# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_paper _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- Dalton.cif' _publ_contact_author ; Prof St\'ephane Baudron Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; _publ_contact_author_email hosseini@unistra.fr _publ_contact_author_fax '33 3 68 85 13 23' _publ_contact_author_phone '33 3 68 85 13 25' _publ_requested_category FM loop_ _publ_author_name _publ_author_address A.Beziau ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; S.A.Baudron ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; M.W.Hosseini ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; _publ_section_title ; Heterometallic coordination polymers incorporating dipyrrin based heteroleptic copper and cobalt complexes: to Ag-pi or not? ; _publ_contact_author_name 'Prof Stephane Baudron' ###Material relevant to compound 1 at 173K ######## data_compound1 _database_code_depnum_ccdc_archive 'CCDC 868785' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H19 Cu N5 O2, C2 H3 N ' _chemical_formula_sum 'C29 H22 Cu N6 O2' _chemical_formula_weight 550.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.8320(7) _cell_length_b 13.9122(8) _cell_length_c 14.6677(9) _cell_angle_alpha 90.00 _cell_angle_beta 117.7200(10) _cell_angle_gamma 90.00 _cell_volume 2498.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5617 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 27.28 _exptl_crystal_description plate _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9141 _exptl_absorpt_correction_T_max 0.9388 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17670 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5515 _reflns_number_gt 4597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.8882P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5515 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 C1 C 0.00061(19) 0.69601(18) -0.11995(18) 0.0281(5) Uani 1 1 d . . . H1 H 0.0510 0.7179 -0.1405 0.034 Uiso 1 1 calc R . . C2 C -0.0595(2) 0.61019(19) -0.1555(2) 0.0374(6) Uani 1 1 d . . . H2 H -0.0571 0.5674 -0.2032 0.045 Uiso 1 1 calc R . . C3 C -0.1218(2) 0.60230(18) -0.1063(2) 0.0338(6) Uani 1 1 d . . . H3 H -0.1695 0.5524 -0.1133 0.041 Uiso 1 1 calc R . . C4 C -0.10005(18) 0.68494(16) -0.04198(17) 0.0229(5) Uani 1 1 d . . . C5 C -0.14701(17) 0.70876(15) 0.02058(17) 0.0213(5) Uani 1 1 d . . . C6 C -0.13014(17) 0.79416(15) 0.07703(16) 0.0195(4) Uani 1 1 d . . . C7 C -0.17813(19) 0.82131(16) 0.13921(18) 0.0246(5) Uani 1 1 d . . . H7 H -0.2298 0.7865 0.1493 0.030 Uiso 1 1 calc R . . C8 C -0.13454(18) 0.90876(16) 0.18232(18) 0.0243(5) Uani 1 1 d . . . H8 H -0.1508 0.9448 0.2268 0.029 Uiso 1 1 calc R . . C9 C -0.06000(17) 0.93279(15) 0.14530(16) 0.0203(4) Uani 1 1 d . . . H9 H -0.0184 0.9887 0.1629 0.024 Uiso 1 1 calc R . . C10 C -0.21885(18) 0.63398(15) 0.03167(18) 0.0233(5) Uani 1 1 d . . . C11 C -0.3302(2) 0.63082(19) -0.0288(2) 0.0397(7) Uani 1 1 d . . . H11 H -0.3657 0.6785 -0.0775 0.048 Uiso 1 1 calc R . . C12 C -0.3889(2) 0.5557(2) -0.0164(2) 0.0447(7) Uani 1 1 d . . . H12 H -0.4639 0.5541 -0.0593 0.054 Uiso 1 1 calc R . . C13 C -0.2391(2) 0.4916(2) 0.1119(3) 0.0501(8) Uani 1 1 d . . . H13 H -0.2062 0.4446 0.1620 0.060 Uiso 1 1 calc R . . C14 C -0.1737(2) 0.5631(2) 0.1044(2) 0.0458(8) Uani 1 1 d . . . H14 H -0.0990 0.5630 0.1486 0.055 Uiso 1 1 calc R . . C15 C 0.23854(17) 0.89921(15) -0.00107(16) 0.0186(4) Uani 1 1 d . . . C16 C 0.30885(17) 0.87271(15) -0.04984(16) 0.0199(4) Uani 1 1 d . . . C17 C 0.32032(19) 0.77654(16) -0.06961(17) 0.0243(5) Uani 1 1 d . . . H17 H 0.2819 0.7288 -0.0557 0.029 Uiso 1 1 calc R . . C18 C 0.3896(2) 0.75316(17) -0.11009(19) 0.0300(5) Uani 1 1 d . . . H18 H 0.3977 0.6885 -0.1211 0.036 Uiso 1 1 calc R . . C19 C 0.43059(19) 0.90969(17) -0.11845(18) 0.0279(5) Uani 1 1 d . . . H19 H 0.4664 0.9561 -0.1372 0.033 Uiso 1 1 calc R . . C20 C 0.36545(17) 0.94069(16) -0.07590(17) 0.0235(5) Uani 1 1 d . . . H20 H 0.3596 1.0058 -0.0649 0.028 Uiso 1 1 calc R . . C21 C 0.27139(17) 0.97526(15) 0.06894(17) 0.0214(5) Uani 1 1 d . . . H21 H 0.3369 1.0059 0.0840 0.026 Uiso 1 1 calc R . . C22 C 0.21208(16) 1.00816(14) 0.11769(15) 0.0175(4) Uani 1 1 d . . . C23 C 0.25542(16) 1.09286(14) 0.18940(15) 0.0177(4) Uani 1 1 d . . . C24 C 0.33544(19) 1.15324(15) 0.18976(17) 0.0229(5) Uani 1 1 d . . . H24 H 0.3634 1.1433 0.1439 0.027 Uiso 1 1 calc R . . C25 C 0.37294(19) 1.22832(16) 0.25932(17) 0.0252(5) Uani 1 1 d . . . H25 H 0.4260 1.2684 0.2579 0.030 Uiso 1 1 calc R . . C26 C 0.26076(19) 1.18872(17) 0.32687(18) 0.0281(5) Uani 1 1 d . . . H26 H 0.2346 1.2003 0.3739 0.034 Uiso 1 1 calc R . . C27 C 0.21741(19) 1.11231(17) 0.25983(18) 0.0260(5) Uani 1 1 d . . . H27 H 0.1632 1.0743 0.2619 0.031 Uiso 1 1 calc R . . N1 N -0.02321(15) 0.74198(13) -0.05349(14) 0.0212(4) Uani 1 1 d . . . N2 N -0.05641(14) 0.86547(12) 0.08197(13) 0.0181(4) Uani 1 1 d . . . N3 N -0.34586(18) 0.48630(15) 0.05186(19) 0.0398(6) Uani 1 1 d . . . N4 N 0.44570(17) 0.81756(15) -0.13455(17) 0.0321(5) Uani 1 1 d . . . N5 N 0.33820(15) 1.24705(13) 0.32815(14) 0.0220(4) Uani 1 1 d . . . O1 O 0.15364(13) 0.84799(10) -0.02665(12) 0.0235(3) Uani 1 1 d . . . O2 O 0.12343(12) 0.97227(10) 0.10804(11) 0.0207(3) Uani 1 1 d . . . Cu1 Cu 0.05459(2) 0.852311(17) 0.034751(19) 0.01701(10) Uani 1 1 d . . . C28 C 0.5538(4) 0.6617(2) 0.1804(3) 0.0704(11) Uani 1 1 d . . . H28A H 0.5473 0.6462 0.2411 0.106 Uiso 1 1 calc R . . H28B H 0.6174 0.6310 0.1836 0.106 Uiso 1 1 calc R . . H28C H 0.4901 0.6396 0.1206 0.106 Uiso 1 1 calc R . . C29 C 0.5637(2) 0.7652(2) 0.1741(2) 0.0383(6) Uani 1 1 d . . . N6 N 0.5710(2) 0.84553(19) 0.1709(2) 0.0540(7) 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 C1 0.0253(12) 0.0354(13) 0.0270(12) -0.0085(10) 0.0151(10) -0.0067(10) C2 0.0352(14) 0.0381(14) 0.0425(15) -0.0235(12) 0.0210(12) -0.0121(12) C3 0.0285(13) 0.0304(13) 0.0424(15) -0.0151(11) 0.0166(11) -0.0125(11) C4 0.0186(11) 0.0205(10) 0.0278(12) -0.0038(9) 0.0093(9) -0.0052(9) C5 0.0150(10) 0.0204(10) 0.0256(11) 0.0003(8) 0.0069(9) -0.0027(8) C6 0.0163(10) 0.0197(10) 0.0224(11) 0.0036(8) 0.0087(8) -0.0010(8) C7 0.0212(11) 0.0264(11) 0.0313(12) 0.0032(9) 0.0164(10) -0.0018(9) C8 0.0264(12) 0.0233(11) 0.0287(12) 0.0000(9) 0.0175(10) 0.0009(9) C9 0.0196(11) 0.0175(10) 0.0245(11) 0.0017(8) 0.0109(9) 0.0015(8) C10 0.0215(11) 0.0193(10) 0.0308(12) -0.0019(9) 0.0135(10) -0.0035(9) C11 0.0221(13) 0.0382(14) 0.0506(16) 0.0176(12) 0.0099(12) -0.0054(11) C12 0.0211(13) 0.0423(15) 0.0613(18) 0.0152(13) 0.0112(12) -0.0079(12) C13 0.0335(15) 0.0358(15) 0.068(2) 0.0248(14) 0.0128(14) -0.0028(12) C14 0.0230(13) 0.0405(15) 0.0605(19) 0.0182(13) 0.0082(13) -0.0059(12) C15 0.0171(10) 0.0189(10) 0.0216(10) 0.0019(8) 0.0105(8) -0.0002(8) C16 0.0176(11) 0.0212(10) 0.0199(10) -0.0027(8) 0.0079(9) -0.0009(8) C17 0.0271(12) 0.0217(11) 0.0267(12) -0.0019(9) 0.0147(10) -0.0025(9) C18 0.0344(14) 0.0253(12) 0.0367(14) -0.0060(10) 0.0219(12) 0.0020(10) C19 0.0250(12) 0.0319(12) 0.0325(13) -0.0025(10) 0.0182(10) -0.0058(10) C20 0.0207(11) 0.0233(10) 0.0275(12) -0.0024(9) 0.0120(9) -0.0021(9) C21 0.0181(11) 0.0223(10) 0.0256(11) -0.0032(9) 0.0117(9) -0.0041(9) C22 0.0162(10) 0.0157(9) 0.0192(10) 0.0026(8) 0.0071(8) -0.0003(8) C23 0.0158(10) 0.0175(9) 0.0185(10) 0.0001(8) 0.0068(8) -0.0001(8) C24 0.0243(12) 0.0250(11) 0.0223(11) -0.0032(8) 0.0134(9) -0.0054(9) C25 0.0245(12) 0.0267(11) 0.0253(12) -0.0018(9) 0.0123(10) -0.0092(9) C26 0.0291(13) 0.0313(12) 0.0308(13) -0.0084(10) 0.0198(11) -0.0060(10) C27 0.0231(12) 0.0265(11) 0.0327(13) -0.0066(10) 0.0165(10) -0.0076(9) N1 0.0189(9) 0.0229(9) 0.0228(9) -0.0024(7) 0.0105(8) -0.0035(7) N2 0.0159(9) 0.0156(8) 0.0217(9) 0.0030(7) 0.0079(7) 0.0010(7) N3 0.0315(12) 0.0281(11) 0.0594(15) 0.0083(10) 0.0208(11) -0.0061(9) N4 0.0310(11) 0.0355(11) 0.0391(12) -0.0058(9) 0.0241(10) -0.0006(9) N5 0.0218(9) 0.0219(9) 0.0215(9) -0.0016(7) 0.0094(8) -0.0017(7) O1 0.0245(8) 0.0213(8) 0.0302(8) -0.0051(6) 0.0174(7) -0.0074(6) O2 0.0212(8) 0.0189(7) 0.0265(8) -0.0038(6) 0.0149(6) -0.0055(6) Cu1 0.01704(15) 0.01580(14) 0.02074(15) -0.00156(9) 0.01093(11) -0.00325(9) C28 0.100(3) 0.0422(18) 0.061(2) -0.0057(15) 0.031(2) -0.0040(19) C29 0.0398(16) 0.0447(16) 0.0313(14) -0.0024(11) 0.0175(12) -0.0047(13) N6 0.0628(19) 0.0470(16) 0.0477(15) -0.0004(12) 0.0218(14) -0.0128(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.329(3) . ? C1 C2 1.409(3) . ? C1 H1 0.9300 . ? C2 C3 1.362(4) . ? C2 H2 0.9300 . ? C3 C4 1.428(3) . ? C3 H3 0.9300 . ? C4 C5 1.389(3) . ? C4 N1 1.398(3) . ? C5 C6 1.404(3) . ? C5 C10 1.499(3) . ? C6 N2 1.400(3) . ? C6 C7 1.407(3) . ? C7 C8 1.374(3) . ? C7 H7 0.9300 . ? C8 C9 1.411(3) . ? C8 H8 0.9300 . ? C9 N2 1.336(3) . ? C9 H9 0.9300 . ? C10 C14 1.371(3) . ? C10 C11 1.375(3) . ? C11 C12 1.387(4) . ? C11 H11 0.9300 . ? C12 N3 1.317(3) . ? C12 H12 0.9300 . ? C13 N3 1.323(3) . ? C13 C14 1.383(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O1 1.272(3) . ? C15 C21 1.395(3) . ? C15 C16 1.497(3) . ? C16 C20 1.390(3) . ? C16 C17 1.394(3) . ? C17 C18 1.380(3) . ? C17 H17 0.9300 . ? C18 N4 1.339(3) . ? C18 H18 0.9300 . ? C19 N4 1.337(3) . ? C19 C20 1.382(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.393(3) . ? C21 H21 0.9300 . ? C22 O2 1.269(2) . ? C22 C23 1.506(3) . ? C23 C27 1.386(3) . ? C23 C24 1.387(3) . ? C24 C25 1.382(3) . ? C24 H24 0.9300 . ? C25 N5 1.330(3) . ? C25 H25 0.9300 . ? C26 N5 1.337(3) . ? C26 C27 1.381(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? N1 Cu1 1.9732(18) . ? N2 Cu1 1.9648(19) . ? N5 Cu1 2.3692(18) 2 ? O1 Cu1 1.9595(16) . ? O2 Cu1 1.9736(14) . ? Cu1 N5 2.3692(18) 2_545 ? C28 C29 1.452(4) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N6 1.126(3) . ? 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 C1 C2 112.0(2) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? C3 C2 C1 106.4(2) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.2(2) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? C5 C4 N1 124.05(19) . . ? C5 C4 C3 127.6(2) . . ? N1 C4 C3 108.4(2) . . ? C4 C5 C6 126.2(2) . . ? C4 C5 C10 116.34(19) . . ? C6 C5 C10 117.4(2) . . ? N2 C6 C5 123.2(2) . . ? N2 C6 C7 109.16(19) . . ? C5 C6 C7 127.6(2) . . ? C8 C7 C6 107.3(2) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.0(2) . . ? C7 C8 H8 127.0 . . ? C9 C8 H8 127.0 . . ? N2 C9 C8 111.81(19) . . ? N2 C9 H9 124.1 . . ? C8 C9 H9 124.1 . . ? C14 C10 C11 116.6(2) . . ? C14 C10 C5 119.9(2) . . ? C11 C10 C5 123.5(2) . . ? C10 C11 C12 119.2(2) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N3 C12 C11 124.6(2) . . ? N3 C12 H12 117.7 . . ? C11 C12 H12 117.7 . . ? N3 C13 C14 123.8(3) . . ? N3 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C10 C14 C13 120.0(2) . . ? C10 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? O1 C15 C21 125.6(2) . . ? O1 C15 C16 115.91(18) . . ? C21 C15 C16 118.49(18) . . ? C20 C16 C17 117.6(2) . . ? C20 C16 C15 122.55(19) . . ? C17 C16 C15 119.9(2) . . ? C18 C17 C16 119.0(2) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? N4 C18 C17 124.2(2) . . ? N4 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? N4 C19 C20 124.6(2) . . ? N4 C19 H19 117.7 . . ? C20 C19 H19 117.7 . . ? C19 C20 C16 118.7(2) . . ? C19 C20 H20 120.6 . . ? C16 C20 H20 120.6 . . ? C22 C21 C15 124.0(2) . . ? C22 C21 H21 118.0 . . ? C15 C21 H21 118.0 . . ? O2 C22 C21 125.63(19) . . ? O2 C22 C23 115.84(18) . . ? C21 C22 C23 118.53(18) . . ? C27 C23 C24 117.2(2) . . ? C27 C23 C22 120.49(19) . . ? C24 C23 C22 122.28(19) . . ? C25 C24 C23 119.0(2) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? N5 C25 C24 124.4(2) . . ? N5 C25 H25 117.8 . . ? C24 C25 H25 117.8 . . ? N5 C26 C27 123.8(2) . . ? N5 C26 H26 118.1 . . ? C27 C26 H26 118.1 . . ? C26 C27 C23 119.4(2) . . ? C26 C27 H27 120.3 . . ? C23 C27 H27 120.3 . . ? C1 N1 C4 106.09(18) . . ? C1 N1 Cu1 127.57(16) . . ? C4 N1 Cu1 125.15(15) . . ? C9 N2 C6 105.73(18) . . ? C9 N2 Cu1 126.74(15) . . ? C6 N2 Cu1 125.83(14) . . ? C12 N3 C13 115.8(2) . . ? C19 N4 C18 115.9(2) . . ? C25 N5 C26 116.12(19) . . ? C25 N5 Cu1 117.44(14) . 2 ? C26 N5 Cu1 124.62(15) . 2 ? C15 O1 Cu1 126.45(14) . . ? C22 O2 Cu1 126.13(14) . . ? O1 Cu1 N2 173.23(7) . . ? O1 Cu1 N1 87.66(7) . . ? N2 Cu1 N1 91.52(7) . . ? O1 Cu1 O2 90.75(6) . . ? N2 Cu1 O2 89.27(7) . . ? N1 Cu1 O2 173.12(7) . . ? O1 Cu1 N5 94.34(7) . 2_545 ? N2 Cu1 N5 92.39(7) . 2_545 ? N1 Cu1 N5 90.63(7) . 2_545 ? O2 Cu1 N5 96.17(6) . 2_545 ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C29 C28 178.7(3) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.359 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.086 #===END ###Material relevant to compound 2 at 173K ## data_compound2 _database_code_depnum_ccdc_archive 'CCDC 868786' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H29 Co N8 O2, 0.65(C5 H12), 1.35(C H Cl3), H2 O ' _chemical_formula_sum 'C45.60 H40.14 Cl4.05 Co N8 O3' _chemical_formula_weight 950.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.2041(5) _cell_length_b 13.8215(4) _cell_length_c 19.8539(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.1510(10) _cell_angle_gamma 90.00 _cell_volume 4486.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9974 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.52 _exptl_crystal_description plate _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1958.4 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9359 _exptl_absorpt_correction_T_max 0.9933 _exptl_absorpt_process_details sadabs _exptl_special_details ; A n-pentane and a CHCl3 molecule occupy the same site, the PARt command has been used. Another CHCl3 molecule shows rotational around its CH axis. Two positions have been modeled. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26044 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.53 _reflns_number_total 9942 _reflns_number_gt 8627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+8.1259P] 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 9942 _refine_ls_number_parameters 605 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1479 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.072 _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 C1 C 0.0993(2) 0.4619(2) 0.45934(16) 0.0344(6) Uani 1 1 d . A 1 H1 H 0.0511 0.4975 0.4487 0.041 Uiso 1 1 calc R A 1 C2 C 0.1783(2) 0.5017(2) 0.48546(18) 0.0413(7) Uani 1 1 d . A 1 H2 H 0.1912 0.5667 0.4948 0.050 Uiso 1 1 calc R A 1 C3 C 0.2324(2) 0.4270(2) 0.49454(17) 0.0360(7) Uani 1 1 d . A 1 H3 H 0.2891 0.4314 0.5115 0.043 Uiso 1 1 calc R A 1 C4 C 0.18555(17) 0.3414(2) 0.47322(15) 0.0284(6) Uani 1 1 d . A 1 C5 C 0.21405(17) 0.2469(2) 0.47557(15) 0.0273(6) Uani 1 1 d . A 1 C6 C 0.16417(16) 0.1657(2) 0.45661(14) 0.0256(5) Uani 1 1 d . A 1 C7 C 0.18693(18) 0.0667(2) 0.46696(16) 0.0311(6) Uani 1 1 d . A 1 H7 H 0.2399 0.0425 0.4837 0.037 Uiso 1 1 calc R A 1 C8 C 0.11610(19) 0.0134(2) 0.44771(16) 0.0327(6) Uani 1 1 d . A 1 H8 H 0.1118 -0.0536 0.4493 0.039 Uiso 1 1 calc R A 1 C9 C 0.05140(18) 0.0799(2) 0.42508(15) 0.0281(6) Uani 1 1 d . A 1 H9 H -0.0036 0.0630 0.4093 0.034 Uiso 1 1 calc R A 1 C10 C 0.30464(17) 0.2322(2) 0.50401(17) 0.0313(6) Uani 1 1 d . A 1 C11 C 0.3554(2) 0.2530(3) 0.46386(19) 0.0396(7) Uani 1 1 d . A 1 H11 H 0.3338 0.2765 0.4179 0.047 Uiso 1 1 calc R A 1 C12 C 0.4383(2) 0.2383(3) 0.4930(2) 0.0505(9) Uani 1 1 d . A 1 H12 H 0.4714 0.2520 0.4651 0.061 Uiso 1 1 calc R A 1 C13 C 0.4245(2) 0.1859(4) 0.5967(3) 0.0681(13) Uani 1 1 d . A 1 H13 H 0.4479 0.1631 0.6427 0.082 Uiso 1 1 calc R A 1 C14 C 0.3402(2) 0.1974(3) 0.5717(2) 0.0525(10) Uani 1 1 d . A 1 H14 H 0.3082 0.1818 0.6002 0.063 Uiso 1 1 calc R A 1 C15 C -0.06784(19) 0.1737(2) 0.26893(15) 0.0322(6) Uani 1 1 d . A 1 H15 H -0.0220 0.1733 0.2535 0.039 Uiso 1 1 calc R A 1 C16 C -0.1456(2) 0.1370(2) 0.22961(17) 0.0387(7) Uani 1 1 d . A 1 H16 H -0.1595 0.1081 0.1851 0.046 Uiso 1 1 calc R A 1 C17 C -0.1961(2) 0.1523(2) 0.26979(17) 0.0383(7) Uani 1 1 d . A 1 H17 H -0.2513 0.1367 0.2574 0.046 Uiso 1 1 calc R A 1 C18 C -0.14840(17) 0.1965(2) 0.33408(16) 0.0301(6) Uani 1 1 d . A 1 C19 C -0.17071(17) 0.2181(2) 0.39406(16) 0.0296(6) Uani 1 1 d . A 1 C20 C -0.11638(17) 0.2492(2) 0.45854(15) 0.0284(6) Uani 1 1 d . A 1 C21 C -0.1308(2) 0.2566(2) 0.52509(17) 0.0348(7) Uani 1 1 d . A 1 H21 H -0.1804 0.2463 0.5335 0.042 Uiso 1 1 calc R A 1 C22 C -0.0586(2) 