# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_y3 #TrackingRef 'CC1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H30 Cu F20 N12 O9 S2' _chemical_formula_weight 1450.52 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' _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 17.7530(15) _cell_length_b 17.8428(15) _cell_length_c 19.7082(17) _cell_angle_alpha 102.910(2) _cell_angle_beta 102.857(2) _cell_angle_gamma 90.683(2) _cell_volume 5920.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2908 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8573 _exptl_absorpt_correction_T_max 0.9350 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32538 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 21.32 _reflns_number_total 11135 _reflns_number_gt 5040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material Shelxl-97 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11135 _refine_ls_number_parameters 1666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1518 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2412 _refine_ls_wR_factor_gt 0.2092 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.47584(6) 0.72566(6) 0.42249(5) 0.0422(3) Uani 1 1 d . . . S1 S 0.53212(12) 0.78868(12) 0.63852(11) 0.0393(5) Uani 1 1 d . . . S2A S 0.3987(3) 0.6661(3) 0.2340(3) 0.0691(14) Uiso 0.51 1 d P . . S2B S 0.4651(3) 0.6954(3) 0.2350(3) 0.0660(14) Uiso 0.49 1 d P . . F1 F 0.6846(5) 1.0739(4) 0.2519(5) 0.122(3) Uani 1 1 d . . . F2 F 0.7354(5) 1.0489(5) 0.1286(5) 0.135(3) Uani 1 1 d . . . F3 F 0.6428(5) 0.9689(4) 0.0056(4) 0.134(3) Uani 1 1 d . . . F4 F 0.5028(5) 0.9123(5) 0.0046(4) 0.122(2) Uani 1 1 d . . . F5 F 0.4456(4) 0.9388(4) 0.1231(4) 0.102(2) Uani 1 1 d . . . F6 F 0.8274(4) 0.4488(5) 0.2311(4) 0.126(3) Uani 1 1 d . . . F7 F 0.7960(5) 0.3432(5) 0.1049(5) 0.137(3) Uani 1 1 d . . . F8 F 0.7044(4) 0.3750(4) -0.0126(3) 0.105(2) Uani 1 1 d . . . F9 F 0.6438(5) 0.5142(5) -0.0053(4) 0.128(3) Uani 1 1 d . . . F10 F 0.6756(5) 0.6208(4) 0.1216(4) 0.119(2) Uani 1 1 d . . . F11 F 0.1840(5) 0.2934(5) 0.2392(5) 0.144(3) Uani 1 1 d . . . F12 F 0.0732(5) 0.2626(5) 0.1152(6) 0.168(4) Uani 1 1 d . . . F13 F 0.1070(5) 0.2827(4) -0.0073(5) 0.154(4) Uani 1 1 d . . . F14 F 0.2481(5) 0.3364(5) -0.0050(4) 0.135(3) Uani 1 1 d . . . F15 F 0.3617(4) 0.3678(4) 0.1140(4) 0.120(2) Uani 1 1 d . . . F16 F 0.0385(5) 0.9200(5) 0.2279(4) 0.126(3) Uani 1 1 d . . . F17 F 0.0086(5) 0.9631(5) 0.1029(4) 0.133(3) Uani 1 1 d . . . F18 F 0.0388(4) 0.8715(4) -0.0146(3) 0.101(2) Uani 1 1 d . . . F19 F 0.0989(6) 0.7344(4) -0.0077(4) 0.127(3) Uani 1 1 d . . . F20 F 0.1262(5) 0.6873(4) 0.1163(4) 0.118(3) Uani 1 1 d . . . N1 N 0.4557(4) 0.8383(4) 0.4272(3) 0.0423(17) Uani 1 1 d . . . C2 C 0.4181(5) 0.8759(5) 0.4758(5) 0.053(2) Uani 1 1 d . . . H2 H 0.4075 0.8518 0.5103 0.063 Uiso 1 1 calc R . . C3 C 0.3953(5) 0.9491(5) 0.4753(5) 0.057(3) Uani 1 1 d . . . H3 H 0.3671 0.9734 0.5074 0.069 Uiso 1 1 calc R . . C4 C 0.4145(5) 0.9857(5) 0.4273(5) 0.058(3) Uani 1 1 d . . . H4 H 0.3986 1.0351 0.4268 0.069 Uiso 1 1 calc R . . C5 C 0.4562(5) 0.9521(4) 0.3801(4) 0.042(2) Uani 1 1 d . . . C6 C 0.4753(4) 0.8733(4) 0.3812(4) 0.040(2) Uani 1 1 d . . . H6 H 0.5020 0.8470 0.3486 0.048 Uiso 1 1 calc R . . N7 N 0.4812(5) 0.9916(4) 0.3378(4) 0.059(2) Uani 1 1 d . . . H7 H 0.4717 1.0396 0.3458 0.070 Uiso 1 1 calc R . . C8 C 0.5195(6) 0.9684(5) 0.2837(6) 0.066(3) Uani 1 1 d . . . O9 O 0.5366(6) 0.9028(4) 0.2668(5) 0.113(3) Uani 1 1 d . . . N10 N 0.5344(5) 1.0241(4) 0.2529(5) 0.077(3) Uani 1 1 d . . . H10 H 0.5262 1.0709 0.2712 0.092 Uiso 1 1 calc R . . C11 C 0.5637(6) 1.0075(5) 0.1898(6) 0.064(3) Uani 1 1 d . . . C12 C 0.6357(7) 1.0345(6) 0.1890(7) 0.076(3) Uani 1 1 d . . . C13 C 0.6643(7) 1.0210(7) 0.1301(8) 0.091(4) Uani 1 1 d . . . C14 C 0.6155(7) 0.9795(7) 0.0653(7) 0.083(4) Uani 1 1 d . . . C15 C 0.5477(8) 0.9542(7) 0.0669(7) 0.090(4) Uani 1 1 d . . . C16 C 0.5209(7) 0.9661(6) 0.1272(7) 0.079(3) Uani 1 1 d . . . N17 N 0.5885(4) 0.7498(4) 0.4273(3) 0.0422(17) Uani 1 1 d . . . C18 C 0.6281(6) 0.8123(5) 0.4746(5) 0.058(3) Uani 1 1 d . . . H18 H 0.6047 0.8401 0.5092 0.069 Uiso 1 1 calc R . . C19 C 0.7007(5) 0.8361(5) 0.4737(5) 0.051(2) Uani 1 1 d . . . H19 H 0.7249 0.8811 0.5052 0.062 Uiso 1 1 calc R . . C20 C 0.7376(5) 0.7940(5) 0.4266(5) 0.056(3) Uani 1 1 d . . . H20 H 0.7874 0.8099 0.4257 0.068 Uiso 1 1 calc R . . C21 C 0.7010(5) 0.7264(5) 0.3791(4) 0.047(2) Uani 1 1 d . . . C22 C 0.6240(4) 0.7070(5) 0.3806(5) 0.046(2) Uani 1 1 d . . . H22 H 0.5975 0.6635 0.3483 0.055 Uiso 1 1 calc R . . N23 N 0.7432(4) 0.6788(4) 0.3352(4) 0.058(2) Uani 1 1 d . . . H23 H 0.7924 0.6898 0.3456 0.070 Uiso 1 1 calc R . . C24 C 0.7170(5) 0.6191(5) 0.2796(5) 0.060(3) Uani 1 1 d . . . O25 O 0.6508(4) 0.5922(5) 0.2623(4) 0.106(3) Uani 1 1 d . . . N26 N 0.7703(4) 0.5930(5) 0.2426(5) 0.077(3) Uani 1 1 d . . . H26 H 0.8172 0.6126 0.2588 0.093 Uiso 1 1 calc R . . C27 C 0.7530(6) 0.5350(6) 0.1785(5) 0.066(3) Uani 1 1 d . . . C28 C 0.7814(6) 0.4655(7) 0.1720(6) 0.077(3) Uani 1 1 d . . . C29 C 0.7648(6) 0.4124(6) 0.1079(7) 0.080(3) Uani 1 1 d . . . C30 C 0.7207(6) 0.4291(6) 0.0502(6) 0.069(3) Uani 1 1 d . . . C31 C 0.6902(7) 0.4954(7) 0.0527(6) 0.079(3) Uani 1 1 d . . . C32 C 0.7069(6) 0.5516(6) 0.1177(6) 0.076(3) Uani 1 1 d . . . N33 N 0.4986(4) 0.6144(4) 0.4253(3) 0.0421(17) Uani 1 1 d . . . C34 C 0.5633(5) 0.5993(5) 0.4707(5) 0.053(2) Uani 1 1 d . . . H34 H 0.5941 0.6397 0.5037 0.064 Uiso 1 1 calc R . . C35 C 0.5838(5) 0.5240(6) 0.4680(5) 0.060(3) Uani 1 1 d . . . H35 H 0.6267 0.5139 0.5007 0.072 Uiso 1 1 calc R . . C36 C 0.5416(5) 0.4662(5) 0.4183(5) 0.061(3) Uani 1 1 d . . . H36 H 0.5588 0.4167 0.4133 0.073 Uiso 1 1 calc R . . C37 C 0.4734(5) 0.4785(5) 0.3745(4) 0.046(2) Uani 1 1 d . . . C38 C 0.4539(5) 0.5573(5) 0.3779(4) 0.048(2) Uani 1 1 d . . . H38 H 0.4100 0.5681 0.3468 0.058 Uiso 1 1 calc R . . N39 N 0.4262(5) 0.4166(4) 0.3300(4) 0.064(2) Uani 1 1 d . . . H39 H 0.4372 0.3721 0.3379 0.076 Uiso 1 1 calc R . . C40 C 0.3645(7) 0.4177(6) 0.2751(6) 0.083(3) Uani 1 1 d . . . O41 O 0.3399(6) 0.4742(4) 0.2593(5) 0.126(4) Uani 1 1 d . . . N42 N 0.3345(6) 0.3434(5) 0.2421(6) 0.093(3) Uani 1 1 d . . . H42 H 0.3510 0.3051 0.2598 0.112 Uiso 1 1 calc R . . C43 C 0.2749(7) 0.3316(5) 0.1774(8) 0.087(4) Uani 1 1 d . . . C44 C 0.1991(8) 0.3053(6) 0.1810(8) 0.101(5) Uani 1 1 d . . . C45 C 0.1429(10) 0.2888(7) 0.1172(10) 0.123(6) Uani 1 1 d . . . C46 C 0.1599(7) 0.2982(7) 0.0562(9) 0.113(6) Uani 1 1 d . . . C47 C 0.2307(9) 0.3250(7) 0.0553(7) 0.100(5) Uani 1 1 d . . . C48 C 0.2909(8) 0.3439(6) 0.1153(7) 0.090(4) Uani 1 1 d . . . N49 N 0.3643(4) 0.7030(4) 0.4248(3) 0.0416(17) Uani 1 1 d . . . C50 C 0.3462(5) 0.6648(4) 0.4705(4) 0.047(2) Uani 1 1 d . . . H50 H 0.3865 0.6515 0.5038 0.056 Uiso 1 1 calc R . . C51 C 0.2727(5) 0.6441(5) 0.4717(5) 0.060(3) Uani 1 1 d . . . H51 H 0.2627 0.6174 0.5046 0.072 Uiso 1 1 calc R . . C52 C 0.2152(6) 0.6639(5) 0.4233(5) 0.064(3) Uani 1 1 d . . . H52 H 0.1645 0.6477 0.4210 0.077 Uiso 1 1 calc R . . C53 C 0.2288(5) 0.7081(5) 0.3763(5) 0.054(2) Uani 1 1 d . . . C54 C 0.3073(5) 0.7246(5) 0.3786(4) 0.047(2) Uani 1 1 d . . . H54 H 0.3195 0.7514 0.3467 0.057 Uiso 1 1 calc R . . N55 N 0.1660(4) 0.7343(5) 0.3300(4) 0.065(2) Uani 1 1 d . . . H55 H 0.1212 0.7307 0.3393 0.078 Uiso 1 1 calc R . . C56 C 0.1688(6) 0.7641(7) 0.2733(5) 0.071(3) Uani 1 1 d . . . O57 O 0.2267(4) 0.7750(6) 0.2540(4) 0.107(3) Uani 1 1 d . . . N58 N 0.0949(4) 0.7793(6) 0.2405(4) 0.078(3) Uani 1 1 d . . . H58 H 0.0565 0.7747 0.2596 0.094 Uiso 1 1 calc R . . C59 C 0.0835(5) 0.8024(6) 0.1756(6) 0.065(3) Uani 1 1 d . . . C60 C 0.0545(6) 0.8732(7) 0.1695(6) 0.078(3) Uani 1 1 d . . . C61 C 0.0366(7) 0.8942(7) 0.1052(7) 0.084(3) Uani 1 1 d . . . C62 C 0.0534(6) 0.8478(7) 0.0484(6) 0.074(3) Uani 1 1 d . . . C63 C 0.0842(7) 0.7807(7) 0.0507(6) 0.080(3) Uani 1 1 d . . . C64 C 0.0995(6) 0.7563(7) 0.1143(6) 0.079(3) Uani 1 1 d . . . O65 O 0.5103(5) 0.7557(5) 0.5655(5) 0.106(3) Uiso 1 1 d . . . O68 O 0.4482(3) 0.6978(3) 0.3030(3) 0.0525(15) Uani 1 1 d . . . C69 C 0.3888(8) 0.7355(8) 0.1827(7) 0.106(4) Uiso 1 1 d . . . C70 C 0.4511(9) 0.6026(8) 0.1867(8) 0.122(5) Uiso 1 1 d . . . O4A O 0.4971(14) 0.7236(13) 0.6619(12) 0.192(8) Uiso 0.64 1 d P . . O4B O 0.4572(8) 0.8354(7) 0.6441(7) 0.030(3) Uiso 0.36 1 d P . . O5A O 0.4858(11) 0.8172(11) 0.6812(10) 0.132(6) Uiso 0.56 1 d P . . O5B O 0.5992(8) 0.7387(8) 0.6574(7) 0.055(4) Uiso 0.44 1 d P . . O6A O 0.5561(14) 0.7524(13) 0.6942(12) 0.103(7) Uiso 0.37 1 d P . . O6B O 0.5847(5) 0.8574(5) 0.6476(5) 0.053(2) Uiso 0.63 1 d P . . Cu2 Cu 0.98503(6) 0.23539(6) 0.42185(5) 0.0419(3) Uani 1 1 d . . . S3 S 0.96360(13) 0.71990(12) 0.36326(12) 0.0403(6) Uani 1 1 d . . . S4A S 0.9024(4) 0.1741(3) 0.2344(3) 0.0796(16) Uiso 0.51 1 d P . . S4B S 0.9658(4) 0.1987(3) 0.2328(3) 0.0777(16) Uiso 0.49 1 d P . . F21 F 1.3226(5) -0.0559(5) 0.2284(4) 0.123(2) Uani 1 1 d . . . F22 F 1.2903(5) -0.1613(5) 0.1018(4) 0.130(3) Uani 1 1 d . . . F23 F 1.2070(4) -0.1260(4) -0.0168(3) 0.101(2) Uani 1 1 d . . . F24 F 1.1517(5) 0.0152(4) -0.0118(4) 0.116(2) Uani 1 1 d . . . F25 F 1.1848(4) 0.1222(4) 0.1146(4) 0.108(2) Uani 1 1 d . . . F26 F 0.6914(5) -0.2003(4) 0.2534(5) 0.120(2) Uani 1 1 d . . . F27 F 0.5768(4) -0.2337(4) 0.1326(5) 0.132(3) Uani 1 1 d . . . F28 F 0.6060(5) -0.2146(4) 0.0088(4) 0.127(3) Uani 1 1 d . . . F29 F 0.7445(5) -0.1585(4) 0.0054(4) 0.122(3) Uani 1 1 d . . . F30 F 0.8600(4) -0.1259(4) 0.1236(4) 0.104(2) Uani 1 1 d . . . F31 F 0.5383(5) 0.4162(5) 0.2279(4) 0.123(2) Uani 1 1 d . . . F32 F 0.5057(5) 0.4567(5) 0.1016(4) 0.128(3) Uani 1 1 d . . . F33 F 0.5346(4) 0.3657(4) -0.0162(4) 0.105(2) Uani 1 1 d . . . F34 F 0.5987(6) 0.2307(4) -0.0082(4) 0.131(3) Uani 1 1 d . . . F35 F 0.6306(5) 0.1858(4) 0.1166(4) 0.121(3) Uani 1 1 d . . . F36 F 1.1904(6) 0.5761(5) 0.2412(6) 0.141(3) Uani 1 1 d . . . F37 F 1.2406(5) 0.5472(6) 0.1186(6) 0.160(4) Uani 1 1 d . . . F38 F 1.1480(6) 0.4654(5) -0.0025(5) 0.144(3) Uani 1 1 d . . . F39 F 1.0077(6) 0.4087(5) -0.0017(5) 0.135(3) Uani 1 1 d . . . F40 F 0.9508(5) 0.4394(4) 0.1164(5) 0.125(2) Uani 1 1 d . . . N71 N 1.0976(4) 0.2583(4) 0.4238(4) 0.0422(17) Uani 1 1 d . . . C72 C 1.1387(5) 0.3198(5) 0.4704(5) 0.051(2) Uani 1 1 d . . . H72 H 1.1159 0.3497 0.5045 0.061 Uiso 1 1 calc R . . C73 C 1.2125(6) 0.3398(5) 0.4692(5) 0.058(3) Uani 1 1 d . . . H73 H 1.2388 0.3832 0.5017 0.070 Uiso 1 1 calc R . . C74 C 1.2478(5) 0.2968(5) 0.4210(5) 0.058(3) Uani 1 1 d . . . H74 H 1.2976 0.3115 0.4192 0.070 Uiso 1 1 calc R . . C75 C 1.2090(5) 0.2311(5) 0.3746(4) 0.047(2) Uani 1 1 d . . . C76 C 1.1311(5) 0.2141(5) 0.3764(5) 0.046(2) Uani 1 1 d . . . H76 H 1.1031 0.1716 0.3439 0.055 Uiso 1 1 calc R . . N77 N 1.2479(4) 0.1808(5) 0.3299(4) 0.060(2) Uani 1 1 d . . . H77 H 1.2975 0.1877 0.3405 0.071 Uiso 1 1 calc R . . C78 C 1.2173(6) 0.1235(6) 0.2729(5) 0.063(3) Uani 1 1 d . . . O79 O 1.1503(4) 0.1045(4) 0.2517(4) 0.091(3) Uani 1 1 d . . . N80 N 1.2719(5) 0.0918(5) 0.2387(5) 0.079(3) Uani 1 1 d . . . H80 H 1.3197 0.1072 0.2573 0.095 Uiso 1 1 calc R . . C81 C 1.2539(6) 0.0350(7) 0.1744(6) 0.066(3) Uani 1 1 d . . . C82 C 1.2795(6) -0.0368(8) 0.1690(6) 0.077(3) Uani 1 1 d . . . C83 C 1.2635(6) -0.0905(7) 0.1050(8) 0.078(3) Uani 1 1 d . . . C84 C 1.2210(7) -0.0713(7) 0.0455(6) 0.071(3) Uani 1 1 d . . . C85 C 1.1937(6) -0.0017(7) 0.0486(6) 0.068(3) Uani 1 1 d . . . C86 C 1.2109(6) 0.0508(6) 0.1122(6) 0.065(3) Uani 1 1 d . . . N87 N 1.0079(4) 0.1246(4) 0.4269(4) 0.0435(17) Uani 1 1 d . . . C88 C 1.0712(5) 0.1123(5) 0.4741(5) 0.050(2) Uani 1 1 d . . . H88 H 1.1013 0.1540 0.5058 0.060 Uiso 1 1 calc R . . C89 C 1.0918(5) 0.0387(6) 0.4758(5) 0.061(3) Uani 1 1 d . . . H89 H 1.1344 0.0308 0.5100 0.073 Uiso 1 1 calc R . . C90 C 1.0499(5) -0.0231(6) 0.4274(5) 0.058(3) Uani 1 1 d . . . H90 H 1.0662 -0.0726 0.4262 0.069 Uiso 1 1 calc R . . C91 C 0.9830(5) -0.0112(5) 0.3803(4) 0.042(2) Uani 1 1 d . . . C92 C 0.9650(5) 0.0662(5) 0.3812(5) 0.044(2) Uani 1 1 d . . . H92 H 0.9218 0.0759 0.3486 0.053 Uiso 1 1 calc R . . N93 N 0.9359(5) -0.0736(4) 0.3388(4) 0.058(2) Uani 1 1 d . . . H93 H 0.9485 -0.1176 0.3472 0.070 Uiso 1 1 calc R . . C94 C 0.8717(7) -0.0745(6) 0.2860(6) 0.069(3) Uani 1 1 d . . . O95 O 0.8464(5) -0.0183(4) 0.2679(4) 0.107(3) Uani 1 1 d . . . N96 N 0.8402(5) -0.1490(4) 0.2545(5) 0.076(3) Uani 1 1 d . . . H96 H 0.8575 -0.1866 0.2729 0.092 Uiso 1 1 calc R . . C97 C 0.7789(7) -0.1634(5) 0.1914(7) 0.072(3) Uani 1 1 d . . . C98 C 0.7050(8) -0.1887(6) 0.1931(8) 0.085(3) Uani 1 1 d . . . C99 C 0.6460(8) -0.2069(7) 0.1310(10) 0.094(4) Uani 1 1 d . . . C100 C 0.6629(8) -0.1973(7) 0.0678(8) 0.083(4) Uani 1 1 d . . . C101 C 0.7304(10) -0.1693(7) 0.0659(7) 0.085(4) Uani 1 1 d . . . C102 C 0.7885(7) -0.1511(6) 0.1281(8) 0.080(3) Uani 1 1 d . . . N103 N 0.8760(4) 0.2128(4) 0.4263(4) 0.0415(17) Uani 1 1 d . . . C104 C 0.8594(5) 0.1750(5) 0.4725(4) 0.045(2) Uani 1 1 d . . . H104 H 0.9003 0.1640 0.5067 0.055 Uiso 1 1 calc R . . C105 C 0.7859(6) 0.1510(5) 0.4735(5) 0.059(3) Uani 1 1 d . . . H105 H 0.7776 0.1238 0.5066 0.071 Uiso 1 1 calc R . . C106 C 0.7255(6) 0.1683(6) 0.4245(5) 0.061(3) Uani 1 1 d . . . H106 H 0.6752 0.1507 0.4219 0.073 Uiso 1 1 calc R . . C107 C 0.7395(5) 0.2118(5) 0.3789(5) 0.051(2) Uani 1 1 d . . . C108 C 0.8161(5) 0.2332(5) 0.3798(5) 0.047(2) Uani 1 1 d . . . H108 H 0.8258 0.2616 0.3482 0.057 Uiso 1 1 calc R . . N109 N 0.6736(4) 0.2353(5) 0.3324(4) 0.061(2) Uani 1 1 d . . . H109 H 0.6290 0.2278 0.3409 0.073 Uiso 1 1 calc R . . C110 C 0.6749(6) 0.2675(7) 0.2778(6) 0.067(3) Uani 1 1 d . . . O111 O 0.7309(4) 0.2877(6) 0.2600(4) 0.119(4) Uani 1 1 d . . . N112 N 0.5992(5) 0.2756(5) 0.2412(5) 0.075(2) Uani 1 1 d . . . H112 H 0.5608 0.2658 0.2585 0.090 Uiso 1 1 calc R . . C113 C 0.5855(5) 0.2997(6) 0.1767(6) 0.061(3) Uani 1 1 d . . . C114 C 0.5546(6) 0.3689(7) 0.1704(6) 0.074(3) Uani 1 1 d . . . C115 C 0.5362(7) 0.3888(7) 0.1050(8) 0.080(3) Uani 1 1 d . . . C116 C 0.5519(6) 0.3431(8) 0.0479(6) 0.069(3) Uani 1 1 d . . . C117 C 0.5847(8) 0.2767(8) 0.0502(6) 0.081(3) Uani 1 1 d . . . C118 C 0.5997(7) 0.2547(7) 0.1148(7) 0.079(3) Uani 1 1 d . . . N119 N 0.9640(4) 0.3484(4) 0.4247(4) 0.0430(17) Uani 1 1 d . . . C120 C 0.9231(5) 0.3868(5) 0.4706(5) 0.056(3) Uani 1 1 d . . . H120 H 0.9112 0.3638 0.5051 0.068 Uiso 1 1 calc R . . C121 C 0.8991(5) 0.4586(5) 0.4672(5) 0.059(3) Uani 1 1 d . . . H121 H 0.8690 0.4830 0.4976 0.070 Uiso 1 1 calc R . . C122 C 0.9194(6) 0.4941(6) 0.4191(6) 0.064(3) Uani 1 1 d . . . H122 H 0.9028 0.5428 0.4164 0.077 Uiso 1 1 calc R . . C123 C 0.9642(5) 0.4585(5) 0.3744(5) 0.043(2) Uani 1 1 d . . . C124 C 0.9835(5) 0.3823(5) 0.3784(4) 0.045(2) Uani 1 1 d . . . H124 H 1.0110 0.3556 0.3467 0.054 Uiso 1 1 calc R . . N125 N 0.9902(5) 0.4986(4) 0.3318(4) 0.061(2) Uani 1 1 d . . . H125 H 0.9823 0.5469 0.3399 0.074 Uiso 1 1 calc R . . C126 C 1.0272(7) 0.4725(6) 0.2778(6) 0.074(3) Uani 1 1 d . . . O127 O 1.0466(6) 0.4076(4) 0.2628(5) 0.130(4) Uani 1 1 d . . . N128 N 1.0402(6) 0.5272(5) 0.2429(6) 0.093(3) Uani 1 1 d . . . H128 H 1.0303 0.5740 0.2594 0.112 Uiso 1 1 calc R . . C129 C 1.0695(9) 0.5098(6) 0.1803(7) 0.078(3) Uani 1 1 d . . . C130 C 1.1421(9) 0.5359(7) 0.1802(8) 0.089(4) Uani 1 1 d . . . C131 C 1.1714(10) 0.5219(9) 0.1208(12) 0.118(5) Uani 1 1 d . . . C132 C 1.1212(12) 0.4779(9) 0.0573(11) 0.112(6) Uani 1 1 d . . . C133 C 1.0538(11) 0.4522(8) 0.0597(8) 0.100(4) Uani 1 1 d . . . C134 C 1.0275(8) 0.4660(7) 0.1188(9) 0.087(4) Uani 1 1 d . . . O135 O 0.9760(5) 0.7225(5) 0.4373(4) 0.109(3) Uani 1 1 d . . . O140 O 0.9547(4) 0.2043(3) 0.3030(3) 0.0549(16) Uani 1 1 d . . . C141 C 0.8929(10) 0.2378(9) 0.1834(8) 0.128(5) Uani 1 1 d . . . C142 C 0.9479(10) 0.1072(8) 0.1848(7) 0.127(5) Uani 1 1 d . . . O1A O 0.8867(8) 0.7631(8) 0.3578(8) 0.057(4) Uiso 0.45 1 d P . . O1B O 0.9566(12) 0.6519(11) 0.3145(11) 0.152(7) Uiso 0.55 1 d P . . O2A O 0.8956(13) 0.7261(12) 0.3185(12) 0.153(7) Uiso 0.55 1 d P . . O2B O 1.0209(9) 0.6639(8) 0.3409(8) 0.065(4) Uiso 0.45 1 d P . . O3A O 1.0096(5) 0.7831(5) 0.3511(4) 0.101(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0408(7) 0.0425(6) 0.0447(7) 0.0117(5) 0.0106(5) 0.0075(5) S1 0.0411(14) 0.0413(13) 0.0366(13) 0.0076(10) 0.0124(11) 0.0019(11) F1 0.129(6) 0.093(5) 0.139(7) 0.007(5) 0.042(5) -0.018(5) F2 0.111(6) 0.142(6) 0.204(9) 0.089(6) 0.091(6) 0.022(5) F3 0.195(8) 0.118(6) 0.132(6) 0.047(5) 0.107(6) 0.050(5) F4 0.159(7) 0.120(6) 0.103(6) 0.035(5) 0.050(6) 0.039(5) F5 0.108(5) 0.103(5) 0.110(5) 0.025(4) 0.052(4) 0.007(4) F6 0.105(6) 0.138(6) 0.111(6) 0.008(5) -0.005(5) 0.043(5) F7 0.155(7) 0.105(5) 0.142(7) 0.012(5) 0.031(6) 0.056(5) F8 0.126(6) 0.105(5) 0.070(4) -0.020(4) 0.035(4) -0.011(4) F9 0.164(8) 0.122(6) 0.085(5) 0.018(4) 0.003(5) 0.020(5) F10 0.149(7) 0.072(4) 0.124(6) 0.014(4) 0.015(5) 0.028(5) F11 0.150(8) 0.136(7) 0.161(9) 0.070(6) 0.031(7) 0.005(6) F12 0.078(6) 0.139(7) 0.267(12) 0.057(7) -0.011(7) -0.017(5) F13 0.138(7) 0.098(5) 0.167(8) -0.007(5) -0.050(7) 0.016(5) F14 0.155(8) 0.113(6) 0.111(6) 0.004(5) 0.000(6) 0.028(5) F15 0.092(5) 0.115(6) 0.139(7) 0.020(5) 0.010(5) -0.002(5) F16 0.130(6) 0.164(7) 0.099(5) 0.040(5) 0.046(5) 0.080(5) F17 0.151(7) 0.132(6) 0.119(6) 0.044(5) 0.019(5) 0.057(6) F18 0.114(5) 0.121(5) 0.077(4) 0.052(4) 0.010(4) -0.002(4) F19 0.203(8) 0.109(5) 0.068(5) 0.008(4) 0.042(5) 0.017(5) F20 0.176(7) 0.088(5) 0.106(5) 0.047(4) 0.038(5) 0.043(5) N1 0.043(4) 0.041(4) 0.042(4) 0.004(4) 0.014(4) 0.007(3) C2 0.054(6) 0.047(6) 0.057(6) -0.001(5) 0.024(5) -0.002(5) C3 0.056(6) 0.056(7) 0.065(7) 0.000(5) 0.038(6) 0.009(5) C4 0.056(6) 0.043(6) 0.072(7) 0.012(5) 0.010(6) 0.018(5) C5 0.057(6) 0.028(5) 0.039(5) 0.000(4) 0.013(5) 0.004(4) C6 0.033(5) 0.038(5) 0.045(5) 0.006(4) 0.006(4) 0.008(4) N7 0.083(6) 0.030(4) 0.066(5) 0.008(4) 0.025(5) 0.011(4) C8 0.091(8) 0.038(6) 0.080(8) 0.026(6) 0.027(7) 0.015(6) O9 0.205(9) 0.050(5) 0.139(7) 0.043(4) 0.131(7) 0.048(5) N10 0.115(7) 0.039(5) 0.091(7) 0.015(5) 0.055(6) 0.012(5) C11 0.087(9) 0.040(6) 0.070(8) 0.015(6) 0.028(7) 0.006(6) C12 0.093(10) 0.056(7) 0.101(10) 0.031(7) 0.050(9) 0.025(7) C13 0.088(10) 0.088(9) 0.136(13) 0.069(9) 0.061(11) 0.040(8) C14 0.099(11) 0.094(9) 0.088(10) 0.039(8) 0.069(10) 0.027(8) C15 0.114(12) 0.090(9) 0.068(10) 0.023(8) 0.018(9) 0.026(9) C16 0.093(10) 0.073(8) 0.097(10) 0.044(8) 0.052(9) 0.023(7) N17 0.039(4) 0.041(4) 0.046(4) 0.012(4) 0.009(4) 0.006(4) C18 0.080(8) 0.030(5) 0.054(6) 0.002(5) 0.003(6) 0.003(5) C19 0.050(6) 0.043(5) 0.049(6) -0.004(5) 0.002(5) -0.016(5) C20 0.041(6) 0.053(6) 0.061(7) 0.003(5) -0.007(5) -0.022(5) C21 0.043(6) 0.057(6) 0.043(6) 0.016(5) 0.010(5) 0.009(5) C22 0.028(5) 0.047(5) 0.056(6) 0.003(5) 0.005(5) -0.007(4) N23 0.037(5) 0.077(6) 0.052(5) -0.002(4) 0.012(4) -0.016(4) C24 0.034(6) 0.069(7) 0.070(7) -0.006(6) 0.024(6) -0.015(5) O25 0.059(5) 0.127(6) 0.103(6) -0.056(5) 0.044(5) -0.023(5) N26 0.040(5) 0.093(6) 0.083(7) -0.014(5) 0.016(5) -0.005(5) C27 0.046(7) 0.089(9) 0.055(7) 0.000(7) 0.015(6) -0.009(6) C28 0.063(8) 0.086(9) 0.076(9) 0.011(8) 0.012(7) 0.029(7) C29 0.068(8) 0.076(9) 0.099(11) 0.004(8) 0.040(8) 0.027(7) C30 0.079(9) 0.057(7) 0.073(9) 0.003(7) 0.031(7) -0.001(7) C31 0.073(8) 0.102(10) 0.055(8) 0.016(8) 0.005(7) -0.006(8) C32 0.072(8) 0.071(8) 0.080(9) 0.008(7) 0.021(7) -0.005(7) N33 0.040(4) 0.046(4) 0.041(4) 0.015(4) 0.005(4) 0.002(4) C34 0.038(6) 0.073(7) 0.049(6) 0.019(5) 0.005(5) -0.001(5) C35 0.031(6) 0.076(8) 0.082(8) 0.045(6) 0.005(5) 0.023(6) C36 0.060(7) 0.043(6) 0.086(8) 0.019(6) 0.027(6) 0.019(6) C37 0.062(7) 0.040(6) 0.035(5) 0.015(4) 0.004(5) 0.015(5) C38 0.048(6) 0.057(6) 0.050(6) 0.024(5) 0.021(5) 0.014(5) N39 0.075(6) 0.055(5) 0.064(6) 0.027(5) 0.008(5) 0.012(5) C40 0.092(9) 0.046(7) 0.091(9) 0.017(6) -0.022(7) 0.009(7) O41 0.147(8) 0.041(5) 0.140(8) 0.016(5) -0.067(6) 0.015(5) N42 0.087(7) 0.044(6) 0.129(9) 0.016(5) -0.009(7) 0.002(5) C43 0.068(9) 0.039(6) 0.126(13) 0.001(7) -0.018(9) -0.001(6) C44 0.096(12) 0.054(7) 0.123(13) 0.022(8) -0.042(11) 0.005(7) C45 0.141(18) 0.058(8) 0.160(18) 0.033(11) 0.007(16) 0.008(10) C46 0.053(9) 0.066(9) 0.164(18) -0.016(10) -0.046(11) -0.001(7) C47 0.147(15) 0.067(8) 0.066(10) 0.001(7) -0.007(11) 0.039(9) C48 0.105(12) 0.054(7) 0.095(11) 0.014(7) -0.010(10) 0.011(7) N49 0.056(5) 0.043(4) 0.027(4) 0.010(3) 0.010(4) 0.013(4) C50 0.056(7) 0.039(5) 0.051(6) 0.026(5) 0.010(5) 0.012(5) C51 0.058(7) 0.080(7) 0.061(7) 0.045(6) 0.026(6) 0.015(6) C52 0.055(7) 0.071(7) 0.076(8) 0.014(6) 0.037(6) -0.011(6) C53 0.051(7) 0.078(7) 0.041(6) 0.014(5) 0.028(5) 0.004(5) C54 0.047(6) 0.056(6) 0.045(6) 0.020(5) 0.017(5) 0.009(5) N55 0.023(4) 0.114(7) 0.064(6) 0.030(5) 0.010(4) 0.011(4) C56 0.048(7) 0.125(9) 0.060(7) 0.054(7) 0.022(6) 0.007(6) O57 0.047(5) 0.210(9) 0.111(6) 0.117(6) 0.032(5) 0.032(5) N58 0.041(5) 0.142(8) 0.067(6) 0.056(6) 0.012(5) 0.018(5) C59 0.037(6) 0.092(8) 0.072(8) 0.033(7) 0.013(6) 0.009(6) C60 0.064(7) 0.109(10) 0.062(8) 0.014(7) 0.021(6) 0.023(7) C61 0.077(8) 0.092(9) 0.092(10) 0.046(8) 0.010(7) 0.046(7) C62 0.075(8) 0.092(9) 0.054(8) 0.029(7) 0.001(6) 0.001(7) C63 0.080(8) 0.086(9) 0.071(9) 0.027(8) 0.009(7) -0.012(7) C64 0.072(8) 0.101(9) 0.062(8) 0.021(8) 0.013(7) -0.005(7) O68 0.068(4) 0.063(4) 0.021(3) 0.003(3) 0.005(3) 0.004(3) Cu2 0.0403(7) 0.0422(6) 0.0433(7) 0.0098(5) 0.0099(5) 0.0075(5) S3 0.0378(14) 0.0382(13) 0.0424(14) 0.0079(10) 0.0058(11) -0.0010(11) F21 0.116(6) 0.139(6) 0.101(6) 0.019(5) 0.006(5) 0.047(5) F22 0.150(7) 0.100(5) 0.124(6) 0.004(4) 0.017(5) 0.054(5) F23 0.123(6) 0.096(4) 0.073(4) -0.011(4) 0.031(4) 0.000(4) F24 0.152(7) 0.113(5) 0.067(5) 0.016(4) 0.000(4) 0.006(5) F25 0.135(6) 0.069(4) 0.110(5) 0.016(4) 0.015(5) 0.009(4) F26 0.129(6) 0.120(6) 0.122(6) 0.052(5) 0.032(5) -0.008(5) F27 0.070(5) 0.115(6) 0.196(9) 0.021(5) 0.015(5) -0.013(4) F28 0.125(6) 0.090(5) 0.122(6) -0.002(4) -0.033(5) 0.013(4) F29 0.154(7) 0.113(6) 0.091(6) 0.018(4) 0.016(5) 0.021(5) F30 0.093(5) 0.107(5) 0.113(6) 0.034(4) 0.015(4) 0.007(4) F31 0.144(6) 0.144(6) 0.099(5) 0.032(5) 0.054(5) 0.066(5) F32 0.136(7) 0.137(6) 0.122(6) 0.051(5) 0.029(5) 0.055(5) F33 0.113(5) 0.126(5) 0.082(5) 0.053(4) 0.009(4) 0.007(4) F34 0.214(9) 0.105(5) 0.074(5) 0.004(4) 0.050(5) 0.023(5) F35 0.185(8) 0.086(5) 0.115(6) 0.049(4) 0.055(5) 0.048(5) F36 0.151(8) 0.104(6) 0.165(8) 0.006(5) 0.057(7) -0.020(5) F37 0.131(7) 0.163(7) 0.245(10) 0.097(7) 0.116(7) 0.017(6) F38 0.198(9) 0.132(6) 0.151(7) 0.058(5) 0.113(7) 0.048(6) F39 0.170(8) 0.129(6) 0.124(7) 0.048(5) 0.052(6) 0.044(6) F40 0.131(6) 0.115(5) 0.155(7) 0.050(5) 0.069(6) 0.025(5) N71 0.037(4) 0.044(4) 0.039(4) 0.003(4) 0.001(4) 0.007(4) C72 0.056(7) 0.038(5) 0.053(6) 0.000(5) 0.008(5) 0.014(5) C73 0.064(7) 0.052(6) 0.048(6) -0.008(5) 0.011(6) -0.007(5) C74 0.042(6) 0.064(6) 0.058(7) 0.008(5) -0.003(5) -0.016(5) C75 0.046(6) 0.059(6) 0.037(5) 0.010(5) 0.009(5) 0.006(5) C76 0.031(5) 0.054(6) 0.046(6) 0.004(5) 0.003(4) 0.000(4) N77 0.030(4) 0.090(6) 0.047(5) -0.006(5) 0.007(4) -0.003(4) C78 0.038(6) 0.084(7) 0.060(7) -0.011(6) 0.024(6) -0.004(6) O79 0.043(4) 0.116(6) 0.085(5) -0.041(4) 0.020(4) -0.006(4) N80 0.052(6) 0.104(7) 0.062(6) -0.018(5) 0.008(5) 0.000(5) C81 0.032(6) 0.091(9) 0.073(9) 0.008(7) 0.018(6) 0.002(6) C82 0.061(8) 0.101(10) 0.060(8) 0.010(8) 0.002(6) 0.024(7) C83 0.058(7) 0.072(8) 0.099(10) -0.004(8) 0.027(7) 0.026(6) C84 0.073(8) 0.075(8) 0.051(8) -0.015(7) 0.014(6) -0.015(7) C85 0.057(7) 0.066(8) 0.071(9) 0.004(7) 0.006(6) 0.000(6) C86 0.057(7) 0.068(8) 0.069(8) 0.010(7) 0.015(6) 0.004(6) N87 0.046(5) 0.042(4) 0.042(4) 0.016(4) 0.003(4) 0.002(4) C88 0.040(6) 0.057(6) 0.053(6) 0.022(5) 0.003(5) 0.004(5) C89 0.041(6) 0.075(8) 0.068(7) 0.035(6) -0.002(5) 0.012(6) C90 0.051(6) 0.055(6) 0.076(7) 0.030(6) 0.017(6) 0.018(5) C91 0.058(6) 0.032(5) 0.033(5) 0.013(4) 0.004(5) 0.010(5) C92 0.043(6) 0.045(6) 0.049(6) 0.018(5) 0.012(5) 0.011(5) N93 0.064(6) 0.045(5) 0.060(5) 0.025(4) -0.008(5) 0.009(4) C94 0.081(8) 0.038(6) 0.074(8) 0.010(6) -0.005(7) 0.011(6) O95 0.121(7) 0.034(4) 0.123(7) 0.021(4) -0.063(5) 0.006(4) N96 0.077(6) 0.043(5) 0.091(7) 0.015(5) -0.019(5) -0.003(4) C97 0.088(10) 0.032(6) 0.090(10) 