# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Rahul Banerjee' _publ_contact_author_email R.BANERJEE@NCL.RES.IN _publ_section_title ; Synthesis and Structural Comparisons of Five New Fluorinated Metal Organic Frameworks (F-MOFs) ; loop_ _publ_author_name 'Rahul Banerjee' 'Chandan Dey' 'Pradip Pachfule' 'Tamas Panda' # Attachment 'Rahul_submit_cif.txt' data_F-MOF1 _database_code_depnum_ccdc_archive 'CCDC 745103' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'F-MOF 1' _chemical_melting_point ? _chemical_formula_moiety 'C41 H25 Cu F6 N4 O4, C17 H10 F6 O4, C17 H9 F6 O4, C H O2, H2 O' _chemical_formula_sum 'C76 H47 Cu F18 N4 O15' _chemical_formula_weight 1661.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/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 19.358(5) _cell_length_b 13.756(4) _cell_length_c 26.012(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.951(4) _cell_angle_gamma 90.00 _cell_volume 6822(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8315 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.12 _exptl_crystal_description Cubic _exptl_crystal_colour Green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9486 _exptl_absorpt_correction_T_max 0.9653 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51721 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 26.02 _reflns_number_total 13429 _reflns_number_gt 11209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+6.1660P] 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 13429 _refine_ls_number_parameters 1026 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.10001(12) 0.32420(17) 0.85896(9) 0.0204(5) Uani 1 1 d . . . H1 H 0.1377 0.3684 0.8590 0.025 Uiso 1 1 calc R . . C2 C 0.07340(12) 0.27399(17) 0.81370(9) 0.0204(5) Uani 1 1 d . . . H2 H 0.0927 0.2845 0.7830 0.024 Uiso 1 1 calc R . . C3 C 0.01831(12) 0.20794(17) 0.81295(9) 0.0191(5) Uani 1 1 d . . . C4 C -0.01042(12) 0.19583(17) 0.85785(10) 0.0206(5) Uani 1 1 d . . . H4 H -0.0483 0.1519 0.8576 0.025 Uiso 1 1 calc R . . C5 C 0.01556(12) 0.24717(18) 0.90317(10) 0.0205(5) Uani 1 1 d . . . H5 H -0.0053 0.2389 0.9334 0.025 Uiso 1 1 calc R . . C6 C 0.07204(12) 0.31066(16) 0.90450(9) 0.0174(5) Uani 1 1 d . . . C7 C 0.10626(12) 0.36682(17) 0.95415(9) 0.0189(5) Uani 1 1 d . . . C8 C 0.18712(12) 0.35944(17) 0.96207(9) 0.0180(5) Uani 