Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_section_title ; Influence of anions on the dimensionality of extended networks based on Cu(I) cations and 1,4,5,8,9,12-hexaazatriphenylene (HAT) ligands ; _publ_contact_author_name 'Kim R. Dunbar' _publ_contact_author_address ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; _publ_contact_author_email dunbar@mail.chem.tamu.edu _publ_contact_author_fax (979)8457177 _publ_contact_author_phone (979)8625235 loop_ _publ_author_name _publ_author_address 'Mikhail Shatruk' ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; 'Abdellatif Chouai' ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; 'Kim R. Dunbar' ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; # Attachment 'shatruk.cif' data_d:\ms036\try1 _database_code_depnum_ccdc_archive 'CCDC 285143' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.86 H31.08 B3 Cu3 F12 N20.86 O6.02' _chemical_formula_weight 1409.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 16.766(12) _cell_length_b 13.565(13) _cell_length_c 24.967(19) _cell_angle_alpha 90.00 _cell_angle_beta 103.80(4) _cell_angle_gamma 90.00 _cell_volume 5514(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 131 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2818 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1000 CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43773 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11252 _reflns_number_gt 6919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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. The disorder was observed for one of the BF4 moieties and two of the nitromethane molecules. For the BF4 moiety and one of the nitromethane molecules the disorder was modeled with two different orientations, the total occupancy of both orientations being fixed at 1. The other nitromethane molecule was disordered around an inversion center. The occupancy of oxygen atoms of this molecule was fixes at 0.5 while the position of carbon/nitrogen atom was refined as mixed with fixed occupancies of 0.5 for each element and restrained positional and thermal parameters for both atoms. The occupancies of the remaining non-disordered nitromethane and water molecules were refined as free variables ; _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^)+(0.1035P)^2^+15.4775P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11252 _refine_ls_number_parameters 788 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1301 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.2153 _refine_ls_wR_factor_gt 0.1847 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.020 _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 0.33539(4) 0.64558(5) 0.14048(3) 0.0343(2) Uani 1 1 d . . . Cu2 Cu 0.28384(5) 1.13268(5) 0.07970(3) 0.0322(2) Uani 1 1 d . . . Cu3 Cu 0.17122(5) 1.16013(6) -0.19972(3) 0.0389(2) Uani 1 1 d . . . F1 F 0.3696(4) 0.9790(4) 0.2515(2) 0.0930(18) Uani 1 1 d . . . F2 F 0.2764(4) 0.8685(5) 0.2135(2) 0.101(2) Uani 1 1 d . . . F3 F 0.3575(8) 0.8375(5) 0.2938(4) 0.205(5) Uani 1 1 d . . . F4 F 0.2658(5) 0.9488(6) 0.2872(3) 0.137(3) Uani 1 1 d . . . F5 F 0.0181(3) 0.2157(4) 0.1796(2) 0.0769(15) Uani 1 1 d . . . F6 F -0.1010(4) 0.2055(5) 0.1997(4) 0.134(3) Uani 1 1 d . . . F7 F -0.0049(6) 0.1122(6) 0.2434(3) 0.158(4) Uani 1 1 d . . . F8 F -0.0628(4) 0.0812(4) 0.1562(2) 0.0944(19) Uani 1 1 d . . . F9A F 0.5712(7) 0.3533(8) -0.0109(4) 0.091(3) Uiso 0.610(11) 1 d P A -6 F10A F 0.5013(6) 0.2325(7) 0.0233(4) 0.042(3) Uiso 0.610(11) 1 d P A -6 F11A F 0.6020(5) 0.1965(6) -0.0149(3) 0.073(3) Uiso 0.610(11) 1 d P A -6 F12A F 0.4773(6) 0.2567(8) -0.0671(4) 0.065(3) Uiso 0.610(11) 1 d P A -6 F9B F 0.4864(11) 0.3769(13) -0.0208(7) 0.111(7) Uiso 0.390(11) 1 d P A -7 F10B F 0.5957(8) 0.2981(10) -0.0243(5) 0.062(4) Uiso 0.390(11) 1 d P A -7 F11B F 0.4804(8) 0.2210(12) -0.0665(6) 0.056(4) Uiso 0.390(11) 1 d P A -7 F12B F 0.5065(12) 0.2547(14) 0.0301(8) 0.067(6) Uiso 0.390(11) 1 d P A -7 O1S O 0.1757(14) -0.0248(18) 0.4345(9) 0.227(9) Uiso 0.720(12) 1 d P B -1 O2S O 0.1532(7) 0.1241(9) 0.4413(5) 0.110(4) Uiso 0.720(12) 1 d P B -1 O3S O 0.3298(9) 0.0829(10) 0.4323(6) 0.117(5) Uiso 0.639(10) 1 d P C -2 O4S O 0.3418(8) 0.1301(9) 0.3556(5) 0.102(4) Uiso 0.639(10) 1 d P C -2 O5S O 0.4413(8) 0.4985(9) 0.4353(6) 0.079(4) Uiso 0.50 1 d P . . O6S O 0.4028(11) 0.5318(14) 0.5064(7) 0.131(6) Uiso 0.50 1 d PD . . O7SA O 0.2208(8) 0.5919(11) 0.4549(6) 0.064(4) Uiso 0.506(14) 1 d P D -4 O8SA O 0.2939(9) 0.5908(11) 0.3966(6) 0.089(5) Uiso 0.506(14) 1 d P D -4 O7SB O 0.2027(9) 0.7252(11) 0.4571(6) 0.083(5) Uiso 0.494(14) 1 d P D -5 O8SB O 0.2236(11) 0.5672(14) 0.4348(8) 0.094(6) Uiso 0.494(14) 1 d P D -5 O1W O 0.5090(18) -0.087(2) 0.3411(12) 0.118(14) Uiso 0.30(2) 1 d P . . N1 N 0.2762(3) 0.5833(3) 0.19448(19) 0.0284(11) Uani 1 1 d . . . N2 N 0.3277(3) 0.5120(4) 0.1078(2) 0.0326(11) Uani 1 1 d . . . N3 N 0.4473(3) 0.7058(4) 0.1741(2) 0.0310(11) Uani 1 1 d . . . N4 N 0.3081(3) 0.7797(3) 0.1120(2) 0.0287(11) Uani 1 1 d . . . N5 N 0.5845(3) 0.8258(4) 0.2138(3) 0.0493(16) Uani 1 1 d . . . N6 N 0.5719(3) 1.0296(4) 0.1918(2) 0.0425(14) Uani 1 1 d . . . N7 N 0.2923(3) 0.9823(4) 0.0901(2) 0.0319(11) Uani 1 1 d . . . N8 N 0.4243(3) 1.1034(4) 0.1246(2) 0.0315(11) Uani 1 1 d . . . N9 N 0.2534(3) 0.1828(3) 0.1500(2) 0.0285(11) Uani 1 1 d . . . N10 N 0.3218(3) 0.3084(4) 0.0855(2) 0.0407(13) Uani 1 1 d . . . N11 N 0.2513(3) 1.1528(3) -0.0023(2) 0.0306(11) Uani 1 1 d . . . N12 N 0.1221(3) 1.1275(4) 0.0481(2) 0.0340(12) Uani 1 1 d . . . N13 N -0.0396(3) 1.1250(4) -0.0157(2) 0.0376(12) Uani 1 1 d . . . N14 N -0.0701(3) 1.1305(4) -0.1298(2) 0.0425(14) Uani 1 1 d . . . N15 N 0.0633(3) 1.1519(4) -0.1792(2) 0.0313(11) Uani 1 1 d . . . N16 N 0.2167(3) 1.1636(4) -0.1177(2) 0.0341(12) Uani 1 1 d . . . N17 N 0.2113(3) 0.4558(4) 0.2618(2) 0.0310(11) Uani 1 1 d . . . N18 N 0.2019(3) 0.2607(3) 0.2414(2) 0.0299(11) Uani 1 1 d . . . N1S N 0.1637(9) 0.0609(11) 0.4136(6) 0.100(5) Uiso 0.720(12) 1 d P B -1 N2S N 0.3652(9) 0.0788(11) 0.3931(6) 0.089(4) Uiso 0.639(10) 1 d P C -2 N3S N 0.4609(6) 0.5065(7) 0.4807(4) 0.086(3) Uiso 0.50 1 d PD . . N4SA N 0.2541(9) 0.6384(11) 0.4214(6) 0.047(3) Uiso 0.506(14) 1 d P D -4 N4SB N 0.2331(12) 0.6587(15) 0.4372(8) 0.072(5) Uiso 0.494(14) 1 d P D -5 C1 C 0.2474(4) 0.6164(4) 0.2365(3) 0.0325(14) Uani 1 1 d . . . H1 H 0.2484 0.6838 0.2435 0.039 Uiso 1 1 calc R . . C2 C 0.2705(3) 0.4854(4) 0.1851(2) 0.0260(12) Uani 1 1 d . . . C3 C 0.2984(3) 0.4468(4) 0.1390(2) 0.0278(12) Uani 1 1 d . . . C4 C 0.2945(4) 0.3463(4) 0.1279(2) 0.0300(13) Uani 1 1 d . . . C5 C 0.3495(5) 0.3728(5) 0.0548(3) 0.0511(19) Uani 1 1 d . . . H5 H 0.3683 0.3496 0.0250 0.061 Uiso 1 1 calc R . . C6 C 0.3522(4) 0.4746(5) 0.0649(3) 0.0441(17) Uani 1 1 d . . . H6 H 0.3713 0.5167 0.0413 0.053 Uiso 1 1 calc R . . C7 C 0.5162(4) 0.6693(5) 0.2035(3) 0.0439(17) Uani 