# Electronic Supplementary Material (ESI) for Chemical Communications # 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 # Attachment 'compound4.cif' data_import #TrackingRef 'compound4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H48 Cl6 Cu2 F6 N4 O6 P2 S2' _chemical_formula_sum 'C53 H48 Cl6 Cu2 F6 N4 O6 P2 S2' _chemical_formula_weight 1416.79 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.724(4) _cell_length_b 14.984(4) _cell_length_c 26.752(7) _cell_angle_alpha 90 _cell_angle_beta 98.041(2) _cell_angle_gamma 90 _cell_volume 5844(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 20.76 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method none _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 38234 _diffrn_reflns_av_R_equivalents 0.1176 _diffrn_reflns_av_sigmaI/netI 0.1752 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.41 _reflns_number_total 11632 _reflns_number_gt 6223 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1097P)^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 11632 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1670 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2366 _refine_ls_wR_factor_gt 0.1883 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.82424(6) 0.20582(5) 0.09540(3) 0.0235(2) Uani 1 1 d . . . Cu2 Cu 0.82947(6) 0.13987(5) 0.18253(3) 0.0247(2) Uani 1 1 d . . . P1 P 0.89117(13) 0.06761(11) 0.11875(6) 0.0216(4) Uani 1 1 d . . . P2 P 0.88955(13) 0.33143(11) 0.12692(6) 0.0224(4) Uani 1 1 d . . . N1 N 0.8524(4) 0.1738(3) 0.02575(19) 0.0235(13) Uani 1 1 d . . . N2 N 0.8881(4) 0.0404(4) 0.2283(2) 0.0263(14) Uani 1 1 d . . . N3 N 0.8011(4) 0.2466(3) 0.2242(2) 0.0232(13) Uani 1 1 d . . . N4 N 0.9470(4) 0.3688(4) 0.0303(2) 0.0346(15) Uani 1 1 d . . . S1 S 0.62884(13) 0.16890(12) 0.12474(7) 0.0311(5) Uani 1 1 d . . . O1 O 0.5889(3) 0.2448(3) 0.14650(19) 0.0415(14) Uani 1 1 d . . . O2 O 0.6782(3) 0.1901(3) 0.08224(17) 0.0309(12) Uani 1 1 d . . . O3 O 0.6749(3) 0.1044(3) 0.16053(17) 0.0326(12) Uani 1 1 d . . . C1 C 0.9727(5) 0.0938(4) 0.0749(2) 0.0230(16) Uani 1 1 d . . . C2 C 1.0588(5) 0.0748(4) 0.0956(2) 0.0197(15) Uani 1 1 d . . . C3 C 1.1444(5) 0.0964(5) 0.0720(3) 0.0320(18) Uani 1 1 d . . . H3A H 1.1361 0.1530 0.0543 0.038 Uiso 1 1 calc R . . H3B H 1.1536 0.0506 0.0475 0.038 Uiso 1 1 calc R . . C4 C 1.2292(5) 0.1015(5) 0.1121(3) 0.0372(19) Uani 1 1 d . . . H4A H 1.2838 0.1077 0.0959 0.045 Uiso 1 1 calc R . . H4B H 1.2249 0.1534 0.1333 0.045 Uiso 1 1 calc R . . C5 C 1.2365(5) 0.0183(5) 0.1442(3) 0.0328(18) Uani 1 1 d . . . H5A H 1.2947 0.0181 0.1662 0.039 Uiso 1 1 calc R . . H5B H 1.2343 -0.0339 0.1226 0.039 Uiso 1 1 calc R . . C6 C 1.1577(5) 0.0146(5) 0.1759(3) 0.0354(19) Uani 1 1 d . . . H6A H 1.1559 -0.0444 0.1907 0.042 Uiso 1 1 calc R . . H6B H 1.1695 0.0573 0.2033 0.042 Uiso 1 1 calc R . . C7 C 1.0658(5) 0.0346(4) 0.1459(2) 0.0212(15) Uani 1 1 d . . . C8 C 0.9836(5) 0.0249(4) 0.1632(2) 0.0212(15) Uani 1 1 d . . . C9 C 0.9593(5) -0.0057(4) 0.2124(2) 0.0207(15) Uani 1 1 d . . . C10 C 0.9994(5) -0.0771(4) 0.2405(3) 0.0284(17) Uani 1 1 d . . . H10 H 1.0470 -0.1092 0.2296 0.034 Uiso 1 1 calc R . . C11 C 0.9666(5) -0.0998(5) 0.2854(3) 0.0320(18) Uani 1 1 d . . . H11 H 0.9922 -0.1479 0.3044 0.038 Uiso 1 1 calc R . . C12 C 0.8977(5) -0.0524(5) 0.3015(3) 0.0339(18) Uani 1 1 d . . . H12 H 0.8769 -0.0663 0.3318 0.041 Uiso 1 1 calc R . . C13 C 0.8595(5) 0.0166(4) 0.2720(3) 0.0311(18) Uani 1 1 d . . . H13 H 0.8116 0.0484 0.2828 0.037 Uiso 1 1 calc R . . C14 C 0.9333(5) 0.1312(4) 0.0254(2) 0.0231(16) Uani 1 1 d . . . C15 C 0.9727(5) 0.1215(4) -0.0188(2) 0.0270(17) Uani 1 1 d . . . H15 H 1.0293 0.0937 -0.0183 0.032 Uiso 1 1 calc R . . C16 C 0.9251(5) 0.1547(4) -0.0637(3) 0.0325(18) Uani 1 1 d . . . H16 H 0.9494 0.1493 -0.0938 0.039 Uiso 1 1 calc R . . C17 C 0.8416(5) 0.1956(4) -0.0627(3) 0.0324(18) Uani 1 1 d . . . H17 H 0.8085 0.2171 -0.0924 0.039 Uiso 1 1 calc R . . C18 C 0.8075(5) 0.2045(4) -0.0182(2) 0.0303(17) Uani 1 1 d . . . H18 H 0.7513 0.2327 -0.0182 0.036 Uiso 1 1 calc R . . C19 C 0.8296(5) -0.0299(4) 0.0898(2) 0.0246(16) Uani 1 1 d . . . C20 C 0.8611(5) -0.1172(4) 0.1011(2) 0.0268(17) Uani 1 1 d . . . H20 H 0.9111 -0.1270 0.1258 0.032 Uiso 1 1 calc R . . C21 C 0.8172(5) -0.1878(4) 0.0752(3) 0.0313(18) Uani 1 1 d . . . H21 H 0.8387 -0.2454 0.0823 0.038 Uiso 1 1 calc R . . C22 C 0.7421(6) -0.1756(5) 0.0388(3) 0.0348(19) Uani 1 1 d . . . H22 H 0.7134 -0.2241 0.0216 0.042 Uiso 1 1 calc R . . C23 C 0.7098(5) -0.0893(5) 0.0283(3) 0.0339(18) Uani 1 1 d . . . H23 H 0.6593 -0.0803 0.0037 0.041 Uiso 1 1 calc R . . C24 C 0.7521(5) -0.0165(5) 0.0540(3) 0.0289(17) Uani 1 1 d . . . H24 H 0.7291 0.0407 0.0474 0.035 Uiso 1 1 calc R . . C31 C 0.9250(5) 0.3296(4) 0.1949(2) 0.0213(15) Uani 1 1 d . . . C32 C 1.0154(5) 0.3400(4) 0.2055(3) 0.0269(17) Uani 1 1 d . . . C33 C 1.0694(5) 0.3354(5) 0.2584(3) 0.041(2) Uani 1 1 d . . . H33A H 1.0604 0.3905 0.2761 0.050 Uiso 1 1 calc R . . H33B H 1.0455 0.2870 0.2768 0.050 Uiso 1 1 calc R . . C34 C 1.1692(6) 0.3214(7) 0.2579(4) 0.061(3) Uani 1 1 d . . . H34A H 1.2010 0.3359 0.2912 0.073 Uiso 1 1 calc R . . H34B H 1.1793 0.2585 0.2521 0.073 Uiso 1 1 calc R . . C35 C 1.2096(7) 0.3710(8) 0.2218(4) 0.081(3) Uani 1 1 d . . . H35A H 1.2727 0.3514 0.2233 0.097 Uiso 1 1 calc R . . H35B H 1.2113 0.4331 0.2322 0.097 Uiso 1 1 calc R . . C36 C 1.1655(5) 0.3671(5) 0.1669(3) 0.039(2) Uani 1 1 d . . . H36A H 1.1795 0.4218 0.1501 0.046 Uiso 1 1 calc R . . H36B H 1.1922 0.3179 0.1504 0.046 Uiso 1 1 calc R . . C37 C 1.0635(5) 0.3552(4) 0.1608(3) 0.0298(17) Uani 1 1 d . . . C38 C 1.0064(5) 0.3566(4) 0.1167(3) 0.0270(16) Uani 1 1 d . . . C39 C 1.0246(5) 0.3706(4) 0.0648(3) 0.0276(17) Uani 1 1 d . . . C40 C 1.1087(5) 0.3842(5) 0.0491(3) 0.043(2) Uani 1 1 d . . . H40 H 1.1619 0.3836 0.0724 0.052 Uiso 1 1 calc R . . C41 C 1.1135(6) 0.3985(6) -0.0012(3) 0.052(2) Uani 1 1 d . . . H41 H 1.1699 0.4099 -0.0117 0.063 Uiso 1 1 calc R . . C42 C 1.0377(6) 0.3963(5) -0.0351(3) 0.045(2) Uani 1 1 d . . . H42 H 1.0411 0.4035 -0.0693 0.054 Uiso 1 1 calc R . . C43 C 0.9544(6) 0.3832(5) -0.0183(3) 0.038(2) Uani 1 1 d . . . H43 H 0.9013 0.3843 -0.0416 0.046 Uiso 1 1 calc R . . C44 C 0.8575(5) 0.3192(4) 0.2307(2) 0.0220(15) Uani 1 1 d . . . C45 C 0.8488(5) 0.3833(4) 0.2674(3) 0.0294(17) Uani 1 1 d . . . H45 H 0.8873 0.4328 0.2709 0.035 Uiso 1 1 calc R . . C46 C 0.7816(5) 0.3721(5) 0.2989(3) 0.0313(18) Uani 1 1 d . . . H46 H 0.7761 0.4130 0.3244 0.038 Uiso 1 1 calc R . . C47 C 0.7231(5) 0.2995(4) 0.2916(2) 0.0293(17) Uani 1 1 d . . . H47 H 0.6772 0.2913 0.3117 0.035 Uiso 1 1 calc R . . C48 C 0.7347(5) 0.2395(4) 0.2538(3) 0.0273(17) Uani 1 1 d . . . H48 H 0.6943 0.1916 0.2485 0.033 Uiso 1 1 calc R . . C49 C 0.8205(5) 0.4324(4) 0.1156(3) 0.0265(17) Uani 1 1 d . . . C50 C 0.8460(5) 0.5110(4) 0.1401(3) 0.0301(17) Uani 1 1 d . . . H50 H 0.8997 0.5139 0.1629 0.036 Uiso 1 1 calc R . . C51 C 0.7908(6) 0.5865(5) 0.1304(3) 0.040(2) Uani 1 1 d . . . H51 H 0.8070 0.6395 0.1474 0.048 Uiso 1 1 calc R . . C52 C 0.7121(6) 0.5824(5) 0.0957(3) 0.044(2) Uani 1 1 d . . . H52 H 0.6751 0.6326 0.0892 0.053 Uiso 1 1 calc R . . C53 C 0.6886(6) 0.5033(5) 0.0706(3) 0.044(2) Uani 1 1 d . . . H53 H 0.6364 0.5011 0.0466 0.053 Uiso 1 1 calc R . . C54 C 0.7410(5) 0.4279(5) 0.0803(3) 0.0323(18) Uani 1 1 d . . . H54 H 0.7239 0.3747 0.0638 0.039 Uiso 1 1 calc R . . C100 C 0.5298(6) 0.1056(6) 0.0942(3) 0.046(2) Uani 1 1 d . . . C200 C 1.0827(7) 0.6472(6) 0.2417(3) 0.052(2) Uani 1 1 d . . . C900 C 0.9898(10) 1.3207(7) 0.4078(7) 0.157(8) Uani 1 1 d . . . H90A H 0.9773 1.3078 0.4418 0.188 Uiso 1 1 calc R . . H90B H 0.9458 1.3652 0.3936 0.188 Uiso 1 1 calc R . . C901 C 1.1961(7) 1.1244(7) 0.3671(4) 0.072(3) Uani 1 1 d . . . H90C H 1.1745 1.1855 0.3631 0.087 Uiso 1 1 calc R . . H90D H 1.2592 1.1230 0.3605 0.087 Uiso 1 1 calc R . . C902 C 1.0377(6) 0.8816(6) 0.4309(4) 0.062(3) Uani 1 1 d . . . H90E H 1.0399 0.9454 0.4249 0.075 Uiso 1 1 calc R . . H90F H 0.9896 0.8567 0.4063 0.075 Uiso 1 1 calc R . . F1 F 0.4796(3) 0.1540(3) 0.0599(2) 0.0671(16) Uani 1 1 d . . . F2 F 0.5555(3) 0.0323(3) 0.0720(2) 0.0580(14) Uani 1 1 d . . . F3 F 0.4774(3) 0.0801(3) 0.1286(2) 0.0649(15) Uani 1 1 d . . . F11 F 1.0295(5) 0.5770(4) 0.2466(2) 0.0865(19) Uani 1 1 d . . . F12 F 1.0694(5) 0.7080(4) 0.27565(19) 0.089(2) Uani 1 1 d . . . F13 F 1.1691(4) 0.6200(4) 0.2528(2) 0.0855(19) Uani 1 1 d . . . S2 S 1.06290(14) 0.69250(13) 0.17776(7) 0.0351(5) Uani 1 1 d . . . O11 O 0.9687(4) 0.7164(4) 0.1710(2) 0.0577(17) Uani 1 1 d . . . O12 O 1.1252(4) 0.7676(3) 0.18032(19) 0.0450(14) Uani 1 1 d . . . O13 O 1.0857(4) 0.6185(4) 0.1483(2) 0.0567(17) Uani 1 1 d . . . Cl1 Cl 0.9724(2) 1.2273(3) 0.37326(15) 0.1198(13) Uani 1 1 d . . . Cl2 Cl 1.1002(2) 1.3667(2) 0.41186(17) 0.1275(14) Uani 1 1 d . . . Cl3 Cl 1.1296(2) 1.0572(2) 0.32367(12) 0.0966(10) Uani 1 1 d . . . Cl4 Cl 1.1917(2) 1.08948(19) 0.42987(11) 0.0895(9) Uani 1 1 d . . . Cl5 Cl 1.0105(2) 0.86313(17) 0.49153(10) 0.0801(9) Uani 1 1 d . . . Cl6 Cl 1.1432(2) 0.8340(2) 0.42200(15) 0.1044(12) 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 0.0276(5) 0.0211(5) 0.0236(5) -0.0013(3) 0.0096(4) 0.0005(4) Cu2 0.0293(5) 0.0227(5) 0.0246(5) 0.0000(3) 0.0122(4) 0.0017(4) P1 0.0239(11) 0.0234(10) 0.0190(9) -0.0001(7) 0.0081(8) 0.0000(8) P2 0.0240(10) 0.0226(10) 0.0221(9) -0.0015(7) 0.0086(8) -0.0008(8) N1 0.026(3) 0.028(3) 0.018(3) -0.004(2) 0.009(3) -0.003(3) N2 0.029(4) 0.031(3) 0.021(3) 0.003(2) 0.011(3) 0.000(3) N3 0.025(3) 0.020(3) 0.026(3) 0.003(2) 0.009(3) 0.003(3) N4 0.042(4) 0.036(4) 0.028(3) 0.003(3) 0.011(3) -0.003(3) S1 0.0259(11) 0.0319(11) 0.0367(11) -0.0068(8) 0.0081(9) 0.0006(8) O1 0.032(3) 0.045(3) 0.051(3) -0.025(3) 0.014(3) 0.006(3) O2 0.033(3) 0.034(3) 0.028(3) 0.001(2) 0.012(2) 0.002(2) O3 0.030(3) 0.033(3) 0.036(3) 0.001(2) 0.009(2) -0.004(2) C1 0.032(4) 0.012(3) 0.028(4) 0.002(3) 0.014(3) 0.002(3) C2 0.018(4) 0.021(4) 0.024(4) -0.006(3) 0.018(3) 0.000(3) C3 0.027(4) 0.038(4) 0.035(4) 0.004(3) 0.017(4) -0.003(3) C4 0.021(4) 0.053(5) 0.039(5) 0.000(4) 0.010(4) -0.008(4) C5 0.028(4) 0.043(5) 0.028(4) 0.000(3) 0.007(4) 0.001(4) C6 0.023(4) 0.046(5) 0.038(4) 0.004(3) 0.008(4) 0.004(4) C7 0.021(4) 0.017(3) 0.029(4) -0.004(3) 0.014(3) -0.004(3) C8 0.029(4) 0.016(3) 0.019(3) 0.002(2) 0.007(3) -0.001(3) C9 0.025(4) 0.021(4) 0.018(3) -0.003(3) 0.010(3) 0.000(3) C10 0.027(4) 0.023(4) 0.035(4) 0.001(3) 0.003(4) 0.000(3) C11 0.042(5) 0.027(4) 0.028(4) 0.006(3) 0.007(4) -0.006(4) C12 0.046(5) 0.028(4) 0.031(4) 0.004(3) 0.017(4) 0.000(4) C13 0.033(5) 0.033(4) 0.030(4) -0.003(3) 0.016(4) 0.001(4) C14 0.029(4) 0.021(4) 0.020(3) -0.004(3) 0.009(3) -0.004(3) C15 0.027(4) 0.030(4) 0.026(4) -0.003(3) 0.013(3) 0.003(3) C16 0.040(5) 0.034(4) 0.026(4) 0.001(3) 0.011(4) -0.003(4) C17 0.043(5) 0.031(4) 0.024(4) -0.003(3) 0.009(4) -0.006(4) C18 0.032(4) 0.031(4) 0.029(4) 0.000(3) 0.006(4) 0.006(3) C19 0.028(4) 0.032(4) 0.017(3) 0.004(3) 0.015(3) -0.003(3) C20 0.030(4) 0.029(4) 0.024(4) 0.003(3) 0.013(3) -0.006(3) C21 0.046(5) 0.018(4) 0.034(4) -0.001(3) 0.023(4) -0.002(3) C22 0.050(5) 0.024(4) 0.033(4) -0.010(3) 0.017(4) -0.012(4) C23 0.025(4) 0.045(5) 0.032(4) -0.001(3) 0.008(4) -0.005(4) C24 0.026(4) 0.028(4) 0.034(4) 0.003(3) 0.005(4) 0.002(3) C31 0.022(4) 0.023(4) 0.022(4) -0.003(3) 0.011(3) 0.000(3) C32 0.027(4) 0.026(4) 0.030(4) -0.003(3) 0.012(3) 0.000(3) C33 0.036(5) 0.056(5) 0.032(4) 0.003(4) 0.006(4) -0.003(4) C34 0.030(5) 0.096(8) 0.055(6) 0.008(5) 0.004(5) 0.007(5) C35 0.035(6) 0.142(10) 0.063(7) 0.009(7) 0.003(5) -0.018(6) C36 0.031(5) 0.050(5) 0.037(5) -0.004(4) 0.012(4) -0.006(4) C37 0.028(4) 0.026(4) 0.037(4) 0.000(3) 0.010(4) -0.005(3) C38 0.031(4) 0.022(4) 0.030(4) 0.001(3) 0.011(3) 0.000(3) C39 0.028(4) 0.019(4) 0.038(4) 0.003(3) 0.011(4) -0.002(3) C40 0.018(4) 0.075(6) 0.040(5) 0.007(4) 0.013(4) -0.004(4) C41 0.042(6) 0.083(7) 0.038(5) -0.003(4) 0.027(5) -0.010(5) C42 0.060(6) 0.042(5) 0.037(5) -0.005(4) 0.023(5) 0.001(4) C43 0.040(5) 0.037(5) 0.038(5) -0.002(3) 0.007(4) -0.004(4) C44 0.026(4) 0.024(4) 0.019(3) 0.001(3) 0.011(3) 0.004(3) C45 0.038(5) 0.023(4) 0.029(4) 0.000(3) 0.011(4) 0.006(3) C46 0.031(5) 0.033(4) 0.030(4) -0.004(3) 0.009(4) 0.007(4) C47 0.038(5) 0.027(4) 0.026(4) 0.003(3) 0.013(4) 0.003(4) C48 0.023(4) 0.028(4) 0.033(4) 0.002(3) 0.010(3) 0.007(3) C49 0.033(5) 0.023(4) 0.028(4) -0.002(3) 0.020(4) -0.008(3) C50 0.035(5) 0.031(4) 0.027(4) -0.001(3) 0.016(4) -0.002(4) C51 0.065(6) 0.023(4) 0.039(5) 0.002(3) 0.031(5) -0.004(4) C52 0.051(6) 0.029(5) 0.060(6) 0.008(4) 0.036(5) 0.011(4) C53 0.033(5) 0.041(5) 0.057(5) 0.017(4) 0.005(4) 0.009(4) C54 0.026(4) 0.028(4) 0.042(5) 0.000(3) 0.002(4) 0.001(3) C100 0.038(5) 0.046(5) 0.057(6) -0.010(4) 0.020(5) 0.001(4) C200 0.082(8) 0.035(5) 0.040(5) 0.010(4) 0.015(5) 0.006(5) C900 0.181(16) 0.050(8) 0.29(2) 0.030(10) 0.200(16) 0.024(8) C901 0.062(7) 0.086(7) 0.072(7) -0.027(5) 0.020(6) -0.040(6) C902 0.055(6) 0.051(6) 0.079(7) 0.013(5) 0.001(6) -0.003(5) F1 0.054(3) 0.066(3) 0.072(4) -0.006(3) -0.023(3) -0.007(3) F2 0.038(3) 0.048(3) 0.091(4) -0.039(3) 0.018(3) -0.017(2) F3 0.039(3) 0.087(4) 0.075(4) -0.020(3) 0.030(3) -0.028(3) F11 0.120(5) 0.065(4) 0.081(4) 0.025(3) 0.035(4) -0.020(4) F12 0.159(6) 0.077(4) 0.038(3) 0.005(3) 0.034(4) 0.017(4) F13 0.087(5) 0.087(4) 0.074(4) 0.023(3) -0.020(4) 0.031(4) S2 0.0335(12) 0.0389(12) 0.0333(11) 0.0027(8) 0.0063(9) 0.0047(10) O11 0.034(4) 0.059(4) 0.080(5) 0.004(3) 0.007(3) 0.007(3) O12 0.048(4) 0.048(3) 0.039(3) 0.007(2) 0.007(3) -0.010(3) O13 0.068(4) 0.054(4) 0.049(4) -0.019(3) 0.011(3) 0.012(3) Cl1 0.081(2) 0.133(3) 0.152(3) 0.062(3) 0.038(2) -0.007(2) Cl2 0.069(2) 0.118(3) 0.197(4) 0.027(3) 0.021(3) 0.024(2) Cl3 0.086(2) 0.108(2) 0.097(2) -0.0442(18) 0.0171(19) -0.0342(18) Cl4 0.097(2) 0.083(2) 0.089(2) -0.0082(16) 0.0151(19) -0.0307(17) Cl5 0.100(2) 0.0691(17) 0.0661(17) -0.0050(13) -0.0054(17) -0.0089(16) Cl6 0.0559(19) 0.091(2) 0.172(3) 0.042(2) 0.037(2) 0.0034(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.023(5) . ? Cu1 O2 2.143(5) . ? Cu1 P2 2.2252(19) . ? Cu1 P1 2.341(2) . ? Cu1 Cu2 2.5228(12) . ? Cu2 N3 2.026(5) . ? Cu2 N2 2.043(5) . ? Cu2 P1 2.3115(19) . ? Cu2 O3 2.331(5) . ? P1 C8 1.795(6) . ? P1 C1 1.834(7) . ? P1 C19 1.832(7) . ? P2 C38 1.818(7) . ? P2 C31 1.821(6) . ? P2 C49 1.824(7) . ? N1 C18 1.347(8) . ? N1 C14 1.352(8) . ? N2 C13 1.345(8) . ? N2 C9 1.373(8) . ? N3 C48 1.346(8) . ? N3 C44 1.365(8) . ? N4 C43 1.338(9) . ? N4 C39 1.364(9) . ? S1 O1 1.440(5) . ? S1 O3 1.459(5) . ? S1 O2 1.468(5) . ? S1 C100 1.833(8) . ? C1 C2 1.341(9) . ? C1 C14 1.479(9) . ? C2 C7 1.463(9) . ? C2 C3 1.523(9) . ? C3 C4 1.531(9) . ? C4 C5 1.507(9) . ? C5 C6 1.531(10) . ? C6 C7 1.504(9) . ? C7 C8 1.362(9) . ? C8 C9 1.485(9) . ? C9 C10 1.391(9) . ? C10 C11 1.397(10) . ? C11 C12 1.358(10) . ? C12 C13 1.371(9) . ? C14 C15 1.396(9) . ? C15 C16 1.395(9) . ? C16 C17 1.376(10) . ? C17 C18 1.362(9) . ? C19 C24 1.398(9) . ? C19 C20 1.407(9) . ? C20 C21 1.378(9) . ? C21 C22 1.378(10) . ? C22 C23 1.392(10) . ? C23 C24 1.390(9) . ? C31 C32 1.331(9) . ? C31 C44 1.480(9) . ? C32 C37 1.490(10) . ? C32 C33 1.524(9) . ? C33 C34 1.486(11) . ? C34 C35 1.415(12) . ? C35 C36 1.522(11) . ? C36 C37 1.499(10) . ? C37 C38 1.349(9) . ? C38 C39 1.467(9) . ? C39 C40 1.377(10) . ? C40 C41 1.374(10) . ? C41 C42 1.337(11) . ? C42 C43 1.378(11) . ? C44 C45 1.393(9) . ? C45 C46 1.397(10) . ? C46 C47 1.383(9) . ? C47 C48 1.382(9) . ? C49 C50 1.375(9) . ? C49 C54 1.398(9) . ? C50 C51 1.395(10) . ? C51 C52 1.383(11) . ? C52 C53 1.382(11) . ? C53 C54 1.372(10) . ? C100 F1 1.314(9) . ? C100 F2 1.328(9) . ? C100 F3 1.337(9) . ? C200 F12 1.320(10) . ? C200 F11 1.328(10) . ? C200 F13 1.330(10) . ? C200 S2 1.826(8) . ? C900 Cl1 1.677(14) . ? C900 Cl2 1.754(14) . ? C901 Cl3 1.734(8) . ? C901 Cl4 1.768(10) . ? C902 Cl5 1.747(10) . ? C902 Cl6 1.757(10) . ? S2 O11 1.420(6) . ? S2 O13 1.428(5) . ? S2 O12 1.448(5) . ? 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 O2 98.8(2) . . ? N1 Cu1 P2 114.59(16) . . ? O2 Cu1 P2 121.72(13) . . ? N1 Cu1 P1 84.43(16) . . ? O2 Cu1 P1 108.80(13) . . ? P2 Cu1 P1 120.25(7) . . ? N1 Cu1 Cu2 140.76(16) . . ? O2 Cu1 Cu2 90.52(12) . . ? P2 Cu1 Cu2 91.46(6) . . ? P1 Cu1 Cu2 56.61(5) . . ? N3 Cu2 N2 110.4(2) . . ? N3 Cu2 P1 155.30(17) . . ? N2 Cu2 P1 85.66(16) . . ? N3 Cu2 O3 92.8(2) . . ? N2 Cu2 O3 107.50(19) . . ? P1 Cu2 O3 100.23(13) . . ? N3 Cu2 Cu1 102.55(15) . . ? N2 Cu2 Cu1 142.74(16) . . ? P1 Cu2 Cu1 57.72(5) . . ? O3 Cu2 Cu1 87.33(12) . . ? C8 P1 C1 89.8(3) . . ? C8 P1 C19 106.3(3) . . ? C1 P1 C19 103.3(3) . . ? C8 P1 Cu2 91.0(2) . . ? C1 P1 Cu2 137.0(2) . . ? C19 P1 Cu2 117.5(2) . . ? C8 P1 Cu1 138.1(2) . . ? C1 P1 Cu1 85.9(2) . . ? C19 P1 Cu1 115.3(2) . . ? Cu2 P1 Cu1 65.68(6) . . ? C38 P2 C31 90.4(3) . . ? C38 P2 C49 108.7(3) . . ? C31 P2 C49 104.7(3) . . ? C38 P2 Cu1 119.1(2) . . ? C31 P2 Cu1 114.5(2) . . ? C49 P2 Cu1 115.9(2) . . ? C18 N1 C14 118.7(6) . . ? C18 N1 Cu1 125.8(5) . . ? C14 N1 Cu1 114.3(4) . . ? C13 N2 C9 118.8(6) . . ? C13 N2 Cu2 123.9(5) . . ? C9 N2 Cu2 117.3(4) . . ? C48 N3 C44 117.8(6) . . ? C48 N3 Cu2 119.0(4) . . ? C44 N3 Cu2 122.0(4) . . ? C43 N4 C39 118.6(7) . . ? O1 S1 O3 115.9(3) . . ? O1 S1 O2 114.6(3) . . ? O3 S1 O2 114.6(3) . . ? O1 S1 C100 104.2(3) . . ? O3 S1 C100 102.6(4) . . ? O2 S1 C100 102.5(3) . . ? S1 O2 Cu1 119.4(3) . . ? S1 O3 Cu2 111.3(3) . . ? C2 C1 C14 132.8(6) . . ? C2 C1 P1 110.8(5) . . ? C14 C1 P1 116.3(5) . . ? C1 C2 C7 114.1(6) . . ? C1 C2 C3 125.0(6) . . ? C7 C2 C3 120.9(6) . . ? C2 C3 C4 111.1(6) . . ? C5 C4 C3 110.1(6) . . ? C4 C5 C6 110.3(6) . . ? C7 C6 C5 113.1(6) . . ? C8 C7 C2 113.8(6) . . ? C8 C7 C6 125.0(6) . . ? C2 C7 C6 121.0(6) . . ? C7 C8 C9 132.0(6) . . ? C7 C8 P1 111.4(5) . . ? C9 C8 P1 116.3(5) . . ? N2 C9 C10 120.3(6) . . ? N2 C9 C8 114.1(5) . . ? C10 C9 C8 125.5(6) . . ? C9 C10 C11 118.7(7) . . ? C12 C11 C10 120.6(7) . . ? C11 C12 C13 118.4(7) . . ? N2 C13 C12 123.2(7) . . ? N1 C14 C15 121.6(6) . . ? N1 C14 C1 114.1(6) . . ? C15 C14 C1 124.2(6) . . ? C16 C15 C14 118.3(7) . . ? C17 C16 C15 119.0(7) . . ? C18 C17 C16 119.9(7) . . ? N1 C18 C17 122.3(7) . . ? C24 C19 C20 119.6(6) . . ? C24 C19 P1 118.9(5) . . ? C20 C19 P1 121.4(5) . . ? C21 C20 C19 119.3(7) . . ? C22 C21 C20 121.8(7) . . ? C21 C22 C23 119.0(6) . . ? C24 C23 C22 120.7(7) . . ? C23 C24 C19 119.6(6) . . ? C32 C31 C44 128.1(6) . . ? C32 C31 P2 110.4(5) . . ? C44 C31 P2 121.5(5) . . ? C31 C32 C37 114.9(6) . . ? C31 C32 C33 124.6(7) . . ? C37 C32 C33 120.5(6) . . ? C34 C33 C32 112.8(7) . . ? C35 C34 C33 116.2(8) . . ? C34 C35 C36 118.4(8) . . ? C37 C36 C35 113.3(7) . . ? C38 C37 C32 113.3(6) . . ? C38 C37 C36 125.9(7) . . ? C32 C37 C36 120.8(6) . . ? C37 C38 C39 131.0(7) . . ? C37 C38 P2 110.7(5) . . ? C39 C38 P2 118.3(5) . . ? N4 C39 C40 120.0(7) . . ? N4 C39 C38 113.0(6) . . ? C40 C39 C38 127.0(7) . . ? C41 C40 C39 119.5(8) . . ? C42 C41 C40 120.6(8) . . ? C41 C42 C43 118.6(8) . . ? N4 C43 C42 122.5(8) . . ? N3 C44 C45 121.6(6) . . ? N3 C44 C31 117.0(5) . . ? C45 C44 C31 121.3(6) . . ? C44 C45 C46 119.0(7) . . ? C47 