# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andy Hor' _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Substituent-dependent structures and catalysis of benzimidazole-tethered N-heterocyclic carbene complexes of Ag(I), Ni(II) and Pd(II) ; loop_ _publ_author_name 'Andy Hor' 'Jian Jin Hu' 'L L Koh' 'F W Li' # Attachment 'NHC2.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 760767' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H23 Cl N4 O' _chemical_formula_weight 370.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.9938(5) _cell_length_b 12.8455(13) _cell_length_c 30.023(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.145(3) _cell_angle_gamma 90.00 _cell_volume 1924.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1895 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 25.39 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.215 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8820 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13565 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4430 _reflns_number_gt 3062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.3942P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4430 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1412 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.47996(11) 0.37538(4) 0.31795(2) 0.03808(18) Uani 1 1 d . . . N1 N 0.3110(4) 0.68540(14) 0.34212(6) 0.0359(5) Uani 1 1 d . . . N2 N 0.1100(4) 0.59024(14) 0.39357(6) 0.0360(5) Uani 1 1 d . . . N3 N 0.0086(4) 0.60152(14) 0.27114(6) 0.0350(5) Uani 1 1 d . . . N4 N 0.1924(4) 0.61927(14) 0.20796(6) 0.0363(5) Uani 1 1 d . . . C1 C 0.1292(5) 0.61463(16) 0.34984(7) 0.0326(5) Uani 1 1 d . . . C2 C 0.4234(5) 0.70879(17) 0.38425(8) 0.0352(5) Uani 1 1 d . . . C3 C 0.6296(5) 0.77762(18) 0.39637(9) 0.0438(6) Uani 1 1 d . . . H3 H 0.7184 0.8163 0.3748 0.053 Uiso 1 1 calc R . . C4 C 0.6981(6) 0.7868(2) 0.44080(9) 0.0503(7) Uani 1 1 d . . . H4 H 0.8356 0.8331 0.4498 0.060 Uiso 1 1 calc R . . C5 C 0.5689(6) 0.7293(2) 0.47308(9) 0.0543(7) Uani 1 1 d . . . H5 H 0.6211 0.7380 0.5033 0.065 Uiso 1 1 calc R . . C6 C 0.3658(6) 0.6599(2) 0.46170(9) 0.0484(7) Uani 1 1 d . . . H6 H 0.2781 0.6211 0.4833 0.058 Uiso 1 1 calc R . . C7 C 0.2984(5) 0.65059(18) 0.41655(8) 0.0371(5) Uani 1 1 d . . . C8 C -0.0613(6) 0.5111(2) 0.41297(9) 0.0485(7) Uani 1 1 d . . . H8A H -0.2066 0.4933 0.3915 0.058 Uiso 1 1 calc R . . H8B H -0.1420 0.5397 0.4396 0.058 Uiso 1 1 calc R . . C9 C 0.0927(7) 0.4144(2) 0.42538(11) 0.0711(9) Uani 1 1 d . . . H9A H 0.1724 0.3858 0.3991 0.107 Uiso 1 1 calc R . . H9B H -0.0277 0.3635 0.4377 0.107 Uiso 1 1 calc R . . H9C H 0.2328 0.4313 0.4474 0.107 Uiso 1 1 calc R . . C10 C -0.0463(5) 0.5631(2) 0.31518(7) 0.0411(6) Uani 1 1 d . . . H10A H -0.0167 0.4877 0.3162 0.049 Uiso 1 1 calc R . . H10B H -0.2345 0.5763 0.3214 0.049 Uiso 1 1 calc R . . C11 C 0.1859(5) 0.56134(18) 0.24434(7) 0.0353(5) Uani 1 1 d . . . H11 H 0.2900 0.5016 0.2502 0.042 Uiso 1 1 calc R . . C12 C -0.1013(5) 0.68917(18) 0.25096(8) 0.0403(6) Uani 1 1 d . . . H12 H -0.2318 0.7330 0.2627 0.048 Uiso 1 1 calc R . . C13 C 0.0126(5) 0.69997(18) 0.21158(8) 0.0394(6) Uani 1 1 d . . . H13 H -0.0232 0.7526 0.1904 0.047 Uiso 1 1 calc R . . C14 C 0.3587(5) 0.60033(19) 0.16932(8) 0.0406(6) Uani 1 1 d . . . H14A H 0.4698 0.5384 0.1749 0.049 Uiso 1 1 calc R . . H14B H 0.4783 0.6598 0.1653 0.049 Uiso 1 1 calc R . . C15 C 0.1870(5) 0.58450(17) 0.12749(8) 0.0347(5) Uani 1 1 d . . . C16 C -0.0173(5) 0.51204(19) 0.12600(8) 0.0434(6) Uani 1 1 d . . . H16 H -0.0524 0.4725 0.1515 0.052 Uiso 1 1 calc R . . C17 C -0.1703(6) 0.4973(2) 0.08734(9) 0.0511(7) Uani 1 1 d . . . H17 H -0.3097 0.4481 0.0867 0.061 Uiso 1 1 calc R . . C18 C -0.1199(6) 0.5545(2) 0.04963(9) 0.0522(7) Uani 1 1 d . . . H18 H -0.2244 0.5444 0.0233 0.063 Uiso 1 1 calc R . . C19 C 0.0836(6) 0.6259(2) 0.05096(9) 0.0525(7) Uani 1 1 d . . . H19 H 0.1195 0.6648 0.0253 0.063 Uiso 1 1 calc R . . C20 C 0.2361(6) 0.64118(19) 0.08957(8) 0.0449(6) Uani 1 1 d . . . H20 H 0.3748 0.6907 0.0901 0.054 Uiso 1 1 calc R . . O1S O 0.3792(5) 0.87614(17) 0.28599(8) 0.0758(7) Uani 1 1 d . . . H1SA H 0.336(6) 0.810(3) 0.2979(10) 0.080 Uiso 1 1 d . . . H1SB H 0.376(7) 0.866(2) 0.2535(11) 0.080 Uiso 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 Cl1 0.0322(3) 0.0281(3) 0.0540(4) -0.0042(2) 0.0021(3) -0.0058(2) N1 0.0355(11) 0.0335(10) 0.0387(11) -0.0034(8) 0.0005(9) -0.0016(9) N2 0.0347(11) 0.0364(10) 0.0373(11) -0.0014(8) 0.0042(9) -0.0022(9) N3 0.0342(11) 0.0350(10) 0.0356(11) -0.0061(8) -0.0014(9) -0.0010(8) N4 0.0368(11) 0.0367(10) 0.0351(11) -0.0007(9) -0.0020(9) 0.0051(9) C1 0.0325(12) 0.0306(11) 0.0348(13) -0.0026(9) 0.0034(10) 0.0036(10) C2 0.0353(13) 0.0314(11) 0.0389(13) -0.0029(10) -0.0005(10) 0.0057(10) C3 0.0442(15) 0.0332(12) 0.0537(16) -0.0044(11) -0.0029(12) -0.0013(11) C4 0.0488(17) 0.0422(14) 0.0587(18) -0.0138(13) -0.0128(14) 0.0006(12) C5 0.0609(18) 0.0550(16) 0.0459(16) -0.0127(14) -0.0119(14) 0.0111(15) C6 0.0559(17) 0.0497(15) 0.0394(14) -0.0037(12) -0.0002(13) 0.0065(13) C7 0.0370(13) 0.0360(12) 0.0380(13) -0.0048(10) -0.0003(11) 0.0072(10) C8 0.0497(16) 0.0517(15) 0.0450(15) 0.0020(12) 0.0122(13) -0.0097(13) C9 0.092(3) 0.0488(17) 0.074(2) 0.0167(15) 0.0175(19) -0.0075(17) C10 0.0384(14) 0.0461(14) 0.0389(14) -0.0046(11) 0.0038(11) -0.0055(11) C11 0.0351(13) 0.0342(12) 0.0363(13) -0.0005(10) -0.0052(10) 0.0040(10) C12 0.0355(13) 0.0370(13) 0.0477(15) -0.0088(11) -0.0052(11) 0.0085(11) C13 0.0411(14) 0.0342(12) 0.0422(15) -0.0001(10) -0.0065(11) 0.0083(11) C14 0.0383(14) 0.0450(14) 0.0388(14) -0.0006(11) 0.0058(11) 0.0049(11) C15 0.0353(13) 0.0318(11) 0.0373(13) 0.0005(10) 0.0053(10) 0.0068(10) C16 0.0481(16) 0.0412(13) 0.0416(15) 0.0028(11) 0.0103(12) -0.0003(12) C17 0.0485(16) 0.0495(15) 0.0554(17) -0.0119(13) 0.0049(13) -0.0084(13) C18 0.0516(17) 0.0597(17) 0.0449(16) -0.0094(13) -0.0030(13) 0.0077(14) C19 0.0609(18) 0.0571(17) 0.0395(15) 0.0099(13) 0.0003(13) 0.0035(15) C20 0.0483(15) 0.0413(14) 0.0452(15) 0.0079(11) 0.0022(12) -0.0037(12) O1S 0.113(2) 0.0538(13) 0.0614(14) -0.0042(11) 0.0097(13) -0.0352(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.312(3) . ? N1 C2 1.397(3) . ? N2 C1 1.357(3) . ? N2 C7 1.383(3) . ? N2 C8 1.463(3) . ? N3 C11 1.323(3) . ? N3 C12 1.382(3) . ? N3 C10 1.447(3) . ? N4 C11 1.323(3) . ? N4 C13 1.379(3) . ? N4 C14 1.472(3) . ? C1 C10 1.490(3) . ? C2 C7 1.391(3) . ? C2 C3 1.395(3) . ? C3 C4 1.370(3) . ? C4 C5 1.396(4) . ? C5 C6 1.384(4) . ? C6 C7 1.390(3) . ? C8 C9 1.501(4) . ? C12 C13 1.338(3) . ? C14 C15 1.508(3) . ? C15 C16 1.381(3) . ? C15 C20 1.381(3) . ? C16 C17 1.378(4) . ? C17 C18 1.380(4) . ? C18 C19 1.369(4) . ? C19 C20 1.377(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C2 104.28(19) . . ? C1 N2 C7 106.37(19) . . ? C1 N2 C8 127.5(2) . . ? C7 N2 C8 126.0(2) . . ? C11 N3 C12 108.4(2) . . ? C11 N3 C10 125.2(2) . . ? C12 N3 C10 126.3(2) . . ? C11 N4 C13 108.7(2) . . ? C11 N4 C14 126.1(2) . . ? C13 N4 C14 125.1(2) . . ? N1 C1 N2 113.9(2) . . ? N1 C1 C10 125.3(2) . . ? N2 C1 C10 120.8(2) . . ? C7 C2 C3 120.3(2) . . ? C7 C2 N1 109.9(2) . . ? C3 C2 N1 129.8(2) . . ? C4 C3 C2 117.6(2) . . ? C3 C4 C5 121.7(3) . . ? C6 C5 C4 121.5(3) . . ? C5 C6 C7 116.4(3) . . ? N2 C7 C6 132.1(2) . . ? N2 C7 C2 105.6(2) . . ? C6 C7 C2 122.4(2) . . ? N2 C8 C9 111.9(2) . . ? N3 C10 C1 111.11(19) . . ? N4 C11 N3 108.7(2) . . ? C13 C12 N3 107.3(2) . . ? C12 C13 N4 107.0(2) . . ? N4 C14 C15 111.0(2) . . ? C16 C15 C20 118.8(2) . . ? C16 C15 C14 121.0(2) . . ? C20 C15 C14 120.2(2) . . ? C17 C16 C15 120.4(2) . . ? C16 C17 C18 120.4(3) . . ? C19 C18 C17 119.4(3) . . ? C18 C19 C20 120.4(3) . . ? C19 C20 C15 120.6(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.493 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.053 #===END data_1b _database_code_depnum_ccdc_archive 'CCDC 760768' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H29 Cl N4 O2' _chemical_formula_weight 416.94 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2268(7) _cell_length_b 9.7074(5) _cell_length_c 16.0600(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.8680(10) _cell_angle_gamma 90.00 _cell_volume 2202.05(19) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3289 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 25.39 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.198 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9108 _exptl_absorpt_correction_T_max 0.9689 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15263 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5046 _reflns_number_gt 3965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.4346P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5046 _refine_ls_number_parameters 278 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 N1 N 0.73417(10) 0.60438(14) 0.05483(9) 0.0421(3) Uani 1 1 d . . . N2 N 0.83221(10) 0.42780(13) 0.09108(9) 0.0374(3) Uani 1 1 d . . . N3 N 0.82280(10) 0.75742(13) 0.19616(9) 0.0378(3) Uani 1 1 d . . . N4 N 0.74211(10) 0.93465(14) 0.22547(8) 0.0364(3) Uani 1 1 d . . . C1 C 0.81375(12) 0.56546(16) 0.09828(11) 0.0379(4) Uani 1 1 d . . . C2 C 0.69697(13) 0.48499(17) 0.01617(11) 0.0398(4) Uani 1 1 d . . . C3 C 0.61260(14) 0.4642(2) -0.03582(13) 0.0490(5) Uani 1 1 d . . . H3 H 0.5708 0.5375 -0.0509 0.059 Uiso 1 1 calc R . . C4 C 0.59250(15) 0.3322(2) -0.06439(13) 0.0551(5) Uani 1 1 d . . . H4 H 0.5359 0.3154 -0.0995 0.066 Uiso 1 1 calc R . . C5 C 0.65429(15) 0.2232(2) -0.04233(12) 0.0509(5) Uani 1 1 d . . . H5 H 0.6383 0.1347 -0.0632 0.061 Uiso 1 1 calc R . . C6 C 0.73754(14) 0.24114(18) 0.00869(11) 0.0452(4) Uani 1 1 d . . . H6 H 0.7791 0.1675 0.0233 0.054 Uiso 1 1 calc R . . C7 C 0.75741(12) 0.37461(17) 0.03789(10) 0.0374(4) Uani 1 1 d . . . C8 C 0.91455(13) 0.34879(18) 0.12776(11) 0.0446(4) Uani 1 1 d . . . H8A H 0.8945 0.2549 0.1394 0.054 Uiso 1 1 calc R . . H8B H 0.9399 0.3909 0.1812 0.054 Uiso 1 1 calc R . . C9 C 0.99126(14) 0.3425(2) 0.07138(14) 0.0592(5) Uani 1 1 d . . . H9A H 0.9656 0.3059 0.0172 0.089 Uiso 1 1 calc R . . H9B H 1.0419 0.2833 0.0963 0.089 Uiso 1 1 calc R . . H9C H 1.0159 0.4344 0.0642 0.089 Uiso 1 1 calc R . . C10 C 0.87826(13) 0.66177(17) 0.15046(12) 0.0431(4) Uani 1 1 d . . . H10A H 0.9215 0.6089 0.1905 0.052 Uiso 1 1 calc R . . H10B H 0.9162 0.7140 0.1143 0.052 Uiso 1 1 calc R . . C11 C 0.79193(12) 0.87996(17) 0.16924(10) 0.0365(4) Uani 1 1 d . . . H11 H 0.8035 0.9214 0.1185 0.044 Uiso 1 1 calc R . . C12 C 0.79077(14) 0.73184(18) 0.27199(11) 0.0451(4) Uani 1 1 d . . . H12 H 0.8019 0.6519 0.3047 0.054 Uiso 1 1 calc R . . C13 C 0.74050(14) 0.84237(18) 0.29061(11) 0.0458(4) Uani 1 1 d . . . H13 H 0.7100 0.8546 0.3389 0.055 Uiso 1 1 calc R . . C14 C 0.70312(11) 1.07337(16) 0.22151(10) 0.0356(4) Uani 1 1 d . . . C15 C 0.75531(12) 1.17560(17) 0.26694(10) 0.0374(4) Uani 1 1 d . . . C16 C 0.71762(12) 1.30760(18) 0.26298(11) 0.0410(4) Uani 1 1 d . . . H16 H 0.7518 1.3791 0.2921 0.049 Uiso 1 1 calc R . . C17 C 0.63069(12) 1.33721(18) 0.21712(11) 0.0413(4) Uani 1 1 d . . . C18 C 0.58189(13) 1.23168(19) 0.17343(11) 0.0448(4) Uani 1 1 d . . . H18 H 0.5231 1.2511 0.1424 0.054 Uiso 1 1 calc R . . C19 C 0.61669(12) 1.09763(18) 0.17363(10) 0.0399(4) Uani 1 1 d . . . C20 C 0.84807(13) 1.14506(19) 0.31933(12) 0.0471(4) Uani 1 1 d . . . H20A H 0.8798 1.2309 0.3360 0.071 Uiso 1 1 calc R . . H20B H 0.8878 1.0908 0.2868 0.071 Uiso 1 1 calc R . . H20C H 0.8363 1.0938 0.3689 0.071 Uiso 1 1 calc R . . C21 C 0.59210(15) 1.48222(19) 0.21494(14) 0.0548(5) Uani 1 1 d . . . H21A H 0.6152 1.5327 0.1693 0.082 Uiso 1 1 calc R . . H21B H 0.6129 1.5278 0.2677 0.082 Uiso 1 1 calc R . . H21C H 0.5235 1.4793 0.2064 0.082 Uiso 1 1 calc R . . C22 C 0.56378(15) 0.9853(2) 0.12312(14) 0.0542(5) Uani 1 1 d . . . H22A H 0.5974 0.9612 0.0761 0.081 Uiso 1 1 calc R . . H22B H 0.5007 1.0174 0.1025 0.081 Uiso 1 1 calc R . . H22C H 0.5592 0.9049 0.1583 0.081 Uiso 1 1 calc R . . O1W O 0.68898(12) 0.85114(17) -0.04867(10) 0.0647(4) Uani 1 1 d D . . H1W H 0.6954(18) 0.781(2) -0.0161(14) 0.080 Uiso 1 1 d D . . H2W H 0.7465(13) 0.883(3) -0.0379(16) 0.080 Uiso 1 1 d D . . O2W O 0.87669(11) 0.95761(19) -0.00363(10) 0.0656(4) Uani 1 1 d D . . H3W H 0.9004(18) 0.974(3) -0.0494(13) 0.080 Uiso 1 1 d D . . H4W H 0.9235(15) 0.967(3) 0.0345(14) 0.080 Uiso 1 1 d D . . Cl1 Cl 1.01740(4) 0.98717(5) 0.16028(3) 0.05048(15) 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 N1 0.0427(8) 0.0336(7) 0.0497(9) -0.0039(6) 0.0043(6) 0.0037(6) N2 0.0463(8) 0.0298(7) 0.0359(7) -0.0016(6) 0.0049(6) 0.0045(6) N3 0.0430(8) 0.0309(7) 0.0392(7) -0.0043(6) 0.0039(6) -0.0013(6) N4 0.0422(8) 0.0343(7) 0.0337(7) -0.0025(6) 0.0080(6) -0.0023(6) C1 0.0443(9) 0.0306(8) 0.0398(9) -0.0022(7) 0.0091(7) 0.0033(7) C2 0.0441(9) 0.0358(9) 0.0405(9) -0.0019(7) 0.0089(7) 0.0000(7) C3 0.0447(10) 0.0461(10) 0.0555(12) -0.0030(9) 0.0025(9) 0.0029(8) C4 0.0529(11) 0.0559(12) 0.0551(12) -0.0089(9) 0.0010(9) -0.0101(10) C5 0.0636(12) 0.0431(10) 0.0465(10) -0.0097(8) 0.0089(9) -0.0126(9) C6 0.0631(12) 0.0342(9) 0.0394(9) -0.0021(7) 0.0111(8) 0.0013(8) C7 0.0466(9) 0.0346(8) 0.0321(8) -0.0013(7) 0.0090(7) -0.0009(7) C8 0.0601(11) 0.0349(9) 0.0367(9) 0.0018(7) -0.0030(8) 0.0109(8) C9 0.0505(11) 0.0559(12) 0.0704(14) 0.0128(10) 0.0041(10) 0.0134(10) C10 0.0436(10) 0.0339(9) 0.0513(10) -0.0060(8) 0.0041(8) 0.0022(7) C11 0.0418(9) 0.0339(8) 0.0342(8) -0.0025(7) 0.0067(7) -0.0021(7) C12 0.0604(11) 0.0366(9) 0.0379(9) 0.0035(7) 0.0035(8) -0.0037(8) C13 0.0613(12) 0.0419(10) 0.0356(9) 0.0002(7) 0.0117(8) -0.0045(8) C14 0.0397(9) 0.0338(8) 0.0350(8) -0.0020(7) 0.0120(7) 0.0006(7) C15 0.0398(9) 0.0388(9) 0.0345(8) -0.0022(7) 0.0083(7) -0.0005(7) C16 0.0471(10) 0.0370(9) 0.0402(9) -0.0054(7) 0.0105(7) -0.0030(7) C17 0.0462(10) 0.0402(9) 0.0402(9) 0.0022(7) 0.0158(7) 0.0049(8) C18 0.0387(9) 0.0526(11) 0.0434(10) 0.0007(8) 0.0065(7) 0.0054(8) C19 0.0389(9) 0.0453(10) 0.0364(9) -0.0043(7) 0.0078(7) -0.0024(8) C20 0.0476(10) 0.0448(10) 0.0472(10) -0.0050(8) -0.0013(8) -0.0010(8) C21 0.0594(12) 0.0446(10) 0.0626(13) 0.0045(9) 0.0163(10) 0.0124(9) C22 0.0474(11) 0.0595(12) 0.0543(12) -0.0138(9) -0.0002(9) -0.0055(9) O1W 0.0686(10) 0.0586(9) 0.0642(10) 0.0046(7) -0.0031(8) 0.0082(8) O2W 0.0491(9) 0.0949(12) 0.0541(9) 0.0012(9) 0.0116(7) -0.0039(8) Cl1 0.0630(3) 0.0478(3) 0.0399(3) 0.00393(19) 0.0033(2) -0.0025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.312(2) . ? N1 C2 1.389(2) . ? N2 C1 1.369(2) . ? N2 C7 1.383(2) . ? N2 C8 1.464(2) . ? N3 C11 1.323(2) . ? N3 C12 1.373(2) . ? N3 C10 1.470(2) . ? N4 C11 1.324(2) . ? N4 C13 1.380(2) . ? N4 C14 1.455(2) . ? C1 C10 1.495(2) . ? C2 C7 1.392(2) . ? C2 C3 1.393(3) . ? C3 C4 1.379(3) . ? C4 C5 1.394(3) . ? C5 C6 1.368(3) . ? C6 C7 1.395(2) . ? C8 C9 1.500(3) . ? C12 C13 1.343(3) . ? C14 C19 1.390(2) . ? C14 C15 1.392(2) . ? C15 C16 1.388(2) . ? C15 C20 1.507(2) . ? C16 C17 1.392(2) . ? C17 C18 1.381(2) . ? C17 C21 1.510(2) . ? C18 C19 1.392(2) . ? C19 C22 1.506(2) . ? 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 C1 N1 C2 104.82(14) . . ? C1 N2 C7 105.98(13) . . ? C1 N2 C8 129.03(14) . . ? C7 N2 C8 124.95(14) . . ? C11 N3 C12 108.66(14) . . ? C11 N3 C10 125.59(15) . . ? C12 N3 C10 125.69(14) . . ? C11 N4 C13 108.40(14) . . ? C11 N4 C14 125.01(13) . . ? C13 N4 C14 126.39(14) . . ? N1 C1 N2 113.46(15) . . ? N1 C1 C10 123.42(14) . . ? N2 C1 C10 123.12(15) . . ? N1 C2 C7 109.84(15) . . ? N1 C2 C3 130.08(16) . . ? C7 C2 C3 120.07(16) . . ? C4 C3 C2 117.62(18) . . ? C3 C4 C5 121.41(18) . . ? C6 C5 C4 122.01(17) . . ? C5 C6 C7 116.45(18) . . ? N2 C7 C2 105.91(14) . . ? N2 C7 C6 131.65(16) . . ? C2 C7 C6 122.43(16) . . ? N2 C8 C9 112.53(14) . . ? N3 C10 C1 110.16(14) . . ? N3 C11 N4 108.77(14) . . ? C13 C12 N3 107.17(15) . . ? C12 C13 N4 106.99(16) . . ? C19 C14 C15 123.37(15) . . ? C19 C14 N4 119.23(15) . . ? C15 C14 N4 117.40(14) . . ? C16 C15 C14 117.08(16) . . ? C16 C15 C20 120.99(16) . . ? C14 C15 C20 121.92(15) . . ? C15 C16 C17 121.94(16) . . ? C18 C17 C16 118.47(16) . . ? C18 C17 C21 121.36(17) . . ? C16 C17 C21 120.17(17) . . ? C17 C18 C19 122.35(16) . . ? C14 C19 C18 116.77(16) . . ? C14 C19 C22 121.82(16) . . ? C18 C19 C22 121.40(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O2W 0.874(16) 2.002(17) 2.874(2) 175(2) . O1W H1W N1 0.856(16) 2.097(17) 2.943(2) 170(2) . O2W H3W Cl1 0.859(17) 2.276(17) 3.1295(16) 172(2) 3_775 O2W H4W Cl1 0.855(17) 2.292(18) 3.1239(17) 164(2) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.266 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.043 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 760769' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Ag4 Cl4 N8' _chemical_formula_weight 1206.08 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.040(4) _cell_length_b 9.580(3) _cell_length_c 16.361(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.899(7) _cell_angle_gamma 90.00 _cell_volume 2019.