1 1 d . . . H7 H 0.5200 0.6023 0.2118 0.053 Uiso 1 1 calc R . . C8 C 0.5832(4) 0.7300(6) 0.2224(4) 0.060(2) Uani 1 1 d . . . H8 H 0.6312 0.7009 0.2426 0.073 Uiso 1 1 calc R . . C9 C 0.2389(3) 0.8199(4) 0.0827(2) 0.0327(14) Uani 1 1 d . . . H9 H 0.1942 0.7793 0.0685 0.039 Uiso 1 1 calc R . . C10 C 0.2316(4) 0.9204(4) 0.0728(3) 0.0354(14) Uani 1 1 d . . . H10 H 0.1814 0.9450 0.0531 0.043 Uiso 1 1 calc R . . C11 C 0.3707(3) 0.8441(4) 0.1301(2) 0.0242(12) Uani 1 1 d . . . C12 C 0.4460(3) 0.8035(4) 0.1635(2) 0.0274(12) Uani 1 1 d . . . C13 C 0.5133(4) 0.8640(4) 0.1835(3) 0.0363(14) Uani 1 1 d . . . C14 C 0.5077(4) 0.9698(4) 0.1714(2) 0.0305(13) Uani 1 1 d . . . C15 C 0.4334(3) 1.0075(4) 0.1388(2) 0.0256(12) Uani 1 1 d . . . C16 C 0.3647(3) 0.9436(4) 0.1191(2) 0.0247(12) Uani 1 1 d . . . C17 C 0.5607(4) 1.1238(5) 0.1775(3) 0.0452(17) Uani 1 1 d . . . H17 H 0.6033 1.1679 0.1909 0.054 Uiso 1 1 calc R . . C18 C 0.4885(4) 1.1600(5) 0.1437(3) 0.0392(15) Uani 1 1 d . . . H18 H 0.4855 1.2264 0.1341 0.047 Uiso 1 1 calc R . . C19 C 0.0582(4) 1.1198(5) 0.0703(3) 0.0385(15) Uani 1 1 d . . . H19 H 0.0672 1.1144 0.1084 0.046 Uiso 1 1 calc R . . C20 C -0.0213(4) 1.1195(5) 0.0386(3) 0.0380(15) Uani 1 1 d . . . H20 H -0.0640 1.1153 0.0564 0.046 Uiso 1 1 calc R . . C21 C 0.3092(4) 1.1653(5) -0.0293(3) 0.0402(15) Uani 1 1 d . . . H21 H 0.3633 1.1711 -0.0092 0.048 Uiso 1 1 calc R . . C22 C 0.2927(4) 1.1703(5) -0.0868(3) 0.0406(15) Uani 1 1 d . . . H22 H 0.3360 1.1784 -0.1038 0.049 Uiso 1 1 calc R . . C23 C 0.1055(3) 1.1354(4) -0.0073(2) 0.0273(12) Uani 1 1 d . . . C24 C 0.1734(3) 1.1455(4) -0.0333(2) 0.0273(12) Uani 1 1 d . . . C25 C 0.1573(3) 1.1521(4) -0.0904(2) 0.0281(12) Uani 1 1 d . . . C26 C 0.0740(3) 1.1470(4) -0.1236(2) 0.0291(13) Uani 1 1 d . . . C27 C 0.0081(3) 1.1367(4) -0.0993(2) 0.0318(13) Uani 1 1 d . . . C28 C 0.0246(3) 1.1319(4) -0.0398(3) 0.0313(13) Uani 1 1 d . . . C29 C -0.0789(4) 1.1358(5) -0.1834(3) 0.0465(18) Uani 1 1 d . . . H29 H -0.1317 1.1322 -0.2059 0.056 Uiso 1 1 calc R . . C30 C -0.0131(4) 1.1467(5) -0.2088(3) 0.0391(15) Uani 1 1 d . . . H30 H -0.0235 1.1503 -0.2471 0.047 Uiso 1 1 calc R . . C31 C 0.2159(3) 0.5529(4) 0.2704(3) 0.0314(13) Uani 1 1 d . . . H31 H 0.1976 0.5790 0.2998 0.038 Uiso 1 1 calc R . . C32 C 0.2389(3) 0.4224(4) 0.2186(2) 0.0273(12) Uani 1 1 d . . . C33 C 0.2335(3) 0.3185(4) 0.2072(2) 0.0258(12) Uani 1 1 d . . . C34 C 0.2601(3) 0.2808(4) 0.1620(2) 0.0278(13) Uani 1 1 d . . . C35 C 0.1970(4) 0.1651(5) 0.2292(3) 0.0356(14) Uani 1 1 d . . . H35 H 0.1767 0.1221 0.2518 0.043 Uiso 1 1 calc R . . C36 C 0.2217(4) 0.1271(5) 0.1833(3) 0.0347(14) Uani 1 1 d . . . H36 H 0.2156 0.0599 0.1760 0.042 Uiso 1 1 calc R . . C37 C 0.0611(5) 0.5648(9) 0.1362(4) 0.079(3) Uani 1 1 d . . . H37 H 0.0507 0.6079 0.1627 0.094 Uiso 1 1 calc R . . C38 C 0.0520(6) 0.4670(11) 0.1422(5) 0.095(4) Uani 1 1 d . . . H38 H 0.0344 0.4441 0.1725 0.114 Uiso 1 1 calc R . . C39 C 0.0673(7) 0.4024(9) 0.1062(6) 0.097(4) Uani 1 1 d . . . H39 H 0.0615 0.3354 0.1120 0.117 Uiso 1 1 calc R . . C40 C 0.0920(7) 0.4339(11) 0.0601(6) 0.108(5) Uani 1 1 d . . . H40 H 0.1017 0.3893 0.0341 0.130 Uiso 1 1 calc R . . C41 C 0.1020(6) 0.5369(11) 0.0539(5) 0.091(3) Uani 1 1 d . . . H41 H 0.1200 0.5612 0.0239 0.110 Uiso 1 1 calc R . . C42 C 0.0849(5) 0.6004(7) 0.0925(5) 0.076(3) Uani 1 1 d . . . H42 H 0.0898 0.6681 0.0884 0.092 Uiso 1 1 calc R . . C1S C 0.1492(14) 0.0689(17) 0.3600(9) 0.155(9) Uiso 0.720(12) 1 d P B -1 H1S1 H 0.1359 0.0053 0.3435 0.232 Uiso 0.720(12) 1 calc PR B -1 H1S2 H 0.1971 0.0944 0.3500 0.232 Uiso 0.720(12) 1 calc PR B -1 H1S3 H 0.1039 0.1131 0.3472 0.232 Uiso 0.720(12) 1 calc PR B -1 C2S C 0.4285(11) -0.0056(13) 0.4001(7) 0.100(6) Uiso 0.639(10) 1 d P C -2 H2S1 H 0.4140 -0.0563 0.4228 0.151 Uiso 0.639(10) 1 calc PR C -2 H2S2 H 0.4821 0.0194 0.4171 0.151 Uiso 0.639(10) 1 calc PR C -2 H2S3 H 0.4288 -0.0325 0.3645 0.151 Uiso 0.639(10) 1 calc PR C -2 C3S C 0.4609(6) 0.5065(7) 0.4807(4) 0.086(3) Uiso 0.50 1 d P . . C4SA C 0.2482(14) 0.7437(17) 0.4145(9) 0.093(7) Uiso 0.506(14) 1 d P D -4 H4S4 H 0.3005 0.7732 0.4306 0.139 Uiso 0.506(14) 1 calc PR D -4 H4S5 H 0.2077 0.7689 0.4324 0.139 Uiso 0.506(14) 1 calc PR D -4 H4S6 H 0.2325 0.7593 0.3759 0.139 Uiso 0.506(14) 1 calc PR D -4 C4SB C 0.2945(12) 0.6946(15) 0.4032(8) 0.070(6) Uiso 0.494(14) 1 d P D -5 H4S1 H 0.2761 0.7566 0.3860 0.104 Uiso 0.494(14) 1 calc PR D -5 H4S2 H 0.2970 0.6468 0.3753 0.104 Uiso 0.494(14) 1 calc PR D -5 H4S3 H 0.3480 0.7025 0.4272 0.104 Uiso 0.494(14) 1 calc PR D -5 B1 B 0.3205(6) 0.9047(7) 0.2621(4) 0.055(2) Uani 1 1 d . . . B2 B -0.0344(5) 0.1489(7) 0.1937(4) 0.054(2) Uani 1 1 d . . . B3A B 0.5347(10) 0.2627(11) -0.0172(6) 0.039(4) Uiso 0.610(11) 1 d P A -6 B3B B 0.507(2) 0.283(3) -0.0255(14) 0.065(9) Uiso 0.390(11) 1 d P A -7 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 0.0261(4) 0.0274(4) 0.0481(5) 0.0034(3) 0.0061(3) 0.0001(3) Cu2 0.0328(4) 0.0264(4) 0.0377(4) -0.0016(3) 0.0089(3) 0.0035(3) Cu3 0.0335(4) 0.0458(5) 0.0405(5) 0.0044(4) 0.0149(4) 0.0056(4) F1 0.096(4) 0.074(4) 0.100(4) -0.004(3) 0.004(3) -0.046(3) F2 0.089(4) 0.144(5) 0.087(4) -0.062(4) 0.053(3) -0.070(4) F3 0.315(14) 0.054(4) 0.192(9) 0.033(5) -0.049(9) 0.038(6) F4 0.174(7) 0.138(6) 0.129(6) -0.051(5) 0.094(6) -0.016(5) F5 0.066(3) 0.086(4) 0.086(4) -0.014(3) 0.032(3) -0.032(3) F6 0.079(4) 0.088(4) 0.256(9) -0.050(5) 0.081(5) -0.031(4) F7 0.210(9) 0.182(8) 0.064(4) 0.022(5) -0.003(5) -0.089(7) F8 0.153(6) 0.072(3) 0.067(3) -0.018(3) 0.042(3) -0.050(4) N1 0.025(3) 0.025(2) 0.033(3) -0.004(2) 0.001(2) 0.002(2) N2 0.031(3) 0.032(3) 0.035(3) 0.002(2) 0.009(2) 0.006(2) N3 0.026(3) 0.028(3) 0.036(3) 0.002(2) 0.004(2) 0.003(2) N4 0.021(3) 0.027(3) 0.039(3) 0.001(2) 0.010(2) 0.004(2) N5 0.030(3) 0.031(3) 0.074(4) 0.006(3) -0.013(3) 0.002(2) N6 0.032(3) 0.033(3) 0.057(4) 0.001(3) -0.001(3) -0.001(2) N7 0.020(3) 0.035(3) 0.038(3) -0.001(2) 0.002(2) 0.004(2) N8 0.031(3) 0.027(3) 0.038(3) 0.000(2) 0.011(2) 0.001(2) N9 0.024(3) 0.025(2) 0.033(3) -0.001(2) 0.001(2) 0.003(2) N10 0.046(3) 0.034(3) 0.043(3) -0.005(2) 0.014(3) 0.007(3) N11 0.021(2) 0.027(3) 0.039(3) -0.001(2) -0.001(2) -0.003(2) N12 0.024(3) 0.037(3) 0.038(3) -0.005(2) 0.001(2) 0.002(2) N13 0.023(3) 0.051(3) 0.039(3) -0.001(3) 0.008(2) 0.005(2) N14 0.022(3) 0.066(4) 0.035(3) 0.001(3) -0.001(2) 0.005(3) N15 0.024(3) 0.035(3) 0.034(3) -0.001(2) 0.006(2) 0.006(2) N16 0.029(3) 0.036(3) 0.038(3) 0.003(2) 0.009(2) 0.004(2) N17 0.020(2) 0.037(3) 0.036(3) -0.006(2) 0.007(2) 0.000(2) N18 0.021(2) 0.029(3) 0.038(3) -0.004(2) 0.004(2) -0.005(2) C1 0.026(3) 0.025(3) 0.045(4) -0.010(3) 0.005(3) -0.001(2) C2 0.016(3) 0.027(3) 0.032(3) -0.002(2) 0.000(2) 0.000(2) C3 0.019(3) 0.031(3) 0.031(3) 0.001(2) 0.000(2) 0.003(2) C4 0.031(3) 0.025(3) 0.033(3) 0.002(2) 0.006(3) 0.005(2) C5 0.073(5) 0.048(4) 0.040(4) -0.002(3) 0.029(4) 0.008(4) C6 0.053(4) 0.045(4) 0.038(4) 