0.2814(2) 0.57437(17) 0.0385(7) Uani 1 1 d . A 1 H22 H -0.0495 0.2910 0.6226 0.046 Uiso 1 1 calc R A 1 C23 C -0.00002(19) 0.2897(2) 0.53790(15) 0.0327(6) Uani 1 1 d . A 1 H23 H 0.0546 0.3061 0.5589 0.039 Uiso 1 1 calc R A 1 C24 C -0.25845(18) 0.2061(2) 0.38956(17) 0.0347(7) Uani 1 1 d . A 1 C25 C -0.2937(2) 0.1175(3) 0.3924(2) 0.0533(10) Uani 1 1 d . A 1 H25 H -0.2628 0.0611 0.3979 0.064 Uiso 1 1 calc R A 1 C26 C -0.3756(2) 0.1135(3) 0.3871(3) 0.0646(12) Uani 1 1 d . A 1 H26 H -0.3978 0.0530 0.3905 0.077 Uiso 1 1 calc R A 1 C27 C -0.3895(2) 0.2735(3) 0.3775(3) 0.0766(16) Uani 1 1 d . A 1 H27 H -0.4218 0.3286 0.3726 0.092 Uiso 1 1 calc R A 1 C28 C -0.3076(2) 0.2860(3) 0.3840(3) 0.0625(12) Uani 1 1 d . A 1 H28 H -0.2861 0.3478 0.3846 0.075 Uiso 1 1 calc R A 1 C29 C 0.2467(2) 0.3883(3) 0.2315(2) 0.0445(8) Uani 1 1 d . A 1 H29 H 0.3027 0.3890 0.2548 0.053 Uiso 1 1 calc R A 1 C30 C 0.19468(19) 0.3742(2) 0.27193(18) 0.0371(7) Uani 1 1 d . A 1 H30 H 0.2155 0.3639 0.3205 0.044 Uiso 1 1 calc R A 1 C31 C 0.11126(17) 0.3759(2) 0.23810(15) 0.0266(6) Uani 1 1 d . A 1 C32 C 0.08350(19) 0.3900(2) 0.16545(16) 0.0333(6) Uani 1 1 d . A 1 H32 H 0.0278 0.3919 0.1411 0.040 Uiso 1 1 calc R A 1 C33 C 0.1406(2) 0.4011(3) 0.12988(18) 0.0427(8) Uani 1 1 d . A 1 H33 H 0.1216 0.4091 0.0810 0.051 Uiso 1 1 calc R A 1 C34 C 0.05332(16) 0.3662(2) 0.28002(14) 0.0249(5) Uani 1 1 d . A 1 C35 C -0.01141(18) 0.4314(2) 0.26707(16) 0.0307(6) Uani 1 1 d . A 1 H35 H -0.0214 0.4711 0.2274 0.037 Uiso 1 1 calc R A 1 C36 C -0.06209(16) 0.4413(2) 0.30915(15) 0.0259(5) Uani 1 1 d . A 1 C37 C -0.12900(17) 0.5153(2) 0.29162(15) 0.0275(6) Uani 1 1 d . A 1 C38 C -0.1696(2) 0.5356(3) 0.34012(17) 0.0393(7) Uani 1 1 d . A 1 H38 H -0.1540 0.5057 0.3843 0.047 Uiso 1 1 calc R A 1 C39 C -0.2337(2) 0.6009(3) 0.32213(19) 0.0459(8) Uani 1 1 d . A 1 H39 H -0.2607 0.6130 0.3552 0.055 Uiso 1 1 calc R A 1 C40 C -0.2193(2) 0.6278(3) 0.2146(2) 0.0449(8) Uani 1 1 d . A 1 H40 H -0.2361 0.6591 0.1709 0.054 Uiso 1 1 calc R A 1 C41 C -0.1544(2) 0.5635(2) 0.22747(17) 0.0376(7) Uani 1 1 d . A 1 H41 H -0.1283 0.5531 0.1935 0.045 Uiso 1 1 calc R A 1 N1 N 0.10272(14) 0.36601(17) 0.45188(12) 0.0271(5) Uani 1 1 d . A 1 N2 N 0.07931(13) 0.17055(16) 0.42919(12) 0.0238(4) Uani 1 1 d . A 1 N3 N 0.47386(18) 0.2059(3) 0.5582(2) 0.0593(9) Uani 1 1 d . A 1 N4 N -0.06922(14) 0.20901(17) 0.33108(12) 0.0274(5) Uani 1 1 d . A 1 N5 N -0.03440(14) 0.27060(17) 0.46889(12) 0.0270(5) Uani 1 1 d . A 1 N6 N -0.42484(19) 0.1890(3) 0.3777(2) 0.0615(9) Uani 1 1 d . A 1 N7 N 0.22128(18) 0.4009(2) 0.16173(17) 0.0447(7) Uani 1 1 d . A 1 N8 N -0.25905(17) 0.6474(2) 0.26036(16) 0.0435(7) Uani 1 1 d . A 1 O1 O 0.06993(12) 0.29858(14) 0.32620(10) 0.0264(4) Uani 1 1 d . A 1 O2 O -0.05504(12) 0.39293(14) 0.36539(10) 0.0277(4) Uani 1 1 d . A 1 Co1 Co 0.01556(2) 0.28398(3) 0.396173(19) 0.02348(11) Uani 1 1 d . A 1 C42 C 0.6410(2) 0.3922(3) 0.1237(2) 0.0569(10) Uani 1 1 d . B 1 H42 H 0.6002 0.3452 0.0975 0.068 Uiso 1 1 calc R B 1 Cl1 Cl 0.6546(2) 0.3790(4) 0.21470(17) 0.0976(10) Uani 0.713(13) 1 d P B 1 Cl2 Cl 0.7352(2) 0.3643(3) 0.1114(2) 0.0884(11) Uani 0.713(13) 1 d P B 1 Cl3 Cl 0.6082(4) 0.5068(3) 0.0932(5) 0.120(2) Uani 0.713(13) 1 d P B 1 Cl1B Cl 0.6246(12) 0.4351(18) 0.2001(7) 0.147(7) Uani 0.287(13) 1 d P B 2 Cl2B Cl 0.7345(6) 0.3573(10) 0.1379(14) 0.180(7) Uani 0.287(13) 1 d P B 2 Cl3B Cl 0.6126(9) 0.4967(12) 0.0717(13) 0.146(7) Uani 0.287(13) 1 d P B 2 O3 O 0.40688(17) 0.2602(2) 0.3110(2) 0.0666(9) Uani 1 1 d D . . C43 C 0.4426(13) 0.4803(17) 0.3597(11) 0.226(3) Uani 0.351(6) 1 d PD C 1 H43 H 0.4266 0.4127 0.3483 0.272 Uiso 0.351(6) 1 calc PR C 1 Cl4 Cl 0.3820(7) 0.5549(11) 0.3922(8) 0.226(3) Uani 0.351(6) 1 d PD C 1 Cl5 Cl 0.5342(6) 0.5062(8) 0.4202(6) 0.226(3) Uani 0.351(6) 1 d PD C 1 Cl6 Cl 0.4501(4) 0.5579(5) 0.2934(4) 0.226(3) Uani 0.351(6) 1 d PD C 1 C44 C 0.3628(8) 0.6120(8) 0.4404(8) 0.142(6) Uani 0.649(6) 1 d PD C 2 H44A H 0.4168 0.6186 0.4735 0.214 Uiso 0.649(6) 1 calc PR C 2 H44B H 0.3250 0.5965 0.4656 0.214 Uiso 0.649(6) 1 calc PR C 2 H44C H 0.3468 0.6717 0.4152 0.214 Uiso 0.649(6) 1 calc PR C 2 C45 C 0.3625(4) 0.5317(6) 0.3882(4) 0.0541(17) Uani 0.649(6) 1 d PD C 2 H45A H 0.3160 0.5381 0.3457 0.065 Uiso 0.649(6) 1 calc PR C 2 H45B H 0.3603 0.4688 0.4092 0.065 Uiso 0.649(6) 1 calc PR C 2 C46 C 0.4444(9) 0.5446(19) 0.3710(9) 0.248(13) Uani 0.649(6) 1 d PD C 2 H46A H 0.4778 0.4888 0.3910 0.298 Uiso 0.649(6) 1 calc PR C 2 H46B H 0.4714 0.6003 0.3980 0.298 Uiso 0.649(6) 1 calc PR C 2 C47 C 0.4501(4) 0.5579(5) 0.2934(4) 0.226(3) Uani 0.649(6) 1 d PD C 2 H47A H 0.4235 0.5059 0.2617 0.272 Uiso 0.649(6) 1 calc PR C 2 H47B H 0.4292 0.6200 0.2728 0.272 Uiso 0.649(6) 1 calc PR C 2 C48 C 0.5449(7) 0.5519(10) 0.3152(9) 0.167(7) Uani 0.649(6) 1 d PD C 2 H48A H 0.5661 0.6106 0.3019 0.251 Uiso 0.649(6) 1 calc PR C 2 H48B H 0.5605 0.4981 0.2918 0.251 Uiso 0.649(6) 1 calc PR C 2 H48C H 0.5668 0.5434 0.3656 0.251 Uiso 0.649(6) 1 calc PR C 2 H3A H 0.3666(15) 0.227(2) 0.2843(18) 0.049 Uiso 1 1 d D D 2 H3B H 0.4523(14) 0.232(2) 0.3332(18) 0.049 Uiso 1 1 d D E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0365(16) 0.0299(15) 0.0354(15) -0.0031(12) 0.0091(13) 0.0061(12) C2 0.0469(19) 0.0282(15) 0.0455(18) -0.0069(13) 0.0094(15) -0.0009(13) C3 0.0327(16) 0.0351(16) 0.0376(16) -0.0034(13) 0.0072(13) -0.0030(12) C4 0.0271(14) 0.0314(14) 0.0268(13) 0.0003(11) 0.0085(11) 0.0007(11) C5 0.0249(13) 0.0317(14) 0.0271(13) 0.0032(11) 0.0108(11) 0.0026(11) C6 0.0248(13) 0.0282(13) 0.0256(13) 0.0050(11) 0.0105(11) 0.0066(10) C7 0.0317(15) 0.0294(14) 0.0339(15) 0.0032(12) 0.0126(12) 0.0073(11) C8 0.0377(16) 0.0252(14) 0.0361(15) 0.0015(12) 0.0130(13) 0.0045(12) C9 0.0276(14) 0.0280(13) 0.0280(13) 0.0009(11) 0.0076(11) -0.0008(11) C10 0.0237(14) 0.0315(15) 0.0390(16) 0.0038(12) 0.0104(12) 0.0024(11) C11 0.0337(16) 0.0455(18) 0.0429(18) 0.0016(15) 0.0167(14) -0.0003(14) C12 0.0293(17) 0.062(2) 0.064(2) 0.001(2) 0.0211(17) -0.0014(16) C13 0.033(2) 0.095(3) 0.069(3) 0.042(3) 0.0049(19) 0.008(2) C14 0.0299(17) 0.075(3) 0.051(2) 0.028(2) 0.0105(16) 0.0026(17) C15 0.0348(16) 0.0357(15) 0.0276(14) -0.0021(12) 0.0123(12) 0.0006(12) C16 0.0408(18) 0.0425(18) 0.0301(15) -0.0057(13) 0.0074(13) -0.0046(14) C17 0.0291(15) 0.0459(18) 0.0368(16) 0.0002(14) 0.0058(13) -0.0021(13) C18 0.0255(14) 0.0320(14) 0.0331(15) 0.0030(12) 0.0096(12) 0.0025(11) C19 0.0276(14) 0.0263(13) 0.0378(15) 0.0051(12) 0.0146(12) 0.0052(11) C20 0.0294(14) 0.0271(13) 0.0328(14) 0.0061(11) 0.0157(12) 0.0072(11) C21 0.0411(17) 0.0330(15) 0.0376(16) 0.0089(13) 0.0230(14) 0.0118(13) C22 0.0464(19) 0.0463(18) 0.0280(15) 0.0056(13) 0.0191(14) 0.0152(15) C23 0.0327(15) 0.0392(16) 0.0252(13) 0.0005(12) 0.0074(12) 0.0081(12) C24 0.0271(15) 0.0374(16) 0.0419(17) -0.0011(13) 0.0141(13) 0.0036(12) C25 0.0406(19) 0.0418(19) 0.086(3) 0.0161(19) 0.031(2) 0.0050(15) C26 0.044(2) 0.058(2) 0.101(4) 0.011(2) 0.036(2) -0.0058(19) C27 0.032(2) 0.058(3) 0.141(5) -0.001(3) 0.029(3) 0.0124(18) C28 0.037(2) 0.039(2) 0.112(4) -0.003(2) 0.024(2) 0.0030(15) C29 0.0325(17) 0.048(2) 0.059(2) 0.0020(17) 0.0227(16) 0.0023(14) C30 0.0314(16) 0.0445(18) 0.0370(16) 0.0042(14) 0.0133(13) 0.0033(13) C31 0.0287(14) 0.0251(13) 0.0300(14) 0.0007(11) 0.0149(12) 0.0022(10) C32 0.0332(15) 0.0375(16) 0.0319(15) 0.0008(12) 0.0139(13) 0.0004(12) C33 0.051(2) 0.0488(19) 0.0365(17) 0.0030(15) 0.0261(16) 0.0007(16) C34 0.0257(13) 0.0272(13) 0.0235(12) 0.0000(10) 0.0101(11) 0.0013(10) C35 0.0310(15) 0.0339(15) 0.0298(14) 0.0081(12) 0.0132(12) 0.0072(12) C36 0.0239(13) 0.0265(13) 0.0271(13) 0.0011(11) 0.0075(11) 0.0022(10) C37 0.0244(13) 0.0281(13) 0.0299(14) 0.0011(11) 0.0082(11) 0.0023(11) C38 0.0356(16) 0.0488(19) 0.0345(16) 0.0052(14) 0.0124(13) 0.0160(14) C39 0.0409(18) 0.058(2) 0.0423(18) 0.0006(16) 0.0178(15) 0.0186(16) C40 0.0412(18) 0.0472(19) 0.0482(19) 0.0177(16) 0.0166(16) 0.0171(15) C41 0.0373(17) 0.0410(17) 0.0384(17) 0.0119(14) 0.0174(14) 0.0128(13) N1 0.0287(12) 0.0267(11) 0.0272(11) 0.0001(9) 0.0107(10) 0.0046(9) N2 0.0236(11) 0.0245(11) 0.0234(11) 0.0010(9) 0.0076(9) 0.0031(9) N3 0.0278(15) 0.070(2) 0.078(2) 0.0185(19) 0.0135(16) 0.0048(14) N4 0.0239(11) 0.0327(12) 0.0264(11) 0.0024(10) 0.0089(9) 0.0035(9) N5 0.0281(12) 0.0296(12) 0.0248(11) 0.0023(9) 0.0104(10) 0.0063(9) N6 0.0332(16) 0.063(2) 0.094(3) -0.009(2) 0.0278(18) -0.0036(15) N7 0.0453(17) 0.0451(16) 0.0565(18) 0.0026(14) 0.0343(15) 0.0006(13) N8 0.0343(15) 0.0446(16) 0.0509(17) 0.0055(13) 0.0122(13) 0.0139(12) O1 0.0262(10) 0.0293(10) 0.0256(9) 0.0039(8) 0.0109(8) 0.0065(8) O2 0.0280(10) 0.0306(10) 0.0265(9) 0.0039(8) 0.0116(8) 0.0073(8) Co1 0.0234(2) 0.02542(19) 0.02294(19) 0.00168(14) 0.00917(15) 0.00433(14) C42 0.045(2) 0.060(2) 0.065(3) -0.005(2) 0.0165(19) -0.0143(18) Cl1 0.112(2) 0.123(3) 0.0639(13) -0.0072(15) 0.0360(13) 0.001(2) Cl2 0.0784(19) 0.0697(15) 0.147(3) -0.0193(14) 0.078(2) -0.0162(12) Cl3 0.092(3) 0.0524(16) 0.181(5) 0.005(2) -0.007(2) 0.0047(15) Cl1B 0.147(11) 0.203(16) 0.106(7) -0.061(8) 0.060(7) -0.109(11) Cl2B 0.049(5) 0.134(8) 0.290(17) -0.004(10) -0.046(6) -0.002(4) Cl3B 0.056(5) 0.144(11) 0.236(17) 0.102(11) 0.040(8) -0.006(6) O3 0.0329(14) 0.0575(18) 0.096(2) -0.0107(17) 0.0010(15) -0.0080(13) C43 0.183(5) 0.214(6) 0.257(7) -0.005(4) 0.033(4) -0.059(4) Cl4 0.183(5) 0.214(6) 0.257(7) -0.005(4) 0.033(4) -0.059(4) Cl5 0.183(5) 0.214(6) 0.257(7) -0.005(4) 0.033(4) -0.059(4) Cl6 0.183(5) 0.214(6) 0.257(7) -0.005(4) 0.033(4) -0.059(4) C44 0.125(10) 0.098(8) 0.239(17) -0.050(9) 0.106(11) -0.037(7) C45 0.038(3) 0.069(4) 0.052(3) -0.011(3) 0.009(3) -0.014(3) C46 0.124(13) 0.48(4) 0.168(16) -0.08(2) 0.078(12) -0.126(18) C47 0.183(5) 0.214(6) 0.257(7) -0.005(4) 0.033(4) -0.059(4) C48 0.134(11) 0.145(12) 0.28(2) 0.016(12) 0.141(13) 0.012(9) _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 C1 N1 1.337(4) . ? C1 C2 1.407(5) . ? C1 H1 0.9300 . ? C2 C3 1.363(4) . ? C2 H2 0.9300 . ? C3 C4 1.421(4) . ? C3 H3 0.9300 . ? C4 C5 1.391(4) . ? C4 N1 1.397(4) . ? C5 C6 1.391(4) . ? C5 C10 1.497(4) . ? C6 N2 1.392(3) . ? C6 C7 1.421(4) . ? C7 C8 1.372(4) . ? C7 H7 0.9300 . ? C8 C9 1.405(4) . ? C8 H8 0.9300 . ? C9 N2 1.335(4) . ? C9 H9 0.9300 . ? C10 C14 1.378(5) . ? C10 C11 1.383(4) . ? C11 C12 1.377(5) . ? C11 H11 0.9300 . ? C12 N3 1.326(5) . ? C12 H12 0.9300 . ? C13 N3 1.337(5) . ? C13 C14 1.388(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N4 1.334(4) . ? C15 C16 1.416(4) . ? C15 H15 0.9300 . ? C16 C17 1.367(4) . ? C16 H16 0.9300 . ? C17 C18 1.422(4) . ? C17 H17 0.9300 . ? C18 C19 1.392(4) . ? C18 N4 1.393(4) . ? C19 C20 1.397(4) . ? C19 C24 1.493(4) . ? C20 N5 1.392(4) . ? C20 C21 1.422(4) . ? C21 C22 1.365(5) . ? C21 H21 0.9300 . ? C22 C23 1.417(4) . ? C22 H22 0.9300 . ? C23 N5 1.339(4) . ? C23 H23 0.9300 . ? C24 C28 1.374(5) . ? C24 C25 1.376(5) . ? C25 C26 1.381(5) . ? C25 H25 0.9300 . ? C26 N6 1.320(5) . ? C26 H26 0.9300 . ? C27 N6 1.318(6) . ? C27 C28 1.386(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 N7 1.329(5) . ? C29 C30 1.389(4) . ? C29 H29 0.9300 . ? C30 C31 1.382(4) . ? C30 H30 0.9300 . ? C31 C32 1.385(4) . ? C31 C34 1.490(3) . ? C32 C33 1.385(4) . ? C32 H32 0.9300 . ? C33 N7 1.334(5) . ? C33 H33 0.9300 . ? C34 O1 1.278(3) . ? C34 C35 1.393(4) . ? C35 C36 1.390(4) . ? C35 H35 0.9300 . ? C36 O2 1.275(3) . ? C36 C37 1.498(4) . ? C37 C41 1.382(4) . ? C37 C38 1.383(4) . ? C38 C39 1.382(4) . ? C38 H38 0.9300 . ? C39 N8 1.332(4) . ? C39 H39 0.9300 . ? C40 N8 1.325(4) . ? C40 C41 1.388(4) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? N1 Co1 1.930(2) . ? N2 Co1 1.908(2) . ? N4 Co1 1.923(2) . ? N5 Co1 1.905(2) . ? O1 Co1 1.9120(18) . ? O2 Co1 1.9116(19) . ? C42 Cl3 1.726(7) . ? C42 Cl2 1.755(5) . ? C42 Cl1 1.757(6) . ? C42 H42 0.9800 . ? O3 H3A 0.863(17) . ? O3 H3B 0.861(17) . ? C43 Cl5 1.696(19) . ? C43 Cl4 1.729(19) . ? C43 Cl6 1.734(19) . ? C43 H43 0.9800 . ? C44 C45 1.518(12) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.560(12) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? 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 C1 C2 111.0(3) . . ? N1 C1 H1 124.5 . . ? C2 C1 H1 124.5 . . ? C3 C2 C1 107.1(3) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 107.0(3) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 N1 123.7(3) . . ? C5 C4 C3 127.7(3) . . ? N1 C4 C3 108.5(3) . . ? C4 C5 C6 124.5(3) . . ? C4 C5 C10 117.0(3) . . ? C6 C5 C10 118.4(3) . . ? C5 C6 N2 123.4(2) . . ? C5 C6 C7 128.2(3) . . ? N2 C6 C7 108.1(2) . . ? C8 C7 C6 107.2(3) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 106.5(3) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C8 111.1(3) . . ? N2 C9 H9 124.4 . . ? C8 C9 H9 124.4 . . ? C14 C10 C11 117.8(3) . . ? C14 C10 C5 120.6(3) . . ? C11 C10 C5 121.6(3) . . ? C12 C11 C10 119.0(3) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? N3 C12 C11 124.3(3) . . ? N3 C12 H12 117.9 . . ? C11 C12 H12 117.9 . . ? N3 C13 C14 123.4(4) . . ? N3 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C10 C14 C13 119.1(3) . . ? C10 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N4 C15 C16 110.8(3) . . ? N4 C15 H15 124.6 . . ? C16 C15 H15 124.6 . . ? C17 C16 C15 106.6(3) . . ? C17 C16 H16 126.7 . . ? C15 C16 H16 126.7 . . ? C16 C17 C18 107.2(3) . . ? C16 C17 H17 126.4 . . ? C18 C17 H17 126.4 . . ? C19 C18 N4 122.9(3) . . ? C19 C18 C17 128.6(3) . . ? N4 C18 C17 108.3(3) . . ? C18 C19 C20 124.4(3) . . ? C18 C19 C24 117.9(3) . . ? C20 C19 C24 117.7(3) . . ? N5 C20 C19 124.0(2) . . ? N5 C20 C21 108.0(3) . . ? C19 C20 C21 127.8(3) . . ? C22 C21 C20 107.5(3) . . ? C22 C21 H21 126.3 . . ? C20 C21 H21 126.3 . . ? C21 C22 C23 106.7(3) . . ? C21 C22 H22 126.6 . . ? C23 C22 H22 126.6 . . ? N5 C23 C22 110.5(3) . . ? N5 C23 H23 124.8 . . ? C22 C23 H23 124.8 . . ? C28 C24 C25 116.8(3) . . ? C28 C24 C19 120.0(3) . . ? C25 C24 C19 123.2(3) . . ? C24 C25 C26 119.0(4) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? N6 C26 C25 125.0(4) . . ? N6 C26 H26 117.5 . . ? C25 C26 H26 117.5 . . ? N6 C27 C28 124.5(4) . . ? N6 C27 H27 117.7 . . ? C28 C27 H27 117.7 . . ? C24 C28 C27 119.3(4) . . ? C24 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? N7 C29 C30 124.0(3) . . ? N7 C29 H29 118.0 . . ? C30 C29 H29 118.0 . . ? C31 C30 C29 118.4(3) . . ? C31 C30 H30 120.8 . . ? C29 C30 H30 120.8 . . ? C30 C31 C32 118.5(3) . . ? C30 C31 C34 120.1(3) . . ? C32 C31 C34 121.4(3) . . ? C31 C32 C33 118.5(3) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? N7 C33 C32 123.8(3) . . ? N7 C33 H33 118.1 . . ? C32 C33 H33 118.1 . . ? O1 C34 C35 126.4(2) . . ? O1 C34 C31 115.3(2) . . ? C35 C34 C31 118.3(2) . . ? C36 C35 C34 124.6(3) . . ? C36 C35 H35 117.7 . . ? C34 C35 H35 117.7 . . ? O2 C36 C35 124.7(3) . . ? O2 C36 C37 114.7(2) . . ? C35 C36 C37 120.6(2) . . ? C41 C37 C38 117.4(3) . . ? C41 C37 C36 122.8(3) . . ? C38 C37 C36 119.7(3) . . ? C39 C38 C37 119.2(3) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? N8 C39 C38 124.0(3) . . ? N8 C39 H39 118.0 . . ? C38 C39 H39 118.0 . . ? N8 C40 C41 124.2(3) . . ? N8 C40 H40 117.9 . . ? C41 C40 H40 117.9 . . ? C37 C41 C40 118.9(3) . . ? C37 C41 H41 120.5 . . ? C40 C41 H41 120.5 . . ? C1 N1 C4 106.5(2) . . ? C1 N1 Co1 126.4(2) . . ? C4 N1 Co1 124.59(19) . . ? C9 N2 C6 107.0(2) . . ? C9 N2 Co1 126.34(19) . . ? C6 N2 Co1 126.48(18) . . ? C12 N3 C13 116.5(3) . . ? C15 N4 C18 107.1(2) . . ? C15 N4 Co1 126.2(2) . . ? C18 N4 Co1 125.84(19) . . ? C23 N5 C20 107.3(2) . . ? C23 N5 Co1 126.6(2) . . ? C20 N5 Co1 125.74(19) . . ? C27 N6 C26 115.2(3) . . ? C29 N7 C33 116.8(3) . . ? C40 N8 C39 116.2(3) . . ? C34 O1 Co1 123.22(17) . . ? C36 O2 Co1 124.82(17) . . ? N5 Co1 N2 90.39(10) . . ? N5 Co1 O2 85.81(9) . . ? N2 Co1 O2 175.46(9) . . ? N5 Co1 O1 177.60(9) . . ? N2 Co1 O1 88.70(9) . . ? O2 Co1 O1 95.19(8) . . ? N5 Co1 N4 91.73(10) . . ? N2 Co1 N4 91.30(10) . . ? O2 Co1 N4 86.34(9) . . ? O1 Co1 N4 90.51(9) . . ? N5 Co1 N1 94.36(10) . . ? N2 Co1 N1 91.43(10) . . ? O2 Co1 N1 91.33(9) . . ? O1 Co1 N1 83.44(9) . . ? N4 Co1 N1 173.31(10) . . ? Cl3 C42 Cl2 111.6(3) . . ? Cl3 C42 Cl1 112.3(4) . . ? Cl2 C42 Cl1 106.7(3) . . ? Cl3 C42 H42 108.7 . . ? Cl2 C42 H42 108.7 . . ? Cl1 C42 H42 108.7 . . ? H3A O3 H3B 120(3) . . ? Cl5 C43 Cl4 98.3(12) . . ? Cl5 C43 Cl6 97.7(12) . . ? Cl4 C43 Cl6 96.4(12) . . ? Cl5 C43 H43 119.8 . . ? Cl4 C43 H43 119.8 . . ? Cl6 C43 H43 119.8 . . ? C45 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C45 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C44 C45 C46 104.8(10) . . ? C44 C45 H45A 110.8 . . ? C46 C45 H45A 110.8 . . ? C44 C45 H45B 110.8 . . ? C46 C45 H45B 110.8 . . ? H45A C45 H45B 108.9 . . ? C45 C46 H46A 106.3 . . ? C45 C46 H46B 106.3 . . ? H46A C46 H46B 106.4 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.384 _refine_diff_density_min -0.898 _refine_diff_density_rms 0.071 #===END ###Material relevant to compound 5 at 173K ## data_compound5 _database_code_depnum_ccdc_archive 'CCDC 868787' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H78 Ag4 B4 Cu4 F16 N20 O9' _chemical_formula_weight 2832.