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1784 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.52 _exptl_crystal_description 'Thin Plate' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 2.218 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7767 _exptl_absorpt_correction_T_max 0.9570 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10445 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3553 _reflns_number_gt 2784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+28.5309P] 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 3553 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1883 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.38524(9) 0.58013(10) 0.47965(7) 0.0401(4) Uani 1 1 d . . . Ag2 Ag 0.18410(9) 0.59855(12) 0.36454(7) 0.0414(4) Uani 1 1 d . . . Cl1 Cl 0.5060(2) 0.4787(3) 0.37639(17) 0.0201(6) Uani 1 1 d . . . Cl2 Cl 0.1932(3) 0.4471(3) 0.4774(2) 0.0323(8) Uani 1 1 d . . . N1 N 0.3585(8) 0.8139(10) 0.4478(6) 0.022(2) Uani 1 1 d . . . N2 N 0.3714(8) 1.0240(9) 0.3920(6) 0.021(2) Uani 1 1 d . . . N3 N 0.2607(8) 0.8114(10) 0.2487(6) 0.020(2) Uani 1 1 d . . . N4 N 0.1047(8) 0.7504(11) 0.2007(7) 0.033(3) Uani 1 1 d . . . C1 C 0.3655(9) 0.8818(11) 0.3804(7) 0.019(3) Uani 1 1 d . . . C2 C 0.3629(8) 0.9153(12) 0.5106(8) 0.023(3) Uani 1 1 d . . . C3 C 0.3600(10) 0.9003(14) 0.5925(8) 0.032(3) Uani 1 1 d . . . H3 H 0.3529 0.8128 0.6157 0.038 Uiso 1 1 calc R . . C4 C 0.3680(10) 1.0207(14) 0.6409(8) 0.031(3) Uani 1 1 d . . . H4 H 0.3675 1.0137 0.6975 0.037 Uiso 1 1 calc R . . C5 C 0.3770(10) 1.1522(14) 0.6051(8) 0.031(3) Uani 1 1 d . . . H5 H 0.3828 1.2312 0.6384 0.037 Uiso 1 1 calc R . . C6 C 0.3774(9) 1.1663(11) 0.5221(8) 0.020(3) Uani 1 1 d . . . H6 H 0.3828 1.2538 0.4984 0.024 Uiso 1 1 calc R . . C7 C 0.3696(9) 1.0472(11) 0.4743(7) 0.019(3) Uani 1 1 d . . . C8 C 0.3786(10) 1.1322(13) 0.3316(8) 0.031(3) Uani 1 1 d . . . H8A H 0.4027 1.0912 0.2838 0.037 Uiso 1 1 calc R . . H8B H 0.4299 1.2003 0.3552 0.037 Uiso 1 1 calc R . . C9 C 0.2760(12) 1.2068(14) 0.3034(10) 0.043(4) Uani 1 1 d . . . H9A H 0.2250 1.1403 0.2793 0.065 Uiso 1 1 calc R . . H9B H 0.2855 1.2764 0.2630 0.065 Uiso 1 1 calc R . . H9C H 0.2528 1.2506 0.3500 0.065 Uiso 1 1 calc R . . C10 C 0.3626(10) 0.8121(12) 0.2983(7) 0.023(3) Uani 1 1 d . . . H10A H 0.4105 0.8596 0.2678 0.028 Uiso 1 1 calc R . . H10B H 0.3863 0.7166 0.3072 0.028 Uiso 1 1 calc R . . C11 C 0.1841(10) 0.7258(13) 0.2624(8) 0.027(3) Uani 1 1 d . . . C12 C 0.2302(11) 0.8881(14) 0.1777(9) 0.036(3) Uani 1 1 d . . . H12 H 0.2704 0.9527 0.1544 0.043 Uiso 1 1 calc R . . C13 C 0.1318(12) 0.8523(14) 0.1485(8) 0.037(4) Uani 1 1 d . . . H13 H 0.0901 0.8891 0.1023 0.045 Uiso 1 1 calc R . . C14 C 0.0042(11) 0.6769(16) 0.1896(10) 0.043(4) Uani 1 1 d . . . H14A H -0.0484 0.7364 0.1589 0.052 Uiso 1 1 calc R . . H14B H -0.0155 0.6592 0.2434 0.052 Uiso 1 1 calc R . . C15 C 0.0077(10) 0.5381(15) 0.1435(9) 0.034(3) Uani 1 1 d . . . C16 C -0.0816(11) 0.5013(16) 0.0892(9) 0.039(4) Uani 1 1 d . . . H16 H -0.1384 0.5612 0.0800 0.046 Uiso 1 1 calc R . . C17 C -0.0839(11) 0.3749(17) 0.0497(9) 0.044(4) Uani 1 1 d . . . H17 H -0.1431 0.3496 0.0133 0.053 Uiso 1 1 calc R . . C18 C -0.0006(12) 0.2838(15) 0.0625(9) 0.044(4) Uani 1 1 d . . . H18 H -0.0042 0.1975 0.0362 0.053 Uiso 1 1 calc R . . C19 C 0.0873(11) 0.3232(16) 0.1145(9) 0.042(4) Uani 1 1 d . . . H19 H 0.1449 0.2648 0.1226 0.050 Uiso 1 1 calc R . . C20 C 0.0899(12) 0.4529(14) 0.1555(10) 0.043(4) Uani 1 1 d . . . H20 H 0.1492 0.4793 0.1913 0.052 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 Ag1 0.0544(8) 0.0243(5) 0.0417(7) 0.0058(5) 0.0075(6) 0.0082(5) Ag2 0.0467(7) 0.0411(6) 0.0375(7) 0.0070(5) 0.0103(5) -0.0116(5) Cl1 0.0266(15) 0.0177(13) 0.0170(14) 0.0008(11) 0.0067(12) 0.0073(11) Cl2 0.0391(19) 0.0253(15) 0.0348(18) 0.0066(14) 0.0129(16) -0.0017(13) N1 0.023(6) 0.020(5) 0.024(6) 0.001(4) 0.009(5) 0.000(4) N2 0.025(5) 0.015(5) 0.024(6) 0.003(4) 0.004(5) -0.004(4) N3 0.024(6) 0.026(5) 0.010(5) 0.003(4) 0.001(4) -0.003(4) N4 0.027(6) 0.034(6) 0.038(7) -0.008(6) 0.004(5) -0.001(5) C1 0.018(6) 0.017(5) 0.023(7) -0.001(5) 0.009(5) 0.001(5) C2 0.010(6) 0.026(6) 0.032(7) -0.005(6) -0.004(5) 0.004(5) C3 0.027(7) 0.037(7) 0.036(8) -0.006(6) 0.020(6) -0.004(6) C4 0.030(7) 0.046(8) 0.019(7) -0.006(6) 0.010(6) -0.010(6) C5 0.037(8) 0.035(7) 0.024(7) -0.014(6) 0.014(6) 0.000(6) C6 0.020(6) 0.014(5) 0.029(7) -0.001(5) 0.010(5) 0.000(5) C7 0.013(6) 0.023(6) 0.024(7) 0.001(5) 0.005(5) -0.005(5) C8 0.040(8) 0.025(6) 0.030(8) 0.007(6) 0.014(6) -0.005(6) C9 0.057(10) 0.030(7) 0.042(9) 0.006(7) 0.006(8) 0.010(7) C10 0.033(7) 0.022(6) 0.018(6) 0.001(5) 0.015(6) 0.005(5) C11 0.030(7) 0.027(6) 0.026(7) 0.004(6) 0.010(6) -0.004(6) C12 0.038(8) 0.037(8) 0.033(8) -0.010(7) 0.002(7) 0.004(6) C13 0.051(9) 0.032(7) 0.023(7) -0.004(6) -0.015(7) 0.009(7) C14 0.025(8) 0.051(9) 0.051(10) -0.020(8) -0.002(7) -0.002(7) C15 0.019(7) 0.047(8) 0.033(8) -0.002(7) 0.000(6) -0.013(6) C16 0.026(7) 0.056(9) 0.039(8) -0.005(7) 0.020(7) -0.003(7) C17 0.023(8) 0.064(10) 0.044(9) -0.020(8) -0.001(7) -0.023(7) C18 0.051(10) 0.036(8) 0.043(9) -0.008(7) 0.003(8) -0.001(7) C19 0.030(8) 0.050(9) 0.043(9) -0.002(7) -0.001(7) 0.012(7) C20 0.042(9) 0.037(8) 0.049(10) -0.006(7) 0.000(8) 0.018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.314(9) . ? Ag1 Cl1 2.616(3) 3_666 ? Ag1 Cl1 2.664(3) . ? Ag1 Cl2 2.805(4) . ? Ag1 Ag2 2.9882(19) . ? Ag1 Ag1 3.338(2) 3_666 ? Ag2 C11 2.068(12) . ? Ag2 Cl2 2.337(3) . ? Cl1 Ag1 2.616(3) 3_666 ? N1 C1 1.295(15) . ? N1 C2 1.409(15) . ? N2 C7 1.368(15) . ? N2 C1 1.376(14) . ? N2 C8 1.445(15) . ? N3 C11 1.338(15) . ? N3 C12 1.380(17) . ? N3 C10 1.446(15) . ? N4 C11 1.350(17) . ? N4 C13 1.378(18) . ? N4 C14 1.474(17) . ? C1 C10 1.495(16) . ? C2 C3 1.354(18) . ? C2 C7 1.405(16) . ? C3 C4 1.393(18) . ? C4 C5 1.402(19) . ? C5 C6 1.366(17) . ? C6 C7 1.377(16) . ? C8 C9 1.524(19) . ? C12 C13 1.343(19) . ? C14 C15 1.532(19) . ? C15 C20 1.337(19) . ? C15 C16 1.397(19) . ? C16 C17 1.37(2) . ? C17 C18 1.38(2) . ? C18 C19 1.37(2) . ? C19 C20 1.41(2) . ? 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 Ag1 Cl1 117.0(3) . 3_666 ? N1 Ag1 Cl1 107.1(2) . . ? Cl1 Ag1 Cl1 101.59(9) 3_666 . ? N1 Ag1 Cl2 109.5(3) . . ? Cl1 Ag1 Cl2 105.82(10) 3_666 . ? Cl1 Ag1 Cl2 116.10(10) . . ? N1 Ag1 Ag2 73.4(3) . . ? Cl1 Ag1 Ag2 151.77(8) 3_666 . ? Cl1 Ag1 Ag2 99.73(8) . . ? Cl2 Ag1 Ag2 47.45(7) . . ? N1 Ag1 Ag1 126.1(2) . 3_666 ? Cl1 Ag1 Ag1 51.43(7) 3_666 3_666 ? Cl1 Ag1 Ag1 50.16(7) . 3_666 ? Cl2 Ag1 Ag1 124.39(8) . 3_666 ? Ag2 Ag1 Ag1 145.63(6) . 3_666 ? C11 Ag2 Cl2 176.3(4) . . ? C11 Ag2 Ag1 115.7(4) . . ? Cl2 Ag2 Ag1 62.17(9) . . ? Ag1 Cl1 Ag1 78.41(9) 3_666 . ? Ag2 Cl2 Ag1 70.38(9) . . ? C1 N1 C2 106.0(10) . . ? C1 N1 Ag1 130.5(8) . . ? C2 N1 Ag1 121.0(8) . . ? C7 N2 C1 106.7(10) . . ? C7 N2 C8 124.7(10) . . ? C1 N2 C8 128.6(10) . . ? C11 N3 C12 110.0(11) . . ? C11 N3 C10 123.6(10) . . ? C12 N3 C10 126.1(10) . . ? C11 N4 C13 110.3(11) . . ? C11 N4 C14 124.9(12) . . ? C13 N4 C14 124.7(12) . . ? N1 C1 N2 112.9(10) . . ? N1 C1 C10 123.1(10) . . ? N2 C1 C10 124.0(10) . . ? C3 C2 C7 121.8(11) . . ? C3 C2 N1 130.2(11) . . ? C7 C2 N1 108.0(11) . . ? C2 C3 C4 117.6(12) . . ? C3 C4 C5 120.6(12) . . ? C6 C5 C4 121.2(11) . . ? C5 C6 C7 118.1(11) . . ? N2 C7 C6 132.9(10) . . ? N2 C7 C2 106.4(10) . . ? C6 C7 C2 120.6(11) . . ? N2 C8 C9 113.3(11) . . ? N3 C10 C1 113.6(9) . . ? N3 C11 N4 105.8(11) . . ? N3 C11 Ag2 126.2(9) . . ? N4 C11 Ag2 127.7(9) . . ? C13 C12 N3 107.4(13) . . ? C12 C13 N4 106.4(12) . . ? N4 C14 C15 112.4(11) . . ? C20 C15 C16 120.6(14) . . ? C20 C15 C14 122.8(13) . . ? C16 C15 C14 116.5(12) . . ? C17 C16 C15 118.6(14) . . ? C16 C17 C18 121.8(13) . . ? C19 C18 C17 118.8(13) . . ? C18 C19 C20 119.6(14) . . ? C15 C20 C19 120.6(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.126 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.190 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 760770' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H52.50 Ag2 Cl2 N9.50' _chemical_formula_weight 1037.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0160(14) _cell_length_b 19.4130(19) _cell_length_c 19.940(2) _cell_angle_alpha 62.731(2) _cell_angle_beta 88.669(2) _cell_angle_gamma 87.496(2) _cell_volume 4817.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3936 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 22.52 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8766 _exptl_absorpt_correction_T_max 0.9809 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33829 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.1207 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.50 _reflns_number_total 22017 _reflns_number_gt 12075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There are three solvent molecules of acetonitrile and one of them was disordered into two positions with occupancy ratio 60:40. All the solvents were refined isotropically. ; _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^)+(0.0841P)^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 22017 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1392 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1904 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.979 _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 Ag1 Ag 0.24145(3) -0.12401(3) 0.12932(3) 0.04544(15) Uani 1 1 d . . . Ag2 Ag 0.23807(3) 0.01244(3) 0.21419(3) 0.04303(15) Uani 1 1 d . . . Ag3 Ag 0.25163(3) 0.36222(3) 0.61155(3) 0.04681(16) Uani 1 1 d . . . Ag4 Ag 0.24860(3) 0.47159(3) 0.72589(3) 0.03867(14) Uani 1 1 d . . . Cl1 Cl 0.30815(11) -0.26456(10) 0.20063(11) 0.0495(4) Uani 1 1 d . . . Cl2 Cl 0.18687(12) -0.07580(11) -0.00870(10) 0.0527(5) Uani 1 1 d . . . Cl3 Cl 0.18869(13) 0.42295(12) 0.47495(10) 0.0590(5) Uani 1 1 d . . . Cl4 Cl 0.33358(12) 0.22512(11) 0.66381(12) 0.0580(5) Uani 1 1 d . . . N1 N 0.3620(4) -0.0397(3) 0.1219(3) 0.0424(13) Uani 1 1 d . . . N2 N 0.5106(4) -0.0141(3) 0.1373(3) 0.0420(13) Uani 1 1 d . . . N3 N 0.4112(4) -0.1017(3) 0.3031(3) 0.0399(13) Uani 1 1 d . . . N4 N 0.3425(4) -0.0499(3) 0.3654(3) 0.0489(15) Uani 1 1 d . . . N5 N 0.1163(4) -0.1138(3) 0.2036(3) 0.0378(12) Uani 1 1 d . . . N6 N -0.0302(4) -0.0780(3) 0.2256(3) 0.0431(14) Uani 1 1 d . . . N7 N 0.0615(4) 0.0807(3) 0.1082(3) 0.0387(13) Uani 1 1 d . . . N8 N 0.1195(4) 0.1665(3) 0.1318(3) 0.0409(13) Uani 1 1 d . . . N9 N 0.3627(3) 0.4516(3) 0.6086(3) 0.0387(13) Uani 1 1 d . . . N10 N 0.5078(4) 0.4853(3) 0.6220(3) 0.0409(13) Uani 1 1 d . . . N11 N 0.4348(4) 0.3705(3) 0.7902(3) 0.0375(12) Uani 1 1 d . . . N12 N 0.3677(4) 0.3978(3) 0.8722(3) 0.0407(13) Uani 1 1 d . . . N13 N 0.1284(3) 0.3601(3) 0.6922(3) 0.0368(12) Uani 1 1 d . . . N14 N -0.0198(3) 0.3795(3) 0.7274(3) 0.0396(13) Uani 1 1 d . . . N15 N 0.0648(3) 0.5500(3) 0.6270(3) 0.0345(12) Uani 1 1 d . . . N16 N 0.1326(4) 0.6238(3) 0.6635(3) 0.0427(13) Uani 1 1 d . . . C1 C 0.4346(4) -0.0600(4) 0.1675(4) 0.0365(15) Uani 1 1 d . . . C2 C 0.3919(4) 0.0251(4) 0.0563(4) 0.0400(16) Uani 1 1 d . . . C3 C 0.3422(5) 0.0695(4) -0.0106(4) 0.0510(19) Uani 1 1 d . . . H3 H 0.2784 0.0599 -0.0162 0.061 Uiso 1 1 calc R . . C4 C 0.3903(6) 0.1279(4) -0.0678(4) 0.060(2) Uani 1 1 d . . . H4 H 0.3588 0.1593 -0.1135 0.072 Uiso 1 1 calc R . . C5 C 0.4855(6) 0.1412(4) -0.0592(5) 0.064(2) Uani 1 1 d . . . H5 H 0.5173 0.1801 -0.1002 0.077 Uiso 1 1 calc R . . C6 C 0.5345(5) 0.0989(4) 0.0079(5) 0.055(2) Uani 1 1 d . . . H6 H 0.5976 0.1091 0.0144 0.066 Uiso 1 1 calc R . . C7 C 0.4841(5) 0.0402(4) 0.0653(4) 0.0430(17) Uani 1 1 d . . . C8 C 0.6015(5) -0.0171(5) 0.1729(5) 0.059(2) Uani 1 1 d . . . H8A H 0.6532 -0.0055 0.1358 0.071 Uiso 1 1 calc R . . H8B H 0.6139 -0.0695 0.2138 0.071 Uiso 1 1 calc R . . C9 C 0.5998(6) 0.0409(6) 0.2042(6) 0.086(3) Uani 1 1 d . . . H9A H 0.5877 0.0927 0.1637 0.129 Uiso 1 1 calc R . . H9B H 0.6610 0.0386 0.2271 0.129 Uiso 1 1 calc R . . H9C H 0.5497 0.0286 0.2419 0.129 Uiso 1 1 calc R . . C10 C 0.4329(5) -0.1273(4) 0.2447(4) 0.0431(16) Uani 1 1 d . . . H10A H 0.3846 -0.1632 0.2467 0.052 Uiso 1 1 calc R . . H10B H 0.4952 -0.1551 0.2553 0.052 Uiso 1 1 calc R . . C11 C 0.3378(4) -0.0522(4) 0.2984(4) 0.0422(17) Uani 1 1 d . . . C12 C 0.4589(5) -0.1287(4) 0.3694(4) 0.0511(19) Uani 1 1 d . . . H12 H 0.5117 -0.1639 0.3844 0.061 Uiso 1 1 calc R . . C13 C 0.4169(6) -0.0960(4) 0.4098(5) 0.059(2) Uani 1 1 d . . . H13 H 0.4344 -0.1030 0.4578 0.071 Uiso 1 1 calc R . . C14 C 0.2766(5) -0.0017(4) 0.3852(4) 0.0524(19) Uani 1 1 d . . . C15 C 0.3069(6) 0.0675(5) 0.3757(5) 0.069(2) Uani 1 1 d . . . C16 C 0.2442(7) 0.1102(5) 0.3988(6) 0.094(3) Uani 1 1 d . . . H16 H 0.2637 0.1581 0.3936 0.113 Uiso 1 1 calc R . . C17 C 0.1555(7) 0.0859(6) 0.4289(6) 0.085(3) Uani 1 1 d . . . C18 C 0.1289(6) 0.0171(6) 0.4350(5) 0.079(3) Uani 1 1 d . . . H18 H 0.0678 0.0002 0.4544 0.095 Uiso 1 1 calc R . . C19 C 0.1877(6) -0.0309(5) 0.4139(5) 0.063(2) Uani 1 1 d . . . C20 C 0.4011(7) 0.0995(6) 0.3415(7) 0.112(4) Uani 1 1 d . . . H20A H 0.4513 0.0735 0.3782 0.168 Uiso 1 1 calc R . . H20B H 0.4000 0.1547 0.3265 0.168 Uiso 1 1 calc R . . H20C H 0.4130 0.0912 0.2976 0.168 Uiso 1 1 calc R . . C21 C 0.0923(8) 0.1351(6) 0.4548(7) 0.120(5) Uani 1 1 d . . . H21A H 0.0960 0.1138 0.5092 0.181 Uiso 1 1 calc R . . H21B H 0.0267 0.1349 0.4404 0.181 Uiso 1 1 calc R . . H21C H 0.1138 0.1878 0.4313 0.181 Uiso 1 1 calc R . . C22 C 0.1568(7) -0.1065(6) 0.4231(6) 0.092(3) Uani 1 1 d . . . H22A H 0.1333 -0.1006 0.3754 0.138 Uiso 1 1 calc R . . H22B H 0.1062 -0.1248 0.4606 0.138 Uiso 1 1 calc R . . H22C H 0.2104 -0.1436 0.4395 0.138 Uiso 1 1 calc R . . C23 C 0.0457(4) -0.0609(3) 0.1786(4) 0.0362(14) Uani 1 1 d . . . C24 C 0.0839(5) -0.1692(4) 0.2723(4) 0.0406(16) Uani 1 1 d . . . C25 C 0.1278(6) -0.2388(4) 0.3234(4) 0.0529(19) Uani 1 1 d . . . H25 H 0.1898 -0.2538 0.3150 0.063 Uiso 1 1 calc R . . C26 C 0.0756(7) -0.2856(5) 0.3879(5) 0.069(2) Uani 1 1 d . . . H26 H 0.1036 -0.3323 0.4243 0.083 Uiso 1 1 calc R . . C27 C -0.0178(6) -0.2640(5) 0.3991(5) 0.071(3) Uani 1 1 d . . . H27 H -0.0522 -0.2979 0.4417 0.085 Uiso 1 1 calc R . . C28 C -0.0596(5) -0.1954(5) 0.3499(4) 0.062(2) Uani 1 1 d . . . H28 H -0.1216 -0.1808 0.3587 0.074 Uiso 1 1 calc R . . C29 C -0.0085(5) -0.1476(4) 0.2866(4) 0.0434(16) Uani 1 1 d . . . C30 C -0.1178(5) -0.0316(5) 0.2174(5) 0.063(2) Uani 1 1 d . . . H30A H -0.1715 -0.0661 0.2381 0.075 Uiso 1 1 calc R . . H30B H -0.1300 0.0019 0.1637 0.075 Uiso 1 1 calc R . . C31 C -0.1115(6) 0.0178(6) 0.2576(5) 0.082(3) Uani 1 1 d . . . H31A H -0.1018 -0.0154 0.3111 0.123 Uiso 1 1 calc R . . H31B H -0.1703 0.0486 0.2502 0.123 Uiso 1 1 calc R . . H31C H -0.0584 0.0520 0.2373 0.123 Uiso 1 1 calc R . . C32 C 0.0474(4) 0.0092(3) 0.1029(4) 0.0379(15) Uani 1 1 d . . . H32A H 0.0991 0.0020 0.0724 0.046 Uiso 1 1 calc R . . H32B H -0.0129 0.0141 0.0770 0.046 Uiso 1 1 calc R . . C33 C 0.1336(4) 0.0916(4) 0.1452(4) 0.0391(15) Uani 1 1 d . . . C34 C 0.0031(5) 0.1469(4) 0.0732(4) 0.0436(17) Uani 1 1 d . . . H34 H -0.0516 0.1530 0.0443 0.052 Uiso 1 1 calc R . . C35 C 0.0393(5) 0.1992(4) 0.0883(4) 0.0481(18) Uani 1 1 d . . . H35 H 0.0148 0.2501 0.0723 0.058 Uiso 1 1 calc R . . C36 C 0.1788(5) 0.2086(4) 0.1573(5) 0.0532(19) Uani 1 1 d . . . C37 C 0.2716(6) 0.2271(4) 0.1270(5) 0.062(2) Uani 1 1 d . . . C38 C 0.3224(7) 0.2739(5) 0.1482(6) 0.082(3) Uani 1 1 d . . . H38 H 0.3844 0.2870 0.1288 0.098 Uiso 1 1 calc R . . C39 C 0.2873(9) 0.3015(6) 0.1952(7) 0.097(4) Uani 1 1 d . . . C40 C 0.1960(10) 0.2802(6) 0.2252(7) 0.105(4) Uani 1 1 d . . . H40 H 0.1712 0.2980 0.2590 0.126 Uiso 1 1 calc R . . C41 C 0.1409(7) 0.2339(5) 0.2069(5) 0.068(2) Uani 1 1 d . . . C42 C 0.3149(6) 0.1986(5) 0.0759(5) 0.069(2) Uani 1 1 d . . . H42A H 0.3563 0.2373 0.0400 0.104 Uiso 1 1 calc R . . H42B H 0.2649 0.1885 0.0490 0.104 Uiso 1 1 calc R . . H42C H 0.3520 0.1510 0.1051 0.104 Uiso 1 1 calc R . . C43 C 0.3412(10) 0.3534(8) 0.2200(10) 0.175(7) Uani 1 1 d . . . H43A H 0.4088 0.3388 0.2246 0.263 Uiso 1 1 calc R . . H43B H 0.3166 0.3468 0.2684 0.263 Uiso 1 1 calc R . . H43C H 0.3323 0.4072 0.1827 0.263 Uiso 1 1 calc R . . C44 C 0.0455(8) 0.2061(6) 0.2456(6) 0.099(4) Uani 1 1 d . . . H44A H -0.0054 0.2279 0.2088 0.148 Uiso 1 1 calc R . . H44B H 0.0354 0.2228 0.2843 0.148 Uiso 1 1 calc R . . H44C H 0.0454 0.1500 0.2685 0.148 Uiso 1 1 calc R . . C45 C 0.4392(4) 0.4325(3) 0.6504(4) 0.0371(15) Uani 1 1 d . . . C46 C 0.3810(4) 0.5233(4) 0.5479(4) 0.0415(16) Uani 1 1 d . . . C47 C 0.3250(5) 0.5695(4) 0.4857(4) 0.0500(19) Uani 1 1 d . . . H47 H 0.2636 0.5555 0.4797 0.060 Uiso 1 1 calc R . . C48 C 0.3637(6) 0.6363(4) 0.4339(4) 0.060(2) Uani 1 1 d . . . H48 H 0.3269 0.6700 0.3919 0.072 Uiso 1 1 calc R . . C49 C 0.4562(6) 0.6568(4) 0.4407(5) 0.060(2) Uani 1 1 d . . . H49 H 0.4808 0.7024 0.4022 0.072 Uiso 1 1 calc R . . C50 C 0.5119(6) 0.6116(4) 0.5026(5) 0.056(2) Uani 1 1 d . . . H50 H 0.5737 0.6253 0.5080 0.067 Uiso 1 1 calc R . . C51 C 0.4716(5) 0.5449(4) 0.5562(4) 0.0419(16) Uani 1 1 d . . . C52 C 0.6007(5) 0.4849(5) 0.6553(5) 0.057(2) Uani 1 1 d . . . H52A H 0.6483 0.5073 0.6149 0.068 Uiso 1 1 calc R . . H52B H 0.6216 0.4312 0.6886 0.068 Uiso 1 1 calc R . . C53 C 0.5957(7) 0.5305(5) 0.6997(5) 0.082(3) Uani 1 1 d . . . H53A H 0.5692 0.5822 0.6683 0.123 Uiso 1 1 calc R . . H53B H 0.6594 0.5340 0.7157 0.123 Uiso 1 1 calc R . . H53C H 0.5554 