0.003(3) 0.020(3) 0.009(3) C7 0.028(3) 0.035(3) 0.061(5) 0.008(3) -0.006(3) 0.005(3) C8 0.028(4) 0.048(4) 0.090(6) 0.013(4) -0.016(4) 0.004(3) C9 0.017(3) 0.037(3) 0.041(4) -0.001(3) 0.002(3) -0.001(2) C10 0.022(3) 0.034(3) 0.045(4) 0.004(3) -0.002(3) 0.009(3) C11 0.018(3) 0.029(3) 0.026(3) -0.001(2) 0.006(2) 0.002(2) C12 0.019(3) 0.026(3) 0.037(3) 0.001(2) 0.007(2) 0.003(2) C13 0.024(3) 0.034(3) 0.047(4) 0.002(3) 0.001(3) 0.004(3) C14 0.025(3) 0.029(3) 0.036(3) -0.003(3) 0.004(3) 0.000(2) C15 0.025(3) 0.025(3) 0.028(3) -0.003(2) 0.009(2) 0.003(2) C16 0.019(3) 0.029(3) 0.027(3) 0.002(2) 0.006(2) 0.006(2) C17 0.044(4) 0.030(3) 0.058(5) -0.004(3) 0.004(3) -0.008(3) C18 0.037(4) 0.029(3) 0.051(4) 0.000(3) 0.009(3) -0.001(3) C19 0.030(3) 0.047(4) 0.038(4) -0.001(3) 0.006(3) 0.005(3) C20 0.029(3) 0.049(4) 0.034(4) 0.001(3) 0.003(3) 0.007(3) C21 0.024(3) 0.044(4) 0.052(4) 0.006(3) 0.007(3) -0.001(3) C22 0.029(3) 0.048(4) 0.046(4) 0.002(3) 0.012(3) 0.000(3) C23 0.024(3) 0.023(3) 0.035(3) -0.004(2) 0.008(2) 0.002(2) C24 0.021(3) 0.020(3) 0.037(3) -0.005(2) 0.001(2) 0.002(2) C25 0.021(3) 0.023(3) 0.040(3) 0.001(2) 0.007(2) 0.003(2) C26 0.025(3) 0.028(3) 0.034(3) 0.000(2) 0.006(2) 0.006(2) C27 0.022(3) 0.037(3) 0.035(3) 0.000(3) 0.005(2) 0.003(3) C28 0.022(3) 0.033(3) 0.038(3) 0.000(3) 0.006(3) 0.007(2) C29 0.019(3) 0.072(5) 0.042(4) 0.001(4) -0.006(3) 0.005(3) C30 0.037(4) 0.046(4) 0.034(3) 0.000(3) 0.006(3) 0.004(3) C31 0.021(3) 0.036(3) 0.039(3) -0.011(3) 0.009(3) 0.006(2) C32 0.019(3) 0.031(3) 0.028(3) -0.006(2) -0.001(2) 0.002(2) C33 0.018(3) 0.028(3) 0.029(3) -0.002(2) 0.000(2) -0.001(2) C34 0.021(3) 0.024(3) 0.034(3) -0.005(2) -0.003(2) 0.004(2) C35 0.023(3) 0.040(4) 0.042(4) 0.003(3) 0.004(3) -0.005(3) C36 0.025(3) 0.031(3) 0.042(4) -0.012(3) -0.003(3) 0.000(3) C37 0.048(5) 0.104(8) 0.081(7) -0.011(6) 0.010(5) -0.019(5) C38 0.060(6) 0.119(10) 0.093(9) 0.039(8) -0.009(6) -0.014(7) C39 0.083(8) 0.070(7) 0.112(10) 0.003(7) -0.030(8) -0.008(6) C40 0.059(7) 0.118(11) 0.119(10) -0.059(9) -0.035(7) 0.032(7) C41 0.055(6) 0.135(11) 0.081(7) 0.022(7) 0.009(5) 0.019(7) C42 0.041(5) 0.063(6) 0.120(9) 0.015(6) 0.011(5) -0.001(4) B1 0.071(6) 0.044(5) 0.055(6) -0.007(4) 0.025(5) -0.006(5) B2 0.038(5) 0.074(6) 0.056(6) -0.018(5) 0.020(4) -0.020(4) _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 N4 1.967(5) . ? Cu1 N2 1.979(5) . ? Cu1 N3 2.034(5) . ? Cu1 N1 2.038(5) . ? Cu2 N11 2.007(5) . ? Cu2 N7 2.056(5) . ? Cu2 N9 2.057(5) 1_565 ? Cu2 N8 2.388(5) . ? Cu2 N10 2.462(6) 1_565 ? Cu3 N18 1.986(5) 4_575 ? Cu3 N15 1.998(5) . ? Cu3 N16 2.008(5) . ? Cu3 N17 2.040(5) 4_575 ? F1 B1 1.366(10) . ? F2 B1 1.353(11) . ? F3 B1 1.269(12) . ? F4 B1 1.364(11) . ? F5 B2 1.367(10) . ? F6 B2 1.393(11) . ? F7 B2 1.319(12) . ? F8 B2 1.317(10) . ? F9A B3A 1.366(18) . ? F10A B3A 1.332(17) . ? F11A B3A 1.433(18) . ? F12A B3A 1.383(19) . ? F9B B3B 1.34(4) . ? F10B B3B 1.49(4) . ? F11B B3B 1.31(4) . ? F12B B3B 1.44(4) . ? O1S N1S 1.27(2) . ? O2S N1S 1.141(15) . ? O3S N2S 1.261(17) . ? O4S N2S 1.158(16) . ? O5S N3S 1.109(14) . ? O6S N3S 1.333(14) . ? O7SA N4SA 1.28(2) . ? O8SA N4SA 1.202(19) . ? O7SB N4SB 1.20(2) . ? O8SB N4SB 1.25(3) . ? N1 C1 1.333(7) . ? N1 C2 1.348(7) . ? N2 C6 1.337(8) . ? N2 C3 1.345(7) . ? N3 C7 1.310(8) . ? N3 C12 1.352(7) . ? N4 C9 1.332(7) . ? N4 C11 1.357(7) . ? N5 C8 1.318(9) . ? N5 C13 1.355(8) . ? N6 C17 1.328(8) . ? N6 C14 1.347(8) . ? N7 C10 1.311(8) . ? N7 C16 1.362(7) . ? N8 C18 1.316(8) . ? N8 C15 1.347(7) . ? N9 C36 1.325(8) . ? N9 C34 1.361(7) . ? N9 Cu2 2.057(5) 1_545 ? N10 C5 1.318(9) . ? N10 C4 1.350(8) . ? N10 Cu2 2.462(6) 1_545 ? N11 C21 1.317(8) . ? N11 C24 1.355(7) . ? N12 C19 1.323(8) . ? N12 C23 1.349(8) . ? N13 C20 1.319(8) . ? N13 C28 1.357(7) . ? N14 C29 1.312(9) . ? N14 C27 1.353(8) . ? N15 C30 1.318(8) . ? N15 C26 1.360(7) . ? N16 C22 1.325(8) . ? N16 C25 1.344(7) . ? N17 C31 1.333(8) . ? N17 C32 1.348(7) . ? N17 Cu3 2.040(5) 4_576 ? N18 C35 1.330(8) . ? N18 C33 1.355(7) . ? N18 Cu3 1.986(5) 4_576 ? N1S C1S 1.31(2) . ? N2S C2S 1.54(2) . ? N3S C3S 1.440(18) 3_666 ? N3S N3S 1.440(18) 3_666 ? N4SA C4SA 1.44(3) . ? N4SB C4SB 1.56(3) . ? C1 C31 1.398(9) . ? C2 C32 1.386(8) . ? C2 C3 1.440(8) . ? C3 C4 1.390(8) . ? C4 C34 1.444(8) . ? C5 C6 1.401(10) . ? C7 C8 1.382(10) . ? C9 C10 1.386(8) . ? C11 C16 1.376(8) . ? C11 C12 1.445(8) . ? C12 C13 1.387(8) . ? C13 C14 1.466(8) . ? C14 C15 1.411(8) . ? C15 C16 1.432(8) . ? C17 C18 1.390(9) . ? C19 C20 1.378(9) . ? C21 C22 1.399(9) . ? C23 C28 1.405(8) . ? C23 C24 1.446(8) . ? C24 C25 1.388(8) . ? C25 C26 1.445(8) . ? C26 C27 1.388(8) . ? C27 C28 1.445(8) . ? C29 C30 1.405(9) . ? C32 C33 1.436(8) . ? C33 C34 1.404(8) . ? C35 C36 1.407(9) . ? C37 C42 1.337(13) . ? C37 C38 1.349(15) . ? C38 C39 1.323(16) . ? C39 C40 1.379(18) . ? C40 C41 1.421(17) . ? C41 C42 1.375(15) . ? 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 N4 Cu1 N2 135.4(2) . . ? N4 Cu1 N3 83.7(2) . . ? N2 Cu1 N3 120.0(2) . . ? N4 Cu1 N1 120.94(19) . . ? N2 Cu1 N1 84.2(2) . . ? N3 Cu1 N1 116.1(2) . . ? N11 Cu2 N7 104.91(19) . . ? N11 Cu2 N9 139.71(19) . 1_565 ? N7 Cu2 N9 104.1(2) . 1_565 ? N11 Cu2 N8 119.95(19) . . ? N7 Cu2 N8 75.22(17) . . ? N9 Cu2 N8 94.13(18) 1_565 . ? N11 Cu2 N10 86.10(18) . 1_565 ? N7 Cu2 N10 160.64(19) . 1_565 ? N9 Cu2 N10 75.10(18) 1_565 1_565 ? N8 Cu2 N10 85.50(18) . 1_565 ? N18 Cu3 N15 129.1(2) 4_575 . ? N18 Cu3 N16 129.8(2) 4_575 . ? N15 Cu3 N16 83.5(2) . . ? N18 Cu3 N17 84.0(2) 4_575 4_575 ? N15 Cu3 N17 119.9(2) . 4_575 ? N16 Cu3 N17 114.3(2) . 4_575 ? C1 N1 C2 116.4(5) . . ? C1 N1 Cu1 134.9(4) . . ? C2 N1 Cu1 108.6(4) . . ? C6 N2 C3 116.0(5) . . ? C6 N2 Cu1 132.5(5) . . ? C3 N2 Cu1 111.2(4) . . ? C7 N3 C12 116.8(5) . . ? C7 N3 Cu1 133.1(4) . . ? C12 N3 Cu1 110.1(4) . . ? C9 N4 C11 115.0(5) . . ? C9 N4 Cu1 132.4(4) . . ? C11 N4 Cu1 112.4(4) . . ? C8 N5 C13 114.9(6) . . ? C17 N6 C14 115.4(6) . . ? C10 N7 C16 116.8(5) . . ? C10 N7 Cu2 124.7(4) . . ? C16 N7 Cu2 118.4(4) . . ? C18 N8 C15 115.9(5) . . ? C18 N8 Cu2 134.6(4) . . ? C15 N8 Cu2 108.8(4) . . ? C36 N9 C34 116.3(5) . . ? C36 N9 Cu2 124.4(4) . 1_545 ? C34 N9 Cu2 119.2(4) . 1_545 ? C5 N10 C4 115.8(5) . . ? C5 N10 Cu2 136.9(5) . 1_545 ? C4 N10 Cu2 106.5(4) . 1_545 ? C21 N11 C24 116.3(5) . . ? C21 N11 Cu2 119.0(4) . . ? C24 N11 Cu2 124.3(4) . . ? C19 N12 C23 116.5(5) . . ? C20 N13 C28 116.5(5) . . ? C29 N14 C27 115.4(6) . . ? C30 N15 C26 116.4(5) . . ? C30 N15 Cu3 132.6(4) . . ? C26 N15 Cu3 110.9(4) . . ? C22 N16 C25 116.1(5) . . ? C22 N16 Cu3 132.3(4) . . ? C25 N16 Cu3 111.5(4) . . ? C31 N17 C32 116.4(5) . . ? C31 N17 Cu3 134.2(4) . 4_576 ? C32 N17 Cu3 109.4(4) . 4_576 ? C35 N18 C33 115.7(5) . . ? C35 N18 Cu3 133.1(4) . 4_576 ? C33 N18 Cu3 111.2(4) . 4_576 ? O2S N1S O1S 118.2(18) . . ? O2S N1S C1S 122.6(18) . . ? O1S N1S C1S 118(2) . . ? O4S N2S O3S 118.0(16) . . ? O4S N2S C2S 128.9(16) . . ? O3S N2S C2S 112.6(14) . . ? O5S N3S O6S 116.4(14) . . ? O5S N3S C3S 132.2(15) . 