1 1 d . . . C9 C 0.23231(12) 0.43410(18) 0.98281(10) 0.0228(5) Uani 1 1 d . . . H9 H 0.2136 0.4953 0.9904 0.027 Uiso 1 1 calc R . . C10 C 0.30456(13) 0.41967(18) 0.99249(10) 0.0240(5) Uani 1 1 d . . . H10 H 0.3348 0.4710 1.0066 0.029 Uiso 1 1 calc R . . C11 C 0.33256(12) 0.33078(17) 0.98166(9) 0.0198(5) Uani 1 1 d . . . C12 C 0.28765(12) 0.25638(18) 0.96052(9) 0.0203(5) Uani 1 1 d . . . H12 H 0.3064 0.1955 0.9526 0.024 Uiso 1 1 calc R . . C13 C 0.21582(12) 0.27067(17) 0.95101(9) 0.0207(5) Uani 1 1 d . . . H13 H 0.1857 0.2193 0.9368 0.025 Uiso 1 1 calc R . . C14 C 0.41013(12) 0.31174(18) 0.99396(9) 0.0210(5) Uani 1 1 d . . . C15 C -0.00955(12) 0.15013(17) 0.76493(10) 0.0204(5) Uani 1 1 d . . . C16 C 0.08047(12) 0.47321(18) 0.94681(10) 0.0216(5) Uani 1 1 d . . . C17 C 0.08457(12) 0.32616(18) 1.00435(10) 0.0218(5) Uani 1 1 d . . . C18 C 0.63824(12) 0.60320(17) 0.43814(9) 0.0170(5) Uani 1 1 d . . . C19 C 0.73656(12) 0.70860(18) 0.41895(9) 0.0216(5) Uani 1 1 d . . . H19 H 0.7165 0.7014 0.3832 0.026 Uiso 1 1 calc R . . C20 C 0.70308(12) 0.66772(16) 0.45718(9) 0.0171(5) Uani 1 1 d . . . C21 C 0.73283(12) 0.68067(18) 0.50960(9) 0.0207(5) Uani 1 1 d . . . H21 H 0.7110 0.6527 0.5361 0.025 Uiso 1 1 calc R . . C22 C 0.79406(12) 0.73418(18) 0.52311(10) 0.0226(5) Uani 1 1 d . . . H22 H 0.8131 0.7440 0.5589 0.027 Uiso 1 1 calc R . . C23 C 0.82785(12) 0.77346(17) 0.48500(10) 0.0209(5) Uani 1 1 d . . . C24 C 0.79866(12) 0.75958(18) 0.43256(10) 0.0223(5) Uani 1 1 d . . . H24 H 0.8216 0.7853 0.4061 0.027 Uiso 1 1 calc R . . C25 C 0.89676(13) 0.82608(17) 0.49976(10) 0.0232(5) Uani 1 1 d . . . C26 C 0.56873(12) 0.74773(17) 0.39979(9) 0.0202(5) Uani 1 1 d . . . H26 H 0.5909 0.7828 0.4296 0.024 Uiso 1 1 calc R . . C27 C 0.51783(12) 0.79290(18) 0.36338(10) 0.0217(5) Uani 1 1 d . . . H27 H 0.5051 0.8583 0.3689 0.026 Uiso 1 1 calc R . . C28 C 0.48527(11) 0.74360(17) 0.31898(9) 0.0174(5) Uani 1 1 d . . . C29 C 0.50616(12) 0.64875(17) 0.31078(9) 0.0181(5) Uani 1 1 d . . . H29 H 0.4860 0.6152 0.2799 0.022 Uiso 1 1 calc R . . C30 C 0.55646(11) 0.60292(17) 0.34765(9) 0.0181(5) Uani 1 1 d . . . H30 H 0.5698 0.5379 0.3419 0.022 Uiso 1 1 calc R . . C31 C 0.58754(11) 0.65153(17) 0.39292(9) 0.0161(5) Uani 1 1 d . . . C32 C 0.42670(12) 0.79297(17) 0.28274(9) 0.0184(5) Uani 1 1 d . . . C33 C 0.66741(13) 0.50531(18) 