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3262(3) _cell_length_b 13.6246(3) _cell_length_c 17.0399(3) _cell_angle_alpha 67.5880(10) _cell_angle_beta 77.9490(10) _cell_angle_gamma 76.3120(10) _cell_volume 2754.60(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9948 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.52 _exptl_crystal_description platelet _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1406 _exptl_absorpt_coefficient_mu 1.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8607 _exptl_absorpt_correction_T_max 0.9697 _exptl_absorpt_process_details sadabs _exptl_special_details ; One of the tetrafluoroborate anion shows positional disorder. It has been modeled over two positions and the thermal parameters of the constituting atoms have been constrained. The structure contains one water molecule for which the H atoms have not been introduced but are taken into account in the compound's formula. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53389 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 29.41 _reflns_number_total 14644 _reflns_number_gt 9773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+13.8688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14644 _refine_ls_number_parameters 740 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.2060 _refine_ls_wR_factor_gt 0.1833 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6161(5) 0.9731(5) 0.3081(4) 0.0243(12) Uani 1 1 d . . . H1 H 0.6267 0.9156 0.3589 0.029 Uiso 1 1 calc R . . C2 C 0.5985(5) 0.9621(5) 0.2334(4) 0.0265(12) Uani 1 1 d . . . H2 H 0.5945 0.8988 0.2263 0.032 Uiso 1 1 calc R . . C3 C 0.5885(5) 1.0641(5) 0.1734(4) 0.0263(12) Uani 1 1 d . . . H3 H 0.5758 1.0832 0.1173 0.032 Uiso 1 1 calc R . . C4 C 0.6011(4) 1.1355(4) 0.2124(3) 0.0211(11) Uani 1 1 d . . . C5 C 0.6043(4) 1.2452(4) 0.1752(3) 0.0228(11) Uani 1 1 d . . . C6 C 0.6161(5) 1.3115(4) 0.2172(3) 0.0225(11) Uani 1 1 d . . . C7 C 0.6215(5) 1.4242(5) 0.1818(4) 0.0285(13) Uani 1 1 d . . . H7 H 0.6176 1.4686 0.1250 0.034 Uiso 1 1 calc R . . C8 C 0.6331(5) 1.4545(5) 0.2462(4) 0.0290(13) Uani 1 1 d . . . H8 H 0.6393 1.5228 0.2421 0.035 Uiso 1 1 calc R . . C9 C 0.6338(5) 1.3602(4) 0.3211(4) 0.0265(12) Uani 1 1 d . . . H9 H 0.6408 1.3578 0.3750 0.032 Uiso 1 1 calc R . . C10 C 0.5957(5) 1.2962(5) 0.0821(3) 0.0242(12) Uani 1 1 d . . . C11 C 0.6760(5) 1.3460(5) 0.0242(4) 0.0290(13) Uani 1 1 d . . . H11 H 0.7341 1.3507 0.0440 0.035 Uiso 1 1 calc R . . C12 C 0.6679(5) 1.3882(5) -0.0624(4) 0.0328(14) Uani 1 1 d . . . H12 H 0.7219 1.4206 -0.1000 0.039 Uiso 1 1 calc R . . C13 C 0.5094(6) 1.3383(5) -0.0404(4) 0.0349(15) Uani 1 1 d . . . H13 H 0.4521 1.3352 -0.0621 0.042 Uiso 1 1 calc R . . C14 C 0.5111(5) 1.2939(5) 0.0484(4) 0.0313(14) Uani 1 1 d . . . H14 H 0.4554 1.2630 0.0844 0.038 Uiso 1 1 calc R . . C15 C 0.6379(5) 0.6565(5) 0.5996(4) 0.0297(13) Uani 1 1 d . . . H15 H 0.6388 0.6120 0.5694 0.036 Uiso 1 1 calc R . . C16 C 0.6401(5) 0.7642(5) 0.5547(4) 0.0267(13) Uani 1 1 d . . . H16 H 0.6426 0.7912 0.4955 0.032 Uiso 1 1 calc R . . C17 C 0.6385(4) 0.8325(4) 0.5983(3) 0.0191(10) Uani 1 1 d . . . C18 C 0.6385(5) 0.7872(5) 0.6855(4) 0.0245(12) Uani 1 1 d . . . H18 H 0.6394 0.8297 0.7169 0.029 Uiso 1 1 calc R . . C19 C 0.6371(5) 0.6774(4) 0.7264(4) 0.0247(12) Uani 1 1 d . . . H19 H 0.6380 0.6480 0.7853 0.030 Uiso 1 1 calc R . . C20 C 0.6359(4) 0.9508(4) 0.5502(3) 0.0193(11) Uani 1 1 d . . . C21 C 0.6211(4) 1.0199(4) 0.5961(4) 0.0223(11) Uani 1 1 d . . . H21 H 0.6163 0.9903 0.6555 0.027 Uiso 1 1 calc R . . C22 C 0.6134(4) 1.1321(4) 0.5567(3) 0.0209(11) Uani 1 1 d . . . C23 C 0.5967(5) 1.2007(4) 0.6103(4) 0.0229(11) Uani 1 1 d . . . C24 C 0.6186(5) 1.1612(5) 0.6938(4) 0.0244(12) Uani 1 1 d . . . H24 H 0.6417 1.0880 0.7208 0.029 Uiso 1 1 calc R . . C25 C 0.6056(5) 1.2331(5) 0.7365(4) 0.0273(13) Uani 1 1 d . . . H25 H 0.6216 1.2064 0.7923 0.033 Uiso 1 1 calc R . . C26 C 0.5486(7) 1.3755(5) 0.6214(5) 0.049(2) Uani 1 1 d . . . H26 H 0.5247 1.4489 0.5961 0.058 Uiso 1 1 calc R . . C27 C 0.5590(7) 1.3102(5) 0.5753(4) 0.0425(18) Uani 1 1 d . . . H27 H 0.5409 1.3391 0.5201 0.051 Uiso 1 1 calc R . . N1 N 0.6160(4) 1.0754(4) 0.2980(3) 0.0211(9) Uani 1 1 d . . . N2 N 0.6230(4) 1.2757(4) 0.3040(3) 0.0214(9) Uani 1 1 d . . . N3 N 0.5861(5) 1.3846(4) -0.0951(3) 0.0334(12) Uani 1 1 d . . . N4 N 0.6344(4) 0.6126(4) 0.6857(3) 0.0261(11) Uani 1 1 d . . . N5 N 0.5713(5) 1.3384(4) 0.7017(3) 0.0319(12) Uani 1 1 d . . . O1 O 0.6487(3) 0.9806(3) 0.4682(2) 0.0252(9) Uani 1 1 d . . . O2 O 0.6202(4) 1.1817(3) 0.4768(3) 0.0280(9) Uani 1 1 d . . . Cu1 Cu 0.62958(5) 1.12798(5) 0.38525(4) 0.02064(16) Uani 1 1 d . . . Ag1 Ag 0.57107(5) 0.45828(4) 0.76318(3) 0.03922(16) Uani 1 1 d . . . C28 C 0.8523(5) 0.7978(5) 0.3485(4) 0.0269(12) Uani 1 1 d . . . H28 H 0.8463 0.7458 0.4030 0.032 Uiso 1 1 calc R . . C29 C 0.8540(5) 0.7793(5) 0.2738(4) 0.0276(13) Uani 1 1 d . . . H29 H 0.8489 0.7147 0.2695 0.033 Uiso 1 1 calc R . . C30 C 0.8648(4) 0.8753(5) 0.2067(4) 0.0248(12) Uani 1 1 d . . . H30 H 0.8690 0.8876 0.1486 0.030 Uiso 1 1 calc R . . C31 C 0.8683(4) 0.9512(4) 0.2440(3) 0.0214(11) Uani 1 1 d . . . C32 C 0.8784(4) 1.0601(4) 0.2021(3) 0.0226(11) Uani 1 1 d . . . C33 C 0.8755(4) 1.1338(4) 0.2420(3) 0.0211(11) Uani 1 1 d . . . C34 C 0.8822(4) 1.2456(4) 0.2041(4) 0.0237(12) Uani 1 1 d . . . H34 H 0.8913 1.2852 0.1458 0.028 Uiso 1 1 calc R . . C35 C 0.8728(5) 1.2838(5) 0.2685(4) 0.0271(13) Uani 1 1 d . . . H35 H 0.8739 1.3542 0.2629 0.032 Uiso 1 1 calc R . . C36 C 0.8612(4) 1.1965(4) 0.3450(4) 0.0223(11) Uani 1 1 d . . . H36 H 0.8539 1.2010 0.3991 0.027 Uiso 1 1 calc R . . C37 C 0.8966(5) 1.1028(5) 0.1058(3) 0.0249(12) Uani 1 1 d . . . C38 C 0.9818(5) 1.1517(5) 0.0619(4) 0.0303(13) Uani 1 1 d . . . H38 H 1.0311 1.1554 0.0916 0.036 Uiso 1 1 calc R . . C39 C 0.9930(5) 1.1950(5) -0.0268(4) 0.0323(14) Uani 1 1 d . . . H39 H 1.0502 1.2282 -0.0556 0.039 Uiso 1 1 calc R . . C40 C 0.8448(5) 1.1410(5) -0.0299(4) 0.0285(13) Uani 1 1 d . . . H40 H 0.7977 1.1368 -0.0613 0.034 Uiso 1 1 calc R . . C41 C 0.8279(5) 1.0958(5) 0.0577(4) 0.0257(12) Uani 1 1 d . . . H41 H 0.7713 1.0609 0.0846 0.031 Uiso 1 1 calc R . . C42 C 0.9106(5) 0.5147(5) 0.7587(4) 0.0294(13) Uani 1 1 d . . . H42 H 0.9079 0.4858 0.8180 0.035 Uiso 1 1 calc R . . C43 C 0.9001(5) 0.6260(4) 0.7191(4) 0.0283(13) Uani 1 1 d . . . H43 H 0.8895 0.6702 0.7514 0.034 Uiso 1 1 calc R . . C44 C 0.9058(4) 0.6705(4) 0.6299(3) 0.0201(11) Uani 1 1 d . . . C45 C 0.9222(6) 0.6001(5) 0.5851(4) 0.0368(16) Uani 1 1 d . . . H45 H 0.9270 0.6263 0.5257 0.044 Uiso 1 1 calc R . . C46 C 0.9313(7) 0.4906(5) 0.6304(4) 0.0433(18) Uani 1 1 d . . . H46 H 0.9427 0.4443 0.5998 0.052 Uiso 1 1 calc R . . C47 C 0.8925(4) 0.7883(4) 0.5813(3) 0.0188(10) Uani 1 1 d . . . C48 C 0.8906(5) 0.8588(4) 0.6235(4) 0.0241(12) Uani 1 1 d . . . H48 H 0.8971 0.8303 0.6816 0.029 Uiso 1 1 calc R . . C49 C 0.8795(4) 0.9707(4) 0.5821(3) 0.0192(10) Uani 1 1 d . . . C50 C 0.8776(4) 1.0410(4) 0.6320(3) 0.0209(11) Uani 1 1 d . . . C51 C 0.8751(5) 1.0025(4) 0.7206(4) 0.0238(12) Uani 1 1 d . . . H51 H 0.8723 0.9302 0.7523 0.029 Uiso 1 1 calc R . . C52 C 0.8767(5) 1.0723(5) 0.7607(4) 0.0271(13) Uani 1 1 d . . . H52 H 0.8764 1.0451 0.8198 0.033 Uiso 1 1 calc R . . C53 C 0.8782(5) 1.2148(5) 0.6343(4) 0.0297(13) Uani 1 1 d . . . H53 H 0.8788 1.2878 0.6043 0.036 Uiso 1 1 calc R . . C54 C 0.8767(5) 1.1507(4) 0.5895(4) 0.0250(12) Uani 1 1 d . . . H54 H 0.8751 1.1805 0.5307 0.030 Uiso 1 1 calc R . . N6 N 0.8604(4) 0.9008(4) 0.3324(3) 0.0218(10) Uani 1 1 d . . . N7 N 0.8617(4) 1.1061(4) 0.3315(3) 0.0211(9) Uani 1 1 d . . . N8 N 0.9259(4) 1.1910(4) -0.0724(3) 0.0306(12) Uani 1 1 d . . . N9 N 0.9245(4) 0.4474(4) 0.7162(3) 0.0286(11) Uani 1 1 d . . . N10 N 0.8789(4) 1.1779(4) 0.7193(3) 0.0256(10) Uani 1 1 d . . . O3 O 0.8840(3) 0.8172(3) 0.5024(2) 0.0233(8) Uani 1 1 d . . . O4 O 0.8696(3) 1.0206(3) 0.5030(2) 0.0231(8) Uani 1 1 d . . . Cu2 Cu 0.86635(5) 0.96103(5) 0.41744(4) 0.01916(15) Uani 1 1 d . . . Ag2 Ag 0.94659(4) 0.26765(3) 0.78171(3) 0.03277(14) Uani 1 1 d . . . B1 B 0.2230(8) 0.5114(7) 0.5803(6) 0.048(2) Uani 1 1 d . . . F1 F 0.3275(5) 0.4868(6) 0.5640(5) 0.098(2) Uani 1 1 d . . . F2 F 0.1748(6) 0.4642(6) 0.5442(5) 0.094(2) Uani 1 1 d . . . F3 F 0.1912(6) 0.6212(4) 0.5517(4) 0.090(2) Uani 1 1 d . . . F4 F 0.1914(6) 0.4742(5) 0.6693(4) 0.0836(19) Uani 1 1 d . . . B2 B 0.6586(12) 0.9613(15) 0.9662(12) 0.095(10) Uani 0.530(5) 1 d PD A 1 F5 F 0.6362(9) 1.0641(10) 0.9554(9) 0.109 Uani 0.530(5) 1 d PD A 1 F6 F 0.5892(8) 0.8996(11) 1.0215(8) 0.109 Uani 0.530(5) 1 d PD A 1 F8 F 0.7572(7) 0.9144(11) 0.9806(8) 0.109 Uani 0.530(5) 1 d PD A 1 F7 F 0.6572(9) 0.9512(11) 0.8866(7) 0.109 Uani 0.530(5) 1 d PD A 1 B2A B 0.7761(14) 0.7029(16) 0.9148(12) 0.109 Uani 0.470(5) 1 d PD A 2 F5A F 0.7335(9) 0.7905(11) 0.8555(9) 0.109 Uani 0.470(5) 1 d PD A 2 F6A F 0.8769(8) 0.7067(12) 0.8961(9) 0.109 Uani 0.470(5) 1 d PD A 2 F7A F 0.7533(10) 0.6137(11) 0.9068(9) 0.109 Uani 0.470(5) 1 d PD A 2 F8A F 0.7429(10) 0.6879(13) 1.0002(8) 0.109 Uani 0.470(5) 1 d PD A 2 O5 O 0.1454(18) 0.3913(18) 0.8472(11) 0.121(8) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(3) 0.022(3) 0.023(3) -0.008(2) -0.005(2) -0.003(2) C2 0.032(3) 0.028(3) 0.023(3) -0.013(2) -0.002(2) -0.006(2) C3 0.031(3) 0.029(3) 0.022(3) -0.012(2) -0.004(2) -0.005(2) C4 0.026(3) 0.021(2) 0.016(2) -0.007(2) -0.003(2) -0.001(2) C5 0.024(3) 0.023(3) 0.017(2) -0.005(2) -0.002(2) -0.001(2) C6 0.030(3) 0.018(2) 0.017(2) -0.003(2) -0.005(2) -0.002(2) C7 0.038(3) 0.020(3) 0.022(3) -0.001(2) -0.007(2) -0.001(2) C8 0.035(3) 0.021(3) 0.029(3) -0.008(2) 0.000(2) -0.006(2) C9 0.036(3) 0.019(2) 0.025(3) -0.009(2) -0.004(2) -0.003(2) C10 0.033(3) 0.023(3) 0.016(2) -0.008(2) -0.004(2) -0.001(2) C11 0.033(3) 0.029(3) 0.022(3) -0.005(2) -0.006(2) -0.005(2) C12 0.043(4) 0.032(3) 0.020(3) -0.005(3) 0.000(3) -0.009(3) C13 0.042(4) 0.035(3) 0.026(3) -0.003(3) -0.013(3) -0.008(3) C14 0.042(4) 0.031(3) 0.019(3) -0.004(2) -0.007(2) -0.008(3) C15 0.052(4) 0.017(2) 0.023(3) -0.011(2) -0.003(3) -0.008(2) C16 0.042(3) 0.023(3) 0.014(2) -0.002(2) -0.002(2) -0.011(2) C17 0.022(3) 0.018(2) 0.019(2) -0.009(2) 0.001(2) -0.0052(19) C18 0.032(3) 0.023(3) 0.020(3) -0.008(2) -0.003(2) -0.005(2) C19 0.033(3) 0.021(3) 0.019(3) -0.006(2) -0.004(2) -0.003(2) C20 0.021(3) 0.020(2) 0.015(2) -0.005(2) 0.0004(19) -0.005(2) C21 0.029(3) 0.020(2) 0.017(2) -0.007(2) 0.001(2) -0.005(2) C22 0.027(3) 0.020(2) 0.018(2) -0.009(2) -0.003(2) -0.002(2) C23 0.029(3) 0.020(2) 0.020(3) -0.008(2) -0.005(2) -0.001(2) C24 0.034(3) 0.020(2) 0.021(3) -0.010(2) -0.004(2) -0.004(2) C25 0.039(3) 0.022(3) 0.021(3) -0.008(2) -0.005(2) -0.003(2) C26 0.098(6) 0.020(3) 0.033(4) -0.016(3) -0.031(4) 0.010(3) C27 0.081(5) 0.022(3) 0.029(3) -0.011(3) -0.025(3) 0.004(3) N1 0.024(2) 0.020(2) 0.017(2) -0.0053(18) -0.0018(17) -0.0029(18) N2 0.028(2) 0.017(2) 0.018(2) -0.0050(18) -0.0039(18) -0.0031(18) N3 0.051(3) 0.027(3) 0.019(2) -0.002(2) -0.008(2) -0.007(2) N4 0.035(3) 0.019(2) 0.023(2) -0.007(2) -0.003(2) -0.0036(19) N5 0.051(3) 0.023(2) 0.023(3) -0.012(2) -0.008(2) 0.000(2) O1 0.044(2) 0.0140(17) 0.0181(18) -0.0056(15) -0.0079(17) -0.0020(16) O2 0.049(3) 0.0163(18) 0.0176(19) -0.0049(16) -0.0091(18) -0.0014(17) Cu1 0.0308(4) 0.0155(3) 0.0148(3) -0.0047(2) -0.0046(3) -0.0022(3) Ag1 0.0831(4) 0.0195(2) 0.0185(2) -0.00444(18) -0.0110(2) -0.0153(2) C28 0.034(3) 0.020(3) 0.022(3) -0.004(2) -0.001(2) -0.007(2) C29 0.037(3) 0.020(3) 0.028(3) -0.014(2) -0.004(2) -0.001(2) C30 0.027(3) 0.025(3) 0.024(3) -0.012(2) -0.006(2) 0.000(2) C31 0.026(3) 0.020(2) 0.017(2) -0.010(2) -0.001(2) 0.001(2) C32 0.027(3) 0.023(3) 0.016(2) -0.009(2) -0.002(2) 0.001(2) C33 0.027(3) 0.018(2) 0.016(2) -0.004(2) -0.002(2) -0.004(2) C34 0.029(3) 0.018(2) 0.021(3) -0.005(2) -0.004(2) -0.002(2) C35 0.034(3) 0.019(3) 0.024(3) -0.003(2) -0.004(2) -0.004(2) C36 0.031(3) 0.018(2) 0.019(3) -0.008(2) -0.007(2) 0.000(2) C37 0.038(3) 0.023(3) 0.012(2) -0.010(2) -0.001(2) 0.003(2) C38 0.039(3) 0.036(3) 0.016(3) -0.011(2) -0.002(2) -0.006(3) C39 0.037(3) 0.039(3) 0.020(3) -0.009(3) 0.006(2) -0.014(3) C40 0.034(3) 0.031(3) 0.021(3) -0.014(3) -0.009(2) 0.003(2) C41 0.029(3) 0.028(3) 0.019(3) -0.011(2) -0.002(2) 0.000(2) C42 0.045(4) 0.019(3) 0.022(3) -0.004(2) -0.005(3) -0.005(2) C43 0.050(4) 0.016(2) 0.018(3) -0.005(2) -0.007(2) -0.003(2) C44 0.026(3) 0.015(2) 0.017(2) -0.004(2) -0.003(2) -0.003(2) C45 0.072(5) 0.018(3) 0.019(3) -0.005(2) -0.004(3) -0.010(3) C46 0.085(6) 0.018(3) 0.026(3) -0.008(3) -0.006(3) -0.007(3) C47 0.023(3) 0.015(2) 0.018(2) -0.006(2) -0.002(2) -0.0039(19) C48 0.033(3) 0.021(3) 0.016(2) -0.003(2) -0.006(2) -0.004(2) C49 0.021(3) 0.020(2) 0.018(2) -0.007(2) -0.0029(19) -0.0049(19) C50 0.025(3) 0.021(2) 0.019(2) -0.009(2) -0.003(2) -0.003(2) C51 0.035(3) 0.016(2) 0.020(3) -0.008(2) -0.003(2) -0.002(2) C52 0.037(3) 0.024(3) 0.023(3) -0.010(2) -0.008(2) -0.001(2) C53 0.044(4) 0.018(3) 0.028(3) -0.006(2) -0.009(3) -0.006(2) C54 0.039(3) 0.018(2) 0.017(2) -0.002(2) -0.007(2) -0.006(2) N6 0.027(2) 0.019(2) 0.017(2) -0.0065(18) -0.0003(18) 0.0003(18) N7 0.030(2) 0.016(2) 0.016(2) -0.0055(17) -0.0018(18) -0.0023(18) N8 0.044(3) 0.030(3) 0.016(2) -0.006(2) -0.001(2) -0.008(2) N9 0.044(3) 0.016(2) 0.023(2) -0.005(2) -0.004(2) -0.004(2) N10 0.034(3) 0.021(2) 0.023(2) -0.010(2) -0.007(2) -0.0024(19) O3 0.038(2) 0.0151(17) 0.0154(17) -0.0050(15) -0.0055(16) -0.0008(15) O4 0.037(2) 0.0149(17) 0.0165(18) -0.0036(15) -0.0038(16) -0.0044(15) Cu2 0.0287(4) 0.0141(3) 0.0132(3) -0.0046(2) -0.0022(2) -0.0019(2) Ag2 0.0650(4) 0.0172(2) 0.0169(2) -0.00442(17) -0.0071(2) -0.0098(2) B1 0.057(6) 0.040(4) 0.048(5) -0.009(4) -0.015(4) -0.015(4) F1 0.061(4) 0.090(5) 0.120(6) -0.020(4) -0.005(4) -0.004(3) F2 0.105(5) 0.121(6) 0.096(5) -0.067(5) -0.016(4) -0.042(4) F3 0.139(6) 0.040(3) 0.082(4) -0.009(3) -0.040(4) 0.002(3) F4 0.130(6) 0.073(4) 0.057(3) -0.020(3) -0.006(3) -0.043(4) B2 0.047(13) 0.15(3) 0.13(3) -0.10(2) -0.009(14) -0.013(15) F5 0.055 0.121 0.103 0.000 0.001 0.000 F6 0.055 0.121 0.103 0.000 0.001 0.000 F8 0.055 0.121 0.103 0.000 0.001 0.000 F7 0.055 0.121 0.103 0.000 0.001 0.000 B2A 0.055 0.121 0.103 0.000 0.001 0.000 F5A 0.055 0.121 0.103 0.000 0.001 0.000 F6A 0.055 0.121 0.103 0.000 0.001 0.000 F7A 0.055 0.121 0.103 0.000 0.001 0.000 F8A 0.055 0.121 0.103 0.000 0.001 0.000 O5 0.168(19) 0.153(18) 0.069(10) -0.026(11) 0.013(11) -0.123(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.337(7) . ? C1 C2 1.409(8) . ? C1 H1 0.9300 . ? C2 C3 1.371(8) . ? C2 H2 0.9300 . ? C3 C4 1.427(8) . ? C3 H3 0.9300 . ? C4 C5 1.390(8) . ? C4 N1 1.403(7) . ? C5 C6 1.401(9) . ? C5 C10 1.487(7) . ? C6 N2 1.385(7) . ? C6 C7 1.433(8) . ? C7 C8 1.358(9) . ? C7 H7 0.9300 . ? C8 C9 1.425(8) . ? C8 H8 0.9300 . ? C9 N2 1.335(8) . ? C9 H9 0.9300 . ? C10 C14 1.379(9) . ? C10 C11 1.404(8) . ? C11 C12 1.383(8) . ? C11 H11 0.9300 . ? C12 N3 1.340(9) . ? C12 H12 0.9300 . ? C13 N3 1.331(9) . ? C13 C14 1.402(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N4 1.353(8) . ? C15 C16 1.377(8) . ? C15 H15 0.9300 . ? C16 C17 1.387(8) . ? C16 H16 0.9300 . ? C17 C18 1.375(8) . ? C17 C20 1.500(7) . ? C18 C19 1.393(8) . ? C18 H18 0.9300 . ? C19 N4 1.323(8) . ? C19 H19 0.9300 . ? C20 O1 1.284(6) . ? C20 C21 1.395(8) . ? C21 C22 1.403(7) . ? C21 H21 0.9300 . ? C22 O2 1.262(7) . ? C22 C23 1.493(8) . ? C23 C24 1.384(8) . ? C23 C27 1.388(8) . ? C24 C25 1.389(9) . ? C24 H24 0.9300 . ? C25 N5 1.331(7) . ? C25 H25 0.9300 . ? C26 N5 1.339(8) . ? C26 C27 1.364(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? N1 Cu1 1.935(5) . ? N2 Cu1 1.954(4) . ? N3 Ag1 2.267(5) 1_564 ? N4 Ag1 2.266(5) . ? N5 Ag1 2.251(5) 1_565 ? O1 Cu1 1.959(4) . ? O2 Cu1 1.932(4) . ? Ag1 N5 2.251(5) 1_545 ? Ag1 N3 2.267(5) 1_546 ? C28 N6 1.350(7) . ? C28 C29 1.383(9) . ? C28 H28 0.9300 . ? C29 C30 1.386(8) . ? C29 Ag2 2.640(6) 2_766 ? C29 H29 0.9300 . ? C30 C31 1.418(8) . ? C30 H30 0.9300 . ? C31 N6 1.389(7) . ? C31 C32 1.406(8) . ? C32 C33 1.401(8) . ? C32 C37 1.503(7) . ? C33 N7 1.407(7) . ? C33 C34 1.427(7) . ? C34 C35 1.355(9) . ? C34 H34 0.9300 . ? C35 C36 1.400(7) . ? C35 H35 0.9300 . ? C36 N7 1.335(7) . ? C36 H36 0.9300 . ? C37 C38 1.383(9) . ? C37 C41 1.391(9) . ? C38 C39 1.388(8) . ? C38 H38 0.9300 . ? C39 N8 1.324(9) . ? C39 H39 0.9300 . ? C40 N8 1.342(8) . ? C40 C41 1.371(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 N9 1.332(8) . ? C42 C43 1.390(8) . ? C42 H42 0.9300 . ? C43 C44 1.399(8) . ? C43 H43 0.9300 . ? C44 C45 1.392(9) . ? C44 C47 1.485(7) . ? C45 C46 1.383(8) . ? C45 H45 0.9300 . ? C46 N9 1.344(8) . ? C46 H46 0.9300 . ? C47 O3 1.269(6) . ? C47 C48 1.397(8) . ? C48 C49 1.399(7) . ? C48 H48 0.9300 . ? C49 O4 1.277(6) . ? C49 C50 1.498(8) . ? C50 C54 1.388(7) . ? C50 C51 1.392(8) . ? C51 C52 1.373(9) . ? C51 H51 0.9300 . ? C52 N10 1.343(7) . ? C52 H52 0.9300 . ? C53 N10 1.341(8) . ? C53 C54 1.367(9) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? N6 Cu2 1.941(5) . ? N7 Cu2 1.956(4) . ? N8 Ag2 2.284(5) 1_564 ? N9 Ag2 2.245(5) . ? N10 Ag2 2.314(5) 1_565 ? O3 Cu2 1.937(4) . ? O4 Cu2 1.932(4) . ? Ag2 N8 2.284(5) 1_546 ? Ag2 N10 2.314(5) 1_545 ? Ag2 C29 2.640(6) 2_766 ? B1 F1 1.348(12) . ? B1 F2 1.368(11) . ? B1 F3 1.373(11) . ? B1 F4 1.407(11) . ? B2 F5 1.309(16) . ? B2 F8 1.346(15) . ? B2 F6 1.361(16) . ? B2 F7 1.418(16) . ? B2A F6A 1.323(16) . ? B2A F5A 1.329(16) . ? B2A F7A 1.380(17) . ? B2A F8A 1.380(17) . ? 