Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Wei-Yin Sun' 'Hong-Wei Bu' 'Taka-aki Okamura' 'Xing-Mei Ouyang' 'Wen-xia Tang' 'Norikazu Ueyama' _publ_contact_author_name 'Prof Wei-Yin Sun' _publ_contact_author_address ; Prof Wei-Yin Sun Coordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing 210093 CHINA ; _publ_contact_author_email SUNWY@NJU.EDU.CN _publ_section_title ; Syntheses, structures and photoluminescent properties of cadmium(II), silver(I) and copper(I) complexes with novel long chain tetradentate ligands ; data_[Cd(L1)Br2]_(1) _database_code_CSD 201027 _audit_creation_date 'Thu Feb 13 13:17:04 2003' _audit_creation_method SHELXL-97 _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cd(L1)Br2] _chemical_formula_sum 'C24 H28 Br2 Cd N6' _chemical_formula_weight 672.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 10.504(7) _cell_length_b 11.790(7) _cell_length_c 21.347(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.46(3) _cell_angle_gamma 90.00 _cell_volume 2621(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 14584 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 3.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.468 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22547 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.0900 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5876 _reflns_number_gt 3521 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1985)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^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 5876 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.23043(3) 0.59348(2) 0.620118(13) 0.02996(8) Uani 1 1 d . . . Br1 Br -0.03655(4) 0.62856(3) 0.594879(19) 0.04141(11) Uani 1 1 d . . . Br2 Br 0.49356(3) 0.57906(3) 0.644118(19) 0.04086(11) Uani 1 1 d . . . N1 N 0.2444(3) 0.4726(2) 0.53079(13) 0.0301(7) Uani 1 1 d . . . H1 H 0.1612 0.4525 0.5143 0.036 Uiso 1 1 calc R . . N2 N 0.2332(3) 0.7244(2) 0.53237(13) 0.0338(7) Uani 1 1 d . . . H2 H 0.1595 0.7685 0.5310 0.041 Uiso 1 1 calc R . . N11 N 0.1954(3) -0.0667(2) 0.71570(15) 0.0441(9) Uani 1 1 d . . . N12 N 0.2362(3) -0.2402(3) 0.68283(14) 0.0392(8) Uani 1 1 d . . . N21 N 0.2504(3) 1.1243(2) 0.28863(13) 0.0348(8) Uani 1 1 d . . . N22 N 0.2016(3) 1.0288(2) 0.20045(13) 0.0312(7) Uani 1 1 d . . . C1 C 0.2961(4) 0.5466(3) 0.48349(17) 0.0369(9) Uani 1 1 d . . . H3 H 0.2924 0.5060 0.4427 0.044 Uiso 1 1 calc R . . H4 H 0.3870 0.5653 0.4982 0.044 Uiso 1 1 calc R . . C2 C 0.2181(4) 0.6544(3) 0.47455(16) 0.0387(10) Uani 1 1 d . . . H5 H 0.2459 0.6987 0.4393 0.046 Uiso 1 1 calc R . . H6 H 0.1264 0.6350 0.4631 0.046 Uiso 1 1 calc R . . C10 C 0.3216(3) 0.3662(3) 0.53913(17) 0.0358(9) Uani 1 1 d . . . H7 H 0.4117 0.3859 0.5550 0.043 Uiso 1 1 calc R . . H8 H 0.3210 0.3292 0.4975 0.043 Uiso 1 1 calc R . . C11 C 0.2725(3) 0.2833(3) 0.58425(17) 0.0319(9) Uani 1 1 d . . . C12 C 0.1520(4) 0.2341(3) 0.57368(18) 0.0384(9) Uani 1 1 d . . . H9 H 0.0971 0.2533 0.5362 0.046 Uiso 1 1 calc R . . C13 C 0.1080(4) 0.1577(3) 0.61577(19) 0.0457(11) Uani 1 1 d . . . H10 H 0.0243 0.1263 0.6068 0.055 Uiso 1 1 calc R . . C14 C 0.1852(4) 0.1276(3) 0.67016(19) 0.0404(10) Uani 1 1 d . . . C15 C 0.3068(4) 0.1764(3) 0.68139(18) 0.0410(10) Uani 1 1 d . . . H11 H 0.3617 0.1568 0.7187 0.049 Uiso 1 1 calc R . . C16 C 0.3496(4) 0.2528(3) 0.63945(17) 0.0371(9) Uani 1 1 d . . . H12 H 0.4330 0.2848 0.6486 0.045 Uiso 1 1 calc R . . C17 C 0.1368(4) 0.0473(3) 0.7174(2) 0.0533(12) Uani 1 1 d . . . H13 H 0.1568 0.0792 0.7604 0.064 Uiso 1 1 calc R . . H14 H 0.0423 0.0404 0.7079 0.064 Uiso 1 1 calc R . . C20 C 0.3432(3) 0.8039(3) 0.53757(17) 0.0377(10) Uani 1 1 d . . . H15 H 0.4225 0.7594 0.5355 0.045 Uiso 1 1 calc R . . H16 H 0.3510 0.8403 0.5797 0.045 Uiso 1 1 calc R . . C21 C 0.3366(3) 0.8961(3) 0.48813(16) 0.0333(9) Uani 1 1 d . . . C22 C 0.4241(4) 0.8993(3) 0.44508(17) 0.0409(10) Uani 1 1 d . . . H17 H 0.4881 0.8421 0.4463 0.049 Uiso 1 1 calc R . . C23 C 0.4201(4) 0.9850(3) 0.39998(17) 0.0400(10) Uani 1 1 d . . . H18 H 0.4811 0.9857 0.3708 0.048 Uiso 1 1 calc R . . C24 C 0.3277(4) 1.0693(3) 0.39745(16) 0.0342(9) Uani 1 1 d . . . C25 C 0.2403(4) 1.0668(3) 0.44082(17) 0.0417(10) Uani 1 1 d . . . H19 H 0.1764 1.1241 0.4396 0.050 Uiso 1 1 calc R . . C26 C 0.2448(4) 0.9819(3) 0.48581(17) 0.0412(10) Uani 1 1 d . . . H20 H 0.1847 0.9821 0.5154 0.049 Uiso 1 1 calc R . . C27 C 0.3221(4) 1.1617(3) 0.34783(16) 0.0455(11) Uani 1 1 d . . . H21 H 0.2807 1.2300 0.3631 0.055 Uiso 1 1 calc R . . H22 H 0.4105 1.1826 0.3407 0.055 Uiso 1 1 calc R . . C101 C 0.1632(4) -0.1484(3) 0.67285(17) 0.0393(10) Uani 1 1 d . . . H23 H 0.0954 -0.1414 0.6390 0.047 Uiso 1 1 calc R . . C102 C 0.3199(4) -0.2135(4) 0.7341(2) 0.0657(14) Uani 1 1 d . . . H24 H 0.3864 -0.2617 0.7532 0.079 Uiso 1 1 calc R . . C103 C 0.2949(5) -0.1079(4) 0.7544(2) 0.0738(16) Uani 1 1 d . . . H25 H 0.3401 -0.0699 0.7898 0.089 Uiso 1 1 calc R . . C201 C 0.2909(4) 1.0506(3) 0.24740(17) 0.0365(9) Uani 1 1 d . . . H26 H 0.3744 1.0181 0.2519 0.044 Uiso 1 1 calc R . . C202 C 0.0982(4) 1.0925(3) 0.21226(18) 0.0373(9) Uani 1 1 d . . . H27 H 0.0180 1.0949 0.1859 0.045 Uiso 1 1 calc R . . C203 C 0.1264(4) 1.1513(3) 0.26670(18) 0.0416(10) Uani 1 1 d . . . H28 H 0.0713 1.2010 0.2857 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03622(16) 0.02695(14) 0.02567(15) 0.00270(12) 0.00007(12) -0.00181(12) Br1 0.0352(2) 0.0464(2) 0.0404(3) -0.0049(2) -0.00367(19) 0.00011(19) Br2 0.0348(2) 0.0406(2) 0.0449(3) 0.0056(2) -0.0037(2) -0.00426(19) N1 0.0329(17) 0.0295(17) 0.0279(17) -0.0006(14) 0.0038(14) -0.0038(14) N2 0.0404(18) 0.0283(17) 0.0308(18) 0.0036(14) -0.0020(15) -0.0049(14) N11 0.067(2) 0.0250(18) 0.042(2) -0.0011(15) 0.0122(19) -0.0077(17) N12 0.0468(19) 0.0313(18) 0.037(2) -0.0009(15) -0.0048(16) -0.0015(16) N21 0.052(2) 0.0296(18) 0.0240(17) 0.0011(14) 0.0093(16) -0.0041(16) N22 0.0436(19) 0.0261(17) 0.0246(17) -0.0024(13) 0.0064(15) -0.0027(15) C1 0.041(2) 0.038(2) 0.032(2) 0.0029(18) 0.0068(18) -0.0073(19) C2 0.048(2) 0.036(2) 0.031(2) 0.0077(18) 0.0001(19) -0.007(2) C10 0.038(2) 0.036(2) 0.034(2) -0.0055(18) 0.0077(18) 0.0015(19) C11 0.041(2) 0.025(2) 0.033(2) -0.0047(17) 0.0139(19) 0.0034(17) C12 0.042(2) 0.039(2) 0.035(2) -0.0039(19) 0.0057(19) -0.0013(19) C13 0.048(3) 0.037(2) 0.053(3) -0.010(2) 0.012(2) -0.013(2) C14 0.062(3) 0.0197(19) 0.043(3) -0.0070(18) 0.023(2) 0.000(2) C15 0.051(3) 0.033(2) 0.039(2) 0.0043(19) 0.005(2) 0.008(2) C16 0.043(2) 0.029(2) 0.040(2) -0.0020(19) 0.008(2) 0.0011(18) C17 0.077(3) 0.029(2) 0.059(3) -0.003(2) 0.031(3) -0.003(2) C20 0.047(2) 0.032(2) 0.033(2) 0.0013(17) 0.0004(19) -0.0057(19) C21 0.041(2) 0.031(2) 0.027(2) 0.0018(17) 0.0009(18) -0.0023(18) C22 0.044(2) 0.039(2) 0.040(2) 0.0047(19) 0.004(2) 0.0047(19) C23 0.048(2) 0.043(3) 0.031(2) -0.0009(19) 0.014(2) -0.007(2) C24 0.054(2) 0.024(2) 0.024(2) -0.0040(16) 0.0027(19) -0.0109(19) C25 0.055(3) 0.037(2) 0.034(2) 0.0018(19) 0.007(2) 0.010(2) C26 0.050(3) 0.040(2) 0.037(2) 0.0085(19) 0.020(2) 0.005(2) C27 0.074(3) 0.036(2) 0.026(2) -0.0019(18) 0.003(2) -0.010(2) C101 0.049(2) 0.043(2) 0.026(2) 0.0012(19) 0.0041(19) -0.002(2) C102 0.077(3) 0.044(3) 0.064(3) -0.010(2) -0.035(3) 0.007(3) C103 0.094(4) 0.050(3) 0.066(3) -0.019(3) -0.029(3) -0.008(3) C201 0.049(2) 0.029(2) 0.031(2) 0.0011(18) 0.004(2) 0.0032(19) C202 0.037(2) 0.036(2) 0.040(2) 0.000(2) 0.0104(19) -0.007(2) C203 0.049(3) 0.036(2) 0.044(3) -0.002(2) 0.021(2) -0.001(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 Cd1 N22 2.291(3) 4_576 ? Cd1 N12 2.371(3) 1_565 ? Cd1 N1 2.400(3) . ? Cd1 N2 2.430(3) . ? Cd1 Br2 2.7500(19) . ? Cd1 Br1 2.8167(19) . ? N1 C1 1.489(4) . ? N1 C10 1.491(4) . ? N1 H1 0.9300 . ? N2 C2 1.476(4) . ? N2 C20 1.481(4) . ? N2 H2 0.9300 . ? N11 C103 1.338(5) . ? N11 C101 1.341(4) . ? N11 C17 1.480(5) . ? N12 C101 1.327(5) . ? N12 C102 1.349(4) . ? N12 Cd1 2.371(3) 1_545 ? N21 C201 1.345(4) . ? N21 C203 1.364(5) . ? N21 C27 1.453(4) . ? N22 C201 1.306(4) . ? N22 C202 1.370(4) . ? N22 Cd1 2.291(3) 4_575 ? C1 C2 1.511(5) . ? C1 H3 0.9900 . ? C1 H4 0.9900 . ? C2 H5 0.9900 . ? C2 H6 0.9900 . ? C10 C11 1.510(5) . ? C10 H7 0.9900 . ? C10 H8 0.9900 . ? C11 C12 1.383(5) . ? C11 C16 1.388(5) . ? C12 C13 1.393(5) . ? C12 H9 0.9500 . ? C13 C14 1.374(5) . ? C13 H10 0.9500 . ? C14 C15 1.393(5) . ? C14 C17 1.518(5) . ? C15 C16 1.386(5) . ? C15 H11 0.9500 . ? C16 H12 0.9500 . ? C17 H13 0.9900 . ? C17 H14 0.9900 . ? C20 C21 1.510(5) . ? C20 H15 0.9900 . ? C20 H16 0.9900 . ? C21 C22 1.382(5) . ? C21 C26 1.394(5) . ? C22 C23 1.393(5) . ? C22 H17 0.9500 . ? C23 C24 1.385(5) . ? C23 H18 0.9500 . ? C24 C25 1.387(5) . ? C24 C27 1.516(5) . ? C25 C26 1.384(5) . ? C25 H19 0.9500 . ? C26 H20 0.9500 . ? C27 H21 0.9900 . ? C27 H22 0.9900 . ? C101 H23 0.9500 . ? C102 C103 1.355(6) . ? C102 H24 0.9500 . ? C103 H25 0.9500 . ? C201 H26 0.9500 . ? C202 C203 1.353(5) . ? C202 H27 0.9500 . ? C203 H28 0.9500 . ? 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 Cd1 N12 95.41(11) 4_576 1_565 ? N22 Cd1 N1 104.41(11) 4_576 . ? N12 Cd1 N1 160.04(10) 1_565 . ? N22 Cd1 N2 173.14(10) 4_576 . ? N12 Cd1 N2 84.72(11) 1_565 . ? N1 Cd1 N2 75.90(10) . . ? N22 Cd1 Br2 92.81(8) 4_576 . ? N12 Cd1 Br2 89.68(8) 1_565 . ? N1 Cd1 Br2 86.99(7) . . ? N2 Cd1 Br2 94.05(8) . . ? N22 Cd1 Br1 90.60(8) 4_576 . ? N12 Cd1 Br1 86.47(8) 1_565 . ? N1 Cd1 Br1 95.59(7) . . ? N2 Cd1 Br1 82.56(8) . . ? Br2 Cd1 Br1 175.083(16) . . ? C1 N1 C10 109.5(3) . . ? C1 N1 Cd1 104.9(2) . . ? C10 N1 Cd1 119.5(2) . . ? C1 N1 H1 107.5 . . ? C10 N1 H1 107.5 . . ? Cd1 N1 H1 107.5 . . ? C2 N2 C20 114.5(3) . . ? C2 N2 Cd1 106.2(2) . . ? C20 N2 Cd1 115.6(2) . . ? C2 N2 H2 106.7 . . ? C20 N2 H2 106.7 . . ? Cd1 N2 H2 106.7 . . ? C103 N11 C101 105.6(3) . . ? C103 N11 C17 127.5(4) . . ? C101 N11 C17 126.9(4) . . ? C101 N12 C102 104.0(3) . . ? C101 N12 Cd1 127.7(2) . 1_545 ? C102 N12 Cd1 128.1(3) . 1_545 ? C201 N21 C203 107.2(3) . . ? C201 N21 C27 126.4(3) . . ? C203 N21 C27 126.3(3) . . ? C201 N22 C202 105.0(3) . . ? C201 N22 Cd1 123.1(3) . 4_575 ? C202 N22 Cd1 131.9(2) . 