C46 C45 119.3(6) . . ? C48 C47 C46 118.4(7) . . ? N3 C48 C47 123.6(7) . . ? C50 C49 C54 120.6(6) . . ? C50 C49 P2 121.5(6) . . ? C54 C49 P2 117.9(5) . . ? C49 C50 C51 119.6(7) . . ? C52 C51 C50 120.0(7) . . ? C53 C52 C51 119.6(7) . . ? C54 C53 C52 121.2(8) . . ? C53 C54 C49 119.0(7) . . ? F1 C100 F2 108.1(7) . . ? F1 C100 F3 108.5(7) . . ? F2 C100 F3 107.4(7) . . ? F1 C100 S1 111.1(6) . . ? F2 C100 S1 111.6(6) . . ? F3 C100 S1 109.9(6) . . ? F12 C200 F11 109.4(8) . . ? F12 C200 F13 106.7(8) . . ? F11 C200 F13 107.1(7) . . ? F12 C200 S2 111.6(6) . . ? F11 C200 S2 111.6(6) . . ? F13 C200 S2 110.2(7) . . ? Cl1 C900 Cl2 115.5(7) . . ? Cl3 C901 Cl4 111.9(5) . . ? Cl5 C902 Cl6 112.5(5) . . ? O11 S2 O13 115.3(4) . . ? O11 S2 O12 114.3(3) . . ? O13 S2 O12 115.7(4) . . ? O11 S2 C200 103.7(4) . . ? O13 S2 C200 102.1(4) . . ? O12 S2 C200 103.2(4) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.781 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.150 _database_code_depnum_ccdc_archive 'CCDC 927129' ####################################################################### # # 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_sq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H126 Cl0 Cu6 F0 N12 O0 P6 S6' _chemical_formula_sum 'C144 H126 Cl0 Cu6 F0 N12 O0 P6 S6' _chemical_formula_weight 2783.99 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' Cl Cl 0.1484 0.1585 '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 16.956(2) _cell_length_b 18.436(3) _cell_length_c 19.618(2) _cell_angle_alpha 109.285(2) _cell_angle_beta 102.617(3) _cell_angle_gamma 113.337(2) _cell_volume 4864(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.20 _cell_measurement_theta_max 26.41 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1434 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method none _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 34019 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_sigmaI/netI 0.2256 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.41 _reflns_number_total 19288 _reflns_number_gt 8036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0809P)^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 19288 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1301 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1864 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _refine_ls_shift/su_max 0.003 _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 0.53561(5) 0.56337(5) 0.30949(4) 0.0260(2) Uani 1 1 d . . . Cu2 Cu 0.28169(5) 0.30236(5) 0.24540(4) 0.0273(2) Uani 1 1 d . . . Cu3 Cu 0.78913(5) 0.71966(5) 0.54202(4) 0.0266(2) Uani 1 1 d . . . P1 P 0.30357(11) 0.48867(11) 0.26355(9) 0.0220(4) Uani 1 1 d . . . P2 P 0.27210(11) 0.17698(11) 0.33925(9) 0.0244(4) Uani 1 1 d . . . P3 P 0.72166(11) 0.55242(10) 0.36484(8) 0.0197(3) Uani 1 1 d . . . S1 S 0.39291(10) 0.45392(11) 0.30571(9) 0.0252(4) Uani 1 1 d . . . S2 S 0.26333(15) 0.28565(12) 0.35927(11) 0.0444(5) Uani 1 1 d . . . S3 S 0.65413(10) 0.59759(11) 0.42278(8) 0.0238(4) Uani 1 1 d . . . N1 N 0.5151(4) 0.6667(3) 0.3268(3) 0.0270(12) Uani 1 1 d . . . N2 N 0.1530(4) 0.2741(4) 0.1810(3) 0.0282(12) Uani 1 1 d . . . N11 N 0.3387(3) 0.2298(3) 0.2069(3) 0.0258(12) Uani 1 1 d . . . N12 N 0.8214(3) 0.8345(3) 0.5353(3) 0.0253(12) Uani 1 1 d . . . N21 N 0.8849(3) 0.6814(3) 0.5540(3) 0.0242(12) Uani 1 1 d . . . N22 N 0.5514(3) 0.5066(3) 0.2095(3) 0.0251(12) Uani 1 1 d . . . C1 C 0.3528(4) 0.5724(4) 0.2317(4) 0.0262(15) Uani 1 1 d . . . C2 C 0.3006(5) 0.5362(5) 0.1541(4) 0.0319(16) Uani 1 1 d . . . C3 C 0.3295(5) 0.5829(6) 0.1045(4) 0.055(2) Uani 1 1 d . . . H3A H 0.3518 0.6472 0.1347 0.066 Uiso 1 1 calc R . . H3B H 0.3821 0.5777 0.0942 0.066 Uiso 1 1 calc R . . C4 C 0.2488(6) 0.5431(7) 0.0268(4) 0.064(3) Uani 1 1 d . . . H4A H 0.2729 0.5654 -0.0081 0.077 Uiso 1 1 calc R . . H4B H 0.2036 0.5623 0.0363 0.077 Uiso 1 1 calc R . . C5 C 0.1975(6) 0.4394(7) -0.0148(4) 0.069(3) Uani 1 1 d . . . H5A H 0.1496 0.4149 -0.0680 0.083 Uiso 1 1 calc R . . H5B H 0.2431 0.4195 -0.0206 0.083 Uiso 1 1 calc R . . C6 C 0.1514(5) 0.4067(5) 0.0349(3) 0.0405(18) Uani 1 1 d . . . H6A H 0.1225 0.3410 0.0107 0.049 Uiso 1 1 calc R . . H6B H 0.1005 0.4204 0.0341 0.049 Uiso 1 1 calc R . . C7 C 0.2174(5) 0.4470(5) 0.1197(3) 0.0299(16) Uani 1 1 d . . . C8 C 0.2090(4) 0.4086(4) 0.1670(3) 0.0297(15) Uani 1 1 d . . . C9 C 0.1310(4) 0.3246(4) 0.1527(3) 0.0252(14) Uani 1 1 d . . . C10 C 0.0391(4) 0.2982(5) 0.1100(4) 0.0375(17) Uani 1 1 d . . . H10 H 0.0258 0.3336 0.0889 0.045 Uiso 1 1 calc R . . C11 C -0.0336(5) 0.2181(5) 0.0985(4) 0.0406(18) Uani 1 1 d . . . H11 H -0.0974 0.2003 0.0725 0.049 Uiso 1 1 calc R . . C12 C -0.0112(5) 0.1661(5) 0.1254(4) 0.0442(19) Uani 1 1 d . . . H12 H -0.0590 0.1098 0.1154 0.053 Uiso 1 1 calc R . . C13 C 0.0821(5) 0.1970(5) 0.1673(4) 0.0360(17) Uani 1 1 d . . . H13 H 0.0967 0.1616 0.1875 0.043 Uiso 1 1 calc R . . C14 C 0.4357(4) 0.6623(4) 0.2866(4) 0.0282(15) Uani 1 1 d . . . C15 C 0.4294(5) 0.7372(5) 0.2985(4) 0.0417(18) Uani 1 1 d . . . H15 H 0.3715 0.7311 0.2713 0.050 Uiso 1 1 calc R . . C16 C 0.5064(5) 0.8216(5) 0.3495(5) 0.048(2) Uani 1 1 d . . . H16 H 0.5031 0.8737 0.3562 0.057 Uiso 1 1 calc R . . C17 C 0.5877(5) 0.8275(5) 0.3900(4) 0.0430(19) Uani 1 1 d . . . H17 H 0.6421 0.8841 0.4258 0.052 Uiso 1 1 calc R . . C18 C 0.5890(5) 0.7500(5) 0.3780(4) 0.0326(16) Uani 1 1 d . . . H18 H 0.6452 0.7552 0.4075 0.039 Uiso 1 1 calc R . . C19 C 0.2548(4) 0.5254(4) 0.3302(3) 0.0226(13) Uani 1 1 d . . . C20 C 0.2495(5) 0.4974(4) 0.3892(4) 0.0350(16) Uani 1 1 d . . . H20 H 0.2703 0.4574 0.3928 0.042 Uiso 1 1 calc R . . C21 C 0.2137(5) 0.5292(4) 0.4415(4) 0.0360(17) Uani 1 1 d . . . H21 H 0.2110 0.5113 0.4816 0.043 Uiso 1 1 calc R . . C22 C 0.1823(5) 0.5856(5) 0.4366(4) 0.0404(18) Uani 1 1 d . . . H22 H 0.1595 0.6080 0.4738 0.049 Uiso 1 1 calc R . . C23 C 0.1837(5) 0.6105(4) 0.3765(4) 0.0366(17) Uani 1 1 d . . . H23 H 0.1597 0.6481 0.3721 0.044 Uiso 1 1 calc R . . C24 C 0.2197(4) 0.5812(4) 0.3237(4) 0.0321(16) Uani 1 1 d . . . H24 H 0.2206 0.5986 0.2832 0.039 Uiso 1 1 calc R . . C101 C 0.2503(4) 0.1137(4) 0.2372(3) 0.0238(14) Uani 1 1 d . . . C102 C 0.1727(4) 0.0331(4) 0.2067(3) 0.0281(15) Uani 1 1 d . . . C103 C 0.1214(5) -0.0337(4) 0.1200(3) 0.0378(18) Uani 1 1 d . . . H10A H 0.1673 -0.0416 0.0994 0.045 Uiso 1 1 calc R . . H10B H 0.0926 -0.0094 0.0911 0.045 Uiso 1 1 calc R . . C104 C 0.0435(5) -0.1263(6) 0.1031(4) 0.061(2) Uani 1 1 d . . . H10C H 0.0011 -0.1602 0.0465 0.073 Uiso 1 1 calc R . . H10D H 0.0730 -0.1602 0.1146 0.073 Uiso 1 1 calc R . . C105 C -0.0126(5) -0.1191(5) 0.1510(4) 0.0441(19) Uani 1 1 d . . . H10E H -0.0636 -0.1794 0.1357 0.053 Uiso 1 1 calc R . . H10F H -0.0415 -0.0845 0.1404 0.053 Uiso 1 1 calc R . . C106 C 0.0485(5) -0.0737(4) 0.2377(4) 0.0368(17) Uani 1 1 d . . . H10G H 0.0103 -0.0664 0.2682 0.044 Uiso 1 1 calc R . . H10H H 0.0706 -0.1125 0.2488 0.044 Uiso 1 1 calc R . . C107 C 0.1322(4) 0.0163(4) 0.2654(3) 0.0257(14) Uani 1 1 d . . . C108 C 0.8232(4) 0.9144(4) 0.6622(3) 0.0209(13) Uani 1 1 d . . . C109 C 0.8366(4) 0.9107(4) 0.5889(3) 0.0195(13) Uani 1 1 d . . . C110 C 0.8583(5) 0.9859(4) 0.5778(4) 0.0339(17) Uani 1 1 d . . . H110 H 0.8642 1.0379 0.6158 0.041 Uiso 1 1 calc R . . C111 C 0.8713(6) 0.9827(5) 0.5082(4) 0.052(2) Uani 1 1 d . . . H111 H 0.8885 1.0334 0.4993 0.063 Uiso 1 1 calc R . . C112 C 0.8586(6) 0.9055(5) 0.4540(4) 0.054(2) Uani 1 1 d . . . H112 H 0.8675 0.9020 0.4071 0.065 Uiso 1 1 calc R . . C113 C 0.8328(5) 0.8331(5) 0.4680(4) 0.0367(17) Uani 1 1 d . . . H113 H 0.8222 0.7792 0.4289 0.044 Uiso 1 1 calc R . . C114 C 0.3156(4) 0.1479(4) 0.2025(3) 0.0239(14) Uani 1 1 d . . . C115 C 0.3553(4) 0.1008(4) 0.1703(4) 0.0350(16) Uani 1 1 d . . . H115 H 0.3368 0.0437 0.1676 0.042 Uiso 1 1 calc R . . C116 C 0.4221(5) 0.1349(5) 0.1414(4) 0.0433(19) Uani 1 1 d . . . H116 H 0.4499 0.1027 0.1193 0.052 Uiso 1 1 calc R . . C117 C 0.4453(5) 0.2166(5) 0.1465(4) 0.0385(18) Uani 1 1 d . . . H117 H 0.4904 0.2427 0.1277 0.046 Uiso 1 1 calc R . . C118 C 0.4038(4) 0.2625(5) 0.1790(3) 0.0318(16) Uani 1 1 d . . . H118 H 0.4219 0.3196 0.1817 0.038 Uiso 1 1 calc R . . C119 C 0.3805(5) 0.1984(5) 0.4031(4) 0.0379(18) Uani 1 1 d . . . C120 C 0.3943(5) 0.1276(7) 0.3959(5) 0.057(2) Uani 1 1 d . . . H120 H 0.3470 0.0686 0.3569 0.069 Uiso 1 1 calc R . . C121 C 0.4790(6) 0.1436(8) 0.4467(5) 0.081(3) Uani 1 1 d . . . H121 H 0.4889 0.0955 0.4432 0.097 Uiso 1 1 calc R . . C122 C 0.5466(8) 0.2295(7) 0.5012(6) 0.082(3) Uiso 1 1 d . . . H122 H 0.6042 0.2405 0.5349 0.098 Uiso 1 1 calc R . . C123 C 0.5342(7) 0.2969(7) 0.5080(6) 0.081(3) Uiso 1 1 d . . . H123 H 0.5837 0.3551 0.5467 0.097 Uiso 1 1 calc R . . C124 C 0.4488(5) 0.2875(6) 0.4597(4) 0.069(3) Uani 1 1 d . . . H124 H 0.4399 0.3366 0.4655 0.083 Uiso 1 1 calc R . . C201 C 0.8472(4) 0.6220(4) 0.4130(3) 0.0220(13) Uani 1 1 d . . . C202 C 0.8807(4) 0.6526(4) 0.3662(3) 0.0250(14) Uani 1 1 d . . . C203 C 0.9794(4) 0.7225(5) 0.3877(4) 0.0427(19) Uani 1 1 d . . . H20A H 0.9900 0.7815 0.4222 0.051 Uiso 1 1 calc R . . H20B H 1.0234 0.7111 0.4188 0.051 Uiso 1 1 calc R . . C204 C 1.0029(5) 0.7266(5) 0.3191(4) 0.050(2) Uani 1 1 d . . . H20C H 1.0082 0.6742 0.2914 0.060 Uiso 1 1 calc R . . H20D H 1.0639 0.7811 0.3383 0.060 Uiso 1 1 calc R . . C205 C 0.9256(5) 0.7274(5) 0.2616(4) 0.0434(19) Uani 1 1 d . . . H20E H 0.9162 0.7767 0.2901 0.052 Uiso 1 1 calc R . . H20F H 0.9443 0.7369 0.2194 0.052 Uiso 1 1 calc R . . C206 C 0.8355(4) 0.6387(4) 0.2259(3) 0.0276(15) Uani 1 1 d . . . H20G H 0.7850 0.6400 0.1907 0.033 Uiso 1 1 calc R . . H20H H 0.8443 0.5910 0.1931 0.033 Uiso 1 1 calc R . . C207 C 0.8053(4) 0.6162(4) 0.2853(3) 0.0197(13) Uani 1 1 d . . . C208 C 0.7170(4) 0.5632(4) 0.2767(3) 0.0187(13) Uani 1 1 d . . . C209 C 0.6311(4) 0.5114(4) 0.2030(3) 0.0201(13) Uani 1 1 d . . . C210 C 0.6324(4) 0.4671(5) 0.1320(3) 0.0330(16) Uani 1 1 d . . . H210 H 0.6885 0.4691 0.1298 0.040 Uiso 1 1 calc R . . C211 C 0.5513(5) 0.4195(5) 0.0634(4) 0.044(2) Uani 1 1 d . . . H211 H 0.5517 0.3900 0.0136 0.053 Uiso 1 1 calc R . . C212 C 0.4707(5) 0.4159(5) 0.0689(4) 0.0425(19) Uani 1 1 d . . . H212 H 0.4141 0.3842 0.0231 0.051 Uiso 1 1 calc R . . C213 C 0.4737(4) 0.4589(5) 0.1419(4) 0.0324(16) Uani 1 1 d . . . H213 H 0.4172 0.4550 0.1452 0.039 Uiso 1 1 calc R . . C214 C 0.9050(4) 0.6418(4) 0.4928(3) 0.0234(14) Uani 1 1 d . . . C215 C 0.9741(4) 0.6198(5) 0.5047(4) 0.0369(18) Uani 1 1 d . . . H215 H 0.9849 0.5899 0.4612 0.044 Uiso 1 1 calc R . . C216 C 1.0265(5) 0.6414(6) 0.5793(4) 0.060(3) Uani 1 1 d . . . H216 H 1.0754 0.6281 0.5881 0.072 Uiso 1 1 calc R . . C217 C 1.0093(5) 0.6813(5) 0.6403(4) 0.047(2) Uani 1 1 d . . . H217 H 1.0466 0.6974 0.6925 0.056 Uiso 1 1 calc R . . C218 C 0.9367(5) 0.6986(4) 0.6264(4) 0.0353(17) Uani 1 1 d . . . H218 H 0.9226 0.7236 0.6696 0.042 Uiso 1 1 calc R . . C219 C 0.6893(4) 0.4384(4) 0.3424(3) 0.0232(14) Uani 1 1 d . . . C220 C 0.7351(5) 0.4032(5) 0.3062(4) 0.0434(19) Uani 1 1 d . . . H220 H 0.7814 0.4380 0.2927 0.052 Uiso 1 1 calc R . . C221 C 0.7142(6) 0.3165(5) 0.2892(5) 0.060(2) Uani 1 1 d . . . H221 H 0.7461 0.2919 0.2641 0.072 Uiso 1 1 calc R . . C222 C 0.6468(5) 0.2669(5) 0.3091(4) 0.046(2) Uani 1 1 d . . . H222 H 0.6326 0.2080 0.2982 0.055 Uiso 1 1 calc R . . C223 C 0.6007(6) 0.3013(5) 0.3439(4) 0.054(2) Uani 1 1 d . . . H223 H 0.5544 0.2663 0.3573 0.065 Uiso 1 1 calc R . . C224 C 0.6206(5) 0.3887(4) 0.3605(4) 0.0380(17) Uani 1 1 d . . . H224 H 0.5871 0.4125 0.3837 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0269(4) 0.0327(5) 0.0245(4) 0.0142(4) 0.0142(4) 0.0176(4) Cu2 0.0280(4) 0.0344(5) 0.0275(4) 0.0162(4) 0.0160(4) 0.0188(4) Cu3 0.0359(5) 0.0258(5) 0.0222(4) 0.0119(4) 0.0170(4) 0.0159(4) P1 0.0211(8) 0.0285(10) 0.0206(8) 0.0141(7) 0.0115(7) 0.0125(8) P2 0.0263(9) 0.0221(9) 0.0200(8) 0.0068(7) 0.0140(7) 0.0081(8) P3 0.0243(9) 0.0217(9) 0.0163(8) 0.0098(7) 0.0113(7) 0.0121(7) S1 0.0212(8) 0.0336(10) 0.0270(8) 0.0185(8) 0.0118(7) 0.0147(8) S2 0.0826(15) 0.0255(10) 0.0422(10) 0.0190(9) 0.0500(11) 0.0267(10) S3 0.0222(8) 0.0315(9) 0.0205(8) 0.0108(7) 0.0126(7) 0.0151(8) N1 0.028(3) 0.028(3) 0.034(3) 0.019(3) 0.016(3) 0.016(3) N2 0.028(3) 0.033(3) 0.025(3) 0.008(3) 0.010(2) 0.021(3) N11 0.024(3) 0.034(3) 0.026(3) 0.014(3) 0.016(2) 0.017(3) N12 0.037(3) 0.026(3) 0.029(3) 0.017(3) 0.026(3) 0.021(3) N21 0.027(3) 0.024(3) 0.020(3) 0.010(2) 0.010(2) 0.011(2) N22 0.018(3) 0.034(3) 0.022(3) 0.015(3) 0.006(2) 0.012(3) C1 0.024(3) 0.032(4) 0.044(4) 0.030(3) 0.022(3) 0.018(3) C2 0.042(4) 0.042(4) 0.034(4) 0.028(4) 0.020(3) 0.030(4) C3 0.068(6) 0.098(7) 0.054(5) 0.062(5) 0.040(5) 0.058(6) C4 0.065(6) 0.110(8) 0.046(5) 0.058(6) 0.037(5) 0.046(6) C5 0.071(6) 0.127(9) 0.036(5) 0.050(6) 0.029(5) 0.060(7) C6 0.037(4) 0.061(5) 0.022(3) 0.018(4) 0.008(3) 0.026(4) C7 0.038(4) 0.051(5) 0.019(3) 0.021(3) 0.016(3) 0.032(4) C8 0.030(4) 0.045(4) 0.018(3) 0.010(3) 0.011(3) 0.025(4) C9 0.024(3) 0.024(4) 0.027(3) 0.002(3) 0.014(3) 0.018(3) C10 0.029(4) 0.041(5) 0.033(4) 0.008(3) 0.007(3) 0.020(4) C11 0.026(4) 0.041(5) 0.030(4) 0.002(3) 0.002(3) 0.013(4) C12 0.024(4) 0.037(5) 0.048(5) 0.005(4) 0.009(4) 0.010(4) C13 0.039(4) 0.034(4) 0.036(4) 0.012(3) 0.021(3) 0.019(4) C14 0.031(4) 0.041(4) 0.040(4) 0.031(4) 0.025(3) 0.026(3) C15 0.037(4) 0.051(5) 0.062(5) 0.043(4) 0.026(4) 0.026(4) C16 0.051(5) 0.037(5) 0.070(5) 0.038(4) 0.037(5) 0.018(4) C17 0.036(4) 0.036(5) 0.066(5) 0.030(4) 0.023(4) 0.020(4) C18 0.029(4) 0.044(5) 0.045(4) 0.028(4) 0.021(3) 0.027(4) C19 0.016(3) 0.023(3) 0.022(3) 0.009(3) 0.006(3) 0.006(3) C20 0.039(4) 0.037(4) 0.027(4) 0.016(3) 0.014(3) 0.017(4) C21 0.043(4) 0.037(4) 0.039(4) 0.021(4) 0.029(4) 0.020(4) C22 0.045(5) 0.040(5) 0.034(4) 0.011(4) 0.029(4) 0.018(4) C23 0.044(4) 0.033(4) 0.037(4) 0.013(3) 0.018(4) 0.025(4) C24 0.034(4) 0.032(4) 0.032(4) 0.012(3) 0.015(3) 0.019(3) C101 0.020(3) 0.025(4) 0.032(4) 0.014(3) 0.012(3) 0.016(3) C102 0.030(4) 0.024(4) 0.023(3) 0.009(3) 0.007(3) 0.012(3) C103 0.056(5) 0.031(4) 0.015(3) 0.008(3) 0.018(3) 0.013(4) C104 0.052(5) 0.072(6) 0.025(4) 0.005(4) 0.001(4) 0.023(5) C105 0.029(4) 0.035(4) 0.030(4) 0.010(3) -0.002(3) -0.007(3) C106 0.034(4) 0.030(4) 0.036(4) 0.012(3) 0.014(3) 0.011(3) C107 0.024(3) 0.017(3) 0.028(4) 0.007(3) 0.006(3) 0.008(3) C108 0.021(3) 0.020(3) 0.024(3) 0.007(3) 0.016(3) 0.011(3) C109 0.024(3) 0.014(3) 0.019(3) 0.008(3) 0.011(3) 0.007(3) C110 0.053(5) 0.021(4) 0.027(4) 0.009(3) 0.023(3) 0.016(3) C111 0.076(6) 0.038(5) 0.065(5) 0.036(4) 0.046(5) 0.031(5) C112 0.106(7) 0.033(5) 0.044(4) 0.023(4) 0.055(5) 0.036(5) C113 0.062(5) 0.034(4) 0.041(4) 0.023(4) 0.039(4) 0.033(4) C114 0.022(3) 0.029(4) 0.025(3) 0.009(3) 0.013(3) 0.017(3) C115 0.028(4) 0.026(4) 0.041(4) 0.008(3) 0.011(3) 0.013(3) C116 0.032(4) 0.056(5) 0.037(4) 0.011(4) 0.015(4) 0.026(4) C117 0.036(4) 0.072(6) 0.027(4) 0.027(4) 0.024(3) 0.035(4) C118 0.022(3) 0.042(4) 0.028(4) 0.015(3) 0.009(3) 0.014(3) C119 0.027(4) 0.059(5) 0.020(4) 0.016(4) 0.015(3) 0.015(4) C120 0.031(4) 0.097(8) 0.046(5) 0.037(5) 0.014(4) 0.033(5) C121 0.066(6) 0.156(11) 0.075(7) 0.074(8) 0.050(6) 0.076(8) C124 0.040(5) 0.094(7) 0.036(5) 0.012(5) 0.023(4) 0.011(5) C201 0.025(3) 0.021(3) 0.026(3) 0.015(3) 0.010(3) 0.014(3) C202 0.035(4) 0.030(4) 0.023(3) 0.016(3) 0.021(3) 0.020(3) C203 0.022(4) 0.051(5) 0.037(4) 0.018(4) 0.014(3) 0.004(4) C204 0.039(5) 0.057(5) 0.053(5) 0.034(4) 0.029(4) 0.012(4) C205 0.056(5) 0.032(4) 0.042(4) 0.026(4) 0.027(4) 0.011(4) C206 0.039(4) 0.030(4) 0.025(3) 0.020(3) 0.019(3) 0.018(3) C207 0.029(3) 0.019(3) 0.020(3) 0.011(3) 0.016(3) 0.014(3) C208 0.028(3) 0.025(3) 0.012(3) 0.008(3) 0.015(3) 0.018(3) C209 0.021(3) 0.025(4) 0.015(3) 0.012(3) 0.005(3) 0.011(3) C210 0.026(4) 0.053(5) 0.021(3) 0.017(3) 0.008(3) 0.022(4) C211 0.035(4) 0.071(6) 0.025(4) 0.018(4) 0.018(3) 0.027(4) C212 0.043(4) 0.077(6) 0.019(3) 0.025(4) 0.021(3) 0.035(4) C213 0.027(4) 0.051(5) 0.034(4) 0.027(4) 0.022(3) 0.022(4) C214 0.025(3) 0.027(4) 0.024(3) 0.017(3) 0.017(3) 0.011(3) C215 0.031(4) 0.067(5) 0.028(4) 0.027(4) 0.020(3) 0.030(4) C216 0.040(5) 0.125(8) 0.029(4) 0.040(5) 0.013(4) 0.051(5) C217 0.042(5) 0.073(6) 0.019(4) 0.015(4) 0.002(3) 0.036(4) C218 0.036(4) 0.034(4) 0.024(4) 0.009(3) 0.010(3) 0.011(3) C219 0.030(4) 0.017(3) 0.015(3) 0.007(3) 0.008(3) 0.007(3) C220 0.052(5) 0.031(4) 0.059(5) 0.017(4) 0.040(4) 0.024(4) C221 0.073(6) 0.041(5) 0.082(6) 0.029(5) 0.042(5) 0.036(5) C222 0.070(6) 0.029(4) 0.041(4) 0.019(4) 0.023(4) 0.025(4) C223 0.069(6) 0.032(5) 0.036(4) 0.014(4) 0.020(4) 0.005(4) C224 0.046(4) 0.022(4) 0.028(4) 0.007(3) 0.014(3) 0.006(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 2.004(5) . ? Cu1 N22 2.027(5) . ? Cu1 S3 2.3440(17) . ? Cu1 S1 2.4261(17) . ? Cu2 N11 1.993(5) . ? Cu2 N2 2.023(5) . ? Cu2 S1 2.3302(19) . ? Cu2 S2 2.4217(18) . ? Cu3 N21 2.009(5) . ? Cu3 N12 2.025(5) . ? Cu3 S2 2.3150(17) 2_666 ? Cu3 S3 2.4246(18) . ? P1 C19 1.783(6) . ? P1 C8 1.814(6) . ? P1 C1 1.821(6) . ? P1 S1 1.990(2) . ? P2 C119 1.788(7) . ? P2 C108 1.800(6) 2_666 ? P2 C101 1.815(6) . ? P2 S2 1.983(2) . ? P3 C208 1.792(5) . ? P3 C201 1.797(6) . ? P3 C219 1.811(6) . ? P3 S3 1.999(2) . ? S2 Cu3 2.3150(17) 2_666 ? N1 C14 1.359(7) . ? N1 C18 1.358(8) . ? N2 C13 1.338(8) . ? N2 C9 1.354(7) . ? N11 C118 1.355(7) . ? N11 C114 1.369(7) . ? N12 C109 1.329(7) . ? N12 C113 1.369(7) . ? N21 C218 1.352(7) . ? N21 C214 1.375(7) . ? N22 C213 1.348(7) . ? N22 C209 1.356(7) . ? C1 C2 1.349(8) . ? C1 C14 1.482(9) . ? C2 C7 1.471(9) . ? C2 C3 1.534(9) . ? C3 C4 1.513(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.555(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.507(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.512(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.339(8) . ? C8 C9 1.467(9) . ? C9 C10 1.389(8) . ? C10 C11 1.402(9) . ? C10 H10 0.9500 . ? C11 C12 1.371(9) . ? C11 H11 0.9500 . ? C12 C13 1.383(9) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.375(9) . ? C15 C16 1.385(9) . ? C15 H15 0.9500 . ? C16 C17 1.375(9) . ? C16 H16 0.9500 . ? C17 C18 1.380(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.403(8) . ? C19 C20 1.421(8) . ? C20 C21 1.387(8) . ? C20 H20 0.9500 . ? C21 C22 1.362(9) . ? C21 H21 0.9500 . ? C22 C23 1.401(9) . ? C22 H22 0.9500 . ? C23 C24 1.380(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C101 C102 1.347(8) . ? C101 C114 1.465(8) . ? C102 C103 1.513(8) . ? C102 C107 1.520(8) . ? C103 C104 1.555(10) . ? C103 H10A 0.9900 . ? C103 H10B 0.9900 . ? C104 C105 1.488(9) . ? C104 H10C 0.9900 . ? C104 H10D 0.9900 . ? C105 C106 1.506(8) . ? C105 H10E 0.9900 . ? C105 H10F 0.9900 . ? C106 C107 1.505(8) . ? C106 H10G 0.9900 . ? C106 H10H 0.9900 . ? C107 C108 1.337(8) 2_666 ? C108 C107 1.337(8) 2_666 ? C108 C109 1.487(7) . ? C108 P2 1.800(6) 2_666 ? C109 C110 1.391(8) . ? C110 C111 1.417(8) . ? C110 H110 0.9500 . ? C111 C112 1.363(9) . ? C111 H111 0.9500 . ? C112 C113 1.371(9) . ? C112 H112 0.9500 . ? C113 H113 0.9500 . ? C114 C115 1.376(8) . ? C115 C116 1.398(9) . ? C115 H115 0.9500 . ? C116 C117 1.360(10) . ? C116 H116 0.9500 . ? C117 C118 1.388(9) . ? C117 H117 0.9500 . ? C118 H118 0.9500 . ? C119 C120 1.383(10) . ? C119 C124 1.414(10) . ? C120 C121 1.410(10) . ? C120 H120 0.9500 . ? C121 C122 1.369(13) . ? C121 H121 0.9500 . ? C122 C123 1.310(12) . ? C122 H122 0.9500 . ? C123 C124 1.455(12) . ? C123 H123 0.9500 . ? C124 H124 0.9500 . ? C201 C202 1.341(7) . ? C201 C214 1.488(8) . ? C202 C203 1.504(8) . ? C202 C207 1.528(8) . ? C203 C204 1.502(8) . ? C203 H20A 0.9900 . ? C203 H20B 0.9900 . ? C204 C205 1.540(9) . ? C204 H20C 0.9900 . ? C204 H20D 0.9900 . ? C205 C206 1.516(8) . ? C205 H20E 0.9900 . ? C205 H20F 0.9900 . ? C206 C207 1.484(7) . ? C206 H20G 0.9900 . ? C206 H20H 0.9900 . ? C207 C208 1.360(8) . ? C208 C209 1.480(7) . ? C209 C210 1.372(8) . ? C210 C211 1.388(8) . ? C210 H210 0.9500 . ? C211 C212 1.372(9) . ? C211 H211 0.9500 . ? C212 C213 1.367(8) . ? C212 H212 0.9500 . ? C213 H213 0.9500 . ? C214 C215 1.381(8) . ? C215 C216 1.363(8) . ? C215 H215 0.9500 . ? C216 C217 1.342(9) . ? C216 H216 0.9500 . ? C217 C218 1.384(9) . ? C217 H217 0.9500 . ? C218 H218 0.9500 . ? C219 C220 1.365(8) . ? C219 C224 1.368(8) . ? C220 C221 1.392(9) . ? C220 H220 0.9500 . ? C221 C222 1.378(10) . ? C221 H221 0.9500 . ? C222 C223 1.348(10) . ? C222 H222 0.9500 . ? C223 C224 1.412(9) . ? C223 H223 0.9500 . ? C224 H224 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N22 118.13(19) . . ? N1 Cu1 S3 110.21(15) . . ? N22 Cu1 S3 112.37(14) . . ? N1 Cu1 S1 102.29(15) . . ? N22 Cu1 S1 108.29(15) . . ? S3 Cu1 S1 104.10(6) . . ? N11 Cu2 N2 123.0(2) . . ? N11 Cu2 S1 110.10(15) . . ? N2 Cu2 S1 112.53(16) . . ? N11 Cu2 S2 104.86(15) . . ? N2 Cu2 S2 102.75(15) . . ? S1 Cu2 S2 100.32(6) . . ? N21 Cu3 N12 119.78(19) . . ? N21 Cu3 S2 106.08(14) . 