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 C1 C2 112.6(5) . . ? N1 C1 H1 123.7 . . ? C2 C1 H1 123.7 . . ? C3 C2 C1 105.6(5) . . ? C3 C2 H2 127.2 . . ? C1 C2 H2 127.2 . . ? C2 C3 C4 107.6(5) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? C5 C4 N1 123.0(5) . . ? C5 C4 C3 128.5(5) . . ? N1 C4 C3 108.4(5) . . ? C4 C5 C6 125.9(5) . . ? C4 C5 C10 116.9(5) . . ? C6 C5 C10 117.2(5) . . ? N2 C6 C5 123.6(5) . . ? N2 C6 C7 108.2(5) . . ? C5 C6 C7 128.2(5) . . ? C8 C7 C6 107.6(5) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 106.0(5) . . ? C7 C8 H8 127.0 . . ? C9 C8 H8 127.0 . . ? N2 C9 C8 111.2(5) . . ? N2 C9 H9 124.4 . . ? C8 C9 H9 124.4 . . ? C14 C10 C11 117.2(5) . . ? C14 C10 C5 122.1(5) . . ? C11 C10 C5 120.7(5) . . ? C12 C11 C10 119.3(6) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? N3 C12 C11 123.4(6) . . ? N3 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? N3 C13 C14 122.9(6) . . ? N3 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C10 C14 C13 119.7(6) . . ? C10 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? N4 C15 C16 122.8(6) . . ? N4 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C17 119.8(5) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 117.4(5) . . ? C18 C17 C20 122.6(5) . . ? C16 C17 C20 120.0(5) . . ? C17 C18 C19 119.5(6) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? N4 C19 C18 123.3(5) . . ? N4 C19 H19 118.3 . . ? C18 C19 H19 118.3 . . ? O1 C20 C21 124.7(5) . . ? O1 C20 C17 116.2(5) . . ? C21 C20 C17 119.1(5) . . ? C20 C21 C22 123.0(5) . . ? C20 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? O2 C22 C21 124.6(5) . . ? O2 C22 C23 115.7(5) . . ? C21 C22 C23 119.7(5) . . ? C24 C23 C27 117.5(6) . . ? C24 C23 C22 123.3(5) . . ? C27 C23 C22 119.2(5) . . ? C23 C24 C25 118.6(5) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? N5 C25 C24 123.4(6) . . ? N5 C25 H25 118.3 . . ? C24 C25 H25 118.3 . . ? N5 C26 C27 122.7(6) . . ? N5 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C26 C27 C23 120.2(6) . . ? C26 C27 H27 119.9 . . ? C23 C27 H27 119.9 . . ? C1 N1 C4 105.7(5) . . ? C1 N1 Cu1 126.4(4) . . ? C4 N1 Cu1 127.9(4) . . ? C9 N2 C6 106.9(5) . . ? C9 N2 Cu1 125.5(4) . . ? C6 N2 Cu1 127.4(4) . . ? C13 N3 C12 117.5(5) . . ? C13 N3 Ag1 119.3(4) . 1_564 ? C12 N3 Ag1 123.1(4) . 1_564 ? C19 N4 C15 117.1(5) . . ? C19 N4 Ag1 117.6(4) . . ? C15 N4 Ag1 122.0(4) . . ? C25 N5 C26 117.5(6) . . ? C25 N5 Ag1 123.4(4) . 1_565 ? C26 N5 Ag1 118.5(4) . 1_565 ? C20 O1 Cu1 127.7(4) . . ? C22 O2 Cu1 129.6(4) . . ? O2 Cu1 N1 171.2(2) . . ? O2 Cu1 N2 88.95(18) . . ? N1 Cu1 N2 91.86(19) . . ? O2 Cu1 O1 89.23(16) . . ? N1 Cu1 O1 90.68(18) . . ? N2 Cu1 O1 174.83(19) . . ? N5 Ag1 N4 120.38(19) 1_545 . ? N5 Ag1 N3 114.46(19) 1_545 1_546 ? N4 Ag1 N3 118.1(2) . 1_546 ? N6 C28 C29 111.5(5) . . ? N6 C28 H28 124.3 . . ? C29 C28 H28 124.3 . . ? C28 C29 C30 107.0(5) . . ? C28 C29 Ag2 105.2(4) . 2_766 ? C30 C29 Ag2 81.0(4) . 2_766 ? C28 C29 H29 126.5 . . ? C30 C29 H29 126.5 . . ? Ag2 C29 H29 84.9 2_766 . ? C29 C30 C31 106.4(5) . . ? C29 C30 H30 126.8 . . ? C31 C30 H30 126.8 . . ? N6 C31 C32 123.2(5) . . ? N6 C31 C30 108.9(5) . . ? C32 C31 C30 127.9(5) . . ? C33 C32 C31 125.8(5) . . ? C33 C32 C37 115.8(5) . . ? C31 C32 C37 118.3(5) . . ? C32 C33 N7 123.0(5) . . ? C32 C33 C34 129.1(5) . . ? N7 C33 C34 107.9(5) . . ? C35 C34 C33 107.6(5) . . ? C35 C34 H34 126.2 . . ? C33 C34 H34 126.2 . . ? C34 C35 C36 106.5(5) . . ? C34 C35 H35 126.8 . . ? C36 C35 H35 126.8 . . ? N7 C36 C35 112.3(5) . . ? N7 C36 H36 123.9 . . ? C35 C36 H36 123.9 . . ? C38 C37 C41 117.6(5) . . ? C38 C37 C32 121.2(5) . . ? C41 C37 C32 121.2(5) . . ? C37 C38 C39 119.4(6) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? N8 C39 C38 122.9(6) . . ? N8 C39 H39 118.6 . . ? C38 C39 H39 118.6 . . ? N8 C40 C41 123.3(6) . . ? N8 C40 H40 118.4 . . ? C41 C40 H40 118.4 . . ? C40 C41 C37 119.1(6) . . ? C40 C41 H41 120.4 . . ? C37 C41 H41 120.4 . . ? N9 C42 C43 123.4(6) . . ? N9 C42 H42 118.3 . . ? C43 C42 H42 118.3 . . ? C42 C43 C44 118.9(6) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C45 C44 C43 117.8(5) . . ? C45 C44 C47 118.8(5) . . ? C43 C44 C47 123.4(5) . . ? C46 C45 C44 119.0(6) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? N9 C46 C45 123.6(6) . . ? N9 C46 H46 118.2 . . ? C45 C46 H46 118.2 . . ? O3 C47 C48 124.6(5) . . ? O3 C47 C44 116.1(5) . . ? C48 C47 C44 119.3(5) . . ? C47 C48 C49 122.8(5) . . ? C47 C48 H48 118.6 . . ? C49 C48 H48 118.6 . . ? O4 C49 C48 125.2(5) . . ? O4 C49 C50 115.2(5) . . ? C48 C49 C50 119.6(5) . . ? C54 C50 C51 117.2(5) . . ? C54 C50 C49 119.6(5) . . ? C51 C50 C49 123.3(5) . . ? C52 C51 C50 119.2(5) . . ? C52 C51 H51 120.4 . . ? C50 C51 H51 120.4 . . ? N10 C52 C51 123.6(5) . . ? N10 C52 H52 118.2 . . ? C51 C52 H52 118.2 . . ? N10 C53 C54 123.4(5) . . ? N10 C53 H53 118.3 . . ? C54 C53 H53 118.3 . . ? C53 C54 C50 119.9(5) . . ? C53 C54 H54 120.1 . . ? C50 C54 H54 120.1 . . ? C28 N6 C31 106.2(5) . . ? C28 N6 Cu2 125.6(4) . . ? C31 N6 Cu2 128.1(4) . . ? C36 N7 C33 105.6(4) . . ? C36 N7 Cu2 126.8(4) . . ? C33 N7 Cu2 126.9(4) . . ? C39 N8 C40 117.7(5) . . ? C39 N8 Ag2 121.1(4) . 1_564 ? C40 N8 Ag2 121.2(4) . 1_564 ? C42 N9 C46 117.4(5) . . ? C42 N9 Ag2 122.5(4) . . ? C46 N9 Ag2 120.1(4) . . ? C53 N10 C52 116.6(5) . . ? C53 N10 Ag2 120.5(4) . 1_565 ? C52 N10 Ag2 118.4(4) . 1_565 ? C47 O3 Cu2 129.1(4) . . ? C49 O4 Cu2 128.3(4) . . ? O4 Cu2 O3 90.00(16) . . ? O4 Cu2 N6 178.93(19) . . ? O3 Cu2 N6 89.75(18) . . ? O4 Cu2 N7 88.65(18) . . ? O3 Cu2 N7 174.89(19) . . ? N6 Cu2 N7 91.69(19) . . ? N9 Ag2 N8 121.29(19) . 1_546 ? N9 Ag2 N10 114.76(18) . 1_545 ? N8 Ag2 N10 111.72(19) 1_546 1_545 ? N9 Ag2 C29 98.53(19) . 2_766 ? N8 Ag2 C29 107.66(19) 1_546 2_766 ? N10 Ag2 C29 98.96(19) 1_545 2_766 ? F1 B1 F2 111.1(9) . . ? F1 B1 F3 110.3(8) . . ? F2 B1 F3 110.7(8) . . ? F1 B1 F4 109.9(8) . . ? F2 B1 F4 108.1(7) . . ? F3 B1 F4 106.6(8) . . ? F5 B2 F8 114.9(14) . . ? F5 B2 F6 116.0(14) . . ? F8 B2 F6 111.3(14) . . ? F5 B2 F7 107.7(15) . . ? F8 B2 F7 101.1(13) . . ? F6 B2 F7 104.0(13) . . ? F6A B2A F5A 103.8(13) . . ? F6A B2A F7A 112.3(16) . . ? F5A B2A F7A 108.4(15) . . ? F6A B2A F8A 110.7(15) . . ? F5A B2A F8A 119.4(16) . . ? F7A B2A F8A 102.6(13) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 29.41 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 2.014 _refine_diff_density_min -2.258 _refine_diff_density_rms 0.174 #===END ###Material relevant to compound 6 at 173K ## data_compound6 _database_code_depnum_ccdc_archive 'CCDC 868788' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H19 Ag Cu F3 N5 O5 S' _chemical_formula_sum 'C28 H19 Ag Cu F3 N5 O5 S' _chemical_formula_weight 765.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.4564(4) _cell_length_b 29.9025(15) _cell_length_c 11.4789(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.4240(10) _cell_angle_gamma 90.00 _cell_volume 2894.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6210 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.40 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 1.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8603 _exptl_absorpt_correction_T_max 0.9406 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18166 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.01 _reflns_number_total 6158 _reflns_number_gt 4910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+14.9578P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0130(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6158 _refine_ls_number_parameters 431 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2002 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.136 _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 C1 C 0.5716(8) 0.0711(2) 0.6908(6) 0.0314(14) Uani 1 1 d . . . H1 H 0.5831 0.0436 0.7286 0.038 Uiso 1 1 calc R . . C2 C 0.6510(9) 0.1109(2) 0.7296(6) 0.0345(15) Uani 1 1 d . . . H2 H 0.7213 0.1143 0.7953 0.041 Uiso 1 1 calc R . . C3 C 0.6021(8) 0.1435(2) 0.6492(6) 0.0300(14) Uani 1 1 d . . . H3 H 0.6344 0.1732 0.6503 0.036 Uiso 1 1 calc R . . C4 C 0.4935(8) 0.1231(2) 0.5649(5) 0.0266(13) Uani 1 1 d . . . C5 C 0.4096(9) 0.1439(2) 0.4686(5) 0.0292(13) Uani 1 1 d . . . C6 C 0.3031(9) 0.1229(2) 0.3888(6) 0.0322(14) Uani 1 1 d . . . C7 C 0.2129(10) 0.1432(2) 0.2913(6) 0.0391(16) Uani 1 1 d . . . H7 H 0.2139 0.1732 0.2696 0.047 Uiso 1 1 calc R . . C8 C 0.1258(10) 0.1098(3) 0.2373(6) 0.0416(18) Uani 1 1 d . . . H8 H 0.0559 0.1125 0.1711 0.050 Uiso 1 1 calc R . . C9 C 0.1617(9) 0.0704(2) 0.3006(5) 0.0343(15) Uani 1 1 d . . . H9 H 0.1178 0.0426 0.2814 0.041 Uiso 1 1 calc R . . C10 C 0.4380(9) 0.1927(2) 0.4491(6) 0.0338(15) Uani 1 1 d . . . C11 C 0.3853(10) 0.2246(2) 0.5249(6) 0.0385(16) Uani 1 1 d . . . H11 H 0.3399 0.2160 0.5927 0.046 Uiso 1 1 calc R . . C12 C 0.4015(10) 0.2697(2) 0.4978(7) 0.0411(17) Uani 1 1 d . . . H12 H 0.3650 0.2907 0.5491 0.049 Uiso 1 1 calc R . . C13 C 0.5249(14) 0.2532(3) 0.3334(7) 0.059(3) Uani 1 1 d . . . H13 H 0.5770 0.2624 0.2691 0.071 Uiso 1 1 calc R . . C14 C 0.5110(13) 0.2079(2) 0.3539(7) 0.053(2) Uani 1 1 d . . . H14 H 0.5514 0.1875 0.3028 0.064 Uiso 1 1 calc R . . C16 C 0.6144(9) 0.1273(2) 1.0922(6) 0.0354(15) Uani 1 1 d . . . H16 H 0.6601 0.1536 1.0676 0.042 Uiso 1 1 calc R . . C17 C 0.6719(8) 0.1088(2) 1.1983(6) 0.0323(14) Uani 1 1 d . . . H17 H 0.7551 0.1223 1.2427 0.039 Uiso 1 1 calc R . . C18 C 0.6043(8) 0.0701(2) 1.2372(5) 0.0282(13) Uani 1 1 d . . . C19 C 0.4806(9) 0.0518(3) 1.1681(6) 0.0381(16) Uani 1 1 d . . . H19 H 0.4312 0.0259 1.1919 0.046 Uiso 1 1 calc R . . C20 C 0.4298(10) 0.0719(3) 1.0629(6) 0.045(2) Uani 1 1 d . . . H20 H 0.3460 0.0590 1.0176 0.054 Uiso 1 1 calc R . . C21 C 0.3384(8) -0.0472(2) 0.6506(5) 0.0261(12) Uani 1 1 d . . . C22 C 0.2123(8) -0.0660(2) 0.5806(5) 0.0278(13) Uani 1 1 d . . . H22 H 0.1685 -0.0927 0.6049 0.033 Uiso 1 1 calc R . . C23 C 0.1491(8) -0.0469(2) 0.4765(5) 0.0274(13) Uani 1 1 d . . . C24 C -0.0253(8) 0.0714(2) 0.5977(5) 0.0282(13) Uani 1 1 d . . . C25 C 0.0708(8) 0.0476(2) 0.6809(5) 0.0296(13) Uani 1 1 d . . . H25 H 0.0590 0.0168 0.6884 0.036 Uiso 1 1 calc R . . C26 C 0.1824(8) 0.0701(2) 0.7511(5) 0.0294(13) Uani 1 1 d . . . H26 H 0.2468 0.0537 0.8047 0.035 Uiso 1 1 calc R . . C27 C 0.1103(9) 0.1374(2) 0.6682(6) 0.0329(14) Uani 1 1 d . . . H27 H 0.1225 0.1683 0.6643 0.040 Uiso 1 1 calc R . . C28 C -0.0027(8) 0.1175(2) 0.5932(6) 0.0316(14) Uani 1 1 d . . . H28 H -0.0640 0.1347 0.5395 0.038 Uiso 1 1 calc R . . N1 N 0.4781(7) 0.07811(17) 0.5930(4) 0.0277(11) Uani 1 1 d . . . N2 N 0.2660(7) 0.07760(18) 0.3914(4) 0.0290(11) Uani 1 1 d . . . N3 N 0.4664(9) 0.28454(19) 0.4024(5) 0.0426(15) Uani 1 1 d . . . N4 N 0.4963(7) 0.1090(2) 1.0240(5) 0.0349(13) Uani 1 1 d . . . N5 N 0.2041(7) 0.11462(18) 0.7470(4) 0.0281(11) Uani 1 1 d . . . O1 O 0.4106(6) -0.01113(14) 0.6263(4) 0.0302(10) Uani 1 1 d . . . O2 O 0.1878(6) -0.00859(15) 0.4386(4) 0.0306(10) Uani 1 1 d . . . Cu1 Cu 0.33870(10) 0.03401(2) 0.51086(6) 0.0264(2) Uani 1 1 d . . . Ag1 Ag 0.42483(7) 0.142951(17) 0.84624(4) 0.0386(2) Uani 1 1 d . . . C29 C -0.047(2) 0.2831(6) 0.4929(15) 0.0598(12) Uani 0.50 1 d PD . . O3 O 0.1010(15) 0.2556(4) 0.6725(13) 0.058(3) Uani 0.50 1 d P . . O4 O -0.1536(18) 0.2271(6) 0.606(3) 0.124(9) Uani 0.50 1 d P . . O5 O -0.1421(18) 0.2990(5) 0.6832(14) 0.072(4) Uani 0.50 1 d P . . F1 F 0.021(2) 0.3158(8) 0.4715(18) 0.141(9) Uani 0.50 1 d P . . F2 F 0.029(2) 0.2597(11) 0.4163(15) 0.195(14) Uani 0.50 1 d P . . F3 F -0.175(2) 0.2963(8) 0.4260(15) 0.144(9) Uani 0.50 1 d P . . S1 S -0.0637(6) 0.26351(15) 0.6276(5) 0.0598(12) Uani 0.50 1 d PD . . C30 C -0.0779(4) 0.02542(11) 0.9981(2) 0.0405(7) Uani 0.50 1 d PD A -1 O6 O 0.0290(16) 0.0615(5) 0.9854(17) 0.043(2) Uani 0.50 1 d PD A -1 O7 O -0.1685(15) 0.0182(5) 1.0912(11) 0.043(2) Uani 0.50 1 d PD A -1 O8 O -0.1652(18) 0.0142(6) 0.8897(11) 0.043(2) Uani 0.50 1 d PD A -1 F4 F -0.0088(14) 0.0620(4) 0.9829(15) 0.045(2) Uani 0.50 1 d PD A -1 F5 F -0.1206(13) 0.0239(4) 1.1096(9) 0.045(2) Uani 0.50 1 d PD A -1 F6 F -0.1937(14) 0.0145(5) 0.9159(9) 0.045(2) Uani 0.50 1 d PD A -1 S2 S -0.0779(4) 0.02542(11) 0.9981(2) 0.0405(7) Uani 0.50 1 d PD A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(4) 0.026(3) 0.030(3) -0.003(2) 0.000(3) 0.000(3) C2 0.040(4) 0.029(3) 0.033(3) -0.005(3) -0.006(3) -0.004(3) C3 0.033(4) 0.025(3) 0.031(3) -0.002(2) 0.000(3) -0.002(2) C4 0.029(3) 0.025(3) 0.026(3) -0.002(2) 0.000(2) 0.000(2) C5 0.040(4) 0.024(3) 0.024(3) 0.000(2) 0.002(3) 0.003(3) C6 0.041(4) 0.027(3) 0.028(3) 0.000(2) 0.000(3) -0.001(3) C7 0.046(4) 0.033(4) 0.037(3) 0.002(3) -0.006(3) -0.001(3) C8 0.050(5) 0.039(4) 0.033(3) 0.002(3) -0.012(3) 0.000(3) C9 0.039(4) 0.039(4) 0.024(3) 0.005(3) -0.003(3) -0.003(3) C10 0.047(4) 0.024(3) 0.030(3) -0.002(2) -0.005(3) 0.000(3) C11 0.052(5) 0.023(3) 0.041(4) -0.002(3) 0.007(3) 0.000(3) C12 0.050(5) 0.027(3) 0.047(4) -0.003(3) 0.005(3) -0.001(3) C13 0.123(9) 0.028(4) 0.029(3) 0.000(3) 0.017(4) 0.000(4) C14 0.104(7) 0.024(3) 0.034(4) -0.002(3) 0.020(4) 0.005(4) C16 0.045(4) 0.030(3) 0.030(3) 0.006(3) -0.004(3) -0.007(3) C17 0.030(4) 0.036(3) 0.030(3) 0.005(3) -0.004(3) -0.006(3) C18 0.029(3) 0.032(3) 0.023(3) 0.002(2) -0.002(2) 0.004(3) C19 0.040(4) 0.041(4) 0.031(3) 0.008(3) -0.006(3) -0.011(3) C20 0.046(5) 0.049(4) 0.037(4) 0.013(3) -0.014(3) -0.025(4) C21 0.029(3) 0.026(3) 0.023(3) 0.000(2) -0.001(2) -0.002(2) C22 0.028(3) 0.026(3) 0.029(3) -0.002(2) -0.003(2) -0.005(2) C23 0.028(3) 0.025(3) 0.029(3) -0.003(2) 0.000(2) -0.002(2) C24 0.029(3) 0.033(3) 0.022(3) -0.001(2) -0.001(2) 0.000(3) C25 0.032(4) 0.031(3) 0.026(3) 0.000(2) 0.001(3) -0.003(3) C26 0.033(4) 0.027(3) 0.028(3) 0.005(2) -0.002(3) -0.004(3) C27 0.036(4) 0.027(3) 0.035(3) 0.001(2) -0.003(3) -0.003(3) C28 0.028(4) 0.031(3) 0.034(3) -0.002(3) -0.006(3) -0.002(3) N1 0.031(3) 0.025(2) 0.027(2) 0.0011(19) -0.002(2) -0.001(2) N2 0.031(3) 0.030(3) 0.025(2) -0.003(2) -0.001(2) -0.003(2) N3 0.068(5) 0.023(3) 0.035(3) 0.003(2) -0.005(3) -0.002(3) N4 0.035(3) 0.036(3) 0.032(3) 0.006(2) -0.008(2) -0.006(2) N5 0.030(3) 0.029(3) 0.024(2) -0.006(2) -0.003(2) -0.006(2) O1 0.033(3) 0.025(2) 0.030(2) 0.0023(17) -0.0076(19) -0.0049(18) O2 0.035(3) 0.028(2) 0.028(2) 0.0015(17) -0.0039(19) 0.0002(19) Cu1 0.0319(5) 0.0229(4) 0.0235(4) -0.0002(3) -0.0038(3) -0.0012(3) Ag1 0.0537(4) 0.0283(3) 0.0313(3) -0.00094(19) -0.0136(2) -0.0061(2) C29 0.046(2) 0.036(2) 0.099(4) -0.007(2) 0.017(2) 0.0022(17) O3 0.048(7) 0.047(7) 0.080(9) -0.013(6) 0.014(6) 0.003(5) O4 0.038(9) 0.071(11) 0.26(3) -0.036(14) -0.023(12) -0.008(7) O5 0.067(9) 0.064(9) 0.090(10) 0.009(8) 0.022(8) 0.035(7) F1 0.121(14) 0.176(19) 0.137(15) 0.085(14) 0.085(12) 0.062(13) F2 0.083(11) 0.42(4) 0.082(11) -0.096(18) -0.025(9) 0.107(18) F3 0.099(12) 0.24(2) 0.089(11) -0.045(13) -0.021(9) 0.087(14) S1 0.046(2) 0.036(2) 0.099(4) -0.007(2) 0.017(2) 0.0022(17) C30 0.0437(18) 0.0469(16) 0.0308(13) -0.0006(11) 0.0020(12) -0.0091(13) O6 0.030(5) 0.056(5) 0.044(4) -0.010(3) 0.012(3) -0.005(3) O7 0.030(5) 0.056(5) 0.044(4) -0.010(3) 0.012(3) -0.005(3) O8 0.030(5) 0.056(5) 0.044(4) -0.010(3) 0.012(3) -0.005(3) F4 0.036(4) 0.052(4) 0.047(3) -0.001(3) -0.003(3) -0.001(3) F5 0.036(4) 0.052(4) 0.047(3) -0.001(3) -0.003(3) -0.001(3) F6 0.036(4) 0.052(4) 0.047(3) -0.001(3) -0.003(3) -0.001(3) S2 0.0437(18) 0.0469(16) 0.0308(13) -0.0006(11) 0.0020(12) -0.0091(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.340(8) . ? C1 C2 1.422(9) . ? C1 H1 0.9300 . ? C2 C3 1.383(9) . ? C2 Ag1 2.601(8) . ? C2 H2 0.9300 . ? C3 C4 1.419(8) . ? C3 H3 0.9300 . ? C4 N1 1.392(8) . ? C4 C5 1.411(8) . ? C5 C6 1.385(9) . ? C5 C10 1.500(9) . ? C6 N2 1.390(8) . ? C6 C7 1.440(9) . ? C7 C8 1.363(10) . ? C7 H7 0.9300 . ? C8 C9 1.406(10) . ? C8 H8 0.9300 . ? C9 N2 1.330(8) . ? C9 H9 0.9300 . ? C10 C14 1.373(11) . ? C10 C11 1.387(10) . ? C11 C12 1.393(10) . ? C11 H11 0.9300 . ? C12 N3 1.339(10) . ? C12 H12 0.9300 . ? C13 N3 1.346(10) . ? C13 C14 1.381(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C16 N4 1.337(9) . ? C16 C17 1.392(9) . ? C16 H16 0.9300 . ? C17 C18 1.379(9) . ? C17 H17 0.9300 . ? C18 C19 1.376(9) . ? C18 C21 1.505(8) 3_657 ? C19 C20 1.388(9) . ? C19 H19 0.9300 . ? C20 N4 1.336(9) . ? C20 H20 0.9300 . ? C21 O1 1.281(8) . ? C21 C22 1.403(8) . ? C21 C18 1.505(8) 3_657 ? C22 C23 1.394(8) . ? C22 H22 0.9300 . ? C23 O2 1.277(8) . ? C23 C24 1.490(8) 3_556 ? C24 C28 1.393(9) . ? C24 C25 1.400(9) . ? C24 C23 1.490(8) 3_556 ? C25 C26 1.370(9) . ? C25 H25 0.9300 . ? C26 N5 1.345(8) . ? C26 H26 0.9300 . ? C27 N5 1.342(8) . ? C27 C28 1.373(9) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N1 Cu1 1.961(5) . ? N2 Cu1 1.956(5) . ? N3 Ag1 2.282(6) 4_565 ? N4 Ag1 2.317(5) . ? N5 Ag1 2.274(5) . ? O1 Cu1 1.956(4) . ? O2 Cu1 1.943(5) . ? Ag1 N3 2.282(6) 4_566 ? C29 F1 1.17(3) . ? C29 F2 1.33(2) . ? C29 F3 1.34(2) . ? C29 S1 1.669(16) . ? O3 S1 1.467(14) . ? O4 S1 1.340(16) . ? O5 S1 1.427(14) . ? C30 F4 1.257(12) . ? C30 F6 1.346(11) . ? C30 F5 1.358(11) . ? 