4_575 ? N1 C1 C2 109.8(3) . . ? N1 C1 H3 109.7 . . ? C2 C1 H3 109.7 . . ? N1 C1 H4 109.7 . . ? C2 C1 H4 109.7 . . ? H3 C1 H4 108.2 . . ? N2 C2 C1 111.5(3) . . ? N2 C2 H5 109.3 . . ? C1 C2 H5 109.3 . . ? N2 C2 H6 109.3 . . ? C1 C2 H6 109.3 . . ? H5 C2 H6 108.0 . . ? N1 C10 C11 113.3(3) . . ? N1 C10 H7 108.9 . . ? C11 C10 H7 108.9 . . ? N1 C10 H8 108.9 . . ? C11 C10 H8 108.9 . . ? H7 C10 H8 107.7 . . ? C12 C11 C16 116.8(3) . . ? C12 C11 C10 123.2(3) . . ? C16 C11 C10 119.9(3) . . ? C11 C12 C13 122.6(4) . . ? C11 C12 H9 118.7 . . ? C13 C12 H9 118.7 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H10 119.9 . . ? C12 C13 H10 119.9 . . ? C13 C14 C15 117.8(4) . . ? C13 C14 C17 120.7(4) . . ? C15 C14 C17 121.5(4) . . ? C16 C15 C14 121.7(4) . . ? C16 C15 H11 119.2 . . ? C14 C15 H11 119.2 . . ? C15 C16 C11 120.9(4) . . ? C15 C16 H12 119.5 . . ? C11 C16 H12 119.5 . . ? N11 C17 C14 112.0(3) . . ? N11 C17 H13 109.2 . . ? C14 C17 H13 109.2 . . ? N11 C17 H14 109.2 . . ? C14 C17 H14 109.2 . . ? H13 C17 H14 107.9 . . ? N2 C20 C21 116.0(3) . . ? N2 C20 H15 108.3 . . ? C21 C20 H15 108.3 . . ? N2 C20 H16 108.3 . . ? C21 C20 H16 108.3 . . ? H15 C20 H16 107.4 . . ? C22 C21 C26 118.3(3) . . ? C22 C21 C20 120.7(3) . . ? C26 C21 C20 121.1(3) . . ? C21 C22 C23 121.1(4) . . ? C21 C22 H17 119.5 . . ? C23 C22 H17 119.5 . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H18 119.8 . . ? C22 C23 H18 119.8 . . ? C23 C24 C25 118.7(3) . . ? C23 C24 C27 120.4(4) . . ? C25 C24 C27 120.8(3) . . ? C26 C25 C24 120.8(4) . . ? C26 C25 H19 119.6 . . ? C24 C25 H19 119.6 . . ? C25 C26 C21 120.7(4) . . ? C25 C26 H20 119.6 . . ? C21 C26 H20 119.6 . . ? N21 C27 C24 111.0(3) . . ? N21 C27 H21 109.4 . . ? C24 C27 H21 109.4 . . ? N21 C27 H22 109.4 . . ? C24 C27 H22 109.4 . . ? H21 C27 H22 108.0 . . ? N12 C101 N11 112.8(3) . . ? N12 C101 H23 123.6 . . ? N11 C101 H23 123.6 . . ? N12 C102 C103 109.9(4) . . ? N12 C102 H24 125.0 . . ? C103 C102 H24 125.0 . . ? N11 C103 C102 107.7(4) . . ? N11 C103 H25 126.1 . . ? C102 C103 H25 126.1 . . ? N22 C201 N21 111.9(3) . . ? N22 C201 H26 124.1 . . ? N21 C201 H26 124.1 . . ? C203 C202 N22 110.4(3) . . ? C203 C202 H27 124.8 . . ? N22 C202 H27 124.8 . . ? C202 C203 N21 105.5(3) . . ? C202 C203 H28 127.2 . . ? N21 C203 H28 127.2 . . ? 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 N22 Cd1 N1 C1 -165.9(2) 4_576 . . . ? N12 Cd1 N1 C1 7.0(4) 1_565 . . . ? N2 Cd1 N1 C1 21.2(2) . . . . ? Br2 Cd1 N1 C1 -73.8(2) . . . . ? Br1 Cd1 N1 C1 102.0(2) . . . . ? N22 Cd1 N1 C10 -42.8(3) 4_576 . . . ? N12 Cd1 N1 C10 130.1(3) 1_565 . . . ? N2 Cd1 N1 C10 144.3(3) . . . . ? Br2 Cd1 N1 C10 49.4(2) . . . . ? Br1 Cd1 N1 C10 -134.8(2) . . . . ? N22 Cd1 N2 C2 -83.5(9) 4_576 . . . ? N12 Cd1 N2 C2 -174.8(2) 1_565 . . . ? N1 Cd1 N2 C2 10.0(2) . . . . ? Br2 Cd1 N2 C2 95.9(2) . . . . ? Br1 Cd1 N2 C2 -87.7(2) . . . . ? N22 Cd1 N2 C20 148.4(8) 4_576 . . . ? N12 Cd1 N2 C20 57.0(2) 1_565 . . . ? N1 Cd1 N2 C20 -118.1(3) . . . . ? Br2 Cd1 N2 C20 -32.3(2) . . . . ? Br1 Cd1 N2 C20 144.2(2) . . . . ? C10 N1 C1 C2 179.8(3) . . . . ? Cd1 N1 C1 C2 -50.8(3) . . . . ? C20 N2 C2 C1 87.7(4) . . . . ? Cd1 N2 C2 C1 -41.1(3) . . . . ? N1 C1 C2 N2 66.0(4) . . . . ? C1 N1 C10 C11 -177.4(3) . . . . ? Cd1 N1 C10 C11 61.7(4) . . . . ? N1 C10 C11 C12 62.4(5) . . . . ? N1 C10 C11 C16 -117.7(3) . . . . ? C16 C11 C12 C13 0.1(5) . . . . ? C10 C11 C12 C13 180.0(4) . . . . ? C11 C12 C13 C14 -0.4(6) . . . . ? C12 C13 C14 C15 0.4(6) . . . . ? C12 C13 C14 C17 178.1(3) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C17 C14 C15 C16 -177.7(3) . . . . ? C14 C15 C16 C11 -0.3(6) . . . . ? C12 C11 C16 C15 0.2(5) . . . . ? C10 C11 C16 C15 -179.7(3) . . . . ? C103 N11 C17 C14 98.3(5) . . . . ? C101 N11 C17 C14 -78.1(5) . . . . ? C13 C14 C17 N11 106.4(4) . . . . ? C15 C14 C17 N11 -76.0(5) . . . . ? C2 N2 C20 C21 64.3(4) . . . . ? Cd1 N2 C20 C21 -171.8(2) . . . . ? N2 C20 C21 C22 -114.8(4) . . . . ? N2 C20 C21 C26 67.1(5) . . . . ? C26 C21 C22 C23 -0.8(5) . . . . ? C20 C21 C22 C23 -179.0(3) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C22 C23 C24 C25 0.4(5) . . . . ? C22 C23 C24 C27 -179.2(3) . . . . ? C23 C24 C25 C26 0.0(5) . . . . ? C27 C24 C25 C26 179.5(3) . . . . ? C24 C25 C26 C21 -0.7(6) . . . . ? C22 C21 C26 C25 1.1(6) . . . . ? C20 C21 C26 C25 179.3(3) . . . . ? C201 N21 C27 C24 -74.0(5) . . . . ? C203 N21 C27 C24 101.1(4) . . . . ? C23 C24 C27 N21 84.0(4) . . . . ? C25 C24 C27 N21 -95.5(4) . . . . ? C102 N12 C101 N11 -1.0(5) . . . . ? Cd1 N12 C101 N11 -176.8(2) 1_545 . . . ? C103 N11 C101 N12 0.8(5) . . . . ? C17 N11 C101 N12 177.9(3) . . . . ? C101 N12 C102 C103 0.8(5) . . . . ? Cd1 N12 C102 C103 176.6(3) 1_545 . . . ? C101 N11 C103 C102 -0.3(5) . . . . ? C17 N11 C103 C102 -177.3(4) . . . . ? N12 C102 C103 N11 -0.4(6) . . . . ? C202 N22 C201 N21 0.1(4) . . . . ? Cd1 N22 C201 N21 -179.6(2) 4_575 . . . ? C203 N21 C201 N22 0.3(4) . . . . ? C27 N21 C201 N22 176.2(3) . . . . ? C201 N22 C202 C203 -0.5(4) . . . . ? Cd1 N22 C202 C203 179.2(2) 4_575 . . . ? N22 C202 C203 N21 0.6(4) . . . . ? C201 N21 C203 C202 -0.5(4) . . . . ? C27 N21 C203 C202 -176.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.526 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.094 #====END data_[Ag3(L1)2](ClO4)3_(2) _database_code_CSD 201028 _audit_creation_date 'Mon Dec 2 22:06:46 2002' _audit_creation_method SHELXL-97 _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Ag3(L1)2](ClO4)3 _chemical_formula_sum 'C48 H56 Ag3 Cl3 N12 O12' _chemical_formula_weight 1423.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.879(7) _cell_length_b 9.997(12) _cell_length_c 35.53(3) _cell_angle_alpha 94.69(9) _cell_angle_beta 90.38(7) _cell_angle_gamma 115.90(8) _cell_volume 2824(5) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 19741 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27740 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.47 _reflns_number_total 12802 _reflns_number_gt 7554 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^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 12802 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.69420(5) 0.33576(5) 0.228115(11) 0.04725(12) Uani 1 1 d . . . Ag2 Ag 0.33998(6) -0.02463(7) 0.520961(13) 0.06834(17) Uani 1 1 d . . . Ag3 Ag 0.34657(6) -0.62605(5) 0.014662(11) 0.05556(14) Uani 1 1 d . . . Cl1 Cl 0.79792(17) 0.43589(16) 0.05224(4) 0.0526(3) Uani 1 1 d . . . Cl2 Cl 0.36332(18) -0.30459(18) 0.23684(4) 0.0622(4) Uani 1 1 d . . . Cl3 Cl 0.2126(4) -0.3281(2) 0.44076(6) 0.1066(9) Uani 1 1 d . . . O11 O 0.8522(6) 0.5880(5) 0.04673(17) 0.0897(16) Uani 1 1 d . . . O12 O 0.8298(6) 0.4157(6) 0.09025(12) 0.0805(14) Uani 1 1 d . . . O13 O 0.6242(5) 0.3545(6) 0.04183(14) 0.0790(13) Uani 1 1 d . . . O14 O 0.8891(6) 0.3763(6) 0.02790(14) 0.0822(14) Uani 1 1 d . . . O21 O 0.3106(8) -0.3467(6) 0.19798(14) 0.0927(16) Uani 1 1 d . . . O22 O 0.3459(13) -0.4316(7) 0.2526(2) 0.204(6) Uani 1 1 d . . . O23 O 0.2680(7) -0.2365(11) 0.2526(2) 0.173(4) Uani 1 1 d . . . O24 O 0.5310(5) -0.1970(5) 0.24120(18) 0.0903(17) Uani 1 1 d . . . O31 O 0.0968(9) -0.4765(7) 0.4329(2) 0.128(2) Uani 1 1 d . . . O32 O 0.3591(10) -0.3053(12) 0.4558(2) 0.172(4) Uani 1 1 d . . . O33 O 0.1228(15) -0.2877(12) 0.4722(3) 0.199(5) Uani 1 1 d . . . O34 O 0.2037(12) -0.2389(9) 0.4133(2) 0.176(4) Uani 1 1 d . . . N1 N 0.5157(5) 0.2509(5) 0.28221(11) 0.0397(9) Uani 1 1 d . . . H1 H 0.5569 0.3296 0.3011 0.048 Uiso 1 1 calc R . . N2 N 0.7524(5) 0.1483(5) 0.24858(11) 0.0401(9) Uani 1 1 d . . . H2 H 0.6722 0.0583 0.2369 0.048 Uiso 1 1 calc R . . N3 N 0.6617(5) 0.4261(5) 0.17167(11) 0.0408(9) Uani 1 1 d . . . H3 H 0.7198 0.3980 0.1535 0.049 Uiso 1 1 calc R . . N4 N 0.8845(5) 0.5990(5) 0.23921(11) 0.0441(10) Uani 1 1 d . . . H4 H 0.9864 0.6065 0.2485 0.053 Uiso 1 1 calc R . . N101 N 0.1005(7) 0.1418(8) 0.44757(13) 0.0655(15) Uani 1 1 d . . . N102 N 0.2518(7) 0.0961(7) 0.48888(12) 0.0604(13) Uani 1 1 d . . . N201 N 0.1359(5) -1.0388(5) -0.05444(12) 0.0457(10) Uani 1 1 d . . . N202 N 0.2758(6) -0.8355(5) -0.01647(12) 0.0496(11) Uani 1 1 d . . . N301 N 0.2959(6) -0.3172(5) 0.09444(13) 0.0531(11) Uani 1 1 d . . . N302 N 0.3855(6) -0.4412(5) 0.05387(12) 0.0517(11) Uani 1 1 d . . . N401 N 0.3641(6) -0.3687(6) 0.57839(11) 0.0509(11) Uani 1 1 d . . . N402 N 0.3835(6) -0.1658(7) 0.55571(12) 0.0594(13) Uani 1 1 d . . . C1 C 0.5482(7) 0.1284(6) 0.29614(14) 0.0482(12) Uani 1 1 d . . . H5 H 0.5302 0.1256 0.3236 0.058 Uiso 1 1 calc R . . H6 H 0.4672 0.0315 0.2832 0.058 Uiso 1 1 calc R . . C2 C 0.7215(7) 0.1484(7) 0.28929(14) 0.0491(13) Uani 1 1 d . . . H7 H 0.8028 0.2441 0.3027 0.059 Uiso 1 1 calc R . . H8 H 0.7384 0.0666 0.2996 0.059 Uiso 1 1 calc R . . C3 C 0.7441(7) 0.5916(6) 0.17804(14) 0.0467(12) Uani 1 1 d . . . H9 H 0.6684 0.6260 0.1916 0.056 Uiso 1 1 calc R . . H10 H 0.7657 0.6344 0.1534 0.056 Uiso 1 1 calc R . . C4 C 0.9086(6) 0.6472(7) 0.20103(15) 0.0512(13) Uani 1 1 d . . . H11 H 0.9823 0.6096 0.1878 0.061 Uiso 1 1 calc R . . H12 H 0.9655 0.7577 0.2027 0.061 Uiso 1 1 calc R . . C10 C 0.3342(6) 0.2096(7) 0.27621(13) 0.0479(13) Uani 1 1 d . . . H13 H 0.2837 0.1181 0.2584 0.057 Uiso 1 1 calc R . . H14 H 0.3229 0.2905 0.2640 0.057 Uiso 1 1 calc R . . C11 C 0.2359(6) 0.1823(6) 0.31138(13) 0.0440(12) Uani 1 1 d . . . C12 C 0.2122(7) 0.2968(7) 0.33090(14) 0.0482(13) Uani 1 1 d . . . H15 H 0.2551 0.3921 0.3214 0.058 Uiso 1 1 calc R . . C13 C 0.1265(7) 0.2739(8) 0.36415(15) 0.0581(16) Uani 1 1 d . . . H16 H 0.1111 0.3536 0.3771 0.070 Uiso 1 1 calc R . . C14 C 0.0641(7) 0.1377(8) 0.37842(15) 0.0576(16) Uani 1 1 d . . . C15 C 0.0844(7) 0.0200(8) 0.35841(16) 0.0595(15) Uani 1 1 d . . . H17 H 0.0393 -0.0758 0.3676 0.071 Uiso 1 1 calc R . . C16 C 0.1697(7) 0.0429(7) 0.32541(14) 0.0517(13) Uani 1 1 d . . . H18 H 0.1834 -0.0372 0.3121 0.062 Uiso 1 1 calc R . . C17 C -0.0207(9) 0.1136(11) 0.41565(17) 0.086(3) Uani 1 1 d . . . H19 H -0.0747 0.1815 0.4197 0.104 Uiso 1 1 calc R . . H20 H -0.1093 0.0096 0.4148 0.104 Uiso 1 1 calc R . . C20 C 0.9163(7) 0.1555(7) 0.24008(15) 0.0479(12) Uani 1 1 d . . . H21 H 0.9259 0.0690 0.2496 0.057 Uiso 1 1 calc R . . H22 H 1.0053 0.2477 0.2532 0.057 Uiso 1 1 calc R . . C21 C 0.9405(6) 0.1543(6) 0.19804(14) 0.0418(11) Uani 1 1 d . . . C22 C 1.0302(6) 0.2831(6) 0.18179(16) 0.0478(12) Uani 1 1 d . . . H23 H 1.0827 0.3743 0.1975 0.057 Uiso 1 1 calc R . . C23 C 1.0469(7) 0.2849(6) 0.14337(15) 0.0483(12) Uani 1 1 d . . . H24 H 1.1089 0.3767 0.1328 0.058 Uiso 1 1 calc R . . C24 C 0.9729(6) 0.1520(6) 0.11989(15) 0.0443(11) Uani 1 1 d . . . C25 C 0.8820(8) 0.0199(6) 0.13588(16) 0.0553(14) Uani 1 1 d . . . H25 H 0.8299 -0.0716 0.1203 0.066 Uiso 1 1 calc R . . C26 C 0.8669(7) 0.0214(6) 0.17487(16) 0.0542(13) Uani 1 1 d . . . H26 H 0.8055 -0.0697 0.1857 0.065 Uiso 1 1 calc R . . C27 C 1.0006(7) 0.1559(6) 0.07822(15) 0.0515(13) Uani 1 1 d . . . H27 H 1.0161 0.2543 0.0708 0.062 Uiso 1 1 calc R . . H28 H 1.1054 0.1467 0.0733 0.062 Uiso 1 1 calc R . . C30 C 0.4864(7) 0.3721(6) 0.15669(17) 0.0526(13) Uani 1 1 d . . . H29 H 0.4848 0.4259 0.1346 0.063 Uiso 1 1 calc R . . H30 H 0.4191 0.3931 0.1764 0.063 Uiso 1 1 calc R . . C31 C 0.4106(6) 0.2072(6) 0.14510(14) 0.0440(12) Uani 1 1 d . . . C32 C 0.3926(7) 0.1536(7) 0.10726(15) 0.0546(14) Uani 1 1 d . . . H31 H 0.4292 0.2219 0.0884 0.065 Uiso 