C17B C 0.2305(4) 0.4420(4) 0.2602(2) 0.0432(9) Uani 1 1 d . . . H17D H 0.3097 0.4234 0.2882 0.065 Uiso 1 1 calc R . . H17E H 0.2474 0.5162 0.246 0.065 Uiso 1 1 calc R . . H17F H 0.2003 0.3781 0.2197 0.065 Uiso 1 1 calc R . . C18A C -0.2840(8) -0.5193(7) 0.1078(4) 0.118(3) Uani 1 1 d . . . H18A H -0.3454 -0.4991 0.0701 0.177 Uiso 1 1 calc R . . H18B H -0.3187 -0.5064 0.1489 0.177 Uiso 1 1 calc R . . H18C H -0.2694 -0.6024 0.0955 0.177 Uiso 1 1 calc R . . C18B C -0.1237(6) 0.6709(5) 0.3408(3) 0.0748(18) Uani 1 1 d . . . H18D H -0.1393 0.699 0.3863 0.112 Uiso 1 1 calc R . . H18E H -0.206 0.6466 0.3076 0.112 Uiso 1 1 calc R . . H18F H -0.0763 0.7347 0.3279 0.112 Uiso 1 1 calc R . . C19A C -0.0195(4) -0.1168(4) 0.2048(2) 0.0476(10) Uani 1 1 d . . . H19A H -0.1051 -0.0963 0.2093 0.071 Uiso 1 1 calc R . . H19B H 0.016 -0.0649 0.1792 0.071 Uiso 1 1 calc R . . H19C H 0.037 -0.1067 0.2503 0.071 Uiso 1 1 calc R . . C19B C -0.0161(5) 0.2947(4) 0.4256(2) 0.0508(11) Uani 1 1 d . . . H19D H -0.1028 0.2985 0.4338 0.076 Uiso 1 1 calc R . . H19E H 0.0471 0.3127 0.4694 0.076 Uiso 1 1 calc R . . H19F H -0.0088 0.2152 0.4007 0.076 Uiso 1 1 calc R . . C21A C 0.4136(4) -0.0227(3) 0.09930(19) 0.0334(8) Uani 1 1 d . . . H21A H 0.3508 0.0062 0.0642 0.04 Uiso 1 1 calc R . . C21B C 0.4063(4) 0.0891(3) 0.41729(18) 0.0306(7) Uani 1 1 d . . . H21B H 0.4443 0.1444 0.4621 0.037 Uiso 1 1 calc R . . C22A C 0.5053(4) -0.0974(3) 0.06355(19) 0.0345(8) Uani 1 1 d . . . C22B C 0.5155(4) 0.0434(3) 0.38447(18) 0.0331(8) Uani 1 1 d . . . C23A C 0.4754(4) -0.2047(4) 0.0161(2) 0.0439(9) Uani 1 1 d . . . H23A H 0.3897 -0.2416 0.0015 0.053 Uiso 1 1 calc R . . C23B C 0.6059(4) 0.1061(4) 0.3598(2) 0.0410(9) Uani 1 1 d . . . H23B H 0.6036 0.1882 0.3612 0.049 Uiso 1 1 calc R . . C24A C 0.5764(5) -0.2576(4) -0.0100(2) 0.0493(11) Uani 1 1 d . . . H24A H 0.5582 -0.3312 -0.0419 0.059 Uiso 1 1 calc R . . C24B C 0.7000(5) 0.0449(4) 0.3331(3) 0.0516(11) Uani 1 1 d . . . H24B H 0.7611 0.0854 0.3158 0.062 Uiso 1 1 calc R . . C25A C 0.7020(5) -0.2019(4) 0.0109(2) 0.0454(10) Uani 1 1 d . . . H25A H 0.7683 -0.2387 -0.0067 0.054 Uiso 1 1 calc R . . C25B C 0.7029(5) -0.0782(5) 0.3323(3) 0.0553(12) Uani 1 1 d . . . H25B H 0.7672 -0.1184 0.3147 0.066 Uiso 1 1 calc R . . C26A C 0.7326(4) -0.0918(4) 0.0579(2) 0.0386(8) Uani 1 1 d . . . H26A H 0.8179 -0.0538 0.0711 0.046 Uiso 1 1 calc R . . C26B C 0.6134(4) -0.1413(4) 0.3567(2) 0.0464(10) Uani 1 1 d . . . H26B H 0.6168 -0.223 0.3564 0.056 Uiso 1 1 calc R . . C27A C 0.6325(4) -0.0394(3) 0.08489(18) 0.0339(8) Uani 1 1 d . . . C27B C 0.5180(4) -0.0795(3) 0.38191(19) 0.0367(9) Uani 1 1 d . . . C28A C 0.6328(4) 0.0733(3) 0.13561(19) 0.0366(8) Uani 1 1 d . . . C28B C 0.4074(4) -0.1224(3) 0.40967(19) 0.0395(9) Uani 1 1 d . . . C29A C 0.7341(5) 0.1623(4) 0.1708(2) 0.0477(10) Uani 1 1 d . . . H29A H 0.8187 0.1566 0.1641 0.057 Uiso 1 1 calc R . . C29B C 0.3636(5) -0.2376(4) 0.4173(2) 0.0515(12) Uani 1 1 d . . . H29B H 0.4069 -0.3041 0.4039 0.062 Uiso 1 1 calc R . . C30A C 0.7051(6) 0.2607(4) 0.2164(2) 0.0601(13) Uani 1 1 d . . . H30A H 0.7721 0.3206 0.2411 0.072 Uiso 1 1 calc R . . C30B C 0.2544(6) -0.2498(5) 0.4453(3) 0.0634(14) Uani 1 1 d . . . H30B H 0.225 -0.3251 0.4513 0.076 Uiso 1 1 calc R . . C31A C 0.5798(7) 0.2715(4) 0.2259(2) 0.0625(14) Uani 1 1 d . . . H31A H 0.5633 0.3384 0.2565 0.075 Uiso 1 1 calc R . . C31B C 0.1893(6) -0.1516(5) 0.4644(3) 0.0661(15) Uani 1 1 d . . . H31B H 0.1154 -0.1621 0.4822 0.079 Uiso 1 1 calc R . . C32A C 0.4777(5) 0.1831(4) 0.1901(2) 0.0506(11) Uani 1 1 d . . . H32A H 0.3927 0.1907 0.1958 0.061 Uiso 1 1 calc R . . C32B C 0.2313(5) -0.0382(5) 0.4576(2) 0.0549(12) Uani 1 1 d . . . H32B H 0.1871 0.0277 0.471 0.066 