0.010(6) 0.015(8) -0.006(6) C98 0.087(10) 0.064(7) 0.095(11) 0.018(7) 0.007(9) 0.001(7) C99 0.077(10) 0.058(8) 0.139(14) 0.023(9) 0.009(11) 0.009(7) C100 0.071(10) 0.055(7) 0.092(11) -0.011(7) -0.018(9) 0.004(7) C101 0.108(12) 0.065(8) 0.068(10) 0.008(7) -0.001(9) 0.012(8) C102 0.072(9) 0.048(7) 0.110(11) 0.019(7) 0.001(9) -0.003(6) N103 0.049(5) 0.044(4) 0.037(4) 0.014(4) 0.017(4) 0.009(4) C104 0.050(6) 0.049(5) 0.047(6) 0.027(5) 0.014(5) 0.018(5) C105 0.072(8) 0.062(6) 0.064(7) 0.042(5) 0.031(6) 0.017(6) C106 0.055(7) 0.070(6) 0.073(7) 0.031(6) 0.035(6) 0.003(5) C107 0.050(6) 0.061(6) 0.045(6) 0.007(5) 0.024(5) 0.002(5) C108 0.049(6) 0.050(5) 0.052(6) 0.022(5) 0.018(5) 0.011(5) N109 0.035(5) 0.091(6) 0.066(6) 0.036(5) 0.014(4) -0.001(4) C110 0.032(6) 0.111(8) 0.074(8) 0.054(7) 0.010(6) 0.014(6) O111 0.038(4) 0.250(10) 0.118(7) 0.140(7) 0.017(4) 0.012(5) N112 0.045(6) 0.119(7) 0.076(6) 0.055(6) 0.011(5) 0.006(5) C113 0.031(6) 0.082(8) 0.065(8) 0.017(7) 0.003(5) -0.004(5) C114 0.064(7) 0.088(9) 0.075(9) 0.022(7) 0.022(7) 0.023(6) C115 0.069(8) 0.074(8) 0.110(11) 0.050(8) 0.018(8) 0.033(6) C116 0.065(7) 0.096(9) 0.048(7) 0.029(7) 0.006(6) 0.011(7) C117 0.096(9) 0.085(9) 0.064(9) 0.023(7) 0.016(7) -0.006(8) C118 0.076(8) 0.077(8) 0.084(9) 0.020(8) 0.016(7) -0.007(7) N119 0.043(4) 0.043(4) 0.044(4) 0.009(4) 0.012(4) -0.001(4) C120 0.064(7) 0.049(6) 0.054(6) -0.008(5) 0.028(5) -0.008(5) C121 0.050(6) 0.050(6) 0.075(7) -0.001(5) 0.028(6) 0.011(5) C122 0.054(7) 0.056(6) 0.081(8) 0.016(6) 0.010(6) 0.025(5) C123 0.044(5) 0.032(5) 0.048(6) 0.006(4) 0.007(5) 0.008(4) C124 0.046(6) 0.050(6) 0.037(5) 0.003(4) 0.011(5) 0.009(5) N125 0.088(6) 0.029(4) 0.069(6) 0.006(4) 0.026(5) 0.020(4) C126 0.095(9) 0.050(7) 0.102(9) 0.035(7) 0.054(7) 0.016(6) O127 0.219(10) 0.059(5) 0.181(9) 0.057(5) 0.158(8) 0.064(6) N128 0.127(8) 0.057(6) 0.119(8) 0.032(6) 0.064(7) 0.010(5) C129 0.110(11) 0.048(7) 0.094(10) 0.030(7) 0.049(10) 0.026(7) C130 0.108(12) 0.077(9) 0.110(12) 0.036(8) 0.069(10) 0.020(8) C131 0.124(15) 0.072(10) 0.195(19) 0.076(11) 0.069(15) 0.038(10) C132 0.138(15) 0.082(10) 0.170(18) 0.058(11) 0.118(15) 0.036(10) C133 0.150(15) 0.083(10) 0.075(10) 0.025(8) 0.034(11) 0.032(10) C134 0.095(10) 0.075(9) 0.117(12) 0.039(9) 0.061(10) 0.017(8) O135 0.130(7) 0.151(7) 0.042(5) 0.025(4) 0.014(5) -0.017(6) O140 0.073(4) 0.069(4) 0.014(3) 0.001(3) 0.000(3) -0.004(3) C141 0.146(13) 0.117(11) 0.109(11) 0.018(8) 0.011(10) 0.028(10) C142 0.192(15) 0.106(10) 0.080(9) 0.013(7) 0.030(10) 0.053(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N17 2.017(7) . ? Cu1 N49 2.028(7) . ? Cu1 N1 2.031(6) . ? Cu1 N33 2.042(7) . ? Cu1 O68 2.235(5) . ? S1 O5A 1.330(19) . ? S1 O6A 1.39(2) . ? S1 O65 1.392(8) . ? S1 O6B 1.486(8) . ? S1 O4A 1.52(2) . ? S1 O5B 1.526(14) . ? S1 O4B 1.589(14) . ? S2A S2B 1.278(7) . ? S2A O68 1.432(7) . ? S2A C70 1.719(16) . ? S2A C69 1.752(15) . ? S2B O68 1.428(7) . ? S2B C70 1.699(15) . ? S2B C69 1.772(15) . ? F1 C12 1.379(14) . ? F2 C13 1.360(14) . ? F3 C14 1.346(12) . ? F4 C15 1.358(14) . ? F5 C16 1.396(13) . ? F6 C28 1.359(13) . ? F7 C29 1.354(13) . ? F8 C30 1.360(12) . ? F9 C31 1.362(13) . ? F10 C32 1.354(13) . ? F11 C44 1.294(18) . ? F12 C45 1.31(2) . ? F13 C46 1.357(16) . ? F14 C47 1.349(16) . ? F15 C48 1.330(16) . ? F16 C60 1.351(12) . ? F17 C61 1.338(13) . ? F18 C62 1.372(12) . ? F19 C63 1.339(13) . ? F20 C64 1.330(14) . ? N1 C6 1.310(10) . ? N1 C2 1.350(10) . ? C2 C3 1.375(12) . ? C2 H2 0.9300 . ? C3 C4 1.361(12) . ? C3 H3 0.9300 . ? C4 C5 1.357(12) . ? C4 H4 0.9300 . ? C5 N7 1.346(10) . ? C5 C6 1.454(11) . ? C6 H6 0.9300 . ? N7 C8 1.379(12) . ? N7 H7 0.8600 . ? C8 O9 1.205(11) . ? C8 N10 1.327(12) . ? N10 C11 1.425(12) . ? N10 H10 0.8600 . ? C11 C16 1.344(15) . ? C11 C12 1.365(15) . ? C12 C13 1.341(16) . ? C13 C14 1.414(18) . ? C14 C15 1.291(18) . ? C15 C16 1.350(16) . ? N17 C22 1.336(10) . ? N17 C18 1.355(10) . ? C18 C19 1.357(12) . ? C18 H18 0.9300 . ? C19 C20 1.351(12) . ? C19 H19 0.9300 . ? C20 C21 1.399(11) . ? C20 H20 0.9300 . ? C21 C22 1.415(11) . ? C21 N23 1.417(11) . ? C22 H22 0.9300 . ? N23 C24 1.339(11) . ? N23 H23 0.8600 . ? C24 O25 1.208(10) . ? C24 N26 1.346(11) . ? N26 C27 1.414(12) . ? N26 H26 0.8600 . ? C27 C28 1.336(15) . ? C27 C32 1.387(15) . ? C28 C29 1.368(16) . ? C29 C30 1.325(16) . ? C30 C31 1.303(16) . ? C31 C32 1.408(15) . ? N33 C38 1.329(10) . ? N33 C34 1.360(10) . ? C34 C35 1.388(12) . ? C34 H34 0.9300 . ? C35 C36 1.338(12) . ? C35 H35 0.9300 . ? C36 C37 1.373(12) . ? C36 H36 0.9300 . ? C37 N39 1.381(11) . ? C37 C38 1.441(11) . ? C38 H38 0.9300 . ? N39 C40 1.361(12) . ? N39 H39 0.8600 . ? C40 O41 1.181(12) . ? C40 N42 1.382(13) . ? N42 C43 1.435(15) . ? N42 H42 0.8600 . ? C43 C48 1.378(18) . ? C43 C44 1.442(19) . ? C44 C45 1.39(2) . ? C45 C46 1.35(2) . ? C46 C47 1.35(2) . ? C47 C48 1.380(18) . ? N49 C54 1.325(10) . ? N49 C50 1.334(10) . ? C50 C51 1.358(12) . ? C50 H50 0.9300 . ? C51 C52 1.343(13) . ? C51 H51 0.9300 . ? C52 C53 1.400(13) . ? C52 H52 0.9300 . ? C53 C54 1.410(12) . ? C53 N55 1.430(11) . ? C54 H54 0.9300 . ? N55 C56 1.350(12) . ? N55 H55 0.8600 . ? C56 O57 1.199(11) . ? C56 N58 1.388(12) . ? N58 C59 1.401(12) . ? N58 H58 0.8600 . ? C59 C64 1.390(15) . ? C59 C60 1.391(15) . ? C60 C61 1.372(16) . ? C61 C62 1.331(15) . ? C62 C63 1.328(16) . ? C63 C64 1.390(16) . ? O4A O6A 1.15(3) . ? O4A O5A 1.65(3) . ? O4B O5A 0.917(19) . ? O5A O6A 1.73(3) . ? O5B O6A 1.16(2) . ? Cu2 N103 1.998(7) . ? Cu2 N71 2.025(6) . ? Cu2 N87 2.042(7) . ? Cu2 N119 2.045(7) . ? Cu2 O140 2.221(5) . ? S3 O2A 1.35(2) . ? S3 O1B 1.35(2) . ? S3 O135 1.417(7) . ? S3 O3A 1.476(9) . ? S3 O2B 1.502(15) . ? S3 O1A 1.570(14) . ? S4A S4B 1.212(8) . ? S4A O140 1.445(8) . ? S4A C141 1.665(16) . ? S4A C142 1.698(15) . ? S4B O140 1.423(8) . ? S4B C142 1.681(15) . ? S4B C141 1.695(16) . ? F21 C82 1.364(13) . ? F22 C83 1.348(12) . ? F23 C84 1.358(11) . ? F24 C85 1.355(13) . ? F25 C86 1.356(12) . ? F26 C98 1.323(14) . ? F27 C99 1.323(15) . ? F28 C100 1.333(13) . ? F29 C101 1.324(15) . ? F30 C102 1.369(13) . ? F31 C114 1.343(12) . ? F32 C115 1.343(12) . ? F33 C116 1.381(11) . ? F34 C117 1.330(13) . ? F35 C118 1.357(13) . ? F36 C130 1.355(16) . ? F37 C131 1.318(17) . ? F38 C132 1.341(15) . ? F39 C133 1.365(16) . ? F40 C134 1.423(14) . ? N71 C76 1.333(10) . ? N71 C72 1.347(10) . ? C72 C73 1.360(12) . ? C72 H72 0.9300 . ? C73 C74 1.355(12) . ? C73 H73 0.9300 . ? C74 C75 1.381(12) . ? C74 H74 0.9300 . ? C75 N77 1.411(11) . ? C75 C76 1.422(11) . ? C76 H76 0.9300 . ? N77 C78 1.342(11) . ? N77 H77 0.8600 . ? C78 O79 1.188(10) . ? C78 N80 1.360(12) . ? N80 C81 1.405(13) . ? N80 H80 0.8600 . ? C81 C82 1.354(15) . ? C81 C86 1.381(15) . ? C82 C83 1.372(15) . ? C83 C84 1.362(16) . ? C84 C85 1.332(15) . ? C85 C86 1.357(14) . ? N87 C92 1.318(10) . ? N87 C88 1.344(10) . ? C88 C89 1.373(12) . ? C88 H88 0.9300 . ? C89 C90 1.368(12) . ? C89 H89 0.9300 . ? C90 C91 1.385(12) . ? C90 H90 0.9300 . ? C91 N93 1.369(10) . ? C91 C92 1.418(11) . ? C92 H92 0.9300 . ? N93 C94 1.360(12) . ? N93 H93 0.8600 . ? C94 O95 1.197(11) . ? C94 N96 1.387(12) . ? N96 C97 1.429(13) . ? N96 H96 0.8600 . ? C97 C102 1.360(16) . ? C97 C98 1.393(16) . ? C98 C99 1.395(17) . ? C99 C100 1.389(18) . ? C100 C101 1.306(18) . ? C101 C102 1.387(16) . ? N103 C104 1.327(10) . ? N103 C108 1.351(10) . ? C104 C105 1.374(12) . ? C104 H104 0.9300 . ? C105 C106 1.364(13) . ? C105 H105 0.9300 . ? C106 C107 1.370(12) . ? C106 H106 0.9300 . ? C107 C108 1.402(12) . ? C107 N109 1.446(11) . ? C108 H108 0.9300 . ? N109 C110 1.332(12) . ? N109 H109 0.8600 . ? C110 O111 1.203(11) . ? C110 N112 1.402(12) . ? N112 C113 1.403(12) . ? N112 H112 0.8600 . ? C113 C114 1.376(14) . ? C113 C118 1.378(15) . ? C114 C115 1.383(16) . ? C115 C116 1.320(15) . ? C116 C117 1.332(16) . ? C117 C118 1.387(16) . ? N119 C124 1.306(10) . ? N119 C120 1.357(10) . ? C120 C121 1.365(12) . ? C120 H120 0.9300 . ? C121 C122 1.359(13) . ? C121 H121 0.9300 . ? C122 C123 1.372(12) . ? C122 H122 0.9300 . ? C123 N125 1.366(11) . ? C123 C124 1.420(11) . ? C124 H124 0.9300 . ? N125 C126 1.369(12) . ? N125 H125 0.8600 . ? C126 O127 1.204(11) . ? C126 N128 1.359(12) . ? N128 C129 1.417(14) . ? N128 H128 0.8600 . ? C129 C134 1.341(17) . ? C129 C130 1.365(17) . ? C130 C131 1.358(19) . ? C131 C132 1.42(2) . ? C132 C133 1.29(2) . ? C133 C134 1.323(17) . ? O1A O2A 0.94(2) . ? O1B O2B 1.14(2) . ? O1B O2A 1.72(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 N17 Cu1 N49 176.2(3) . . ? N17 Cu1 N1 89.6(3) . . ? N49 Cu1 N1 90.3(3) . . ? N17 Cu1 N33 89.9(3) . . ? N49 Cu1 N33 89.9(3) . . ? N1 Cu1 N33 176.0(3) . . ? N17 Cu1 O68 91.4(2) . . ? N49 Cu1 O68 92.4(2) . . ? N1 Cu1 O68 91.8(2) . . ? N33 Cu1 O68 92.2(2) . . ? O5A S1 O6A 79.0(12) . . ? O5A S1 O65 126.9(9) . . ? O6A S1 O65 128.4(10) . . ? O5A S1 O6B 101.0(8) . . ? O6A S1 O6B 110.4(11) . . ? O65 S1 O6B 106.7(5) . . ? O5A S1 O4A 70.7(11) . . ? O6A S1 O4A 46.2(11) . . ? O65 S1 O4A 96.1(9) . . ? O6B S1 O4A 155.6(10) . . ? O5A S1 O5B 125.1(10) . . ? O6A S1 O5B 46.6(10) . . ? O65 S1 O5B 97.9(6) . . ? O6B S1 O5B 92.9(6) . . ? O4A S1 O5B 75.1(10) . . ? O5A S1 O4B 35.2(8) . . ? O6A S1 O4B 113.4(11) . . ? O65 S1 O4B 97.1(6) . . ? O6B S1 O4B 95.4(6) . . ? O4A S1 O4B 90.2(10) . . ? O5B S1 O4B 160.0(7) . . ? S2B S2A O68 63.3(4) . . ? S2B S2A C70 67.2(6) . . ? O68 S2A C70 107.1(7) . . ? S2B S2A C69 69.6(6) . . ? O68 S2A C69 109.5(6) . . ? C70 S2A C69 98.9(7) . . ? S2A S2B O68 63.6(4) . . ? S2A S2B C70 68.9(6) . . ? O68 S2B C70 108.3(7) . . ? S2A S2B C69 67.9(6) . . ? O68 S2B C69 108.6(6) . . ? C70 S2B C69 98.9(7) . . ? C6 N1 C2 120.0(7) . . ? C6 N1 Cu1 120.6(5) . . ? C2 N1 Cu1 119.2(6) . . ? N1 C2 C3 121.0(8) . . ? N1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 119.4(8) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 121.7(8) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? N7 C5 C4 121.0(8) . . ? N7 C5 C6 122.8(8) . . ? C4 C5 C6 116.0(8) . . ? N1 C6 C5 121.6(7) . . ? N1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C5 N7 C8 131.0(8) . . ? C5 N7 H7 114.5 . . ? C8 N7 H7 114.5 . . ? O9 C8 N10 124.5(10) . . ? O9 C8 N7 121.6(9) . . ? N10 C8 N7 113.9(9) . . ? C8 N10 C11 120.8(8) . . ? C8 N10 H10 119.6 . . ? C11 N10 H10 119.6 . . ? C16 C11 C12 116.3(11) . . ? C16 C11 N10 121.6(11) . . ? C12 C11 N10 122.1(11) . . ? C13 C12 C11 123.4(14) . . ? C13 C12 F1 116.8(13) . . ? C11 C12 F1 119.7(11) . . ? C12 C13 F2 123.7(16) . . ? C12 C13 C14 117.7(13) . . ? F2 C13 C14 118.5(13) . . ? C15 C14 F3 124.0(16) . . ? C15 C14 C13 118.2(12) . . ? F3 C14 C13 117.8(13) . . ? C14 C15 C16 123.2(14) . . ? C14 C15 F4 117.2(14) . . ? C16 C15 F4 119.6(15) . . ? C11 C16 C15 121.2(13) . . ? C11 C16 F5 119.8(11) . . ? C15 C16 F5 118.9(14) . . ? C22 N17 C18 118.6(7) . . ? C22 N17 Cu1 120.3(5) . . ? C18 N17 Cu1 120.9(6) . . ? N17 C18 C19 122.7(9) . . ? N17 C18 H18 118.6 . . ? C19 C18 H18 118.6 . . ? C20 C19 C18 119.6(8) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.1(8) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 117.4(8) . . ? C20 C21 N23 119.3(8) . . ? C22 C21 N23 123.1(8) . . ? N17 C22 C21 121.4(8) . . ? N17 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C24 N23 C21 128.8(8) . . ? C24 N23 H23 115.6 . . ? C21 N23 H23 115.6 . . ? O25 C24 N23 123.6(9) . . ? O25 C24 N26 122.5(9) . . ? N23 C24 N26 113.9(8) . . ? C24 N26 C27 123.0(8) . . ? C24 N26 H26 118.5 . . ? C27 N26 H26 118.5 . . ? C28 C27 C32 117.4(11) . . ? C28 C27 N26 123.7(12) . . ? C32 C27 N26 118.9(11) . . ? C27 C28 F6 118.0(11) . . ? C27 C28 C29 121.2(12) . . ? F6 C28 C29 120.9(12) . . ? C30 C29 F7 121.1(12) . . ? C30 C29 C28 120.8(12) . . ? F7 C29 C28 118.2(13) . . ? C31 C30 C29 121.5(11) . . ? C31 C30 F8 118.9(13) . . ? C29 C30 F8 119.5(12) . . ? C30 C31 F9 123.2(12) . . ? C30 C31 C32 119.0(12) . . ? F9 C31 C32 117.8(13) . . ? F10 C32 C27 119.8(11) . . ? F10 C32 C31 120.1(12) . . ? C27 C32 C31 120.1(12) . . ? C38 N33 C34 120.5(7) . . ? C38 N33 Cu1 119.3(6) . . ? C34 N33 Cu1 119.8(6) . . ? N33 C34 C35 120.5(9) . . ? N33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C36 C35 C34 119.8(9) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 121.3(9) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C36 C37 N39 120.0(8) . . ? C36 C37 C38 117.3(9) . . ? N39 C37 C38 122.7(9) . . ? N33 C38 C37 120.2(8) . . ? N33 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 N39 C37 127.8(8) . . ? C40 N39 H39 116.1 . . ? C37 N39 H39 116.1 . . ? O41 C40 N39 124.5(10) . . ? O41 C40 N42 125.5(11) . . ? N39 C40 N42 110.0(10) . . ? C40 N42 C43 118.3(9) . . ? C40 N42 H42 120.8 . . ? C43 N42 H42 120.8 . . ? C48 C43 N42 120.8(13) . . ? C48 C43 C44 122.5(14) . . ? N42 C43 C44 116.6(15) . . ? F11 C44 C45 120.7(17) . . ? F11 C44 C43 122.7(14) . . ? C45 C44 C43 116.5(17) . . ? F12 C45 C46 119(2) . . ? F12 C45 C44 121(2) . . ? C46 C45 C44 120.5(19) . . ? C45 C46 C47 121.4(17) . . ? C45 C46 F13 122.6(18) . . ? C47 C46 F13 116(2) . . ? C46 C47 F14 122.0(17) . . ? C46 C47 C48 123.4(16) . . ? F14 C47 C48 114.5(18) . . ? F15 C48 C43 120.9(13) . . ? F15 C48 C47 123.4(17) . . ? C43 C48 C47 115.6(15) . . ? C54 N49 C50 118.4(7) . . ? C54 N49 Cu1 119.8(6) . . ? C50 N49 Cu1 121.8(6) . . ? N49 C50 C51 124.4(8) . . ? N49 C50 H50 117.8 . . ? C51 C50 H50 117.8 . . ? C52 C51 C50 117.0(8) . . ? C52 C51 H51 121.5 . . ? C50 C51 H51 121.5 . . ? C51 C52 C53 122.4(9) . . ? C51 C52 H52 118.8 . . ? C53 C52 H52 118.8 . . ? C52 C53 C54 115.5(9) . . ? C52 C53 N55 121.1(8) . . ? C54 C53 N55 123.4(8) . . ? N49 C54 C53 122.1(8) . . ? N49 C54 H54 118.9 . . ? C53 C54 H54 118.9 . . ? C56 N55 C53 127.6(8) . . ? C56 N55 H55 116.2 . . ? C53 N55 H55 116.2 . . ? O57 C56 N55 124.9(10) . . ? O57 C56 N58 125.3(9) . . ? N55 C56 N58 109.8(8) . . ? C56 N58 C59 119.0(8) . . ? C56 N58 H58 120.5 . . ? C59 N58 H58 120.5 . . ? C64 C59 C60 116.4(10) . . ? C64 C59 N58 122.6(11) . . ? C60 C59 N58 121.0(11) . . ? F16 C60 C61 119.4(12) . . ? F16 C60 C59 118.4(11) . . ? C61 C60 C59 122.0(11) . . ? C62 C61 F17 122.1(12) . . ? C62 C61 C60 118.6(11) . . ? F17 C61 C60 119.0(13) . . ? C63 C62 C61 122.7(11) . . ? C63 C62 F18 119.4(12) . . ? C61 C62 F18 117.9(12) . . ? C62 C63 F19 121.5(11) . . ? C62 C63 C64 119.9(13) . . ? F19 C63 C64 118.6(13) . . ? F20 C64 C63 120.4(12) . . ? F20 C64 C59 119.4(11) . . ? C63 C64 C59 120.1(13) . . ? S2B O68 S2A 53.1(3) . . ? S2B O68 Cu1 154.1(4) . . ? S2A O68 Cu1 152.8(4) . . ? S2A C69 S2B 42.5(4) . . ? S2B C70 S2A 43.9(4) . . ? O6A O4A S1 60.9(16) . . ? O6A O4A O5A 73.7(19) . . ? S1 O4A O5A 49.4(9) . . ? O5A O4B S1 56.8(15) . . ? O4B O5A S1 88.0(18) . . ? O4B O5A O4A 115(2) . . ? S1 O5A O4A 59.9(11) . . ? O4B O5A O6A 138(2) . . ? S1 O5A O6A 51.9(10) . . ? O4A O5A O6A 39.5(10) . . ? O6A O5B S1 60.3(14) . . ? O4A O6A O5B 107(2) . . ? O4A O6A S1 72.9(19) . . ? O5B O6A S1 73.1(15) . . ? O4A O6A O5A 66.7(18) . . ? O5B O6A O5A 122(2) . . ? S1 O6A O5A 49.1(10) . . ? N103 Cu2 N71 176.5(3) . . ? N103 Cu2 N87 89.2(3) . . ? N71 Cu2 N87 89.8(3) . . ? N103 Cu2 N119 90.6(3) . . ? N71 Cu2 N119 90.1(3) . . ? N87 Cu2 N119 175.8(3) . . ? N103 Cu2 O140 92.0(2) . . ? N71 Cu2 O140 91.4(2) . . ? N87 Cu2 O140 92.1(2) . . ? N119 Cu2 O140 92.1(2) . . ? O2A S3 O1B 79.1(11) . . ? O2A S3 O135 126.6(10) . . ? O1B S3 O135 121.0(9) . . ? O2A S3 O3A 99.0(9) . . ? O1B S3 O3A 116.2(9) . . ? O135 S3 O3A 110.7(5) . . ? O2A S3 O2B 121.9(11) . . ? O1B S3 O2B 46.7(9) . . ? O135 S3 O2B 102.0(7) . . ? O3A S3 O2B 90.1(6) . . ? O2A S3 O1A 36.7(9) . . ? O1B S3 O1A 113.3(10) . . ? O135 S3 O1A 95.8(6) . . ? O3A S3 O1A 94.8(6) . . ? O2B S3 O1A 158.6(8) . . ? S4B S4A O140 64.1(5) . . ? S4B S4A C141 70.2(7) . . ? O140 S4A C141 111.5(7) . . ? S4B S4A C142 68.3(7) . . ? O140 S4A C142 108.3(7) . . ? C141 S4A C142 98.2(8) . . ? S4A S4B O140 65.9(5) . . ? S4A S4B C142 69.7(7) . . ? O140 S4B C142 110.3(7) . . ? S4A S4B C141 67.5(7) . . ? O140 S4B C141 110.9(7) . . ? C142 S4B C141 97.7(8) . . ? C76 N71 C72 118.9(7) . . ? C76 N71 Cu2 120.0(5) . . ? C72 N71 Cu2 121.0(6) . . ? N71 C72 C73 122.1(8) . . ? N71 C72 H72 118.9 . . ? C73 C72 H72 118.9 . . ? C74 C73 C72 120.4(8) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C73 C74 C75 119.2(9) . . ? C73 C74 H74 120.4 . . ? C75 C74 H74 120.4 . . ? C74 C75 N77 120.1(8) . . ? C74 C75 C76 118.1(8) . . ? N77 C75 C76 121.7(8) . . ? N71 C76 C75 121.0(8) . . ? N71 C76 H76 119.5 . . ? C75 C76 H76 119.5 . . ? C78 N77 C75 128.3(8) . . ? C78 N77 H77 115.8 . . ? C75 N77 H77 115.8 . . ? O79 C78 N77 125.1(9) . . ? O79 C78 N80 122.8(9) . . ? N77 C78 N80 111.9(9) . . ? C78 N80 C81 123.0(9) . . ? C78 N80 H80 118.5 . . ? C81 N80 H80 118.5 . . ? C82 C81 C86 116.3(10) . . ? C82 C81 N80 122.5(11) . . ? C86 C81 N80 121.2(11) . . ? C81 C82 F21 119.2(11) . . ? C81 C82 C83 121.5(11) . . ? F21 C82 C83 119.3(12) . . ? F22 C83 C84 120.9(12) . . ? F22 C83 C82 119.7(13) . . ? C84 C83 C82 119.4(11) . . ? C85 C84 F23 121.5(12) . . ? C85 C84 C83 121.1(10) . . ? F23 C84 C83 117.5(12) . . ? C84 C85 F24 119.3(11) . . ? C84 C85 C86 118.6(11) . . ? F24 C85 C86 122.1(11) . . ? F25 C86 C85 118.3(11) . . ? F25 C86 C81 118.6(10) . . ? C85 C86 C81 123.1(11) . . ? C92 N87 C88 120.4(7) . . ? C92 N87 Cu2 120.7(6) . . ? C88 N87 Cu2 118.7(6) . . ? N87 C88 C89 120.6(8) . . ? N87 C88 H88 119.7 . . ? C89 C88 H88 119.7 . . ? C90 C89 C88 120.3(9) . . ? C90 C89 H89 119.8 . . ? C88 C89 H89 119.8 . . ? C89 C90 C91 119.5(8) . . ? C89 C90 H90 120.3 . . ? C91 C90 H90 120.3 . . ? N93 C91 C90 119.1(8) . . ? N93 C91 C92 123.6(8) . . ? C90 C91 C92 117.2(8) . . ? N87 C92 C91 121.8(8) . . ? N87 C92 H92 119.1 . . ? C91 C92 H92 119.1 . . ? C94 N93 C91 128.0(8) . . ? C94 N93 H93 116.0 . . ? C91 N93 H93 116.0 . . ? O95 C94 N93 124.3(9) . . ? O95 C94 N96 124.3(10) . . ? N93 C94 N96 111.4(9) . . ? C94 N96 C97 120.0(8) . . ? C94 N96 H96 120.0 . . ? C97 N96 H96 120.0 . . ? C102 C97 C98 116.8(12) . . ? C102 C97 N96 122.7(11) . . ? C98 C97 N96 120.5(12) . . ? F26 C98 C97 119.9(13) . . ? F26 C98 C99 119.1(14) . . ? C97 C98 C99 120.8(14) . . ? F27 C99 C100 121.5(15) . . ? F27 C99 C98 120.5(16) . . ? C100 C99 C98 118.0(13) . . ? C101 C100 F28 120.4(16) . . ? C101 C100 C99 122.0(13) . . ? F28 C100 C99 117.5(15) . . ? C100 C101 F29 121.0(14) . . ? C100 C101 C102 119.4(14) . . ? F29 C101 C102 119.5(15) . . ? C97 C102 F30 119.1(12) . . ? C97 C102 C101 122.6(13) . . ? F30 C102 C101 118.1(14) . . ? C104 N103 C108 117.6(7) . . ? C104 N103 Cu2 121.9(6) . . ? C108 N103 Cu2 120.5(5) . . ? N103 C104 C105 124.6(8) . . ? N103 C104 H104 117.7 . . ? C105 C104 H104 117.7 . . ? C106 C105 C104 117.9(8) . . ? C106 C105 H105 121.1 . . ? C104 C105 H105 121.1 . . ? C105 C106 C107 119.5(9) . . ? C105 C106 H106 120.2 . . ? C107 C106 H106 120.2 . . ? C106 C107 C108 119.5(9) . . ? C106 C107 N109 117.9(8) . . ? C108 C107 N109 122.6(8) . . ? N103 C108 C107 120.7(8) . . ? N103 C108 H108 119.7 . . ? C107 C108 H108 119.7 . . ? C110 N109 C107 126.6(8) . . ? C110 N109 H109 116.7 . . ? C107 N109 H109 116.7 . . ? O111 C110 N109 127.4(9) . . ? O111 C110 N112 122.3(9) . . ? N109 C110 N112 110.3(9) . . ? C110 N112 C113 120.7(8) . . ? C110 N112 H112 119.6 . . ? C113 N112 H112 119.6 . . ? C114 C113 C118 115.4(11) . . ? C114 C113 N112 122.2(10) . . ? C118 C113 N112 122.4(11) . . ? F31 C114 C113 119.5(11) . . ? F31 C114 C115 119.3(11) . . ? C113 C114 C115 121.1(11) . . ? C116 C115 F32 120.9(12) . . ? C116 C115 C114 120.2(11) . . ? F32 C115 C114 118.8(12) . . ? C115 C116 C117 122.3(11) . . ? C115 C116 F33 118.7(12) . . ? C117 C116 F33 119.0(11) . . ? F34 C117 C116 121.5(11) . . ? F34 C117 C118 120.7(13) . . ? C116 C117 C118 117.7(12) . . ? F35 C118 C113 119.1(11) . . ? F35 C118 C117 117.8(12) . . ? C113 C118 C117 123.1(12) . . ? C124 N119 C120 118.9(7) . . ? C124 N119 Cu2 120.6(6) . . ? C120 N119 Cu2 120.2(6) . . ? N119 C120 C121 121.6(9) . . ? N119 C120 H120 119.2 . . ? C121 C120 H120 119.2 . . ? C122 C121 C120 119.5(8) . . ? C122 C121 H121 120.3 . . ? C120 C121 H121 120.3 . . ? C121 C122 C123 120.5(9) . . ? C121 C122 H122 119.8 . . ? C123 C122 H122 119.8 . . ? N125 C123 C122 119.1(8) . . ? N125 C123 C124 124.0(8) . . ? C122 C123 C124 116.8(8) . . ? N119 C124 C123 122.5(8) . . ? N119 C124 H124 118.7 . . ? C123 C124 H124 118.7 . . ? C123 N125 C126 129.0(8) . . ? C123 N125 H125 115.5 . . ? C126 N125 H125 115.5 . . ? O127 C126 N128 123.1(10) . . ? O127 C126 N125 123.5(9) . . ? N128 C126 N125 113.4(10) . . ? C126 N128 C129 122.2(9) . . ? C126 N128 H128 118.9 . . ? C129 N128 H128 118.9 . . ? C134 C129 C130 117.1(12) . . ? C134 C129 N128 121.3(13) . . ? C130 C129 N128 121.6(14) . . ? F36 C130 C131 115.9(15) . . ? F36 C130 C129 121.0(13) . . ? C131 C130 C129 123.1(16) . . ? F37 C131 C130 125(2) . . ? F37 C131 C132 119.6(18) . . ? C130 C131 C132 115.7(16) . . ? C133 C132 F38 124(2) . . ? C133 C132 C131 119.5(15) . . ? F38 C132 C131 116.7(17) . . ? C132 C133 C134 123.2(17) . . ? C132 C133 F39 118.2(16) . . ? C134 C133 F39 118.6(18) . . ? C133 C134 C129 121.2(14) . . ? C133 C134 F40 120.0(17) . . ? C129 C134 F40 118.7(13) . . ? S4B O140 S4A 50.0(4) . . ? S4B O140 Cu2 156.8(5) . . ? S4A O140 Cu2 153.2(4) . . ? S4A C141 S4B 42.3(5) . . ? S4B C142 S4A 42.0(4) . . ? O2A O1A S3 58.8(16) . . ? O2B O1B S3 73.5(14) . . ? O2B O1B O2A 119.9(19) . . ? S3 O1B O2A 50.3(10) . . ? O1A O2A S3 84.5(19) . . ? O1A O2A O1B 131(2) . . ? S3 O2A O1B 50.6(10) . . ? O1B O2B S3 59.8(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N112 H112 O6A 0.86 2.50 3.36(3) 174.9 2_666 N112 H112 O5A 0.86 2.34 3.076(19) 143.4 2_666 N112 H112 O4A 0.86 2.03 2.83(2) 153.4 2_666 N109 H109 O4A 0.86 2.40 3.15(2) 144.8 2_666 N109 H109 O5A 0.86 2.10 2.906(19) 156.6 2_666 N109 H109 O4B 0.86 2.00 2.805(15) 155.0 2_666 N80 H80 O6B 0.86 2.20 2.970(12) 149.5 2_766 N77 H77 O6B 0.86 2.23 3.016(11) 151.4 2_766 N77 H77 O5B 0.86 2.23 2.991(15) 147.3 2_766 N42 H42 O6A 0.86 2.09 2.87(3) 149.3 2_666 N42 H42 O5B 0.86 2.00 2.784(17) 151.2 2_666 N39 H39 O6A 0.86 2.18 2.98(2) 153.8 2_666 N39 H39 O5B 0.86 2.10 2.876(15) 149.9 2_666 N39 H39 O4A 0.86 2.08 2.88(2) 154.8 2_666 N10 H10 O5A 0.86 2.04 2.90(2) 176.1 2_676 N10 H10 O4B 0.86 2.05 2.830(15) 151.0 2_676 N7 H7 O4B 0.86 2.50 3.178(14) 136.8 2_676 N7 H7 O6B 0.86 2.10 2.930(11) 163.2 2_676 _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 21.32 _diffrn_measured_fraction_theta_full 0.839 _refine_diff_density_max 1.143 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.078 # _vrf_REFLT03_y3 ; PROBLEM: Reflection count<85% complete >From the CIF:_diffrn_reflns_theta_max 21.32 >From the CIF:_diffrn_reflns_theta_full 21.32 >From the CIF:_reflns_number_total 11135 TEST 2: Reflns within_diffrn_reflns_theta_max count of symmetry unique reflns 13276 completeness(_total/calc) 83.8% RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_THETM01_y3 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5116 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT022_y3 ; PROBLM: Ratio Uniqe/Expected Reflections (too)Low......0.84 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT241_y3 ; PROBLEM: Check high Ueq as compared to neighbors for X RESPONSE: X is a part of disordered moiety. ; _vrf_PLAT242_y3 ; PROBLEM: Check low Ueq as compared to neighbors for S1 RESPONSE: atom is a part or attached with either disordered moiety or atom with high thermal parameter. ; _database_code_depnum_ccdc_archive 'CCDC 926124' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form # Attachment 'CC2.cif' data_bcam26_0m #TrackingRef 'CC2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H42 Cd2 F20 N12 O17 S4' _chemical_formula_weight 1840.02 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' Cd Cd -0.8075 1.2024 '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 14.0690(15) _cell_length_b 16.4751(18) _cell_length_c 17.8873(19) _cell_angle_alpha 70.271(2) _cell_angle_beta 81.333(2) _cell_angle_gamma 67.876(2) _cell_volume 3614.