0.42242(10) 0.0239(5) Uani 1 1 d . . . C34 C 0.59402(13) 0.5825(2) 0.48128(10) 0.0263(6) Uani 1 1 d . . . C35 C 0.88097(12) 1.03968(17) 0.32801(10) 0.0206(5) Uani 1 1 d . . . C36 C 0.83850(13) 0.98105(19) 0.35332(10) 0.0253(5) Uani 1 1 d . . . H36 H 0.8497 0.9717 0.3900 0.030 Uiso 1 1 calc R . . C37 C 0.77976(13) 0.93634(19) 0.32482(10) 0.0246(5) Uani 1 1 d . . . H37 H 0.7515 0.8955 0.3421 0.029 Uiso 1 1 calc R . . C38 C 0.76169(12) 0.95068(17) 0.27095(9) 0.0179(5) Uani 1 1 d . . . C39 C 0.80380(13) 1.01197(17) 0.24658(9) 0.0211(5) Uani 1 1 d . . . H39 H 0.7917 1.0241 0.2102 0.025 Uiso 1 1 calc R . . C40 C 0.86261(13) 1.05489(18) 0.27470(10) 0.0219(5) Uani 1 1 d . . . H40 H 0.8910 1.0955 0.2574 0.026 Uiso 1 1 calc R . . C41 C 0.63730(13) 1.05232(18) 0.20934(9) 0.0226(5) Uani 1 1 d . . . H41 H 0.6503 1.0718 0.2447 0.027 Uiso 1 1 calc R . . C42 C 0.59472(13) 1.11221(18) 0.17465(10) 0.0228(5) Uani 1 1 d . . . H42 H 0.5770 1.1708 0.1867 0.027 Uiso 1 1 calc R . . C43 C 0.57785(12) 1.08669(17) 0.12208(9) 0.0195(5) Uani 1 1 d . . . C44 C 0.60487(12) 1.00122(18) 0.10501(9) 0.0199(5) Uani 1 1 d . . . H44 H 0.5957 0.9851 0.0690 0.024 Uiso 1 1 calc R . . C45 C 0.64527(12) 0.93906(18) 0.14042(9) 0.0198(5) Uani 1 1 d . . . H45 H 0.6619 0.8796 0.1286 0.024 Uiso 1 1 calc R . . C46 C 0.66151(12) 0.96361(17) 0.19319(9) 0.0177(5) Uani 1 1 d . . . C47 C 0.70165(12) 0.89614(17) 0.23570(9) 0.0184(5) Uani 1 1 d . . . C48 C 0.64601(13) 0.85481(19) 0.26600(10) 0.0243(5) Uani 1 1 d . . . C49 C 0.73639(13) 0.80940(17) 0.21175(10) 0.0227(5) Uani 1 1 d . . . C50 C 0.52723(12) 1.14857(18) 0.08626(9) 0.0209(5) Uani 1 1 d . . . C51 C 0.94606(13) 1.08731(17) 0.35659(10) 0.0235(5) Uani 1 1 d . . . C52 C 0.19404(14) 0.9766(2) 0.19294(12) 0.0323(6) Uani 1 1 d . . . H52 H 0.1748 0.9488 0.2208 0.039 Uiso 1 1 calc R . . C53 C 0.27917(12) 0.97979(17) 0.14128(9) 0.0189(5) Uani 1 1 d . . . C54 C 0.24827(13) 1.05894(18) 0.11184(10) 0.0228(5) Uani 1 1 d . . . C55 C 0.18576(14) 1.0964(2) 0.12530(11) 0.0305(6) Uani 1 1 d . . . H55 H 0.1625 1.1497 0.1066 0.037 Uiso 1 1 calc R . . C56 C 0.28126(14) 1.09661(18) 0.07101(10) 0.0261(6) Uani 1 1 d . . . H56 H 0.2608 1.1503 0.0510 0.031 Uiso 1 1 calc R . . C57 C 0.34125(14) 1.05701(19) 0.06033(10) 0.0267(6) Uani 1 1 d . . . H57 H 0.3625 1.0840 0.0333 0.032 Uiso 1 1 calc R . . C58 