# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'S.Chowdhury' 'P.B.Iveson' 'M.G.B.Drew' 'D.A.Tocher ' 'D.Datta' _publ_contact_author_name 'Dr Dipankar Datta' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICDD@MAHENDRA.IACS.RES.IN' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; A novel copper(I) complex which is a monomeric single helix in solid state but a dimeric double helix in solution. New aspects of self-processes ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; data_1 _database_code_CSD 157534 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28.5 H25 Cl2 Cu N6 O4 ' _chemical_formula_weight 649.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.32(3) _cell_length_b 20.70(3) _cell_length_c 18.71(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.190(10) _cell_angle_gamma 90.00 _cell_volume 5900(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_type 'DIFABS (Walker and Stuart,1983)' _exptl_absorpt_correction_T_min 0.412 _exptl_absorpt_correction_T_max 1.000 _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10667 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1648 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.07 _reflns_number_total 10667 _reflns_number_gt 4361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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^)+(0.1147P)^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_number_reflns 10667 _refine_ls_number_parameters 732 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.2344 _refine_ls_R_factor_gt 0.0907 _refine_ls_wR_factor_ref 0.2517 _refine_ls_wR_factor_gt 0.1916 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.257 _refine_ls_shift/su_mean 0.010 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 0.20716(7) 0.65630(5) 0.28058(6) 0.0592(4) Uani 1 d . . . C1A C 0.3558(7) 0.5826(5) 0.4707(7) 0.104(4) Uani 1 d . . . H1A1 H 0.4136 0.5953 0.4609 0.125 Uiso 1 calc R . . H1A2 H 0.3546 0.5369 0.4788 0.125 Uiso 1 calc R . . H1A3 H 0.3408 0.6049 0.5126 0.125 Uiso 1 calc R . . C2A C 0.2921(5) 0.5993(4) 0.4088(5) 0.051(2) Uani 1 d . . . N3A N 0.2907(4) 0.6558(3) 0.3779(4) 0.0467(17) Uani 1 d . . . N4A N 0.3531(4) 0.7004(3) 0.3996(4) 0.0536(19) Uani 1 d . . . C5A C 0.3279(5) 0.7579(4) 0.4151(4) 0.0420(19) Uani 1 d . . . C6A C 0.2357(5) 0.7798(3) 0.4158(5) 0.042(2) Uani 1 d . . . N7A N 0.1769(4) 0.7817(3) 0.3608(4) 0.0474(17) Uani 1 d . . . N8A N 0.1987(4) 0.7545(3) 0.2979(4) 0.0468(17) Uani 1 d . . . C9A C 0.2174(5) 0.7905(4) 0.2440(5) 0.045(2) Uani 1 d . . . C10A C 0.2226(7) 0.8624(4) 0.2484(6) 0.082(3) Uani 1 d . . . H10A H 0.2020 0.8767 0.2924 0.098 Uiso 1 calc R . . H10B H 0.1868 0.8810 0.2083 0.098 Uiso 1 calc R . . H10C H 0.2824 0.8758 0.2472 0.098 Uiso 1 calc R . . C91A C 0.2326(5) 0.7548(4) 0.1778(5) 0.050(2) Uani 1 d . . . C96A C 0.2507(5) 0.7849(4) 0.1156(5) 0.055(2) Uani 1 d . . . H96A H 0.2554 0.8296 0.1137 0.066 Uiso 1 calc R . . C95A C 0.2616(6) 0.7477(5) 0.0559(6) 0.072(3) Uani 1 d . . . H95A H 0.2730 0.7679 0.0136 0.087 Uiso 1 calc R . . C94A C 0.2561(6) 0.6823(5) 0.0579(6) 0.072(3) Uani 1 d . . . H94A H 0.2626 0.6570 0.0178 0.086 Uiso 1 calc R . . C93A C 0.2399(5) 0.6551(5) 0.1241(6) 0.068(3) Uani 1 d . . . H93A H 0.2358 0.6104 0.1269 0.082 Uiso 1 calc R . . N92A N 0.2303(4) 0.6894(3) 0.1833(4) 0.0544(19) Uani 1 d . . . C21A C 0.2246(5) 0.5527(4) 0.3782(5) 0.049(2) Uani 1 d . . . C26A C 0.2148(6) 0.4929(4) 0.4074(5) 0.065(3) Uani 1 d . . . H26A H 0.2530 0.4796 0.4467 0.078 Uiso 1 calc R . . C25A C 0.1473(7) 0.4513(5) 0.3786(7) 0.085(3) Uani 1 d . . . H25A H 0.1392 0.4109 0.3986 0.102 Uiso 1 calc R . . C24A C 0.0939(7) 0.4729(5) 0.3197(6) 0.075(3) Uani 1 d . . . H24A H 0.0479 0.4470 0.2998 0.091 Uiso 1 calc R . . C23A C 0.1078(6) 0.5328(4) 0.2896(6) 0.066(3) Uani 1 d . . . H23A H 0.0724 0.5461 0.2488 0.080 Uiso 1 calc R . . N22A N 0.1734(4) 0.5725(3) 0.3196(4) 0.0509(18) Uani 1 d . . . C51A C 0.3977(5) 0.8060(4) 0.4320(5) 0.049(2) Uani 1 d . . . C52A C 0.4867(5) 0.7872(4) 0.4474(5) 0.057(2) Uani 1 d . . . H52A H 0.5017 0.7436 0.4479 0.069 Uiso 1 calc R . . C53A C 0.5526(6) 0.8343(5) 0.4618(6) 0.085(3) Uani 1 d . . . H53A H 0.6106 0.8214 0.4730 0.102 Uiso 1 calc R . . C54A C 0.5325(6) 0.8985(5) 0.4594(6) 0.078(3) Uani 1 d . . . H54A H 0.5765 0.9293 0.4686 0.094 Uiso 1 calc R . . C55A C 0.4479(7) 0.9170(5) 0.4435(6) 0.084(3) Uani 1 d . . . H55A H 0.4340 0.9608 0.4428 0.101 Uiso 1 calc R . . C56A C 0.3813(5) 0.8716(4) 0.4282(6) 0.071(3) Uani 1 d . . . H56A H 0.3243 0.8858 0.4150 0.085 Uiso 1 calc R . . C61A