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1828 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7388 _exptl_absorpt_correction_T_max 0.8522 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30827 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 24.11 _reflns_number_total 11435 _reflns_number_gt 8097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material Shelxl-97 _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^)+(0.1243P)^2^+1.0433P] 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 11435 _refine_ls_number_parameters 968 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1966 _refine_ls_wR_factor_gt 0.1769 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.84455(4) 0.55587(4) 0.22875(3) 0.02471(18) Uani 1 1 d . . . Cd2 Cd 0.39620(4) 0.54458(4) 0.26098(3) 0.02648(18) Uani 1 1 d . . . S1 S 1.04598(14) 0.61774(13) 0.22215(10) 0.0263(4) Uani 1 1 d . . . S2 S 1.02756(15) 0.34727(13) 0.24719(11) 0.0315(5) Uani 1 1 d . . . S3 S 0.59610(13) 0.61241(13) 0.19418(10) 0.0238(4) Uani 1 1 d . . . S4 S 0.59474(17) 0.35639(15) 0.24367(13) 0.0429(5) Uani 1 1 d . . . F1 F 0.6894(4) 0.1495(4) 0.7371(4) 0.0703(17) Uani 1 1 d . . . F2 F 0.7725(5) -0.0360(4) 0.7734(4) 0.086(2) Uani 1 1 d . . . F3 F 0.6761(5) -0.1306(4) 0.7335(4) 0.088(2) Uani 1 1 d . . . F4 F 0.4887(6) -0.0375(4) 0.6661(4) 0.084(2) Uani 1 1 d . . . F5 F 0.4008(4) 0.1454(4) 0.6357(3) 0.0601(14) Uani 1 1 d . . . F6 F 0.5498(5) -0.1251(3) 0.1493(3) 0.0653(16) Uani 1 1 d . . . F7 F 0.6668(4) -0.0370(4) 0.1706(3) 0.0652(16) Uani 1 1 d . . . F8 F 0.3724(5) -0.0273(4) 0.0695(3) 0.0667(16) Uani 1 1 d . . . F9 F 0.3130(4) 0.1563(4) 0.0090(3) 0.0566(14) Uani 1 1 d . . . F10 F 0.6124(4) 0.1473(3) 0.1050(3) 0.0559(14) Uani 1 1 d . . . F11 F 1.1064(7) -0.0520(4) 0.1702(4) 0.115(3) Uani 1 1 d . . . F12 F 0.9799(8) -0.1268(4) 0.1425(4) 0.126(4) Uani 1 1 d . . . F13 F 1.0778(5) 0.1284(4) 0.0985(3) 0.0702(18) Uani 1 1 d . . . F14 F 0.8196(6) -0.0191(5) 0.0433(5) 0.109(3) Uani 1 1 d . . . F15 F 0.7897(5) 0.1612(4) -0.0275(4) 0.0780(19) Uani 1 1 d . . . F16 F 1.1324(4) -0.1228(3) 0.7184(3) 0.0607(15) Uani 1 1 d . . . F17 F 0.9397(4) -0.0202(4) 0.6658(3) 0.0576(14) Uani 1 1 d . . . F18 F 0.8742(4) 0.1645(3) 0.6243(3) 0.0493(13) Uani 1 1 d . . . F19 F 1.1942(4) 0.1474(3) 0.6903(3) 0.0607(15) Uani 1 1 d . . . F20 F 1.2582(4) -0.0387(4) 0.7331(4) 0.0750(18) Uani 1 1 d . . . N1 N 0.8486(4) 0.5517(4) 0.0997(3) 0.0237(13) Uani 1 1 d . . . C2 C 0.8483(6) 0.6268(5) 0.0401(4) 0.0307(18) Uani 1 1 d . . . H2 H 0.8394 0.6806 0.0510 0.037 Uiso 1 1 calc R . . C3 C 0.8613(6) 0.6258(6) -0.0385(4) 0.0319(18) Uani 1 1 d . . . H3 H 0.8613 0.6785 -0.0797 0.038 Uiso 1 1 calc R . . C4 C 0.8738(6) 0.5470(5) -0.0542(4) 0.0293(18) Uani 1 1 d . . . H4 H 0.8812 0.5462 -0.1066 0.035 Uiso 1 1 calc R . . C5 C 0.8755(5) 0.4692(5) 0.0064(4) 0.0241(16) Uani 1 1 d . . . C6 C 0.8605(5) 0.4738(5) 0.0838(4) 0.0269(17) Uani 1 1 d . . . H6 H 0.8585 0.4221 0.1255 0.032 Uiso 1 1 calc R . . N7 N 0.8904(5) 0.3898(4) -0.0127(3) 0.0291(15) Uani 1 1 d . . . H7 H 0.8934 0.3959 -0.0626 0.035 Uiso 1 1 calc R . . C8 C 0.9009(6) 0.3033(5) 0.0376(4) 0.0293(17) Uani 1 1 d . . . O9 O 0.8944(5) 0.2839(4) 0.1092(3) 0.0426(15) Uani 1 1 d . . . N10 N 0.9161(5) 0.2419(4) -0.0031(4) 0.0360(16) Uani 1 1 d . . . H10 H 0.9169 0.2606 -0.0542 0.043 Uiso 1 1 calc R . . C11 C 0.9303(7) 0.1496(6) 0.0371(5) 0.041(2) Uani 1 1 d . . . C12 C 0.8682(8) 0.1077(7) 0.0242(7) 0.062(3) Uani 1 1 d . . . C13 C 0.8807(11) 0.0186(8) 0.0592(8) 0.077(4) Uani 1 1 d . . . C14 C 0.9630(13) -0.0378(7) 0.1096(6) 0.084(5) Uani 1 1 d . . . C15 C 1.0271(10) 0.0012(7) 0.1224(5) 0.070(4) Uani 1 1 d . . . C16 C 1.0142(8) 0.0916(6) 0.0874(5) 0.050(3) Uani 1 1 d . . . N17 N 0.8444(4) 0.5570(4) 0.3580(3) 0.0252(14) Uani 1 1 d . . . C18 C 0.8857(5) 0.4802(5) 0.4184(4) 0.0266(17) Uani 1 1 d . . . H18 H 0.9159 0.4241 0.4081 0.032 Uiso 1 1 calc R . . C19 C 0.8847(5) 0.4821(5) 0.4956(4) 0.0233(16) Uani 1 1 d . . . C20 C 0.8402(6) 0.5662(5) 0.5099(4) 0.0302(18) Uani 1 1 d . . . H20 H 0.8388 0.5692 0.5610 0.036 Uiso 1 1 calc R . . C21 C 0.7979(6) 0.6453(5) 0.4490(4) 0.0309(18) Uani 1 1 d . . . H21 H 0.7682 0.7021 0.4583 0.037 Uiso 1 1 calc R . . C22 C 0.8006(6) 0.6384(5) 0.3732(4) 0.0290(17) Uani 1 1 d . . . H22 H 0.7714 0.6914 0.3318 0.035 Uiso 1 1 calc R . . N23 N 0.9254(5) 0.4035(4) 0.5606(3) 0.0269(14) Uani 1 1 d . . . H23 H 0.9252 0.4139 0.6046 0.032 Uiso 1 1 calc R . . C24 C 0.9647(6) 0.3140(5) 0.5634(4) 0.0296(17) Uani 1 1 d . . . O25 O 0.9698(4) 0.2863(3) 0.5064(3) 0.0383(14) Uani 1 1 d . . . N26 N 1.0003(5) 0.2557(4) 0.6360(4) 0.0344(16) Uani 1 1 d . . . H26 H 1.0026 0.2790 0.6718 0.041 Uiso 1 1 calc R . . C27 C 1.0330(6) 0.1609(5) 0.6553(4) 0.0323(18) Uani 1 1 d . . . C28 C 0.9721(6) 0.1141(6) 0.6491(5) 0.038(2) Uani 1 1 d . . . C29 C 1.0021(7) 0.0218(6) 0.6694(5) 0.041(2) Uani 1 1 d . . . C30 C 1.1013(7) -0.0313(5) 0.6993(5) 0.043(2) Uani 1 1 d . . . C31 C 1.1625(7) 0.0133(6) 0.7067(5) 0.044(2) Uani 1 1 d . . . C32 C 1.1308(6) 0.1049(6) 0.6841(5) 0.039(2) Uani 1 1 d . . . O33 O 1.0037(4) 0.5679(4) 0.1889(3) 0.0316(12) Uani 1 1 d . . . O34 O 1.0995(4) 0.5553(3) 0.2965(3) 0.0306(12) Uani 1 1 d . . . O35 O 1.1218(4) 0.6472(4) 0.1642(3) 0.0315(12) Uani 1 1 d . . . O36 O 0.9629(4) 0.6968(4) 0.2384(3) 0.0327(12) Uani 1 1 d . . . O37 O 0.9172(4) 0.3964(4) 0.2728(3) 0.0318(12) Uani 1 1 d . . . C38 C 1.0359(7) 0.2319(6) 0.2679(6) 0.056(3) Uani 1 1 d . . . H38A H 1.0108 0.2102 0.3211 0.083 Uiso 1 1 calc R . . H38B H 1.1061 0.1940 0.2627 0.083 Uiso 1 1 calc R . . H38C H 0.9951 0.2288 0.2311 0.083 Uiso 1 1 calc R . . C39 C 1.1045(7) 0.3324(6) 0.3235(5) 0.050(2) Uani 1 1 d . . . H39A H 1.0908 0.3908 0.3310 0.075 Uiso 1 1 calc R . . H39B H 1.1756 0.3072 0.3090 0.075 Uiso 1 1 calc R . . H39C H 1.0888 0.2910 0.3719 0.075 Uiso 1 1 calc R . . O40 O 0.7812(4) 0.7170(4) 0.1823(3) 0.0441(15) Uani 1 1 d . . . O41 O 0.6768(4) 0.5668(3) 0.2564(3) 0.0301(12) Uani 1 1 d . . . O42 O 0.6103(4) 0.6959(4) 0.1402(3) 0.0340(13) Uani 1 1 d . . . O43 O 0.6019(4) 0.5489(3) 0.1507(3) 0.0289(12) Uani 1 1 d . . . O44 O 0.4958(4) 0.6360(4) 0.2369(3) 0.0351(13) Uani 1 1 d . . . N45 N 0.3815(4) 0.5515(4) 0.1324(3) 0.0268(14) Uani 1 1 d . . . C46 C 0.3709(5) 0.6299(5) 0.0738(4) 0.0304(18) Uani 1 1 d . . . H46 H 0.3703 0.6811 0.0854 0.036 Uiso 1 1 calc R . . C47 C 0.3608(5) 0.6366(5) -0.0045(4) 0.0294(17) Uani 1 1 d . . . H47 H 0.3517 0.6922 -0.0446 0.035 Uiso 1 1 calc R . . C48 C 0.3644(5) 0.5607(5) -0.0222(4) 0.0304(18) Uani 1 1 d . . . H48 H 0.3574 0.5645 -0.0743 0.036 Uiso 1 1 calc R . . C49 C 0.3786(5) 0.4777(5) 0.0385(4) 0.0267(17) Uani 1 1 d . . . C50 C 0.3839(5) 0.4769(5) 0.1159(4) 0.0260(17) Uani 1 1 d . . . H50 H 0.3892 0.4231 0.1575 0.031 Uiso 1 1 calc R . . N51 N 0.3868(4) 0.4013(4) 0.0169(3) 0.0281(14) Uani 1 1 d . . . H51 H 0.3725 0.4118 -0.0313 0.034 Uiso 1 1 calc R . . C52 C 0.4148(6) 0.3125(5) 0.0639(4) 0.0309(18) Uani 1 1 d . . . O53 O 0.4265(5) 0.2853(4) 0.1356(3) 0.0420(14) Uani 1 1 d . . . N54 N 0.4286(5) 0.2530(4) 0.0219(4) 0.0381(17) Uani 1 1 d . . . H54 H 0.4182 0.2751 -0.0283 0.046 Uiso 1 1 calc R . . C55 C 0.4586(6) 0.1582(5) 0.0571(4) 0.0340(19) Uani 1 1 d . . . C56 C 0.4025(7) 0.1089(6) 0.0493(4) 0.039(2) Uani 1 1 d . . . C57 C 0.4300(8) 0.0170(7) 0.0797(5) 0.049(2) Uani 1 1 d . . . C58 C 0.5210(7) -0.0336(5) 0.1205(4) 0.040(2) Uani 1 1 d . . . C59 C 0.5779(7) 0.0135(6) 0.1291(5) 0.046(2) Uani 1 1 d . . . C60 C 0.5516(7) 0.1058(5) 0.0985(4) 0.035(2) Uani 1 1 d . . . N61 N 0.3688(5) 0.5513(4) 0.3895(3) 0.0287(14) Uani 1 1 d . . . C62 C 0.4010(5) 0.4744(5) 0.4492(4) 0.0265(17) Uani 1 1 d . . . H62 H 0.4324 0.4185 0.4386 0.032 Uiso 1 1 calc R . . C63 C 0.3884(5) 0.4757(5) 0.5283(4) 0.0242(16) Uani 1 1 d . . . C64 C 0.3421(6) 0.5582(5) 0.5431(4) 0.0312(18) Uani 1 1 d . . . H64 H 0.3340 0.5607 0.5949 0.037 Uiso 1 1 calc R . . C65 C 0.3072(7) 0.6383(6) 0.4801(5) 0.042(2) Uani 1 1 d . . . H65 H 0.2749 0.6951 0.4890 0.050 Uiso 1 1 calc R . . C66 C 0.3217(7) 0.6316(6) 0.4038(5) 0.043(2) Uani 1 1 d . . . H66 H 0.2977 0.6848 0.3612 0.052 Uiso 1 1 calc R . . N67 N 0.4223(5) 0.3958(4) 0.5934(3) 0.0315(15) Uani 1 1 d . . . H67 H 0.4128 0.4045 0.6391 0.038 Uiso 1 1 calc R . . C68 C 0.4675(6) 0.3076(6) 0.5942(4) 0.0341(19) Uani 1 1 d . . . O69 O 0.4814(4) 0.2803(4) 0.5361(3) 0.0401(14) Uani 1 1 d . . . N70 N 0.5010(5) 0.2484(4) 0.6681(4) 0.0375(16) Uani 1 1 d . . . H70 H 0.4948 0.2704 0.7066 0.045 Uiso 1 1 calc R . . C71 C 0.5448(7) 0.1535(6) 0.6820(4) 0.039(2) Uani 1 1 d . . . C72 C 0.4961(7) 0.1032(6) 0.6662(5) 0.045(2) Uani 1 1 d . . . C73 C 0.5394(8) 0.0101(7) 0.6808(6) 0.055(3) Uani 1 1 d . . . C74 C 0.6339(8) -0.0383(6) 0.7179(5) 0.057(3) Uani 1 1 d . . . C75 C 0.6817(8) 0.0118(7) 0.7352(6) 0.059(3) Uani 1 1 d . . . C76 C 0.6405(7) 0.1036(6) 0.7175(5) 0.048(2) Uani 1 1 d . . . O77 O 0.5272(4) 0.4059(4) 0.2997(3) 0.0486(16) Uani 1 1 d . . . C78 C 0.5949(10) 0.2433(7) 0.2771(9) 0.100(5) Uani 1 1 d . . . H78A H 0.6051 0.2185 0.3334 0.151 Uiso 1 1 calc R . . H78B H 0.6494 0.2063 0.2505 0.151 Uiso 1 1 calc R . . H78C H 0.5304 0.2433 0.2659 0.151 Uiso 1 1 calc R . . C79 C 0.7225(6) 0.3356(6) 0.2642(6) 0.051(2) Uani 1 1 d . . . H79A H 0.7313 0.3932 0.2556 0.077 Uiso 1 1 calc R . . H79B H 0.7691 0.3038 0.2297 0.077 Uiso 1 1 calc R . . H79C H 0.7365 0.2985 0.3185 0.077 Uiso 1 1 calc R . . O80 O 0.2547(4) 0.6878(4) 0.2283(3) 0.0352(13) Uani 1 1 d . . . O81 O 0.2981(4) 0.4512(4) 0.2995(3) 0.0453(15) 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 Cd1 0.0267(3) 0.0298(3) 0.0200(3) -0.0125(2) 0.0002(2) -0.0085(2) Cd2 0.0274(3) 0.0310(3) 0.0207(3) -0.0120(2) 0.0020(2) -0.0073(2) S1 0.0288(10) 0.0362(11) 0.0176(9) -0.0085(8) -0.0026(7) -0.0143(9) S2 0.0373(11) 0.0265(11) 0.0280(10) -0.0108(8) -0.0020(8) -0.0058(9) S3 0.0229(9) 0.0308(11) 0.0188(9) -0.0084(8) -0.0048(7) -0.0084(8) S4 0.0421(13) 0.0344(13) 0.0492(13) -0.0169(10) 0.0002(10) -0.0071(10) F1 0.058(4) 0.053(4) 0.088(4) 0.000(3) -0.030(3) -0.014(3) F2 0.054(4) 0.058(4) 0.106(5) 0.005(4) -0.015(3) 0.003(3) F3 0.108(5) 0.037(4) 0.088(5) -0.017(3) 0.010(4) 0.001(3) F4 0.126(6) 0.063(4) 0.061(4) -0.015(3) -0.010(4) -0.031(4) F5 0.060(4) 0.056(3) 0.056(3) -0.004(3) -0.016(3) -0.017(3) F6 0.097(4) 0.030(3) 0.047(3) -0.007(2) 0.012(3) -0.009(3) F7 0.076(4) 0.048(3) 0.048(3) -0.003(3) -0.011(3) -0.002(3) F8 0.091(4) 0.060(4) 0.059(4) -0.025(3) 0.004(3) -0.033(3) F9 0.057(3) 0.058(3) 0.054(3) -0.014(3) -0.012(3) -0.017(3) F10 0.063(3) 0.050(3) 0.051(3) -0.003(3) -0.021(3) -0.020(3) F11 0.204(9) 0.046(4) 0.046(4) -0.010(3) -0.041(5) 0.020(5) F12 0.256(10) 0.032(4) 0.057(4) -0.010(3) 0.053(5) -0.041(5) F13 0.096(5) 0.050(4) 0.051(3) -0.022(3) -0.040(3) 0.009(3) F14 0.119(6) 0.081(5) 0.162(7) -0.078(5) 0.076(5) -0.069(5) F15 0.054(4) 0.071(4) 0.129(6) -0.061(4) 0.003(4) -0.019(3) F16 0.078(4) 0.028(3) 0.066(4) -0.006(3) -0.012(3) -0.011(3) F17 0.070(4) 0.046(3) 0.062(4) -0.016(3) -0.003(3) -0.026(3) F18 0.050(3) 0.039(3) 0.052(3) -0.008(2) -0.013(2) -0.010(2) F19 0.048(3) 0.039(3) 0.094(4) -0.023(3) -0.023(3) -0.003(3) F20 0.062(4) 0.045(3) 0.102(5) -0.015(3) -0.032(3) 0.002(3) N1 0.024(3) 0.029(4) 0.022(3) -0.011(3) 0.002(2) -0.011(3) C2 0.029(4) 0.031(5) 0.035(4) -0.016(4) 0.004(3) -0.010(3) C3 0.037(5) 0.040(5) 0.017(4) -0.008(3) 0.007(3) -0.016(4) C4 0.033(4) 0.037(5) 0.017(4) -0.013(3) 0.002(3) -0.009(4) C5 0.024(4) 0.032(4) 0.020(4) -0.012(3) 0.005(3) -0.012(3) C6 0.022(4) 0.027(4) 0.030(4) -0.011(3) 0.001(3) -0.004(3) N7 0.035(4) 0.033(4) 0.017(3) -0.012(3) -0.004(3) -0.005(3) C8 0.029(4) 0.031(5) 0.026(4) -0.009(4) -0.002(3) -0.009(3) O9 0.066(4) 0.034(3) 0.023(3) -0.014(2) 0.000(3) -0.008(3) N10 0.057(5) 0.027(4) 0.024(3) -0.012(3) -0.005(3) -0.010(3) C11 0.054(6) 0.035(5) 0.031(5) -0.020(4) 0.008(4) -0.008(4) C12 0.060(7) 0.055(7) 0.081(8) -0.045(6) 0.034(6) -0.025(6) C13 0.105(10) 0.041(7) 0.095(9) -0.049(7) 0.060(8) -0.036(7) C14 0.172(15) 0.029(7) 0.042(6) -0.018(5) 0.057(8) -0.043(8) C15 0.134(11) 0.021(6) 0.017(4) 0.003(4) -0.007(5) 0.010(6) C16 0.084(7) 0.029(5) 0.030(5) -0.014(4) -0.003(5) -0.006(5) N17 0.025(3) 0.028(4) 0.023(3) -0.010(3) 0.000(3) -0.007(3) C18 0.029(4) 0.024(4) 0.028(4) -0.011(3) 0.004(3) -0.009(3) C19 0.022(4) 0.030(4) 0.022(4) -0.012(3) -0.001(3) -0.010(3) C20 0.042(5) 0.035(5) 0.019(4) -0.014(3) 0.005(3) -0.017(4) C21 0.042(5) 0.023(4) 0.027(4) -0.012(3) 0.000(3) -0.007(4) C22 0.036(4) 0.026(4) 0.026(4) -0.010(3) 0.002(3) -0.011(4) N23 0.037(4) 0.023(4) 0.021(3) -0.007(3) -0.007(3) -0.007(3) C24 0.032(4) 0.029(5) 0.028(4) -0.006(3) -0.004(3) -0.013(4) O25 0.064(4) 0.029(3) 0.023(3) -0.010(2) -0.004(3) -0.014(3) N26 0.052(4) 0.033(4) 0.024(3) -0.015(3) -0.005(3) -0.013(3) C27 0.049(5) 0.021(4) 0.025(4) -0.010(3) -0.001(4) -0.008(4) C28 0.035(5) 0.036(5) 0.035(5) -0.014(4) -0.004(4) 0.001(4) C29 0.062(6) 0.032(5) 0.031(5) -0.016(4) 0.002(4) -0.016(5) C30 0.055(6) 0.015(5) 0.045(5) -0.005(4) -0.002(4) 0.000(4) C31 0.044(5) 0.032(5) 0.044(5) -0.009(4) -0.010(4) 0.003(4) C32 0.044(5) 0.032(5) 0.044(5) -0.016(4) -0.007(4) -0.010(4) O33 0.027(3) 0.050(3) 0.030(3) -0.029(3) 0.000(2) -0.013(2) O34 0.043(3) 0.034(3) 0.016(2) -0.008(2) -0.007(2) -0.012(3) O35 0.020(3) 0.054(4) 0.027(3) -0.021(3) 0.000(2) -0.012(2) O36 0.028(3) 0.042(3) 0.034(3) -0.018(3) -0.006(2) -0.012(2) O37 0.031(3) 0.045(3) 0.025(3) -0.017(2) -0.002(2) -0.014(3) C38 0.056(6) 0.031(5) 0.083(7) -0.018(5) -0.033(5) -0.006(4) C39 0.057(6) 0.050(6) 0.050(6) -0.011(5) -0.030(5) -0.020(5) O40 0.047(4) 0.035(3) 0.050(4) -0.014(3) -0.020(3) -0.007(3) O41 0.029(3) 0.044(3) 0.019(3) -0.008(2) -0.003(2) -0.016(2) O42 0.045(3) 0.042(3) 0.021(3) -0.009(2) -0.008(2) -0.020(3) O43 0.034(3) 0.035(3) 0.020(3) -0.012(2) -0.007(2) -0.010(2) O44 0.028(3) 0.055(4) 0.028(3) -0.016(3) -0.004(2) -0.018(3) N45 0.024(3) 0.032(4) 0.022(3) -0.009(3) -0.003(2) -0.006(3) C46 0.028(4) 0.027(4) 0.036(4) -0.014(4) 0.002(3) -0.007(3) C47 0.029(4) 0.029(4) 0.026(4) -0.006(3) -0.001(3) -0.007(3) C48 0.027(4) 0.043(5) 0.017(4) -0.008(3) -0.004(3) -0.009(4) C49 0.018(4) 0.038(5) 0.021(4) -0.013(3) 0.000(3) -0.003(3) C50 0.027(4) 0.030(4) 0.018(4) -0.008(3) 0.001(3) -0.007(3) N51 0.033(4) 0.034(4) 0.018(3) -0.007(3) -0.006(3) -0.010(3) C52 0.031(4) 0.036(5) 0.018(4) -0.006(4) 0.001(3) -0.006(4) O53 0.068(4) 0.037(3) 0.018(3) -0.009(2) -0.004(3) -0.014(3) N54 0.054(4) 0.037(4) 0.018(3) -0.003(3) -0.010(3) -0.012(3) C55 0.054(5) 0.038(5) 0.011(4) -0.004(3) -0.004(3) -0.018(4) C56 0.049(5) 0.033(5) 0.023(4) -0.011(4) -0.006(4) 0.002(4) C57 0.074(7) 0.060(7) 0.030(5) -0.024(5) 0.017(5) -0.041(6) C58 0.070(6) 0.024(5) 0.014(4) -0.008(3) 0.001(4) -0.005(4) C59 0.053(6) 0.041(6) 0.023(4) -0.005(4) -0.007(4) 0.006(5) C60 0.051(5) 0.024(5) 0.023(4) -0.004(3) -0.007(4) -0.005(4) N61 0.036(4) 0.027(4) 0.023(3) -0.011(3) -0.001(3) -0.007(3) C62 0.022(4) 0.036(5) 0.019(4) -0.013(3) 0.002(3) -0.004(3) C63 0.021(4) 0.032(4) 0.023(4) -0.010(3) -0.003(3) -0.010(3) C64 0.034(4) 0.036(5) 0.026(4) -0.014(4) -0.005(3) -0.008(4) C65 0.055(6) 0.035(5) 0.039(5) -0.025(4) 0.002(4) -0.009(4) C66 0.051(6) 0.036(5) 0.032(5) -0.008(4) 0.008(4) -0.010(4) N67 0.039(4) 0.030(4) 0.019(3) -0.006(3) -0.005(3) -0.004(3) C68 0.033(4) 0.045(5) 0.021(4) -0.008(4) 0.001(3) -0.013(4) O69 0.051(4) 0.042(4) 0.025(3) -0.015(3) -0.001(3) -0.010(3) N70 0.047(4) 0.036(4) 0.026(4) -0.012(3) -0.007(3) -0.006(3) C71 0.052(5) 0.035(5) 0.022(4) -0.004(4) -0.003(4) -0.012(4) C72 0.054(6) 0.035(5) 0.027(4) -0.001(4) -0.002(4) -0.003(4) C73 0.081(8) 0.050(7) 0.050(6) -0.027(5) 0.009(5) -0.034(6) C74 0.074(7) 0.032(6) 0.034(5) 0.001(4) 0.004(5) 0.002(5) C75 0.052(6) 0.041(6) 0.053(6) -0.003(5) 0.009(5) 0.003(5) C76 0.046(6) 0.033(6) 0.044(5) 0.001(4) -0.001(4) -0.003(4) O77 0.044(3) 0.045(4) 0.030(3) -0.005(3) 0.013(3) 0.004(3) C78 0.093(10) 0.045(7) 0.165(14) -0.025(8) 0.002(9) -0.034(7) C79 0.031(5) 0.048(6) 0.066(6) -0.023(5) -0.005(4) 0.000(4) O80 0.034(3) 0.035(3) 0.033(3) -0.014(2) -0.004(2) -0.003(2) O81 0.043(3) 0.059(4) 0.030(3) 0.001(3) -0.006(3) -0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O41 2.288(5) . ? Cd1 O33 2.306(5) . ? Cd1 N17 2.319(6) . ? Cd1 O37 2.322(5) . ? Cd1 N1 2.323(5) . ? Cd1 O40 2.341(5) . ? Cd2 O77 2.289(5) . ? Cd2 N45 2.300(6) . ? Cd2 N61 2.306(6) . ? Cd2 O81 2.311(6) . ? Cd2 O44 2.320(5) . ? Cd2 O80 2.399(5) . ? S1 O36 1.468(5) . ? S1 O35 1.472(5) . ? S1 O33 1.479(5) . ? S1 O34 1.480(5) . ? S2 O37 1.538(5) . ? S2 C39 1.764(8) . ? S2 C38 1.771(8) . ? S3 O42 1.454(5) . ? S3 O43 1.474(5) . ? S3 O44 1.480(5) . ? S3 O41 1.505(5) . ? S4 O77 1.501(6) . ? S4 C78 1.753(10) . ? S4 C79 1.770(9) . ? F1 C76 1.346(11) . ? F2 C75 1.365(11) . ? F3 C74 1.352(10) . ? F4 C73 1.344(11) . ? F5 C72 1.357(10) . ? F6 C58 1.333(9) . ? F7 C59 1.373(10) . ? F8 C57 1.342(10) . ? F9 C56 1.367(9) . ? F10 C60 1.318(9) . ? F11 C15 1.338(13) . ? F12 C14 1.323(11) . ? F13 C16 1.322(11) . ? F14 C13 1.343(14) . ? F15 C12 1.369(13) . ? F16 C30 1.334(9) . ? F17 C29 1.325(10) . ? F18 C28 1.364(9) . ? F19 C32 1.360(9) . ? F20 C31 1.349(10) . ? N1 C2 1.332(9) . ? N1 C6 1.352(9) . ? C2 C3 1.394(10) . ? C2 H2 0.9300 . ? C3 C4 1.362(10) . ? C3 H3 0.9300 . ? C4 C5 1.367(10) . ? C4 H4 0.9300 . ? C5 C6 1.393(10) . ? C5 N7 1.396(9) . ? C6 H6 0.9300 . ? N7 C8 1.370(9) . ? N7 H7 0.8600 . ? C8 O9 1.209(9) . ? C8 N10 1.374(9) . ? N10 C11 1.394(10) . ? N10 H10 0.8600 . ? C11 C12 1.385(13) . ? C11 C16 1.417(13) . ? C12 C13 1.340(15) . ? C13 C14 1.397(19) . ? C14 C15 1.370(18) . ? C15 C16 1.358(13) . ? N17 C18 1.348(9) . ? N17 C22 1.351(9) . ? C18 C19 1.389(10) . ? C18 H18 0.9300 . ? C19 C20 1.383(10) . ? C19 N23 1.408(9) . ? C20 C21 1.376(10) . ? C20 H20 0.9300 . ? C21 C22 1.392(10) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? N23 C24 1.352(9) . ? N23 H23 0.8600 . ? C24 O25 1.232(9) . ? C24 N26 1.362(9) . ? N26 C27 1.383(9) . ? N26 H26 0.8600 . ? C27 C28 1.387(11) . ? C27 C32 1.395(11) . ? C28 C29 1.346(11) . ? C29 C30 1.411(12) . ? C30 C31 1.369(12) . ? C31 C32 1.332(11) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? N45 C46 1.334(9) . ? N45 C50 1.347(9) . ? C46 C47 1.392(10) . ? C46 H46 0.9300 . ? C47 C48 1.372(10) . ? C47 H47 0.9300 . ? C48 C49 1.395(10) . ? C48 H48 0.9300 . ? C49 C50 1.393(9) . ? C49 N51 1.397(9) . ? C50 H50 0.9300 . ? N51 C52 1.356(9) . ? N51 H51 0.8600 . ? C52 O53 1.223(8) . ? C52 N54 1.368(10) . ? N54 C55 1.390(10) . ? N54 H54 0.8600 . ? C55 C56 1.376(11) . ? C55 C60 1.419(11) . ? C56 C57 1.344(12) . ? C57 C58 1.392(13) . ? C58 C59 1.361(13) . ? C59 C60 1.351(11) . ? N61 C62 1.324(9) . ? N61 C66 1.330(10) . ? C62 C63 1.406(9) . ? C62 H62 0.9300 . ? C63 C64 1.366(10) . ? C63 N67 1.405(9) . ? C64 C65 1.387(11) . ? C64 H64 0.9300 . ? C65 C66 1.386(11) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? N67 C68 1.345(10) . ? N67 H67 0.8600 . ? C68 O69 1.227(9) . ? C68 N70 1.375(9) . ? N70 C71 1.394(10) . ? N70 H70 0.8600 . ? C71 C72 1.370(12) . ? C71 C76 1.402(12) . ? C72 C73 1.366(13) . ? C73 C74 1.398(14) . ? C74 C75 1.371(15) . ? C75 C76 1.339(13) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 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 O41 Cd1 O33 171.24(18) . . ? O41 Cd1 N17 85.08(18) . . ? O33 Cd1 N17 97.57(18) . . ? O41 Cd1 O37 97.40(18) . . ? O33 Cd1 O37 91.01(18) . . ? N17 Cd1 O37 89.06(18) . . ? O41 Cd1 N1 95.93(18) . . ? O33 Cd1 N1 81.59(18) . . ? N17 Cd1 N1 178.6(2) . . ? O37 Cd1 N1 89.81(18) . . ? O41 Cd1 O40 85.99(19) . . ? O33 Cd1 O40 85.60(19) . . ? N17 Cd1 O40 91.3(2) . . ? O37 Cd1 O40 176.60(19) . . ? N1 Cd1 O40 89.8(2) . . ? O77 Cd2 N45 99.1(2) . . ? O77 Cd2 N61 91.2(2) . . ? N45 Cd2 N61 166.3(2) . . ? O77 Cd2 O81 82.1(2) . . ? N45 Cd2 O81 87.2(2) . . ? N61 Cd2 O81 85.4(2) . . ? O77 Cd2 O44 96.6(2) . . ? N45 Cd2 O44 99.05(19) . . ? N61 Cd2 O44 88.53(19) . . ? O81 Cd2 O44 173.79(18) . . ? O77 Cd2 O80 176.62(18) . . ? N45 Cd2 O80 83.65(19) . . ? N61 Cd2 O80 85.71(19) . . ? O81 Cd2 O80 96.15(19) . . ? O44 Cd2 O80 84.85(18) . . ? O36 S1 O35 111.3(3) . . ? O36 S1 O33 109.9(3) . . ? O35 S1 O33 107.9(3) . . ? O36 S1 O34 109.6(3) . . ? O35 S1 O34 108.2(3) . . ? O33 S1 O34 109.9(3) . . ? O37 S2 C39 104.8(4) . . ? O37 S2 C38 104.3(4) . . ? C39 S2 C38 99.4(4) . . ? O42 S3 O43 110.9(3) . . ? O42 S3 O44 109.9(3) . . ? O43 S3 O44 109.9(3) . . ? O42 S3 O41 109.2(3) . . ? O43 S3 O41 110.4(3) . . ? O44 S3 O41 106.5(3) . . ? O77 S4 C78 107.8(5) . . ? O77 S4 C79 106.2(4) . . ? C78 S4 C79 100.0(6) . . ? C2 N1 C6 119.6(6) . . ? C2 N1 Cd1 118.1(5) . . ? C6 N1 Cd1 122.1(5) . . ? N1 C2 C3 120.9(7) . . ? N1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 119.4(7) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.3(7) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 118.3(7) . . ? C4 C5 N7 118.2(6) . . ? C6 C5 N7 123.5(6) . . ? N1 C6 C5 121.5(7) . . ? N1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C8 N7 C5 128.4(6) . . ? C8 N7 H7 115.8 . . ? C5 N7 H7 115.8 . . ? O9 C8 N7 124.2(7) . . ? O9 C8 N10 123.9(7) . . ? N7 C8 N10 111.9(6) . . ? C8 N10 C11 121.1(6) . . ? C8 N10 H10 119.4 . . ? C11 N10 H10 119.4 . . ? C12 C11 N10 121.5(9) . . ? C12 C11 C16 116.3(9) . . ? N10 C11 C16 122.0(8) . . ? C13 C12 F15 118.9(11) . . ? C13 C12 C11 123.7(12) . . ? F15 C12 C11 117.4(9) . . ? C12 C13 F14 121.3(14) . . ? C12 C13 C14 119.5(13) . . ? F14 C13 C14 119.0(11) . . ? F12 C14 C15 120.9(15) . . ? F12 C14 C13 120.9(14) . . ? C15 C14 C13 118.2(10) . . ? F11 C15 C16 118.7(12) . . ? F11 C15 C14 118.8(11) . . ? C16 C15 C14 122.5(11) . . ? F13 C16 C15 122.3(10) . . ? F13 C16 C11 118.0(8) . . ? C15 C16 C11 119.7(10) . . ? C18 N17 C22 118.9(6) . . ? C18 N17 Cd1 122.9(5) . . ? C22 N17 Cd1 118.2(5) . . ? N17 C18 C19 122.1(7) . . ? N17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C20 C19 C18 118.2(7) . . ? C20 C19 N23 117.7(6) . . ? C18 C19 N23 124.0(6) . . ? C21 C20 C19 120.5(7) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 118.4(7) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? N17 C22 C21 121.9(7) . . ? N17 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C24 N23 C19 129.0(6) . . ? C24 N23 H23 115.5 . . ? C19 N23 H23 115.5 . . ? O25 C24 N23 124.4(7) . . ? O25 C24 N26 122.3(7) . . ? N23 C24 N26 113.3(6) . . ? C24 N26 C27 123.4(6) . . ? C24 N26 H26 118.3 . . ? C27 N26 H26 118.3 . . ? N26 C27 C28 123.5(7) . . ? N26 C27 C32 121.5(7) . . ? C28 C27 C32 114.9(7) . . ? C29 C28 F18 117.8(8) . . ? C29 C28 C27 124.2(8) . . ? F18 C28 C27 117.9(7) . . ? F17 C29 C28 122.1(8) . . ? F17 C29 C30 119.5(7) . . ? C28 C29 C30 118.3(8) . . ? F16 C30 C31 122.6(8) . . ? F16 C30 C29 118.8(8) . . ? C31 C30 C29 118.6(7) . . ? C32 C31 F20 121.3(9) . . ? C32 C31 C30 121.1(8) . . ? F20 C31 C30 117.5(8) . . ? C31 C32 F19 119.8(8) . . ? C31 C32 C27 122.8(8) . . ? F19 C32 C27 117.4(7) . . ? S1 O33 Cd1 121.6(3) . . ? S2 O37 Cd1 120.4(3) . . ? S2 C38 H38A 109.5 . . ? S2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? S2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? S2 C39 H39A 109.5 . . ? S2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? S2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? S3 O41 Cd1 123.3(3) . . ? S3 O44 Cd2 120.3(3) . . ? C46 N45 C50 119.7(6) . . ? C46 N45 Cd2 119.8(5) . . ? C50 N45 Cd2 120.4(5) . . ? N45 C46 C47 121.2(7) . . ? N45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C48 C47 C46 119.6(7) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C49 119.5(7) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C50 C49 C48 117.8(7) . . ? C50 C49 N51 124.9(7) . . ? C48 C49 N51 117.3(6) . . ? N45 C50 C49 122.0(7) . . ? N45 C50 H50 119.0 . . ? C49 C50 H50 119.0 . . ? C52 N51 C49 126.9(6) . . ? C52 N51 H51 116.6 . . ? C49 N51 H51 116.6 . . ? O53 C52 N51 126.2(7) . . ? O53 C52 N54 121.6(7) . . ? N51 C52 N54 112.2(6) . . ? C52 N54 C55 122.8(6) . . ? C52 N54 H54 118.6 . . ? C55 N54 H54 118.6 . . ? C56 C55 N54 121.5(7) . . ? C56 C55 C60 116.0(7) . . ? N54 C55 C60 122.4(7) . . ? C57 C56 F9 118.0(8) . . ? C57 C56 C55 123.9(8) . . ? F9 C56 C55 118.1(7) . . ? F8 C57 C56 121.1(9) . . ? F8 C57 C58 119.3(9) . . ? C56 C57 C58 119.6(8) . . ? F6 C58 C59 122.5(8) . . ? F6 C58 C57 119.9(9) . . ? C59 C58 C57 117.7(8) . . ? C60 C59 C58 123.4(8) . . ? C60 C59 F7 119.5(9) . . ? C58 C59 F7 117.2(8) . . ? F10 C60 C59 120.7(8) . . ? F10 C60 C55 119.8(7) . . ? C59 C60 C55 119.5(8) . . ? C62 N61 C66 120.1(7) . . ? C62 N61 Cd2 119.3(5) . . ? C66 N61 Cd2 120.6(5) . . ? N61 C62 C63 