0.5045 0.7438 0.123 Uiso 1 1 calc R . . C54 C 0.4503(5) 0.3586(4) 0.7232(4) 0.0406(16) Uani 1 1 d . . . H54A H 0.4047 0.3214 0.7239 0.049 Uiso 1 1 calc R . . H54B H 0.5148 0.3360 0.7252 0.049 Uiso 1 1 calc R . . C55 C 0.3564(4) 0.4066(4) 0.8023(4) 0.0383(15) Uani 1 1 d . . . C56 C 0.4953(5) 0.3407(4) 0.8518(4) 0.0453(17) Uani 1 1 d . . . H56 H 0.5539 0.3135 0.8564 0.054 Uiso 1 1 calc R . . C57 C 0.4539(5) 0.3583(4) 0.9033(4) 0.0480(18) Uani 1 1 d . . . H57 H 0.4780 0.3464 0.9511 0.058 Uiso 1 1 calc R . . C58 C 0.3007(5) 0.4232(4) 0.9139(4) 0.0427(16) Uani 1 1 d . . . C59 C 0.3300(5) 0.4793(4) 0.9330(4) 0.0521(19) Uani 1 1 d . . . C60 C 0.2710(6) 0.4972(5) 0.9795(5) 0.062(2) Uani 1 1 d . . . H60 H 0.2898 0.5350 0.9930 0.075 Uiso 1 1 calc R . . C61 C 0.1841(6) 0.4614(5) 1.0075(5) 0.061(2) Uani 1 1 d . . . C62 C 0.1584(5) 0.4097(5) 0.9820(4) 0.0540(19) Uani 1 1 d . . . H62 H 0.0986 0.3870 0.9971 0.065 Uiso 1 1 calc R . . C63 C 0.2141(5) 0.3890(4) 0.9360(4) 0.0446(17) Uani 1 1 d . . . C64 C 0.4214(6) 0.5219(5) 0.9038(5) 0.069(2) Uani 1 1 d . . . H64A H 0.4253 0.5616 0.9202 0.104 Uiso 1 1 calc R . . H64B H 0.4221 0.5458 0.8491 0.104 Uiso 1 1 calc R . . H64C H 0.4756 0.4855 0.9233 0.104 Uiso 1 1 calc R . . C65 C 0.1225(7) 0.4803(6) 1.0594(6) 0.096(3) Uani 1 1 d . . . H65A H 0.0762 0.4404 1.0836 0.144 Uiso 1 1 calc R . . H65B H 0.0893 0.5300 1.0308 0.144 Uiso 1 1 calc R . . H65C H 0.1619 0.4829 1.0975 0.144 Uiso 1 1 calc R . . C66 C 0.1803(5) 0.3309(5) 0.9123(5) 0.062(2) Uani 1 1 d . . . H66A H 0.1485 0.3579 0.8639 0.094 Uiso 1 1 calc R . . H66B H 0.1361 0.2968 0.9497 0.094 Uiso 1 1 calc R . . H66C H 0.2347 0.3004 0.9080 0.094 Uiso 1 1 calc R . . C67 C 0.0520(4) 0.4090(4) 0.6758(4) 0.0355(14) Uani 1 1 d . . . C68 C 0.1048(4) 0.2957(4) 0.7580(4) 0.0369(15) Uani 1 1 d . . . C69 C 0.1563(5) 0.2267(4) 0.7995(4) 0.0464(17) Uani 1 1 d . . . H69 H 0.2183 0.2185 0.7849 0.056 Uiso 1 1 calc R . . C70 C 0.1136(5) 0.1702(4) 0.8634(4) 0.0522(19) Uani 1 1 d . . . H70 H 0.1470 0.1231 0.8928 0.063 Uiso 1 1 calc R . . C71 C 0.0223(5) 0.1826(4) 0.8839(4) 0.0499(18) Uani 1 1 d . . . H71 H -0.0048 0.1433 0.9275 0.060 Uiso 1 1 calc R . . C72 C -0.0311(5) 0.2504(4) 0.8429(4) 0.0505(18) Uani 1 1 d . . . H72 H -0.0937 0.2575 0.8572 0.061 Uiso 1 1 calc R . . C73 C 0.0123(5) 0.3074(4) 0.7798(4) 0.0386(15) Uani 1 1 d . . . C74 C -0.1116(5) 0.4171(5) 0.7275(4) 0.057(2) Uani 1 1 d . . . H74A H -0.1615 0.3788 0.7439 0.069 Uiso 1 1 calc R . . H74B H -0.1268 0.4570 0.6762 0.069 Uiso 1 1 calc R . . C75 C -0.1091(6) 0.4545(5) 0.7813(5) 0.078(3) Uani 1 1 d . . . H75A H -0.0946 0.4148 0.8320 0.118 Uiso 1 1 calc R . . H75B H -0.1708 0.4793 0.7810 0.118 Uiso 1 1 calc R . . H75C H -0.0604 0.4930 0.7644 0.118 Uiso 1 1 calc R . . C76 C 0.0495(4) 0.4863(4) 0.6078(4) 0.0381(15) Uani 1 1 d . . . H76A H 0.0991 0.4866 0.5722 0.046 Uiso 1 1 calc R . . H76B H -0.0125 0.4949 0.5830 0.046 Uiso 1 1 calc R . . C77 C 0.1421(4) 0.5536(3) 0.6654(4) 0.0382(15) Uani 1 1 d . . . C78 C 0.0079(5) 0.6180(4) 0.6011(4) 0.0527(19) Uani 1 1 d . . . H78 H -0.0486 0.6296 0.5728 0.063 Uiso 1 1 calc R . . C79 C 0.0504(5) 0.6634(4) 0.6249(4) 0.0521(19) Uani 1 1 d . . . H79 H 0.0286 0.7131 0.6169 0.062 Uiso 1 1 calc R . . C80 C 0.1978(5) 0.6543(4) 0.6961(4) 0.0484(18) Uani 1 1 d . . . C81 C 0.2786(6) 0.6914(4) 0.6545(5) 0.059(2) Uani 1 1 d . . . C82 C 0.3394(6) 0.7215(5) 0.6874(6) 0.078(3) Uani 1 1 d . . . H82 H 0.3946 0.7458 0.6610 0.094 Uiso 1 1 calc R . . C83 C 0.3215(7) 0.7169(5) 0.7575(6) 0.077(3) Uani 1 1 d . . . C84 C 0.2425(7) 0.6800(5) 0.7967(5) 0.073(3) Uani 1 1 d . . . H84 H 0.2303 0.6771 0.8445 0.088 Uiso 1 1 calc R . . C85 C 0.1795(6) 0.6465(4) 0.7683(4) 0.0541(19) Uani 1 1 d . . . C86 C 0.2975(7) 0.6960(5) 0.5786(5) 0.082(3) Uani 1 1 d . . . H86A H 0.3461 0.7335 0.5528 0.122 Uiso 1 1 calc R . . H86B H 0.2392 0.7120 0.5493 0.122 Uiso 1 1 calc R . . H86C H 0.3196 0.6455 0.5844 0.122 Uiso 1 1 calc R . . C87 C 0.3891(9) 0.7533(7) 0.7920(7) 0.127(5) Uani 1 1 d . . . H87A H 0.3935 0.8082 0.7582 0.191 Uiso 1 1 calc R . . H87B H 0.4520 0.7281 0.7989 0.191 Uiso 1 1 calc R . . H87C H 0.3639 0.7462 0.8404 0.191 Uiso 1 1 calc R . . C88 C 0.0961(6) 0.6045(5) 0.8132(5) 0.071(2) Uani 1 1 d . . . H88A H 0.0377 0.6301 0.7865 0.106 Uiso 1 1 calc R . . H88B H 0.0961 0.6046 0.8618 0.106 Uiso 1 1 calc R . . H88C H 0.0999 0.5515 0.8206 0.106 Uiso 1 1 calc R . . N1S N 0.8496(9) 0.3175(8) 1.0167(7) 0.154(5) Uiso 1 1 d D . . C1S C 0.7950(10) 0.2940(9) 0.9958(9) 0.146(5) Uiso 1 1 d D . . C2S C 0.7048(11) 0.2622(11) 0.9884(10) 0.212(8) Uiso 1 1 d D . . H2S1 H 0.6516 0.2897 0.9987 0.318 Uiso 1 1 calc R . . H2S2 H 0.7038 0.2076 1.0241 0.318 Uiso 1 1 calc R . . H2S3 H 0.6994 0.2684 0.9375 0.318 Uiso 1 1 calc R . . N2S N 0.4511(8) 0.2238(7) 0.4350(6) 0.133(4) Uiso 1 1 d D . . C3S C 0.3811(10) 0.2367(12) 0.4548(11) 0.199(8) Uiso 1 1 d D . . C4S C 0.2892(7) 0.2601(7) 0.4844(6) 0.108(4) Uiso 1 1 d D . . H4S1 H 0.3048 0.2934 0.5066 0.162 Uiso 1 1 calc R . . H4S2 H 0.2599 0.2139 0.5224 0.162 Uiso 1 1 calc R . . H4S3 H 0.2450 0.2876 0.4430 0.162 Uiso 1 1 calc R . . N3S N 0.1586(12) 0.8739(11) 0.6270(11) 0.141(6) Uiso 0.602(12) 1 d PD A 1 C5S C 0.2324(14) 0.9038(17) 0.6117(18) 0.141(6) Uiso 0.602(12) 1 d PD A 1 C6S C 0.3389(12) 0.9349(14) 0.5867(13) 0.141(6) Uiso 0.602(12) 1 d PD A 1 H6S1 H 0.3795 0.9150 0.6309 0.212 Uiso 0.602(12) 1 calc PR A 1 H6S2 H 0.3367 0.9911 0.5628 0.212 Uiso 0.602(12) 1 calc PR A 1 H6S3 H 0.3646 0.9172 0.5514 0.212 Uiso 0.602(12) 1 calc PR A 1 N3Y N 0.265(2) 0.9261(18) 0.610(2) 0.142(9) Uiso 0.398(12) 1 d PD A 2 C5Y C 0.288(3) 0.9872(17) 0.596(2) 0.142(9) Uiso 0.398(12) 1 d PD A 2 C6Y C 0.297(2) 1.0667(17) 0.5939(19) 0.142(9) Uiso 0.398(12) 1 d PD A 2 H6Y1 H 0.2385 1.0973 0.5754 0.213 Uiso 0.398(12) 1 calc PR A 2 H6Y2 H 0.3497 1.0934 0.5605 0.213 Uiso 0.398(12) 1 calc PR A 2 H6Y3 H 0.3102 1.0597 0.6443 0.213 Uiso 0.398(12) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0325(3) 0.0443(3) 0.0483(3) -0.0117(3) 0.0021(2) -0.0004(2) Ag2 0.0347(3) 0.0369(3) 0.0497(3) -0.0137(2) -0.0047(2) 0.0068(2) Ag3 0.0337(3) 0.0487(3) 0.0468(3) -0.0124(3) 0.0027(2) -0.0005(2) Ag4 0.0323(3) 0.0364(3) 0.0422(3) -0.0140(2) -0.0047(2) 0.0065(2) Cl1 0.0364(9) 0.0384(9) 0.0639(12) -0.0157(9) 0.0014(8) 0.0053(7) Cl2 0.0397(9) 0.0667(12) 0.0447(10) -0.0189(9) -0.0030(8) -0.0062(8) Cl3 0.0434(10) 0.0749(13) 0.0450(11) -0.0147(10) -0.0042(8) -0.0111(9) Cl4 0.0402(9) 0.0481(10) 0.0791(14) -0.0244(10) 0.0026(9) 0.0103(8) N1 0.031(3) 0.049(3) 0.045(3) -0.020(3) 0.005(2) -0.005(2) N2 0.030(3) 0.042(3) 0.059(4) -0.026(3) 0.001(3) -0.004(2) N3 0.038(3) 0.034(3) 0.042(3) -0.013(3) -0.003(2) 0.004(2) N4 0.049(3) 0.049(4) 0.042(4) -0.015(3) 0.002(3) 0.012(3) N5 0.040(3) 0.028(3) 0.041(3) -0.012(3) 0.005(2) -0.005(2) N6 0.032(3) 0.047(3) 0.048(4) -0.020(3) 0.005(3) -0.002(2) N7 0.034(3) 0.031(3) 0.045(3) -0.013(3) 0.001(2) 0.002(2) N8 0.037(3) 0.031(3) 0.057(4) -0.022(3) -0.010(3) 0.008(2) N9 0.032(3) 0.039(3) 0.040(3) -0.013(3) 0.003(2) -0.003(2) N10 0.036(3) 0.044(3) 0.050(4) -0.028(3) 0.003(3) 0.000(3) N11 0.039(3) 0.037(3) 0.034(3) -0.014(3) -0.004(2) 0.007(2) N12 0.038(3) 0.043(3) 0.036(3) -0.015(3) -0.004(2) 0.003(2) N13 0.036(3) 0.033(3) 0.036(3) -0.012(2) 0.010(2) -0.006(2) N14 0.027(3) 0.035(3) 0.050(3) -0.014(3) 0.006(2) -0.004(2) N15 0.027(3) 0.030(3) 0.038(3) -0.008(2) -0.007(2) 0.001(2) N16 0.039(3) 0.036(3) 0.047(4) -0.014(3) -0.001(3) 0.003(2) C1 0.026(3) 0.035(3) 0.048(4) -0.019(3) -0.003(3) 0.002(3) C2 0.029(3) 0.038(4) 0.049(4) -0.017(3) 0.006(3) -0.003(3) C3 0.041(4) 0.051(4) 0.050(5) -0.015(4) 0.002(3) 0.001(3) C4 0.068(5) 0.043(4) 0.051(5) -0.008(4) 0.003(4) 0.006(4) C5 0.081(6) 0.038(4) 0.065(6) -0.016(4) 0.029(5) -0.008(4) C6 0.047(4) 0.051(5) 0.070(6) -0.030(4) 0.020(4) -0.012(4) C7 0.042(4) 0.032(4) 0.059(5) -0.024(4) 0.009(3) -0.002(3) C8 0.038(4) 0.075(6) 0.070(6) -0.038(5) -0.006(4) -0.005(4) C9 0.062(6) 0.116(8) 0.110(8) -0.076(7) -0.012(5) -0.012(5) C10 0.036(4) 0.038(4) 0.051(4) -0.017(3) -0.004(3) 0.001(3) C11 0.034(3) 0.032(3) 0.047(4) -0.008(3) 0.001(3) 0.005(3) C12 0.049(4) 0.051(4) 0.044(4) -0.014(4) -0.005(3) 0.012(3) C13 0.067(5) 0.049(5) 0.056(5) -0.019(4) -0.011(4) 0.016(4) C14 0.054(5) 0.054(5) 0.048(5) -0.023(4) 0.005(4) 0.016(4) C15 0.053(5) 0.061(5) 0.094(7) -0.040(5) 0.029(5) 0.003(4) C16 0.099(8) 0.044(5) 0.125(9) -0.027(6) 0.037(7) -0.007(5) C17 0.069(6) 0.069(6) 0.115(8) -0.044(6) 0.034(6) 0.008(5) C18 0.054(5) 0.083(7) 0.095(7) -0.037(6) 0.026(5) 0.001(5) C19 0.064(5) 0.066(6) 0.063(5) -0.033(5) 0.016(4) 0.001(4) C20 0.098(8) 0.076(7) 0.173(12) -0.068(8) 0.059(8) -0.021(6) C21 0.108(9) 0.099(8) 0.156(11) -0.063(8) 0.058(8) 0.018(7) C22 0.066(6) 0.110(8) 0.120(9) -0.070(8) 0.034(6) -0.018(6) C23 0.038(3) 0.032(3) 0.039(4) -0.016(3) 0.002(3) -0.007(3) C24 0.042(4) 0.041(4) 0.032(4) -0.011(3) 0.001(3) -0.005(3) C25 0.061(5) 0.040(4) 0.045(4) -0.008(4) 0.004(4) -0.006(3) C26 0.089(7) 0.049(5) 0.050(5) -0.006(4) -0.006(5) -0.010(4) C27 0.069(6) 0.084(7) 0.044(5) -0.014(5) 0.021(4) -0.042(5) C28 0.041(4) 0.086(6) 0.043(5) -0.016(5) 0.013(4) -0.022(4) C29 0.037(4) 0.045(4) 0.046(4) -0.018(4) 0.004(3) -0.012(3) C30 0.035(4) 0.080(6) 0.065(5) -0.028(5) 0.005(4) 0.015(4) C31 0.067(6) 0.098(7) 0.086(7) -0.048(6) 0.009(5) 0.021(5) C32 0.036(3) 0.034(3) 0.040(4) -0.013(3) -0.002(3) 0.000(3) C33 0.035(3) 0.033(3) 0.045(4) -0.014(3) 0.003(3) 0.002(3) C34 0.041(4) 0.036(4) 0.044(4) -0.010(3) -0.005(3) 0.009(3) C35 0.046(4) 0.037(4) 0.051(5) -0.011(3) -0.016(3) 0.013(3) C36 0.057(5) 0.035(4) 0.069(5) -0.025(4) -0.013(4) 0.009(3) C37 0.062(5) 0.038(4) 0.074(6) -0.015(4) -0.013(4) -0.001(4) C38 0.072(6) 0.059(6) 0.122(9) -0.047(6) -0.012(6) -0.010(5) C39 0.111(9) 0.066(7) 0.125(10) -0.052(7) -0.036(8) 0.000(6) C40 0.163(12) 0.059(6) 0.126(10) -0.072(7) -0.011(9) 0.008(7) C41 0.078(6) 0.058(5) 0.075(6) -0.036(5) -0.009(5) 0.011(5) C42 0.056(5) 0.058(5) 0.083(6) -0.023(5) 0.005(5) -0.009(4) C43 0.163(14) 0.140(13) 0.28(2) -0.144(15) -0.071(14) -0.018(10) C44 0.114(9) 0.083(7) 0.120(9) -0.067(7) 0.009(7) 0.013(6) C45 0.037(4) 0.032(3) 0.046(4) -0.021(3) 0.005(3) 0.003(3) C46 0.036(4) 0.037(4) 0.051(4) -0.020(3) 0.004(3) 0.001(3) C47 0.044(4) 0.044(4) 0.052(5) -0.014(4) 0.002(3) 0.009(3) C48 0.080(6) 0.044(4) 0.044(5) -0.012(4) 0.002(4) 0.012(4) C49 0.080(6) 0.036(4) 0.058(5) -0.018(4) 0.033(5) -0.016(4) C50 0.059(5) 0.057(5) 0.060(5) -0.034(4) 0.015(4) -0.014(4) C51 0.041(4) 0.041(4) 0.050(4) -0.026(4) 0.015(3) -0.009(3) C52 0.035(4) 0.072(5) 0.066(5) -0.034(5) -0.002(4) -0.013(4) C53 0.090(7) 0.076(6) 0.092(7) -0.046(6) -0.018(6) -0.017(5) C54 0.036(3) 0.040(4) 0.048(4) -0.023(3) 0.000(3) 0.003(3) C55 0.036(3) 0.035(4) 0.041(4) -0.015(3) -0.006(3) 0.006(3) C56 0.032(3) 0.046(4) 0.050(4) -0.015(4) -0.005(3) 0.004(3) C57 0.043(4) 0.053(4) 0.046(4) -0.021(4) -0.013(3) 0.012(3) C58 0.050(4) 0.046(4) 0.033(4) -0.019(3) -0.006(3) 0.002(3) C59 0.060(5) 0.050(4) 0.050(5) -0.026(4) -0.001(4) -0.001(4) C60 0.076(6) 0.051(5) 0.067(6) -0.033(4) 0.002(5) -0.007(4) C61 0.070(6) 0.054(5) 0.053(5) -0.021(4) 0.007(4) 0.004(4) C62 0.045(4) 0.062(5) 0.047(5) -0.018(4) 0.005(3) -0.002(4) C63 0.046(4) 0.046(4) 0.035(4) -0.013(3) -0.002(3) 0.000(3) C64 0.060(5) 0.072(6) 0.087(7) -0.044(5) 0.005(5) -0.012(4) C65 0.109(8) 0.098(8) 0.087(7) -0.050(6) 0.043(6) 0.000(6) C66 0.053(5) 0.064(5) 0.064(5) -0.022(4) 0.010(4) -0.019(4) C67 0.032(3) 0.035(3) 0.044(4) -0.022(3) -0.001(3) -0.004(3) C68 0.036(3) 0.034(3) 0.039(4) -0.016(3) 0.002(3) -0.005(3) C69 0.042(4) 0.043(4) 0.050(4) -0.017(4) 0.002(3) -0.002(3) C70 0.061(5) 0.041(4) 0.049(5) -0.014(4) -0.001(4) -0.008(3) C71 0.063(5) 0.044(4) 0.035(4) -0.010(3) 0.004(3) -0.021(4) C72 0.036(4) 0.052(4) 0.061(5) -0.023(4) 0.009(3) -0.015(3) C73 0.044(4) 0.035(4) 0.037(4) -0.015(3) 0.006(3) -0.012(3) C74 0.035(4) 0.064(5) 0.055(5) -0.013(4) 0.009(3) 0.003(3) C75 0.066(6) 0.089(7) 0.087(7) -0.049(6) 0.013(5) 0.025(5) C76 0.031(3) 0.043(4) 0.038(4) -0.016(3) 0.002(3) -0.004(3) C77 0.038(3) 0.030(3) 0.040(4) -0.010(3) 0.002(3) 0.000(3) C78 0.045(4) 0.050(4) 0.050(5) -0.012(4) -0.011(3) 0.011(3) C79 0.051(4) 0.033(4) 0.061(5) -0.013(4) -0.011(4) 0.015(3) C80 0.053(4) 0.034(4) 0.059(5) -0.022(4) -0.003(4) 0.003(3) C81 0.056(5) 0.042(4) 0.084(6) -0.032(4) 0.023(4) -0.012(4) C82 0.069(6) 0.067(6) 0.114(8) -0.054(6) 0.030(6) -0.030(5) C83 0.076(6) 0.072(6) 0.099(8) -0.051(6) 0.002(6) -0.015(5) C84 0.099(7) 0.067(6) 0.063(6) -0.038(5) -0.003(5) -0.002(5) C85 0.061(5) 0.045(4) 0.056(5) -0.023(4) -0.006(4) -0.001(4) C86 0.090(7) 0.071(6) 0.089(7) -0.041(6) 0.040(6) -0.028(5) C87 0.125(10) 0.123(10) 0.153(12) -0.076(10) -0.018(9) -0.043(8) C88 0.071(6) 0.066(6) 0.072(6) -0.028(5) 0.004(5) -0.009(4) _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 Ag1 N5 2.330(5) . ? Ag1 N1 2.359(5) . ? Ag1 Cl1 2.5737(17) . ? Ag1 Cl2 2.5904(19) . ? Ag2 C33 2.088(6) . ? Ag2 C11 2.092(6) . ? Ag3 N13 2.321(5) . ? Ag3 N9 2.362(5) . ? Ag3 Cl3 2.5817(19) . ? Ag3 Cl4 2.5953(18) . ? Ag4 C77 2.082(6) . ? Ag4 C55 2.092(6) . ? N1 C1 1.303(8) . ? N1 C2 1.407(8) . ? N2 C1 1.361(8) . ? N2 C7 1.384(9) . ? N2 C8 1.459(8) . ? N3 C11 1.351(7) . ? N3 C12 1.359(8) . ? N3 C10 1.480(8) . ? N4 C11 1.361(9) . ? N4 C13 1.381(9) . ? N4 C14 1.459(8) . ? N5 C23 1.323(8) . ? N5 C24 1.379(8) . ? N6 C23 1.349(8) . ? N6 C29 1.369(8) . ? N6 C30 1.457(8) . ? N7 C33 1.344(8) . ? N7 C34 1.386(7) . ? N7 C32 1.461(8) . ? N8 C33 1.358(8) . ? N8 C35 1.378(8) . ? N8 C36 1.442(9) . ? N9 C45 1.305(8) . ? N9 C46 1.393(8) . ? N10 C45 1.350(8) . ? N10 C51 1.380(8) . ? N10 C52 1.474(8) . ? N11 C55 1.352(7) . ? N11 C56 1.383(8) . ? N11 C54 1.467(8) . ? N12 C55 1.337(8) . ? N12 C57 1.396(8) . ? N12 C58 1.455(8) . ? N13 C67 1.340(7) . ? N13 C68 1.381(8) . ? N14 C67 1.365(8) . ? N14 C73 1.372(8) . ? N14 C74 1.451(8) . ? N15 C77 1.363(8) . ? N15 C78 1.397(8) . ? N15 C76 1.477(8) . ? N16 C77 1.347(8) . ? N16 C79 1.389(8) . ? N16 C80 1.427(9) . ? C1 C10 1.496(9) . ? C2 C7 1.371(9) . ? C2 C3 1.395(9) . ? C3 C4 1.375(10) . ? C4 C5 1.400(11) . ? C5 C6 1.387(11) . ? C6 C7 1.393(10) . ? C8 C9 1.518(11) . ? C12 C13 1.347(10) . ? C14 C15 1.355(11) . ? C14 C19 1.389(11) . ? C15 C16 1.393(11) . ? C15 C20 1.495(12) . ? C16 C17 1.374(12) . ? C17 C18 1.353(12) . ? C17 C21 1.522(11) . ? C18 C19 1.415(11) . ? C19 C22 1.476(12) . ? C23 C32 1.501(8) . ? C24 C25 1.392(9) . ? C24 C29 1.407(9) . ? C25 C26 1.399(10) . ? C26 C27 1.401(12) . ? C27 C28 1.357(11) . ? C28 C29 1.382(9) . ? C30 C31 1.513(11) . ? C34 C35 1.307(9) . ? C36 C41 1.379(11) . ? C36 C37 1.411(11) . ? C37 C38 1.391(11) . ? C37 C42 1.473(11) . ? C38 C39 1.350(14) . ? C39 C40 1.396(15) . ? C39 C43 1.540(14) . ? C40 C41 1.383(13) . ? C41 C44 1.520(13) . ? C45 C54 1.508(9) . ? C46 C47 1.387(9) . ? C46 C51 1.391(9) . ? C47 C48 1.360(10) . ? C48 C49 1.401(11) . ? C49 C50 1.377(11) . ? C50 C51 1.381(10) . ? C52 C53 1.511(11) . ? C56 C57 1.335(9) . ? C58 C63 1.373(9) . ? C58 C59 1.388(10) . ? C59 C60 1.378(10) . ? C59 C64 1.510(10) . ? C60 C61 1.402(11) . ? C61 C62 1.381(11) . ? C61 C65 1.492(11) . ? C62 C63 1.374(9) . ? C63 C66 1.505(10) . ? C67 C76 1.491(9) . ? C68 C69 1.389(9) . ? C68 C73 1.400(8) . ? C69 C70 1.387(10) . ? C70 C71 1.378(10) . ? C71 C72 1.385(10) . ? C72 C73 1.386(9) . ? C74 C75 1.549(11) . ? C78 C79 1.342(10) . ? C80 C85 1.397(10) . ? C80 C81 1.403(10) . ? C81 C82 1.384(12) . ? C81 C86 1.492(11) . ? C82 C83 1.378(12) . ? C83 C84 1.367(12) . ? C83 C87 1.549(13) . ? C84 C85 1.391(11) . ? C85 C88 1.482(11) . ? N1S C1S 1.089(9) . ? C1S C2S 1.471(9) . ? N2S C3S 1.110(9) . ? C3S C4S 1.541(9) . ? N3S C5S 1.173(8) . ? C5S C6S 1.616(8) . ? N3Y C5Y 1.146(9) . ? C5Y C6Y 1.534(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 N5 Ag1 N1 109.21(18) . . ? N5 Ag1 Cl1 105.52(13) . . ? N1 Ag1 Cl1 108.53(13) . . ? N5 Ag1 Cl2 110.93(14) . . ? N1 Ag1 Cl2 104.90(14) . . ? Cl1 Ag1 Cl2 117.59(7) . . ? C33 Ag2 C11 166.2(3) . . ? N13 Ag3 N9 107.49(18) . . ? N13 Ag3 Cl3 109.46(14) . . ? N9 Ag3 Cl3 103.76(14) . . ? N13 Ag3 Cl4 109.18(13) . . ? N9 Ag3 Cl4 109.53(13) . . ? Cl3 Ag3 Cl4 116.96(7) . . ? C77 Ag4 C55 164.8(3) . . ? C1 N1 C2 104.9(5) . . ? C1 N1 Ag1 124.1(4) . . ? C2 N1 Ag1 126.3(4) . . ? C1 N2 C7 106.5(5) . . ? C1 N2 C8 128.3(6) . . ? C7 N2 C8 125.1(6) . . ? C11 N3 C12 112.1(6) . . ? C11 N3 C10 123.7(6) . . ? C12 N3 C10 124.1(5) . . ? C11 N4 C13 112.4(6) . . ? C11 N4 C14 122.3(6) . . ? C13 N4 C14 125.3(6) . . ? C23 N5 C24 104.2(5) . . ? C23 N5 Ag1 124.7(4) . . ? C24 N5 Ag1 128.8(4) . . ? C23 N6 C29 106.8(5) . . ? C23 N6 C30 128.3(6) . . ? C29 N6 C30 124.8(6) . . ? C33 N7 C34 111.5(5) . . ? C33 N7 C32 124.8(5) . . ? C34 N7 C32 123.7(6) . . ? C33 N8 C35 110.5(5) . . ? C33 N8 C36 126.5(5) . . ? C35 N8 C36 123.0(5) . . ? C45 N9 C46 105.2(5) . . ? C45 N9 Ag3 124.2(4) . . ? C46 N9 Ag3 126.4(4) . . ? C45 N10 C51 106.4(5) . . ? C45 N10 C52 128.5(6) . . ? C51 N10 C52 125.0(6) . . ? C55 N11 C56 111.4(5) . . ? C55 N11 C54 124.5(5) . . ? C56 N11 C54 123.9(5) . . ? C55 N12 C57 111.1(5) . . ? C55 N12 C58 126.6(5) . . ? C57 N12 C58 122.2(5) . . ? C67 N13 C68 105.3(5) . . ? C67 N13 Ag3 127.5(4) . . ? C68 N13 Ag3 