Uiso 1 1 calc R . . C33A C 0.5056(4) 0.0834(3) 0.14582(19) 0.0386(9) Uani 1 1 d . . . C33B C 0.3408(4) -0.0245(3) 0.43042(19) 0.0360(8) Uani 1 1 d . . . N1A N 0.1973(3) -0.2169(3) 0.15457(15) 0.0338(7) Uani 1 1 d . . . N1B N 0.1793(3) 0.2720(2) 0.34229(14) 0.0253(6) Uani 1 1 d . . . N2A N 0.3410(3) -0.0940(3) 0.13629(15) 0.0308(6) Uani 1 1 d . . . N2B N 0.3139(3) 0.1502(2) 0.37397(14) 0.0284(6) Uani 1 1 d . . . Br1A Br -0.06008(4) -0.14566(4) -0.096092(19) 0.03744(11) Uani 1 1 d . . . Br1B Br 0.42885(4) 0.53025(4) 0.59842(2) 0.05005(13) Uani 1 1 d . . . Ag1A Ag 0.08947(3) -0.13563(3) 0.017001(14) 0.03612(9) Uani 1 1 d . . . Ag1B Ag 0.35528(3) 0.38762(2) 0.486573(14) 0.03436(9) 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 C1A 0.0372(19) 0.0322(17) 0.0312(18) 0.0117(14) 0.0125(15) 0.0114(15) C1B 0.0218(15) 0.0219(14) 0.0267(16) 0.0081(12) 0.0007(12) 0.0033(12) C2A 0.057(2) 0.0291(17) 0.0240(17) 0.0088(14) 0.0035(16) 0.0101(16) C2B 0.039(2) 0.0331(17) 0.0218(16) 0.0005(13) -0.0029(14) 0.0091(15) C3A 0.040(2) 0.044(2) 0.0245(17) 0.0072(15) 0.0013(15) 0.0159(17) C3B 0.050(2) 0.0286(17) 0.0230(17) -0.0019(13) -0.0053(15) 0.0127(16) C11A 0.068(3) 0.0306(18) 0.0226(17) 0.0089(14) -0.0010(18) -0.0074(18) C11B 0.0280(17) 0.0258(15) 0.0231(16) 0.0047(12) -0.0014(13) 0.0088(13) C12A 0.115(5) 0.032(2) 0.026(2) 0.0083(16) 0.007(2) -0.004(2) C12B 0.0315(18) 0.0345(17) 0.0269(17) 0.0092(14) 0.0049(14) 0.0090(14) C13A 0.136(6) 0.031(2) 0.043(3) 0.008(2) -0.012(3) -0.025(3) C13B 0.053(2) 0.0366(19) 0.044(2) 0.0191(17) 0.0086(19) 0.0194(18) C14A 0.099(5) 0.054(3) 0.046(3) 0.018(2) -0.003(3) -0.035(3) C14B 0.050(2) 0.043(2) 0.048(2) 0.0103(19) 0.0041(19) 0.0309(19) C15A 0.066(3) 0.067(3) 0.047(3) 0.029(2) -0.007(2) -0.024(2) C15B 0.036(2) 0.057(2) 0.042(2) 0.0070(19) 0.0108(17) 0.0206(18) C16A 0.051(2) 0.040(2) 0.032(2) 0.0148(16) -0.0021(17) -0.0109(18) C16B 0.0279(17) 0.0387(18) 0.0320(19) 0.0077(15) 0.0086(14) 0.0067(14) C17A 0.159(7) 0.041(2) 0.043(3) 0.003(2) 0.019(3) 0.029(3) C17B 0.048(2) 0.054(2) 0.038(2) 0.0224(19) 0.0191(18) 0.0123(19) C18A 0.141(7) 0.101(5) 0.086(5) 0.025(4) -0.009(5) -0.086(5) C18B 0.084(4) 0.077(4) 0.074(4) 0.027(3) 0.017(3) 0.060(3) C19A 0.044(2) 0.045(2) 0.054(3) 0.011(2) 0.014(2) 0.0036(18) C19B 0.053(3) 0.059(3) 0.052(3) 0.021(2) 0.030(2) 0.007(2) C21A 0.0346(19) 0.0388(18) 0.0272(18) 0.0093(15) 0.0056(15) 0.0059(15) C21B 0.0381(19) 0.0257(15) 0.0242(16) 0.0054(13) -0.0034(14) 0.0106(14) C22A 0.0353(19) 0.0427(19) 0.0261(18) 0.0083(15) 0.0070(15) 0.0049(16) C22B 0.0361(19) 0.0321(17) 0.0274(17) 0.0081(14) -0.0049(14) 0.0120(15) C23A 0.045(2) 0.047(2) 0.034(2) -0.0020(17) 0.0096(17) -0.0082(18) C23B 0.041(2) 0.0367(19) 0.043(2) 0.0121(17) -0.0009(17) 0.0080(16) C24A 0.062(3) 0.043(2) 0.041(2) -0.0036(18) 0.023(2) 0.002(2) C24B 0.042(2) 0.062(3) 0.052(3) 0.018(2) 0.004(2) 0.011(2) C25A 0.055(3) 0.042(2) 0.048(2) 0.0134(19) 0.026(2) 0.0107(19) C25B 0.051(3) 0.066(3) 0.051(3) 0.012(2) 0.007(2) 0.034(2) C26A 0.034(2) 0.043(2) 0.042(2) 0.0149(17) 0.0116(17) 0.0015(16) C26B 0.056(3) 0.041(2) 0.043(2) 0.0114(18) 0.004(2) 0.028(2) C27A 0.038(2) 0.0382(18) 0.0261(17) 0.0112(15) 0.0054(15) 0.0037(15) C27B 0.043(2) 0.0343(18) 0.0266(18) 0.0065(14) -0.0082(15) 0.0153(16) C28A 0.047(2) 0.0355(18) 0.0250(18) 0.0097(15) 0.0010(16) 0.0000(16) C28B 0.052(2) 0.0319(17) 0.0278(18) 0.0101(14) -0.0093(16) 0.0078(16) C29A 0.058(3) 0.040(2) 0.038(2) 0.0064(17) 0.0027(19) -0.0090(19) C29B 0.071(3) 0.036(2) 0.039(2) 0.0140(18) -0.011(2) 0.004(2) C30A 0.090(4) 0.043(2) 0.039(2) 0.0035(19) 0.008(3) -0.011(2) C30B 0.081(4) 0.054(3) 0.050(3) 0.025(2) -0.004(3) -0.010(3) C31A 0.114(5) 0.032(2) 0.040(3) -0.0001(18) 0.024(3) 