3_666 ? O6S N3S C3S 111.3(14) . 3_666 ? O5S N3S N3S 132.2(15) . 3_666 ? O6S N3S N3S 111.3(14) . 3_666 ? C3S N3S N3S 0.0(10) 3_666 3_666 ? O8SA N4SA O7SA 117.1(16) . . ? O8SA N4SA C4SA 120.2(17) . . ? O7SA N4SA C4SA 123(2) . . ? O7SB N4SB O8SB 135(2) . . ? O7SB N4SB C4SB 113.0(18) . . ? O8SB N4SB C4SB 112(2) . . ? N1 C1 C31 122.0(5) . . ? N1 C2 C32 121.6(5) . . ? N1 C2 C3 118.3(5) . . ? C32 C2 C3 120.2(5) . . ? N2 C3 C4 122.4(5) . . ? N2 C3 C2 117.2(5) . . ? C4 C3 C2 120.4(5) . . ? N10 C4 C3 121.4(5) . . ? N10 C4 C34 119.1(5) . . ? C3 C4 C34 119.5(5) . . ? N10 C5 C6 123.3(6) . . ? N2 C6 C5 121.0(6) . . ? N3 C7 C8 120.2(6) . . ? N5 C8 C7 125.1(6) . . ? N4 C9 C10 121.9(5) . . ? N7 C10 C9 122.9(5) . . ? N4 C11 C16 123.4(5) . . ? N4 C11 C12 116.5(5) . . ? C16 C11 C12 120.1(5) . . ? N3 C12 C13 122.4(5) . . ? N3 C12 C11 117.2(5) . . ? C13 C12 C11 120.4(5) . . ? N5 C13 C12 120.5(6) . . ? N5 C13 C14 119.6(5) . . ? C12 C13 C14 119.9(5) . . ? N6 C14 C15 121.0(5) . . ? N6 C14 C13 120.4(5) . . ? C15 C14 C13 118.5(5) . . ? N8 C15 C14 122.1(5) . . ? N8 C15 C16 117.5(5) . . ? C14 C15 C16 120.4(5) . . ? N7 C16 C11 119.9(5) . . ? N7 C16 C15 119.4(5) . . ? C11 C16 C15 120.7(5) . . ? N6 C17 C18 123.4(6) . . ? N8 C18 C17 122.1(6) . . ? N12 C19 C20 121.9(6) . . ? N13 C20 C19 123.1(6) . . ? N11 C21 C22 122.9(6) . . ? N16 C22 C21 121.4(6) . . ? N12 C23 C28 121.7(5) . . ? N12 C23 C24 118.5(5) . . ? C28 C23 C24 119.9(5) . . ? N11 C24 C25 120.5(5) . . ? N11 C24 C23 120.3(5) . . ? C25 C24 C23 119.1(5) . . ? N16 C25 C24 122.8(5) . . ? N16 C25 C26 116.6(5) . . ? C24 C25 C26 120.7(5) . . ? N15 C26 C27 121.8(5) . . ? N15 C26 C25 117.2(5) . . ? C27 C26 C25 121.0(5) . . ? N14 C27 C26 121.7(6) . . ? N14 C27 C28 119.9(5) . . ? C26 C27 C28 118.4(5) . . ? N13 C28 C23 120.3(6) . . ? N13 C28 C27 118.8(5) . . ? C23 C28 C27 121.0(5) . . ? N14 C29 C30 123.8(6) . . ? N15 C30 C29 120.9(6) . . ? N17 C31 C1 121.7(5) . . ? N17 C32 C2 121.9(5) . . ? N17 C32 C33 118.1(5) . . ? C2 C32 C33 120.0(5) . . ? N18 C33 C34 122.7(5) . . ? N18 C33 C32 117.3(5) . . ? C34 C33 C32 119.9(5) . . ? N9 C34 C33 120.6(5) . . ? N9 C34 C4 119.6(5) . . ? C33 C34 C4 119.9(5) . . ? N18 C35 C36 121.9(6) . . ? N9 C36 C35 122.8(6) . . ? C42 C37 C38 120.6(11) . . ? C39 C38 C37 122.1(12) . . ? C38 C39 C40 120.5(12) . . ? C39 C40 C41 117.6(11) . . ? C42 C41 C40 119.3(11) . . ? C37 C42 C41 120.0(10) . . ? F3 B1 F2 112.3(8) . . ? F3 B1 F4 108.1(10) . . ? F2 B1 F4 106.7(8) . . ? F3 B1 F1 115.0(10) . . ? F2 B1 F1 108.6(7) . . ? F4 B1 F1 105.5(7) . . ? F8 B2 F7 113.4(9) . . ? F8 B2 F5 115.2(7) . . ? F7 B2 F5 111.9(8) . . ? F8 B2 F6 107.2(8) . . ? F7 B2 F6 103.7(8) . . ? F5 B2 F6 104.1(8) . . ? F10A B3A F9A 116.5(12) . . ? F10A B3A F12A 109.7(12) . . ? F9A B3A F12A 110.7(13) . . ? F10A B3A F11A 104.3(12) . . ? F9A B3A F11A 103.4(12) . . ? F12A B3A F11A 111.9(12) . . ? F11B B3B F9B 129(3) . . ? F11B B3B F12B 120(3) . . ? F9B B3B F12B 96(2) . . ? F11B B3B F10B 105(2) . . ? F9B B3B F10B 98(2) . . ? F12B B3B F10B 105(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.189 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.118 #===END data_d:\ms089\p43_21_2 _database_code_depnum_ccdc_archive 'CCDC 285144' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H6 Cu F6 N6 P' _chemical_formula_weight 442.74 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' '-x+1/2, y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 11.4992(3) _cell_length_b 11.4992(3) _cell_length_c 12.7341(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1683.85(10) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 240 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1000 CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27447 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.31 _reflns_number_total 2100 _reflns_number_gt 2063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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. The P-F and F-F interatomic distances in the PF6 moiety were fixed at reasonable average values found via the Cambridge Structural Database. ; _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^)+(0.0896P)^2^+5.9138P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.002(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(5) _refine_ls_number_reflns 2100 _refine_ls_number_parameters 151 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1877 _refine_ls_goodness_of_fit_ref 1.232 _refine_ls_restrained_S_all 1.235 _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 0.85266(5) 0.85266(5) 0.0000 0.0219(3) Uani 1 2 d S . . P1 P 1.3565(10) 0.9545(13) -0.0181(11) 0.260(12) Uani 0.50 1 d PD . . F1 F 1.4891(14) 0.919(2) -0.023(3) 0.77(11) Uani 0.50 1 d PD . . F2 F 1.323(2) 0.827(2) -0.052(3) 0.50(2) Uani 0.50 1 d PD . . F3 F 1.360(2) 0.978(3) -0.1404(16) 0.39(4) Uani 0.50 1 d PD . . F4 F 1.391(2) 1.0864(15) -0.003(3) 0.35(3) Uani 0.50 1 d PD . . F5 F 1.362(3) 0.9394(19) 0.1061(17) 0.57(7) Uani 0.50 1 d PD . . F6 F 1.2242(14) 0.986(3) -0.0097(14) 0.202(14) Uani 0.50 1 d PD . . N1 N 1.0005(4) 0.8013(4) 0.0710(3) 0.0186(8) Uani 1 1 d . . . N2 N 0.7029(4) 0.7928(4) 0.0890(3) 0.0220(9) Uani 1 1 d . . . N3 N 0.8966(4) 0.9943(4) 0.1645(4) 0.0264(10) Uani 1 1 d . . . C1 C 1.0556(5) 0.7101(5) 0.0307(4) 0.0227(10) Uani 1 1 d . . . H1 H 1.0257 0.6762 -0.0298 0.027 Uiso 1 1 calc R . . C2 C 1.1564(6) 0.6626(5) 0.0749(4) 0.0274(11) Uani 1 1 d . . . H2 H 1.1913 0.5987 0.0432 0.033 Uiso 1 1 calc R . . C3 C 1.1488(5) 0.8010(4) 0.2028(3) 0.0184(9) Uani 1 1 d . . . C4 C 1.0490(4) 0.8475(5) 0.1591(4) 0.0179(8) Uani 1 1 d . . . C5 C 0.9963(4) 0.9501(4) 0.2066(4) 0.0192(9) Uani 1 1 d . . . C6 C 0.8553(6) 1.0896(5) 0.2067(5) 0.0308(12) Uani 1 1 d . . . H6 H 0.7879 1.1223 0.1792 0.037 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 0.0182(3) 0.0182(3) 0.0291(4) 0.0043(3) -0.0043(3) -0.0025(3) P1 0.163(10) 0.323(18) 0.295(17) 0.261(16) -0.154(11) -0.183(12) F1 0.31(5) 0.56(9) 1.4(2) 0.81(13) -0.62(11) -0.36(6) F2 0.50(3) 0.58(4) 0.41(7) 0.28(5) -0.27(5) -0.500 F3 0.17(3) 0.56(7) 0.43(6) 0.45(6) 0.00(4) 0.02(4) F4 0.38(5) 0.16(3) 0.53(7) 0.25(4) -0.21(6) -0.15(3) F5 0.69(9) 0.19(3) 0.81(10) 0.34(5) -0.70(9) -0.31(5) F6 0.16(2) 0.35(4) 0.092(12) 0.06(2) -0.029(16) -0.03(3) N1 0.0174(19) 0.0170(19) 0.0214(18) -0.0001(16) -0.0048(16) -0.0023(16) N2 0.028(2) 0.020(2) 0.0181(19) -0.0005(16) -0.0016(17) -0.0040(18) N3 0.024(2) 0.025(2) 0.030(2) -0.0037(19) -0.0062(19) 0.0046(18) C1 0.023(2) 0.024(2) 0.021(2) 0.0006(18) -0.0049(19) -0.001(2) C2 0.034(3) 0.024(3) 0.024(2) -0.0050(19) -0.002(2) 0.005(2) C3 0.019(2) 0.018(2) 0.0181(19) 0.0001(17) 0.0016(19) 0.0024(19) C4 0.0151(19) 0.018(2) 0.020(2) 0.000(2) 0.0000(16) 0.0004(19) C5 0.018(2) 0.020(2) 0.020(2) -0.0004(18) -0.0049(17) 0.0007(18) C6 0.024(2) 0.023(2) 0.046(3) -0.009(2) -0.011(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 2.014(4) 7 ? Cu1 N1 2.014(4) . ? Cu1 N2 2.173(5) 7 ? Cu1 N2 2.173(5) . ? P1 F6 1.566(15) . ? P1 F4 1.578(15) . ? P1 F1 1.579(15) . ? P1 F3 1.582(14) . ? P1 F2 1.583(16) . ? P1 F5 1.592(16) . ? N1 C1 1.329(7) . ? N1 C4 1.360(6) . ? N2 C2 1.324(7) 5_465 ? N2 C3 1.354(6) 5_465 ? N3 C6 1.309(7) . ? N3 C5 1.365(7) . ? C1 C2 1.400(8) . ? C2 N2 1.324(7) 5_565 ? C3 N2 1.354(6) 5_565 ? C3 C4 1.384(7) . ? C3 C3 1.452(9) 8_775 ? C4 C5 1.457(7) . ? C5 C5 1.407(9) 8_775 ? C6 C6 1.420(11) 8_775 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 134.1(2) 7 . ? N1 Cu1 N2 109.97(17) 7 7 ? N1 Cu1 N2 105.64(18) . 