124.6(4) . . ? C67 N14 C73 106.3(5) . . ? C67 N14 C74 127.0(5) . . ? C73 N14 C74 126.6(5) . . ? C77 N15 C78 111.2(5) . . ? C77 N15 C76 124.1(5) . . ? C78 N15 C76 124.3(5) . . ? C77 N16 C79 110.9(6) . . ? C77 N16 C80 125.1(5) . . ? C79 N16 C80 124.0(6) . . ? N1 C1 N2 113.1(6) . . ? N1 C1 C10 122.5(6) . . ? N2 C1 C10 124.4(6) . . ? C7 C2 C3 121.4(7) . . ? C7 C2 N1 109.5(6) . . ? C3 C2 N1 129.1(6) . . ? C4 C3 C2 117.1(7) . . ? C3 C4 C5 121.1(7) . . ? C6 C5 C4 122.1(7) . . ? C5 C6 C7 115.8(7) . . ? C2 C7 N2 106.0(6) . . ? C2 C7 C6 122.4(7) . . ? N2 C7 C6 131.5(7) . . ? N2 C8 C9 110.6(6) . . ? N3 C10 C1 111.5(5) . . ? N3 C11 N4 102.8(5) . . ? N3 C11 Ag2 133.3(5) . . ? N4 C11 Ag2 123.9(4) . . ? C13 C12 N3 107.7(6) . . ? C12 C13 N4 105.0(7) . . ? C15 C14 C19 124.6(7) . . ? C15 C14 N4 117.8(7) . . ? C19 C14 N4 117.6(7) . . ? C14 C15 C16 116.4(8) . . ? C14 C15 C20 123.9(7) . . ? C16 C15 C20 119.8(8) . . ? C17 C16 C15 123.4(9) . . ? C18 C17 C16 117.0(8) . . ? C18 C17 C21 122.8(9) . . ? C16 C17 C21 120.2(10) . . ? C17 C18 C19 123.9(8) . . ? C14 C19 C18 114.7(8) . . ? C14 C19 C22 123.2(7) . . ? C18 C19 C22 122.1(8) . . ? N5 C23 N6 113.8(6) . . ? N5 C23 C32 123.0(6) . . ? N6 C23 C32 123.1(5) . . ? N5 C24 C25 129.7(6) . . ? N5 C24 C29 109.8(6) . . ? C25 C24 C29 120.4(6) . . ? C24 C25 C26 117.1(7) . . ? C25 C26 C27 121.1(8) . . ? C28 C27 C26 121.6(7) . . ? C27 C28 C29 118.1(7) . . ? N6 C29 C28 133.0(7) . . ? N6 C29 C24 105.4(5) . . ? C28 C29 C24 121.6(7) . . ? N6 C30 C31 111.6(7) . . ? N7 C32 C23 112.7(5) . . ? N7 C33 N8 103.6(5) . . ? N7 C33 Ag2 129.5(5) . . ? N8 C33 Ag2 126.7(5) . . ? C35 C34 N7 106.4(6) . . ? C34 C35 N8 108.0(6) . . ? C41 C36 C37 121.9(8) . . ? C41 C36 N8 118.9(7) . . ? C37 C36 N8 119.1(7) . . ? C38 C37 C36 116.7(9) . . ? C38 C37 C42 120.4(8) . . ? C36 C37 C42 122.9(8) . . ? C39 C38 C37 123.4(10) . . ? C38 C39 C40 118.0(10) . . ? C38 C39 C43 125.0(13) . . ? C40 C39 C43 117.0(12) . . ? C41 C40 C39 122.1(10) . . ? C36 C41 C40 117.9(9) . . ? C36 C41 C44 121.1(8) . . ? C40 C41 C44 120.8(9) . . ? N9 C45 N10 113.5(6) . . ? N9 C45 C54 123.4(6) . . ? N10 C45 C54 123.1(6) . . ? C47 C46 C51 121.2(7) . . ? C47 C46 N9 129.9(6) . . ? C51 C46 N9 108.9(6) . . ? C48 C47 C46 116.4(7) . . ? C47 C48 C49 122.6(7) . . ? C50 C49 C48 121.3(7) . . ? C49 C50 C51 116.0(7) . . ? N10 C51 C50 131.5(7) . . ? N10 C51 C46 105.9(6) . . ? C50 C51 C46 122.4(7) . . ? N10 C52 C53 112.0(6) . . ? N11 C54 C45 113.0(5) . . ? N12 C55 N11 104.4(5) . . ? N12 C55 Ag4 127.1(4) . . ? N11 C55 Ag4 128.3(5) . . ? C57 C56 N11 106.4(5) . . ? C56 C57 N12 106.6(6) . . ? C63 C58 C59 122.6(7) . . ? C63 C58 N12 119.8(6) . . ? C59 C58 N12 117.5(6) . . ? C60 C59 C58 117.5(7) . . ? C60 C59 C64 119.6(7) . . ? C58 C59 C64 122.9(7) . . ? C59 C60 C61 122.9(8) . . ? C62 C61 C60 115.4(7) . . ? C62 C61 C65 122.7(8) . . ? C60 C61 C65 121.9(8) . . ? C63 C62 C61 124.5(7) . . ? C58 C63 C62 116.9(7) . . ? C58 C63 C66 122.6(6) . . ? C62 C63 C66 120.5(7) . . ? N13 C67 N14 112.4(5) . . ? N13 C67 C76 121.8(6) . . ? N14 C67 C76 125.7(5) . . ? N13 C68 C69 130.2(6) . . ? N13 C68 C73 109.0(5) . . ? C69 C68 C73 120.8(6) . . ? C70 C69 C68 118.0(7) . . ? C71 C70 C69 120.4(7) . . ? C70 C71 C72 122.7(7) . . ? C71 C72 C73 116.8(7) . . ? N14 C73 C72 131.8(6) . . ? N14 C73 C68 106.9(5) . . ? C72 C73 C68 121.3(6) . . ? N14 C74 C75 110.1(6) . . ? N15 C76 C67 112.2(5) . . ? N16 C77 N15 104.5(5) . . ? N16 C77 Ag4 123.3(5) . . ? N15 C77 Ag4 131.9(4) . . ? C79 C78 N15 105.8(6) . . ? C78 C79 N16 107.7(6) . . ? C85 C80 C81 121.8(7) . . ? C85 C80 N16 119.2(7) . . ? C81 C80 N16 119.0(7) . . ? C82 C81 C80 117.4(8) . . ? C82 C81 C86 122.4(8) . . ? C80 C81 C86 120.2(8) . . ? C83 C82 C81 122.1(8) . . ? C84 C83 C82 119.1(9) . . ? C84 C83 C87 119.9(10) . . ? C82 C83 C87 121.1(10) . . ? C83 C84 C85 122.2(9) . . ? C84 C85 C80 117.4(8) . . ? C84 C85 C88 121.0(8) . . ? C80 C85 C88 121.6(7) . . ? N1S C1S C2S 161.5(19) . . ? N2S C3S C4S 174(2) . . ? N3S C5S C6S 171(3) . . ? N3Y C5Y C6Y 164(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.916 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.122 #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 760771' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 Ag2 Cl4 N8 Ni O' _chemical_formula_weight 1067.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3501(11) _cell_length_b 13.1561(14) _cell_length_c 14.9640(16) _cell_angle_alpha 72.683(2) _cell_angle_beta 82.205(3) _cell_angle_gamma 72.986(3) _cell_volume 2036.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1903 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 21.93 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7253 _exptl_absorpt_correction_T_max 0.8471 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12105 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7180 _reflns_number_gt 5425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+17.3144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7180 _refine_ls_number_parameters 518 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.1880 _refine_ls_wR_factor_gt 0.1731 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 2.168 _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 Ni1 Ni 0.63989(17) 0.77321(15) 0.22675(13) 0.0180(5) Uani 1 1 d . . . N1 N 0.5331(11) 0.6813(10) 0.2902(9) 0.021(3) Uani 1 1 d . . . N2 N 0.3659(11) 0.6452(10) 0.3742(9) 0.023(3) Uani 1 1 d . . . N3 N 0.5363(11) 0.8255(10) 0.3954(9) 0.021(3) Uani 1 1 d . . . N4 N 0.7296(12) 0.8147(11) 0.3892(9) 0.026(3) Uani 1 1 d . . . N5 N 0.6336(11) 0.7391(10) 0.1120(9) 0.020(3) Uani 1 1 d . . . N6 N 0.7125(11) 0.6692(10) -0.0078(9) 0.023(3) Uani 1 1 d . . . N7 N 0.8348(11) 0.8234(10) 0.0988(9) 0.023(3) Uani 1 1 d . . . N8 N 0.7482(11) 0.9640(11) 0.1496(9) 0.024(3) Uani 1 1 d . . . C1 C 0.4371(13) 0.7155(12) 0.3452(10) 0.020(3) Uani 1 1 d . . . C2 C 0.5272(14) 0.5791(12) 0.2855(10) 0.023(3) Uani 1 1 d . . . C3 C 0.6079(15) 0.5017(13) 0.2430(11) 0.028(4) Uani 1 1 d . . . H3 H 0.6785 0.5165 0.2068 0.034 Uiso 1 1 calc R . . C4 C 0.5800(18) 0.4041(14) 0.2561(12) 0.036(4) Uani 1 1 d . . . H4 H 0.6332 0.3503 0.2290 0.043 Uiso 1 1 calc R . . C5 C 0.4746(19) 0.3818(14) 0.3087(13) 0.040(5) Uani 1 1 d . . . H5 H 0.4591 0.3134 0.3162 0.048 Uiso 1 1 calc R . . C6 C 0.3929(17) 0.4569(13) 0.3500(12) 0.032(4) Uani 1 1 d . . . H6 H 0.3208 0.4426 0.3839 0.038 Uiso 1 1 calc R . . C7 C 0.4228(14) 0.5546(12) 0.3388(11) 0.024(3) Uani 1 1 d . . . C8 C 0.2571(15) 0.6534(14) 0.4392(11) 0.030(4) Uani 1 1 d . . . H8A H 0.2012 0.6167 0.4247 0.036 Uiso 1 1 calc R . . H8B H 0.2130 0.7313 0.4318 0.036 Uiso 1 1 calc R . . C9 C 0.2950(18) 0.5996(18) 0.5400(12) 0.044(5) Uani 1 1 d . . . H9A H 0.3380 0.5223 0.5474 0.066 Uiso 1 1 calc R . . H9B H 0.2220 0.6053 0.5823 0.066 Uiso 1 1 calc R . . H9C H 0.3490 0.6369 0.5546 0.066 Uiso 1 1 calc R . . C10 C 0.4180(13) 0.8209(13) 0.3714(11) 0.024(3) Uani 1 1 d . . . H10A H 0.3856 0.8844 0.3188 0.029 Uiso 1 1 calc R . . H10B H 0.3583 0.8232 0.4252 0.029 Uiso 1 1 calc R . . C11 C 0.6419(13) 0.8071(12) 0.3399(11) 0.020(3) Uani 1 1 d . . . C12 C 0.5587(15) 0.8440(14) 0.4758(12) 0.031(4) Uani 1 1 d . . . H12 H 0.5004 0.8591 0.5244 0.038 Uiso 1 1 calc R . . C13 C 0.6794(16) 0.8366(15) 0.4723(11) 0.034(4) Uani 1 1 d . . . H13 H 0.7219 0.8448 0.5183 0.041 Uiso 1 1 calc R . . C14 C 0.8597(14) 0.8077(14) 0.3590(13) 0.031(4) Uani 1 1 d . . . H14A H 0.8998 0.8194 0.4077 0.037 Uiso 1 1 calc R . . H14B H 0.8635 0.8676 0.3020 0.037 Uiso 1 1 calc R . . C15 C 0.9312(15) 0.7003(15) 0.3397(11) 0.029(4) Uani 1 1 d . . . C16 C 0.9118(17) 0.6008(17) 0.3905(15) 0.044(5) Uani 1 1 d . . . H16 H 0.8463 0.5987 0.4362 0.053 Uiso 1 1 calc R . . C17 C 0.9883(18) 0.5024(17) 0.3750(17) 0.052(6) Uani 1 1 d . . . H17 H 0.9743 0.4344 0.4106 0.062 Uiso 1 1 calc R . . C18 C 1.0823(17) 0.5044(18) 0.3091(17) 0.051(6) Uani 1 1 d . . . H18 H 1.1332 0.4379 0.2988 0.061 Uiso 1 1 calc R . . C19 C 1.1041(16) 0.6037(18) 0.2566(14) 0.044(5) Uani 1 1 d . . . H19 H 1.1694 0.6046 0.2107 0.053 Uiso 1 1 calc R . . C20 C 1.0297(15) 0.7013(17) 0.2718(12) 0.036(4) Uani 1 1 d . . . H20 H 1.0451 0.7688 0.2367 0.043 Uiso 1 1 calc R . . C21 C 0.7341(14) 0.7059(12) 0.0610(11) 0.022(3) Uani 1 1 d . . . C22 C 0.5366(14) 0.7243(12) 0.0725(10) 0.022(3) Uani 1 1 d . . . C23 C 0.4099(14) 0.7495(14) 0.0945(12) 0.028(4) Uani 1 1 d . . . H23 H 0.3745 0.7809 0.1439 0.034 Uiso 1 1 calc R . . C24 C 0.3397(16) 0.7254(14) 0.0390(12) 0.033(4) Uani 1 1 d . . . H24 H 0.2537 0.7423 0.0509 0.040 Uiso 1 1 calc R . . C25 C 0.3899(17) 0.6774(15) -0.0336(12) 0.035(4) Uani 1 1 d . . . H25 H 0.3377 0.6617 -0.0684 0.042 Uiso 1 1 calc R . . C26 C 0.5150(16) 0.6527(14) -0.0552(13) 0.034(4) Uani 1 1 d . . . H26 H 0.5499 0.6195 -0.1037 0.041 Uiso 1 1 calc R . . C27 C 0.5866(14) 0.6788(12) -0.0026(10) 0.023(3) Uani 1 1 d . . . C28 C 0.8020(15) 0.6241(13) -0.0762(11) 0.027(4) Uani 1 1 d . . . H28A H 0.8733 0.6545 -0.0851 0.032 Uiso 1 1 calc R . . H28B H 0.7640 0.6476 -0.1366 0.032 Uiso 1 1 calc R . . C29 C 0.8453(19) 0.5008(14) -0.0463(14) 0.045(5) Uani 1 1 d . . . H29A H 0.8771 0.4768 0.0157 0.068 Uiso 1 1 calc R . . H29B H 0.9102 0.4756 -0.0903 0.068 Uiso 1 1 calc R . . H29C H 0.7769 0.4702 -0.0450 0.068 Uiso 1 1 calc R . . C30 C 0.8565(13) 0.7157(13) 0.0794(12) 0.023(3) Uani 1 1 d . . . H30A H 0.8921 0.6557 0.1333 0.028 Uiso 1 1 calc R . . H30B H 0.9139 0.7115 0.0246 0.028 Uiso 1 1 calc R . . C31 C 0.7457(13) 0.8601(12) 0.1599(10) 0.019(3) Uani 1 1 d . . . C32 C 0.8918(14) 0.9045(14) 0.0507(12) 0.031(4) Uani 1 1 d . . . H32 H 0.9560 0.8990 0.0041 0.037 Uiso 1 1 calc R . . C33 C 0.8387(14) 0.9923(14) 0.0828(13) 0.031(4) Uani 1 1 d . . . H33 H 0.8589 1.0603 0.0639 0.038 Uiso 1 1 calc R . . C34 C 0.6659(15) 1.0416(13) 0.1989(12) 0.028(4) Uani 1 1 d . . . H34A H 0.6835 1.1137 0.1732 0.034 Uiso 1 1 calc R . . H34B H 0.6852 1.0154 0.2652 0.034 Uiso 1 1 calc R . . C35 C 0.5302(15) 1.0570(12) 0.1930(12) 0.027(4) Uani 1 1 d . . . C36 C 0.4851(16) 1.0351(14) 0.1220(13) 0.036(4) Uani 1 1 d . . . H36 H 0.5397 1.0079 0.0762 0.043 Uiso 1 1 calc R . . C37 C 0.3580(17) 1.0535(15) 0.1178(15) 0.043(5) Uani 1 1 d . . . H37 H 0.3278 1.0361 0.0703 0.052 Uiso 1 1 calc R . . C38 C 0.2778(17) 1.0960(16) 0.1818(16) 0.050(6) Uani 1 1 d . . . H38 H 0.1924 1.1094 0.1779 0.060 Uiso 1 1 calc R . . C39 C 0.3219(18) 1.1193(16) 0.2517(16) 0.053(6) Uani 1 1 d . . . H39 H 0.2667 1.1493 0.2959 0.063 Uiso 1 1 calc R . . C40 C 0.4476(18) 1.0988(14) 0.2577(14) 0.041(5) Uani 1 1 d . . . H40 H 0.4771 1.1138 0.3069 0.050 Uiso 1 1 calc R . . O1S O 0.9114(16) 0.4306(13) 0.1941(13) 0.065(4) Uani 1 1 d D . . H1SA H 0.90(2) 0.376(13) 0.172(15) 0.080 Uiso 1 1 d D . . H1SB H 0.94(2) 0.373(12) 0.242(11) 0.080 Uiso 1 1 d D . . Ag1 Ag 0.06408(14) 0.87725(15) 0.70227(11) 0.0508(5) Uani 1 1 d . . . Ag2 Ag 0.1243(2) 0.9838(5) 0.4652(2) 0.110(2) Uani 0.908(12) 1 d PD . 1 Ag3 Ag 0.098(2) 0.923(2) 0.486(2) 0.061(9) Uiso 0.092(12) 1 d PD . 2 Cl1 Cl 0.2631(4) 0.8963(4) 0.5959(3) 0.0378(11) Uani 1 1 d D . . Cl2 Cl -0.0995(5) 1.0685(4) 0.6771(5) 0.0641(18) Uani 1 1 d . . . Cl3 Cl 0.0806(4) 0.7795(4) 0.8755(3) 0.0350(10) Uani 1 1 d . . . Cl4 Cl -0.0388(4) 0.8005(5) 0.5929(4) 0.0496(14) Uani 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 Ni1 0.0161(10) 0.0217(10) 0.0185(10) -0.0069(8) 0.0011(8) -0.0079(8) N1 0.023(7) 0.020(6) 0.019(7) -0.005(5) 0.001(5) -0.005(5) N2 0.018(6) 0.026(7) 0.023(7) 0.000(6) -0.005(5) -0.010(5) N3 0.021(7) 0.024(7) 0.023(7) -0.013(6) 0.003(5) -0.010(5) N4 0.021(7) 0.039(8) 0.025(7) -0.014(6) 0.002(6) -0.014(6) N5 0.018(6) 0.023(7) 0.021(7) -0.008(6) 0.002(5) -0.010(5) N6 0.024(7) 0.024(7) 0.021(7) -0.006(6) 0.001(6) -0.007(6) N7 0.019(7) 0.027(7) 0.022(7) -0.004(6) 0.001(6) -0.007(6) N8 0.019(7) 0.030(7) 0.027(7) -0.011(6) 0.000(6) -0.008(6) C1 0.018(8) 0.024(8) 0.021(8) -0.004(6) -0.005(6) -0.010(6) C2 0.029(9) 0.020(8) 0.019(8) -0.001(6) -0.011(7) -0.008(7) C3 0.031(9) 0.033(9) 0.024(9) -0.012(7) -0.001(7) -0.010(7) C4 0.054(12) 0.025(9) 0.029(10) -0.011(8) -0.013(9) -0.004(8) C5 0.067(13) 0.024(9) 0.037(10) -0.003(8) -0.022(10) -0.021(9) C6 0.040(10) 0.026(9) 0.031(9) 0.002(8) -0.012(8) -0.017(8) C7 0.028(9) 0.020(8) 0.021(8) 0.001(7) -0.011(7) -0.003(7) C8 0.023(9) 0.037(10) 0.029(9) -0.002(8) 0.000(7) -0.014(7) C9 0.040(11) 0.070(14) 0.029(10) -0.011(10) 0.005(9) -0.030(10) C10 0.018(8) 0.027(8) 0.024(8) -0.007(7) 0.002(7) -0.006(7) C11 0.017(8) 0.022(8) 0.024(8) -0.010(7) 0.002(6) -0.008(6) C12 0.031(9) 0.037(10) 0.031(9) -0.013(8) 0.002(8) -0.015(8) C13 0.037(10) 0.052(11) 0.019(9) -0.013(8) -0.001(8) -0.019(9) C14 0.019(8) 0.043(10) 0.037(10) -0.016(8) -0.003(7) -0.013(7) C15 0.024(9) 0.049(11) 0.019(8) -0.011(8) -0.006(7) -0.016(8) C16 0.028(10) 0.054(12) 0.050(12) -0.013(10) 0.000(9) -0.013(9) C17 0.034(11) 0.045(12) 0.077(16) -0.018(11) -0.006(11) -0.009(9) C18 0.029(11) 0.052(13) 0.082(17) -0.042(12) -0.013(11) 0.004(9) C19 0.017(9) 0.078(15) 0.045(12) -0.034(11) -0.001(8) -0.006(9) C20 0.025(9) 0.061(12) 0.028(9) -0.011(9) -0.007(7) -0.018(9) C21 0.024(8) 0.016(7) 0.025(8) -0.003(6) -0.002(7) -0.006(6) C22 0.029(9) 0.022(8) 0.017(8) -0.002(6) -0.005(7) -0.011(7) C23 0.022(8) 0.035(9) 0.027(9) -0.007(7) 0.000(7) -0.010(7) C24 0.025(9) 0.041(10) 0.029(9) 0.002(8) -0.007(7) -0.011(8) C25 0.042(11) 0.040(10) 0.028(9) -0.003(8) -0.014(8) -0.019(9) C26 0.040(11) 0.033(9) 0.034(10) -0.012(8) -0.006(8) -0.012(8) C27 0.031(9) 0.021(8) 0.018(8) 0.004(6) -0.005(7) -0.016(7) C28 0.029(9) 0.028(9) 0.023(8) -0.013(7) 0.004(7) -0.004(7) C29 0.052(12) 0.026(9) 0.048(12) -0.015(9) 0.009(10) 0.003(9) C30 0.015(8) 0.029(8) 0.030(9) -0.017(7) 0.005(7) -0.006(6) C31 0.017(7) 0.019(7) 0.022(8) -0.005(6) -0.002(6) -0.006(6) C32 0.018(8) 0.043(10) 0.039(10) -0.015(8) 0.009(7) -0.020(7) C33 0.023(9) 0.030(9) 0.045(11) -0.010(8) 0.009(8) -0.017(7) C34 0.035(10) 0.024(8) 0.031(9) -0.011(7) 0.002(8) -0.012(7) C35 0.033(9) 0.017(8) 0.029(9) -0.001(7) 0.001(7) -0.009(7) C36 0.033(10) 0.028(9) 0.040(11) -0.007(8) 0.008(8) -0.004(8) C37 0.033(10) 0.035(10) 0.052(12) 0.006(9) -0.010(9) -0.007(8) C38 0.021(10) 0.039(11) 0.060(14) 0.018(10) 0.002(10) 0.002(8) C39 0.033(11) 0.038(11) 0.058(14) -0.002(10) 0.022(10) 0.013(9) C40 0.051(12) 0.031(10) 0.036(11) -0.012(8) 0.017(9) -0.009(9) O1S 0.066(11) 0.071(11) 0.068(11) -0.033(9) 0.001(9) -0.023(9) Ag1 0.0405(9) 0.0670(11) 0.0379(9) -0.0031(8) -0.0040(7) -0.0144(8) Ag2 0.0410(14) 0.182(5) 0.0699(18) 0.006(2) -0.0059(12) -0.0155(18) Cl1 0.027(2) 0.049(3) 0.040(3) -0.018(2) 0.0067(19) -0.0122(19) Cl2 0.044(3) 0.036(3) 0.106(5) 0.006(3) -0.031(3) -0.015(2) Cl3 0.035(2) 0.036(2) 0.034(2) -0.0077(19) -0.0037(19) -0.0095(19) Cl4 0.030(2) 0.070(3) 0.058(3) -0.045(3) -0.015(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C11 1.879(15) . ? Ni1 C31 1.884(14) . ? Ni1 N5 1.914(13) . ? Ni1 N1 1.922(12) . ? N1 C1 1.325(19) . ? N1 C2 1.388(19) . ? N2 C1 1.342(18) . ? N2 C7 1.40(2) . ? N2 C8 1.46(2) . ? N3 C11 1.365(18) . ? N3 C12 1.37(2) . ? N3 C10 1.458(19) . ? N4 C11 1.359(19) . ? N4 C13 1.37(2) . ? N4 C14 1.47(2) . ? N5 C21 1.321(19) . ? N5 C22 1.403(19) . ? N6 C21 1.34(2) . ? N6 C27 1.39(2) . ? N6 C28 1.470(19) . ? N7 C31 1.349(19) . ? N7 C32 1.38(2) . ? N7 C30 1.474(19) . ? N8 C31 1.337(19) . ? N8 C33 1.38(2) . ? N8 C34 1.47(2) . ? C1 C10 1.50(2) . ? C2 C7 1.40(2) . ? C2 C3 1.40(2) . ? C3 C4 1.36(2) . ? C4 C5 1.40(3) . ? C5 C6 1.37(3) . ? C6 C7 1.38(2) . ? C8 C9 1.52(2) . ? C12 C13 1.34(2) . ? C14 C15 1.50(2) . ? C15 C16 1.37(3) . ? C15 C20 1.40(2) . ? C16 C17 1.40(3) . ? C17 C18 1.35(3) . ? C18 C19 1.38(3) . ? C19 C20 1.38(3) . ? C21 C30 1.50(2) . ? C22 C23 1.39(2) . ? C22 C27 1.40(2) . ? C23 C24 1.38(2) . ? C24 C25 1.39(3) . ? C25 C26 1.38(3) . ? C26 C27 1.38(2) . ? C28 C29 1.49(2) . ? C32 C33 1.33(2) . ? C34 C35 1.51(2) . ? C35 C36 1.37(3) . ? C35 C40 1.37(2) . ? C36 C37 1.40(3) . ? C37 C38 1.36(3) . ? C38 C39 1.36(3) . ? C39 C40 1.38(3) . ? Ag1 Cl3 2.533(5) . ? Ag1 Cl2 2.610(6) . ? Ag1 Cl1 2.611(4) . ? Ag1 Cl4 2.693(5) . ? Ag1 Ag3 3.10(3) . ? Ag1 Ag2 3.261(3) 2_576 ? Ag2 Cl1 2.463(5) . ? Ag2 Cl2 2.497(8) 2_576 ? Ag2 Cl4 2.627(8) 2_576 ? Ag2 Ag2 2.826(5) 2_576 ? Ag2 Ag1 3.261(3) 2_576 ? Ag3 Cl2 2.41(3) 2_576 ? Ag3 Cl1 2.54(2) . ? Ag3 Cl4 2.62(3) . ? Ag3 Ag3 2.62(5) 2_576 ? Cl2 Ag3 2.41(3) 2_576 ? Cl2 Ag2 2.497(8) 2_576 ? Cl4 Ag2 2.627(8) 2_576 ? 