1 1 calc R . . C33 C 0.3219(7) 0.0020(7) 0.09676(15) 0.0576(15) Uani 1 1 d . . . H32 H 0.3116 -0.0333 0.0708 0.069 Uiso 1 1 calc R . . C34 C 0.2663(7) -0.0987(6) 0.12363(16) 0.0499(13) Uani 1 1 d . . . C35 C 0.2887(7) -0.0421(7) 0.16165(15) 0.0550(14) Uani 1 1 d . . . H33 H 0.2568 -0.1089 0.1808 0.066 Uiso 1 1 calc R . . C36 C 0.3558(7) 0.1075(6) 0.17137(14) 0.0516(13) Uani 1 1 d . . . H34 H 0.3645 0.1431 0.1973 0.062 Uiso 1 1 calc R . . C37 C 0.1818(8) -0.2652(7) 0.1131(2) 0.0690(18) Uani 1 1 d . . . H35 H 0.1421 -0.3172 0.1361 0.083 Uiso 1 1 calc R . . H36 H 0.0829 -0.2907 0.0959 0.083 Uiso 1 1 calc R . . C40 C 0.8379(8) 0.6951(6) 0.26439(14) 0.0502(13) Uani 1 1 d . . . H37 H 0.7386 0.7000 0.2529 0.060 Uiso 1 1 calc R . . H38 H 0.9308 0.7973 0.2665 0.060 Uiso 1 1 calc R . . C41 C 0.7982(7) 0.6458(6) 0.30366(13) 0.0441(12) Uani 1 1 d . . . C42 C 0.6709(7) 0.6642(7) 0.32245(15) 0.0551(14) Uani 1 1 d . . . H39 H 0.6069 0.7044 0.3101 0.066 Uiso 1 1 calc R . . C43 C 0.6359(8) 0.6252(7) 0.35881(16) 0.0579(14) Uani 1 1 d . . . H40 H 0.5471 0.6373 0.3710 0.070 Uiso 1 1 calc R . . C44 C 0.7282(8) 0.5689(6) 0.37774(14) 0.0516(13) Uani 1 1 d . . . C45 C 0.8558(8) 0.5515(7) 0.35940(15) 0.0568(15) Uani 1 1 d . . . H41 H 0.9201 0.5127 0.3722 0.068 Uiso 1 1 calc R . . C46 C 0.8922(7) 0.5887(6) 0.32317(14) 0.0501(13) Uani 1 1 d . . . H42 H 0.9810 0.5760 0.3112 0.060 Uiso 1 1 calc R . . C47 C 0.6894(9) 0.5290(7) 0.41846(16) 0.0667(17) Uani 1 1 d . . . H43 H 0.7907 0.5880 0.4352 0.080 Uiso 1 1 calc R . . H44 H 0.5997 0.5559 0.4271 0.080 Uiso 1 1 calc R . . C101 C 0.1303(8) 0.0376(8) 0.46329(17) 0.0632(17) Uani 1 1 d . . . H45 H 0.0696 -0.0667 0.4565 0.076 Uiso 1 1 calc R . . C102 C 0.3018(10) 0.2476(9) 0.48973(17) 0.076(2) Uani 1 1 d . . . H46 H 0.3888 0.3214 0.5060 0.091 Uiso 1 1 calc R . . C103 C 0.2113(11) 0.2755(10) 0.46472(17) 0.078(2) Uani 1 1 d . . . H47 H 0.2219 0.3710 0.4597 0.093 Uiso 1 1 calc R . . C201 C 0.1343(7) -0.9173(6) -0.03554(14) 0.0491(13) Uani 1 1 d . . . H48 H 0.0416 -0.8939 -0.0360 0.059 Uiso 1 1 calc R . . C202 C 0.3775(7) -0.9063(6) -0.02371(16) 0.0542(14) Uani 1 1 d . . . H49 H 0.4892 -0.8722 -0.0139 0.065 Uiso 1 1 calc R . . C203 C 0.2920(7) -1.0321(7) -0.04712(17) 0.0568(14) Uani 1 1 d . . . H50 H 0.3317 -1.1019 -0.0566 0.068 Uiso 1 1 calc R . . C301 C 0.2635(8) -0.4020(7) 0.06088(16) 0.0564(14) Uani 1 1 d . . . H51 H 0.1669 -0.4294 0.0447 0.068 Uiso 1 1 calc R . . C302 C 0.5020(8) -0.3780(6) 0.08357(14) 0.0517(13) Uani 1 1 d . . . H52 H 0.6041 -0.3864 0.0859 0.062 Uiso 1 1 calc R . . C303 C 0.4482(8) -0.3022(7) 0.10883(15) 0.0536(14) Uani 1 1 d . . . H53 H 0.5041 -0.2488 0.1320 0.064 Uiso 1 1 calc R . . C401 C 0.3048(8) -0.3111(8) 0.55246(15) 0.0570(15) Uani 1 1 d . . . H54 H 0.2169 -0.3688 0.5342 0.068 Uiso 1 1 calc R . . C402 C 0.5027(7) -0.1258(8) 0.58559(14) 0.0558(15) Uani 1 1 d . . . H55 H 0.5792 -0.0270 0.5949 0.067 Uiso 1 1 calc R . . C403 C 0.4890(7) -0.2532(7) 0.59885(15) 0.0538(14) Uani 1 1 d . . . H56 H 0.5554 -0.2604 0.6189 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0542(2) 0.0460(2) 0.0497(2) 0.01879(17) 0.00927(18) 0.0271(2) Ag2 0.0776(3) 0.1083(4) 0.0509(2) 0.0406(3) 0.0288(2) 0.0642(3) Ag3 0.0765(3) 0.0442(2) 0.0431(2) -0.00233(17) 0.0089(2) 0.0249(2) Cl1 0.0510(7) 0.0550(8) 0.0541(7) 0.0097(6) 0.0031(6) 0.0247(6) Cl2 0.0481(8) 0.0609(9) 0.0625(8) 0.0020(7) -0.0046(7) 0.0107(7) Cl3 0.161(2) 0.0521(10) 0.0827(13) -0.0048(9) -0.0622(15) 0.0273(12) O11 0.086(3) 0.053(3) 0.136(5) 0.011(3) -0.010(3) 0.036(3) O12 0.096(3) 0.090(4) 0.051(2) 0.007(2) -0.009(2) 0.037(3) O13 0.057(2) 0.087(4) 0.084(3) 0.010(3) -0.006(2) 0.023(2) O14 0.087(3) 0.083(4) 0.089(3) 0.013(3) 0.028(3) 0.047(3) O21 0.132(5) 0.078(4) 0.070(3) 0.005(3) -0.014(3) 0.048(3) O22 0.260(10) 0.075(4) 0.151(6) 0.055(4) -0.119(7) -0.047(5) O23 0.056(3) 0.235(9) 0.172(7) -0.111(7) 0.004(4) 0.033(4) O24 0.046(2) 0.050(3) 0.166(5) 0.007(3) -0.010(3) 0.013(2) O31 0.147(6) 0.079(4) 0.156(6) 0.019(4) -0.039(5) 0.047(4) O32 0.121(6) 0.251(11) 0.117(6) -0.020(6) -0.034(5) 0.064(6) O33 0.245(12) 0.197(10) 0.156(8) -0.024(7) -0.080(8) 0.106(9) O34 0.194(8) 0.124(6) 0.139(6) 0.067(5) -0.040(6) -0.003(6) N1 0.044(2) 0.042(2) 0.038(2) 0.0075(17) 0.0098(18) 0.0226(19) N2 0.046(2) 0.038(2) 0.040(2) 0.0024(17) -0.0007(18) 0.0224(19) N3 0.045(2) 0.040(2) 0.039(2) 0.0062(17) 0.0034(18) 0.0203(19) N4 0.041(2) 0.047(3) 0.044(2) 0.0126(19) 0.0001(19) 0.018(2) N101 0.085(4) 0.107(5) 0.040(2) 0.030(3) 0.029(3) 0.071(4) N102 0.074(3) 0.092(4) 0.036(2) 0.020(2) 0.017(2) 0.054(3) N201 0.050(2) 0.044(3) 0.044(2) 0.0007(19) 0.002(2) 0.023(2) N202 0.065(3) 0.043(3) 0.041(2) -0.0015(19) 0.001(2) 0.025(2) N301 0.059(3) 0.043(3) 0.054(3) -0.006(2) 0.010(2) 0.022(2) N302 0.070(3) 0.044(3) 0.041(2) -0.0029(19) 0.002(2) 0.025(2) N401 0.063(3) 0.064(3) 0.034(2) 0.008(2) 0.004(2) 0.035(3) N402 0.059(3) 0.091(4) 0.043(2) 0.023(3) 0.016(2) 0.044(3) C1 0.061(3) 0.045(3) 0.041(3) 0.008(2) 0.005(2) 0.025(3) C2 0.067(3) 0.052(3) 0.039(2) 0.008(2) 0.003(2) 0.035(3) C3 0.058(3) 0.037(3) 0.044(3) 0.013(2) 0.002(2) 0.018(2) C4 0.044(3) 0.054(3) 0.048(3) 0.018(2) 0.011(2) 0.012(3) C10 0.048(3) 0.061(3) 0.031(2) 0.016(2) 0.009(2) 0.018(3) C11 0.034(2) 0.065(4) 0.030(2) 0.004(2) -0.002(2) 0.018(2) C12 0.054(3) 0.063(4) 0.038(2) 0.013(2) 0.003(2) 0.033(3) C13 0.063(3) 0.095(5) 0.041(3) 0.013(3) 0.008(3) 0.056(4) C14 0.047(3) 0.100(5) 0.041(3) 0.030(3) 0.017(2) 0.042(3) C15 0.049(3) 0.065(4) 0.055(3) 0.022(3) 0.009(3) 0.014(3) C16 0.050(3) 0.055(3) 0.039(3) 0.002(2) 0.003(2) 0.013(3) C17 0.077(4) 0.169(8) 0.050(3) 0.044(4) 0.027(3) 0.083(5) C20 0.049(3) 0.057(3) 0.048(3) 0.001(2) -0.004(2) 0.034(3) C21 0.043(3) 0.044(3) 0.048(3) 0.000(2) 0.002(2) 0.029(2) C22 0.046(3) 0.033(3) 0.058(3) -0.007(2) -0.004(3) 0.014(2) C23 0.051(3) 0.034(3) 0.057(3) 0.001(2) 0.011(3) 0.016(2) C24 0.044(3) 0.043(3) 0.050(3) 0.001(2) -0.001(2) 0.024(2) C25 0.068(4) 0.035(3) 0.054(3) -0.004(2) 0.003(3) 0.015(3) C26 0.064(3) 0.038(3) 0.058(3) 0.005(2) 0.007(3) 0.019(3) C27 0.052(3) 0.046(3) 0.054(3) 0.003(2) 0.003(3) 0.020(3) C30 0.057(3) 0.044(3) 0.060(3) 0.003(3) -0.010(3) 0.025(3) C31 0.045(3) 0.048(3) 0.042(3) -0.001(2) -0.004(2) 0.025(2) C32 0.065(4) 0.058(4) 0.043(3) 0.011(3) 0.001(3) 0.028(3) C33 0.063(4) 0.066(4) 0.041(3) -0.008(3) 0.005(3) 0.028(3) C34 0.046(3) 0.047(3) 0.055(3) -0.006(3) 0.011(3) 0.020(2) C35 0.063(3) 0.051(3) 0.043(3) 0.004(2) 0.008(3) 0.017(3) C36 0.061(3) 0.054(3) 0.034(2) -0.002(2) 0.005(2) 0.021(3) C37 0.059(4) 0.051(4) 0.088(4) -0.017(3) 0.016(3) 0.019(3) C40 0.070(4) 0.041(3) 0.041(3) 0.005(2) -0.002(3) 0.025(3) C41 0.057(3) 0.037(3) 0.038(2) -0.001(2) -0.010(2) 0.021(2) C42 0.063(3) 0.065(4) 0.049(3) 0.010(3) -0.003(3) 0.039(3) C43 0.062(3) 0.068(4) 0.053(3) 0.004(3) 0.004(3) 0.037(3) C44 0.068(4) 0.046(3) 0.039(3) 0.000(2) -0.003(3) 0.024(3) C45 0.076(4) 0.065(4) 0.045(3) 0.005(3) -0.006(3) 0.046(3) C46 0.059(3) 0.053(3) 0.044(3) 0.003(2) 0.000(3) 0.030(3) C47 0.096(5) 0.067(4) 0.042(3) -0.004(3) -0.001(3) 0.042(4) C101 0.069(4) 0.087(5) 0.054(3) 0.033(3) 0.030(3) 0.048(4) C102 0.118(6) 0.094(6) 0.043(3) 0.007(3) 0.018(3) 0.072(5) C103 0.133(7) 0.100(6) 0.044(3) 0.014(3) 0.021(4) 0.089(6) C201 0.065(3) 0.047(3) 0.044(3) 0.005(2) 0.012(3) 0.033(3) C202 0.059(3) 0.044(3) 0.061(3) -0.003(3) -0.012(3) 0.025(3) C203 0.065(4) 0.046(3) 0.066(4) -0.002(3) -0.006(3) 0.033(3) C301 0.065(4) 0.052(3) 0.048(3) -0.004(3) 0.005(3) 0.024(3) C302 0.069(4) 0.055(3) 0.040(3) 0.007(2) 0.003(3) 0.035(3) C303 0.071(4) 0.053(3) 0.038(3) -0.002(2) 0.003(3) 0.030(3) C401 0.062(3) 0.076(5) 0.035(3) 0.014(3) 0.006(3) 0.031(3) C402 0.062(3) 0.076(4) 0.038(3) 0.010(3) 0.012(3) 0.038(3) C403 0.061(3) 0.072(4) 0.040(3) 0.010(3) 0.003(3) 0.039(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.317(5) . ? Ag1 N3 2.332(4) . ? Ag1 N4 2.423(6) . ? Ag1 N1 2.461(5) . ? Ag2 N102 2.100(5) . ? Ag2 N402 2.103(5) . ? Ag2 Ag2 3.081(3) 2_656 ? Ag3 N202 2.113(5) . ? Ag3 N302 2.119(5) . ? Ag3 Ag3 3.054(4) 2_645 ? Cl1 O11 1.412(5) . ? Cl1 O13 1.423(5) . ? Cl1 O12 1.427(5) . ? Cl1 O14 1.450(5) . ? Cl2 O22 1.376(7) . ? Cl2 O23 1.393(7) . ? Cl2 O24 1.403(5) . ? Cl2 O21 1.424(5) . ? Cl3 O32 1.319(8) . ? Cl3 O31 1.390(7) . ? Cl3 O34 1.399(8) . ? Cl3 O33 1.506(13) . ? N1 C10 1.487(6) . ? N1 C1 1.495(7) . ? N1 H1 0.9300 . ? N2 C20 1.460(7) . ? N2 C2 1.474(6) . ? N2 H2 0.9300 . ? N3 C3 1.484(7) . ? N3 C30 1.485(7) . ? N3 H3 0.9300 . ? N4 C40 1.452(7) . ? N4 C4 1.463(6) . ? N4 H4 0.9300 . ? N101 C101 1.342(8) . ? N101 C103 1.355(10) . ? N101 C17 1.480(8) . ? N102 C101 1.296(8) . ? N102 C102 1.377(9) . ? N201 C201 1.344(7) . ? N201 C203 1.380(7) . ? N201 C27 1.462(7) 2_645 ? N202 C201 1.307(7) . ? N202 C202 1.383(7) . ? N301 C301 1.357(7) . ? N301 C303 1.384(7) . ? N301 C37 1.465(7) . ? N302 C301 1.321(8) . ? N302 C302 1.374(7) . ? N401 C401 1.343(7) . ? N401 C403 1.351(8) . ? N401 C47 1.473(8) 2_656 ? N402 C401 1.303(8) . ? N402 C402 1.397(7) . ? C1 C2 1.486(8) . ? C1 H5 0.9900 . ? C1 H6 0.9900 . ? C2 H7 0.9900 . ? C2 H8 0.9900 . ? C3 C4 1.520(7) . ? C3 H9 0.9900 . ? C3 H10 0.9900 . ? C4 H11 0.9900 . ? C4 H12 0.9900 . ? C10 C11 1.504(7) . ? C10 H13 0.9900 . ? C10 H14 0.9900 . ? C11 C12 1.384(8) . ? C11 C16 1.392(8) . ? C12 C13 1.390(8) . ? C12 H15 0.9500 . ? C13 C14 1.369(9) . ? C13 H16 0.9500 . ? C14 C15 1.405(9) . ? C14 C17 1.511(8) . ? C15 C16 1.380(8) . ? C15 H17 0.9500 . ? C16 H18 0.9500 . ? C17 H19 0.9900 . ? C17 H20 0.9900 . ? C20 C21 1.510(7) . ? C20 H21 0.9900 . ? C20 H22 0.9900 . ? C21 C22 1.362(8) . ? C21 C26 1.388(7) . ? C22 C23 1.375(8) . ? C22 H23 0.9500 . ? C23 C24 1.394(7) . ? C23 H24 0.9500 . ? C24 C25 1.384(8) . ? C24 C27 1.503(8) . ? C25 C26 1.392(8) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 N201 1.462(7) 2_645 ? C27 H27 0.9900 . ? C27 H28 0.9900 . ? C30 C31 1.502(8) . ? C30 H29 0.9900 . ? C30 H30 0.9900 . ? C31 C36 1.355(8) . ? C31 C32 1.387(7) . ? C32 C33 1.380(8) . ? C32 H31 0.9500 . ? C33 C34 1.378(8) . ? C33 H32 0.9500 . ? C34 C35 1.399(8) . ? C34 C37 1.509(8) . ? C35 C36 1.358(8) . ? C35 H33 0.9500 . ? C36 H34 0.9500 . ? C37 H35 0.9900 . ? C37 H36 0.9900 . ? C40 C41 1.510(7) . ? C40 H37 0.9900 . ? C40 H38 0.9900 . ? C41 C42 1.389(8) . ? C41 C46 1.406(7) . ? C42 C43 1.378(8) . ? C42 H39 0.9500 . ? C43 C44 1.378(8) . ? C43 H40 0.9500 . ? C44 C45 1.379(8) . ? C44 C47 1.534(8) . ? C45 C46 1.371(8) . ? C45 H41 0.9500 . ? C46 H42 0.9500 . ? C47 N401 1.473(8) 2_656 ? C47 H43 0.9900 . ? C47 H44 0.9900 . ? C101 H45 0.9500 . ? C102 C103 1.319(9) . ? C102 H46 0.9500 . ? C103 H47 0.9500 . ? C201 H48 0.9500 . ? C202 C203 1.355(8) . ? C202 H49 0.9500 . ? C203 H50 0.9500 . ? C301 H51 0.9500 . ? C302 C303 1.348(8) . ? C302 H52 0.9500 . ? C303 H53 0.9500 . ? C401 H54 0.9500 . ? C402 C403 1.351(8) . ? C402 H55 0.9500 . ? C403 H56 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N3 139.24(15) . . ? N2 Ag1 N4 123.34(16) . . ? N3 Ag1 N4 77.85(17) . . ? N2 Ag1 N1 75.70(16) . . ? N3 Ag1 N1 133.40(15) . . ? N4 Ag1 N1 110.70(17) . . ? N102 Ag2 N402 169.8(2) . . ? N102 Ag2 Ag2 99.40(15) . 