0.008(2) C31B 0.064(3) 0.088(4) 0.056(3) 0.040(3) 0.017(3) -0.002(3) C32A 0.077(3) 0.040(2) 0.041(2) 0.0105(18) 0.022(2) 0.015(2) C32B 0.064(3) 0.067(3) 0.040(2) 0.023(2) 0.012(2) 0.017(2) C33A 0.053(2) 0.0374(19) 0.0268(18) 0.0111(15) 0.0070(17) 0.0064(17) C33B 0.044(2) 0.0396(19) 0.0237(17) 0.0115(15) -0.0006(15) 0.0109(16) N1A 0.0481(19) 0.0286(14) 0.0250(15) 0.0085(12) 0.0060(13) 0.0055(13) N1B 0.0285(14) 0.0238(12) 0.0216(13) 0.0040(10) 0.0008(11) 0.0074(11) N2A 0.0294(15) 0.0380(15) 0.0263(15) 0.0088(12) 0.0057(12) 0.0094(12) N2B 0.0353(16) 0.0266(13) 0.0213(14) 0.0049(11) -0.0002(11) 0.0118(12) Br1A 0.0361(2) 0.0483(2) 0.02493(19) 0.00792(15) 0.00176(14) -0.00071(16) Br1B 0.0472(2) 0.0506(2) 0.0400(2) -0.01812(18) 0.01121(19) -0.00500(19) Ag1A 0.03423(16) 0.04847(17) 0.02668(15) 0.01479(12) 0.00353(11) 0.00248(12) Ag1B 0.03917(17) 0.02771(14) 0.02868(15) -0.00266(10) -0.00197(11) 0.00770(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1A N2A 1.333(5) . ? C1A N1A 1.344(4) . ? C1A Ag1A 2.103(4) . ? C1B N2B 1.340(4) . ? C1B N1B 1.349(4) . ? C1B Ag1B 2.085(3) . ? C2A C3A 1.327(6) . ? C2A N1A 1.384(5) . ? C2A H2A 0.93 . ? C2B C3B 1.341(5) . ? C2B N1B 1.371(4) . ? C2B H2B 0.93 . ? C3A N2A 1.391(4) . ? C3A H3A 0.93 . ? C3B N2B 1.373(4) . ? C3B H3B 0.93 . ? C11A C16A 1.387(7) . ? C11A C12A 1.398(6) . ? C11A N1A 1.446(5) . ? C11B C12B 1.380(5) . ? C11B C16B 1.407(5) . ? C11B N1B 1.439(4) . ? C12A C13A 1.415(8) . ? C12A C17A 1.489(9) . ? C12B C13B 1.392(5) . ? C12B C17B 1.511(5) . ? C13A C14A 1.352(9) . ? C13A H13A 0.93 . ? C13B C14B 1.393(6) . ? C13B H13B 0.93 . ? C14A C15A 1.379(8) . ? C14A C18A 1.513(8) . ? C14B C15B 1.378(6) . ? C14B C18B 1.502(5) . ? C15A C16A 1.387(6) . ? C15A H15A 0.93 . ? C15B C16B 1.384(5) . ? C15B H15B 0.93 . ? C16A C19A 1.509(6) . ? C16B C19B 1.508(5) . ? C17A H17A 0.96 . ? C17A H17B 0.96 . ? C17A H17C 0.96 . ? C17B H17D 0.96 . ? C17B H17E 0.96 . ? C17B H17F 0.96 . ? C18A H18A 0.96 . ? C18A H18B 0.96 . ? C18A H18C 0.96 . ? C18B H18D 0.96 . ? C18B H18E 0.96 . ? C18B H18F 0.96 . ? C19A H19A 0.96 . ? C19A H19B 0.96 . ? C19A H19C 0.96 . ? C19B H19D 0.96 . ? C19B H19E 0.96 . ? C19B H19F 0.96 . ? C21A N2A 1.478(5) . ? C21A C33A 1.515(5) . ? C21A C22A 1.522(5) . ? C21A H21A 0.98 . ? C21B N2B 1.464(4) . ? C21B C22B 1.509(5) . ? C21B C33B 1.520(5) . ? C21B H21B 0.98 . ? C22A C23A 1.366(5) . ? C22A C27A 1.393(5) . ? C22B C23B 1.380(6) . ? C22B C27B 1.391(5) . ? C23A C24A 1.397(6) . ? C23A H23A 0.93 . ? C23B C24B 1.381(6) . ? C23B H23B 0.93 . ? C24A C25A 1.369(6) . ? C24A H24A 0.93 . ? C24B C25B 1.399(7) . ? C24B H24B 0.93 . ? C25A C26A 1.387(6) . ? C25A H25A 0.93 . ? C25B C26B 1.373(7) . ? C25B H25B 0.93 . ? C26A C27A 1.394(5) . ? C26A H26A 0.93 . ? C26B C27B 1.383(6) . ? C26B H26B 0.93 . ? C27A C28A 1.472(5) . ? C27B C28B 1.484(6) . ? C28A C29A 1.387(6) . ? C28A C33A 1.400(6) . ? C28B C33B 1.392(5) . ? C28B C29B 1.408(6) . ? C29A C30A 1.394(7) . ? C29A H29A 0.93 . ? C29B C30B 1.390(8) . ? C29B H29B 0.93 . ? C30A C31A 1.377(8) . ? C30A H30A 0.93 . ? C30B C31B 1.378(8) . ? C30B H30B 0.93 . ? C31A C32A 1.391(7) . ? C31A H31A 0.93 . ? C31B C32B 1.378(7) . ? C31B H31B 0.93 . ? C32A C33A 1.386(6) . ? C32A H32A 0.93 . ? C32B C33B 1.385(6) . ? C32B H32B 0.93 . ? Br1A Ag1A 2.4514(6) . ? Br1B Ag1B 2.4418(6) . ? 