121.1(7) . . ? N61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C64 C63 N67 118.1(6) . . ? C64 C63 C62 118.9(7) . . ? N67 C63 C62 123.0(7) . . ? C63 C64 C65 119.5(7) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? C66 C65 C64 118.3(7) . . ? C66 C65 H65 120.8 . . ? C64 C65 H65 120.8 . . ? N61 C66 C65 122.0(8) . . ? N61 C66 H66 119.0 . . ? C65 C66 H66 119.0 . . ? C68 N67 C63 129.1(6) . . ? C68 N67 H67 115.4 . . ? C63 N67 H67 115.4 . . ? O69 C68 N67 125.4(7) . . ? O69 C68 N70 121.7(8) . . ? N67 C68 N70 112.9(7) . . ? C68 N70 C71 121.5(7) . . ? C68 N70 H70 119.3 . . ? C71 N70 H70 119.3 . . ? C72 C71 N70 123.0(8) . . ? C72 C71 C76 116.3(8) . . ? N70 C71 C76 120.6(8) . . ? F5 C72 C73 117.3(9) . . ? F5 C72 C71 120.2(8) . . ? C73 C72 C71 122.5(9) . . ? F4 C73 C72 121.0(10) . . ? F4 C73 C74 118.8(9) . . ? C72 C73 C74 120.0(9) . . ? F3 C74 C75 122.5(10) . . ? F3 C74 C73 120.0(10) . . ? C75 C74 C73 117.5(9) . . ? C76 C75 F2 120.8(11) . . ? C76 C75 C74 122.0(10) . . ? F2 C75 C74 117.2(9) . . ? C75 C76 F1 119.8(9) . . ? C75 C76 C71 121.7(10) . . ? F1 C76 C71 118.5(8) . . ? S4 O77 Cd2 124.4(3) . . ? S4 C78 H78A 109.5 . . ? S4 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? S4 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? S4 C79 H79A 109.5 . . ? S4 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? S4 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N70 H70 O44 0.86 2.16 2.966(8) 155.8 2_666 N67 H67 O44 0.86 2.50 3.218(8) 141.8 2_666 N67 H67 O41 0.86 2.18 2.982(7) 155.3 2_666 N54 H54 O42 0.86 1.96 2.811(8) 169.1 2_665 N51 H51 O43 0.86 2.03 2.825(7) 153.4 2_665 N26 H26 O36 0.86 1.95 2.787(8) 165.6 2_766 N23 H23 O34 0.86 1.95 2.800(7) 170.7 2_766 N10 H10 O35 0.86 2.04 2.846(8) 156.0 2_765 N7 H7 O33 0.86 2.51 3.243(8) 143.5 2_765 N7 H7 O35 0.86 2.22 3.011(7) 152.1 2_765 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 4.314 _refine_diff_density_min -1.286 _refine_diff_density_rms 0.145 # _vrf_PLAT601_bcam26_0m ; PROBLEM: Structure contains Solvent Accessible VOID(S)0f 411 A**3 RESPONSE: We have used SQUEEZE to remove the contributions of disordered solvent molecules (which we could not modelled) within the crystal lattice. Therefore, the contribution of disordered solvent molecules removed by the SQUEEZE process, as a consequence this alert appears. ; _vrf_DIFMX01_bcam26_0m ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given= 4.314 Test value = 3.6 RESPONSE: we have the excess electron density was positioned near the heavy atom Cd.The distance between heavy atom and maxima was 1.18Angstrom. which clearly indicate poor data and/or poor absorption correction and/or Fourier truncation errors and/or Fourier truncation ripples. ; _vrf_DIFMX02_bcam26_0m ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified RESPONSE: we have the excess electron density was positioned near the heavy atom Cd.The distance between heavy atom and maxima was 1.18Angstrom. which clearly indicate poor data and/or poor absorption correction and/or Fourier truncation errors and/or Fourier truncation ripples. ; # end Validation Reply Form # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 0.798 0.857 7.0 -0.3 2 0.283 0.833 0.457 8.4 0.7 3 0.344 0.757 0.570 8.8 0.5 4 0.385 0.794 0.110 12.0 1.5 5 0.614 0.206 0.890 12.0 1.9 6 0.658 0.241 0.434 8.8 0.3 7 0.719 0.164 0.547 8.4 0.2 8 0.750 0.202 0.143 7.0 -0.4 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 926125' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # Attachment 'CC3.cif' data_5110hm #TrackingRef 'CC3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 Cl2 Cu F10 N4 O3' _chemical_formula_weight 756.87 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' Cl Cl 0.1484 0.1585 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.976(14) _cell_length_b 7.960(3) _cell_length_c 8.547(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.420(5) _cell_angle_gamma 90.00 _cell_volume 2905.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4983 _exptl_absorpt_correction_T_max 0.9597 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD Area Detector' _diffrn_measurement_method 'phi-omega scan' _diffrn_detector_area_resol_mean 3 _diffrn_reflns_number 5471 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 22.50 _reflns_number_total 1909 _reflns_number_gt 1740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart Apex' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.3, ORTEP3V2' _computing_publication_material SHELXTL-97 _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^)+(0.1086P)^2^+54.4972P] 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 1909 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1244 _refine_ls_R_factor_gt 0.1141 _refine_ls_wR_factor_ref 0.2736 _refine_ls_wR_factor_gt 0.2674 _refine_ls_goodness_of_fit_ref 1.309 _refine_ls_restrained_S_all 1.309 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.3010(2) 0.2500 0.0235(7) Uani 1 2 d S . . Cl1 Cl 0.02774(7) 0.2323(4) 0.0438(3) 0.0369(9) Uani 1 1 d . . . F1 F 0.1666(2) 0.2642(11) 0.8753(13) 0.078(3) Uani 1 1 d . . . F2 F 0.2197(3) 0.2669(16) 1.0731(16) 0.118(4) Uani 1 1 d . . . F3 F 0.2458(2) -0.0250(19) 1.1781(13) 0.123(5) Uani 1 1 d . . . F4 F 0.2195(3) -0.3180(16) 1.0843(16) 0.120(4) Uani 1 1 d . . . F5 F 0.1658(2) -0.3225(12) 0.8898(13) 0.086(3) Uani 1 1 d . . . N1 N 0.0412(2) 0.3044(12) 0.3942(11) 0.035(2) Uani 1 1 d . . . C2 C 0.0637(3) 0.4092(15) 0.3587(16) 0.043(3) Uani 1 1 d . . . H2 H 0.0600 0.4801 0.2721 0.052 Uiso 1 1 calc R . . C3 C 0.0924(3) 0.4136(15) 0.4479(16) 0.043(3) Uani 1 1 d . . . H3 H 0.1076 0.4888 0.4230 0.052 Uiso 1 1 calc R . . C4 C 0.0987(3) 0.3042(16) 0.5776(15) 0.043(3) Uani 1 1 d . . . H4 H 0.1178 0.3070 0.6402 0.052 Uiso 1 1 calc R . . C5 C 0.0759(3) 0.1945(13) 0.6082(12) 0.028(3) Uani 1 1 d . . . C6 C 0.0480(3) 0.2009(13) 0.5172(13) 0.030(3) Uani 1 1 d . . . H6 H 0.0324 0.1278 0.5419 0.036 Uiso 1 1 calc R . . C7 C 0.0797(2) 0.0706(16) 0.7433(13) 0.035(3) Uani 1 1 d . . . H7A H 0.0654 0.1012 0.8185 0.042 Uiso 1 1 calc R . . H7B H 0.0738 -0.0401 0.7030 0.042 Uiso 1 1 calc R . . N8 N 0.1109(2) 0.0618(12) 0.8246(11) 0.037(2) Uani 1 1 d . . . H8 H 0.1152 0.1195 0.9093 0.044 Uiso 1 1 calc R . . C9 C 0.1335(3) -0.0328(18) 0.7737(15) 0.040(3) Uani 1 1 d . . . O10 O 0.1302(2) -0.1157(13) 0.6535(11) 0.057(3) Uani 1 1 d . . . C11 C 0.1641(3) -0.0257(18) 0.8767(14) 0.043(3) Uani 1 1 d . . . C12 C 0.1795(3) 0.119(2) 0.9257(17) 0.055(4) Uani 1 1 d . . . C13 C 0.2068(3) 0.123(3) 1.027(2) 0.070(5) Uani 1 1 d . . . C14 C 0.2197(4) -0.021(3) 1.081(2) 0.078(5) Uani 1 1 d . . . C15 C 0.2069(4) -0.170(3) 1.033(2) 0.072(5) Uani 1 1 d . . . C16 C 0.1782(3) -0.173(2) 0.9287(18) 0.058(4) Uani 1 1 d . . . O17 O 0.0000 0.5738(14) 0.2500 0.056(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0307(11) 0.0166(11) 0.0215(11) 0.000 -0.0050(8) 0.000 Cl1 0.0446(18) 0.0329(17) 0.0319(17) 0.0010(13) -0.0016(13) 0.0069(13) F1 0.063(6) 0.055(6) 0.111(8) 0.003(5) -0.009(5) -0.011(5) F2 0.073(7) 0.128(10) 0.143(11) -0.034(8) -0.028(7) -0.035(7) F3 0.053(6) 0.210(14) 0.094(8) -0.008(9) -0.042(6) 0.027(7) F4 0.083(7) 0.129(10) 0.139(11) 0.046(8) -0.021(7) 0.053(7) F5 0.068(6) 0.060(6) 0.124(9) 0.015(6) -0.011(6) 0.013(5) N1 0.039(6) 0.025(5) 0.038(6) 0.006(5) -0.011(5) -0.003(5) C2 0.056(9) 0.023(7) 0.049(8) 0.019(6) -0.003(7) 0.002(6) C3 0.029(7) 0.035(7) 0.064(9) 0.010(7) -0.006(6) -0.009(6) C4 0.043(7) 0.038(8) 0.045(8) 0.013(6) -0.013(6) 0.000(6) C5 0.037(7) 0.022(6) 0.023(6) -0.001(5) 0.000(5) 0.002(5) C6 0.035(6) 0.022(6) 0.032(7) 0.009(5) 0.000(5) -0.007(5) C7 0.024(6) 0.053(8) 0.027(7) 0.009(6) -0.004(5) 0.003(6) N8 0.038(6) 0.041(6) 0.030(6) 0.003(5) -0.009(5) 0.002(5) C9 0.033(7) 0.059(9) 0.028(7) 0.015(7) 0.003(6) 0.002(6) O10 0.063(6) 0.077(7) 0.029(5) -0.009(5) -0.010(4) 0.011(5) C11 0.037(7) 0.061(9) 0.030(7) 0.010(7) 0.006(6) 0.016(7) C12 0.039(8) 0.067(11) 0.057(10) 0.005(8) -0.003(7) 0.002(8) C13 0.038(9) 0.091(13) 0.077(12) 0.002(10) -0.009(8) -0.005(9) C14 0.053(10) 0.114(17) 0.061(11) -0.013(11) -0.014(9) 0.019(11) C15 0.049(10) 0.108(15) 0.060(11) 0.008(11) 0.006(8) 0.033(10) C16 0.046(9) 0.068(11) 0.058(10) 0.008(8) 0.007(7) 0.001(8) O17 0.081(10) 0.024(7) 0.053(8) 0.000 -0.032(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.041(9) 2 ? Cu1 N1 2.041(9) . ? Cu1 O17 2.172(12) . ? Cu1 Cl1 2.301(3) . ? Cu1 Cl1 2.301(3) 2 ? F1 C12 1.335(17) . ? F2 C13 1.31(2) . ? F3 C14 1.317(18) . ? F4 C15 1.35(2) . ? F5 C16 1.330(17) . ? N1 C2 1.339(15) . ? N1 C6 1.342(14) . ? C2 C3 1.373(17) . ? C2 H2 0.9300 . ? C3 C4 1.412(17) . ? C3 H3 0.9300 . ? C4 C5 1.359(17) . ? C4 H4 0.9300 . ? C5 C6 1.354(15) . ? C5 C7 1.514(15) . ? C6 H6 0.9300 . ? C7 N8 1.441(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N8 C9 1.340(16) . ? N8 H8 0.8600 . ? C9 O10 1.216(15) . ? C9 C11 1.501(17) . ? C11 C12 1.37(2) . ? C11 C16 1.370(19) . ? C12 C13 1.38(2) . ? C13 C14 1.34(3) . ? C14 C15 1.35(3) . ? C15 C16 1.44(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 178.5(5) 2 . ? N1 Cu1 O17 89.2(3) 2 . ? N1 Cu1 O17 89.2(3) . . ? N1 Cu1 Cl1 91.7(3) 2 . ? N1 Cu1 Cl1 88.7(3) . . ? O17 Cu1 Cl1 103.75(9) . . ? N1 Cu1 Cl1 88.7(3) 2 2 ? N1 Cu1 Cl1 91.7(3) . 2 ? O17 Cu1 Cl1 103.75(9) . 2 ? Cl1 Cu1 Cl1 152.50(17) . 2 ? C2 N1 C6 117.4(10) . . ? C2 N1 Cu1 118.2(8) . . ? C6 N1 Cu1 124.2(8) . . ? N1 C2 C3 121.1(11) . . ? N1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C2 C3 C4 120.1(11) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 117.9(11) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C6 C5 C4 118.5(10) . . ? C6 C5 C7 118.4(10) . . ? C4 C5 C7 123.0(10) . . ? N1 C6 C5 125.0(10) . . ? N1 C6 H6 117.5 . . ? C5 C6 H6 117.5 . . ? N8 C7 C5 114.6(9) . . ? N8 C7 H7A 108.6 . . ? C5 C7 H7A 108.6 . . ? N8 C7 H7B 108.6 . . ? C5 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 N8 C7 122.7(11) . . ? C9 N8 H8 118.6 . . ? C7 N8 H8 118.6 . . ? O10 C9 N8 124.1(11) . . ? O10 C9 C11 121.8(12) . . ? N8 C9 C11 114.1(12) . . ? C12 C11 C16 116.1(12) . . ? C12 C11 C9 125.0(12) . . ? C16 C11 C9 118.9(13) . . ? F1 C12 C11 117.5(12) . . ? F1 C12 C13 118.1(15) . . ? C11 C12 C13 124.3(15) . . ? F2 C13 C14 119.8(15) . . ? F2 C13 C12 121.0(17) . . ? C14 C13 C12 119.1(17) . . ? F3 C14 C13 122.2(19) . . ? F3 C14 C15 117.4(18) . . ? C13 C14 C15 120.3(15) . . ? F4 C15 C14 122.0(16) . . ? F4 C15 C16 118.0(18) . . ? C14 C15 C16 119.9(16) . . ? F5 C16 C11 122.4(13) . . ? F5 C16 C15 117.6(14) . . ? C11 C16 C15 120.0(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 O10 0.86 2.11 2.873(13) 146.7 6_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.586 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.163 # _vrf_THETM01_5110hm ; PROBLEM: The value of sine(theta_max)/wavelength is less that 0.550 Calculated sin(theta_max)/wavelength = 0.5384 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _database_code_depnum_ccdc_archive 'CCDC 926126' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form # Attachment 'CC4 corr.cif' data_sb07d_0m #TrackingRef 'CC4 corr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H22 Cl2 Cu F20 N8 O13' _chemical_formula_weight 1433.18 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' Cl Cl 0.1484 0.1585 '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 tetragonal _symmetry_space_group_name_H-M P4/ncc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 16.0850(7) _cell_length_b 16.0850(7) _cell_length_c 20.6375(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5339.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2852 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8487 _exptl_absorpt_correction_T_max 0.9496 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33626 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 21.57 _reflns_number_total 1556 _reflns_number_gt 1281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 2.4' _computing_publication_material Shelxl-97 _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^)+(0.1627P)^2^+14.5993P] 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 1556 _refine_ls_number_parameters 210 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2269 _refine_ls_wR_factor_gt 0.2069 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.2500 1.2500 0.07496(7) 0.0407(6) Uani 1 4 d S . . Cl1 Cl 0.2500 1.2500 -0.09769(18) 0.0727(12) Uani 1 4 d SD . . Cl2 Cl 0.2500 0.7500 0.2500 0.0600(10) Uani 1 4 d SD . . F1 F 0.3652(3) 0.7166(3) 0.0359(3) 0.0961(16) Uani 1 1 d . . . F2 F 0.3845(4) 0.5575(3) 0.0759(3) 0.1046(19) Uani 1 1 d . . . F3 F 0.4853(4) 0.5234(3) 0.1775(2) 0.1024(19) Uani 1 1 d . . . F4 F 0.5642(4) 0.6477(3) 0.2405(2) 0.0951(17) Uani 1 1 d . . . F5 F 0.5439(3) 0.8050(3) 0.2011(2) 0.0839(14) Uani 1 1 d . . . N1 N 0.2874(3) 1.1302(3) 0.0823(2) 0.0411(13) Uani 1 1 d . . . C2 C 0.3474(4) 1.0985(4) 0.0446(3) 0.0456(16) Uani 1 1 d . . . H2 H 0.3686 1.1313 0.0114 0.055 Uiso 1 1 calc R . . C3 C 0.3789(4) 1.0204(4) 0.0528(3) 0.0480(16) Uani 1 1 d . . . H3 H 0.4208 1.0011 0.0256 0.058 Uiso 1 1 calc R . . C4 C 0.3482(4) 0.9703(4) 0.1012(3) 0.0428(16) Uani 1 1 d . . . C5 C 0.2850(4) 1.0033(4) 0.1398(3) 0.0528(18) Uani 1 1 d . . . H5 H 0.2619 0.9718 0.1731 0.063 Uiso 1 1 calc R . . C6 C 0.2575(4) 1.0815(4) 0.1284(3) 0.0512(18) Uani 1 1 d . . . H6 H 0.2151 1.1023 0.1545 0.061 Uiso 1 1 calc R . . N7 N 0.3753(3) 0.8901(3) 0.1142(3) 0.0529(15) Uani 1 1 d . . . H7 H 0.3431 0.8601 0.1378 0.063 Uiso 1 1 calc R . . C8 C 0.4472(4) 0.8533(5) 0.0938(3) 0.0534(18) Uani 1 1 d . . . O9 O 0.5002(3) 0.8872(3) 0.0623(3) 0.0803(18) Uani 1 1 d . . . C10 C 0.4552(4) 0.7648(4) 0.1161(3) 0.0489(17) Uani 1 1 d . . . C11 C 0.4147(5) 0.7007(5) 0.0870(4) 0.061(2) Uani 1 1 d . . . C12 C 0.4250(5) 0.6189(5) 0.1061(4) 0.070(2) Uani 1 1 d . . . C13 C 0.4754(6) 0.6023(4) 0.1578(4) 0.067(2) Uani 1 1 d . . . C14 C 0.5159(5) 0.6646(5) 0.1886(3) 0.065(2) Uani 1 1 d . . . C15 C 0.5061(5) 0.7447(4) 0.1685(3) 0.0539(19) Uani 1 1 d . . . O16 O 0.2500 1.2500 -0.0304(4) 0.137(5) Uiso 1 4 d SD . . O17 O 0.276(3) 1.301(2) -0.1485(12) 0.137(5) Uiso 0.25 1 d PD . . O18 O 0.206(3) 1.3201(19) -0.1198(16) 0.137(5) Uiso 0.25 1 d PD . . O19 O 0.1654(10) 1.272(3) -0.0970(18) 0.137(5) Uiso 0.25 1 d PD . . O20A O 0.2500 0.7500 0.1820(4) 0.145(5) Uiso 0.56 2 d SPD . . O20B O 0.253(3) 0.6792(18) 0.2106(19) 0.145(5) Uiso 0.22 1 d PD . . O21A O 0.1888(4) 0.6888(4) 0.2500 0.145(5) Uiso 0.56 2 d SPD . . O21B O 0.1881(4) 0.8119(4) 0.2500 0.145(5) Uiso 0.44 2 d SPD . . O22 O 0.2500 1.2500 -0.2778(6) 0.086(3) Uiso 1 4 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0366(7) 0.0366(7) 0.0488(11) 0.000 0.000 0.000 Cl1 0.0891(19) 0.0891(19) 0.040(2) 0.000 0.000 0.000 Cl2 0.0577(14) 0.0577(14) 0.065(2) 0.000 0.000 -0.0167(16) F1 0.096(4) 0.089(3) 0.103(4) -0.003(3) -0.038(3) 0.008(3) F2 0.130(5) 0.064(3) 0.121(4) -0.019(3) -0.004(4) -0.027(3) F3 0.183(6) 0.046(3) 0.078(3) 0.010(2) 0.021(3) 0.011(3) F4 0.145(5) 0.076(3) 0.064(3) 0.004(2) -0.021(3) 0.027(3) F5 0.109(4) 0.061(3) 0.082(3) -0.009(2) -0.016(3) 0.002(2) N1 0.040(3) 0.039(3) 0.044(3) 0.002(2) 0.006(2) 0.000(2) C2 0.045(4) 0.046(4) 0.046(4) 0.006(3) 0.008(3) -0.002(3) C3 0.047(4) 0.047(4) 0.050(4) 0.001(3) 0.011(3) 0.006(3) C4 0.039(3) 0.041(4) 0.047(4) 0.001(3) 0.006(3) 0.001(3) C5 0.058(4) 0.047(4) 0.054(4) 0.014(3) 0.021(3) 0.003(3) C6 0.051(4) 0.053(4) 0.050(4) 0.001(4) 0.019(3) 0.005(3) N7 0.052(3) 0.043(3) 0.063(4) 0.009(3) 0.016(3) 0.006(3) C8 0.052(4) 0.058(4) 0.050(4) 0.005(3) 0.007(3) 0.007(4) O9 0.068(3) 0.071(3) 0.102(4) 0.031(3) 0.041(3) 0.023(3) C10 0.052(4) 0.042(4) 0.052(4) 0.003(3) 0.010(3) 0.006(3) C11 0.058(4) 0.060(5) 0.064(4) -0.005(4) 0.000(4) 0.005(4) C12 0.081(6) 0.052(5) 0.076(5) -0.005(4) 0.011(5) -0.011(4) C13 0.106(6) 0.039(4) 0.055(4) 0.007(4) 0.026(5) 0.010(4) C14 0.092(6) 0.058(5) 0.044(4) 0.001(4) 0.004(4) 0.018(4) C15 0.068(5) 0.039(4) 0.055(4) -0.008(3) 0.006(4) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.025(5) 2_575 ? Cu1 N1 2.025(5) . ? Cu1 N1 2.025(5) 3_665 ? Cu1 N1 2.025(5) 4_465 ? Cu1 O16 2.175(9) . ? Cl1 O16 1.388(8) . ? Cl1 O17 1.393(9) 3_665 ? Cl1 O17 1.393(9) 2_575 ? Cl1 O17 1.393(9) . ? Cl1 O17 1.393(9) 4_465 ? Cl1 O18 1.406(9) 3_665 ? Cl1 O18 1.406(9) . ? Cl1 O18 1.406(9) 2_575 ? Cl1 O18 1.406(9) 4_465 ? Cl1 O19 1.408(9) 2_575 ? Cl1 O19 1.408(9) . ? Cl1 O19 1.408(9) 3_665 ? Cl2 O21A 1.392(9) 2_565 ? Cl2 O21A 1.392(9) . ? Cl2 O20B 1.400(9) . ? Cl2 O20B 1.400(9) 2_565 ? Cl2 O20B 1.400(9) 8_665 ? Cl2 O20B 1.400(9) 7_455 ? Cl2 O20A 1.402(9) 1 ? Cl2 O20A 1.402(9) . ? Cl2 O20A 1.403(9) 7_455 ? Cl2 O21B 1.408(9) 2_565 ? Cl2 O21B 1.408(9) . ? F1 C11 1.345(9) . ? F2 C12 1.337(9) . ? F3 C13 1.342(8) . ? F4 C14 1.351(9) . ? F5 C15 1.328(8) . ? N1 C6 1.322(8) . ? N1 C2 1.339(8) . ? C2 C3 1.366(9) . ? C2 H2 0.9300 . ? C3 C4 1.375(9) . ? C3 H3 0.9300 . ? C4 N7 1.388(8) . ? C4 C5 1.397(9) . ? C5 C6 1.354(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N7 C8 1.365(9) . ? N7 H7 0.8600 . ? C8 O9 1.203(8) . ? C8 C10 1.501(10) . ? C10 C11 1.359(10) . ? C10 C15 1.395(10) . ? C11 C12 1.383(11) . ? C12 C13 1.367(12) . ? C13 C14 1.353(11) . ? C14 C15 1.362(10) . ? O17 O18 0.93(5) 4_465 ? O17 O19 1.20(4) 4_465 ? O17 O17 1.30(4) 3_665 ? O17 O17 1.30(4) 4_465 ? O17 O18 1.31(6) . ? O18 O17 0.93(5) 3_665 ? O18 O19 1.11(4) . ? O18 O19 1.19(4) 4_465 ? O19 O18 1.19(4) 3_665 ? O19 O17 1.20(4) 3_665 ? O20A O20A 0.000(17) 1 ? O20A O20B 1.28(4) 2_565 ? O20A O20B 1.28(4) . ? O20B O21B 1.26(4) 2_565 ? O20B O20A 1.28(4) 1 ? O20B O21A 1.32(4) . ? O21A O20B 1.32(4) 7_455 ? O21B O20B 1.26(4) 2_565 ? O21B O20B 1.26(4) 7_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 171.5(3) 2_575 . ? N1 Cu1 N1 89.68(2) 2_575 3_665 ? N1 Cu1 N1 89.68(2) . 3_665 ? N1 Cu1 N1 89.68(2) 2_575 4_465 ? N1 Cu1 N1 89.68(2) . 4_465 ? N1 Cu1 N1 171.5(3) 3_665 4_465 ? N1 Cu1 O16 94.27(14) 2_575 . ? N1 Cu1 O16 94.27(14) . . ? N1 Cu1 O16 94.27(14) 3_665 . ? N1 Cu1 O16 94.27(14) 4_465 . ? O16 Cl1 O17 138.8(14) . 3_665 ? O16 Cl1 O17 138.8(14) . 2_575 ? O17 Cl1 O17 55.6(17) 3_665 2_575 ? O16 Cl1 O17 138.8(14) . . ? O17 Cl1 O17 55.6(17) 3_665 . ? O17 Cl1 O17 82(3) 2_575 . ? O16 Cl1 O17 138.8(14) . 4_465 ? O17 Cl1 O17 82(3) 3_665 4_465 ? O17 Cl1 O17 55.6(17) 2_575 4_465 ? O17 Cl1 O17 55.6(17) . 4_465 ? O16 Cl1 O18 108.9(14) . 3_665 ? O17 Cl1 O18 56(3) 3_665 3_665 ? O17 Cl1 O18 39(2) 2_575 3_665 ? O17 Cl1 O18 107(2) . 3_665 ? O17 Cl1 O18 94(2) 4_465 3_665 ? O16 Cl1 O18 108.9(14) . . ? O17 Cl1 O18 39(2) 3_665 . ? O17 Cl1 O18 94(2) 2_575 . ? O17 Cl1 O18 56(3) . . ? O17 Cl1 O18 107(2) 4_465 . ? O18 Cl1 O18 84.0(9) 3_665 . ? O16 Cl1 O18 108.9(14) . 2_575 ? O17 Cl1 O18 107(2) 3_665 2_575 ? O17 Cl1 O18 56(3) 2_575 2_575 ? O17 Cl1 O18 94(2) . 2_575 ? O17 Cl1 O18 39(2) 4_465 2_575 ? O18 Cl1 O18 84.0(9) 3_665 2_575 ? O18 Cl1 O18 142(3) . 2_575 ? O16 Cl1 O18 108.9(14) . 4_465 ? O17 Cl1 O18 94(2) 3_665 4_465 ? O17 Cl1 O18 107(2) 2_575 4_465 ? O17 Cl1 O18 39(2) . 4_465 ? O17 Cl1 O18 56(3) 4_465 4_465 ? O18 Cl1 O18 142(3) 3_665 4_465 ? O18 Cl1 O18 84.0(9) . 4_465 ? O18 Cl1 O18 84.0(9) 2_575 4_465 ? O16 Cl1 O19 89.4(15) . 2_575 ? O17 Cl1 O19 131(2) 3_665 2_575 ? O17 Cl1 O19 99(3) 2_575 2_575 ? O17 Cl1 O19 82(3) . 2_575 ? O17 Cl1 O19 50.5(18) 4_465 2_575 ? O18 Cl1 O19 130.5(18) 3_665 2_575 ? O18 Cl1 O19 133.9(18) . 2_575 ? O18 Cl1 O19 46.6(19) 2_575 2_575 ? O18 Cl1 O19 49.9(19) 4_465 2_575 ? O16 Cl1 O19 89.4(15) . . ? O17 Cl1 O19 50.5(18) 3_665 . ? O17 Cl1 O19 82(3) 2_575 . ? O17 Cl1 O19 99(3) . . ? O17 Cl1 O19 131(2) 4_465 . ? O18 Cl1 O19 49.9(19) 3_665 . ? O18 Cl1 O19 46.6(19) . . ? O18 Cl1 O19 133.9(18) 2_575 . ? O18 Cl1 O19 130.5(18) 4_465 . ? O19 Cl1 O19 179(3) 2_575 . ? O16 Cl1 O19 89.4(15) . 3_665 ? O17 Cl1 O19 99(3) 3_665 3_665 ? O17 Cl1 O19 50.5(18) 2_575 3_665 ? O17 Cl1 O19 131(2) . 3_665 ? O17 Cl1 O19 82(3) 4_465 3_665 ? O18 Cl1 O19 46.6(19) 3_665 3_665 ? O18 Cl1 O19 130.5(18) . 3_665 ? O18 Cl1 O19 49.9(19) 2_575 3_665 ? O18 Cl1 O19 133.9(18) 4_465 3_665 ? O19 Cl1 O19 89.99(4) 2_575 3_665 ? O19 Cl1 O19 89.99(4) . 3_665 ? O21A Cl2 O21A 180.000(1) 2_565 . ? O21A Cl2 O20B 123.6(18) 2_565 . ? O21A Cl2 O20B 56.4(18) . . ? O21A Cl2 O20B 56.4(18) 2_565 2_565 ? O21A Cl2 O20B 123.6(18) . 2_565 ? O20B Cl2 O20B 109(4) . 2_565 ? O21A Cl2 O20B 56.4(18) 2_565 8_665 ? O21A Cl2 O20B 123.6(18) . 8_665 ? O20B Cl2 O20B 107(4) . 8_665 ? O20B Cl2 O20B 113(4) 2_565 8_665 ? O21A Cl2 O20B 123.6(18) 2_565 7_455 ? O21A Cl2 O20B 56.4(18) . 7_455 ? O20B Cl2 O20B 113(4) . 7_455 ? O20B Cl2 O20B 107(4) 2_565 7_455 ? O20B Cl2 O20B 109(4) 8_665 7_455 ? O21A Cl2 O20A 90.000(1) 2_565 1 ? O21A Cl2 O20A 90.000(1) . 1 ? O20B Cl2 O20A 54.5(19) . 1 ? O20B Cl2 O20A 54.5(19) 2_565 1 ? O20B Cl2 O20A 125.5(19) 8_665 1 ? O20B Cl2 O20A 125.5(19) 7_455 1 ? O21A Cl2 O20A 90.000(1) 2_565 . ? O21A Cl2 O20A 90.000(1) . . ? O20B Cl2 O20A 54.5(19) . . ? O20B Cl2 O20A 54.5(19) 2_565 . ? O20B Cl2 O20A 125.5(19) 8_665 . ? O20B Cl2 O20A 125.5(19) 7_455 . ? O20A Cl2 O20A 0.000(1) 1 . ? O21A Cl2 O20A 90.002(1) 2_565 7_455 ? O21A Cl2 O20A 89.998(1) . 7_455 ? O20B Cl2 O20A 125.5(19) . 7_455 ? O20B Cl2 O20A 125.5(19) 2_565 7_455 ? O20B Cl2 O20A 54.5(19) 8_665 7_455 ? O20B Cl2 O20A 54.5(19) 7_455 7_455 ? O20A Cl2 O20A 179.998(1) 1 7_455 ? O20A Cl2 O20A 179.998(1) . 7_455 ? O21A Cl2 O21B 90.002(1) 2_565 2_565 ? O21A Cl2 O21B 89.998(1) . 2_565 ? O20B Cl2 O21B 53.4(18) . 2_565 ? O20B Cl2 O21B 126.7(18) 2_565 2_565 ? O20B Cl2 O21B 53.4(18) 8_665 2_565 ? O20B Cl2 O21B 126.6(18) 7_455 2_565 ? O20A Cl2 O21B 90.0 1 2_565 ? O20A Cl2 O21B 90.0 . 2_565 ? O20A Cl2 O21B 89.996(1) 7_455 2_565 ? O21A Cl2 O21B 90.000(1) 2_565 . ? O21A Cl2 O21B 90.000(1) . . ? O20B Cl2 O21B 126.6(18) . . ? O20B Cl2 O21B 53.4(18) 2_565 . ? O20B Cl2 O21B 126.6(18) 8_665 . ? O20B Cl2 O21B 53.4(18) 7_455 . ? O20A Cl2 O21B 90.000(1) 1 . ? O20A Cl2 O21B 90.000(1) . . ? O20A Cl2 O21B 90.001(1) 7_455 . ? O21B Cl2 O21B 179.996(2) 2_565 . ? C6 N1 C2 117.1(5) . . ? C6 N1 Cu1 120.5(4) . . ? C2 N1 Cu1 122.2(4) . . ? N1 C2 C3 123.1(6) . . ? N1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C2 C3 C4 119.7(6) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 N7 124.9(6) . . ? C3 C4 C5 117.0(6) . . ? N7 C4 C5 118.1(5) . . ? C6 C5 C4 119.4(6) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? N1 C6 C5 123.8(6) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? C8 N7 C4 127.6(6) . . ? C8 N7 H7 116.2 . . ? C4 N7 H7 116.2 . . ? O9 C8 N7 124.7(7) . . ? O9 C8 C10 122.3(6) . . ? N7 C8 C10 112.9(6) . . ? C11 C10 C15 116.6(6) . . ? C11 C10 C8 122.9(6) . . ? C15 C10 C8 120.5(6) . . ? F1 C11 C10 119.0(7) . . ? F1 C11 C12 118.4(7) . . ? C10 C11 C12 122.5(7) . . ? F2 C12 C13 120.6(7) . . ? F2 C12 C11 120.8(8) . . ? C13 C12 C11 118.7(7) . . ? F3 C13 C14 120.1(8) . . ? F3 C13 C12 119.4(8) . . ? C14 C13 C12 120.5(7) . . ? F4 C14 C13 119.9(7) . . ? F4 C14 C15 119.9(7) . . ? C13 C14 C15 120.1(7) . . ? F5 C15 C14 118.9(7) . . ? F5 C15 C10 119.5(6) . . ? C14 C15 C10 121.6(7) . . ? Cl1 O16 Cu1 180.000(1) . . ? O18 O17 O19 62(3) 4_465 4_465 ? O18 O17 O17 133.6(12) 4_465 3_665 ? O19 O17 O17 95(4) 4_465 3_665 ? O18 O17 O17 70(5) 4_465 4_465 ? O19 O17 O17 117(3) 4_465 4_465 ? O17 O17 O17 90.001(9) 3_665 4_465 ? O18 O17 O18 113(4) 4_465 . ? O19 O17 O18 56(3) 4_465 . ? O17 O17 O18 42(3) 3_665 . ? O17 O17 O18 119(2) 4_465 . ? O18 O17 Cl1 71.4(13) 4_465 . ? O19 O17 Cl1 65.4(11) 4_465 . ? O17 O17 Cl1 62.2(9) 3_665 . ? O17 O17 Cl1 62.2(9) 4_465 . ? O18 O17 Cl1 62.6(14) . . ? O17 O18 O19 71(3) 3_665 . ? O17 O18 O19 121(3) 3_665 4_465 ? O19 O18 O19 120(4) . 4_465 ? O17 O18 O17 68(4) 3_665 . ? O19 O18 O17 122(2) . . ? O19 O18 O17 57(2) 4_465 . ? O17 O18 Cl1 69.9(12) 3_665 . ? O19 O18 Cl1 66.8(11) . . ? O19 O18 Cl1 65.1(11) 4_465 . ? O17 O18 Cl1 61.6(14) . . ? O18 O19 O18 110(4) . 3_665 ? O18 O19 O17 47(3) . 3_665 ? O18 O19 O17 67(4) 3_665 3_665 ? O18 O19 Cl1 66.6(11) . . ? O18 O19 Cl1 64.9(11) 3_665 . ? O17 O19 Cl1 64.1(10) 3_665 . ? O20A O20A O20B 0(10) 1 2_565 ? O20A O20A O20B 0(10) 1 . ? O20B O20A O20B 125(2) 2_565 . ? O20A O20A Cl2 0(10) 1 . ? O20B O20A Cl2 62.7(11) 2_565 . ? O20B O20A Cl2 62.7(10) . . ? O21B O20B O20A 103(2) 2_565 1 ? O21B O20B O20A 103(2) 2_565 . ? O20A O20B O20A 0.0(7) 1 . ? O21B O20B O21A 100(2) 2_565 . ? O20A O20B O21A 99(2) 1 . ? O20A O20B O21A 99(2) . . ? O21B O20B Cl2 63.7(11) 2_565 . ? O20A O20B Cl2 62.9(11) 1 . ? O20A O20B Cl2 62.9(11) . . ? O21A O20B Cl2 61.5(10) . . ? O20B O21A O20B 124(2) . 