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 C1 C2 111.4(6) . . ? N1 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C3 C2 C1 105.8(6) . . ? C3 C2 Ag1 83.7(4) . . ? C1 C2 Ag1 97.0(5) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? Ag1 C2 H2 89.5 . . ? C2 C3 C4 107.3(6) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 123.8(5) . . ? N1 C4 C3 108.9(5) . . ? C5 C4 C3 127.3(6) . . ? C6 C5 C4 125.5(6) . . ? C6 C5 C10 116.6(6) . . ? C4 C5 C10 118.0(6) . . ? C5 C6 N2 124.4(6) . . ? C5 C6 C7 126.9(6) . . ? N2 C6 C7 108.7(6) . . ? C8 C7 C6 106.2(6) . . ? C8 C7 H7 126.9 . . ? C6 C7 H7 126.9 . . ? C7 C8 C9 107.0(6) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? N2 C9 C8 111.8(6) . . ? N2 C9 H9 124.1 . . ? C8 C9 H9 124.1 . . ? C14 C10 C11 117.3(6) . . ? C14 C10 C5 121.8(6) . . ? C11 C10 C5 120.8(6) . . ? C10 C11 C12 118.8(7) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N3 C12 C11 123.9(7) . . ? N3 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? N3 C13 C14 122.9(8) . . ? N3 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C10 C14 C13 120.6(7) . . ? C10 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? N4 C16 C17 123.0(6) . . ? N4 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 119.4(6) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 117.6(6) . . ? C19 C18 C21 119.5(6) . 3_657 ? C17 C18 C21 122.9(6) . 3_657 ? C18 C19 C20 119.9(7) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? N4 C20 C19 122.8(6) . . ? N4 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? O1 C21 C22 124.6(5) . . ? O1 C21 C18 116.2(5) . 3_657 ? C22 C21 C18 119.3(6) . 3_657 ? C23 C22 C21 123.4(6) . . ? C23 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? O2 C23 C22 124.6(6) . . ? O2 C23 C24 115.7(5) . 3_556 ? C22 C23 C24 119.6(6) . 3_556 ? C28 C24 C25 117.0(6) . . ? C28 C24 C23 123.9(6) . 3_556 ? C25 C24 C23 119.0(6) . 3_556 ? C26 C25 C24 119.3(6) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? N5 C26 C25 123.7(6) . . ? N5 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? N5 C27 C28 123.3(6) . . ? N5 C27 H27 118.4 . . ? C28 C27 H27 118.4 . . ? C27 C28 C24 119.8(6) . . ? C27 C28 H28 120.1 . . ? C24 C28 H28 120.1 . . ? C1 N1 C4 106.6(5) . . ? C1 N1 Cu1 126.2(4) . . ? C4 N1 Cu1 127.1(4) . . ? C9 N2 C6 106.2(6) . . ? C9 N2 Cu1 126.5(5) . . ? C6 N2 Cu1 127.2(4) . . ? C12 N3 C13 116.3(6) . . ? C12 N3 Ag1 118.9(5) . 4_565 ? C13 N3 Ag1 123.5(5) . 4_565 ? C20 N4 C16 117.3(6) . . ? C20 N4 Ag1 124.7(4) . . ? C16 N4 Ag1 117.9(4) . . ? C27 N5 C26 116.8(5) . . ? C27 N5 Ag1 124.6(4) . . ? C26 N5 Ag1 117.4(4) . . ? C21 O1 Cu1 126.9(4) . . ? C23 O2 Cu1 128.3(4) . . ? O2 Cu1 O1 89.78(18) . . ? O2 Cu1 N2 88.7(2) . . ? O1 Cu1 N2 178.1(2) . . ? O2 Cu1 N1 175.3(2) . . ? O1 Cu1 N1 89.7(2) . . ? N2 Cu1 N1 91.9(2) . . ? N5 Ag1 N3 126.7(2) . 4_566 ? N5 Ag1 N4 115.2(2) . . ? N3 Ag1 N4 98.2(2) 4_566 . ? N5 Ag1 C2 102.3(2) . . ? N3 Ag1 C2 113.1(2) 4_566 . ? N4 Ag1 C2 98.0(2) . . ? F1 C29 F2 92(2) . . ? F1 C29 F3 91.2(19) . . ? F2 C29 F3 101.0(16) . . ? F1 C29 S1 124.3(18) . . ? F2 C29 S1 120.5(17) . . ? F3 C29 S1 121.0(16) . . ? O4 S1 O5 114.3(11) . . ? O4 S1 O3 116.5(10) . . ? O5 S1 O3 115.1(9) . . ? O4 S1 C29 101.4(15) . . ? O5 S1 C29 103.2(9) . . ? O3 S1 C29 103.7(9) . . ? F4 C30 F6 115.7(9) . . ? F4 C30 F5 108.6(10) . . ? F6 C30 F5 114.9(6) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.492 _refine_diff_density_min -1.104 _refine_diff_density_rms 0.217 #===END ###Material relevant to compound 7 at 173K ## data_compound7 _database_code_depnum_ccdc_archive 'CCDC 868789' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H32 Ag Co N9 O2, F6 Sb, C2 H3 N, H2 O ' _chemical_formula_sum 'C45 H37 Ag Co F6 N10 O3 Sb' _chemical_formula_weight 1168.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2277(3) _cell_length_b 13.9112(3) _cell_length_c 14.0886(3) _cell_angle_alpha 89.9420(10) _cell_angle_beta 70.7410(10) _cell_angle_gamma 84.9120(10) _cell_volume 2252.45(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9956 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 27.47 _exptl_crystal_description platelet _exptl_crystal_colour dark-orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8552 _exptl_absorpt_correction_T_max 0.9573 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41471 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.52 _reflns_number_total 10263 _reflns_number_gt 8665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+3.2842P] 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 10263 _refine_ls_number_parameters 612 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _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 C1 C 0.0096(3) 0.1486(2) -0.2240(2) 0.0243(6) Uani 1 1 d . . . H1 H 0.0126 0.2065 -0.1925 0.029 Uiso 1 1 calc R . . C2 C -0.0901(3) 0.1212(2) -0.2431(2) 0.0283(6) Uani 1 1 d . . . H2 H -0.1626 0.1563 -0.2259 0.034 Uiso 1 1 calc R . . C3 C -0.0587(3) 0.0329(2) -0.2919(2) 0.0253(6) Uani 1 1 d . . . H3 H -0.1058 -0.0030 -0.3153 0.030 Uiso 1 1 calc R . . C4 C 0.0592(2) 0.0063(2) -0.3002(2) 0.0189(5) Uani 1 1 d . . . C5 C 0.1249(2) -0.08044(19) -0.3364(2) 0.0189(5) Uani 1 1 d . . . C6 C 0.2370(2) -0.10519(19) -0.3330(2) 0.0178(5) Uani 1 1 d . . . C7 C 0.3033(3) -0.1962(2) -0.3544(2) 0.0220(6) Uani 1 1 d . . . H7 H 0.2836 -0.2512 -0.3801 0.026 Uiso 1 1 calc R . . C8 C 0.4028(3) -0.1882(2) -0.3299(2) 0.0262(6) Uani 1 1 d . . . H8 H 0.4626 -0.2364 -0.3356 0.031 Uiso 1 1 calc R . . C9 C 0.3955(3) -0.0922(2) -0.2947(2) 0.0242(6) Uani 1 1 d . . . H9 H 0.4510 -0.0670 -0.2725 0.029 Uiso 1 1 calc R . . C10 C 0.0731(2) -0.1567(2) -0.3781(2) 0.0208(5) Uani 1 1 d . . . C11 C 0.0791(3) -0.1592(3) -0.4778(2) 0.0335(7) Uani 1 1 d . . . H11 H 0.1097 -0.1096 -0.5199 0.040 Uiso 1 1 calc R . . C12 C 0.0389(3) -0.2365(3) -0.5142(3) 0.0419(9) Uani 1 1 d . . . H12 H 0.0440 -0.2373 -0.5815 0.050 Uiso 1 1 calc R . . C13 C -0.0155(3) -0.3047(3) -0.3625(3) 0.0406(9) Uani 1 1 d . . . H13 H -0.0488 -0.3543 -0.3219 0.049 Uiso 1 1 calc R . . C14 C 0.0217(3) -0.2303(2) -0.3184(3) 0.0338(7) Uani 1 1 d . . . H14 H 0.0121 -0.2300 -0.2501 0.041 Uiso 1 1 calc R . . C15 C 0.4998(3) 0.1280(2) -0.3885(2) 0.0248(6) Uani 1 1 d . . . H15 H 0.4917 0.1106 -0.4494 0.030 Uiso 1 1 calc R . . C16 C 0.5972(3) 0.1691(2) -0.3791(2) 0.0292(7) Uani 1 1 d . . . H16 H 0.6632 0.1831 -0.4313 0.035 Uiso 1 1 calc R . . C17 C 0.5760(3) 0.1845(2) -0.2780(2) 0.0250(6) Uani 1 1 d . . . H17 H 0.6245 0.2114 -0.2487 0.030 Uiso 1 1 calc R . . C18 C 0.4661(2) 0.15152(19) -0.2272(2) 0.0195(5) Uani 1 1 d . . . C19 C 0.4095(2) 0.14813(19) -0.1236(2) 0.0186(5) Uani 1 1 d . . . C20 C 0.3029(2) 0.11208(19) -0.0783(2) 0.0179(5) Uani 1 1 d . . . C21 C 0.2475(3) 0.0958(2) 0.0259(2) 0.0215(6) Uani 1 1 d . . . H21 H 0.2724 0.1131 0.0786 0.026 Uiso 1 1 calc R . . C22 C 0.1506(3) 0.0498(2) 0.0332(2) 0.0252(6) Uani 1 1 d . . . H22 H 0.0976 0.0294 0.0920 0.030 Uiso 1 1 calc R . . C23 C 0.1465(3) 0.0392(2) -0.0655(2) 0.0223(6) Uani 1 1 d . . . H23 H 0.0893 0.0097 -0.0817 0.027 Uiso 1 1 calc R . . C24 C 0.4727(2) 0.1803(2) -0.0563(2) 0.0199(5) Uani 1 1 d . . . C25 C 0.5615(3) 0.1202(2) -0.0409(2) 0.0283(6) Uani 1 1 d . . . H25 H 0.5829 0.0596 -0.0727 0.034 Uiso 1 1 calc R . . C26 C 0.6180(3) 0.1512(2) 0.0224(3) 0.0311(7) Uani 1 1 d . . . H26 H 0.6768 0.1099 0.0329 0.037 Uiso 1 1 calc R . . C27 C 0.5074(3) 0.2965(2) 0.0528(2) 0.0274(6) Uani 1 1 d . . . H27 H 0.4894 0.3576 0.0838 0.033 Uiso 1 1 calc R . . C28 C 0.4457(3) 0.2702(2) -0.0080(2) 0.0275(6) Uani 1 1 d . . . H28 H 0.3865 0.3126 -0.0165 0.033 Uiso 1 1 calc R . . C29 C 0.3165(3) 0.0670(3) -0.7077(2) 0.0313(7) Uani 1 1 d . . . H29 H 0.3266 0.0046 -0.7347 0.038 Uiso 1 1 calc R . . C30 C 0.2972(3) 0.0785(2) -0.6057(2) 0.0247(6) Uani 1 1 d . . . H30 H 0.2940 0.0249 -0.5657 0.030 Uiso 1 1 calc R . . C31 C 0.2827(2) 0.1713(2) -0.5637(2) 0.0206(5) Uani 1 1 d . . . C32 C 0.2870(3) 0.2480(2) -0.6277(2) 0.0299(7) Uani 1 1 d . . . H32 H 0.2773 0.3113 -0.6032 0.036 Uiso 1 1 calc R . . C33 C 0.3058(3) 0.2286(3) -0.7280(2) 0.0359(8) Uani 1 1 d . . . H33 H 0.3077 0.2808 -0.7696 0.043 Uiso 1 1 calc R . . C34 C 0.2675(2) 0.1831(2) -0.4544(2) 0.0201(5) Uani 1 1 d . . . C35 C 0.2475(3) 0.2749(2) -0.4087(2) 0.0268(6) Uani 1 1 d . . . H35 H 0.2412 0.3280 -0.4473 0.032 Uiso 1 1 calc R . . C36 C 0.2367(3) 0.2914(2) -0.3086(2) 0.0214(6) Uani 1 1 d . . . C37 C 0.2423(3) 0.3911(2) -0.2724(2) 0.0236(6) Uani 1 1 d . . . C38 C 0.3046(4) 0.4027(2) -0.2078(3) 0.0383(8) Uani 1 1 d . . . H38 H 0.3377 0.3491 -0.1842 0.046 Uiso 1 1 calc R . . C39 C 0.3174(4) 0.4946(2) -0.1785(3) 0.0425(9) Uani 1 1 d . . . H39 H 0.3613 0.5014 -0.1366 0.051 Uiso 1 1 calc R . . C40 C 0.2074(3) 0.5620(2) -0.2679(3) 0.0366(8) Uani 1 1 d . . . H40 H 0.1720 0.6168 -0.2876 0.044 Uiso 1 1 calc R . . C41 C 0.1922(3) 0.4727(2) -0.3032(3) 0.0341(7) Uani 1 1 d . . . H41 H 0.1494 0.4680 -0.3464 0.041 Uiso 1 1 calc R . . C42 C 0.0347(4) -0.2575(3) -0.0469(3) 0.0456(9) Uani 1 1 d . . . C43 C -0.0626(4) -0.3113(3) 0.0050(3) 0.0569(11) Uani 1 1 d . . . H43A H -0.1240 -0.2684 0.0492 0.085 Uiso 1 1 calc R . . H43B H -0.0381 -0.3604 0.0435 0.085 Uiso 1 1 calc R . . H43C H -0.0901 -0.3408 -0.0433 0.085 Uiso 1 1 calc R . . N1 N 0.0984(2) 0.08087(16) -0.25671(17) 0.0188(5) Uani 1 1 d . . . N2 N 0.2985(2) -0.04241(16) -0.29736(17) 0.0179(4) Uani 1 1 d . . . N3 N -0.0063(3) -0.3092(2) -0.4587(2) 0.0400(7) Uani 1 1 d . . . N4 N 0.4208(2) 0.11724(17) -0.29871(17) 0.0197(5) Uani 1 1 d . . . N5 N 0.2358(2) 0.07732(16) -0.13221(16) 0.0173(4) Uani 1 1 d . . . N6 N 0.5915(2) 0.23806(18) 0.06910(19) 0.0253(5) Uani 1 1 d . . . N7 N 0.3214(3) 0.1406(2) -0.7695(2) 0.0348(6) Uani 1 1 d . . . N8 N 0.2693(3) 0.57407(18) -0.2078(2) 0.0309(6) Uani 1 1 d . . . N9 N 0.1107(3) -0.2151(3) -0.0881(3) 0.0596(10) Uani 1 1 d . . . O1 O 0.27989(18) 0.10418(14) -0.41152(14) 0.0204(4) Uani 1 1 d . . . O2 O 0.22762(18) 0.22782(13) -0.24154(14) 0.0202(4) Uani 1 1 d . . . Co1 Co 0.25977(3) 0.09301(2) -0.27208(3) 0.01586(9) Uani 1 1 d . . . Ag1 Ag 0.31059(2) -0.278577(17) -0.17007(2) 0.03318(8) Uani 1 1 d . . . F1 F 0.8893(6) 0.4257(5) 0.7047(4) 0.204(3) Uani 1 1 d . . . F2 F 0.8782(8) 0.3809(4) 0.8846(7) 0.241(5) Uani 1 1 d . . . F3 F 0.7230(4) 0.3373(3) 0.8128(4) 0.1160(15) Uani 1 1 d . . . F4 F 0.6909(8) 0.5188(4) 0.7746(5) 0.211(4) Uani 1 1 d . . . F5 F 0.6739(5) 0.4768(4) 0.9533(3) 0.161(2) Uani 1 1 d . . . F6 F 0.8475(6) 0.5611(3) 0.8455(4) 0.168(3) Uani 1 1 d . . . Sb1 Sb 0.78462(3) 0.447551(19) 0.83133(2) 0.04686(9) Uani 1 1 d . . . C44 C 0.4343(6) 0.4827(4) 0.4128(5) 0.0828(18) Uani 1 1 d . . . C45 C 0.3770(7) 0.5785(4) 0.4157(6) 0.103(2) Uani 1 1 d . . . H45A H 0.2969 0.5793 0.4572 0.154 Uiso 1 1 calc R . . H45B H 0.3815 0.5963 0.3488 0.154 Uiso 1 1 calc R . . H45C H 0.4146 0.6235 0.4431 0.154 Uiso 1 1 calc R . . N10 N 0.4774(6) 0.4093(4) 0.4122(6) 0.124(3) Uani 1 1 d . . . O3 O 0.1306(4) 0.4652(3) 0.4887(3) 0.0740(10) Uani 1 1 d D . . H3B H 0.095(5) 0.518(3) 0.472(6) 0.129 Uiso 1 1 d D . . H3A H 0.093(5) 0.412(3) 0.494(6) 0.129 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0269(15) 0.0222(14) 0.0232(14) -0.0011(11) -0.0079(12) 0.0000(11) C2 0.0206(15) 0.0332(16) 0.0304(16) 0.0034(13) -0.0087(12) 0.0023(12) C3 0.0226(15) 0.0302(15) 0.0276(15) 0.0049(12) -0.0135(12) -0.0057(12) C4 0.0212(13) 0.0215(13) 0.0166(12) 0.0030(10) -0.0090(11) -0.0054(10) C5 0.0233(14) 0.0208(13) 0.0150(12) 0.0032(10) -0.0083(11) -0.0074(11) C6 0.0228(14) 0.0169(12) 0.0154(12) 0.0007(10) -0.0080(10) -0.0043(10) C7 0.0281(15) 0.0181(13) 0.0195(13) 0.0001(10) -0.0070(11) -0.0039(11) C8 0.0237(15) 0.0245(14) 0.0282(15) 0.0019(12) -0.0063(12) 0.0010(12) C9 0.0231(15) 0.0247(14) 0.0283(15) 0.0030(11) -0.0125(12) -0.0043(11) C10 0.0205(14) 0.0200(13) 0.0253(14) -0.0010(11) -0.0117(11) -0.0030(10) C11 0.0396(19) 0.0412(19) 0.0246(16) 0.0032(13) -0.0133(14) -0.0190(15) C12 0.050(2) 0.050(2) 0.0326(18) -0.0032(16) -0.0190(17) -0.0210(18) C13 0.051(2) 0.0286(17) 0.054(2) 0.0107(15) -0.0299(19) -0.0192(15) C14 0.048(2) 0.0312(16) 0.0322(17) 0.0079(13) -0.0224(15) -0.0178(15) C15 0.0277(15) 0.0288(15) 0.0177(13) 0.0001(11) -0.0057(12) -0.0077(12) C16 0.0249(15) 0.0350(17) 0.0256(15) 0.0039(13) -0.0035(12) -0.0109(13) C17 0.0245(15) 0.0278(15) 0.0251(14) 0.0010(11) -0.0098(12) -0.0095(12) C18 0.0221(14) 0.0184(12) 0.0199(13) -0.0013(10) -0.0084(11) -0.0051(10) C19 0.0228(14) 0.0154(12) 0.0206(13) -0.0003(10) -0.0111(11) -0.0014(10) C20 0.0219(13) 0.0185(12) 0.0158(12) -0.0003(10) -0.0095(11) -0.0031(10) C21 0.0252(14) 0.0253(14) 0.0155(13) 0.0014(10) -0.0086(11) -0.0023(11) C22 0.0257(15) 0.0330(16) 0.0171(13) 0.0067(11) -0.0064(11) -0.0064(12) C23 0.0224(14) 0.0271(14) 0.0200(14) 0.0058(11) -0.0089(11) -0.0083(11) C24 0.0211(14) 0.0230(13) 0.0179(13) -0.0005(10) -0.0085(11) -0.0061(11) C25 0.0351(17) 0.0234(14) 0.0321(16) -0.0087(12) -0.0200(14) 0.0023(12) C26 0.0336(17) 0.0284(16) 0.0382(18) -0.0074(13) -0.0231(15) 0.0050(13) C27 0.0364(17) 0.0200(14) 0.0299(16) -0.0057(11) -0.0167(14) -0.0011(12) C28 0.0325(17) 0.0240(14) 0.0307(16) -0.0028(12) -0.0174(14) 0.0009(12) C29 0.0273(16) 0.0432(19) 0.0242(15) -0.0114(13) -0.0099(13) -0.0021(14) C30 0.0261(15) 0.0301(15) 0.0198(14) -0.0016(11) -0.0094(12) -0.0059(12) C31 0.0210(14) 0.0277(14) 0.0155(13) -0.0004(10) -0.0087(11) -0.0043(11) C32 0.0382(18) 0.0328(16) 0.0206(14) 0.0023(12) -0.0124(13) -0.0032(13) C33 0.044(2) 0.045(2) 0.0202(15) 0.0060(14) -0.0131(14) 0.0002(16) C34 0.0249(14) 0.0221(13) 0.0151(13) 0.0018(10) -0.0082(11) -0.0061(11) C35 0.0454(19) 0.0198(14) 0.0203(14) 0.0036(11) -0.0167(13) -0.0073(13) C36 0.0272(15) 0.0183(13) 0.0203(13) 0.0006(10) -0.0091(11) -0.0049(11) C37 0.0350(16) 0.0191(13) 0.0199(13) -0.0001(10) -0.0124(12) -0.0068(12) C38 0.066(2) 0.0203(15) 0.044(2) 0.0020(13) -0.0391(19) -0.0057(15) C39 0.073(3) 0.0248(16) 0.051(2) 0.0005(15) -0.048(2) -0.0082(16) C40 0.053(2) 0.0177(14) 