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 N2A C1A N1A 105.4(3) . . ? N2A C1A Ag1A 128.2(3) . . ? N1A C1A Ag1A 126.3(3) . . ? N2B C1B N1B 104.6(3) . . ? N2B C1B Ag1B 128.8(2) . . ? N1B C1B Ag1B 126.2(2) . . ? C3A C2A N1A 106.9(3) . . ? C3A C2A H2A 126.6 . . ? N1A C2A H2A 126.6 . . ? C3B C2B N1B 106.3(3) . . ? C3B C2B H2B 126.8 . . ? N1B C2B H2B 126.8 . . ? C2A C3A N2A 106.7(3) . . ? C2A C3A H3A 126.6 . . ? N2A C3A H3A 126.6 . . ? C2B C3B N2B 107.0(3) . . ? C2B C3B H3B 126.5 . . ? N2B C3B H3B 126.5 . . ? C16A C11A C12A 121.6(4) . . ? C16A C11A N1A 119.5(3) . . ? C12A C11A N1A 118.9(4) . . ? C12B C11B C16B 122.6(3) . . ? C12B C11B N1B 118.8(3) . . ? C16B C11B N1B 118.6(3) . . ? C11A C12A C13A 116.5(5) . . ? C11A C12A C17A 121.3(5) . . ? C13A C12A C17A 122.3(5) . . ? C11B C12B C13B 117.6(3) . . ? C11B C12B C17B 121.7(3) . . ? C13B C12B C17B 120.6(3) . . ? C14A C13A C12A 122.5(5) . . ? C14A C13A H13A 118.7 . . ? C12A C13A H13A 118.7 . . ? C12B C13B C14B 121.5(4) . . ? C12B C13B H13B 119.3 . . ? C14B C13B H13B 119.3 . . ? C13A C14A C15A 119.4(5) . . ? C13A C14A C18A 120.4(6) . . ? C15A C14A C18A 120.2(7) . . ? C15B C14B C13B 119.1(3) . . ? C15B C14B C18B 120.9(4) . . ? C13B C14B C18B 120.0(4) . . ? C14A C15A C16A 121.0(6) . . ? C14A C15A H15A 119.5 . . ? C16A C15A H15A 119.5 . . ? C14B C15B C16B 121.7(4) . . ? C14B C15B H15B 119.2 . . ? C16B C15B H15B 119.2 . . ? C11A C16A C15A 118.9(4) . . ? C11A C16A C19A 121.3(4) . . ? C15A C16A C19A 119.8(5) . . ? C15B C16B C11B 117.5(3) . . ? C15B C16B C19B 120.2(4) . . ? C11B C16B C19B 122.2(3) . . ? C12A C17A H17A 109.5 . . ? C12A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C12A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C12B C17B H17D 109.5 . . ? C12B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C12B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C14A C18A H18A 109.5 . . ? C14A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C14A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C14B C18B H18D 109.5 . . ? C14B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C14B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C16A C19A H19A 109.5 . . ? C16A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C16A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C16B C19B H19D 109.5 . . ? C16B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C16B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? N2A C21A C33A 114.9(3) . . ? N2A C21A C22A 111.5(3) . . ? C33A C21A C22A 102.7(3) . . ? N2A C21A H21A 109.2 . . ? C33A C21A H21A 109.2 . . ? C22A C21A H21A 109.2 . . ? N2B C21B C22B 114.1(3) . . ? N2B C21B C33B 112.1(3) . . ? C22B C21B C33B 103.1(3) . . ? N2B C21B H21B 109.1 . . ? C22B C21B H21B 109.1 . . ? C33B C21B H21B 109.1 . . ? C23A C22A C27A 121.6(4) . . ? C23A C22A C21A 128.4(4) . . ? C27A C22A C21A 110.0(3) . . ? C23B C22B C27B 120.7(4) . . ? C23B C22B C21B 129.2(3) . . ? C27B C22B C21B 110.1(3) . . ? C22A C23A C24A 118.5(4) . . ? C22A C23A H23A 120.7 . . ? C24A C23A H23A 120.7 . . ? C22B C23B C24B 118.8(4) . . ? C22B C23B H23B 120.6 . . ? C24B C23B H23B 120.6 . . ? C25A C24A C23A 120.4(4) . . ? C25A C24A H24A 119.8 . . ? C23A C24A H24A 119.8 . . ? C23B C24B C25B 119.7(5) . . ? C23B C24B H24B 120.1 . . ? C25B C24B H24B 120.1 . . ? C24A C25A C26A 121.4(4) . . ? C24A C25A H25A 119.3 . . ? C26A C25A H25A 119.3 . . ? C26B C25B C24B 121.8(4) . . ? C26B C25B H25B 119.1 . . ? C24B C25B H25B 119.1 . . ? C25A C26A C27A 118.5(4) . . ? C25A C26A H26A 120.8 . . ? C27A C26A H26A 120.8 . . ? C25B C26B C27B 117.8(4) . . ? C25B C26B H26B 121.1 . . ? C27B C26B H26B 121.1 . . ? C22A C27A C26A 119.6(3) . . ? C22A C27A C28A 108.6(3) . . ? C26A C27A C28A 131.8(4) . . ? C26B C27B C22B 121.0(4) . . ? C26B C27B C28B 130.5(4) . . ? C22B C27B C28B 108.5(3) . . ? C29A C28A C33A 120.4(4) . . ? C29A C28A C27A 130.6(4) . . ? C33A C28A C27A 109.0(3) . . ? C33B C28B C29B 119.4(4) . . ? C33B C28B C27B 108.6(3) . . ? C29B C28B C27B 131.9(4) . . ? C28A C29A C30A 118.0(5) . . ? C28A C29A H29A 121 . . ? C30A C29A H29A 121 . . ? C30B C29B C28B 118.6(4) . . ? C30B C29B