# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof T. P. Radhakrishnan' _publ_contact_author_address ; School of Chemistry University of Hyderabad Hyderabad 500046 INDIA ; _publ_contact_author_email TPRSC@UOHYD.ERNET.IN _publ_section_title ; Helical and Network Coordination Polymers Based on a Novel C2-symmetric Ligand : SHG Enhancement through Specific Metal Coordination ; loop_ _publ_author_name T.P.Radhakrishnan 'S.Philip Anthony' data_BCDC.H2O _database_code_depnum_ccdc_archive 'CCDC 228200' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(4-cyanophenyl)-(1R,2R)-cyclohexanediamine hydrate ; _chemical_name_common 'Bis(4-cyanophenyl)-(1R,2R)-cyclohexanediamine hydrate' _chemical_formula_moiety ? _chemical_formula_sum 'C20 H22 N4 O' _chemical_formula_weight 334.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.886(3) _cell_length_b 15.27(3) _cell_length_c 15.765(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1898(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Cuboid _exptl_crystal_colour Colorless _exptl_crystal_size_max '0.76 mm' _exptl_crystal_size_mid '0.56 mm' _exptl_crystal_size_min '0.40 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.07 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3431 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 30.96 _reflns_number_total 3405 _reflns_number_gt 1520 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 1520 _refine_ls_number_parameters 242 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1205 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1635 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N7 N 0.6350(3) 0.53504(14) 0.05609(16) 0.0626(7) Uani 1 d . . . H7 H 0.5733 0.5046 0.0901 0.075 Uiso 1 calc R . . N8 N 0.8452(3) 0.39473(14) 0.10152(14) 0.0585(7) Uani 1 d . . . H8 H 0.8946 0.4424 0.1167 0.070 Uiso 1 calc R . . N16 N 0.6598(5) 0.9690(2) 0.1335(3) 0.1288(16) Uani 1 d . . . N24 N 0.9075(5) 0.05284(19) 0.3707(2) 0.0895(10) Uani 1 d . . . O25 O 0.3613(11) 0.4140(4) 0.1239(8) 0.447(9) Uani 1 d D . . H25A H 0.33(3) 0.469(7) 0.158(10) 0.670 Uiso 1 d D . . H25B H 0.36(3) 0.359(6) 0.159(10) 0.670 Uiso 1 d D . . C1 C 0.7273(4) 0.48801(17) -0.00979(16) 0.0513(7) Uani 1 d . . . H1 H 0.8371 0.5169 -0.0179 0.062 Uiso 1 calc R . . C2 C 0.7599(4) 0.39429(16) 0.01981(16) 0.0490(6) Uani 1 d . . . H2 H 0.6500 0.3652 0.0269 0.059 Uiso 1 calc R . . C3 C 0.8598(4) 0.34467(19) -0.04797(18) 0.0613(8) Uani 1 d . . . H3A H 0.9706 0.3714 -0.0545 0.074 Uiso 1 calc R . . H3B H 0.8763 0.2846 -0.0297 0.074 Uiso 1 calc R . . C4 C 0.7687(6) 0.3453(2) -0.1327(2) 0.0768(10) Uani 1 d . . . H4A H 0.8376 0.3155 -0.1747 0.092 Uiso 1 calc R . . H4B H 0.6623 0.3138 -0.1276 0.092 Uiso 1 calc R . . C5 C 0.7342(6) 0.4379(2) -0.16169(19) 0.0825(11) Uani 1 d . . . H5A H 0.6703 0.4367 -0.2143 0.099 Uiso 1 calc R . . H5B H 0.8407 0.4677 -0.1723 0.099 Uiso 1 calc R . . C6 C 0.6344(5) 0.4876(2) -0.09464(19) 0.0707(9) Uani 1 d . . . H6A H 0.5240 0.4605 -0.0875 0.085 Uiso 1 calc R . . H6B H 0.6169 0.5474 -0.1134 0.085 Uiso 1 calc R . . C9 C 0.6384(4) 0.62379(17) 0.06828(17) 0.0503(6) Uani 1 d . . . C10 C 0.7270(4) 0.68118(17) 0.01478(19) 0.0579(7) Uani 1 d . . . H10 H 0.7852 0.6590 -0.0318 0.069 Uiso 1 calc R . . C11 C 0.7288(4) 0.76957(17) 0.0303(2) 0.0625(8) Uani 1 d . . . H11 H 0.7879 0.8066 -0.0060 0.075 Uiso 1 calc R . . C12 C 0.6436(4) 0.80470(18) 0.0997(2) 0.0571(7) Uani 1 d . . . C13 C 0.5517(4) 0.74828(18) 0.1523(2) 0.0613(8) Uani 1 d . . . H13 H 0.4909 0.7709 0.1978 0.074 Uiso 1 calc R . . C14 C 0.5507(4) 0.66009(19) 0.13711(19) 0.0587(8) Uani 1 d . . . H14 H 0.4904 0.6234 0.1733 0.070 Uiso 1 calc R . . C15 C 0.6514(5) 0.8962(2) 0.1173(3) 