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 C11 Ni1 C31 94.4(6) . . ? C11 Ni1 N5 178.6(6) . . ? C31 Ni1 N5 86.6(6) . . ? C11 Ni1 N1 88.2(6) . . ? C31 Ni1 N1 177.3(6) . . ? N5 Ni1 N1 90.8(5) . . ? C1 N1 C2 106.0(12) . . ? C1 N1 Ni1 121.7(10) . . ? C2 N1 Ni1 132.0(10) . . ? C1 N2 C7 106.9(12) . . ? C1 N2 C8 127.5(14) . . ? C7 N2 C8 125.2(13) . . ? C11 N3 C12 110.9(13) . . ? C11 N3 C10 123.2(12) . . ? C12 N3 C10 125.8(13) . . ? C11 N4 C13 110.7(13) . . ? C11 N4 C14 126.8(13) . . ? C13 N4 C14 122.4(14) . . ? C21 N5 C22 105.6(13) . . ? C21 N5 Ni1 122.3(10) . . ? C22 N5 Ni1 131.2(10) . . ? C21 N6 C27 107.2(12) . . ? C21 N6 C28 128.1(13) . . ? C27 N6 C28 124.7(13) . . ? C31 N7 C32 110.6(13) . . ? C31 N7 C30 123.7(12) . . ? C32 N7 C30 125.3(13) . . ? C31 N8 C33 110.8(13) . . ? C31 N8 C34 126.4(13) . . ? C33 N8 C34 122.9(13) . . ? N1 C1 N2 112.7(13) . . ? N1 C1 C10 121.0(13) . . ? N2 C1 C10 126.3(14) . . ? N1 C2 C7 108.6(14) . . ? N1 C2 C3 131.4(14) . . ? C7 C2 C3 119.8(14) . . ? C4 C3 C2 117.4(16) . . ? C3 C4 C5 121.7(17) . . ? C6 C5 C4 122.1(16) . . ? C5 C6 C7 116.1(16) . . ? C6 C7 N2 131.6(15) . . ? C6 C7 C2 122.7(16) . . ? N2 C7 C2 105.6(13) . . ? N2 C8 C9 110.4(13) . . ? N3 C10 C1 108.4(12) . . ? N4 C11 N3 104.1(13) . . ? N4 C11 Ni1 135.7(11) . . ? N3 C11 Ni1 120.2(11) . . ? C13 C12 N3 107.0(15) . . ? C12 C13 N4 107.4(15) . . ? N4 C14 C15 114.6(13) . . ? C16 C15 C20 118.6(17) . . ? C16 C15 C14 123.0(16) . . ? C20 C15 C14 118.2(16) . . ? C15 C16 C17 120.6(19) . . ? C18 C17 C16 120(2) . . ? C17 C18 C19 120.5(19) . . ? C20 C19 C18 119.7(18) . . ? C19 C20 C15 120.3(18) . . ? N5 C21 N6 113.2(13) . . ? N5 C21 C30 120.9(14) . . ? N6 C21 C30 125.8(14) . . ? C23 C22 N5 131.2(15) . . ? C23 C22 C27 120.8(14) . . ? N5 C22 C27 108.1(13) . . ? C24 C23 C22 115.8(16) . . ? C23 C24 C25 123.3(16) . . ? C26 C25 C24 120.8(16) . . ? C25 C26 C27 117.0(17) . . ? C26 C27 N6 131.8(16) . . ? C26 C27 C22 122.3(15) . . ? N6 C27 C22 105.9(13) . . ? N6 C28 C29 112.6(13) . . ? N7 C30 C21 107.4(12) . . ? N8 C31 N7 105.0(12) . . ? N8 C31 Ni1 134.1(11) . . ? N7 C31 Ni1 120.5(11) . . ? C33 C32 N7 106.9(14) . . ? C32 C33 N8 106.7(14) . . ? N8 C34 C35 115.1(13) . . ? C36 C35 C40 118.5(17) . . ? C36 C35 C34 122.0(15) . . ? C40 C35 C34 119.4(17) . . ? C35 C36 C37 120.0(18) . . ? C38 C37 C36 121(2) . . ? C37 C38 C39 119.6(18) . . ? C38 C39 C40 120.1(19) . . ? C35 C40 C39 121(2) . . ? Cl3 Ag1 Cl2 110.4(2) . . ? Cl3 Ag1 Cl1 119.97(16) . . ? Cl2 Ag1 Cl1 110.37(18) . . ? Cl3 Ag1 Cl4 119.74(17) . . ? Cl2 Ag1 Cl4 95.78(18) . . ? Cl1 Ag1 Cl4 97.62(16) . . ? Cl3 Ag1 Ag3 161.3(5) . . ? Cl2 Ag1 Ag3 88.1(5) . . ? Cl1 Ag1 Ag3 51.8(4) . . ? Cl4 Ag1 Ag3 53.1(4) . . ? Cl3 Ag1 Ag2 145.31(13) . 2_576 ? Cl2 Ag1 Ag2 48.81(18) . 2_576 ? Cl1 Ag1 Ag2 94.65(13) . 2_576 ? Cl4 Ag1 Ag2 51.28(17) . 2_576 ? Ag3 Ag1 Ag2 47.7(4) . 2_576 ? Cl1 Ag2 Cl2 133.6(3) . 2_576 ? Cl1 Ag2 Cl4 121.2(3) . 2_576 ? Cl2 Ag2 Cl4 100.30(19) 2_576 2_576 ? Cl1 Ag2 Ag2 110.07(18) . 2_576 ? Cl2 Ag2 Ag2 97.3(3) 2_576 2_576 ? Cl4 Ag2 Ag2 78.0(2) 2_576 2_576 ? Cl1 Ag2 Ag1 174.2(3) . 2_576 ? Cl2 Ag2 Ag1 51.86(13) 2_576 2_576 ? Cl4 Ag2 Ag1 53.13(12) 2_576 2_576 ? Ag2 Ag2 Ag1 68.81(10) 2_576 2_576 ? Cl2 Ag3 Cl1 134.5(12) 2_576 . ? Cl2 Ag3 Cl4 112.6(8) 2_576 . ? Cl1 Ag3 Cl4 101.6(11) . . ? Cl2 Ag3 Ag3 104.7(14) 2_576 2_576 ? Cl1 Ag3 Ag3 110.2(13) . 2_576 ? Cl4 Ag3 Ag3 79.9(13) . 2_576 ? Cl2 Ag3 Ag1 168.0(10) 2_576 . ? Cl1 Ag3 Ag1 54.0(5) . . ? Cl4 Ag3 Ag1 55.4(6) . . ? Ag3 Ag3 Ag1 75.4(13) 2_576 . ? Ag2 Cl1 Ag3 20.4(6) . . ? Ag2 Cl1 Ag1 85.86(15) . . ? Ag3 Cl1 Ag1 74.1(7) . . ? Ag3 Cl2 Ag2 20.7(5) 2_576 2_576 ? Ag3 Cl2 Ag1 89.1(6) 2_576 . ? Ag2 Cl2 Ag1 79.3(2) 2_576 . ? Ag3 Cl4 Ag2 58.9(5) . 2_576 ? Ag3 Cl4 Ag1 71.5(5) . . ? Ag2 Cl4 Ag1 75.59(17) 2_576 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.828 _refine_diff_density_min -2.425 _refine_diff_density_rms 0.146 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 760772' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H58 Cl2 N8 Ni O3' _chemical_formula_weight 900.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.880(6) _cell_length_b 13.061(5) _cell_length_c 22.335(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.268(8) _cell_angle_gamma 90.00 _cell_volume 4648(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 917 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 18.28 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8733 _exptl_absorpt_correction_T_max 0.9550 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13065 _diffrn_reflns_av_R_equivalents 0.1254 _diffrn_reflns_av_sigmaI/netI 0.1388 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4097 _reflns_number_gt 2408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atom of the water was located from different map and refined with restraint in bond length(DFIX) and thermal parameters. The residue peaks are assigned as two methanol with half occupancy. ; _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^)+(0.1162P)^2^+38.4674P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4097 _refine_ls_number_parameters 300 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1838 _refine_ls_R_factor_gt 0.1169 _refine_ls_wR_factor_ref 0.3023 _refine_ls_wR_factor_gt 0.2699 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.0000 0.0369(5) Uani 1 2 d S . . N1 N 0.0672(5) -0.1170(5) 0.0303(3) 0.0450(18) Uani 1 1 d . . . N2 N 0.1416(5) -0.2305(5) 0.1018(4) 0.053(2) Uani 1 1 d . . . N3 N 0.1085(5) 0.0333(5) 0.1268(3) 0.0425(18) Uani 1 1 d . . . N4 N 0.1218(4) 0.1627(5) 0.0718(3) 0.0406(17) Uani 1 1 d . . . C1 C 0.0960(5) -0.1928(6) -0.0019(5) 0.043(2) Uani 1 1 d . . . C2 C 0.0906(6) -0.2011(7) -0.0654(5) 0.053(2) Uani 1 1 d . . . H2 H 0.0610 -0.1530 -0.0959 0.063 Uiso 1 1 calc R . . C3 C 0.1299(6) -0.2819(7) -0.0809(5) 0.062(3) Uani 1 1 d . . . H3 H 0.1278 -0.2897 -0.1233 0.074 Uiso 1 1 calc R . . C4 C 0.1736(7) -0.3544(7) -0.0359(7) 0.073(3) Uani 1 1 d . . . H4 H 0.2003 -0.4087 -0.0492 0.088 Uiso 1 1 calc R . . C5 C 0.1794(7) -0.3501(7) 0.0265(6) 0.069(3) Uani 1 1 d . . . H5 H 0.2068 -0.4006 0.0561 0.083 Uiso 1 1 calc R . . C6 C 0.1407(5) -0.2629(6) 0.0431(5) 0.052(3) Uani 1 1 d . . . C7 C 0.0953(6) -0.1401(6) 0.0912(4) 0.047(2) Uani 1 1 d . . . C8 C 0.1806(7) -0.2836(8) 0.1622(5) 0.071(3) Uani 1 1 d . . . H8A H 0.2059 -0.2328 0.1953 0.086 Uiso 1 1 calc R . . H8B H 0.2256 -0.3278 0.1584 0.086 Uiso 1 1 calc R . . C9 C 0.1189(7) -0.3477(8) 0.1818(5) 0.071(3) Uani 1 1 d . . . H9A H 0.0764 -0.3036 0.1887 0.106 Uiso 1 1 calc R . . H9B H 0.1483 -0.3838 0.2208 0.106 Uiso 1 1 calc R . . H9C H 0.0924 -0.3968 0.1487 0.106 Uiso 1 1 calc R . . C10 C 0.0872(6) -0.0722(6) 0.1416(4) 0.052(3) Uani 1 1 d . . . H10A H 0.1255 -0.0941 0.1830 0.063 Uiso 1 1 calc R . . H10B H 0.0297 -0.0744 0.1428 0.063 Uiso 1 1 calc R . . C11 C 0.0788(5) 0.0723(6) 0.0682(4) 0.038(2) Uani 1 1 d . . . C12 C 0.1684(6) 0.0978(7) 0.1687(4) 0.058(3) Uani 1 1 d . . . H12 H 0.1968 0.0871 0.2121 0.070 Uiso 1 1 calc R . . C13 C 0.1764(6) 0.1777(7) 0.1335(4) 0.049(2) Uani 1 1 d . . . H13 H 0.2124 0.2339 0.1478 0.059 Uiso 1 1 calc R . . C14 C 0.1176(5) 0.2254(6) 0.0174(4) 0.040(2) Uani 1 1 d . . . C15 C 0.1415(5) 0.1821(6) -0.0314(4) 0.044(2) Uani 1 1 d . . . C16 C 0.1352(6) 0.2394(6) -0.0846(5) 0.053(2) Uani 1 1 d . . . H16 H 0.1495 0.2104 -0.1181 0.064 Uiso 1 1 calc R . . C17 C 0.1069(6) 0.3424(7) -0.0887(5) 0.052(2) Uani 1 1 d . . . C18 C 0.0869(6) 0.3832(6) -0.0388(5) 0.053(2) Uani 1 1 d . . . H18 H 0.0698 0.4520 -0.0410 0.064 Uiso 1 1 calc R . . C19 C 0.0909(6) 0.3266(6) 0.0143(4) 0.046(2) Uani 1 1 d . . . C20 C 0.1792(6) 0.0748(6) -0.0273(5) 0.058(3) Uani 1 1 d . . . H20A H 0.1346 0.0244 -0.0382 0.087 Uiso 1 1 calc R . . H20B H 0.2167 0.0625 0.0155 0.087 Uiso 1 1 calc R . . H20C H 0.2104 0.0695 -0.0568 0.087 Uiso 1 1 calc R . . C21 C 0.0997(8) 0.4054(8) -0.1474(5) 0.076(3) Uani 1 1 d . . . H21A H 0.0613 0.4620 -0.1504 0.114 Uiso 1 1 calc R . . H21B H 0.0787 0.3626 -0.1848 0.114 Uiso 1 1 calc R . . H21C H 0.1545 0.4320 -0.1445 0.114 Uiso 1 1 calc R . . C22 C 0.0707(6) 0.3769(7) 0.0679(5) 0.059(3) Uani 1 1 d . . . H22A H 0.0409 0.3290 0.0859 0.088 Uiso 1 1 calc R . . H22B H 0.0357 0.4365 0.0521 0.088 Uiso 1 1 calc R . . H22C H 0.1223 0.3978 0.1003 0.088 Uiso 1 1 calc R . . O2S O 0.0531(13) 0.0256(16) 0.3103(9) 0.106(6) Uani 0.50 1 d P A -1 H2S H 0.0950 -0.0073 0.3099 0.159 Uiso 0.50 1 calc PR A -1 C2S C 0.046(3) 0.109(2) 0.2752(13) 0.17(3) Uani 0.50 1 d P A -1 H2S1 H 0.0248 0.1652 0.2946 0.253 Uiso 0.50 1 calc PR A -1 H2S2 H 0.0069 0.0967 0.2330 0.253 Uiso 0.50 1 calc PR A -1 H2S3 H 0.1002 0.1278 0.2726 0.253 Uiso 0.50 1 calc PR A -1 O1W O 0.0000 -0.1738(15) 0.2500 0.198(11) Uani 1 2 d SD . . H1W H 0.027(18) -0.126(14) 0.274(13) 0.298 Uiso 1 1 d D . . Cl1 Cl 0.2173(2) -0.0640(3) 0.30863(16) 0.1008(12) Uani 1 1 d . . . O1S O 0.3217(11) -0.1000(16) 0.2243(6) 0.094(6) Uani 0.50 1 d P . . H1S H 0.2939 -0.1055 0.2486 0.141 Uiso 0.50 1 calc PR . . C1S C 0.3998(14) -0.1229(15) 0.2547(8) 0.055(5) Uani 0.50 1 d P . . H1S1 H 0.4337 -0.1068 0.2283 0.082 Uiso 0.50 1 calc PR . . H1S2 H 0.4043 -0.1954 0.2646 0.082 Uiso 0.50 1 calc PR . . H1S3 H 0.4194 -0.0836 0.2936 0.082 Uiso 0.50 1 calc PR . . 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 Ni1 0.0581(10) 0.0105(6) 0.0371(8) 0.0021(7) 0.0090(7) 0.0018(7) N1 0.067(5) 0.015(3) 0.046(5) 0.012(3) 0.010(4) -0.001(3) N2 0.063(5) 0.024(4) 0.061(5) 0.011(4) 0.004(4) 0.006(3) N3 0.075(5) 0.013(3) 0.034(4) 0.003(3) 0.010(4) 0.000(3) N4 0.056(5) 0.019(3) 0.040(4) -0.005(3) 0.007(3) -0.005(3) C1 0.043(5) 0.014(4) 0.065(6) -0.004(4) 0.008(4) 0.003(3) C2 0.059(6) 0.030(5) 0.066(7) -0.011(5) 0.017(5) -0.001(4) C3 0.066(7) 0.035(6) 0.078(7) -0.012(5) 0.015(6) -0.014(5) C4 0.068(7) 0.025(5) 0.126(11) -0.010(6) 0.031(7) 0.004(5) C5 0.073(7) 0.028(5) 0.099(9) 0.000(6) 0.019(7) -0.004(5) C6 0.043(5) 0.018(4) 0.082(8) 0.009(5) 0.002(5) 0.004(4) C7 0.058(6) 0.021(4) 0.058(6) 0.013(4) 0.015(5) -0.002(4) C8 0.071(7) 0.044(6) 0.078(8) 0.027(6) -0.003(6) 0.004(5) C9 0.103(9) 0.039(6) 0.062(7) 0.021(5) 0.016(6) 0.005(6) C10 0.082(7) 0.022(4) 0.044(5) 0.014(4) 0.009(5) -0.015(4) C11 0.063(6) 0.015(4) 0.035(5) 0.000(3) 0.014(4) -0.002(4) C12 0.083(7) 0.043(6) 0.040(5) -0.001(5) 0.010(5) -0.006(5) C13 0.072(6) 0.034(5) 0.034(5) 0.005(4) 0.008(5) -0.004(4) C14 0.053(5) 0.016(4) 0.041(5) -0.006(4) -0.001(4) -0.015(4) C15 0.056(6) 0.021(4) 0.048(5) 0.002(4) 0.010(4) -0.006(4) C16 0.083(7) 0.027(5) 0.054(6) 0.001(4) 0.027(5) 0.007(5) C17 0.059(6) 0.037(5) 0.055(6) 0.016(5) 0.009(5) 0.001(4) C18 0.074(7) 0.020(4) 0.063(6) 0.005(4) 0.021(5) 0.001(4) C19 0.060(6) 0.022(4) 0.053(6) -0.003(4) 0.014(5) 0.000(4) C20 0.081(7) 0.026(5) 0.070(7) -0.005(5) 0.030(6) 0.010(5) C21 0.109(9) 0.056(7) 0.060(7) 0.028(6) 0.025(6) -0.005(6) C22 0.084(7) 0.025(5) 0.072(7) -0.003(5) 0.033(6) -0.003(5) O2S 0.134(17) 0.113(17) 0.069(11) -0.011(11) 0.030(11) -0.003(12) C2S 0.40(8) 0.054(16) 0.11(3) 0.013(16) 0.16(4) 0.07(3) O1W 0.33(3) 0.098(15) 0.25(3) 0.000 0.21(3) 0.000 Cl1 0.115(3) 0.091(3) 0.084(2) 0.047(2) 0.0167(19) 0.006(2) O1S 0.109(13) 0.146(16) 0.036(8) -0.045(10) 0.036(9) -0.082(13) C1S 0.094(17) 0.047(11) 0.029(10) -0.003(9) 0.028(11) 0.007(11) _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 Ni1 N1 1.891(7) . ? Ni1 N1 1.891(7) 5 ? Ni1 C11 1.909(8) . ? Ni1 C11 1.909(8) 5 ? N1 C7 1.318(11) . ? N1 C1 1.401(11) . ? N2 C6 1.373(12) . ? N2 C7 1.393(11) . ? N2 C8 1.465(11) . ? N3 C11 1.338(10) . ? N3 C12 1.409(11) . ? N3 C10 1.488(10) . ? N4 C11 1.374(10) . ? N4 C13 1.396(10) . ? N4 C14 1.448(10) . ? C1 C6 1.385(12) . ? C1 C2 1.397(13) . ? C2 C3 1.350(13) . ? C3 C4 1.402(15) . ? C4 C5 1.366(16) . ? C5 C6 1.422(14) . ? C7 C10 1.475(13) . ? C8 C9 1.510(14) . ? C12 C13 1.339(12) . ? C14 C19 1.390(11) . ? C14 C15 1.399(12) . ? C15 C16 1.378(12) . ? C15 C20 1.530(11) . ? C16 C17 1.420(12) . ? C17 C18 1.373(13) . ? C17 C21 1.519(12) . ? C18 C19 1.382(12) . ? C19 C22 1.499(12) . ? O2S C2S 1.33(3) . ? O1S C1S 1.30(2) . ? 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 Ni1 N1 179.997(1) . 5 ? N1 Ni1 C11 86.3(3) . . ? N1 Ni1 C11 93.7(3) 5 . ? N1 Ni1 C11 93.7(3) . 5 ? N1 Ni1 C11 86.3(3) 5 5 ? C11 Ni1 C11 179.997(1) . 5 ? C7 N1 C1 107.5(7) . . ? C7 N1 Ni1 121.6(6) . . ? C1 N1 Ni1 131.0(6) . . ? C6 N2 C7 105.7(7) . . ? C6 N2 C8 126.4(8) . . ? C7 N2 C8 127.9(9) . . ? C11 N3 C12 112.1(7) . . ? C11 N3 C10 122.0(7) . . ? C12 N3 C10 125.4(7) . . ? C11 N4 C13 110.0(7) . . ? C11 N4 C14 124.0(6) . . ? C13 N4 C14 125.6(7) . . ? C6 C1 C2 121.5(8) . . ? C6 C1 N1 107.0(8) . . ? C2 C1 N1 131.3(8) . . ? C3 C2 C1 116.7(9) . . ? C2 C3 C4 122.1(11) . . ? C5 C4 C3 123.2(10) . . ? C4 C5 C6 114.5(10) . . ? N2 C6 C1 108.7(8) . . ? N2 C6 C5 129.4(9) . . ? C1 C6 C5 121.9(11) . . ? N1 C7 N2 111.1(8) . . ? N1 C7 C10 123.9(7) . . ? N2 C7 C10 124.6(8) . . ? N2 C8 C9 112.8(8) . . ? C7 C10 N3 107.2(7) . . ? N3 C11 N4 104.5(7) . . ? N3 C11 Ni1 122.0(6) . . ? N4 C11 Ni1 133.3(6) . . ? C13 C12 N3 105.4(8) . . ? C12 C13 N4 108.0(8) . . ? C19 C14 C15 121.3(8) . . ? C19 C14 N4 120.3(8) . . ? C15 C14 N4 118.5(7) . . ? C16 C15 C14 119.4(8) . . ? C16 C15 C20 117.4(8) . . ? C14 C15 C20 123.1(8) . . ? C15 C16 C17 119.9(9) . . ? C18 C17 C16 118.9(8) . . ? C18 C17 C21 121.2(9) . . ? C16 C17 C21 119.9(9) . . ? C17 C18 C19 122.3(8) . . ? C18 C19 C14 118.2(8) . . ? C18 C19 C22 119.4(8) . . ? C14 C19 C22 122.3(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2S H2S Cl1 0.83 2.20 3.02(2) 168.5 . O1W H1W O2S 0.850(5) 2.13(10) 2.93(3) 158(26) . O1S H1S Cl1 0.83 2.22 3.011(16) 160.8 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.473 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.108 #===END data_4a _database_code_depnum_ccdc_archive 'CCDC 760773' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 Ag2 Cl4 N8 O Pd' _chemical_formula_weight 1114.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.284(3) _cell_length_b 13.141(5) _cell_length_c 15.104(4) _cell_angle_alpha 73.16(3) _cell_angle_beta 83.08(2) _cell_angle_gamma 73.60(4) _cell_volume 2054.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4751 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.84 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 1.681 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6504 _exptl_absorpt_correction_T_max 0.9059 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26695 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9403 _reflns_number_gt 7414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+5.5899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9403 _refine_ls_number_parameters 523 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Pd1 Pd 0.63616(3) 0.77443(3) 0.22744(2) 0.01975(10) Uani 1 1 d . . . N1 N 0.5178(4) 0.6796(3) 0.2962(3) 0.0242(8) Uani 1 1 d . . . N2 N 0.3529(3) 0.6462(3) 0.3818(3) 0.0257(8) Uani 1 1 d . . . N3 N 0.5284(4) 0.8280(3) 0.3982(3) 0.0250(8) Uani 1 1 d . . . N4 N 0.7202(4) 0.8217(3) 0.3945(3) 0.0271(8) Uani 1 1 d . . . N5 N 0.6341(3) 0.7328(3) 0.1067(3) 0.0227(8) Uani 1 1 d . . . N6 N 0.7166(3) 0.6678(3) -0.0125(3) 0.0230(8) Uani 1 1 d . . . N7 N 0.8336(3) 0.8275(3) 0.0942(3) 0.0231(8) Uani 1 1 d . . . N8 N 0.7508(3) 0.9685(3) 0.1445(3) 0.0252(8) Uani 1 1 d . . . C1 C 0.4250(4) 0.7166(4) 0.3496(3) 0.0244(9) Uani 1 1 d . . . C2 C 0.5091(4) 0.5773(4) 0.2930(3) 0.0264(10) Uani 1 1 d . . . C3 C 0.5860(5) 0.5004(4) 0.2507(3) 0.0303(11) Uani 1 1 d . . . H3 H 0.6559 0.5143 0.2137 0.036 Uiso 1 1 calc R . . C4 C 0.5546(5) 0.4026(4) 0.2657(4) 0.0377(12) Uani 1 1 d . . . H4 H 0.6051 0.3483 0.2387 0.045 Uiso 1 1 calc R . . C5 C 0.4515(6) 0.3814(4) 0.3190(4) 0.0405(13) Uani 1 1 d . . . H5 H 0.4334 0.3138 0.3262 0.049 Uiso 1 1 calc R . . C6 C 0.3742(5) 0.4563(4) 0.3621(4) 0.0370(12) Uani 1 1 d . . . H6 H 0.3046 0.4415 0.3991 0.044 Uiso 1 1 calc R . . C7 C 0.4058(4) 0.5556(4) 0.3476(3) 0.0267(10) Uani 1 1 d . . . C8 C 0.2465(4) 0.6558(4) 0.4480(3) 0.0322(11) Uani 1 1 d . . . H8A H 0.1885 0.6189 0.4356 0.039 Uiso 1 1 calc R . . H8B H 0.2034 0.7338 0.4399 0.039 Uiso 1 1 calc R . . C9 C 0.2864(5) 0.6054(6) 0.5464(4) 0.0461(15) Uani 1 1 d . . . H9A H 0.3219 0.5268 0.5562 0.069 Uiso 1 1 calc R . . H9B H 0.2153 0.6180 0.5886 0.069 Uiso 1 1 calc R . . H9C H 0.3476 0.6387 0.5576 0.069 Uiso 1 1 calc R . . C10 C 0.4084(4) 0.8227(4) 0.3733(3) 0.0270(10) Uani 1 1 d . . . H10A H 0.3772 0.8848 0.3202 0.032 Uiso 1 1 calc R . . H10B H 0.3482 0.8272 0.4254 0.032 Uiso 1 1 calc R . . C11 C 0.6338(4) 0.8133(4) 0.3454(3) 0.0241(9) Uani 1 1 d . . . C12 C 0.5481(5) 0.8474(4) 0.4790(3) 0.0335(11) Uani 1 1 d . . . H12 H 0.4888 0.8607 0.5265 0.040 Uiso 1 1 calc R . . C13 C 0.6673(5) 0.8439(5) 0.4771(4) 0.0371(12) Uani 1 1 d . . . H13 H 0.7082 0.8544 0.5231 0.045 Uiso 1 1 calc R . . C14 C 0.8505(4) 0.8178(4) 0.3664(4) 0.0328(11) Uani 1 1 d . . . H14A H 0.8902 0.8270 0.4168 0.039 Uiso 1 1 calc R . . H14B H 0.8534 0.8803 0.3125 0.039 Uiso 1 1 calc R . . C15 C 0.9233(5) 0.7145(4) 0.3427(3) 0.0322(11) Uani 1 1 d . . . C16 C 0.9069(5) 0.6125(5) 0.3909(4) 0.0450(14) Uani 1 1 d . . . H16 H 0.8437 0.6077 0.4373 0.054 Uiso 1 1 calc R . . C17 C 0.9824(6) 0.5162(5) 0.3721(5) 0.0502(15) Uani 1 1 d . . . H17 H 0.9703 0.4475 0.4064 0.060 Uiso 1 1 calc R . . C18 C 1.0742(6) 0.5217(6) 0.3038(5) 0.0507(16) Uani 1 1 d . . . H18 H 1.1242 0.4574 0.2898 0.061 Uiso 1 1 calc R . . C19 C 1.0916(5) 0.6244(6) 0.2557(4) 0.0472(15) Uani 1 1 d . . . H19 H 1.1557 0.6287 0.2099 0.057 Uiso 1 1 calc R . . C20 C 1.0167(5) 0.7205(5) 0.2736(4) 0.0380(12) Uani 1 1 d . . . H20 H 1.0288 0.7892 0.2394 0.046 Uiso 1 1 calc R . . C21 C 0.7356(4) 0.7047(4) 0.0572(3) 0.0221(9) Uani 1 1 d . . . C22 C 0.5398(4) 0.7153(4) 0.0660(3) 0.0237(9) Uani 1 1 d . . . C23 C 0.4127(4) 0.7361(4) 0.0874(3) 0.0285(10) Uani 1 1 d . . . H23 H 0.3765 0.7661 0.1367 0.034 Uiso 1 1 calc R . . C24 C 0.3435(5) 0.7103(4) 0.0319(4) 0.0326(11) Uani 1 1 d . . . H24 H 0.2575 0.7234 0.0438 0.039 Uiso 1 1 calc R . . C25 C 0.3966(5) 0.6653(4) -0.0414(4) 0.0344(11) Uani 1 1 d . . . H25 H 0.3457 0.6478 -0.0766 0.041 Uiso 1 1 calc R . . C26 C 0.5216(5) 0.6458(4) -0.0634(3) 0.0312(11) Uani 1 1 d . . . H26 H 0.5574 0.6159 -0.1129 0.037 Uiso 1 1 calc R . . C27 C 0.5921(4) 0.6727(4) -0.0083(3) 0.0248(9) Uani 1 1 d . . . C28 C 0.8083(4) 0.6276(4) -0.0809(3) 0.0274(10) Uani 1 1 d . . . H28A H 0.8800 0.6573 -0.0855 0.033 Uiso 1 1 calc R . . H28B H 0.7719 0.6537 -0.1418 0.033 Uiso 1 1 calc R . . C29 C 0.8498(6) 0.5035(5) -0.0538(4) 0.0454(14) Uani 1 1 d . . . H29A H 0.8838 0.4775 0.0072 0.068 Uiso 1 1 calc R . . H29B H 0.9127 0.4791 -0.0984 0.068 Uiso 1 1 calc R . . H29C H 0.7798 0.4741 -0.0528 0.068 Uiso 1 1 calc R . . C30 C 0.8555(4) 0.7188(4) 0.0783(3) 0.0256(10) Uani 1 1 d . . . H30A H 0.8894 0.6613 0.1335 0.031 Uiso 1 1 calc R . . H30B H 0.9154 0.7123 0.0263 0.031 Uiso 1 1 calc R . . C31 C 0.7479(4) 0.8636(4) 0.1563(3) 0.0216(9) Uani 1 1 d . . . C32 C 0.8891(4) 0.9084(4) 0.0438(4) 0.0301(11) Uani 1 1 d . . . H32 H 0.9511 0.9024 -0.0033 0.036 Uiso 1 1 calc R . . C33 C 0.8380(4) 0.9973(4) 0.0749(4) 0.0309(11) Uani 1 1 d . . . H33 H 0.8571 1.0657 0.0540 0.037 Uiso 1 1 calc R . . C34 C 0.6709(5) 1.0468(4) 0.1931(4) 0.0306(11) Uani 1 1 d . . . H34A H 0.6889 1.1186 0.1674 0.037 Uiso 1 1 calc R . . H34B H 0.6910 1.0214 0.2586 0.037 Uiso 1 1 calc R . . C35 C 0.5355(5) 1.0608(4) 0.1865(3) 0.0276(10) Uani 1 1 d . . . C36 C 0.4863(5) 1.0397(4) 0.1166(4) 0.0330(11) Uani 1 1 d . . . H36 H 0.5388 1.0147 0.0698 0.040 Uiso 1 1 calc R . . C37 C 0.3597(5) 1.0552(5) 0.1148(4) 0.0437(14) Uani 1 1 d . . . H37 H 0.3272 1.0394 0.0673 0.052 Uiso 1 1 calc R . . C38 C 0.2816(5) 1.0932(5) 0.1817(5) 0.0492(16) Uani 1 1 d . . . H38 H 0.1958 1.1044 0.1798 0.059 Uiso 1 1 calc R . . C39 C 0.3295(6) 1.1148(5) 0.2516(4) 0.0496(16) Uani 1 1 d . . . H39 H 0.2762 1.1413 0.2974 0.060 Uiso 1 1 calc R . . C40 C 0.4555(5) 1.0979(4) 0.2548(4) 0.0392(13) Uani 1 1 d . . . H40 H 0.4875 1.1116 0.3036 0.047 Uiso 1 1 calc R . . O1S O 0.8921(5) 0.4419(4) 0.1903(3) 0.0591(12) Uani 1 1 d D . . H2S H 0.891(7) 0.383(4) 0.176(5) 0.070 Uiso 1 1 d D . . H1S H 0.916(7) 0.410(6) 0.245(2) 0.070 Uiso 1 1 d D . . Ag1 Ag 0.93779(4) 1.13527(4) 0.29379(3) 0.04805(14) Uani 1 1 d . . . Ag2 Ag 0.88029(7) 0.98398(9) 0.52710(7) 0.0850(4) Uani 0.7468(18) 1 d P . 