H29B 120.7 . . ? C28B C29B H29B 120.7 . . ? C31A C30A C29A 121.7(5) . . ? C31A C30A H30A 119.2 . . ? C29A C30A H30A 119.2 . . ? C31B C30B C29B 120.7(5) . . ? C31B C30B H30B 119.6 . . ? C29B C30B H30B 119.6 . . ? C30A C31A C32A 120.5(4) . . ? C30A C31A H31A 119.7 . . ? C32A C31A H31A 119.7 . . ? C30B C31B C32B 121.4(5) . . ? C30B C31B H31B 119.3 . . ? C32B C31B H31B 119.3 . . ? C33A C32A C31A 118.4(5) . . ? C33A C32A H32A 120.8 . . ? C31A C32A H32A 120.8 . . ? C31B C32B C33B 118.5(5) . . ? C31B C32B H32B 120.8 . . ? C33B C32B H32B 120.8 . . ? C32A C33A C28A 120.9(4) . . ? C32A C33A C21A 129.3(4) . . ? C28A C33A C21A 109.7(3) . . ? C32B C33B C28B 121.4(4) . . ? C32B C33B C21B 129.0(4) . . ? C28B C33B C21B 109.6(4) . . ? C1A N1A C2A 110.4(3) . . ? C1A N1A C11A 123.8(3) . . ? C2A N1A C11A 125.8(3) . . ? C1B N1B C2B 111.2(3) . . ? C1B N1B C11B 124.6(3) . . ? C2B N1B C11B 124.3(3) . . ? C1A N2A C3A 110.5(3) . . ? C1A N2A C21A 123.9(3) . . ? C3A N2A C21A 125.0(3) . . ? C1B N2B C3B 111.0(3) . . ? C1B N2B C21B 124.9(3) . . ? C3B N2B C21B 123.7(3) . . ? C1A Ag1A Br1A 172.76(9) . . ? C1B Ag1B Br1B 173.22(9) . . ? _database_code_depnum_ccdc_archive 'CCDC 969668' ####################################################################### # # 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_complex_7 _audit_creation_date 2013-10-26T13:08:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C33 H33 N2 Rh' _chemical_formula_moiety 'C33 H33 N2 Rh' _chemical_formula_weight 560.52 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system Monoclinic _space_group_name_H-M_alt 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 17.2079(8) _cell_length_b 9.2276(9) _cell_length_c 17.4436(11) _cell_angle_alpha 90 _cell_angle_beta 103.472(4) _cell_angle_gamma 90 _cell_volume 2693.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 1.80 _cell_measurement_reflns_used 9999 _cell_measurement_theta_max 36.29 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160.0 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; 'SADABS, Sheldrick, Bruker, 2000' ; _exptl_absorpt_correction_T_min 0.7027 _exptl_absorpt_correction_T_max 0.7464 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'Incoatec I\mS Microsource ' _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 63604 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0126 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5381 _reflns_number_gt 4921 _reflns_threshold_expression >2\s(I) _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.975 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0300P)^2^+1.8063P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5381 _refine_ls_number_parameters 344 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.587 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.82327(12) 0.2491(2) 0.61113(11) 0.0277(4) Uani 1 1 d . . . C2 C 0.69301(13) 0.2555(2) 0.61303(14) 0.0390(5) Uani 1 1 d . . . H2 H 0.6387 0.2763 0.5987 0.047 Uiso 1 1 calc R . . C3 C 0.73108(12) 0.1785(3) 0.67645(13) 0.0395(5) Uani 1 1 d . . . H3 H 0.7085 0.1368 0.7147 0.047 Uiso 1 1 calc R . . C11 C 0.73525(10) 0.3886(2) 0.50366(11) 0.0292(4) Uani 1 1 d . . . C12 C 0.72834(12) 0.3246(3) 0.43006(12) 0.0391(5) Uani 1 1 d . . . C13 C 0.71462(13) 0.4156(3) 0.36451(12) 0.0466(6) Uani 1 1 d . . . H13 H 0.7109 0.3752 0.3149 0.056 Uiso 1 1 calc R . . C14 C 0.70637(12) 0.5628(3) 0.37063(14) 0.0470(6) Uani 1 1 d . . . C15 C 0.71318(12) 0.6220(3) 0.44484(15) 0.0449(5) Uani 1 1 d . . . H15 H 0.7079 0.7217 0.4495 0.054 Uiso 1 1 calc R . . C16 C 0.72763(11) 0.5371(2) 0.51267(12) 0.0354(4) Uani 1 1 d . . . C17 C 0.73400(19) 0.1627(3) 0.42157(15) 0.0625(7) Uani 1 1 d . . . H17A H 0.7843 0.1293 