0.051(2) -0.0003(13) -0.0330(18) -0.0036(14) C41 0.047(2) 0.0239(15) 0.0439(19) -0.0010(13) -0.0307(17) -0.0059(14) C42 0.045(2) 0.057(2) 0.0296(18) -0.0073(17) -0.0113(17) 0.018(2) C43 0.062(3) 0.057(3) 0.049(2) -0.006(2) -0.016(2) 0.001(2) N1 0.0234(12) 0.0186(11) 0.0163(11) -0.0009(8) -0.0090(9) -0.0022(9) N2 0.0198(11) 0.0190(11) 0.0176(11) 0.0014(8) -0.0088(9) -0.0058(9) N3 0.0443(18) 0.0367(16) 0.0479(18) -0.0080(13) -0.0249(15) -0.0127(13) N4 0.0240(12) 0.0215(11) 0.0148(11) 0.0002(9) -0.0066(9) -0.0073(9) N5 0.0195(11) 0.0188(11) 0.0158(11) 0.0002(8) -0.0080(9) -0.0042(9) N6 0.0304(14) 0.0248(12) 0.0261(13) -0.0022(10) -0.0158(11) -0.0051(10) N7 0.0336(15) 0.0548(18) 0.0178(12) -0.0042(12) -0.0119(11) 0.0004(13) N8 0.0447(16) 0.0201(12) 0.0352(15) -0.0014(10) -0.0221(13) -0.0072(11) N9 0.041(2) 0.075(3) 0.051(2) -0.0001(19) -0.0057(17) 0.0154(19) O1 0.0290(11) 0.0191(9) 0.0157(9) 0.0001(7) -0.0100(8) -0.0053(8) O2 0.0303(11) 0.0162(9) 0.0155(9) -0.0010(7) -0.0090(8) -0.0042(8) Co1 0.02075(19) 0.01544(17) 0.01343(17) 0.00045(13) -0.00760(14) -0.00487(13) Ag1 0.03988(15) 0.02670(13) 0.04228(15) -0.00734(10) -0.02526(12) -0.00645(10) F1 0.203(6) 0.229(7) 0.106(4) -0.053(4) 0.060(4) -0.073(5) F2 0.340(10) 0.132(5) 0.391(11) -0.006(6) -0.324(10) 0.033(5) F3 0.123(3) 0.073(2) 0.164(4) -0.029(2) -0.057(3) -0.039(2) F4 0.355(10) 0.118(4) 0.236(7) -0.044(4) -0.226(8) 0.087(5) F5 0.186(5) 0.158(5) 0.087(3) -0.046(3) 0.032(3) -0.042(4) F6 0.280(7) 0.100(3) 0.147(4) 0.011(3) -0.078(5) -0.118(4) Sb1 0.0672(2) 0.03495(14) 0.03925(15) -0.00077(10) -0.01735(13) -0.01026(12) C44 0.088(4) 0.060(3) 0.087(4) -0.013(3) -0.006(3) -0.027(3) C45 0.135(6) 0.059(4) 0.110(6) -0.003(3) -0.034(5) -0.011(4) N10 0.112(5) 0.055(3) 0.185(7) -0.011(4) -0.020(5) -0.011(3) O3 0.101(3) 0.056(2) 0.088(3) 0.0098(19) -0.059(2) -0.027(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 C1 N1 1.329(4) . ? C1 C2 1.415(4) . ? C1 H1 0.9300 . ? C2 C3 1.368(5) . ? C2 H2 0.9300 . ? C3 C4 1.423(4) . ? C3 H3 0.9300 . ? C4 C5 1.386(4) . ? C4 N1 1.402(3) . ? C5 C6 1.399(4) . ? C5 C10 1.496(4) . ? C6 N2 1.396(3) . ? C6 C7 1.418(4) . ? C7 C8 1.383(4) . ? C7 H7 0.9300 . ? C8 C9 1.411(4) . ? C8 Ag1 2.549(3) . ? C8 H8 0.9300 . ? C9 N2 1.330(4) . ? C9 H9 0.9300 . ? C10 C11 1.383(4) . ? C10 C14 1.384(4) . ? C11 C12 1.387(5) . ? C11 H11 0.9300 . ? C12 N3 1.323(5) . ? C12 H12 0.9300 . ? C13 N3 1.324(5) . ? C13 C14 1.391(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N4 1.332(4) . ? C15 C16 1.411(4) . ? C15 H15 0.9300 . ? C16 C17 1.375(4) . ? C16 H16 0.9300 . ? C17 C18 1.416(4) . ? C17 H17 0.9300 . ? C18 C19 1.397(4) . ? C18 N4 1.402(3) . ? C19 C20 1.388(4) . ? C19 C24 1.497(4) . ? C20 N5 1.401(3) . ? C20 C21 1.427(4) . ? C21 C22 1.370(4) . ? C21 H21 0.9300 . ? C22 C23 1.417(4) . ? C22 H22 0.9300 . ? C23 N5 1.335(3) . ? C23 H23 0.9300 . ? C24 C28 1.384(4) . ? C24 C25 1.385(4) . ? C25 C26 1.385(4) . ? C25 H25 0.9300 . ? C26 N6 1.338(4) . ? C26 H26 0.9300 . ? C27 N6 1.333(4) . ? C27 C28 1.384(4) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 N7 1.335(5) . ? C29 C30 1.385(4) . ? C29 H29 0.9300 . ? C30 C31 1.393(4) . ? C30 H30 0.9300 . ? C31 C32 1.389(4) . ? C31 C34 1.496(4) . ? C32 C33 1.379(4) . ? C32 H32 0.9300 . ? C33 N7 1.328(5) . ? C33 H33 0.9300 . ? C34 O1 1.274(3) . ? C34 C35 1.396(4) . ? C35 C36 1.389(4) . ? C35 H35 0.9300 . ? C36 O2 1.278(3) . ? C36 C37 1.494(4) . ? C37 C41 1.379(4) . ? C37 C38 1.384(4) . ? C38 C39 1.381(4) . ? C38 H38 0.9300 . ? C39 N8 1.335(4) . ? C39 H39 0.9300 . ? C40 N8 1.328(4) . ? C40 C41 1.389(4) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 N9 1.135(6) . ? C42 C43 1.446(7) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? N1 Co1 1.936(2) . ? N2 Co1 1.906(2) . ? N4 Co1 1.939(2) . ? N5 Co1 1.910(2) . ? N6 Ag1 2.240(2) 2_655 ? N8 Ag1 2.259(2) 1_565 ? N9 Ag1 2.417(4) . ? O1 Co1 1.9056(19) . ? O2 Co1 1.9015(19) . ? Ag1 N6 2.240(2) 2_655 ? Ag1 N8 2.259(2) 1_545 ? F1 Sb1 1.827(5) . ? F2 Sb1 1.763(4) . ? F3 Sb1 1.822(3) . ? F4 Sb1 1.826(5) . ? F5 Sb1 1.823(4) . ? F6 Sb1 1.855(4) . ? C44 N10 1.106(8) . ? C44 C45 1.443(9) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? O3 H3B 0.890(19) . ? O3 H3A 0.900(19) . ? 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 C1 C2 111.4(3) . . ? N1 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C3 C2 C1 106.5(3) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.3(3) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? C5 C4 N1 123.6(2) . . ? C5 C4 C3 128.0(3) . . ? N1 C4 C3 108.2(2) . . ? C4 C5 C6 124.7(2) . . ? C4 C5 C10 119.2(2) . . ? C6 C5 C10 116.0(2) . . ? N2 C6 C5 123.4(2) . . ? N2 C6 C7 108.0(2) . . ? C5 C6 C7 128.4(2) . . ? C8 C7 C6 107.3(2) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.2(3) . . ? C7 C8 Ag1 88.23(18) . . ? C9 C8 Ag1 103.37(19) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? Ag1 C8 H8 80.4 . . ? N2 C9 C8 111.1(3) . . ? N2 C9 H9 124.5 . . ? C8 C9 H9 124.5 . . ? C11 C10 C14 117.5(3) . . ? C11 C10 C5 121.8(3) . . ? C14 C10 C5 120.6(3) . . ? C10 C11 C12 119.1(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N3 C12 C11 123.9(3) . . ? N3 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? N3 C13 C14 124.0(3) . . ? N3 C13 H13 118.0 . . ? C14 C13 H13 118.0 . . ? C10 C14 C13 118.7(3) . . ? C10 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? N4 C15 C16 111.1(3) . . ? N4 C15 H15 124.4 . . ? C16 C15 H15 124.4 . . ? C17 C16 C15 106.8(3) . . ? C17 C16 H16 126.6 . . ? C15 C16 H16 126.6 . . ? C16 C17 C18 106.8(3) . . ? C16 C17 H17 126.6 . . ? C18 C17 H17 126.6 . . ? C19 C18 N4 123.2(2) . . ? C19 C18 C17 128.1(3) . . ? N4 C18 C17 108.7(2) . . ? C20 C19 C18 125.2(2) . . ? C20 C19 C24 117.5(2) . . ? C18 C19 C24 117.1(2) . . ? C19 C20 N5 123.6(2) . . ? C19 C20 C21 127.8(2) . . ? N5 C20 C21 108.4(2) . . ? C22 C21 C20 106.7(2) . . ? C22 C21 H21 126.6 . . ? C20 C21 H21 126.6 . . ? C21 C22 C23 107.1(2) . . ? C21 C22 H22 126.4 . . ? C23 C22 H22 126.4 . . ? N5 C23 C22 110.8(2) . . ? N5 C23 H23 124.6 . . ? C22 C23 H23 124.6 . . ? C28 C24 C25 117.8(3) . . ? C28 C24 C19 121.8(3) . . ? C25 C24 C19 120.4(3) . . ? C24 C25 C26 119.4(3) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? N6 C26 C25 122.7(3) . . ? N6 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? N6 C27 C28 122.9(3) . . ? N6 C27 H27 118.5 . . ? C28 C27 H27 118.5 . . ? C27 C28 C24 119.4(3) . . ? C27 C28 H28 120.3 . . ? C24 C28 H28 120.3 . . ? N7 C29 C30 123.7(3) . . ? N7 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? C29 C30 C31 119.2(3) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C32 C31 C30 117.3(3) . . ? C32 C31 C34 123.8(3) . . ? C30 C31 C34 118.9(2) . . ? C33 C32 C31 118.9(3) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? N7 C33 C32 124.6(3) . . ? N7 C33 H33 117.7 . . ? C32 C33 H33 117.7 . . ? O1 C34 C35 125.2(2) . . ? O1 C34 C31 114.2(2) . . ? C35 C34 C31 120.5(2) . . ? C36 C35 C34 123.6(3) . . ? C36 C35 H35 118.2 . . ? C34 C35 H35 118.2 . . ? O2 C36 C35 126.6(3) . . ? O2 C36 C37 113.7(2) . . ? C35 C36 C37 119.6(2) . . ? C41 C37 C38 118.2(3) . . ? C41 C37 C36 123.3(3) . . ? C38 C37 C36 118.5(3) . . ? C39 C38 C37 119.5(3) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? N8 C39 C38 122.8(3) . . ? N8 C39 H39 118.6 . . ? C38 C39 H39 118.6 . . ? N8 C40 C41 124.0(3) . . ? N8 C40 H40 118.0 . . ? C41 C40 H40 118.0 . . ? C37 C41 C40 118.2(3) . . ? C37 C41 H41 120.9 . . ? C40 C41 H41 120.9 . . ? N9 C42 C43 179.5(5) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C1 N1 C4 106.7(2) . . ? C1 N1 Co1 127.2(2) . . ? C4 N1 Co1 124.63(19) . . ? C9 N2 C6 107.5(2) . . ? C9 N2 Co1 126.06(19) . . ? C6 N2 Co1 126.11(19) . . ? C12 N3 C13 116.7(3) . . ? C15 N4 C18 106.5(2) . . ? C15 N4 Co1 126.6(2) . . ? C18 N4 Co1 124.96(19) . . ? C23 N5 C20 106.9(2) . . ? C23 N5 Co1 126.60(19) . . ? C20 N5 Co1 126.23(18) . . ? C27 N6 C26 117.8(3) . . ? C27 N6 Ag1 123.2(2) . 2_655 ? C26 N6 Ag1 118.9(2) . 2_655 ? C33 N7 C29 116.4(3) . . ? C40 N8 C39 117.2(3) . . ? C40 N8 Ag1 122.2(2) . 1_565 ? C39 N8 Ag1 120.2(2) . 1_565 ? C42 N9 Ag1 127.1(3) . . ? C34 O1 Co1 124.92(18) . . ? C36 O2 Co1 123.25(18) . . ? O2 Co1 O1 95.21(8) . . ? O2 Co1 N2 176.20(9) . . ? O1 Co1 N2 87.53(9) . . ? O2 Co1 N5 86.54(9) . . ? O1 Co1 N5 177.57(9) . . ? N2 Co1 N5 90.80(10) . . ? O2 Co1 N1 91.21(9) . . ? O1 Co1 N1 84.89(9) . . ? N2 Co1 N1 91.65(10) . . ? N5 Co1 N1 93.41(10) . . ? O2 Co1 N4 84.71(9) . . ? O1 Co1 N4 89.97(9) . . ? N2 Co1 N4 92.67(10) . . ? N5 Co1 N4 91.86(10) . . ? N1 Co1 N4 173.14(10) . . ? N6 Ag1 N8 129.36(10) 2_655 1_545 ? N6 Ag1 N9 106.11(12) 2_655 . ? N8 Ag1 N9 95.79(14) 1_545 . ? N6 Ag1 C8 103.31(10) 2_655 . ? N8 Ag1 C8 110.64(10) 1_545 . ? N9 Ag1 C8 110.80(12) . . ? F2 Sb1 F3 90.3(3) . . ? F2 Sb1 F5 93.1(4) . . ? F3 Sb1 F5 93.6(2) . . ? F2 Sb1 F4 178.4(4) . . ? F3 Sb1 F4 91.1(3) . . ? F5 Sb1 F4 87.8(3) . . ? F2 Sb1 F1 91.5(4) . . ? F3 Sb1 F1 87.4(3) . . ? F5 Sb1 F1 175.3(4) . . ? F4 Sb1 F1 87.7(4) . . ? F2 Sb1 F6 91.2(3) . . ? F3 Sb1 F6 177.9(2) . . ? F5 Sb1 F6 87.8(3) . . ? F4 Sb1 F6 87.4(3) . . ? F1 Sb1 F6 91.1(3) . . ? N10 C44 C45 178.9(8) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? H3B O3 H3A 115(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.130 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.111 #===END ###Material relevant to compound 8 at 173K ## data_compound8 _database_code_depnum_ccdc_archive 'CCDC 868790' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H64 Ag2 Co2 N18 O4, C6 H6, 2(C F3 O3 S), 4(C2 H3 N)' _chemical_formula_sum 'C102 H82 Ag2 Co2 F6 N22 O10 S2' _chemical_formula_weight 2287.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4775(9) _cell_length_b 14.1836(10) _cell_length_c 14.2334(11) _cell_angle_alpha 92.645(2) _cell_angle_beta 101.045(2) _cell_angle_gamma 103.095(3) _cell_volume 2397.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8163 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.10 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1162 _exptl_absorpt_coefficient_mu 0.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8450 _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27655 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.69 _reflns_number_total 10945 _reflns_number_gt 8311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+18.9687P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10945 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.2539 _refine_ls_wR_factor_gt 0.2398 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 C1 C 0.1135(6) 0.2033(5) 1.1083(5) 0.0249(13) Uani 1 1 d . . . H1 H 0.0554 0.2306 1.0803 0.030 Uiso 1 1 calc R . . C2 C 0.1223(6) 0.1661(5) 1.1992(5) 0.0288(14) Uani 1 1 d . . . H2 H 0.0729 0.1650 1.2407 0.035 Uiso 1 1 calc R . . C3 C 0.2179(6) 0.1321(5) 1.2140(5) 0.0268(14) Uani 1 1 d . . . H3 H 0.2449 0.1018 1.2670 0.032 Uiso 1 1 calc R . . C4 C 0.2683(5) 0.1519(5) 1.1330(4) 0.0221(12) Uani 1 1 d . . . C5 C 0.3731(6) 0.1405(5) 1.1195(5) 0.0246(13) Uani 1 1 d . . . C6 C 0.4212(6) 0.1725(5) 1.0432(5) 0.0255(13) Uani 1 1 d . . . C7 C 0.5346(6) 0.1802(5) 1.0336(5) 0.0301(15) Uani 1 1 d . . . H7 H 0.5889 0.1568 1.0737 0.036 Uiso 1 1 calc R . . C8 C 0.5479(6) 0.2286(5) 0.9537(5) 0.0309(15) Uani 1 1 d . . . H8 H 0.6129 0.2444 0.9292 0.037 Uiso 1 1 calc R . . C9 C 0.4443(6) 0.2499(5) 0.9162(5) 0.0279(14) Uani 1 1 d . . . H9 H 0.4304 0.2826 0.8617 0.034 Uiso 1 1 calc R . . C10 C 0.4412(6) 0.0939(5) 1.1924(5) 0.0287(14) Uani 1 1 d . . . C11 C 0.5001(7) 0.1442(6) 1.2799(5) 0.0396(19) Uani 1 1 d . . . H11 H 0.4932 0.2062 1.2974 0.048 Uiso 1 1 calc R . . C12 C 0.5685(9) 0.0994(7) 1.3395(7) 0.053(3) Uani 1 1 d . . . H12 H 0.6094 0.1343 1.3970 0.064 Uiso 1 1 calc R . . C13 C 0.5223(8) -0.0373(7) 1.2379(6) 0.046(2) Uani 1 1 d . . . H13 H 0.5279 -0.1003 1.2232 0.055 Uiso 1 1 calc R . . C14 C 0.4540(7) 0.0015(6) 1.1722(6) 0.0363(17) Uani 1 1 d . . . H14 H 0.4163 -0.0341 1.1142 0.044 Uiso 1 1 calc R . . C15 C -0.0277(6) 0.1191(5) 0.8710(5) 0.0272(14) Uani 1 1 d . . . H15 H -0.0182 0.0585 0.8879 0.033 Uiso 1 1 calc R . . C16 C -0.1283(6) 0.1364(6) 0.8167(5) 0.0340(16) Uani 1 1 d . . . H16 H -0.1947 0.0900 0.7915 0.041 Uiso 1 1 calc R . . C17 C -0.1094(6) 0.2324(6) 0.8088(5) 0.0316(15) Uani 1 1 d . . . H17 H -0.1605 0.2650 0.7774 0.038 Uiso 1 1 calc R . . C18 C 0.0034(5) 0.2752(5) 0.8573(4) 0.0217(12) Uani 1 1 d . . . C19 C -0.0617(5) 0.6263(5) 0.1308(4) 0.0210(12) Uani 1 1 d . . . C20 C 0.1714(5) 0.4099(5) 0.9199(4) 0.0212(12) Uani 1 1 d . . . C21 C 0.2301(6) 0.5086(5) 0.9461(4) 0.0244(13) Uani 1 1 d . . . H21 H 0.2048 0.5632 0.9277 0.029 Uiso 1 1 calc R . . C22 C 0.3330(6) 0.5077(5) 1.0047(5) 0.0245(13) Uani 1 1 d . . . H22 H 0.3900 0.5615 1.0329 0.029 Uiso 1 1 calc R . . C23 C 0.3333(5) 0.4098(5) 1.0126(4) 0.0231(13) Uani 1 1 d . . . H23 H 0.3921 0.3887 1.0491 0.028 Uiso 1 1 calc R . . C24 C 0.0011(5) 0.5543(5) 0.1717(4) 0.0219(12) Uani 1 1 d . . . C25 C 0.0898(7) 0.5348(6) 0.1340(5) 0.0321(16) Uani 1 1 d . . . H25 H 0.1110 0.5660 0.0821 0.039 Uiso 1 1 calc R . . C26 C 0.1454(7) 0.4688(6) 0.1748(5) 0.0370(17) Uani 1 1 d . . . H26 H 0.2042 0.4559 0.1489 0.044 Uiso 1 1 calc R . . C27 C 0.0343(6) 0.4400(5) 0.2854(5) 0.0268(14) Uani 1 1 d . . . H27 H 0.0153 0.4078 0.3375 0.032 Uiso 1 1 calc R . . C28 C -0.0276(6) 0.5047(5) 0.2484(5) 0.0270(14) Uani 1 1 d . . . H28 H -0.0874 0.5146 0.2746 0.032 Uiso 1 1 calc R . . C29 C 0.1764(6) -0.2097(5) 0.9497(6) 0.0332(16) Uani 1 1 d . . . H29 H 0.1698 -0.2323 1.0091 0.040 Uiso 1 1 calc R . . C30 C 0.1838(6) -0.1126(5) 0.9403(5) 0.0293(14) Uani 1 1 d . . . H30 H 0.1820 -0.0713 0.9923 0.035 Uiso 1 1 calc R . . C31 C 0.1940(5) -0.0766(5) 0.8527(5) 0.0235(13) Uani 1 1 d . . . C32 C 0.1987(6) -0.1414(5) 0.7785(5) 0.0318(15) Uani 1 1 d . . . H32 H 0.2071 -0.1200 0.7190 0.038 Uiso 1 1 calc R . . C33 C 0.1910(7) -0.2373(5) 0.7938(6) 0.0366(17) Uani 1 1 d . . . H33 H 0.1947 -0.2796 0.7432 0.044 Uiso 1 1 calc R . . C34 C 0.1998(5) 0.0297(4) 0.8434(4) 0.0210(12) Uani 1 1 d . . . C35 C 0.2143(6) 0.0700(5) 0.7588(5) 0.0268(14) Uani 1 1 d . . . H35 H 0.2208 0.0294 0.7081 0.032 Uiso 1 1 calc R . . C36 C 0.2196(5) 0.1667(5) 0.7445(4) 0.0227(13) Uani 1 1 d . . . C37 C 0.2270(6) 0.2021(5) 0.6483(4) 0.0256(14) Uani 1 1 d . . . C38 C 0.2690(6) 0.1558(5) 0.5816(5) 0.0290(15) Uani 1 1 d . . . H38 H 0.2961 0.1010 0.5955 0.035 Uiso 1 1 calc R . . C39 C 0.2697(7) 0.1932(5) 0.4931(5) 0.0319(16) Uani 1 1 d . . . H39 H 0.2987 0.1619 0.4485 0.038 Uiso 1 1 calc R . . C40 C 0.1908(7) 0.3148(5) 0.5336(5) 0.0318(15) Uani 1 1 d . . . H40 H 0.1638 0.3692 0.5177 0.038 Uiso 1 1 calc R . . C41 C 0.1865(6) 0.2839(5) 0.6237(5) 0.0303(15) Uani 1 1 d . . . H41 H 0.1574 0.3167 0.6671 0.036 Uiso 1 1 calc R . . C42 C 0.4761(7) 0.3950(7) 0.2458(6) 0.0397(18) Uani 1 1 d . . . C43 C 0.5801(9) 0.4252(12) 0.2103(8) 0.081(4) Uani 1 1 d . . . H43A H 0.5778 0.3819 0.1557 0.121 Uiso 1 1 calc R . . H43B H 0.6432 0.4232 0.2601 0.121 Uiso 1 1 calc R . . H43C H 0.5875 0.4902 0.1918 0.121 Uiso 1 1 calc R . . N1 N 0.1980(4) 0.1945(4) 1.0680(3) 0.0195(10) Uani 1 1 d . . . N2 N 0.3684(5) 0.2171(4) 0.9691(4) 0.0225(11) Uani 1 1 d . . . N3 N 0.5816(8) 0.0091(6) 1.3219(6) 0.055(2) Uani 1 1 d . . . N4 N 0.0509(4) 0.2016(4) 0.8943(4) 0.0220(11) Uani 1 1 d . . . N5 N 0.2394(4) 0.3504(4) 0.9618(4) 0.0197(10) Uani 1 1 d . . . N6 N 0.1192(5) 0.4219(4) 0.2502(4) 0.0285(12) Uani 1 1 d . . . N7 N 0.1783(6) -0.2738(4) 0.8782(5) 0.0359(14) Uani 1 1 d . . . N8 N 0.2316(5) 0.2713(4) 0.4678(4) 0.0280(12) Uani 1 1 d . . . N9 N 0.3976(6) 0.3728(5) 0.2712(5) 0.0441(17) Uani 1 1 d . . . O1 O 0.1876(4) 0.0758(3) 0.9194(3) 0.0252(10) Uani 1 1 d . . . O2 O 0.2211(4) 0.2342(3) 0.8086(3) 0.0242(9) Uani 1 1 d . . . Co1 Co 0.21074(7) 0.21309(6) 0.93794(6) 0.0185(2) Uani 1 1 d . . . Ag1 Ag 0.23108(5) 0.32974(5) 0.32404(4) 0.03688(19) Uani 1 1 d . . . C44 C 0.8548(10) 0.3383(8) 0.5084(7) 0.060(3) Uani 1 1 d . . . O3 O 0.7933(6) 0.4438(6) 0.3826(5) 0.063(2) Uani 1 1 d . . . O4 O 0.7537(6) 0.4708(5) 0.5403(5) 0.0558(17) Uani 1 1 d . . . O5 O 0.6487(6) 0.3281(5) 0.4343(5) 0.0603(19) Uani 1 1 d . . . F1 F 0.9575(6) 0.3968(7) 0.5333(6) 0.091(2) Uani 1 1 d . . . F2 F 0.8572(9) 0.2663(7) 0.4446(6) 0.109(3) Uani 1 1 d . . . F3 F 0.8350(10) 0.2955(7) 0.5859(6) 0.117(3) Uani 1 1 d . . . S1 S 0.75048(18) 0.40192(15) 0.46166(14) 0.0389(5) Uani 1 1 d . . . C45 C 0.6298(11) 0.0786(10) 