C 0.2080(4) 0.8054(4) 0.4826(5) 0.045(2) Uani 1 d . . . C62A C 0.1379(5) 0.8502(4) 0.4831(5) 0.054(2) Uani 1 d . . . H62A H 0.1093 0.8651 0.4399 0.065 Uiso 1 calc R . . C63A C 0.1114(6) 0.8722(4) 0.5485(7) 0.075(3) Uani 1 d . . . H63A H 0.0664 0.9023 0.5483 0.090 Uiso 1 calc R . . C64A C 0.1514(7) 0.8494(5) 0.6123(7) 0.078(3) Uani 1 d . . . H64A H 0.1326 0.8638 0.6552 0.094 Uiso 1 calc R . . C65A C 0.2180(6) 0.8061(5) 0.6140(6) 0.077(3) Uani 1 d . . . H65A H 0.2452 0.7918 0.6579 0.092 Uiso 1 calc R . . C66A C 0.2462(6) 0.7828(4) 0.5497(6) 0.064(3) Uani 1 d . . . H66A H 0.2906 0.7520 0.5516 0.077 Uiso 1 calc R . . Cu2 Cu 0.52610(7) 0.67867(5) 1.03190(7) 0.0591(4) Uani 1 d . . . C1B C 0.3890(6) 0.5962(5) 0.8384(6) 0.079(3) Uani 1 d . . . H1B1 H 0.3661 0.5535 0.8440 0.095 Uiso 1 calc R . . H1B2 H 0.4234 0.5968 0.7984 0.095 Uiso 1 calc R . . H1B3 H 0.3413 0.6262 0.8298 0.095 Uiso 1 calc R . . C2B C 0.4451(5) 0.6149(4) 0.9050(5) 0.045(2) Uani 1 d . . . N3B N 0.4367(4) 0.6679(3) 0.9378(4) 0.0481(17) Uani 1 d . . . N4B N 0.3702(4) 0.7106(3) 0.9141(4) 0.0464(17) Uani 1 d . . . C5B C 0.3938(4) 0.7659(4) 0.8896(4) 0.042(2) Uani 1 d . . . C6B C 0.4888(5) 0.7834(3) 0.8780(5) 0.047(2) Uani 1 d . . . N7B N 0.5496(4) 0.7909(3) 0.9305(4) 0.0513(18) Uani 1 d . . . N8B N 0.5324(4) 0.7746(3) 0.9973(4) 0.0470(17) Uani 1 d . . . C9B C 0.5204(5) 0.8173(4) 1.0456(5) 0.048(2) Uani 1 d . . . C10B C 0.5190(6) 0.8883(4) 1.0306(5) 0.073(3) Uani 1 d . . . H10D H 0.5490 0.8967 0.9891 0.088 Uiso 1 calc R . . H10E H 0.5479 0.9108 1.0713 0.088 Uiso 1 calc R . . H10F H 0.4593 0.9028 1.0218 0.088 Uiso 1 calc R . . N92B N 0.5051(4) 0.7250(3) 1.1220(4) 0.0526(18) Uani 1 d . . . C93B C 0.4881(5) 0.6986(5) 1.1836(6) 0.067(3) Uani 1 d . . . H93B H 0.4854 0.6538 1.1868 0.080 Uiso 1 calc R . . C94B C 0.4740(6) 0.7357(6) 1.2441(6) 0.078(3) Uani 1 d . . . H94B H 0.4643 0.7161 1.2873 0.094 Uiso 1 calc R . . C95B C 0.4749(6) 0.8005(5) 1.2376(6) 0.067(3) Uani 1 d . . . H95B H 0.4661 0.8259 1.2772 0.081 Uiso 1 calc R . . C96B C 0.4885(5) 0.8302(4) 1.1739(5) 0.059(2) Uani 1 d . . . H96B H 0.4864 0.8749 1.1693 0.071 Uiso 1 calc R . . C91B C 0.5053(5) 0.7908(4) 1.1164(5) 0.047(2) Uani 1 d . . . C21B C 0.5182(5) 0.5730(3) 0.9359(5) 0.047(2) Uani 1 d . . . N22B N 0.5696(4) 0.5963(3) 0.9930(4) 0.0530(19) Uani 1 d . . . C23B C 0.6392(6) 0.5622(4) 1.0213(6) 0.064(3) Uani 1 d . . . H23B H 0.6733 0.5783 1.0614 0.077 Uiso 1 calc R . . C24B C 0.6619(6) 0.5034(4) 0.9926(6) 0.066(3) Uani 1 d . . . H24B H 0.7120 0.4813 1.0117 0.079 Uiso 1 calc R . . C25B C 0.6087(6) 0.4786(4) 0.9353(6) 0.064(3) Uani 1 d . . . H25B H 0.6216 0.4383 0.9169 0.077 Uiso 1 calc R . . C26B C 0.5353(5) 0.5127(4) 0.9040(5) 0.055(2) Uani 1 d . . . H26B H 0.4999 0.4968 0.8644 0.066 Uiso 1 calc R . . C51B C 0.3272(5) 0.8138(4) 0.8655(4) 0.048(2) Uani 1 d . . . C52B C 0.3477(6) 0.8784(4) 0.8567(5) 0.064(3) Uani 1 d . . . H52B H 0.4054 0.8921 0.8673 0.077 Uiso 1 calc R . . C53B C 0.2833(7) 0.9231(5) 0.8322(6) 0.077(3) Uani 1 d . . . H53B H 0.2978 0.9662 0.8258 0.092 Uiso 1 calc R . . C55B C 0.1747(6) 0.8408(6) 0.8271(6) 0.080(3) Uani 1 d . . . H55B H 0.1162 0.8283 0.8180 0.096 Uiso 1 calc R . . C54B C 0.1975(7) 0.9023(5) 0.8175(6) 0.082(3) Uani 1 d . . . H54B H 0.1545 0.9319 0.8005 0.098 Uiso 1 calc R . . C56B C 0.2385(5) 0.7954(4) 0.8508(5) 0.060(2) Uani 1 d . . . H56B H 0.2224 0.7526 0.8569 0.072 Uiso 1 calc R . . C61B C 0.5077(5) 0.7953(4) 0.8030(5) 0.050(2) Uani 1 d . . . C62B C 0.4609(6) 0.7656(5) 0.7468(6) 0.073(3) Uani 1 d . . . H62B H 0.4146 0.7384 0.7550 0.087 Uiso 1 calc R . . C63B C 0.4813(8) 0.7754(6) 0.6769(6) 0.092(3) Uani 1 d . . . H63B H 0.4475 0.7567 0.6381 0.111 Uiso 1 calc R . . C64B C 0.5524(9) 0.8132(6) 0.6665(7) 0.097(4) Uani 1 d . . . H64B H 0.5687 0.8180 0.6203 0.117 Uiso 1 calc R . . C65B C 0.5980(8) 0.8429(6) 0.7201(8) 0.092(4) Uani 1 d . . . H65B H 0.6429 0.8711 0.7113 0.110 Uiso 1 calc R . . C66B C 0.5788(6) 0.8320(4) 0.7913(6) 0.070(3) Uani 1 d . . . H66B H 0.6143 0.8496 0.8298 0.084 Uiso 1 calc R . . Cl4 Cl 0.4793(2) 0.53217(16) 1.3002(2) 0.1073(11) Uani 0.547(10) d PD A 1 O43 O 0.5118(10) 0.5349(9) 1.3765(7) 0.143(2) Uiso 0.547(10) d PD A 1 O44 O 0.4790(11) 0.4581(6) 1.2864(10) 0.143(2) Uiso 0.547(10) d PD A 1 O41 O 0.3950(9) 0.5566(8) 1.2783(10) 0.143(2) Uiso 0.547(10) d PD A 1 O42 O 0.5453(11) 0.5539(8) 1.2548(10) 0.143(2) Uiso 0.547(10) d PD A 1 Cl6 Cl 0.4793(2) 0.53217(16) 1.3002(2) 0.1073(11) Uani 0.453(10) d PD A 2 O61 O 0.4963(12) 0.5916(8) 1.3437(10) 0.143(2) Uiso 0.453(10) d PD A 2 O62 O 