7 ? N1 Cu1 N2 105.64(18) 7 . ? N1 Cu1 N2 109.97(17) . . ? N2 Cu1 N2 76.7(2) 7 . ? F6 P1 F4 90.8(11) . . ? F6 P1 F1 177.8(12) . . ? F4 P1 F1 90.6(9) . . ? F6 P1 F3 93.2(9) . . ? F4 P1 F3 87.1(9) . . ? F1 P1 F3 88.6(10) . . ? F6 P1 F2 89.5(9) . . ? F4 P1 F2 170.9(19) . . ? F1 P1 F2 89.4(11) . . ? F3 P1 F2 84(2) . . ? F6 P1 F5 89.9(10) . . ? F4 P1 F5 88.5(11) . . ? F1 P1 F5 88.5(9) . . ? F3 P1 F5 174.6(13) . . ? F2 P1 F5 100.5(18) . . ? C1 N1 C4 115.5(4) . . ? C1 N1 Cu1 117.4(3) . . ? C4 N1 Cu1 127.0(4) . . ? C2 N2 C3 116.7(5) 5_465 5_465 ? C2 N2 Cu1 129.0(4) 5_465 . ? C3 N2 Cu1 114.3(3) 5_465 . ? C6 N3 C5 117.1(5) . . ? N1 C1 C2 123.2(5) . . ? N2 C2 C1 121.1(5) 5_565 . ? N2 C3 C4 122.1(4) 5_565 . ? N2 C3 C3 117.3(3) 5_565 8_775 ? C4 C3 C3 120.6(3) . 8_775 ? N1 C4 C3 121.4(5) . . ? N1 C4 C5 119.2(4) . . ? C3 C4 C5 119.3(4) . . ? N3 C5 C5 120.9(3) . 8_775 ? N3 C5 C4 119.2(4) . . ? C5 C5 C4 119.9(3) 8_775 . ? N3 C6 C6 122.0(3) . 8_775 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.932 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.168 #===END data_f:\ms087\pna21 _database_code_depnum_ccdc_archive 'CCDC 285145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H42 Cu4 F24 N20 O4 Sb4' _chemical_formula_weight 2256.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 13.3899(18) _cell_length_b 14.2532(16) _cell_length_c 37.468(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7150.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 155(2) _cell_measurement_reflns_used 290 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4344 _exptl_absorpt_coefficient_mu 2.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 155(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1000 CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67498 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14548 _reflns_number_gt 12964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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. The crystal structure was refined as a racemic inversion twin which resulted in the final BASF parameter of 0.48. All attempts to solve the structure in the centrosymmetric space group Pnma failed. ; _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^)+(0.0655P)^2^+28.1870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(6) _refine_ls_number_reflns 14548 _refine_ls_number_parameters 893 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.114 _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 Sb1 Sb 0.70253(5) 0.24740(6) 0.45985(2) 0.0456(2) Uani 1 1 d . . . Sb2 Sb 0.48203(5) 0.67118(4) 0.391641(18) 0.03264(14) Uani 1 1 d . . . Sb3 Sb 0.28518(5) 0.25177(6) 0.13907(2) 0.0462(2) Uani 1 1 d . . . Sb4 Sb 0.06176(5) -0.16760(5) 0.209493(19) 0.03651(16) Uani 1 1 d . . . Cu1 Cu 0.23032(8) -0.24819(8) 0.50903(3) 0.0314(3) Uani 1 1 d . . . Cu2 Cu 0.48084(8) 0.03310(8) 0.39023(4) 0.0342(2) Uani 1 1 d . . . Cu3 Cu 0.55248(8) 0.03204(8) 0.21011(4) 0.0334(3) Uani 1 1 d . . . Cu4 Cu 0.30839(7) -0.25459(8) 0.09123(3) 0.0291(3) Uani 1 1 d . . . F1 F 0.7516(9) 0.1391(8) 0.4811(3) 0.124(4) Uani 1 1 d . . . F2 F 0.8278(7) 0.3035(10) 0.4592(3) 0.127(5) Uani 1 1 d . . . F3 F 0.6820(7) 0.3001(8) 0.5046(2) 0.099(3) Uani 1 1 d . . . F4 F 0.5753(6) 0.1946(8) 0.4600(3) 0.097(3) Uani 1 1 d . . . F5 F 0.7246(10) 0.1914(8) 0.4156(2) 0.121(4) Uani 1 1 d . . . F6 F 0.6543(9) 0.3521(7) 0.4381(4) 0.134(5) Uani 1 1 d . . . F7 F 0.5826(5) 0.5824(5) 0.38441(18) 0.0589(19) Uani 1 1 d . . . F8 F 0.4877(4) 0.6497(5) 0.44105(18) 0.0518(18) Uani 1 1 d . . . F9 F 0.5777(7) 0.7652(7) 0.3974(2) 0.099(4) Uani 1 1 d . . . F10 F 0.4753(6) 0.6980(6) 0.34273(19) 0.064(2) Uani 1 1 d . . . F11 F 0.3891(4) 0.5733(5) 0.38668(17) 0.0533(16) Uani 1 1 d . . . F12 F 0.3772(7) 0.7539(6) 0.4015(2) 0.087(3) Uani 1 1 d . . . F13 F 0.4131(7) 0.2024(10) 0.1381(3) 0.139(6) Uani 1 1 d . . . F14 F 0.3028(11) 0.2982(15) 0.1845(3) 0.190(8) Uani 1 1 d . . . F15 F 0.3416(12) 0.3553(8) 0.1200(5) 0.196(8) Uani 1 1 d . . . F16 F 0.2708(7) 0.2139(11) 0.0933(2) 0.130(5) Uani 1 1 d . . . F17 F 0.2356(19) 0.1506(10) 0.1602(6) 0.246(12) Uani 1 1 d . . . F18 F 0.1606(6) 0.3024(9) 0.1381(3) 0.123(5) Uani 1 1 d . . . F19 F 0.1652(10) -0.2512(7) 0.2028(3) 0.125(5) Uani 1 1 d . . . F20 F 0.1504(5) -0.0698(6) 0.2118(2) 0.083(3) Uani 1 1 d . . . F21 F 0.0666(7) -0.1815(7) 0.25846(19) 0.081(3) Uani 1 1 d . . . F22 F -0.0270(10) -0.2663(7) 0.2059(3) 0.126(5) Uani 1 1 d . . . F23 F 0.0553(5) -0.1531(5) 0.15938(18) 0.0521(19) Uani 1 1 d . . . F24 F -0.0411(4) -0.0807(5) 0.21415(19) 0.059(2) Uani 1 1 d . . . N1 N 0.2756(5) -0.1391(5) 0.4728(2) 0.0244(15) Uani 1 1 d . . . N2 N 0.3754(5) -0.2419(5) 0.5228(2) 0.0256(15) Uani 1 1 d . . . N3 N 0.5842(5) -0.2440(5) 0.5227(2) 0.0263(15) Uani 1 1 d . . . N4 N 0.6868(5) -0.1436(5) 0.47261(19) 0.0262(16) Uani 1 1 d . . . N5 N 0.5826(5) -0.0290(5) 0.42344(19) 0.0242(15) Uani 1 1 d . . . N6 N 0.3809(5) -0.0287(5) 0.4228(2) 0.0274(16) Uani 1 1 d . . . N7 N 0.4984(6) 0.0035(5) 0.33697(19) 0.0298(16) Uani 1 1 d . . . N8 N 0.4749(5) 0.1665(5) 0.3728(2) 0.0240(16) Uani 1 1 d . . . N9 N 0.4653(5) 0.3381(5) 0.3351(2) 0.0310(17) Uani 1 1 d . . . N10 N 0.4991(6) 0.3374(5) 0.2616(2) 0.0305(17) Uani 1 1 d . . . N11 N 0.5352(5) 0.1670(5) 0.2268(2) 0.0258(16) Uani 1 1 d . . . N12 N 0.5310(5) 0.0026(5) 0.2624(2) 0.0268(15) Uani 1 1 d . . . N13 N 0.4508(5) -0.0316(5) 0.1763(2) 0.0251(15) Uani 1 1 d . . . N14 N 0.6543(5) -0.0327(5) 0.17862(18) 0.0231(15) Uani 1 1 d . . . N15 N 0.7631(5) -0.1393(5) 0.12831(18) 0.0256(15) Uani 1 1 d . . . N16 N 0.6650(5) -0.2409(5) 0.07793(19) 0.0232(15) Uani 1 1 d . . . N17 N 0.4519(5) -0.2454(5) 0.0780(2) 0.0259(16) Uani 1 1 d . . . N18 N 0.3489(5) -0.1443(5) 0.1270(2) 0.0289(17) Uani 1 1 d . . . C1 C 0.4277(7) -0.2866(9) 0.5469(3) 0.042(3) Uani 1 1 d . . . H1 H 0.3943 -0.3180 0.5651 0.051 Uiso 1 1 calc R . . C2 C 0.5326(7) -0.2888(8) 0.5462(3) 0.043(3) Uani 1 1 d . . . H2 H 0.5661 -0.3238 0.5634 0.052 Uiso 1 1 calc R . . C3 C 0.7325(7) -0.0920(7) 0.4478(2) 0.032(2) Uani 1 1 d . . . H3 H 0.8019 -0.0934 0.4468 0.038 Uiso 1 1 calc R . . C4 C 0.6819(7) -0.0363(6) 0.4235(3) 0.034(2) Uani 1 1 d . . . H4 H 0.7184 -0.0030 0.4066 0.041 Uiso 1 1 calc R . . C5 C 0.2807(6) -0.0340(6) 0.4240(2) 0.030(2) Uani 1 1 d . . . H5 H 0.2443 0.0000 0.4073 0.036 Uiso 1 1 calc R . . C6 C 0.2284(6) -0.0875(7) 0.4490(2) 0.031(2) Uani 1 1 d . . . H6 H 0.1589 -0.0869 0.4488 0.037 Uiso 1 1 calc R . . C7 C 0.4295(5) -0.1910(6) 0.4995(2) 0.0219(17) Uani 1 1 d . . . C8 C 0.5327(5) -0.1912(6) 0.4992(2) 0.0206(16) Uani 1 1 d . . . C9 C 0.5860(6) -0.1364(6) 0.4724(2) 0.0194(16) Uani 1 1 d . . . C10 C 0.5347(6) -0.0820(6) 0.4488(2) 0.0247(18) Uani 1 1 d . . . C11 C 0.4273(6) -0.0814(6) 0.4482(2) 0.0183(16) Uani 1 1 d . . . C12 C 0.3735(6) -0.1348(5) 0.4730(2) 0.0190(15) Uani 1 1 d . . . C13 C 0.5131(7) -0.0758(6) 0.3192(2) 0.036(2) Uani 1 1 d . . . H13 H 0.5138 -0.1323 0.3317 0.043 Uiso 1 1 calc R . . C14 C 0.5276(8) -0.0768(7) 0.2822(3) 0.045(2) Uani 1 1 d . . . H14 H 0.5353 -0.1343 0.2708 0.054 Uiso 1 1 calc R . . C15 C 0.5374(7) 0.2477(6) 0.2093(3) 0.036(2) Uani 1 1 d . . . H15 H 0.5534 0.2483 0.1852 0.043 Uiso 1 1 calc R . . C16 C 0.5158(8) 0.3322(8) 0.2267(3) 0.040(2) Uani 1 1 d . . . H16 H 0.5131 0.3870 0.2133 0.048 Uiso 1 1 calc R . . C17 C 0.4500(8) 0.3325(7) 0.3701(3) 0.038(2) Uani 1 1 d . . . H17 H 0.4346 0.3872 0.3825 0.046 Uiso 1 1 calc R . . C18 C 0.4559(6) 0.2484(7) 0.3891(3) 0.034(2) Uani 1 1 d . . . H18 H 0.4464 0.2492 0.4137 0.040 Uiso 1 1 calc R . . C19 C 0.5021(6) 0.0846(6) 0.3183(2) 0.0249(16) Uani 1 1 d . . . C20 C 0.5181(6) 0.0842(6) 0.2819(2) 0.0246(16) Uani 1 1 d . . . C21 C 0.5191(5) 0.1718(6) 0.2630(2) 0.0236(17) Uani 1 1 d . . . C22 C 0.5012(5) 0.2554(6) 0.2793(2) 0.0242(17) Uani 1 1 d . . . C23 C 0.4826(6) 0.2565(5) 0.3180(2) 0.0246(16) Uani 1 1 d . . . C24 C 0.4864(5) 0.1714(5) 0.3370(2) 0.0184(15) Uani 1 1 d . . . C25 C 0.3518(7) -0.0347(8) 0.1754(3) 0.045(3) Uani 1 1 d . . . H25 H 0.3148 0.0021 0.1911 0.054 Uiso 1 1 calc R . . C26 C 0.3015(7) -0.0942(7) 0.1505(3) 0.038(2) Uani 1 1 d . . . H26 H 0.2321 -0.0971 0.1511 0.046 Uiso 1 1 calc R . . C27 C 0.5069(7) -0.2902(8) 0.0523(3) 0.037(2) Uani 1 1 d . . . H27 H 0.4746 -0.3250 0.0348 0.045 Uiso 1 1 calc R . . C28 C 0.6118(7) -0.2840(8) 0.0522(2) 0.038(2) Uani 1 1 d . . . H28 H 0.6463 -0.3113 0.0333 0.045 Uiso 1 1 calc R . . C29 C 0.8066(6) -0.0903(7) 0.1540(2) 0.032(2) Uani 1 1 d . . . H29 H 0.8759 -0.0915 0.1558 0.038 Uiso 1 1 calc R . . C30 C 0.7528(7) -0.0372(7) 0.1786(2) 0.033(2) Uani 1 1 d . . . H30 H 0.7877 -0.0033 0.1958 0.039 Uiso 1 1 calc R . . C31 C 0.5000(6) -0.0825(6) 0.1520(2) 0.0229(18) Uani 1 1 d . . . C32 C 0.4496(6) -0.1398(5) 0.1275(2) 0.0200(16) Uani 1 1 d . . . C33 C 0.5033(5) -0.1945(6) 0.1015(2) 0.0171(16) Uani 1 1 d . . . C34 C 0.6093(5) -0.1918(5) 0.10184(19) 0.0175(15) Uani 1 1 d . . . C35 C 0.6619(6) -0.1372(6) 0.1281(2) 0.0223(17) Uani 1 1 d . . . C36 C 0.6087(6) -0.0825(6) 0.1529(2) 0.0209(16) Uani 1 1 d . . . C1S C 0.3636(8) -0.4985(11) 0.5360(4) 0.165(10) Uiso 1 1 d G . . H1S H 0.2988 -0.4980 0.5271 0.198 Uiso 1 1 calc R . . C2S C 0.3798(10) -0.4984(11) 0.5726(4) 0.128(7) Uiso 1 1 d G . . H2S H 0.3257 -0.4978 0.5882 0.154 Uiso 1 1 calc R . . C3S C 0.4766(12) -0.4992(12) 0.5860(4) 0.139(6) Uiso 1 1 d G . . H3S H 0.4874 -0.4992 0.6105 0.167 Uiso 1 1 calc R . . C4S C 0.5574(9) -0.5001(14) 0.5626(4) 0.139(6) Uiso 1 1 d G . . H4S H 0.6222 -0.5007 0.5716 0.167 Uiso 1 1 calc R . . C5S C 0.5412(9) -0.5002(12) 0.5260(4) 0.116(7) Uiso 1 1 d G . . H5S H 0.5952 -0.5008 0.5104 0.140 Uiso 1 1 calc R . . C6S C 0.4444(10) -0.4994(10) 0.5127(4) 0.095(5) Uiso 1 1 d G . . H6S H 0.4336 -0.4995 0.4881 0.114 Uiso 1 1 calc R . . C7S C 0.7404(7) 0.4454(6) 0.2849(3) 0.076(4) Uani 1 1 d G . . H7S H 0.7426 0.5045 0.2744 0.091 Uiso 1 1 calc R . . C8S C 0.7570(7) 0.3657(8) 0.2644(2) 0.077(4) Uani 1 1 d G . . H8S H 0.7702 0.3715 0.2401 0.092 Uiso 1 1 calc R . . C9S C 0.7537(6) 0.2774(6) 0.2801(3) 0.084(5) Uani 1 1 d G . . H9S H 0.7648 0.2241 0.2663 0.101 Uiso 1 1 calc R . . C10S C 0.7339(7) 0.2687(6) 0.3163(3) 0.071(4) Uani 1 1 d G . . H10S H 0.7317 0.2097 0.3268 0.085 Uiso 1 1 calc R . . C11S C 0.7174(6) 0.3484(8) 0.3369(2) 0.079(4) Uani 1 1 d G . . H11S H 0.7042 0.3426 0.3612 0.094 Uiso 1 1 calc R . . C12S C 0.7207(7) 0.4367(6) 0.3212(3) 0.075(4) Uani 1 1 d G . . H12S H 0.7096 0.4900 0.3350 0.090 Uiso 1 1 calc R . . C13S C 0.5419(6) -0.0619(5) 0.02185(16) 0.066(4) Uani 1 1 d G . . H13S H 0.5441 -0.1032 0.0027 0.079 Uiso 1 1 calc R . . C14S C 0.6301(6) -0.0302(5) 0.03724(16) 0.063(4) Uani 1 1 d G . . H14S H 0.6913 -0.0502 0.0283 0.076 Uiso 1 1 calc R . . C15S C 0.6268(5) 0.0315(5) 0.06595(16) 0.070(4) Uani 1 1 d G . . H15S H 0.6858 0.0528 0.0762 0.084 Uiso 1 1 calc R . . C16S C 0.5353(5) 0.0615(4) 0.07926(14) 0.056(3) Uani 1 1 d G . . H16S H 0.5331 0.1028 0.0985 0.067 Uiso 1 1 calc R . . C17S C 0.4471(5) 0.0297(4) 0.06386(16) 0.071(5) Uani 1 1 d G . . H17S H 0.3859 0.0498 0.0728 0.086 Uiso 1 1 calc R . . C18S C 0.4504(6) -0.0320(5) 0.03516(17) 0.064(4) Uani 1 1 d G . . H18S H 0.3914 -0.0532 0.0249 0.076 Uiso 1 1 calc R . . N1S N 0.2905(4) 0.4872(3) 0.29294(14) 0.063(3) Uiso 1 1 d GD . . O1S O 0.2383(5) 0.4797(4) 0.32057(15) 0.090(3) Uiso 1 1 d GD . . O2S O 0.2631(4) 0.4541(4) 0.26360(15) 0.088(3) Uiso 1 1 d GD . . C19S C 0.3887(4) 0.5349(4) 0.29310(16) 0.045(2) Uiso 1 1 d GD . . H19A H 0.4345 0.5010 0.2782 0.068 Uiso 1 1 calc R . . H19B H 0.4142 0.5369 0.3170 0.068 Uiso 1 1 calc R . . H19C H 0.3812 0.5976 0.2842 0.068 Uiso 1 1 calc R . . N2S N 0.2748(16) -0.2393(14) 0.2916(5) 0.145(8) Uiso 1 1 d D . . O3S O 0.250(2) -0.3162(16) 0.2753(6) 0.233(10) Uiso 1 1 d D . . O4S O 0.3279(13) -0.1807(12) 0.2791(4) 0.150(6) Uiso 1 1 d D . . C20S C 0.2261(16) -0.2288(14) 0.3262(5) 0.115(7) Uiso 1 1 d D . . H20A H 0.2640 -0.1862 0.3407 0.173 Uiso 1 1 calc R . . H20B H 0.2225 -0.2888 0.3378 0.173 Uiso 1 1 calc R . . H20C H 0.1599 -0.2045 0.3228 0.173 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 Sb1 0.0352(3) 0.0703(6) 0.0313(4) 0.0054(3) 0.0002(3) -0.0167(3) Sb2 0.0414(3) 0.0320(3) 0.0246(3) -0.0084(3) -0.0009(3) -0.0024(2) Sb3 0.0332(3) 0.0707(6) 0.0347(4) 0.0042(3) 0.0013(3) 0.0139(3) Sb4 0.0462(4) 0.0374(4) 0.0260(3) -0.0104(3) -0.0010(3) 0.0048(3) Cu1 0.0160(5) 0.0446(7) 0.0337(7) -0.0013(5) 0.0002(4) -0.0057(5) Cu2 0.0435(6) 0.0330(6) 0.0260(6) 0.0079(6) 0.0035(5) 0.0031(4) Cu3 0.0402(6) 0.0338(6) 0.0262(6) -0.0091(6) 0.0037(5) 0.0004(4) Cu4 0.0155(5) 0.0416(7) 0.0302(6) 0.0012(5) -0.0002(4) -0.0059(4) F1 0.135(9) 0.126(8) 0.111(8) -0.006(7) -0.064(7) 0.052(7) F2 0.059(5) 0.213(13) 0.110(8) -0.059(9) 0.039(6) -0.078(7) F3 0.076(5) 0.149(8) 0.072(6) -0.045(6) 0.041(5) -0.023(6) F4 0.049(4) 0.133(8) 0.108(7) 0.036(7) -0.017(5) -0.051(5) F5 0.181(11) 0.136(9) 0.047(5) -0.028(6) 0.016(6) -0.080(8) F6 0.143(10) 0.078(6) 0.179(12) 0.083(7) -0.037(9) -0.036(6) F7 0.042(3) 0.089(5) 0.045(4) -0.015(4) 0.000(3) 0.028(3) F8 0.046(4) 0.084(5) 0.025(3) -0.004(3) 0.000(3) 0.002(3) F9 0.124(7) 0.108(7) 0.066(5) -0.048(5) 0.024(5) -0.093(6) F10 0.117(6) 0.045(4) 0.030(4) 0.003(3) -0.001(4) -0.016(4) F11 