0.5939(10) 0.073(3) Uani 1 1 d . . . C46 C 0.5804(15) 0.1610(10) 0.5912(12) 0.098(5) Uani 1 1 d . . . H46A H 0.6072 0.2024 0.5449 0.147 Uiso 1 1 calc R . . H46B H 0.6011 0.1967 0.6536 0.147 Uiso 1 1 calc R . . H46C H 0.5000 0.1390 0.5734 0.147 Uiso 1 1 calc R . . N10 N 0.6680(12) 0.0111(11) 0.5898(10) 0.101(4) Uani 1 1 d . . . C47 C 0.4671(19) 0.6248(11) 0.3248(15) 0.111(7) Uani 1 1 d . . . C48 C 0.4994(11) 0.5902(12) 0.4180(15) 0.115(7) Uani 1 1 d . . . H48A H 0.5246 0.6443 0.4664 0.172 Uiso 1 1 calc R . . H48B H 0.5591 0.5581 0.4167 0.172 Uiso 1 1 calc R . . H48C H 0.4358 0.5454 0.4324 0.172 Uiso 1 1 calc R . . N11 N 0.439(3) 0.6547(14) 0.2557(17) 0.216(14) Uani 1 1 d . . . C50 C 1.0356(10) 0.0081(10) 0.4136(9) 0.073(3) Uani 1 1 d . . . H50 H 1.0602 0.0141 0.3559 0.087 Uiso 1 1 calc R . . C51 C 0.9847(10) 0.0796(9) 0.4469(10) 0.070(3) Uani 1 1 d . . . H51 H 0.9746 0.1310 0.4107 0.084 Uiso 1 1 calc R . . C52 C 0.9502(10) 0.0718(9) 0.5342(11) 0.076(4) Uani 1 1 d . . . H52 H 0.9182 0.1187 0.5577 0.091 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 C1 0.025(3) 0.024(3) 0.029(3) 0.000(2) 0.005(2) 0.014(3) C2 0.032(3) 0.029(4) 0.025(3) 0.001(3) 0.008(3) 0.007(3) C3 0.034(3) 0.022(3) 0.023(3) 0.005(2) 0.003(3) 0.005(3) C4 0.028(3) 0.019(3) 0.020(3) 0.002(2) -0.001(2) 0.012(3) C5 0.028(3) 0.020(3) 0.025(3) 0.001(2) -0.002(2) 0.014(3) C6 0.024(3) 0.021(3) 0.030(3) -0.002(2) -0.003(2) 0.012(3) C7 0.023(3) 0.028(4) 0.039(4) -0.004(3) 0.001(3) 0.013(3) C8 0.025(3) 0.029(4) 0.039(4) 0.000(3) 0.007(3) 0.007(3) C9 0.031(3) 0.022(3) 0.028(3) 0.000(3) 0.003(3) 0.006(3) C10 0.033(3) 0.031(4) 0.023(3) 0.000(3) -0.001(3) 0.015(3) C11 0.054(5) 0.030(4) 0.030(4) 0.000(3) -0.013(3) 0.018(4) C12 0.064(6) 0.042(5) 0.044(5) -0.002(4) -0.026(4) 0.024(5) C13 0.058(5) 0.036(5) 0.046(5) 0.000(4) -0.008(4) 0.031(4) C14 0.043(4) 0.026(4) 0.040(4) 0.002(3) -0.007(3) 0.022(3) C15 0.027(3) 0.023(3) 0.031(3) 0.003(3) 0.002(3) 0.009(3) C16 0.024(3) 0.031(4) 0.040(4) 0.000(3) -0.004(3) 0.001(3) C17 0.025(3) 0.037(4) 0.031(3) 0.005(3) -0.005(3) 0.010(3) C18 0.024(3) 0.023(3) 0.022(3) 0.004(2) 0.001(2) 0.016(3) C19 0.025(3) 0.022(3) 0.022(3) 0.004(2) 0.006(2) 0.016(3) C20 0.025(3) 0.021(3) 0.021(3) 0.005(2) 0.006(2) 0.010(3) C21 0.031(3) 0.020(3) 0.025(3) 0.005(2) 0.007(2) 0.010(3) C22 0.029(3) 0.018(3) 0.025(3) -0.002(2) 0.004(2) 0.005(3) C23 0.023(3) 0.023(3) 0.022(3) 0.002(2) 0.001(2) 0.007(3) C24 0.025(3) 0.022(3) 0.021(3) 0.004(2) 0.002(2) 0.013(3) C25 0.044(4) 0.035(4) 0.032(3) 0.016(3) 0.019(3) 0.027(4) C26 0.046(4) 0.041(4) 0.036(4) 0.015(3) 0.017(3) 0.025(4) C27 0.035(4) 0.022(3) 0.027(3) 0.008(2) 0.008(3) 0.013(3) C28 0.028(3) 0.029(4) 0.026(3) 0.007(3) 0.005(2) 0.010(3) C29 0.031(4) 0.029(4) 0.041(4) 0.011(3) 0.006(3) 0.011(3) C30 0.029(3) 0.024(3) 0.035(4) 0.006(3) 0.006(3) 0.006(3) C31 0.021(3) 0.017(3) 0.032(3) 0.003(2) -0.003(2) 0.010(3) C32 0.040(4) 0.022(3) 0.031(3) -0.002(3) -0.001(3) 0.011(3) C33 0.048(4) 0.021(4) 0.042(4) -0.003(3) 0.001(3) 0.017(3) C34 0.023(3) 0.016(3) 0.021(3) -0.002(2) -0.002(2) 0.007(2) C35 0.037(4) 0.024(3) 0.020(3) -0.001(2) 0.002(2) 0.013(3) C36 0.019(3) 0.025(3) 0.023(3) 0.001(2) -0.002(2) 0.008(3) C37 0.033(3) 0.021(3) 0.021(3) 0.001(2) -0.002(2) 0.010(3) C38 0.042(4) 0.024(3) 0.020(3) 0.000(2) -0.002(3) 0.014(3) C39 0.048(4) 0.033(4) 0.017(3) 0.001(3) 0.002(3) 0.021(3) C40 0.045(4) 0.025(4) 0.030(3) 0.005(3) 0.006(3) 0.019(3) C41 0.038(4) 0.027(4) 0.029(3) 0.005(3) 0.003(3) 0.016(3) C42 0.040(4) 0.049(5) 0.036(4) 0.011(3) 0.013(3) 0.017(4) C43 0.046(6) 0.150(13) 0.055(6) 0.032(7) 0.024(5) 0.026(7) N1 0.023(2) 0.018(3) 0.018(2) 0.0024(18) 0.0006(18) 0.008(2) N2 0.026(3) 0.018(3) 0.024(3) 0.0011(19) 0.000(2) 0.009(2) N3 0.071(5) 0.043(4) 0.046(4) -0.002(3) -0.021(4) 0.031(4) N4 0.022(2) 0.020(3) 0.023(2) 0.003(2) -0.0014(19) 0.007(2) N5 0.022(2) 0.019(3) 0.020(2) 0.0025(19) 0.0017(19) 0.010(2) N6 0.036(3) 0.028(3) 0.026(3) 0.008(2) 0.001(2) 0.018(3) N7 0.036(3) 0.021(3) 0.050(4) 0.007(3) 0.001(3) 0.010(3) N8 0.037(3) 0.026(3) 0.023(3) 0.005(2) -0.001(2) 0.018(3) N9 0.043(4) 0.042(4) 0.048(4) 0.004(3) 0.011(3) 0.010(3) O1 0.033(2) 0.019(2) 0.025(2) 0.0053(17) 0.0038(18) 0.008(2) O2 0.032(2) 0.019(2) 0.022(2) 0.0023(16) 0.0002(17) 0.012(2) Co1 0.0221(4) 0.0155(4) 0.0182(4) 0.0023(3) 0.0003(3) 0.0086(3) Ag1 0.0375(3) 0.0440(4) 0.0366(3) 0.0198(2) 0.0076(2) 0.0218(3) C44 0.079(8) 0.058(6) 0.044(5) -0.005(4) 0.007(5) 0.027(6) O3 0.066(4) 0.078(5) 0.048(4) 0.023(3) 0.025(3) 0.005(4) O4 0.067(4) 0.048(4) 0.047(4) -0.006(3) 0.016(3) 0.001(3) O5 0.064(4) 0.052(4) 0.050(4) -0.001(3) 0.005(3) -0.007(3) F1 0.057(4) 0.125(7) 0.089(5) -0.010(5) 0.002(4) 0.035(4) F2 0.161(8) 0.108(6) 0.069(5) -0.021(4) -0.007(5) 0.087(6) F3 0.188(10) 0.113(7) 0.060(4) 0.043(4) 0.014(5) 0.061(7) S1 0.0430(11) 0.0382(11) 0.0323(9) 0.0050(8) 0.0077(8) 0.0034(9) C45 0.069(8) 0.072(8) 0.087(9) 0.018(7) 0.026(6) 0.022(7) C46 0.143(14) 0.072(9) 0.114(12) 0.036(8) 0.081(11) 0.047(10) N10 0.104(10) 0.101(10) 0.100(10) 0.024(8) 0.017(8) 0.032(8) C47 0.165(18) 0.063(9) 0.109(13) -0.010(9) 0.085(14) -0.006(10) C48 0.051(7) 0.107(12) 0.172(18) -0.059(12) 0.038(9) -0.007(8) N11 0.37(4) 0.114(14) 0.160(19) 0.023(13) 0.15(2) -0.038(18) C50 0.059(7) 0.084(9) 0.061(7) 0.006(6) 0.001(5) -0.001(6) C51 0.053(6) 0.058(7) 0.086(9) 0.010(6) -0.007(6) 0.004(5) C52 0.051(6) 0.056(7) 0.104(10) -0.002(7) -0.007(6) 0.001(5) _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 C1 N1 1.319(8) . ? C1 C2 1.414(9) . ? C1 H1 0.9300 . ? C2 C3 1.369(10) . ? C2 H2 0.9300 . ? C3 C4 1.425(9) . ? C3 H3 0.9300 . ? C4 C5 1.400(9) . ? C4 N1 1.404(8) . ? C5 C6 1.385(10) . ? C5 C10 1.489(9) . ? C6 N2 1.390(8) . ? C6 C7 1.428(9) . ? C7 C8 1.373(11) . ? C7 H7 0.9300 . ? C8 C9 1.404(10) . ? C8 H8 0.9300 . ? C9 N2 1.336(9) . ? C9 H9 0.9300 . ? C10 C14 1.380(11) . ? C10 C11 1.389(10) . ? C11 C12 1.367(11) . ? C11 H11 0.9300 . ? C12 N3 1.346(12) . ? C12 H12 0.9300 . ? C13 N3 1.333(11) . ? C13 C14 1.362(11) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N4 1.326(8) . ? C15 C16 1.421(10) . ? C15 H15 0.9300 . ? C16 C17 1.341(11) . ? C16 H16 0.9300 . ? C17 C18 1.423(9) . ? C17 H17 0.9300 . ? C18 N4 1.390(8) . ? C18 C19 1.408(9) 2_566 ? C19 C20 1.388(9) 2_566 ? C19 C18 1.408(9) 2_566 ? C19 C24 1.497(9) . ? C20 C19 1.388(9) 2_566 ? C20 N5 1.402(8) . ? C20 C21 1.421(9) . ? C21 C22 1.393(9) . ? C21 H21 0.9300 . ? C22 C23 1.400(9) . ? C22 H22 0.9300 . ? C23 N5 1.334(8) . ? C23 H23 0.9300 . ? C24 C28 1.386(9) . ? C24 C25 1.393(9) . ? C25 C26 1.373(11) . ? C25 H25 0.9300 . ? C26 N6 1.342(9) . ? C26 H26 0.9300 . ? C27 N6 1.325(9) . ? C27 C28 1.388(10) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 N7 1.340(10) . ? C29 C30 1.374(10) . ? C29 H29 0.9300 . ? C30 C31 1.387(9) . ? C30 H30 0.9300 . ? C31 C32 1.386(10) . ? C31 C34 1.505(9) . ? C32 C33 1.373(10) . ? C32 H32 0.9300 . ? C33 N7 1.353(10) . ? C33 H33 0.9300 . ? C34 O1 1.290(8) . ? C34 C35 1.382(9) . ? C35 C36 1.385(10) . ? C35 H35 0.9300 . ? C36 O2 1.286(8) . ? C36 C37 1.492(9) . ? C37 C38 1.377(10) . ? C37 C41 1.399(10) . ? C38 C39 1.390(9) . ? C38 H38 0.9300 . ? C39 N8 1.339(10) . ? C39 H39 0.9300 . ? C40 N8 1.337(9) . ? C40 C41 1.382(10) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 N9 1.093(11) . ? C42 C43 1.464(13) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? N1 Co1 1.914(5) . ? N2 Co1 1.919(6) . ? N4 Co1 1.938(5) . ? N5 Co1 1.900(5) . ? N6 Ag1 2.270(6) . ? N8 Ag1 2.242(6) . ? N9 Ag1 2.308(7) . ? O1 Co1 1.900(5) . ? O2 Co1 1.903(4) . ? C44 F3 1.321(13) . ? C44 F1 1.331(14) . ? C44 F2 1.344(12) . ? C44 S1 1.792(12) . ? O3 S1 1.432(6) . ? O4 S1 1.440(7) . ? O5 S1 1.425(7) . ? C45 N10 1.166(18) . ? C45 C46 1.44(2) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 N11 1.11(3) . ? C47 C48 1.45(3) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C50 C52 1.409(18) 2_756 ? C50 C51 1.422(19) . ? C50 H50 0.9300 . ? C51 C52 1.392(19) . ? C51 H51 0.9300 . ? C52 C50 1.409(18) 2_756 ? C52 H52 0.9300 . ? 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 C1 C2 111.6(6) . . ? N1 C1 H1 124.2 . . ? C2 C1 H1 124.2 . . ? C3 C2 C1 106.4(6) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.1(6) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? C5 C4 N1 123.3(6) . . ? C5 C4 C3 128.6(6) . . ? N1 C4 C3 107.9(6) . . ? C6 C5 C4 124.5(6) . . ? C6 C5 C10 116.2(6) . . ? C4 C5 C10 119.3(6) . . ? C5 C6 N2 123.3(6) . . ? C5 C6 C7 127.6(6) . . ? N2 C6 C7 108.4(6) . . ? C8 C7 C6 106.7(6) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? C7 C8 C9 106.8(6) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N2 C9 C8 111.2(6) . . ? N2 C9 H9 124.4 . . ? C8 C9 H9 124.4 . . ? C14 C10 C11 117.9(7) . . ? C14 C10 C5 120.7(6) . . ? C11 C10 C5 121.3(6) . . ? C12 C11 C10 117.7(7) . . ? C12 C11 H11 121.2 . . ? C10 C11 H11 121.2 . . ? N3 C12 C11 125.6(8) . . ? N3 C12 H12 117.2 . . ? C11 C12 H12 117.2 . . ? N3 C13 C14 124.4(8) . . ? N3 C13 H13 117.8 . . ? C14 C13 H13 117.8 . . ? C13 C14 C10 119.6(7) . . ? C13 C14 H14 120.2 . . ? C10 C14 H14 120.2 . . ? N4 C15 C16 110.5(6) . . ? N4 C15 H15 124.7 . . ? C16 C15 H15 124.7 . . ? C17 C16 C15 106.9(6) . . ? C17 C16 H16 126.5 . . ? C15 C16 H16 126.5 . . ? C16 C17 C18 107.5(6) . . ? C16 C17 H17 126.2 . . ? C18 C17 H17 126.2 . . ? N4 C18 C19 123.2(6) . 2_566 ? N4 C18 C17 108.1(6) . . ? C19 C18 C17 128.7(6) 2_566 . ? C20 C19 C18 125.1(6) 2_566 2_566 ? C20 C19 C24 117.4(6) 2_566 . ? C18 C19 C24 117.5(6) 2_566 . ? C19 C20 N5 123.1(6) 2_566 . ? C19 C20 C21 128.1(6) 2_566 . ? N5 C20 C21 108.6(5) . . ? C22 C21 C20 106.6(6) . . ? C22 C21 H21 126.7 . . ? C20 C21 H21 126.7 . . ? C21 C22 C23 106.2(6) . . ? C21 C22 H22 126.9 . . ? C23 C22 H22 126.9 . . ? N5 C23 C22 112.0(6) . . ? N5 C23 H23 124.0 . . ? C22 C23 H23 124.0 . . ? C28 C24 C25 117.9(6) . . ? C28 C24 C19 120.8(6) . . ? C25 C24 C19 121.3(6) . . ? C26 C25 C24 119.0(6) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N6 C26 C25 123.3(7) . . ? N6 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? N6 C27 C28 123.2(6) . . ? N6 C27 H27 118.4 . . ? C28 C27 H27 118.4 . . ? C24 C28 C27 118.9(6) . . ? C24 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? N7 C29 C30 123.8(7) . . ? N7 C29 H29 118.1 . . ? C30 C29 H29 118.1 . . ? C29 C30 C31 119.6(7) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 117.4(6) . . ? C32 C31 C34 123.9(6) . . ? C30 C31 C34 118.7(6) . . ? C33 C32 C31 119.5(7) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? N7 C33 C32 123.6(7) . . ? N7 C33 H33 118.2 . . ? C32 C33 H33 118.2 . . ? O1 C34 C35 125.2(6) . . ? O1 C34 C31 113.8(5) . . ? C35 C34 C31 121.0(6) . . ? C34 C35 C36 124.4(6) . . ? C34 C35 H35 117.8 . . ? C36 C35 H35 117.8 . . ? O2 C36 C35 126.1(6) . . ? O2 C36 C37 113.4(6) . . ? C35 C36 C37 120.6(6) . . ? C38 C37 C41 118.7(6) . . ? C38 C37 C36 122.6(6) . . ? C41 C37 C36 118.7(6) . . ? C37 C38 C39 118.2(7) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? N8 C39 C38 124.4(7) . . ? N8 C39 H39 117.8 . . ? C38 C39 H39 117.8 . . ? N8 C40 C41 124.0(7) . . ? N8 C40 H40 118.0 . . ? C41 C40 H40 118.0 . . ? C40 C41 C37 118.5(7) . . ? C40 C41 H41 120.8 . . ? C37 C41 H41 120.8 . . ? N9 C42 C43 179.0(10) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C1 N1 C4 106.9(5) . . ? C1 N1 Co1 127.2(4) . . ? C4 N1 Co1 125.1(4) . . ? C9 N2 C6 106.9(6) . . ? C9 N2 Co1 126.7(5) . . ? C6 N2 Co1 125.7(5) . . ? C13 N3 C12 114.8(7) . . ? C15 N4 C18 107.0(5) . . ? C15 N4 Co1 125.9(5) . . ? C18 N4 Co1 125.0(4) . . ? C23 N5 C20 106.5(5) . . ? C23 N5 Co1 126.8(4) . . ? C20 N5 Co1 126.4(4) . . ? C27 N6 C26 117.6(6) . . ? C27 N6 Ag1 121.8(4) . . ? C26 N6 Ag1 120.2(5) . . ? C29 N7 C33 116.1(6) . . ? C40 N8 C39 116.4(6) . . ? C40 N8 Ag1 119.6(5) . . ? C39 N8 Ag1 124.1(5) . . ? C42 N9 Ag1 178.6(8) . . ? C34 O1 Co1 124.3(4) . . ? C36 O2 Co1 124.0(4) . . ? N5 Co1 O1 177.2(2) . . ? N5 Co1 O2 86.8(2) . . ? O1 Co1 O2 95.00(19) . . ? N5 Co1 N1 92.1(2) . . ? O1 Co1 N1 86.2(2) . . ? O2 Co1 N1 178.4(2) . . ? N5 Co1 N2 91.7(2) . . ? O1 Co1 N2 86.2(2) . . ? O2 Co1 N2 90.0(2) . . ? N1 Co1 N2 91.1(2) . . ? N5 Co1 N4 91.9(2) . . ? O1 Co1 N4 90.4(2) . . ? O2 Co1 N4 85.6(2) . . ? N1 Co1 N4 93.4(2) . . ? N2 Co1 N4 174.2(2) . . ? N8 Ag1 N6 127.9(2) . . ? N8 Ag1 N9 119.4(2) . . ? N6 Ag1 N9 106.0(2) . . ? F3 C44 F1 106.3(9) . . ? F3 C44 F2 105.2(10) . . ? F1 C44 F2 108.5(10) . . ? F3 C44 S1 112.6(9) . . ? F1 C44 S1 112.4(8) . . ? F2 C44 S1 111.4(7) . . ? O5 S1 O3 114.4(4) . . ? O5 S1 O4 115.1(4) . . ? O3 S1 O4 114.9(4) . . ? O5 S1 C44 104.6(5) . . ? O3 S1 C44 101.4(5) . . ? O4 S1 C44 104.2(5) . . ? N10 C45 C46 175.7(16) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N11 C47 C48 176(2) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C52 C50 C51 121.6(12) 2_756 . ? C52 C50 H50 119.2 2_756 . ? C51 C50 H50 119.2 . . ? C52 C51 C50 119.3(12) . . ? C52 C51 H51 120.3 . . ? C50 C51 H51 120.3 . . ? C51 C52 C50 119.1(13) . 2_756 ? C51 C52 H52 120.5 . . ? C50 C52 H52 120.5 2_756 . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 3.362 _refine_diff_density_min -1.338 _refine_diff_density_rms 0.163 #===END ###Material relevant to compound 9 at 173K ## data_compound9 _database_code_depnum_ccdc_archive 'CCDC 868791' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H32 Ag Co N9 O2, C6 H6, C F3 O3 S' _chemical_formula_sum 'C50 H38 Ag Co F3 N9 O5 S' _chemical_formula_weight 1100.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4689(7) _cell_length_b 24.9231(14) _cell_length_c 15.5837(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.821(2) _cell_angle_gamma 90.00 _cell_volume 5169.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9946 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9097 _exptl_absorpt_correction_T_max 0.9385 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41850 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.58 _reflns_number_total 11781 _reflns_number_gt 9823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+26.0601P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11781 _refine_ls_number_parameters 590 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2635 _refine_ls_wR_factor_gt 0.2446 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _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 C1 C 0.7941(5) 0.0610(3) 0.6072(4) 0.0406(14) Uani 1 1 d . . . H1 H 0.7568 0.0585 0.5519 0.049 Uiso 1 1 calc R . . C2 C 0.8792(6) 0.0288(3) 0.6388(5) 0.0489(16) Uani 1 1 d . . . H2 H 0.9075 0.0023 0.6082 0.059 Uiso 1 1 calc R . . C3 C 0.9112(5) 0.0441(3) 0.7219(5) 0.0441(15) Uani 1 1 d . . . H3 H 0.9654 0.0298 0.7591 0.053 Uiso 1 1 calc R . . C4 C 0.8474(4) 0.0858(2) 0.7420(4) 0.0334(12) Uani 1 1 d . . . C5 C 0.8447(4) 0.1105(2) 0.8212(4) 0.0330(12) Uani 1 1 d . . . C6 C 0.7698(4) 0.1450(2) 0.8399(3) 0.0310(11) Uani 1 1 d . . . C7 C 0.7549(5) 0.1666(3) 0.9220(4) 0.0420(14) Uani 1 1 d . . . H7 H 0.7970 0.1623 0.9747 0.050 Uiso 1 1 calc R . . C8 C 0.6670(5) 0.1945(3) 0.9082(4) 0.0420(14) Uani 1 1 d . . . H8 H 0.6376 0.2129 0.9498 0.050 Uiso 1 1 calc R . . C9 C 0.6290(5) 0.1905(2) 0.8195(4) 0.0355(12) Uani 1 1 d . . . H9 H 0.5693 0.2060 0.7930 0.043 Uiso 1 1 calc R . . C10 C 0.9287(4) 0.0989(3) 0.8934(4) 0.0365(12) Uani 1 1 d . . . C11 C 1.0236(5) 0.1172(4) 0.8898(5) 0.059(2) Uani 1 1 d . . . H11 H 1.0374 0.1355 0.8409 0.070 Uiso 1 1 calc R . . C12 C 1.0995(5) 0.1084(4) 0.9597(5) 0.058(2) Uani 1 1 d . . . H12 H 1.1629 0.1223 0.9568 0.069 Uiso 1 1 calc R . . C13 C 0.9929(5) 0.0623(3) 1.0333(4) 0.0403(14) Uani 1 1 d . . . H13 H 0.9813 0.0434 1.0823 0.048 Uiso 1 1 calc R . . C14 C 0.9136(5) 0.0696(3) 0.9666(4) 0.0396(13) Uani 1 1 d . . . H14 H 0.8508 0.0552 0.9706 0.048 Uiso 1 1 calc R . . C15 C 0.7448(5) 0.1736(3) 0.4845(4) 0.0404(13) Uani 1 1 d . . . H15 H 0.8077 0.1864 0.5090 0.048 Uiso 1 1 calc R . . C16 C 0.7081(6) 0.1725(3) 0.3949(4) 0.0508(17) Uani 1 1 d . . . H16 H 0.7419 0.1841 0.3505 0.061 Uiso 1 1 calc R . . C17 C 0.6144(6) 0.1514(3) 0.3855(4) 0.0442(15) Uani 1 1 d . . . H17 H 0.5720 0.1458 0.3333 0.053 Uiso 1 1 calc R . . C18 C 0.5923(4) 0.1392(2) 0.4698(4) 0.0339(12) Uani 1 1 d . . . C19 C 0.5087(4) 0.1135(2) 0.4921(4) 0.0327(12) Uani 1 1 d . . . C20 C 0.4972(4) 0.0971(2) 0.5753(4) 0.0317(11) Uani 1 1 d . . . C21 C 0.4203(5) 0.0659(3) 0.6020(4) 0.0430(14) Uani 1 1 d . . . H21 H 0.3621 0.0543 0.5669 0.052 Uiso 1 1 calc R . . C22 C 