2_656 ? N402 Ag2 Ag2 90.07(15) . 2_656 ? N202 Ag3 N302 168.68(18) . . ? N202 Ag3 Ag3 113.62(16) . 2_645 ? N302 Ag3 Ag3 77.37(16) . 2_645 ? O11 Cl1 O13 109.8(3) . . ? O11 Cl1 O12 112.0(3) . . ? O13 Cl1 O12 110.5(3) . . ? O11 Cl1 O14 108.7(3) . . ? O13 Cl1 O14 108.1(3) . . ? O12 Cl1 O14 107.7(3) . . ? O22 Cl2 O23 115.0(7) . . ? O22 Cl2 O24 109.7(5) . . ? O23 Cl2 O24 106.3(4) . . ? O22 Cl2 O21 107.1(4) . . ? O23 Cl2 O21 107.4(4) . . ? O24 Cl2 O21 111.4(4) . . ? O32 Cl3 O31 116.0(6) . . ? O32 Cl3 O34 120.3(6) . . ? O31 Cl3 O34 111.8(4) . . ? O32 Cl3 O33 105.9(5) . . ? O31 Cl3 O33 97.6(6) . . ? O34 Cl3 O33 100.8(7) . . ? C10 N1 C1 113.1(4) . . ? C10 N1 Ag1 117.3(3) . . ? C1 N1 Ag1 106.1(3) . . ? C10 N1 H1 106.5 . . ? C1 N1 H1 106.5 . . ? Ag1 N1 H1 106.5 . . ? C20 N2 C2 113.3(4) . . ? C20 N2 Ag1 116.6(3) . . ? C2 N2 Ag1 105.3(3) . . ? C20 N2 H2 107.0 . . ? C2 N2 H2 107.0 . . ? Ag1 N2 H2 107.0 . . ? C3 N3 C30 110.4(4) . . ? C3 N3 Ag1 107.0(3) . . ? C30 N3 Ag1 115.7(3) . . ? C3 N3 H3 107.8 . . ? C30 N3 H3 107.8 . . ? Ag1 N3 H3 107.8 . . ? C40 N4 C4 111.4(4) . . ? C40 N4 Ag1 119.2(3) . . ? C4 N4 Ag1 102.8(3) . . ? C40 N4 H4 107.6 . . ? C4 N4 H4 107.6 . . ? Ag1 N4 H4 107.6 . . ? C101 N101 C103 106.3(6) . . ? C101 N101 C17 125.8(7) . . ? C103 N101 C17 127.7(6) . . ? C101 N102 C102 104.5(5) . . ? C101 N102 Ag2 125.1(5) . . ? C102 N102 Ag2 130.3(5) . . ? C201 N201 C203 106.7(5) . . ? C201 N201 C27 127.0(5) . 2_645 ? C203 N201 C27 126.3(5) . 2_645 ? C201 N202 C202 106.1(4) . . ? C201 N202 Ag3 127.4(4) . . ? C202 N202 Ag3 126.2(4) . . ? C301 N301 C303 106.8(5) . . ? C301 N301 C37 125.7(5) . . ? C303 N301 C37 127.2(5) . . ? C301 N302 C302 107.0(5) . . ? C301 N302 Ag3 120.9(4) . . ? C302 N302 Ag3 128.7(4) . . ? C401 N401 C403 107.4(5) . . ? C401 N401 C47 125.6(5) . 2_656 ? C403 N401 C47 126.8(5) . 2_656 ? C401 N402 C402 106.4(5) . . ? C401 N402 Ag2 125.5(4) . . ? C402 N402 Ag2 128.0(5) . . ? C2 C1 N1 112.2(4) . . ? C2 C1 H5 109.2 . . ? N1 C1 H5 109.2 . . ? C2 C1 H6 109.2 . . ? N1 C1 H6 109.2 . . ? H5 C1 H6 107.9 . . ? N2 C2 C1 111.1(4) . . ? N2 C2 H7 109.4 . . ? C1 C2 H7 109.4 . . ? N2 C2 H8 109.4 . . ? C1 C2 H8 109.4 . . ? H7 C2 H8 108.0 . . ? N3 C3 C4 111.1(4) . . ? N3 C3 H9 109.4 . . ? C4 C3 H9 109.4 . . ? N3 C3 H10 109.4 . . ? C4 C3 H10 109.4 . . ? H9 C3 H10 108.0 . . ? N4 C4 C3 112.4(4) . . ? N4 C4 H11 109.1 . . ? C3 C4 H11 109.1 . . ? N4 C4 H12 109.1 . . ? C3 C4 H12 109.1 . . ? H11 C4 H12 107.9 . . ? N1 C10 C11 115.2(4) . . ? N1 C10 H13 108.5 . . ? C11 C10 H13 108.5 . . ? N1 C10 H14 108.5 . . ? C11 C10 H14 108.5 . . ? H13 C10 H14 107.5 . . ? C12 C11 C16 118.7(5) . . ? C12 C11 C10 120.4(5) . . ? C16 C11 C10 120.9(5) . . ? C11 C12 C13 120.8(6) . . ? C11 C12 H15 119.6 . . ? C13 C12 H15 119.6 . . ? C14 C13 C12 120.7(6) . . ? C14 C13 H16 119.6 . . ? C12 C13 H16 119.6 . . ? C13 C14 C15 118.9(5) . . ? C13 C14 C17 121.3(7) . . ? C15 C14 C17 119.7(6) . . ? C16 C15 C14 120.3(6) . . ? C16 C15 H17 119.9 . . ? C14 C15 H17 119.9 . . ? C15 C16 C11 120.6(6) . . ? C15 C16 H18 119.7 . . ? C11 C16 H18 119.7 . . ? N101 C17 C14 111.4(5) . . ? N101 C17 H19 109.3 . . ? C14 C17 H19 109.3 . . ? N101 C17 H20 109.3 . . ? C14 C17 H20 109.3 . . ? H19 C17 H20 108.0 . . ? N2 C20 C21 110.9(4) . . ? N2 C20 H21 109.5 . . ? C21 C20 H21 109.5 . . ? N2 C20 H22 109.5 . . ? C21 C20 H22 109.5 . . ? H21 C20 H22 108.0 . . ? C22 C21 C26 118.4(5) . . ? C22 C21 C20 121.3(5) . . ? C26 C21 C20 120.3(5) . . ? C21 C22 C23 122.0(5) . . ? C21 C22 H23 119.0 . . ? C23 C22 H23 119.0 . . ? C22 C23 C24 119.9(5) . . ? C22 C23 H24 120.0 . . ? C24 C23 H24 120.0 . . ? C25 C24 C23 118.9(5) . . ? C25 C24 C27 122.1(5) . . ? C23 C24 C27 118.9(5) . . ? C24 C25 C26 119.9(5) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.8(5) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? N201 C27 C24 114.3(5) 2_645 . ? N201 C27 H27 108.7 2_645 . ? C24 C27 H27 108.7 . . ? N201 C27 H28 108.7 2_645 . ? C24 C27 H28 108.7 . . ? H27 C27 H28 107.6 . . ? N3 C30 C31 110.5(4) . . ? N3 C30 H29 109.6 . . ? C31 C30 H29 109.6 . . ? N3 C30 H30 109.6 . . ? C31 C30 H30 109.6 . . ? H29 C30 H30 108.1 . . ? C36 C31 C32 118.6(5) . . ? C36 C31 C30 120.7(5) . . ? C32 C31 C30 120.8(5) . . ? C33 C32 C31 120.5(5) . . ? C33 C32 H31 119.7 . . ? C31 C32 H31 119.7 . . ? C34 C33 C32 120.6(5) . . ? C34 C33 H32 119.7 . . ? C32 C33 H32 119.7 . . ? C33 C34 C35 117.9(5) . . ? C33 C34 C37 122.0(5) . . ? C35 C34 C37 120.1(6) . . ? C36 C35 C34 120.6(5) . . ? C36 C35 H33 119.7 . . ? C34 C35 H33 119.7 . . ? C31 C36 C35 121.8(5) . . ? C31 C36 H34 119.1 . . ? C35 C36 H34 119.1 . . ? N301 C37 C34 111.6(5) . . ? N301 C37 H35 109.3 . . ? C34 C37 H35 109.3 . . ? N301 C37 H36 109.3 . . ? C34 C37 H36 109.3 . . ? H35 C37 H36 108.0 . . ? N4 C40 C41 114.6(4) . . ? N4 C40 H37 108.6 . . ? C41 C40 H37 108.6 . . ? N4 C40 H38 108.6 . . ? C41 C40 H38 108.6 . . ? H37 C40 H38 107.6 . . ? C42 C41 C46 117.8(5) . . ? C42 C41 C40 119.8(5) . . ? C46 C41 C40 122.3(5) . . ? C43 C42 C41 121.0(5) . . ? C43 C42 H39 119.5 . . ? C41 C42 H39 119.5 . . ? C42 C43 C44 120.8(6) . . ? C42 C43 H40 119.6 . . ? C44 C43 H40 119.6 . . ? C43 C44 C45 118.5(5) . . ? C43 C44 C47 120.0(6) . . ? C45 C44 C47 121.5(5) . . ? C46 C45 C44 121.7(5) . . ? C46 C45 H41 119.2 . . ? C44 C45 H41 119.2 . . ? C45 C46 C41 120.1(5) . . ? C45 C46 H42 119.9 . . ? C41 C46 H42 119.9 . . ? N401 C47 C44 111.8(5) 2_656 . ? N401 C47 H43 109.3 2_656 . ? C44 C47 H43 109.3 . . ? N401 C47 H44 109.3 2_656 . ? C44 C47 H44 109.3 . . ? H43 C47 H44 107.9 . . ? N102 C101 N101 112.0(7) . . ? N102 C101 H45 124.0 . . ? N101 C101 H45 124.0 . . ? C103 C102 N102 110.2(7) . . ? C103 C102 H46 124.9 . . ? N102 C102 H46 124.9 . . ? C102 C103 N101 106.8(7) . . ? C102 C103 H47 126.6 . . ? N101 C103 H47 126.6 . . ? N202 C201 N201 111.8(5) . . ? N202 C201 H48 124.1 . . ? N201 C201 H48 124.1 . . ? C203 C202 N202 109.0(5) . . ? C203 C202 H49 125.5 . . ? N202 C202 H49 125.5 . . ? C202 C203 N201 106.4(5) . . ? C202 C203 H50 126.8 . . ? N201 C203 H50 126.8 . . ? N302 C301 N301 110.3(5) . . ? N302 C301 H51 124.9 . . ? N301 C301 H51 124.9 . . ? C303 C302 N302 109.1(5) . . ? C303 C302 H52 125.5 . . ? N302 C302 H52 125.5 . . ? C302 C303 N301 106.8(5) . . ? C302 C303 H53 126.6 . . ? N301 C303 H53 126.6 . . ? N402 C401 N401 111.1(5) . . ? N402 C401 H54 124.5 . . ? N401 C401 H54 124.5 . . ? C403 C402 N402 107.4(6) . . ? C403 C402 H55 126.3 . . ? N402 C402 H55 126.3 . . ? N401 C403 C402 107.7(5) . . ? N401 C403 H56 126.1 . . ? C402 C403 H56 126.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C10 -128.1(4) . . . . ? N3 Ag1 N1 C10 18.5(4) . . . . ? N4 Ag1 N1 C10 111.3(4) . . . . ? N2 Ag1 N1 C1 -0.5(3) . . . . ? N3 Ag1 N1 C1 146.1(3) . . . . ? N4 Ag1 N1 C1 -121.2(3) . . . . ? N3 Ag1 N2 C20 63.3(4) . . . . ? N4 Ag1 N2 C20 -48.9(4) . . . . ? N1 Ag1 N2 C20 -154.5(4) . . . . ? N3 Ag1 N2 C2 -170.2(3) . . . . ? N4 Ag1 N2 C2 77.7(4) . . . . ? N1 Ag1 N2 C2 -27.9(3) . . . . ? N2 Ag1 N3 C3 -139.6(3) . . . . ? N4 Ag1 N3 C3 -12.0(3) . . . . ? N1 Ag1 N3 C3 95.2(4) . . . . ? N2 Ag1 N3 C30 96.8(4) . . . . ? N4 Ag1 N3 C30 -135.5(4) . . . . ? N1 Ag1 N3 C30 -28.4(4) . . . . ? N2 Ag1 N4 C40 -112.5(3) . . . . ? N3 Ag1 N4 C40 105.7(4) . . . . ? N1 Ag1 N4 C40 -26.4(4) . . . . ? N2 Ag1 N4 C4 123.7(3) . . . . ? N3 Ag1 N4 C4 -18.1(3) . . . . ? N1 Ag1 N4 C4 -150.1(3) . . . . ? N402 Ag2 N102 C101 -54.9(13) . . . . ? Ag2 Ag2 N102 C101 102.4(4) 2_656 . . . ? N402 Ag2 N102 C102 123.9(12) . . . . ? Ag2 Ag2 N102 C102 -78.8(5) 2_656 . . . ? N302 Ag3 N202 C201 76.0(10) . . . . ? Ag3 Ag3 N202 C201 -118.3(4) 2_645 . . . ? N302 Ag3 N202 C202 -110.8(10) . . . . ? Ag3 Ag3 N202 C202 54.9(5) 2_645 . . . ? N202 Ag3 N302 C301 -67.6(11) . . . . ? Ag3 Ag3 N302 C301 125.9(5) 2_645 . . . ? N202 Ag3 N302 C302 88.7(11) . . . . ? Ag3 Ag3 N302 C302 -77.9(5) 2_645 . . . ? N102 Ag2 N402 C401 54.4(14) . . . . ? Ag2 Ag2 N402 C401 -103.3(5) 2_656 . . . ? N102 Ag2 N402 C402 -127.7(11) . . . . ? Ag2 Ag2 N402 C402 74.6(4) 2_656 . . . ? C10 N1 C1 C2 159.9(4) . . . . ? Ag1 N1 C1 C2 29.9(5) . . . . ? C20 N2 C2 C1 -175.3(5) . . . . ? Ag1 N2 C2 C1 56.1(5) . . . . ? N1 C1 C2 N2 -60.7(6) . . . . ? C30 N3 C3 C4 167.7(4) . . . . ? Ag1 N3 C3 C4 41.0(5) . . . . ? C40 N4 C4 C3 -81.8(6) . . . . ? Ag1 N4 C4 C3 47.0(5) . . . . ? N3 C3 C4 N4 -64.1(6) . . . . ? C1 N1 C10 C11 65.3(6) . . . . ? Ag1 N1 C10 C11 -170.6(4) . . . . ? N1 C10 C11 C12 93.3(6) . . . . ? N1 C10 C11 C16 -85.5(6) . . . . ? C16 C11 C12 C13 1.0(7) . . . . ? C10 C11 C12 C13 -177.7(5) . . . . ? C11 C12 C13 C14 0.3(8) . . . . ? C12 C13 C14 C15 -1.6(8) . . . . ? C12 C13 C14 C17 176.5(5) . . . . ? C13 C14 C15 C16 1.6(8) . . . . ? C17 C14 C15 C16 -176.5(5) . . . . ? C14 C15 C16 C11 -0.3(8) . . . . ? C12 C11 C16 C15 -1.0(8) . . . . ? C10 C11 C16 C15 177.8(5) . . . . ? C101 N101 C17 C14 -96.3(8) . . . . ? C103 N101 C17 C14 78.1(9) . . . . ? C13 C14 C17 N101 -91.2(7) . . . . ? C15 C14 C17 N101 86.8(8) . . . . ? C2 N2 C20 C21 179.7(4) . . . . ? Ag1 N2 C20 C21 -57.7(5) . . . . ? N2 C20 C21 C22 99.2(6) . . . . ? N2 C20 C21 C26 -78.8(6) . . . . ? C26 C21 C22 C23 1.1(8) . . . . ? C20 C21 C22 C23 -176.9(5) . . . . ? C21 C22 C23 C24 -0.9(8) . . . . ? C22 C23 C24 C25 0.6(8) . . . . ? C22 C23 C24 C27 -176.9(5) . . . . ? C23 C24 C25 C26 -0.5(8) . . . . ? C27 C24 C25 C26 176.8(5) . . . . ? C22 C21 C26 C25 -1.0(8) . . . . ? C20 C21 C26 C25 177.0(5) . . . . ? C24 C25 C26 C21 0.7(9) . . . . ? C25 C24 C27 N201 31.0(7) . . . 2_645 ? C23 C24 C27 N201 -151.6(5) . . . 2_645 ? C3 N3 C30 C31 172.0(4) . . . . ? Ag1 N3 C30 C31 -66.2(5) . . . . ? N3 C30 C31 C36 77.7(7) . . . . ? N3 C30 C31 C32 -103.5(6) . . . . ? C36 C31 C32 C33 -0.7(8) . . . . ? C30 C31 C32 C33 -179.6(5) . . . . ? C31 C32 C33 C34 0.8(9) . . . . ? C32 C33 C34 C35 -2.0(9) . . . . ? C32 C33 C34 C37 177.4(5) . . . . ? C33 C34 C35 C36 3.2(9) . . . . ? C37 C34 C35 C36 -176.2(5) . . . . ? C32 C31 C36 C35 1.9(9) . . . . ? C30 C31 C36 C35 -179.2(5) . . . . ? C34 C35 C36 C31 -3.2(9) . . . . ? C301 N301 C37 C34 -128.1(6) . . . . ? C303 N301 C37 C34 58.5(9) . . . . ? C33 C34 C37 N301 64.2(8) . . . . ? C35 C34 C37 N301 -116.4(6) . . . . ? C4 N4 C40 C41 175.7(4) . . . . ? Ag1 N4 C40 C41 56.2(6) . . . . ? N4 C40 C41 C42 -143.3(5) . . . . ? N4 C40 C41 C46 40.4(7) . . . . ? C46 C41 C42 C43 -1.2(9) . . . . ? C40 C41 C42 C43 -177.7(5) . . . . ? C41 C42 C43 C44 1.0(10) . . . . ? C42 C43 C44 C45 -0.4(9) . . . . ? C42 C43 C44 C47 178.8(6) . . . . ? C43 C44 C45 C46 0.0(9) . . . . ? C47 C44 C45 C46 -179.2(6) . . . . ? C44 C45 C46 C41 -0.2(9) . . . . ? C42 C41 C46 C45 0.8(8) . . . . ? C40 C41 C46 C45 177.2(5) . . . . ? C43 C44 C47 N401 117.9(6) . . . 