7_455 ? O20B O21A Cl2 62.1(10) . . ? O20B O21A Cl2 62.1(10) 7_455 . ? O20B O21B O20B 126(2) 2_565 7_455 ? O20B O21B Cl2 63.0(10) 2_565 . ? O20B O21B Cl2 63.0(10) 7_455 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 O20B 0.86 2.24 3.07(3) 162.2 2_565 N7 H7 O20A 0.86 2.49 3.332(7) 165.6 1 N7 H7 O21A 0.86 2.50 3.245(7) 145.7 2_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.287 _refine_diff_density_min -1.269 _refine_diff_density_rms 0.094 # _vrf_REFNR01_sb07d_0m ; PROBLEM: Ratio of reflections to parameters is < 6 for a centrosymmetric structure sine(theta)/lambda 0.4114 Proportion of unique data used 1.0000 Ratio reflections to parameters 4.4291 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_THETM01_sb07d_0m ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4114 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT241_sb07d_0m ; PROBLEM: Check high Ueq as compared to neighbors for O16 RESPONSE: O16 is a part of disordered perchlorate anion. ; _vrf_PLAT242_sb07d_0m ; PROBLEM: Check low Ueq as compared to neighbors for atom X RESPONSE: X is a attached with or a part of disordered perchlorate anion. ; _vrf_PLAT088_sb07d_0m ; PROBLEM: Poor Data / Parameter Ratio .................... 4.43 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT306_sb07d_0m ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O22 RESPONSE: We are unable to locate the H-atoms associated with the solvent water molecule containing O22. ; _database_code_depnum_ccdc_archive 'CCDC 926127' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form # Attachment 'CC5.cif' data_y #TrackingRef 'CC5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H24 B2 Cu F28 N8 O6' _chemical_formula_weight 1425.91 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' B B 0.0013 0.0007 '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' _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 15.859(2) _cell_length_b 20.759(3) _cell_length_c 16.412(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.950(3) _cell_angle_gamma 90.00 _cell_volume 5402.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2828 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8413 _exptl_absorpt_correction_T_max 0.9060 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean 3 _diffrn_reflns_number 26493 _diffrn_reflns_av_R_equivalents 0.0884 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 19.00 _reflns_number_total 4317 _reflns_number_gt 2890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material Shelxl-97 _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^)+(0.1080P)^2^+43.8067P] 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 4317 _refine_ls_number_parameters 836 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.2206 _refine_ls_wR_factor_gt 0.1891 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.25375(9) 0.92120(7) 0.74501(8) 0.0408(6) Uani 1 1 d . . . F1 F 0.0291(5) 0.7910(4) 1.1928(4) 0.066(2) Uani 1 1 d . . . F2 F 0.0291(5) 0.7509(4) 1.3496(4) 0.064(2) Uani 1 1 d . . . F3 F 0.0778(4) 0.8312(3) 1.4701(4) 0.060(2) Uani 1 1 d . . . F4 F 0.1258(5) 0.9531(3) 1.4353(4) 0.062(2) Uani 1 1 d . . . F5 F 0.1231(5) 0.9943(4) 1.2801(4) 0.065(2) Uani 1 1 d . . . F6 F -0.2758(4) 0.9616(4) 0.6086(4) 0.067(2) Uani 1 1 d . . . F7 F -0.4383(5) 0.9241(4) 0.6015(5) 0.075(2) Uani 1 1 d . . . F8 F -0.4812(5) 0.8180(4) 0.5169(5) 0.082(3) Uani 1 1 d . . . F9 F -0.3624(5) 0.7451(4) 0.4442(5) 0.091(3) Uani 1 1 d . . . F10 F -0.1998(5) 0.7837(4) 0.4503(4) 0.070(2) Uani 1 1 d . . . F11 F 0.5526(5) 0.8046(4) 0.3081(5) 0.089(3) Uani 1 1 d . . . F12 F 0.5703(6) 0.7670(5) 0.1522(5) 0.106(3) Uani 1 1 d . . . F13 F 0.4831(6) 0.8293(4) 0.0320(4) 0.094(3) Uani 1 1 d . . . F14 F 0.3800(6) 0.9285(4) 0.0686(5) 0.097(3) Uani 1 1 d . . . F15 F 0.3634(6) 0.9657(4) 0.2248(4) 0.079(2) Uani 1 1 d . . . F16 F 0.7104(5) 0.8553(7) 1.0957(6) 0.173(6) Uani 1 1 d . . . F17 F 0.8718(5) 0.8154(8) 1.1214(7) 0.221(9) Uani 1 1 d . . . F18 F 0.9877(5) 0.8348(4) 1.0062(5) 0.080(2) Uani 1 1 d . . . F19 F 0.9442(5) 0.9015(4) 0.8716(5) 0.090(3) Uani 1 1 d . . . F20 F 0.7845(5) 0.9410(5) 0.8465(5) 0.097(3) Uani 1 1 d . . . F22 F 0.6463(7) 0.2403(5) 0.7735(14) 0.252(11) Uani 1 1 d . . . F23 F 0.7411(7) 0.1878(6) 0.7011(8) 0.154(5) Uani 1 1 d . . . F24 F 0.7632(6) 0.2880(5) 0.7498(5) 0.104(3) Uani 1 1 d . . . F25 F 0.2960(6) 0.3051(5) 0.7066(7) 0.122(4) Uani 1 1 d . . . F26 F 0.1569(6) 0.2882(7) 0.7088(6) 0.147(5) Uani 1 1 d . . . F27 F 0.2302(6) 0.2914(5) 0.8261(5) 0.115(3) Uani 1 1 d . . . F28 F 0.2456(6) 0.2113(5) 0.7386(5) 0.098(3) Uani 1 1 d . . . B1 B 0.7254(12) 0.2336(10) 0.7597(9) 0.060(5) Uani 1 1 d . . . B2 B 0.2328(11) 0.2766(11) 0.7477(11) 0.064(5) Uani 1 1 d . . . N1 N 0.2150(6) 0.9132(5) 0.8610(6) 0.041(3) Uani 1 1 d . . . C2 C 0.2452(7) 0.8666(6) 0.9108(8) 0.043(3) Uani 1 1 d . . . H2 H 0.2843 0.8378 0.8901 0.052 Uiso 1 1 calc R . . C3 C 0.2214(8) 0.8595(6) 0.9900(7) 0.042(3) Uani 1 1 d . . . H3 H 0.2458 0.8276 1.0224 0.051 Uiso 1 1 calc R . . C4 C 0.1608(7) 0.9001(6) 1.0217(7) 0.037(3) Uani 1 1 d . . . C5 C 0.1282(7) 0.9479(6) 0.9717(7) 0.040(3) Uani 1 1 d . . . H5 H 0.0880 0.9767 0.9906 0.048 Uiso 1 1 calc R . . C6 C 0.1573(8) 0.9518(6) 0.8919(7) 0.045(3) Uani 1 1 d . . . H6 H 0.1346 0.9836 0.8582 0.054 Uiso 1 1 calc R . . N7 N 0.1403(6) 0.8920(5) 1.1040(6) 0.042(3) Uani 1 1 d . . . H7 H 0.1739 0.8680 1.1323 0.051 Uiso 1 1 calc R . . C8 C 0.0740(9) 0.9175(7) 1.1445(7) 0.043(3) Uani 1 1 d . . . O9 O 0.0240(6) 0.9546(5) 1.1177(5) 0.066(3) Uani 1 1 d . . . C10 C 0.0741(7) 0.8939(7) 1.2317(7) 0.042(3) Uani 1 1 d . . . C11 C 0.0522(8) 0.8327(7) 1.2531(8) 0.046(3) Uani 1 1 d . . . C12 C 0.0524(8) 0.8118(7) 1.3317(8) 0.045(3) Uani 1 1 d . . . C13 C 0.0763(8) 0.8526(8) 1.3933(8) 0.044(3) Uani 1 1 d . . . C14 C 0.0997(8) 0.9137(8) 1.3749(8) 0.047(3) Uani 1 1 d . . . C15 C 0.0986(8) 0.9337(7) 1.2946(8) 0.049(3) Uani 1 1 d . . . N16 N 0.1335(6) 0.9144(5) 0.7029(6) 0.040(3) Uani 1 1 d . . . C17 C 0.0811(8) 0.8712(6) 0.7341(7) 0.042(3) Uani 1 1 d . . . H17 H 0.1004 0.8476 0.7788 0.051 Uiso 1 1 calc R . . C18 C 0.0026(8) 0.8589(5) 0.7064(7) 0.037(3) Uani 1 1 d . . . H18 H -0.0311 0.8282 0.7312 0.045 Uiso 1 1 calc R . . C19 C -0.0264(7) 0.8940(6) 0.6391(7) 0.032(3) Uani 1 1 d . . . C20 C 0.0250(8) 0.9397(6) 0.6061(7) 0.039(3) Uani 1 1 d . . . H20 H 0.0062 0.9642 0.5619 0.046 Uiso 1 1 calc R . . C21 C 0.1040(8) 0.9491(5) 0.6384(7) 0.040(3) Uani 1 1 d . . . H21 H 0.1385 0.9802 0.6156 0.048 Uiso 1 1 calc R . . N22 N -0.1095(6) 0.8812(4) 0.6095(6) 0.044(3) Uani 1 1 d . . . H22 H -0.1432 0.8633 0.6432 0.053 Uiso 1 1 calc R . . C23 C -0.1425(8) 0.8944(6) 0.5327(8) 0.040(3) Uani 1 1 d . . . O24 O -0.1030(5) 0.9168(4) 0.4775(5) 0.050(2) Uani 1 1 d . . . C25 C -0.2333(8) 0.8756(7) 0.5273(7) 0.039(3) Uani 1 1 d . . . C26 C -0.2948(11) 0.9082(7) 0.5650(8) 0.047(3) Uani 1 1 d . . . C27 C -0.3776(11) 0.8913(8) 0.5623(8) 0.054(4) Uani 1 1 d . . . C28 C -0.4001(9) 0.8368(9) 0.5202(9) 0.056(4) Uani 1 1 d . . . C29 C -0.3419(11) 0.8008(8) 0.4830(8) 0.060(4) Uani 1 1 d . . . C30 C -0.2586(9) 0.8215(8) 0.4852(8) 0.053(4) Uani 1 1 d . . . N31 N 0.2920(6) 0.9115(5) 0.6293(5) 0.040(3) Uani 1 1 d . . . C32 C 0.2633(7) 0.8634(6) 0.5797(7) 0.043(3) Uani 1 1 d . . . H32 H 0.2237 0.8346 0.5996 0.052 Uiso 1 1 calc R . . C33 C 0.2905(7) 0.8560(6) 0.5018(7) 0.037(3) Uani 1 1 d . . . H33 H 0.2683 0.8233 0.4692 0.045 Uiso 1 1 calc R . . C34 C 0.3507(8) 0.8968(6) 0.4711(7) 0.039(3) Uani 1 1 d . . . C35 C 0.3811(7) 0.9450(6) 0.5206(8) 0.044(3) Uani 1 1 d . . . H35 H 0.4214 0.9737 0.5019 0.052 Uiso 1 1 calc R . . C36 C 0.3506(7) 0.9504(6) 0.5993(7) 0.037(3) Uani 1 1 d . . . H36 H 0.3722 0.9828 0.6327 0.045 Uiso 1 1 calc R . . N37 N 0.3788(7) 0.8871(5) 0.3903(6) 0.044(3) Uani 1 1 d . . . H37 H 0.3457 0.8653 0.3586 0.053 Uiso 1 1 calc R . . C38 C 0.4510(9) 0.9081(6) 0.3574(8) 0.045(3) Uani 1 1 d . . . O39 O 0.5057(6) 0.9371(4) 0.3929(5) 0.057(2) Uani 1 1 d . . . C40 C 0.4592(8) 0.8875(7) 0.2693(7) 0.042(3) Uani 1 1 d . . . C41 C 0.4149(9) 0.9169(7) 0.2082(9) 0.054(4) Uani 1 1 d . . . C42 C 0.4237(10) 0.8983(8) 0.1277(9) 0.064(4) Uani 1 1 d . . . C43 C 0.4750(11) 0.8489(9) 0.1080(9) 0.066(4) Uani 1 1 d . . . C44 C 0.5197(10) 0.8174(8) 0.1694(10) 0.068(4) Uani 1 1 d . . . C45 C 0.5097(9) 0.8381(8) 0.2481(9) 0.059(4) Uani 1 1 d . . . N46 N 0.3741(6) 0.9165(5) 0.7865(6) 0.039(2) Uani 1 1 d . . . C47 C 0.4303(9) 0.8742(6) 0.7565(7) 0.041(3) Uani 1 1 d . . . H47 H 0.4134 0.8486 0.7127 0.049 Uiso 1 1 calc R . . C48 C 0.5108(9) 0.8668(6) 0.7867(7) 0.047(3) Uani 1 1 d . . . H48 H 0.5476 0.8376 0.7630 0.056 Uiso 1 1 calc R . . C49 C 0.5368(8) 0.9039(6) 0.8538(7) 0.042(3) Uani 1 1 d . . . C50 C 0.4792(9) 0.9471(6) 0.8838(7) 0.045(3) Uani 1 1 d . . . H50 H 0.4944 0.9732 0.9277 0.054 Uiso 1 1 calc R . . C51 C 0.4002(8) 0.9523(6) 0.8501(7) 0.043(3) Uani 1 1 d . . . H51 H 0.3630 0.9819 0.8722 0.051 Uiso 1 1 calc R . . N52 N 0.6185(6) 0.8940(4) 0.8841(6) 0.045(3) Uani 1 1 d . . . H52 H 0.6521 0.8730 0.8533 0.053 Uiso 1 1 calc R . . C53 C 0.6513(8) 0.9143(6) 0.9580(8) 0.043(3) Uani 1 1 d . . . O54 O 0.6128(5) 0.9431(5) 1.0084(6) 0.063(3) Uani 1 1 d . . . C55 C 0.7433(8) 0.8963(6) 0.9679(8) 0.042(3) Uani 1 1 d . . . C56 C 0.8049(10) 0.9079(6) 0.9160(7) 0.044(3) Uani 1 1 d . . . C57 C 0.8863(9) 0.8887(7) 0.9274(9) 0.053(4) Uani 1 1 d . . . C58 C 0.9096(9) 0.8557(7) 0.9967(9) 0.055(4) Uani 1 1 d . . . C59 C 0.8503(11) 0.8472(9) 1.0538(10) 0.095(6) Uani 1 1 d . . . C60 C 0.7689(11) 0.8672(9) 1.0398(10) 0.087(5) Uani 1 1 d . . . O61A O 0.2526(5) 1.0306(4) 0.7448(5) 0.025(2) Uiso 0.75 1 d P . . O61B O 0.3218(19) 1.0731(15) 0.7355(18) 0.052(9) Uiso 0.25 1 d P . . O62 O 0.1326(5) 0.1117(4) 0.6907(5) 0.060(2) Uani 1 1 d . . . F21A F 0.7621(10) 0.2113(9) 0.8340(10) 0.101(5) Uiso 0.60 1 d P . . F21B F 0.7372(19) 0.1818(17) 0.804(2) 0.132(11) Uiso 0.40 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 Cu1 0.0431(10) 0.0578(11) 0.0214(9) -0.0003(7) -0.0078(7) -0.0010(8) F1 0.092(6) 0.073(5) 0.033(4) -0.002(4) -0.017(4) -0.014(4) F2 0.095(6) 0.056(5) 0.041(4) 0.002(4) -0.006(4) -0.011(4) F3 0.091(6) 0.068(5) 0.022(5) 0.004(4) -0.003(4) 0.001(4) F4 0.091(6) 0.066(5) 0.029(4) -0.006(4) -0.005(4) -0.008(4) F5 0.101(6) 0.061(6) 0.032(4) 0.001(4) 0.003(4) -0.008(5) F6 0.060(5) 0.076(6) 0.066(5) -0.010(5) -0.014(4) 0.003(4) F7 0.051(5) 0.089(6) 0.084(6) 0.008(5) 0.001(5) 0.009(5) F8 0.047(6) 0.088(6) 0.111(7) 0.020(5) -0.019(5) -0.015(4) F9 0.087(6) 0.086(6) 0.101(7) -0.025(6) -0.026(5) -0.030(5) F10 0.062(5) 0.087(6) 0.061(5) -0.020(4) -0.009(4) -0.006(5) F11 0.101(6) 0.117(7) 0.048(5) -0.014(5) -0.008(5) 0.044(6) F12 0.115(7) 0.141(9) 0.062(6) -0.031(6) 0.004(5) 0.035(7) F13 0.153(8) 0.107(7) 0.021(5) -0.011(5) 0.006(5) -0.027(6) F14 0.149(8) 0.103(7) 0.039(5) 0.014(5) -0.036(5) -0.004(6) F15 0.112(7) 0.078(6) 0.048(5) 0.006(4) -0.016(5) 0.024(6) F16 0.045(6) 0.373(19) 0.101(8) 0.136(10) -0.013(6) 0.007(8) F17 0.050(6) 0.45(2) 0.165(11) 0.228(15) -0.019(6) 0.010(9) F18 0.046(5) 0.100(6) 0.092(6) 0.013(5) -0.027(4) 0.000(5) F19 0.057(5) 0.151(8) 0.061(5) 0.019(5) 0.008(5) -0.001(5) F20 0.062(5) 0.148(8) 0.082(6) 0.067(6) 0.005(5) -0.001(5) F22 0.066(8) 0.076(8) 0.62(4) 0.004(13) 0.035(12) 0.002(6) F23 0.120(9) 0.175(11) 0.167(11) -0.101(10) -0.004(8) -0.041(8) F24 0.154(9) 0.085(7) 0.073(6) -0.003(5) 0.000(6) -0.060(7) F25 0.099(7) 0.119(8) 0.150(9) 0.043(7) 0.042(7) -0.007(6) F26 0.076(7) 0.268(15) 0.095(7) 0.015(8) -0.002(6) 0.040(8) F27 0.126(8) 0.161(10) 0.058(6) -0.056(6) -0.005(5) 0.007(7) F28 0.142(8) 0.073(7) 0.079(6) -0.010(5) 0.003(5) -0.012(6) B1 0.066(14) 0.073(15) 0.039(10) 0.015(10) -0.030(9) -0.005(11) B2 0.050(13) 0.091(17) 0.052(13) 0.008(12) 0.005(10) -0.002(11) N1 0.041(7) 0.054(7) 0.028(6) -0.012(6) -0.006(5) 0.008(6) C2 0.046(8) 0.048(9) 0.036(9) 0.004(7) -0.016(7) 0.012(7) C3 0.045(8) 0.061(9) 0.021(9) 0.009(7) -0.007(7) -0.001(7) C4 0.035(8) 0.061(9) 0.015(8) -0.008(7) -0.005(7) 0.004(7) C5 0.048(8) 0.046(8) 0.027(9) 0.005(7) -0.009(7) 0.005(7) C6 0.049(9) 0.062(10) 0.022(9) 0.007(7) -0.013(7) -0.008(8) N7 0.038(7) 0.064(7) 0.024(7) 0.003(5) -0.010(5) 0.011(6) C8 0.048(9) 0.061(10) 0.020(9) -0.003(7) -0.005(8) 0.015(8) O9 0.069(7) 0.092(7) 0.037(5) 0.010(5) -0.002(5) 0.041(6) C10 0.044(8) 0.058(11) 0.024(10) -0.002(9) -0.008(6) 0.001(7) C11 0.058(9) 0.055(11) 0.024(10) -0.006(9) -0.009(7) -0.002(7) C12 0.064(9) 0.039(10) 0.031(10) 0.004(9) -0.013(7) -0.006(7) C13 0.049(9) 0.063(11) 0.021(10) 0.003(10) -0.008(7) 0.003(8) C14 0.050(9) 0.059(12) 0.032(11) -0.007(9) 0.001(7) -0.002(8) C15 0.069(10) 0.052(11) 0.026(10) 0.015(9) -0.001(7) 0.000(8) N16 0.047(7) 0.042(6) 0.032(7) 0.002(5) 0.010(6) -0.007(6) C17 0.038(9) 0.068(10) 0.021(7) -0.005(7) -0.019(7) 0.016(8) C18 0.053(10) 0.039(8) 0.019(7) 0.013(6) -0.009(7) 0.001(7) C19 0.030(8) 0.037(8) 0.028(8) -0.003(7) 0.003(7) -0.006(7) C20 0.045(9) 0.040(8) 0.031(7) -0.002(6) -0.017(7) -0.003(7) C21 0.062(10) 0.039(8) 0.020(7) 0.015(6) -0.007(7) 0.001(7) N22 0.040(7) 0.059(7) 0.034(7) 0.011(5) -0.002(6) -0.003(5) C23 0.048(10) 0.041(8) 0.030(10) -0.002(7) -0.006(8) 0.000(7) O24 0.053(6) 0.072(6) 0.024(5) 0.009(5) -0.009(4) -0.010(5) C25 0.043(11) 0.056(10) 0.018(7) -0.002(7) -0.011(7) -0.005(9) C26 0.056(12) 0.049(10) 0.034(8) -0.002(8) -0.021(8) -0.013(10) C27 0.055(14) 0.064(11) 0.043(9) 0.003(8) -0.013(8) 0.000(10) C28 0.021(11) 0.083(13) 0.063(10) 0.022(10) -0.015(9) -0.003(10) C29 0.048(13) 0.085(13) 0.046(9) 0.005(9) -0.018(9) -0.013(11) C30 0.039(11) 0.088(13) 0.033(8) 0.003(9) -0.011(8) 0.019(10) N31 0.032(6) 0.057(7) 0.029(6) 0.000(6) -0.006(5) -0.011(6) C32 0.052(8) 0.058(9) 0.020(8) -0.001(7) -0.002(7) -0.004(7) C33 0.038(8) 0.043(8) 0.030(9) -0.006(7) -0.013(6) -0.004(7) C34 0.044(8) 0.048(9) 0.024(9) -0.003(7) -0.007(7) -0.002(7) C35 0.046(8) 0.048(9) 0.037(9) 0.010(7) -0.009(7) -0.012(7) C36 0.029(7) 0.065(9) 0.017(8) -0.011(6) -0.005(6) -0.001(7) N37 0.046(7) 0.061(7) 0.026(7) -0.003(5) -0.010(6) -0.012(6) C38 0.046(10) 0.056(9) 0.034(10) 0.002(7) -0.008(8) -0.011(8) O39 0.053(6) 0.083(7) 0.035(5) -0.013(5) 0.000(5) -0.017(5) C40 0.042(8) 0.056(10) 0.028(10) -0.004(8) 0.007(8) 0.001(8) C41 0.066(10) 0.059(11) 0.039(12) -0.002(9) -0.004(9) 0.004(9) C42 0.086(12) 0.066(12) 0.039(13) 0.004(10) -0.013(10) -0.017(10) C43 0.104(13) 0.072(12) 0.022(11) 0.001(10) 0.002(10) -0.011(11) C44 0.083(12) 0.079(12) 0.042(12) -0.018(10) 0.016(10) 0.006(10) C45 0.064(10) 0.080(12) 0.034(11) -0.003(10) -0.009(8) 0.002(10) N46 0.039(6) 0.055(7) 0.023(6) 0.001(5) -0.006(5) 0.003(6) C47 0.049(9) 0.043(9) 0.030(7) -0.004(6) -0.010(7) 0.002(7) C48 0.058(10) 0.063(9) 0.020(7) -0.012(7) 0.002(7) -0.001(8) C49 0.045(10) 0.050(9) 0.031(8) 0.001(7) -0.007(8) 0.004(8) C50 0.056(10) 0.055(9) 0.024(7) -0.007(7) -0.013(8) 0.002(8) C51 0.044(9) 0.065(9) 0.018(7) -0.007(7) -0.008(6) -0.005(7) N52 0.040(7) 0.059(7) 0.033(7) -0.006(6) -0.008(6) 0.010(5) C53 0.047(10) 0.055(9) 0.027(9) 0.000(7) -0.011(8) -0.004(7) O54 0.052(6) 0.098(8) 0.038(6) -0.020(5) -0.013(5) 0.010(5) C55 0.048(11) 0.057(9) 0.021(8) 0.003(7) -0.013(9) -0.005(7) C56 0.058(12) 0.057(9) 0.017(9) 0.008(7) -0.004(9) -0.016(8) C57 0.028(10) 0.090(11) 0.043(11) -0.017(9) 0.011(9) -0.005(8) C58 0.043(12) 0.081(11) 0.040(10) 0.010(8) -0.014(10) -0.014(8) C59 0.044(13) 0.173(18) 0.067(13) 0.061(12) -0.008(11) -0.015(11) C60 0.045(12) 0.161(17) 0.056(12) 0.029(11) 0.018(11) -0.015(11) O62 0.063(6) 0.067(6) 0.049(5) 0.001(5) -0.014(4) 0.005(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 Cu1 N31 2.013(9) . ? Cu1 N1 2.016(9) . ? Cu1 N46 2.019(9) . ? Cu1 N16 2.023(10) . ? Cu1 O61A 2.272(8) . ? F1 C11 1.361(13) . ? F2 C12 1.351(13) . ? F3 C13 1.336(13) . ? F4 C14 1.346(14) . ? F5 C15 1.340(14) . ? F6 C26 1.352(14) . ? F7 C27 1.350(15) . ? F8 C28 1.345(14) . ? F9 C29 1.356(16) . ? F10 C30 1.354(14) . ? F11 C45 1.376(15) . ? F12 C44 1.351(16) . ? F13 C43 1.320(15) . ? F14 C42 1.338(15) . ? F15 C41 1.333(15) . ? F16 C60 1.338(15) . ? F17 C59 1.330(16) . ? F18 C58 1.319(15) . ? F19 C57 1.333(14) . ? F20 C56 1.366(13) . ? F22 B1 1.286(19) . ? F23 B1 1.38(2) . ? F23 F21B 1.69(3) . ? F24 B1 1.29(2) . ? F25 B2 1.352(18) . ? F26 B2 1.374(18) . ? F27 B2 1.324(18) . ? F28 B2 1.38(2) . ? B1 F21B 1.31(3) . ? B1 F21A 1.42(2) . ? N1 C6 1.324(14) . ? N1 C2 1.348(14) . ? C2 C3 1.368(15) . ? C3 C4 1.387(15) . ? C4 C5 1.382(15) . ? C4 N7 1.405(14) . ? C5 C6 1.399(16) . ? N7 C8 1.359(14) . ? C8 O9 1.186(13) . ? C8 C10 1.512(17) . ? C10 C11 1.365(16) . ? C10 C15 1.373(17) . ? C11 C12 1.362(16) . ? C12 C13 1.368(16) . ? C13 C14 1.357(17) . ? C14 C15 1.382(17) . ? N16 C17 1.331(14) . ? N16 C21 1.358(13) . ? C17 C18 1.342(15) . ? C18 C19 1.394(15) . ? C19 C20 1.369(15) . ? C19 N22 1.422(14) . ? C20 C21 1.367(15) . ? N22 C23 1.384(14) . ? C23 O24 1.204(13) . ? C23 C25 1.493(17) . ? C25 C26 1.346(17) . ? C25 C30 1.374(17) . ? C26 C27 1.360(18) . ? C27 C28 1.370(18) . ? C28 C29 1.343(18) . ? C29 C30 1.389(18) . ? N31 C36 1.331(14) . ? N31 C32 1.362(14) . ? C32 C33 1.366(15) . ? C33 C34 1.376(15) . ? C34 C35 1.372(15) . ? C34 N37 1.421(14) . ? C35 C36 1.391(15) . ? N37 C38 1.347(15) . ? C38 O39 1.199(13) . ? C38 C40 1.515(17) . ? C40 C45 1.350(17) . ? C40 C41 1.360(17) . ? C41 C42 1.386(18) . ? C42 C43 1.352(19) . ? C43 C44 1.386(19) . ? C44 C45 1.374(18) . ? N46 C51 1.342(13) . ? N46 C47 1.348(14) . ? C47 C48 1.371(15) . ? C48 C49 1.401(16) . ? C49 C50 1.376(16) . ? C49 N52 1.396(14) . ? C50 C51 1.365(15) . ? N52 C53 1.378(15) . ? C53 O54 1.196(13) . ? C53 C55 1.513(17) . ? C55 C56 1.329(16) . ? C55 C60 1.381(18) . ? C56 C57 1.361(17) . ? C57 C58 1.374(17) . ? C58 C59 1.350(18) . ? C59 C60 1.37(2) . ? O61A O61B 1.42(3) . ? F21A F21B 0.88(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 N31 Cu1 N1 169.5(4) . . ? N31 Cu1 N46 90.9(4) . . ? N1 Cu1 N46 88.8(4) . . ? N31 Cu1 N16 88.2(4) . . ? N1 Cu1 N16 90.9(4) . . ? N46 Cu1 N16 173.2(4) . . ? N31 Cu1 O61A 95.8(4) . . ? N1 Cu1 O61A 94.7(4) . . ? N46 Cu1 O61A 93.2(4) . . ? N16 Cu1 O61A 93.6(4) . . ? B1 F23 F21B 49.1(13) . . ? F22 B1 F24 112.6(17) . . ? F22 B1 F21B 97(2) . . ? F24 B1 F21B 137(2) . . ? F22 B1 F23 112.8(16) . . ? F24 B1 F23 115.2(15) . . ? F21B B1 F23 78.1(19) . . ? F22 B1 F21A 105.7(17) . . ? F24 B1 F21A 102.0(15) . . ? F21B B1 F21A 37.2(15) . . ? F23 B1 F21A 107.3(16) . . ? F27 B2 F25 114.7(16) . . ? F27 B2 F26 111.7(14) . . ? F25 B2 F26 110.0(14) . . ? F27 B2 F28 109.8(14) . . ? F25 B2 F28 105.4(14) . . ? F26 B2 F28 104.5(15) . . ? C6 N1 C2 116.3(10) . . ? C6 N1 Cu1 122.3(9) . . ? C2 N1 Cu1 121.4(9) . . ? N1 C2 C3 123.6(11) . . ? C2 C3 C4 119.6(11) . . ? C5 C4 C3 118.0(11) . . ? C5 C4 N7 124.5(11) . . ? C3 C4 N7 117.5(11) . . ? C4 C5 C6 118.1(11) . . ? N1 C6 C5 124.4(11) . . ? C8 N7 C4 128.1(10) . . ? O9 C8 N7 126.1(11) . . ? O9 C8 C10 123.5(12) . . ? N7 C8 C10 110.4(11) . . ? C11 C10 C15 115.8(11) . . ? C11 C10 C8 123.3(12) . . ? C15 C10 C8 120.9(13) . . ? F1 C11 C12 118.9(13) . . ? F1 C11 C10 118.1(12) . . ? C12 C11 C10 123.0(12) . . ? F2 C12 C11 120.6(13) . . ? F2 C12 C13 119.5(12) . . ? C11 C12 C13 119.9(13) . . ? F3 C13 C14 121.3(12) . . ? F3 C13 C12 119.5(14) . . ? C14 C13 C12 119.2(12) . . ? F4 C14 C13 119.2(12) . . ? F4 C14 C15 121.2(14) . . ? C13 C14 C15 119.6(13) . . ? F5 C15 C10 120.6(12) . . ? F5 C15 C14 116.9(13) . . ? C10 C15 C14 122.4(13) . . ? C17 N16 C21 116.6(10) . . ? C17 N16 Cu1 120.5(8) . . ? C21 N16 Cu1 122.7(9) . . ? N16 C17 C18 125.4(11) . . ? C17 C18 C19 117.5(11) . . ? C20 C19 C18 119.0(11) . . ? C20 C19 N22 123.2(11) . . ? C18 C19 N22 117.8(11) . . ? C21 C20 C19 119.5(11) . . ? N16 C21 C20 121.9(11) . . ? C23 N22 C19 127.6(10) . . ? O24 C23 N22 124.6(11) . . ? O24 C23 C25 124.8(11) . . ? N22 C23 C25 110.7(11) . . ? C26 C25 C30 115.7(12) . . ? C26 C25 C23 123.1(13) . . ? C30 C25 C23 121.1(13) . . ? C25 C26 F6 119.9(14) . . ? C25 C26 C27 124.3(13) . . ? F6 C26 C27 115.8(15) . . ? F7 C27 C26 123.4(15) . . ? F7 C27 C28 118.4(15) . . ? C26 C27 C28 118.1(14) . . ? C29 C28 F8 119.0(16) . . ? C29 C28 C27 121.0(14) . . ? F8 C28 C27 120.0(16) . . ? C28 C29 F9 121.7(15) . . ? C28 C29 C30 118.4(15) . . ? F9 C29 C30 119.8(16) . . ? F10 C30 C25 119.3(13) . . ? F10 C30 C29 118.1(15) . . ? C25 C30 C29 122.4(14) . . ? C36 N31 C32 116.9(9) . . ? C36 N31 Cu1 120.7(8) . . ? C32 N31 Cu1 122.3(8) . . ? N31 C32 C33 122.3(11) . . ? C32 C33 C34 120.3(11) . . ? C35 C34 C33 118.1(11) . . ? C35 C34 N37 122.9(12) . . ? C33 C34 N37 118.9(11) . . ? C34 C35 C36 118.9(11) . . ? N31 C36 C35 123.4(11) . . ? C38 N37 C34 127.6(10) . . ? O39 C38 N37 125.5(11) . . ? O39 C38 C40 122.2(12) . . ? N37 C38 C40 112.2(12) . . ? C45 C40 C41 116.9(12) . . ? C45 C40 C38 121.4(13) . . ? C41 C40 C38 121.7(13) . . ? F15 C41 C40 120.1(13) . . ? F15 C41 C42 118.6(15) . . ? C40 C41 C42 121.3(14) . . ? F14 C42 C43 119.3(15) . . ? F14 C42 C41 120.0(17) . . ? C43 C42 C41 120.7(15) . . ? F13 C43 C42 121.8(16) . . ? F13 C43 C44 119.1(17) . . ? C42 C43 C44 119.1(14) . . ? F12 C44 C45 121.1(16) . . ? F12 C44 C43 120.8(14) . . ? C45 C44 C43 118.1(15) . . ? C40 C45 C44 123.9(14) . . ? C40 C45 F11 119.2(13) . . ? C44 C45 F11 116.9(15) . . ? C51 N46 C47 116.6(10) . . ? C51 N46 Cu1 120.9(9) . . ? C47 N46 Cu1 122.4(8) . . ? N46 C47 C48 123.9(11) . . ? C47 C48 C49 118.8(12) . . ? C50 C49 N52 125.9(11) . . ? C50 C49 C48 116.8(11) . . ? N52 C49 C48 117.3(12) . . ? C51 C50 C49 121.1(11) . . ? N46 C51 C50 122.7(11) . . ? C53 N52 C49 127.0(11) . . ? O54 C53 N52 124.9(12) . . ? O54 C53 C55 123.5(11) . . ? N52 C53 C55 111.6(12) . . ? C56 C55 C60 114.7(12) . . ? C56 C55 C53 127.2(12) . . ? C60 C55 C53 118.0(13) . . ? C55 C56 C57 124.4(12) . . ? C55 C56 F20 117.4(13) . . ? C57 C56 F20 118.2(14) . . ? F19 C57 C56 120.7(14) . . ? F19 C57 C58 119.3(14) . . ? C56 C57 C58 120.0(13) . . ? F18 C58 C59 122.6(14) . . ? F18 C58 C57 120.1(14) . . ? C59 C58 C57 117.3(14) . . ? F17 C59 C58 118.1(16) . . ? F17 C59 C60 121.1(16) . . ? C58 C59 C60 120.6(14) . . ? F16 C60 C59 119.4(16) . . ? F16 C60 C55 118.0(15) . . ? C59 C60 C55 122.5(13) . . ? O61B O61A Cu1 128.0(13) . . ? F21B F21A B1 64(3) . . ? F21A F21B B1 78(3) . . ? F21A F21B F23 119(3) . . ? B1 F21B F23 52.8(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N52 H52 F25 0.86 1.91 2.744(13) 162.4 2_656 N37 H37 F23 0.86 2.01 2.862(13) 171.9 3_666 N22 H22 F27 0.86 2.10 2.887(13) 151.6 2_556 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 19.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.940 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.089 # _vrf_REFNR01_y ; PROBLM: Ratio of reflections to parameters is < 6 for a centrosymmetric structure sine(theta)/lambda 0.4581 Proportion of unique data used 1.0000 Ratio reflections to parameters 5.1516 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_THETM01_y ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4581 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT088_y ; PROBLEM: Poor Data / Parameter Ratio .................... 5.15 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT306_y ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O62 RESPONSE: We are unable to locate the H-atoms associated with the solvent water molecule containing O62. ; _database_code_depnum_ccdc_archive 'CCDC 926128' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form # Attachment 'CC6 corrected.cif' data_sb56_0m #TrackingRef 'CC6 corrected.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H48 Cl4 Cu2 F40 N16 O12' _chemical_formula_weight 2646.32 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' Cl Cl 0.1484 0.1585 '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 tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 22.2079(12) _cell_length_b 22.2079(12) _cell_length_c 11.9119(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5874.