Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Calhorda, Maria' 'de Biani, Fabrizia Fabrizi' 'Drew, Michael G. B.' 'Felix, Vitor' 'Liu, Huizhang' 'Novosad, J.' 'Veiros, Luis' 'Zanello, Piero' _publ_contact_author_name 'Prof Maria Calhorda' _publ_contact_author_address ; ITQB Av da Republica EAN Apt 127 Oeiras 2781-901 PORTUGAL ; _publ_contact_author_email 'MJC@ITQB.UNL.PT' _publ_requested_journal 'Dalton transactions' _publ_section_title ; New Cu(I) and Ag(I) binuclear complxes containing the dppa ligand ; data_compound_1 _database_code_CSD 188189 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H63 Cu F12 N3 O6 P8' _chemical_formula_weight 1605.55 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' '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 15.857(22) _cell_length_b 15.857(22) _cell_length_c 33.280(41) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8368(19) _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 ? _exptl_crystal_colour White _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3284 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type 'No absorption correction' _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 'MAR research image plate system' _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 19175 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.1224 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.09 _reflns_number_total 7424 _reflns_number_gt 3149 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'W. Kabsch, J. Appl. Crystallogr. 21,916,1983' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1804P)^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 7424 _refine_ls_number_parameters 463 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2332 _refine_ls_R_factor_gt 0.1011 _refine_ls_wR_factor_ref 0.3151 _refine_ls_wR_factor_gt 0.2643 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.7500 0.2500 0.12808(3) 0.0582(4) Uani 1 d S . . O2 O 0.6508(3) 0.3243(3) 0.12925(13) 0.0643(13) Uani 1 d . . . P3 P 0.63994(13) 0.41032(12) 0.14682(6) 0.0654(6) Uani 1 d . . . N4 N 0.7282(4) 0.4645(4) 0.14777(16) 0.0659(16) Uani 1 d . . . HN4 H 0.7307 0.5125 0.1359 0.079 Uiso 1 calc R . . P5 P 0.81352(13) 0.42726(12) 0.17165(5) 0.0620(6) Uani 1 d . . . O6 O 0.8078(3) 0.3334(3) 0.17211(13) 0.0684(14) Uani 1 d . . . O7 O 0.8076(3) 0.3196(3) 0.08059(13) 0.0719(14) Uani 1 d . . . P8 P 0.81917(12) 0.31555(13) 0.03663(6) 0.0646(6) Uani 1 d . . . N9 N 0.7500 0.2500 0.0149(2) 0.061(2) Uani 1 d SD . . HN9 H 0.7500 0.2500 -0.0108(4) 0.09(4) Uiso 1 d SD . . C11 C 0.6049(5) 0.4041(5) 0.1977(2) 0.074(2) Uani 1 d . . . C12 C 0.5922(8) 0.3279(7) 0.2142(3) 0.131(4) Uani 1 d . . . H12 H 0.5988 0.2802 0.1983 0.157 Uiso 1 calc R . . C13 C 0.5692(12) 0.3177(8) 0.2548(4) 0.189(7) Uani 1 d . . . H13 H 0.5628 0.2638 0.2654 0.227 Uiso 1 calc R . . C14 C 0.5562(6) 0.3865(8) 0.2784(3) 0.162(6) Uani 1 d . . . H14 H 0.5400 0.3807 0.3051 0.195 Uiso 1 calc R . . C15 C 0.5678(6) 0.4645(8) 0.2617(3) 0.143(5) Uani 1 d R . . H15 H 0.5595 0.5124 0.2773 0.171 Uiso 1 calc R . . C16 C 0.5923(6) 0.4733(6) 0.2212(3) 0.098(3) Uani 1 d . . . H16 H 0.5999 0.5268 0.2104 0.117 Uiso 1 calc R . . C21 C 0.5721(5) 0.4725(5) 0.1175(3) 0.074(2) Uani 1 d . . . C22 C 0.5924(7) 0.4841(7) 0.0776(3) 0.116(3) Uani 1 d . . . H22 H 0.6419 0.4597 0.0681 0.140 Uiso 1 calc R . . C23 C 0.5427(11) 0.5309(9) 0.0501(5) 0.166(6) Uani 1 d . . . H23 H 0.5589 0.5383 0.0235 0.199 Uiso 1 calc R . . C25 C 0.4457(10) 0.5529(10) 0.1016(7) 0.174(7) Uani 1 d . . . H25 H 0.3946 0.5760 0.1097 0.209 Uiso 1 calc R . . C24 C 0.4725(13) 0.5631(11) 0.0643(6) 0.166(7) Uani 1 d . . . H24 H 0.4395 0.5952 0.0470 0.199 Uiso 1 calc R . . C26 C 0.4964(7) 0.5060(8) 0.1293(4) 0.132(4) Uani 1 d . . . H26 H 0.4777 0.4982 0.1555 0.158 Uiso 1 calc R . . C31 C 0.8093(5) 0.4675(5) 0.2221(2) 0.066(2) Uani 1 d . . . C32 C 0.7987(6) 0.5525(6) 0.2295(2) 0.084(3) Uani 1 d . . . H32 H 0.7966 0.5902 0.2081 0.101 Uiso 1 calc R . . C33 C 0.7911(6) 0.5817(7) 0.2684(3) 0.105(3) Uani 1 d . . . H33 H 0.7828 0.6389 0.2731 0.126 Uiso 1 calc R . . C34 C 0.7958(7) 0.5266(9) 0.2999(3) 0.114(3) Uani 1 d . . . H34 H 0.7905 0.5463 0.3260 0.137 Uiso 1 calc R . . C35 C 0.8082(7) 0.4434(8) 0.2930(3) 0.118(4) Uani 1 d . . . H35 H 0.8125 0.4064 0.3146 0.141 Uiso 1 calc R . . C36 C 0.8145(6) 0.4125(6) 0.2536(2) 0.093(3) Uani 1 d . . . H36 H 0.8222 0.3552 0.2489 0.112 Uiso 1 calc R . . C41 C 0.9051(4) 0.4667(5) 0.14630(19) 0.0600(18) Uani 1 d . . . C42 C 0.9194(6) 0.5521(6) 0.1402(2) 0.087(3) Uani 1 d . . . H42 H 0.8799 0.5912 0.1490 0.105 Uiso 1 calc R . . C43 C 0.9920(7) 0.5796(7) 0.1210(3) 0.103(3) Uani 1 d . . . H43 H 1.0003 0.6367 0.1159 0.124 Uiso 1 calc R . . C44 C 1.0516(7) 0.5215(8) 0.1095(3) 0.107(3) Uani 1 d . . . H44 H 1.1026 0.5392 0.0987 0.129 Uiso 1 calc R . . C45 C 1.0358(8) 0.4397(9) 0.1140(4) 0.132(4) Uani 1 d . . . H45 H 1.0740 0.4007 0.1038 0.159 Uiso 1 calc R . . C46 C 0.9634(6) 0.4105(6) 0.1337(3) 0.090(3) Uani 1 d . . . H46 H 0.9556 0.3531 0.1380 0.108 Uiso 1 calc R . . C51 C 0.9215(5) 0.2790(4) 0.0222(2) 0.070(2) Uani 1 d . . . C52 C 0.9717(7) 0.2393(5) 0.0503(3) 0.095(3) Uani 1 d . . . H52 H 0.9522 0.2315 0.0764 0.114 Uiso 1 calc R . . C53 C 1.0538(6) 0.2101(6) 0.0392(4) 0.104(3) Uani 1 d . . . H53 H 1.0873 0.1834 0.0582 0.125 Uiso 1 calc R . . C54 C 1.0834(7) 0.2207(7) 0.0014(4) 0.117(4) Uani 1 d . . . H54 H 1.1374 0.2030 -0.0053 0.140 Uiso 1 calc R . . C55 C 1.0321(8) 0.2583(7) -0.0271(4) 0.124(4) Uani 1 d . . . H55 H 1.0516 0.2648 -0.0532 0.149 Uiso 1 calc R . . C56 C 0.9514(6) 0.2865(6) -0.0168(2) 0.093(3) Uani 1 d . . . H56 H 0.9173 0.3106 -0.0364 0.111 Uiso 1 calc R . . C61 C 0.8052(5) 0.4164(5) 0.0132(2) 0.070(2) Uani 1 d . . . C62 C 0.7491(7) 0.4346(6) -0.0152(4) 0.137(5) Uani 1 d . . . H62 H 0.7132 0.3920 -0.0240 0.165 Uiso 1 calc R . . C63 C 0.7416(8) 0.5134(8) -0.0320(5) 0.157(6) Uani 1 d . . . H63 H 0.7046 0.5219 -0.0533 0.188 Uiso 1 calc R . . C64 C 0.7858(9) 0.5760(7) -0.0184(5) 0.140(5) Uani 1 d . . . H64 H 0.7807 0.6301 -0.0289 0.168 Uiso 1 calc R . . C65 C 0.8403(14) 0.5578(10) 0.0122(6) 0.268(12) Uani 1 d . . . H65 H 0.8715 0.6014 0.0236 0.321 Uiso 1 calc R . . C66 C 0.8505(11) 0.4773(8) 0.0266(5) 0.229(10) Uani 1 d . . . H66 H 0.8907 0.4668 0.0464 0.274 Uiso 1 calc R . . P9 P 0.7500 0.7500 0.11733(9) 0.0813(10) Uani 1 d S . . F91 F 0.8481(4) 0.7383(4) 0.11717(19) 0.134(2) Uani 1 d . . . F92 F 0.7500 0.7500 0.0711(2) 0.180(4) Uani 1 d S . . F93 F 0.7500 0.7500 0.1639(3) 0.218(6) Uani 1 d S . . F94 F 0.7388(4) 0.6521(4) 0.1182(3) 0.191(4) Uani 1 d . . . P10 P 0.7500 0.2500 -0.11570(11) 0.1004(13) Uani 1 d S . . F101 F 0.7500 0.2500 -0.0712(3) 0.315(11) Uani 1 d S . . F102 F 0.7423(7) 0.3443(6) -0.1191(4) 0.233(5) Uani 1 d . . . F103 F 0.8472(5) 0.2548(7) -0.1160(3) 0.209(4) Uani 1 d . . . F104 F 0.7500 0.2500 -0.1609(4) 0.250(8) Uani 1 d S . . 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 0.0643(9) 0.0583(8) 0.0519(7) 0.000 0.000 0.0026(6) O2 0.070(3) 0.053(3) 0.071(3) -0.010(2) 0.000(2) 0.007(2) P3 0.0682(14) 0.0592(13) 0.0688(12) -0.0101(10) -0.0040(10) 0.0059(11) N4 0.073(4) 0.064(4) 0.061(3) -0.005(3) -0.010(3) 0.012(3) P5 0.0765(14) 0.0554(13) 0.0541(10) -0.0012(9) -0.0051(9) 0.0061(10) O6 0.089(4) 0.051(3) 0.065(3) -0.001(2) -0.010(3) 0.005(2) O7 0.080(3) 0.080(4) 0.055(3) -0.013(2) -0.001(2) 0.006(3) P8 0.0661(13) 0.0692(14) 0.0585(11) -0.0063(10) 0.0001(10) -0.0042(11) N9 0.074(6) 0.068(5) 0.041(4) 0.000 0.000 -0.007(4) C11 0.091(6) 0.053(5) 0.078(5) -0.003(5) 0.012(4) 0.002(4) C12 0.174(11) 0.099(9) 0.120(8) -0.023(7) 0.065(8) 0.018(8) C13 0.32(2) 0.104(9) 0.144(11) -0.012(8) 0.130(13) -0.003(11) C14 0.253(17) 0.120(10) 0.114(9) -0.002(9) 0.070(10) 0.036(11) C15 0.188(13) 0.134(11) 0.106(9) -0.046(8) 0.033(8) 0.039(9) C16 0.122(8) 0.090(7) 0.081(6) -0.021(5) 0.002(5) 0.010(6) C21 0.067(6) 0.066(5) 0.089(6) -0.016(4) 0.000(4) 0.009(4) C22 0.105(8) 0.114(8) 0.130(9) 0.020(7) -0.019(7) 0.033(6) C23 0.144(13) 0.165(13) 0.189(14) 0.058(11) -0.032(12) 0.030(11) C25 0.106(11) 0.150(14) 0.266(19) -0.074(15) -0.073(14) 0.075(10) C24 0.153(17) 0.124(12) 0.220(19) 0.029(14) -0.060(16) 0.017(10) C26 0.090(8) 0.142(10) 0.163(11) -0.015(8) -0.026(7) 0.038(8) C31 0.074(5) 0.066(5) 