0.0816(11) Uani 1 d . . . C17 C 0.8529(4) 0.32593(15) 0.15560(17) 0.0467(6) Uani 1 d . . . C18 C 0.9468(4) 0.33281(17) 0.23183(17) 0.0546(7) Uani 1 d . . . H18 H 1.0019 0.3851 0.2444 0.065 Uiso 1 calc R . . C19 C 0.9583(4) 0.26478(18) 0.28704(18) 0.0573(7) Uani 1 d . . . H19 H 1.0205 0.2712 0.3368 0.069 Uiso 1 calc R . . C20 C 0.8777(4) 0.18557(17) 0.26996(18) 0.0524(7) Uani 1 d . . . C21 C 0.7840(4) 0.17733(17) 0.19624(18) 0.0572(7) Uani 1 d . . . H21 H 0.7295 0.1247 0.1845 0.069 Uiso 1 calc R . . C22 C 0.7703(4) 0.24580(15) 0.14018(18) 0.0526(7) Uani 1 d . . . H22 H 0.7055 0.2391 0.0913 0.063 Uiso 1 calc R . . C23 C 0.8942(4) 0.1120(2) 0.3263(2) 0.0654(8) Uani 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 N7 0.0714(17) 0.0496(13) 0.0669(15) 0.0061(12) 0.0200(15) 0.0011(13) N8 0.0747(16) 0.0430(11) 0.0578(14) 0.0010(11) -0.0158(14) -0.0114(12) N16 0.099(3) 0.0655(19) 0.222(5) -0.035(3) 0.003(3) -0.001(2) N24 0.102(2) 0.0708(16) 0.096(2) 0.0257(17) -0.002(2) 0.0205(18) O25 0.284(9) 0.193(5) 0.86(2) 0.156(9) 0.377(13) 0.059(6) C1 0.0526(17) 0.0501(14) 0.0513(15) -0.0009(12) 0.0012(14) 0.0018(13) C2 0.0520(15) 0.0484(13) 0.0466(14) -0.0028(12) -0.0050(13) -0.0057(13) C3 0.0672(19) 0.0582(16) 0.0585(17) -0.0081(14) 0.0029(16) 0.0040(16) C4 0.094(3) 0.082(2) 0.0543(17) -0.0163(16) -0.001(2) -0.010(2) C5 0.104(3) 0.094(2) 0.0494(17) -0.0023(17) -0.009(2) -0.018(2) C6 0.073(2) 0.073(2) 0.0658(19) 0.0096(16) -0.0171(19) -0.0014(18) C9 0.0498(15) 0.0495(14) 0.0517(14) 0.0043(12) 0.0014(15) 0.0035(13) C10 0.0583(17) 0.0577(15) 0.0576(17) 0.0022(14) 0.0088(15) 0.0042(15) C11 0.0601(19) 0.0510(15) 0.077(2) 0.0124(15) -0.0022(19) -0.0023(15) C12 0.0522(17) 0.0502(14) 0.0690(18) 0.0004(14) -0.0120(17) 0.0045(14) C13 0.0606(18) 0.0628(17) 0.0605(17) -0.0071(15) 0.0011(16) 0.0105(15) C14 0.0612(18) 0.0600(17) 0.0547(16) 0.0018(14) 0.0066(16) 0.0049(16) C15 0.063(2) 0.0628(19) 0.119(3) -0.011(2) -0.010(2) 0.0030(18) C17 0.0497(14) 0.0415(12) 0.0487(14) -0.0060(11) -0.0025(13) 0.0016(12) C18 0.0635(18) 0.0461(14) 0.0541(16) -0.0063(13) -0.0106(15) -0.0065(14) C19 0.0597(18) 0.0607(16) 0.0514(15) -0.0020(14) -0.0107(15) 0.0012(15) C20 0.0515(16) 0.0516(14) 0.0542(16) 0.0018(13) 0.0037(14) 0.0080(13) C21 0.0623(17) 0.0424(13) 0.0670(18) -0.0028(13) 0.0005(16) -0.0042(14) C22 0.0568(16) 0.0472(13) 0.0538(14) -0.0038(12) -0.0106(14) -0.0077(13) C23 0.0661(19) 0.0585(17) 0.072(2) 0.0093(16) 0.0044(17) 0.0164(16) _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 N7 C9 1.369(4) . ? N7 C1 1.457(4) . ? N8 C17 1.354(4) . ? N8 C2 1.453(3) . ? N16 C15 1.142(4) . ? N24 C23 1.148(4) . ? C1 C6 1.525(4) . ? C1 C2 1.527(4) . ? C2 C3 1.529(4) . ? C3 C4 1.517(4) . ? C4 C5 1.511(5) . ? C5 C6 1.521(5) . ? C9 C14 1.401(4) . ? C9 C10 1.402(4) . ? C10 C11 1.372(4) . ? C11 C12 1.391(4) . ? C12 C13 1.398(4) . ? C12 C15 1.427(5) . ? C13 C14 1.368(5) . ? C17 C22 1.407(4) . ? C17 C18 1.416(4) . ? C18 C19 1.358(4) . ? C19 C20 1.393(4) . ? C20 C21 1.383(4) . ? C20 C23 1.438(4) . ? C21 C22 1.373(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 C9 N7 C1 125.3(2) . . ? C17 N8 C2 125.1(2) . . ? N7 C1 C6 112.8(2) . . ? N7 C1 C2 109.1(2) . . ? C6 C1 C2 110.2(2) . . ? N8 C2 C3 112.5(2) . . ? N8 C2 C1 110.1(2) . . ? C3 C2 C1 109.7(2) . . ? C4 C3 C2 111.6(3) . . ? C5 C4 C3 111.0(3) . . ? C4 C5 C6 110.5(3) . . ? C5 C6 C1 111.3(3) . . ? N7 C9 C14 119.4(3) . . ? N7 C9 C10 123.0(3) . . ? C14 C9 C10 117.7(3) . . ? C11 C10 C9 120.8(3) . . ? C10 C11 C12 121.0(3) . . ? C11 C12 C13 118.6(3) . . ? C11 C12 C15 120.7(3) . . ? C13 C12 C15 120.7(3) . . ? C14 C13 C12 120.4(3) . . ? C13 C14 C9 121.5(3) . . ? N16 C15 C12 178.1(5) . . ? N8 C17 C22 123.0(3) . . ? N8 