2_666 ? N12 Cu3 S2 112.56(14) . 2_666 ? N21 Cu3 S3 105.41(15) . . ? N12 Cu3 S3 108.40(15) . . ? S2 Cu3 S3 103.16(7) 2_666 . ? C19 P1 C8 108.5(3) . . ? C19 P1 C1 109.0(3) . . ? C8 P1 C1 93.1(3) . . ? C19 P1 S1 113.5(2) . . ? C8 P1 S1 117.2(2) . . ? C1 P1 S1 113.7(2) . . ? C119 P2 C108 108.8(3) . 2_666 ? C119 P2 C101 109.7(3) . . ? C108 P2 C101 93.6(3) 2_666 . ? C119 P2 S2 113.7(3) . . ? C108 P2 S2 116.4(2) 2_666 . ? C101 P2 S2 112.9(2) . . ? C208 P3 C201 93.3(3) . . ? C208 P3 C219 108.3(3) . . ? C201 P3 C219 109.2(3) . . ? C208 P3 S3 116.61(19) . . ? C201 P3 S3 113.8(2) . . ? C219 P3 S3 113.7(2) . . ? P1 S1 Cu2 94.92(8) . . ? P1 S1 Cu1 100.02(8) . . ? Cu2 S1 Cu1 144.29(7) . . ? P2 S2 Cu3 93.34(8) . 2_666 ? P2 S2 Cu2 99.64(8) . . ? Cu3 S2 Cu2 162.51(10) 2_666 . ? P3 S3 Cu1 95.11(8) . . ? P3 S3 Cu3 98.38(8) . . ? Cu1 S3 Cu3 143.66(8) . . ? C14 N1 C18 115.9(5) . . ? C14 N1 Cu1 125.8(4) . . ? C18 N1 Cu1 118.0(4) . . ? C13 N2 C9 117.6(6) . . ? C13 N2 Cu2 114.5(4) . . ? C9 N2 Cu2 127.9(4) . . ? C118 N11 C114 116.4(5) . . ? C118 N11 Cu2 117.2(4) . . ? C114 N11 Cu2 126.3(4) . . ? C109 N12 C113 117.1(5) . . ? C109 N12 Cu3 128.2(4) . . ? C113 N12 Cu3 114.6(4) . . ? C218 N21 C214 116.7(5) . . ? C218 N21 Cu3 119.4(4) . . ? C214 N21 Cu3 123.8(4) . . ? C213 N22 C209 116.5(5) . . ? C213 N22 Cu1 116.1(4) . . ? C209 N22 Cu1 127.4(4) . . ? C2 C1 C14 130.3(5) . . ? C2 C1 P1 107.5(5) . . ? C14 C1 P1 122.2(4) . . ? C1 C2 C7 115.3(5) . . ? C1 C2 C3 122.0(6) . . ? C7 C2 C3 122.6(6) . . ? C4 C3 C2 111.7(6) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 111.3(7) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 108.2(6) . . ? C6 C5 H5A 110.0 . . ? C4 C5 H5A 110.1 . . ? C6 C5 H5B 110.0 . . ? C4 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C5 C6 C7 114.3(6) . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C2 116.0(6) . . ? C8 C7 C6 126.4(6) . . ? C2 C7 C6 117.6(5) . . ? C7 C8 C9 128.9(6) . . ? C7 C8 P1 107.7(5) . . ? C9 C8 P1 122.5(5) . . ? N2 C9 C10 122.3(6) . . ? N2 C9 C8 117.4(5) . . ? C10 C9 C8 120.2(6) . . ? C9 C10 C11 118.6(7) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 118.8(7) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C13 118.9(7) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? N2 C13 C12 123.6(7) . . ? N2 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? N1 C14 C15 122.2(6) . . ? N1 C14 C1 117.5(5) . . ? C15 C14 C1 120.2(6) . . ? C14 C15 C16 120.8(7) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 117.8(7) . . ? C17 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? C16 C17 C18 118.9(7) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N1 C18 C17 124.3(6) . . ? N1 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? C24 C19 C20 119.3(5) . . ? C24 C19 P1 120.0(4) . . ? C20 C19 P1 120.7(5) . . ? C21 C20 C19 119.2(6) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 121.3(6) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 119.7(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.9(6) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C19 119.4(6) . . ? C23 C24 H24 120.3 . . ? C19 C24 H24 120.3 . . ? C102 C101 C114 129.8(6) . . ? C102 C101 P2 108.0(4) . . ? C114 C101 P2 121.9(4) . . ? C101 C102 C103 124.7(6) . . ? C101 C102 C107 114.6(5) . . ? C103 C102 C107 120.4(5) . . ? C102 C103 C104 113.4(5) . . ? C102 C103 H10A 108.9 . . ? C104 C103 H10A 108.9 . . ? C102 C103 H10B 108.9 . . ? C104 C103 H10B 108.9 . . ? H10A C103 H10B 107.7 . . ? C105 C104 C103 112.6(6) . . ? C105 C104 H10C 109.1 . . ? C103 C104 H10C 109.1 . . ? C105 C104 H10D 109.1 . . ? C103 C104 H10D 109.1 . . ? H10C C104 H10D 107.8 . . ? C104 C105 C106 110.7(6) . . ? C104 C105 H10E 109.5 . . ? C106 C105 H10E 109.5 . . ? C104 C105 H10F 109.5 . . ? C106 C105 H10F 109.5 . . ? H10E C105 H10F 108.1 . . ? C107 C106 C105 113.4(5) . . ? C107 C106 H10G 108.9 . . ? C105 C106 H10G 108.9 . . ? C107 C106 H10H 108.9 . . ? C105 C106 H10H 108.9 . . ? H10G C106 H10H 107.7 . . ? C108 C107 C106 127.1(6) 2_666 . ? C108 C107 C102 114.5(5) 2_666 . ? C106 C107 C102 118.4(5) . . ? C107 C108 C109 128.7(5) 2_666 . ? C107 C108 P2 109.0(4) 2_666 2_666 ? C109 C108 P2 121.8(4) . 2_666 ? N12 C109 C110 123.3(5) . . ? N12 C109 C108 118.7(5) . . ? C110 C109 C108 117.9(5) . . ? C109 C110 C111 118.0(6) . . ? C109 C110 H110 121.0 . . ? C111 C110 H110 121.0 . . ? C112 C111 C110 118.9(7) . . ? C112 C111 H111 120.6 . . ? C110 C111 H111 120.6 . . ? C111 C112 C113 119.3(6) . . ? C111 C112 H112 120.4 . . ? C113 C112 H112 120.4 . . ? N12 C113 C112 123.3(6) . . ? N12 C113 H113 118.3 . . ? C112 C113 H113 118.3 . . ? N11 C114 C115 121.6(6) . . ? N11 C114 C101 117.6(5) . . ? C115 C114 C101 120.8(6) . . ? C114 C115 C116 121.6(7) . . ? C114 C115 H115 119.2 . . ? C116 C115 H115 119.2 . . ? C117 C116 C115 116.4(6) . . ? C117 C116 H116 121.8 . . ? C115 C116 H116 121.8 . . ? C116 C117 C118 120.8(6) . . ? C116 C117 H117 119.6 . . ? C118 C117 H117 119.6 . . ? N11 C118 C117 123.1(7) . . ? N11 C118 H118 118.4 . . ? C117 C118 H118 118.4 . . ? C120 C119 C124 122.5(8) . . ? C120 C119 P2 119.1(6) . . ? C124 C119 P2 118.4(7) . . ? C119 C120 C121 119.6(9) . . ? C119 C120 H120 120.2 . . ? C121 C120 H120 120.2 . . ? C120 C121 C122 119.0(10) . . ? C120 C121 H121 120.5 . . ? C122 C121 H121 120.5 . . ? C123 C122 C121 121.7(11) . . ? C123 C122 H122 119.1 . . ? C121 C122 H122 119.1 . . ? C122 C123 C124 123.7(11) . . ? C122 C123 H123 118.2 . . ? C124 C123 H123 118.2 . . ? C123 C124 C119 113.5(9) . . ? C123 C124 H124 123.2 . . ? C119 C124 H124 123.2 . . ? C202 C201 C214 125.4(5) . . ? C202 C201 P3 110.0(4) . . ? C214 C201 P3 124.7(4) . . ? C201 C202 C203 127.2(6) . . ? C201 C202 C207 113.7(5) . . ? C203 C202 C207 118.8(5) . . ? C204 C203 C202 115.1(6) . . ? C204 C203 H20A 108.5 . . ? C202 C203 H20A 108.5 . . ? C204 C203 H20B 108.5 . . ? C202 C203 H20B 108.5 . . ? H20A C203 H20B 107.5 . . ? C203 C204 C205 109.8(6) . . ? C203 C204 H20C 109.7 . . ? C205 C204 H20C 109.7 . . ? C203 C204 H20D 109.7 . . ? C205 C204 H20D 109.7 . . ? H20C C204 H20D 108.2 . . ? C206 C205 C204 108.5(5) . . ? C206 C205 H20E 110.0 . . ? C204 C205 H20E 110.0 . . ? C206 C205 H20F 110.0 . . ? C204 C205 H20F 110.0 . . ? H20E C205 H20F 108.4 . . ? C207 C206 C205 113.8(5) . . ? C207 C206 H20G 108.8 . . ? C205 C206 H20G 108.8 . . ? C207 C206 H20H 108.8 . . ? C205 C206 H20H 108.8 . . ? H20G C206 H20H 107.7 . . ? C208 C207 C206 128.2(5) . . ? C208 C207 C202 113.4(5) . . ? C206 C207 C202 118.3(5) . . ? C207 C208 C209 125.9(5) . . ? C207 C208 P3 109.5(4) . . ? C209 C208 P3 124.1(4) . . ? N22 C209 C210 122.1(5) . . ? N22 C209 C208 117.2(5) . . ? C210 C209 C208 120.6(5) . . ? C209 C210 C211 119.8(6) . . ? C209 C210 H210 120.1 . . ? C211 C210 H210 120.1 . . ? C212 C211 C210 118.6(6) . . ? C212 C211 H211 120.7 . . ? C210 C211 H211 120.7 . . ? C213 C212 C211 118.4(6) . . ? C213 C212 H212 120.8 . . ? C211 C212 H212 120.8 . . ? N22 C213 C212 124.5(6) . . ? N22 C213 H213 117.8 . . ? C212 C213 H213 117.8 . . ? N21 C214 C215 121.6(5) . . ? N21 C214 C201 116.6(5) . . ? C215 C214 C201 121.8(5) . . ? C216 C215 C214 119.5(6) . . ? C216 C215 H215 120.3 . . ? C214 C215 H215 120.3 . . ? C217 C216 C215 120.2(7) . . ? C217 C216 H216 119.9 . . ? C215 C216 H216 119.9 . . ? C216 C217 C218 119.3(6) . . ? C216 C217 H217 120.3 . . ? C218 C217 H217 120.3 . . ? N21 C218 C217 122.7(6) . . ? N21 C218 H218 118.7 . . ? C217 C218 H218 118.7 . . ? C220 C219 C224 120.8(6) . . ? C220 C219 P3 118.0(5) . . ? C224 C219 P3 121.2(5) . . ? C219 C220 C221 120.3(7) . . ? C219 C220 H220 119.9 . . ? C221 C220 H220 119.9 . . ? C222 C221 C220 119.1(7) . . ? C222 C221 H221 120.4 . . ? C220 C221 H221 120.4 . . ? C223 C222 C221 120.7(7) . . ? C223 C222 H222 119.7 . . ? C221 C222 H222 119.7 . . ? C222 C223 C224 120.5(7) . . ? C222 C223 H223 119.7 . . ? C224 C223 H223 119.7 . . ? C219 C224 C223 118.5(7) . . ? C219 C224 H224 120.7 . . ? C223 C224 H224 120.7 . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.445 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 927130' ####################################################################### # # 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_sq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C148 H126 Cl0 Cu6 F12 N12 O12 P6 S10' _chemical_formula_sum 'C148 H126 Cl0 Cu6 F12 N12 O12 P6 S10' _chemical_formula_weight 3380.27 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.961(1) _cell_length_b 18.271(2) _cell_length_c 19.021(2) _cell_angle_alpha 118.348(2) _cell_angle_beta 104.380(3) _cell_angle_gamma 101.818(2) _cell_volume 4103(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 26.42 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1726 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method none _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 23008 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.42 _reflns_number_total 16408 _reflns_number_gt 10042 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0948P)^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 16408 _refine_ls_number_parameters 929 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1908 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.43653(5) 0.52864(4) 0.72532(4) 0.01962(17) Uani 1 1 d . . . Cu2 Cu 0.43905(5) 0.25595(4) 0.52633(4) 0.01836(17) Uani 1 1 d . . . P1 P 0.26475(10) 0.32359(8) 0.56190(9) 0.0146(3) Uani 1 1 d . . . P2 P 0.41341(10) 0.77231(9) 0.58365(9) 0.0141(3) Uani 1 1 d . . . P3 P 0.66225(10) 0.66519(8) 0.81413(9) 0.0147(3) Uani 1 1 d . . . S1 S 0.41003(10) 0.38583(8) 0.59849(9) 0.0201(3) Uani 1 1 d . . . S2 S 0.52409(10) 0.72786(9) 0.58264(9) 0.0185(3) Uani 1 1 d . . . S3 S 0.54326(10) 0.62804(8) 0.71073(9) 0.0182(3) Uani 1 1 d . . . S300 S 0.90490(10) 0.13104(9) 0.49082(10) 0.0221(3) Uani 1 1 d . . . S400 S 0.97245(12) 0.81712(10) 0.10197(10) 0.0282(4) Uani 1 1 d . . . N1 N 0.3007(3) 0.5352(3) 0.7052(3) 0.0208(10) Uani 1 1 d . . . N2 N 0.3188(3) 0.1428(3) 0.4693(3) 0.0170(10) Uani 1 1 d . . . N101 N 0.5664(3) 0.2649(3) 0.6027(3) 0.0228(11) Uani 1 1 d . . . N102 N 0.4913(3) 0.8316(3) 0.7870(3) 0.0163(10) Uani 1 1 d . . . N201 N 0.7246(3) 0.8333(3) 0.7819(3) 0.0196(10) Uani 1 1 d . . . N202 N 0.5047(3) 0.5196(3) 0.8257(3) 0.0205(10) Uani 1 1 d . . . C1 C 0.2215(4) 0.3769(3) 0.6465(4) 0.0186(12) Uani 1 1 d . . . C2 C 0.1945(4) 0.3201(4) 0.6719(4) 0.0214(12) Uani 1 1 d . . . C3 C 0.1608(5) 0.3420(4) 0.7453(4) 0.0312(15) Uani 1 1 d . . . H3A H 0.1987 0.4047 0.7922 0.037 Uiso 1 1 calc R . . H3B H 0.0911 0.3338 0.7247 0.037 Uiso 1 1 calc R . . C4 C 0.1731(10) 0.2853(6) 0.7799(6) 0.090(4) Uani 1 1 d . . . H4A H 0.2426 0.3096 0.8188 0.108 Uiso 1 1 calc R . . H4B H 0.1342 0.2913 0.8148 0.108 Uiso 1 1 calc R . . C5 C 0.1459(7) 0.1929(5) 0.7184(5) 0.058(2) Uani 1 1 d . . . H5A H 0.0737 0.1657 0.6903 0.070 Uiso 1 1 calc R . . H5B H 0.1672 0.1666 0.7502 0.070 Uiso 1 1 calc R . . C6 C 0.1847(5) 0.1659(4) 0.6483(4) 0.0255(13) Uani 1 1 d . . . H6A H 0.1377 0.1075 0.5977 0.031 Uiso 1 1 calc R . . H6B H 0.2471 0.1595 0.6686 0.031 Uiso 1 1 calc R . . C7 C 0.2023(4) 0.2310(3) 0.6204(3) 0.0166(11) Uani 1 1 d . . . C8 C 0.2329(4) 0.2190(3) 0.5564(3) 0.0149(11) Uani 1 1 d . . . C9 C 0.2381(4) 0.1362(3) 0.4892(3) 0.0154(11) Uani 1 1 d . . . C10 C 0.1592(4) 0.0537(3) 0.4463(3) 0.0172(11) Uani 1 1 d . . . H10 H 0.1038 0.0509 0.4603 0.021 Uiso 1 1 calc R . . C11 C 0.1638(4) -0.0231(3) 0.3836(3) 0.0221(13) Uani 1 1 d . . . H11 H 0.1116 -0.0781 0.3548 0.026 Uiso 1 1 calc R . . C12 C 0.2471(4) -0.0180(4) 0.3633(4) 0.0200(12) Uani 1 1 d . . . H12 H 0.2526 -0.0692 0.3220 0.024 Uiso 1 1 calc R . . C13 C 0.3216(4) 0.0663(3) 0.4071(3) 0.0186(12) Uani 1 1 d . . . H13 H 0.3767 0.0705 0.3928 0.022 Uiso 1 1 calc R . . C14 C 0.2171(4) 0.4663(3) 0.6800(4) 0.0220(13) Uani 1 1 d . . . C15 C 0.1292(5) 0.4778(4) 0.6819(4) 0.0359(16) Uani 1 1 d . . . H15 H 0.0730 0.4295 0.6633 0.043 Uiso 1 1 calc R . . C16 C 0.1256(6) 0.5640(4) 0.7122(5) 0.051(2) Uani 1 1 d . . . H16 H 0.0679 0.5738 0.7161 0.061 Uiso 1 1 calc R . . C17 C 0.2087(5) 0.6322(4) 0.7357(5) 0.0404(17) Uani 1 1 d . . . H17 H 0.2079 0.6890 0.7535 0.049 Uiso 1 1 calc R . . C18 C 0.2943(5) 0.6155(4) 0.7327(4) 0.0297(15) Uani 1 1 d . . . H18 H 0.3511 0.6632 0.7509 0.036 Uiso 1 1 calc R . . C19 C 0.1903(4) 0.3124(3) 0.4648(3) 0.0183(12) Uani 1 1 d . . . C20 C 0.0886(4) 0.2916(4) 0.4412(4) 0.0274(14) Uani 1 1 d . . . H20 H 0.0586 0.2812 0.4748 0.033 Uiso 1 1 calc R . . C21 C 0.0313(5) 0.2861(5) 0.3684(4) 0.0365(16) Uani 1 1 d . . . H21 H -0.0366 0.2731 0.3537 0.044 Uiso 1 1 calc R . . C22 C 0.0749(5) 0.2998(4) 0.3173(4) 0.0371(17) Uani 1 1 d . . . H22 H 0.0361 0.2959 0.2682 0.045 Uiso 1 1 calc R . . C23 C 0.1750(6) 0.3191(4) 0.3386(4) 0.0358(17) Uani 1 1 d . . . H23 H 0.2034 0.3277 0.3034 0.043 Uiso 1 1 calc R . . C24 C 0.2348(5) 0.3262(4) 0.4125(4) 0.0229(13) Uani 1 1 d . . . H24 H 0.3028 0.3397 0.4270 0.027 Uiso 1 1 calc R . . C101 C 0.6029(4) 0.1778(4) 0.4783(4) 0.0171(11) Uani 1 1 d . . . C102 C 0.5860(4) 0.0900(4) 0.4230(4) 0.0212(12) Uani 1 1 d . . . C103 C 0.5790(5) 0.0215(4) 0.4458(5) 0.0301(15) Uani 1 1 d . . . H10A H 0.6335 0.0478 0.5013 0.036 Uiso 1 1 calc R . . H10B H 0.5173 0.0085 0.4536 0.036 Uiso 1 1 calc R . . C104 C 0.5818(6) -0.0653(4) 0.3808(5) 0.048(2) Uani 1 1 d . . . H10C H 0.5583 -0.1104 0.3923 0.058 Uiso 1 1 calc R . . H10D H 0.6500 -0.0572 0.3867 0.058 Uiso 1 1 calc R . . C105 C 0.5173(6) -0.0977(4) 0.2885(5) 0.050(2) Uani 1 1 d . . . H10E H 0.5185 -0.1551 0.2482 0.060 Uiso 1 1 calc R . . H10F H 0.4490 -0.1069 0.2828 0.060 Uiso 1 1 calc R . . C106 C 0.5500(5) -0.0339(4) 0.2640(5) 0.0345(16) Uani 1 1 d . . . H10G H 0.4998 -0.0536 0.2086 0.041 Uiso 1 1 calc R . . H10H H 0.6114 -0.0356 0.2563 0.041 Uiso 1 1 calc R . . C107 C 0.5669(4) 0.0617(3) 0.3307(4) 0.0177(12) Uani 1 1 d . . . C108 C 0.4346(4) 0.8732(3) 0.6845(4) 0.0166(11) Uani 1 1 d . . . C109 C 0.4397(4) 0.8754(3) 0.7633(3) 0.0162(11) Uani 1 1 d . . . C110 C 0.3888(4) 0.9185(4) 0.8120(4) 0.0243(13) Uani 1 1 d . . . H110 H 0.3531 0.9477 0.7953 0.029 Uiso 1 1 calc R . . C111 C 0.3915(5) 0.9177(4) 0.8842(4) 0.0286(14) Uani 1 1 d . . . H111 H 0.3588 0.9475 0.9172 0.034 Uiso 1 1 calc R . . C112 C 0.4422(4) 0.8732(4) 0.9079(4) 0.0252(13) Uani 1 1 d . . . H112 H 0.4440 0.8713 0.9562 0.030 Uiso 1 1 calc R . . C113 C 0.4908(4) 0.8310(4) 0.8571(4) 0.0195(12) Uani 1 1 d . . . H113 H 0.5251 0.8003 0.8727 0.023 Uiso 1 1 calc R . . C114 C 0.6289(4) 0.2264(4) 0.5734(4) 0.0217(12) Uani 1 1 d . . . C115 C 0.7150(5) 0.2321(5) 0.6282(4) 0.0356(16) Uani 1 1 d . . . H115 H 0.7568 0.2059 0.6058 0.043 Uiso 1 1 calc R . . C116 C 0.7375(5) 0.2782(5) 0.7180(4) 0.0462(19) Uani 1 1 d . . . H116 H 0.7938 0.2820 0.7562 0.055 Uiso 1 1 calc R . . C117 C 0.6737(6) 0.3180(6) 0.7484(5) 0.047(2) Uani 1 1 d . . . H117 H 0.6870 0.3497 0.8076 0.056 Uiso 1 1 calc R . . C118 C 0.5901(5) 0.3098(4) 0.6893(4) 0.0316(15) Uani 1 1 d . . . H118 H 0.5480 0.3367 0.7104 0.038 Uiso 1 1 calc R . . C119 C 0.2972(4) 0.6866(3) 0.5491(4) 0.0183(12) Uani 1 1 d . . . C120 C 0.2958(4) 0.6067(4) 0.5444(3) 0.0220(13) Uani 1 1 d . . . H120 H 0.3546 0.5981 0.5612 0.026 Uiso 1 1 calc R . . C122 C 0.1172(5) 0.5527(4) 0.4886(4) 0.0338(15) Uani 1 1 d . . . H122 H 0.0565 0.5077 0.4679 0.041 Uiso 1 1 calc R . . C123 C 0.1189(5) 0.6310(4) 0.4936(5) 0.0378(17) Uani 1 1 d . . . H123 H 0.0592 0.6381 0.4762 0.045 Uiso 1 1 calc R . . C124 C 0.2092(4) 0.6994(4) 0.5247(4) 0.0264(14) Uani 1 1 d . . . H124 H 0.2104 0.7525 0.5290 0.032 Uiso 1 1 calc R . . C201 C 0.7345(4) 0.7841(3) 0.8801(4) 0.0183(12) Uani 1 1 d . . . C202 C 0.7336(4) 0.8185(3) 0.9605(3) 0.0185(12) Uani 1 1 d . . . C203 C 0.7728(5) 0.9175(4) 1.0303(4) 0.0319(15) Uani 1 1 d . . . H20A H 0.7298 0.9438 1.0119 0.038 Uiso 1 1 calc R . . H20B H 0.8386 0.9458 1.0355 0.038 Uiso 1 1 calc R . . C204 C 0.7796(5) 0.9389(4) 1.1191(4) 0.0306(15) Uani 1 1 d . . . H20C H 0.7875 1.0010 1.1556 0.037 Uiso 1 1 calc R . . H20D H 0.8376 0.9312 1.1466 0.037 Uiso 1 1 calc R . . C205 C 0.6860(5) 0.8774(4) 1.1110(4) 0.0324(15) Uani 1 1 d . . . H20E H 0.6273 0.8812 1.0793 0.039 Uiso 1 1 calc R . . H20F H 0.6879 0.8963 1.1686 0.039 Uiso 1 1 calc R . . C206 C 0.6806(4) 0.7800(4) 1.0625(4) 0.0261(13) Uani 1 1 d . . . H20G H 0.7371 0.7757 1.0964 0.031 Uiso 1 1 calc R . . H20H H 0.6201 0.7404 1.0555 0.031 Uiso 1 1 calc R . . C207 C 0.6815(4) 0.7510(4) 0.9738(3) 0.0180(12) Uani 1 1 d . . . C208 C 0.6379(4) 0.6655(3) 0.9022(3) 0.0171(11) Uani 1 1 d . . . C209 C 0.5906(4) 0.5838(3) 0.8970(3) 0.0182(12) Uani 1 1 d . . . C210 C 0.6347(4) 0.5700(4) 0.9608(4) 0.0217(12) Uani 1 1 d . . . H210 H 0.6940 0.6136 1.0081 0.026 Uiso 1 1 calc R . . C211 C 0.5898(5) 0.4906(4) 0.9534(4) 0.0268(14) Uani 1 1 d . . . H211 H 0.6186 0.4799 0.9952 0.032 Uiso 1 1 calc R . . C212 C 0.5023(5) 0.4287(4) 0.8833(4) 0.0309(15) Uani 1 1 d . . . H212 H 0.4697 0.3760 0.8780 0.037 Uiso 1 1 calc R . . C213 C 0.4627(4) 0.4438(4) 0.8217(4) 0.0242(13) Uani 1 1 d . . . H213 H 0.4036 0.3999 0.7742 0.029 Uiso 1 1 calc R . . C214 C 0.7836(4) 0.8341(3) 0.8480(3) 0.0183(12) Uani 1 1 d . . . C215 C 0.8865(4) 0.8785(4) 0.8855(4) 0.0253(13) Uani 1 1 d . . . H215 H 0.9260 0.8762 0.9301 0.030 Uiso 1 1 calc R . . C216 C 0.9296(4) 0.9262(4) 0.8556(4) 0.0336(16) Uani 1 1 d . . . H216 H 0.9982 0.9578 0.8807 0.040 Uiso 1 1 calc R . . C217 C 0.8678(4) 