0.058(4) -0.008(4) -0.006(4) 0.003(4) C32 0.114(7) 0.078(6) 0.062(5) -0.010(4) -0.006(5) 0.006(5) C33 0.109(8) 0.104(8) 0.101(7) -0.040(6) -0.005(6) -0.003(6) C34 0.137(9) 0.132(10) 0.073(6) -0.022(7) -0.010(6) -0.007(8) C35 0.153(10) 0.137(10) 0.063(6) 0.008(6) -0.001(6) -0.036(8) C36 0.126(8) 0.095(7) 0.057(5) 0.007(5) -0.011(5) 0.014(6) C41 0.063(5) 0.063(5) 0.054(4) -0.005(4) -0.007(4) 0.005(4) C42 0.086(7) 0.087(7) 0.089(6) 0.012(5) 0.008(5) -0.006(5) C43 0.103(8) 0.099(8) 0.107(7) 0.022(6) 0.013(6) -0.020(7) C44 0.109(9) 0.108(9) 0.104(7) 0.016(7) 0.017(6) -0.007(7) C45 0.114(10) 0.116(10) 0.167(11) -0.005(8) 0.039(8) 0.035(8) C46 0.063(6) 0.089(7) 0.119(7) -0.010(5) 0.016(5) 0.008(5) C51 0.075(5) 0.054(5) 0.080(5) 0.007(4) -0.004(4) -0.001(4) C52 0.107(8) 0.084(6) 0.094(6) 0.011(5) 0.013(6) 0.007(6) C53 0.081(7) 0.110(8) 0.122(8) 0.022(7) -0.011(6) 0.019(6) C54 0.092(8) 0.108(8) 0.150(11) 0.008(8) 0.021(8) 0.013(6) C55 0.116(9) 0.130(9) 0.126(9) -0.001(8) 0.052(8) -0.008(8) C56 0.082(7) 0.124(8) 0.072(5) -0.004(5) 0.012(5) 0.008(6) C61 0.078(5) 0.059(5) 0.074(5) -0.006(4) -0.007(4) -0.003(4) C62 0.138(9) 0.059(6) 0.216(13) 0.037(7) -0.069(9) -0.014(6) C63 0.163(12) 0.077(8) 0.230(15) 0.036(9) -0.083(11) -0.021(8) C64 0.144(11) 0.068(8) 0.209(15) 0.027(9) -0.001(10) 0.029(8) C65 0.40(3) 0.088(11) 0.31(2) 0.028(13) -0.18(2) -0.084(14) C66 0.34(2) 0.078(9) 0.265(18) 0.059(10) -0.177(17) -0.100(11) P9 0.074(2) 0.089(3) 0.082(2) 0.000 0.000 0.0090(18) F91 0.091(4) 0.130(5) 0.182(6) 0.007(4) 0.008(4) 0.023(4) F92 0.208(10) 0.257(13) 0.076(5) 0.000 0.000 0.021(9) F93 0.170(9) 0.399(19) 0.085(6) 0.000 0.000 -0.082(11) F94 0.128(6) 0.082(5) 0.363(12) 0.041(5) -0.026(6) 0.002(4) P10 0.088(3) 0.128(4) 0.086(2) 0.000 0.000 0.018(2) F101 0.40(2) 0.50(3) 0.048(5) 0.000 0.000 -0.12(2) F102 0.206(10) 0.135(7) 0.358(15) 0.064(7) 0.054(8) 0.045(7) F103 0.107(6) 0.275(11) 0.245(9) -0.046(7) -0.031(5) 0.003(6) F104 0.182(11) 0.44(3) 0.133(10) 0.000 0.000 -0.020(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 Cu1 O2 1.966(5) . ? Cu1 O2 1.966(5) 2_655 ? Cu1 O7 2.133(5) . ? Cu1 O7 2.133(5) 2_655 ? Cu1 O6 2.177(5) 2_655 ? Cu1 O6 2.177(5) . ? O2 P3 1.495(5) . ? P3 N4 1.642(7) . ? P3 C21 1.756(9) . ? P3 C11 1.785(8) . ? N4 P5 1.676(6) . ? P5 O6 1.490(5) . ? P5 C41 1.792(8) . ? P5 C31 1.799(7) . ? O7 P8 1.476(5) . ? P8 N9 1.675(4) . ? P8 C51 1.789(8) . ? P8 C61 1.793(8) . ? N9 P8 1.675(4) 2_655 ? C11 C12 1.342(12) . ? C11 C16 1.362(11) . ? C12 C13 1.406(15) . ? C13 C14 1.362(13) . ? C14 C15 1.3680 . ? C15 C16 1.411(11) . ? C21 C26 1.371(13) . ? C21 C22 1.378(12) . ? C22 C23 1.417(15) . ? C23 C24 1.31(2) . ? C25 C24 1.32(2) . ? C25 C26 1.431(18) . ? C31 C36 1.364(10) . ? C31 C32 1.379(11) . ? C32 C33 1.380(11) . ? C33 C34 1.366(13) . ? C34 C35 1.354(14) . ? C35 C36 1.404(12) . ? C41 C46 1.352(10) . ? C41 C42 1.388(11) . ? C42 C43 1.387(12) . ? C43 C44 1.374(13) . ? C44 C45 1.328(14) . ? C45 C46 1.400(14) . ? C51 C52 1.380(11) . ? C51 C56 1.388(10) . ? C52 C53 1.431(12) . ? C53 C54 1.353(14) . ? C54 C55 1.382(15) . ? C55 C56 1.398(13) . ? C61 C66 1.284(13) . ? C61 C62 1.329(12) . ? C62 C63 1.376(14) . ? C63 C64 1.296(15) . ? C64 C65 1.366(17) . ? C65 C66 1.374(18) . ? P9 F92 1.539(8) . ? P9 F93 1.551(9) . ? P9 F94 1.563(7) . ? P9 F94 1.563(7) 2_665 ? P9 F91 1.566(6) 2_665 ? P9 F91 1.566(6) . ? P10 F101 1.482(10) . ? P10 F102 1.504(9) . ? P10 F102 1.504(9) 2_655 ? P10 F104 1.505(13) . ? P10 F103 1.542(8) 2_655 ? P10 F103 1.543(8) . ? 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 O2 Cu1 O2 177.7(3) . 2_655 ? O2 Cu1 O7 92.71(18) . . ? O2 Cu1 O7 88.97(18) 2_655 . ? O2 Cu1 O7 88.98(18) . 2_655 ? O2 Cu1 O7 92.71(18) 2_655 2_655 ? O7 Cu1 O7 84.4(3) . 2_655 ? O2 Cu1 O6 90.80(19) . 2_655 ? O2 Cu1 O6 87.68(18) 2_655 2_655 ? O7 Cu1 O6 173.52(16) . 2_655 ? O7 Cu1 O6 90.2(2) 2_655 2_655 ? O2 Cu1 O6 87.68(18) . . ? O2 Cu1 O6 90.80(19) 2_655 . ? O7 Cu1 O6 90.2(2) . . ? O7 Cu1 O6 173.52(16) 2_655 . ? O6 Cu1 O6 95.4(3) 2_655 . ? P3 O2 Cu1 130.3(3) . . ? O2 P3 N4 112.8(3) . . ? O2 P3 C21 111.4(3) . . ? N4 P3 C21 103.8(4) . . ? O2 P3 C11 110.9(3) . . ? N4 P3 C11 106.0(3) . . ? C21 P3 C11 111.6(4) . . ? P3 N4 P5 120.9(4) . . ? O6 P5 N4 107.9(3) . . ? O6 P5 C41 113.7(3) . . ? N4 P5 C41 107.9(3) . . ? O6 P5 C31 110.0(3) . . ? N4 P5 C31 106.7(3) . . ? C41 P5 C31 110.2(3) . . ? P5 O6 Cu1 128.7(3) . . ? P8 O7 Cu1 139.9(3) . . ? O7 P8 N9 111.9(3) . . ? O7 P8 C51 113.1(3) . . ? N9 P8 C51 106.1(3) . . ? O7 P8 C61 112.1(3) . . ? N9 P8 C61 106.6(3) . . ? C51 P8 C61 106.5(4) . . ? P8 N9 P8 128.9(5) 2_655 . ? C12 C11 C16 117.9(8) . . ? C12 C11 P3 119.1(7) . . ? C16 C11 P3 123.0(7) . . ? C11 C12 C13 122.5(10) . . ? C14 C13 C12 120.0(11) . . ? C13 C14 C15 118.0(7) . . ? C14 C15 C16 121.0(6) . . ? C11 C16 C15 120.6(9) . . ? C26 C21 C22 115.4(9) . . ? C26 C21 P3 126.5(8) . . ? C22 C21 P3 117.9(7) . . ? C21 C22 C23 124.2(12) . . ? C24 C23 C22 116.3(16) . . ? C24 C25 C26 119.2(16) . . ? C23 C24 C25 124.3(19) . . ? C21 C26 C25 120.5(13) . . ? C36 C31 C32 119.8(7) . . ? C36 C31 P5 119.1(6) . . ? C32 C31 P5 121.1(6) . . ? C31 C32 C33 120.3(8) . . ? C34 C33 C32 120.0(10) . . ? C35 C34 C33 120.1(10) . . ? C34 C35 C36 120.6(10) . . ? C31 C36 C35 119.2(9) . . ? C46 C41 C42 119.0(8) . . ? C46 C41 P5 118.1(7) . . ? C42 C41 P5 122.9(6) . . ? C43 C42 C41 120.7(9) . . ? C44 C43 C42 119.1(10) . . ? C45 C44 C43 119.6(11) . . ? C44 C45 C46 122.1(10) . . ? C41 C46 C45 119.2(9) . . ? C52 C51 C56 118.4(8) . . ? C52 C51 P8 119.3(7) . . ? C56 C51 P8 122.2(6) . . ? C51 C52 C53 119.8(8) . . ? C54 C53 C52 121.1(10) . . ? C53 C54 C55 119.1(10) . . ? C54 C55 C56 120.6(10) . . ? C51 C56 C55 120.9(9) . . ? C66 C61 C62 117.3(9) . . ? C66 C61 P8 116.8(8) . . ? C62 C61 P8 125.8(7) . . ? C61 C62 C63 123.0(10) . . ? C64 C63 C62 120.4(12) . . ? C63 C64 C65 116.2(12) . . ? C64 C65 C66 122.0(13) . . ? C61 C66 C65 120.8(13) . . ? F92 P9 F93 180.000(1) . . ? F92 P9 F94 91.0(4) . . ? F93 P9 F94 89.0(4) . . ? F92 P9 F94 91.0(4) . 2_665 ? F93 P9 F94 89.0(4) . 2_665 ? F94 P9 F94 177.9(7) . 2_665 ? F92 P9 F91 89.8(3) . 2_665 ? F93 P9 F91 90.2(3) . 2_665 ? F94 P9 F91 90.2(3) . 2_665 ? F94 P9 F91 89.8(3) 2_665 2_665 ? F92 P9 F91 89.8(2) . . ? F93 P9 F91 90.2(3) . . ? F94 P9 F91 89.8(3) . . ? F94 P9 F91 90.2(3) 2_665 . ? F91 P9 F91 179.6(5) 2_665 . ? F101 P10 F102 94.3(5) . . ? F101 P10 F102 94.3(5) . 2_655 ? F102 P10 F102 171.4(9) . 2_655 ? F101 P10 F104 180.0 . . ? F102 P10 F104 85.7(5) . . ? F102 P10 F104 85.7(5) 2_655 . ? F101 P10 F103 90.3(4) . 2_655 ? F102 P10 F103 88.1(5) . 2_655 ? F102 P10 F103 91.8(5) 2_655 2_655 ? F104 P10 F103 89.7(4) . 2_655 ? F101 P10 F103 90.3(4) . . ? F102 P10 F103 91.8(5) . . ? F102 P10 F103 88.1(5) 2_655 . ? F104 P10 F103 89.7(4) . . ? F103 P10 F103 179.3(7) 2_655 . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.876 _refine_diff_density_max 0.845 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.120 #==END data_compound_2 _database_code_CSD 188190 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Cu2(dppa)2(CH3CN)3][PF6]2 _chemical_formula_sum 'C54 H51 Cu2 F12 N5 P6' _chemical_formula_weight 1310.90 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' _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 10.437(15) _cell_length_b 11.923(15) _cell_length_c 23.021(32) _cell_angle_alpha 90.32(1) _cell_angle_beta 94.00(1) _cell_angle_gamma 90.40(1) _cell_volume 2858(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour White _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type 'No absorption correction' _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 'MAR research image plate system' _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 9961 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.13 _reflns_number_total 9961 _reflns_number_gt 7532 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'W. Kabsch, J. Appl. Crystallogr. 