C 0.37336(13) 0.97507(18) 0.08911(9) 0.0222(5) Uani 1 1 d . . . C59 C 0.34165(12) 0.93698(17) 0.12938(9) 0.0190(5) Uani 1 1 d . . . C60 C 0.42559(12) 0.81652(18) 0.14883(10) 0.0221(5) Uani 1 1 d . . . H60 H 0.4443 0.7626 0.1695 0.027 Uiso 1 1 calc R . . C61 C 0.46014(13) 0.84903(19) 0.10898(10) 0.0263(6) Uani 1 1 d . . . H61 H 0.5012 0.8168 0.1026 0.032 Uiso 1 1 calc R . . C62 C 0.43428(13) 0.92784(19) 0.07917(10) 0.0256(5) Uani 1 1 d . . . H62 H 0.4574 0.9503 0.0520 0.031 Uiso 1 1 calc R . . C63 C 0.21640(14) 0.66328(18) 0.13751(10) 0.0255(5) Uani 1 1 d . . . H63 H 0.2454 0.6750 0.1122 0.031 Uiso 1 1 calc R . . C64 C 0.16105(14) 0.59686(19) 0.12547(10) 0.0288(6) Uani 1 1 d . . . H64 H 0.1525 0.5658 0.0924 0.035 Uiso 1 1 calc R . . C65 C 0.11949(14) 0.57695(18) 0.16150(10) 0.0261(6) Uani 1 1 d . . . H65 H 0.0820 0.5317 0.1538 0.031 Uiso 1 1 calc R . . C66 C 0.13278(12) 0.62436(17) 0.21026(10) 0.0217(5) Uani 1 1 d . . . C67 C 0.18850(12) 0.69206(17) 0.21860(9) 0.0178(5) Uani 1 1 d . . . C68 C 0.09171(13) 0.60848(18) 0.25064(10) 0.0255(5) Uani 1 1 d . . . H68 H 0.0550 0.5617 0.2454 0.031 Uiso 1 1 calc R . . C69 C 0.10442(13) 0.65894(18) 0.29588(11) 0.0252(5) Uani 1 1 d . . . H69 H 0.0763 0.6474 0.3218 0.030 Uiso 1 1 calc R . . C70 C 0.15988(12) 0.72986(18) 0.30537(10) 0.0216(5) Uani 1 1 d . . . C71 C 0.20218(12) 0.74525(17) 0.26718(9) 0.0186(5) Uani 1 1 d . . . C72 C 0.26831(13) 0.86163(19) 0.31816(10) 0.0255(5) Uani 1 1 d . . . H72 H 0.3059 0.9070 0.3230 0.031 Uiso 1 1 calc R . . C73 C 0.22837(14) 0.8511(2) 0.35782(10) 0.0289(6) Uani 1 1 d . . . H73 H 0.2386 0.8889 0.3888 0.035 Uiso 1 1 calc R . . C74 C 0.17418(14) 0.78540(19) 0.35130(10) 0.0264(5) Uani 1 1 d . . . H74 H 0.1464 0.7775 0.3778 0.032 Uiso 1 1 calc R . . C75 C 0.15921(15) 1.0552(2) 0.16541(12) 0.0367(7) Uani 1 1 d . . . H75 H 0.1172 1.0798 0.1747 0.044 Uiso 1 1 calc R . . C78 C 0.3670(7) 0.5725(10) 0.1480(4) 0.237(6) Uiso 1 1 d D . . H78 H 0.3826 0.6371 0.1440 0.285 Uiso 1 1 calc R . . Cu1 Cu 0.311107(14) 0.82512(2) 0.214580(11) 0.01770(9) Uani 1 1 d . . . F1 F 0.66934(8) 0.77894(11) 0.29642(6) 0.0309(4) Uani 1 1 d . . . F2 F 0.58860(8) 0.82404(12) 0.23349(6) 0.0308(4) Uani 1 1 d . . . F3 F 0.62465(8) 0.92226(12) 0.29689(6) 0.0299(3) Uani 1 1 d . . . F4 F 0.68956(8) 0.74723(10) 0.18572(6) 0.0293(3) Uani 1 1 d . . . F5 