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2620 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8278 _exptl_absorpt_correction_T_max 0.9032 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55537 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.80 _reflns_number_total 5650 _reflns_number_gt 4823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material Shelxl-97 _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^)+(0.1501P)^2^+44.7474P] 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 5650 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0982 _refine_ls_wR_factor_ref 0.2771 _refine_ls_wR_factor_gt 0.2629 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.2500 0.2500 0.87212(13) 0.0211(4) Uani 1 4 d S . . Cu2 Cu 0.2500 0.2500 0.41649(12) 0.0201(4) Uani 1 4 d S . . Cl1 Cl 0.2500 0.2500 0.6542(2) 0.0201(6) Uani 1 4 d S . . Cl2 Cl 0.2500 0.2500 0.1978(2) 0.0243(6) Uani 1 4 d S . . Cl3 Cl 0.59752(15) 0.32454(16) 0.5367(3) 0.0348(7) Uani 0.50 1 d P . . F1 F -0.07009(19) -0.00984(18) 1.0716(4) 0.0443(11) Uani 1 1 d . . . F2 F -0.1835(2) -0.0468(2) 1.0300(5) 0.0583(14) Uani 1 1 d . . . F3 F -0.2629(2) 0.0290(2) 0.9297(5) 0.0563(13) Uani 1 1 d . . . F4 F -0.23003(19) 0.1432(2) 0.8808(5) 0.0580(14) Uani 1 1 d . . . F5 F -0.11670(18) 0.17987(18) 0.9194(4) 0.0450(11) Uani 1 1 d . . . F6 F 0.59475(19) 0.34805(19) 0.2638(4) 0.0418(10) Uani 1 1 d . . . F7 F 0.7086(2) 0.3730(3) 0.2145(5) 0.0646(15) Uani 1 1 d . . . F8 F 0.7540(2) 0.4847(3) 0.2588(5) 0.0783(19) Uani 1 1 d . . . F9 F 0.6839(2) 0.5694(2) 0.3538(5) 0.0698(17) Uani 1 1 d . . . F10 F 0.5688(2) 0.5457(2) 0.4027(4) 0.0510(12) Uani 1 1 d . . . N1 N 0.1723(2) 0.2045(2) 0.8906(4) 0.0221(10) Uani 1 1 d . . . C2 C 0.1481(3) 0.1975(3) 0.9921(6) 0.0286(14) Uani 1 1 d . . . H2 H 0.1696 0.2115 1.0537 0.034 Uiso 1 1 calc R . . C3 C 0.0922(3) 0.1703(3) 1.0118(5) 0.0265(13) Uani 1 1 d . . . H3 H 0.0772 0.1667 1.0843 0.032 Uiso 1 1 calc R . . C4 C 0.0597(3) 0.1489(3) 0.9202(5) 0.0243(13) Uani 1 1 d . . . C5 C 0.0865(3) 0.1547(3) 0.8140(6) 0.0288(14) Uani 1 1 d . . . H5 H 0.0668 0.1403 0.7506 0.035 Uiso 1 1 calc R . . C6 C 0.1414(3) 0.1816(3) 0.8041(5) 0.0255(13) Uani 1 1 d . . . H6 H 0.1584 0.1841 0.7329 0.031 Uiso 1 1 calc R . . N7 N 0.0027(2) 0.1247(2) 0.9266(5) 0.0254(11) Uani 1 1 d . . . H7 H -0.0167 0.1213 0.8644 0.030 Uiso 1 1 calc R . . C8 C -0.0260(3) 0.1056(3) 1.0198(5) 0.0270(13) Uani 1 1 d . . . O9 O -0.0045(2) 0.1029(2) 1.1130(4) 0.0356(11) Uani 1 1 d . . . C10 C -0.0898(3) 0.0857(3) 0.9978(6) 0.0303(14) Uani 1 1 d . . . C11 C -0.1085(3) 0.0290(3) 1.0246(6) 0.0326(15) Uani 1 1 d . . . C12 C -0.1665(3) 0.0090(3) 1.0027(7) 0.0392(17) Uani 1 1 d . . . C13 C -0.2077(3) 0.0471(3) 0.9544(7) 0.0393(17) Uani 1 1 d . . . C14 C -0.1903(3) 0.1053(3) 0.9275(7) 0.0386(16) Uani 1 1 d . . . C15 C -0.1323(3) 0.1237(3) 0.9485(6) 0.0334(15) Uani 1 1 d . . . N16 N 0.3281(2) 0.2986(2) 0.4190(4) 0.0211(10) Uani 1 1 d . . . C17 C 0.3730(3) 0.2851(3) 0.4903(5) 0.0260(13) Uani 1 1 d . . . H17 H 0.3663 0.2558 0.5445 0.031 Uiso 1 1 calc R . . C18 C 0.4289(3) 0.3128(3) 0.4869(5) 0.0274(13) Uani 1 1 d . . . H18 H 0.4587 0.3020 0.5379 0.033 Uiso 1 1 calc R . . C19 C 0.4399(3) 0.3570(3) 0.4060(5) 0.0256(13) Uani 1 1 d . . . C20 C 0.3925(3) 0.3724(3) 0.3338(5) 0.0281(13) Uani 1 1 d . . . H20 H 0.3972 0.4029 0.2810 0.034 Uiso 1 1 calc R . . C21 C 0.3389(3) 0.3414(3) 0.3426(5) 0.0252(13) Uani 1 1 d . . . H21 H 0.3083 0.3509 0.2922 0.030 Uiso 1 1 calc R . . N22 N 0.4968(2) 0.3817(2) 0.3993(5) 0.0301(12) Uani 1 1 d . . . H22 H 0.5258 0.3612 0.4277 0.036 Uiso 1 1 calc R . . C23 C 0.5111(3) 0.4354(3) 0.3522(6) 0.0312(15) Uani 1 1 d . . . O24 O 0.4737(2) 0.4737(2) 0.3249(5) 0.0382(12) Uani 1 1 d . . . C25 C 0.5768(3) 0.4461(3) 0.3352(6) 0.0312(15) Uani 1 1 d . . . C26 C 0.6149(3) 0.4040(3) 0.2884(6) 0.0323(15) Uani 1 1 d . . . C27 C 0.6742(3) 0.4159(4) 0.2627(7) 0.0430(18) Uani 1 1 d . . . C28 C 0.6966(3) 0.4722(5) 0.2842(8) 0.053(2) Uani 1 1 d . . . C29 C 0.6612(4) 0.5155(4) 0.3314(7) 0.047(2) Uani 1 1 d . . . C30 C 0.6016(3) 0.5022(3) 0.3554(7) 0.0400(17) Uani 1 1 d . . . O31 O -0.0482(3) 0.0976(3) 0.7227(5) 0.0520(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0160(5) 0.0160(5) 0.0314(8) 0.000 0.000 0.000 Cu2 0.0148(4) 0.0148(4) 0.0308(8) 0.000 0.000 0.000 Cl1 0.0189(8) 0.0189(8) 0.0224(14) 0.000 0.000 0.000 Cl2 0.0213(9) 0.0213(9) 0.0302(15) 0.000 0.000 0.000 Cl3 0.0299(16) 0.0428(18) 0.0319(17) -0.0014(14) 0.0006(13) 0.0102(13) F1 0.034(2) 0.029(2) 0.070(3) 0.011(2) 0.003(2) 0.0004(17) F2 0.039(2) 0.030(2) 0.106(4) 0.007(2) 0.007(3) -0.0134(19) F3 0.028(2) 0.056(3) 0.086(4) -0.001(3) 0.001(2) -0.014(2) F4 0.028(2) 0.056(3) 0.090(4) 0.016(3) -0.009(2) 0.003(2) F5 0.031(2) 0.030(2) 0.074(3) 0.015(2) -0.004(2) -0.0029(17) F6 0.039(2) 0.036(2) 0.050(3) -0.0082(19) 0.0033(19) -0.0074(18) F7 0.031(2) 0.096(4) 0.066(3) 0.002(3) 0.014(2) 0.011(3) F8 0.026(2) 0.106(5) 0.103(5) 0.041(4) -0.002(3) -0.027(3) F9 0.066(3) 0.052(3) 0.091(4) 0.019(3) -0.036(3) -0.041(3) F10 0.058(3) 0.035(2) 0.060(3) -0.008(2) -0.009(2) -0.016(2) N1 0.020(2) 0.019(2) 0.027(3) -0.001(2) 0.000(2) -0.0019(19) C2 0.026(3) 0.028(3) 0.032(3) -0.002(3) -0.009(3) -0.004(3) C3 0.024(3) 0.029(3) 0.026(3) 0.000(3) 0.001(2) -0.004(2) C4 0.023(3) 0.019(3) 0.031(3) -0.002(2) 0.002(2) -0.001(2) C5 0.033(3) 0.024(3) 0.029(3) -0.002(3) -0.004(3) -0.006(3) C6 0.023(3) 0.026(3) 0.028(3) -0.003(2) 0.001(2) 0.000(2) N7 0.020(2) 0.026(3) 0.030(3) 0.000(2) -0.001(2) -0.001(2) C8 0.025(3) 0.025(3) 0.031(4) 0.001(3) 0.006(3) 0.000(2) O9 0.030(2) 0.041(3) 0.036(3) 0.006(2) -0.001(2) -0.005(2) C10 0.022(3) 0.031(3) 0.038(4) 0.002(3) 0.000(3) -0.001(3) C11 0.028(3) 0.029(3) 0.041(4) 0.004(3) 0.005(3) 0.002(3) C12 0.030(4) 0.027(3) 0.061(5) 0.000(3) 0.009(3) -0.009(3) C13 0.022(3) 0.039(4) 0.058(5) -0.003(3) 0.003(3) -0.009(3) C14 0.023(3) 0.039(4) 0.053(4) 0.004(3) 0.002(3) 0.002(3) C15 0.029(3) 0.025(3) 0.046(4) 0.002(3) 0.006(3) -0.002(3) N16 0.018(2) 0.018(2) 0.027(3) 0.000(2) 0.001(2) 0.0026(19) C17 0.022(3) 0.024(3) 0.032(3) 0.002(3) 0.003(2) 0.000(2) C18 0.023(3) 0.029(3) 0.030(3) 0.001(3) -0.004(3) 0.001(2) C19 0.021(3) 0.023(3) 0.033(3) -0.002(2) 0.004(2) -0.003(2) C20 0.030(3) 0.022(3) 0.032(3) 0.004(3) 0.002(3) -0.003(3) C21 0.022(3) 0.022(3) 0.031(3) 0.002(2) 0.000(2) 0.000(2) N22 0.022(3) 0.030(3) 0.038(3) 0.000(2) 0.004(2) -0.008(2) C23 0.026(3) 0.032(3) 0.035(4) -0.008(3) 0.005(3) -0.008(3) O24 0.033(3) 0.028(2) 0.054(3) -0.001(2) 0.005(2) -0.004(2) C25 0.031(3) 0.033(3) 0.030(3) -0.004(3) 0.000(3) -0.013(3) C26 0.029(3) 0.037(4) 0.031(3) 0.006(3) -0.001(3) -0.004(3) C27 0.027(4) 0.060(5) 0.042(4) 0.009(4) 0.001(3) -0.004(3) C28 0.028(4) 0.080(6) 0.053(5) 0.026(5) 0.000(4) -0.016(4) C29 0.042(4) 0.048(5) 0.052(5) 0.014(4) -0.019(4) -0.030(4) C30 0.038(4) 0.036(4) 0.046(4) -0.002(3) -0.009(3) -0.011(3) O31 0.057(4) 0.048(3) 0.052(3) -0.015(3) -0.016(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.012(5) 2 ? Cu1 N1 2.012(5) 4 ? Cu1 N1 2.012(5) 3 ? Cu1 N1 2.012(5) . ? Cu1 Cl1 2.596(3) . ? Cu2 N16 2.043(5) . ? Cu2 N16 2.043(5) 3 ? Cu2 N16 2.043(5) 4 ? Cu2 N16 2.043(5) 2 ? Cu2 Cl2 2.605(3) . ? Cl3 Cl3 0.000(9) 1 ? F1 C11 1.336(8) . ? F2 C12 1.336(8) . ? F3 C13 1.324(8) . ? F4 C14 1.341(8) . ? F5 C15 1.339(8) . ? F6 C26 1.351(8) . ? F7 C27 1.348(10) . ? F8 C28 1.340(9) . ? F9 C29 1.327(9) . ? F10 C30 1.336(9) . ? N1 C2 1.332(8) . ? N1 C6 1.339(8) . ? C2 C3 1.399(9) . ? C2 H2 0.9300 . ? C3 C4 1.391(9) . ? C3 H3 0.9300 . ? C4 N7 1.378(8) . ? C4 C5 1.404(9) . ? C5 C6 1.362(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N7 C8 1.348(8) . ? N7 H7 0.8600 . ? C8 O9 1.210(8) . ? C8 C10 1.507(9) . ? C10 C11 1.365(9) . ? C10 C15 1.395(10) . ? C11 C12 1.387(10) . ? C12 C13 1.371(11) . ? C13 C14 1.386(10) . ? C14 C15 1.376(10) . ? N16 C21 1.337(8) . ? N16 C17 1.344(8) . ? C17 C18 1.384(9) . ? C17 H17 0.9300 . ? C18 C19 1.398(9) . ? C18 H18 0.9300 . ? C19 N22 1.380(8) . ? C19 C20 1.401(9) . ? C20 C21 1.381(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? N22 C23 1.355(9) . ? N22 H22 0.8600 . ? C23 O24 1.233(9) . ? C23 C25 1.493(9) . ? C25 C26 1.378(10) . ? C25 C30 1.382(9) . ? C26 C27 1.379(10) . ? C27 C28 1.370(13) . ? C28 C29 1.365(13) . ? C29 C30 1.385(11) . ? O31 O31 0.000(18) 1 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 89.32(3) 2 4 ? N1 Cu1 N1 89.32(3) 2 3 ? N1 Cu1 N1 167.5(3) 4 3 ? N1 Cu1 N1 167.5(3) 2 . ? N1 Cu1 N1 89.32(3) 4 . ? N1 Cu1 N1 89.32(3) 3 . ? N1 Cu1 Cl1 96.27(15) 2 . ? N1 Cu1 Cl1 96.27(15) 4 . ? N1 Cu1 Cl1 96.27(15) 3 . ? N1 Cu1 Cl1 96.27(15) . . ? N16 Cu2 N16 89.987(5) . 3 ? N16 Cu2 N16 89.989(5) . 4 ? N16 Cu2 N16 178.3(3) 3 4 ? N16 Cu2 N16 178.3(3) . 2 ? N16 Cu2 N16 89.988(5) 3 2 ? N16 Cu2 N16 89.987(5) 4 2 ? N16 Cu2 Cl2 90.83(14) . . ? N16 Cu2 Cl2 90.83(14) 3 . ? N16 Cu2 Cl2 90.83(14) 4 . ? N16 Cu2 Cl2 90.83(14) 2 . ? C2 N1 C6 116.5(5) . . ? C2 N1 Cu1 120.3(4) . . ? C6 N1 Cu1 123.2(4) . . ? N1 C2 C3 124.1(6) . . ? N1 C2 H2 117.9 . . ? C3 C2 H2 117.9 . . ? C4 C3 C2 118.4(6) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? N7 C4 C3 124.6(6) . . ? N7 C4 C5 118.3(6) . . ? C3 C4 C5 117.1(6) . . ? C6 C5 C4 119.8(6) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? N1 C6 C5 124.0(6) . . ? N1 C6 H6 118.0 . . ? C5 C6 H6 118.0 . . ? C8 N7 C4 127.0(6) . . ? C8 N7 H7 116.5 . . ? C4 N7 H7 116.5 . . ? O9 C8 N7 125.8(6) . . ? O9 C8 C10 121.1(6) . . ? N7 C8 C10 113.1(6) . . ? C11 C10 C15 116.8(6) . . ? C11 C10 C8 121.1(6) . . ? C15 C10 C8 122.2(6) . . ? F1 C11 C10 119.9(6) . . ? F1 C11 C12 117.7(6) . . ? C10 C11 C12 122.3(6) . . ? F2 C12 C13 119.0(6) . . ? F2 C12 C11 120.9(7) . . ? C13 C12 C11 120.1(6) . . ? F3 C13 C12 121.6(6) . . ? F3 C13 C14 119.3(7) . . ? C12 C13 C14 119.1(6) . . ? F4 C14 C15 120.3(6) . . ? F4 C14 C13 119.9(6) . . ? C15 C14 C13 119.8(7) . . ? F5 C15 C14 118.2(6) . . ? F5 C15 C10 119.8(6) . . ? C14 C15 C10 122.0(6) . . ? C21 N16 C17 117.1(5) . . ? C21 N16 Cu2 121.1(4) . . ? C17 N16 Cu2 121.4(4) . . ? N16 C17 C18 123.2(6) . . ? N16 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C17 C18 C19 119.2(6) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? N22 C19 C18 118.7(6) . . ? N22 C19 C20 123.6(6) . . ? C18 C19 C20 117.6(6) . . ? C21 C20 C19 118.7(6) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? N16 C21 C20 124.1(6) . . ? N16 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? C23 N22 C19 126.1(6) . . ? C23 N22 H22 116.9 . . ? C19 N22 H22 116.9 . . ? O24 C23 N22 123.9(6) . . ? O24 C23 C25 120.9(6) . . ? N22 C23 C25 115.2(6) . . ? C26 C25 C30 116.0(6) . . ? C26 C25 C23 123.1(6) . . ? C30 C25 C23 120.6(7) . . ? F6 C26 C25 120.6(6) . . ? F6 C26 C27 116.3(7) . . ? C25 C26 C27 123.0(7) . . ? F7 C27 C28 121.2(7) . . ? F7 C27 C26 120.1(7) . . ? C28 C27 C26 118.7(8) . . ? F8 C28 C29 119.7(8) . . ? F8 C28 C27 119.5(9) . . ? C29 C28 C27 120.7(7) . . ? F9 C29 C28 120.0(8) . . ? F9 C29 C30 121.0(9) . . ? C28 C29 C30 119.0(7) . . ? F10 C30 C25 120.5(7) . . ? F10 C30 C29 117.0(7) . . ? C25 C30 C29 122.5(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 O31 0.86 1.90 2.745(8) 166.5 1 N22 H22 Cl3 0.86 2.21 3.050(7) 165.3 1 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.80 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.118 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.123 # _vrf_PLAT306_sb56_0m ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O31 RESPONSE: We are unable to locate the H-atoms associated with the solvent water molecule containing O31. ; _vrf_PLAT601_sb56_0m ; PROBLEM: Structure contains Solvent Accessible VOID(S)0f 466 A**3 RESPONSE: We have used SQUEEZE to remove the contributions of disordered solvent molecules (which we could not modelled) within the crystal lattice. Therefore, the contribution of disordered solvent molecules removed by the SQUEEZE process, as a consequence this alert appears. ; # end Validation Reply Form # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 0.750 0.000 11.1 1.8 2 0.750 0.250 0.000 11.1 1.8 3 0.072 0.258 0.207 12.3 1.1 4 0.242 0.072 0.207 12.3 0.7 5 0.258 0.428 0.207 12.3 0.9 6 0.428 0.242 0.207 12.3 1.1 7 0.572 0.758 0.793 12.3 0.9 8 0.742 0.572 0.793 12.3 1.0 9 0.758 0.928 0.793 12.3 1.3 10 0.928 0.742 0.793 12.3 0.9 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 926129' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # Attachment 'CC7 DIS.cif' data_yu #TrackingRef 'CC7 DIS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H20 Cl4 Cu2 F20 N8 O5' _chemical_formula_weight 1437.60 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' Cl Cl 0.1484 0.1585 '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)/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 20.7225(11) _cell_length_b 10.7393(6) _cell_length_c 23.8872(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.5360(10) _cell_angle_gamma 90.00 _cell_volume 5208.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'sky blue' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7388 _exptl_absorpt_correction_T_max 0.8742 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40938 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 23.13 _reflns_number_total 7352 _reflns_number_gt 5427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material 'Shelxl 97' _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^)+(0.1000P)^2^+0.4437P] 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 7352 _refine_ls_number_parameters 781 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1258 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 Cu1 Cu 0.44298(3) 0.17989(5) 0.35676(2) 0.03436(19) Uani 1 1 d . . . Cu2 Cu 0.56560(3) 0.41055(5) 0.38550(2) 0.03351(19) Uani 1 1 d . . . Cl1 Cl 0.38839(6) 0.06401(11) 0.28019(5) 0.0438(3) Uani 1 1 d . . . Cl2 Cl 0.49422(6) 0.25838(11) 0.44463(5) 0.0387(3) Uani 1 1 d . . . Cl3 Cl 0.50599(5) 0.33226(11) 0.30057(5) 0.0351(3) Uani 1 1 d . . . Cl4 Cl 0.63077(6) 0.50973(12) 0.46183(5) 0.0438(3) Uani 1 1 d . . . N1 N 0.36752(18) 0.3037(4) 0.34893(15) 0.0352(9) Uani 1 1 d . . . C2 C 0.3482(2) 0.3584(5) 0.3936(2) 0.0475(13) Uani 1 1 d . . . H2 H 0.3714 0.3403 0.4302 0.057 Uiso 1 1 calc R . . C3 C 0.2963(2) 0.4394(5) 0.3880(2) 0.0496(14) Uani 1 1 d . . . H3 H 0.2855 0.4753 0.4203 0.060 Uiso 1 1 calc R . . C4 C 0.2600(2) 0.4678(5) 0.3345(2) 0.0411(12) Uani 1 1 d . . . C5 C 0.2803(2) 0.4136(5) 0.2881(2) 0.0430(13) Uani 1 1 d . . . H5 H 0.2584 0.4311 0.2510 0.052 Uiso 1 1 calc R . . C6 C 0.3330(2) 0.3341(5) 0.2978(2) 0.0418(12) Uani 1 1 d . . . H6 H 0.3455 0.2986 0.2661 0.050 Uiso 1 1 calc R . . N7 N 0.20410(19) 0.5406(4) 0.33141(17) 0.0461(11) Uani 1 1 d . . . H7 H 0.1979 0.5707 0.3633 0.055 Uiso 1 1 calc R . . C8 C 0.1580(2) 0.5704(5) 0.2846(2) 0.0425(12) Uani 1 1 d . . . O9 O 0.16450(18) 0.5577(4) 0.23544(15) 0.0547(10) Uani 1 1 d . . . C10 C 0.0953(2) 0.6203(5) 0.2982(2) 0.0396(12) Uani 1 1 d . . . C11 C 0.0682(3) 0.7322(5) 0.2773(2) 0.0502(14) Uani 1 1 d . . . C12 C 0.0090(3) 0.7730(6) 0.2879(3) 0.0594(17) Uani 1 1 d . . . C13 C -0.0240(3) 0.7045(7) 0.3206(3) 0.0647(18) Uani 1 1 d . . . C14 C 0.0006(3) 0.5938(6) 0.3413(3) 0.0592(16) Uani 1 1 d . . . C15 C 0.0592(3) 0.5526(5) 0.3310(2) 0.0481(14) Uani 1 1 d . . . N16 N 0.51068(18) 0.0437(3) 0.37029(15) 0.0335(9) Uani 1 1 d . . . C17 C 0.5204(2) -0.0300(5) 0.4165(2) 0.0395(12) Uani 1 1 d . . . H17 H 0.4938 -0.0183 0.4431 0.047 Uiso 1 1 calc R . . C18 C 0.5674(2) -0.1219(4) 0.4269(2) 0.0393(12) Uani 1 1 d . . . H18 H 0.5712 -0.1727 0.4590 0.047 Uiso 1 1 calc R . . C19 C 0.6092(2) -0.1375(4) 0.38865(19) 0.0341(11) Uani 1 1 d . . . C20 C 0.5989(2) -0.0633(4) 0.3404(2) 0.0399(12) Uani 1 1 d . . . H20 H 0.6252 -0.0723 0.3133 0.048 Uiso 1 1 calc R . . C21 C 0.5494(2) 0.0239(5) 0.3326(2) 0.0410(12) Uani 1 1 d . . . H21 H 0.5424 0.0715 0.2995 0.049 Uiso 1 1 calc R . . N22 N 0.65838(19) -0.2280(4) 0.40107(17) 0.0431(10) Uani 1 1 d . . . H22 H 0.6531 -0.2851 0.4250 0.052 Uiso 1 1 calc R . . C23 C 0.7140(3) -0.2344(5) 0.3789(2) 0.0440(13) Uani 1 1 d . . . O24 O 0.72620(19) -0.1669(4) 0.34231(17) 0.0681(12) Uani 1 1 d . . . C25 C 0.7624(3) -0.3308(5) 0.4068(2) 0.0465(13) Uani 1 1 d . . . C26 C 0.8009(4) -0.3088(7) 0.4589(3) 0.076(2) Uani 1 1 d . . . C27 C 0.8487(4) -0.3937(9) 0.4822(3) 0.102(3) Uani 1 1 d . . . C28 C 0.8576(4) -0.4989(8) 0.4537(4) 0.092(3) Uani 1 1 d . . . C29 C 0.8211(3) -0.5198(6) 0.4021(4) 0.086(2) Uani 1 1 d . . . C30 C 0.7728(3) -0.4385(6) 0.3794(3) 0.0669(18) Uani 1 1 d . . . N31 N 0.50232(18) 0.5516(3) 0.37867(15) 0.0338(9) Uani 1 1 d . . . C32 C 0.4665(2) 0.5724(4) 0.4183(2) 0.0404(12) Uani 1 1 d . . . H32 H 0.4736 0.5213 0.4504 0.048 Uiso 1 1 calc R . . C33 C 0.4199(2) 0.6638(4) 0.4150(2) 0.0395(12) Uani 1 1 d . . . H33 H 0.3958 0.6736 0.4437 0.047 Uiso 1 1 calc R . . C34 C 0.4097(2) 0.7410(4) 0.36792(19) 0.0331(11) Uani 1 1 d . . . C35 C 0.4483(2) 0.7237(4) 0.3273(2) 0.0382(12) Uani 1 1 d . . . H35 H 0.4438 0.7767 0.2959 0.046 Uiso 1 1 calc R . . C36 C 0.4928(2) 0.6286(4) 0.3335(2) 0.0370(11) Uani 1 1 d . . . H36 H 0.5174 0.6166 0.3054 0.044 Uiso 1 1 calc R . . N37 N 0.36343(19) 0.8388(4) 0.35933(17) 0.0388(10) Uani 1 1 d . . . H37 H 0.3680 0.8930 0.3339 0.047 Uiso 1 1 calc R . . C38 C 0.3131(2) 0.8576(5) 0.3860(2) 0.0406(12) Uani 1 1 d . . . O39 O 0.30277(19) 0.7973(4) 0.42647(16) 0.0626(11) Uani 1 1 d . . . C40 C 0.2679(2) 0.9610(5) 0.3607(2) 0.0420(12) Uani 1 1 d . . . C41 C 0.2347(3) 0.9576(5) 0.3048(3) 0.0533(15) Uani 1 1 d . . . C42 C 0.1925(3) 1.0504(6) 0.2812(3) 0.0610(16) Uani 1 1 d . . . C43 C 0.1820(3) 1.1490(5) 0.3145(3) 0.0559(16) Uani 1 1 d . . . C44 C 0.2125(3) 1.1545(5) 0.3700(3) 0.0591(16) Uani 1 1 d . . . C45 C 0.2555(3) 1.0612(5) 0.3925(2) 0.0524(15) Uani 1 1 d . . . N46 N 0.63677(18) 0.2856(4) 0.38389(15) 0.0347(9) Uani 1 1 d . . . C47 C 0.6652(2) 0.2228(5) 0.4303(2) 0.0398(12) Uani 1 1 d . . . H47 H 0.6460 0.2268 0.4623 0.048 Uiso 1 1 calc R . . C48 C 0.7209(2) 0.1527(4) 0.4337(2) 0.0390(12) Uani 1 1 d . . . H48 H 0.7385 0.1096 0.4671 0.047 Uiso 1 1 calc R . . C49 C 0.7506(2) 0.1467(4) 0.3870(2) 0.0380(12) Uani 1 1 d . . . C50 C 0.7186(2) 0.2044(5) 0.3367(2) 0.0411(12) Uani 1 1 d . . . H50 H 0.7346 0.1962 0.3032 0.049 Uiso 1 1 calc R . . C51 C 0.6631(2) 0.2735(5) 0.3375(2) 0.0425(12) Uani 1 1 d . . . H51 H 0.6428 0.3138 0.3042 0.051 Uiso 1 1 calc R . . N52 N 0.81131(19) 0.0889(4) 0.38701(17) 0.0435(11) Uani 1 1 d . . . H52 H 0.8189 0.0660 0.3544 0.052 Uiso 1 1 calc R . . C53 C 0.8589(3) 0.0658(6) 0.4334(2) 0.0531(15) Uani 1 1 d . . . O54 O 0.8522(2) 0.0746(5) 0.48190(17) 0.0860(16) Uani 1 1 d . . . C55 C 0.9248(2) 0.0295(5) 0.4193(2) 0.0474(14) Uani 1 1 d . . . C56 C 0.9560(3) -0.0785(6) 0.4413(2) 0.0551(15) Uani 1 1 d . . . C57 C 1.0167(3) -0.1132(6) 0.4317(2) 0.0547(15) Uani 1 1 d . . . C58 C 1.0477(3) -0.0365(6) 0.4001(2) 0.0557(15) Uani 1 1 d . . . C59 C 1.0189(3) 0.0733(6) 0.3788(3) 0.0600(16) Uani 1 1 d . . . C60 C 0.9582(3) 0.1032(6) 0.3884(2) 0.0527(15) Uani 1 1 d . . . O61 O 0.1867(2) 0.6643(4) 0.43596(18) 0.0799(13) Uani 1 1 d . . . F1 F 0.08184(17) 0.4423(3) 0.35204(15) 0.0728(10) Uani 1 1 d . . . F2 F -0.03262(19) 0.5247(4) 0.37267(17) 0.0960(13) Uani 1 1 d . . . F3 F -0.08049(16) 0.7484(4) 0.33157(18) 0.1004(15) Uani 1 1 d . . . F4 F -0.0134(2) 0.8862(3) 0.26818(17) 0.0946(14) Uani 1 1 d . . . F5 F 0.10123(18) 0.8041(3) 0.24655(15) 0.0732(10) Uani 1 1 d . . . F6 F 0.7352(2) -0.4634(4) 0.3290(2) 0.127(2) Uani 1 1 d . . . F7 F 0.8331(2) -0.6229(4) 0.3743(3) 0.157(3) Uani 1 1 d . . . F11 F 0.24417(18) 0.8612(3) 0.27178(15) 0.0791(11) Uani 1 1 d . . . F12 F 0.1590(2) 1.0442(4) 0.22726(18) 0.0973(14) Uani 1 1 d . . . F13 F 0.14145(17) 1.2407(3) 0.29151(18) 0.0839(12) Uani 1 1 d . . . F14 F 0.2000(2) 1.2488(3) 0.40228(17) 0.0921(13) Uani 1 1 d . . . F15 F 0.2868(2) 1.0697(3) 0.44712(15) 0.0829(12) Uani 1 1 d . . . F16 F 0.92668(18) -0.1571(4) 0.47189(17) 0.0875(12) Uani 1 1 d . . . F17 F 1.04281(17) -0.2226(3) 0.45022(16) 0.0817(11) Uani 1 1 d . . . F18 F 1.10638(16) -0.0696(4) 0.38922(15) 0.0760(11) Uani 1 1 d . . . F19 F 1.04974(18) 0.1470(4) 0.34786(18) 0.0940(13) Uani 1 1 d . . . F20 F 0.93176(16) 0.2111(3) 0.36722(16) 0.0765(10) Uani 1 1 d . . . F8A F 0.9022(3) -0.5893(6) 0.4697(3) 0.0808(17) Uiso 0.68 1 d P . . F8B F 0.9146(5) -0.5490(9) 0.4959(4) 0.049(2) Uiso 0.32 1 d P . . F9A F 0.8772(4) -0.3959(8) 0.5322(4) 0.111(3) Uiso 0.60 1 d P . . F9B F 0.8987(4) -0.3298(8) 0.5359(3) 0.052(2) Uiso 0.40 1 d P . . F10A F 0.8000(3) -0.1847(5) 0.4842(2) 0.0685(14) Uiso 0.68 1 d P . . F10B F 0.7757(5) -0.2419(10) 0.4903(4) 0.052(2) Uiso 0.32 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 Cu1 0.0315(3) 0.0380(4) 0.0333(3) 0.0014(3) 0.0057(3) 0.0075(3) Cu2 0.0331(3) 0.0357(4) 0.0313(3) -0.0008(3) 0.0051(3) 0.0088(3) Cl1 0.0444(7) 0.0392(7) 0.0444(7) 0.0011(6) 0.0009(6) -0.0003(6) Cl2 0.0386(7) 0.0445(7) 0.0321(6) 0.0001(5) 0.0046(5) 0.0083(6) Cl3 0.0360(7) 0.0410(7) 0.0291(6) 0.0007(5) 0.0080(5) 0.0054(5) Cl4 0.0487(8) 0.0419(7) 0.0378(7) -0.0008(6) 0.0012(6) 0.0002(6) N1 0.032(2) 0.043(2) 0.031(2) 0.0002(18) 0.0065(18) 0.0060(18) C2 0.040(3) 0.067(4) 0.034(3) -0.004(3) 0.005(2) 0.012(3) C3 0.041(3) 0.069(4) 0.038(3) -0.007(3) 0.006(2) 0.022(3) C4 0.034(3) 0.045(3) 0.044(3) -0.001(2) 0.006(2) 0.007(2) C5 0.041(3) 0.056(3) 0.033(3) 0.006(2) 0.010(2) 0.010(3) C6 0.045(3) 0.051(3) 0.031(3) 0.008(2) 0.012(2) 0.014(3) N7 0.042(3) 0.059(3) 0.036(2) -0.001(2) 0.004(2) 0.022(2) C8 0.043(3) 0.042(3) 0.043(3) -0.001(2) 0.010(3) 0.005(2) O9 0.054(2) 0.070(3) 0.040(2) 0.0032(19) 0.0093(18) 0.018(2) C10 0.036(3) 0.041(3) 0.039(3) -0.002(2) 0.002(2) 0.011(2) C11 0.054(4) 0.038(3) 0.051(3) -0.008(3) -0.007(3) 0.005(3) C12 0.049(4) 0.049(4) 0.069(4) -0.020(3) -0.015(3) 0.026(3) C13 0.031(3) 0.084(5) 0.076(4) -0.031(4) 0.005(3) 0.009(3) C14 0.049(4) 0.071(4) 0.060(4) -0.010(3) 0.015(3) -0.007(3) C15 0.044(3) 0.053(3) 0.047(3) 0.000(3) 0.009(3) 0.011(3) N16 0.034(2) 0.034(2) 0.030(2) 0.0047(18) 0.0026(18) 0.0062(18) C17 0.038(3) 0.046(3) 0.037(3) -0.004(2) 0.012(2) 0.001(2) C18 0.039(3) 0.038(3) 0.039(3) 0.010(2) 0.006(2) 0.007(2) C19 0.034(3) 0.031(3) 0.038(3) 0.003(2) 0.007(2) 0.003(2) C20 0.046(3) 0.038(3) 0.037(3) 0.004(2) 0.013(2) 0.012(2) C21 0.051(3) 0.041(3) 0.031(3) 0.004(2) 0.005(2) 0.009(2) N22 0.044(3) 0.037(2) 0.051(3) 0.015(2) 0.018(2) 0.012(2) C23 0.047(3) 0.038(3) 0.048(3) 0.005(3) 0.013(3) 0.007(2) O24 0.062(3) 0.077(3) 0.075(3) 0.036(2) 0.036(2) 0.025(2) C25 0.041(3) 0.047(3) 0.056(4) 0.016(3) 0.020(3) 0.015(3) C26 0.091(5) 0.089(5) 0.055(4) 0.020(4) 0.030(4) 0.048(4) C27 0.087(6) 0.176(9) 0.045(4) 0.053(5) 0.019(4) 0.070(6) C28 0.061(5) 0.083(5) 0.144(8) 0.073(6) 0.054(5) 0.062(4) C29 0.044(4) 0.048(4) 0.162(8) 0.008(5) 0.012(5) 0.012(3) C30 0.038(3) 0.047(4) 0.115(6) 0.004(4) 0.012(4) 0.007(3) N31 0.036(2) 0.033(2) 0.032(2) -0.0005(18) 0.0067(18) 0.0100(18) C32 0.049(3) 0.039(3) 0.033(3) 0.009(2) 0.008(2) 0.014(2) C33 0.047(3) 0.039(3) 0.035(3) 0.004(2) 0.015(2) 0.010(2) C34 0.033(3) 0.033(3) 0.032(3) 0.004(2) 0.005(2) 0.007(2) C35 0.043(3) 0.039(3) 0.033(3) 0.009(2) 0.009(2) 0.001(2) C36 0.042(3) 0.037(3) 0.032(3) 0.002(2) 0.009(2) 0.005(2) N37 0.039(2) 0.035(2) 0.046(2) 0.0130(19) 0.015(2) 0.0113(19) C38 0.038(3) 0.043(3) 0.042(3) 0.007(3) 0.012(2) 0.008(2) O39 0.061(3) 0.071(3) 0.065(3) 0.031(2) 0.034(2) 0.027(2) C40 0.036(3) 0.038(3) 0.056(3) 0.006(3) 0.018(3) 0.006(2) C41 0.040(3) 0.052(4) 0.065(4) 0.006(3) 0.004(3) 0.009(3) C42 0.042(3) 0.063(4) 0.073(4) 0.012(3) -0.001(3) 0.008(3) C43 0.037(3) 0.049(4) 0.084(5) 0.024(3) 0.018(3) 0.013(3) C44 0.062(4) 0.043(3) 0.084(5) 0.007(3) 0.042(4) 0.015(3) C45 0.055(4) 0.059(4) 0.047(4) 0.012(3) 0.020(3) 0.013(3) N46 0.031(2) 0.041(2) 0.032(2) 0.0012(19) 0.0079(18) 0.0075(18) C47 0.039(3) 0.051(3) 0.030(3) 0.001(2) 0.010(2) 0.013(2) C48 0.038(3) 0.040(3) 0.039(3) 0.006(2) 0.008(2) 0.010(2) C49 0.034(3) 0.042(3) 0.038(3) -0.007(2) 0.006(2) 0.005(2) C50 0.035(3) 0.056(3) 0.034(3) 0.001(2) 0.013(2) 0.015(2) C51 0.044(3) 0.051(3) 0.032(3) 0.004(2) 0.006(2) 0.008(3) N52 0.035(2) 0.060(3) 0.035(2) -0.004(2) 0.0061(19) 0.018(2) C53 0.043(3) 0.073(4) 0.042(3) 0.005(3) 0.005(3) 0.018(3) O54 0.054(3) 