2_656 ? C45 C44 C47 N401 -62.9(8) . . . 2_656 ? C102 N102 C101 N101 0.5(6) . . . . ? Ag2 N102 C101 N101 179.6(3) . . . . ? C103 N101 C101 N102 -0.2(6) . . . . ? C17 N101 C101 N102 175.2(5) . . . . ? C101 N102 C102 C103 -0.6(7) . . . . ? Ag2 N102 C102 C103 -179.6(4) . . . . ? N102 C102 C103 N101 0.5(8) . . . . ? C101 N101 C103 C102 -0.2(7) . . . . ? C17 N101 C103 C102 -175.5(5) . . . . ? C202 N202 C201 N201 0.9(6) . . . . ? Ag3 N202 C201 N201 175.2(3) . . . . ? C203 N201 C201 N202 -0.8(6) . . . . ? C27 N201 C201 N202 179.2(5) 2_645 . . . ? C201 N202 C202 C203 -0.6(7) . . . . ? Ag3 N202 C202 C203 -175.0(4) . . . . ? N202 C202 C203 N201 0.1(7) . . . . ? C201 N201 C203 C202 0.4(7) . . . . ? C27 N201 C203 C202 -179.6(5) 2_645 . . . ? C302 N302 C301 N301 -0.8(7) . . . . ? Ag3 N302 C301 N301 159.9(4) . . . . ? C303 N301 C301 N302 0.5(7) . . . . ? C37 N301 C301 N302 -174.1(6) . . . . ? C301 N302 C302 C303 0.9(7) . . . . ? Ag3 N302 C302 C303 -157.9(4) . . . . ? N302 C302 C303 N301 -0.6(7) . . . . ? C301 N301 C303 C302 0.0(7) . . . . ? C37 N301 C303 C302 174.5(6) . . . . ? C402 N402 C401 N401 0.3(6) . . . . ? Ag2 N402 C401 N401 178.6(3) . . . . ? C403 N401 C401 N402 -0.9(6) . . . . ? C47 N401 C401 N402 -176.4(5) 2_656 . . . ? C401 N402 C402 C403 0.4(6) . . . . ? Ag2 N402 C402 C403 -177.9(4) . . . . ? C401 N401 C403 C402 1.1(6) . . . . ? C47 N401 C403 C402 176.6(5) 2_656 . . . ? N402 C402 C403 N401 -0.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.753 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.102 #====END data_[Ag(L2)]NO3_(3) _database_code_CSD 201029 _audit_creation_date 'Wed Feb 12 22:25:15 2003' _audit_creation_method SHELXL-97 _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ag(L2)]NO3 ' _chemical_formula_sum 'C24 H24 Ag N7 O3' _chemical_formula_weight 566.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.8499(4) _cell_length_b 9.4345(4) _cell_length_c 16.5889(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.7920(10) _cell_angle_gamma 90.00 _cell_volume 2409.11(15) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 10186 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11763 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2755 _reflns_number_gt 2429 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1985)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+2.5281P] 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 2755 _refine_ls_number_parameters 174 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.297 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.29005(3) 0.2500 0.04432(13) Uani 1 2 d S . . O1 O 0.2927(5) 0.7667(14) 0.5674(5) 0.096(3) Uani 0.50 1 d PD . . O2 O 0.2543(7) 0.7195(11) 0.4342(5) 0.099(4) Uani 0.50 1 d PD . . O3 O 0.1652(4) 0.7983(6) 0.4981(5) 0.0863(19) Uani 0.50 1 d PD . . N1 N 0.01992(15) 0.4863(2) 0.33999(14) 0.0383(5) Uani 1 1 d . . . N2 N 0.2500 0.7500 0.5000 0.091(2) Uani 1 2 d SD . . N11 N -0.18780(15) -0.0282(2) 0.30170(14) 0.0380(5) Uani 1 1 d . . . N12 N -0.09842(15) 0.1159(3) 0.25894(14) 0.0400(5) Uani 1 1 d . . . C1 C -0.0149(2) 0.6107(3) 0.29025(18) 0.0450(7) Uani 1 1 d . . . H1 H 0.0054 0.6981 0.3220 0.054 Uiso 1 1 calc R . . H2 H -0.0792 0.6092 0.2778 0.054 Uiso 1 1 calc R . . C10 C 0.05693(18) 0.5074(3) 0.41511(17) 0.0399(6) Uani 1 1 d . . . H3 H 0.0585 0.6018 0.4354 0.048 Uiso 1 1 calc R . . C11 C 0.09771(18) 0.3965(3) 0.47352(17) 0.0375(6) Uani 1 1 d . . . C12 C 0.0863(2) 0.2526(3) 0.4573(2) 0.0507(8) Uani 1 1 d . . . H4 H 0.0472 0.2218 0.4077 0.061 Uiso 1 1 calc R . . C13 C 0.1312(2) 0.1537(3) 0.51238(19) 0.0522(8) Uani 1 1 d . . . H5 H 0.1227 0.0556 0.5004 0.063 Uiso 1 1 calc R . . C14 C 0.18852(18) 0.1963(3) 0.58516(18) 0.0395(6) Uani 1 1 d . . . C15 C 0.1971(2) 0.3394(3) 0.60234(19) 0.0470(7) Uani 1 1 d . . . H6 H 0.2346 0.3701 0.6529 0.056 Uiso 1 1 calc R . . C16 C 0.1525(2) 0.4387(3) 0.54763(18) 0.0453(7) Uani 1 1 d . . . H7 H 0.1593 0.5367 0.5608 0.054 Uiso 1 1 calc R . . C17 C 0.23989(19) 0.0888(3) 0.6446(2) 0.0458(7) Uani 1 1 d . . . H8 H 0.2594 0.0119 0.6128 0.055 Uiso 1 1 calc R . . H9 H 0.2921 0.1350 0.6794 0.055 Uiso 1 1 calc R . . C101 C -0.14486(18) 0.0962(3) 0.31396(17) 0.0395(6) Uani 1 1 d . . . H10 H -0.1478 0.1613 0.3569 0.047 Uiso 1 1 calc R . . C102 C -0.11189(19) -0.0041(3) 0.20955(18) 0.0420(6) Uani 1 1 d . . . H11 H -0.0862 -0.0213 0.1643 0.050 Uiso 1 1 calc R . . C103 C -0.16676(19) -0.0929(3) 0.23509(17) 0.0407(6) Uani 1 1 d . . . H12 H -0.1868 -0.1822 0.2117 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0511(2) 0.02881(16) 0.0513(2) 0.000 0.00868(14) 0.000 O1 0.098(7) 0.103(7) 0.080(6) 0.021(5) 0.010(5) -0.013(6) O2 0.180(12) 0.062(4) 0.077(6) -0.015(4) 0.074(7) -0.007(7) O3 0.106(5) 0.052(3) 0.103(5) -0.025(3) 0.030(4) -0.010(3) N1 0.0444(13) 0.0306(11) 0.0397(12) -0.0011(9) 0.0098(10) 0.0034(9) N2 0.164(7) 0.047(3) 0.072(4) 0.004(3) 0.043(5) -0.035(4) N11 0.0382(12) 0.0352(12) 0.0389(12) 0.0049(9) 0.0056(9) -0.0007(9) N12 0.0425(13) 0.0364(12) 0.0401(12) 0.0011(10) 0.0077(10) -0.0023(9) C1 0.0577(18) 0.0307(13) 0.0444(15) -0.0006(12) 0.0080(13) 0.0064(12) C10 0.0461(16) 0.0336(13) 0.0417(15) -0.0045(11) 0.0141(12) -0.0011(11) C11 0.0416(14) 0.0366(14) 0.0363(14) -0.0016(11) 0.0134(11) -0.0023(11) C12 0.067(2) 0.0390(15) 0.0394(16) -0.0040(12) -0.0004(14) -0.0053(14) C13 0.074(2) 0.0344(14) 0.0446(16) -0.0031(13) 0.0075(15) -0.0043(15) C14 0.0377(14) 0.0406(15) 0.0421(14) 0.0040(12) 0.0129(11) -0.0033(11) C15 0.0498(17) 0.0436(15) 0.0427(15) 0.0012(13) 0.0015(13) -0.0132(13) C16 0.0537(17) 0.0357(14) 0.0448(16) -0.0038(12) 0.0087(13) -0.0088(12) C17 0.0379(15) 0.0472(16) 0.0531(17) 0.0086(14) 0.0121(13) -0.0008(12) C101 0.0410(15) 0.0364(14) 0.0385(14) -0.0015(11) 0.0042(11) -0.0009(11) C102 0.0503(16) 0.0379(14) 0.0379(14) 0.0019(12) 0.0106(12) 0.0042(12) C103 0.0472(16) 0.0299(13) 0.0404(15) -0.0003(11) 0.0012(12) 0.0002(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 Ag1 N12 2.295(2) . ? Ag1 N12 2.295(2) 2 ? Ag1 N1 2.352(2) . ? Ag1 N1 2.352(2) 2 ? O1 O2 0.750(11) 7_566 ? O1 N2 1.171(8) . ? O1 O3 1.532(12) 7_566 ? O2 O1 0.750(11) 7_566 ? O2 N2 1.146(6) . ? O2 O3 1.495(12) 7_566 ? O3 N2 1.413(6) . ? O3 O2 1.495(12) 7_566 ? O3 O1 1.532(12) 7_566 ? N1 C10 1.260(4) . ? N1 C1 1.465(4) . ? N2 O2 1.146(6) 7_566 ? N2 O1 1.171(8) 7_566 ? N2 O3 1.412(6) 7_566 ? N11 C101 1.348(4) . ? N11 C103 1.371(4) . ? N11 C17 1.467(4) 5_556 ? N12 C101 1.315(4) . ? N12 C102 1.384(4) . ? C1 C1 1.519(6) 2 ? C1 H1 0.9900 . ? C1 H2 0.9900 . ? C10 C11 1.467(4) . ? C10 H3 0.9500 . ? C11 C16 1.384(4) . ? C11 C12 1.388(4) . ? C12 C13 1.379(5) . ? C12 H4 0.9500 . ? C13 C14 1.386(4) . ? C13 H5 0.9500 . ? C14 C15 1.380(4) . ? C14 C17 1.510(4) . ? C15 C16 1.377(4) . ? C15 H6 0.9500 . ? C16 H7 0.9500 . ? C17 N11 1.467(4) 5_556 ? C17 H8 0.9900 . ? C17 H9 0.9900 . ? C101 H10 0.9500 . ? C102 C103 1.346(4) . ? C102 H11 0.9500 . ? C103 H12 0.9500 . ? 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 N12 Ag1 N12 88.54(12) . 2 ? N12 Ag1 N1 120.87(8) . . ? N12 Ag1 N1 127.90(8) 2 . ? N12 Ag1 N1 127.90(8) . 2 ? N12 Ag1 N1 120.87(8) 2 2 ? N1 Ag1 N1 76.16(11) . 2 ? O2 O1 N2 69.3(8) 7_566 . ? O2 O1 O3 129.8(12) 7_566 7_566 ? N2 O1 O3 61.3(5) . 7_566 ? O1 O2 N2 73.0(8) 7_566 . ? O1 O2 O3 135.2(12) 7_566 7_566 ? N2 O2 O3 63.1(5) . 7_566 ? N2 O3 O2 46.3(3) . 7_566 ? N2 O3 O1 46.7(3) . 7_566 ? O2 O3 O1 92.8(5) 7_566 7_566 ? C10 N1 C1 117.0(2) . . ? C10 N1 Ag1 135.4(2) . . ? C1 N1 Ag1 107.32(16) . . ? O2 N2 O2 179.997(2) 7_566 . ? O2 N2 O1 142.2(5) 7_566 7_566 ? O2 N2 O1 37.7(5) . 7_566 ? O2 N2 O1 37.8(5) 7_566 . ? O2 N2 O1 142.3(5) . . ? O1 N2 O1 179.999(4) 7_566 . ? O2 N2 O3 109.4(6) 7_566 7_566 ? O2 N2 O3 70.6(6) . 7_566 ? O1 N2 O3 107.9(5) 7_566 7_566 ? O1 N2 O3 72.1(5) . 7_566 ? O2 N2 O3 70.6(6) 7_566 . ? O2 N2 O3 109.4(6) . . ? O1 N2 O3 72.1(5) 7_566 . ? O1 N2 O3 107.9(5) . . ? O3 N2 O3 180.0(5) 7_566 . ? C101 N11 C103 107.3(2) . . ? C101 N11 C17 125.8(3) . 5_556 ? C103 N11 C17 126.6(2) . 5_556 ? C101 N12 C102 105.2(2) . . ? C101 N12 Ag1 130.37(19) . . ? C102 N12 Ag1 123.97(19) . . ? N1 C1 C1 109.9(2) . 2 ? N1 C1 H1 109.7 . . ? C1 C1 H1 109.7 2 . ? N1 C1 H2 109.7 . . ? C1 C1 H2 109.7 2 . ? H1 C1 H2 108.2 . . ? N1 C10 C11 124.6(3) . . ? N1 C10 H3 117.7 . . ? C11 C10 H3 117.7 . . ? C16 C11 C12 118.6(3) . . ? C16 C11 C10 117.8(3) . . ? C12 C11 C10 123.6(3) . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H4 119.7 . . ? C11 C12 H4 119.7 . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H5 119.7 . . ? C14 C13 H5 119.7 . . ? C15 C14 C13 118.4(3) . . ? C15 C14 C17 120.7(3) . . ? C13 C14 C17 120.9(3) . . ? C16 C15 C14 121.3(3) . . ? C16 C15 H6 119.3 . . ? C14 C15 H6 119.3 . . ? C15 C16 C11 120.3(3) . . ? C15 C16 H7 119.8 . . ? C11 C16 H7 119.8 . . ? N11 C17 C14 111.4(2) 5_556 . ? N11 C17 H8 109.4 5_556 . ? C14 C17 H8 109.4 . . ? N11 C17 H9 109.4 5_556 . ? C14 C17 H9 109.4 . . ? H8 C17 H9 108.0 . . ? N12 C101 N11 111.4(3) . . ? N12 C101 H10 124.3 . . ? N11 C101 H10 124.3 . . ? C103 C102 N12 110.0(3) . . ? C103 C102 H11 125.0 . . ? N12 C102 H11 125.0 . . ? C102 C103 N11 106.0(2) . . ? C102 C103 H12 127.0 . . ? N11 C103 H12 127.0 . . ? 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 N12 Ag1 N1 C10 75.3(3) . . . . ? N12 Ag1 N1 C10 -40.0(3) 2 . . . ? N1 Ag1 N1 C10 -158.6(3) 2 . . . ? N12 Ag1 N1 C1 -110.48(19) . . . . ? N12 Ag1 N1 C1 134.20(18) 2 . . . ? N1 Ag1 N1 C1 15.65(15) 2 . . . ? O1 O2 N2 O2 -2(15) 7_566 . . 7_566 ? O3 O2 N2 O2 -173(15) 7_566 . . 7_566 ? O3 O2 N2 O1 -171.0(17) 7_566 . . 7_566 ? O1 O2 N2 O1 180.002(6) 7_566 . . . ? O3 O2 N2 O1 9.0(17) 7_566 . . . ? O1 O2 N2 O3 171.0(17) 7_566 . . 7_566 ? O1 O2 N2 O3 -9.0(17) 7_566 . . . ? O3 O2 N2 O3 180.001(4) 7_566 . . . ? O3 O1 N2 O2 171.1(17) 7_566 . . 7_566 ? O2 O1 N2 O2 180.000(9) 7_566 . . . ? O3 O1 N2 O2 -8.9(17) 7_566 . . . ? O2 O1 N2 O1 105(17) 7_566 . . 7_566 ? O3 O1 N2 O1 -83(17) 7_566 . . 7_566 ? O2 O1 N2 O3 -171.1(17) 7_566 . . 7_566 ? O2 O1 N2 O3 8.9(17) 7_566 . . . ? O3 O1 N2 O3 179.999(4) 7_566 . . . ? O1 O3 N2 O2 -174.2(11) 7_566 . . 7_566 ? O2 O3 N2 O2 180.000(4) 7_566 . . . ? O1 O3 N2 O2 5.8(11) 7_566 . . . ? O2 O3 N2 O1 174.2(11) 7_566 . . 7_566 ? O2 O3 N2 O1 -5.8(11) 7_566 . . . ? O1 O3 N2 O1 179.998(4) 7_566 . . . ? O2 O3 N2 O3 23(7) 7_566 . . 7_566 ? O1 O3 N2 O3 -152(7) 7_566 . . 