C17 C18 120.0(2) . . ? C22 C17 C18 117.0(2) . . ? C19 C18 C17 121.5(3) . . ? C18 C19 C20 120.7(3) . . ? C21 C20 C19 119.0(3) . . ? C21 C20 C23 119.7(3) . . ? C19 C20 C23 121.2(3) . . ? C22 C21 C20 120.9(3) . . ? C21 C22 C17 121.0(3) . . ? N24 C23 C20 179.5(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.16 _refine_diff_density_min -0.23 _refine_diff_density_rms 0.05 #===END data_CUBCDCPF6THF _database_code_depnum_ccdc_archive 'CCDC 228201' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(BCDC)Hexafluorophosphate.Tetrahydrofuran ; _chemical_name_common Copper(BCDC)Hexafluorophosphate.Tetrahydrofuran _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 Cu0.50 F3 N2 O P0.50' _chemical_formula_weight 334.56 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M P22121 _symmetry_Int_Tables_number 18 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 9.5577(9) _cell_length_b 10.4800(12) _cell_length_c 15.639(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1566.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Cube _exptl_crystal_colour Colorless _exptl_crystal_size_max '0.56 mm' _exptl_crystal_size_mid '0.52 mm' _exptl_crystal_size_min '0.48 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.82 _exptl_absorpt_correction_type 'Empirical (psi-scan)' _exptl_absorpt_correction_T_min 0.9756 _exptl_absorpt_correction_T_max 0.9990 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3086 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 31.96 _reflns_number_total 3030 _reflns_number_gt 1530 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+0.0143P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.0424(439) _refine_ls_number_reflns 1530 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1522 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.2112 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.55299(11) 1.0000 1.0000 0.0492(4) Uani 1 d S . . N3 N 0.7317(6) 0.8805(5) 0.9588(3) 0.0446(13) Uani 1 d . . . H3 H 0.7429 0.8185 0.9990 0.054 Uiso 1 calc R . . N4 N 0.5226(7) 0.5776(6) 0.5994(4) 0.0605(16) Uani 1 d . . . C5 C 0.8581(7) 0.9584(6) 0.9599(4) 0.0483(17) Uani 1 d . . . H5 H 0.8558 1.0148 0.9099 0.058 Uiso 1 calc R . . C6 C 0.9936(8) 0.8799(8) 0.9559(5) 0.063(2) Uani 1 d . . . H6A H 0.9937 0.8195 1.0029 0.076 Uiso 1 calc R . . H6B H 0.9939 0.8312 0.9031 0.076 Uiso 1 calc R . . C7 C 1.1243(9) 0.9570(10) 0.9600(5) 0.080(3) Uani 1 d . . . H7A H 1.1318 1.0094 0.9091 0.096 Uiso 1 calc R . . H7B H 1.2046 0.9004 0.9618 0.096 Uiso 1 calc R . . C8 C 0.6909(7) 0.8195(6) 0.8823(3) 0.0419(15) Uani 1 d . . . C9 C 0.7366(8) 0.8564(8) 0.8022(4) 0.0545(18) Uani 1 d . . . H9 H 0.8001 0.9233 0.7972 0.065 Uiso 1 calc R . . C10 C 0.6899(9) 0.7959(9) 0.7297(4) 0.066(2) Uani 1 d . . . H10 H 0.7193 0.8239 0.6762 0.079 Uiso 1 calc R . . C11 C 0.5997(8) 0.6943(8) 0.7361(4) 0.0571(17) Uani 1 d . . . C12 C 0.5505(9) 0.6555(8) 0.8159(4) 0.062(2) Uani 1 d . . . H12 H 0.4870 0.5886 0.8203 0.075 Uiso 1 calc R . . C13 C 0.5971(8) 0.7173(7) 0.8879(4) 0.0558(18) Uani 1 d . . . H13 H 0.5658 0.6907 0.9414 0.067 Uiso 1 calc R . . C14 C 0.5549(9) 0.6290(8) 0.6593(4) 0.0587(17) Uani 1 d . . . P2 P 0.2591(4) 0.5000 1.0000 0.0806(9) Uani 1 d S . . F15 F 0.1592(15) 0.5999(12) 1.0290(6) 0.244(7) Uani 1 d . . . F16 F 0.2582(11) 0.5478(8) 0.9062(5) 0.158(3) Uani 1 d . . . F17 F 0.3769(15) 0.5866(18) 1.0273(7) 0.298(11) Uani 1 d . . . O18 O 0.7739(12) 0.7251(11) 1.1142(5) 0.132(3) Uani 1 d . . . C19 C 0.792(2) 0.6042(17) 1.1031(12) 0.197(8) Uani 1 d . . . H19A H 0.8380 0.5892 1.0487 0.236 Uiso 1 calc R . . H19B H 0.7020 0.5614 1.1021 0.236 Uiso 1 calc R . . C20 C 0.879(3) 0.552(2) 1.1735(14) 0.183(11) Uani 1 d . . . H20A H 0.8562 0.4639 1.1864 0.220 Uiso 1 calc R . . H20B H 0.9781 0.5607 1.1625 0.220 Uiso 1 calc R . . C21 C 0.832(3) 0.636(3) 1.2362(11) 0.265(16) Uani 1 d . . . H21A H 0.9010 0.6432 1.2812 0.318 Uiso 1 calc R . . H21B H 0.7454 0.6042 1.2611 0.318 Uiso 1 calc R . . C22 C 0.810(3) 0.752(2) 1.1980(10) 0.227(15) Uani 1 d . . . H22A H 0.7349 0.7980 1.2265 0.272 Uiso 1 calc R . . H22B H 0.8941 0.8037 1.2002 0.272 Uiso 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 Cu1 0.0527(6) 0.0644(7) 0.0305(4) 0.0110(6) 0.000 0.000 N3 0.054(3) 0.051(3) 0.028(2) -0.003(2) 0.000(2) 0.005(3) N4 0.056(4) 0.084(4) 0.041(3) -0.015(3) -0.005(3) -0.004(4) C5 0.061(4) 0.053(4) 0.031(3) -0.008(2) 0.004(3) -0.002(3) C6 0.057(4) 0.075(5) 0.056(4) -0.016(4) 0.004(3) 0.008(4) C7 0.044(4) 0.122(9) 0.075(5) -0.049(5) 0.002(4) -0.002(5) C8 0.050(4) 0.049(4) 0.027(2) -0.009(2) -0.001(2) 0.006(3) C9 0.068(4) 0.061(4) 0.034(3) -0.002(3) 0.003(3) -0.017(4) C10 0.085(6) 0.081(5) 0.030(3) -0.004(4) 0.000(3) -0.005(5) C11 0.065(4) 0.071(4) 0.035(3) -0.014(3) -0.004(3) -0.010(4) C12 0.066(5) 0.079(5) 0.042(3) -0.015(3) -0.005(4) -0.028(5) C13 0.067(4) 0.064(4) 0.036(3) -0.004(3) 0.002(3) -0.016(4) C14 0.064(4) 0.076(4) 0.035(3) -0.013(3) -0.009(3) 0.006(4) P2 0.0781(19) 0.097(2) 0.0665(16) -0.019(2) 0.000 0.000 F15 0.349(15) 0.256(11) 0.127(8) 0.018(7) 0.048(9) 0.201(12) F16 0.205(8) 0.181(8) 0.087(4) 0.012(5) 0.022(5) 0.002(7) F17 0.278(15) 0.46(2) 0.157(11) -0.075(12) 0.064(10) -0.241(18) O18 0.178(8) 0.134(7) 0.085(5) 0.039(5) -0.025(6) 0.023(7) C19 0.33(2) 0.121(12) 0.138(14) 0.056(11) -0.039(16) -0.055(15) C20 0.16(2) 0.20(2) 0.188(18) 0.079(17) 0.031(18) 0.054(19) C21 0.39(4) 0.28(3) 0.118(14) 0.084(18) -0.11(2) 0.00(3) C22 0.41(5) 0.18(2) 0.089(11) 0.032(13) 0.030(18) 0.04(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 Cu1 N4 1.897(6) 4_656 ? Cu1 N4 1.897(6) 2_665 ? Cu1 N3 2.213(6) 3_577 ? Cu1 N3 2.213(6) . ? N3 C8 1.412(7) . ? N3 C5 1.459(9) . ? N4 C14 1.124(8) . ? N4 Cu1 1.897(6) 2_664 ? C5 C5 1.529(11) 3_577 ? C5 C6 1.535(10) . ? C6 C7 1.489(12) . ? C7 C7 1.542(15) 3_577 ? C8 C9 1.382(9) . ? C8 C13 1.400(10) . ? C9 C10 1.373(10) . ? C10 C11 1.374(12) . ? C11 C12 1.394(10) . ? C11 C14 1.447(9) . ? C12 C13 1.374(9) . ? P2 F15 1.488(9) 3_567 ? P2 F15 1.488(9) . ? P2 F17 1.508(12) . ? P2 F17 1.508(11) 3_567 ? P2 F16 1.551(8) 3_567 ? P2 F16 1.551(8) . ? O18 C19 1.291(18) . ? O18 C22 1.39(2) . ? C19 C20 1.48(3) . ? C20 C21 1.39(3) . ? C21 C22 1.38(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 N4 Cu1 N4 135.2(4) 4_656 2_665 ? N4 Cu1 N3 106.8(2) 4_656 3_577 ? N4 Cu1 N3 107.3(2) 2_665 3_577 ? N4 Cu1 N3 107.3(2) 4_656 . ? N4 Cu1 N3 106.8(2) 2_665 . ? N3 Cu1 N3 79.0(3) 3_577 . ? C8 N3 C5 119.4(5) . . ? C8 N3 Cu1 106.9(4) . . ? C5 N3 Cu1 108.6(4) . . ? C14 N4 Cu1 173.2(7) . 2_664 ? N3 C5 C5 109.2(4) . 3_577 ? N3 C5 C6 113.5(5) . . ? C5 C5 C6 109.8(4) 3_577 . ? C7 C6 C5 114.5(7) . . ? C6 C7 C7 110.7(6) . 3_577 ? C9 C8 C13 118.3(6) . . ? C9 C8 N3 123.7(6) . . ? C13 C8 N3 118.0(5) . . ? C10 C9 C8 121.1(7) . . ? C9 C10 C11 120.1(7) . . ? C10 C11 C12 120.2(6) . . ? C10 C11 C14 119.5(6) . . ? C12 C11 C14 120.3(7) . . ? C13 C12 C11 119.2(7) . . ? C12 C13 C8 121.1(6) . . ? N4 C14 C11 178.7(9) . . ? F15 P2 F15 100.1(13) 3_567 . ? F15 P2 F17 171.6(11) 3_567 . ? F15 P2 F17 88.2(9) . . ? F15 P2 F17 88.2(9) 3_567 3_567 ? F15 P2 F17 171.6(11) . 3_567 ? F17 P2 F17 83.4(14) . 3_567 ? F15 P2 F16 93.3(5) 3_567 3_567 ? F15 P2 F16 86.3(5) . 3_567 ? F17 P2 F16 86.0(6) . 