1 Ag3 Ag 0.9232(3) 1.1106(2) 0.48505(19) 0.0798(10) Uani 0.2532(18) 1 d P . 2 Cl1 Cl 0.92044(12) 1.22396(11) 0.12285(9) 0.0344(3) Uani 1 1 d . . . Cl2 Cl 1.08986(15) 0.93920(12) 0.34404(15) 0.0645(5) Uani 1 1 d . . . Cl3 Cl 0.74194(12) 1.10557(13) 0.39974(10) 0.0427(3) Uani 1 1 d . . . Cl4 Cl 1.04936(14) 1.22520(14) 0.38962(12) 0.0525(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01888(17) 0.02276(18) 0.01939(17) -0.00718(13) 0.00204(12) -0.00784(13) N1 0.026(2) 0.0228(19) 0.0233(19) -0.0034(15) 0.0010(16) -0.0095(16) N2 0.0209(19) 0.027(2) 0.028(2) -0.0031(16) -0.0010(16) -0.0094(16) N3 0.025(2) 0.025(2) 0.025(2) -0.0083(16) 0.0040(16) -0.0078(16) N4 0.024(2) 0.038(2) 0.022(2) -0.0107(17) -0.0009(16) -0.0088(17) N5 0.0218(19) 0.027(2) 0.0232(19) -0.0095(16) -0.0015(15) -0.0089(15) N6 0.0237(19) 0.0243(19) 0.0227(19) -0.0091(16) -0.0001(15) -0.0063(15) N7 0.0181(18) 0.028(2) 0.027(2) -0.0101(16) 0.0011(15) -0.0089(15) N8 0.0198(19) 0.026(2) 0.032(2) -0.0100(17) 0.0019(16) -0.0092(16) C1 0.022(2) 0.025(2) 0.024(2) -0.0037(19) 0.0010(18) -0.0062(18) C2 0.031(2) 0.026(2) 0.022(2) -0.0028(19) -0.0074(19) -0.0085(19) C3 0.037(3) 0.030(3) 0.022(2) -0.004(2) -0.005(2) -0.008(2) C4 0.052(3) 0.031(3) 0.031(3) -0.009(2) -0.009(2) -0.009(2) C5 0.061(4) 0.025(3) 0.040(3) -0.003(2) -0.012(3) -0.020(3) C6 0.038(3) 0.033(3) 0.040(3) 0.000(2) -0.008(2) -0.017(2) C7 0.027(2) 0.026(2) 0.027(2) -0.0020(19) -0.0064(19) -0.0098(19) C8 0.023(2) 0.039(3) 0.033(3) -0.004(2) 0.001(2) -0.012(2) C9 0.037(3) 0.069(4) 0.029(3) -0.005(3) -0.001(2) -0.019(3) C10 0.020(2) 0.029(2) 0.033(3) -0.011(2) 0.0020(19) -0.0061(19) C11 0.024(2) 0.022(2) 0.027(2) -0.0083(19) 0.0030(18) -0.0071(18) C12 0.035(3) 0.047(3) 0.024(2) -0.017(2) 0.006(2) -0.014(2) C13 0.041(3) 0.050(3) 0.024(3) -0.014(2) 0.001(2) -0.014(3) C14 0.023(2) 0.045(3) 0.035(3) -0.014(2) -0.003(2) -0.012(2) C15 0.027(3) 0.042(3) 0.029(3) -0.010(2) -0.009(2) -0.007(2) C16 0.038(3) 0.048(3) 0.047(3) -0.011(3) 0.008(3) -0.013(3) C17 0.043(3) 0.039(3) 0.067(4) -0.015(3) -0.003(3) -0.007(3) C18 0.035(3) 0.061(4) 0.063(4) -0.037(4) -0.011(3) -0.001(3) C19 0.029(3) 0.081(5) 0.042(3) -0.036(3) 0.008(2) -0.014(3) C20 0.024(3) 0.058(4) 0.035(3) -0.016(3) -0.002(2) -0.011(2) C21 0.024(2) 0.018(2) 0.024(2) -0.0052(17) 0.0004(18) -0.0068(17) C22 0.027(2) 0.023(2) 0.023(2) -0.0049(18) -0.0027(18) -0.0084(18) C23 0.026(2) 0.030(3) 0.029(3) -0.006(2) 0.002(2) -0.011(2) C24 0.023(2) 0.042(3) 0.033(3) -0.005(2) -0.001(2) -0.013(2) C25 0.031(3) 0.038(3) 0.037(3) -0.006(2) -0.009(2) -0.014(2) C26 0.038(3) 0.035(3) 0.026(2) -0.011(2) -0.005(2) -0.012(2) C27 0.025(2) 0.022(2) 0.026(2) -0.0049(18) -0.0007(19) -0.0071(18) C28 0.027(2) 0.029(2) 0.028(2) -0.012(2) 0.0053(19) -0.0076(19) C29 0.051(4) 0.035(3) 0.049(3) -0.019(3) 0.014(3) -0.005(3) C30 0.020(2) 0.030(2) 0.032(3) -0.018(2) 0.0015(19) -0.0053(18) C31 0.020(2) 0.025(2) 0.022(2) -0.0093(18) -0.0006(17) -0.0064(17) C32 0.020(2) 0.039(3) 0.037(3) -0.015(2) 0.010(2) -0.015(2) C33 0.027(2) 0.031(3) 0.039(3) -0.010(2) 0.009(2) -0.019(2) C34 0.033(3) 0.027(2) 0.036(3) -0.016(2) 0.001(2) -0.009(2) C35 0.032(3) 0.019(2) 0.028(2) -0.0046(19) 0.004(2) -0.0056(19) C36 0.026(3) 0.031(3) 0.035(3) -0.007(2) 0.000(2) 0.000(2) C37 0.033(3) 0.042(3) 0.048(3) 0.000(3) -0.011(3) -0.006(2) C38 0.025(3) 0.041(3) 0.061(4) 0.008(3) 0.006(3) -0.001(2) C39 0.039(3) 0.046(3) 0.046(4) -0.007(3) 0.024(3) 0.001(3) C40 0.042(3) 0.033(3) 0.037(3) -0.011(2) 0.009(2) -0.004(2) O1S 0.068(3) 0.058(3) 0.059(3) -0.024(3) 0.003(3) -0.021(3) Ag1 0.0433(3) 0.0534(3) 0.0426(3) -0.0037(2) -0.0047(2) -0.0132(2) Ag2 0.0470(5) 0.1021(7) 0.0841(6) 0.0180(5) -0.0134(4) -0.0249(4) Ag3 0.0841(19) 0.0790(18) 0.0737(17) -0.0409(14) -0.0235(13) 0.0119(13) Cl1 0.0346(7) 0.0378(7) 0.0326(6) -0.0098(5) -0.0014(5) -0.0120(5) Cl2 0.0434(9) 0.0341(8) 0.1098(15) 0.0036(9) -0.0322(9) -0.0119(6) Cl3 0.0327(7) 0.0562(9) 0.0434(8) -0.0222(7) 0.0089(6) -0.0134(6) Cl4 0.0397(8) 0.0637(10) 0.0640(10) -0.0402(8) -0.0109(7) -0.0016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C31 1.974(4) . ? Pd1 C11 1.986(5) . ? Pd1 N5 2.054(4) . ? Pd1 N1 2.066(4) . ? N1 C1 1.312(6) . ? N1 C2 1.390(6) . ? N2 C1 1.351(6) . ? N2 C7 1.386(6) . ? N2 C8 1.469(6) . ? N3 C11 1.349(6) . ? N3 C12 1.373(6) . ? N3 C10 1.473(6) . ? N4 C11 1.340(6) . ? N4 C13 1.390(6) . ? N4 C14 1.470(6) . ? N5 C21 1.312(6) . ? N5 C22 1.393(6) . ? N6 C21 1.341(6) . ? N6 C27 1.383(6) . ? N6 C28 1.472(6) . ? N7 C31 1.349(6) . ? N7 C32 1.377(6) . ? N7 C30 1.463(6) . ? N8 C31 1.347(6) . ? N8 C33 1.394(6) . ? N8 C34 1.472(6) . ? C1 C10 1.494(6) . ? C2 C3 1.389(7) . ? C2 C7 1.393(7) . ? C3 C4 1.378(7) . ? C4 C5 1.380(8) . ? C5 C6 1.379(8) . ? C6 C7 1.398(7) . ? C8 C9 1.507(7) . ? C12 C13 1.330(7) . ? C14 C15 1.493(7) . ? C15 C16 1.380(8) . ? C15 C20 1.393(7) . ? C16 C17 1.395(8) . ? C17 C18 1.373(9) . ? C18 C19 1.391(9) . ? C19 C20 1.387(8) . ? C21 C30 1.498(6) . ? C22 C27 1.393(6) . ? C22 C23 1.397(6) . ? C23 C24 1.379(7) . ? C24 C25 1.398(7) . ? C25 C26 1.377(7) . ? C26 C27 1.392(6) . ? C28 C29 1.508(7) . ? C32 C33 1.337(7) . ? C34 C35 1.499(7) . ? C35 C36 1.378(7) . ? C35 C40 1.392(7) . ? C36 C37 1.388(7) . ? C37 C38 1.371(9) . ? C38 C39 1.372(10) . ? C39 C40 1.381(8) . ? Ag1 Cl1 2.5125(16) . ? Ag1 Cl2 2.616(2) . ? Ag1 Cl3 2.6210(16) . ? Ag1 Cl4 2.7105(17) . ? Ag1 Ag3 2.802(3) . ? Ag1 Ag2 3.3248(15) 2_776 ? Ag2 Cl3 2.495(2) . ? Ag2 Cl2 2.531(2) 2_776 ? Ag2 Cl4 2.603(2) 2_776 ? Ag2 Ag2 2.8383(18) 2_776 ? Ag2 Ag1 3.3248(16) 2_776 ? Ag3 Cl4 2.414(4) . ? Ag3 Cl2 2.469(4) 2_776 ? Ag3 Cl3 2.571(3) . ? Ag3 Ag3 2.871(5) 2_776 ? Cl2 Ag3 2.469(4) 2_776 ? Cl2 Ag2 2.532(2) 2_776 ? Cl4 Ag2 2.603(2) 2_776 ? 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 C31 Pd1 C11 96.67(18) . . ? C31 Pd1 N5 84.87(16) . . ? C11 Pd1 N5 178.38(16) . . ? C31 Pd1 N1 177.32(16) . . ? C11 Pd1 N1 85.99(17) . . ? N5 Pd1 N1 92.47(15) . . ? C1 N1 C2 106.9(4) . . ? C1 N1 Pd1 121.4(3) . . ? C2 N1 Pd1 131.6(3) . . ? C1 N2 C7 106.8(4) . . ? C1 N2 C8 127.6(4) . . ? C7 N2 C8 125.3(4) . . ? C11 N3 C12 110.8(4) . . ? C11 N3 C10 124.8(4) . . ? C12 N3 C10 124.4(4) . . ? C11 N4 C13 109.9(4) . . ? C11 N4 C14 127.6(4) . . ? C13 N4 C14 122.4(4) . . ? C21 N5 C22 106.3(4) . . ? C21 N5 Pd1 122.0(3) . . ? C22 N5 Pd1 131.4(3) . . ? C21 N6 C27 106.9(4) . . ? C21 N6 C28 128.0(4) . . ? C27 N6 C28 125.1(4) . . ? C31 N7 C32 111.4(4) . . ? C31 N7 C30 123.3(4) . . ? C32 N7 C30 125.1(4) . . ? C31 N8 C33 110.7(4) . . ? C31 N8 C34 126.4(4) . . ? C33 N8 C34 122.8(4) . . ? N1 C1 N2 112.1(4) . . ? N1 C1 C10 121.9(4) . . ? N2 C1 C10 125.9(4) . . ? C3 C2 N1 131.1(5) . . ? C3 C2 C7 121.1(4) . . ? N1 C2 C7 107.8(4) . . ? C4 C3 C2 116.5(5) . . ? C3 C4 C5 122.4(5) . . ? C6 C5 C4 122.1(5) . . ? C5 C6 C7 115.9(5) . . ? N2 C7 C2 106.5(4) . . ? N2 C7 C6 131.5(5) . . ? C2 C7 C6 122.0(5) . . ? N2 C8 C9 111.3(4) . . ? N3 C10 C1 109.0(4) . . ? N4 C11 N3 105.3(4) . . ? N4 C11 Pd1 134.5(3) . . ? N3 C11 Pd1 119.9(3) . . ? C13 C12 N3 106.7(4) . . ? C12 C13 N4 107.3(4) . . ? N4 C14 C15 114.8(4) . . ? C16 C15 C20 118.8(5) . . ? C16 C15 C14 122.3(5) . . ? C20 C15 C14 118.7(5) . . ? C15 C16 C17 121.3(6) . . ? C18 C17 C16 120.2(6) . . ? C17 C18 C19 118.7(6) . . ? C20 C19 C18 121.5(5) . . ? C19 C20 C15 119.5(6) . . ? N5 C21 N6 112.7(4) . . ? N5 C21 C30 120.9(4) . . ? N6 C21 C30 126.4(4) . . ? C27 C22 N5 107.8(4) . . ? C27 C22 C23 121.4(4) . . ? N5 C22 C23 130.7(4) . . ? C24 C23 C22 116.2(5) . . ? C23 C24 C25 122.3(5) . . ? C26 C25 C24 121.7(5) . . ? C25 C26 C27 116.4(5) . . ? N6 C27 C26 131.7(4) . . ? N6 C27 C22 106.3(4) . . ? C26 C27 C22 122.0(4) . . ? N6 C28 C29 111.0(4) . . ? N7 C30 C21 109.0(4) . . ? N8 C31 N7 104.6(4) . . ? N8 C31 Pd1 133.5(3) . . ? N7 C31 Pd1 121.3(3) . . ? C33 C32 N7 106.8(4) . . ? C32 C33 N8 106.6(4) . . ? N8 C34 C35 113.7(4) . . ? C36 C35 C40 118.5(5) . . ? C36 C35 C34 123.8(4) . . ? C40 C35 C34 117.7(5) . . ? C35 C36 C37 120.5(5) . . ? C38 C37 C36 120.5(6) . . ? C37 C38 C39 119.6(5) . . ? C38 C39 C40 120.3(5) . . ? C39 C40 C35 120.6(6) . . ? Cl1 Ag1 Cl2 116.77(7) . . ? Cl1 Ag1 Cl3 120.85(5) . . ? Cl2 Ag1 Cl3 100.97(6) . . ? Cl1 Ag1 Cl4 116.87(6) . . ? Cl2 Ag1 Cl4 94.33(6) . . ? Cl3 Ag1 Cl4 102.70(6) . . ? Cl1 Ag1 Ag3 160.59(7) . . ? Cl2 Ag1 Ag3 81.66(8) . . ? Cl3 Ag1 Ag3 56.49(7) . . ? Cl4 Ag1 Ag3 51.91(8) . . ? Cl1 Ag1 Ag2 147.79(4) . 2_776 ? Cl2 Ag1 Ag2 48.66(6) . 2_776 ? Cl3 Ag1 Ag2 91.33(5) . 2_776 ? Cl4 Ag1 Ag2 49.83(5) . 2_776 ? Ag3 Ag1 Ag2 41.60(6) . 2_776 ? Cl3 Ag2 Cl2 118.93(7) . 2_776 ? Cl3 Ag2 Cl4 137.51(7) . 2_776 ? Cl2 Ag2 Cl4 99.07(6) 2_776 2_776 ? Cl3 Ag2 Ag2 106.60(6) . 2_776 ? Cl2 Ag2 Ag2 80.79(7) 2_776 2_776 ? Cl4 Ag2 Ag2 97.06(7) 2_776 2_776 ? Cl3 Ag2 Ag1 169.45(6) . 2_776 ? Cl2 Ag2 Ag1 50.89(4) 2_776 2_776 ? Cl4 Ag2 Ag1 52.73(4) 2_776 2_776 ? Ag2 Ag2 Ag1 70.82(4) 2_776 2_776 ? Cl4 Ag3 Cl2 124.49(12) . 2_776 ? Cl4 Ag3 Cl3 113.25(12) . . ? Cl2 Ag3 Cl3 118.38(14) 2_776 . ? Cl4 Ag3 Ag1 62.09(8) . . ? Cl2 Ag3 Ag1 171.60(13) 2_776 . ? Cl3 Ag3 Ag1 58.20(6) . . ? Cl4 Ag3 Ag3 105.12(16) . 2_776 ? Cl2 Ag3 Ag3 82.82(13) 2_776 2_776 ? Cl3 Ag3 Ag3 102.44(14) . 2_776 ? Ag1 Ag3 Ag3 90.41(11) . 2_776 ? Ag3 Cl2 Ag2 41.74(8) 2_776 2_776 ? Ag3 Cl2 Ag1 104.64(10) 2_776 . ? Ag2 Cl2 Ag1 80.45(7) 2_776 . ? Ag2 Cl3 Ag3 41.16(8) . . ? Ag2 Cl3 Ag1 89.19(6) . . ? Ag3 Cl3 Ag1 65.30(8) . . ? Ag3 Cl4 Ag2 52.62(8) . 2_776 ? Ag3 Cl4 Ag1 65.99(7) . . ? Ag2 Cl4 Ag1 77.45(6) 2_776 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.671 _refine_diff_density_min -2.087 _refine_diff_density_rms 0.139 #===END data_4b _database_code_depnum_ccdc_archive 'CCDC 760774' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H64 Cl2 N8 O4 Pd' _chemical_formula_weight 994.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6719(8) _cell_length_b 10.8574(7) _cell_length_c 11.6284(8) _cell_angle_alpha 67.763(2) _cell_angle_beta 84.498(2) _cell_angle_gamma 76.012(2) _cell_volume 1210.17(15) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2348 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 23.77 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8988 _exptl_absorpt_correction_T_max 0.9680 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8644 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5445 _reflns_number_gt 4984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^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 5445 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 1.0000 0.02533(11) Uani 1 2 d S . . N1 N 0.1852(2) -0.0410(2) 0.9467(2) 0.0304(5) Uani 1 1 d . . . N2 N 0.3487(3) -0.0513(3) 0.8154(3) 0.0440(7) Uani 1 1 d . . . N3 N 0.0471(2) 0.1875(2) 0.7472(2) 0.0330(5) Uani 1 1 d . . . N4 N -0.0554(2) 0.3115(2) 0.8465(2) 0.0294(5) Uani 1 1 d . . . Cl1 Cl 0.18809(10) 0.23265(9) 0.39721(8) 0.0548(2) Uani 1 1 d . . . C1 C 0.2982(3) -0.0992(3) 1.0156(3) 0.0372(7) Uani 1 1 d . . . C2 C 0.3182(3) -0.1352(3) 1.1413(3) 0.0455(8) Uani 1 1 d . . . H2 H 0.2496 -0.1262 1.1967 0.055 Uiso 1 1 calc R . . C3 C 0.4460(4) -0.1852(4) 1.1807(4) 0.0607(11) Uani 1 1 d . . . H3 H 0.4642 -0.2114 1.2653 0.073 Uiso 1 1 calc R . . C4 C 0.5473(4) -0.1975(4) 1.0985(5) 0.0747(14) Uani 1 1 d . . . H4 H 0.6320 -0.2330 1.1295 0.090 Uiso 1 1 calc R . . C5 C 0.5284(3) -0.1597(4) 0.9741(5) 0.0668(12) Uani 1 1 d . . . H5 H 0.5976 -0.1680 0.9190 0.080 Uiso 1 1 calc R . . C6 C 0.4009(3) -0.1083(3) 0.9332(4) 0.0473(9) Uani 1 1 d . . . C7 C 0.4230(4) -0.0433(4) 0.7003(4) 0.0639(11) Uani 1 1 d . . . H7A H 0.5079 -0.0273 0.7078 0.077 Uiso 1 1 calc R . . H7B H 0.3780 0.0343 0.6305 0.077 Uiso 1 1 calc R . . C8 C 0.4407(5) -0.1710(4) 0.6737(4) 0.0778(13) Uani 1 1 d . . . H8A H 0.4938 -0.2463 0.7379 0.117 Uiso 1 1 calc R . . H8B H 0.4827 -0.1586 0.5936 0.117 Uiso 1 1 calc R . . H8C H 0.3571 -0.1909 0.6725 0.117 Uiso 1 1 calc R . . C9 C 0.2198(3) -0.0110(3) 0.8275(3) 0.0360(7) Uani 1 1 d . . . C10 C 0.1240(3) 0.0654(3) 0.7258(3) 0.0401(7) Uani 1 1 d . . . H10A H 0.1687 0.0926 0.6455 0.048 Uiso 1 1 calc R . . H10B H 0.0673 0.0072 0.7245 0.048 Uiso 1 1 calc R . . C11 C -0.0094(3) 0.1806(3) 0.8568(2) 0.0289(6) Uani 1 1 d . . . C12 C 0.0361(3) 0.3218(3) 0.6673(3) 0.0406(7) Uani 1 1 d . . . H12 H 0.0681 0.3523 0.5855 0.049 Uiso 1 1 calc R . . C13 C -0.0287(3) 0.3996(3) 0.7289(3) 0.0374(7) Uani 1 1 d . . . H13 H -0.0518 0.4955 0.6985 0.045 Uiso 1 1 calc R . . C14 C -0.1086(3) 0.3506(3) 0.9499(3) 0.0299(6) Uani 1 1 d . . . C15 C -0.0280(3) 0.3177(3) 1.0503(3) 0.0321(6) Uani 1 1 d . . . C16 C -0.0825(3) 0.3508(3) 1.1509(3) 0.0392(7) Uani 1 1 d . . . H16 H -0.0304 0.3285 1.2198 0.047 Uiso 1 1 calc R . . C17 C -0.2104(3) 0.4153(3) 1.1532(3) 0.0422(7) Uani 1 1 d . . . C18 C -0.2854(3) 0.4505(3) 1.0508(3) 0.0399(7) Uani 1 1 d . . . H18 H -0.3720 0.4968 1.0510 0.048 Uiso 1 1 calc R . . C19 C -0.2372(3) 0.4198(3) 0.9472(3) 0.0339(6) Uani 1 1 d . . . C20 C 0.1144(3) 0.2560(3) 1.0493(3) 0.0404(7) Uani 1 1 d . . . H20A H 0.1595 0.2849 1.0998 0.061 Uiso 1 1 calc R . . H20B H 0.1469 0.2861 0.9647 0.061 Uiso 1 1 calc R . . H20C H 0.1285 0.1573 1.0829 0.061 Uiso 1 1 calc R . . C21 C -0.2660(4) 0.4514(4) 1.2645(3) 0.0561(9) Uani 1 1 d . . . H21A H -0.2199 0.5127 1.2758 0.084 Uiso 1 1 calc R . . H21B H -0.2568 0.3688 1.3382 0.084 Uiso 1 1 calc R . . H21C H -0.3567 0.4956 1.2504 0.084 Uiso 1 1 calc R . . C22 C -0.3208(3) 0.4648(3) 0.8349(3) 0.0432(7) Uani 1 1 d . . . H22A H -0.3118 0.5547 0.7786 0.065 Uiso 1 1 calc R . . H22B H -0.4103 0.4680 0.8608 0.065 Uiso 1 1 calc R . . H22C H -0.2941 0.4005 0.7929 0.065 Uiso 1 1 calc R . . O1S O 0.3488(4) 0.2914(4) 0.5644(3) 0.0833(9) Uani 1 1 d . . . H1S H 0.3115 0.2725 0.5160 0.125 Uiso 1 1 calc R . . C1S C 0.3818(6) 0.4113(5) 0.5040(4) 0.0878(16) Uani 1 1 d . . . H1SA H 0.3045 0.4824 0.4739 0.132 Uiso 1 1 calc R . . H1SB H 0.4375 0.4059 0.4343 0.132 Uiso 1 1 calc R . . H1SC H 0.4272 0.4325 0.5601 0.132 Uiso 1 1 calc R . . O2S O 0.1312(4) -0.0076(3) 0.3406(3) 0.0826(10) Uani 1 1 d . . . H2S H 0.1496 0.0596 0.3469 0.124 Uiso 1 1 calc R . . C2S C 0.1601(6) -0.1195(5) 0.4516(4) 0.0926(17) Uani 1 1 d . . . H2SA H 0.2517 -0.1406 0.4682 0.139 Uiso 1 1 calc R . . H2SB H 0.1373 -0.1977 0.4447 0.139 Uiso 1 1 calc R . . H2SC H 0.1114 -0.0981 0.5190 0.139 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 Pd1 0.02348(16) 0.02152(15) 0.02634(16) -0.00536(11) 0.00010(11) -0.00233(11) N1 0.0245(11) 0.0262(11) 0.0345(12) -0.0070(9) -0.0015(10) -0.0009(9) N2 0.0351(14) 0.0310(13) 0.0574(17) -0.0119(12) 0.0160(13) -0.0054(11) N3 0.0371(13) 0.0268(11) 0.0294(12) -0.0066(9) 0.0029(10) -0.0040(10) N4 0.0259(11) 0.0239(11) 0.0312(12) -0.0041(9) -0.0013(9) -0.0019(9) Cl1 0.0725(6) 0.0453(5) 0.0454(5) -0.0092(4) -0.0075(4) -0.0204(4) C1 0.0281(14) 0.0243(13) 0.0536(18) -0.0080(13) -0.0020(13) -0.0052(11) C2 0.0404(17) 0.0318(15) 0.057(2) -0.0054(14) -0.0140(15) -0.0084(14) C3 0.050(2) 0.0381(18) 0.082(3) -0.0013(18) -0.033(2) -0.0102(16) C4 0.0329(19) 0.040(2) 0.129(4) -0.004(2) -0.027(2) -0.0014(16) C5 0.0280(17) 0.0382(19) 0.117(4) -0.013(2) 0.006(2) -0.0047(15) C6 0.0281(15) 0.0268(15) 0.076(2) -0.0091(15) 0.0071(16) -0.0042(12) C7 0.054(2) 0.047(2) 0.076(3) -0.0171(19) 0.037(2) -0.0089(17) C8 0.078(3) 0.071(3) 0.080(3) -0.036(2) 0.030(3) -0.009(2) C9 0.0373(16) 0.0246(13) 0.0414(16) -0.0108(12) 0.0109(13) -0.0048(12) C10 0.0522(19) 0.0309(14) 0.0322(15) -0.0113(12) 0.0081(13) -0.0035(14) C11 0.0258(13) 0.0285(13) 0.0292(13) -0.0086(11) 0.0014(11) -0.0045(11) C12 0.0477(18) 0.0302(14) 0.0315(15) -0.0006(12) 0.0043(13) -0.0057(13) C13 0.0412(17) 0.0253(13) 0.0355(15) -0.0021(12) -0.0001(13) -0.0042(12) C14 0.0293(14) 0.0193(12) 0.0361(15) -0.0063(11) 0.0024(11) -0.0039(11) C15 0.0316(14) 0.0224(13) 0.0385(15) -0.0067(11) -0.0038(12) -0.0051(11) C16 0.0466(18) 0.0312(15) 0.0377(16) -0.0109(12) -0.0054(14) -0.0058(13) C17 0.0502(19) 0.0330(15) 0.0418(17) -0.0145(13) 0.0105(15) -0.0094(14) C18 0.0334(16) 0.0298(15) 0.0497(18) -0.0123(13) 0.0061(14) -0.0013(12) C19 0.0306(14) 0.0227(13) 0.0403(16) -0.0050(11) -0.0012(12) -0.0018(11) C20 0.0303(15) 0.0398(16) 0.0490(18) -0.0158(14) -0.0093(13) -0.0013(13) C21 0.070(3) 0.0466(19) 0.051(2) -0.0222(16) 0.0111(18) -0.0087(18) C22 0.0319(15) 0.0376(16) 0.0492(18) -0.0084(14) -0.0070(14) 0.0023(13) O1S 0.093(3) 0.092(2) 0.0662(19) -0.0204(18) -0.0167(18) -0.031(2) C1S 0.124(5) 0.103(4) 0.059(3) -0.041(3) 0.013(3) -0.053(4) O2S 0.132(3) 0.0610(18) 0.0607(18) -0.0198(15) -0.0213(18) -0.027(2) C2S 0.143(5) 0.070(3) 0.064(3) -0.017(2) -0.036(3) -0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.009(2) . ? Pd1 N1 2.009(2) 2_557 ? Pd1 C11 2.023(3) 2_557 ? Pd1 C11 2.023(3) . ? N1 C9 1.334(4) . ? N1 C1 1.389(4) . ? N2 C9 1.350(4) . ? N2 C6 1.381(5) . ? N2 C7 1.473(4) . ? N3 C11 1.341(3) . ? N3 C12 1.384(4) . ? N3 C10 1.476(4) . ? N4 C11 1.348(3) . ? N4 C13 1.391(3) . ? N4 C14 1.445(4) . ? C1 C2 1.387(5) . ? C1 C6 1.396(4) . ? C2 C3 1.392(5) . ? C3 C4 1.390(7) . ? C4 C5 1.367(7) . ? C5 C6 1.394(5) . ? C7 C8 1.497(6) . ? C9 C10 1.487(4) . ? C12 C13 1.337(4) . ? C14 C19 1.393(4) . ? C14 C15 1.400(4) . ? C15 C16 1.387(4) . ? C15 C20 1.506(4) . ? C16 C17 1.379(4) . ? C17 C18 1.376(5) . ? C17 C21 1.518(4) . ? C18 C19 1.389(4) . ? C19 C22 1.506(4) . ? O1S C1S 1.339(5) . ? O2S C2S 1.395(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 Pd1 N1 180.0 . 