0.164(5) 0.039(2) 0.008(3) 0.005(2) 0.045(3) C55 0.034(3) 0.067(4) 0.038(3) 0.001(3) -0.003(2) 0.019(3) C56 0.047(3) 0.072(4) 0.044(3) 0.007(3) 0.004(3) 0.008(3) C57 0.042(3) 0.062(4) 0.056(4) -0.003(3) -0.002(3) 0.020(3) C58 0.037(3) 0.079(4) 0.051(3) -0.010(3) 0.010(3) 0.011(3) C59 0.047(4) 0.069(4) 0.065(4) 0.006(3) 0.013(3) 0.012(3) C60 0.042(3) 0.062(4) 0.051(3) -0.002(3) 0.001(3) 0.016(3) O61 0.076(3) 0.095(3) 0.074(3) -0.023(3) 0.027(2) -0.001(3) F1 0.078(2) 0.066(2) 0.082(2) 0.0271(19) 0.032(2) 0.0170(19) F2 0.069(3) 0.129(4) 0.103(3) 0.001(3) 0.047(2) -0.003(2) F3 0.042(2) 0.134(4) 0.121(3) -0.057(3) 0.006(2) 0.028(2) F4 0.097(3) 0.062(2) 0.109(3) -0.010(2) -0.019(2) 0.047(2) F5 0.086(3) 0.051(2) 0.079(2) 0.0136(19) 0.009(2) 0.0012(18) F6 0.070(3) 0.094(3) 0.192(5) -0.076(3) -0.031(3) 0.030(2) F7 0.077(3) 0.052(3) 0.329(8) -0.049(4) 0.008(4) 0.023(2) F11 0.082(3) 0.061(2) 0.080(2) -0.016(2) -0.018(2) 0.0197(19) F12 0.086(3) 0.084(3) 0.099(3) 0.015(2) -0.037(2) 0.012(2) F13 0.061(2) 0.064(2) 0.129(3) 0.039(2) 0.023(2) 0.0265(19) F14 0.127(3) 0.068(2) 0.096(3) 0.006(2) 0.058(3) 0.040(2) F15 0.118(3) 0.075(2) 0.059(2) 0.0009(18) 0.026(2) 0.036(2) F16 0.071(2) 0.096(3) 0.099(3) 0.040(2) 0.026(2) 0.027(2) F17 0.064(2) 0.078(3) 0.098(3) 0.014(2) 0.005(2) 0.039(2) F18 0.046(2) 0.107(3) 0.076(2) -0.008(2) 0.0161(17) 0.0276(19) F19 0.061(2) 0.115(3) 0.114(3) 0.035(3) 0.037(2) 0.012(2) F20 0.059(2) 0.071(2) 0.100(3) 0.021(2) 0.017(2) 0.0228(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N16 2.007(4) . ? Cu1 N1 2.032(4) . ? Cu1 Cl1 2.3122(13) . ? Cu1 Cl2 2.3134(12) . ? Cu1 Cl3 2.6239(13) . ? Cu2 N31 1.989(4) . ? Cu2 N46 2.000(4) . ? Cu2 Cl4 2.3018(13) . ? Cu2 Cl3 2.3121(12) . ? N1 C6 1.327(6) . ? N1 C2 1.347(6) . ? C2 C3 1.369(7) . ? C3 C4 1.381(7) . ? C4 N7 1.386(6) . ? C4 C5 1.390(7) . ? C5 C6 1.369(7) . ? N7 C8 1.356(6) . ? C8 O9 1.216(6) . ? C8 C10 1.499(7) . ? C10 C11 1.378(7) . ? C10 C15 1.391(7) . ? C11 F5 1.344(7) . ? C11 C12 1.372(8) . ? C12 F4 1.352(7) . ? C12 C13 1.354(9) . ? C13 F3 1.336(6) . ? C13 C14 1.347(9) . ? C14 F2 1.338(7) . ? C14 C15 1.361(8) . ? C15 F1 1.335(6) . ? N16 C21 1.336(6) . ? N16 C17 1.340(6) . ? C17 C18 1.374(7) . ? C18 C19 1.389(6) . ? C19 C20 1.383(6) . ? C19 N22 1.396(6) . ? C20 C21 1.374(7) . ? N22 C23 1.362(6) . ? C23 O24 1.202(6) . ? C23 C25 1.501(7) . ? C25 C26 1.358(8) . ? C25 C30 1.368(8) . ? C26 F10B 1.229(11) . ? C26 C27 1.379(9) . ? C26 F10A 1.466(9) . ? C27 F9A 1.222(10) . ? C27 C28 1.351(12) . ? C27 F9B 1.630(12) . ? C28 C29 1.329(11) . ? C28 F8A 1.342(8) . ? C28 F8B 1.492(12) . ? C29 F7 1.340(9) . ? C29 C30 1.357(9) . ? C30 F6 1.323(8) . ? N31 C32 1.334(6) . ? N31 C36 1.341(6) . ? C32 C33 1.368(6) . ? C33 C34 1.379(6) . ? C34 C35 1.387(6) . ? C34 N37 1.409(6) . ? C35 C36 1.365(6) . ? N37 C38 1.342(6) . ? C38 O39 1.217(6) . ? C38 C40 1.500(7) . ? C40 C41 1.375(7) . ? C40 C45 1.370(7) . ? C41 F11 1.340(6) . ? C41 C42 1.371(8) . ? C42 F12 1.337(7) . ? C42 C43 1.369(8) . ? C43 F13 1.339(6) . ? C43 C44 1.352(8) . ? C44 F14 1.329(6) . ? C44 C45 1.377(8) . ? C45 F15 1.338(6) . ? N46 C47 1.331(6) . ? N46 C51 1.335(6) . ? C47 C48 1.367(6) . ? C48 C49 1.381(6) . ? C49 C50 1.395(7) . ? C49 N52 1.402(6) . ? C50 C51 1.372(7) . ? N52 C53 1.351(6) . ? C53 O54 1.199(6) . ? C53 C55 1.519(7) . ? C55 C60 1.363(8) . ? C55 C56 1.381(8) . ? C56 F16 1.339(7) . ? C56 C57 1.374(8) . ? C57 F17 1.332(6) . ? C57 C58 1.361(8) . ? C58 F18 1.341(6) . ? C58 C59 1.373(8) . ? C59 F19 1.330(7) . ? C59 C60 1.361(8) . ? C60 F20 1.337(6) . ? O61 O61 0.000(9) 1 ? F8A F8B 0.763(10) . ? F9A F9B 0.832(9) . ? F10A F10B 0.825(9) . ? 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 N16 Cu1 N1 172.48(15) . . ? N16 Cu1 Cl1 87.19(11) . . ? N1 Cu1 Cl1 91.91(11) . . ? N16 Cu1 Cl2 86.57(11) . . ? N1 Cu1 Cl2 92.88(11) . . ? Cl1 Cu1 Cl2 167.68(5) . . ? N16 Cu1 Cl3 97.66(11) . . ? N1 Cu1 Cl3 89.86(11) . . ? Cl1 Cu1 Cl3 98.38(4) . . ? Cl2 Cu1 Cl3 92.97(4) . . ? N31 Cu2 N46 170.44(15) . . ? N31 Cu2 Cl4 89.15(11) . . ? N46 Cu2 Cl4 90.44(11) . . ? N31 Cu2 Cl3 88.70(11) . . ? N46 Cu2 Cl3 90.33(11) . . ? Cl4 Cu2 Cl3 171.56(5) . . ? Cu2 Cl3 Cu1 90.64(4) . . ? C6 N1 C2 115.5(4) . . ? C6 N1 Cu1 120.6(3) . . ? C2 N1 Cu1 123.9(3) . . ? N1 C2 C3 123.5(5) . . ? C2 C3 C4 120.2(5) . . ? C3 C4 N7 118.0(4) . . ? C3 C4 C5 116.7(4) . . ? N7 C4 C5 125.2(4) . . ? C6 C5 C4 119.0(5) . . ? N1 C6 C5 125.1(4) . . ? C8 N7 C4 128.3(4) . . ? O9 C8 N7 125.0(5) . . ? O9 C8 C10 121.2(5) . . ? N7 C8 C10 113.7(4) . . ? C11 C10 C15 115.7(5) . . ? C11 C10 C8 122.8(5) . . ? C15 C10 C8 121.5(4) . . ? F5 C11 C12 119.3(5) . . ? F5 C11 C10 118.9(5) . . ? C12 C11 C10 121.8(6) . . ? F4 C12 C13 120.8(6) . . ? F4 C12 C11 118.7(7) . . ? C13 C12 C11 120.4(6) . . ? F3 C13 C14 121.4(7) . . ? F3 C13 C12 119.0(7) . . ? C14 C13 C12 119.6(5) . . ? F2 C14 C13 119.7(6) . . ? F2 C14 C15 119.9(6) . . ? C13 C14 C15 120.4(6) . . ? F1 C15 C14 118.6(5) . . ? F1 C15 C10 119.2(4) . . ? C14 C15 C10 122.2(5) . . ? C21 N16 C17 116.6(4) . . ? C21 N16 Cu1 120.1(3) . . ? C17 N16 Cu1 123.3(3) . . ? N16 C17 C18 124.0(4) . . ? C17 C18 C19 118.7(4) . . ? C20 C19 C18 117.8(4) . . ? C20 C19 N22 124.3(4) . . ? C18 C19 N22 118.0(4) . . ? C21 C20 C19 119.4(4) . . ? N16 C21 C20 123.4(4) . . ? C23 N22 C19 126.2(4) . . ? O24 C23 N22 124.8(5) . . ? O24 C23 C25 121.3(5) . . ? N22 C23 C25 113.8(4) . . ? C26 C25 C30 117.7(5) . . ? C26 C25 C23 120.4(5) . . ? C30 C25 C23 121.8(5) . . ? F10B C26 C25 114.6(7) . . ? F10B C26 C27 120.0(7) . . ? C25 C26 C27 119.9(7) . . ? F10B C26 F10A 34.2(5) . . ? C25 C26 F10A 118.8(5) . . ? C27 C26 F10A 120.2(7) . . ? F9A C27 C28 112.9(8) . . ? F9A C27 C26 125.1(9) . . ? C28 C27 C26 120.6(7) . . ? F9A C27 F9B 29.8(5) . . ? C28 C27 F9B 128.3(7) . . ? C26 C27 F9B 109.4(8) . . ? C29 C28 F8A 111.9(9) . . ? C29 C28 C27 120.0(6) . . ? F8A C28 C27 128.1(10) . . ? C29 C28 F8B 142.4(9) . . ? F8A C28 F8B 30.7(4) . . ? C27 C28 F8B 97.4(9) . . ? C28 C29 F7 118.1(7) . . ? C28 C29 C30 119.9(7) . . ? F7 C29 C30 121.9(8) . . ? F6 C30 C29 119.1(7) . . ? F6 C30 C25 119.1(5) . . ? C29 C30 C25 121.8(7) . . ? C32 N31 C36 117.0(4) . . ? C32 N31 Cu2 121.4(3) . . ? C36 N31 Cu2 121.6(3) . . ? N31 C32 C33 124.5(4) . . ? C32 C33 C34 118.0(4) . . ? C33 C34 C35 118.4(4) . . ? C33 C34 N37 123.7(4) . . ? C35 C34 N37 117.9(4) . . ? C36 C35 C34 119.6(4) . . ? N31 C36 C35 122.5(4) . . ? C38 N37 C34 127.9(4) . . ? O39 C38 N37 125.0(4) . . ? O39 C38 C40 121.3(4) . . ? N37 C38 C40 113.7(4) . . ? C41 C40 C45 116.6(5) . . ? C41 C40 C38 121.5(5) . . ? C45 C40 C38 121.9(5) . . ? F11 C41 C42 118.4(5) . . ? F11 C41 C40 119.2(5) . . ? C42 C41 C40 122.3(6) . . ? F12 C42 C41 121.8(6) . . ? F12 C42 C43 119.1(5) . . ? C41 C42 C43 119.0(6) . . ? F13 C43 C44 120.2(6) . . ? F13 C43 C42 119.3(6) . . ? C44 C43 C42 120.4(5) . . ? F14 C44 C43 119.6(5) . . ? F14 C44 C45 121.0(6) . . ? C43 C44 C45 119.4(6) . . ? F15 C45 C40 119.1(5) . . ? F15 C45 C44 118.7(5) . . ? C40 C45 C44 122.2(6) . . ? C47 N46 C51 117.2(4) . . ? C47 N46 Cu2 121.9(3) . . ? C51 N46 Cu2 120.4(3) . . ? N46 C47 C48 123.8(4) . . ? C47 C48 C49 119.1(4) . . ? C48 C49 C50 117.6(4) . . ? C48 C49 N52 124.4(4) . . ? C50 C49 N52 118.0(4) . . ? C51 C50 C49 118.9(4) . . ? N46 C51 C50 123.2(4) . . ? C53 N52 C49 126.2(4) . . ? O54 C53 N52 124.8(5) . . ? O54 C53 C55 121.1(5) . . ? N52 C53 C55 114.1(5) . . ? C60 C55 C56 116.3(5) . . ? C60 C55 C53 123.2(5) . . ? C56 C55 C53 120.4(5) . . ? F16 C56 C57 116.9(5) . . ? F16 C56 C55 120.5(5) . . ? C57 C56 C55 122.6(6) . . ? F17 C57 C58 120.8(5) . . ? F17 C57 C56 120.5(6) . . ? C58 C57 C56 118.6(5) . . ? F18 C58 C57 119.6(6) . . ? F18 C58 C59 120.0(6) . . ? C57 C58 C59 120.4(5) . . ? F19 C59 C60 121.0(6) . . ? F19 C59 C58 119.7(5) . . ? C60 C59 C58 119.2(6) . . ? F20 C60 C55 119.6(5) . . ? F20 C60 C59 117.6(6) . . ? C55 C60 C59 122.8(5) . . ? F8B F8A C28 85.6(11) . . ? F8A F8B C28 63.8(10) . . ? F9B F9A C27 103.3(12) . . ? F9A F9B C27 46.8(8) . . ? F10B F10A C26 57.0(8) . . ? F10A F10B C26 88.8(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N52 H52 O9 0.86 2.24 3.083(5) 165.5 2_645 N7 H7 O61 0.86 2.06 2.914(6) 172.7 1 N37 H37 Cl1 0.86 2.33 3.175(4) 168.9 1_565 N22 H22 Cl4 0.86 2.45 3.271(4) 159.8 1_545 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.13 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.583 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.070 # _vrf_THETM01_yu ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5116 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT213_yu ; PROBLEM: Atom C28 has ADP max/min Ratio.....5.0 prola RESPONSE: C28 is attached to disordered F atom. ; _vrf_PLAT306_yu ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O61 RESPONSE: We are unable to locate the H-atoms associated with the solvent water molecule containing O61. ; _vrf_PLAT434_yu ; PROBLEM: Short inter HL...HL contact F14..F10B. 2.52Ang RESPONSE: F14 interact with disordered F10 atom, hence this alert appears. ; _vrf_REFNR01_yu ; PROBLEM: Ratio of reflections to parameters is < 10 for a centrosymmetric structure sine(theta)/lambda 0.5527 Proportion of unique data used 1.0000 Ratio reflections to parameters 9.4136 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT088_yu ; PROBLEM: Poor Data / Parameter Ratio .................... 9.41 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _database_code_depnum_ccdc_archive 'CCDC 926130' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form # Attachment 'CC8.cif' data_ty #TrackingRef 'CC8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H10 Cl2 Cu F10 N4 O2' _chemical_formula_weight 710.80 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' Cl Cl 0.1484 0.1585 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1671(9) _cell_length_b 14.9959(12) _cell_length_c 7.1861(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.349(2) _cell_angle_gamma 90.00 _cell_volume 1289.82(17) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description NEEDLE _exptl_crystal_colour 'DEEP BLUE' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 1.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7845 _exptl_absorpt_correction_T_max 0.9028 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7004 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 19.57 _reflns_number_total 1135 _reflns_number_gt 939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material 'Shelxl 97' _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^)+(0.1000P)^2^+0.5000P] 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 1135 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 1.0000 1.0000 0.0362(5) Uani 1 2 d S . . Cl1 Cl 0.41286(16) 1.03592(11) 1.2420(2) 0.0580(7) Uani 1 1 d . . . N1 N 0.4337(5) 0.8778(3) 0.9904(7) 0.0343(13) Uani 1 1 d . . . C2 C 0.4960(5) 0.8043(5) 0.9839(8) 0.0401(17) Uani 1 1 d . . . H2 H 0.5719 0.8113 0.9830 0.048 Uiso 1 1 calc R . . C3 C 0.4534(6) 0.7191(4) 0.9786(8) 0.0395(16) Uani 1 1 d . . . H3 H 0.5001 0.6702 0.9760 0.047 Uiso 1 1 calc R . . C4 C 0.3409(6) 0.7072(4) 0.9771(8) 0.0333(16) Uani 1 1 d . . . C5 C 0.2757(5) 0.7825(4) 0.9837(8) 0.0385(17) Uani 1 1 d . . . H5 H 0.1996 0.7774 0.9848 0.046 Uiso 1 1 calc R . . C6 C 0.3256(6) 0.8645(4) 0.9886(8) 0.0379(17) Uani 1 1 d . . . H6 H 0.2805 0.9144 0.9908 0.045 Uiso 1 1 calc R . . N7 N 0.2987(5) 0.6199(3) 0.9668(7) 0.0405(14) Uani 1 1 d . . . H7 H 0.3438 0.5782 0.9472 0.049 Uiso 1 1 calc R . . C8 C 0.1938(7) 0.5944(5) 0.9844(9) 0.0464(18) Uani 1 1 d . . . O9 O 0.1230(4) 0.6437(3) 1.0185(9) 0.0800(18) Uani 1 1 d . . . C10 C 0.1714(6) 0.4971(4) 0.9500(10) 0.0414(18) Uani 1 1 d . . . C11 C 0.2307(6) 0.4313(5) 1.0510(11) 0.049(2) Uani 1 1 d . . . C12 C 0.2072(7) 0.3449(6) 1.0214(14) 0.065(2) Uani 1 1 d . . . C13 C 0.1233(11) 0.3197(5) 0.8853(19) 0.080(3) Uani 1 1 d . . . C14 C 0.0623(8) 0.3827(9) 0.7786(12) 0.082(3) Uani 1 1 d . . . C15 C 0.0850(7) 0.4704(6) 0.8120(12) 0.062(2) Uani 1 1 d . . . F1 F 0.3158(4) 0.4516(3) 1.1931(7) 0.0807(14) Uani 1 1 d . . . F5 F 0.0216(5) 0.5317(4) 0.7059(7) 0.1059(18) Uani 1 1 d . . . F2A F 0.2812(8) 0.2837(6) 1.1694(16) 0.067(3) Uiso 0.49 1 d P . . F2B F 0.2554(8) 0.2762(7) 1.0841(16) 0.068(3) Uiso 0.51 1 d P . . F3A F 0.1205(8) 0.2227(6) 0.8894(14) 0.067(3) Uiso 0.47 1 d P . . F3B F 0.0740(7) 0.2412(6) 0.8167(12) 0.065(2) Uiso 0.53 1 d P . . F4A F -0.0431(8) 0.3750(6) 0.6293(11) 0.076(3) Uiso 0.55 1 d P . . F4B F -0.0007(9) 0.3407(8) 0.6494(15) 0.072(3) Uiso 0.45 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 Cu1 0.0438(8) 0.0276(8) 0.0390(8) 0.0009(5) 0.0124(5) -0.0029(5) Cl1 0.0862(14) 0.0393(11) 0.0590(12) -0.0103(8) 0.0414(10) -0.0184(10) N1 0.037(4) 0.026(3) 0.040(3) 0.001(2) 0.009(2) 0.005(3) C2 0.036(4) 0.038(5) 0.049(4) 0.004(3) 0.016(3) -0.003(4) C3 0.039(5) 0.035(5) 0.047(4) 0.003(3) 0.015(3) 0.003(3) C4 0.045(5) 0.027(5) 0.028(4) 0.000(3) 0.008(3) -0.005(4) C5 0.033(4) 0.037(5) 0.046(4) 0.003(3) 0.008(3) -0.002(4) C6 0.043(5) 0.029(4) 0.041(4) 0.001(3) 0.007(3) 0.007(3) N7 0.040(4) 0.029(4) 0.056(4) -0.006(3) 0.018(3) -0.004(3) C8 0.043(5) 0.041(5) 0.056(4) -0.007(3) 0.012(4) -0.003(4) O9 0.052(3) 0.044(3) 0.155(6) -0.016(3) 0.046(3) -0.004(3) C10 0.041(4) 0.039(5) 0.048(5) -0.008(4) 0.016(4) -0.013(4) C11 0.052(5) 0.025(5) 0.077(6) -0.011(4) 0.027(5) -0.016(4) C12 0.054(6) 0.055(8) 0.094(7) 0.006(5) 0.030(5) 0.004(5) C13 0.123(10) 0.026(5) 0.111(8) -0.032(6) 0.074(8) -0.039(6) C14 0.083(7) 0.111(9) 0.051(6) -0.040(6) 0.009(5) -0.075(7) C15 0.066(6) 0.067(6) 0.055(5) -0.005(5) 0.020(5) -0.023(5) F1 0.061(3) 0.069(3) 0.104(4) 0.009(3) -0.006(3) -0.007(2) F5 0.102(4) 0.123(4) 0.078(4) 0.023(3) -0.022(3) -0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.998(5) . ? Cu1 N1 1.998(5) 3_677 ? Cu1 Cl1 2.2584(16) 3_677 ? Cu1 Cl1 2.2584(16) . ? N1 C6 1.329(8) . ? N1 C2 1.344(8) . ? C2 C3 1.376(9) . ? C2 H2 0.9300 . ? C3 C4 1.379(8) . ? C3 H3 0.9300 . ? C4 C5 1.386(8) . ? C4 N7 1.403(8) . ? C5 C6 1.369(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N7 C8 1.360(8) . ? N7 H7 0.8600 . ? C8 O9 1.194(8) . ? C8 C10 1.497(9) . ? C10 C11 1.353(9) . ? C10 C15 1.368(10) . ? C11 C12 1.336(11) . ? C11 F1 1.352(8) . ? C12 F2B 1.230(11) . ? C12 C13 1.336(12) . ? C12 F2A 1.562(13) . ? C13 C14 1.351(13) . ? C13 F3B 1.373(12) . ? C13 F3A 1.456(12) . ? C14 F4B 1.262(12) . ? C14 C15 1.356(12) . ? C14 F4A 1.521(13) . ? C15 F5 1.345(9) . ? F2A F2B 0.647(12) . ? F3A F3B 0.751(10) . ? F4A F4B 0.724(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 Cu1 N1 180.000(1) . 3_677 ? N1 Cu1 Cl1 89.84(15) . 3_677 ? N1 Cu1 Cl1 90.16(15) 3_677 3_677 ? N1 Cu1 Cl1 90.17(15) . . ? N1 Cu1 Cl1 89.83(15) 3_677 . ? Cl1 Cu1 Cl1 180.00(8) 3_677 . ? C6 N1 C2 116.1(5) . . ? C6 N1 Cu1 122.1(4) . . ? C2 N1 Cu1 121.8(4) . . ? N1 C2 C3 123.4(6) . . ? N1 C2 H2 118.3 . . ? C3 C2 H2 118.3 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 117.9(6) . . ? C3 C4 N7 118.4(6) . . ? C5 C4 N7 123.7(6) . . ? C6 C5 C4 118.6(6) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 124.7(6) . . ? N1 C6 H6 117.6 . . ? C5 C6 H6 117.6 . . ? C8 N7 C4 126.8(5) . . ? C8 N7 H7 116.6 . . ? C4 N7 H7 116.6 . . ? O9 C8 N7 124.6(6) . . ? O9 C8 C10 121.4(7) . . ? N7 C8 C10 113.9(6) . . ? C11 C10 C15 116.2(7) . . ? C11 C10 C8 123.9(7) . . ? C15 C10 C8 119.9(7) . . ? C12 C11 F1 116.8(8) . . ? C12 C11 C10 122.9(8) . . ? F1 C11 C10 120.3(6) . . ? F2B C12 C13 106.4(11) . . ? F2B C12 C11 132.9(11) . . ? C13 C12 C11 120.3(8) . . ? F2B C12 F2A 23.1(6) . . ? C13 C12 F2A 127.1(10) . . ? C11 C12 F2A 112.4(9) . . ? C12 C13 C14 119.2(7) . . ? C12 C13 F3B 137.2(13) . . ? C14 C13 F3B 103.7(12) . . ? C12 C13 F3A 106.6(12) . . ? C14 C13 F3A 134.2(12) . . ? F3B C13 F3A 30.6(4) . . ? F4B C14 C13 105.5(13) . . ? F4B C14 C15 133.8(13) . . ? C13 C14 C15 120.2(8) . . ? F4B C14 F4A 28.2(6) . . ? C13 C14 F4A 130.9(11) . . ? C15 C14 F4A 108.5(11) . . ? F5 C15 C14 119.0(9) . . ? F5 C15 C10 119.9(8) . . ? C14 C15 C10 121.1(8) . . ? F2B F2A C12 48.3(14) . . ? F2A F2B C12 108.6(18) . . ? F3B F3A C13 68.6(13) . . ? F3A F3B C13 80.8(14) . . ? F4B F4A C14 55.5(13) . . ? F4A F4B C14 96.2(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 Cl1 0.86 2.50 3.287(5) 152.3 4_575 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 19.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.365 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.062 # _vrf_REFNR01_ty ; PROBLEM: Ratio of reflections to parameters is < 6 for a centrosymmetric structure sine(theta)/lambda 0.4114 Proportion of unique data used 1.0000 Ratio reflections to parameters 4.4291 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_THETM01_ty ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4114 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT088_ty ; PROBLEM: Poor Data / Parameter Ratio .................... 4.43 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _database_code_depnum_ccdc_archive 'CCDC 926131' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form # Attachment 'CC9 CORR Y_final.cif' data_y_CC9 #TrackingRef 'CC9 CORR Y_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H45 Cu N12 O15 S' _chemical_formula_weight 1137.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/n _symmetry_space_group_name_Hall '-P 4a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 17.8802(14) _cell_length_b 17.8802(14) _cell_length_c 8.4406(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2698.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8596 _exptl_absorpt_correction_T_max 0.9261 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean 3 _diffrn_reflns_number 27596 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 24.19 _reflns_number_total 2172 _reflns_number_gt 1943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.4' _computing_publication_material Shelxl-97 _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^)+(0.1094P)^2^+16.7802P] 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 2172 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2412 _refine_ls_wR_factor_gt 0.2371 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.812 _refine_ls_shift/su_mean 0.053 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.2500 0.2500 0.27148(17) 0.0203(5) Uani 1 4 d S . . S1 S 0.7500 0.2500 0.5000 0.0211(7) Uani 1 4 d S . . N1 N 0.2672(2) 0.3631(3) 0.2642(6) 0.0221(11) Uani 1 1 d . . . C2 C 0.2392(3) 0.4081(3) 0.3751(8) 0.0244(13) Uani 1 1 d . . . H2 H 0.2120 0.3872 0.4579 0.029 Uiso 1 1 calc R . . C3 C 0.2490(3) 0.4852(3) 0.3716(8) 0.0251(13) Uani 1 1 d . . . C4 C 0.2860(3) 0.5157(3) 0.2431(8) 0.0299(14) Uani 1 1 d . . . H4 H 0.2917 0.5672 0.2352 0.036 Uiso 1 1 calc R . . C5 C 0.3141(3) 0.4699(3) 0.1275(8) 0.0312(15) Uani 1 1 d . . . H5 H 0.3387 0.4900 0.0403 0.037 Uiso 1 1 calc R . . C6 C 0.3054(3) 0.3935(3) 0.1421(8) 0.0271(13) Uani 1 1 d . . . H6 H 0.3263 0.3623 0.0661 0.033 Uiso 1 1 calc R . . N7 N 0.2224(3) 0.5353(3) 0.4886(6) 0.0292(12) Uani 1 1 d . . . H7 H 0.2219 0.5821 0.4644 0.035 Uiso 1 1 calc R . . C8 C 0.1978(4) 0.5167(3) 0.6342(8) 0.0311(15) Uani 1 1 d . . . O9 O 0.1984(3) 0.4519(3) 0.6866(6) 0.0499(14) Uani 1 1 d . . . N10 N 0.1743(3) 0.5765(3) 0.7204(6) 0.0292(12) Uani 1 1 d . . . H10 H 0.1737 0.6193 0.6737 0.035 Uiso 1 1 calc R . . C11 C 0.1506(3) 0.5745(3) 0.8797(8) 0.0294(14) Uani 1 1 d . . . C12 C 0.1135(4) 0.5146(4) 0.9472(9) 0.0360(16) Uani 1 1 d . . . H12 H 0.1050 0.4714 0.8883 0.043 Uiso 1 1 calc R . . C13 C 0.0893(4) 0.5188(4) 1.1013(10) 0.0450(18) Uani 1 1 d . . . H13 H 0.0649 0.4781 1.1464 0.054 Uiso 1 1 calc R . . C14 C 0.1005(4) 0.5827(4) 1.1907(9) 0.0413(17) Uani 1 1 d . . . H14 H 0.0831 0.5854 1.2944 0.050 Uiso 1 1 calc R . . C15 C 0.1382(4) 0.6427(4) 1.1233(9) 0.0373(17) Uani 1 1 d . . . H15 H 0.1469 0.6856 1.1829 0.045 Uiso 1 1 calc R . . C16 C 0.1625(3) 0.6392(3) 0.9708(8) 0.0288(14) Uani 1 1 d . . . H16 H 0.1872 0.6799 0.9265 0.035 Uiso 1 1 calc R . . O17 O 0.2500 0.2500 0.5452(11) 0.0278(18) Uani 1 4 d S . . H17 H 0.2169 0.2778 0.5776 0.042 Uiso 0.25 1 calc PR . . O18 O 0.7234(2) 0.3125(2) 0.5997(6) 0.0342(11) Uani 1 1 d . . . O19A O 0.1477(5) 0.3117(5) 0.7517(11) 0.083(3) Uani 0.85 1 d P . . O19B O 0.0895(15) 0.3471(18) 0.759(4) 0.036(7) Uani 0.15 1 d P . . O20 O 0.2500 0.2500 0.9696(11) 0.035(2) Uani 1 4 d S . . O21 O 0.9724(11) 0.5436(11) 0.504(2) 0.041(5) Uiso 0.25 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 Cu1 0.0119(5) 0.0119(5) 0.0371(9) 0.000 0.000 0.000 S1 0.0131(8) 0.0131(8) 0.0373(17) 0.000 0.000 0.000 N1 0.014(2) 0.016(2) 0.037(3) -0.001(2) -0.001(2) -0.0007(19) C2 0.018(3) 0.018(3) 0.038(4) 0.001(2) 0.001(2) -0.001(2) C3 0.019(3) 0.015(3) 0.041(4) -0.001(2) -0.001(3) 0.002(2) C4 0.027(3) 0.017(3) 0.046(4) 0.001(3) 0.004(3) -0.005(2) C5 0.027(3) 0.021(3) 0.046(4) 0.003(3) 0.007(3) -0.002(2) C6 0.022(3) 0.020(3) 0.039(4) 0.001(3) 0.003(3) -0.002(2) N7 0.033(3) 0.011(2) 0.044(3) 0.002(2) 0.008(2) 0.001(2) C8 0.035(3) 0.016(3) 0.042(4) 0.000(3) -0.001(3) -0.002(2) O9 0.085(4) 0.020(2) 0.045(3) 0.000(2) 0.013(3) 0.005(2) N10 0.031(3) 0.016(2) 0.040(3) -0.001(2) 0.001(2) 0.001(2) C11 0.019(3) 0.019(3) 0.051(4) -0.003(3) -0.008(3) 0.002(2) C12 0.038(4) 0.026(3) 0.044(4) -0.005(3) 0.002(3) -0.001(3) C13 0.038(4) 0.029(4) 0.068(5) 0.008(3) -0.004(4) -0.006(3) C14 0.041(4) 0.041(4) 0.042(4) -0.001(3) -0.001(3) 0.009(3) C15 0.031(3) 0.024(3) 0.057(5) 0.001(3) -0.017(3) 0.003(3) C16 0.025(3) 0.022(3) 0.039(4) 0.000(3) -0.005(3) 0.003(2) O17 0.022(3) 0.022(3) 0.038(5) 0.000 0.000 0.000 O18 0.025(2) 0.024(2) 0.054(3) -0.011(2) 0.006(2) -0.0009(17) O19A 0.079(6) 0.074(6) 0.096(7) 0.005(5) 0.000(5) 0.004(5) O19B 0.019(14) 0.047(18) 0.043(17) -0.009(14) 0.000(12) 0.029(13) O20 0.032(3) 0.032(3) 0.043(5) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.046(5) 2 ? Cu1 N1 2.046(5) 4 ? Cu1 N1 2.046(5) 3 ? Cu1 N1 2.046(5) . ? Cu1 O17 2.310(9) . ? S1 O18 1.478(4) 8_656 ? S1 O18 1.478(4) 7_666 ? S1 O18 1.478(4) 2_655 ? S1 O18 1.478(4) . ? N1 C2 1.334(8) . ? N1 C6 1.351(8) . ? C2 C3 1.390(8) . ? C2 H2 0.9300 . ? C3 C4 1.382(9) . ? C3 N7 1.415(8) . ? C4 C5 1.369(9) . ? C4 H4 0.9300 . ? C5 C6 1.380(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N7 C8 1.348(9) . ? N7 H7 0.8600 . ? C8 O9 1.240(8) . ? C8 N10 1.360(8) . ? N10 C11 1.410(9) . ? N10 H10 0.8600 . ? C11 C12 1.384(9) . ? C11 C16 1.405(9) . ? C12 C13 1.373(11) . ? C12 H12 0.9300 . ? C13 C14 1.384(10) . ? C13 H13 0.9300 . ? C14 C15 1.389(10) . ? C14 H14 0.9300 . ? C15 C16 1.360(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? O17 H17 0.8200 . ? O19A O19B 1.22(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 Cu1 N1 89.948(9) 2 4 ? N1 Cu1 N1 89.948(10) 2 3 ? N1 Cu1 N1 176.5(3) 4 3 ? N1 Cu1 N1 176.5(3) 2 . ? N1 Cu1 N1 89.949(9) 4 . ? N1 Cu1 N1 89.947(9) 3 . ? N1 Cu1 O17 91.73(15) 2 . ? N1 Cu1 O17 91.73(15) 4 . ? N1 Cu1 O17 91.73(15) 3 . ? N1 Cu1 O17 91.73(15) . . ? O18 S1 O18 110.6(4) 8_656 7_666 ? O18 S1 O18 108.93(19) 8_656 2_655 ? O18 S1 O18 108.93(19) 7_666 2_655 ? O18 S1 O18 108.93(19) 8_656 . ? O18 S1 O18 108.93(19) 7_666 . ? O18 S1 O18 110.6(4) 2_655 . ? C2 N1 C6 118.8(5) . . ? C2 N1 Cu1 121.3(4) . . ? C6 N1 Cu1 119.8(4) . . ? N1 C2 C3 122.5(6) . . ? N1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? C4 C3 C2 117.9(6) . . ? C4 C3 N7 117.3(5) . . ? C2 C3 N7 124.8(6) . . ? C5 C4 C3 120.0(6) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.1(6) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N1 C6 C5 121.6(6) . . ? N1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 N7 C3 126.1(5) . . ? C8 N7 H7 116.9 . . ? C3 N7 H7 116.9 . . ? O9 C8 N7 123.6(6) . . ? O9 C8 N10 123.1(6) . . ? N7 C8 N10 113.3(5) . . ? C8 N10 C11 125.6(5) . . ? C8 N10 H10 117.2 . . ? C11 N10 H10 117.2 . . ? C12 C11 C16 119.0(6) . . ? C12 C11 N10 123.8(6) . . ? C16 C11 N10 117.1(6) . . ? C13 C12 C11 119.9(6) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 121.1(7) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 119.0(7) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 120.5(7) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 120.5(6) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? Cu1 O17 H17 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10 O18 0.86 1.98 2.827(7) 168.3 3 N7 H7 O18 0.86 2.19 2.982(6) 152.8 5_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.19 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.711 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.124 # _vrf_SHFSU01_y ; PROBLEM: The absolute value of parameter shift to su ratio > 0.20 Absolute value of parameter shift to su ratio 0.514 additional refinement cycles may be required. RESPONSE: We have done adequate additional rfinement cycle. ; _vrf_PLAT080_y ; PROBLEM: Maximum Shift/Error...... 