0.4657(13) 0.4754(8) 1.3335(11) 0.143(2) Uiso 0.453(10) d PD A 2 O63 O 0.3995(11) 0.5520(10) 1.2452(10) 0.143(2) Uiso 0.453(10) d PD A 2 O64 O 0.5509(12) 0.5305(10) 1.2524(11) 0.143(2) Uiso 0.453(10) d PD A 2 Cl5 Cl -0.13619(15) 0.50307(12) 0.14501(17) 0.0804(8) Uani 0.368(7) d PD B 1 O51 O -0.2029(10) 0.4546(8) 0.1421(12) 0.1022(16) Uiso 0.368(7) d PD B 1 O53 O -0.0517(10) 0.4825(9) 0.1221(11) 0.1022(16) Uiso 0.368(7) d PD B 1 O54 O -0.166(2) 0.5614(9) 0.1063(14) 0.1022(16) Uiso 0.368(7) d PD B 1 O52 O -0.1149(12) 0.5217(9) 0.2245(8) 0.1022(16) Uiso 0.368(7) d PD B 1 Cl7 Cl -0.13619(15) 0.50307(12) 0.14501(17) 0.0804(8) Uani 0.632(7) d PD B 2 O71 O -0.1634(7) 0.4489(5) 0.0909(6) 0.1022(16) Uiso 0.632(7) d PD B 2 O72 O -0.1835(7) 0.4877(5) 0.2053(6) 0.1022(16) Uiso 0.632(7) d PD B 2 O73 O -0.0434(6) 0.4995(6) 0.1593(7) 0.1022(16) Uiso 0.632(7) d PD B 2 O74 O -0.1642(12) 0.5642(6) 0.1139(9) 0.1022(16) Uiso 0.632(7) d PD B 2 C91 C 0.7010(10) 0.4495(6) 1.3322(9) 0.152(6) Uani 1 d . C 1 H91A H 0.7172 0.4555 1.2840 0.182 Uiso 1 calc R C 1 H91B H 0.6479 0.4742 1.3366 0.182 Uiso 1 calc R C 1 Cl92 Cl 0.7816(4) 0.4756(3) 1.3923(3) 0.215(3) Uani 1 d . C 1 Cl93 Cl 0.6814(4) 0.3652(2) 1.3480(3) 0.191(2) Uani 1 d . C 1 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 0.0606(7) 0.0546(6) 0.0632(9) 0.0051(6) 0.0104(6) -0.0002(5) C1A 0.097(8) 0.090(8) 0.122(12) 0.009(7) -0.009(8) 0.001(6) C2A 0.035(5) 0.062(6) 0.056(6) 0.008(5) 0.003(4) 0.019(4) N3A 0.039(4) 0.045(4) 0.056(5) -0.004(4) 0.004(3) 0.005(3) N4A 0.039(4) 0.048(4) 0.074(6) -0.005(4) 0.007(4) 0.001(3) C5A 0.041(5) 0.047(5) 0.038(5) -0.002(4) 0.004(4) 0.002(4) C6A 0.037(5) 0.045(4) 0.045(6) 0.000(4) 0.013(4) 0.003(3) N7A 0.040(4) 0.046(4) 0.056(6) -0.001(4) 0.009(4) 0.004(3) N8A 0.039(4) 0.047(4) 0.055(5) -0.004(4) 0.010(4) -0.001(3) C9A 0.035(4) 0.054(5) 0.045(6) 0.004(5) -0.002(4) 0.006(3) C10A 0.108(8) 0.059(6) 0.081(9) 0.001(5) 0.026(7) 0.008(5) C91A 0.040(5) 0.053(5) 0.056(7) 0.010(5) 0.000(4) 0.004(4) C96A 0.054(5) 0.051(5) 0.059(7) 0.011(5) 0.006(5) 0.010(4) C95A 0.060(6) 0.083(7) 0.078(9) 0.019(6) 0.026(6) 0.012(5) C94A 0.063(6) 0.092(8) 0.062(8) -0.002(6) 0.014(5) 0.009(5) C93A 0.056(6) 0.071(6) 0.080(8) -0.010(6) 0.017(5) 0.007(4) N92A 0.042(4) 0.056(5) 0.068(6) -0.001(4) 0.014(4) 0.008(3) C21A 0.041(5) 0.041(5) 0.067(7) 0.005(4) 0.021(5) 0.001(4) C26A 0.063(6) 0.055(6) 0.074(8) 0.015(5) -0.006(5) 0.013(5) C25A 0.089(8) 0.056(6) 0.111(11) 0.010(7) 0.018(8) -0.002(6) C24A 0.083(7) 0.059(6) 0.085(9) -0.002(6) 0.008(7) -0.007(5) C23A 0.064(6) 0.071(6) 0.064(8) 0.002(5) 0.004(5) -0.003(5) N22A 0.047(4) 0.055(4) 0.051(5) 0.004(4) 0.009(4) 0.001(3) C51A 0.038(5) 0.054(5) 0.057(6) -0.006(4) 0.014(4) 0.005(4) C52A 0.048(5) 0.059(5) 0.064(7) -0.001(5) 0.002(5) 0.003(4) C53A 0.042(6) 0.104(9) 0.114(10) -0.021(7) 0.021(6) -0.002(5) C54A 0.049(6) 0.078(7) 0.112(10) -0.023(6) 0.032(6) -0.026(5) C55A 0.067(7) 0.059(6) 0.126(11) -0.012(6) 0.012(7) -0.015(5) C56A 0.041(5) 0.067(6) 0.107(9) -0.010(6) 0.014(5) 0.003(4) C61A 0.026(4) 0.049(5) 0.060(7) 0.000(4) 0.001(4) -0.003(3) C62A 0.044(5) 0.060(5) 0.056(7) -0.007(5) -0.004(4) -0.008(4) C63A 0.054(6) 0.063(6) 0.112(11) -0.024(7) 0.026(7) -0.002(4) C64A 0.076(7) 0.099(8) 0.064(8) -0.014(7) 0.027(6) 0.007(6) C65A 0.071(7) 0.077(7) 0.083(9) -0.009(6) 0.007(6) -0.006(5) C66A 0.056(6) 0.064(6) 0.074(8) 0.000(6) 0.013(6) 0.005(4) Cu2 0.0614(7) 0.0534(6) 0.0619(9) -0.0065(6) 0.0044(6) -0.0002(5) C1B 0.080(7) 0.082(7) 0.073(8) -0.011(6) -0.002(6) 0.018(5) C2B 0.044(5) 0.046(5) 0.043(6) 0.002(4) 0.003(4) -0.003(4) N3B 0.048(4) 0.045(4) 0.052(5) 0.011(4) 0.010(3) -0.002(3) N4B 0.045(4) 0.046(4) 0.048(5) 0.003(3) 0.003(3) 0.001(3) C5B 0.029(4) 0.051(5) 0.046(6) -0.005(4) 0.011(4) 0.005(3) C6B 0.047(5) 0.039(4) 0.055(7) -0.007(4) 0.005(5) 0.005(4) N7B 0.059(5) 0.043(4) 0.054(6) -0.009(4) 0.014(4) -0.006(3) N8B 0.041(4) 0.051(4) 0.050(5) 0.005(4) 0.005(3) -0.002(3) C9B 0.040(4) 0.042(4) 0.061(7) -0.012(5) 0.006(4) -0.006(3) C10B 0.096(7) 0.057(6) 0.069(8) -0.003(5) 0.018(6) 0.006(5) N92B 0.047(4) 0.061(5) 0.048(5) -0.010(4) 0.003(4) -0.004(3) C93B 0.057(6) 0.064(6) 0.079(9) 0.010(6) 0.006(6) -0.008(4) C94B 0.062(6) 0.111(9) 0.061(8) -0.001(7) 0.005(5) -0.008(6) C95B 0.061(6) 0.074(7) 0.066(8) -0.012(6) 0.005(5) 0.012(5) C96B 0.052(5) 0.065(6) 0.058(7) -0.003(5) -0.003(5) 0.004(4) C91B 0.038(5) 0.050(5) 0.054(7) -0.008(5) 0.008(4) 0.000(4) C21B 0.052(5) 0.039(5) 0.052(7) -0.004(4) 0.018(5) -0.010(4) N22B 0.053(4) 0.043(4) 0.064(6) 0.001(4) 0.013(4) 0.003(3) C23B 