21,916,1983' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1152P)^2^+8.8945P] 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 9961 _refine_ls_number_parameters 694 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2225 _refine_ls_wR_factor_gt 0.2039 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.26744(6) 0.39539(6) 0.26199(3) 0.0338(2) Uani 1 d . . . N100 N 0.1792(5) 0.3798(5) 0.3386(2) 0.0430(12) Uani 1 d . . . C101 C 0.1356(6) 0.3788(6) 0.3819(3) 0.0448(15) Uani 1 d . . . C102 C 0.0787(9) 0.3798(8) 0.4382(3) 0.070(2) Uani 1 d . . . H10A H 0.1435 0.3989 0.4684 0.084 Uiso 1 calc R . . H10B H 0.0440 0.3069 0.4456 0.084 Uiso 1 calc R . . H10C H 0.0113 0.4342 0.4376 0.084 Uiso 1 calc R . . N200 N 0.2888(5) 0.5703(5) 0.2595(2) 0.0470(13) Uani 1 d . . . C201 C 0.2666(6) 0.6635(5) 0.2564(3) 0.0467(15) Uani 1 d . . . C202 C 0.2370(7) 0.7807(6) 0.2499(4) 0.068(2) Uani 1 d . . . H20A H 0.2951 0.8148 0.2246 0.081 Uiso 1 calc R . . H20B H 0.2456 0.8169 0.2874 0.081 Uiso 1 calc R . . H20C H 0.1504 0.7885 0.2335 0.081 Uiso 1 calc R . . P2 P 0.47872(13) 0.35376(11) 0.27428(6) 0.0270(3) Uani 1 d . . . N3 N 0.5177(4) 0.2213(4) 0.2965(2) 0.0291(10) Uani 1 d D . . HN3 H 0.595(2) 0.218(5) 0.312(2) 0.023(14) Uiso 1 d D . . P4 P 0.39873(13) 0.12851(11) 0.30831(6) 0.0275(3) Uani 1 d . . . Cu5 Cu 0.24452(6) 0.15969(6) 0.23726(3) 0.0366(2) Uani 1 d . . . N300 N 0.3283(5) 0.1490(5) 0.1620(2) 0.0448(12) Uani 1 d . . . C302 C 0.4230(8) 0.1304(8) 0.0619(3) 0.067(2) Uani 1 d . . . H30A H 0.3578 0.1012 0.0342 0.081 Uiso 1 calc R . . H30B H 0.4943 0.0799 0.0648 0.081 Uiso 1 calc R . . H30C H 0.4513 0.2024 0.0492 0.081 Uiso 1 calc R . . C301 C 0.3709(6) 0.1418(6) 0.1183(3) 0.0465(15) Uani 1 d . . . P6 P 0.02940(13) 0.15619(11) 0.22753(6) 0.0278(3) Uani 1 d . . . N7 N -0.0139(4) 0.2883(4) 0.2066(2) 0.0301(10) Uani 1 d D . . HN7 H -0.0930(17) 0.289(4) 0.194(2) 0.020(13) Uiso 1 d D . . P8 P 0.10143(13) 0.38324(11) 0.19278(6) 0.0279(3) Uani 1 d . . . C11 C 0.5624(5) 0.4417(4) 0.3301(2) 0.0321(12) Uani 1 d . . . C12 C 0.6909(6) 0.4691(5) 0.3293(3) 0.0463(15) Uani 1 d . . . H12 H 0.7366 0.4468 0.2981 0.056 Uiso 1 calc R . . C13 C 0.7529(8) 0.5301(6) 0.3751(4) 0.066(2) Uani 1 d . . . H13 H 0.8398 0.5478 0.3746 0.079 Uiso 1 calc R . . C14 C 0.6857(9) 0.5636(7) 0.4206(3) 0.069(2) Uani 1 d . . . H14 H 0.7276 0.6036 0.4512 0.082 Uiso 1 calc R . . C15 C 0.5554(9) 0.5391(7) 0.4222(3) 0.067(2) Uani 1 d . . . H15 H 0.5099 0.5627 0.4532 0.080 Uiso 1 calc R . . C16 C 0.4956(7) 0.4791(6) 0.3768(3) 0.0508(16) Uani 1 d . . . H16 H 0.4083 0.4630 0.3772 0.061 Uiso 1 calc R . . C21 C 0.5683(5) 0.3773(4) 0.2099(2) 0.0304(11) Uani 1 d . . . C22 C 0.6257(6) 0.2909(5) 0.1814(3) 0.0379(13) Uani 1 d . . . H22 H 0.6269 0.2194 0.1973 0.045 Uiso 1 calc R . . C23 C 0.6816(6) 0.3093(6) 0.1293(3) 0.0480(16) Uani 1 d . . . H23 H 0.7196 0.2504 0.1103 0.058 Uiso 1 calc R . . C24 C 0.6806(7) 0.4159(7) 0.1057(3) 0.0570(19) Uani 1 d . . . H24 H 0.7180 0.4289 0.0709 0.068 Uiso 1 calc R . . C25 C 0.6237(7) 0.5030(6) 0.1341(3) 0.0558(19) Uani 1 d . . . H25 H 0.6234 0.5744 0.1181 0.067 Uiso 1 calc R . . C26 C 0.5672(6) 0.4853(5) 0.1860(3) 0.0475(16) Uani 1 d . . . H26 H 0.5291 0.5443 0.2048 0.057 Uiso 1 calc R . . C31 C 0.3659(6) 0.1389(4) 0.3848(2) 0.0347(12) Uani 1 d . . . C32 C 0.4549(7) 0.1797(6) 0.4269(3) 0.0512(16) Uani 1 d . . . H32 H 0.5338 0.2065 0.4163 0.061 Uiso 1 calc R . . C33 C 0.4275(9) 0.1811(7) 0.4847(3) 0.070(2) Uani 1 d . . . H33 H 0.4873 0.2097 0.5129 0.084 Uiso 1 calc R . . C34 C 0.3118(10) 0.1402(7) 0.5006(3) 0.072(2) Uani 1 d . . . H34 H 0.2946 0.1397 0.5397 0.087 Uiso 1 calc R . . C35 C 0.2203(9) 0.0995(8) 0.4591(4) 0.072(2) Uani 1 d . . . H35 H 0.1420 0.0721 0.4701 0.087 Uiso 1 calc R . . C36 C 0.2469(7) 0.1003(6) 0.4004(3) 0.0517(17) Uani 1 d . . . H36 H 0.1856 0.0751 0.3720 0.062 Uiso 1 calc R . . C41 C 0.4802(5) -0.0061(4) 0.3038(3) 0.0337(12) Uani 1 d . . . C42 C 0.4866(8) -0.0827(6) 0.3495(3) 0.0564(19) Uani 1 d . . . H42 H 0.4554 -0.0634 0.3851 0.068 Uiso 1 calc R . . C43 C 0.5393(9) -0.1872(6) 0.3419(4) 0.071(2) Uani 1 d . . . H43 H 0.5417 -0.2383 0.3724 0.085 Uiso 1 calc R . . C44 C 0.5879(7) -0.2168(6) 0.2907(4) 0.060(2) Uani 1 d . . . H44 H 0.6269 -0.2862 0.2870 0.072 Uiso 1 calc R . . C45 C 0.5791(7) -0.1438(6) 0.2444(4) 0.062(2) Uani 1 d . . . H45 H 0.6086 -0.1650 0.2088 0.074 Uiso 1 calc R . . C46 C 0.5259(7) -0.0383(5) 0.2512(3) 0.0485(16) Uani 1 d . . . H46 H 0.5210 0.0112 0.2201 0.058 Uiso 1 calc R . . C51 C -0.0463(6) 0.0643(4) 0.1713(2) 0.0353(12) Uani 1 d . . . C52 C 0.0260(7) 0.0255(6) 0.1272(3) 0.0537(17) Uani 1 d . . . H52 H 0.1140 0.0392 0.1295 0.064 Uiso 1 calc R . . C53 C -0.0300(10) -0.0330(7) 0.0801(3) 0.072(2) Uani 1 d . . . H53 H 0.0193 -0.0576 0.0504 0.087 Uiso 1 calc R . . C54 C -0.1604(11) -0.0542(7) 0.0776(4) 0.076(3) Uani 1 d . . . H54 H -0.1992 -0.0929 0.0458 0.092 Uiso 1 calc R . . C55 C -0.2326(8) -0.0195(6) 0.1208(4) 0.068(2) Uani 1 d . . . H55 H -0.3202 -0.0356 0.1187 0.081 Uiso 1 calc R . . C56 C -0.1764(6) 0.0407(5) 0.1687(3) 0.0514(17) Uani 1 d . . . H56 H -0.2261 0.0644 0.1984 0.062 Uiso 1 calc R . . C61 C -0.0611(5) 0.1281(5) 0.2908(2) 0.0325(12) Uani 1 d . . . C62 C -0.1167(6) 0.2134(5) 0.3213(3) 0.0407(14) Uani 1 d . . . H62 H -0.1143 0.2864 0.3075 0.049 Uiso 1 calc R . . C63 C -0.1759(7) 0.1911(6) 0.3722(3) 0.0521(17) Uani 1 d . . . H63 H -0.2133 0.2489 0.3922 0.062 Uiso 1 calc R . . C64 C -0.1791(7) 0.0829(7) 0.3930(3) 0.061(2) Uani 1 d . . . H64 H -0.2180 0.0679 0.4273 0.073 Uiso 1 calc R . . C65 C -0.1245(8) -0.0032(7) 0.3631(4) 0.068(2) Uani 1 d . . . H65 H -0.1276 -0.0760 0.3771 0.081 Uiso 1 calc R . . C66 C -0.0647(7) 0.0185(6) 0.3119(3) 0.0536(18) Uani 1 d . . . H66 H -0.0276 -0.0395 0.2920 0.064 Uiso 1 calc R . . C71 C 0.1340(6) 0.3697(5) 0.1165(2) 0.0341(12) Uani 1 d . . . C72 C 0.0483(7) 0.3225(6) 0.0748(3) 0.0491(16) Uani 1 d . . . H72 H -0.0296 0.2937 0.0856 0.059 Uiso 1 calc R . . C73 C 0.0772(9) 0.3178(7) 0.0173(3) 0.069(2) Uani 1 d . . . H73 H 0.0198 0.2843 -0.0103 0.082 Uiso 1 calc R . . C74 C 0.1910(9) 0.3628(7) 0.0007(3) 0.071(2) Uani 1 d . . . H74 H 0.2097 0.3608 -0.0382 0.086 Uiso 1 calc R . . C75 C 0.2770(8) 0.4108(8) 0.0418(3) 0.070(2) Uani 1 d . . . H75 H 0.3531 0.4423 0.0306 0.084 Uiso 1 calc R . . C76 C 0.2505(7) 0.4121(6) 0.0998(3) 0.0532(17) Uani 1 d . . . H76 H 0.3105 0.4415 0.1277 0.064 Uiso 1 calc R . . C81 C 0.0124(5) 0.5152(4) 0.1943(3) 0.0341(12) Uani 1 d . . . C82 C -0.0343(6) 0.5488(6) 0.2465(3) 0.0508(17) Uani 1 d . . . H82 H -0.0259 0.5018 0.2786 0.061 Uiso 1 calc R . . C83 C -0.0936(7) 0.6526(6) 0.2513(4) 0.061(2) Uani 1 d . . . H83 H -0.1238 0.6752 0.2865 0.073 Uiso 1 calc R . . C84 C -0.1073(7) 0.7214(6) 0.2035(4) 0.0581(19) Uani 1 d . . . H84 H -0.1488 0.7899 0.2060 0.070 Uiso 1 calc R . . C85 C -0.0601(10) 0.6889(6) 0.1530(4) 0.073(3) Uani 1 d . . . H85 H -0.0682 0.7363 0.1211 0.088 Uiso 1 calc R . . C86 C 0.0001(8) 0.5867(6) 0.1476(3) 0.0581(19) Uani 1 d . . . H86 H 0.0321 0.5663 0.1124 0.070 Uiso 1 calc R . . P11 P 0.3590(2) -0.21761(19) 0.07170(9) 0.0650(6) Uani 1 d D . . F111 F 0.4127(16) -0.2830(14) 0.1291(7) 0.107(3) Uiso 0.457(18) d PD . . F121 F 0.4424(16) -0.3069(13) 0.0376(7) 0.107(3) Uiso 0.457(18) d PD . . F131 F 0.3115(16) -0.1566(14) 0.0136(6) 0.107(3) Uiso 0.457(18) d PD . . F141 F 0.2159(12) -0.2459(15) 0.0809(8) 0.107(3) Uiso 0.457(18) d PD . . F151 F 0.3511(18) -0.1179(12) 0.1190(6) 0.107(3) Uiso 0.457(18) d PD . . F161 F 0.4819(16) -0.1466(14) 0.0902(8) 0.107(3) Uiso 0.457(18) d P . . F112 F 0.3658(16) -0.3047(13) 0.1226(7) 0.121(3) Uiso 0.543(18) d PD . . F122 F 0.3857(16) -0.3146(12) 0.0289(6) 0.121(3) Uiso 0.543(18) d PD . . F132 F 0.3507(16) -0.1282(13) 0.0206(6) 0.121(3) Uiso 0.543(18) d PD . . F142 F 0.2313(13) -0.2887(13) 0.0526(7) 0.121(3) Uiso 0.543(18) d PD . . F152 F 0.2800(17) -0.1310(12) 0.1059(6) 0.121(3) Uiso 0.543(18) d PD . . F162 F 0.5030(15) -0.1802(14) 0.0657(7) 0.121(3) Uiso 0.543(18) d P . . P21 P 0.1443(2) 0.73027(19) 0.43160(9) 0.0660(6) Uani 1 d D . . F211 F 0.110(2) 0.8261(15) 0.4753(8) 0.124(4) Uiso 0.406(12) d PD . . F221 F 0.148(2) 0.8317(15) 0.3872(8) 0.124(4) Uiso 0.406(12) d PD . . F231 F 0.133(2) 0.6345(15) 0.4780(8) 0.124(4) Uiso 0.406(12) d PD . . F241 F 0.2838(14) 0.7706(17) 0.4204(9) 0.124(4) Uiso 0.406(12) d PD . . F251 F 0.0607(19) 0.6481(15) 0.3905(8) 0.124(4) Uiso 0.406(12) d PD . . F261 F 0.166(2) 0.6367(17) 0.3855(9) 0.124(4) Uiso 0.406(12) d P . . F212 F 0.0443(14) 0.8061(13) 0.4618(7) 0.139(3) Uiso 0.594(12) d PD . . F222 F 0.0998(15) 0.8014(13) 0.3754(6) 0.139(3) Uiso 0.594(12) d PD . . F232 F 0.1859(15) 0.6649(13) 0.4899(6) 0.139(3) Uiso 0.594(12) d PD . . F242 F 0.2592(13) 0.8062(12) 0.4602(7) 0.139(3) Uiso 0.594(12) d PD . . F252 F 0.0075(12) 0.6767(12) 0.4328(7) 0.139(3) Uiso 0.594(12) d PD . . F262 F 0.2515(16) 0.6613(13) 0.4050(7) 0.139(3) Uiso 0.594(12) d P . . 