0.9258(4) 0.7871(4) 0.0296(14) Uani 1 1 d . . . H217 H 0.8944 0.9570 0.7655 0.036 Uiso 1 1 calc R . . C218 C 0.7685(4) 0.8794(4) 0.7525(4) 0.0238(13) Uani 1 1 d . . . H218 H 0.7281 0.8789 0.7063 0.029 Uiso 1 1 calc R . . C219 C 0.7394(4) 0.6016(3) 0.7852(3) 0.0185(12) Uani 1 1 d . . . C220 C 0.7039(5) 0.5219(4) 0.7045(4) 0.0260(13) Uani 1 1 d . . . H220 H 0.6394 0.4997 0.6639 0.031 Uiso 1 1 calc R . . C221 C 0.7671(5) 0.4752(4) 0.6853(4) 0.0321(15) Uani 1 1 d . . . H221 H 0.7440 0.4209 0.6318 0.039 Uiso 1 1 calc R . . C222 C 0.8632(5) 0.5090(4) 0.7448(4) 0.0350(16) Uani 1 1 d . . . H222 H 0.9043 0.4772 0.7313 0.042 Uiso 1 1 calc R . . C223 C 0.8987(5) 0.5889(4) 0.8238(4) 0.0358(16) Uani 1 1 d . . . H223 H 0.9640 0.6115 0.8633 0.043 Uiso 1 1 calc R . . C224 C 0.8373(4) 0.6369(4) 0.8451(4) 0.0265(14) Uani 1 1 d . . . H224 H 0.8613 0.6914 0.8986 0.032 Uiso 1 1 calc R . . C300 C 0.8793(4) 0.0832(4) 0.3761(4) 0.0264(14) Uani 1 1 d . . . C400 C 1.0717(6) 0.7777(5) 0.1181(5) 0.049(2) Uani 1 1 d . . . Cu3 Cu 0.57459(5) 0.77179(4) 0.72819(4) 0.01880(17) Uani 1 1 d . . . O300 O 0.9541(3) 0.0784(3) 0.5089(3) 0.0322(10) Uani 1 1 d . . . O301 O 0.9664(3) 0.2239(3) 0.5334(3) 0.0302(10) Uani 1 1 d . . . O302 O 0.8061(3) 0.1159(3) 0.4903(3) 0.0335(11) Uani 1 1 d . . . O400 O 0.9855(3) 0.8445(3) 0.0448(3) 0.0379(11) Uani 1 1 d . . . O401 O 0.9920(3) 0.8879(3) 0.1889(3) 0.0374(11) Uani 1 1 d . . . O402 O 0.8835(3) 0.7384(3) 0.0617(3) 0.0423(12) Uani 1 1 d . . . F300 F 0.8173(3) -0.0027(2) 0.3266(3) 0.0449(10) Uani 1 1 d . . . F301 F 0.8355(3) 0.1264(3) 0.3463(2) 0.0411(9) Uani 1 1 d . . . F302 F 0.9615(3) 0.0870(2) 0.3601(2) 0.0384(9) Uani 1 1 d . . . F400 F 1.0714(4) 0.7503(4) 0.1721(4) 0.0774(16) Uani 1 1 d . . . F401 F 1.0639(4) 0.7084(3) 0.0420(3) 0.0721(15) Uani 1 1 d . . . F402 F 1.1615(3) 0.8420(4) 0.1527(3) 0.0697(15) Uani 1 1 d . . . C121 C 0.2033(5) 0.5411(4) 0.5136(4) 0.0298(15) Uani 1 1 d . . . H121 H 0.2007 0.4882 0.5102 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0199(4) 0.0172(3) 0.0219(4) 0.0126(3) 0.0064(3) 0.0050(3) Cu2 0.0157(3) 0.0184(3) 0.0221(4) 0.0108(3) 0.0104(3) 0.0065(3) P1 0.0163(7) 0.0130(6) 0.0171(7) 0.0094(6) 0.0085(6) 0.0051(5) P2 0.0164(7) 0.0172(6) 0.0163(7) 0.0120(6) 0.0095(6) 0.0089(5) P3 0.0184(7) 0.0130(6) 0.0131(7) 0.0080(6) 0.0063(6) 0.0049(5) S1 0.0163(7) 0.0154(6) 0.0261(7) 0.0092(6) 0.0114(6) 0.0038(5) S2 0.0185(7) 0.0276(7) 0.0213(7) 0.0178(6) 0.0116(6) 0.0145(6) S3 0.0193(7) 0.0165(6) 0.0156(6) 0.0104(6) 0.0028(6) 0.0023(5) S300 0.0199(7) 0.0252(7) 0.0288(8) 0.0182(7) 0.0123(6) 0.0104(6) S400 0.0290(8) 0.0303(8) 0.0251(8) 0.0170(7) 0.0082(7) 0.0102(7) N1 0.026(3) 0.020(2) 0.018(2) 0.010(2) 0.011(2) 0.011(2) N2 0.017(2) 0.020(2) 0.021(2) 0.015(2) 0.009(2) 0.0068(19) N101 0.021(3) 0.034(3) 0.029(3) 0.023(2) 0.018(2) 0.014(2) N102 0.018(2) 0.022(2) 0.017(2) 0.014(2) 0.010(2) 0.0095(19) N201 0.021(2) 0.018(2) 0.023(2) 0.013(2) 0.010(2) 0.009(2) N202 0.027(3) 0.021(2) 0.014(2) 0.011(2) 0.009(2) 0.009(2) C1 0.012(3) 0.022(3) 0.022(3) 0.012(2) 0.008(2) 0.008(2) C2 0.016(3) 0.027(3) 0.020(3) 0.014(3) 0.007(2) 0.006(2) C3 0.044(4) 0.030(3) 0.026(3) 0.014(3) 0.025(3) 0.015(3) C4 0.207(13) 0.063(6) 0.085(7) 0.064(6) 0.117(9) 0.074(7) C5 0.106(7) 0.056(5) 0.045(5) 0.041(4) 0.048(5) 0.032(5) C6 0.031(3) 0.022(3) 0.026(3) 0.015(3) 0.012(3) 0.008(3) C7 0.016(3) 0.016(2) 0.015(3) 0.009(2) 0.002(2) 0.005(2) C8 0.014(3) 0.017(2) 0.018(3) 0.013(2) 0.006(2) 0.006(2) C9 0.025(3) 0.018(2) 0.016(3) 0.016(2) 0.009(2) 0.011(2) C10 0.016(3) 0.023(3) 0.017(3) 0.016(2) 0.004(2) 0.006(2) C11 0.031(3) 0.007(2) 0.017(3) 0.005(2) 0.001(2) 0.002(2) C12 0.027(3) 0.021(3) 0.017(3) 0.012(2) 0.010(2) 0.012(2) C13 0.025(3) 0.019(3) 0.020(3) 0.011(2) 0.015(2) 0.012(2) C14 0.018(3) 0.017(3) 0.020(3) 0.004(2) 0.006(2) 0.003(2) C15 0.027(3) 0.028(3) 0.043(4) 0.013(3) 0.018(3) 0.007(3) C16 0.041(4) 0.032(4) 0.075(6) 0.017(4) 0.035(4) 0.023(3) C17 0.039(4) 0.026(3) 0.053(5) 0.018(3) 0.017(4) 0.018(3) C18 0.029(3) 0.014(3) 0.034(4) 0.006(3) 0.010(3) 0.009(2) C19 0.026(3) 0.012(2) 0.020(3) 0.011(2) 0.008(2) 0.008(2) C20 0.026(3) 0.032(3) 0.024(3) 0.019(3) 0.008(3) 0.001(3) C21 0.027(3) 0.048(4) 0.042(4) 0.036(4) 0.009(3) 0.007(3) C22 0.049(4) 0.034(3) 0.033(4) 0.027(3) 0.007(3) 0.015(3) C23 0.070(5) 0.031(3) 0.027(3) 0.022(3) 0.031(4) 0.027(3) C24 0.032(3) 0.026(3) 0.023(3) 0.017(3) 0.018(3) 0.016(3) C101 0.007(2) 0.028(3) 0.030(3) 0.021(3) 0.012(2) 0.012(2) C102 0.015(3) 0.038(3) 0.034(3) 0.031(3) 0.018(3) 0.014(2) C103 0.028(3) 0.041(4) 0.055(4) 0.044(4) 0.025(3) 0.018(3) C104 0.061(5) 0.033(4) 0.060(5) 0.038(4) 0.017(4) 0.014(4) C105 0.055(5) 0.023(3) 0.068(6) 0.026(4) 0.024(4) 0.008(3) C106 0.050(4) 0.028(3) 0.043(4) 0.026(3) 0.028(4) 0.020(3) C107 0.014(3) 0.015(2) 0.032(3) 0.016(2) 0.014(2) 0.007(2) C108 0.013(3) 0.016(2) 0.025(3) 0.014(2) 0.010(2) 0.003(2) C109 0.011(3) 0.016(2) 0.018(3) 0.009(2) 0.004(2) 0.000(2) C110 0.030(3) 0.027(3) 0.027(3) 0.018(3) 0.016(3) 0.017(3) C111 0.038(4) 0.025(3) 0.033(4) 0.016(3) 0.025(3) 0.016(3) C112 0.029(3) 0.023(3) 0.025(3) 0.013(3) 0.013(3) 0.009(3) C113 0.016(3) 0.026(3) 0.021(3) 0.016(3) 0.007(2) 0.007(2) C114 0.019(3) 0.036(3) 0.019(3) 0.019(3) 0.010(2) 0.012(3) C115 0.030(4) 0.064(4) 0.035(4) 0.035(4) 0.017(3) 0.034(3) C116 0.043(4) 0.078(5) 0.029(4) 0.034(4) 0.010(3) 0.033(4) C117 0.057(5) 0.085(6) 0.037(4) 0.044(4) 0.032(4) 0.050(5) C118 0.036(4) 0.046(4) 0.025(3) 0.023(3) 0.021(3) 0.019(3) C119 0.019(3) 0.017(2) 0.020(3) 0.009(2) 0.012(2) 0.007(2) C120 0.025(3) 0.022(3) 0.014(3) 0.010(2) 0.004(2) 0.006(2) C122 0.026(3) 0.027(3) 0.037(4) 0.015(3) 0.009(3) 0.000(3) C123 0.018(3) 0.027(3) 0.057(5) 0.016(3) 0.016(3) 0.006(3) C124 0.024(3) 0.018(3) 0.032(3) 0.009(3) 0.012(3) 0.011(2) C201 0.016(3) 0.015(2) 0.022(3) 0.012(2) 0.004(2) 0.006(2) C202 0.020(3) 0.021(3) 0.015(3) 0.008(2) 0.006(2) 0.015(2) C203 0.031(3) 0.023(3) 0.030(3) 0.007(3) 0.012(3) 0.008(3) C204 0.030(3) 0.022(3) 0.022(3) 0.003(3) 0.007(3) 0.008(3) C205 0.041(4) 0.037(3) 0.019(3) 0.011(3) 0.015(3) 0.021(3) C206 0.026(3) 0.033(3) 0.020(3) 0.015(3) 0.008(3) 0.015(3) C207 0.017(3) 0.025(3) 0.019(3) 0.016(2) 0.007(2) 0.012(2) C208 0.013(3) 0.023(3) 0.016(3) 0.011(2) 0.005(2) 0.010(2) C209 0.027(3) 0.016(2) 0.019(3) 0.012(2) 0.013(2) 0.011(2) C210 0.028(3) 0.025(3) 0.014(3) 0.011(2) 0.009(2) 0.011(2) C211 0.039(4) 0.035(3) 0.028(3) 0.027(3) 0.018(3) 0.023(3) C212 0.038(4) 0.032(3) 0.030(3) 0.024(3) 0.014(3) 0.009(3) C213 0.026(3) 0.020(3) 0.022(3) 0.012(3) 0.007(3) 0.002(2) C214 0.025(3) 0.010(2) 0.013(3) 0.004(2) 0.004(2) 0.003(2) C215 0.016(3) 0.023(3) 0.030(3) 0.014(3) 0.003(3) 0.005(2) C216 0.016(3) 0.028(3) 0.048(4) 0.020(3) 0.012(3) -0.004(3) C217 0.025(3) 0.032(3) 0.041(4) 0.028(3) 0.013(3) 0.007(3) C218 0.031(3) 0.023(3) 0.027(3) 0.019(3) 0.013(3) 0.011(3) C219 0.022(3) 0.016(2) 0.018(3) 0.010(2) 0.010(2) 0.005(2) C220 0.029(3) 0.023(3) 0.022(3) 0.009(3) 0.012(3) 0.010(3) C221 0.044(4) 0.027(3) 0.027(3) 0.011(3) 0.023(3) 0.018(3) C222 0.036(4) 0.039(4) 0.045(4) 0.024(3) 0.026(3) 0.026(3) C223 0.030(3) 0.042(4) 0.025(3) 0.010(3) 0.005(3) 0.024(3) C224 0.029(3) 0.033(3) 0.021(3) 0.014(3) 0.008(3) 0.021(3) C300 0.029(3) 0.021(3) 0.029(3) 0.014(3) 0.011(3) 0.010(3) C400 0.047(5) 0.060(5) 0.033(4) 0.023(4) 0.011(4) 0.019(4) Cu3 0.0173(3) 0.0234(3) 0.0224(4) 0.0155(3) 0.0101(3) 0.0099(3) O300 0.037(3) 0.041(2) 0.041(3) 0.033(2) 0.019(2) 0.024(2) O301 0.033(2) 0.026(2) 0.030(2) 0.015(2) 0.014(2) 0.0071(19) O302 0.021(2) 0.035(2) 0.051(3) 0.024(2) 0.021(2) 0.0138(19) O400 0.042(3) 0.046(3) 0.031(2) 0.030(2) 0.009(2) 0.009(2) O401 0.040(3) 0.033(2) 0.030(2) 0.013(2) 0.014(2) 0.010(2) O402 0.028(3) 0.045(3) 0.035(3) 0.019(2) 0.009(2) -0.005(2) F300 0.053(3) 0.034(2) 0.040(2) 0.0178(19) 0.017(2) 0.0111(19) F301 0.052(2) 0.049(2) 0.039(2) 0.032(2) 0.018(2) 0.030(2) F302 0.045(2) 0.046(2) 0.042(2) 0.029(2) 0.026(2) 0.0258(19) F400 0.083(4) 0.115(4) 0.087(4) 0.084(4) 0.035(3) 0.062(3) F401 0.065(3) 0.072(3) 0.060(3) 0.018(3) 0.020(3) 0.044(3) F402 0.027(2) 0.107(4) 0.044(3) 0.029(3) 0.008(2) 0.011(2) C121 0.032(4) 0.014(3) 0.038(4) 0.013(3) 0.014(3) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.012(5) . ? Cu1 N202 2.028(5) . ? Cu1 S3 2.3315(15) . ? Cu1 S1 2.4307(15) . ? Cu2 N101 2.010(5) . ? Cu2 N2 2.016(4) . ? Cu2 S1 2.3084(16) . ? Cu2 S2 2.4022(16) 2_666 ? P1 C19 1.794(6) . ? P1 C1 1.801(5) . ? P1 C8 1.817(5) . ? P1 S1 1.997(2) . ? P2 C101 1.801(6) 2_666 ? P2 C119 1.802(5) . ? P2 C108 1.811(5) . ? P2 S2 1.988(2) . ? P3 C208 1.798(6) . ? P3 C201 1.799(5) . ? P3 C219 1.801(6) . ? P3 S3 1.999(2) . ? S2 Cu3 2.3414(17) . ? S2 Cu2 2.4023(16) 2_666 ? S3 Cu3 2.4121(16) . ? S300 O300 1.436(4) . ? S300 O301 1.438(4) . ? S300 O302 1.443(4) . ? S300 C300 1.818(6) . ? S400 O400 1.433(5) . ? S400 O401 1.437(5) . ? S400 O402 1.445(4) . ? S400 C400 1.799(8) . ? N1 C18 1.337(7) . ? N1 C14 1.365(7) . ? N2 C9 1.351(7) . ? N2 C13 1.354(6) . ? N101 C118 1.348(7) . ? N101 C114 1.355(7) . ? N102 C113 1.342(7) . ? N102 C109 1.364(7) . ? N102 Cu3 2.021(4) . ? N201 C214 1.338(7) . ? N201 C218 1.361(7) . ? N201 Cu3 2.020(5) . ? N202 C213 1.358(7) . ? N202 C209 1.368(7) . ? C1 C2 1.369(8) . ? C1 C14 1.468(7) . ? C2 C7 1.499(8) . ? C2 C3 1.505(8) . ? C3 C4 1.485(11) . ? C4 C5 1.412(11) . ? C5 C6 1.495(9) . ? C6 C7 1.519(8) . ? C7 C8 1.342(7) . ? C8 C9 1.481(7) . ? C9 C10 1.398(7) . ? C10 C11 1.374(7) . ? C11 C12 1.391(8) . ? C12 C13 1.387(7) . ? C14 C15 1.380(8) . ? C15 C16 1.415(9) . ? C16 C17 1.364(9) . ? C17 C18 1.386(9) . ? C19 C20 1.388(8) . ? C19 C24 1.412(8) . ? C20 C21 1.380(9) . ? C21 C22 1.383(9) . ? C22 C23 1.370(10) . ? C23 C24 1.397(9) . ? C101 C102 1.358(8) . ? C101 C114 1.482(8) . ? C101 P2 1.801(6) 2_666 ? C102 C103 1.501(8) . ? C102 C107 1.502(8) . ? C103 C104 1.496(9) . ? C104 C105 1.516(11) . ? C105 C106 1.486(9) . ? C106 C107 1.510(8) . ? C107 C108 1.354(7) 2_666 ? C108 C107 1.354(7) 2_666 ? C108 C109 1.464(8) . ? C109 C110 1.400(8) . ? C110 C111 1.371(8) . ? C111 C112 1.367(9) . ? C112 C113 1.388(8) . ? C114 C115 1.388(8) . ? C115 C116 1.404(9) . ? C116 C117 1.391(10) . ? C117 C118 1.384(9) . ? C119 C124 1.390(8) . ? C119 C120 1.415(8) . ? C120 C121 1.395(8) . ? C122 C121 1.354(9) . ? C122 C123 1.382(9) . ? C123 C124 1.396(8) . ? C201 C202 1.355(8) . ? C201 C214 1.490(8) . ? C202 C207 1.480(8) . ? C202 C203 1.509(7) . ? C203 C204 1.512(9) . ? C204 C205 1.527(9) . ? C205 C206 1.540(8) . ? C206 C207 1.513(8) . ? C207 C208 1.358(7) . ? C208 C209 1.461(7) . ? C209 C210 1.390(8) . ? C210 C211 1.392(8) . ? C211 C212 1.366(9) . ? C212 C213 1.352(9) . ? C214 C215 1.390(8) . ? C215 C216 1.386(9) . ? C216 C217 1.394(9) . ? C217 C218 1.351(8) . ? C219 C220 1.384(7) . ? C219 C224 1.396(8) . ? C220 C221 1.401(8) . ? C221 C222 1.376(9) . ? C222 C223 1.369(9) . ? C223 C224 1.397(8) . ? C300 F300 1.334(6) . ? C300 F302 1.335(7) . ? C300 F301 1.351(7) . ? C400 F400 1.339(9) . ? C400 F402 1.341(9) . ? C400 F401 1.352(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 N1 Cu1 N202 119.27(19) . . ? N1 Cu1 S3 113.19(14) . . ? N202 Cu1 S3 113.43(14) . . ? N1 Cu1 S1 104.83(13) . . ? N202 Cu1 S1 102.57(13) . . ? S3 Cu1 S1 100.53(6) . . ? N101 Cu2 N2 116.38(19) . . ? N101 Cu2 S1 110.09(14) . . ? N2 Cu2 S1 113.53(13) . . ? N101 Cu2 S2 105.72(13) . 2_666 ? N2 Cu2 S2 110.20(13) . 2_666 ? S1 Cu2 S2 99.27(6) . 2_666 ? C19 P1 C1 109.9(3) . . ? C19 P1 C8 113.0(2) . . ? C1 P1 C8 93.4(2) . . ? C19 P1 S1 111.9(2) . . ? C1 P1 S1 113.07(18) . . ? C8 P1 S1 114.31(18) . . ? C101 P2 C119 110.2(3) 2_666 . ? C101 P2 C108 93.7(3) 2_666 . ? C119 P2 C108 109.0(2) . . ? C101 P2 S2 113.60(17) 2_666 . ? C119 P2 S2 112.26(19) . . ? C108 P2 S2 116.60(19) . . ? C208 P3 C201 93.3(3) . . ? C208 P3 C219 108.8(3) . . ? C201 P3 C219 111.2(3) . . ? C208 P3 S3 116.26(18) . . ? C201 P3 S3 113.04(19) . . ? C219 P3 S3 112.67(19) . . ? P1 S1 Cu2 95.43(7) . . ? P1 S1 Cu1 98.52(7) . . ? Cu2 S1 Cu1 154.79(8) . . ? P2 S2 Cu3 94.18(7) . . ? P2 S2 Cu2 99.19(7) . 2_666 ? Cu3 S2 Cu2 148.77(7) . 2_666 ? P3 S3 Cu1 94.69(7) . . ? P3 S3 Cu3 98.21(6) . . ? Cu1 S3 Cu3 140.72(7) . . ? O300 S300 O301 115.4(3) . . ? O300 S300 O302 115.9(3) . . ? O301 S300 O302 114.4(3) . . ? O300 S300 C300 102.3(3) . . ? O301 S300 C300 104.1(3) . . ? O302 S300 C300 102.0(3) . . ? O400 S400 O401 115.9(3) . . ? O400 S400 O402 113.8(3) . . ? O401 S400 O402 114.9(3) . . ? O400 S400 C400 103.1(3) . . ? O401 S400 C400 103.3(3) . . ? O402 S400 C400 103.4(3) . . ? C18 N1 C14 117.1(5) . . ? C18 N1 Cu1 118.2(4) . . ? C14 N1 Cu1 123.5(4) . . ? C9 N2 C13 117.6(4) . . ? C9 N2 Cu2 126.2(4) . . ? C13 N2 Cu2 116.1(4) . . ? C118 N101 C114 117.2(5) . . ? C118 N101 Cu2 117.9(4) . . ? C114 N101 Cu2 124.8(4) . . ? C113 N102 C109 117.9(5) . . ? C113 N102 Cu3 116.7(4) . . ? C109 N102 Cu3 125.3(4) . . ? C214 N201 C218 117.7(5) . . ? C214 N201 Cu3 122.9(4) . . ? C218 N201 Cu3 119.3(4) . . ? C213 N202 C209 117.2(5) . . ? C213 N202 Cu1 117.7(4) . . ? C209 N202 Cu1 125.1(4) . . ? C2 C1 C14 127.7(5) . . ? C2 C1 P1 108.5(4) . . ? C14 C1 P1 123.9(4) . . ? C1 C2 C7 114.1(5) . . ? C1 C2 C3 125.1(5) . . ? C7 C2 C3 120.8(5) . . ? C4 C3 C2 112.8(6) . . ? C5 C4 C3 117.1(8) . . ? C4 C5 C6 118.5(7) . . ? C5 C6 C7 114.8(5) . . ? C8 C7 C2 115.4(5) . . ? C8 C7 C6 125.3(5) . . ? C2 C7 C6 119.0(5) . . ? C7 C8 C9 128.2(5) . . ? C7 C8 P1 108.2(4) . . ? C9 C8 P1 123.5(4) . . ? N2 C9 C10 121.5(5) . . ? N2 C9 C8 118.7(4) . . ? C10 C9 C8 119.8(5) . . ? C11 C10 C9 119.8(5) . . ? C10 C11 C12 119.6(5) . . ? C13 C12 C11 117.5(5) . . ? N2 C13 C12 123.9(5) . . ? N1 C14 C15 122.1(5) . . ? N1 C14 C1 117.9(5) . . ? C15 C14 C1 120.0(5) . . ? C14 C15 C16 119.3(6) . . ? C17 C16 C15 118.4(6) . . ? C16 C17 C18 118.8(6) . . ? N1 C18 C17 124.3(6) . . ? C20 C19 C24 119.4(5) . . ? C20 C19 P1 120.2(4) . . ? C24 C19 P1 120.5(4) . . ? C21 C20 C19 120.6(6) . . ? C20 C21 C22 120.1(6) . . ? C23 C22 C21 120.5(6) . . ? C22 C23 C24 120.6(6) . . ? C23 C24 C19 118.9(6) . . ? C102 C101 C114 127.1(5) . . ? C102 C101 P2 108.4(4) . 2_666 ? C114 C101 P2 124.4(4) . 2_666 ? C101 C102 C103 125.6(5) . . ? C101 C102 C107 114.6(5) . . ? C103 C102 C107 119.7(5) . . ? C104 C103 C102 115.8(6) . . ? C103 C104 C105 110.9(6) . . ? C106 C105 C104 113.2(6) . . ? C105 C106 C107 113.4(6) . . ? C108 C107 C102 114.8(5) 2_666 . ? C108 C107 C106 125.9(5) 2_666 . ? C102 C107 C106 119.2(5) . . ? C107 C108 C109 128.5(5) 2_666 . ? C107 C108 P2 108.2(4) 2_666 . ? C109 C108 P2 122.9(4) . . ? N102 C109 C110 120.1(5) . . ? N102 C109 C108 119.2(5) . . ? C110 C109 C108 120.6(5) . . ? C111 C110 C109 120.2(5) . . ? C112 C111 C110 120.1(6) . . ? C111 C112 C113 117.5(6) . . ? N102 C113 C112 124.1(5) . . ? N101 C114 C115 123.1(5) . . ? N101 C114 C101 116.9(5) . . ? C115 C114 C101 120.0(5) . . ? C114 C115 C116 118.7(6) . . ? C117 C116 C115 118.4(6) . . ? C118 C117 C116 119.0(6) . . ? N101 C118 C117 123.5(6) . . ? C124 C119 C120 120.8(5) . . ? C124 C119 P2 118.6(4) . . ? C120 C119 P2 120.5(4) . . ? C121 C120 C119 117.9(5) . . ? C121 C122 C123 120.5(6) . . ? C122 C123 C124 120.6(6) . . ? C119 C124 C123 118.6(5) . . ? C202 C201 C214 127.3(5) . . ? C202 C201 P3 108.6(4) . . ? C214 C201 P3 124.1(4) . . ? C201 C202 C207 114.7(5) . . ? C201 C202 C203 124.6(5) . . ? C207 C202 C203 120.5(5) . . ? C202 C203 C204 114.5(5) . . ? C203 C204 C205 110.7(5) . . ? C204 C205 C206 109.3(5) . . ? C207 C206 C205 110.3(5) . . ? C208 C207 C202 114.8(5) . . ? C208 C207 C206 125.3(5) . . ? C202 C207 C206 119.9(5) . . ? C207 C208 C209 127.6(5) . . ? C207 C208 P3 108.5(4) . . ? C209 C208 P3 123.4(4) . . ? N202 C209 C210 121.2(5) . . ? N202 C209 C208 118.2(5) . . ? C210 C209 C208 120.5(5) . . ? C209 C210 C211 119.7(5) . . ? C212 C211 C210 118.2(6) . . ? C213 C212 C211 120.3(6) . . ? C212 C213 N202 123.3(5) . . ? N201 C214 C215 122.1(5) . . ? N201 C214 C201 117.2(5) . . ? C215 C214 C201 120.7(5) . . ? C216 C215 C214 119.3(6) . . ? C215 C216 C217 118.4(5) . . ? C218 C217 C216 119.1(6) . . ? C217 C218 N201 123.4(6) . . ? C220 C219 C224 120.9(5) . . ? C220 C219 P3 121.0(5) . . ? C224 C219 P3 118.1(4) . . ? C219 C220 C221 118.6(6) . . ? C222 C221 C220 120.6(6) . . ? C223 C222 C221 120.6(6) . . ? C222 C223 C224 120.2(6) . . ? C219 C224 C223 119.0(5) . . ? F300 C300 F302 107.4(5) . . ? F300 C300 F301 106.5(5) . . ? F302 C300 F301 106.5(5) . . ? F300 C300 S300 111.4(4) . . ? F302 C300 S300 112.8(4) . . ? F301 C300 S300 111.9(4) . . ? F400 C400 F402 107.4(6) . . ? F400 C400 F401 108.0(7) . . ? F402 C400 F401 106.5(6) . . ? F400 C400 S400 111.1(5) . . ? F402 C400 S400 112.0(6) . . ? F401 C400 S400 111.7(5) . . ? N201 Cu3 N102 120.53(18) . . ? N201 Cu3 S2 105.70(14) . . ? N102 Cu3 S2 113.03(13) . . ? N201 Cu3 S3 105.15(13) . . ? N102 Cu3 S3 109.53(13) . . ? S2 Cu3 S3 100.88(5) . . ? C122 C121 C120 121.5(6) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.663 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.145 _database_code_depnum_ccdc_archive 'CCDC 927131' ####################################################################### # # 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_sq3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H126 Cl0 Cu6 F0 N12 O0 P6 S0 Se6' _chemical_formula_sum 'C144 H126 Cl0 Cu6 F0 N12 O0 P6 S0 Se6' _chemical_formula_weight 3065.39 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' P P 0.1023 0.0942 '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' Se Se -0.0929 2.2259 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.136(3) _cell_length_b 33.131(6) _cell_length_c 17.782(9) _cell_angle_alpha 90 _cell_angle_beta 107.947(9) _cell_angle_gamma 90 _cell_volume 9604(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.23 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3084 _exptl_absorpt_coefficient_mu 1.878 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method none _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 51706 _diffrn_reflns_av_R_equivalents 0.1532 _diffrn_reflns_av_sigmaI/netI 0.3536 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 21602 _reflns_number_gt 7148 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^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 21602 _refine_ls_number_parameters 759 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1880 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 0.782 _refine_ls_restrained_S_all 0.782 _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 0.28458(6) 0.03409(3) 0.10041(6) 0.0268(3) Uani 1 1 d . . . Cu2 Cu 0.46530(6) -0.08256(3) 0.18899(6) 0.0292(3) Uani 1 1 d . . . Cu3 Cu 0.27039(6) 0.09629(3) -0.15291(6) 0.0308(3) Uani 1 1 d . . . Se1 Se 0.26130(5) 0.07087(3) -0.02639(5) 0.0290(2) Uani 1 1 d . . . Se2 Se 0.37283(5) -0.02363(3) 0.10333(5) 0.0240(2) Uani 1 1 d . . . Se3 Se 0.59781(5) -0.06320(3) 0.16560(5) 0.0267(2) Uani 1 1 d . . . P1 P 0.33035(13) 0.12072(7) 0.03638(12) 0.0230(5) Uani 1 1 d . . . P2 P 0.26330(13) -0.05967(7) 0.06817(12) 0.0231(5) Uani 1 1 d . . . P3 P 0.65027(13) -0.04932(7) 0.28917(12) 0.0221(5) Uani 1 1 d . . . N1 N 0.2937(4) 0.1553(2) -0.1470(4) 0.0306(18) Uani 