0.4528 0.094 Uiso 1 1 calc R . . H17B H 0.7301 0.1388 0.3672 0.094 Uiso 1 1 calc R . . H17C H 0.6912 0.1169 0.4392 0.094 Uiso 1 1 calc R . . C18 C 0.68923(15) 0.6576(4) 0.29762(17) 0.0705(9) Uani 1 1 d . . . H18A H 0.7076 0.6098 0.2562 0.106 Uiso 1 1 calc R . . H18B H 0.7165 0.7485 0.3095 0.106 Uiso 1 1 calc R . . H18C H 0.6328 0.6745 0.2809 0.106 Uiso 1 1 calc R . . C19 C 0.73445(15) 0.6033(3) 0.59277(15) 0.0526(6) Uani 1 1 d . . . H19A H 0.6915 0.5691 0.6145 0.079 Uiso 1 1 calc R . . H19B H 0.7316 0.7069 0.5881 0.079 Uiso 1 1 calc R . . H19C H 0.7846 0.5761 0.6268 0.079 Uiso 1 1 calc R . . C21 C 0.88632(11) 0.1307(2) 0.72443(10) 0.0283(4) Uani 1 1 d . . . C22 C 0.91108(11) -0.0203(2) 0.73981(11) 0.0288(4) Uani 1 1 d . . . C23 C 0.89704(13) -0.1441(2) 0.69285(13) 0.0381(5) Uani 1 1 d . . . H23 H 0.8640 -0.1404 0.6425 0.046 Uiso 1 1 calc R . . C24 C 0.93337(15) -0.2732(2) 0.72276(16) 0.0466(6) Uani 1 1 d . . . H24 H 0.9239 -0.3566 0.6920 0.056 Uiso 1 1 calc R . . C25 C 0.98365(14) -0.2803(2) 0.79784(16) 0.0441(6) Uani 1 1 d . . . H25 H 1.0073 -0.3680 0.8166 0.053 Uiso 1 1 calc R . . C26 C 0.99855(12) -0.1588(2) 0.84446(13) 0.0359(4) Uani 1 1 d . . . H26 H 1.0328 -0.1634 0.8943 0.043 Uiso 1 1 calc R . . C27 C 0.96177(11) -0.0288(2) 0.81626(11) 0.0290(4) Uani 1 1 d . . . C28 C 0.96298(11) 0.1118(2) 0.85370(11) 0.0297(4) Uani 1 1 d . . . C29 C 1.00010(14) 0.1613(2) 0.92874(12) 0.0434(5) Uani 1 1 d . . . H29 H 1.0352 0.1019 0.9637 0.052 Uiso 1 1 calc R . . C30 C 0.98391(18) 0.3001(3) 0.95030(14) 0.0561(7) Uani 1 1 d . . . H30 H 1.0079 0.3338 1.0005 0.067 Uiso 1 1 calc R . . C31 C 0.93238(17) 0.3900(2) 0.89811(14) 0.0541(7) Uani 1 1 d . . . H31 H 0.9211 0.4821 0.9143 0.065 Uiso 1 1 calc R . . C32 C 0.89756(14) 0.3446(2) 0.82234(13) 0.0406(5) Uani 1 1 d . . . H32 H 0.8643 0.4064 0.7872 0.049 Uiso 1 1 calc R . . C33 C 0.91293(12) 0.2057(2) 0.79962(11) 0.0289(4) Uani 1 1 d . . . C41 C 1.06350(12) 0.2466(2) 0.71065(13) 0.0385(5) Uani 1 1 d D . . C42 C 1.09027(12) 0.4015(2) 0.70545(12) 0.0393(5) Uani 1 1 d . . . H42A H 1.1482 0.4049 0.7207 0.047 Uiso 1 1 calc R . . H42B H 1.0701 0.4597 0.7429 0.047 Uiso 1 1 calc R . . C43 C 1.06225(12) 0.4687(2) 0.62309(12) 0.0360(4) Uani 1 1 d . . . H43A H 1.0594 0.5731 0.6283 0.043 Uiso 1 1 calc R . . H43B H 1.1014 0.4478 0.5926 0.043 Uiso 1 1 calc R . . C44 C 0.98124(11) 0.4125(2) 0.57882(11) 0.0301(4) Uani 1 1 d D . . C45 C 0.96986(12) 0.2944(2) 0.52759(11) 0.0331(4) Uani 1 1 d D . . C46 C 1.03623(14) 0.2041(2) 0.50940(14) 0.0437(5) Uani 1 1 d . . . H46A H 1.0627 0.2593 0.4755 0.052 Uiso 1 1 calc R . . H46B H 1.0134 0.1183 0.4807 0.052 Uiso 1 1 calc R . . C47 C 1.09805(14) 0.1578(3) 0.58288(15) 0.0484(6) Uani 1 1 d . . . H47A H 1.1216 0.0667 0.5722 0.058 Uiso 1 1 calc R . . H47B H 1.1403 0.2297 0.5942 0.058 Uiso 1 1 calc R . . C48 C 1.06383(12) 0.1396(2) 0.65525(15) 0.0423(5) Uani 1 1 d D . . N1 N 0.75078(9) 0.29839(18) 0.57288(9) 0.0290(3) Uani 1 1 d . . . N2 N 0.81046(9) 0.17412(18) 0.67299(9) 0.0296(3) Uani 1 1 d . . . Rh1 Rh 0.944562(8) 0.231197(16) 0.636958(8) 0.02776(6) Uani 1 1 d . . . H41 H 1.0579(15) 0.217(2) 0.7692(6) 0.051(7) Uiso 1 1 d D . . H44 H 0.9331(8) 0.4906(17) 0.5716(12) 0.034(5) Uiso 1 1 d D . . H45 H 0.9143(7) 0.290(3) 0.4831(10) 0.047(7) Uiso 1 1 d D . . H48 H 1.0540(14) 0.0292(9) 0.6718(14) 0.052(7) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0231(9) 0.0382(10) 0.0215(9) -0.0003(7) 0.0046(8) -0.0021(7) C2 0.0242(10) 0.0572(13) 0.0387(12) -0.0010(9) 0.0133(10) -0.0055(9) C3 0.0278(10) 0.0561(13) 0.0382(11) 0.0018(10) 0.0148(10) -0.0092(9) C11 0.0162(8) 0.0473(11) 0.0224(9) 0.0003(8) 0.0011(8) 0.0017(7) C12 0.0281(10) 0.0600(14) 0.0268(10) -0.0050(9) 0.0017(9) 