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 0.0299(4) 0.0361(4) 0.0350(4) -0.0012(3) -0.0001(3) 0.0019(3) N100 0.041(3) 0.048(3) 0.040(3) 0.001(2) 0.006(2) 0.000(2) C101 0.042(3) 0.057(4) 0.036(3) 0.003(3) 0.002(3) -0.004(3) C102 0.078(6) 0.095(6) 0.040(4) 0.003(4) 0.014(4) -0.003(5) N200 0.042(3) 0.039(3) 0.059(3) -0.003(3) -0.002(3) -0.005(2) C201 0.036(3) 0.039(4) 0.065(4) -0.014(3) 0.004(3) -0.011(3) C202 0.059(5) 0.042(4) 0.100(6) -0.001(4) -0.007(5) 0.003(4) P2 0.0257(7) 0.0244(6) 0.0309(7) 0.0020(5) 0.0017(5) -0.0016(5) N3 0.021(2) 0.028(2) 0.037(2) 0.0066(19) -0.0029(19) -0.0029(19) P4 0.0288(7) 0.0242(6) 0.0293(7) 0.0020(5) 0.0001(6) -0.0017(5) Cu5 0.0285(4) 0.0462(4) 0.0348(4) -0.0008(3) -0.0007(3) 0.0032(3) N300 0.036(3) 0.060(3) 0.039(3) 0.000(2) 0.006(2) -0.001(3) C302 0.068(5) 0.093(6) 0.042(4) -0.001(4) 0.014(4) 0.003(5) C301 0.037(3) 0.059(4) 0.043(4) -0.001(3) 0.000(3) 0.002(3) P6 0.0257(7) 0.0258(6) 0.0318(7) 0.0017(5) 0.0012(6) -0.0019(5) N7 0.025(2) 0.024(2) 0.041(3) 0.0046(19) -0.001(2) -0.0009(19) P8 0.0286(7) 0.0262(7) 0.0284(7) 0.0032(5) -0.0010(6) -0.0013(6) C11 0.038(3) 0.019(2) 0.038(3) 0.002(2) -0.006(2) -0.005(2) C12 0.042(3) 0.040(3) 0.055(4) -0.008(3) -0.013(3) -0.004(3) C13 0.061(5) 0.051(4) 0.081(6) -0.002(4) -0.025(4) -0.012(4) C14 0.092(6) 0.051(4) 0.055(5) -0.008(4) -0.040(5) -0.012(5) C15 0.091(6) 0.065(5) 0.045(4) -0.014(4) -0.001(4) -0.006(5) C16 0.060(4) 0.051(4) 0.042(4) -0.012(3) 0.006(3) -0.015(3) C21 0.028(3) 0.028(3) 0.035(3) 0.004(2) 0.001(2) -0.003(2) C22 0.041(3) 0.034(3) 0.039(3) 0.001(2) 0.007(3) -0.006(3) C23 0.045(4) 0.055(4) 0.045(4) 0.001(3) 0.006(3) 0.005(3) C24 0.052(4) 0.076(5) 0.045(4) 0.013(4) 0.019(3) 0.005(4) C25 0.063(4) 0.046(4) 0.061(4) 0.022(3) 0.023(4) 0.000(3) C26 0.049(4) 0.036(3) 0.059(4) 0.010(3) 0.014(3) 0.003(3) C31 0.047(3) 0.026(3) 0.031(3) 0.003(2) 0.000(3) -0.002(2) C32 0.057(4) 0.055(4) 0.041(4) -0.006(3) 0.004(3) -0.007(3) C33 0.094(6) 0.080(6) 0.034(4) -0.014(4) 0.000(4) -0.016(5) C34 0.109(7) 0.068(5) 0.042(4) 0.000(4) 0.023(5) -0.018(5) C35 0.076(5) 0.090(6) 0.054(5) 0.010(4) 0.026(4) -0.023(5) C36 0.048(4) 0.061(4) 0.046(4) 0.006(3) 0.002(3) -0.019(3) C41 0.032(3) 0.026(3) 0.042(3) 0.006(2) -0.007(2) -0.006(2) C42 0.087(5) 0.041(4) 0.041(4) 0.008(3) 0.000(4) 0.016(4) C43 0.107(7) 0.034(4) 0.069(5) 0.012(3) -0.015(5) 0.019(4) C44 0.058(4) 0.031(3) 0.089(6) 0.003(3) -0.007(4) 0.014(3) C45 0.055(4) 0.052(4) 0.080(5) -0.007(4) 0.021(4) 0.017(4) C46 0.053(4) 0.037(3) 0.057(4) 0.008(3) 0.016(3) 0.006(3) C51 0.042(3) 0.024(3) 0.038(3) 0.003(2) -0.006(3) -0.006(2) C52 0.062(4) 0.056(4) 0.044(4) -0.014(3) 0.010(3) -0.017(4) C53 0.111(8) 0.058(5) 0.048(4) -0.018(4) 0.005(5) -0.013(5) C54 0.115(8) 0.050(4) 0.057(5) -0.005(4) -0.040(5) -0.016(5) C55 0.064(5) 0.044(4) 0.089(6) -0.007(4) -0.037(5) -0.005(4) C56 0.040(4) 0.036(3) 0.076(5) -0.009(3) -0.011(3) 0.002(3) C61 0.028(3) 0.030(3) 0.039(3) 0.005(2) 0.000(2) -0.007(2) C62 0.040(3) 0.040(3) 0.042(3) 0.003(3) 0.006(3) -0.006(3) C63 0.046(4) 0.067(5) 0.044(4) 0.000(3) 0.010(3) -0.001(3) C64 0.054(4) 0.085(6) 0.046(4) 0.016(4) 0.018(3) 0.000(4) C65 0.079(5) 0.051(4) 0.076(5) 0.028(4) 0.022(5) -0.008(4) C66 0.062(4) 0.037(3) 0.064(4) 0.015(3) 0.015(4) 0.004(3) C71 0.040(3) 0.031(3) 0.031(3) 0.007(2) 0.001(2) 0.003(2) C72 0.048(4) 0.054(4) 0.044(4) -0.003(3) -0.001(3) -0.006(3) C73 0.088(6) 0.076(5) 0.041(4) -0.014(4) 0.003(4) -0.013(5) C74 0.097(7) 0.082(6) 0.037(4) 0.003(4) 0.017(4) -0.023(5) C75 0.076(5) 0.087(6) 0.050(4) 0.010(4) 0.026(4) -0.029(5) C76 0.054(4) 0.067(4) 0.038(3) 0.006(3) 0.003(3) -0.023(4) C81 0.030(3) 0.026(3) 0.045(3) 0.007(2) -0.006(2) -0.003(2) C82 0.044(4) 0.047(4) 0.064(4) 0.020(3) 0.017(3) 0.014(3) C83 0.056(4) 0.048(4) 0.082(5) 0.007(4) 0.021(4) 0.016(3) C84 0.053(4) 0.033(3) 0.087(6) 0.006(3) -0.009(4) 0.013(3) C85 0.120(8) 0.035(4) 0.062(5) 0.013(3) -0.020(5) 0.020(4) C86 0.091(6) 0.037(3) 0.045(4) 0.003(3) -0.007(4) 0.012(4) P11 0.0735(14) 0.0651(13) 0.0581(12) 0.0008(10) 0.0169(11) -0.0054(11) P21 0.0769(14) 0.0661(13) 0.0571(12) -0.0033(10) 0.0212(11) -0.0096(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 Cu1 N100 2.054(6) . ? Cu1 N200 2.098(6) . ? Cu1 P2 2.263(3) . ? Cu1 P8 2.274(3) . ? Cu1 Cu5 2.869(4) . ? N100 C101 1.125(8) . ? C101 C102 1.463(9) . ? N200 C201 1.138(8) . ? C201 C202 1.439(10) . ? P2 N3 1.706(5) . ? P2 C11 1.825(6) . ? P2 C21 1.829(6) . ? N3 P4 1.694(5) . ? P4 C31 1.820(6) . ? P4 C41 1.828(6) . ? P4 Cu5 2.248(3) . ? Cu5 N300 1.999(6) . ? Cu5 P6 2.241(4) . ? N300 C301 1.131(8) . ? C302 C301 1.448(9) . ? P6 N7 1.705(5) . ? P6 C61 1.823(6) . ? P6 C51 1.825(6) . ? N7 P8 1.694(5) . ? P8 C71 1.819(6) . ? P8 C81 1.834(6) . ? C11 C12 1.380(9) . ? C11 C16 1.394(9) . ? C12 C13 1.396(10) . ? C13 C14 1.359(12) . ? C14 C15 1.392(12) . ? C15 C16 1.374(10) . ? C21 C22 1.381(8) . ? C21 C26 1.403(8) . ? C22 C23 1.387(8) . ? C23 C24 1.385(10) . ? C24 C25 1.383(10) . ? C25 C26 1.384(9) . ? C31 C32 1.380(9) . ? C31 C36 1.393(9) . ? C32 C33 1.381(10) . ? C33 C34 1.372(12) . ? C34 C35 1.386(12) . ? C35 C36 1.397(10) . ? C41 C46 1.385(9) . ? C41 C42 1.396(8) . ? C42 C43 1.381(10) . ? C43 C44 1.362(11) . ? C44 C45 1.379(11) . ? C45 C46 1.392(9) . ? C51 C56 1.382(9) . ? C51 C52 1.384(9) . ? C52 C53 1.380(10) . ? C53 C54 1.379(13) . ? C54 C55 1.355(13) . ? C55 C56 1.404(10) . ? C61 C62 1.385(8) . ? C61 C66 1.398(8) . ? C62 C63 1.388(9) . ? C63 C64 1.379(11) . ? C64 C65 1.381(11) . ? C65 C66 1.395(10) . ? C71 C72 1.379(9) . ? C71 C76 1.393(9) . ? C72 C73 1.379(10) . ? C73 C74 1.379(12) . ? C74 C75 1.377(12) . ? C75 C76 1.381(10) . ? C81 C86 1.377(9) . ? C81 C82 1.385(9) . ? C82 C83 1.395(9) . ? C83 C84 1.376(10) . ? C84 C85 1.350(11) . ? C85 C86 1.383(10) . ? P11 F122 1.554(13) . ? P11 F141 1.558(13) . ? P11 F161 1.564(17) . ? P11 F152 1.568(12) . ? P11 F112 1.568(13) . ? P11 F131 1.577(13) . ? P11 F162 1.580(16) . ? P11 F132 1.591(13) . ? P11 F111 1.607(13) . ? P11 F142 1.609(13) . ? P11 F121 1.614(13) . ? P11 F151 1.614(13) . ? F111 F112 0.56(2) . ? F121 F122 0.62(2) . ? F121 F162 1.74(2) . ? F131 F132 0.54(2) . ? F141 F142 0.851(17) . ? F141 F152 1.61(2) . ? F151 F152 0.796(18) . ? F151 F161 1.60(3) . ? F161 F162 0.737(17) . ? F122 F142 1.77(2) . ? P21 F262 1.550(15) . ? P21 F252 1.562(12) . ? P21 F261 1.57(2) . ? P21 F241 1.569(15) . ? P21 F251 1.575(15) . ? P21 F231 1.576(15) . ? P21 F211 1.577(15) . ? P21 F212 1.580(12) . ? P21 F221 1.590(15) . ? P21 F232 1.592(12) . ? P21 F222 1.594(13) . ? P21 F242 1.600(13) . ? F211 F212 0.77(2) . ? F211 F242 1.64(2) . ? F221 F222 0.66(2) . ? F221 F241 1.73(2) . ? F231 F232 0.70(2) . ? F231 F252 1.70(2) . ? F241 F242 1.056(19) . ? F241 F262 1.38(2) . ? F251 F261 1.13(3) . ? F251 F252 1.20(2) . ? F261 F262 1.01(2) . ? F212 F252 1.71(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 N100 Cu1 N200 99.8(2) . . ? N100 Cu1 P2 111.31(16) . . ? N200 Cu1 P2 97.13(16) . . ? N100 Cu1 P8 103.35(19) . . ? N200 Cu1 P8 96.46(16) . . ? P2 Cu1 P8 139.78(7) . . ? N100 Cu1 Cu5 92.52(16) . . ? N200 Cu1 Cu5 166.85(16) . . ? P2 Cu1 Cu5 82.53(5) . . ? P8 Cu1 Cu5 76.04(4) . . ? C101 N100 Cu1 174.6(5) . . ? N100 C101 C102 179.0(8) . . ? C201 N200 Cu1 162.1(6) . . ? N200 C201 C202 177.7(9) . . ? N3 P2 C11 103.0(2) . . ? N3 P2 C21 105.1(2) . . ? C11 P2 C21 103.7(3) . . ? N3 P2 Cu1 117.27(16) . . ? C11 P2 Cu1 111.93(19) . . ? C21 P2 Cu1 114.37(19) . . ? P4 N3 P2 119.3(3) . . ? N3 P4 C31 107.7(3) . . ? N3 P4 C41 102.3(3) . . ? C31 P4 C41 103.4(3) . . ? N3 P4 Cu5 105.38(18) . . ? C31 P4 Cu5 121.3(2) . . ? C41 P4 Cu5 115.1(2) . . ? N300 Cu5 P6 114.11(17) . . ? N300 Cu5 P4 106.61(19) . . ? P6 Cu5 P4 137.08(8) . . ? N300 Cu5 Cu1 101.39(17) . . ? P6 Cu5 Cu1 95.72(4) . . ? P4 Cu5 Cu1 88.89(6) . . ? C301 N300 Cu5 177.2(5) . . ? N300 C301 C302 178.5(8) . . ? N7 P6 C61 104.8(2) . . ? N7 P6 C51 104.9(3) . . ? C61 P6 C51 103.6(3) . . ? N7 P6 Cu5 105.19(17) . . ? C61 P6 Cu5 119.59(19) . . ? C51 P6 Cu5 117.3(2) . . ? P8 N7 P6 119.4(3) . . ? N7 