0.057(6) 0.053(5) 0.081(8) -0.005(5) 0.007(5) 0.006(4) C24B 0.049(5) 0.070(6) 0.077(8) 0.012(6) 0.003(5) 0.008(5) C25B 0.069(6) 0.060(6) 0.066(8) -0.001(5) 0.016(6) 0.025(5) C26B 0.055(5) 0.061(5) 0.051(6) 0.000(5) 0.013(5) -0.009(4) C51B 0.048(5) 0.057(5) 0.040(6) 0.006(4) 0.012(4) 0.004(4) C52B 0.061(6) 0.065(6) 0.067(7) 0.005(5) 0.015(5) 0.004(5) C53B 0.076(7) 0.067(6) 0.087(9) 0.007(6) 0.010(6) 0.019(5) C55B 0.058(6) 0.096(8) 0.084(9) 0.002(7) -0.001(6) 0.019(6) C54B 0.084(8) 0.077(8) 0.084(9) 0.010(6) 0.012(7) 0.037(6) C56B 0.055(6) 0.063(6) 0.064(7) 0.006(5) 0.008(5) 0.009(5) C61B 0.041(5) 0.054(5) 0.055(7) 0.002(5) 0.014(5) 0.005(4) C62B 0.060(6) 0.091(7) 0.069(8) 0.002(6) 0.016(6) 0.001(5) C63B 0.115(10) 0.116(9) 0.046(8) 0.000(7) 0.015(7) 0.017(7) C64B 0.102(10) 0.116(10) 0.079(10) 0.031(8) 0.034(8) 0.006(8) C65B 0.087(8) 0.098(8) 0.094(11) 0.013(8) 0.026(8) -0.014(6) C66B 0.079(7) 0.062(6) 0.071(8) 0.012(5) 0.024(6) -0.001(5) Cl4 0.106(2) 0.119(3) 0.102(3) -0.040(2) 0.031(2) -0.0291(18) Cl6 0.106(2) 0.119(3) 0.102(3) -0.040(2) 0.031(2) -0.0291(18) Cl5 0.0610(15) 0.0782(17) 0.102(2) 0.0110(15) 0.0107(15) 0.0036(12) Cl7 0.0610(15) 0.0782(17) 0.102(2) 0.0110(15) 0.0107(15) 0.0036(12) C91 0.154(13) 0.132(12) 0.150(16) 0.007(11) -0.075(12) 0.003(10) Cl92 0.223(6) 0.245(6) 0.179(6) -0.050(5) 0.029(5) -0.091(5) Cl93 0.283(6) 0.151(4) 0.142(4) -0.009(3) 0.032(4) -0.047(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 Cu1 N22A 1.973(7) . ? Cu1 N92A 2.012(8) . ? Cu1 N8A 2.064(7) . ? Cu1 N3A 2.110(7) . ? C1A C2A 1.473(13) . ? C2A N3A 1.304(10) . ? C2A C21A 1.483(12) . ? N3A N4A 1.359(9) . ? N4A C5A 1.293(9) . ? C5A C51A 1.471(11) . ? C5A C6A 1.485(10) . ? C6A N7A 1.294(10) . ? C6A C61A 1.461(11) . ? N7A N8A 1.377(9) . ? N8A C9A 1.310(10) . ? C9A C91A 1.483(11) . ? C9A C10A 1.493(11) . ? C91A N92A 1.358(10) . ? C91A C96A 1.373(11) . ? C96A C95A 1.382(12) . ? C95A C94A 1.356(12) . ? C94A C93A 1.407(13) . ? C93A N92A 1.337(11) . ? C21A N22A 1.341(11) . ? C21A C26A 1.370(11) . ? C26A C25A 1.407(13) . ? C25A C24A 1.375(14) . ? C24A C23A 1.388(12) . ? C23A N22A 1.369(11) . ? C51A C56A 1.380(11) . ? C51A C52A 1.418(11) . ? C52A C53A 1.408(12) . ? C53A C54A 1.365(12) . ? C54A C55A 1.353(13) . ? C55A C56A 1.395(12) . ? C61A C66A 1.407(12) . ? C61A C62A 1.420(10) . ? C62A C63A 1.406(13) . ? C63A C64A 1.365(14) . ? C64A C65A 1.356(13) . ? C65A C66A 1.407(13) . ? Cu2 N22B 1.995(7) . ? Cu2 N92B 1.995(7) . ? Cu2 N8B 2.093(7) . ? Cu2 N3B 2.123(8) . ? C1B C2B 1.488(12) . ? C2B N3B 1.270(9) . ? C2B C21B 1.483(11) . ? N3B N4B 1.386(8) . ? N4B C5B 1.299(9) . ? C5B C51B 1.458(11) . ? C5B C6B 1.538(11) . ? C6B N7B 1.287(10) . ? C6B C61B 1.484(12) . ? N7B N8B 1.348(9) . ? N8B C9B 1.292(10) . ? C9B C91B 1.474(12) . ? C9B C10B 1.495(11) . ? N92B C93B 1.327(11) . ? N92B C91B 1.367(10) . ? C93B C94B 1.403(13) . ? C94B C95B 1.348(13) . ? C95B C96B 1.378(13) . ? C96B C91B 1.395(11) . ? C21B N22B 1.348(10) . ? C21B C26B 1.420(11) . ? N22B C23B 1.340(10) . ? C23B C24B 1.390(12) . ? C24B C25B 1.375(13) . ? C25B C26B 1.401(12) . ? C51B C52B 1.387(11) . ? C51B C56B 1.410(11) . ? C52B C53B 1.394(12) . ? C53B C54B 1.382(14) . ? C55B C54B 1.337(13) . ? C55B C56B 1.394(12) . ? C61B C62B 1.356(13) . ? C61B C66B 1.365(11) . ? C62B C63B 1.392(13) . ? C63B C64B 1.374(15) . ? C64B C65B 1.312(15) . ? C65B C66B 1.413(15) . ? Cl4 O41 1.406(12) . ? Cl4 O43 1.462(12) . ? Cl4 O42 1.460(12) . ? Cl4 O44 1.555(12) . ? Cl6 O62 1.356(13) . ? Cl6 O61 1.483(13) . ? Cl6 O64 1.490(13) . ? Cl6 O63 1.566(13) . ? Cl5 O51 1.429(12) . ? Cl5 O54 1.457(13) . ? Cl5 O53 1.470(13) . ? Cl5 O52 1.538(13) . ? Cl7 O73 1.421(10) . ? Cl7 O74 1.439(10) . ? Cl7 O72 1.442(9) . ? Cl7 O71 1.537(10) . ? C91 Cl92 1.667(14) . ? C91 Cl93 1.800(14) . ? 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 N22A Cu1 N92A 135.5(3) . . ? N22A Cu1 N8A 141.6(3) . . ? N92A Cu1 N8A 80.1(3) . . ? N22A Cu1 N3A 80.5(3) . . ? N92A Cu1 N3A 129.3(3) . . ? N8A Cu1 N3A 84.9(3) . . ? N3A C2A C1A 122.4(8) . . ? N3A C2A C21A 115.7(8) . . ? C1A C2A C21A 121.8(8) . . ? C2A N3A N4A 120.0(7) . . ? C2A N3A Cu1 111.5(5) . . ? N4A N3A Cu1 126.6(5) . . ? C5A N4A N3A 118.3(6) . . ? N4A C5A C51A 116.3(7) . . ? N4A C5A C6A 126.2(7) . . ? C51A C5A C6A 117.5(6) . . ? N7A C6A C61A 115.3(7) . . ? N7A C6A C5A 125.7(7) . . ? C61A C6A C5A 118.9(8) . . ? C6A N7A N8A 117.0(6) . . ? C9A N8A N7A 121.2(6) . . ? C9A N8A Cu1 114.5(5) . . ? N7A N8A Cu1 124.2(5) . . ? N8A C9A C91A 115.3(7) . . ? N8A C9A C10A 122.7(8) . . ? C91A C9A C10A 122.0(8) . . ? N92A