7_566 ? N12 Ag1 N12 C101 127.3(3) 2 . . . ? N1 Ag1 N12 C101 -7.2(3) . . . . ? N1 Ag1 N12 C101 -103.6(2) 2 . . . ? N12 Ag1 N12 C102 -43.78(18) 2 . . . ? N1 Ag1 N12 C102 -178.26(19) . . . . ? N1 Ag1 N12 C102 85.3(2) 2 . . . ? C10 N1 C1 C1 130.6(3) . . . 2 ? Ag1 N1 C1 C1 -44.8(3) . . . 2 ? C1 N1 C10 C11 -178.2(3) . . . . ? Ag1 N1 C10 C11 -4.4(5) . . . . ? N1 C10 C11 C16 165.5(3) . . . . ? N1 C10 C11 C12 -12.5(5) . . . . ? C16 C11 C12 C13 -2.4(5) . . . . ? C10 C11 C12 C13 175.5(3) . . . . ? C11 C12 C13 C14 0.0(6) . . . . ? C12 C13 C14 C15 2.3(5) . . . . ? C12 C13 C14 C17 -178.2(3) . . . . ? C13 C14 C15 C16 -2.3(5) . . . . ? C17 C14 C15 C16 178.2(3) . . . . ? C14 C15 C16 C11 -0.1(5) . . . . ? C12 C11 C16 C15 2.5(5) . . . . ? C10 C11 C16 C15 -175.6(3) . . . . ? C15 C14 C17 N11 98.0(3) . . . 5_556 ? C13 C14 C17 N11 -81.5(4) . . . 5_556 ? C102 N12 C101 N11 -0.8(3) . . . . ? Ag1 N12 C101 N11 -173.16(17) . . . . ? C103 N11 C101 N12 0.7(3) . . . . ? C17 N11 C101 N12 174.8(2) 5_556 . . . ? C101 N12 C102 C103 0.7(3) . . . . ? Ag1 N12 C102 C103 173.65(18) . . . . ? N12 C102 C103 N11 -0.3(3) . . . . ? C101 N11 C103 C102 -0.2(3) . . . . ? C17 N11 C103 C102 -174.3(3) 5_556 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.789 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.059 #====END data_[Cu(L2)]ClO4_(4) _database_code_CSD 201030 _audit_creation_date 'Sun Apr 15 21:32:26 2001' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_common ? _chemical_melting_point ' ?' _chemical_formula_moiety [Cu(L2)]ClO4 _chemical_formula_sum 'C24 H24 Cl Cu N6 O4' _chemical_formula_weight 559.48 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7180(7) _cell_length_b 10.1127(7) _cell_length_c 19.0653(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.971(3) _cell_angle_gamma 90.00 _cell_volume 2501.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 12501 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10204 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.6506 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5701 _reflns_number_gt 2025 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^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 5701 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1501 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 0.670 _refine_ls_restrained_S_all 0.670 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.76404(4) 0.30916(4) 0.48526(2) 0.04077(14) Uani 1 1 d . . . Cl1 Cl 0.69957(7) -0.20196(10) 0.67280(5) 0.0455(3) Uani 1 1 d . . . O1 O 0.7680(2) -0.3092(3) 0.67500(13) 0.0832(9) Uani 1 1 d . . . O2 O 0.6642(3) -0.2088(4) 0.73335(17) 0.1271(14) Uani 1 1 d . . . O3 O 0.7503(3) -0.0803(3) 0.67736(19) 0.1104(12) Uani 1 1 d . . . O4 O 0.6154(2) -0.2044(3) 0.60652(15) 0.1087(13) Uani 1 1 d . . . N1 N 0.6964(2) 0.4662(2) 0.51146(15) 0.0342(7) Uani 1 1 d . . . N2 N 0.8103(3) 0.4624(3) 0.41004(18) 0.0550(10) Uani 1 1 d . . . N11 N 0.3910(2) -0.0014(3) 0.65084(14) 0.0347(7) Uani 1 1 d . . . N12 N 0.2898(2) -0.1490(2) 0.57692(14) 0.0340(7) Uani 1 1 d . . . N21 N 1.0264(2) -0.1330(3) 0.33094(14) 0.0333(7) Uani 1 1 d . . . N22 N 1.1135(2) -0.2468(3) 0.43023(14) 0.0376(8) Uani 1 1 d . . . C1 C 0.7400(3) 0.5889(3) 0.49207(18) 0.0493(11) Uani 1 1 d . . . H1 H 0.8085 0.6054 0.5292 0.059 Uiso 1 1 calc R . . H2 H 0.6947 0.6643 0.4936 0.059 Uiso 1 1 calc R . . C2 C 0.7506(3) 0.5802(4) 0.4166(2) 0.0630(13) Uani 1 1 d . . . H3 H 0.6812 0.5759 0.3788 0.076 Uiso 1 1 calc R . . H4 H 0.7855 0.6606 0.4070 0.076 Uiso 1 1 calc R . . C10 C 0.6365(3) 0.4795(3) 0.54967(17) 0.0362(9) Uani 1 1 d . . . H5 H 0.6176 0.5671 0.5579 0.043 Uiso 1 1 calc R . . C11 C 0.5940(3) 0.3722(3) 0.58200(18) 0.0311(9) Uani 1 1 d . . . C12 C 0.5911(3) 0.2416(3) 0.56032(19) 0.0438(11) Uani 1 1 d . . . H6 H 0.6148 0.2190 0.5202 0.053 Uiso 1 1 calc R . . C13 C 0.5549(3) 0.1434(3) 0.59541(19) 0.0454(11) Uani 1 1 d . . . H7 H 0.5545 0.0541 0.5797 0.054 Uiso 1 1 calc R . . C14 C 0.5188(3) 0.1744(3) 0.65368(17) 0.0342(9) Uani 1 1 d . . . C15 C 0.5200(3) 0.3036(4) 0.67454(16) 0.0426(9) Uani 1 1 d . . . H8 H 0.4965 0.3260 0.7147 0.051 Uiso 1 1 calc R . . C16 C 0.5548(3) 0.4031(4) 0.63844(19) 0.0460(10) Uani 1 1 d . . . H9 H 0.5517 0.4927 0.6525 0.055 Uiso 1 1 calc R . . C17 C 0.4850(3) 0.0652(3) 0.69585(18) 0.0417(10) Uani 1 1 d . . . H10 H 0.5410 -0.0008 0.7131 0.050 Uiso 1 1 calc R . . H11 H 0.4733 0.1038 0.7402 0.050 Uiso 1 1 calc R . . C20 C 0.7957(3) 0.4183(3) 0.3463(2) 0.0439(10) Uani 1 1 d . . . H15 H 0.7457 0.4614 0.3063 0.053 Uiso 1 1 calc R . . C21 C 0.8498(3) 0.3053(4) 0.32872(17) 0.0347(8) Uani 1 1 d . . . C22 C 0.8072(3) 0.2399(3) 0.26166(19) 0.0462(11) Uani 1 1 d . . . H16 H 0.7444 0.2702 0.2270 0.055 Uiso 1 1 calc R . . C23 C 0.8561(3) 0.1313(4) 0.24548(19) 0.0437(10) Uani 1 1 d . . . H17 H 0.8253 0.0857 0.2001 0.052 Uiso 1 1 calc R . . C24 C 0.9482(3) 0.0873(3) 0.29328(18) 0.0357(9) Uani 1 1 d . . . C25 C 0.9921(3) 0.1549(3) 0.35968(18) 0.0430(10) Uani 1 1 d . . . H18 H 1.0567 0.1268 0.3929 0.052 Uiso 1 1 calc R . . C26 C 0.9432(3) 0.2624(3) 0.37791(18) 0.0413(10) Uani 1 1 d . . . H19 H 0.9731 0.3066 0.4238 0.050 Uiso 1 1 calc R . . C27 C 1.0022(3) -0.0306(3) 0.27377(16) 0.0411(10) Uani 1 1 d . . . H20 H 0.9577 -0.0689 0.2264 0.049 Uiso 1 1 calc R . . H21 H 1.0669 -0.0006 0.2664 0.049 Uiso 1 1 calc R . . C101 C 0.3852(3) -0.1192(3) 0.61642(17) 0.0365(9) Uani 1 1 d . . . H12 H 0.4430 -0.1739 0.6203 0.044 Uiso 1 1 calc R . . C102 C 0.2318(3) -0.0446(4) 0.5866(2) 0.0467(10) Uani 1 1 d . . . H13 H 0.1593 -0.0365 0.5645 0.056 Uiso 1 1 calc R . . C103 C 0.2936(3) 0.0452(3) 0.6326(2) 0.0439(10) Uani 1 1 d . . . H14 H 0.2726 0.1258 0.6489 0.053 Uiso 1 1 calc R . . C201 C 1.1161(3) -0.1473(3) 0.38612(18) 0.0355(9) Uani 1 1 d . . . H22 H 1.1745 -0.0923 0.3927 0.043 Uiso 1 1 calc R . . C202 C 1.0165(3) -0.2980(4) 0.40138(18) 0.0461(10) Uani 1 1 d . . . H23 H 0.9910 -0.3719 0.4209 0.055 Uiso 1 1 calc R . . C203 C 0.9619(3) -0.2280(3) 0.3408(2) 0.0443(10) Uani 1 1 d . . . H24 H 0.8923 -0.2423 0.3111 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0451(3) 0.0317(3) 0.0437(3) 0.0016(2) 0.0120(2) 0.0051(3) Cl1 0.0405(6) 0.0435(6) 0.0494(6) -0.0063(5) 0.0104(5) -0.0002(6) O1 0.060(2) 0.084(2) 0.0838(19) -0.0289(19) -0.0064(16) 0.039(2) O2 0.185(4) 0.121(3) 0.126(3) 0.048(2) 0.120(3) 0.042(3) O3 0.095(3) 0.068(2) 0.161(3) 0.006(2) 0.033(3) -0.040(2) O4 0.077(2) 0.094(2) 0.107(2) -0.056(2) -0.036(2) 0.050(2) N1 0.035(2) 0.0290(17) 0.0430(18) 0.0029(14) 0.0194(17) -0.0004(15) N2 0.079(3) 0.0365(19) 0.065(2) 0.0156(17) 0.045(2) 0.0254(19) N11 0.036(2) 0.0326(19) 0.0402(18) 0.0019(14) 0.0191(16) -0.0036(17) N12 0.035(2) 0.0318(19) 0.0386(17) 0.0031(13) 0.0175(16) 0.0037(16) N21 0.036(2) 0.0283(17) 0.0340(17) 0.0029(13) 0.0093(16) 0.0034(16) N22 0.037(2) 0.0348(19) 0.0369(17) 0.0025(14) 0.0070(16) -0.0006(15) C1 0.074(3) 0.021(2) 0.066(3) 0.0007(18) 0.040(2) 0.000(2) C2 0.093(4) 0.039(3) 0.082(3) 0.020(2) 0.064(3) 0.019(3) C10 0.040(3) 0.025(2) 0.043(2) -0.0021(16) 0.012(2) 0.0028(19) C11 0.028(2) 0.034(2) 0.033(2) -0.0053(17) 0.0129(18) -0.0047(18) C12 0.057(3) 0.036(2) 0.045(2) -0.0123(18) 0.026(2) -0.013(2) C13 0.057(3) 0.031(2) 0.055(3) -0.0135(18) 0.029(2) -0.009(2) C14 0.034(2) 0.038(2) 0.0304(18) -0.0080(19) 0.0101(17) -0.009(2) C15 0.054(3) 0.051(2) 0.0315(19) -0.015(2) 0.0260(18) -0.007(3) C16 0.058(3) 0.035(2) 0.057(3) -0.0046(19) 0.034(2) -0.002(2) C17 0.047(3) 0.040(2) 0.040(2) -0.0033(18) 0.017(2) -0.009(2) C20 0.042(3) 0.045(3) 0.051(2) 0.015(2) 0.023(2) 0.008(2) C21 0.030(2) 0.035(2) 0.045(2) 0.013(2) 0.0196(18) 0.006(2) C22 0.036(3) 0.050(3) 0.044(2) 0.0081(19) 0.001(2) 0.010(2) C23 0.037(3) 0.047(2) 0.042(2) 0.0067(19) 0.005(2) 0.008(2) C24 0.039(3) 0.038(2) 0.035(2) 0.0067(18) 0.019(2) 0.008(2) C25 0.027(2) 0.056(3) 0.041(2) 0.0014(18) 0.0040(19) 0.014(2) C26 0.041(3) 0.046(3) 0.037(2) 0.0019(18) 0.013(2) 0.006(2) C27 0.046(3) 0.047(2) 0.031(2) 0.0042(17) 0.013(2) 0.009(2) C101 0.047(3) 0.033(2) 0.036(2) -0.0012(17) 0.022(2) 0.007(2) C102 0.030(3) 0.043(3) 0.071(3) 0.003(2) 0.022(2) 0.003(2) C103 0.046(3) 0.023(2) 0.072(3) -0.0048(19) 0.030(2) 0.003(2) C201 0.035(3) 0.031(2) 0.040(2) -0.0041(17) 0.011(2) 0.0037(18) C202 0.044(3) 0.039(2) 0.055(2) 0.001(2) 0.015(2) -0.003(2) C203 0.030(2) 0.047(2) 0.051(2) 0.000(2) 0.0059(19) 0.004(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 N1 1.984(3) . ? Cu1 N12 2.001(3) 3_656 ? Cu1 N22 2.014(3) 3_756 ? Cu1 N2 2.335(3) . ? Cl1 O2 1.392(3) . ? Cl1 O3 1.402(3) . ? Cl1 O4 1.408(2) . ? Cl1 O1 1.426(3) . ? N1 C10 1.271(4) . ? N1 C1 1.475(4) . ? N2 C20 1.248(4) . ? N2 C2 1.474(4) . ? N11 C101 1.350(4) . ? N11 C103 1.351(4) . ? N11 C17 1.460(4) . ? N12 C101 1.315(4) . ? N12 C102 1.371(4) . ? N12 Cu1 2.001(3) 3_656 ? N21 C201 1.341(4) . ? N21 C203 1.360(4) . ? N21 C27 1.461(4) . ? N22 C201 1.319(4) . ? N22 C202 1.366(4) . ? N22 Cu1 2.014(3) 3_756 ? C1 C2 1.496(4) . ? C1 H1 0.9900 . ? C1 H2 0.9900 . ? C2 H3 0.9900 . ? C2 H4 0.9900 . ? C10 C11 1.460(4) . ? C10 H5 0.9500 . ? C11 C12 1.380(4) . ? C11 C16 1.386(4) . ? C12 C13 1.378(4) . ? C12 H6 0.9500 . ? C13 C14 1.391(4) . ? C13 H7 0.9500 . ? C14 C15 1.365(5) . ? C14 C17 1.524(4) . ? C15 C16 1.388(4) . ? C15 H8 0.9500 . ? C16 H9 0.9500 . ? C17 H10 0.9900 . ? C17 H11 0.9900 . ? C20 C21 1.460(5) . ? C20 H15 0.9500 . ? C21 C26 1.388(4) . ? C21 C22 1.389(4) . ? C22 C23 1.372(4) . ? C22 H16 0.9500 . ? C23 C24 1.370(4) . ? C23 H17 0.9500 . ? C24 C25 1.392(4) . ? C24 C27 1.513(4) . ? C25 C26 1.380(4) . ? C25 H18 0.9500 . ? C26 H19 0.9500 . ? C27 H20 0.9900 . ? C27 H21 0.9900 . ? C101 H12 0.9500 . ? C102 C103 1.352(4) . ? C102 H13 0.9500 . ? C103 H14 0.9500 . ? C201 H22 0.9500 . ? C202 C203 1.354(4) . ? C202 H23 0.9500 . ? C203 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N12 133.18(12) . 3_656 ? N1 Cu1 N22 112.70(11) . 3_756 ? N12 Cu1 N22 105.79(11) 3_656 3_756 ? N1 Cu1 N2 82.30(11) . . ? N12 Cu1 N2 107.16(11) 3_656 . ? N22 Cu1 N2 112.11(12) 3_756 . ? O2 Cl1 O3 107.0(2) . . ? O2 Cl1 O4 109.7(2) . . ? O3 Cl1 O4 108.5(2) . . ? O2 Cl1 O1 110.0(2) . . ? O3 Cl1 O1 110.92(19) . . ? O4 Cl1 O1 110.69(16) . . ? C10 N1 C1 116.4(3) . . ? C10 N1 Cu1 132.2(2) . . ? C1 N1 Cu1 110.4(2) . . ? C20 N2 C2 116.9(3) . . ? C20 N2 Cu1 111.8(3) . . ? C2 N2 Cu1 102.4(2) . . ? C101 N11 C103 106.6(3) . . ? C101 N11 C17 126.5(3) . . ? C103 N11 C17 126.9(3) . . ? C101 N12 C102 105.0(3) . . ? C101 N12 Cu1 129.2(2) . 3_656 ? C102 N12 Cu1 125.8(3) . 3_656 ? C201 N21 C203 106.7(3) . . ? C201 N21 C27 126.1(3) . . ? C203 N21 C27 127.1(3) . . ? C201 N22 C202 104.9(3) . . ? C201 N22 Cu1 124.1(3) . 3_756 ? C202 N22 Cu1 130.8(3) . 