1 1 d . . . N2 N 0.3384(4) 0.0711(2) 0.1971(4) 0.0309(18) Uani 1 1 d . . . N11 N 0.1667(4) 0.0214(2) 0.0931(4) 0.0237(16) Uani 1 1 d . . . N12 N 0.4232(4) -0.13007(18) 0.1174(4) 0.0177(15) Uiso 1 1 d . . . N21 N 0.4620(4) -0.0696(2) 0.2985(4) 0.0244(17) Uani 1 1 d . . . N22 N 0.1756(4) 0.0694(2) -0.2342(3) 0.0241(16) Uani 1 1 d . . . C1 C 0.2954(5) 0.1691(3) -0.0085(5) 0.026(2) Uiso 1 1 d . . . C2 C 0.2583(5) 0.1890(2) 0.0352(5) 0.0218(19) Uani 1 1 d . . . C3 C 0.2048(5) 0.2259(3) 0.0098(5) 0.037(2) Uani 1 1 d . . . H3A H 0.1506 0.2177 -0.0229 0.044 Uiso 1 1 calc R . . H3B H 0.2281 0.2433 -0.0216 0.044 Uiso 1 1 calc R . . C4 C 0.1975(6) 0.2497(3) 0.0833(6) 0.050(3) Uani 1 1 d . . . H4A H 0.2490 0.2634 0.1084 0.060 Uiso 1 1 calc R . . H4B H 0.1553 0.2702 0.0655 0.060 Uiso 1 1 calc R . . C5 C 0.1767(6) 0.2234(3) 0.1440(5) 0.046(3) Uani 1 1 d . . . H5A H 0.1263 0.2087 0.1191 0.055 Uiso 1 1 calc R . . H5B H 0.1680 0.2402 0.1854 0.055 Uiso 1 1 calc R . . C6 C 0.2456(6) 0.1936(3) 0.1800(5) 0.041(3) Uani 1 1 d . . . H6A H 0.2279 0.1746 0.2131 0.050 Uiso 1 1 calc R . . H6B H 0.2927 0.2081 0.2134 0.050 Uiso 1 1 calc R . . C7 C 0.2713(5) 0.1698(3) 0.1158(5) 0.028(2) Uani 1 1 d . . . C8 C 0.3085(4) 0.1344(2) 0.1263(4) 0.0199(19) Uani 1 1 d . . . C9 C 0.3411(5) 0.1106(3) 0.2010(5) 0.022(2) Uani 1 1 d . . . C10 C 0.3798(5) 0.1300(3) 0.2697(5) 0.035(2) Uani 1 1 d . . . H10 H 0.3860 0.1579 0.2704 0.042 Uiso 1 1 calc R . . C11 C 0.4103(5) 0.1075(3) 0.3399(5) 0.043(3) Uani 1 1 d . . . H11 H 0.4334 0.1204 0.3881 0.051 Uiso 1 1 calc R . . C12 C 0.4055(6) 0.0667(3) 0.3364(5) 0.045(3) Uani 1 1 d . . . H12 H 0.4249 0.0510 0.3816 0.053 Uiso 1 1 calc R . . C13 C 0.3706(5) 0.0492(3) 0.2627(4) 0.037(3) Uani 1 1 d . . . H13 H 0.3695 0.0212 0.2588 0.044 Uiso 1 1 calc R . . C14 C 0.3080(5) 0.1825(3) -0.0849(5) 0.030(2) Uani 1 1 d . . . C15 C 0.3355(5) 0.2216(3) -0.0881(5) 0.037(2) Uani 1 1 d . . . H15 H 0.3440 0.2387 -0.0447 0.044 Uiso 1 1 calc R . . C16 C 0.3505(6) 0.2354(3) -0.1566(5) 0.040(3) Uani 1 1 d . . . H16 H 0.3694 0.2615 -0.1594 0.048 Uiso 1 1 calc R . . C17 C 0.3369(6) 0.2097(3) -0.2196(6) 0.053(3) Uani 1 1 d . . . H17 H 0.3464 0.2180 -0.2659 0.064 Uiso 1 1 calc R . . C18 C 0.3087(5) 0.1712(3) -0.2129(5) 0.039(2) Uani 1 1 d . . . H18 H 0.2989 0.1545 -0.2569 0.046 Uiso 1 1 calc R . . C19 C 0.4391(5) 0.1159(3) 0.0601(4) 0.025(2) Uani 1 1 d . . . C20 C 0.4739(5) 0.0805(2) 0.0404(5) 0.025(2) Uiso 1 1 d . . . H20 H 0.4409 0.0595 0.0136 0.030 Uiso 1 1 calc R . . C21 C 0.5608(6) 0.0777(3) 0.0625(5) 0.040(3) Uani 1 1 d . . . H21 H 0.5849 0.0543 0.0508 0.048 Uiso 1 1 calc R . . C22 C 0.6099(6) 0.1091(3) 0.1010(6) 0.041(3) Uani 1 1 d . . . H22 H 0.6666 0.1071 0.1138 0.049 Uiso 1 1 calc R . . C23 C 0.5748(5) 0.1433(3) 0.1206(5) 0.040(3) Uani 1 1 d . . . H23 H 0.6082 0.1641 0.1476 0.048 Uiso 1 1 calc R . . C24 C 0.4882(5) 0.1472(3) 0.1001(5) 0.033(2) Uani 1 1 d . . . H24 H 0.4648 0.1704 0.1132 0.039 Uiso 1 1 calc R . . C31 C 0.1872(5) -0.0497(2) 0.1174(5) 0.0230(19) Uiso 1 1 d . . . C32 C 0.1873(5) -0.0819(3) 0.1661(5) 0.029(2) Uani 1 1 d . . . C33 C 0.1362(5) -0.0853(3) 0.2231(5) 0.042(3) Uani 1 1 d . . . H33A H 0.0807 -0.0932 0.1938 0.050 Uiso 1 1 calc R . . H33B H 0.1337 -0.0590 0.2466 0.050 Uiso 1 1 calc R . . C34 C 0.1739(6) -0.1172(3) 0.2912(5) 0.043(3) Uani 1 1 d . . . H34A H 0.2263 -0.1075 0.3253 0.051 Uiso 1 1 calc R . . H34B H 0.1374 -0.1206 0.3230 0.051 Uiso 1 1 calc R . . C35 C 0.1853(6) -0.1568(3) 0.2551(6) 0.048(3) Uani 1 1 d . . . H35A H 0.1342 -0.1648 0.2164 0.058 Uiso 1 1 calc R . . H35B H 0.2003 -0.1774 0.2958 0.058 Uiso 1 1 calc R . . C36 C 0.2532(5) -0.1533(3) 0.2146(6) 0.042(3) Uani 1 1 d . . . H36A H 0.3061 -0.1511 0.2550 0.050 Uiso 1 1 calc R . . H36B H 0.2537 -0.1778 0.1847 0.050 Uiso 1 1 calc R . . C37 C 0.2413(5) -0.1172(3) 0.1596(5) 0.030(2) Uani 1 1 d . . . C38 C 0.2837(5) -0.1099(3) 0.1071(5) 0.029(2) Uani 1 1 d . . . C39 C 0.3407(5) -0.1389(3) 0.0893(5) 0.032(2) Uani 1 1 d . . . C40 C 0.3101(5) -0.1720(3) 0.0408(5) 0.038(2) Uani 1 1 d . . . H40 H 0.2540 -0.1769 0.0218 0.045 Uiso 1 1 calc R . . C41 C 0.3669(6) -0.1980(3) 0.0211(6) 0.041(3) Uani 1 1 d . . . H41 H 0.3495 -0.2203 -0.0116 0.049 Uiso 1 1 calc R . . C42 C 0.4501(5) -0.1886(3) 0.0532(5) 0.035(2) Uani 1 1 d . . . H42 H 0.4891 -0.2051 0.0423 0.042 Uiso 1 1 calc R . . C43 C 0.4737(5) -0.1571(3) 0.0981(5) 0.033(2) Uani 1 1 d . . . H43 H 0.5299 -0.1527 0.1188 0.040 Uiso 1 1 calc R . . C44 C 0.1356(5) -0.0147(3) 0.1064(4) 0.0201(19) Uani 1 1 d . . . C45 C 0.0546(5) -0.0175(3) 0.1067(4) 0.026(2) Uani 1 1 d . . . H45 H 0.0330 -0.0426 0.1132 0.031 Uiso 1 1 calc R . . C46 C 0.0071(5) 0.0158(3) 0.0977(4) 0.026(2) Uani 1 1 d . . . H46 H -0.0467 0.0132 0.0985 0.031 Uiso 1 1 calc R . . C47 C 0.0358(5) 0.0533(3) 0.0877(5) 0.036(2) Uani 1 1 d . . . H47 H 0.0037 0.0763 0.0831 0.043 Uiso 1 1 calc R . . C48 C 0.1180(4) 0.0549(2) 0.0845(4) 0.0222(19) Uani 1 1 d . . . H48 H 0.1393 0.0798 0.0762 0.027 Uiso 1 1 calc R . . C49 C 0.2177(5) -0.0625(3) -0.0382(5) 0.024(2) Uani 1 1 d . . . C50 C 0.1604(5) -0.0927(3) -0.0705(5) 0.031(2) Uani 1 1 d . . . H50 H 0.1454 -0.1111 -0.0379 0.038 Uiso 1 1 calc R . . C51 C 0.1261(6) -0.0948(3) -0.1521(6) 0.049(3) Uani 1 1 d . . . H51 H 0.0873 -0.1146 -0.1742 0.059 Uiso 1 1 calc R . . C52 C 0.1485(6) -0.0683(3) -0.2004(6) 0.047(3) Uani 1 1 d . . . H52 H 0.1257 -0.0703 -0.2550 0.057 Uiso 1 1 calc R . . C53 C 0.2042(5) -0.0390(3) -0.1682(5) 0.035(2) Uani 1 1 d . . . H53 H 0.2190 -0.0211 -0.2018 0.042 Uiso 1 1 calc R . . C54 C 0.2402(5) -0.0345(3) -0.0866(5) 0.030(2) Uani 1 1 d . . . H54 H 0.2774 -0.0140 -0.0655 0.036 Uiso 1 1 calc R . . C61 C 0.6095(5) -0.0764(2) 0.3584(4) 0.0183(18) Uani 1 1 d . . . C62 C 0.6696(5) -0.0978(3) 0.4072(4) 0.024(2) Uani 1 1 d . . . C63 C 0.6652(5) -0.1214(3) 0.4776(5) 0.033(2) Uani 1 1 d . . . H63A H 0.6101 -0.1319 0.4672 0.040 Uiso 1 1 calc R . . H63B H 0.6762 -0.1034 0.5228 0.040 Uiso 1 1 calc R . . C64 C 0.7266(6) -0.1568(3) 0.4983(6) 0.051(3) Uani 1 1 d . . . H64A H 0.7248 -0.1695 0.5468 0.061 Uiso 1 1 calc R . . H64B H 0.7115 -0.1769 0.4565 0.061 Uiso 1 1 calc R . . C65 C 0.8125(6) -0.1417(3) 0.5082(5) 0.047(3) Uani 1 1 d . . . H65A H 0.8511 -0.1639 0.5246 0.056 Uiso 1 1 calc R . . H65B H 0.8270 -0.1212 0.5491 0.056 Uiso 1 1 calc R . . C66 C 0.8182(5) -0.1240(3) 0.4306(4) 0.035(2) Uani 1 1 d . . . H66A H 0.8698 -0.1095 0.4415 0.041 Uiso 1 1 calc R . . H66B H 0.8195 -0.1461 0.3952 0.041 Uiso 1 1 calc R . . C67 C 0.7508(5) -0.0962(3) 0.3893(5) 0.027(2) Uani 1 1 d . . . C68 C 0.7513(5) -0.0702(3) 0.3322(5) 0.029(2) Uani 1 1 d . . . C69 C 0.1759(4) 0.0593(3) -0.3062(5) 0.024(2) Uani 1 1 d . . . C70 C 0.1124(5) 0.0394(3) -0.3606(5) 0.032(2) Uiso 1 1 d . . . H70 H 0.1155 0.0327 -0.4104 0.039 Uiso 1 1 calc R . . C71 C 0.0443(5) 0.0298(3) -0.3385(5) 0.047(3) Uani 1 1 d . . . H71 H 0.0005 0.0160 -0.3730 0.057 Uiso 1 1 calc R . . C72 C 0.0422(5) 0.0410(3) -0.2636(5) 0.045(3) Uani 1 1 d . . . H72 H -0.0034 0.0356 -0.2474 0.054 Uiso 1 1 calc R . . C73 C 0.1088(5) 0.0601(3) -0.2154(5) 0.038(3) Uani 1 1 d . . . H73 H 0.1075 0.0671 -0.1651 0.046 Uiso 1 1 calc R . . C74 C 0.5280(5) -0.0670(2) 0.3647(5) 0.024(2) Uani 1 1 d . . . C75 C 0.5208(5) -0.0556(3) 0.4380(5) 0.035(2) Uani 1 1 d . . . H75 H 0.5668 -0.0541 0.4825 0.043 Uiso 1 1 calc R . . C76 C 0.4416(5) -0.0466(3) 0.4429(5) 0.038(3) Uani 1 1 d . . . H76 H 0.4353 -0.0390 0.4911 0.046 Uiso 1 1 calc R . . C77 C 0.3756(5) -0.0489(3) 0.3781(5) 0.034(2) Uani 1 1 d . . . H77 H 0.3234 -0.0429 0.3805 0.041 Uiso 1 1 calc R . . C78 C 0.3877(5) -0.0607(3) 0.3072(5) 0.029(2) Uani 1 1 d . . . H78 H 0.3418 -0.0627 0.2627 0.035 Uiso 1 1 calc R . . C79 C 0.6440(5) 0.0038(3) 0.3075(4) 0.025(2) Uani 1 1 d . . . C80 C 0.6932(6) 0.0193(3) 0.3819(6) 0.050(3) Uani 1 1 d . . . H80 H 0.7300 0.0025 0.4176 0.060 Uiso 1 1 calc R . . C81 C 0.6863(7) 0.0593(4) 0.4010(6) 0.060(3) Uani 1 1 d . . . H81 H 0.7171 0.0691 0.4502 0.071 Uiso 1 1 calc R . . C82 C 0.6321(7) 0.0853(3) 0.3455(7) 0.062(3) Uani 1 1 d . . . H82 H 0.6287 0.1125 0.3567 0.074 Uiso 1 1 calc R . . C83 C 0.5853(7) 0.0695(3) 0.2757(7) 0.055(3) Uani 1 1 d . . . H83 H 0.5479 0.0861 0.2401 0.066 Uiso 1 1 calc R . . C84 C 0.5916(5) 0.0293(3) 0.2557(5) 0.037(2) Uani 1 1 d . . . H84 H 0.5598 0.0198 0.2067 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0248(6) 0.0337(7) 0.0213(6) 0.0003(5) 0.0062(4) -0.0006(5) Cu2 0.0235(6) 0.0459(8) 0.0170(6) -0.0062(5) 0.0043(4) 0.0009(5) Cu3 0.0341(7) 0.0413(7) 0.0173(6) -0.0017(5) 0.0082(5) -0.0023(6) Se1 0.0403(6) 0.0297(6) 0.0166(5) -0.0020(4) 0.0082(4) -0.0042(4) Se2 0.0189(4) 0.0322(6) 0.0207(5) 0.0004(4) 0.0056(3) -0.0002(4) Se3 0.0228(5) 0.0429(6) 0.0134(4) -0.0008(4) 0.0042(3) 0.0005(4) P1 0.0274(13) 0.0284(14) 0.0118(11) -0.0005(10) 0.0042(9) 0.0013(11) P2 0.0187(12) 0.0329(15) 0.0184(12) -0.0003(11) 0.0067(9) 0.0024(10) P3 0.0185(12) 0.0329(14) 0.0139(11) 0.0010(10) 0.0033(9) 0.0029(10) N1 0.044(5) 0.031(5) 0.015(4) 0.008(4) 0.008(3) 0.008(4) N2 0.016(4) 0.047(5) 0.029(5) -0.001(4) 0.006(3) -0.006(4) N11 0.025(4) 0.029(5) 0.013(4) 0.003(3) 0.001(3) 0.012(4) N21 0.020(4) 0.041(5) 0.014(4) 0.000(3) 0.008(3) -0.008(4) N22 0.014(4) 0.045(5) 0.010(4) 0.002(3) -0.002(3) 0.003(3) C2 0.023(5) 0.012(4) 0.029(5) 0.010(4) 0.005(4) 0.009(4) C3 0.046(6) 0.025(6) 0.038(6) -0.016(5) 0.010(5) -0.002(5) C4 0.061(8) 0.031(6) 0.062(8) 0.002(6) 0.025(6) 0.013(5) C5 0.051(7) 0.054(7) 0.036(6) -0.019(5) 0.017(5) 0.012(6) C6 0.047(7) 0.045(7) 0.030(6) -0.009(5) 0.009(5) 0.005(5) C7 0.035(5) 0.025(5) 0.022(5) -0.011(4) 0.006(4) -0.002(4) C8 0.018(4) 0.031(5) 0.010(4) 0.000(4) 0.003(3) -0.007(4) C9 0.028(5) 0.020(5) 0.021(5) 0.000(4) 0.011(4) -0.003(4) C10 0.053(6) 0.033(6) 0.019(5) -0.008(5) 0.010(4) -0.013(5) C11 0.038(6) 0.074(8) 0.012(5) -0.007(5) 0.000(4) -0.017(6) C12 0.054(7) 0.059(8) 0.017(5) 0.005(5) 0.005(4) -0.021(6) C13 0.045(6) 0.061(7) 0.005(5) 0.001(5) 0.007(4) -0.007(5) C14 0.024(5) 0.032(6) 0.035(6) 0.006(5) 0.013(4) 0.004(4) C15 0.045(6) 0.032(6) 0.029(6) -0.007(5) 0.006(4) -0.006(5) C16 0.053(7) 0.033(6) 0.033(6) 0.004(5) 0.011(5) -0.013(5) C17 0.074(8) 0.053(8) 0.038(7) 0.031(6) 0.025(6) 0.011(6) C18 0.034(6) 0.048(7) 0.022(5) -0.001(5) -0.009(4) 0.011(5) C19 0.027(5) 0.040(6) 0.007(4) 0.002(4) 0.003(3) 0.005(4) C21 0.048(7) 0.044(7) 0.027(6) 0.004(5) 0.011(5) 0.010(5) C22 0.040(6) 0.046(7) 0.040(6) 0.006(5) 0.016(5) 0.006(5) C23 0.029(6) 0.053(7) 0.030(6) -0.006(5) -0.004(4) 0.001(5) C24 0.035(6) 0.027(6) 0.037(6) -0.010(5) 0.012(4) -0.007(5) C32 0.018(5) 0.042(6) 0.028(5) 0.005(4) 0.010(4) 0.010(4) C33 0.043(6) 0.050(7) 0.039(6) -0.006(5) 0.024(5) -0.007(5) C34 0.051(7) 0.046(7) 0.042(6) 0.011(5) 0.029(5) -0.008(5) C35 0.045(7) 0.053(7) 0.049(7) 0.026(6) 0.019(5) -0.007(5) C36 0.043(6) 0.031(6) 0.048(7) 0.014(5) 0.009(5) -0.005(5) C37 0.029(5) 0.041(6) 0.013(5) -0.001(4) -0.003(4) -0.009(4) C38 0.031(5) 0.034(6) 0.021(5) -0.001(4) 0.007(4) 0.006(4) C39 0.015(5) 0.038(6) 0.042(6) 0.016(5) 0.009(4) -0.007(4) C40 0.014(5) 0.046(7) 0.049(6) -0.014(5) 0.002(4) 0.012(5) C41 0.036(6) 0.027(6) 0.066(7) -0.015(5) 0.025(5) -0.010(5) C42 0.036(6) 0.037(6) 0.037(6) 0.011(5) 0.018(5) 0.012(5) C43 0.028(5) 0.044(6) 0.029(6) 0.004(5) 0.009(4) 0.011(5) C44 0.014(4) 0.028(5) 0.011(4) -0.003(4) -0.007(3) 0.000(4) C45 0.036(5) 0.027(5) 0.018(5) 0.003(4) 0.014(4) -0.006(4) C46 0.020(5) 0.043(6) 0.016(5) -0.001(4) 0.008(4) 0.000(4) C47 0.033(6) 0.043(6) 0.036(6) 0.006(5) 0.017(4) 0.021(5) C48 0.017(4) 0.019(5) 0.030(5) -0.002(4) 0.005(4) 0.001(4) C49 0.018(5) 0.029(5) 0.018(5) -0.008(4) -0.005(3) 0.012(4) C50 0.033(5) 0.037(6) 0.032(6) -0.007(5) 0.020(4) -0.002(5) C51 0.034(6) 0.066(8) 0.053(7) -0.025(6) 0.022(5) -0.016(6) C52 0.042(6) 0.072(8) 0.024(6) -0.010(6) 0.006(5) 0.000(6) C53 0.029(5) 0.057(7) 0.017(5) 0.003(5) 0.003(4) 0.013(5) C54 0.038(6) 0.027(5) 0.021(5) -0.002(4) 0.005(4) 0.013(4) C61 0.024(5) 0.023(5) 0.006(4) 0.002(4) 0.001(3) 0.006(4) C62 0.028(5) 0.036(6) 0.009(4) 0.002(4) 0.008(4) 0.004(4) C63 0.028(5) 0.035(6) 0.032(6) 0.002(5) 0.002(4) -0.002(5) C64 0.079(9) 0.053(7) 0.027(6) 0.018(5) 0.027(5) 0.014(6) C65 0.043(7) 0.073(8) 0.016(5) 0.000(5) -0.002(4) -0.004(6) C66 0.031(5) 0.057(7) 0.008(5) 0.009(4) -0.005(4) 0.003(5) C67 0.034(5) 0.026(5) 0.021(5) -0.010(4) 0.009(4) -0.002(4) C68 0.026(5) 0.047(6) 0.016(5) 0.013(4) 0.012(4) 0.010(4) C69 0.006(4) 0.042(6) 0.021(5) 0.009(4) -0.003(3) 0.001(4) C71 0.029(6) 0.080(8) 0.029(6) 0.003(6) 0.002(4) -0.009(6) C72 0.015(5) 0.092(9) 0.033(6) 0.001(6) 0.014(4) 0.010(5) C73 0.020(5) 0.074(8) 0.013(5) -0.005(5) -0.005(4) 0.009(5) C74 0.027(5) 0.024(5) 0.024(5) -0.005(4) 0.011(4) 0.001(4) C75 0.035(6) 0.061(7) 0.009(5) -0.004(5) 0.004(4) -0.007(5) C76 0.028(5) 0.073(8) 0.018(5) -0.008(5) 0.013(4) 0.000(5) C77 0.020(5) 0.064(7) 0.025(5) -0.004(5) 0.015(4) -0.001(5) C78 0.013(4) 0.047(6) 0.029(5) -0.002(5) 0.008(4) -0.006(4) C79 0.021(5) 0.047(6) 0.005(4) -0.005(4) 0.003(3) -0.008(4) C80 0.050(7) 0.056(8) 0.033(6) 0.004(6) -0.005(5) 0.006(6) C81 0.075(9) 0.060(9) 0.037(7) -0.020(6) 0.007(6) -0.002(7) C82 0.098(10) 0.036(7) 0.058(8) -0.010(7) 0.034(7) -0.002(7) C83 0.087(9) 0.026(6) 0.065(8) 0.012(6) 0.044(7) 0.022(6) C84 0.032(5) 0.046(7) 0.028(5) 0.004(5) 0.003(4) 0.007(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 N11 2.028(7) . ? Cu1 N2 2.081(7) . ? Cu1 Se2 2.4285(14) . ? Cu1 Se1 2.4847(14) . ? Cu2 N21 2.012(6) . ? Cu2 N12 2.013(6) . ? Cu2 Se3 2.5144(14) . ? Cu2 Se2 2.6749(14) . ? Cu3 N1 1.991(7) . ? Cu3 N22 2.018(6) . ? Cu3 Se1 2.4518(14) . ? Cu3 Se3 2.5822(15) 3_655 ? Se1 P1 2.135(2) . ? Se2 P2 2.149(2) . ? Se3 P3 2.152(2) . ? Se3 Cu3 2.5822(15) 3_655 ? P1 C19 1.787(8) . ? P1 C8 1.808(7) . ? P1 C1 1.809(8) . ? P2 C38 1.796(9) . ? P2 C31 1.811(8) . ? P2 C49 1.812(8) . ? P3 C79 1.800(9) . ? P3 C68 1.801(8) . ? P3 C61 1.827(7) . ? N1 C18 1.379(10) . ? N1 C14 1.387(10) . ? N2 C9 1.312(10) . ? N2 C13 1.341(10) . ? N11 C44 1.359(10) . ? N11 C48 1.368(9) . ? N12 C43 1.362(9) . ? N12 C39 1.377(9) . ? N21 C78 1.360(9) . ? N21 C74 1.361(10) . ? N22 C73 1.325(10) . ? N22 C69 1.326(9) . ? C1 C2 1.323(10) . ? C1 C14 1.506(11) . ? C2 C3 1.511(10) . ? C2 C7 1.522(11) . ? C3 C4 1.565(11) . ? C4 C5 1.514(12) . ? C5 C6 1.520(12) . ? C6 C7 1.557(10) . ? C7 C8 1.321(11) . ? C8 C9 1.497(11) . ? C9 C10 1.358(11) . ? C10 C11 1.410(12) . ? C11 C12 1.353(12) . ? C12 C13 1.388(12) . ? C14 C15 1.388(11) . ? C15 C16 1.397(11) . ? C16 C17 1.366(13) . ? C17 C18 1.383(13) . ? C19 C24 1.385(11) . ? C19 C20 1.408(11) . ? C20 C21 1.421(11) . ? C21 C22 1.380(12) . ? C22 C23 1.378(12) . ? C23 C24 1.421(11) . ? C31 C32 1.373(11) . ? C31 C44 1.436(10) . ? C32 C37 1.517(11) . ? C32 C33 1.535(10) . ? C33 C34 1.587(12) . ? C34 C35 1.502(12) . ? C35 C36 1.549(11) . ? C36 C37 1.518(11) . ? C37 C38 1.370(10) . ? C38 C39 1.471(11) . ? C39 C40 1.395(12) . ? C40 C41 1.422(11) . ? C41 C42 1.397(11) . ? C42 C43 1.300(11) . ? C44 C45 1.393(10) . ? C45 C46 1.352(10) . ? C46 C47 1.365(11) . ? C47 C48 1.428(10) . ? C49 C50 1.395(11) . ? C49 C54 1.398(11) . ? C50 C51 1.390(12) . ? C51 C52 1.364(13) . ? C52 C53 1.360(12) . ? C53 C54 1.399(11) . ? C61 C62 1.329(10) . ? C61 C74 1.468(10) . ? C62 C63 1.497(10) . ? C62 C67 1.521(10) . ? C63 C64 1.544(11) . ? C64 C65 1.513(12) . ? C65 C66 1.531(11) . ? C66 C67 1.482(11) . ? C67 C68 1.334(11) . ? C68 C69 1.502(10) 3_655 ? C69 C70 1.380(11) . ? C69 C68 1.502(10) 3_655 ? C70 C71 1.379(11) . ? C71 C72 1.393(11) . ? C72 C73 1.355(11) . ? C74 C75 1.399(10) . ? C75 C76 1.419(11) . ? C76 C77 1.345(11) . ? C77 C78 1.396(10) . ? C79 C84 1.364(11) . ? C79 C80 1.427(12) . ? C80 C81 1.379(13) . ? C81 C82 1.420(14) . ? C82 C83 1.359(14) . ? C83 C84 1.390(12) . ? 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 N11 Cu1 N2 110.7(2) . . ? N11 Cu1 Se2 116.1(2) . . ? N2 Cu1 Se2 109.3(2) . . ? N11 Cu1 Se1 99.52(18) . . ? N2 Cu1 Se1 111.5(2) . . ? Se2 Cu1 Se1 109.29(5) . . ? N21 Cu2 N12 131.9(3) . . ? N21 Cu2 Se3 113.69(18) . . ? N12 Cu2 Se3 105.14(17) . . ? N21 Cu2 Se2 101.9(2) . . ? N12 Cu2 Se2 100.17(18) . . ? Se3 Cu2 Se2 97.26(5) . . ? N1 Cu3 N22 125.1(3) . . ? N1 Cu3 Se1 110.9(2) . . ? N22 Cu3 Se1 103.94(18) . . ? N1 Cu3 Se3 104.8(2) . 3_655 ? N22 Cu3 Se3 106.42(19) . 3_655 ? Se1 Cu3 Se3 103.82(5) . 3_655 ? P1 Se1 Cu3 91.85(7) . . ? P1 Se1 Cu1 89.83(7) . . ? Cu3 Se1 Cu1 164.44(5) . . ? P2 Se2 Cu1 87.08(7) . . ? P2 Se2 Cu2 94.08(7) . . ? Cu1 Se2 Cu2 147.42(5) . . ? P3 Se3 Cu2 90.00(7) . . ? P3 Se3 Cu3 94.50(7) . 3_655 ? Cu2 Se3 Cu3 139.90(5) . 3_655 ? C19 P1 C8 107.4(3) . . ? C19 P1 C1 111.3(4) . . ? C8 P1 C1 92.2(4) . . ? C19 P1 Se1 115.1(3) . . ? C8 P1 Se1 115.0(3) . . ? C1 P1 Se1 113.6(3) . . ? C38 P2 C31 93.8(4) . . ? C38 P2 C49 108.9(4) . . ? C31 P2 C49 111.7(4) . . ? C38 P2 Se2 110.8(3) . . ? C31 P2 Se2 116.9(3) . . ? C49 P2 Se2 113.0(3) . . ? C79 P3 C68 113.7(4) . . ? C79 P3 C61 107.5(3) . . ? C68 P3 C61 92.4(4) . . ? C79 P3 Se3 111.4(3) . . ? C68 P3 Se3 113.3(3) . . ? C61 P3 Se3 117.2(3) . . ? C18 N1 C14 113.3(7) . . ? C18 N1 Cu3 114.6(6) . . ? C14 N1 Cu3 131.5(6) . . ? C9 N2 C13 119.7(8) . . ? C9 N2 Cu1 129.2(6) . . ? C13 N2 Cu1 111.1(6) . . ? C44 N11 C48 118.4(7) . . ? C44 N11 Cu1 127.4(5) . . ? C48 N11 Cu1 113.6(5) . . ? C43 N12 C39 115.5(7) . . ? C43 N12 Cu2 122.8(6) . . ? C39 N12 Cu2 121.5(5) . . ? C78 N21 C74 116.5(6) . . ? C78 N21 Cu2 117.5(5) . . ? C74 N21 Cu2 125.9(5) . . ? C73 N22 C69 116.4(7) . . ? C73 N22 Cu3 119.3(5) . . ? C69 N22 Cu3 124.2(5) . . ? C2 C1 C14 127.7(8) . . ? C2 C1 P1 109.7(6) . . ? C14 C1 P1 122.6(6) . . ? C1 C2 C3 125.8(8) . . ? C1 C2 C7 112.8(7) . . ? C3 C2 C7 121.3(7) . . ? C2 C3 C4 110.8(7) . . ? C5 C4 C3 113.7(8) . . ? C4 C5 C6 110.6(8) . . ? C5 C6 C7 112.2(7) . . ? C8 C7 C2 115.4(7) . . ? C8 C7 C6 125.4(8) . . ? C2 C7 C6 119.1(7) . . ? C7 C8 C9 128.6(7) . . ? C7 C8 P1 108.7(6) . . ? C9 C8 P1 122.0(6) . . ? N2 C9 C10 121.3(8) . . ? N2 C9 C8 118.7(7) . . ? C10 C9 C8 119.7(8) . . ? C9 C10 C11 119.4(9) . . ? C12 C11 C10 119.1(9) . . ? C11 C12 C13 117.7(9) . . ? N2 C13 C12 122.4(9) . . ? C15 C14 N1 123.7(8) . . ? C15 C14 C1 117.1(8) . . ? N1 C14 C1 119.2(7) . . ? C14 C15 C16 119.7(8) . . ? C17 C16 C15 118.8(9) . . ? C16 C17 C18 118.7(9) . . ? N1 C18 C17 125.9(9) . . ? C24 C19 C20 121.0(8) . . ? C24 C19 P1 118.5(6) . . ? C20 C19 P1 120.5(7) . . ? C19 C20 C21 118.3(8) . . ? C22 C21 C20 120.9(9) . . ? C23 C22 C21 120.0(9) . . ? C22 C23 C24 120.8(9) . . ? C19 C24 C23 119.0(8) . . ? C32 C31 C44 126.6(7) . . ? C32 C31 P2 107.6(6) . . ? C44 C31 P2 125.8(6) . . ? C31 C32 C37 115.7(7) . . ? C31 C32 C33 125.5(7) . . ? C37 C32 C33 118.7(7) . . ? C32 C33 C34 111.8(7) . . ? C35 C34 C33 109.4(8) . . ? C34 C35 C36 110.4(7) . . ? C37 C36 C35 112.8(7) . . ? C38 C37 C36 125.7(8) . . ? C38 C37 C32 112.3(7) . . ? C36 C37 C32 121.5(7) . . ? C37 C38 C39 124.0(8) . . ? C37 C38 P2 110.2(6) . . ? C39 C38 P2 125.7(6) . . ? N12 C39 C40 122.7(8) . . ? N12 C39 C38 117.4(8) . . ? C40 C39 C38 119.8(7) . . ? C39 C40 C41 118.2(8) . . ? C42 C41 C40 117.0(9) . . ? C43 C42 C41 121.0(9) . . ? C42 C43 N12 125.5(9) . . ? N11 C44 C45 120.3(7) . . ? N11 C44 C31 118.6(7) . . ? C45 C44 C31 121.1(8) . . ? C46 C45 C44 120.5(8) . . ? C45 C46 C47 122.0(8) . . ? C46 C47 C48 116.1(8) . . ? N11 C48 C47 122.6(8) . . ? C50 C49 C54 121.0(8) . . ? C50 C49 P2 119.3(7) . . ? C54 C49 P2 119.7(7) . . ? C51 C50 C49 118.9(8) . . ? C52 C51 C50 121.0(10) . . ? C53 C52 C51 119.5(9) . . ? C52 C53 C54 122.7(9) . . ? C49 C54 C53 116.9(9) . . ? C62 C61 C74 128.8(7) . . ? C62 C61 P3 108.8(6) . . ? C74 C61 P3 121.2(6) . . ? C61 C62 C63 126.6(7) . . ? C61 C62 C67 114.8(7) . . ? C63 C62 C67 118.5(7) . . ? C62 C63 C64 113.0(7) . . ? C65 C64 C63 110.1(8) . . ? C64 C65 C66 110.6(7) . . ? C67 C66 C65 115.3(7) . . ? C68 C67 C66 126.2(7) . . ? C68 C67 C62 113.7(7) . . ? C66 C67 C62 120.0(7) . . ? C67 C68 C69 126.2(7) . 