C91A C96A 121.7(8) . . ? N92A C91A C9A 115.1(8) . . ? C96A C91A C9A 123.1(8) . . ? C91A C96A C95A 119.0(8) . . ? C94A C95A C96A 121.4(9) . . ? C95A C94A C93A 116.1(10) . . ? N92A C93A C94A 124.3(9) . . ? C93A N92A C91A 117.4(8) . . ? C93A N92A Cu1 127.9(6) . . ? C91A N92A Cu1 114.6(6) . . ? N22A C21A C26A 121.5(8) . . ? N22A C21A C2A 116.1(7) . . ? C26A C21A C2A 122.4(9) . . ? C21A C26A C25A 120.5(9) . . ? C24A C25A C26A 117.2(10) . . ? C25A C24A C23A 120.8(10) . . ? N22A C23A C24A 120.5(10) . . ? C21A N22A C23A 119.4(7) . . ? C21A N22A Cu1 114.6(5) . . ? C23A N22A Cu1 125.9(7) . . ? C56A C51A C52A 116.5(7) . . ? C56A C51A C5A 122.1(7) . . ? C52A C51A C5A 121.2(7) . . ? C53A C52A C51A 120.1(8) . . ? C54A C53A C52A 120.9(9) . . ? C55A C54A C53A 119.3(8) . . ? C54A C55A C56A 121.1(9) . . ? C51A C56A C55A 121.8(8) . . ? C66A C61A C62A 116.9(8) . . ? C66A C61A C6A 120.8(7) . . ? C62A C61A C6A 122.2(8) . . ? C63A C62A C61A 120.5(9) . . ? C64A C63A C62A 120.3(9) . . ? C65A C64A C63A 121.0(10) . . ? C64A C65A C66A 120.4(11) . . ? C65A C66A C61A 120.9(9) . . ? N22B Cu2 N92B 144.0(3) . . ? N22B Cu2 N8B 131.9(3) . . ? N92B Cu2 N8B 79.8(3) . . ? N22B Cu2 N3B 79.6(3) . . ? N92B Cu2 N3B 127.1(3) . . ? N8B Cu2 N3B 83.7(3) . . ? N3B C2B C21B 115.4(8) . . ? N3B C2B C1B 123.4(7) . . ? C21B C2B C1B 121.2(8) . . ? C2B N3B N4B 120.4(7) . . ? C2B N3B Cu2 113.7(5) . . ? N4B N3B Cu2 125.8(5) . . ? C5B N4B N3B 116.9(6) . . ? N4B C5B C51B 119.7(6) . . ? N4B C5B C6B 124.1(6) . . ? C51B C5B C6B 116.0(7) . . ? N7B C6B C61B 120.1(8) . . ? N7B C6B C5B 122.6(8) . . ? C61B C6B C5B 117.2(8) . . ? C6B N7B N8B 118.6(7) . . ? C9B N8B N7B 122.3(7) . . ? C9B N8B Cu2 114.7(6) . . ? N7B N8B Cu2 123.0(5) . . ? N8B C9B C91B 115.0(7) . . ? N8B C9B C10B 122.8(8) . . ? C91B C9B C10B 122.2(7) . . ? C93B N92B C91B 118.7(8) . . ? C93B N92B Cu2 127.0(7) . . ? C91B N92B Cu2 114.3(6) . . ? N92B C93B C94B 122.5(9) . . ? C95B C94B C93B 118.0(10) . . ? C94B C95B C96B 121.7(10) . . ? C95B C96B C91B 117.7(9) . . ? N92B C91B C96B 121.4(8) . . ? N92B C91B C9B 116.2(7) . . ? C96B C91B C9B 122.3(8) . . ? N22B C21B C26B 122.0(8) . . ? N22B C21B C2B 116.8(7) . . ? C26B C21B C2B 121.1(8) . . ? C23B N22B C21B 119.8(7) . . ? C23B N22B Cu2 126.1(7) . . ? C21B N22B Cu2 113.9(5) . . ? N22B C23B C24B 122.1(9) . . ? C25B C24B C23B 118.4(8) . . ? C24B C25B C26B 121.3(8) . . ? C25B C26B C21B 116.4(8) . . ? C52B C51B C56B 117.6(7) . . ? C52B C51B C5B 122.1(8) . . ? C56B C51B C5B 120.3(7) . . ? C51B C52B C53B 121.1(9) . . ? C54B C53B C52B 119.0(9) . . ? C54B C55B C56B 120.0(10) . . ? C55B C54B C53B 121.7(9) . . ? C55B C56B C51B 120.6(9) . . ? C62B C61B C66B 119.5(9) . . ? C62B C61B C6B 121.2(8) . . ? C66B C61B C6B 119.0(9) . . ? C61B C62B C63B 120.6(10) . . ? C64B C63B C62B 118.7(12) . . ? C65B C64B C63B 121.5(12) . . ? C64B C65B C66B 119.9(11) . . ? C61B C66B C65B 119.5(11) . . ? O41 Cl4 O43 118.4(9) . . ? O41 Cl4 O42 113.1(10) . . ? O43 Cl4 O42 111.8(10) . . ? O41 Cl4 O44 108.7(9) . . ? O43 Cl4 O44 101.3(8) . . ? O42 Cl4 O44 101.3(8) . . ? O62 Cl6 O61 119.5(11) . . ? O62 Cl6 O64 114.5(10) . . ? O61 Cl6 O64 104.6(10) . . ? O62 Cl6 O63 112.5(11) . . ? O61 Cl6 O63 102.8(9) . . ? O64 Cl6 O63 100.6(10) . . ? O51 Cl5 O54 112.2(12) . . ? O51 Cl5 O53 115.7(10) . . ? O54 Cl5 O53 109.6(12) . . ? O51 Cl5 O52 106.8(10) . . ? O54 Cl5 O52 107.2(12) . . ? O53 Cl5 O52 104.7(10) . . ? O73 Cl7 O74 111.7(8) . . ? O73 Cl7 O72 114.8(7) . . ? O74 Cl7 O72 110.9(8) . . ? O73 Cl7 O71 106.3(6) . . ? O74 Cl7 O71 109.1(9) . . ? O72 Cl7 O71 103.4(6) . . ? Cl92 C91 Cl93 109.1(8) . . ? _refine_diff_density_max 0.564 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.074 #===END data_2 _database_code_CSD 157535 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 Ag Cl N6 O6 ' _chemical_formula_weight 687.88 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' '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 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 28.01(4) _cell_length_b 15.30(2) _cell_length_c 20.37(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.937(10) _cell_angle_gamma 90.00 _cell_volume 6888(16) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type none _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6929 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.11 _reflns_number_total 4502 _reflns_number_gt 2608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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^)+(0.1812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4502 _refine_ls_number_parameters 378 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2586 _refine_ls_wR_factor_gt 0.2224 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.496 _refine_ls_shift/su_mean 0.037 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 -0.07394(3) 0.09938(4) 0.70123(5) 0.0827(5) Uani 1 d . . . C1 C 0.0047(5) -0.1352(6) 0.8838(7) 0.095(3) Uani 1 d . . . H1A H 0.0231 -0.1778 0.8709 0.115 Uiso 1 calc R . . H1B H -0.0233 -0.1637 0.8890 0.115 Uiso 1 calc R . . H1C H 0.0356 -0.1067 0.9352 0.115 Uiso 1 calc R . . C2 C -0.0281(4) -0.0689(5) 0.8155(6) 0.068(2) Uani 1 d . . . N3 N -0.0183(3) 0.0156(4) 0.8263(5) 0.0677(18) Uani 1 d . . . N4 N 0.0272(3) 0.0372(4) 0.9088(5) 0.0715(19) Uani 1 d . . . C5 C 0.0322(3) 0.1199(5) 0.9287(6) 0.065(2) Uani 1 d . . . C6 C -0.0080(4) 0.1931(5) 0.8707(5) 0.071(2) Uani 1 d . . . N7 N 0.0097(3) 0.2480(4) 0.8398(5) 0.079(2) Uani 1 d . . . N8 N 0.0643(3) 0.2251(4) 0.8552(4) 0.0750(19) Uani 1 d . . . C9 C 0.0975(5) 0.2911(5) 0.8676(7) 0.090(3) Uani 1 d . . . C10 C 0.0845(7) 0.3816(6) 0.8749(11) 0.145(6) Uani 1 d . . . H10A H 0.1003 0.4202 0.8554 0.174 Uiso 1 calc R . . H10B H 0.1030 0.3944 0.9321 0.174 Uiso 1 calc R . . H10C H 0.0415 0.3896 0.8419 0.174 Uiso 1 calc R . . C51 C 0.0776(4) 0.1436(5) 1.0157(6) 0.071(2) Uani 1 d . . . C52 C 0.1193(5) 0.0814(7) 1.0754(8) 0.096(3) Uani 1 d . . . H52 H 0.1190 0.0251 1.0581 0.115 Uiso 1 calc R . . C53 C 0.1605(5) 0.1023(9) 1.1588(9) 0.107(4) Uani 1 d . . . H53 H 0.1874 0.0603 1.1969 0.129 Uiso 1 calc R . . C54 C 0.1613(5) 0.1858(10) 1.1852(8) 0.108(3) Uani 1 d . . . H54 H 0.1883 0.1993 1.2415 0.129 Uiso 1 calc R . . C55 C 0.1233(5) 0.2482(8) 1.1303(8) 0.100(3) Uani 1 d . . . H55 H 0.1249 0.3045 1.1487 0.120 Uiso 1 calc R . . C56 C 0.0812(4) 0.2273(6) 1.0450(6) 0.079(2) Uani 1 d . . . H56 H 0.0553 0.2705 1.0076 0.095 Uiso 1 calc R . . C61 C -0.0651(4) 0.2106(5) 0.8581(5) 0.076(2) Uani 1 d . . . C62 C -0.0903(4) 0.1477(6) 0.8771(6) 0.087(3) Uani 1 d . . . H62 H -0.0711 0.0939 0.8976 0.104 Uiso 1 calc R . . C63 C -0.1444(5) 0.1635(9) 0.8661(8) 0.122(4) Uani 1 d . . . H63 H -0.1606 0.1212 0.8800 0.146 Uiso 1 calc R . . C64 C -0.1721(5) 0.2422(10) 0.8346(8) 0.126(4) Uani 1 d . . . H64 H -0.2082 0.2529 0.8262 0.151 Uiso 1 calc R . . C65 C -0.1489(6) 0.3059(8) 0.8150(8) 0.121(4) Uani 1 d . . . H65 H -0.1687 0.3593 0.7942 0.145 Uiso 1 calc R . . C66 C -0.0958(4) 0.2910(6) 0.8261(6) 0.093(3) Uani 1 d . . . H66 H -0.0801 0.3344 0.8124 0.112 Uiso 1 calc R . . C91 C 0.1534(5) 0.2711(6) 0.8771(7) 0.092(3) Uani 1 d . . . N92 N 0.1585(3) 0.1887(5) 0.8563(5) 0.089(2) Uani 1 d . . . C93 C 0.2076(5) 0.1672(10) 0.8642(7) 0.121(4) Uani 1 d . . . H93 H 0.2100 0.1115 0.8482 0.145 Uiso 1 calc R . . C94 C 0.2568(5) 0.2259(11) 0.8960(8) 0.125(4) Uani 1 d . . . H94 H 0.2914 0.2082 0.9029 0.150 Uiso 1 calc R . . C95 C 0.2519(6) 0.3081(11) 0.9159(9) 0.137(5) Uani 1 d . . . H95 H 0.2821 0.3493 0.9339 0.164 Uiso 1 calc R . . C96 C 0.2010(6) 0.3291(7) 0.9087(7) 0.114(4) Uani 1 d . . . H96 H 0.1984 0.3842 0.9256 0.137 Uiso 1 calc R . . C21 C -0.0759(5) -0.1010(5) 0.7286(7) 0.076(3) Uani 1 d . . . N22 N -0.1013(4) -0.0440(5) 0.6660(6) 0.087(2) Uani 1 d . . . C23 C -0.1445(5) -0.0722(7) 0.5886(8) 0.100(3) Uani 1 d . . . H23 H -0.1632 -0.0313 0.5459 0.119 Uiso 1 calc R . . C24 C -0.1629(5) -0.1564(9) 0.5682(9) 0.121(4) Uani 1 d . . . H24 H -0.1925 -0.1738 0.5135 0.146 Uiso 1 calc R . . C25 C -0.1352(7) -0.2150(8) 0.6336(11) 0.127(4) Uani 1 d . . . H25 H -0.1465 -0.2735 0.6226 0.153 Uiso 1 calc R . . C26 C -0.0914(6) -0.1896(6) 0.7143(8) 0.099(3) Uani 1 d . . . H26 H -0.0728 -0.2297 0.7578 0.118 Uiso 1 calc R . . Cl1 Cl 0.20199(15) -0.4349(2) 0.8292(2) 0.1270(11) Uani 0.524(9) d PD A 1 O11 O 0.2215(9) -0.3419(9) 0.8503(13) 0.169(3) Uiso 0.524(9) d PD A 1 O12 O 0.1485(7) -0.4551(12) 0.8174(13) 0.169(3) Uiso 0.524(9) d PD A 1 O13 O 0.2543(7) -0.4836(12) 0.8984(10) 0.169(3) Uiso 0.524(9) d PD A 1 O14 O 0.1989(8) -0.4546(11) 0.7537(9) 0.169(3) Uiso 0.524(9) d PD A 1 Cl2 Cl 0.20199(15) -0.4349(2) 0.8292(2) 0.1270(11) Uani 0.476(9) d PD A 2 O21 O 0.1528(7) -0.4887(12) 0.7605(10) 0.169(3) Uiso 0.476(9) d PD A 2 O22 O 0.1874(10) -0.4416(13) 0.8932(12) 0.169(3) Uiso 0.476(9) d PD A 2 O23 O 0.2603(7) -0.4762(14) 0.8723(13) 0.169(3) Uiso 0.476(9) d PD A 2 O24 O 0.2004(10) -0.3458(9) 0.8130(14) 0.169(3) Uiso 0.476(9) d PD A 2 O91 O -0.010(2) 0.423(3) 1.067(3) 0.225(17) Uiso 0.33 d P . 2 O92 O 0.225(3) -0.419(4) 1.086(4) 0.27(3) Uiso 0.33 d P . 2 O93 O 0.009(3) 0.516(4) 0.980(4) 0.28(2) Uiso 0.33 d P . 