0.51 RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT214_y ; PROBLEM: Atom O19B (Anion/Solvent)ADPmax/min Ratio 1.17 obalt RESPONSE: O19B is a part of a disordered O atom. ; _database_code_depnum_ccdc_archive 'CCDC 926132' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form # Attachment 'CP1.cif' data_05110gm #TrackingRef 'CP1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 Cu F10 N4 O7 S' _chemical_formula_weight 782.03 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 4.8692(8) _cell_length_b 47.735(8) _cell_length_c 6.2805(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.129(4) _cell_angle_gamma 90.00 _cell_volume 1459.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8203 _exptl_absorpt_correction_T_max 0.9635 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Smart Apex' _diffrn_measurement_method Phi-Omega _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5684 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.00 _reflns_number_total 2286 _reflns_number_gt 1945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart Apex' _computing_cell_refinement 'Bruker Smart Apex' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material Shelxl-97 _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^)+(0.1060P)^2^+4.2956P] 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 2286 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0949 _refine_ls_wR_factor_ref 0.2359 _refine_ls_wR_factor_gt 0.2200 _refine_ls_goodness_of_fit_ref 1.261 _refine_ls_restrained_S_all 1.261 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.9089(3) 0.2500 0.5075(2) 0.0177(5) Uani 1 2 d S . . S1 S 1.4665(6) 0.2500 0.8202(4) 0.0269(8) Uani 1 2 d S . . F1 F 0.6519(15) 0.07904(12) 0.2964(11) 0.0677(19) Uani 1 1 d . . . F2 F 0.8394(18) 0.03006(16) 0.1631(16) 0.112(3) Uani 1 1 d . . . F3 F 0.684(2) 0.00918(15) -0.2150(17) 0.123(3) Uani 1 1 d . . . F4 F 0.311(2) 0.03759(17) -0.4641(14) 0.119(3) Uani 1 1 d . . . F5 F 0.1323(16) 0.08762(15) -0.3379(12) 0.085(2) Uani 1 1 d . . . N1 N 0.8413(13) 0.20814(15) 0.4977(10) 0.0273(17) Uani 1 1 d . . . C2 C 0.941(2) 0.19117(19) 0.6509(15) 0.039(2) Uani 1 1 d . . . H2 H 1.0632 0.1982 0.7536 0.047 Uiso 1 1 calc R . . C3 C 0.866(2) 0.1636(2) 0.6567(16) 0.050(3) Uani 1 1 d . . . H3 H 0.9303 0.1524 0.7677 0.060 Uiso 1 1 calc R . . C4 C 0.700(2) 0.1525(2) 0.5066(16) 0.049(3) Uani 1 1 d . . . H4 H 0.6592 0.1334 0.5090 0.059 Uiso 1 1 calc R . . C5 C 0.5913(18) 0.16952(18) 0.3473(15) 0.035(2) Uani 1 1 d . . . C6 C 0.6798(18) 0.19724(17) 0.3489(13) 0.029(2) Uani 1 1 d . . . H6 H 0.6211 0.2088 0.2379 0.035 Uiso 1 1 calc R . . C7 C 0.391(2) 0.15971(19) 0.1792(17) 0.046(3) Uani 1 1 d . . . H7A H 0.2079 0.1593 0.2376 0.055 Uiso 1 1 calc R . . H7B H 0.3893 0.1728 0.0613 0.055 Uiso 1 1 calc R . . N8 N 0.4609(13) 0.13186(14) 0.1012(12) 0.0341(18) Uani 1 1 d . . . H8 H 0.6310 0.1276 0.0859 0.041 Uiso 1 1 calc R . . C9 C 0.2689(16) 0.11276(17) 0.0529(15) 0.031(2) Uani 1 1 d . . . O10 O 0.0285(12) 0.11678(14) 0.0573(12) 0.051(2) Uani 1 1 d . . . C11 C 0.3849(18) 0.08492(18) -0.0175(14) 0.033(2) Uani 1 1 d . . . C12 C 0.565(2) 0.0701(2) 0.1069(17) 0.042(2) Uani 1 1 d . . . C13 C 0.671(3) 0.0444(2) 0.039(2) 0.065(3) Uani 1 1 d . . . C14 C 0.584(3) 0.0339(2) -0.149(3) 0.075(4) Uani 1 1 d . . . C15 C 0.401(3) 0.0479(2) -0.280(2) 0.067(4) Uani 1 1 d . . . C16 C 0.297(2) 0.0737(2) -0.2093(16) 0.046(3) Uani 1 1 d . . . O17 O 1.3423(16) 0.2500 0.6053(12) 0.032(2) Uani 1 2 d S . . O18 O 1.3910(15) 0.22517(19) 0.9362(13) 0.074(3) Uani 1 1 d . . . O19 O 1.7749(14) 0.2500 0.8004(12) 0.031(2) Uani 1 2 d S . . O20 O 0.9965(18) 0.2500 0.2040(13) 0.041(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0143(7) 0.0260(8) 0.0130(7) 0.000 0.0015(5) 0.000 S1 0.0162(16) 0.0473(19) 0.0172(15) 0.000 0.0000(12) 0.000 F1 0.087(5) 0.044(4) 0.071(4) 0.011(3) -0.028(4) 0.002(3) F2 0.098(6) 0.064(5) 0.173(9) 0.008(5) -0.036(6) 0.043(5) F3 0.146(8) 0.045(4) 0.177(9) -0.039(5) 0.020(7) 0.025(5) F4 0.188(10) 0.075(5) 0.093(6) -0.054(5) 0.007(6) -0.024(6) F5 0.102(6) 0.072(5) 0.081(5) -0.013(4) -0.043(5) 0.008(4) N1 0.018(4) 0.037(4) 0.027(4) 0.002(3) -0.007(3) -0.001(3) C2 0.047(6) 0.038(6) 0.032(5) 0.004(4) -0.008(4) -0.002(5) C3 0.064(7) 0.043(6) 0.043(6) 0.013(5) -0.011(6) 0.003(5) C4 0.064(7) 0.030(5) 0.052(7) 0.009(5) -0.009(6) -0.005(5) C5 0.036(5) 0.026(5) 0.043(6) -0.002(4) 0.000(5) 0.006(4) C6 0.037(5) 0.025(5) 0.025(5) 0.002(4) 0.001(4) 0.009(4) C7 0.046(6) 0.026(5) 0.066(7) -0.007(5) -0.013(6) 0.002(4) N8 0.011(3) 0.033(4) 0.058(5) -0.006(4) 0.002(3) 0.008(3) C9 0.014(4) 0.027(5) 0.051(6) -0.002(4) -0.003(4) -0.001(4) O10 0.017(3) 0.045(4) 0.091(6) -0.015(4) -0.005(3) 0.005(3) C11 0.029(5) 0.028(5) 0.041(5) 0.006(4) -0.004(4) -0.006(4) C12 0.037(6) 0.030(5) 0.060(7) 0.000(5) -0.001(5) -0.001(4) C13 0.069(8) 0.039(6) 0.088(10) 0.007(7) 0.005(7) 0.021(6) C14 0.097(11) 0.031(6) 0.099(11) -0.019(7) 0.019(9) 0.010(7) C15 0.092(10) 0.044(7) 0.065(8) -0.014(6) 0.006(7) -0.018(7) C16 0.043(6) 0.046(6) 0.048(6) -0.004(5) -0.003(5) -0.002(5) O17 0.024(5) 0.053(6) 0.020(4) 0.000 0.003(4) 0.000 O18 0.049(5) 0.107(7) 0.064(5) 0.062(5) -0.017(4) -0.025(4) O19 0.002(4) 0.061(6) 0.030(5) 0.000 -0.001(3) 0.000 O20 0.037(5) 0.064(6) 0.023(5) 0.000 0.007(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O20 1.961(8) . ? Cu1 O19 1.964(8) 1_455 ? Cu1 N1 2.026(7) 4_565 ? Cu1 N1 2.026(7) . ? Cu1 O17 2.186(8) . ? S1 O18 1.443(7) 4_565 ? S1 O18 1.443(7) . ? S1 O17 1.468(8) . ? S1 O19 1.509(8) . ? F1 C12 1.326(12) . ? F2 C13 1.311(13) . ? F3 C14 1.347(13) . ? F4 C15 1.323(14) . ? F5 C16 1.308(11) . ? N1 C6 1.316(10) . ? N1 C2 1.342(11) . ? C2 C3 1.365(13) . ? C2 H2 0.9300 . ? C3 C4 1.338(14) . ? C3 H3 0.9300 . ? C4 C5 1.388(13) . ? C4 H4 0.9300 . ? C5 C6 1.392(12) . ? C5 C7 1.499(13) . ? C6 H6 0.9300 . ? C7 N8 1.460(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N8 C9 1.336(10) . ? N8 H8 0.8600 . ? C9 O10 1.187(10) . ? C9 C11 1.513(12) . ? C11 C12 1.363(13) . ? C11 C16 1.379(13) . ? C12 C13 1.399(14) . ? C13 C14 1.347(18) . ? C14 C15 1.369(19) . ? C15 C16 1.410(16) . ? O19 Cu1 1.964(8) 1_655 ? 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 O20 Cu1 O19 173.2(3) . 1_455 ? O20 Cu1 N1 90.5(2) . 4_565 ? O19 Cu1 N1 88.4(2) 1_455 4_565 ? O20 Cu1 N1 90.5(2) . . ? O19 Cu1 N1 88.4(2) 1_455 . ? N1 Cu1 N1 161.1(4) 4_565 . ? O20 Cu1 O17 92.6(3) . . ? O19 Cu1 O17 94.2(3) 1_455 . ? N1 Cu1 O17 99.43(18) 4_565 . ? N1 Cu1 O17 99.43(18) . . ? O18 S1 O18 110.5(8) 4_565 . ? O18 S1 O17 111.1(4) 4_565 . ? O18 S1 O17 111.1(4) . . ? O18 S1 O19 107.8(4) 4_565 . ? O18 S1 O19 107.8(4) . . ? O17 S1 O19 108.5(5) . . ? C6 N1 C2 118.3(8) . . ? C6 N1 Cu1 120.4(5) . . ? C2 N1 Cu1 121.1(6) . . ? N1 C2 C3 120.3(8) . . ? N1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 121.6(9) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.3(9) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 116.0(8) . . ? C4 C5 C7 124.0(8) . . ? C6 C5 C7 120.0(8) . . ? N1 C6 C5 124.2(8) . . ? N1 C6 H6 117.9 . . ? C5 C6 H6 117.9 . . ? N8 C7 C5 111.6(7) . . ? N8 C7 H7A 109.3 . . ? C5 C7 H7A 109.3 . . ? N8 C7 H7B 109.3 . . ? C5 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9 N8 C7 122.0(7) . . ? C9 N8 H8 119.0 . . ? C7 N8 H8 119.0 . . ? O10 C9 N8 124.8(8) . . ? O10 C9 C11 121.5(8) . . ? N8 C9 C11 113.7(7) . . ? C12 C11 C16 119.0(9) . . ? C12 C11 C9 122.0(8) . . ? C16 C11 C9 119.0(8) . . ? F1 C12 C11 122.4(9) . . ? F1 C12 C13 116.3(9) . . ? C11 C12 C13 121.3(10) . . ? F2 C13 C14 120.7(11) . . ? F2 C13 C12 120.5(12) . . ? C14 C13 C12 118.7(11) . . ? C13 C14 F3 118.9(13) . . ? C13 C14 C15 122.6(11) . . ? F3 C14 C15 118.5(13) . . ? F4 C15 C14 123.1(12) . . ? F4 C15 C16 118.9(12) . . ? C14 C15 C16 117.9(11) . . ? F5 C16 C11 121.2(9) . . ? F5 C16 C15 118.0(10) . . ? C11 C16 C15 120.5(10) . . ? S1 O17 Cu1 129.5(5) . . ? S1 O19 Cu1 115.3(4) . 1_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 O10 0.86 2.01 2.874(9) 178.2 1_655 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.924 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.146 # _vrf_PLAT213_05110gm ; PROBLEM: Atom O19 has ADP max/min Ratio....5.60 prola RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _database_code_depnum_ccdc_archive 'CCDC 926133' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form # Attachment 'CP2.cif' data_sbo753h_0m #TrackingRef 'CP2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H34 Cu F26 N8 O7 Si' _chemical_formula_weight 1468.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.460(15) _cell_length_b 8.054(3) _cell_length_c 18.087(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.341(6) _cell_angle_gamma 90.00 _cell_volume 6120(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2940 _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8699 _exptl_absorpt_correction_T_max 0.9554 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean 3 _diffrn_reflns_number 12591 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 23.99 _reflns_number_total 4655 _reflns_number_gt 2760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.4' _computing_publication_material Shelxl-97 _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4655 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1386 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.2937 _refine_ls_wR_factor_gt 0.2497 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.53913(13) 0.7500 0.0394(4) Uani 1 2 d S . . Si1 Si 0.5000 0.0462(3) 0.7500 0.0427(7) Uani 1 2 d S . . F1 F 0.65726(19) 0.4240(10) 0.8521(5) 0.139(3) Uani 1 1 d . . . F2 F 0.7033(2) 0.4600(18) 0.7706(6) 0.204(5) Uani 1 1 d . . . F3 F 0.7317(2) 0.7538(18) 0.7560(6) 0.211(5) Uani 1 1 d . . . F4 F 0.7120(2) 1.0181(15) 0.8250(7) 0.193(5) Uani 1 1 d . . . F5 F 0.66665(16) 0.9914(10) 0.9131(5) 0.137(3) Uani 1 1 d . . . F6 F 0.33352(17) 1.3004(9) 0.8626(4) 0.117(2) Uani 1 1 d . . . F7 F 0.2769(2) 1.3424(13) 0.9111(5) 0.175(4) Uani 1 1 d . . . F8 F 0.24411(17) 1.0826(16) 0.9484(5) 0.197(5) Uani 1 1 d . . . F9 F 0.26781(18) 0.7721(14) 0.9359(5) 0.175(4) Uani 1 1 d . . . F10 F 0.32370(15) 0.7263(9) 0.8879(4) 0.119(2) Uani 1 1 d . . . F11 F 0.5000 0.2549(6) 0.7500 0.0593(16) Uani 1 2 d S . . F12 F 0.46201(13) 0.0446(6) 0.7161(5) 0.129(3) Uani 1 1 d . . . F13 F 0.5000 -0.1630(6) 0.7500 0.0561(15) Uani 1 2 d S . . F14 F 0.4898(2) 0.0442(6) 0.8343(3) 0.126(3) Uani 1 1 d . . . N1 N 0.52298(12) 0.5399(6) 0.8558(3) 0.0402(13) Uani 1 1 d . . . C2 C 0.51803(18) 0.4163(9) 0.9025(4) 0.0522(19) Uani 1 1 d . . . H2 H 0.5034 0.3337 0.8859 0.063 Uiso 1 1 calc R . . C3 C 0.5339(2) 0.4081(11) 0.9737(5) 0.082(3) Uani 1 1 d . . . H3 H 0.5295 0.3238 1.0059 0.098 Uiso 1 1 calc R . . C4 C 0.5567(2) 0.5284(12) 0.9974(5) 0.082(3) Uani 1 1 d . . . H4 H 0.5682 0.5228 1.0452 0.098 Uiso 1 1 calc R . . C5 C 0.56225(18) 0.6554(9) 0.9500(4) 0.056(2) Uani 1 1 d . . . C6 C 0.54419(17) 0.6574(8) 0.8805(4) 0.0474(18) Uani 1 1 d . . . H6 H 0.5469 0.7456 0.8489 0.057 Uiso 1 1 calc R . . C7 C 0.5858(2) 0.7897(11) 0.9736(5) 0.076(3) Uani 1 1 d . . . H7A H 0.5748 0.8956 0.9710 0.091 Uiso 1 1 calc R . . H7B H 0.5951 0.7713 1.0251 0.091 Uiso 1 1 calc R . . N8 N 0.61113(18) 0.7977(9) 0.9275(4) 0.073(2) Uani 1 1 d . . . H8 H 0.6110 0.8769 0.8956 0.088 Uiso 1 1 calc R . . C9 C 0.6348(3) 0.6842(14) 0.9334(6) 0.085(3) Uani 1 1 d . . . O10 O 0.63612(19) 0.5704(9) 0.9797(5) 0.108(3) Uani 1 1 d . . . C11 C 0.6600(2) 0.7102(17) 0.8847(6) 0.089(3) Uani 1 1 d . . . C12 C 0.6703(3) 0.578(2) 0.8474(8) 0.106(4) Uani 1 1 d . . . C13 C 0.6937(5) 0.593(3) 0.8045(10) 0.132(5) Uani 1 1 d . . . C14 C 0.7067(4) 0.741(4) 0.7985(10) 0.136(6) Uani 1 1 d . . . C15 C 0.6977(4) 0.873(3) 0.8315(12) 0.135(6) Uani 1 1 d . . . C16 C 0.6748(3) 0.8547(18) 0.8751(8) 0.105(4) Uani 1 1 d . . . N17 N 0.45755(13) 0.5495(6) 0.7868(3) 0.0447(14) Uani 1 1 d . . . C18 C 0.44993(17) 0.6892(8) 0.8206(4) 0.0467(18) Uani 1 1 d . . . H18 H 0.4659 0.7673 0.8336 0.056 Uiso 1 1 calc R . . C19 C 0.41973(16) 0.7248(8) 0.8377(4) 0.0441(17) Uani 1 1 d . . . C20 C 0.39652(18) 0.6055(10) 0.8201(5) 0.058(2) Uani 1 1 d . . . H20 H 0.3760 0.6251 0.8301 0.070 Uiso 1 1 calc R . . C21 C 0.40368(18) 0.4555(10) 0.7874(4) 0.060(2) Uani 1 1 d . . . H21 H 0.3884 0.3725 0.7774 0.072 Uiso 1 1 calc R . . C22 C 0.43455(18) 0.4345(9) 0.7702(4) 0.056(2) Uani 1 1 d . . . H22 H 0.4394 0.3373 0.7464 0.067 Uiso 1 1 calc R . . C23 C 0.41482(17) 0.8881(9) 0.8753(4) 0.056(2) Uani 1 1 d . . . H23A H 0.4296 0.8939 0.9215 0.067 Uiso 1 1 calc R . . H23B H 0.4202 0.9773 0.8433 0.067 Uiso 1 1 calc R . . N24 N 0.38291(14) 0.9160(7) 0.8922(4) 0.0562(17) Uani 1 1 d . . . H24 H 0.3782 0.8800 0.9340 0.067 Uiso 1 1 calc R . . C25 C 0.36096(19) 0.9930(11) 0.8471(5) 0.061(2) Uani 1 1 d . . . O26 O 0.36501(15) 1.0465(10) 0.7836(4) 0.093(2) Uani 1 1 d . . . C27 C 0.3305(2) 1.0148(14) 0.8747(5) 0.070(2) Uani 1 1 d . . . C28 C 0.3171(3) 1.1662(18) 0.8804(6) 0.095(3) Uani 1 1 d . . . C29 C 0.2895(4) 1.199(2) 0.9046(8) 0.117(5) Uani 1 1 d . . . C30 C 0.2726(4) 1.075(3) 0.9238(9) 0.137(7) Uani 1 1 d . . . C31 C 0.2834(3) 0.915(3) 0.9189(7) 0.139(6) Uani 1 1 d . . . C32 C 0.3134(3) 0.8901(19) 0.8937(6) 0.097(3) Uani 1 1 d . . . O33 O 0.40088(14) 0.0738(8) 0.6715(3) 0.0794(18) Uani 1 1 d . . . O34 O 0.3836(2) 0.7629(10) 0.0291(4) 0.045(2) 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 Cu1 0.0488(7) 0.0258(6) 0.0434(7) 0.000 0.0061(5) 0.000 Si1 0.0505(15) 0.0193(13) 0.0596(17) 0.000 0.0119(13) 0.000 F1 0.145(6) 0.114(6) 0.156(7) -0.045(5) 0.017(5) -0.015(5) F2 0.152(8) 0.284(15) 0.175(10) -0.059(9) 0.020(7) 0.004(8) F3 0.111(6) 0.338(17) 0.189(9) 0.057(10) 0.040(6) 0.028(8) F4 0.113(6) 0.211(11) 0.255(12) 0.096(9) 0.026(7) -0.033(7) F5 0.103(5) 0.082(5) 0.222(9) 0.019(5) 0.006(5) -0.026(4) F6 0.126(5) 0.106(5) 0.119(5) -0.003(4) 0.020(4) 0.040(4) F7 0.158(7) 0.217(9) 0.155(7) -0.032(7) 0.034(6) 0.123(7) F8 0.082(5) 0.374(16) 0.145(7) -0.028(8) 0.052(5) 0.066(7) F9 0.111(6) 0.247(11) 0.184(9) 0.009(8) 0.071(6) -0.040(7) F10 0.103(4) 0.109(5) 0.155(6) 0.004(5) 0.055(4) -0.024(4) F11 0.082(4) 0.017(3) 0.080(4) 0.000 0.018(3) 0.000 F12 0.067(3) 0.056(3) 0.248(8) -0.020(4) -0.029(4) 0.010(3) F13 0.084(4) 0.019(3) 0.071(4) 0.000 0.031(3) 0.000 F14 0.270(9) 0.034(3) 0.092(4) -0.009(3) 0.091(5) -0.021(4) N1 0.053(3) 0.029(3) 0.040(3) 0.005(3) 0.009(2) 0.002(3) C2 0.066(5) 0.037(4) 0.055(5) 0.006(3) 0.016(4) -0.011(3) C3 0.122(8) 0.062(6) 0.056(5) 0.021(4) -0.005(5) -0.025(5) C4 0.115(8) 0.074(6) 0.048(5) 0.018(5) -0.013(5) -0.017(6) C5 0.067(5) 0.047(4) 0.052(5) 0.000(4) 0.005(4) -0.003(4) C6 0.071(5) 0.028(4) 0.045(4) 0.002(3) 0.015(4) -0.008(3) C7 0.087(6) 0.064(6) 0.070(6) -0.009(5) -0.011(5) -0.010(5) N8 0.082(5) 0.054(5) 0.078(5) 0.002(4) -0.006(4) -0.014(4) C9 0.089(7) 0.075(7) 0.081(7) 0.011(6) -0.021(6) -0.010(6) O10 0.138(6) 0.066(4) 0.112(6) 0.023(4) -0.004(5) 0.003(4) C11 0.068(6) 0.109(10) 0.083(7) 0.005(7) -0.006(6) 0.003(7) C12 0.091(9) 0.139(14) 0.085(8) 0.000(9) -0.001(7) -0.003(9) C13 0.148(15) 0.140(15) 0.105(11) -0.033(11) 0.007(11) 0.013(13) C14 0.083(10) 0.21(2) 0.111(12) 0.023(14) 0.011(9) 0.000(14) C15 0.088(11) 0.152(17) 0.159(15) 0.032(14) 0.002(10) -0.014(11) C16 0.083(8) 0.099(10) 0.128(10) 0.024(8) -0.005(7) -0.022(8) N17 0.058(3) 0.022(3) 0.054(3) 0.002(3) 0.006(3) -0.001(3) C18 0.066(5) 0.027(4) 0.045(4) 0.001(3) 0.004(3) -0.001(3) C19 0.052(4) 0.029(4) 0.050(4) -0.002(3) 0.006(3) 0.004(3) C20 0.050(4) 0.049(5) 0.076(5) -0.014(4) 0.011(4) 0.004(4) C21 0.055(5) 0.054(5) 0.071(5) -0.017(4) 0.011(4) -0.006(4) C22 0.067(5) 0.034(4) 0.066(5) -0.011(3) 0.006(4) -0.007(3) C23 0.060(5) 0.042(4) 0.067(5) -0.003(4) 0.017(4) -0.002(4) N24 0.061(4) 0.044(4) 0.065(4) -0.009(3) 0.016(3) 0.010(3) C25 0.056(5) 0.064(5) 0.063(5) -0.007(4) 0.011(4) 0.008(4) O26 0.077(4) 0.119(6) 0.087(5) 0.013(4) 0.022(4) 0.017(4) C27 0.052(5) 0.100(8) 0.061(5) 0.001(5) 0.021(4) 0.005(5) C28 0.077(7) 0.117(10) 0.095(8) 0.013(7) 0.024(6) 0.026(7) C29 0.098(11) 0.155(15) 0.101(10) -0.013(9) 0.027(8) 0.046(10) C30 0.082(10) 0.23(2) 0.100(10) -0.010(12) 0.024(8) 0.067(12) C31 0.068(8) 0.27(2) 0.089(9) 0.015(11) 0.025(7) -0.041(11) C32 0.072(7) 0.126(11) 0.096(8) -0.012(8) 0.024(6) 0.016(7) O33 0.080(4) 0.087(4) 0.071(4) -0.016(3) 0.008(3) -0.003(3) O34 0.097(7) 0.025(4) 0.018(4) 0.006(4) 0.027(4) 0.000(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 Cu1 N17 2.011(6) . ? Cu1 N17 2.011(6) 2_656 ? Cu1 N1 2.018(5) 2_656 ? Cu1 N1 2.018(5) . ? Cu1 F11 2.289(5) . ? Cu1 F13 2.399(5) 1_565 ? Si1 F12 1.640(5) 2_656 ? Si1 F12 1.640(5) . ? Si1 F14 1.644(6) 2_656 ? Si1 F14 1.644(6) . ? Si1 F11 1.680(6) . ? Si1 F13 1.685(6) . ? F1 C12 1.370(16) . ? F2 C13 1.326(18) . ? F3 C14 1.400(17) . ? F4 C15 1.332(19) . ? F5 C16 1.367(16) . ? F6 C28 1.351(14) . ? F7 C29 1.288(16) . ? F8 C30 1.350(17) . ? F9 C31 1.380(19) . ? F10 C32 1.398(14) . ? F13 Cu1 2.399(5) 1_545 ? N1 C6 1.338(8) . ? N1 C2 1.342(8) . ? C2 C3 1.366(11) . ? C2 H2 0.9300 . ? C3 C4 1.394(12) . ? C3 H3 0.9300 . ? C4 C5 1.376(11) . ? C4 H4 0.9300 . ? C5 C6 1.375(9) . ? C5 C7 1.492(11) . ? C6 H6 0.9300 . ? C7 N8 1.455(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N8 C9 1.353(12) . ? N8 H8 0.8600 . ? C9 O10 1.237(11) . ? C9 C11 1.494(15) . ? C11 C16 1.345(16) . ? C11 C12 1.365(17) . ? C12 C13 1.35(2) . ? C13 C14 1.32(2) . ? C14 C15 1.31(2) . ? C15 C16 1.35(2) . ? N17 C18 1.343(8) . ? N17 C22 1.348(9) . ? C18 C19 1.392(10) . ? C18 H18 0.9300 . ? C19 C20 1.380(10) . ? C19 C23 1.509(10) . ? C20 C21 1.398(11) . ? C20 H20 0.9300 . ? C21 C22 1.401(11) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 N24 1.449(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? N24 C25 1.303(10) . ? N24 H24 0.8600 . ? C25 O26 1.261(10) . ? C25 C27 1.462(12) . ? C27 C32 1.314(16) . ? C27 C28 1.357(15) . ? C28 C29 1.332(17) . ? C29 C30 1.31(2) . ? C30 C31 1.38(2) . ? C31 C32 1.429(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 N17 Cu1 N17 175.2(3) . 2_656 ? N17 Cu1 N1 88.9(2) . 2_656 ? N17 Cu1 N1 91.1(2) 2_656 2_656 ? N17 Cu1 N1 91.1(2) . . ? N17 Cu1 N1 88.9(2) 2_656 . ? N1 Cu1 N1 179.7(3) 2_656 . ? N17 Cu1 F11 92.38(15) . . ? N17 Cu1 F11 92.38(15) 2_656 . ? N1 Cu1 F11 90.17(15) 2_656 . ? N1 Cu1 F11 90.17(15) . . ? N17 Cu1 F13 87.62(15) . 1_565 ? N17 Cu1 F13 87.62(15) 2_656 1_565 ? N1 Cu1 F13 89.83(15) 2_656 1_565 ? N1 Cu1 F13 89.83(15) . 1_565 ? F11 Cu1 F13 180.000(2) . 1_565 ? F12 Si1 F12 179.1(4) 2_656 . ? F12 Si1 F14 88.3(4) 2_656 2_656 ? F12 Si1 F14 91.7(4) . 2_656 ? F12 Si1 F14 91.7(4) 2_656 . ? F12 Si1 F14 88.3(4) . . ? F14 Si1 F14 178.9(4) 2_656 . ? F12 Si1 F11 90.5(2) 2_656 . ? F12 Si1 F11 90.5(2) . . ? F14 Si1 F11 90.56(19) 2_656 . ? F14 Si1 F11 90.56(19) . . ? F12 Si1 F13 89.5(2) 2_656 . ? F12 Si1 F13 89.5(2) . . ? F14 Si1 F13 89.44(19) 2_656 . ? F14 Si1 F13 89.44(19) . . ? F11 Si1 F13 180.000(2) . . ? Si1 F11 Cu1 180.000(1) . . ? Si1 F13 Cu1 180.000(1) . 1_545 ? C6 N1 C2 118.2(6) . . ? C6 N1 Cu1 121.9(4) . . ? C2 N1 Cu1 119.8(5) . . ? N1 C2 C3 122.0(7) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C2 C3 C4 118.8(8) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 120.0(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 117.1(7) . . ? C6 C5 C7 120.9(7) . . ? C4 C5 C7 122.0(7) . . ? N1 C6 C5 123.8(6) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? N8 C7 C5 112.9(7) . . ? N8 C7 H7A 109.0 . . ? C5 C7 H7A 109.0 . . ? N8 C7 H7B 109.0 . . ? C5 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 N8 C7 121.9(8) . . ? C9 N8 H8 119.0 . . ? C7 N8 H8 119.0 . . ? O10 C9 N8 120.9(11) . . ? O10 C9 C11 122.6(11) . . ? N8 C9 C11 116.4(10) . . ? C16 C11 C12 114.8(14) . . ? C16 C11 C9 125.7(14) . . ? C12 C11 C9 119.4(12) . . ? C13 C12 C11 122.2(15) . . ? C13 C12 F1 117.0(17) . . ? C11 C12 F1 120.8(14) . . ? C14 C13 F2 122(2) . . ? C14 C13 C12 118.4(18) . . ? F2 C13 C12 120(2) . . ? C15 C14 C13 122.8(19) . . ? C15 C14 F3 119(2) . . ? C13 C14 F3 118(3) . . ? C14 C15 F4 120(2) . . ? C14 C15 C16 117.7(19) . . ? F4 C15 C16 122(2) . . ? C11 C16 C15 124.0(17) . . ? C11 C16 F5 118.4(15) . . ? C15 C16 F5 117.6(15) . . ? C18 N17 C22 117.5(6) . . ? C18 N17 Cu1 118.2(5) . . ? C22 N17 Cu1 123.6(5) . . ? N17 C18 C19 124.4(6) . . ? N17 C18 H18 117.8 . . ? C19 C18 H18 117.8 . . ? C20 C19 C18 117.1(6) . . ? C20 C19 C23 124.7(7) . . ? C18 C19 C23 118.1(6) . . ? C19 C20 C21 120.5(7) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 117.8(7) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? N17 C22 C21 122.6(7) . . ? N17 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? N24 C23 C19 115.1(6) . . ? N24 C23 H23A 108.5 . . ? C19 C23 H23A 108.5 . . ? N24 C23 H23B 108.5 . . ? C19 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C25 N24 C23 123.2(7) . . ? C25 N24 H24 118.4 . . ? C23 N24 H24 118.4 . . ? O26 C25 N24 123.6(8) . . ? O26 C25 C27 120.9(8) . . ? N24 C25 C27 115.5(8) . . ? C32 C27 C28 114.3(10) . . ? C32 C27 C25 123.2(10) . . ? C28 C27 C25 122.5(11) . . ? C29 C28 F6 115.5(13) . . ? C29 C28 C27 126.9(14) . . ? F6 C28 C27 117.6(10) . . ? F7 C29 C30 114.2(16) . . ? F7 C29 C28 127.0(18) . . ? C30 C29 C28 118.8(16) . . ? C29 C30 F8 127.4(19) . . ? C29 C30 C31 119.9(15) . . ? F8 C30 C31 113(2) . . ? C30 C31 F9 126.2(15) . . ? C30 C31 C32 118.0(16) . . ? F9 C31 C32 115.8(18) . . ? C27 C32 F10 120.7(10) . . ? C27 C32 C31 122.1(14) . . ? F10 C32 C31 117.2(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 O33 0.86 2.02 2.854(9) 164.5 2_666 N24 H24 O34 0.86 1.95 2.763(10) 158.2 1_556 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.036 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.116 # _vrf_CHEMW03_sbo753h_0m ; PROBLEM: The ratio of given/expected molecular weight as calculated from the atom site data lies outside the range 0.90 <> 1.10 RESPONSE: We have used SQUEEZE to remove the contributions of disordered solvent molecules (which we could not modelled) within the crystal lattice. Therefore, the contribution of disordered solvent molecules removed by the SQUEEZE process are included in the overall formula, formula weight, density, F(000) etc. The output of the PLATON (generated as .sqf file) is also appended to the bottom of the CIF. ; _vrf_PLAT043_sbo753h_0m ; PROBLEM: Check Reported Molecular Weight ...... 1692.15 RESPONSE: We have used SQUEEZE to remove the contributions of disordered solvent molecules (which we could not modelled) within the crystal lattice. Therefore, the contribution of disordered solvent molecules removed by the SQUEEZE process are included in the overall formula, formula weight, density, F(000) etc. The output of the PLATON (generated as .sqf file) is also appended to the bottom of the CIF. ; _vrf_PLAT051_sbo753h_0m ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by 42.70 % RESPONSE:RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The situation did not improve even after recrystallisation and fresh data collection. ; _vrf_PLAT242_sbo753h_0m ; PROBLEM: Check low Ueq as compared to neighbors for Si1 RESPONSE:This happens because the atom is attached with highly fluctional atom, these atoms show high thermal parameter. ; _vrf_PLAT306_sbo753h_0m ; PROBLEM:Isolated Oxygen Atom (H-atoms Missing ?) ....... O33 RESPONSE:We are unable to locate hydrogen atom associated with solvent water molecule containing O33. ; # end Validation Reply Form # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 51 10 ' ' 2 0.500 0.000 1.000 51 10 ' ' 3 0.000 0.500 0.500 51 10 ' ' 4 0.000 0.500 1.000 51 10 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 926134'