F 0.77772(8) 0.75766(11) 0.24862(6) 0.0304(3) Uani 1 1 d . . . F6 F 0.77697(7) 0.83969(10) 0.17827(6) 0.0245(3) Uani 1 1 d . . . F7 F 0.62592(8) 0.52210(12) 0.51857(6) 0.0350(4) Uani 1 1 d . . . F8 F 0.58038(8) 0.66460(13) 0.50537(6) 0.0345(4) Uani 1 1 d . . . F9 F 0.71852(8) 0.47121(10) 0.45945(6) 0.0299(3) Uani 1 1 d . . . F10 F 0.69502(8) 0.51407(11) 0.37899(6) 0.0291(3) Uani 1 1 d . . . F11 F 0.10974(7) 0.51834(10) 0.91048(6) 0.0255(3) Uani 1 1 d . . . F12 F 0.01079(7) 0.47804(10) 0.93131(6) 0.0261(3) Uani 1 1 d . . . F13 F 0.09517(7) 0.52666(10) 0.99072(6) 0.0268(3) Uani 1 1 d . . . F14 F 0.12144(8) 0.36681(12) 1.04769(6) 0.0302(3) Uani 1 1 d . . . F15 F 0.09621(7) 0.23039(11) 1.00887(6) 0.0264(3) Uani 1 1 d . . . F16 F 0.01654(7) 0.34070(11) 1.00655(6) 0.0260(3) Uani 1 1 d . . . F17 F 0.53252(8) 0.54242(14) 0.46128(6) 0.0395(4) Uani 1 1 d . . . F18 F 0.61801(8) 0.43564(11) 0.41340(7) 0.0352(4) Uani 1 1 d . . . N1 N 0.36739(10) 0.85870(15) 0.15874(8) 0.0190(4) Uani 1 1 d . . . N2 N 0.25276(10) 0.93957(15) 0.18153(8) 0.0223(4) Uani 1 1 d . . . N3 N 0.23027(10) 0.71071(15) 0.18277(8) 0.0210(4) Uani 1 1 d . . . N4 N 0.25592(10) 0.81074(14) 0.27372(8) 0.0201(4) Uani 1 1 d . . . O1 O 0.98741(10) 1.12869(15) 0.33391(8) 0.0363(5) Uani 1 1 d . . . O2 O 0.95388(9) 1.07920(14) 0.40787(7) 0.0298(4) Uani 1 1 d . . . H2A H 0.9904 1.1086 0.4217 0.045 Uiso 1 1 calc R . . O3 O 0.92656(9) 0.84791(14) 0.46122(7) 0.0283(4) Uani 1 1 d . . . H3A H 0.9681 0.8652 0.4723 0.043 Uiso 1 1 calc R . . O4 O 0.92063(9) 0.84243(13) 0.54651(7) 0.0291(4) Uani 1 1 d . . . O5 O 0.38635(8) 0.73806(12) 0.24984(6) 0.0202(3) Uani 1 1 d . . . O6 O 0.41735(9) 0.88136(12) 0.28619(7) 0.0244(4) Uani 1 1 d . . . O7 O 0.52627(9) 1.13039(13) 0.03623(6) 0.0236(4) Uani 1 1 d . . . H7A H 0.4978 1.1680 0.0181 0.035 Uiso 1 1 calc R . . O8 O 0.48941(10) 1.20766(13) 0.10241(7) 0.0280(4) Uani 1 1 d . . . O9 O 0.02039(10) 0.17104(13) 0.72481(7) 0.0266(4) Uani 1 1 d . . . H9A H 0.0016 0.1384 0.6988 0.040 Uiso 1 1 calc R . . O10 O -0.05595(10) 0.08963(14) 0.76445(7) 0.0299(4) Uani 1 1 d . . . O11 O 0.44681(9) 0.37897(13) 1.01966(7) 0.0256(4) Uani 1 1 d . . . O12 O 0.43300(9) 0.23359(13) 0.97940(7) 0.0236(4) Uani 1 1 d . . . O13 O 0.96814(12) 0.09540(15) 0.63753(7) 0.0381(5) Uani 1 1 d D . . H13A H 0.9647 0.1004 0.6008 0.046 Uiso 1 1 