2 O94 O 0.094(3) 0.563(4) 1.003(4) 0.30(3) Uiso 0.33 d P B 2 O95 O 0.321(5) -0.050(6) 0.933(6) 0.43(5) Uiso 0.33 d P . 2 O96 O 0.022(4) 0.602(4) 0.870(6) 0.36(4) Uiso 0.33 d P . 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 0.0871(7) 0.0677(6) 0.0917(8) 0.0068(3) 0.0541(6) 0.0057(3) C1 0.119(8) 0.073(6) 0.098(9) -0.002(6) 0.068(7) -0.006(5) C2 0.075(5) 0.065(5) 0.077(7) -0.003(5) 0.053(6) -0.006(4) N3 0.073(4) 0.057(4) 0.071(6) -0.010(4) 0.042(4) -0.008(3) N4 0.065(4) 0.069(4) 0.082(6) 0.003(4) 0.046(5) 0.006(3) C5 0.054(5) 0.078(6) 0.063(7) -0.004(5) 0.037(5) -0.002(4) C6 0.070(5) 0.068(5) 0.063(6) -0.012(4) 0.034(5) 0.002(4) N7 0.094(5) 0.064(4) 0.083(6) 0.007(4) 0.056(5) 0.001(4) N8 0.083(5) 0.070(4) 0.073(5) -0.001(4) 0.048(4) -0.008(3) C9 0.110(7) 0.065(6) 0.109(9) -0.014(5) 0.075(7) -0.023(5) C10 0.177(12) 0.077(7) 0.230(18) -0.023(8) 0.150(14) -0.026(7) C51 0.063(5) 0.083(6) 0.072(8) 0.004(5) 0.044(6) -0.003(4) C52 0.076(7) 0.113(7) 0.083(9) -0.002(7) 0.041(7) 0.003(6) C53 0.062(6) 0.150(12) 0.087(10) 0.005(8) 0.034(7) -0.001(6) C54 0.073(7) 0.154(11) 0.080(9) -0.023(9) 0.039(7) -0.031(7) C55 0.087(7) 0.122(8) 0.100(10) -0.023(8) 0.063(8) -0.029(7) C56 0.076(6) 0.082(6) 0.070(8) -0.015(5) 0.040(6) -0.014(4) C61 0.064(5) 0.086(6) 0.062(6) -0.003(5) 0.031(5) 0.011(4) C62 0.078(6) 0.094(6) 0.086(8) 0.018(5) 0.050(6) 0.018(5) C63 0.105(8) 0.150(10) 0.128(11) 0.042(8) 0.080(8) 0.043(8) C64 0.077(7) 0.170(12) 0.125(11) 0.014(9) 0.060(8) 0.030(8) C65 0.108(9) 0.126(9) 0.111(10) 0.005(8) 0.058(8) 0.038(7) C66 0.096(7) 0.079(6) 0.090(8) 0.001(5) 0.050(6) 0.015(5) C91 0.106(7) 0.090(6) 0.086(8) -0.016(6) 0.062(6) -0.037(5) N92 0.077(5) 0.097(6) 0.089(6) -0.006(5) 0.049(5) -0.014(4) C93 0.084(7) 0.186(12) 0.098(10) -0.017(8) 0.059(7) -0.006(7) C94 0.080(8) 0.186(13) 0.108(11) 0.021(10) 0.057(8) -0.010(9) C95 0.107(10) 0.182(14) 0.111(11) 0.010(10) 0.062(9) -0.054(10) C96 0.135(9) 0.105(7) 0.103(9) -0.016(7) 0.074(8) -0.044(7) C21 0.090(7) 0.062(5) 0.100(9) -0.009(6) 0.070(7) -0.013(4) N22 0.083(5) 0.080(5) 0.090(7) -0.007(6) 0.049(5) -0.013(5) C23 0.100(8) 0.094(7) 0.087(9) -0.011(7) 0.049(7) -0.016(6) C24 0.120(9) 0.129(10) 0.116(12) -0.044(9) 0.073(9) -0.056(8) C25 0.160(12) 0.107(9) 0.141(14) -0.025(9) 0.106(11) -0.041(8) C26 0.133(9) 0.075(6) 0.096(9) -0.017(6) 0.075(8) -0.022(6) Cl1 0.117(2) 0.1014(19) 0.146(3) 0.015(2) 0.072(2) 0.0198(17) Cl2 0.117(2) 0.1014(19) 0.146(3) 0.015(2) 0.072(2) 0.0198(17) _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 N22 2.289(8) . ? Ag1 N92 2.331(7) 6_557 ? Ag1 N8 2.340(7) 6_557 ? Ag1 N3 2.384(8) . ? Ag1 Ag1 3.315(5) 6_557 ? C1 C2 1.495(13) . ? C2 N3 1.313(10) . ? C2 C21 1.501(14) . ? N3 N4 1.386(10) . ? N4 C5 1.310(10) . ? C5 C51 1.456(12) . ? C5 C6 1.512(12) . ? C6 N7 1.316(10) . ? C6 C61 1.481(10) . ? N7 N8 1.404(9) . ? N8 C9 1.287(9) . ? N8 Ag1 2.340(7) 6_557 ? C9 C10 1.463(13) . ? C9 C91 1.488(13) . ? C51 C56 1.390(12) . ? C51 C52 1.415(13) . ? C52 C53 1.382(16) . ? C53 C54 1.381(15) . ? C54 C55 1.354(15) . ? C55 C56 1.412(14) . ? C61 C62 1.380(12) . ? C61 C66 1.410(11) . ? C62 C63 1.410(12) . ? C63 C64 1.362(16) . ? C64 C65 1.361(16) . ? C65 C66 1.378(14) . ? C91 N92 1.365(11) . ? C91 C96 1.386(13) . ? N92 C93 1.325(11) . ? N92 Ag1 2.331(7) 6_557 ? C93 C94 1.424(17) . ? C94 C95 1.354(18) . ? C95 C96 1.380(17) . ? C21 N22 1.332(12) . ? C21 C26 1.399(12) . ? N22 C23 1.339(14) . ? C23 C24 1.354(15) . ? C24 C25 1.381(17) . ? C25 C26 1.370(16) . ? Cl1 O12 1.399(12) . ? Cl1 O13 1.467(13) . ? Cl1 O11 1.489(13) . ? Cl1 O14 1.518(12) . ? Cl2 O24 1.397(13) . ? Cl2 O23 1.440(13) . ? Cl2 O21 1.471(13) . ? Cl2 O22 1.590(13) . ? 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 N22 Ag1 N92 111.3(3) . 6_557 ? N22 Ag1 N8 138.7(3) . 6_557 ? N92 Ag1 N8 70.1(3) 6_557 6_557 ? N22 Ag1 N3 72.1(3) . . ? N92 Ag1 N3 130.3(2) 6_557 . ? N8 Ag1 N3 140.3(2) 6_557 . ? N22 Ag1 Ag1 104.0(2) . 6_557 ? N92 Ag1 Ag1 144.1(2) 6_557 6_557 ? N8 Ag1 Ag1 79.37(17) 6_557 6_557 ? N3 Ag1 Ag1 66.68(15) . 6_557 ? N3 C2 C1 124.5(9) . . ? N3 C2 C21 117.6(8) . . ? C1 C2 C21 117.9(8) . . ? C2 N3 N4 112.3(7) . . ? C2 N3 Ag1 114.7(6) . . ? N4 N3 Ag1 132.6(4) . . ? C5 N4 N3 116.7(7) . . ? N4 C5 C51 117.7(8) . . ? N4 C5 C6 126.0(8) . . ? C51 C5 C6 116.2(7) . . ? N7 C6 C61 119.2(7) . . ? N7 C6 C5 121.8(7) . . ? C61 C6 C5 118.4(7) . . ? C6 N7 N8 114.5(6) . . ? C9 N8 N7 113.9(7) . . ? C9 N8 Ag1 117.0(6) . 6_557 ? N7 N8 Ag1 122.3(5) . 