0.0043(9) C13 0.0292(11) 0.0851(18) 0.0237(10) 0.0012(10) 0.0026(9) 0.0024(11) C14 0.0175(9) 0.0812(18) 0.0416(13) 0.0203(12) 0.0050(10) 0.0027(10) C15 0.0248(10) 0.0494(13) 0.0602(15) 0.0105(11) 0.0090(11) 0.0033(9) C16 0.0198(9) 0.0481(12) 0.0378(11) -0.0024(9) 0.0056(9) 0.0002(8) C17 0.0757(19) 0.0662(17) 0.0423(14) -0.0198(12) 0.0068(14) 0.0109(14) C18 0.0353(13) 0.115(3) 0.0618(17) 0.0459(17) 0.0118(13) 0.0086(14) C19 0.0511(14) 0.0530(14) 0.0538(15) -0.0185(11) 0.0127(12) -0.0046(11) C21 0.0262(9) 0.0357(10) 0.0225(9) 0.0050(7) 0.0047(8) -0.0060(7) C22 0.0277(9) 0.0345(10) 0.0282(9) 0.0015(7) 0.0143(8) -0.0065(7) C23 0.0365(11) 0.0446(12) 0.0371(11) -0.0082(9) 0.0168(10) -0.0091(9) C24 0.0460(13) 0.0369(11) 0.0661(17) -0.0149(10) 0.0319(13) -0.0076(9) C25 0.0375(12) 0.0366(11) 0.0655(16) 0.0059(10) 0.0266(12) 0.0057(9) C26 0.0276(10) 0.0401(11) 0.0428(12) 0.0086(9) 0.0138(9) 0.0011(8) C27 0.0243(9) 0.0344(10) 0.0307(10) 0.0052(7) 0.0110(8) -0.0048(7) C28 0.0293(10) 0.0325(10) 0.0273(9) 0.0059(7) 0.0064(8) -0.0070(7) C29 0.0490(13) 0.0433(12) 0.0311(11) 0.0092(9) -0.0043(10) -0.0116(10) C30 0.082(2) 0.0438(13) 0.0325(12) -0.0044(10) -0.0063(13) -0.0186(13) C31 0.0838(19) 0.0303(11) 0.0436(13) -0.0047(9) 0.0054(13) -0.0113(11) C32 0.0547(14) 0.0280(10) 0.0360(11) 0.0054(8) 0.0044(10) -0.0057(9) C33 0.0312(10) 0.0303(9) 0.0255(9) 0.0057(7) 0.0069(8) -0.0082(7) C41 0.0176(9) 0.0592(14) 0.0370(12) 0.0205(10) 0.0024(9) 0.0032(8) C42 0.0281(10) 0.0546(13) 0.0339(11) 0.0041(9) 0.0044(9) -0.0006(9) C43 0.0354(11) 0.0368(10) 0.0370(11) 0.0052(8) 0.0112(9) -0.0041(8) C44 0.0316(10) 0.0330(10) 0.0279(9) 0.0105(7) 0.0111(8) 0.0040(8) C45 0.0364(11) 0.0384(10) 0.0279(10) 0.0086(8) 0.0142(9) -0.0022(8) C46 0.0528(14) 0.0374(11) 0.0492(13) 0.0007(9) 0.0286(12) -0.0021(10) C47 0.0392(12) 0.0432(12) 0.0696(16) 0.0024(11) 0.0264(12) 0.0075(10) C48 0.0270(10) 0.0408(12) 0.0594(14) 0.0190(10) 0.0105(10) 0.0073(8) N1 0.0200(8) 0.0428(9) 0.0237(8) -0.0013(6) 0.0041(7) -0.0010(6) N2 0.0243(8) 0.0412(9) 0.0235(8) 0.0023(7) 0.0060(7) -0.0063(7) Rh1 0.02001(9) 0.03765(10) 0.02613(9) 0.01115(6) 0.00637(7) 0.00025(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.342(2) . ? C1 N1 1.349(2) . ? C1 Rh1 2.037(2) . ? C2 C3 1.349(3) . ? C2 N1 1.400(2) . ? C2 H2 0.9300 . ? C3 N2 1.382(2) . ? C3 H3 0.9300 . ? C11 C16 1.389(3) . ? C11 C12 1.393(3) . ? C11 N1 1.440(2) . ? C12 C13 1.394(3) . ? C12 C17 1.507(4) . ? C13 C14 1.372(4) . ? C13 H13 0.9300 . ? C14 C15 1.385(3) . ? C14 C18 1.516(3) . ? C15 C16 1.392(3) . ? C15 H15 0.9300 . ? C16 C19 1.504(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C21 N2 1.457(2) . ? C21 C33 1.459(3) . ? C21 C22 1.463(3) . ? C21 Rh1 2.2148(18) . ? C22 C23 1.394(3) . ? C22 C27 1.415(3) . ? C23 C24 1.389(3) . ? C23 H23 0.9300 . ? C24 C25 1.393(4) . ? C24 H24 0.9300 . ? C25 C26 1.373(3) . ? C25 H25 0.9300 . ? C26 C27 1.392(3) . ? C26 H26 0.9300 . ? C27 C28 1.451(3) . ? C28 C29 1.393(3) . ? C28 C33 1.416(3) . ? C29 C30 1.382(4) . ? C29 H29 0.9300 . ? C30 C31 1.388(4) . ? C30 H30 0.9300 . ? C31 C32 1.383(3) . ? C31 H31 0.9300 . ? C32 C33 1.385(3) . ? C32 H32 0.9300 . ? C41 C48 1.383(3) . ? C41 C42 1.511(3) . ? C41 Rh1 2.153(2) . ? C41 H41 1.0830(3) . ? C42 C43 1.536(3) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.519(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.394(3) . ? C44 Rh1 2.1271(19) . ? C44 H44 1.0830(3) . ? C45 C46 1.506(3) . ? C45 Rh1 2.1345(19) . ? C45 H45 1.0830(3) . ? C46 C47 1.524(4) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.522(3) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 Rh1 2.173(2) . ? C48 H48 1.0830(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 N2 C1 