d D . . H13B H 0.9333 0.0530 0.6291 0.046 Uiso 1 1 d D . . O14 O 0.35887(13) 0.55310(18) 0.20810(9) 0.0501(6) Uani 1 1 d D . . O15 O 0.35894(14) 0.5281(2) 0.10428(10) 0.0591(7) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0169(11) 0.0201(12) 0.0232(12) 0.0028(10) 0.0004(9) -0.0020(9) C2 0.0199(12) 0.0216(12) 0.0196(12) 0.0026(10) 0.0034(9) 0.0002(9) C3 0.0179(11) 0.0163(11) 0.0222(12) 0.0010(9) 0.0004(9) 0.0029(9) C4 0.0157(11) 0.0194(12) 0.0260(12) 0.0021(10) 0.0017(9) -0.0022(9) C5 0.0174(11) 0.0218(12) 0.0227(12) 0.0018(10) 0.0047(9) 0.0014(9) C6 0.0147(11) 0.0158(11) 0.0204(11) 0.0005(9) -0.0006(9) 0.0038(9) C7 0.0166(11) 0.0184(12) 0.0210(12) 0.0003(9) 0.0016(9) 0.0009(9) C8 0.0170(11) 0.0183(11) 0.0178(11) 0.0038(9) 0.0004(9) 0.0020(9) C9 0.0194(12) 0.0203(12) 0.0271(13) -0.0024(10) -0.0001(10) 0.0036(9) C10 0.0194(12) 0.0212(13) 0.0296(13) -0.0018(10) -0.0011(10) -0.0015(10) C11 0.0164(11) 0.0228(12) 0.0192(12) 0.0057(9) 0.0005(9) 0.0027(9) C12 0.0200(12) 0.0188(12) 0.0216(12) 0.0025(9) 0.0020(9) 0.0055(9) C13 0.0201(12) 0.0175(12) 0.0228(12) 0.0006(9) -0.0006(9) -0.0002(9) C14 0.0181(12) 0.0251(13) 0.0188(12) 0.0057(10) 0.0002(9) 0.0023(10) C15 0.0198(12) 0.0185(12) 0.0224(12) 0.0004(10) 0.0027(9) 0.0015(9) C16 0.0160(11) 0.0230(13) 0.0244(12) -0.0020(10) -0.0008(9) 0.0026(9) C17 0.0176(12) 0.0263(13) 0.0203(12) -0.0020(10) -0.0001(9) 0.0007(10) C18 0.0157(11) 0.0182(11) 0.0162(11) 0.0017(9) 0.0001(9) -0.0002(9) C19 0.0188(12) 0.0258(13) 0.0181(11) 0.0043(10) -0.0026(9) -0.0011(10) C20 0.0139(11) 0.0154(11) 0.0209(12) 0.0011(9) 0.0002(9) 0.0014(8) C21 0.0195(12) 0.0239(13) 0.0188(12) 0.0005(10) 0.0036(9) 0.0008(9) C22 0.0194(12) 0.0250(13) 0.0209(12) -0.0035(10) -0.0031(9) 0.0023(10) C23 0.0161(11) 0.0182(12) 0.0264(13) 0.0022(10) -0.0022(9) 0.0021(9) C24 0.0179(12) 0.0246(13) 0.0233(12) 0.0072(10) 0.0003(9) -0.0017(9) C25 0.0185(12) 0.0184(12) 0.0302(14) 0.0014(10) -0.0027(10) 0.0023(9) C26 0.0180(12) 0.0207(12) 0.0204(12) -0.0022(10) -0.0008(9) -0.0010(9) C27 0.0179(12) 0.0167(12) 0.0290(13) -0.0016(10) -0.0004(10) 0.0013(9) C28 0.0124(11) 0.0175(11) 0.0215(12) 0.0030(9) 0.0010(9) -0.0014(8) C29 0.0162(11) 0.0189(12) 0.0184(11) -0.0014(9) 0.0008(9) -0.0016(9) C30 0.0150(11) 0.0160(11) 0.0227(12) -0.0005(9) 0.0015(9) 0.0002(9) C31 0.0107(10) 0.0183(11) 0.0190(11) 