P8 C71 107.9(3) . . ? N7 P8 C81 101.6(3) . . ? C71 P8 C81 102.8(3) . . ? N7 P8 Cu1 114.93(18) . . ? C71 P8 Cu1 119.8(2) . . ? C81 P8 Cu1 107.6(2) . . ? C12 C11 C16 118.4(6) . . ? C12 C11 P2 122.6(5) . . ? C16 C11 P2 118.9(5) . . ? C11 C12 C13 120.6(7) . . ? C14 C13 C12 119.6(8) . . ? C13 C14 C15 121.2(7) . . ? C16 C15 C14 118.5(7) . . ? C15 C16 C11 121.6(7) . . ? C22 C21 C26 119.5(5) . . ? C22 C21 P2 122.2(4) . . ? C26 C21 P2 118.0(4) . . ? C21 C22 C23 120.9(6) . . ? C24 C23 C22 119.6(6) . . ? C25 C24 C23 119.9(6) . . ? C24 C25 C26 121.0(6) . . ? C25 C26 C21 119.2(6) . . ? C32 C31 C36 119.9(6) . . ? C32 C31 P4 122.6(5) . . ? C36 C31 P4 117.4(5) . . ? C31 C32 C33 120.4(7) . . ? C34 C33 C32 119.9(8) . . ? C33 C34 C35 120.9(7) . . ? C34 C35 C36 119.2(7) . . ? C31 C36 C35 119.6(7) . . ? C46 C41 C42 118.5(6) . . ? C46 C41 P4 118.8(4) . . ? C42 C41 P4 122.4(5) . . ? C43 C42 C41 119.9(7) . . ? C44 C43 C42 121.2(7) . . ? C43 C44 C45 119.9(6) . . ? C44 C45 C46 119.7(7) . . ? C41 C46 C45 120.8(6) . . ? C56 C51 C52 119.1(6) . . ? C56 C51 P6 121.5(5) . . ? C52 C51 P6 119.1(5) . . ? C53 C52 C51 121.3(7) . . ? C54 C53 C52 118.9(8) . . ? C55 C54 C53 120.9(7) . . ? C54 C55 C56 120.5(8) . . ? C51 C56 C55 119.2(7) . . ? C62 C61 C66 119.3(6) . . ? C62 C61 P6 121.9(4) . . ? C66 C61 P6 118.6(5) . . ? C61 C62 C63 120.9(6) . . ? C64 C63 C62 119.8(7) . . ? C63 C64 C65 120.1(6) . . ? C64 C65 C66 120.4(7) . . ? C65 C66 C61 119.5(6) . . ? C72 C71 C76 119.2(6) . . ? C72 C71 P8 123.3(5) . . ? C76 C71 P8 117.5(5) . . ? C71 C72 C73 120.5(7) . . ? C74 C73 C72 120.2(8) . . ? C75 C74 C73 119.9(7) . . ? C74 C75 C76 120.2(7) . . ? C75 C76 C71 120.0(7) . . ? C86 C81 C82 118.6(6) . . ? C86 C81 P8 122.8(5) . . ? C82 C81 P8 118.3(4) . . ? C81 C82 C83 120.6(6) . . ? C84 C83 C82 119.6(7) . . ? C85 C84 C83 119.5(6) . . ? C84 C85 C86 121.7(7) . . ? C81 C86 C85 119.9(7) . . ? F122 P11 F141 98.4(11) . . ? F122 P11 F161 112.8(8) . . ? F141 P11 F161 148.3(12) . . ? F122 P11 F152 158.6(11) . . ? F141 P11 F152 61.8(8) . . ? F161 P11 F152 87.8(11) . . ? F122 P11 F112 88.7(9) . . ? F141 P11 F112 75.6(8) . . ? F161 P11 F112 99.2(9) . . ? F152 P11 F112 93.6(8) . . ? F122 P11 F131 82.5(9) . . ? F141 P11 F131 88.1(8) . . ? F161 P11 F131 100.6(9) . . ? F152 P11 F131 88.4(9) . . ? F112 P11 F131 160.2(8) . . ? F122 P11 F162 86.3(8) . . ? F141 P11 F162 175.3(12) . . ? F161 P11 F162 27.1(6) . . ? F152 P11 F162 113.5(11) . . ? F112 P11 F162 104.8(8) . . ? F131 P11 F162 92.4(9) . . ? F122 P11 F132 92.0(9) . . ? F141 P11 F132 103.9(8) . . ? F161 P11 F132 80.9(9) . . ? F152 P11 F132 85.6(8) . . ? F112 P11 F132 179.2(9) . . ? F131 P11 F132 19.8(8) . . ? F162 P11 F132 75.7(8) . . ? F122 P11 F111 95.0(9) . . ? F141 P11 F111 93.9(8) . . ? F161 P11 F111 78.9(9) . . ? F152 P11 F111 94.5(9) . . ? F112 P11 F111 20.4(8) . . ? F131 P11 F111 177.1(9) . . ? F162 P11 F111 85.9(9) . . ? F132 P11 F111 159.8(8) . . ? F122 P11 F142 67.9(10) . . ? F141 P11 F142 31.1(6) . . ? F161 P11 F142 179.0(9) . . ? F152 P11 F142 91.4(7) . . ? F112 P11 F142 81.4(8) . . ? F131 P11 F142 78.8(8) . . ? F162 P11 F142 153.5(11) . . ? F132 P11 F142 98.5(8) . . ? F111 P11 F142 101.8(8) . . ? F122 P11 F121 22.4(7) . . ? F141 P11 F121 118.8(11) . . ? F161 P11 F121 91.4(8) . . ? F152 P11 F121 178.9(10) . . ? F112 P11 F121 85.7(9) . . ? F131 P11 F121 92.6(9) . . ? F162 P11 F121 65.9(8) . . ? F132 P11 F121 95.1(9) . . ? F111 P11 F121 84.6(9) . . ? F142 P11 F121 89.4(10) . . ? F122 P11 F151 172.4(11) . . ? F141 P11 F151 88.1(8) . . ? F161 P11 F151 60.3(11) . . ? F152 P11 F151 28.9(6) . . ? F112 P11 F151 89.2(9) . . ? F131 P11 F151 101.6(9) . . ? F162 P11 F151 87.2(11) . . ? F132 P11 F151 90.1(8) . . ? F111 P11 F151 80.6(9) . . ? F142 P11 F151 119.0(8) . . ? F121 P11 F151 150.1(11) . . ? F112 F111 P11 76(2) . . ? F122 F121 P11 73.3(19) . . ? F122 F121 F162 124(2) . . ? P11 F121 F162 56.1(7) . . ? F132 F131 P11 82(2) . . ? F142 F141 P11 77.7(13) . . ? F142 F141 F152 133.2(17) . . ? P11 F141 F152 59.4(7) . . ? F152 F151 F161 127.0(18) . . ? F152 F151 P11 72.3(14) . . ? F161 F151 P11 58.3(8) . . ? F162 F161 P11 78(2) . . ? F162 F161 F151 138(3) . . ? P11 F161 F151 61.4(9) . . ? F111 F112 P11 84(2) . . ? F121 F122 P11 84(2) . . ? F121 F122 F142 139(2) . . ? P11 F122 F142 57.5(7) . . ? F131 F132 P11 79(2) . . ? F141 F142 P11 71.1(13) . . ? F141 F142 F122 124.6(16) . . ? P11 F142 F122 54.6(7) . . ? F151 F152 P11 78.8(14) . . ? F151 F152 F141 130.5(19) . . ? P11 F152 F141 58.8(7) . . ? F161 F162 P11 75(2) . . ? F161 F162 F121 129(2) . . ? P11 F162 F121 58.0(7) . . ? F262 P21 F252 118.5(9) . . ? F262 P21 F261 37.8(8) . . ? F252 P21 F261 84.5(11) . . ? F262 P21 F241 52.6(8) . . ? F252 P21 F241 169.7(10) . . ? F261 P21 F241 85.4(11) . . ? F262 P21 F251 79.6(10) . . ? F252 P21 F251 45.1(8) . . ? F261 P21 F251 42.0(10) . . ? F241 P21 F251 124.6(12) . . ? F262 P21 F231 88.2(10) . . ? F252 P21 F231 65.5(9) . . ? F261 P21 F231 87.9(11) . . ? F241 P21 F231 116.2(10) . . ? F251 P21 F231 84.0(10) . . ? F262 P21 F211 146.9(10) . . ? F252 P21 F211 91.8(10) . . ? F261 P21 F211 175.0(11) . . ? F241 P21 F211 98.1(11) . . ? F251 P21 F211 133.4(12) . . ? F231 P21 F211 93.6(11) . . ? F262 P21 F212 175.1(9) . . ? F252 P21 F212 65.9(8) . . ? F261 P21 F212 147.1(11) . . ? F241 P21 F212 123.3(10) . . ? F251 P21 F212 105.3(10) . . ? F231 P21 F212 92.2(10) . . ? F211 P21 F212 28.2(8) . . ? F262 P21 F221 96.1(10) . . ? F252 P21 F221 112.4(9) . . ? F261 P21 F221 95.5(11) . . ? F241 P21 F221 66.6(10) . . ? F251 P21 F221 96.9(10) . . ? F231 P21 F221 175.8(11) . . ? F211 P21 F221 82.7(11) . . ? F212 P21 F221 83.6(10) . . ? F262 P21 F232 84.6(8) . . ? F252 P21 F232 88.9(8) . . ? F261 P21 F232 100.1(9) . . ? F241 P21 F232 94.9(9) . . ? F251 P21 F232 108.0(9) . . ? F231 P21 F232 25.4(9) . . ? F211 P21 F232 83.2(9) . . ? F212 P21 F232 93.6(8) . . ? F221 P21 F232 154.8(10) . . ? F262 P21 F222 98.3(8) . . ? F252 P21 F222 91.0(8) . . ? F261 P21 F222 83.1(9) . . ? F241 P21 F222 85.8(9) . . ? F251 P21 F222 74.1(9) . . ? F231 P21 F222 155.5(10) . . ? F211 P21 F222 93.6(10) . . ? F212 P21 F222 83.4(8) . . ? F221 P21 F222 23.8(9) . . ? F232 P21 F222 176.8(8) . . ? F262 P21 F242 85.4(8) . . ? F252 P21 F242 151.3(9) . . ? F261 P21 F242 122.3(10) . . ? F241 P21 F242 38.9(7) . . ? F251 P21 F242 163.5(10) . . ? F231 P21 F242 102.4(10) . . ? F211 P21 F242 62.0(9) . . ? F212 P21 F242 89.8(8) . . ? F221 P21 F242 77.8(9) . . ? F232 P21 F242 77.1(8) . . ? F222 P21 F242 101.6(8) . . ? F212 F211 P21 76.1(16) . . ? F212 F211 F242 135(2) . . ? P21 F211 F242 59.7(7) . . ? F222 F221 P21 78.5(19) . . ? F222 F221 F241 122(3) . . ? P21 F221 F241 56.1(8) . . ? F232 F231 P21 78.5(18) . . ? F232 F231 F252 130(2) . . ? P21 F231 F252 56.9(7) . . ? F242 F241 F262 121.9(18) . . ? F242 F241 P21 72.2(11) . . ? F262 F241 P21 63.0(9) . . ? F242 F241 F221 88.3(16) . . ? F262 F241 F221 96.4(14) . . ? P21 F241 F221 57.3(8) . . ? F261 F251 F252 129.0(19) . . ? F261 F251 P21 68.6(14) . . ? F252 F251 P21 66.9(9) . . ? F262 F261 F251 139(2) . . ? F262 F261 P21 70.3(16) . . ? F251 F261 P21 69.4(13) . . ? F211 F212 P21 75.6(16) . . ? F211 F212 F252 127(2) . . ? P21 F212 F252 56.6(6) . . ? F221 F222 P21 77.8(19) . . ? F231 F232 P21 76.1(18) . . ? F241 F242 P21 68.9(11) . . ? F241 F242 F211 122.4(15) . . ? P21 F242 F211 58.3(7) . . ? F251 F252 P21 68.0(9) . . ? F251 F252 F231 91.7(14) . . ? P21 F252 F231 57.7(7) . . ? F251 F252 F212 117.8(13) . . ? P21 F252 F212 57.6(6) . . ? F231 F252 F212 83.8(11) . . ? F261 F262 F241 125(2) . . ? F261 F262 P21 71.9(15) . . ? F241 F262 P21 64.4(9) . . ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 26.13 _diffrn_measured_fraction_theta_full 0.875 _refine_diff_density_max 1.587 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.107 #==END data_compound_3 _database_code_CSD 188191 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H66 Cu2 F12 N6 O2 P6' _chemical_formula_weight 1468.11 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 14.776(22) _cell_length_b 14.433(22) _cell_length_c 17.546(27) _cell_angle_alpha 90.00 _cell_angle_beta 99.34(1) _cell_angle_gamma 90.00 _cell_volume 3692(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour White _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type 'No absorption correction' _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 'MAR research image plate system' _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 11992 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.1065 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.01 _reflns_number_total 6920 _reflns_number_gt 3247 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'W. Kabsch, J. Appl. Crystallogr. 