2_557 ? N1 Pd1 C11 95.91(10) . 2_557 ? N1 Pd1 C11 84.09(10) 2_557 2_557 ? N1 Pd1 C11 84.09(10) . . ? N1 Pd1 C11 95.91(10) 2_557 . ? C11 Pd1 C11 180.0 2_557 . ? C9 N1 C1 106.7(2) . . ? C9 N1 Pd1 122.3(2) . . ? C1 N1 Pd1 131.0(2) . . ? C9 N2 C6 107.4(3) . . ? C9 N2 C7 127.8(3) . . ? C6 N2 C7 124.8(3) . . ? C11 N3 C12 110.9(2) . . ? C11 N3 C10 122.2(2) . . ? C12 N3 C10 126.4(2) . . ? C11 N4 C13 110.3(2) . . ? C11 N4 C14 123.3(2) . . ? C13 N4 C14 125.9(2) . . ? C2 C1 N1 130.4(3) . . ? C2 C1 C6 121.6(3) . . ? N1 C1 C6 107.8(3) . . ? C1 C2 C3 116.1(4) . . ? C4 C3 C2 121.8(4) . . ? C5 C4 C3 122.4(4) . . ? C4 C5 C6 116.4(4) . . ? N2 C6 C5 131.6(4) . . ? N2 C6 C1 106.7(3) . . ? C5 C6 C1 121.6(4) . . ? N2 C7 C8 112.0(3) . . ? N1 C9 N2 111.3(3) . . ? N1 C9 C10 121.6(3) . . ? N2 C9 C10 127.0(3) . . ? N3 C10 C9 108.7(2) . . ? N3 C11 N4 105.2(2) . . ? N3 C11 Pd1 121.42(19) . . ? N4 C11 Pd1 133.1(2) . . ? C13 C12 N3 106.7(2) . . ? C12 C13 N4 106.8(2) . . ? C19 C14 C15 121.9(3) . . ? C19 C14 N4 119.7(3) . . ? C15 C14 N4 118.4(2) . . ? C16 C15 C14 117.4(3) . . ? C16 C15 C20 119.8(3) . . ? C14 C15 C20 122.7(3) . . ? C17 C16 C15 122.2(3) . . ? C18 C17 C16 118.6(3) . . ? C18 C17 C21 120.8(3) . . ? C16 C17 C21 120.6(3) . . ? C17 C18 C19 122.2(3) . . ? C18 C19 C14 117.6(3) . . ? C18 C19 C22 120.6(3) . . ? C14 C19 C22 121.8(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.879 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.085 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 760775' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 Cl2 N8 Ni O3' _chemical_formula_weight 844.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7175(6) _cell_length_b 13.9369(7) _cell_length_c 14.0231(7) _cell_angle_alpha 66.4730(10) _cell_angle_beta 66.4010(10) _cell_angle_gamma 71.5880(10) _cell_volume 2051.96(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4337 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 25.02 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8283 _exptl_absorpt_correction_T_max 0.9376 _exptl_absorpt_process_details ? _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 graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27158 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9416 _reflns_number_gt 7073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+0.3587P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9416 _refine_ls_number_parameters 517 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.058 _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 Ni1 Ni 0.74027(3) 0.77776(2) 0.60684(3) 0.02100(11) Uani 1 1 d . . . Cl1 Cl 0.08634(6) 0.77527(5) 0.56399(6) 0.02774(16) Uani 1 1 d . . . Cl2 Cl 0.52836(8) 0.78505(7) 0.10611(9) 0.0558(3) Uani 1 1 d . . . N1 N 0.76727(19) 0.87478(16) 0.45885(18) 0.0226(5) Uani 1 1 d . . . N2 N 0.86065(19) 0.99603(17) 0.31562(19) 0.0260(5) Uani 1 1 d . . . N3 N 0.75844(19) 0.97724(17) 0.59899(18) 0.0236(5) Uani 1 1 d . . . N4 N 0.60285(19) 0.93301(17) 0.72853(19) 0.0254(5) Uani 1 1 d . . . N5 N 0.78450(18) 0.65472(16) 0.56004(17) 0.0205(4) Uani 1 1 d . . . N6 N 0.76769(18) 0.49888(16) 0.56369(17) 0.0199(4) Uani 1 1 d . . . N7 N 0.66936(18) 0.59919(17) 0.78937(18) 0.0228(5) Uani 1 1 d . . . N8 N 0.74623(19) 0.68226(17) 0.83654(19) 0.0248(5) Uani 1 1 d . . . C1 C 0.8304(2) 0.9486(2) 0.4247(2) 0.0235(6) Uani 1 1 d . . . C2 C 0.7517(2) 0.8759(2) 0.3651(2) 0.0246(6) Uani 1 1 d . . . C3 C 0.6893(2) 0.8182(2) 0.3524(3) 0.0299(6) Uani 1 1 d . . . H3 H 0.6475 0.7676 0.4133 0.036 Uiso 1 1 calc R . . C4 C 0.6911(3) 0.8380(2) 0.2460(3) 0.0355(7) Uani 1 1 d . . . H4 H 0.6497 0.8001 0.2341 0.043 Uiso 1 1 calc R . . C5 C 0.7521(3) 0.9119(2) 0.1576(3) 0.0386(8) Uani 1 1 d . . . H5 H 0.7515 0.9231 0.0864 0.046 Uiso 1 1 calc R . . C6 C 0.8142(3) 0.9703(2) 0.1691(3) 0.0350(7) Uani 1 1 d . . . H6 H 0.8560 1.0208 0.1080 0.042 Uiso 1 1 calc R . . C7 C 0.8117(2) 0.9504(2) 0.2751(2) 0.0275(6) Uani 1 1 d . . . C8 C 0.9422(3) 1.0706(2) 0.2486(3) 0.0346(7) Uani 1 1 d . . . H8A H 0.9380 1.1145 0.2913 0.042 Uiso 1 1 calc R . . H8B H 0.9200 1.1189 0.1827 0.042 Uiso 1 1 calc R . . C9 C 1.0661(3) 1.0099(3) 0.2143(3) 0.0523(9) Uani 1 1 d . . . H9A H 1.0900 0.9662 0.2794 0.079 Uiso 1 1 calc R . . H9B H 1.1189 1.0604 0.1660 0.079 Uiso 1 1 calc R . . H9C H 1.0692 0.9639 0.1752 0.079 Uiso 1 1 calc R . . C10 C 0.8616(2) 0.9761(2) 0.5019(2) 0.0251(6) Uani 1 1 d . . . H10A H 0.9279 0.9226 0.5231 0.030 Uiso 1 1 calc R . . H10B H 0.8847 1.0469 0.4664 0.030 Uiso 1 1 calc R . . C11 C 0.6959(2) 0.8980(2) 0.6519(2) 0.0234(5) Uani 1 1 d . . . C12 C 0.7063(2) 1.0616(2) 0.6415(2) 0.0289(6) Uani 1 1 d . . . H12 H 0.7339 1.1257 0.6181 0.035 Uiso 1 1 calc R . . C13 C 0.6091(3) 1.0339(2) 0.7224(3) 0.0306(6) Uani 1 1 d . . . H13 H 0.5543 1.0753 0.7675 0.037 Uiso 1 1 calc R . . C14 C 0.5068(2) 0.8763(2) 0.8040(2) 0.0300(6) Uani 1 1 d . . . H14A H 0.4453 0.9234 0.8443 0.036 Uiso 1 1 calc R . . H14B H 0.5361 0.8131 0.8584 0.036 Uiso 1 1 calc R . . C15 C 0.4529(2) 0.8403(2) 0.7484(2) 0.0279(6) Uani 1 1 d . . . C16 C 0.4597(2) 0.8877(2) 0.6391(2) 0.0297(6) Uani 1 1 d . . . H16 H 0.5016 0.9445 0.5954 0.036 Uiso 1 1 calc R . . C17 C 0.4060(3) 0.8535(2) 0.5922(3) 0.0354(7) Uani 1 1 d . . . H17 H 0.4123 0.8863 0.5168 0.042 Uiso 1 1 calc R . . C18 C 0.3437(3) 0.7721(3) 0.6549(3) 0.0409(8) Uani 1 1 d . . . H18 H 0.3057 0.7494 0.6237 0.049 Uiso 1 1 calc R . . C19 C 0.3374(3) 0.7242(3) 0.7639(3) 0.0456(9) Uani 1 1 d . . . H19 H 0.2952 0.6677 0.8075 0.055 Uiso 1 1 calc R . . C20 C 0.3916(3) 0.7568(2) 0.8109(3) 0.0374(7) Uani 1 1 d . . . H20 H 0.3869 0.7224 0.8858 0.045 Uiso 1 1 calc R . . C21 C 0.7275(2) 0.57373(19) 0.6143(2) 0.0207(5) Uani 1 1 d . . . C22 C 0.8710(2) 0.62919(19) 0.4693(2) 0.0202(5) Uani 1 1 d . . . C23 C 0.9614(2) 0.6806(2) 0.3880(2) 0.0230(5) Uani 1 1 d . . . H23 H 0.9720 0.7452 0.3877 0.028 Uiso 1 1 calc R . . C24 C 1.0346(2) 0.6340(2) 0.3084(2) 0.0245(6) Uani 1 1 d . . . H24 H 1.0960 0.6679 0.2515 0.029 Uiso 1 1 calc R . . C25 C 1.0206(2) 0.5378(2) 0.3094(2) 0.0244(6) Uani 1 1 d . . . H25 H 1.0724 0.5085 0.2527 0.029 Uiso 1 1 calc R . . C26 C 0.9338(2) 0.4845(2) 0.3904(2) 0.0221(5) Uani 1 1 d . . . H26 H 0.9252 0.4186 0.3917 0.026 Uiso 1 1 calc R . . C27 C 0.8595(2) 0.53235(19) 0.4700(2) 0.0191(5) Uani 1 1 d . . . C28 C 0.7278(2) 0.3965(2) 0.6038(2) 0.0249(6) Uani 1 1 d . . . H28A H 0.7154 0.3649 0.6836 0.030 Uiso 1 1 calc R . . H28B H 0.7896 0.3465 0.5674 0.030 Uiso 1 1 calc R . . C29 C 0.6163(3) 0.4095(3) 0.5823(3) 0.0390(7) Uani 1 1 d . . . H29A H 0.5555 0.4608 0.6161 0.058 Uiso 1 1 calc R . . H29B H 0.5912 0.3407 0.6138 0.058 Uiso 1 1 calc R . . H29C H 0.6297 0.4357 0.5031 0.058 Uiso 1 1 calc R . . C30 C 0.6326(2) 0.5668(2) 0.7220(2) 0.0243(6) Uani 1 1 d . . . H30A H 0.5594 0.6141 0.7101 0.029 Uiso 1 1 calc R . . H30B H 0.6183 0.4929 0.7595 0.029 Uiso 1 1 calc R . . C31 C 0.7198(2) 0.6852(2) 0.7508(2) 0.0236(6) Uani 1 1 d . . . C32 C 0.6622(2) 0.5441(2) 0.8979(2) 0.0265(6) Uani 1 1 d . . . H32 H 0.6297 0.4817 0.9424 0.032 Uiso 1 1 calc R . . C33 C 0.7103(2) 0.5963(2) 0.9279(2) 0.0283(6) Uani 1 1 d . . . H33 H 0.7181 0.5781 0.9979 0.034 Uiso 1 1 calc R . . C34 C 0.8045(3) 0.7598(2) 0.8345(2) 0.0297(6) Uani 1 1 d . . . H34A H 0.7443 0.8152 0.8640 0.036 Uiso 1 1 calc R . . H34B H 0.8475 0.7953 0.7576 0.036 Uiso 1 1 calc R . . C35 C 0.8884(2) 0.7101(2) 0.8998(2) 0.0254(6) Uani 1 1 d . . . C36 C 0.9944(2) 0.6462(2) 0.8618(2) 0.0290(6) Uani 1 1 d . . . H36 H 1.0119 0.6301 0.7967 0.035 Uiso 1 1 calc R . . C37 C 1.0743(2) 0.6061(2) 0.9186(2) 0.0296(6) Uani 1 1 d . . . H37 H 1.1457 0.5612 0.8934 0.036 Uiso 1 1 calc R . . C38 C 1.0502(2) 0.6312(2) 1.0122(2) 0.0305(6) Uani 1 1 d . . . H38 H 1.1062 0.6053 1.0498 0.037 Uiso 1 1 calc R . . C39 C 0.9454(3) 0.6936(2) 1.0508(2) 0.0328(7) Uani 1 1 d . . . H39 H 0.9288 0.7103 1.1153 0.039 Uiso 1 1 calc R . . C40 C 0.8641(3) 0.7319(2) 0.9953(2) 0.0313(6) Uani 1 1 d . . . H40 H 0.7910 0.7736 1.0231 0.038 Uiso 1 1 calc R . . O1S O 0.3472(2) 0.69206(18) 0.0936(2) 0.0503(6) Uani 1 1 d . . . H1S H 0.4030 0.7043 0.1020 0.075 Uiso 1 1 calc R . . C1S C 0.2594(3) 0.7871(3) 0.0811(3) 0.0533(10) Uani 1 1 d . . . H1S1 H 0.2243 0.8043 0.1499 0.080 Uiso 1 1 calc R . . H1S2 H 0.1989 0.7754 0.0625 0.080 Uiso 1 1 calc R . . H1S3 H 0.2953 0.8462 0.0223 0.080 Uiso 1 1 calc R . . O2S O 0.6476(2) 0.54522(19) 0.1967(2) 0.0472(6) Uani 1 1 d . . . H2S H 0.6124 0.6081 0.1762 0.071 Uiso 1 1 calc R . . C2S C 0.7094(3) 0.5382(3) 0.2651(3) 0.0452(8) Uani 1 1 d . . . H2S1 H 0.7755 0.5753 0.2207 0.068 Uiso 1 1 calc R . . H2S2 H 0.7383 0.4631 0.3000 0.068 Uiso 1 1 calc R . . H2S3 H 0.6569 0.5712 0.3216 0.068 Uiso 1 1 calc R . . O1W O 0.6407(5) 0.9762(4) 0.9594(4) 0.1396(18) Uani 1 1 d D . . H1WA H 0.654(7) 0.902(3) 1.010(6) 0.209 Uiso 1 1 d D . . H1WB H 0.599(7) 1.051(3) 0.939(7) 0.209 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 Ni1 0.02419(18) 0.01645(17) 0.0278(2) -0.01252(14) -0.01190(14) 0.00136(13) Cl1 0.0335(4) 0.0164(3) 0.0375(4) -0.0137(3) -0.0115(3) -0.0027(3) Cl2 0.0563(5) 0.0561(5) 0.0814(7) -0.0473(5) -0.0460(5) 0.0212(4) N1 0.0268(11) 0.0192(10) 0.0306(12) -0.0136(9) -0.0166(10) 0.0020(9) N2 0.0264(12) 0.0217(11) 0.0319(13) -0.0129(10) -0.0105(10) 0.0004(9) N3 0.0277(12) 0.0190(11) 0.0326(13) -0.0136(10) -0.0180(10) 0.0029(9) N4 0.0269(12) 0.0231(11) 0.0331(13) -0.0171(10) -0.0146(10) 0.0042(9) N5 0.0208(11) 0.0176(10) 0.0259(11) -0.0111(9) -0.0082(9) -0.0006(8) N6 0.0203(10) 0.0192(10) 0.0244(11) -0.0111(9) -0.0068(9) -0.0038(8) N7 0.0225(11) 0.0234(11) 0.0266(12) -0.0144(9) -0.0078(9) -0.0007(9) N8 0.0276(12) 0.0225(11) 0.0312(13) -0.0143(10) -0.0160(10) 0.0029(9) C1 0.0241(13) 0.0177(12) 0.0330(15) -0.0120(11) -0.0146(12) 0.0032(10) C2 0.0256(13) 0.0197(13) 0.0338(15) -0.0157(11) -0.0163(12) 0.0076(10) C3 0.0314(15) 0.0256(14) 0.0427(17) -0.0199(13) -0.0206(13) 0.0055(11) C4 0.0341(16) 0.0371(17) 0.051(2) -0.0314(16) -0.0250(15) 0.0112(13) C5 0.0469(18) 0.0374(17) 0.0392(18) -0.0252(15) -0.0248(15) 0.0143(14) C6 0.0415(17) 0.0296(15) 0.0346(16) -0.0166(13) -0.0179(14) 0.0090(13) C7 0.0275(14) 0.0252(14) 0.0336(15) -0.0172(12) -0.0146(12) 0.0069(11) C8 0.0410(17) 0.0257(15) 0.0337(16) -0.0096(13) -0.0080(14) -0.0062(13) C9 0.0367(19) 0.045(2) 0.069(3) -0.0229(19) -0.0019(18) -0.0109(16) C10 0.0282(14) 0.0220(13) 0.0322(15) -0.0126(11) -0.0134(12) -0.0031(11) C11 0.0255(13) 0.0211(13) 0.0301(14) -0.0120(11) -0.0167(11) 0.0030(10) C12 0.0362(16) 0.0197(13) 0.0436(17) -0.0176(12) -0.0241(14) 0.0034(11) C13 0.0354(16) 0.0231(14) 0.0423(17) -0.0214(13) -0.0191(14) 0.0066(12) C14 0.0291(15) 0.0260(14) 0.0316(15) -0.0139(12) -0.0065(12) 0.0014(11) C15 0.0229(13) 0.0230(13) 0.0358(16) -0.0155(12) -0.0075(12) 0.0042(11) C16 0.0269(14) 0.0249(14) 0.0400(17) -0.0116(13) -0.0148(13) -0.0008(11) C17 0.0299(15) 0.0342(16) 0.0474(19) -0.0169(14) -0.0190(14) 0.0015(13) C18 0.0282(16) 0.0369(17) 0.066(2) -0.0252(17) -0.0158(16) -0.0032(13) C19 0.0280(16) 0.0379(18) 0.066(2) -0.0214(17) -0.0015(16) -0.0103(14) C20 0.0298(16) 0.0334(16) 0.0417(18) -0.0164(14) -0.0009(14) -0.0042(13) C21 0.0189(12) 0.0209(12) 0.0272(14) -0.0125(11) -0.0098(11) -0.0003(10) C22 0.0221(12) 0.0179(12) 0.0226(13) -0.0085(10) -0.0109(10) 0.0016(10) C23 0.0224(13) 0.0187(12) 0.0293(14) -0.0073(11) -0.0119(11) -0.0010(10) C24 0.0245(13) 0.0252(13) 0.0219(13) -0.0036(11) -0.0093(11) -0.0046(11) C25 0.0252(13) 0.0248(13) 0.0210(13) -0.0101(11) -0.0078(11) 0.0028(11) C26 0.0256(13) 0.0190(12) 0.0249(13) -0.0115(11) -0.0110(11) 0.0018(10) C27 0.0210(12) 0.0166(12) 0.0215(13) -0.0064(10) -0.0110(10) 0.0001(10) C28 0.0294(14) 0.0205(13) 0.0281(14) -0.0130(11) -0.0061(12) -0.0060(11) C29 0.0378(17) 0.0418(18) 0.0452(19) -0.0138(15) -0.0121(15) -0.0186(14) C30 0.0244(13) 0.0268(14) 0.0259(14) -0.0151(11) -0.0062(11) -0.0033(11) C31 0.0226(13) 0.0204(13) 0.0322(15) -0.0166(11) -0.0114(11) 0.0046(10) C32 0.0265(14) 0.0264(14) 0.0240(14) -0.0103(11) -0.0063(11) -0.0006(11) C33 0.0323(15) 0.0274(14) 0.0269(15) -0.0105(12) -0.0133(12) 0.0000(12) C34 0.0405(16) 0.0226(13) 0.0371(16) -0.0131(12) -0.0250(14) 0.0014(12) C35 0.0295(14) 0.0202(13) 0.0301(15) -0.0096(11) -0.0133(12) -0.0019(11) C36 0.0325(15) 0.0300(15) 0.0264(14) -0.0130(12) -0.0062(12) -0.0071(12) C37 0.0222(14) 0.0299(15) 0.0355(16) -0.0136(13) -0.0050(12) -0.0043(11) C38 0.0283(14) 0.0328(15) 0.0330(16) -0.0083(13) -0.0157(12) -0.0036(12) C39 0.0328(15) 0.0405(17) 0.0308(15) -0.0192(13) -0.0135(13) 0.0008(13) C40 0.0293(15) 0.0346(16) 0.0358(16) -0.0203(13) -0.0146(13) 0.0046(12) O1S 0.0691(17) 0.0338(12) 0.0474(14) -0.0095(11) -0.0169(13) -0.0149(12) C1S 0.050(2) 0.042(2) 0.052(2) -0.0085(17) -0.0044(18) -0.0111(17) O2S 0.0545(15) 0.0462(14) 0.0439(14) -0.0203(12) -0.0192(12) -0.0002(12) C2S 0.051(2) 0.0456(19) 0.0381(19) -0.0147(16) -0.0126(16) -0.0077(16) O1W 0.160(4) 0.123(4) 0.119(4) -0.027(3) -0.082(3) 0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C11 1.868(2) . ? Ni1 C31 1.876(3) . ? Ni1 N5 1.919(2) . ? Ni1 N1 1.933(2) . ? N1 C1 1.325(3) . ? N1 C2 1.400(3) . ? N2 C1 1.345(3) . ? N2 C7 1.392(3) . ? N2 C8 1.470(4) . ? N3 C11 1.353(3) . ? N3 C12 1.388(3) . ? N3 C10 1.466(4) . ? N4 C11 1.352(3) . ? N4 C13 1.400(3) . ? N4 C14 1.465(4) . ? N5 C21 1.329(3) . ? N5 C22 1.396(3) . ? N6 C21 1.348(3) . ? N6 C27 1.390(3) . ? N6 C28 1.483(3) . ? N7 C31 1.353(3) . ? N7 C32 1.384(3) . ? N7 C30 1.464(3) . ? N8 C31 1.355(3) . ? N8 C33 1.392(4) . ? N8 C34 1.478(3) . ? C1 C10 1.499(4) . ? C2 C3 1.392(4) . ? C2 C7 1.392(4) . ? C3 C4 1.396(4) . ? C4 C5 1.384(5) . ? C5 C6 1.386(4) . ? C6 C7 1.388(4) . ? C8 C9 1.518(4) . ? C12 C13 1.339(4) . ? C14 C15 1.513(4) . ? C15 C16 1.384(4) . ? C15 C20 1.393(4) . ? C16 C17 1.394(4) . ? C17 C18 1.379(4) . ? C18 C19 1.382(5) . ? C19 C20 1.384(5) . ? C21 C30 1.498(4) . ? C22 C23 1.398(4) . ? C22 C27 1.399(3) . ? C23 C24 1.379(4) . ? C24 C25 1.401(4) . ? C25 C26 1.379(4) . ? C26 C27 1.392(3) . ? C28 C29 1.506(4) . ? C32 C33 1.346(4) . ? C34 C35 1.505(4) . ? C35 C40 1.385(4) . ? C35 C36 1.393(4) . ? C36 C37 1.382(4) . ? C37 C38 1.384(4) . ? C38 C39 1.375(4) . ? C39 C40 1.387(4) . ? O1S C1S 1.438(4) . ? O2S C2S 1.422(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Ni1 C31 92.39(11) . . ? C11 Ni1 N5 179.40(10) . . ? C31 Ni1 N5 87.89(10) . . ? C11 Ni1 N1 86.65(10) . . ? C31 Ni1 N1 177.40(10) . . ? N5 Ni1 N1 93.10(9) . . ? C1 N1 C2 105.7(2) . . ? C1 N1 Ni1 119.76(17) . . ? C2 N1 Ni1 133.43(18) . . ? C1 N2 C7 106.6(2) . . ? C1 N2 C8 127.5(2) . . ? C7 N2 C8 125.4(2) . . ? C11 N3 C12 111.7(2) . . ? C11 N3 C10 122.7(2) . . ? C12 N3 C10 125.3(2) . . ? C11 N4 C13 110.0(2) . . ? C11 N4 C14 125.3(2) . . ? C13 N4 C14 124.6(2) . . ? C21 N5 C22 105.8(2) . . ? C21 N5 Ni1 122.16(17) . . ? C22 N5 Ni1 132.04(17) . . ? C21 N6 C27 107.0(2) . . ? C21 N6 C28 126.8(2) . . ? C27 N6 C28 126.1(2) . . ? C31 N7 C32 111.6(2) . . ? C31 N7 C30 123.5(2) . . ? C32 N7 C30 124.8(2) . . ? C31 N8 C33 110.8(2) . . ? C31 N8 C34 125.0(2) . . ? C33 N8 C34 124.2(2) . . ? N1 C1 N2 112.9(2) . . ? N1 C1 C10 122.4(2) . . ? N2 C1 C10 124.7(2) . . ? C3 C2 C7 120.8(3) . . ? C3 C2 N1 131.0(3) . . ? C7 C2 N1 108.2(2) . . ? C2 C3 C4 116.9(3) . . ? C5 C4 C3 121.3(3) . . ? C4 C5 C6 122.4(3) . . ? C5 C6 C7 116.0(3) . . ? C6 C7 C2 122.6(3) . . ? C6 C7 N2 130.9(3) . . ? C2 C7 N2 106.5(2) . . ? N2 C8 C9 110.2(2) . . ? N3 C10 C1 107.6(2) . . ? N4 C11 N3 104.8(2) . . ? N4 C11 Ni1 133.9(2) . . ? N3 C11 Ni1 121.17(19) . . ? C13 C12 N3 105.9(2) . . ? C12 C13 N4 107.6(2) . . ? N4 C14 C15 113.9(2) . . ? C16 C15 C20 118.6(3) . . ? C16 C15 C14 123.1(3) . . ? C20 C15 C14 118.3(3) . . ? C15 C16 C17 120.9(3) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 118.9(3) . . ? C18 C19 C20 121.3(3) . . ? C19 C20 C15 120.0(3) . . ? N5 C21 N6 112.6(2) . . ? N5 C21 C30 122.5(2) . . ? N6 C21 C30 124.9(2) . . ? N5 C22 C23 131.4(2) . . ? N5 C22 C27 108.4(2) . . ? C23 C22 C27 120.1(2) . . ? C24 C23 C22 117.5(2) . . ? C23 C24 C25 121.6(2) . . ? C26 C25 C24 121.8(2) . . ? C25 C26 C27 116.4(2) . . ? N6 C27 C26 131.2(2) . . ? N6 C27 C22 106.2(2) . . ? C26 C27 C22 122.5(2) . . ? N6 C28 C29 112.5(2) . . ? N7 C30 C21 108.5(2) . . ? N7 C31 N8 104.4(2) . . ? N7 C31 Ni1 122.02(19) . . ? N8 C31 Ni1 133.6(2) . . ? C33 C32 N7 106.4(2) . . ? C32 C33 N8 106.8(2) . . ? N8 C34 C35 113.3(2) . . ? C40 C35 C36 119.1(3) . . ? C40 C35 C34 120.4(2) . . ? C36 C35 C34 120.4(2) . . ? C37 C36 C35 120.2(3) . . ? C36 C37 C38 120.1(3) . . ? C39 C38 C37 120.1(3) . . ? C38 C39 C40 119.8(3) . . ? C35 C40 C39 120.6(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB Cl2 1.00(2) 2.36(3) 3.341(5) 170(7) 2_676 O1W H1WA Cl2 1.00(2) 2.28(7) 3.007(6) 129(7) 1_556 O2S H2S Cl2 0.84 2.33 3.168(3) 175.2 . O1S H1S Cl2 0.84 2.25 3.067(3) 163.8 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.839 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.084 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 760776' #TrackingRef 'NHC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 Cl2 N8 O3 Pd' _chemical_formula_weight 892.