3_567 ? F17 P2 F16 94.5(6) 3_567 3_567 ? F15 P2 F16 86.3(5) 3_567 . ? F15 P2 F16 93.3(5) . . ? F17 P2 F16 94.5(6) . . ? F17 P2 F16 86.0(6) 3_567 . ? F16 P2 F16 179.3(8) 3_567 . ? C19 O18 C22 107.2(14) . . ? O18 C19 C20 109.7(17) . . ? C21 C20 C19 96.4(18) . . ? C20 C21 C22 107.6(17) . . ? O18 C22 C21 105.4(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.67 _refine_diff_density_min -0.35 _refine_diff_density_rms 0.07 #===END data_AGBCDCCLO4 _database_code_depnum_ccdc_archive 'CCDC 228202' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I)(BCDC)Perchlorate ; _chemical_name_common Silver(i)(BCDC)Perchlorate _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Ag2 Cl2 N8 O8' _chemical_formula_weight 1047.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.488(3) _cell_length_b 14.094(3) _cell_length_c 31.354(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4193.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Cube _exptl_crystal_colour Colorless _exptl_crystal_size_max '0.64 mm' _exptl_crystal_size_mid '0.60 mm' _exptl_crystal_size_min '0.48 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.12 _exptl_absorpt_correction_type 'Empirical (psi-scan)' _exptl_absorpt_correction_T_min 0.9557 _exptl_absorpt_correction_T_max 0.9998 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4401 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.47 _reflns_number_total 4368 _reflns_number_gt 3794 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+4.6990P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0893(521) _refine_ls_number_reflns 3794 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.39632(13) 0.26979(6) 0.871087(18) 0.0909(3) Uani 1 d . . . Ag2 Ag 0.10609(10) -0.23457(5) 0.882467(19) 0.0735(3) Uani 1 d . . . Cl1 Cl 0.2404(3) 0.0237(2) 0.86408(7) 0.0798(9) Uani 1 d . . . Cl2 Cl 0.2799(3) -0.4721(2) 0.88781(7) 0.0843(9) Uani 1 d . . . O1 O 0.2967(13) 0.0962(7) 0.8895(3) 0.156(5) Uani 1 d . . . O2 O 0.3504(11) -0.0094(10) 0.8380(3) 0.157(5) Uani 1 d . . . O3 O 0.1844(12) -0.0466(7) 0.8907(3) 0.137(4) Uani 1 d . . . O4 O 0.1720(14) -0.5113(12) 0.9110(5) 0.213(7) Uani 1 d . . . O5 O 0.2201(14) -0.4012(8) 0.8636(3) 0.171(6) Uani 1 d . . . O6 O 0.3555(9) -0.5357(6) 0.8624(2) 0.110(3) Uani 1 d . . . O7 O 0.1330(11) 0.0505(9) 0.8372(3) 0.146(4) Uani 1 d . . . O8 O 0.3707(13) -0.4434(10) 0.9195(4) 0.177(6) Uani 1 d . . . N1 N 0.3531(9) 0.2503(5) 0.8058(2) 0.070(2) Uani 1 d . . . N2 N 0.1321(7) 0.0872(5) 0.61646(19) 0.0544(17) Uani 1 d . . . H2 H 0.0420 0.0877 0.6134 0.065 Uiso 1 calc R . . N3 N 0.3290(7) -0.0742(5) 0.62146(19) 0.0528(17) Uani 1 d . . . H3 H 0.4193 -0.0718 0.6192 0.063 Uiso 1 calc R . . N4 N 0.1133(9) -0.2043(5) 0.8167(2) 0.0655(19) Uani 1 d . . . N5 N 0.1374(9) -0.2613(5) 0.9474(2) 0.067(2) Uani 1 d . . . N6 N 0.3377(7) -0.4431(5) 1.13566(18) 0.0511(17) Uani 1 d . . . H6 H 0.4276 -0.4490 1.1379 0.061 Uiso 1 calc R . . N7 N 0.1424(7) -0.6046(5) 1.13349(19) 0.0508(17) Uani 1 d . . . H7 H 0.0522 -0.6078 1.1359 0.061 Uiso 1 calc R . . N8 N 0.3756(10) -0.7108(5) 0.9373(2) 0.070(2) Uani 1 d . . . C1 C 0.3210(9) 0.2197(6) 0.7742(2) 0.054(2) Uani 1 d . . . C2 C 0.2782(10) 0.1829(6) 0.7338(2) 0.055(2) Uani 1 d . . . C3 C 0.3647(9) 0.1899(6) 0.6981(2) 0.054(2) Uani 1 d . . . H3' H 0.4535 0.2171 0.7005 0.065 Uiso 1 calc R . . C4 C 0.3192(10) 0.1565(6) 0.6591(3) 0.056(2) Uani 1 d . . . H4 H 0.3782 0.1608 0.6355 0.067 Uiso 1 calc R . . C5 C 0.1854(8) 0.1164(6) 0.6548(2) 0.0477(19) Uani 1 d . . . C6 C 0.1011(9) 0.1100(6) 0.6910(2) 0.0532(19) Uani 1 d . . . H6' H 0.0118 0.0833 0.6885 0.064 Uiso 1 calc R . . C7 C 0.1445(8) 0.1415(6) 0.7300(3) 0.052(2) Uani 1 d . . . H7' H 0.0863 0.1357 0.7537 0.063 Uiso 1 calc R . . C8 C 0.2170(8) 0.0551(6) 0.5803(2) 0.0439(18) Uani 1 d . . . H8 H 0.3069 0.0893 0.5808 0.053 Uiso 1 calc R . . C9 C 0.1416(9) 0.0789(6) 0.5386(2) 