0.4462(6) 0.0557(3) 0.6883(5) 0.0507(17) Uani 1 1 d . . . H22 H 0.4096 0.0361 0.7234 0.061 Uiso 1 1 calc R . . C23 C 0.5400(5) 0.0811(3) 0.7140(4) 0.0412(14) Uani 1 1 d . . . H23 H 0.5755 0.0805 0.7701 0.049 Uiso 1 1 calc R . . C24 C 0.4252(5) 0.1008(3) 0.4201(4) 0.0376(13) Uani 1 1 d . . . C25 C 0.3653(7) 0.1422(4) 0.3816(6) 0.079(3) Uani 1 1 d . . . H25 H 0.3740 0.1771 0.4024 0.095 Uiso 1 1 calc R . . C26 C 1.2923(7) 0.1305(4) 1.3117(6) 0.080(3) Uani 1 1 d . . . H26 H 1.2521 0.1584 1.2867 0.096 Uiso 1 1 calc R . . C27 C 1.3327(6) 0.0429(3) 1.3153(4) 0.0472(16) Uani 1 1 d . . . H27 H 1.3224 0.0084 1.2929 0.057 Uiso 1 1 calc R . . C28 C 0.4079(5) 0.0505(3) 0.3871(4) 0.0437(15) Uani 1 1 d . . . H28 H 0.4455 0.0216 0.4118 0.052 Uiso 1 1 calc R . . C29 C 1.4467(5) 0.1159(3) 1.1339(5) 0.0448(15) Uani 1 1 d . . . H29 H 1.4538 0.0792 1.1444 0.054 Uiso 1 1 calc R . . C30 C 1.5327(5) 0.1475(2) 1.1432(4) 0.0370(12) Uani 1 1 d . . . H30 H 1.5956 0.1319 1.1588 0.044 Uiso 1 1 calc R . . C31 C 1.5245(4) 0.2017(2) 1.1292(4) 0.0347(12) Uani 1 1 d . . . C32 C 1.4285(5) 0.2229(3) 1.1047(8) 0.075(3) Uani 1 1 d . . . H32 H 1.4195 0.2594 1.0938 0.090 Uiso 1 1 calc R . . C33 C 1.3463(6) 0.1881(4) 1.0967(9) 0.088(4) Uani 1 1 d . . . H33 H 1.2825 0.2026 1.0807 0.106 Uiso 1 1 calc R . . C34 C 0.6129(4) 0.2607(2) 0.6396(3) 0.0292(11) Uani 1 1 d . . . C35 C 0.7098(4) 0.2813(2) 0.6505(4) 0.0320(11) Uani 1 1 d . . . H35 H 0.7176 0.3184 0.6502 0.038 Uiso 1 1 calc R . . C36 C 0.7964(4) 0.2493(2) 0.6621(3) 0.0289(10) Uani 1 1 d . . . C37 C 0.8987(4) 0.2744(3) 0.6712(4) 0.0354(12) Uani 1 1 d . . . C38 C 0.9168(5) 0.3264(3) 0.6949(5) 0.0477(16) Uani 1 1 d . . . H38 H 0.8647 0.3487 0.7056 0.057 Uiso 1 1 calc R . . C39 C 1.0148(6) 0.3456(3) 0.7028(6) 0.058(2) Uani 1 1 d . . . H39 H 1.0261 0.3808 0.7214 0.070 Uiso 1 1 calc R . . C40 C 1.0729(6) 0.2679(5) 0.6617(8) 0.089(4) Uani 1 1 d . . . H40 H 1.1261 0.2473 0.6487 0.107 Uiso 1 1 calc R . . C41 C 0.9799(5) 0.2443(4) 0.6544(6) 0.063(2) Uani 1 1 d . . . H41 H 0.9715 0.2085 0.6383 0.076 Uiso 1 1 calc R . . C43 C 1.4415(7) -0.0607(4) 1.0395(7) 0.066(2) Uani 1 1 d . . . H43A H 1.5085 -0.0477 1.0578 0.100 Uiso 1 1 calc R . . H43B H 1.4262 -0.0593 0.9774 0.100 Uiso 1 1 calc R . . H43C H 1.4366 -0.0971 1.0586 0.100 Uiso 1 1 calc R . . C44 C 1.3718(6) -0.0280(3) 1.0766(5) 0.0444(15) Uani 1 1 d . . . N1 N 0.7755(4) 0.09517(19) 0.6686(3) 0.0307(9) Uani 1 1 d . . . N2 N 0.6902(3) 0.16143(19) 0.7782(3) 0.0301(9) Uani 1 1 d . . . N3 N 1.0862(4) 0.0812(2) 1.0308(3) 0.0397(12) Uani 1 1 d . . . N4 N 0.6754(4) 0.15342(19) 0.5296(3) 0.0315(10) Uani 1 1 d . . . N5 N 0.5708(4) 0.10600(19) 0.6473(3) 0.0320(10) Uani 1 1 d . . . N6 N 1.2761(5) 0.0815(3) 1.2781(4) 0.0497(14) Uani 1 1 d . . . N7 N 1.0917(5) 0.3182(3) 0.6861(5) 0.067(2) Uani 1 1 d . . . N8 N 1.3539(5) 0.1357(3) 1.1106(5) 0.0584(17) Uani 1 1 d . . . N9 N 1.3163(5) -0.0019(3) 1.1059(4) 0.0535(15) Uani 1 1 d . . . O1 O 0.5890(3) 0.21145(15) 0.6378(2) 0.0298(8) Uani 1 1 d . . . O2 O 0.7979(3) 0.19846(16) 0.6635(2) 0.0310(8) Uani 1 1 d . . . Co1 Co 0.68280(5) 0.15357(3) 0.65402(5) 0.02644(19) Uani 1 1 d . . . Ag1 Ag 1.20936(4) 0.07636(2) 1.13840(3) 0.04747(19) Uani 1 1 d . . . C42 C 0.2037(7) 0.9728(4) 0.7257(8) 0.074(3) Uani 1 1 d . . . O3 O 0.2474(5) 0.9194(2) 0.8677(6) 0.080(2) Uani 1 1 d . . . O4 O 0.1680(7) 1.0051(3) 0.8694(6) 0.109(3) Uani 1 1 d . . . O5 O 0.3406(6) 0.9990(3) 0.8490(5) 0.089(2) Uani 1 1 d . . . F1 F 0.1140(6) 0.9494(3) 0.7050(6) 0.129(3) Uani 1 1 d . . . F2 F 0.1955(6) 1.0204(3) 0.6897(4) 0.102(2) Uani 1 1 d . . . F3 F 0.2672(8) 0.9463(5) 0.6832(6) 0.154(4) Uani 1 1 d . . . S1 S 0.24490(16) 0.97428(7) 0.83999(15) 0.0562(5) Uani 1 1 d . . . C45 C -0.0010(8) 0.1691(7) 0.4331(8) 0.165(4) Uani 1 1 d G . . H45 H -0.0651 0.1713 0.4011 0.198 Uiso 1 1 calc R . . C46 C 0.0716(12) 0.2067(6) 0.4204(8) 0.165(4) Uani 1 1 d G . . H46 H 0.0561 0.2341 0.3800 0.198 Uiso 1 1 calc R . . C47 C 0.1675(10) 0.2034(6) 0.4681(10) 0.165(4) Uani 1 1 d G . . H47 H 0.2161 0.2285 0.4597 0.198 Uiso 1 1 calc R . . C48 C 0.1907(8) 0.1625(7) 0.5286(8) 0.165(4) Uani 1 1 d G . . H48 H 0.2548 0.1603 0.5605 0.198 Uiso 1 1 calc R . . C49 C 0.1181(12) 0.1249(6) 0.5412(8) 0.165(4) Uani 1 1 d G . . H49 H 0.1336 0.0976 0.5817 0.198 Uiso 1 1 calc R . . C50 C 0.0222(10) 0.1282(6) 0.4935(10) 0.165(4) Uani 1 1 d G . . H50 H -0.0264 0.1031 0.5020 0.198 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 C1 0.050(4) 0.038(3) 0.034(3) 0.000(2) 0.004(3) 0.009(3) C2 0.056(4) 0.039(3) 0.052(4) -0.003(3) 0.011(3) 0.019(3) C3 0.036(3) 0.045(4) 0.050(4) 0.008(3) 0.003(3) 0.014(3) C4 0.027(3) 0.035(3) 0.037(3) 0.006(2) -0.001(2) 0.005(2) C5 0.025(2) 0.039(3) 0.032(3) 0.006(2) -0.005(2) -0.002(2) C6 0.027(2) 0.036(3) 0.027(2) 0.003(2) -0.008(2) -0.001(2) C7 0.045(3) 0.042(3) 0.036(3) -0.004(3) -0.002(3) 0.001(3) C8 0.050(4) 0.043(3) 0.033(3) -0.004(2) 0.005(3) 0.009(3) C9 0.035(3) 0.039(3) 0.032(3) 0.001(2) 0.001(2) 0.008(2) C10 0.025(3) 0.042(3) 0.037(3) 0.001(2) -0.009(2) 0.001(2) C11 0.033(3) 0.087(6) 0.053(4) 0.023(4) -0.004(3) -0.009(4) C12 0.027(3) 0.088(6) 0.053(4) 0.022(4) -0.012(3) -0.015(3) C13 0.032(3) 0.046(3) 0.039(3) 0.006(3) -0.009(2) -0.003(3) C14 0.029(3) 0.046(3) 0.040(3) 0.005(3) -0.007(2) -0.006(2) C15 0.043(3) 0.043(3) 0.035(3) 0.002(2) 0.005(2) -0.002(3) C16 0.067(5) 0.052(4) 0.034(3) 0.004(3) 0.011(3) -0.002(3) C17 0.054(4) 0.046(4) 0.030(3) -0.001(3) -0.002(3) 0.005(3) C18 0.038(3) 0.034(3) 0.026(2) -0.001(2) -0.007(2) 0.009(2) C19 0.030(3) 0.027(3) 0.036(3) -0.004(2) -0.010(2) 0.006(2) C20 0.027(3) 0.030(3) 0.035(3) 0.001(2) -0.006(2) 0.002(2) C21 0.029(3) 0.051(4) 0.045(3) 0.008(3) -0.008(2) -0.002(3) C22 0.044(4) 0.053(4) 0.053(4) 0.011(3) 0.002(3) -0.013(3) C23 0.039(3) 0.043(3) 0.039(3) 0.008(3) -0.001(3) -0.013(3) C24 0.033(3) 0.039(3) 0.037(3) -0.007(2) -0.007(2) 0.003(2) C25 0.079(6) 0.060(5) 0.080(6) -0.034(5) -0.043(5) 0.037(5) C26 0.077(6) 0.080(6) 0.067(5) -0.031(5) -0.038(5) 0.047(5) C27 0.055(4) 0.045(4) 0.035(3) -0.003(3) -0.013(3) -0.009(3) C28 0.055(4) 0.036(3) 0.033(3) 0.000(2) -0.015(3) 0.000(3) C29 0.037(3) 0.037(3) 0.062(4) -0.002(3) 0.013(3) -0.005(3) C30 0.029(3) 0.034(3) 0.048(3) -0.001(2) 0.008(2) 0.000(2) C31 0.028(3) 0.036(3) 0.039(3) -0.006(2) 0.002(2) -0.004(2) C32 0.030(3) 0.034(4) 0.153(10) -0.003(5) -0.013(4) -0.006(3) C33 0.026(3) 0.051(5) 0.178(12) -0.002(6) -0.016(5) -0.006(3) C34 0.026(2) 0.032(3) 0.028(2) 0.001(2) 0.0007(19) 0.004(2) C35 0.028(3) 0.029(3) 0.038(3) -0.002(2) 0.001(2) 0.000(2) C36 0.025(2) 0.032(3) 0.028(2) 0.000(2) -0.0009(19) 0.000(2) C37 0.026(3) 0.043(3) 0.035(3) 0.002(2) 0.000(2) -0.002(2) C38 0.036(3) 0.041(4) 0.064(4) 0.006(3) 0.001(3) -0.006(3) C39 0.055(5) 0.049(4) 0.067(5) 0.008(4) -0.002(4) -0.024(4) C40 0.033(4) 0.113(9) 0.126(9) -0.052(7) 0.025(5) -0.014(5) C41 0.029(3) 0.072(5) 0.089(6) -0.031(5) 0.009(3) -0.007(3) C43 0.061(5) 0.066(5) 0.075(6) -0.009(4) 0.020(4) -0.006(4) C44 0.050(4) 0.037(3) 0.045(3) -0.002(3) 0.002(3) -0.007(3) N1 0.030(2) 0.028(2) 0.032(2) 0.0015(18) -0.0019(18) 0.0042(18) N2 0.024(2) 0.035(2) 0.030(2) 0.0006(18) -0.0029(17) 0.0040(18) N3 0.027(2) 0.051(3) 0.036(3) 0.001(2) -0.012(2) -0.005(2) N4 0.034(2) 0.029(2) 0.031(2) 0.0017(18) 0.0005(19) 0.0013(18) N5 0.029(2) 0.032(2) 0.032(2) 0.0031(18) -0.0047(18) 0.0001(18) N6 0.039(3) 0.065(4) 0.041(3) -0.013(3) -0.006(2) 0.007(3) N7 0.032(3) 0.087(6) 0.079(5) -0.004(4) 0.003(3) -0.021(3) N8 0.035(3) 0.040(3) 0.098(5) -0.012(3) 0.003(3) -0.012(2) N9 0.056(4) 0.049(3) 0.052(3) -0.003(3) -0.002(3) -0.005(3) O1 0.0239(17) 0.0297(19) 0.0330(19) 0.0013(15) -0.0043(14) 0.0008(14) O2 0.0245(18) 0.033(2) 0.0333(19) 0.0007(15) -0.0030(14) 0.0034(15) Co1 0.0236(3) 0.0269(4) 0.0266(4) 0.0012(3) -0.0033(3) 0.0014(3) Ag1 0.0304(3) 0.0621(4) 0.0434(3) -0.0034(2) -0.0148(2) -0.0021(2) C42 0.060(5) 0.052(5) 0.108(8) -0.017(5) 0.003(5) -0.006(4) O3 0.063(4) 0.043(3) 0.127(6) 0.008(3) -0.008(4) 0.002(3) O4 0.141(8) 0.085(5) 0.120(7) 0.028(5) 0.081(6) 0.043(5) O5 0.090(5) 0.106(6) 0.072(4) -0.001(4) 0.015(4) -0.055(5) F1 0.090(5) 0.101(5) 0.174(8) 0.029(5) -0.052(5) -0.043(4) F2 0.127(6) 0.090(5) 0.086(4) 0.021(3) 0.004(4) -0.031(4) F3 0.155(8) 0.185(9) 0.115(6) -0.076(6) 0.001(6) 0.056(7) S1 0.0544(11) 0.0353(9) 0.0832(14) -0.0011(8) 0.0241(10) -0.0071(7) C45 0.132(6) 0.226(12) 0.142(7) -0.032(6) 0.031(6) 0.028(7) C46 0.132(6) 0.226(12) 0.142(7) -0.032(6) 0.031(6) 0.028(7) C47 0.132(6) 0.226(12) 0.142(7) -0.032(6) 0.031(6) 0.028(7) C48 0.132(6) 0.226(12) 0.142(7) -0.032(6) 0.031(6) 0.028(7) C49 0.132(6) 0.226(12) 0.142(7) -0.032(6) 0.031(6) 0.028(7) C50 0.132(6) 0.226(12) 0.142(7) -0.032(6) 0.031(6) 0.028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.333(8) . ? C1 C2 1.424(9) . ? C1 H1 0.9300 . ? C2 C3 1.356(10) . ? C2 H2 0.9300 . ? C3 C4 1.414(9) . ? C3 H3 0.9300 . ? C4 C5 1.384(9) . ? C4 N1 1.400(7) . ? C5 C6 1.390(8) . ? C5 C10 1.497(7) . ? C6 N2 1.389(6) . ? C6 C7 1.430(9) . ? C7 C8 1.362(9) . ? C7 H7 0.9300 . ? C8 C9 1.402(8) . ? C8 H8 0.9300 . ? C9 N2 1.334(7) . ? C9 H9 0.9300 . ? C10 C11 1.367(9) . ? C10 C14 1.394(9) . ? C11 C12 1.393(9) . ? C11 H11 0.9300 . ? C12 N3 1.334(9) . ? C12 H12 0.9300 . ? C13 N3 1.348(8) . ? C13 C14 1.384(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N4 1.351(8) . ? C15 C16 1.407(9) . ? C15 H15 0.9300 . ? C16 C17 1.355(11) . ? C16 H16 0.9300 . ? C17 C18 1.423(9) . ? C17 H17 0.9300 . ? C18 C19 1.385(9) . ? C18 N4 1.388(7) . ? C19 C20 1.392(8) . ? C19 C24 1.496(7) . ? C20 N5 1.396(7) . ? C20 C21 1.408(9) . ? C21 C22 1.361(10) . ? C21 H21 0.9300 . ? C22 C23 1.415(9) . ? C22 H22 0.9300 . ? C23 N5 1.329(8) . ? C23 H23 0.9300 . ? C24 C28 1.362(9) . ? C24 C25 1.388(10) . ? C25 C26 1.382(11) 1_454 ? C25 H25 0.9300 . ? C26 N6 1.332(11) . ? C26 C25 1.382(11) 1_656 ? C26 H26 0.9300 . ? C27 N6 1.307(9) . ? C27 C28 1.402(8) 1_656 ? C27 H27 0.9300 . ? C28 C27 1.402(8) 1_454 ? C28 H28 0.9300 . ? C29 N8 1.340(9) . ? C29 C30 1.391(9) . ? C29 H29 0.9300 . ? C30 C31 1.371(9) . ? C30 H30 0.9300 . ? C31 C32 1.394(9) . ? C31 C34 1.504(7) 4_666 ? C32 C33 1.397(10) . ? C32 H32 0.9300 . ? C33 N8 1.326(11) . ? C33 H33 0.9300 . ? C34 O1 1.268(7) . ? C34 C35 1.388(8) . ? C34 C31 1.504(7) 4_465 ? C35 C36 1.401(8) . ? C35 H35 0.9300 . ? C36 O2 1.268(7) . ? C36 C37 1.500(8) . ? C37 C38 1.360(10) . ? C37 C41 1.384(10) . ? C38 C39 1.391(10) . ? C38 H38 0.9300 . ? C39 N7 1.300(12) . ? C39 H39 0.9300 . ? C40 N7 1.322(13) . ? C40 C41 1.373(11) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C43 C44 1.430(11) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 N9 1.139(10) . ? N1 Co1 1.909(5) . ? N2 Co1 1.932(5) . ? N3 Ag1 2.174(5) . ? N4 Co1 1.926(5) . ? N5 Co1 1.909(5) . ? N6 Ag1 2.227(6) . ? N8 Ag1 2.535(6) . ? N9 Ag1 2.521(7) . ? O1 Co1 1.908(4) . ? O2 Co1 1.899(4) . ? C42 F2 1.311(12) . ? C42 F3 1.335(13) . ? C42 F1 1.336(11) . ? C42 S1 1.783(12) . ? O3 S1 1.434(6) . ? O4 S1 1.419(7) . ? O5 S1 1.416(7) . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C45 H45 0.9300 . ? C46 C47 1.3900 . ? C46 H46 0.9300 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 C49 1.3900 . ? C48 H48 0.9300 . ? C49 C50 1.3900 . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? 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 C1 C2 110.0(6) . . ? N1 C1 H1 125.0 . . ? C2 C1 H1 125.0 . . ? C3 C2 C1 107.0(6) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 107.6(6) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? C5 C4 N1 123.0(5) . . ? C5 C4 C3 128.6(5) . . ? N1 C4 C3 108.0(5) . . ? C4 C5 C6 125.6(5) . . ? C4 C5 C10 117.7(5) . . ? C6 C5 C10 116.7(5) . . ? N2 C6 C5 123.0(5) . . ? N2 C6 C7 108.0(5) . . ? C5 C6 C7 128.8(5) . . ? C8 C7 C6 106.8(5) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C7 C8 C9 107.2(6) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N2 C9 C8 110.9(5) . . ? N2 C9 H9 124.6 . . ? C8 C9 H9 124.6 . . ? C11 C10 C14 117.6(6) . . ? C11 C10 C5 120.5(6) . . ? C14 C10 C5 121.9(5) . . ? C10 C11 C12 119.6(7) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? N3 C12 C11 123.6(6) . . ? N3 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? N3 C13 C14 123.2(6) . . ? N3 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C10 119.4(6) . . ? C13 C14 H14 120.3 . . ? C10 C14 H14 120.3 . . ? N4 C15 C16 110.1(6) . . ? N4 C15 H15 125.0 . . ? C16 C15 H15 125.0 . . ? C17 C16 C15 107.1(6) . . ? C17 C16 H16 126.4 . . ? C15 C16 H16 126.4 . . ? C16 C17 C18 107.8(6) . . ? C16 C17 H17 126.1 . . ? C18 C17 H17 126.1 . . ? C19 C18 N4 123.6(5) . . ? C19 C18 C17 128.5(5) . . ? N4 C18 C17 107.7(6) . . ? C18 C19 C20 125.5(5) . . ? C18 C19 C24 117.2(5) . . ? C20 C19 C24 117.3(5) . . ? C19 C20 N5 122.4(5) . . ? C19 C20 C21 129.0(5) . . ? N5 C20 C21 108.3(5) . . ? C22 C21 C20 107.8(6) . . ? C22 C21 H21 126.1 . . ? C20 C21 H21 126.1 . . ? C21 C22 C23 106.1(6) . . ? C21 C22 H22 126.9 . . ? C23 C22 H22 126.9 . . ? N5 C23 C22 111.1(6) . . ? N5 C23 H23 124.5 . . ? C22 C23 H23 124.5 . . ? C28 C24 C25 117.8(6) . . ? C28 C24 C19 122.8(6) . . ? C25 C24 C19 119.3(6) . . ? C26 C25 C24 118.7(8) 1_454 . ? C26 C25 H25 120.7 1_454 . ? C24 C25 H25 120.7 . . ? N6 C26 C25 123.9(8) . 1_656 ? N6 C26 H26 118.1 . . ? C25 C26 H26 118.1 1_656 . ? N6 C27 C28 123.7(7) . 1_656 ? N6 C27 H27 118.1 . . ? C28 C27 H27 118.1 1_656 . ? C24 C28 C27 119.1(6) . 1_454 ? C24 C28 H28 120.4 . . ? C27 C28 H28 120.4 1_454 . ? N8 C29 C30 123.1(6) . . ? N8 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? C31 C30 C29 119.9(6) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 117.7(6) . . ? C30 C31 C34 123.7(5) . 4_666 ? C32 C31 C34 118.7(6) . 4_666 ? C31 C32 C33 118.7(7) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? N8 C33 C32 123.8(7) . . ? N8 C33 H33 118.1 . . ? C32 C33 H33 118.1 . . ? O1 C34 C35 126.3(5) . . ? O1 C34 C31 114.0(5) . 4_465 ? C35 C34 C31 119.7(5) . 4_465 ? C34 C35 C36 123.5(5) . . ? C34 C35 H35 118.2 . . ? C36 C35 H35 118.2 . . ? O2 C36 C35 125.6(5) . . ? O2 C36 C37 113.7(5) . . ? C35 C36 C37 120.6(5) . . ? C38 C37 C41 117.0(6) . . ? C38 C37 C36 123.2(6) . . ? C41 C37 C36 119.8(6) . . ? C37 C38 C39 118.7(7) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? N7 C39 C38 125.2(8) . . ? N7 C39 H39 117.4 . . ? C38 C39 H39 117.4 . . ? N7 C40 C41 124.2(9) . . ? N7 C40 H40 117.9 . . ? C41 C40 H40 117.9 . . ? C40 C41 C37 119.3(8) . . ? C40 C41 H41 120.3 . . ? C37 C41 H41 120.3 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N9 C44 C43 179.8(9) . . ? C1 N1 C4 107.3(5) . . ? C1 N1 Co1 126.4(4) . . ? C4 N1 Co1 125.6(4) . . ? C9 N2 C6 107.1(5) . . ? C9 N2 Co1 126.7(4) . . ? C6 N2 Co1 125.4(4) . . ? C12 N3 C13 116.5(5) . . ? C12 N3 Ag1 119.0(4) . . ? C13 N3 Ag1 124.2(4) . . ? C15 N4 C18 107.3(5) . . ? C15 N4 Co1 126.2(4) . . ? C18 N4 Co1 126.0(4) . . ? C23 N5 C20 106.6(5) . . ? C23 N5 Co1 125.8(4) . . ? C20 N5 Co1 126.9(4) . . ? C27 N6 C26 116.8(6) . . ? C27 N6 Ag1 120.8(5) . . ? C26 N6 Ag1 117.0(6) . . ? C39 N7 C40 115.6(7) . . ? C33 N8 C29 117.0(6) . . ? C33 N8 Ag1 124.1(5) . . ? C29 N8 Ag1 116.5(5) . . ? C44 N9 Ag1 162.5(6) . . ? C34 O1 Co1 124.6(3) . . ? C36 O2 Co1 125.2(3) . . ? O2 Co1 O1 94.62(17) . . ? O2 Co1 N1 85.90(19) . . ? O1 Co1 N1 179.11(19) . . ? O2 Co1 N5 177.41(18) . . ? O1 Co1 N5 87.75(19) . . ? N1 Co1 N5 91.7(2) . . ? O2 Co1 N4 89.74(19) . . ? O1 Co1 N4 86.41(18) . . ? N1 Co1 N4 92.9(2) . . ? N5 Co1 N4 91.4(2) . . ? O2 Co1 N2 86.90(18) . . ? O1 Co1 N2 89.26(18) . . ? N1 Co1 N2 91.5(2) . . ? N5 Co1 N2 92.1(2) . . ? N4 Co1 N2 174.3(2) . . ? N3 Ag1 N6 153.7(2) . . ? N3 Ag1 N9 106.2(2) . . ? N6 Ag1 N9 94.8(2) . . ? N3 Ag1 N8 110.6(2) . . ? N6 Ag1 N8 85.8(3) . . ? N9 Ag1 N8 86.5(2) . . ? F2 C42 F3 104.7(11) . . ? F2 C42 F1 106.1(9) . . ? F3 C42 F1 106.8(9) . . ? F2 C42 S1 113.7(7) . . ? F3 C42 S1 112.4(8) . . ? F1 C42 S1 112.5(9) . . ? O5 S1 O4 115.5(6) . . ? O5 S1 O3 114.0(5) . . ? O4 S1 O3 113.8(5) . . ? O5 S1 C42 104.3(5) . . ? O4 S1 C42 101.7(5) . . ? O3 S1 C42 105.7(5) . . ? C46 C45 C50 120.0 . . ? C46 C45 H45 120.0 . . ? C50 C45 H45 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 120.0 . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.0 . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 H50 120.0 . . ? C45 C50 H50 120.0 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.400 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.222 #===END