21,916,1983' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.2000P)^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 0.0058(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6920 _refine_ls_number_parameters 398 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.2088 _refine_ls_R_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.3393 _refine_ls_wR_factor_gt 0.2840 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.089 _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 0.57452(7) 0.93013(8) 0.55403(7) 0.0642(5) Uani 1 d . . . P2 P 0.49510(15) 0.82068(15) 0.47979(12) 0.0499(6) Uani 1 d . . . N3 N 0.4523(5) 0.8531(5) 0.3878(4) 0.0548(17) Uani 1 d D . . HN3 H 0.4296 0.8111 0.3555 0.066 Uiso 1 calc RD . . P4 P 0.54786(14) 1.03592(16) 0.64305(12) 0.0500(6) Uani 1 d . . . C11 C 0.5650(6) 0.7190(6) 0.4635(5) 0.057(2) Uani 1 d . . . C12 C 0.6595(7) 0.7326(7) 0.4614(6) 0.074(3) Uani 1 d . . . H12 H 0.6845 0.7914 0.4709 0.089 Uiso 1 calc R . . C13 C 0.7149(9) 0.6616(10) 0.4458(6) 0.093(4) Uani 1 d . . . H13 H 0.7771 0.6709 0.4453 0.112 Uiso 1 calc R . . C14 C 0.6741(11) 0.5740(8) 0.4305(7) 0.100(4) Uani 1 d . . . H14 H 0.7099 0.5241 0.4199 0.120 Uiso 1 calc R . . C15 C 0.5839(10) 0.5614(8) 0.4311(8) 0.104(4) Uani 1 d . . . H15 H 0.5587 0.5029 0.4204 0.125 Uiso 1 calc R . . C16 C 0.5271(7) 0.6338(7) 0.4475(6) 0.076(3) Uani 1 d . . . H16 H 0.4649 0.6239 0.4474 0.091 Uiso 1 calc R . . C21 C 0.4002(6) 0.7666(5) 0.5172(5) 0.053(2) Uani 1 d . . . C22 C 0.4156(7) 0.7294(7) 0.5900(6) 0.072(3) Uani 1 d . . . H22 H 0.4747 0.7322 0.6181 0.086 Uiso 1 calc R . . C23 C 0.3467(7) 0.6872(7) 0.6243(6) 0.080(3) Uani 1 d . . . H23 H 0.3594 0.6611 0.6734 0.096 Uiso 1 calc R . . C24 C 0.2606(7) 0.6861(8) 0.5831(7) 0.078(3) Uani 1 d . . . H24 H 0.2126 0.6611 0.6047 0.094 Uiso 1 calc R . . C25 C 0.2444(7) 0.7209(8) 0.5114(8) 0.094(4) Uani 1 d . . . H25 H 0.1856 0.7156 0.4832 0.113 Uiso 1 calc R . . C26 C 0.3111(6) 0.7641(7) 0.4776(5) 0.066(2) Uani 1 d . . . H26 H 0.2965 0.7911 0.4290 0.079 Uiso 1 calc R . . C31 C 0.4456(5) 1.0223(6) 0.6876(5) 0.055(2) Uani 1 d . . . C32 C 0.3854(7) 1.0959(8) 0.6942(5) 0.073(3) Uani 1 d . . . H32 H 0.3989 1.1549 0.6778 0.088 Uiso 1 calc R . . C33 C 0.3068(7) 1.0814(10) 0.7247(6) 0.091(4) Uani 1 d . . . H33 H 0.2661 1.1303 0.7262 0.110 Uiso 1 calc R . . C34 C 0.2868(7) 0.9966(11) 0.7530(7) 0.096(4) Uani 1 d . . . H34 H 0.2343 0.9880 0.7750 0.115 Uiso 1 calc R . . C35 C 0.3465(10) 0.9247(10) 0.7479(8) 0.111(5) Uani 1 d . . . H35 H 0.3345 0.8673 0.7682 0.133 Uiso 1 calc R . . C36 C 0.4241(8) 0.9350(8) 0.7135(7) 0.086(3) Uani 1 d . . . H36 H 0.4613 0.8843 0.7078 0.103 Uiso 1 calc R . . C41 C 0.6429(6) 1.0396(6) 0.7264(5) 0.060(2) Uani 1 d . . . C42 C 0.7313(7) 1.0419(8) 0.7121(6) 0.084(3) Uani 1 d . . . H42 H 0.7425 1.0405 0.6615 0.101 Uiso 1 calc R . . C43 C 0.8048(8) 1.0464(9) 0.7733(8) 0.099(4) Uani 1 d . . . H43 H 0.8644 1.0487 0.7627 0.119 Uiso 1 calc R . . C44 C 0.7908(10) 1.0475(12) 0.8469(9) 0.135(6) Uani 1 d . . . H44 H 0.8399 1.0485 0.8875 0.161 Uiso 1 calc R . . C45 C 0.7009(12) 1.0470(14) 0.8608(8) 0.155(7) Uani 1 d . . . H45 H 0.6899 1.0477 0.9115 0.186 Uiso 1 calc R . . C46 C 0.6279(9) 1.0454(12) 0.8014(6) 0.122(5) Uani 1 d . . . H46 H 0.5683 1.0483 0.8119 0.146 Uiso 1 calc R . . N100 N 0.6819(5) 0.9777(6) 0.5070(4) 0.065(2) Uani 1 d . . . C101 C 0.7440(7) 1.0060(7) 0.4827(5) 0.069(3) Uani 1 d . . . C102 C 0.8198(7) 1.0377(10) 0.4481(7) 0.108(4) Uani 1 d . . . H10A H 0.8397 0.9889 0.4176 0.130 Uiso 1 calc R . . H10B H 0.8694 1.0553 0.4879 0.130 Uiso 1 calc R . . H10C H 0.8012 1.0902 0.4158 0.130 Uiso 1 calc R . . N200 N 0.6476(6) 0.8308(7) 0.6413(6) 0.089(3) Uani 1 d . . . C201 C 0.6787(8) 0.8132(8) 0.7023(8) 0.088(3) Uani 1 d . . . C202 C 0.7187(9) 0.7911(10) 0.7805(7) 0.120(5) Uani 1 d . . . H20A H 0.7828 0.7780 0.7828 0.144 Uiso 1 calc R . . H20B H 0.6885 0.7379 0.7974 0.144 Uiso 1 calc R . . H20C H 0.7115 0.8428 0.8134 0.144 Uiso 1 calc R . . P5 P 0.4926(2) 0.6655(3) 0.8624(2) 0.1103(13) Uani 1 d D . . F511 F 0.5919(7) 0.6257(10) 0.8723(8) 0.155(4) Uiso 0.642(15) d PD . . F521 F 0.5053(9) 0.6890(11) 0.7742(7) 0.155(4) Uiso 0.642(15) d PD . . F531 F 0.3933(8) 0.7138(9) 0.8414(8) 0.155(4) Uiso 0.642(15) d PD . . F541 F 0.4459(9) 0.5747(8) 0.8286(8) 0.155(4) Uiso 0.642(15) d PD . . F551 F 0.5279(9) 0.7674(9) 0.8846(9) 0.155(4) Uiso 0.642(15) d PD . . F561 F 0.4804(9) 0.6437(11) 0.9449(7) 0.155(4) Uiso 0.642(15) d PD . . F522 F 0.5005(14) 0.7477(14) 0.8081(13) 0.151(7) Uiso 0.358(15) d PD . . F542 F 0.4935(15) 0.5983(13) 0.8044(10) 0.151(7) Uiso 0.358(15) d PD . . F512 F 0.5987(9) 0.6591(16) 0.8880(14) 0.151(7) Uiso 0.358(15) d PD . . F562 F 0.4839(15) 0.5697(14) 0.9206(13) 0.151(7) Uiso 0.358(15) d PD . . F532 F 0.3903(12) 0.6721(15) 0.8575(13) 0.151(7) Uiso 0.358(15) d PD . . F552 F 0.5248(16) 0.7069(15) 0.9296(10) 0.151(7) Uiso 0.358(15) d PD . . O50 O 0.4328(7) 0.7201(7) 0.2508(6) 0.123(3) Uani 1 d . . . C51 C 0.4644(11) 0.6850(9) 0.2024(10) 0.114(5) Uani 1 d . . . C52 C 0.5662(13) 0.6627(15) 0.2098(12) 0.198(10) Uani 1 d . . . H52A H 0.5761 0.6226 0.1683 0.237 Uiso 1 calc R . . H52B H 0.5865 0.6325 0.2583 0.237 Uiso 1 calc R . . H52C H 0.6002 0.7191 0.2074 0.237 Uiso 1 calc R . . C53 C 0.4025(14) 0.6644(19) 0.1230(11) 0.223(13) Uani 1 d . . . H53A H 0.4058 0.7154 0.0885 0.268 Uiso 1 calc R . . H53B H 0.3401 0.6562 0.1307 0.268 Uiso 1 calc R . . H53C H 0.4235 0.6090 0.1011 0.268 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 0.0679(7) 0.0663(8) 0.0608(8) -0.0184(5) 0.0175(5) -0.0096(5) P2 0.0582(12) 0.0473(13) 0.0434(12) 0.0003(10) 0.0057(10) 0.0021(10) N3 0.071(4) 0.047(4) 0.047(4) -0.008(3) 0.009(3) -0.001(3) P4 0.0586(12) 0.0518(13) 0.0388(11) -0.0006(9) 0.0058(9) 0.0037(10) C11 0.067(5) 0.055(6) 0.051(5) 0.005(4) 0.011(4) 0.005(4) C12 0.092(7) 0.061(6) 0.069(7) -0.003(5) 0.012(5) 0.018(5) C13 0.104(8) 0.110(10) 0.066(7) 0.006(7) 0.016(6) 0.037(8) C14 0.151(12) 0.069(8) 0.086(9) -0.005(6) 0.035(8) 0.038(8) C15 0.125(11) 0.073(8) 0.124(11) 0.005(7) 0.047(9) -0.002(8) C16 0.091(7) 0.053(6) 0.086(7) -0.010(5) 0.023(6) 0.009(5) C21 0.068(5) 0.042(5) 0.051(5) 0.000(4) 0.015(4) 0.001(4) C22 0.083(6) 0.068(6) 0.061(6) 0.012(5) 0.004(5) -0.006(5) C23 0.083(7) 0.083(7) 0.077(7) 0.022(6) 0.024(6) -0.010(6) C24 0.076(7) 0.084(8) 0.075(7) 0.009(6) 0.014(6) -0.017(5) C25 0.065(6) 0.097(9) 0.116(10) 0.006(8) 0.003(6) -0.002(6) C26 0.060(5) 0.080(7) 0.053(5) 0.015(5) 0.000(4) -0.007(5) C31 0.052(4) 0.069(6) 0.044(5) 0.003(4) 0.004(4) 0.001(4) C32 0.082(6) 0.085(7) 0.054(6) 0.001(5) 0.014(5) 0.015(6) C33 0.075(7) 0.136(12) 0.066(7) -0.012(7) 0.019(6) 0.010(7) C34 0.075(7) 0.140(12) 0.079(8) -0.005(8) 0.030(6) 0.002(8) C35 0.128(10) 0.120(11) 0.096(10) 0.001(8) 0.052(8) -0.039(9) C36 0.095(7) 0.079(8) 0.092(8) 0.004(6) 0.040(6) 0.006(6) C41 0.070(6) 0.060(6) 0.049(5) 0.004(4) 0.005(4) 0.004(4) C42 0.068(6) 0.113(9) 0.066(7) -0.017(6) -0.002(5) -0.021(6) C43 0.076(7) 0.110(10) 0.104(10) -0.002(8) -0.011(7) -0.010(6) C44 0.093(10) 0.220(18) 0.077(10) -0.011(10) -0.025(8) -0.009(10) C45 0.144(14) 0.27(2) 0.048(7) -0.025(10) -0.006(8) -0.003(14) C46 0.086(8) 0.225(17) 0.050(7) -0.010(8) -0.002(6) 0.018(9) N100 0.074(5) 0.071(5) 0.050(4) -0.014(4) 0.010(4) -0.004(4) C101 0.068(6) 0.079(7) 0.061(6) -0.007(5) 0.017(5) -0.006(5) C102 0.081(7) 0.163(12) 0.091(9) -0.025(8) 0.043(6) -0.039(8) N200 0.090(6) 0.089(7) 0.078(7) 0.006(5) -0.014(5) 0.011(5) C201 0.075(7) 0.081(8) 0.103(10) 0.000(7) -0.002(7) -0.001(6) C202 0.129(11) 0.123(11) 0.098(10) 0.047(9) -0.008(8) 0.005(9) P5 0.087(2) 0.137(3) 0.101(3) 0.014(2) -0.0039(19) -0.015(2) O50 0.142(8) 0.124(8) 0.103(7) -0.043(6) 0.020(6) 0.018(6) C51 0.131(11) 0.089(9) 0.130(12) -0.048(9) 0.040(10) -0.003(8) C52 0.176(18) 0.21(2) 0.21(2) -0.083(18) 0.051(16) 0.038(15) C53 0.188(19) 