6_557 ? N8 C9 C10 124.5(9) . . ? N8 C9 C91 116.1(7) . . ? C10 C9 C91 119.3(8) . . ? C56 C51 C52 116.5(9) . . ? C56 C51 C5 122.1(8) . . ? C52 C51 C5 121.4(8) . . ? C53 C52 C51 121.7(10) . . ? C54 C53 C52 119.6(11) . . ? C55 C54 C53 121.0(11) . . ? C54 C55 C56 119.6(10) . . ? C51 C56 C55 121.5(9) . . ? C62 C61 C66 117.9(8) . . ? C62 C61 C6 120.6(7) . . ? C66 C61 C6 121.6(8) . . ? C61 C62 C63 121.3(9) . . ? C64 C63 C62 118.2(11) . . ? C63 C64 C65 122.3(10) . . ? C66 C65 C64 119.7(11) . . ? C65 C66 C61 120.6(10) . . ? N92 C91 C96 118.9(10) . . ? N92 C91 C9 116.8(7) . . ? C96 C91 C9 124.3(10) . . ? C93 N92 C91 119.3(9) . . ? C93 N92 Ag1 125.0(8) . 6_557 ? C91 N92 Ag1 115.5(6) . 6_557 ? N92 C93 C94 122.7(13) . . ? C95 C94 C93 118.4(12) . . ? C94 C95 C96 118.1(11) . . ? C95 C96 C91 122.4(12) . . ? N22 C21 C26 121.3(11) . . ? N22 C21 C2 118.7(7) . . ? C26 C21 C2 119.9(10) . . ? C23 N22 C21 118.7(9) . . ? C23 N22 Ag1 124.4(8) . . ? C21 N22 Ag1 116.6(7) . . ? N22 C23 C24 124.5(12) . . ? C23 C24 C25 116.0(12) . . ? C26 C25 C24 122.1(11) . . ? C25 C26 C21 117.3(11) . . ? O12 Cl1 O13 112.7(10) . . ? O12 Cl1 O11 115.1(10) . . ? O13 Cl1 O11 103.6(10) . . ? O12 Cl1 O14 113.2(10) . . ? O13 Cl1 O14 105.9(9) . . ? O11 Cl1 O14 105.4(9) . . ? O24 Cl2 O23 115.6(10) . . ? O24 Cl2 O21 116.5(11) . . ? O23 Cl2 O21 112.5(11) . . ? O24 Cl2 O22 105.7(10) . . ? O23 Cl2 O22 103.8(10) . . ? O21 Cl2 O22 100.4(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 N3 N4 1.0(10) . . . . ? C21 C2 N3 N4 -179.3(6) . . . . ? C1 C2 N3 Ag1 175.3(6) . . . . ? C21 C2 N3 Ag1 -5.0(8) . . . . ? N22 Ag1 N3 C2 1.9(5) . . . . ? N92 Ag1 N3 C2 105.0(5) 6_557 . . . ? N8 Ag1 N3 C2 -146.1(5) 6_557 . . . ? Ag1 Ag1 N3 C2 -112.7(5) 6_557 . . . ? N22 Ag1 N3 N4 174.7(6) . . . . ? N92 Ag1 N3 N4 -82.2(6) 6_557 . . . ? N8 Ag1 N3 N4 26.7(7) 6_557 . . . ? Ag1 Ag1 N3 N4 60.1(5) 6_557 . . . ? C2 N3 N4 C5 -166.9(6) . . . . ? Ag1 N3 N4 C5 20.1(9) . . . . ? N3 N4 C5 C51 177.0(6) . . . . ? N3 N4 C5 C6 1.9(10) . . . . ? N4 C5 C6 N7 -103.3(9) . . . . ? C51 C5 C6 N7 81.4(10) . . . . ? N4 C5 C6 C61 85.4(9) . . . . ? C51 C5 C6 C61 -89.9(8) . . . . ? C61 C6 N7 N8 -179.9(7) . . . . ? C5 C6 N7 N8 8.9(11) . . . . ? C6 N7 N8 C9 -144.5(9) . . . . ? C6 N7 N8 Ag1 65.5(9) . . . 6_557 ? N7 N8 C9 C10 6.7(15) . . . . ? Ag1 N8 C9 C10 158.4(10) 6_557 . . . ? N7 N8 C9 C91 -175.0(8) . . . . ? Ag1 N8 C9 C91 -23.3(11) 6_557 . . . ? N4 C5 C51 C56 -171.4(6) . . . . ? C6 C5 C51 C56 4.3(10) . . . . ? N4 C5 C51 C52 6.7(10) . . . . ? C6 C5 C51 C52 -177.7(7) . . . . ? C56 C51 C52 C53 1.6(13) . . . . ? C5 C51 C52 C53 -176.6(8) . . . . ? C51 C52 C53 C54 0.0(15) . . . . ? C52 C53 C54 C55 -1.6(15) . . . . ? C53 C54 C55 C56 1.5(14) . . . . ? C52 C51 C56 C55 -1.6(11) . . . . ? C5 C51 C56 C55 176.5(7) . . . . ? C54 C55 C56 C51 0.1(13) . . . . ? N7 C6 C61 C62 169.1(9) . . . . ? C5 C6 C61 C62 -19.4(12) . . . . ? N7 C6 C61 C66 -10.5(12) . . . . ? C5 C6 C61 C66 161.0(8) . . . . ? C66 C61 C62 C63 -0.9(15) . . . . ? C6 C61 C62 C63 179.5(9) . . . . ? C61 C62 C63 C64 1.2(17) . . . . ? C62 C63 C64 C65 -1(2) . . . . ? C63 C64 C65 C66 1(2) . . . . ? C64 C65 C66 C61 -0.4(17) . . . . ? C62 C61 C66 C65 0.5(15) . . . . ? C6 C61 C66 C65 -179.9(9) . . . . ? N8 C9 C91 N92 12.0(14) . . . . ? C10 C9 C91 N92 -169.6(11) . . . . ? N8 C9 C91 C96 -165.0(10) . . . . ? C10 C9 C91 C96 13.4(17) . . . . ? C96 C91 N92 C93 -2.4(15) . . . . ? C9 C91 N92 C93 -179.5(9) . . . . ? C96 C91 N92 Ag1 -177.6(8) . . . 6_557 ? C9 C91 N92 Ag1 5.3(11) . . . 6_557 ? C91 N92 C93 C94 2.0(16) . . . . ? Ag1 N92 C93 C94 176.8(9) 6_557 . . . ? N92 C93 C94 C95 -2.7(19) . . . . ? C93 C94 C95 C96 4(2) . . . . ? C94 C95 C96 C91 -4(2) . . . . ? N92 C91 C96 C95 3.5(17) . . . . ? C9 C91 C96 C95 -179.6(11) . . . . ? N3 C2 C21 N22 6.9(11) . . . . ? C1 C2 C21 N22 -173.4(7) . . . . ? N3 C2 C21 C26 -175.2(7) . . . . ? C1 C2 C21 C26 4.6(11) . . . . ? C26 C21 N22 C23 3.1(13) . . . . ? C2 C21 N22 C23 -179.0(8) . . . . ? C26 C21 N22 Ag1 177.1(7) . . . . ? C2 C21 N22 Ag1 -5.0(9) . . . . ? N92 Ag1 N22 C23 48.2(8) 6_557 . . . ? N8 Ag1 N22 C23 -35.4(9) 6_557 . . . ? N3 Ag1 N22 C23 175.4(8) . . . . ? Ag1 Ag1 N22 C23 -125.2(7) 6_557 . . . ? N92 Ag1 N22 C21 -125.4(6) 6_557 . . . ? N8 Ag1 N22 C21 151.0(6) 6_557 . . . ? N3 Ag1 N22 C21 1.8(6) . . . . ? Ag1 Ag1 N22 C21 61.2(6) 6_557 . . . ? C21 N22 C23 C24 -2.9(15) . . . . ? Ag1 N22 C23 C24 -176.4(8) . . . . ? N22 C23 C24 C25 1.5(16) . . . . ? C23 C24 C25 C26 -0.2(17) . . . . ? C24 C25 C26 C21 0.5(17) . . . . ? N22 C21 C26 C25 -1.9(14) . . . . ? C2 C21 C26 C25 -179.8(9) . . . . ? _refine_diff_density_max 0.842 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.103 #===END