N1 105.38(17) . . ? N2 C1 Rh1 97.60(13) . . ? N1 C1 Rh1 156.70(14) . . ? C3 C2 N1 107.05(18) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 105.99(17) . . ? C2 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? C16 C11 C12 122.20(19) . . ? C16 C11 N1 118.66(17) . . ? C12 C11 N1 119.14(19) . . ? C11 C12 C13 117.5(2) . . ? C11 C12 C17 121.2(2) . . ? C13 C12 C17 121.3(2) . . ? C14 C13 C12 122.2(2) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 118.4(2) . . ? C13 C14 C18 120.6(3) . . ? C15 C14 C18 121.0(3) . . ? C14 C15 C16 122.1(2) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C11 C16 C15 117.5(2) . . ? C11 C16 C19 121.1(2) . . ? C15 C16 C19 121.4(2) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C21 C33 118.14(17) . . ? N2 C21 C22 123.74(16) . . ? C33 C21 C22 105.65(16) . . ? N2 C21 Rh1 86.84(10) . . ? C33 C21 Rh1 108.85(12) . . ? C22 C21 Rh1 111.45(12) . . ? C23 C22 C27 119.51(19) . . ? C23 C22 C21 132.03(19) . . ? C27 C22 C21 108.35(16) . . ? C24 C23 C22 118.8(2) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 121.3(2) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C26 C25 C24 120.5(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 119.2(2) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C26 C27 C22 120.70(19) . . ? C26 C27 C28 130.87(19) . . ? C22 C27 C28 108.39(17) . . ? C29 C28 C33 120.03(19) . . ? C29 C28 C27 132.18(19) . . ? C33 C28 C27 107.74(17) . . ? C30 C29 C28 118.8(2) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 120.9(2) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 120.9(2) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 119.0(2) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C28 120.18(18) . . ? C32 C33 C21 130.94(18) . . ? C28 C33 C21 108.88(17) . . ? C48 C41 C42 125.65(19) . . ? C48 C41 Rh1 72.16(13) . . ? C42 C41 Rh1 106.69(13) . . ? C48 C41 H41 119.8(13) . . ? C42 C41 H41 112.8(13) . . ? Rh1 C41 H41 105.4(14) . . ? C41 C42 C43 113.86(18) . . ? C41 C42 H42A 108.8 . . ? C43 C42 H42A 108.8 . . ? C41 C42 H42B 108.8 . . ? C43 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C44 C43 C42 112.87(16) . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? C42 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C45 C44 C43 124.63(17) . . ? C45 C44 Rh1 71.20(11) . . ? C43 C44 Rh1 111.43(12) . . ? C45 C44 H44 117.1(11) . . ? C43 C44 H44 114.7(11) . . ? Rh1 C44 H44 106.0(11) . . ? C44 C45 C46 124.57(19) . . ? C44 C45 Rh1 70.62(11) . . ? C46 C45 Rh1 111.09(14) . . ? C44 C45 H45 117.4(13) . . ? C46 C45 H45 114.3(13) . . ? Rh1 C45 H45 107.4(13) . . ? C45 C46 C47 113.14(18) . . ? C45 C46 H46A 109.0 . . ? C47 C46 H46A 109.0 . . ? C45 C46 H46B 109.0 . . ? C47 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C48 C47 C46 113.55(18) . . ? C48 C47 H47A 108.9 . . ? C46 C47 H47A 108.9 . . ? C48 C47 H47B 108.9 . . ? C46 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? C41 C48 C47 124.5(2) . . ? C41 C48 Rh1 70.57(12) . . ? C47 C48 Rh1 111.71(14) . . ? C41 C48 H48 117.3(13) . . ? C47 C48 H48 116.1(13) . . ? Rh1 C48 H48 101.8(13) . . ? C1 N1 C2 109.87(17) . . ? C1 N1 C11 125.41(15) . . ? C2 N1 C11 124.63(17) . . ? C1 N2 C3 111.67(17) . . ? C1 N2 C21 110.20(15) . . ? C3 N2 C21 137.20(16) . . ? C1 Rh1 C44 103.50(7) . . ? C1 Rh1 C45 101.07(7) . . ? C44 Rh1 C45 38.18(8) . . ? C1 Rh1 C41 155.41(8) . . ? C44 Rh1 C41 83.48(8) . . ? C45 Rh1 C41 98.75(8) . . ? C1 Rh1 C48 161.44(8) . . ? C44 Rh1 C48 90.06(8) . . ? C45 Rh1 C48 81.68(8) . . ? C41 Rh1 C48 37.27(9) . . ? C1 Rh1 C21 65.26(7) . . ? C44 Rh1 C21 152.87(7) . . ? C45 Rh1 C21 161.70(7) . . ? C41 Rh1 C21 97.82(8) . . ? C48 Rh1 C21 107.42(8) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 969669'