0.050(3) 0.067(4) 0.042(4) -0.015(3) 0.012(3) -0.024(3) F12 0.103(6) 0.080(5) 0.078(6) -0.040(4) -0.023(5) 0.053(5) F13 0.075(6) 0.219(13) 0.124(9) -0.085(10) -0.040(6) 0.093(8) F14 0.148(12) 0.35(2) 0.075(8) -0.093(11) -0.036(8) 0.108(13) F15 0.210(15) 0.107(9) 0.271(18) -0.035(10) 0.171(14) -0.075(9) F16 0.055(5) 0.278(14) 0.056(5) -0.046(8) -0.016(4) 0.016(7) F17 0.37(3) 0.102(10) 0.27(2) 0.095(12) 0.19(2) 0.083(13) F18 0.056(5) 0.178(10) 0.133(9) 0.092(8) 0.053(6) 0.067(6) F19 0.164(10) 0.140(9) 0.071(6) -0.049(6) -0.032(6) 0.115(8) F20 0.059(4) 0.120(6) 0.069(5) -0.063(5) 0.025(4) -0.037(4) F21 0.145(8) 0.079(6) 0.020(4) 0.000(3) -0.006(4) 0.040(5) F22 0.208(13) 0.077(6) 0.094(7) -0.050(6) 0.074(8) -0.098(7) F23 0.057(4) 0.075(5) 0.024(3) -0.013(3) 0.002(3) 0.002(3) F24 0.038(3) 0.095(5) 0.044(4) -0.032(4) -0.009(3) 0.027(3) N1 0.023(3) 0.025(4) 0.025(4) -0.004(3) -0.006(3) 0.000(3) N2 0.018(3) 0.045(4) 0.015(3) 0.001(3) 0.006(3) 0.005(3) N3 0.021(3) 0.035(4) 0.023(4) 0.008(3) -0.005(3) 0.001(3) N4 0.019(3) 0.035(4) 0.025(4) -0.005(3) 0.008(3) -0.006(3) N5 0.027(3) 0.024(4) 0.022(4) 0.000(3) 0.007(3) -0.008(3) N6 0.029(4) 0.025(4) 0.028(4) 0.000(3) -0.006(3) 0.002(3) N7 0.036(4) 0.031(4) 0.022(4) 0.006(3) 0.005(3) 0.000(3) N8 0.012(3) 0.024(4) 0.037(4) 0.001(3) -0.001(3) 0.003(2) N9 0.023(3) 0.028(4) 0.042(5) -0.002(3) 0.006(3) -0.003(3) N10 0.033(4) 0.026(4) 0.033(4) 0.002(3) 0.005(3) 0.005(3) N11 0.018(3) 0.034(4) 0.025(4) -0.005(3) 0.002(3) 0.005(3) N12 0.031(4) 0.021(4) 0.028(4) -0.004(3) 0.004(3) -0.003(3) N13 0.022(3) 0.028(4) 0.026(4) -0.003(3) -0.002(3) -0.003(3) N14 0.025(3) 0.033(4) 0.012(3) 0.003(3) 0.002(3) 0.004(3) N15 0.020(3) 0.039(4) 0.018(4) 0.005(3) 0.003(3) 0.006(3) N16 0.022(3) 0.033(4) 0.015(3) 0.002(3) -0.004(3) 0.003(3) N17 0.015(3) 0.026(4) 0.037(4) -0.003(3) 0.008(3) -0.001(3) N18 0.015(3) 0.034(4) 0.038(5) 0.001(3) -0.001(3) -0.001(3) C1 0.024(4) 0.072(8) 0.031(6) 0.016(5) 0.012(4) 0.005(5) C2 0.021(4) 0.062(7) 0.047(6) 0.018(5) -0.017(4) 0.006(4) C3 0.026(4) 0.041(6) 0.028(5) -0.001(4) 0.003(4) 0.000(4) C4 0.029(5) 0.027(5) 0.045(6) 0.004(4) 0.006(4) 0.000(4) C5 0.022(4) 0.035(5) 0.033(5) 0.008(4) -0.002(4) 0.013(3) C6 0.020(4) 0.042(5) 0.031(5) -0.003(4) -0.012(3) 0.005(3) C7 0.015(4) 0.031(5) 0.020(4) -0.002(4) 0.002(3) -0.003(3) C8 0.014(3) 0.030(4) 0.018(4) -0.003(3) -0.001(3) -0.001(3) C9 0.022(4) 0.024(4) 0.012(4) -0.008(3) -0.003(3) 0.000(3) C10 0.029(4) 0.024(4) 0.021(4) -0.013(4) 0.004(3) -0.009(3) C11 0.021(4) 0.018(4) 0.016(4) -0.008(3) -0.003(3) 0.002(3) C12 0.025(4) 0.018(4) 0.014(3) -0.009(3) 0.009(3) 0.006(3) C13 0.053(6) 0.023(4) 0.031(5) 0.012(4) 0.007(4) -0.004(4) C14 0.056(6) 0.023(5) 0.055(7) -0.013(4) 0.007(5) 0.001(4) C15 0.030(5) 0.032(5) 0.045(6) 0.008(5) 0.005(4) 0.002(4) C16 0.048(6) 0.044(7) 0.028(5) 0.008(5) -0.002(4) 0.003(4) C17 0.056(6) 0.017(5) 0.040(6) -0.007(4) 0.009(5) 0.006(4) C18 0.029(4) 0.055(7) 0.017(5) 0.001(5) 0.004(3) 0.001(4) C19 0.017(3) 0.031(4) 0.026(4) 0.003(3) 0.005(3) -0.001(3) C20 0.023(4) 0.029(4) 0.023(4) -0.003(3) 0.001(3) -0.001(3) C21 0.012(3) 0.034(4) 0.025(4) 0.005(3) 0.003(3) 0.000(3) C22 0.010(3) 0.028(4) 0.035(4) 0.000(3) -0.005(3) -0.001(3) C23 0.019(4) 0.027(4) 0.028(4) -0.004(3) 0.002(3) 0.001(3) C24 0.006(3) 0.023(4) 0.026(4) 0.006(3) 0.002(3) 0.002(2) C25 0.031(5) 0.053(7) 0.051(7) -0.012(5) 0.018(5) 0.007(4) C26 0.023(4) 0.041(6) 0.050(6) -0.013(5) -0.002(4) 0.006(4) C27 0.030(5) 0.059(7) 0.023(5) -0.020(5) 0.010(4) -0.001(5) C28 0.032(5) 0.062(6) 0.019(4) -0.019(4) -0.007(4) -0.001(4) C29 0.017(4) 0.045(6) 0.032(5) -0.001(4) -0.004(4) -0.004(4) C30 0.036(5) 0.042(5) 0.020(4) -0.008(4) -0.006(4) -0.009(4) C31 0.021(4) 0.023(4) 0.025(5) 0.003(4) 0.002(3) 0.001(3) C32 0.016(3) 0.023(4) 0.022(4) 0.000(3) 0.010(3) -0.003(3) C33 0.014(3) 0.020(4) 0.017(4) 0.006(3) 0.000(3) 0.001(3) C34 0.020(4) 0.023(4) 0.010(3) 0.003(3) 0.002(3) 0.000(3) C35 0.017(4) 0.032(5) 0.017(4) 0.005(3) -0.005(3) -0.002(3) C36 0.019(4) 0.023(4) 0.021(4) 0.002(3) 0.002(3) 0.005(3) C7S 0.078(9) 0.079(9) 0.071(10) 0.010(8) -0.012(8) -0.001(8) C8S 0.058(8) 0.101(12) 0.071(9) -0.001(9) -0.021(7) -0.025(8) C9S 0.021(5) 0.100(12) 0.132(16) -0.031(11) -0.020(7) 0.010(6) C10S 0.032(6) 0.074(9) 0.107(13) 0.025(9) -0.019(7) -0.006(5) C11S 0.049(7) 0.109(13) 0.078(10) -0.005(9) -0.015(7) -0.002(7) C12S 0.052(7) 0.091(10) 0.081(10) -0.011(8) -0.022(7) 0.014(7) C13S 0.139(14) 0.033(7) 0.025(6) 0.002(6) 0.000(7) -0.005(7) C14S 0.095(10) 0.053(8) 0.042(7) 0.017(6) 0.015(7) 0.005(7) C15S 0.117(12) 0.047(7) 0.046(8) 0.032(6) -0.032(8) -0.021(7) C16S 0.103(10) 0.032(7) 0.033(7) 0.001(5) 0.001(6) -0.002(6) C17S 0.089(10) 0.068(10) 0.057(10) 0.043(8) 0.007(7) 0.009(7) C18S 0.118(12) 0.034(7) 0.039(8) 0.006(6) -0.014(7) -0.020(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F6 1.819(9) . ? Sb1 F1 1.856(10) . ? Sb1 F2 1.859(8) . ? Sb1 F3 1.859(8) . ? Sb1 F4 1.862(7) . ? Sb1 F5 1.864(9) . ? Sb2 F9 1.866(6) . ? Sb2 F7 1.867(6) . ? Sb2 F12 1.870(7) . ? Sb2 F10 1.874(7) . ? Sb2 F8 1.878(7) . ? Sb2 F11 1.879(6) . ? Sb3 F17 1.773(14) . ? Sb3 F15 1.804(11) . ? Sb3 F16 1.806(9) . ? Sb3 F18 1.817(7) . ? Sb3 F14 1.842(11) . ? Sb3 F13 1.852(8) . ? Sb4 F20 1.833(7) . ? Sb4 F19 1.844(8) . ? Sb4 F22 1.846(7) . ? Sb4 F21 1.847(7) . ? Sb4 F24 1.861(6) . ? Sb4 F23 1.891(7) . ? Cu1 N2 2.012(7) . ? Cu1 N3 2.024(7) 4_445 ? Cu1 N4 2.140(8) 4_445 ? Cu1 N1 2.151(8) . ? Cu2 N8 2.012(7) . ? Cu2 N6 2.014(8) . ? Cu2 N5 2.046(8) . ? Cu2 N7 2.053(7) . ? Cu3 N12 2.023(8) . ? Cu3 N14 2.026(7) . ? Cu3 N11 2.035(8) . ? Cu3 N13 2.069(7) . ? Cu4 N16 1.985(7) 4_445 ? Cu4 N17 1.989(6) . ? Cu4 N18 2.136(8) . ? Cu4 N15 2.141(7) 4_445 ? N1 C12 1.313(11) . ? N1 C6 1.319(11) . ? N2 C1 1.309(13) . ? N2 C7 1.347(11) . ? N3 C2 1.289(13) . ? N3 C8 1.348(11) . ? N3 Cu1 2.024(7) 4_545 ? N4 C3 1.334(12) . ? N4 C9 1.355(11) . ? N4 Cu1 2.140(8) 4_545 ? N5 C4 1.334(12) . ? N5 C10 1.372(11) . ? N6 C5 1.344(11) . ? N6 C11 1.363(11) . ? N7 C13 1.326(12) . ? N7 C19 1.353(11) . ? N8 C18 1.342(13) . ? N8 C24 1.354(11) . ? N9 C17 1.330(14) . ? N9 C23 1.348(11) . ? N10 C16 1.329(13) . ? N10 C22 1.345(11) . ? N11 C15 1.324(12) . ? N11 C21 1.375(11) . ? N12 C14 1.356(13) . ? N12 C20 1.385(11) . ? N13 C25 1.327(12) . ? N13 C31 1.338(11) . ? N14 C30 1.320(11) . ? N14 C36 1.344(11) . ? N15 C29 1.325(12) . ? N15 C35 1.355(10) . ? N15 Cu4 2.141(7) 4_545 ? N16 C28 1.347(11) . ? N16 C34 1.360(10) . ? N16 Cu4 1.985(7) 4_545 ? N17 C33 1.332(11) . ? N17 C27 1.370(11) . ? N18 C26 1.298(12) . ? N18 C32 1.350(10) . ? C1 C2 1.406(13) . ? C3 C4 1.385(13) . ? C5 C6 1.395(13) . ? C7 C8 1.382(11) . ? C7 C12 1.479(12) . ? C8 C9 1.457(12) . ? C9 C10 1.363(12) . ? C10 C11 1.439(12) . ? C11 C12 1.400(11) . ? C13 C14 1.400(12) . ? C15 C16 1.399(15) . ? C17 C18 1.397(14) . ? C19 C20 1.380(10) . ? C19 C24 1.437(11) . ? C20 C21 1.436(11) . ? C21 C22 1.361(12) . ? C22 C23 1.470(10) . ? C23 C24 1.407(11) . ? C25 C26 1.431(14) . ? C27 C28 1.407(14) . ? C29 C30 1.393(13) . ? C31 C32 1.402(12) . ? C31 C36 1.456(11) . ? C32 C33 1.439(11) . ? C33 C34 1.419(11) . ? C34 C35 1.438(11) . ? C35 C36 1.407(12) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C7S C8S 1.3900 . ? C7S C12S 1.3900 . ? C8S C9S 1.3900 . ? C9S C10S 1.3900 . ? C10S C11S 1.3900 . ? C11S C12S 1.3900 . ? C13S C14S 1.3900 . ? C13S C18S 1.3900 . ? C14S C15S 1.3900 . ? C15S C16S 1.3900 . ? C16S C17S 1.3900 . ? C17S C18S 1.3900 . ? N1S O2S 1.2513 . ? N1S O1S 1.2534 . ? N1S C19S 1.4804 . ? N2S O4S 1.192(15) . ? N2S O3S 1.298(16) . ? N2S C20S 1.459(16) . ? 