0.0036(9) 0.0020(8) -0.0017(8) C32 0.0142(11) 0.0187(12) 0.0220(12) 0.0023(9) 0.0019(9) -0.0004(9) C33 0.0217(12) 0.0190(12) 0.0270(13) 0.0023(10) -0.0073(10) 0.0004(10) C34 0.0186(12) 0.0362(15) 0.0227(13) 0.0060(11) 0.0000(10) -0.0052(10) C35 0.0189(12) 0.0164(12) 0.0245(12) -0.0018(9) -0.0017(9) -0.0001(9) C36 0.0255(13) 0.0276(14) 0.0196(12) 0.0041(10) -0.0048(10) -0.0032(10) C37 0.0231(12) 0.0254(13) 0.0233(13) 0.0054(10) -0.0011(10) -0.0057(10) C38 0.0158(11) 0.0163(11) 0.0199(11) -0.0002(9) -0.0020(9) -0.0004(9) C39 0.0231(12) 0.0199(12) 0.0193(12) 0.0014(9) 0.0008(9) -0.0014(9) C40 0.0209(12) 0.0186(12) 0.0262(13) 0.0012(10) 0.0044(10) -0.0018(9) C41 0.0255(13) 0.0229(13) 0.0177(12) -0.0023(10) -0.0007(10) 0.0014(10) C42 0.0250(12) 0.0193(12) 0.0228(12) -0.0033(10) 0.0007(10) 0.0029(10) C43 0.0175(11) 0.0210(12) 0.0193(12) 0.0024(9) 0.0016(9) 0.0006(9) C44 0.0189(11) 0.0245(13) 0.0155(11) -0.0011(9) 0.0008(9) 0.0019(9) C45 0.0190(11) 0.0201(12) 0.0199(12) -0.0019(9) 0.0020(9) 0.0003(9) C46 0.0141(11) 0.0190(12) 0.0188(11) 0.0021(9) -0.0005(9) -0.0029(9) C47 0.0175(11) 0.0182(12) 0.0180(11) 0.0012(9) -0.0011(9) -0.0013(9) C48 0.0230(13) 0.0269(13) 0.0209(12) 0.0028(10) -0.0023(10) -0.0072(10) C49 0.0245(13) 0.0159(12) 0.0249(13) 0.0020(10) -0.0035(10) 0.0000(9) C50 0.0197(12) 0.0205(12) 0.0213(12) 0.0012(10) 0.0002(9) 0.0013(9) C51 0.0216(12) 0.0160(12) 0.0307(14) -0.0020(10) -0.0018(10) -0.0005(9) C52 0.0219(13) 0.0326(15) 0.0438(16) 0.0080(13) 0.0097(12) 0.0085(11) C53 0.0158(11) 0.0185(12) 0.0205(12) -0.0019(9) -0.0023(9) -0.0012(9) C54 0.0236(12) 0.0177(12) 0.0238(12) -0.0022(10) -0.0056(10) 0.0005(9) C55 0.0265(14) 0.0231(13) 0.0378(15) 0.0029(11) -0.0055(11) 0.0079(11) C56 0.0347(14) 0.0193(12) 0.0200(12) 0.0020(10) -0.0070(10) 0.0014(10) C57 0.0331(14) 0.0260(13) 0.0187(12) 0.0010(10) -0.0014(10) -0.0045(11) C58 0.0239(12) 0.0225(13) 0.0188(12) -0.0036(10) 0.0000(9) -0.0050(10) C59 0.0176(11) 0.0173(12) 0.0198(12) -0.0037(9) -0.0033(9) -0.0017(9) C60 0.0172(12) 0.0224(12) 0.0254(13) -0.0031(10) 0.0000(9) 0.0019(9) C61 0.0206(12) 0.0299(14) 0.0286(14) -0.0062(11) 0.0046(10) 0.0003(10) C62 0.0259(13) 0.0303(14) 0.0212(12) -0.0046(11) 0.0056(10) -0.0051(11) C63 0.0310(14) 0.0255(13) 0.0194(12) 0.0008(10) 0.0025(10) 0.0016(10) C64 0.0371(15) 0.0237(13) 0.0221(13) -0.0027(10) -0.0045(11) 