3_655 ? C67 C68 P3 109.9(6) . . ? C69 C68 P3 123.8(6) 3_655 . ? N22 C69 C70 124.1(7) . . ? N22 C69 C68 119.1(7) . 3_655 ? C70 C69 C68 116.7(8) . 3_655 ? C71 C70 C69 117.6(8) . . ? C70 C71 C72 119.0(9) . . ? C73 C72 C71 117.7(8) . . ? N22 C73 C72 125.1(8) . . ? N21 C74 C75 122.3(7) . . ? N21 C74 C61 118.5(7) . . ? C75 C74 C61 119.2(7) . . ? C74 C75 C76 118.4(7) . . ? C77 C76 C75 120.1(8) . . ? C76 C77 C78 118.1(8) . . ? N21 C78 C77 124.6(7) . . ? C84 C79 C80 118.7(9) . . ? C84 C79 P3 123.2(7) . . ? C80 C79 P3 118.0(7) . . ? C81 C80 C79 120.2(10) . . ? C80 C81 C82 119.9(10) . . ? C83 C82 C81 118.4(10) . . ? C82 C83 C84 122.2(10) . . ? C79 C84 C83 120.5(9) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.235 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 927132' ####################################################################### # # 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_revsq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C154 H126 Cl0 Cu8 F30 N12 O40 P6 S10 Se6' _chemical_formula_sum 'C154 H126 Cl0 Cu8 F30 N12 O40 P6 S10 Se6' _chemical_formula_weight 4843.17 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' P P 0.1023 0.0942 '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' Se Se -0.0929 2.2259 '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' 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' _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 16.945(1) _cell_length_b 18.478(1) _cell_length_c 20.154(1) _cell_angle_alpha 107.916(2) _cell_angle_beta 104.980(2) _cell_angle_gamma 112.985(2) _cell_volume 4984.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.18 _cell_measurement_theta_max 27.56 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2410 _exptl_absorpt_coefficient_mu 2.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5922 _exptl_absorpt_correction_T_max 0.8397 _exptl_absorpt_process_details 'Sheldrick,G.M.(2002).SADABS BrukerAXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method none _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 46121 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.56 _reflns_number_total 22033 _reflns_number_gt 13554 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^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 22033 _refine_ls_number_parameters 1205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1710 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.23305(5) 0.70055(4) 0.76136(4) 0.02432(16) Uani 1 1 d . . . Cu2 Cu 0.31814(5) 0.73074(4) 0.54873(4) 0.02481(16) Uani 1 1 d . . . Cu3 Cu 0.04175(5) 0.56798(4) 0.31538(4) 0.02605(16) Uani 1 1 d . . . Cu10 Cu 0.10857(5) 0.15271(5) 0.90824(4) 0.03481(19) Uani 1 1 d . . . Se1 Se 0.27524(5) 0.72014(4) 0.65287(4) 0.03624(17) Uani 1 1 d . . . Se2 Se 0.16511(4) 0.60001(4) 0.43434(3) 0.02640(14) Uani 1 1 d . . . Se3 Se 0.10676(4) 0.54348(3) 0.68577(3) 0.02148(13) Uani 1 1 d . . . N1 N 0.1717(3) 0.7716(3) 0.7865(2) 0.0241(10) Uani 1 1 d . . . N2 N 0.3386(3) 0.8426(3) 0.5401(2) 0.0222(10) Uani 1 1 d . . . N11 N 0.4149(3) 0.6916(3) 0.5560(2) 0.0237(10) Uani 1 1 d . . . N12 N 0.0548(3) 0.5108(3) 0.2190(2) 0.0214(9) Uani 1 1 d . . . N21 N 0.0235(3) 0.6732(3) 0.3332(3) 0.0268(10) Uani 1 1 d . . . N22 N 0.3557(3) 0.7206(3) 0.8308(2) 0.0216(9) Uani 1 1 d . . . P1 P 0.24441(10) 0.82304(9) 0.66115(8) 0.0220(3) Uani 1 1 d . . . P2 P 0.23207(9) 0.55567(9) 0.36832(7) 0.0183(3) Uani 1 1 d . . . P3 P 0.19751(9) 0.50338(9) 0.73942(8) 0.0183(3) Uani 1 1 d . . . C1 C 0.2623(4) 0.8864(3) 0.7568(3) 0.0217(11) Uani 1 1 d . . . C2 C 0.3366(4) 0.9696(3) 0.7868(3) 0.0251(12) Uani 1 1 d . . . C3 C 0.3805(5) 1.0392(4) 0.8681(3) 0.0387(15) Uani 1 1 d . . . H3A H 0.4101 1.0206 0.9020 0.046 Uiso 1 1 calc R . . H3B H 0.3303 1.0434 0.8806 0.046 Uiso 1 1 calc R . . C4 C 0.4547(5) 1.1312(4) 0.8854(4) 0.0446(17) Uani 1 1 d . . . H4A H 0.4231 1.1604 0.8684 0.053 Uiso 1 1 calc R . . H4B H 0.4938 1.1665 0.9407 0.053 Uiso 1 1 calc R . . C5 C 0.5169(4) 1.1250(4) 0.8448(3) 0.0360(14) Uani 1 1 d . . . H5A H 0.5464 1.0935 0.8601 0.043 Uiso 1 1 calc R . . H5B H 0.5669 1.1840 0.8598 0.043 Uiso 1 1 calc R . . C6 C 0.4585(4) 1.0767(3) 0.7576(3) 0.0273(12) Uani 1 1 d . . . H6A H 0.4349 1.1118 0.7419 0.033 Uiso 1 1 calc R . . H6B H 0.4988 1.0702 0.7326 0.033 Uiso 1 1 calc R . . C7 C 0.3749(4) 0.9858(3) 0.7310(3) 0.0210(11) Uani 1 1 d . . . C8 C 0.3321(4) 0.9165(3) 0.6613(3) 0.0206(11) Uani 1 1 d . . . C9 C 0.3459(4) 0.9149(3) 0.5909(3) 0.0206(11) Uani 1 1 d . . . C10 C 0.3612(4) 0.9872(4) 0.5757(3) 0.0284(13) Uani 1 1 d . . . H10 H 0.3627 1.0355 0.6097 0.034 Uiso 1 1 calc R . . C11 C 0.3740(4) 0.9873(4) 0.5111(3) 0.0344(14) Uani 1 1 d . . . H11 H 0.3852 1.0356 0.5015 0.041 Uiso 1 1 calc R . . C12 C 0.3698(4) 0.9139(4) 0.4608(3) 0.0331(14) Uani 1 1 d . . . H12 H 0.3796 0.9121 0.4171 0.040 Uiso 1 1 calc R . . C13 C 0.3509(4) 0.8442(4) 0.4773(3) 0.0277(12) Uani 1 1 d . . . H13 H 0.3461 0.7943 0.4425 0.033 Uiso 1 1 calc R . . C14 C 0.1918(4) 0.8493(4) 0.7860(3) 0.0258(12) Uani 1 1 d . . . C15 C 0.1452(4) 0.8927(4) 0.8069(3) 0.0339(14) Uani 1 1 d . . . H15 H 0.1618 0.9468 0.8065 0.041 Uiso 1 1 calc R . . C16 C 0.0743(5) 0.8565(4) 0.8281(4) 0.0393(15) Uani 1 1 d . . . H16 H 0.0421 0.8850 0.8418 0.047 Uiso 1 1 calc R . . C17 C 0.0527(4) 0.7772(4) 0.8282(4) 0.0395(16) Uani 1 1 d . . . H17 H 0.0055 0.7507 0.8427 0.047 Uiso 1 1 calc R . . C18 C 0.1010(4) 0.7372(4) 0.8069(3) 0.0301(13) Uani 1 1 d . . . H18 H 0.0843 0.6826 0.8064 0.036 Uiso 1 1 calc R . . C19 C 0.1268(4) 0.7853(4) 0.5937(3) 0.0285(13) Uani 1 1 d . . . C20 C 0.1019(5) 0.8487(5) 0.5940(4) 0.0469(17) Uani 1 1 d . . . H20 H 0.1458 0.9084 0.6270 0.056 Uiso 1 1 calc R . . C21 C 0.0103(5) 0.8219(6) 0.5442(4) 0.057(2) Uani 1 1 d . . . H21 H -0.0077 0.8634 0.5443 0.068 Uiso 1 1 calc R . . C22 C -0.0522(5) 0.7345(6) 0.4956(4) 0.063(2) Uani 1 1 d . . . H22 H -0.1125 0.7166 0.4609 0.076 Uiso 1 1 calc R . . C23 C -0.0273(6) 0.6714(6) 0.4969(5) 0.076(3) Uani 1 1 d . . . H23 H -0.0721 0.6117 0.4648 0.092 Uiso 1 1 calc R . . C24 C 0.0631(4) 0.6963(5) 0.5453(4) 0.0453(18) Uani 1 1 d . . . H24 H 0.0805 0.6543 0.5453 0.054 Uiso 1 1 calc R . . OW2 O 0.0011(3) 0.0568(3) 0.9065(2) 0.0375(10) Uani 1 1 d . . . C31 C 0.3597(3) 0.6247(3) 0.4166(3) 0.0190(10) Uani 1 1 d . . . C32 C 0.3893(4) 0.6569(3) 0.3707(3) 0.0206(11) Uani 1 1 d . . . C33 C 0.4910(4) 0.7248(4) 0.3940(4) 0.0360(14) Uani 1 1 d . . . H33A H 0.5036 0.7829 0.4262 0.043 Uiso 1 1 calc R . . H33B H 0.5334 0.7124 0.4248 0.043 Uiso 1 1 calc R . . C34 C 0.5125(4) 0.7266(4) 0.3277(4) 0.0415(16) Uani 1 1 d . . . H34A H 0.5147 0.6741 0.3021 0.050 Uiso 1 1 calc R . . H34B H 0.5745 0.7779 0.3464 0.050 Uiso 1 1 calc R . . C35 C 0.4384(4) 0.7305(4) 0.2702(4) 0.0363(15) Uani 1 1 d . . . H35A H 0.4566 0.7355 0.2293 0.044 Uiso 1 1 calc R . . H35B H 0.4357 0.7828 0.2960 0.044 Uiso 1 1 calc R . . C36 C 0.3405(4) 0.6487(4) 0.2352(3) 0.0296(13) Uani 1 1 d . . . H36A H 0.2935 0.6587 0.2067 0.035 Uiso 1 1 calc R . . H36B H 0.3391 0.5990 0.1987 0.035 Uiso 1 1 calc R . . C37 C 0.3136(4) 0.6249(3) 0.2941(3) 0.0203(11) Uani 1 1 d . . . C38 C 0.2246(4) 0.5712(3) 0.2836(3) 0.0187(10) Uani 1 1 d . . . C39 C 0.1351(4) 0.5203(3) 0.2112(3) 0.0184(10) Uani 1 1 d . . . C40 C 0.1339(4) 0.4818(4) 0.1415(3) 0.0336(14) Uani 1 1 d . . . H40 H 0.1898 0.4873 0.1389 0.040 Uiso 1 1 calc R . . C41 C 0.0500(4) 0.4341(4) 0.0738(3) 0.0368(15) Uani 1 1 d . . . H41 H 0.0489 0.4093 0.0256 0.044 Uiso 1 1 calc R . . C42 C -0.0322(4) 0.4253(4) 0.0815(3) 0.0353(14) Uani 1 1 d . . . H42 H -0.0901 0.3942 0.0381 0.042 Uiso 1 1 calc R . . C43 C -0.0264(4) 0.4628(4) 0.1531(3) 0.0278(12) Uani 1 1 d . . . H43 H -0.0823 0.4548 0.1572 0.033 Uiso 1 1 calc R . . C44 C 0.4209(4) 0.6433(3) 0.4939(3) 0.0225(11) Uani 1 1 d . . . C45 C 0.4847(4) 0.6137(4) 0.5014(4) 0.0367(15) Uani 1 1 d . . . H45 H 0.4852 0.5778 0.4577 0.044 Uiso 1 1 calc R . . C46 C 0.5482(5) 0.6382(5) 0.5750(4) 0.0425(16) Uani 1 1 d . . . H46 H 0.5924 0.6199 0.5812 0.051 Uiso 1 1 calc R . . C47 C 0.5442(5) 0.6892(5) 0.6374(4) 0.0415(16) Uani 1 1 d . . . H47 H 0.5868 0.7080 0.6872 0.050 Uiso 1 1 calc R . . C48 C 0.4759(4) 0.7126(4) 0.6255(3) 0.0327(14) Uani 1 1 d . . . H48 H 0.4719 0.7451 0.6687 0.039 Uiso 1 1 calc R . . C49 C 0.2008(4) 0.4420(3) 0.3422(3) 0.0258(12) Uani 1 1 d . . . C50 C 0.1544(5) 0.3974(4) 0.3760(3) 0.0439(17) Uani 1 1 d . . . H50 H 0.1342 0.4226 0.4104 0.053 Uiso 1 1 calc R . . C51 C 0.1388(7) 0.3111(5) 0.3560(5) 0.072(3) Uani 1 1 d . . . H51 H 0.1081 0.2793 0.3784 0.087 Uiso 1 1 calc R . . OW6 O 0.0984(3) 0.0613(3) 0.8182(2) 0.0366(10) Uani 1 1 d . . . C52 C 0.1669(6) 0.2730(5) 0.3056(5) 0.066(3) Uani 1 1 d . . . H52 H 0.1554 0.2159 0.2931 0.079 Uiso 1 1 calc R . . OW4 O 0.0055(3) 0.1724(3) 0.8309(3) 0.0411(11) Uani 1 1 d . . . C53 C 0.2123(6) 0.3203(5) 0.2735(5) 0.059(2) Uani 1 1 d . . . H53 H 0.2326 0.2950 0.2391 0.071 Uiso 1 1 calc R . . C54 C 0.2289(5) 0.4040(4) 0.2906(4) 0.0449(17) Uani 1 1 d . . . H54 H 0.2590 0.4347 0.2674 0.054 Uiso 1 1 calc R . . C61 C 0.1396(4) 0.4209(3) 0.7666(3) 0.0222(11) Uani 1 1 d . . . C62 C 0.1836(4) 0.4535(3) 0.8430(3) 0.0248(12) Uani 1 1 d . . . C63 C 0.1486(5) 0.4083(4) 0.8901(3) 0.0360(14) Uani 1 1 d . . . H63A H 0.0931 0.4110 0.8917 0.043 Uiso 1 1 calc R . . H63B H 0.1293 0.3464 0.8641 0.043 Uiso 1 1 calc R . . C64 C 0.2225(5) 0.4494(4) 0.9718(3) 0.0394(16) Uani 1 1 d . . . H64A H 0.2694 0.4319 0.9710 0.047 Uiso 1 1 calc R . . H64B H 0.1922 0.4271 1.0016 0.047 Uiso 1 1 calc R . . C65 C 0.2721(5) 0.5497(4) 1.0109(4) 0.0404(16) Uani 1 1 d . . . H65A H 0.2253 0.5678 1.0096 0.048 Uiso 1 1 calc R . . H65B H 0.3147 0.5733 1.0645 0.048 Uiso 1 1 calc R . . C66 C 0.3279(5) 0.5857(4) 0.9694(3) 0.0346(14) Uani 1 1 d . . . H66A H 0.3541 0.6492 0.9917 0.042 Uiso 1 1 calc R . . H66B H 0.3806 0.5753 0.9780 0.042 Uiso 1 1 calc R . . C67 C 0.2693(4) 0.5450(3) 0.8836(3) 0.0223(11) Uani 1 1 d . . . C69 C 0.3704(4) 0.6665(3) 0.8578(3) 0.0179(10) Uani 1 1 d . . . C70 C 0.4609(4) 0.6873(4) 0.9035(3) 0.0251(12) Uani 1 1 d . . . H70 H 0.4688 0.6476 0.9198 0.030 Uiso 1 1 calc R . . C71 C 0.5380(4) 0.7664(4) 0.9242(3) 0.0313(13) Uani 1 1 d . . . H71 H 0.5988 0.7812 0.9550 0.038 Uiso 1 1 calc R . . C72 C 0.5248(4) 0.8234(4) 0.8992(3) 0.0324(14) Uani 1 1 d . . . H72 H 0.5762 0.8779 0.9133 0.039 Uiso 1 1 calc R . . C73 C 0.4330(4) 0.7986(3) 0.8524(3) 0.0271(12) Uani 1 1 d . . . H73 H 0.4245 0.8375 0.8351 0.033 Uiso 1 1 calc R . . C74 C 0.0559(4) 0.3315(4) 0.7102(3) 0.0257(12) Uani 1 1 d . . . C75 C 0.0604(5) 0.2564(4) 0.7022(4) 0.0347(14) Uani 1 1 d . . . H75 H 0.1156 0.2611 0.7325 0.042 Uiso 1 1 calc R . . C76 C -0.0168(5) 0.1756(4) 0.6496(4) 0.0457(17) Uani 1 1 d . . . H76 H -0.0153 0.1246 0.6451 0.055 Uiso 1 1 calc R . . C77 C -0.0965(5) 0.1691(4) 0.6035(4) 0.0412(16) Uani 1 1 d . . . H77 H -0.1488 0.1142 0.5661 0.049 Uiso 1 1 calc R . . OW5 O 0.2272(3) 0.2441(3) 0.9185(3) 0.0512(13) Uani 1 1 d . . . C780 C -0.0976(4) 0.2460(4) 0.6137(4) 0.0346(14) Uani 1 1 d . . . H780 H -0.1519 0.2418 0.5825 0.042 Uiso 1 1 calc R . . C79 C 0.2525(4) 0.4667(3) 0.6815(3) 0.0230(11) Uani 1 1 d . . . C80 C 0.2695(4) 0.4998(4) 0.6304(3) 0.0301(13) Uani 1 1 d . . . H80 H 0.2551 0.5427 0.6273 0.036 Uiso 1 1 calc R . . C81 C 0.3084(4) 0.4684(5) 0.5836(4) 0.0451(17) Uani 1 1 d . . . H81 H 0.3200 0.4905 0.5493 0.054 Uiso 1 1 calc R . . C82 C 0.3297(4) 0.4048(5) 0.5882(4) 0.0477(18) Uani 1 1 d . . . H82 H 0.3550 0.3834 0.5565 0.057 Uiso 1 1 calc R . . C83 C 0.3136(5) 0.3734(5) 0.6391(4) 0.0485(18) Uani 1 1 d . . . H83 H 0.3293 0.3314 0.6425 0.058 Uiso 1 1 calc R . . C84 C 0.2746(4) 0.4026(4) 0.6857(4) 0.0381(15) Uani 1 1 d . . . H84 H 0.2631 0.3798 0.7196 0.046 Uiso 1 1 calc R . . OW3 O 0.1143(3) 0.2406(3) 0.9993(3) 0.0516(12) Uani 1 1 d . . . C100 C 0.4325(5) 0.4201(5) 0.2121(4) 0.0493(18) Uani 1 1 d . . . C200 C 0.2202(5) 0.1051(5) 0.1196(4) 0.0488(18) Uani 1 1 d . . . C300 C 0.8045(7) 0.8916(5) 0.5757(6) 0.067(2) Uani 1 1 d . . . C400 C 0.2139(5) 0.7892(4) 0.2384(4) 0.0406(16) Uani 1 1 d . . . S10 S 0.36053(14) 0.41859(13) 0.12817(10) 0.0460(4) Uani 1 1 d . . . S20 S 0.18928(11) 0.05316(10) 0.01731(9) 0.0310(3) Uani 1 1 d . . . S30 S 0.83799(13) 0.92911(11) 0.67884(12) 0.0472(4) Uani 1 1 d . . . S40 S 0.16032(11) 0.74737(10) 0.13346(9) 0.0331(3) Uani 1 1 d . . . O10 O 0.3676(3) 0.3621(3) 0.0662(3) 0.0511(12) Uani 1 1 d . . . O11 O 0.4080(6) 0.5091(4) 0.1437(4) 0.114(3) Uani 1 1 d . . . O12 O 0.2708(4) 0.3890(5) 0.1275(3) 0.087(2) Uani 1 1 d . . . O20 O 0.8491(4) 1.0152(3) 0.7056(3) 0.0653(16) Uani 1 1 d . . . O21 O 0.9246(3) 0.9278(3) 0.7062(3) 0.0536(13) Uani 1 1 d . . . O22 O 0.7574(4) 0.8620(3) 0.6787(3) 0.0619(15) Uani 1 1 d . . . O30 O 0.2137(3) 0.1231(3) -0.0038(3) 0.0506(12) Uani 1 1 d . . . O31 O 0.0877(3) -0.0082(3) -0.0153(2) 0.0357(10) Uani 1 1 d . . . O32 O 0.2439(4) 0.0110(3) 0.0129(3) 0.0548(14) Uani 1 1 d . . . O40 O 0.1997(4) 0.8248(3) 0.1235(3) 0.0489(12) Uani 1 1 d . . . O41 O 0.0596(3) 0.7107(3) 0.1146(3) 0.0511(12) Uani 1 1 d . . . O42 O 0.1870(3) 0.6834(3) 0.1056(2) 0.0465(12) Uani 1 1 d . . . F100 F 0.5181(3) 0.4454(4) 0.2206(3) 0.107(2) Uani 1 1 d . . . F101 F 0.3959(5) 0.3419(4) 0.2078(3) 0.119(3) Uani 1 1 d . . . F102 F 0.4363(3) 0.4751(3) 0.2764(2) 0.0716(14) Uani 1 1 d . . . F200 F 0.1681(4) 0.1399(4) 0.1325(3) 0.0890(17) Uani 1 1 d . . . F201 F 0.3130(3) 0.1689(3) 0.1596(3) 0.0761(15) Uani 1 1 d . . . F202 F 0.2064(3) 0.0459(3) 0.1465(2) 0.0708(14) Uani 1 1 d . . . F300 F 0.8757(4) 0.9476(3) 0.5654(3) 0.0941(18) Uani 1 1 d . . . F301 F 0.7922(4) 0.8131(3) 0.5420(3) 0.0859(16) Uani 1 1 d . . . F302 F 0.7279(4) 0.8915(4) 0.5417(3) 0.104(2) Uani 1 1 d . . . F400 F 0.3094(3) 0.8287(3) 0.2644(2) 0.0622(12) Uani 1 1 d . . . F401 F 0.1951(3) 0.8479(2) 0.2735(2) 0.0449(9) Uani 1 1 d . . . F402 F 0.1877(4) 0.7252(3) 0.2580(2) 0.0662(13) Uani 1 1 d . . . C68 C 0.2871(3) 0.5821(3) 0.8371(3) 0.0174(10) Uani 1 1 d . . . F500 F 0.8283(6) 0.8385(4) 0.3966(4) 0.131(3) Uani 1 1 d . A . O52 O 0.6635(7) 0.7988(6) 0.2596(6) 0.153(4) Uani 1 1 d . . . O51 O 0.7959(10) 0.8139(12) 0.2412(7) 0.268(9) Uani 1 1 d . . . O50 O 0.7672(6) 0.9288(5) 0.2617(6) 0.179(5) Uani 1 1 d . . . F502 F 0.9086(7) 0.9537(7) 0.3994(8) 0.256(7) Uani 1 1 d . A . F501 F 0.7902(10) 0.9364(7) 0.4124(5) 0.231(6) Uani 1 1 d . A . C501 C 0.8109 0.8903 0.3654 0.148(7) Uani 1 1 d . . . S50 S 0.7673(4) 0.8683(4) 0.2896(3) 0.0310(11) Uani 0.50 1 d P A 1 S51 S 0.7385(5) 0.8395(5) 0.2549(4) 0.0641(19) Uani 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0244(4) 0.0272(4) 0.0324(4) 0.0210(3) 0.0149(3) 0.0154(3) Cu2 0.0353(4) 0.0228(3) 0.0227(4) 0.0136(3) 0.0160(3) 0.0158(3) Cu3 0.0222(4) 0.0256(4) 0.0267(4) 0.0075(3) 0.0120(3) 0.0117(3) Cu10 0.0396(4) 0.0359(4) 0.0427(5) 0.0255(4) 0.0235(4) 0.0218(4) Se1 0.0726(5) 0.0290(3) 0.0364(3) 0.0253(3) 0.0398(3) 0.0334(3) Se2 0.0212(3) 0.0310(3) 0.0222(3) 0.0082(2) 0.0127(2) 0.0101(2) Se3 0.0193(3) 0.0228(3) 0.0254(3) 0.0146(2) 0.0100(2) 0.0104(2) N1 0.026(2) 0.029(3) 0.023(2) 0.015(2) 0.012(2) 0.015(2) N2 0.028(2) 0.018(2) 0.013(2) 0.0069(19) 0.0056(19) 0.0071(19) N11 0.030(3) 0.019(2) 0.018(2) 0.008(2) 0.009(2) 0.011(2) N12 0.020(2) 0.022(2) 0.025(2) 0.013(2) 0.0116(19) 0.0103(19) N21 0.027(3) 0.024(2) 0.030(3) 0.011(2) 0.017(2) 0.012(2) N22 0.023(2) 0.025(2) 0.022(2) 0.014(2) 0.0121(19) 0.013(2) P1 0.0314(8) 0.0177(7) 0.0181(7) 0.0101(6) 0.0119(6) 0.0115(6) P2 0.0191(7) 0.0188(7) 0.0182(7) 0.0107(6) 0.0100(5) 0.0077(5) P3 0.0189(7) 0.0186(7) 0.0216(7) 0.0122(6) 0.0109(6) 0.0095(6) C1 0.031(3) 0.026(3) 0.016(3) 0.011(2) 0.012(2) 0.020(3) C2 0.032(3) 0.020(3) 0.019(3) 0.008(2) 0.006(2) 0.013(2) C3 0.043(4) 0.027(3) 0.025(3) 0.003(3) 0.012(3) 0.009(3) C4 0.050(4) 0.033(4) 0.031(3) 0.007(3) 0.012(3) 0.013(3) C5 0.034(3) 0.029(3) 0.032(3) 0.012(3) 0.010(3) 0.009(3) C6 0.032(3) 0.017(3) 0.023(3) 0.008(2) 0.008(2) 0.008(2) C7 0.025(3) 0.014(2) 0.023(3) 0.009(2) 0.008(2) 0.012(2) C8 0.025(3) 0.021(3) 0.019(3) 0.015(2) 0.007(2) 0.011(2) C9 0.019(3) 0.014(2) 0.019(3) 0.005(2) 0.004(2) 0.003(2) C10 0.038(3) 0.020(3) 0.028(3) 0.014(3) 0.014(3) 0.013(3) C11 0.038(4) 0.028(3) 0.035(3) 0.022(3) 0.013(3) 0.011(3) C12 0.037(4) 0.037(3) 0.024(3) 0.021(3) 0.015(3) 0.012(3) C13 0.033(3) 0.026(3) 0.021(3) 0.012(2) 0.013(2) 0.010(3) C14 0.023(3) 0.024(3) 0.027(3) 0.012(3) 0.008(2) 0.010(2) C15 0.040(4) 0.033(3) 0.032(3) 0.014(3) 0.016(3) 0.021(3) C16 0.038(4) 0.042(4) 0.039(4) 0.009(3) 0.018(3) 0.027(3) C17 0.035(4) 0.045(4) 0.041(4) 0.016(3) 0.026(3) 0.019(3) C18 0.029(3) 0.035(3) 0.030(3) 0.018(3) 0.016(3) 0.015(3) C19 0.025(3) 0.036(3) 0.021(3) 0.015(3) 0.011(2) 0.011(3) C20 0.030(4) 0.057(4) 0.045(4) 0.031(4) 0.009(3) 0.013(3) C21 0.041(4) 0.086(6) 0.051(5) 0.042(5) 0.015(4) 0.034(4) C22 0.027(4) 0.093(7) 0.030(4) 0.008(4) 0.008(3) 0.016(4) C23 0.036(4) 0.077(6) 0.057(5) -0.012(5) 0.022(4) 0.010(4) C24 0.029(4) 0.046(4) 0.035(4) 0.001(3) 0.017(3) 0.008(3) OW2 0.033(2) 0.040(2) 0.043(3) 0.025(2) 0.019(2) 0.016(2) C31 0.013(2) 0.013(2) 0.021(3) 0.004(2) 0.007(2) 0.002(2) C32 0.015(3) 0.022(3) 0.027(3) 0.012(2) 0.010(2) 0.011(2) C33 0.024(3) 0.033(3) 0.048(4) 0.023(3) 0.017(3) 0.008(3) C34 0.022(3) 0.048(4) 0.063(4) 0.038(4) 0.025(3) 0.012(3) C35 0.036(4) 0.045(4) 0.053(4) 0.039(3) 0.031(3) 0.022(3) C36 0.035(3) 0.041(3) 0.040(3) 0.034(3) 0.026(3) 0.025(3) C37 0.027(3) 0.018(3) 0.026(3) 0.015(2) 0.016(2) 0.015(2) C38 0.024(3) 0.023(3) 0.019(3) 0.013(2) 0.013(2) 0.016(2) C39 0.021(3) 0.022(3) 0.015(2) 0.010(2) 0.009(2) 0.011(2) C40 0.027(3) 0.049(4) 0.026(3) 0.017(3) 0.013(3) 0.020(3) C41 0.030(3) 0.049(4) 0.022(3) 0.006(3) 0.018(3) 0.015(3) C42 0.028(3) 0.040(4) 0.021(3) 0.007(3) 0.002(3) 0.014(3) C43 0.021(3) 0.032(3) 0.030(3) 0.014(3) 0.014(2) 0.011(2) C44 0.018(3) 0.021(3) 0.027(3) 0.012(2) 0.009(2) 0.007(2) C45 0.040(4) 0.048(4) 0.028(3) 0.017(3) 0.016(3) 0.027(3) C46 0.040(4) 0.062(5) 0.039(4) 0.031(4) 0.014(3) 0.033(4) C47 0.040(4) 0.057(4) 0.023(3) 0.022(3) 0.003(3) 0.024(3) C48 0.035(3) 0.029(3) 0.018(3) 0.004(3) 0.007(3) 0.011(3) C49 0.025(3) 0.019(3) 0.022(3) 0.008(2) 0.001(2) 0.008(2) C50 0.062(5) 0.033(3) 0.025(3) 0.017(3) 0.016(3) 0.013(3) C51 0.100(7) 0.034(4) 0.061(5) 0.038(4) 0.022(5) 0.010(4) OW6 0.039(3) 0.039(2) 0.042(3) 0.021(2) 0.023(2) 0.025(2) C52 0.077(6) 0.026(4) 