3_756 ? N1 C1 C2 111.5(3) . . ? N1 C1 H1 109.3 . . ? C2 C1 H1 109.3 . . ? N1 C1 H2 109.3 . . ? C2 C1 H2 109.3 . . ? H1 C1 H2 108.0 . . ? N2 C2 C1 111.1(3) . . ? N2 C2 H3 109.4 . . ? C1 C2 H3 109.4 . . ? N2 C2 H4 109.4 . . ? C1 C2 H4 109.4 . . ? H3 C2 H4 108.0 . . ? N1 C10 C11 125.8(3) . . ? N1 C10 H5 117.1 . . ? C11 C10 H5 117.1 . . ? C12 C11 C16 117.9(3) . . ? C12 C11 C10 124.1(3) . . ? C16 C11 C10 118.0(3) . . ? C13 C12 C11 121.6(3) . . ? C13 C12 H6 119.2 . . ? C11 C12 H6 119.2 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H7 119.9 . . ? C14 C13 H7 119.9 . . ? C15 C14 C13 118.3(3) . . ? C15 C14 C17 121.1(3) . . ? C13 C14 C17 120.4(3) . . ? C14 C15 C16 121.5(3) . . ? C14 C15 H8 119.2 . . ? C16 C15 H8 119.2 . . ? C11 C16 C15 120.3(3) . . ? C11 C16 H9 119.9 . . ? C15 C16 H9 119.9 . . ? N11 C17 C14 112.7(3) . . ? N11 C17 H10 109.1 . . ? C14 C17 H10 109.1 . . ? N11 C17 H11 109.1 . . ? C14 C17 H11 109.1 . . ? H10 C17 H11 107.8 . . ? N2 C20 C21 124.8(3) . . ? N2 C20 H15 117.6 . . ? C21 C20 H15 117.6 . . ? C26 C21 C22 119.5(3) . . ? C26 C21 C20 121.1(3) . . ? C22 C21 C20 119.4(3) . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H16 120.1 . . ? C21 C22 H16 120.1 . . ? C24 C23 C22 121.5(4) . . ? C24 C23 H17 119.2 . . ? C22 C23 H17 119.2 . . ? C23 C24 C25 118.6(3) . . ? C23 C24 C27 120.8(3) . . ? C25 C24 C27 120.6(3) . . ? C26 C25 C24 120.9(3) . . ? C26 C25 H18 119.5 . . ? C24 C25 H18 119.5 . . ? C25 C26 C21 119.6(3) . . ? C25 C26 H19 120.2 . . ? C21 C26 H19 120.2 . . ? N21 C27 C24 112.7(3) . . ? N21 C27 H20 109.1 . . ? C24 C27 H20 109.1 . . ? N21 C27 H21 109.1 . . ? C24 C27 H21 109.1 . . ? H20 C27 H21 107.8 . . ? N12 C101 N11 111.8(3) . . ? N12 C101 H12 124.1 . . ? N11 C101 H12 124.1 . . ? C103 C102 N12 109.6(3) . . ? C103 C102 H13 125.2 . . ? N12 C102 H13 125.2 . . ? N11 C103 C102 107.0(3) . . ? N11 C103 H14 126.5 . . ? C102 C103 H14 126.5 . . ? N22 C201 N21 112.0(3) . . ? N22 C201 H22 124.0 . . ? N21 C201 H22 124.0 . . ? C203 C202 N22 109.9(3) . . ? C203 C202 H23 125.0 . . ? N22 C202 H23 125.0 . . ? C202 C203 N21 106.5(3) . . ? C202 C203 H24 126.8 . . ? N21 C203 H24 126.8 . . ? 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 N12 Cu1 N1 C10 66.2(3) 3_656 . . . ? N22 Cu1 N1 C10 -76.6(3) 3_756 . . . ? N2 Cu1 N1 C10 172.6(3) . . . . ? N12 Cu1 N1 C1 -125.3(2) 3_656 . . . ? N22 Cu1 N1 C1 91.9(2) 3_756 . . . ? N2 Cu1 N1 C1 -18.9(2) . . . . ? N1 Cu1 N2 C20 -134.1(3) . . . . ? N12 Cu1 N2 C20 -1.2(3) 3_656 . . . ? N22 Cu1 N2 C20 114.4(3) 3_756 . . . ? N1 Cu1 N2 C2 -8.2(2) . . . . ? N12 Cu1 N2 C2 124.7(3) 3_656 . . . ? N22 Cu1 N2 C2 -119.6(2) 3_756 . . . ? C10 N1 C1 C2 -144.5(3) . . . . ? Cu1 N1 C1 C2 45.0(4) . . . . ? C20 N2 C2 C1 156.0(4) . . . . ? Cu1 N2 C2 C1 33.5(4) . . . . ? N1 C1 C2 N2 -54.2(5) . . . . ? C1 N1 C10 C11 -172.7(3) . . . . ? Cu1 N1 C10 C11 -4.8(5) . . . . ? N1 C10 C11 C12 -17.4(6) . . . . ? N1 C10 C11 C16 162.0(3) . . . . ? C16 C11 C12 C13 -2.8(6) . . . . ? C10 C11 C12 C13 176.6(3) . . . . ? C11 C12 C13 C14 0.7(6) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C12 C13 C14 C17 -176.1(3) . . . . ? C13 C14 C15 C16 0.9(5) . . . . ? C17 C14 C15 C16 177.2(3) . . . . ? C12 C11 C16 C15 3.9(6) . . . . ? C10 C11 C16 C15 -175.6(3) . . . . ? C14 C15 C16 C11 -3.0(6) . . . . ? C101 N11 C17 C14 100.4(4) . . . . ? C103 N11 C17 C14 -76.2(4) . . . . ? C15 C14 C17 N11 115.3(3) . . . . ? C13 C14 C17 N11 -68.4(4) . . . . ? C2 N2 C20 C21 178.1(3) . . . . ? Cu1 N2 C20 C21 -64.4(4) . . . . ? N2 C20 C21 C26 -19.9(6) . . . . ? N2 C20 C21 C22 160.2(4) . . . . ? C26 C21 C22 C23 1.8(5) . . . . ? C20 C21 C22 C23 -178.2(3) . . . . ? C21 C22 C23 C24 -1.9(5) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C22 C23 C24 C27 -178.6(3) . . . . ? C23 C24 C25 C26 1.3(5) . . . . ? C27 C24 C25 C26 -179.8(3) . . . . ? C24 C25 C26 C21 -1.3(5) . . . . ? C22 C21 C26 C25 -0.3(5) . . . . ? C20 C21 C26 C25 179.8(3) . . . . ? C201 N21 C27 C24 -94.8(4) . . . . ? C203 N21 C27 C24 82.0(4) . . . . ? C23 C24 C27 N21 -125.9(3) . . . . ? C25 C24 C27 N21 55.2(5) . . . . ? C102 N12 C101 N11 0.1(4) . . . . ? Cu1 N12 C101 N11 179.80(18) 3_656 . . . ? C103 N11 C101 N12 0.6(4) . . . . ? C17 N11 C101 N12 -176.6(3) . . . . ? C101 N12 C102 C103 -0.7(4) . . . . ? Cu1 N12 C102 C103 179.5(2) 3_656 . . . ? C101 N11 C103 C102 -1.0(4) . . . . ? C17 N11 C103 C102 176.2(3) . . . . ? N12 C102 C103 N11 1.1(4) . . . . ? C202 N22 C201 N21 -0.2(4) . . . . ? Cu1 N22 C201 N21 175.1(2) 3_756 . . . ? C203 N21 C201 N22 0.8(4) . . . . ? C27 N21 C201 N22 178.2(3) . . . . ? C201 N22 C202 C203 -0.5(4) . . . . ? Cu1 N22 C202 C203 -175.4(2) 3_756 . . . ? N22 C202 C203 N21 1.0(4) . . . . ? C201 N21 C203 C202 -1.1(4) . . . . ? C27 N21 C203 C202 -178.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.409 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.061 #====END data_[Cu(L2)]BF4_(5) _database_code_CSD 201031 _audit_creation_date 'Wed Sep 11 21:35:19 2002' _audit_creation_method SHELXL-97 _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu(L2)]BF4 _chemical_formula_sum 'C24 H24 B Cu F4 N6' _chemical_formula_weight 546.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.70(2) _cell_length_b 9.979(16) _cell_length_c 19.23(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.56(15) _cell_angle_gamma 90.00 _cell_volume 2478(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 11796 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.040 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2185 _diffrn_reflns_av_R_equivalents 0.1550 _diffrn_reflns_av_sigmaI/netI 0.1886 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5647 _reflns_number_gt 2255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^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 5647 _refine_ls_number_parameters 323 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1754 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.73533(4) 0.18560(5) 0.01287(3) 0.04262(19) Uani 1 1 d . . . F1 F 0.7344(2) 0.8104(3) -0.17979(16) 0.0915(11) Uani 1 1 d . . . F2 F 0.8777(4) 0.6992(5) -0.1085(3) 0.0525(19) Uiso 0.617(13) 1 d PU . . F2B F 0.8970(7) 0.7396(10) -0.1362(6) 0.070(3) Uiso 0.383(13) 1 d PU . . F3 F 0.8481(8) 0.7205(7) -0.2289(4) 0.104(3) Uiso 0.617(13) 1 d PU . . F3B F 0.8013(9) 0.6971(9) -0.2516(5) 0.068(3) Uiso 0.383(13) 1 d PU . . F4 F 0.7538(5) 0.5824(7) -0.1904(4) 0.087(3) Uiso 0.617(13) 1 d PU . . F4B F 0.7508(10) 0.5978(13) -0.1630(8) 0.103(5) Uiso 0.383(13) 1 d PU . . N1 N 0.8026(3) 0.0278(3) -0.01482(18) 0.0351(9) Uani 1 1 d . . . N2 N 0.6886(3) 0.0273(3) 0.0842(2) 0.0561(12) Uani 1 1 d . . . N11 N 0.8947(3) 0.4922(3) 0.15197(18) 0.0378(9) Uani 1 1 d . . . N12 N 0.7910(3) 0.3450(3) 0.07655(18) 0.0356(9) Uani 1 1 d . . . N21 N 0.5277(3) 0.3733(3) -0.16850(18) 0.0387(9) Uani 1 1 d . . . N22 N 0.6145(3) 0.2528(3) -0.07090(18) 0.0425(9) Uani 1 1 d . . . C1 C 0.7579(4) -0.0975(4) 0.0026(3) 0.0549(14) Uani 1 1 d . . . H1 H 0.8026 -0.1740 0.0002 0.066 Uiso 1 1 calc R . . H2 H 0.6887 -0.1123 -0.0348 0.066 Uiso 1 1 calc R . . C2 C 0.7480(4) -0.0919(5) 0.0772(3) 0.0678(16) Uani 1 1 d . . . H3 H 0.7126 -0.1737 0.0856 0.081 Uiso 1 1 calc R . . H4 H 0.8178 -0.0889 0.1151 0.081 Uiso 1 1 calc R . . C10 C 0.8618(4) 0.0155(4) -0.0536(2) 0.0402(11) Uani 1 1 d . . . H5 H 0.8790 -0.0729 -0.0636 0.048 Uiso 1 1 calc R . . C11 C 1.0946(3) 0.8740(4) 0.0839(2) 0.0350(11) Uani 1 1 d . . . C12 C 1.0949(3) 0.7404(4) 0.0626(2) 0.0451(12) Uani 1 1 d . . . H6 H 1.1210 0.7179 0.0242 0.054 Uiso 1 1 calc R . . C13 C 1.0579(4) 0.6413(4) 0.0965(3) 0.0475(13) Uani 1 1 d . . . H7 H 1.0569 0.5514 0.0802 0.057 Uiso 1 1 calc R . . C14 C 1.0218(3) 0.6697(4) 0.1543(2) 0.0394(11) Uani 1 1 d . . . C15 C 1.0213(4) 0.8001(4) 0.1759(2) 0.0486(12) Uani 1 1 d . . . H8 H 0.9971 0.8215 0.2154 0.058 Uiso 1 1 calc R . . C16 C 1.0565(4) 0.9028(4) 0.1403(3) 0.0500(13) Uani 1 1 d . . . H9 H 1.0540 0.9932 0.1551 0.060 Uiso 1 1 calc R . . C17 C 0.9906(3) 0.5594(4) 0.1960(2) 0.0460(12) Uani 1 1 d . . . H10 H 1.0470 0.4924 0.2120 0.055 Uiso 1 1 calc R . . H11 H 0.9812 0.5975 0.2409 0.055 Uiso 1 1 calc R . . C20 C 0.7020(3) 0.0681(4) 0.1482(3) 0.0475(13) Uani 1 1 d . . . H12 H 0.7506 0.0214 0.1878 0.057 Uiso 1 1 calc R . . C21 C 0.3519(3) 0.8171(4) -0.1667(2) 0.0393(10) Uani 1 1 d . . . C22 C 0.4455(3) 0.7726(4) -0.1186(2) 0.0405(12) Uani 1 1 d . . . H13 H 0.4760 0.8165 -0.0726 0.049 Uiso 1 1 calc R . . C23 C 0.4951(4) 0.6648(4) -0.1370(2) 0.0483(13) Uani 1 1 d . . . H14 H 0.5598 0.6355 -0.1036 0.058 Uiso 1 1 calc R . . C24 C 0.4510(3) 0.5985(4) -0.2040(2) 0.0378(11) Uani 1 1 d . . . C25 C 0.3581(4) 0.6430(4) -0.2523(2) 0.0464(12) Uani 1 1 d . . . H15 H 0.3272 0.5988 -0.2982 0.056 Uiso 1 1 calc R . . C26 C 0.3096(4) 0.7523(4) -0.2337(3) 0.0489(13) Uani 1 1 d . . . H16 H 0.2460 0.7834 -0.2677 0.059 Uiso 1 1 calc R . . C27 C 0.5056(4) 0.4803(4) -0.2238(2) 0.0496(13) Uani 1 1 d . . . H17 H 0.4618 0.4440 -0.2720 0.060 Uiso 1 1 calc R . . H18 H 0.5714 0.5112 -0.2289 0.060 Uiso 1 1 calc R . . C101 C 0.8874(4) 0.3744(4) 0.1159(2) 0.0391(11) Uani 1 1 d . . . H19 H 0.9451 0.3192 0.1187 0.047 Uiso 1 1 calc R . . C102 C 0.7345(4) 0.4503(4) 0.0891(3) 0.0470(12) Uani 1 1 d . . . H20 H 0.6614 0.4587 0.0683 0.056 Uiso 1 1 calc R . . C103 C 0.7971(4) 0.5401(4) 0.1350(2) 0.0458(12) Uani 1 1 d . . . H21 H 0.7768 0.6211 0.1521 0.055 Uiso 1 1 calc R . . C201 C 0.6188(4) 0.3565(4) -0.1133(2) 0.0412(12) Uani 1 1 d . . . H22 H 0.6780 0.4115 -0.1057 0.049 Uiso 1 1 calc R . . C202 C 0.5151(4) 0.2042(4) -0.1012(2) 0.0479(12) Uani 1 1 d . . . H23 H 0.4881 0.1296 -0.0828 0.057 Uiso 1 1 calc R . . C203 C 0.4617(4) 0.2778(4) -0.1606(3) 0.0494(13) Uani 1 1 d . . . H24 H 0.3916 0.2652 -0.1909 0.059 Uiso 1 1 calc R . . B10 B 0.7989(5) 0.7065(5) -0.1779(3) 0.0477(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0495(4) 0.0319(3) 0.0442(3) 0.0022(3) 0.0126(3) 0.0043(3) F1 0.067(2) 0.093(2) 0.089(2) -0.0242(19) -0.0073(18) 0.0358(19) N1 0.039(2) 0.0302(19) 0.040(2) 0.0015(16) 0.018(2) -0.0045(16) N2 0.076(3) 0.044(2) 0.065(3) 0.015(2) 0.046(3) 0.025(2) N11 0.042(2) 0.035(2) 0.042(2) 0.0006(18) 0.022(2) -0.0030(18) N12 0.040(2) 0.032(2) 0.040(2) 0.0047(16) 0.0186(19) 0.0019(17) N21 0.042(2) 0.041(2) 0.034(2) 0.0028(17) 0.014(2) 0.0084(19) N22 0.043(3) 0.039(2) 0.041(2) 0.0042(18) 0.007(2) -0.0022(18) C1 0.078(4) 0.026(2) 0.075(4) 0.002(2) 0.045(3) 0.004(2) C2 0.093(5) 0.043(3) 0.091(4) 0.020(3) 0.061(4) 0.024(3) C10 0.047(3) 0.036(2) 0.039(3) -0.001(2) 0.015(2) -0.001(2) C11 0.031(3) 0.036(2) 0.039(3) -0.001(2) 0.014(2) -0.0011(19) C12 0.063(3) 0.036(3) 0.049(3) -0.012(2) 0.035(3) -0.012(2) C13 0.061(3) 0.036(3) 0.056(3) -0.016(2) 0.033(3) -0.016(2) C14 0.045(3) 0.041(3) 0.033(2) -0.004(2) 0.013(2) -0.008(2) C15 0.066(3) 0.046(3) 0.045(3) -0.006(2) 0.033(3) 