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 F6 Sb1 F1 178.7(6) . . ? F6 Sb1 F2 87.8(6) . . ? F1 Sb1 F2 92.6(6) . . ? F6 Sb1 F3 91.2(6) . . ? F1 Sb1 F3 90.1(5) . . ? F2 Sb1 F3 88.4(4) . . ? F6 Sb1 F4 90.4(5) . . ? F1 Sb1 F4 89.2(5) . . ? F2 Sb1 F4 178.2(6) . . ? F3 Sb1 F4 91.5(4) . . ? F6 Sb1 F5 90.4(6) . . ? F1 Sb1 F5 88.2(6) . . ? F2 Sb1 F5 91.6(5) . . ? F3 Sb1 F5 178.3(6) . . ? F4 Sb1 F5 88.5(5) . . ? F9 Sb2 F7 90.5(4) . . ? F9 Sb2 F12 92.3(5) . . ? F7 Sb2 F12 175.6(4) . . ? F9 Sb2 F10 90.0(4) . . ? F7 Sb2 F10 91.8(3) . . ? F12 Sb2 F10 91.6(4) . . ? F9 Sb2 F8 88.6(4) . . ? F7 Sb2 F8 90.2(3) . . ? F12 Sb2 F8 86.5(3) . . ? F10 Sb2 F8 177.6(4) . . ? F9 Sb2 F11 177.8(5) . . ? F7 Sb2 F11 87.7(3) . . ? F12 Sb2 F11 89.4(4) . . ? F10 Sb2 F11 91.3(3) . . ? F8 Sb2 F11 90.2(3) . . ? F17 Sb3 F15 176.2(11) . . ? F17 Sb3 F16 98.0(9) . . ? F15 Sb3 F16 85.1(7) . . ? F17 Sb3 F18 89.3(8) . . ? F15 Sb3 F18 92.9(7) . . ? F16 Sb3 F18 90.1(5) . . ? F17 Sb3 F14 85.9(10) . . ? F15 Sb3 F14 91.1(9) . . ? F16 Sb3 F14 176.1(9) . . ? F18 Sb3 F14 89.7(6) . . ? F17 Sb3 F13 92.7(9) . . ? F15 Sb3 F13 85.2(8) . . ? F16 Sb3 F13 88.0(4) . . ? F18 Sb3 F13 177.4(6) . . ? F14 Sb3 F13 92.1(5) . . ? F20 Sb4 F19 90.7(5) . . ? F20 Sb4 F22 178.5(4) . . ? F19 Sb4 F22 88.9(6) . . ? F20 Sb4 F21 90.7(4) . . ? F19 Sb4 F21 92.2(4) . . ? F22 Sb4 F21 90.7(5) . . ? F20 Sb4 F24 88.2(4) . . ? F19 Sb4 F24 177.3(5) . . ? F22 Sb4 F24 92.1(5) . . ? F21 Sb4 F24 90.3(3) . . ? F20 Sb4 F23 89.6(4) . . ? F19 Sb4 F23 88.3(4) . . ? F22 Sb4 F23 89.0(4) . . ? F21 Sb4 F23 179.4(4) . . ? F24 Sb4 F23 89.2(3) . . ? N2 Cu1 N3 150.5(3) . 4_445 ? N2 Cu1 N4 117.3(3) . 4_445 ? N3 Cu1 N4 81.9(3) 4_445 4_445 ? N2 Cu1 N1 81.8(3) . . ? N3 Cu1 N1 118.1(3) 4_445 . ? N4 Cu1 N1 101.3(3) 4_445 . ? N8 Cu2 N6 125.7(3) . . ? N8 Cu2 N5 129.2(3) . . ? N6 Cu2 N5 83.4(3) . . ? N8 Cu2 N7 83.3(3) . . ? N6 Cu2 N7 125.1(3) . . ? N5 Cu2 N7 115.2(3) . . ? N12 Cu3 N14 124.4(3) . . ? N12 Cu3 N11 83.3(3) . . ? N14 Cu3 N11 133.3(3) . . ? N12 Cu3 N13 114.1(3) . . ? N14 Cu3 N13 83.5(3) . . ? N11 Cu3 N13 121.8(3) . . ? N16 Cu4 N17 151.0(3) 4_445 . ? N16 Cu4 N18 115.3(3) 4_445 . ? N17 Cu4 N18 82.1(3) . . ? N16 Cu4 N15 82.3(3) 4_445 4_445 ? N17 Cu4 N15 118.8(3) . 4_445 ? N18 Cu4 N15 100.6(3) . 4_445 ? C12 N1 C6 117.2(8) . . ? C12 N1 Cu1 108.2(5) . . ? C6 N1 Cu1 134.1(6) . . ? C1 N2 C7 115.0(7) . . ? C1 N2 Cu1 132.2(7) . . ? C7 N2 Cu1 112.2(5) . . ? C2 N3 C8 116.6(7) . . ? C2 N3 Cu1 131.6(6) . 4_545 ? C8 N3 Cu1 111.1(5) . 4_545 ? C3 N4 C9 114.4(8) . . ? C3 N4 Cu1 135.8(6) . 4_545 ? C9 N4 Cu1 109.2(5) . 4_545 ? C4 N5 C10 115.0(8) . . ? C4 N5 Cu2 134.3(6) . . ? C10 N5 Cu2 110.4(6) . . ? C5 N6 C11 113.5(7) . . ? C5 N6 Cu2 135.1(6) . . ? C11 N6 Cu2 111.2(5) . . ? C13 N7 C19 117.6(7) . . ? C13 N7 Cu2 132.8(6) . . ? C19 N7 Cu2 109.4(6) . . ? C18 N8 C24 115.4(8) . . ? C18 N8 Cu2 133.0(7) . . ? C24 N8 Cu2 111.4(5) . . ? C17 N9 C23 116.4(8) . . ? C16 N10 C22 115.7(8) . . ? C15 N11 C21 116.5(8) . . ? C15 N11 Cu3 131.8(7) . . ? C21 N11 Cu3 111.6(6) . . ? C14 N12 C20 114.0(8) . . ? C14 N12 Cu3 135.2(6) . . ? C20 N12 Cu3 110.8(5) . . ? C25 N13 C31 117.2(8) . . ? C25 N13 Cu3 133.4(7) . . ? C31 N13 Cu3 109.3(5) . . ? C30 N14 C36 115.4(7) . . ? C30 N14 Cu3 134.0(6) . . ? C36 N14 Cu3 110.6(5) . . ? C29 N15 C35 115.6(7) . . ? C29 N15 Cu4 136.0(6) . 4_545 ? C35 N15 Cu4 107.2(6) . 4_545 ? C28 N16 C34 114.6(7) . . ? C28 N16 Cu4 132.6(6) . 4_545 ? C34 N16 Cu4 112.5(5) . 4_545 ? C33 N17 C27 116.2(7) . . ? C33 N17 Cu4 111.7(6) . . ? C27 N17 Cu4 131.6(7) . . ? C26 N18 C32 117.0(8) . . ? C26 N18 Cu4 134.9(6) . . ? C32 N18 Cu4 107.2(6) . . ? N2 C1 C2 122.2(9) . . ? N3 C2 C1 122.5(9) . . ? N4 C3 C4 123.4(9) . . ? N5 C4 C3 122.2(9) . . ? N6 C5 C6 123.7(8) . . ? N1 C6 C5 121.2(8) . . ? N2 C7 C8 122.9(8) . . ? N2 C7 C12 116.9(7) . . ? C8 C7 C12 120.2(7) . . ? N3 C8 C7 120.5(7) . . ? N3 C8 C9 119.9(7) . . ? C7 C8 C9 119.6(7) . . ? N4 C9 C10 123.2(8) . . ? N4 C9 C8 116.4(7) . . ? C10 C9 C8 120.4(8) . . ? C9 C10 N5 121.9(8) . . ? C9 C10 C11 121.0(8) . . ? N5 C10 C11 117.0(8) . . ? N6 C11 C12 122.0(7) . . ? N6 C11 C10 117.9(7) . . ? C12 C11 C10 120.1(7) . . ? N1 C12 C11 122.4(8) . . ? N1 C12 C7 119.0(7) . . ? C11 C12 C7 118.6(7) . . ? N7 C13 C14 121.7(9) . . ? N12 C14 C13 122.7(9) . . ? N11 C15 C16 120.9(11) . . ? N10 C16 C15 122.8(10) . . ? N9 C17 C18 123.1(9) . . ? N8 C18 C17 121.7(9) . . ? N7 C19 C20 120.9(8) . . ? N7 C19 C24 118.5(7) . . ? C20 C19 C24 120.6(8) . . ? C19 C20 N12 123.0(8) . . ? C19 C20 C21 119.0(8) . . ? N12 C20 C21 118.0(7) . . ? C22 C21 N11 121.1(7) . . ? C22 C21 C20 122.5(7) . . ? N11 C21 C20 116.4(7) . . ? N10 C22 C21 122.8(8) . . ? N10 C22 C23 118.3(7) . . ? C21 C22 C23 118.9(7) . . ? N9 C23 C24 120.7(8) . . ? N9 C23 C22 120.5(8) . . ? C24 C23 C22 118.8(7) . . ? N8 C24 C23 122.8(7) . . ? N8 C24 C19 117.2(7) . . ? C23 C24 C19 120.1(7) . . ? N13 C25 C26 120.4(9) . . ? N18 C26 C25 122.6(8) . . ? N17 C27 C28 120.6(8) . . ? N16 C28 C27 123.7(8) . . ? N15 C29 C30 122.7(8) . . ? N14 C30 C29 122.9(8) . . ? N13 C31 C32 121.7(7) . . ? N13 C31 C36 118.4(7) . . ? C32 C31 C36 119.8(7) . . ? N18 C32 C31 121.1(7) . . ? N18 C32 C33 117.7(7) . . ? C31 C32 C33 121.2(7) . . ? N17 C33 C34 122.5(7) . . ? N17 C33 C32 118.9(7) . . ? C34 C33 C32 118.6(7) . . ? N16 C34 C33 121.9(7) . . ? N16 C34 C35 117.4(7) . . ? C33 C34 C35 120.7(7) . . ? N15 C35 C36 121.0(7) . . ? N15 C35 C34 118.8(7) . . ? C36 C35 C34 120.2(7) . . ? N14 C36 C35 122.4(7) . . ? N14 C36 C31 118.1(7) . . ? C35 C36 C31 119.4(7) . . ? C2S C1S C6S 120.0 . . ? C3S C2S C1S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C6S C5S C4S 120.0 . . ? C5S C6S C1S 120.0 . . ? C8S C7S C12S 120.0 . . ? C9S C8S C7S 120.0 . . ? C8S C9S C10S 120.0 . . ? C11S C10S C9S 120.0 . . ? C12S C11S C10S 120.0 . . ? C11S C12S C7S 120.0 . . ? C14S C13S C18S 120.0 . . ? C15S C14S C13S 120.0 . . ? C14S C15S C16S 120.0 . . ? C15S C16S C17S 120.0 . . ? C18S C17S C16S 120.0 . . ? C17S C18S C13S 120.0 . . ? O2S N1S O1S 122.0 . . ? O2S N1S C19S 115.9 . . ? O1S N1S C19S 122.1 . . ? O4S N2S O3S 124(2) . . ? O4S N2S C20S 123(2) . . ? O3S N2S C20S 113.0(18) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.543 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.153