0.068(6) 0.019(4) -0.001(5) 0.025(4) OW4 0.051(3) 0.045(3) 0.045(3) 0.029(2) 0.023(2) 0.032(2) C53 0.062(5) 0.038(4) 0.080(6) 0.018(4) 0.025(4) 0.037(4) C54 0.044(4) 0.037(4) 0.071(5) 0.028(4) 0.033(4) 0.028(3) C61 0.030(3) 0.021(3) 0.024(3) 0.014(2) 0.017(2) 0.014(2) C62 0.031(3) 0.020(3) 0.032(3) 0.016(3) 0.017(3) 0.016(2) C63 0.048(4) 0.033(3) 0.037(3) 0.025(3) 0.025(3) 0.018(3) C64 0.068(5) 0.043(4) 0.032(3) 0.030(3) 0.031(3) 0.034(4) C65 0.063(5) 0.047(4) 0.036(4) 0.031(3) 0.032(3) 0.034(4) C66 0.048(4) 0.029(3) 0.030(3) 0.019(3) 0.015(3) 0.019(3) C67 0.024(3) 0.023(3) 0.030(3) 0.017(2) 0.014(2) 0.016(2) C69 0.027(3) 0.019(3) 0.013(2) 0.005(2) 0.011(2) 0.016(2) C70 0.023(3) 0.031(3) 0.025(3) 0.014(3) 0.009(2) 0.017(3) C71 0.021(3) 0.039(3) 0.026(3) 0.010(3) 0.008(2) 0.014(3) C72 0.023(3) 0.020(3) 0.040(3) 0.011(3) 0.013(3) 0.001(2) C73 0.033(3) 0.019(3) 0.030(3) 0.011(3) 0.016(3) 0.012(2) C74 0.028(3) 0.024(3) 0.032(3) 0.016(3) 0.019(3) 0.014(2) C75 0.048(4) 0.022(3) 0.043(4) 0.020(3) 0.022(3) 0.020(3) C76 0.064(5) 0.021(3) 0.051(4) 0.014(3) 0.030(4) 0.020(3) C77 0.042(4) 0.020(3) 0.041(4) 0.004(3) 0.017(3) 0.006(3) OW5 0.059(3) 0.036(3) 0.057(3) 0.026(2) 0.033(3) 0.014(2) C780 0.027(3) 0.032(3) 0.038(4) 0.012(3) 0.014(3) 0.012(3) C79 0.013(3) 0.024(3) 0.026(3) 0.008(2) 0.008(2) 0.007(2) C80 0.025(3) 0.026(3) 0.034(3) 0.011(3) 0.017(3) 0.009(3) C81 0.034(4) 0.052(4) 0.044(4) 0.016(4) 0.029(3) 0.015(3) C82 0.030(4) 0.056(5) 0.050(4) 0.009(4) 0.025(3) 0.022(3) C83 0.039(4) 0.048(4) 0.061(5) 0.015(4) 0.024(4) 0.031(3) C84 0.037(4) 0.035(3) 0.040(4) 0.011(3) 0.015(3) 0.022(3) OW3 0.056(3) 0.053(3) 0.058(3) 0.026(3) 0.034(3) 0.032(3) C100 0.047(4) 0.049(4) 0.037(4) 0.010(4) 0.009(3) 0.026(4) C200 0.041(4) 0.043(4) 0.038(4) 0.003(3) 0.011(3) 0.016(3) C300 0.069(6) 0.044(5) 0.086(7) 0.027(5) 0.033(5) 0.029(4) C400 0.062(5) 0.045(4) 0.029(3) 0.019(3) 0.019(3) 0.038(4) S10 0.0581(12) 0.0599(12) 0.0459(10) 0.0293(9) 0.0275(9) 0.0456(10) S20 0.0294(8) 0.0317(8) 0.0323(8) 0.0166(7) 0.0121(6) 0.0153(7) S30 0.0443(10) 0.0314(9) 0.0644(12) 0.0191(9) 0.0192(9) 0.0230(8) S40 0.0398(9) 0.0347(8) 0.0297(8) 0.0160(7) 0.0162(7) 0.0217(7) O10 0.059(3) 0.067(3) 0.040(3) 0.023(3) 0.024(2) 0.042(3) O11 0.202(9) 0.062(4) 0.109(6) 0.045(4) 0.072(6) 0.085(5) O12 0.049(3) 0.159(6) 0.048(3) 0.027(4) 0.023(3) 0.063(4) O20 0.066(4) 0.038(3) 0.083(4) 0.018(3) 0.019(3) 0.036(3) O21 0.040(3) 0.038(3) 0.084(4) 0.026(3) 0.024(3) 0.024(2) O22 0.049(3) 0.052(3) 0.089(4) 0.029(3) 0.036(3) 0.028(3) O30 0.037(3) 0.050(3) 0.067(3) 0.043(3) 0.019(2) 0.014(2) O31 0.032(2) 0.036(2) 0.036(2) 0.022(2) 0.0114(19) 0.0118(19) O32 0.060(3) 0.063(3) 0.041(3) 0.010(3) 0.014(2) 0.046(3) O40 0.066(3) 0.053(3) 0.052(3) 0.039(3) 0.035(3) 0.034(3) O41 0.030(3) 0.047(3) 0.062(3) 0.019(3) 0.014(2) 0.015(2) O42 0.063(3) 0.047(3) 0.032(2) 0.009(2) 0.015(2) 0.040(3) F100 0.043(3) 0.155(5) 0.052(3) -0.021(3) -0.004(2) 0.057(3) F101 0.199(7) 0.081(4) 0.071(4) 0.054(3) 0.029(4) 0.069(4) F102 0.040(2) 0.100(4) 0.036(2) 0.004(2) 0.0098(19) 0.027(3) F200 0.072(3) 0.094(4) 0.075(3) 0.001(3) 0.035(3) 0.047(3) F201 0.051(3) 0.063(3) 0.052(3) 0.001(2) 0.013(2) 0.001(2) F202 0.048(3) 0.100(4) 0.044(2) 0.043(3) 0.013(2) 0.016(3) F300 0.116(5) 0.064(3) 0.086(4) 0.037(3) 0.046(4) 0.029(3) F301 0.113(4) 0.045(3) 0.076(3) 0.012(3) 0.034(3) 0.035(3) F302 0.104(5) 0.112(5) 0.087(4) 0.038(4) 0.009(3) 0.073(4) F400 0.052(3) 0.075(3) 0.039(2) 0.009(2) 0.004(2) 0.038(2) F401 0.066(3) 0.047(2) 0.036(2) 0.0185(18) 0.0272(19) 0.039(2) F402 0.128(4) 0.066(3) 0.059(3) 0.048(2) 0.061(3) 0.069(3) C68 0.019(3) 0.020(3) 0.018(3) 0.010(2) 0.009(2) 0.013(2) F500 0.258(9) 0.128(5) 0.162(6) 0.120(5) 0.156(7) 0.151(6) O52 0.138(8) 0.157(8) 0.168(8) 0.104(7) 0.110(7) 0.029(6) O51 0.414(17) 0.66(3) 0.295(13) 0.413(17) 0.326(14) 0.51(2) O50 0.103(6) 0.098(6) 0.252(11) 0.122(7) -0.036(7) 0.019(5) F502 0.128(7) 0.205(9) 0.371(16) 0.230(11) -0.021(9) 0.036(7) F501 0.386(17) 0.242(11) 0.126(7) 0.040(7) 0.077(9) 0.269(12) C501 0.163(15) 0.068(8) 0.25(2) 0.088(12) 0.101(15) 0.076(10) S50 0.027(2) 0.029(2) 0.034(2) 0.012(2) 0.0125(19) 0.0125(17) S51 0.074(5) 0.098(6) 0.100(5) 0.081(5) 0.067(4) 0.067(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 N1 1.997(4) . ? Cu1 N22 1.997(4) . ? Cu1 Se3 2.4632(10) . ? Cu1 Se1 2.5525(10) . ? Cu2 N11 2.025(5) . ? Cu2 N2 2.028(4) . ? Cu2 Se1 2.4296(10) . ? Cu2 Se2 2.5428(10) . ? Cu3 N12 2.020(4) . ? Cu3 N21 2.026(5) . ? Cu3 Se2 2.4572(10) . ? Cu3 Se3 2.5431(10) 2_566 ? Cu10 OW5 1.963(5) . ? Cu10 OW2 1.966(4) . ? Cu10 OW6 1.975(4) . ? Cu10 OW3 1.992(5) . ? Cu10 OW4 2.248(4) . ? Se1 P1 2.1310(16) . ? Se2 P2 2.1366(14) . ? Se3 P3 2.1461(15) . ? Se3 Cu3 2.5431(10) 2_566 ? N1 C14 1.345(7) . ? N1 C18 1.351(7) . ? N2 C13 1.343(7) . ? N2 C9 1.346(6) . ? N11 C48 1.335(7) . ? N11 C44 1.351(7) . ? N12 C43 1.349(7) . ? N12 C39 1.360(6) . ? N21 C780 1.345(7) 2_566 ? N21 C74 1.354(7) 2_566 ? N22 C69 1.349(6) . ? N22 C73 1.352(7) . ? P1 C8 1.784(5) . ? P1 C1 1.792(5) . ? P1 C19 1.799(6) . ? P2 C38 1.798(5) . ? P2 C31 1.801(5) . ? P2 C49 1.809(5) . ? P3 C61 1.792(5) . ? P3 C79 1.806(5) . ? P3 C68 1.807(5) . ? C1 C2 1.356(7) . ? C1 C14 1.489(7) . ? C2 C7 1.485(7) . ? C2 C3 1.489(8) . ? C3 C4 1.527(8) . ? C4 C5 1.508(9) . ? C5 C6 1.520(8) . ? C6 C7 1.520(7) . ? C7 C8 1.334(7) . ? C8 C9 1.490(7) . ? C9 C10 1.403(7) . ? C10 C11 1.373(8) . ? C11 C12 1.383(8) . ? C12 C13 1.366(8) . ? C14 C15 1.379(8) . ? C15 C16 1.373(9) . ? C16 C17 1.366(9) . ? C17 C18 1.365(8) . ? C19 C24 1.380(8) . ? C19 C20 1.392(9) . ? C20 C21 1.396(9) . ? C21 C22 1.358(11) . ? C22 C23 1.392(13) . ? C23 C24 1.383(11) . ? C31 C32 1.344(7) . ? C31 C44 1.476(7) . ? C32 C37 1.483(7) . ? C32 C33 1.515(7) . ? C33 C34 1.479(8) . ? C34 C35 1.516(8) . ? C35 C36 1.522(8) . ? C36 C37 1.502(7) . ? C37 C38 1.357(7) . ? C38 C39 1.486(7) . ? C39 C40 1.356(7) . ? C40 C41 1.392(8) . ? C41 C42 1.392(8) . ? C42 C43 1.353(8) . ? C44 C45 1.386(8) . ? C45 C46 1.394(8) . ? C46 C47 1.355(9) . ? C47 C48 1.378(9) . ? C49 C54 1.367(8) . ? C49 C50 1.370(8) . ? C50 C51 1.412(10) . ? C51 C52 1.351(12) . ? C52 C53 1.360(12) . ? C53 C54 1.368(9) . ? C61 C62 1.332(7) . ? C61 C74 1.487(8) . ? C62 C67 1.502(7) . ? C62 C63 1.531(7) . ? C63 C64 1.509(9) . ? C64 C65 1.518(8) . ? C65 C66 1.515(8) . ? C66 C67 1.506(8) . ? C67 C68 1.349(7) . ? C69 C70 1.392(7) . ? C69 C68 1.474(7) . ? C70 C71 1.367(8) . ? C71 C72 1.366(8) . ? C72 C73 1.392(8) . ? C74 N21 1.354(7) 2_566 ? C74 C75 1.382(7) . ? C75 C76 1.360(9) . ? C76 C77 1.363(10) . ? C77 C780 1.380(9) . ? C780 N21 1.345(7) 2_566 ? C79 C80 1.387(8) . ? C79 C84 1.393(8) . ? C80 C81 1.394(8) . ? C81 C82 1.379(10) . ? C82 C83 1.361(10) . ? C83 C84 1.378(9) . ? C100 F100 1.281(8) . ? C100 F101 1.293(9) . ? C100 F102 1.347(8) . ? C100 S10 1.797(8) . ? C200 F200 1.311(8) . ? C200 F202 1.334(9) . ? C200 F201 1.350(8) . ? C200 S20 1.809(7) . ? C300 F301 1.301(9) . ? C300 F302 1.302(10) . ? C300 F300 1.362(10) . ? C300 S30 1.822(10) . ? C400 F401 1.301(7) . ? C400 F402 1.311(7) . ? C400 F400 1.354(8) . ? C400 S40 1.831(6) . ? S10 O12 1.395(6) . ? S10 O11 1.429(6) . ? S10 O10 1.427(5) . ? S20 O30 1.426(4) . ? S20 O32 1.427(5) . ? S20 O31 1.454(4) . ? S30 O20 1.429(5) . ? S30 O21 1.440(5) . ? S30 O22 1.440(5) . ? S40 O40 1.426(5) . ? S40 O42 1.434(4) . ? S40 O41 1.456(5) . ? F500 C501 1.378(5) . ? O52 S51 1.244(10) . ? O52 S50 1.522(10) . ? O51 S51 1.290(10) . ? O51 S50 1.489(11) . ? O50 S50 1.398(10) . ? O50 S51 1.476(10) . ? F502 C501 1.410(10) . ? F501 C501 1.287(8) . ? C501 S50 1.356(5) . ? C501 S51 1.934(7) . ? 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 N22 126.95(18) . . ? N1 Cu1 Se3 107.74(13) . . ? N22 Cu1 Se3 113.67(13) . . ? N1 Cu1 Se1 106.55(13) . . ? N22 Cu1 Se1 99.32(12) . . ? Se3 Cu1 Se1 97.75(3) . . ? N11 Cu2 N2 123.20(18) . . ? N11 Cu2 Se1 104.22(12) . . ? N2 Cu2 Se1 113.59(12) . . ? N11 Cu2 Se2 105.30(13) . . ? N2 Cu2 Se2 108.59(12) . . ? Se1 Cu2 Se2 99.03(4) . . ? N12 Cu3 N21 119.48(18) . . ? N12 Cu3 Se2 113.32(13) . . ? N21 Cu3 Se2 109.38(14) . . ? N12 Cu3 Se3 109.28(12) . 2_566 ? N21 Cu3 Se3 102.30(13) . 2_566 ? Se2 Cu3 Se3 100.86(4) . 2_566 ? OW5 Cu10 OW2 171.9(2) . . ? OW5 Cu10 OW6 91.97(18) . . ? OW2 Cu10 OW6 87.24(18) . . ? OW5 Cu10 OW3 90.5(2) . . ? OW2 Cu10 OW3 90.20(19) . . ? OW6 Cu10 OW3 177.43(19) . . ? OW5 Cu10 OW4 98.62(19) . . ? OW2 Cu10 OW4 89.43(17) . . ? OW6 Cu10 OW4 91.40(17) . . ? OW3 Cu10 OW4 88.79(18) . . ? P1 Se1 Cu2 89.49(4) . . ? P1 Se1 Cu1 94.51(4) . . ? Cu2 Se1 Cu1 175.99(3) . . ? P2 Se2 Cu3 89.63(5) . . ? P2 Se2 Cu2 95.91(5) . . ? Cu3 Se2 Cu2 139.52(4) . . ? P3 Se3 Cu1 91.71(5) . . ? P3 Se3 Cu3 94.92(5) . 2_566 ? Cu1 Se3 Cu3 140.53(3) . 2_566 ? C14 N1 C18 115.8(5) . . ? C14 N1 Cu1 128.4(4) . . ? C18 N1 Cu1 115.8(4) . . ? C13 N2 C9 117.8(5) . . ? C13 N2 Cu2 114.1(4) . . ? C9 N2 Cu2 128.0(3) . . ? C48 N11 C44 117.0(5) . . ? C48 N11 Cu2 119.3(4) . . ? C44 N11 Cu2 123.7(4) . . ? C43 N12 C39 116.3(4) . . ? C43 N12 Cu3 114.9(3) . . ? C39 N12 Cu3 128.5(4) . . ? C780 N21 C74 117.6(5) 2_566 2_566 ? C780 N21 Cu3 118.2(4) 2_566 . ? C74 N21 Cu3 123.9(4) 2_566 . ? C69 N22 C73 117.0(5) . . ? C69 N22 Cu1 128.3(4) . . ? C73 N22 Cu1 114.7(4) . . ? C8 P1 C1 93.1(2) . . ? C8 P1 C19 111.5(2) . . ? C1 P1 C19 109.0(3) . . ? C8 P1 Se1 114.96(18) . . ? C1 P1 Se1 112.48(17) . . ? C19 P1 Se1 114.0(2) . . ? C38 P2 C31 93.1(2) . . ? C38 P2 C49 107.7(2) . . ? C31 P2 C49 108.6(2) . . ? C38 P2 Se2 119.09(17) . . ? C31 P2 Se2 112.39(17) . . ? C49 P2 Se2 113.80(19) . . ? C61 P3 C79 109.6(2) . . ? C61 P3 C68 93.6(2) . . ? C79 P3 C68 109.4(2) . . ? C61 P3 Se3 113.49(18) . . ? C79 P3 Se3 112.97(19) . . ? C68 P3 Se3 116.14(16) . . ? C2 C1 C14 130.2(5) . . ? C2 C1 P1 108.9(4) . . ? C14 C1 P1 120.2(4) . . ? C1 C2 C7 113.4(5) . . ? C1 C2 C3 125.1(5) . . ? C7 C2 C3 121.4(5) . . ? C2 C3 C4 115.4(5) . . ? C5 C4 C3 110.6(5) . . ? C4 C5 C6 110.5(5) . . ? C7 C6 C5 111.9(5) . . ? C8 C7 C2 115.3(5) . . ? C8 C7 C6 126.1(5) . . ? C2 C7 C6 118.6(5) . . ? C7 C8 C9 127.8(5) . . ? C7 C8 P1 108.9(4) . . ? C9 C8 P1 123.1(4) . . ? N2 C9 C10 120.2(5) . . ? N2 C9 C8 120.2(4) . . ? C10 C9 C8 119.5(5) . . ? C11 C10 C9 120.7(5) . . ? C10 C11 C12 118.6(5) . . ? C13 C12 C11 117.8(5) . . ? N2 C13 C12 124.8(5) . . ? N1 C14 C15 122.4(5) . . ? N1 C14 C1 118.4(5) . . ? C15 C14 C1 119.1(5) . . ? C16 C15 C14 120.4(6) . . ? C17 C16 C15 117.8(6) . . ? C18 C17 C16 119.2(6) . . ? N1 C18 C17 124.4(6) . . ? C24 C19 C20 121.6(6) . . ? C24 C19 P1 120.8(5) . . ? C20 C19 P1 117.6(5) . . ? C19 C20 C21 119.4(7) . . ? C22 C21 C20 119.3(8) . . ? C21 C22 C23 120.9(7) . . ? C24 C23 C22 120.9(8) . . ? C19 C24 C23 117.9(7) . . ? C32 C31 C44 126.0(5) . . ? C32 C31 P2 108.5(4) . . ? C44 C31 P2 125.5(4) . . ? C31 C32 C37 115.3(4) . . ? C31 C32 C33 124.5(5) . . ? C37 C32 C33 120.1(5) . . ? C34 C33 C32 113.8(5) . . ? C33 C34 C35 111.3(5) . . ? C34 C35 C36 111.6(5) . . ? C37 C36 C35 113.5(5) . . ? C38 C37 C32 114.2(4) . . ? C38 C37 C36 126.3(5) . . ? C32 C37 C36 119.4(5) . . ? C37 C38 C39 127.6(4) . . ? C37 C38 P2 108.8(4) . . ? C39 C38 P2 123.0(4) . . ? C40 C39 N12 122.1(5) . . ? C40 C39 C38 121.0(5) . . ? N12 C39 C38 116.8(4) . . ? C39 C40 C41 120.9(5) . . ? C40 C41 C42 117.1(5) . . ? C43 C42 C41 118.9(5) . . ? N12 C43 C42 124.6(5) . . ? N11 C44 C45 121.7(5) . . ? N11 C44 C31 118.5(5) . . ? C45 C44 C31 119.8(5) . . ? C44 C45 C46 119.5(6) . . ? C47 C46 C45 118.6(6) . . ? C46 C47 C48 118.7(6) . . ? N11 C48 C47 124.4(6) . . ? C54 C49 C50 121.3(6) . . ? C54 C49 P2 117.8(5) . . ? C50 C49 P2 120.8(5) . . ? C49 C50 C51 116.8(7) . . ? C52 C51 C50 122.4(7) . . ? C51 C52 C53 118.3(6) . . ? C52 C53 C54 121.6(7) . . ? C49 C54 C53 119.5(7) . . ? C62 C61 C74 127.8(5) . . ? C62 C61 P3 108.9(4) . . ? C74 C61 P3 123.4(4) . . ? C61 C62 C67 114.9(5) . . ? C61 C62 C63 125.0(5) . . ? C67 C62 C63 119.9(5) . . ? C64 C63 C62 113.4(5) . . ? C63 C64 C65 112.3(5) . . ? C66 C65 C64 109.6(5) . . ? C67 C66 C65 113.5(5) . . ? C68 C67 C62 114.7(5) . . ? C68 C67 C66 126.3(5) . . ? C62 C67 C66 119.1(5) . . ? N22 C69 C70 122.3(5) . . ? N22 C69 C68 118.2(4) . . ? C70 C69 C68 119.5(5) . . ? C71 C70 C69 119.6(5) . . ? C70 C71 C72 119.2(5) . . ? C71 C72 C73 119.0(5) . . ? N22 C73 C72 122.9(5) . . ? N21 C74 C75 121.7(5) 2_566 . ? N21 C74 C61 117.9(5) 2_566 . ? C75 C74 C61 120.5(5) . . ? C76 C75 C74 119.3(6) . . ? C75 C76 C77 120.2(6) . . ? C76 C77 C780 118.3(6) . . ? N21 C780 C77 122.9(6) 2_566 . ? C80 C79 C84 119.8(5) . . ? C80 C79 P3 119.9(4) . . ? C84 C79 P3 120.2(4) . . ? C79 C80 C81 119.5(6) . . ? C82 C81 C80 120.2(6) . . ? C83 C82 C81 119.8(6) . . ? C82 C83 C84 121.5(7) . . ? C83 C84 C79 119.3(6) . . ? F100 C100 F101 107.9(7) . . ? F100 C100 F102 107.7(6) . . ? F101 C100 F102 107.6(7) . . ? F100 C100 S10 113.0(6) . . ? F101 C100 S10 110.2(5) . . ? F102 C100 S10 110.2(5) . . ? F200 C200 F202 108.5(6) . . ? F200 C200 F201 109.2(6) . . ? F202 C200 F201 107.4(6) . . ? F200 C200 S20 110.7(5) . . ? F202 C200 S20 110.4(5) . . ? F201 C200 S20 110.5(5) . . ? F301 C300 F302 109.6(8) . . ? F301 C300 F300 107.1(7) . . ? F302 C300 F300 107.7(8) . . ? F301 C300 S30 111.6(6) . . ? F302 C300 S30 111.3(6) . . ? F300 C300 S30 109.3(6) . . ? F401 C400 F402 110.1(5) . . ? F401 C400 F400 107.6(5) . . ? F402 C400 F400 106.5(6) . . ? F401 C400 S40 111.9(4) . . ? F402 C400 S40 112.0(5) . . ? F400 C400 S40 108.5(4) . . ? O12 S10 O11 113.4(5) . . ? O12 S10 O10 116.7(4) . . ? O11 S10 O10 113.1(4) . . ? O12 S10 C100 105.3(4) . . ? O11 S10 C100 102.9(4) . . ? O10 S10 C100 103.6(3) . . ? O30 S20 O32 115.7(3) . . ? O30 S20 O31 114.3(3) . . ? O32 S20 O31 113.8(3) . . ? O30 S20 C200 105.6(3) . . ? O32 S20 C200 103.3(3) . . ? O31 S20 C200 102.0(3) . . ? O20 S30 O21 115.0(3) . . ? O20 S30 O22 115.7(3) . . ? O21 S30 O22 114.9(3) . . ? O20 S30 C300 103.7(4) . . ? O21 S30 C300 103.2(4) . . ? O22 S30 C300 101.7(4) . . ? O40 S40 O42 117.0(3) . . ? O40 S40 O41 112.6(3) . . ? O42 S40 O41 115.1(3) . . ? O40 S40 C400 103.8(3) . . ? O42 S40 C400 103.7(3) . . ? O41 S40 C400 102.3(3) . . ? C67 C68 C69 127.6(5) . . ? C67 C68 P3 107.9(4) . . ? C69 C68 P3 124.1(4) . . ? S51 O52 S50 23.9(4) . . ? S51 O51 S50 25.1(4) . . ? S50 O50 S51 25.3(3) . . ? F501 C501 S50 116.6(5) . . ? F501 C501 F500 104.8(5) . . ? S50 C501 F500 128.1(4) . . ? F501 C501 F502 96.0(8) . . ? S50 C501 F502 112.3(6) . . ? F500 C501 F502 91.8(5) . . ? F501 C501 S51 120.0(5) . . ? S50 C501 S51 9.2(4) . . ? F500 C501 S51 119.7(4) . . ? F502 C501 S51 118.9(6) . . ? C501 S50 O50 124.4(6) . . ? C501 S50 O51 111.4(6) . . ? O50 S50 O51 105.5(8) . . ? C501 S50 O52 107.1(5) . . ? O50 S50 O52 106.2(7) . . ? O51 S50 O52 99.1(8) . . ? O52 S51 O51 129.5(11) . . ? O52 S51 O50 118.2(9) . . ? O51 S51 O50 112.3(10) . . ? O52 S51 C501 90.9(6) . . ? O51 S51 C501 91.5(7) . . ? O50 S51 C501 90.2(5) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.223 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.146 _database_code_depnum_ccdc_archive 'CCDC 927133' ####################################################################### # # 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_import #TrackingRef 'web_deposit_cif_file_0_LESCOP_1366057704.import.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H47 Cl8 Cu F9 N4 O9 P2 S5' _chemical_formula_sum 'C55 H47 Cl8 Cu F9 N4 O9 P2 S5' _chemical_formula_weight 1648.35 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' 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' P P 0.1023 0.0942 '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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnaa loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 15.993(2) _cell_length_b 26.367(3) _cell_length_c 32.189(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13574(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.45 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6664 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method none _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 51614 _diffrn_reflns_av_R_equivalents 0.1208 _diffrn_reflns_av_sigmaI/netI 0.1339 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 26.45 _reflns_number_total 13773 _reflns_number_gt 8270 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+113.4272P] 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 13773 _refine_ls_number_parameters 857 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1770 _refine_ls_R_factor_gt 0.1098 _refine_ls_wR_factor_ref 0.2576 _refine_ls_wR_factor_gt 0.2273 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.73696(6) 0.05570(4) 0.58655(3) 0.0151(2) Uani 1 1 d . . . P1 P 0.74036(13) 0.07249(7) 0.49233(6) 0.0128(4) Uani 1 1 d . . . P2 P 0.74159(13) -0.00424(8) 0.66769(6) 0.0132(4) Uani 1 1 d . . . S1 S 0.81045(13) 0.02975(7) 0.52845(6) 0.0156(4) Uani 1 1 d . . . S2 S 0.66779(13) -0.01056(8) 0.61870(6) 0.0170(4) Uani 1 1 d . . . N1 N 0.6474(4) 0.1096(2) 0.57669(19) 0.0158(15) Uani 1 1 d . . . N2 N 0.9405(4) 0.0638(3) 0.4561(2) 0.0215(16) Uani 1 1 d . . . N3 N 0.8269(4) 0.0910(2) 0.62166(19) 0.0149(14) Uani 1 1 d . . . N4 N 0.5431(4) -0.0421(3) 0.6961(2) 0.0218(16) Uani 1 1 d . . . C1 C 0.7130(5) 0.1340(3) 0.5119(2) 0.0118(16) Uani 1 1 d . . . C2 C 0.7642(5) 0.1689(3) 0.4958(2) 0.0168(17) Uani 1 1 d . . . C3 C 0.7692(5) 0.2242(3) 0.5076(3) 0.0226(19) Uani 1 1 d . . . H3A H 0.7429 0.2293 0.5345 0.027 Uiso 1 1 calc R . . H3B H 0.7395 0.2445 0.4873 0.027 Uiso 1 1 calc R . . C4 C 0.8614(5) 0.2411(3) 0.5096(3) 0.024(2) Uani 1 1 d . . . H4A H 0.8642 0.2768 0.5165 0.029 Uiso 1 1 calc R . . H4B H 0.8901 0.2223 0.5313 0.029 Uiso 1 1 calc R . . C5 C 0.9048(6) 0.2319(3) 0.4682(3) 0.027(2) Uani 1 1 d . . . H5A H 0.8866 0.2575 0.4486 0.033 Uiso 1 1 calc R . . H5B H 0.9647 0.2358 0.4720 0.033 Uiso 1 1 calc R . . C6 C 0.8874(5) 0.1799(3) 0.4503(3) 0.0193(18) Uani 1 1 d . . . H6 H 0.9222 0.1671 0.4297 0.023 Uiso 1 1 calc R . . C7 C 0.8226(5) 0.1521(3) 0.4637(2) 0.0144(17) Uani 1 1 d . . . C8 C 0.8001(5) 0.0996(3) 0.4478(2) 0.0160(17) Uani 1 1 d . . . H8 H 0.7611 0.1038 0.4246 0.019 Uiso 1 1 calc R . . C9 C 0.8678(5) 0.0645(3) 0.4339(2) 0.0162(18) Uani 1 1 d . . . C10 C 0.8572(6) 0.0312(3) 0.4015(3) 0.0218(19) Uani 1 1 d . . . H10 H 0.8092 0.0319 0.3852 0.026 Uiso 1 1 calc R . . C11 C 0.9226(6) -0.0043(3) 0.3939(3) 0.029(2) Uiso 1 1 d . . . H11 H 0.9168 -0.0281 0.3728 0.034 Uiso 1 1 calc R . . C12 C 0.9938(6) -0.0036(4) 0.4173(3) 0.032(2) Uani 1 1 d . . . H12 H 1.0365 -0.0267 0.4121 0.039 Uiso 1 1 calc R . . C13 C 1.0018(6) 0.0308(4) 0.4480(3) 0.030(2) Uani 1 1 d . . . H13 H 1.0505 0.0316 0.4637 0.036 Uiso 1 1 calc R . . C14 C 0.6483(5) 0.1418(3) 0.5444(2) 0.0114(16) Uani 1 1 d . . . C15 C 0.5917(5) 0.1818(3) 0.5418(3) 0.0197(19) Uani 1 1 d . . . H15 H 0.5929 0.2035 0.5189 0.024 Uiso 1 1 calc R . . C16 C 0.5336(6) 0.1894(3) 0.5731(3) 0.029(2) Uani 1 1 d . . . H16 H 0.4960 0.2162 0.5718 0.034 Uiso 1 1 calc R . . C17 C 0.5327(5) 0.1562(3) 0.6063(3) 0.027(2) Uani 1 1 d . . . H17 H 0.4946 0.1602 0.6279 0.033 Uiso 1 1 calc R . . C18 C 0.5896(5) 0.1168(3) 0.6068(3) 0.0182(18) Uani 1 1 d . . . H18 H 