0.000(3) C16 0.064(4) 0.031(2) 0.062(3) -0.008(2) 0.031(3) -0.005(2) C17 0.050(3) 0.047(3) 0.039(3) -0.004(2) 0.012(2) -0.018(2) C20 0.042(3) 0.037(3) 0.066(4) 0.019(3) 0.022(3) 0.013(2) C21 0.039(3) 0.037(2) 0.046(3) 0.015(2) 0.020(2) 0.008(2) C22 0.035(3) 0.049(3) 0.035(3) -0.001(2) 0.009(2) 0.002(2) C23 0.043(3) 0.052(3) 0.045(3) 0.002(2) 0.008(2) 0.013(2) C24 0.036(3) 0.042(3) 0.037(3) 0.010(2) 0.015(2) 0.010(2) C25 0.050(3) 0.049(3) 0.037(3) 0.006(2) 0.010(2) 0.011(2) C26 0.039(3) 0.056(3) 0.046(3) 0.013(3) 0.006(2) 0.012(2) C27 0.060(4) 0.049(3) 0.041(3) 0.009(2) 0.018(3) 0.014(2) C101 0.036(3) 0.041(3) 0.044(3) 0.002(2) 0.018(2) 0.005(2) C102 0.034(3) 0.037(3) 0.075(4) -0.004(2) 0.024(3) 0.000(2) C103 0.053(3) 0.028(2) 0.067(3) 0.001(2) 0.034(3) 0.002(2) C201 0.041(3) 0.032(2) 0.043(3) -0.001(2) 0.005(2) -0.001(2) C202 0.051(3) 0.040(3) 0.053(3) 0.000(3) 0.018(3) -0.005(2) C203 0.039(3) 0.052(3) 0.053(3) -0.002(3) 0.009(3) -0.002(2) B10 0.049(4) 0.040(3) 0.056(4) -0.011(3) 0.021(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.986(4) . ? Cu1 N12 1.996(4) . ? Cu1 N22 2.000(5) . ? Cu1 N2 2.318(5) . ? F1 B10 1.355(6) . ? F2 F2B 0.782(10) . ? F2 B10 1.409(8) . ? F2B B10 1.355(10) . ? F2B F3 1.692(11) . ? F3 F3B 0.685(10) . ? F3 B10 1.371(8) . ? F3B B10 1.432(11) . ? F4 F4B 0.563(15) . ? F4 B10 1.370(8) . ? F4B B10 1.349(13) . ? N1 C10 1.278(5) . ? N1 C1 1.479(5) . ? N2 C20 1.250(6) . ? N2 C2 1.474(6) . ? N11 C101 1.351(5) . ? N11 C103 1.353(6) . ? N11 C17 1.466(5) . ? N12 C101 1.318(6) . ? N12 C102 1.374(5) . ? N21 C201 1.351(6) . ? N21 C203 1.357(6) . ? N21 C27 1.465(5) . ? N22 C201 1.331(5) . ? N22 C202 1.378(6) . ? C1 C2 1.487(7) . ? C1 H1 0.9900 . ? C1 H2 0.9900 . ? C2 H3 0.9900 . ? C2 H4 0.9900 . ? C10 C11 1.466(6) 3_765 ? C10 H5 0.9500 . ? C11 C16 1.381(6) . ? C11 C12 1.395(6) . ? C11 C10 1.466(6) 3_765 ? C12 C13 1.372(6) . ? C12 H6 0.9500 . ? C13 C14 1.387(6) . ? C13 H7 0.9500 . ? C14 C15 1.368(6) . ? C14 C17 1.507(6) . ? C15 C16 1.404(6) . ? C15 H8 0.9500 . ? C16 H9 0.9500 . ? C17 H10 0.9900 . ? C17 H11 0.9900 . ? C20 C21 1.469(6) 3_665 ? C20 H12 0.9500 . ? C21 C22 1.380(6) . ? C21 C26 1.385(6) . ? C21 C20 1.469(6) 3_665 ? C22 C23 1.380(6) . ? C22 H13 0.9500 . ? C23 C24 1.394(6) . ? C23 H14 0.9500 . ? C24 C25 1.375(6) . ? C24 C27 1.511(6) . ? C25 C26 1.384(6) . ? C25 H15 0.9500 . ? C26 H16 0.9500 . ? C27 H17 0.9900 . ? C27 H18 0.9900 . ? C101 H19 0.9500 . ? C102 C103 1.345(6) . ? C102 H20 0.9500 . ? C103 H21 0.9500 . ? C201 H22 0.9500 . ? C202 C203 1.349(6) . ? C202 H23 0.9500 . ? C203 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N12 132.85(17) . . ? N1 Cu1 N22 112.55(17) . . ? N12 Cu1 N22 105.67(18) . . ? N1 Cu1 N2 82.16(18) . . ? N12 Cu1 N2 107.7(2) . . ? N22 Cu1 N2 112.75(18) . . ? F2B F2 B10 69.8(8) . . ? F2 F2B B10 77.3(10) . . ? F2 F2B F3 123.7(11) . . ? B10 F2B F3 52.1(4) . . ? F3B F3 B10 80.8(12) . . ? F3B F3 F2B 131.7(14) . . ? B10 F3 F2B 51.2(5) . . ? F3 F3B B10 71.0(11) . . ? F4B F4 B10 76.0(18) . . ? F4 F4B B10 80.1(19) . . ? C10 N1 C1 116.3(3) . . ? C10 N1 Cu1 132.4(3) . . ? C1 N1 Cu1 110.2(3) . . ? C20 N2 C2 116.7(4) . . ? C20 N2 Cu1 112.5(3) . . ? C2 N2 Cu1 103.0(3) . . ? C101 N11 C103 106.6(4) . . ? C101 N11 C17 126.3(4) . . ? C103 N11 C17 126.9(4) . . ? C101 N12 C102 104.1(4) . . ? C101 N12 Cu1 129.3(3) . . ? C102 N12 Cu1 126.6(3) . . ? C201 N21 C203 107.5(4) . . ? C201 N21 C27 124.9(4) . . ? C203 N21 C27 127.6(4) . . ? C201 N22 C202 104.8(4) . . ? C201 N22 Cu1 124.1(3) . . ? C202 N22 Cu1 131.1(3) . . ? N1 C1 C2 111.4(4) . . ? N1 C1 H1 109.3 . . ? C2 C1 H1 109.3 . . ? N1 C1 H2 109.3 . . ? C2 C1 H2 109.3 . . ? H1 C1 H2 108.0 . . ? N2 C2 C1 110.5(4) . . ? N2 C2 H3 109.6 . . ? C1 C2 H3 109.6 . . ? N2 C2 H4 109.6 . . ? C1 C2 H4 109.6 . . ? H3 C2 H4 108.1 . . ? N1 C10 C11 125.7(4) . 3_765 ? N1 C10 H5 117.1 . . ? C11 C10 H5 117.1 3_765 . ? C16 C11 C12 117.9(4) . . ? C16 C11 C10 117.9(4) . 3_765 ? C12 C11 C10 124.0(4) . 3_765 ? C13 C12 C11 120.7(4) . . ? C13 C12 H6 119.6 . . ? C11 C12 H6 119.6 . . ? C12 C13 C14 121.4(4) . . ? C12 C13 H7 119.3 . . ? C14 C13 H7 119.3 . . ? C15 C14 C13 118.5(4) . . ? C15 C14 C17 120.1(4) . . ? C13 C14 C17 121.2(4) . . ? C14 C15 C16 120.5(4) . . ? C14 C15 H8 119.7 . . ? C16 C15 H8 119.7 . . ? C11 C16 C15 120.9(4) . . ? C11 C16 H9 119.6 . . ? C15 C16 H9 119.6 . . ? N11 C17 C14 112.7(4) . . ? N11 C17 H10 109.1 . . ? C14 C17 H10 109.1 . . ? N11 C17 H11 109.1 . . ? C14 C17 H11 109.1 . . ? H10 C17 H11 107.8 . . ? N2 C20 C21 124.9(4) . 3_665 ? N2 C20 H12 117.6 . . ? C21 C20 H12 117.6 3_665 . ? C22 C21 C26 118.6(4) . . ? C22 C21 C20 121.2(4) . 3_665 ? C26 C21 C20 120.2(4) . 3_665 ? C23 C22 C21 120.5(4) . . ? C23 C22 H13 119.8 . . ? C21 C22 H13 119.8 . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H14 119.7 . . ? C24 C23 H14 119.7 . . ? C25 C24 C23 119.2(4) . . ? C25 C24 C27 120.5(4) . . ? C23 C24 C27 120.4(4) . . ? C24 C25 C26 119.8(4) . . ? C24 C25 H15 120.1 . . ? C26 C25 H15 120.1 . . ? C25 C26 C21 121.4(4) . . ? C25 C26 H16 119.3 . . ? C21 C26 H16 119.3 . . ? N21 C27 C24 112.7(4) . . ? N21 C27 H17 109.1 . . ? C24 C27 H17 109.1 . . ? N21 C27 H18 109.1 . . ? C24 C27 H18 109.1 . . ? H17 C27 H18 107.8 . . ? N12 C101 N11 112.1(4) . . ? N12 C101 H19 124.0 . . ? N11 C101 H19 124.0 . . ? C103 C102 N12 110.6(4) . . ? C103 C102 H20 124.7 . . ? N12 C102 H20 124.7 . . ? C102 C103 N11 106.6(4) . . ? C102 C103 H21 126.7 . . ? N11 C103 H21 126.7 . . ? N22 C201 N21 111.1(4) . . ? N22 C201 H22 124.5 . . ? N21 C201 H22 124.5 . . ? C203 C202 N22 110.2(4) . . ? C203 C202 H23 124.9 . . ? N22 C202 H23 124.9 . . ? C202 C203 N21 106.5(4) . . ? C202 C203 H24 126.8 . . ? N21 C203 H24 126.8 . . ? F4B B10 F1 105.1(7) . . ? F4B B10 F2B 122.0(8) . . ? F1 B10 F2B 109.8(5) . . ? F4B B10 F4 23.9(6) . . ? F1 B10 F4 115.8(6) . . ? F2B B10 F4 128.7(7) . . ? F4B B10 F3 128.8(8) . . ? F1 B10 F3 112.0(5) . . ? F2B B10 F3 76.7(6) . . ? F4 B10 F3 105.5(5) . . ? F4B B10 F2 91.8(7) . . ? F1 B10 F2 110.6(4) . . ? F2B B10 F2 32.8(5) . . ? F4 B10 F2 106.1(5) . . ? F3 B10 F2 106.2(6) . . ? F4B B10 F3B 109.4(8) . . ? F1 B10 F3B 104.7(6) . . ? F2B B10 F3B 104.7(7) . . ? F4 B10 F3B 85.7(5) . . ? F3 B10 F3B 28.2(4) . . ? F2 B10 F3B 132.1(7) . . ? 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 B10 F2 F2B F3 -25.0(8) . . . . ? F2 F2B F3 F3B 23(2) . . . . ? B10 F2B F3 F3B -8.1(16) . . . . ? F2 F2B F3 B10 31.5(11) . . . . ? F2B F3 F3B B10 6.4(12) . . . . ? N12 Cu1 N1 C10 -67.0(5) . . . . ? N22 Cu1 N1 C10 74.6(4) . . . . ? N2 Cu1 N1 C10 -173.9(4) . . . . ? N12 Cu1 N1 C1 125.8(3) . . . . ? N22 Cu1 N1 C1 -92.6(3) . . . . ? N2 Cu1 N1 C1 18.8(3) . . . . ? N1 Cu1 N2 C20 134.9(4) . . . . ? N12 Cu1 N2 C20 2.3(4) . . . . ? N22 Cu1 N2 C20 -113.9(4) . . . . ? N1 Cu1 N2 C2 8.4(3) . . . . ? N12 Cu1 N2 C2 -124.2(3) . . . . ? N22 Cu1 N2 C2 119.6(3) . . . . ? N1 Cu1 N12 C101 -2.6(4) . . . . ? N22 Cu1 N12 C101 -146.0(4) . . . . ? N2 Cu1 N12 C101 93.2(4) . . . . ? N1 Cu1 N12 C102 177.8(3) . . . . ? N22 Cu1 N12 C102 34.3(4) . . . . ? N2 Cu1 N12 C102 -86.4(4) . . . . ? N1 Cu1 N22 C201 -98.9(4) . . . . ? N12 Cu1 N22 C201 52.9(4) . . . . ? N2 Cu1 N22 C201 170.3(3) . . . . ? N1 Cu1 N22 C202 76.5(4) . . . . ? N12 Cu1 N22 C202 -131.7(4) . . . . ? N2 Cu1 N22 C202 -14.3(4) . . . . ? C10 N1 C1 C2 145.2(4) . . . . ? Cu1 N1 C1 C2 -45.3(5) . . . . ? C20 N2 C2 C1 -157.7(5) . . . . ? Cu1 N2 C2 C1 -34.0(5) . . . . ? N1 C1 C2 N2 54.5(6) . . . . ? C1 N1 C10 C11 173.0(4) . . . 3_765 ? Cu1 N1 C10 C11 6.4(7) . . . 3_765 ? C16 C11 C12 C13 0.3(7) . . . . ? C10 C11 C12 C13 176.2(4) 3_765 . . . ? C11 C12 C13 C14 -1.9(7) . . . . ? C12 C13 C14 C15 1.6(7) . . . . ? C12 C13 C14 C17 -174.2(4) . . . . ? C13 C14 C15 C16 0.1(7) . . . . ? C17 C14 C15 C16 176.0(4) . . . . ? C12 C11 C16 C15 1.4(7) . . . . ? C10 C11 C16 C15 -174.8(4) 3_765 . . . ? C14 C15 C16 C11 -1.6(7) . . . . ? C101 N11 C17 C14 99.2(5) . . . . ? C103 N11 C17 C14 -75.6(5) . . . . ? C15 C14 C17 N11 113.9(5) . . . . ? C13 C14 C17 N11 -70.3(6) . . . . ? C2 N2 C20 C21 -178.4(4) . . . 3_665 ? Cu1 N2 C20 C21 62.9(6) . . . 3_665 ? C26 C21 C22 C23 -0.6(6) . . . . ? C20 C21 C22 C23 -179.9(4) 3_665 . . . ? C21 C22 C23 C24 -0.6(7) . . . . ? C22 C23 C24 C25 0.9(7) . . . . ? C22 C23 C24 C27 -179.9(4) . . . . ? C23 C24 C25 C26 -0.1(7) . . . . ? C27 C24 C25 C26 -179.3(4) . . . . ? C24 C25 C26 C21 -1.1(7) . . . . ? C22 C21 C26 C25 1.5(7) . . . . ? C20 C21 C26 C25 -179.3(4) 3_665 . . . ? C201 N21 C27 C24 -96.3(5) . . . . ? C203 N21 C27 C24 80.5(6) . . . . ? C25 C24 C27 N21 -124.4(5) . . . . ? C23 C24 C27 N21 56.4(6) . . . . ? C102 N12 C101 N11 -0.4(5) . . . . ? Cu1 N12 C101 N11 179.9(2) . . . . ? C103 N11 C101 N12 0.5(5) . . . . ? C17 N11 C101 N12 -175.2(3) . . . . ? C101 N12 C102 C103 0.1(5) . . . . ? Cu1 N12 C102 C103 179.9(3) . . . . ? N12 C102 C103 N11 0.2(5) . . . . ? C101 N11 C103 C102 -0.4(5) . . . . ? C17 N11 C103 C102 175.2(4) . . . . ? C202 N22 C201 N21 -0.7(5) . . . . ? Cu1 N22 C201 N21 175.7(3) . . . . ? C203 N21 C201 N22 1.0(5) . . . . ? C27 N21 C201 N22 178.4(4) . . . . ? C201 N22 C202 C203 0.2(5) . . . . ? Cu1 N22 C202 C203 -175.9(3) . . . . ? N22 C202 C203 N21 0.4(5) . . . . ? C201 N21 C203 C202 -0.9(5) . . . . ? C27 N21 C203 C202 -178.1(4) . . . . ? F4 F4B B10 F1 120.3(17) . . . . ? F4 F4B B10 F2B -114.1(17) . . . . ? F4 F4B B10 F3 -15(2) . . . . ? F4 F4B B10 F2 -127.8(17) . . . . ? F4 F4B B10 F3B 8(2) . . . . ? F2 F2B B10 F4B -25.9(12) . . . . ? F3 F2B B10 F4B 127.6(10) . . . . ? F2 F2B B10 F1 97.5(8) . . . . ? F3 F2B B10 F1 -108.9(6) . . . . ? F2 F2B B10 F4 -54.2(11) . . . . ? F3 F2B B10 F4 99.4(8) . . . . ? F2 F2B B10 F3 -153.6(9) . . . . ? F3 F2B B10 F2 153.6(9) . . . . ? F2 F2B B10 F3B -150.6(8) . . . . ? F3 F2B B10 F3B 3.0(6) . . . . ? F4B F4 B10 F1 -67.8(18) . . . . ? F4B F4 B10 F2B 82.5(19) . . . . ? F4B F4 B10 F3 167.7(18) . . . . ? F4B F4 B10 F2 55.3(18) . . . . ? F4B F4 B10 F3B -172.1(19) . . . . ? F3B F3 B10 F4B 53.3(14) . . . . ? F2B F3 B10 F4B -120.6(11) . . . . ? F3B F3 B10 F1 -79.9(12) . . . . ? F2B F3 B10 F1 106.2(6) . . . . ? F3B F3 B10 F2B 173.9(12) . . . . ? F3B F3 B10 F4 46.9(12) . . . . ? F2B F3 B10 F4 -126.9(7) . . . . ? F3B F3 B10 F2 159.3(10) . . . . ? F2B F3 B10 F2 -14.5(5) . . . . ? F2B F3 B10 F3B -173.9(12) . . . . ? F2B F2 B10 F4B 158.2(10) . . . . ? F2B F2 B10 F1 -94.9(9) . . . . ? F2B F2 B10 F4 138.8(9) . . . . ? F2B F2 B10 F3 26.8(9) . . . . ? F2B F2 B10 F3B 39.8(10) . . . . ? F3 F3B B10 F4B -138.5(12) . . . . ? F3 F3B B10 F1 109.4(11) . . . . ? F3 F3B B10 F2B -6.2(12) . . . . ? F3 F3B B10 F4 -135.1(11) . . . . ? F3 F3B B10 F2 -27.2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.619 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.069 #====END