0.36(4) 0.139(17) -0.09(2) 0.066(15) -0.07(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 Cu1 N100 2.023(9) . ? Cu1 N200 2.242(10) . ? Cu1 P2 2.252(3) . ? Cu1 P4 2.264(3) . ? P2 N3 1.701(7) . ? P2 C21 1.818(8) . ? P2 C11 1.843(9) . ? N3 P4 1.690(7) 3_676 ? P4 N3 1.690(7) 3_676 ? P4 C31 1.821(9) . ? P4 C41 1.856(9) . ? C11 C16 1.363(13) . ? C11 C12 1.415(13) . ? C12 C13 1.366(14) . ? C13 C14 1.408(16) . ? C14 C15 1.346(18) . ? C15 C16 1.398(15) . ? C21 C22 1.371(12) . ? C21 C26 1.386(12) . ? C22 C23 1.404(13) . ? C23 C24 1.357(14) . ? C24 C25 1.340(15) . ? C25 C26 1.379(14) . ? C31 C36 1.394(13) . ? C31 C32 1.402(13) . ? C32 C33 1.372(14) . ? C33 C34 1.371(17) . ? C34 C35 1.374(18) . ? C35 C36 1.388(16) . ? C41 C42 1.369(13) . ? C41 C46 1.372(14) . ? C42 C43 1.399(14) . ? C43 C44 1.340(18) . ? C44 C45 1.39(2) . ? C45 C46 1.374(17) . ? N100 C101 1.149(11) . ? C101 C102 1.433(13) . ? N200 C201 1.124(14) . ? C201 C202 1.438(17) . ? P5 F552 1.337(14) . ? P5 F542 1.409(13) . ? P5 F532 1.503(18) . ? P5 F561 1.519(12) . ? P5 F522 1.538(14) . ? P5 F541 1.554(12) . ? P5 F511 1.559(11) . ? P5 F512 1.562(13) . ? P5 F551 1.587(12) . ? P5 F531 1.612(13) . ? P5 F521 1.626(12) . ? P5 F562 1.735(15) . ? F511 F512 0.56(3) . ? F511 F542 1.77(2) . ? F521 F522 1.05(2) . ? F521 F542 1.43(2) . ? F531 F532 0.67(2) . ? F541 F542 0.94(2) . ? F541 F562 1.62(2) . ? F541 F532 1.74(2) . ? F551 F552 1.18(2) . ? F551 F522 1.37(2) . ? F561 F562 1.15(2) . ? F561 F552 1.18(2) . ? F512 F552 1.57(3) . ? O50 C51 1.150(14) . ? C51 C52 1.52(2) . ? C51 C53 1.57(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 N100 Cu1 N200 99.9(4) . . ? N100 Cu1 P2 111.8(2) . . ? N200 Cu1 P2 95.4(3) . . ? N100 Cu1 P4 106.7(2) . . ? N200 Cu1 P4 94.5(3) . . ? P2 Cu1 P4 137.67(11) . . ? N3 P2 C21 105.7(4) . . ? N3 P2 C11 101.7(4) . . ? C21 P2 C11 101.5(4) . . ? N3 P2 Cu1 115.7(3) . . ? C21 P2 Cu1 116.9(3) . . ? C11 P2 Cu1 113.3(3) . . ? P4 N3 P2 123.1(4) 3_676 . ? N3 P4 C31 106.4(4) 3_676 . ? N3 P4 C41 100.7(4) 3_676 . ? C31 P4 C41 103.9(4) . . ? N3 P4 Cu1 114.2(3) 3_676 . ? C31 P4 Cu1 118.2(3) . . ? C41 P4 Cu1 111.6(3) . . ? C16 C11 C12 119.6(8) . . ? C16 C11 P2 121.9(7) . . ? C12 C11 P2 118.3(7) . . ? C13 C12 C11 121.8(11) . . ? C12 C13 C14 117.4(12) . . ? C15 C14 C13 120.8(11) . . ? C14 C15 C16 121.9(12) . . ? C11 C16 C15 118.5(10) . . ? C22 C21 C26 117.3(8) . . ? C22 C21 P2 118.9(7) . . ? C26 C21 P2 123.8(7) . . ? C21 C22 C23 123.2(9) . . ? C24 C23 C22 117.3(10) . . ? C25 C24 C23 120.4(10) . . ? C24 C25 C26 122.8(10) . . ? C25 C26 C21 118.9(9) . . ? C36 C31 C32 118.5(9) . . ? C36 C31 P4 119.1(7) . . ? C32 C31 P4 122.3(7) . . ? C33 C32 C31 120.3(11) . . ? C34 C33 C32 121.6(11) . . ? C33 C34 C35 118.2(11) . . ? C34 C35 C36 122.2(12) . . ? C35 C36 C31 119.1(11) . . ? C42 C41 C46 118.8(9) . . ? C42 C41 P4 118.6(7) . . ? C46 C41 P4 122.5(8) . . ? C41 C42 C43 120.4(11) . . ? C44 C43 C42 121.2(12) . . ? C43 C44 C45 118.1(12) . . ? C46 C45 C44 121.4(13) . . ? C41 C46 C45 120.0(12) . . ? C101 N100 Cu1 177.8(7) . . ? N100 C101 C102 176.4(11) . . ? C201 N200 Cu1 150.7(10) . . ? N200 C201 C202 179.8(11) . . ? F552 P5 F542 154.3(13) . . ? F552 P5 F532 103.5(11) . . ? F542 P5 F532 97.5(10) . . ? F552 P5 F561 48.2(10) . . ? F542 P5 F561 124.2(10) . . ? F532 P5 F561 78.2(10) . . ? F552 P5 F522 98.6(10) . . ? F542 P5 F522 94.1(10) . . ? F532 P5 F522 95.3(9) . . ? F561 P5 F522 141.5(10) . . ? F552 P5 F541 141.8(11) . . ? F542 P5 F541 36.7(9) . . ? F532 P5 F541 69.6(10) . . ? F561 P5 F541 94.3(7) . . ? F522 P5 F541 119.2(10) . . ? F552 P5 F511 82.7(12) . . ? F542 P5 F511 73.0(10) . . ? F532 P5 F511 161.7(10) . . ? F561 P5 F511 94.2(7) . . ? F522 P5 F511 100.8(10) . . ? F541 P5 F511 94.8(7) . . ? F552 P5 F512 65.0(13) . . ? F542 P5 F512 92.2(10) . . ? F532 P5 F512 166.8(12) . . ? F561 P5 F512 89.0(11) . . ? F522 P5 F512 92.9(9) . . ? F541 P5 F512 114.9(10) . . ? F511 P5 F512 20.5(11) . . ? F552 P5 F551 46.8(9) . . ? F542 P5 F551 140.6(10) . . ? F532 P5 F551 104.1(10) . . ? F561 P5 F551 92.5(7) . . ? F522 P5 F551 51.8(9) . . ? F541 P5 F551 169.5(7) . . ? F511 P5 F551 92.7(7) . . ? F512 P5 F551 73.1(10) . . ? F552 P5 F531 100.9(12) . . ? F542 P5 F531 104.3(11) . . ? F532 P5 F531 24.5(9) . . ? F561 P5 F531 93.7(7) . . ? F522 P5 F531 71.5(9) . . ? F541 P5 F531 86.9(6) . . ? F511 P5 F531 171.8(8) . . ? F512 P5 F531 157.7(10) . . ? F551 P5 F531 84.7(6) . . ? F552 P5 F521 131.8(11) . . ? F542 P5 F521 55.8(9) . . ? F532 P5 F521 101.7(10) . . ? F561 P5 F521 179.9(7) . . ? F522 P5 F521 38.5(9) . . ? F541 P5 F521 85.7(7) . . ? F511 P5 F521 86.0(7) . . ? F512 P5 F521 91.1(11) . . ? F551 P5 F521 87.5(6) . . ? F531 P5 F521 86.2(6) . . ? F552 P5 F562 83.6(9) . . ? F542 P5 F562 83.5(9) . . ? F532 P5 F562 85.1(8) . . ? F561 P5 F562 40.9(8) . . ? F522 P5 F562 177.6(11) . . ? F541 P5 F562 58.7(9) . . ? F511 P5 F562 78.4(10) . . ? F512 P5 F562 87.1(9) . . ? F551 P5 F562 130.3(9) . . ? F531 P5 F562 109.2(9) . . ? F521 P5 F562 139.1(9) . . ? F512 F511 P5 80.1(19) . . ? F512 F511 F542 126(2) . . ? P5 F511 F542 49.6(6) . . ? F522 F521 F542 120.4(13) . . ? F522 F521 P5 66.2(10) . . ? F542 F521 P5 54.4(7) . . ? F532 F531 P5 68.5(19) . . ? F542 F541 P5 63.2(10) . . ? F542 F541 F562 107.6(16) . . ? P5 F541 F562 66.2(8) . . ? F542 F541 F532 105.1(15) . . ? P5 F541 F532 53.8(7) . . ? F562 F541 F532 81.4(10) . . ? F552 F551 F522 117.7(13) . . ? F552 F551 P5 55.4(8) . . ? F522 F551 P5 62.2(8) . . ? F562 F561 F552 124.9(18) . . ? F562 F561 P5 79.7(10) . . ? F552 F561 P5 57.8(8) . . ? F521 F522 F551 133.7(17) . . ? F521 F522 P5 75.3(11) . . ? F551 F522 P5 65.9(8) . . ? F541 F542 P5 80.0(12) . . ? F541 F542 F521 130(2) . . ? P5 F542 F521 69.8(8) . . ? F541 F542 F511 111.6(17) . . ? P5 F542 F511 57.4(7) . . ? F521 F542 F511 84.8(11) . . ? F511 F512 P5 79.4(17) . . ? F511 F512 F552 122(3) . . ? P5 F512 F552 50.6(8) . . ? F561 F562 F541 107.3(13) . . ? F561 F562 P5 59.5(8) . . ? F541 F562 P5 55.0(6) . . ? F531 F532 P5 87(2) . . ? F531 F532 F541 122(3) . . ? P5 F532 F541 56.6(7) . . ? F561 F552 F551 143.8(19) . . ? F561 F552 P5 74.0(10) . . ? F551 F552 P5 77.8(11) . . ? F561 F552 F512 102.7(16) . . ? F551 F552 F512 84.8(16) . . ? P5 F552 F512 64.5(10) . . ? O50 C51 C52 123.0(15) . . ? O50 C51 C53 119.4(15) . . ? C52 C51 C53 117.5(14) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.278 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.136 #==END data_compound_4 _database_code_CSD 188192 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ag2(dppa)2(CH3CN)2][PF6]2 _chemical_formula_sum 'C52 H48 Ag2 F12 N4 O0 P6' _chemical_formula_weight 1358.50 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 12.845(19) _cell_length_b 15.362(22) _cell_length_c 15.613(23) _cell_angle_alpha 90.00 _cell_angle_beta 110.90(1) _cell_angle_gamma 90.00 _cell_volume 2878(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour White _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type No absorption correction _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 'MAR research image plate system' _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 10069 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.06 _reflns_number_total 5629 _reflns_number_gt 3878 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'W. Kabsch, J. Appl. Crystallogr. 