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5995(11) _cell_length_b 13.9671(12) _cell_length_c 14.2190(12) _cell_angle_alpha 66.875(2) _cell_angle_beta 72.213(2) _cell_angle_gamma 65.8780(10) _cell_volume 2068.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5640 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7876 _exptl_absorpt_correction_T_max 0.8849 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26609 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9487 _reflns_number_gt 8424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+6.3172P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9487 _refine_ls_number_parameters 517 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.062 _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 Pd1 Pd 0.26240(2) 0.393121(19) 0.223691(18) 0.01576(8) Uani 1 1 d . . . Cl1 Cl 0.91689(6) 0.43542(6) 0.22234(5) 0.01568(15) Uani 1 1 d . . . Cl2 Cl 0.47365(8) 0.89303(8) 0.21852(8) 0.0346(2) Uani 1 1 d . . . N1 N 0.2174(2) 0.4429(2) 0.3533(2) 0.0178(5) Uani 1 1 d . . . N2 N 0.2311(2) 0.4331(2) 0.5095(2) 0.0178(5) Uani 1 1 d . . . N3 N 0.3339(2) 0.2072(2) 0.4082(2) 0.0185(5) Uani 1 1 d . . . N4 N 0.2608(3) 0.1559(2) 0.3257(2) 0.0203(5) Uani 1 1 d . . . N5 N 0.2295(2) 0.5511(2) 0.1200(2) 0.0184(5) Uani 1 1 d . . . N6 N 0.1331(3) 0.6910(2) -0.0008(2) 0.0212(6) Uani 1 1 d . . . N7 N 0.2432(3) 0.4030(2) 0.0210(2) 0.0201(5) Uani 1 1 d . . . N8 N 0.4008(3) 0.2704(2) 0.0634(2) 0.0212(6) Uani 1 1 d . . . C1 C 0.1300(3) 0.5342(3) 0.3787(2) 0.0176(6) Uani 1 1 d . . . C2 C 0.0404(3) 0.6183(3) 0.3266(3) 0.0197(6) Uani 1 1 d . . . H2 H 0.0316 0.6211 0.2629 0.024 Uiso 1 1 calc R . . C3 C -0.0347(3) 0.6972(3) 0.3741(3) 0.0224(7) Uani 1 1 d . . . H3 H -0.0947 0.7549 0.3409 0.027 Uiso 1 1 calc R . . C4 C -0.0231(3) 0.6931(3) 0.4707(3) 0.0229(7) Uani 1 1 d . . . H4 H -0.0752 0.7484 0.4996 0.027 Uiso 1 1 calc R . . C5 C 0.0636(3) 0.6089(3) 0.5243(3) 0.0211(6) Uani 1 1 d . . . H5 H 0.0709 0.6054 0.5888 0.025 Uiso 1 1 calc R . . C6 C 0.1396(3) 0.5294(3) 0.4760(2) 0.0176(6) Uani 1 1 d . . . C7 C 0.2696(3) 0.3904(3) 0.6103(3) 0.0230(7) Uani 1 1 d . . . H7A H 0.2867 0.3112 0.6365 0.028 Uiso 1 1 calc R . . H7B H 0.2058 0.4225 0.6593 0.028 Uiso 1 1 calc R . . C8 C 0.3776(4) 0.4158(4) 0.6035(3) 0.0368(9) Uani 1 1 d . . . H8A H 0.4403 0.3864 0.5533 0.055 Uiso 1 1 calc R . . H8B H 0.4017 0.3828 0.6701 0.055 Uiso 1 1 calc R . . H8C H 0.3594 0.4942 0.5826 0.055 Uiso 1 1 calc R . . C9 C 0.2732(3) 0.3849(3) 0.4336(2) 0.0177(6) Uani 1 1 d . . . C10 C 0.3698(3) 0.2767(3) 0.4392(3) 0.0206(6) Uani 1 1 d . . . H10A H 0.4412 0.2886 0.3934 0.025 Uiso 1 1 calc R . . H10B H 0.3863 0.2400 0.5094 0.025 Uiso 1 1 calc R . . C11 C 0.2869(3) 0.2421(3) 0.3221(2) 0.0177(6) Uani 1 1 d . . . C12 C 0.3390(3) 0.0995(3) 0.4648(3) 0.0214(6) Uani 1 1 d . . . H12 H 0.3681 0.0577 0.5265 0.026 Uiso 1 1 calc R . . C13 C 0.2935(3) 0.0673(3) 0.4125(3) 0.0235(7) Uani 1 1 d . . . H13 H 0.2856 -0.0015 0.4312 0.028 Uiso 1 1 calc R . . C14 C 0.2057(3) 0.1552(3) 0.2482(3) 0.0244(7) Uani 1 1 d . . . H14A H 0.2671 0.1209 0.1993 0.029 Uiso 1 1 calc R . . H14B H 0.1666 0.2307 0.2098 0.029 Uiso 1 1 calc R . . C15 C 0.1170(3) 0.0949(3) 0.2951(3) 0.0206(6) Uani 1 1 d . . . C16 C 0.0112(3) 0.1363(3) 0.3563(3) 0.0249(7) Uani 1 1 d . . . H16 H -0.0039 0.1997 0.3722 0.030 Uiso 1 1 calc R . . C17 C -0.0724(3) 0.0829(3) 0.3939(3) 0.0271(7) Uani 1 1 d . . . H17 H -0.1425 0.1097 0.4362 0.033 Uiso 1 1 calc R . . C18 C -0.0515(3) -0.0094(3) 0.3684(3) 0.0273(7) Uani 1 1 d . . . H18 H -0.1082 -0.0441 0.3927 0.033 Uiso 1 1 calc R . . C19 C 0.0529(3) -0.0506(3) 0.3072(3) 0.0299(8) Uani 1 1 d . . . H19 H 0.0664 -0.1127 0.2897 0.036 Uiso 1 1 calc R . . C20 C 0.1384(3) 0.0009(3) 0.2714(3) 0.0261(7) Uani 1 1 d . . . H20 H 0.2098 -0.0280 0.2315 0.031 Uiso 1 1 calc R . . C21 C 0.2406(3) 0.6472(3) 0.1180(2) 0.0191(6) Uani 1 1 d . . . C22 C 0.3006(3) 0.6637(3) 0.1746(3) 0.0224(7) Uani 1 1 d . . . H22 H 0.3426 0.6052 0.2241 0.027 Uiso 1 1 calc R . . C23 C 0.2951(3) 0.7708(3) 0.1543(3) 0.0271(7) Uani 1 1 d . . . H23 H 0.3346 0.7845 0.1906 0.032 Uiso 1 1 calc R . . C24 C 0.2312(4) 0.8592(3) 0.0799(3) 0.0300(8) Uani 1 1 d . . . H24 H 0.2286 0.9302 0.0689 0.036 Uiso 1 1 calc R . . C25 C 0.1721(3) 0.8437(3) 0.0228(3) 0.0277(8) Uani 1 1 d . . . H25 H 0.1302 0.9023 -0.0267 0.033 Uiso 1 1 calc R . . C26 C 0.1787(3) 0.7352(3) 0.0432(3) 0.0217(7) Uani 1 1 d . . . C27 C 0.0517(3) 0.7543(3) -0.0759(3) 0.0273(7) Uani 1 1 d . . . H27A H 0.0599 0.7099 -0.1174 0.033 Uiso 1 1 calc R . . H27B H 0.0711 0.8198 -0.1222 0.033 Uiso 1 1 calc R . . C28 C -0.0750(4) 0.7874(4) -0.0190(4) 0.0423(10) Uani 1 1 d . . . H28A H -0.0960 0.7225 0.0225 0.063 Uiso 1 1 calc R . . H28B H -0.1270 0.8330 -0.0686 0.063 Uiso 1 1 calc R . . H28C H -0.0817 0.8277 0.0251 0.063 Uiso 1 1 calc R . . C29 C 0.1669(3) 0.5810(3) 0.0475(2) 0.0192(6) Uani 1 1 d . . . C30 C 0.1379(3) 0.5007(3) 0.0227(3) 0.0216(6) Uani 1 1 d . . . H30A H 0.0740 0.4797 0.0748 0.026 Uiso 1 1 calc R . . H30B H 0.1128 0.5344 -0.0443 0.026 Uiso 1 1 calc R . . C31 C 0.3069(3) 0.3469(3) 0.0981(2) 0.0189(6) Uani 1 1 d . . . C32 C 0.2959(3) 0.3613(3) -0.0622(3) 0.0249(7) Uani 1 1 d . . . H32 H 0.2684 0.3861 -0.1241 0.030 Uiso 1 1 calc R . . C33 C 0.3944(3) 0.2781(3) -0.0355(3) 0.0254(7) Uani 1 1 d . . . H33 H 0.4483 0.2338 -0.0755 0.030 Uiso 1 1 calc R . . C34 C 0.4985(3) 0.1929(3) 0.1190(3) 0.0240(7) Uani 1 1 d . . . H34A H 0.5595 0.1536 0.0735 0.029 Uiso 1 1 calc R . . H34B H 0.4702 0.1391 0.1783 0.029 Uiso 1 1 calc R . . C35 C 0.5520(3) 0.2476(3) 0.1563(3) 0.0233(7) Uani 1 1 d . . . C36 C 0.6076(3) 0.1871(3) 0.2426(3) 0.0334(8) Uani 1 1 d . . . H36 H 0.6094 0.1146 0.2773 0.040 Uiso 1 1 calc R . . C37 C 0.6603(4) 0.2338(4) 0.2773(3) 0.0408(10) Uani 1 1 d . . . H37 H 0.6981 0.1920 0.3345 0.049 Uiso 1 1 calc R . . C38 C 0.6572(3) 0.3412(4) 0.2282(3) 0.0387(10) Uani 1 1 d . . . H38 H 0.6927 0.3721 0.2520 0.046 Uiso 1 1 calc R . . C39 C 0.6007(3) 0.4034(4) 0.1426(3) 0.0324(8) Uani 1 1 d . . . H39 H 0.5972 0.4766 0.1096 0.039 Uiso 1 1 calc R . . C40 C 0.5496(3) 0.3567(3) 0.1063(3) 0.0253(7) Uani 1 1 d . . . H40 H 0.5134 0.3982 0.0482 0.030 Uiso 1 1 calc R . . O1S O 0.6631(3) 0.9058(3) 0.3025(2) 0.0431(7) Uani 1 1 d . . . H1S H 0.6088 0.8952 0.2922 0.065 Uiso 1 1 calc R . . C1S C 0.7486(4) 0.9174(4) 0.2104(4) 0.0506(12) Uani 1 1 d . . . H1S1 H 0.7111 0.9739 0.1539 0.076 Uiso 1 1 calc R . . H1S2 H 0.7846 0.8488 0.1949 0.076 Uiso 1 1 calc R . . H1S3 H 0.8081 0.9373 0.2202 0.076 Uiso 1 1 calc R . . O2S O 0.3557(3) 0.8000(3) 0.4540(3) 0.0432(7) Uani 1 1 d . . . H2S H 0.3878 0.8220 0.3939 0.065 Uiso 1 1 calc R . . C2S C 0.2926(4) 0.7333(3) 0.4594(4) 0.0424(10) Uani 1 1 d . . . H2S1 H 0.2648 0.6989 0.5308 0.064 Uiso 1 1 calc R . . H2S2 H 0.3438 0.6776 0.4271 0.064 Uiso 1 1 calc R . . H2S3 H 0.2266 0.7784 0.4239 0.064 Uiso 1 1 calc R . . O1W O 0.3689(9) 0.0349(7) 0.0206(6) 0.141(3) Uani 1 1 d D . . H1WA H 0.379(13) -0.028(7) 0.080(7) 0.212 Uiso 1 1 d D . . H1WB H 0.390(12) 0.084(9) -0.043(6) 0.212 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 Pd1 0.01862(13) 0.01542(12) 0.01485(12) -0.00642(9) -0.00154(9) -0.00642(9) Cl1 0.0198(3) 0.0226(3) 0.0067(3) -0.0076(3) -0.0024(2) -0.0059(3) Cl2 0.0335(5) 0.0437(5) 0.0404(5) -0.0289(4) 0.0142(4) -0.0255(4) N1 0.0188(13) 0.0163(12) 0.0177(13) -0.0061(10) -0.0031(10) -0.0046(10) N2 0.0204(13) 0.0162(12) 0.0177(13) -0.0065(10) -0.0039(10) -0.0053(10) N3 0.0196(13) 0.0159(12) 0.0198(13) -0.0078(10) -0.0015(10) -0.0050(10) N4 0.0246(14) 0.0196(13) 0.0183(13) -0.0074(11) -0.0015(11) -0.0091(11) N5 0.0211(13) 0.0189(13) 0.0176(13) -0.0075(10) -0.0023(10) -0.0078(11) N6 0.0238(14) 0.0213(14) 0.0178(13) -0.0074(11) -0.0025(11) -0.0061(11) N7 0.0247(14) 0.0228(14) 0.0182(13) -0.0084(11) -0.0020(11) -0.0122(11) N8 0.0247(14) 0.0209(13) 0.0199(14) -0.0097(11) 0.0011(11) -0.0097(11) C1 0.0188(15) 0.0154(14) 0.0191(15) -0.0058(12) -0.0011(12) -0.0073(12) C2 0.0220(15) 0.0197(15) 0.0170(15) -0.0038(12) -0.0044(12) -0.0076(12) C3 0.0203(16) 0.0154(14) 0.0272(17) -0.0035(13) -0.0053(13) -0.0039(12) C4 0.0225(16) 0.0172(15) 0.0270(17) -0.0088(13) 0.0002(13) -0.0059(13) C5 0.0242(16) 0.0191(15) 0.0211(16) -0.0087(13) -0.0022(13) -0.0071(13) C6 0.0183(15) 0.0154(14) 0.0188(15) -0.0043(12) -0.0040(12) -0.0057(12) C7 0.0287(17) 0.0208(16) 0.0196(16) -0.0070(13) -0.0085(13) -0.0045(13) C8 0.038(2) 0.039(2) 0.041(2) -0.0084(18) -0.0222(18) -0.0116(18) C9 0.0171(14) 0.0169(14) 0.0210(15) -0.0084(12) -0.0016(12) -0.0061(12) C10 0.0207(15) 0.0183(15) 0.0245(16) -0.0098(13) -0.0071(13) -0.0026(12) C11 0.0180(14) 0.0174(14) 0.0187(15) -0.0081(12) -0.0013(12) -0.0056(12) C12 0.0237(16) 0.0169(15) 0.0211(16) -0.0051(12) -0.0035(13) -0.0052(12) C13 0.0297(18) 0.0189(15) 0.0218(16) -0.0060(13) -0.0036(13) -0.0089(13) C14 0.0353(19) 0.0265(17) 0.0192(16) -0.0080(13) -0.0032(14) -0.0177(15) C15 0.0261(17) 0.0177(15) 0.0193(15) -0.0043(12) -0.0060(13) -0.0083(13) C16 0.0285(18) 0.0216(16) 0.0262(17) -0.0108(14) -0.0085(14) -0.0038(14) C17 0.0212(16) 0.0304(18) 0.0278(18) -0.0112(15) -0.0036(14) -0.0050(14) C18 0.0244(17) 0.0295(18) 0.0299(19) -0.0064(15) -0.0052(14) -0.0128(15) C19 0.0316(19) 0.0247(18) 0.038(2) -0.0140(16) -0.0010(16) -0.0130(15) C20 0.0263(17) 0.0238(17) 0.0317(19) -0.0144(15) 0.0012(14) -0.0104(14) C21 0.0201(15) 0.0197(15) 0.0193(15) -0.0097(12) 0.0027(12) -0.0089(12) C22 0.0225(16) 0.0253(17) 0.0224(16) -0.0119(13) 0.0008(13) -0.0099(13) C23 0.0281(18) 0.0324(19) 0.0300(18) -0.0191(15) 0.0042(14) -0.0166(15) C24 0.038(2) 0.0230(17) 0.0315(19) -0.0141(15) 0.0062(16) -0.0152(15) C25 0.0343(19) 0.0200(16) 0.0247(17) -0.0084(14) 0.0018(15) -0.0083(14) C26 0.0241(16) 0.0229(16) 0.0179(15) -0.0087(13) 0.0021(12) -0.0094(13) C27 0.0336(19) 0.0244(17) 0.0199(16) -0.0054(13) -0.0085(14) -0.0043(15) C28 0.031(2) 0.051(3) 0.037(2) -0.012(2) -0.0130(18) -0.0032(19) C29 0.0202(15) 0.0207(15) 0.0165(14) -0.0070(12) 0.0000(12) -0.0077(12) C30 0.0231(16) 0.0229(16) 0.0218(16) -0.0082(13) -0.0070(13) -0.0070(13) C31 0.0216(15) 0.0188(15) 0.0188(15) -0.0069(12) 0.0008(12) -0.0111(12) C32 0.0320(18) 0.0321(18) 0.0187(16) -0.0133(14) 0.0019(14) -0.0176(15) C33 0.0307(18) 0.0300(18) 0.0219(16) -0.0143(14) 0.0020(14) -0.0149(15) C34 0.0244(17) 0.0197(16) 0.0257(17) -0.0107(13) 0.0003(13) -0.0050(13) C35 0.0183(15) 0.0260(17) 0.0232(16) -0.0114(14) 0.0001(13) -0.0039(13) C36 0.0279(19) 0.031(2) 0.031(2) -0.0091(16) -0.0060(15) -0.0002(15) C37 0.028(2) 0.058(3) 0.034(2) -0.018(2) -0.0126(17) -0.0038(19) C38 0.0234(19) 0.062(3) 0.043(2) -0.028(2) -0.0026(17) -0.0166(19) C39 0.0273(19) 0.040(2) 0.037(2) -0.0177(17) 0.0018(16) -0.0179(17) C40 0.0225(16) 0.0297(18) 0.0240(17) -0.0083(14) -0.0021(13) -0.0101(14) O1S 0.060(2) 0.0385(17) 0.0277(15) -0.0059(13) -0.0112(14) -0.0152(15) C1S 0.046(3) 0.048(3) 0.036(2) -0.002(2) -0.013(2) 0.000(2) O2S 0.0513(19) 0.0353(16) 0.0460(18) -0.0179(14) -0.0016(15) -0.0169(14) C2S 0.044(2) 0.027(2) 0.052(3) -0.0109(19) -0.006(2) -0.0102(18) O1W 0.172(7) 0.128(6) 0.121(6) -0.003(5) -0.008(6) -0.093(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C11 1.978(3) . ? Pd1 C31 1.980(3) . ? Pd1 N1 2.061(3) . ? Pd1 N5 2.070(3) . ? N1 C9 1.324(4) . ? N1 C1 1.393(4) . ? N2 C9 1.352(4) . ? N2 C6 1.390(4) . ? N2 C7 1.470(4) . ? N3 C11 1.352(4) . ? N3 C12 1.384(4) . ? N3 C10 1.469(4) . ? N4 C11 1.351(4) . ? N4 C13 1.386(4) . ? N4 C14 1.476(4) . ? N5 C29 1.322(4) . ? N5 C21 1.394(4) . ? N6 C29 1.352(4) . ? N6 C26 1.384(4) . ? N6 C27 1.470(4) . ? N7 C31 1.345(4) . ? N7 C32 1.387(4) . ? N7 C30 1.466(4) . ? N8 C31 1.345(4) . ? N8 C33 1.393(4) . ? N8 C34 1.465(5) . ? C1 C2 1.394(4) . ? C1 C6 1.399(4) . ? C2 C3 1.381(5) . ? C3 C4 1.402(5) . ? C4 C5 1.383(5) . ? C5 C6 1.395(4) . ? C7 C8 1.507(5) . ? C9 C10 1.494(4) . ? C12 C13 1.348(5) . ? C14 C15 1.508(5) . ? C15 C20 1.384(5) . ? C15 C16 1.388(5) . ? C16 C17 1.391(5) . ? C17 C18 1.376(5) . ? C18 C19 1.377(5) . ? C19 C20 1.395(5) . ? C21 C22 1.390(5) . ? C21 C26 1.396(5) . ? C22 C23 1.383(5) . ? C23 C24 1.405(6) . ? C24 C25 1.377(6) . ? C25 C26 1.398(5) . ? C27 C28 1.522(6) . ? C29 C30 1.496(4) . ? C32 C33 1.341(5) . ? C34 C35 1.509(5) . ? C35 C36 1.393(5) . ? C35 C40 1.397(5) . ? C36 C37 1.384(6) . ? C37 C38 1.373(7) . ? C38 C39 1.393(6) . ? C39 C40 1.384(5) . ? O1S C1S 1.420(6) . ? O2S C2S 1.419(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 C11 Pd1 C31 94.86(13) . . ? C11 Pd1 N1 85.79(12) . . ? C31 Pd1 N1 179.14(12) . . ? C11 Pd1 N5 177.34(12) . . ? C31 Pd1 N5 84.52(12) . . ? N1 Pd1 N5 94.86(10) . . ? C9 N1 C1 106.2(3) . . ? C9 N1 Pd1 122.2(2) . . ? C1 N1 Pd1 131.6(2) . . ? C9 N2 C6 106.6(3) . . ? C9 N2 C7 127.3(3) . . ? C6 N2 C7 126.1(3) . . ? C11 N3 C12 111.1(3) . . ? C11 N3 C10 124.0(3) . . ? C12 N3 C10 124.9(3) . . ? C11 N4 C13 110.5(3) . . ? C11 N4 C14 125.1(3) . . ? C13 N4 C14 124.4(3) . . ? C29 N5 C21 106.2(3) . . ? C29 N5 Pd1 119.3(2) . . ? C21 N5 Pd1 133.4(2) . . ? C29 N6 C26 106.7(3) . . ? C29 N6 C27 127.2(3) . . ? C26 N6 C27 125.7(3) . . ? C31 N7 C32 110.9(3) . . ? C31 N7 C30 123.7(3) . . ? C32 N7 C30 125.3(3) . . ? C31 N8 C33 110.1(3) . . ? C31 N8 C34 125.4(3) . . ? C33 N8 C34 124.4(3) . . ? N1 C1 C2 131.1(3) . . ? N1 C1 C6 108.1(3) . . ? C2 C1 C6 120.7(3) . . ? C3 C2 C1 116.9(3) . . ? C2 C3 C4 122.0(3) . . ? C5 C4 C3 121.7(3) . . ? C4 C5 C6 116.2(3) . . ? N2 C6 C5 131.1(3) . . ? N2 C6 C1 106.5(3) . . ? C5 C6 C1 122.4(3) . . ? N2 C7 C8 112.6(3) . . ? N1 C9 N2 112.6(3) . . ? N1 C9 C10 122.8(3) . . ? N2 C9 C10 124.6(3) . . ? N3 C10 C9 109.6(3) . . ? N4 C11 N3 105.0(3) . . ? N4 C11 Pd1 132.4(2) . . ? N3 C11 Pd1 122.6(2) . . ? C13 C12 N3 106.3(3) . . ? C12 C13 N4 107.1(3) . . ? N4 C14 C15 113.6(3) . . ? C20 C15 C16 119.7(3) . . ? C20 C15 C14 119.4(3) . . ? C16 C15 C14 120.8(3) . . ? C15 C16 C17 119.9(3) . . ? C18 C17 C16 120.1(3) . . ? C17 C18 C19 120.3(3) . . ? C18 C19 C20 119.9(3) . . ? C15 C20 C19 120.1(3) . . ? C22 C21 N5 130.9(3) . . ? C22 C21 C26 121.1(3) . . ? N5 C21 C26 108.0(3) . . ? C23 C22 C21 117.2(3) . . ? C22 C23 C24 121.4(3) . . ? C25 C24 C23 121.9(3) . . ? C24 C25 C26 116.4(3) . . ? N6 C26 C21 106.6(3) . . ? N6 C26 C25 131.3(3) . . ? C21 C26 C25 122.0(3) . . ? N6 C27 C28 110.0(3) . . ? N5 C29 N6 112.4(3) . . ? N5 C29 C30 123.0(3) . . ? N6 C29 C30 124.6(3) . . ? N7 C30 C29 108.9(3) . . ? N8 C31 N7 105.5(3) . . ? N8 C31 Pd1 133.2(3) . . ? N7 C31 Pd1 121.0(2) . . ? C33 C32 N7 106.4(3) . . ? C32 C33 N8 107.1(3) . . ? N8 C34 C35 113.5(3) . . ? C36 C35 C40 118.4(3) . . ? C36 C35 C34 119.1(3) . . ? C40 C35 C34 122.4(3) . . ? C37 C36 C35 120.7(4) . . ? C38 C37 C36 120.7(4) . . ? C37 C38 C39 119.5(4) . . ? C40 C39 C38 120.1(4) . . ? C39 C40 C35 120.6(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.220 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.119