0.054(2) Uani 1 d . . . H9A H 0.1307 0.1471 0.5365 0.065 Uiso 1 calc R . . H9B H 0.0482 0.0509 0.5390 0.065 Uiso 1 calc R . . C10 C 0.2206(11) 0.0431(7) 0.5000(2) 0.065(2) Uani 1 d . . . H10A H 0.3089 0.0772 0.4973 0.078 Uiso 1 calc R . . H10B H 0.1653 0.0555 0.4745 0.078 Uiso 1 calc R . . C11 C 0.2502(10) -0.0625(7) 0.5032(2) 0.062(2) Uani 1 d . . . H11A H 0.1618 -0.0970 0.5024 0.074 Uiso 1 calc R . . H11B H 0.3062 -0.0822 0.4789 0.074 Uiso 1 calc R . . C12 C 0.3275(8) -0.0867(6) 0.5436(2) 0.0465(19) Uani 1 d . . . H12A H 0.4201 -0.0577 0.5430 0.056 Uiso 1 calc R . . H12B H 0.3401 -0.1549 0.5452 0.056 Uiso 1 calc R . . C13 C 0.2486(8) -0.0529(6) 0.5832(2) 0.0459(19) Uani 1 d . . . H13 H 0.1587 -0.0869 0.5848 0.055 Uiso 1 calc R . . C14 C 0.2761(9) -0.0977(5) 0.6607(2) 0.0433(18) Uani 1 d . . . C15 C 0.3640(9) -0.0880(6) 0.6962(2) 0.052(2) Uani 1 d . . . H15 H 0.4550 -0.0649 0.6923 0.063 Uiso 1 calc R . . C16 C 0.3200(9) -0.1115(6) 0.7364(2) 0.055(2) Uani 1 d . . . H16 H 0.3782 -0.1011 0.7598 0.065 Uiso 1 calc R . . C17 C 0.1869(9) -0.1510(5) 0.7416(2) 0.0479(19) Uani 1 d . . . C18 C 0.0986(10) -0.1629(5) 0.7072(2) 0.056(2) Uani 1 d . . . H18 H 0.0096 -0.1890 0.7111 0.067 Uiso 1 calc R . . C19 C 0.1423(9) -0.1360(6) 0.6668(2) 0.051(2) Uani 1 d . . . H19 H 0.0820 -0.1435 0.6437 0.061 Uiso 1 calc R . . C20 C 0.1428(9) -0.1798(5) 0.7835(2) 0.052(2) Uani 1 d . . . C21 C 0.1663(9) -0.2923(6) 0.9797(2) 0.053(2) Uani 1 d . . . C22 C 0.2038(9) -0.3324(5) 1.0197(2) 0.049(2) Uani 1 d . . . C23 C 0.1144(10) -0.3302(5) 1.0549(2) 0.053(2) Uani 1 d . . . H23 H 0.0259 -0.3024 1.0524 0.064 Uiso 1 calc R . . C24 C 0.1551(9) -0.3684(6) 1.0930(2) 0.054(2) Uani 1 d . . . H24 H 0.0923 -0.3684 1.1157 0.064 Uiso 1 calc R . . C25 C 0.2892(8) -0.4074(5) 1.0984(2) 0.0429(18) Uani 1 d . . . C26 C 0.3780(9) -0.4088(6) 1.0629(2) 0.054(2) Uani 1 d . . . H26 H 0.4673 -0.4353 1.0656 0.064 Uiso 1 calc R . . C27 C 0.3385(9) -0.3725(6) 1.0243(2) 0.054(2) Uani 1 d . . . H27 H 0.4002 -0.3743 1.0013 0.065 Uiso 1 calc R . . C28 C 0.2533(8) -0.4729(6) 1.1729(2) 0.0426(18) Uani 1 d . . . H28 H 0.1634 -0.4387 1.1722 0.051 Uiso 1 calc R . . C29 C 0.3322(8) -0.4447(6) 1.2134(2) 0.0467(18) Uani 1 d . . . H29A H 0.3443 -0.3763 1.2140 0.056 Uiso 1 calc R . . H29B H 0.4250 -0.4736 1.2134 0.056 Uiso 1 calc R . . C30 C 0.2515(9) -0.4764(7) 1.2531(2) 0.059(2) Uani 1 d . . . H30A H 0.3065 -0.4617 1.2783 0.071 Uiso 1 calc R . . H30B H 0.1634 -0.4416 1.2549 0.071 Uiso 1 calc R . . C31 C 0.2211(10) -0.5813(7) 1.2520(2) 0.059(2) Uani 1 d . . . H31A H 0.1632 -0.5981 1.2763 0.070 Uiso 1 calc R . . H31B H 0.3090 -0.6161 1.2541 0.070 Uiso 1 calc R . . C32 C 0.1458(9) -0.6097(6) 1.2114(2) 0.050(2) Uani 1 d . . . H32A H 0.1349 -0.6781 1.2110 0.060 Uiso 1 calc R . . H32B H 0.0524 -0.5818 1.2114 0.060 Uiso 1 calc R . . C33 C 0.2226(8) -0.5792(6) 1.1719(2) 0.0433(18) Uani 1 d . . . H33 H 0.3129 -0.6130 1.1710 0.052 Uiso 1 calc R . . C34 C 0.1985(9) -0.6236(6) 1.0943(2) 0.0486(19) Uani 1 d . . . C35 C 0.3341(9) -0.6582(6) 1.0880(2) 0.051(2) Uani 1 d . . . H35 H 0.3929 -0.6673 1.1114 0.062 Uiso 1 calc R . . C36 C 0.3823(10) -0.6791(5) 1.0478(2) 0.0529(19) Uani 1 d . . . H36 H 0.4733 -0.7026 1.0444 0.063 Uiso 1 calc R . . C37 C 0.2995(9) -0.6663(5) 1.0128(2) 0.051(2) Uani 1 d . . . C38 C 0.1602(9) -0.6294(6) 1.0179(2) 0.051(2) Uani 1 d . . . H38 H 0.1019 -0.6190 0.9945 0.061 Uiso 1 calc R . . C39 C 0.1159(9) -0.6101(6) 1.0583(2) 0.0505(19) Uani 1 d . . . H39 H 0.0251 -0.5866 1.0619 0.061 Uiso 1 calc R . . C40 C 0.3439(9) -0.6912(6) 0.9707(2) 0.052(2) Uani 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 Ag1 0.1469(9) 0.0850(6) 0.0410(3) -0.0084(3) -0.0005(4) -0.0165(8) Ag2 