21,916,1983' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^+0.2216P] 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 0.0012(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5629 _refine_ls_number_parameters 349 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.52671(4) 0.42225(3) 0.06000(3) 0.0536(2) Uani 1 d . . . P2 P 0.35001(12) 0.35148(9) -0.02414(9) 0.0477(4) Uani 1 d . . . N3 N 0.2947(4) 0.4022(3) -0.1267(3) 0.0481(10) Uani 1 d D . . HN3 H 0.231(2) 0.379(3) -0.156(3) 0.049(15) Uiso 1 d D . . P4 P 0.37175(11) 0.46549(9) -0.16932(9) 0.0461(3) Uani 1 d . . . N100 N 0.6757(5) 0.3529(4) 0.0295(5) 0.0861(18) Uani 1 d . . . C101 C 0.7391(7) 0.3195(5) 0.0073(5) 0.079(2) Uani 1 d . . . C102 C 0.8187(9) 0.2739(8) -0.0227(6) 0.134(4) Uani 1 d . . . H10A H 0.7986 0.2135 -0.0320 0.161 Uiso 1 calc R . . H10B H 0.8918 0.2792 0.0233 0.161 Uiso 1 calc R . . H10C H 0.8185 0.2988 -0.0791 0.161 Uiso 1 calc R . . C31 C 0.2670(5) 0.5070(4) -0.2729(4) 0.0502(12) Uani 1 d . . . C32 C 0.2651(7) 0.4849(5) -0.3588(4) 0.080(2) Uani 1 d . . . H32 H 0.3187 0.4478 -0.3658 0.096 Uiso 1 calc R . . C33 C 0.1801(8) 0.5196(6) -0.4363(5) 0.098(3) Uani 1 d . . . H33 H 0.1778 0.5051 -0.4948 0.117 Uiso 1 calc R . . C34 C 0.1001(7) 0.5749(5) -0.4261(5) 0.083(2) Uani 1 d . . . H34 H 0.0444 0.5975 -0.4774 0.099 Uiso 1 calc R . . C35 C 0.1037(6) 0.5957(5) -0.3410(5) 0.079(2) Uani 1 d . . . H35 H 0.0492 0.6319 -0.3340 0.095 Uiso 1 calc R . . C36 C 0.1878(6) 0.5638(5) -0.2642(5) 0.0699(17) Uani 1 d . . . H36 H 0.1909 0.5807 -0.2061 0.084 Uiso 1 calc R . . C41 C 0.4568(5) 0.3919(4) -0.2086(4) 0.0552(14) Uani 1 d . . . C42 C 0.4292(6) 0.3067(5) -0.2333(4) 0.0721(18) Uani 1 d . . . H42 H 0.3625 0.2839 -0.2324 0.086 Uiso 1 calc R . . C43 C 0.5025(9) 0.2538(6) -0.2602(6) 0.099(3) Uani 1 d . . . H43 H 0.4841 0.1961 -0.2766 0.119 Uiso 1 calc R . . C44 C 0.6001(9) 0.2874(7) -0.2620(6) 0.105(3) Uani 1 d . . . H44 H 0.6488 0.2519 -0.2781 0.126 Uiso 1 calc R . . C45 C 0.6270(7) 0.3735(8) -0.2401(6) 0.100(3) Uani 1 d . . . H45 H 0.6914 0.3967 -0.2451 0.120 Uiso 1 calc R . . C46 C 0.5577(6) 0.4261(5) -0.2103(5) 0.0722(19) Uani 1 d . . . H46 H 0.5781 0.4831 -0.1919 0.087 Uiso 1 calc R . . C21 C 0.3543(6) 0.2369(4) -0.0505(4) 0.0628(16) Uani 1 d . . . C22 C 0.4567(8) 0.1959(5) -0.0221(6) 0.095(3) Uani 1 d . . . H22 H 0.5210 0.2243 0.0148 0.114 Uiso 1 calc R . . C23 C 0.4605(12) 0.1091(8) -0.0510(9) 0.141(5) Uani 1 d . . . H23 H 0.5285 0.0804 -0.0354 0.169 Uiso 1 calc R . . C24 C 0.365(2) 0.0673(6) -0.1018(9) 0.171(8) Uani 1 d . . . H24 H 0.3688 0.0097 -0.1186 0.205 Uiso 1 calc R . . C25 C 0.2648(13) 0.1061(6) -0.1283(7) 0.135(5) Uani 1 d . . . H25 H 0.2001 0.0765 -0.1625 0.162 Uiso 1 calc R . . C26 C 0.2618(10) 0.1914(5) -0.1027(6) 0.106(3) Uani 1 d . . . H26 H 0.1933 0.2197 -0.1219 0.127 Uiso 1 calc R . . C11 C 0.2454(5) 0.3606(4) 0.0282(4) 0.0550(14) Uani 1 d . . . C12 C 0.2159(6) 0.2909(6) 0.0708(5) 0.087(2) Uani 1 d . . . H12 H 0.2442 0.2358 0.0677 0.105 Uiso 1 calc R . . C13 C 0.1429(8) 0.3036(8) 0.1186(7) 0.112(3) Uani 1 d . . . H13 H 0.1242 0.2569 0.1482 0.134 Uiso 1 calc R . . C14 C 0.1013(9) 0.3807(9) 0.1220(6) 0.114(3) Uani 1 d . . . H14 H 0.0528 0.3876 0.1537 0.137 Uiso 1 calc R . . C15 C 0.1272(8) 0.4520(7) 0.0798(6) 0.101(3) Uani 1 d . . . H15 H 0.0955 0.5062 0.0814 0.121 Uiso 1 calc R . . C16 C 0.2020(7) 0.4405(5) 0.0351(6) 0.086(2) Uani 1 d . . . H16 H 0.2234 0.4886 0.0090 0.104 Uiso 1 calc R . . P5 P -0.05391(16) 0.35439(13) -0.26711(13) 0.0702(5) Uani 1 d . . . F51 F -0.1734(9) 0.3760(11) -0.3311(8) 0.284(7) Uani 1 d . . . F52 F 0.0627(5) 0.3346(8) -0.2116(6) 0.216(4) Uani 1 d . . . F53 F -0.0689(9) 0.2592(5) -0.2981(6) 0.189(4) Uani 1 d . . . F54 F -0.0959(6) 0.3326(5) -0.1887(5) 0.160(3) Uani 1 d . . . F55 F -0.0407(14) 0.4481(5) -0.2379(8) 0.267(8) Uani 1 d . . . F56 F -0.0188(7) 0.3743(5) -0.3506(5) 0.164(3) 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 0.0540(3) 0.0545(3) 0.0481(3) 0.00248(18) 0.0132(2) -0.00307(19) P2 0.0522(8) 0.0478(7) 0.0438(7) 0.0009(6) 0.0181(6) -0.0044(6) N3 0.047(3) 0.056(3) 0.041(2) 0.0039(19) 0.016(2) -0.006(2) P4 0.0461(7) 0.0539(8) 0.0393(7) 0.0017(6) 0.0164(6) -0.0037(6) N100 0.068(4) 0.090(4) 0.105(5) -0.015(4) 0.036(4) 0.016(3) C101 0.083(5) 0.082(5) 0.068(4) -0.009(4) 0.021(4) 0.015(4) C102 0.134(8) 0.189(11) 0.086(6) 0.009(6) 0.048(6) 0.083(8) C31 0.052(3) 0.049(3) 0.050(3) 0.007(2) 0.020(3) -0.009(2) C32 0.105(6) 0.088(5) 0.043(3) 0.008(3) 0.022(4) 0.008(4) C33 0.121(7) 0.110(7) 0.047(4) 0.008(4) 0.013(4) 0.008(6) C34 0.082(5) 0.078(5) 0.065(5) 0.019(4) -0.001(4) -0.003(4) C35 0.069(5) 0.078(5) 0.074(5) 0.006(4) 0.005(4) 0.003(4) C36 0.064(4) 0.081(5) 0.058(4) 0.004(3) 0.014(3) 0.008(3) C41 0.053(3) 0.075(4) 0.038(3) 0.004(3) 0.017(2) 0.002(3) C42 0.085(5) 0.073(4) 0.062(4) -0.018(3) 0.031(4) 0.004(4) C43 0.116(7) 0.104(6) 0.082(5) -0.022(5) 0.041(5) 0.029(5) C44 0.105(7) 0.140(9) 0.079(5) -0.004(6) 0.045(5) 0.043(6) C45 0.071(5) 0.152(9) 0.094(6) 0.017(6) 0.050(5) 0.034(6) C46 0.066(4) 0.092(5) 0.071(4) 0.008(4) 0.039(4) 0.011(3) C21 0.093(5) 0.045(3) 0.048(3) 0.004(3) 0.022(3) 0.000(3) C22 0.122(7) 0.051(4) 0.107(6) 0.005(4) 0.034(5) 0.015(4) C23 0.196(15) 0.083(7) 0.154(11) 0.009(7) 0.076(11) 0.044(8) C24 0.33(2) 0.053(5) 0.106(9) -0.021(5) 0.045(12) -0.002(9) C25 0.203(13) 0.058(5) 0.091(7) 0.005(5) -0.010(7) -0.024(7) C26 0.148(8) 0.058(4) 0.081(5) -0.002(4) 0.003(5) -0.014(5) C11 0.051(3) 0.072(4) 0.041(3) 0.008(3) 0.014(2) -0.007(3) C12 0.077(5) 0.107(6) 0.087(5) 0.029(4) 0.041(4) 0.000(4) C13 0.095(6) 0.155(10) 0.106(7) 0.053(7) 0.060(6) -0.009(6) C14 0.099(7) 0.182(11) 0.083(6) 0.001(7) 0.058(5) -0.013(7) C15 0.108(7) 0.112(6) 0.111(7) -0.022(6) 0.073(6) -0.004(5) C16 0.108(6) 0.076(5) 0.104(6) -0.015(4) 0.072(5) -0.019(4) P5 0.0670(11) 0.0791(12) 0.0762(11) 0.0005(9) 0.0399(9) 0.0088(9) F51 0.153(8) 0.46(2) 0.249(12) 0.142(14) 0.083(8) 0.137(11) F52 0.066(4) 0.329(13) 0.204(8) 0.010(8) -0.013(4) 0.006(6) F53 0.315(11) 0.119(5) 0.186(7) -0.045(5) 0.153(8) -0.084(6) F54 0.198(7) 0.183(7) 0.161(6) 0.009(5) 0.139(6) -0.001(5) F55 0.55(2) 0.104(5) 0.279(12) -0.034(6) 0.305(16) -0.001(9) F56 0.249(9) 0.155(6) 0.140(5) 0.016(5) 0.134(6) 0.008(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 Ag1 N100 2.382(6) . ? Ag1 P2 2.436(3) . ? Ag1 P4 2.450(3) 3_665 ? Ag1 Ag1 2.961(3) 3_665 ? P2 N3 1.692(5) . ? P2 C11 1.810(6) . ? P2 C21 1.812(6) . ? N3 P4 1.684(5) . ? P4 C31 1.811(6) . ? P4 C41 1.824(6) . ? P4 Ag1 2.450(3) 3_665 ? N100 C101 1.117(9) . ? C101 C102 1.448(11) . ? C31 C32 1.376(8) . ? C31 C36 1.384(9) . ? C32 C33 1.413(10) . ? C33 C34 1.386(12) . ? C34 C35 1.350(11) . ? C35 C36 1.387(10) . ? C41 C42 1.374(9) . ? C41 C46 1.408(9) . ? C42 C43 1.417(10) . ? C43 C44 1.365(14) . ? C44 C45 1.378(14) . ? C45 C46 1.398(10) . ? C21 C26 1.369(11) . ? C21 C22 1.381(11) . ? C22 C23 1.414(14) . ? C23 C24 1.36(2) . ? C24 C25 1.34(2) . ? C25 C26 1.375(13) . ? C11 C16 1.368(10) . ? C11 C12 1.382(9) . ? C12 C13 1.405(12) . ? C13 C14 1.308(15) . ? C14 C15 1.379(14) . ? C15 C16 1.386(10) . ? P5 F52 1.470(7) . ? P5 F55 1.502(8) . ? P5 F53 1.531(7) . ? P5 F51 1.540(10) . ? P5 F54 1.540(6) . ? P5 F56 1.554(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N100 Ag1 P2 110.7(2) . . ? N100 Ag1 P4 100.84(19) . 3_665 ? P2 Ag1 P4 148.45(5) . 3_665 ? N100 Ag1 Ag1 104.80(18) . 3_665 ? P2 Ag1 Ag1 93.32(8) . 3_665 ? P4 Ag1 Ag1 79.54(11) 3_665 3_665 ? N3 P2 C11 105.3(3) . . ? N3 P2 C21 105.6(3) . . ? C11 P2 C21 105.4(3) . . ? N3 P2 Ag1 107.49(17) . . ? C11 P2 Ag1 114.9(2) . . ? C21 P2 Ag1 117.2(2) . . ? P4 N3 P2 122.2(3) . . ? N3 P4 C31 101.7(3) . . ? N3 P4 C41 106.3(3) . . ? C31 P4 C41 105.1(3) . . ? N3 P4 Ag1 111.91(19) . 3_665 ? C31 P4 Ag1 114.5(2) . 3_665 ? C41 P4 Ag1 115.9(2) . 3_665 ? C101 N100 Ag1 173.7(6) . . ? N100 C101 C102 178.2(10) . . ? C32 C31 C36 119.6(6) . . ? C32 C31 P4 122.2(5) . . ? C36 C31 P4 118.2(5) . . ? C31 C32 C33 118.8(8) . . ? C34 C33 C32 120.7(7) . . ? C35 C34 C33 119.5(7) . . ? C34 C35 C36 120.6(8) . . ? C31 C36 C35 120.7(7) . . ? C42 C41 C46 119.8(6) . . ? C42 C41 P4 124.0(5) . . ? C46 C41 P4 116.2(5) . . ? C41 C42 C43 119.8(8) . . ? C44 C43 C42 120.1(9) . . ? C43 C44 C45 120.6(8) . . ? C44 C45 C46 120.3(8) . . ? C45 C46 C41 119.4(8) . . ? C26 C21 C22 118.9(7) . . ? C26 C21 P2 122.7(6) . . ? C22 C21 P2 118.3(6) . . ? C21 C22 C23 117.7(10) . . ? C24 C23 C22 120.2(12) . . ? C25 C24 C23 122.5(10) . . ? C24 C25 C26 117.2(11) . . ? C21 C26 C25 123.5(11) . . ? C16 C11 C12 117.9(6) . . ? C16 C11 P2 119.6(5) . . ? C12 C11 P2 122.2(5) . . ? C11 C12 C13 119.8(9) . . ? C14 C13 C12 120.4(9) . . ? C13 C14 C15 121.9(8) . . ? C14 C15 C16 117.9(9) . . ? C11 C16 C15 121.9(8) . . ? F52 P5 F55 92.2(7) . . ? F52 P5 F53 88.6(6) . . ? F55 P5 F53 179.1(7) . . ? F52 P5 F51 175.9(6) . . ? F55 P5 F51 88.2(7) . . ? F53 P5 F51 91.0(8) . . ? F52 P5 F54 93.4(5) . . ? F55 P5 F54 90.0(4) . . ? F53 P5 F54 90.2(4) . . ? F51 P5 F54 90.7(5) . . ? F52 P5 F56 89.8(5) . . ? F55 P5 F56 91.8(4) . . ? F53 P5 F56 88.0(4) . . ? F51 P5 F56 86.2(5) . . ? F54 P5 F56 176.4(5) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.184 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.104 #==END