0.5881 0.0941 0.6289 0.022 Uiso 1 1 calc R . . C19 C 0.6504(5) 0.0395(3) 0.4723(2) 0.0150(17) Uani 1 1 d . . . C20 C 0.6369(5) -0.0109(3) 0.4827(3) 0.0206(19) Uani 1 1 d . . . H20 H 0.6731 -0.0275 0.5008 0.025 Uiso 1 1 calc R . . C21 C 0.5690(5) -0.0366(4) 0.4660(3) 0.027(2) Uani 1 1 d . . . H21 H 0.5597 -0.0704 0.4726 0.032 Uiso 1 1 calc R . . C22 C 0.5157(6) -0.0115(4) 0.4396(3) 0.030(2) Uani 1 1 d . . . H22 H 0.4703 -0.0289 0.4284 0.036 Uiso 1 1 calc R . . C23 C 0.5276(6) 0.0382(3) 0.4292(3) 0.028(2) Uani 1 1 d . . . H23 H 0.4904 0.0545 0.4115 0.034 Uiso 1 1 calc R . . C24 C 0.5960(6) 0.0645(4) 0.4454(3) 0.029(2) Uani 1 1 d . . . H24 H 0.6051 0.0983 0.4384 0.035 Uiso 1 1 calc R . . C31 C 0.7622(5) 0.0592(3) 0.6845(2) 0.0143(16) Uani 1 1 d . . . C32 C 0.7118(5) 0.0715(3) 0.7171(2) 0.0165(18) Uani 1 1 d . . . C33 C 0.7007(6) 0.1233(3) 0.7359(3) 0.025(2) Uani 1 1 d . . . H33A H 0.7150 0.1492 0.7157 0.030 Uiso 1 1 calc R . . H33B H 0.7375 0.1271 0.7597 0.030 Uiso 1 1 calc R . . C34 C 0.6097(6) 0.1297(4) 0.7496(3) 0.035(2) Uani 1 1 d . . . H34A H 0.6031 0.1626 0.7628 0.041 Uiso 1 1 calc R . . H34B H 0.5739 0.1289 0.7253 0.041 Uiso 1 1 calc R . . C35 C 0.5825(6) 0.0888(4) 0.7795(3) 0.035(3) Uani 1 1 d . . . H35A H 0.6078 0.0950 0.8064 0.042 Uiso 1 1 calc R . . H35B H 0.5222 0.0904 0.7829 0.042 Uiso 1 1 calc R . . C36 C 0.6066(5) 0.0367(4) 0.7647(3) 0.026(2) Uani 1 1 d . . . H36 H 0.5813 0.0086 0.7768 0.031 Uiso 1 1 calc R . . C37 C 0.6628(5) 0.0297(3) 0.7349(2) 0.0179(18) Uani 1 1 d . . . C38 C 0.6875(5) -0.0217(3) 0.7168(2) 0.0143(17) Uani 1 1 d . . . H38 H 0.7286 -0.0373 0.7355 0.017 Uiso 1 1 calc R . . C39 C 0.6194(5) -0.0591(3) 0.7092(2) 0.0189(18) Uani 1 1 d . . . C40 C 0.6311(5) -0.1100(3) 0.7129(3) 0.025(2) Uani 1 1 d . . . H40 H 0.6824 -0.1224 0.7219 0.030 Uiso 1 1 calc R . . C41 C 0.5673(6) -0.1436(4) 0.7031(3) 0.038(3) Uani 1 1 d . . . H41 H 0.5764 -0.1784 0.7051 0.045 Uiso 1 1 calc R . . C42 C 0.4898(6) -0.1254(3) 0.6905(4) 0.041(3) Uani 1 1 d . . . H42 H 0.4460 -0.1474 0.6846 0.049 Uiso 1 1 calc R . . C43 C 0.4798(6) -0.0734(4) 0.6870(3) 0.032(2) Uani 1 1 d . . . H43 H 0.4288 -0.0602 0.6783 0.039 Uiso 1 1 calc R . . C44 C 0.8216(5) 0.0931(3) 0.6637(2) 0.0139(17) Uani 1 1 d . . . C45 C 0.8744(5) 0.1255(3) 0.6866(3) 0.0160(18) Uani 1 1 d . . . H45 H 0.8712 0.1262 0.7154 0.019 Uiso 1 1 calc R . . C46 C 0.9311(5) 0.1563(3) 0.6659(3) 0.0193(18) Uani 1 1 d . . . H46 H 0.9648 0.1787 0.6806 0.023 Uiso 1 1 calc R . . C47 C 0.9367(5) 0.1532(3) 0.6233(3) 0.0191(18) Uani 1 1 d . . . H47 H 0.9757 0.1725 0.6089 0.023 Uiso 1 1 calc R . . C48 C 0.8831(5) 0.1208(3) 0.6023(3) 0.0180(18) Uani 1 1 d . . . H48 H 0.8861 0.1196 0.5735 0.022 Uiso 1 1 calc R . . C49 C 0.8354(5) -0.0418(3) 0.6623(2) 0.0133(16) Uani 1 1 d . . . C50 C 0.8952(5) -0.0414(3) 0.6943(2) 0.0169(17) Uani 1 1 d . . . H50 H 0.8882 -0.0209 0.7175 0.020 Uiso 1 1 calc R . . C51 C 0.9651(5) -0.0724(3) 0.6902(3) 0.0226(19) Uani 1 1 d . . . H51 H 1.0054 -0.0725 0.7111 0.027 Uiso 1 1 calc R . . C52 C 0.9755(5) -0.1029(3) 0.6559(3) 0.024(2) Uani 1 1 d . . . H52 H 1.0226 -0.1234 0.6536 0.029 Uiso 1 1 calc R . . C53 C 0.9161(5) -0.1030(3) 0.6249(3) 0.0213(19) Uani 1 1 d . . . H53 H 0.9231 -0.1238 0.6019 0.026 Uiso 1 1 calc R . . C54 C 0.8458(5) -0.0722(3) 0.6278(3) 0.0190(18) Uani 1 1 d . . . H54 H 0.8062 -0.0720 0.6066 0.023 Uiso 1 1 calc R . . C100 C 0.3302(6) 0.0648(4) 0.6488(3) 0.033(2) Uani 1 1 d . . . C200 C 0.1643(6) 0.1232(4) 0.5433(3) 0.029(2) Uani 1 1 d . . . C300 C 0.2166(7) 0.8301(4) 0.6781(3) 0.036(2) Uani 1 1 d . . . C910 C 0.8635(14) 0.3517(5) 0.4007(4) 0.098(7) Uani 1 1 d . . . C920 C 0.1813(10) 0.2271(5) 0.6329(5) 0.086(5) Uani 1 1 d . . . H92A H 0.1496 0.2223 0.6076 0.103 Uiso 1 1 calc R . . H92B H 0.2073 0.1949 0.6398 0.103 Uiso 1 1 calc R . . C930 C 0.0981(6) 0.2428(4) 0.3949(3) 0.036(2) Uani 1 1 d . . . H93A H 0.0977 0.2153 0.4149 0.044 Uiso 1 1 calc R . . H93B H 0.1442 0.2371 0.3759 0.044 Uiso 1 1 calc R . . C960 C 0.4013(15) 0.6951(10) 0.7311(7) 0.059(8) Uani 0.50 1 d P . . H96A H 0.3915 0.6725 0.7544 0.071 Uiso 0.50 1 calc PR . . H96B H 0.4489 0.6818 0.7160 0.071 Uiso 0.50 1 calc PR . . O100 O 0.3669(4) 0.0315(3) 0.7218(2) 0.0406(18) Uani 1 1 d . . . O101 O 0.3980(4) 0.1195(2) 0.7053(2) 0.0370(17) Uani 1 1 d . . . O102 O 0.4803(4) 0.0514(2) 0.67480(18) 0.0273(14) Uani 1 1 d . . . O200 O 0.0100(4) 0.1150(2) 0.52232(18) 0.0263(14) Uani 1 1 d . . . O201 O 0.0638(4) 0.1982(2) 0.5413(2) 0.0328(16) Uani 1 1 d . . . O202 O 0.1015(4) 0.1601(3) 0.47517(19) 0.0395(18) Uani 1 1 d . . . O300 O 0.2963(4) 0.8945(2) 0.72253(18) 0.0284(15) Uani 1 1 d . . . O301 O 0.1681(4) 0.9218(3) 0.6885(2) 0.0333(16) Uani 1 1 d . . . O302 O 0.2935(4) 0.9061(3) 0.64758(19) 0.0352(16) Uani 1 1 d . . . F100 F 0.3276(4) 0.0188(3) 0.63219(19) 0.0518(17) Uani 1 1 d . . . F101 F 0.2520(3) 0.0766(3) 0.66070(18) 0.0576(19) Uani 1 1 d . . . F102 F 0.3522(4) 0.0969(2) 0.61915(16) 0.0429(15) Uani 1 1 d . . . F200 F 0.1484(4) 0.1146(2) 0.58304(16) 0.0377(14) Uani 1 1 d . . . F201 F 0.1843(4) 0.0799(2) 0.5252(2) 0.0546(18) Uani 1 1 d . . . F202 F 0.2321(3) 0.1533(2) 0.54092(18) 0.0431(15) Uani 1 1 d . . . F300 F 0.2836(4) 0.7998(2) 0.6761(2) 0.0590(19) Uani 1 1 d . . . F301 F 0.1689(4) 0.8127(2) 0.7088(2) 0.0560(18) Uani 1 1 d . . . F302 F 0.1737(4) 0.8233(2) 0.64294(18) 0.0514(17) Uani 1 1 d . . . S100 S 0.40105(14) 0.06716(8) 0.69312(6) 0.0213(5) Uani 1 1 d . . . S200 S 0.07522(14) 0.15290(8) 0.51726(6) 0.0205(5) Uani 1 1 d . . . S300 S 0.24702(13) 0.89548(9) 0.68511(7) 0.0254(5) Uani 1 1 d . . . Cl1 Cl 0.4281(4) 0.7500 0.7500 0.0826(16) Uani 1 2 d S . . Cl2 Cl 0.3179(4) 0.6916(2) 0.69978(19) 0.0588(17) Uani 0.50 1 d P . . Cl5 Cl 0.1177(3) 0.24218(18) 0.66958(12) 0.1016(17) Uani 1 1 d . . . Cl6 Cl 0.2621(3) 0.27288(17) 0.62341(11) 0.0953(16) Uani 1 1 d . . . Cl7 Cl 0.1140(2) 0.29972(11) 0.42087(10) 0.0584(9) Uani 1 1 d . . . Cl8 Cl 0.00393(17) 0.24200(10) 0.36693(8) 0.0409(6) Uani 1 1 d . . . Cl9 Cl 0.8044(2) 0.31059(17) 0.37768(15) 0.0931(14) Uani 1 1 d . . . Cl10 Cl 0.8223(5) 0.3651(4) 0.4503(3) 0.046(2) Uani 0.50 1 d P . . Cl50 Cl 0.9649(4) 0.2500 0.7500 0.115(3) Uani 1 2 d S . . Cl51 Cl 0.7880(4) 0.2500 0.7500 0.147(4) Uani 1 2 d S . . C950 C 0.8743(19) 0.2647(9) 0.7237(8) 0.066(8) Uani 0.50 1 d P . . Cl11 Cl 0.8708(15) 0.3653(5) 0.4576(5) 0.208(12) 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 0.0126(5) 0.0169(5) 0.0157(5) -0.0007(4) -0.0039(4) 0.0013(4) P1 0.0098(10) 0.0139(9) 0.0147(10) -0.0015(8) -0.0023(8) 0.0003(8) P2 0.0086(10) 0.0162(10) 0.0148(10) -0.0001(8) -0.0005(8) 0.0002(8) S1 0.0151(10) 0.0162(10) 0.0156(10) -0.0016(8) -0.0039(8) 0.0059(8) S2 0.0144(10) 0.0180(10) 0.0186(10) 0.0009(8) -0.0057(8) -0.0014(9) N1 0.012(4) 0.020(4) 0.016(4) -0.006(3) -0.002(3) 0.003(3) N2 0.013(4) 0.028(4) 0.024(4) 0.010(3) 0.000(3) 0.003(3) N3 0.015(4) 0.014(3) 0.016(3) 0.000(3) -0.003(3) 0.000(3) N4 0.006(3) 0.031(4) 0.028(4) -0.001(3) -0.002(3) 0.001(3) C1 0.008(4) 0.011(4) 0.016(4) 0.003(3) -0.003(3) 0.005(3) C2 0.011(4) 0.017(4) 0.022(4) -0.003(3) -0.008(4) 0.004(3) C3 0.022(5) 0.018(4) 0.027(5) -0.003(4) 0.002(4) -0.003(4) C4 0.025(5) 0.015(4) 0.033(5) 0.003(4) -0.007(4) -0.004(4) C5 0.026(5) 0.019(5) 0.036(5) 0.000(4) 0.005(4) 0.001(4) C6 0.014(4) 0.020(4) 0.024(5) 0.004(4) -0.002(4) 0.002(4) C7 0.012(4) 0.014(4) 0.017(4) 0.003(3) -0.006(3) 0.002(3) C8 0.018(4) 0.012(4) 0.018(4) 0.000(3) 0.002(3) -0.003(3) C9 0.018(4) 0.022(4) 0.009(4) 0.006(3) -0.001(3) -0.007(4) C10 0.022(5) 0.022(4) 0.022(4) 0.003(4) 0.000(4) -0.008(4) C12 0.028(5) 0.030(5) 0.039(6) 0.010(5) 0.011(5) 0.004(4) C13 0.016(5) 0.043(6) 0.030(5) 0.009(5) 0.003(4) 0.014(4) C14 0.005(4) 0.009(4) 0.020(4) -0.005(3) 0.000(3) 0.001(3) C15 0.021(5) 0.015(4) 0.023(5) 0.007(3) 0.002(4) 0.006(4) C16 0.019(5) 0.025(5) 0.042(6) -0.002(4) 0.002(4) 0.003(4) C17 0.015(5) 0.030(5) 0.037(5) 0.003(4) 0.009(4) 0.007(4) C18 0.019(5) 0.015(4) 0.021(4) 0.000(3) -0.001(4) -0.002(4) C19 0.010(4) 0.022(4) 0.013(4) -0.003(3) -0.001(3) 0.003(3) C20 0.020(5) 0.021(4) 0.020(4) 0.000(3) -0.004(4) 0.004(4) C21 0.016(5) 0.031(5) 0.035(5) -0.008(4) -0.001(4) -0.004(4) C22 0.015(5) 0.038(6) 0.037(6) -0.014(4) -0.001(4) -0.008(4) C23 0.023(5) 0.027(5) 0.036(5) 0.001(4) -0.016(4) -0.005(4) C24 0.022(5) 0.040(6) 0.026(5) 0.009(4) -0.006(4) -0.001(4) C31 0.009(4) 0.013(4) 0.022(4) -0.002(3) -0.009(3) 0.003(3) C32 0.010(4) 0.022(4) 0.017(4) -0.003(3) -0.009(3) 0.008(3) C33 0.026(5) 0.026(5) 0.023(5) -0.009(4) -0.006(4) 0.006(4) C34 0.022(5) 0.030(5) 0.051(6) -0.022(5) 0.000(5) 0.008(4) C35 0.020(5) 0.053(7) 0.032(5) -0.030(5) 0.008(4) -0.002(5) C36 0.010(4) 0.043(6) 0.024(5) -0.011(4) -0.002(4) 0.006(4) C37 0.012(4) 0.024(4) 0.018(4) 0.001(3) -0.001(3) 0.005(4) C38 0.008(4) 0.018(4) 0.017(4) 0.005(3) 0.001(3) 0.004(3) C39 0.023(5) 0.018(4) 0.016(4) -0.002(3) 0.007(4) 0.001(4) C40 0.011(4) 0.028(5) 0.036(5) -0.001(4) -0.003(4) 0.006(4) C41 0.024(5) 0.019(5) 0.070(8) -0.003(5) -0.002(5) 0.000(4) C42 0.023(5) 0.016(5) 0.083(8) -0.007(5) -0.012(5) -0.002(4) C43 0.011(5) 0.035(6) 0.051(6) 0.000(5) -0.003(4) 0.001(4) C44 0.015(4) 0.015(4) 0.013(4) -0.002(3) -0.003(3) 0.007(3) C45 0.021(5) 0.006(4) 0.021(4) 0.000(3) -0.007(4) 0.001(3) C46 0.018(4) 0.014(4) 0.025(5) 0.001(3) -0.010(4) -0.002(4) C47 0.013(4) 0.016(4) 0.028(5) 0.007(4) -0.002(4) -0.008(3) C48 0.018(5) 0.017(4) 0.018(4) 0.000(3) 0.005(4) 0.003(4) C49 0.006(4) 0.017(4) 0.017(4) 0.004(3) 0.000(3) 0.000(3) C50 0.014(4) 0.018(4) 0.019(4) -0.003(3) -0.002(3) 0.000(3) C51 0.013(4) 0.024(5) 0.030(5) 0.001(4) -0.009(4) 0.005(4) C52 0.013(4) 0.021(5) 0.038(5) -0.003(4) 0.001(4) 0.006(4) C53 0.017(5) 0.021(4) 0.026(5) -0.005(4) -0.001(4) 0.003(4) C54 0.010(4) 0.022(4) 0.025(5) -0.003(4) -0.003(4) -0.001(4) C100 0.015(5) 0.051(6) 0.033(5) -0.002(5) 0.003(4) -0.003(5) C200 0.019(5) 0.030(5) 0.039(6) -0.002(4) -0.005(4) -0.003(4) C300 0.038(6) 0.038(6) 0.032(6) -0.001(5) -0.009(5) 0.007(5) C910 0.22(2) 0.038(7) 0.038(7) -0.001(6) 0.017(10) 0.049(10) C920 0.089(12) 0.061(9) 0.108(13) -0.008(9) -0.017(10) -0.033(9) C930 0.034(6) 0.032(5) 0.043(6) -0.006(5) 0.005(5) -0.004(5) C960 0.057(16) 0.088(19) 0.033(12) -0.002(12) 0.007(11) -0.060(15) O100 0.032(4) 0.064(5) 0.026(4) 0.016(3) 0.005(3) 0.011(4) O101 0.035(4) 0.038(4) 0.038(4) -0.009(3) -0.002(3) 0.012(3) O102 0.016(3) 0.041(4) 0.025(3) 0.001(3) 0.004(3) 0.007(3) O200 0.022(3) 0.030(3) 0.027(3) -0.005(3) -0.003(3) -0.010(3) O201 0.031(4) 0.018(3) 0.050(4) -0.004(3) -0.007(3) 0.003(3) O202 0.040(4) 0.058(5) 0.020(3) 0.008(3) 0.003(3) -0.012(4) O300 0.014(3) 0.050(4) 0.021(3) 0.001(3) -0.006(3) 0.002(3) O301 0.015(3) 0.045(4) 0.040(4) -0.002(3) -0.004(3) 0.008(3) O302 0.020(4) 0.059(5) 0.026(4) 0.005(3) -0.001(3) -0.006(3) F100 0.041(4) 0.068(4) 0.046(4) -0.013(3) -0.005(3) -0.024(3) F101 0.011(3) 0.121(6) 0.041(4) 0.007(4) -0.001(3) 0.010(3) F102 0.036(3) 0.065(4) 0.028(3) 0.019(3) -0.008(3) -0.005(3) F200 0.041(4) 0.039(3) 0.034(3) 0.011(3) -0.012(3) -0.003(3) F201 0.046(4) 0.033(3) 0.084(5) -0.023(3) -0.005(4) 0.019(3) F202 0.021(3) 0.057(4) 0.052(4) 0.008(3) -0.004(3) -0.007(3) F300 0.064(5) 0.043(4) 0.069(5) -0.017(3) -0.009(4) 0.021(3) F301 0.070(5) 0.042(4) 0.056(4) 0.001(3) 0.011(4) -0.018(3) F302 0.052(4) 0.062(4) 0.040(4) -0.016(3) -0.014(3) -0.018(3) S100 0.0173(11) 0.0307(12) 0.0160(10) 0.0013(9) -0.0004(9) 0.0058(9) S200 0.0220(12) 0.0200(11) 0.0195(11) -0.0005(8) -0.0009(9) -0.0034(9) S300 0.0134(11) 0.0365(13) 0.0263(11) -0.0014(10) -0.0022(9) 0.0008(10) Cl1 0.095(4) 0.071(3) 0.081(4) -0.020(3) 0.000 0.000 Cl2 0.052(4) 0.068(4) 0.056(4) 0.020(3) -0.005(3) -0.013(3) Cl5 0.133(4) 0.114(3) 0.058(2) 0.030(2) -0.014(2) -0.070(3) Cl6 0.117(3) 0.120(3) 0.0492(19) 0.006(2) -0.010(2) -0.082(3) Cl7 0.070(2) 0.0386(15) 0.067(2) -0.0113(14) -0.0161(17) -0.0140(15) Cl8 0.0455(17) 0.0366(14) 0.0404(14) -0.0023(11) -0.0038(12) -0.0033(12) Cl9 0.049(2) 0.094(3) 0.136(4) 0.039(3) -0.016(2) -0.013(2) Cl10 0.059(4) 0.035(4) 0.044(4) 0.018(3) 0.023(3) 0.023(3) Cl50 0.063(4) 0.171(7) 0.112(5) -0.084(5) 0.000 0.000 Cl51 0.071(4) 0.068(4) 0.302(12) -0.066(6) 0.000 0.000 C950 0.09(2) 0.042(14) 0.066(17) -0.025(12) -0.017(15) 0.023(14) Cl11 0.45(3) 0.038(6) 0.132(13) -0.021(7) 0.147(19) -0.050(14) _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 2.043(7) . ? Cu1 N3 2.052(6) . ? Cu1 S2 2.312(2) . ? Cu1 S1 2.312(2) . ? P1 C1 1.795(8) . ? P1 C19 1.801(8) . ? P1 C8 1.865(8) . ? P1 S1 1.969(3) . ? P2 C31 1.788(8) . ? P2 C49 1.806(8) . ? P2 C38 1.860(8) . ? P2 S2 1.977(3) . ? N1 C14 1.341(10) . ? N1 C18 1.352(10) . ? N2 C13 1.336(11) . ? N2 C9 1.364(10) . ? N3 C48 1.346(10) . ? N3 C44 1.356(10) . ? N4 C43 1.339(11) . ? N4 C39 1.366(11) . ? C1 C2 1.336(11) . ? C1 C14 1.486(10) . ? C2 C7 1.465(11) . ? C2 C3 1.507(11) . ? C3 C4 1.542(12) . ? C4 C5 1.521(12) . ? C5 C6 1.513(11) . ? C6 C7 1.340(11) . ? C7 C8 1.518(10) . ? C8 C9 1.493(11) . ? C9 C10 1.373(11) . ? C10 C11 1.426(12) . ? C11 C12 1.366(14) . ? C12 C13 1.346(13) . ? C14 C15 1.394(11) . ? C15 C16 1.385(12) . ? C16 C17 1.382(13) . ? C17 C18 1.380(12) . ? C19 C20 1.388(11) . ? C19 C24 1.393(12) . ? C20 C21 1.388(12) . ? C21 C22 1.373(13) . ? C22 C23 1.366(13) . ? C23 C24 1.396(12) . ? C31 C32 1.362(11) . ? C31 C44 1.468(11) . ? C32 C37 1.470(12) . ? C32 C33 1.505(11) . ? C33 C34 1.529(13) . ? C34 C35 1.510(14) . ? C35 C36 1.504(13) . ? C36 C37 1.329(11) . ? C37 C38 1.526(11) . ? C38 C39 1.490(11) . ? C39 C40 1.360(12) . ? C40 C41 1.388(13) . ? C41 C42 1.390(13) . ? C42 C43 1.384(13) . ? C44 C45 1.409(11) . ? C45 C46 1.387(11) . ? C46 C47 1.378(12) . ? C47 C48 1.386(11) . ? C49 C54 1.381(11) . ? C49 C50 1.403(11) . ? C50 C51 1.390(11) . ? C51 C52 1.378(12) . ? C52 C53 1.377(12) . ? C53 C54 1.390(11) . ? C100 F102 1.323(11) . ? C100 F100 1.328(11) . ? C100 F101 1.345(10) . ? C100 S100 1.821(10) . ? C200 F201 1.320(11) . ? C200 F200 1.323(11) . ? C200 F202 1.346(10) . ? C200 S200 1.830(9) . ? C300 F301 1.330(12) . ? C300 F302 1.335(11) . ? C300 F300 1.339(12) . ? C300 S300 1.805(11) . ? C910 Cl9 1.617(18) . ? C910 Cl10 1.764(16) . ? C910 Cl11 1.87(2) . ? C920 Cl5 1.607(17) . ? C920 Cl6 1.794(14) . ? C930 Cl7 1.737(10) . ? C930 Cl8 1.754(10) . ? C960 Cl1 1.63(2) . ? C960 Cl2 1.67(2) . ? O100 S100 1.425(7) . ? O101 S100 1.434(7) . ? O102 S100 1.459(6) . ? O200 S200 1.453(6) . ? O201 S200 1.434(6) . ? O202 S200 1.431(6) . ? O300 S300 1.439(6) . ? O301 S300 1.445(6) . ? O302 S300 1.446(7) . ? Cl1 C960 1.63(2) 3_566 ? Cl10 Cl11 0.81(3) . ? Cl50 C950 1.72(3) 3_556 ? Cl50 C950 1.72(3) . ? Cl51 C950 1.67(3) 3_556 ? Cl51 C950 1.67(3) . ? C950 C950 1.86(5) 3_556 ? 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 N3 105.2(3) . . ? N1 Cu1 S2 105.1(2) . . ? N3 Cu1 S2 115.54(19) . . ? N1 Cu1 S1 115.89(19) . . ? N3 Cu1 S1 102.89(19) . . ? S2 Cu1 S1 112.43(8) . . ? C1 P1 C19 111.6(4) . . ? C1 P1 C8 92.8(3) . . ? C19 P1 C8 108.7(4) . . ? C1 P1 S1 116.7(3) . . ? C19 P1 S1 112.9(3) . . ? C8 P1 S1 112.4(3) . . ? C31 P2 C49 112.9(4) . . ? C31 P2 C38 93.4(4) . . ? C49 P2 C38 109.4(3) . . ? C31 P2 S2 115.5(3) . . ? C49 P2 S2 111.9(3) . . ? C38 P2 S2 112.3(3) . . ? P1 S1 Cu1 91.08(10) . . ? P2 S2 Cu1 90.45(10) . . ? C14 N1 C18 118.3(7) . . ? C14 N1 Cu1 123.5(5) . . ? C18 N1 Cu1 117.8(5) . . ? C13 N2 C9 122.1(8) . . ? C48 N3 C44 118.5(7) . . ? C48 N3 Cu1 118.6(5) . . ? C44 N3 Cu1 121.6(5) . . ? C43 N4 C39 122.8(8) . . ? C2 C1 C14 127.2(7) . . ? C2 C1 P1 109.7(6) . . ? C14 C1 P1 122.7(5) . . ? C1 C2 C7 117.1(7) . . ? C1 C2 C3 126.9(7) . . ? C7 C2 C3 115.9(7) . . ? C2 C3 C4 110.0(7) . . ? C5 C4 C3 110.7(7) . . ? C6 C5 C4 113.2(7) . . ? C7 C6 C5 121.1(8) . . ? C6 C7 C2 123.6(7) . . ? C6 C7 C8 125.2(7) . . ? C2 C7 C8 111.3(7) . . ? C9 C8 C7 119.6(7) . . ? C9 C8 P1 111.3(5) . . ? C7 C8 P1 102.3(5) . . ? N2 C9 C10 119.6(8) . . ? N2 C9 C8 118.0(7) . . ? C10 C9 C8 122.3(8) . . ? C9 C10 C11 117.4(8) . . ? C12 C11 C10 120.6(9) . . ? C13 C12 C11 119.5(9) . . ? N2 C13 C12 120.9(9) . . ? N1 C14 C15 121.3(7) . . ? N1 C14 C1 117.8(6) . . ? C15 C14 C1 120.8(7) . . ? C16 C15 C14 119.9(8) . . ? C17 C16 C15 118.7(8) . . ? C18 C17 C16 118.5(8) . . ? N1 C18 C17 123.3(8) . . ? C20 C19 C24 120.4(8) . . ? C20 C19 P1 120.0(6) . . ? C24 C19 P1 119.5(6) . . ? C19 C20 C21 119.6(8) . . ? C22 C21 C20 119.5(9) . . ? C23 C22 C21 121.7(8) . . ? C22 C23 C24 119.7(9) . . ? C19 C24 C23 119.0(9) . . ? C32 C31 C44 126.1(7) . . ? C32 C31 P2 110.3(6) . . ? C44 C31 P2 123.5(6) . . ? C31 C32 C37 115.9(7) . . ? C31 C32 C33 126.7(8) . . ? C37 C32 C33 117.4(7) . . ? C32 C33 C34 109.2(7) . . ? C35 C34 C33 112.3(8) . . ? C36 C35 C34 112.1(7) . . ? C37 C36 C35 122.0(9) . . ? C36 C37 C32 122.6(8) . . ? C36 C37 C38 125.1(8) . . ? C32 C37 C38 112.3(7) . . ? C39 C38 C37 117.4(7) . . ? C39 C38 P2 111.4(5) . . ? C37 C38 P2 103.0(5) . . ? C40 C39 N4 118.2(8) . . ? C40 C39 C38 122.6(8) . . ? N4 C39 C38 119.1(7) . . ? C39 C40 C41 120.7(8) . . ? C40 C41 C42 120.0(9) . . ? C43 C42 C41 118.1(9) . . ? N4 C43 C42 120.2(9) . . ? N3 C44 C45 120.7(7) . . ? N3 C44 C31 118.0(7) . . ? C45 C44 C31 121.2(7) . . ? C46 C45 C44 119.6(7) . . ? C47 C46 C45 119.1(7) . . ? C46 C47 C48 118.8(8) . . ? N3 C48 C47 123.3(8) . . ? C54 C49 C50 120.8(7) . . ? C54 C49 P2 119.7(6) . . ? C50 C49 P2 119.5(6) . . ? C51 C50 C49 118.4(7) . . ? C52 C51 C50 121.0(8) . . ? C51 C52 C53 120.0(8) . . ? C52 C53 C54 120.5(8) . . ? C49 C54 C53 119.3(8) . . ? F102 C100 F100 107.5(8) . . ? F102 C100 F101 107.7(8) . . ? F100 C100 F101 107.3(8) . . ? F102 C100 S100 112.2(7) . . ? F100 C100 S100 111.5(7) . . ? F101 C100 S100 110.4(6) . . ? F201 C200 F200 108.9(8) . . ? F201 C200 F202 106.9(8) . . ? F200 C200 F202 108.1(7) . . ? F201 C200 S200 110.9(6) . . ? F200 C200 S200 111.5(6) . . ? F202 C200 S200 110.4(6) . . ? F301 C300 F302 106.9(8) . . ? F301 C300 F300 106.8(8) . . ? F302 C300 F300 106.9(8) . . ? F301 C300 S300 113.0(7) . . ? F302 C300 S300 111.8(7) . . ? F300 C300 S300 111.1(7) . . ? Cl9 C910 Cl10 109.3(12) . . ? Cl9 C910 Cl11 127.8(12) . . ? Cl10 C910 Cl11 25.5(8) . . ? Cl5 C920 Cl6 114.5(8) . . ? Cl7 C930 Cl8 112.6(6) . . ? Cl1 C960 Cl2 119.0(18) . . ? O100 S100 O101 116.4(4) . . ? O100 S100 O102 114.0(4) . . ? O101 S100 O102 114.5(4) . . ? O100 S100 C100 104.2(4) . . ? O101 S100 C100 103.0(4) . . ? O102 S100 C100 102.4(4) . . ? O202 S200 O201 115.9(4) . . ? O202 S200 O200 114.1(4) . . ? O201 S200 O200 114.8(4) . . ? O202 S200 C200 105.2(4) . . ? O201 S200 C200 102.0(4) . . ? O200 S200 C200 102.3(4) . . ? O300 S300 O301 115.1(4) . . ? O300 S300 O302 114.9(4) . . ? O301 S300 O302 114.8(4) . . ? O300 S300 C300 103.6(4) . . ? O301 S300 C300 103.5(4) . . ? O302 S300 C300 102.7(5) . . ? C960 Cl1 C960 149(2) 3_566 . ? Cl11 Cl10 C910 84.7(18) . . ? C950 Cl50 C950 66(2) 3_556 . ? C950 Cl51 C950 68.1(18) 3_556 . ? Cl51 C950 Cl50 113.2(16) . . ? Cl51 C950 C950 56.0(9) . 3_556 ? Cl50 C950 C950 57.2(10) . 3_556 ? Cl10 Cl11 C910 69.8(19) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.803 _refine_diff_density_min -1.501 _refine_diff_density_rms 0.158 _database_code_depnum_ccdc_archive 'CCDC 934187'