0.1076(6) 0.0731(5) 0.0399(3) 0.0129(3) -0.0037(4) 0.0137(5) Cl1 0.0806(17) 0.114(2) 0.0447(11) -0.0010(13) -0.0015(11) -0.0586(18) Cl2 0.0874(18) 0.121(2) 0.0444(11) -0.0010(13) 0.0009(13) 0.0637(18) O1 0.244(12) 0.147(9) 0.077(5) 0.014(6) -0.043(7) -0.129(9) O2 0.118(8) 0.212(13) 0.140(8) -0.015(8) 0.054(7) -0.049(9) O3 0.203(10) 0.131(7) 0.078(5) -0.015(5) 0.060(6) -0.090(8) O4 0.139(10) 0.250(16) 0.251(14) 0.048(13) 0.111(11) 0.047(11) O5 0.252(14) 0.169(10) 0.093(6) -0.010(6) -0.032(8) 0.152(10) O6 0.119(6) 0.134(7) 0.076(4) -0.002(4) 0.030(5) 0.071(6) O7 0.119(8) 0.175(10) 0.143(8) 0.018(7) -0.052(7) -0.035(8) O8 0.181(11) 0.221(13) 0.128(8) -0.051(9) -0.070(8) 0.069(11) N1 0.099(6) 0.063(5) 0.047(4) -0.011(3) 0.005(4) 0.008(5) N2 0.042(4) 0.079(5) 0.042(3) -0.013(3) -0.002(3) 0.003(4) N3 0.037(3) 0.076(5) 0.045(4) 0.005(3) -0.010(3) 0.002(3) N4 0.095(6) 0.056(4) 0.046(3) 0.008(3) -0.001(4) 0.002(5) N5 0.096(6) 0.063(4) 0.043(3) 0.015(3) 0.002(3) 0.005(5) N6 0.042(4) 0.073(5) 0.038(3) 0.012(3) 0.003(3) -0.004(3) N7 0.040(4) 0.068(4) 0.044(3) -0.010(3) -0.003(3) 0.001(3) N8 0.094(6) 0.074(5) 0.044(4) -0.008(3) -0.005(4) -0.001(5) C1 0.071(5) 0.047(5) 0.042(4) -0.002(4) 0.002(4) 0.005(4) C2 0.070(6) 0.052(5) 0.043(4) -0.006(3) 0.000(4) 0.013(4) C3 0.055(5) 0.054(4) 0.054(4) -0.010(4) 0.003(4) -0.012(4) C4 0.058(5) 0.064(5) 0.047(4) -0.005(4) 0.009(4) -0.004(5) C5 0.047(5) 0.045(4) 0.052(4) -0.001(3) 0.001(4) -0.003(4) C6 0.040(4) 0.071(5) 0.048(4) -0.006(4) 0.003(4) 0.011(5) C7 0.043(5) 0.063(5) 0.051(4) -0.006(4) 0.011(4) 0.012(4) C8 0.034(4) 0.055(5) 0.043(4) -0.002(4) -0.002(3) -0.006(4) C9 0.051(5) 0.072(5) 0.040(4) 0.009(4) 0.000(4) 0.004(4) C10 0.072(6) 0.081(6) 0.041(4) 0.014(4) -0.005(4) -0.011(6) C11 0.065(6) 0.078(6) 0.043(4) -0.009(4) 0.002(4) -0.011(5) C12 0.041(4) 0.056(5) 0.042(4) -0.007(4) -0.006(3) 0.000(4) C13 0.040(4) 0.062(5) 0.036(4) -0.003(3) 0.000(3) -0.015(4) C14 0.045(5) 0.045(4) 0.040(4) 0.008(3) 0.000(3) 0.006(4) C15 0.052(5) 0.062(5) 0.043(4) 0.007(4) -0.010(4) -0.002(4) C16 0.055(5) 0.065(6) 0.044(4) 0.008(4) -0.015(4) -0.010(5) C17 0.060(5) 0.043(4) 0.041(4) 0.006(3) 0.002(4) 0.013(4) C18 0.058(5) 0.058(5) 0.051(4) 0.012(4) -0.003(5) -0.012(5) C19 0.059(5) 0.062(5) 0.033(3) 0.000(3) -0.004(3) -0.008(4) C20 0.065(6) 0.044(4) 0.047(4) 0.007(3) -0.002(4) 0.008(4) C21 0.063(5) 0.048(5) 0.049(4) 0.000(3) 0.006(4) -0.003(4) C22 0.066(6) 0.041(4) 0.040(4) 0.007(3) -0.005(4) -0.011(4) C23 0.059(5) 0.054(5) 0.047(4) 0.005(3) -0.004(4) 0.014(5) C24 0.056(5) 0.067(5) 0.038(4) 0.005(4) 0.007(4) 0.007(4) C25 0.046(5) 0.040(4) 0.043(4) 0.006(3) -0.005(4) -0.011(4) C26 0.044(5) 0.071(5) 0.046(4) 0.010(3) 0.004(4) -0.013(5) C27 0.055(5) 0.062(5) 0.045(4) 0.008(4) 0.000(4) -0.006(4) C28 0.036(4) 0.055(5) 0.037(4) 0.003(3) 0.000(3) 0.010(4) C29 0.048(4) 0.056(5) 0.036(4) -0.003(3) -0.001(3) 0.001(4) C30 0.058(5) 0.074(6) 0.046(4) -0.005(4) -0.001(4) 0.012(5) C31 0.059(6) 0.076(6) 0.041(4) 0.011(4) -0.004(4) -0.002(5) C32 0.051(5) 0.059(5) 0.041(4) 0.011(3) -0.003(3) 0.000(4) C33 0.040(4) 0.054(5) 0.037(4) 0.001(3) -0.001(3) 0.007(4) C34 0.054(5) 0.045(4) 0.046(4) -0.005(3) -0.001(4) -0.001(4) C35 0.056(5) 0.063(5) 0.035(4) -0.007(4) -0.008(4) 0.004(4) C36 0.055(5) 0.051(4) 0.052(4) -0.009(3) -0.004(4) 0.002(4) C37 0.062(5) 0.048(4) 0.043(4) -0.004(3) -0.001(4) -0.010(4) C38 0.052(5) 0.061(5) 0.039(4) -0.006(4) -0.012(4) -0.002(4) C39 0.037(4) 0.066(5) 0.048(4) -0.007(4) -0.012(4) 0.002(5) C40 0.060(5) 0.048(4) 0.046(4) -0.001(3) -0.008(4) -0.005(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 N8 2.102(6) 1_565 ? Ag1 N1 2.105(7) . ? Ag2 N5 2.092(6) . ? Ag2 N4 2.106(6) . ? Cl1 O7 1.376(10) . ? Cl1 O3 1.401(8) . ? Cl1 O1 1.401(8) . ? Cl1 O2 1.405(11) . ? Cl2 O8 1.376(10) . ? Cl2 O4 1.373(12) . ? Cl2 O5 1.378(9) . ? Cl2 O6 1.398(7) . ? N1 C1 1.123(10) . ? N2 C5 1.367(9) . ? N2 C8 1.463(9) . ? N3 C14 1.369(9) . ? N3 C13 1.453(9) . ? N4 C20 1.132(9) . ? N5 C21 1.135(10) . ? N6 C25 1.352(9) . ? N6 C28 1.477(9) . ? N7 C34 1.365(10) . ? N7 C33 1.469(9) . ? N8 C40 1.125(10) . ? N8 Ag1 2.102(6) 1_545 ? C1 C2 1.428(11) . ? C2 C3 1.392(11) . ? C2 C7 1.401(12) . ? C3 C4 1.379(11) . ? C4 C5 1.397(12) . ? C5 C6 1.391(10) . ? C6 C7 1.364(11) . ? C8 C9 1.527(10) . ? C8 C13 1.553(12) . ? C9 C10 1.511(11) . ? C10 C11 1.518(14) . ? C11 C12 1.503(10) . ? C12 C13 1.525(10) . ? C14 C15 1.397(10) . ? C14 C19 1.393(11) . ? C15 C16 1.369(11) . ? C16 C17 1.390(12) . ? C17 C18 1.376(11) . ? C17 C20 1.439(11) . ? C18 C19 1.384(10) . ? C21 C22 1.423(11) . ? C22 C23 1.391(11) . ? C22 C27 1.405(12) . ? C23 C24 1.365(10) . ? C24 C25 1.397(11) . ? C25 C26 1.397(10) . ? C26 C27 1.365(10) . ? C28 C33 1.527(12) . ? C28 C29 1.528(10) . ? C29 C30 1.527(10) . ? C30 C31 1.507(13) . ? C31 C32 1.512(10) . ? C32 C33 1.500(10) . ? C34 C35 1.390(11) . ? C34 C39 1.387(10) . ? C35 C36 1.374(10) . ? C36 C37 1.362(11) . ? C37 C38 1.429(12) . ? C37 C40 1.430(11) . ? C38 C39 1.361(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Ag1 N1 163.4(4) 1_565 . ? N5 Ag2 N4 169.9(4) . . ? O7 Cl1 O3 106.2(7) . . ? O7 Cl1 O1 115.5(8) . . ? O3 Cl1 O1 108.7(5) . . ? O7 Cl1 O2 106.5(8) . . ? O3 Cl1 O2 113.2(7) . . ? O1 Cl1 O2 106.8(7) . . ? O8 Cl2 O4 101.7(10) . . ? O8 Cl2 O5 116.3(8) . . ? O4 Cl2 O5 106.1(8) . . ? O8 Cl2 O6 106.2(6) . . ? O4 Cl2 O6 115.3(8) . . ? O5 Cl2 O6 111.3(5) . . ? C1 N1 Ag1 163.9(7) . . ? C5 N2 C8 124.8(7) . . ? C14 N3 C13 126.8(6) . . ? C20 N4 Ag2 165.9(8) . . ? C21 N5 Ag2 166.1(7) . . ? C25 N6 C28 127.1(7) . . ? C34 N7 C33 125.7(7) . . ? C40 N8 Ag1 167.6(8) . 1_545 ? N1 C1 C2 178.5(10) . . ? C3 C2 C7 119.6(7) . . ? C3 C2 C1 121.4(8) . . ? C7 C2 C1 119.0(8) . . ? C4 C3 C2 120.3(8) . . ? C3 C4 C5 120.5(8) . . ? N2 C5 C6 119.0(7) . . ? N2 C5 C4 122.9(7) . . ? C6 C5 C4 118.0(8) . . ? C7 C6 C5 122.4(8) . . ? C6 C7 C2 119.1(8) . . ? N2 C8 C9 109.7(6) . . ? N2 C8 C13 111.3(6) . . ? C9 C8 C13 110.8(6) . . ? C8 C9 C10 112.4(7) . . ? C9 C10 C11 111.4(7) . . ? C12 C11 C10 111.7(7) . . ? C11 C12 C13 112.0(7) . . ? N3 C13 C12 110.5(6) . . ? N3 C13 C8 110.6(6) . . ? C12 C13 C8 110.7(6) . . ? N3 C14 C15 118.2(7) . . ? N3 C14 C19 123.6(7) . . ? C15 C14 C19 118.1(7) . . ? C16 C15 C14 121.9(8) . . ? C15 C16 C17 118.8(7) . . ? C18 C17 C16 120.7(7) . . ? C18 C17 C20 120.3(8) . . ? C16 C17 C20 119.0(8) . . ? C19 C18 C17 120.0(8) . . ? C18 C19 C14 120.4(7) . . ? N4 C20 C17 177.1(10) . . ? N5 C21 C22 179.1(9) . . ? C23 C22 C27 118.8(7) . . ? C23 C22 C21 122.6(8) . . ? C27 C22 C21 118.5(8) . . ? C24 C23 C22 120.8(8) . . ? C23 C24 C25 121.3(7) . . ? N6 C25 C26 118.6(7) . . ? N6 C25 C24 124.2(7) . . ? C26 C25 C24 117.2(7) . . ? C27 C26 C25 122.4(8) . . ? C26 C27 C22 119.4(8) . . ? N6 C28 C33 111.6(6) . . ? N6 C28 C29 108.5(6) . . ? C33 C28 C29 111.5(6) . . ? C28 C29 C30 110.8(7) . . ? C31 C30 C29 111.4(7) . . ? C30 C31 C32 111.7(7) . . ? C33 C32 C31 112.9(7) . . ? N7 C33 C32 110.9(7) . . ? N7 C33 C28 110.8(6) . . ? C32 C33 C28 110.9(7) . . ? N7 C34 C35 123.9(7) . . ? N7 C34 C39 119.0(7) . . ? C35 C34 C39 117.1(7) . . ? C36 C35 C34 121.0(8) . . ? C37 C36 C35 121.2(8) . . ? C36 C37 C38 119.4(8) . . ? C36 C37 C40 122.8(8) . . ? C38 C37 C40 117.8(7) . . ? C39 C38 C37 117.6(7) . . ? C38 C39 C34 123.7(8) . . ? N8 C40 C37 178.4(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.78 _refine_diff_density_min -0.57 _refine_diff_density_rms 0.06 #===END