0.0005(11) C65 0.0255(13) 0.0173(12) 0.0312(14) 0.0017(10) -0.0074(11) -0.0022(10) C66 0.0187(12) 0.0165(12) 0.0269(13) 0.0046(10) -0.0043(10) 0.0032(9) C67 0.0148(11) 0.0166(11) 0.0205(11) 0.0038(9) -0.0015(9) 0.0040(9) C68 0.0186(12) 0.0212(13) 0.0354(14) 0.0087(11) 0.0012(10) -0.0012(10) C69 0.0201(12) 0.0255(13) 0.0309(14) 0.0100(11) 0.0068(10) 0.0033(10) C70 0.0183(12) 0.0220(12) 0.0237(12) 0.0067(10) 0.0014(9) 0.0074(9) C71 0.0154(11) 0.0178(12) 0.0215(12) 0.0043(9) -0.0002(9) 0.0041(9) C72 0.0231(13) 0.0252(13) 0.0263(13) -0.0046(11) -0.0009(10) -0.0005(10) C73 0.0303(14) 0.0308(14) 0.0242(13) -0.0037(11) 0.0003(11) 0.0074(11) C74 0.0276(13) 0.0283(14) 0.0241(13) 0.0044(11) 0.0069(10) 0.0097(11) C75 0.0237(14) 0.0369(16) 0.0498(18) 0.0068(14) 0.0070(13) 0.0135(12) Cu1 0.01324(15) 0.01779(16) 0.02121(16) 0.00174(11) 0.00054(11) 0.00149(10) F1 0.0326(8) 0.0310(8) 0.0263(8) 0.0113(7) -0.0032(6) -0.0103(7) F2 0.0221(8) 0.0411(9) 0.0265(8) 0.0049(7) -0.0031(6) -0.0135(7) F3 0.0254(8) 0.0405(9) 0.0247(8) 0.0002(7) 0.0066(6) -0.0053(7) F4 0.0341(8) 0.0177(7) 0.0327(8) -0.0022(6) -0.0038(6) -0.0053(6) F5 0.0343(8) 0.0221(8) 0.0311(8) 0.0067(6) -0.0050(7) 0.0072(6) F6 0.0234(7) 0.0220(7) 0.0280(8) 0.0003(6) 0.0037(6) 0.0039(6) F7 0.0313(8) 0.0458(10) 0.0261(8) 0.0173(7) 0.0000(6) -0.0072(7) F8 0.0264(8) 0.0543(11) 0.0247(8) 0.0004(7) 0.0099(6) 0.0066(7) F9 0.0314(8) 0.0207(8) 0.0313(8) 0.0023(6) -0.0127(6) 0.0059(6) F10 0.0281(8) 0.0312(8) 0.0261(8) -0.0066(6) -0.0009(6) 0.0105(6) F11 0.0260(7) 0.0186(7) 0.0309(8) 0.0037(6) 0.0024(6) 0.0028(6) F12 0.0160(7) 0.0266(8) 0.0332(8) -0.0034(6) -0.0024(6) 0.0060(6) F13 0.0235(7) 0.0249(8) 0.0299(8) -0.0097(6) -0.0013(6) 0.0057(6) F14 0.0270(8) 0.0424(9) 0.0197(7) -0.0029(7) 0.0003(6) -0.0037(7) F15 0.0264(8) 0.0260(8) 0.0267(8) 0.0077(6) 0.0045(6) 0.0020(6) F16 0.0190(7) 0.0346(8) 0.0255(8) -0.0019(6) 0.0065(6) 0.0011(6) F17 0.0213(8) 0.0624(12) 0.0332(9) 0.0155(8) 0.0002(6) -0.0170(7) F18 0.0348(9) 0.0166(7) 0.0468(10) 0.0041(7) -0.0142(7) -0.0049(6) N1 0.0148(9) 0.0194(10) 0.0216(10) -0.0013(8) 0.0000(8) 0.0002(8) N2 0.0153(10) 0.0223(11) 0.0284(11) 0.0014(9) 0.0009(8) 0.0019(8) N3 0.0205(10) 0.0208(10) 0.0209(10) 0.0014(8) 0.0013(8) 0.0013(8) N4 0.0175(10) 0.0195(10) 0.0218(10) -0.0011(8) -0.0007(8) 0.0015(8) O1 0.0288(10) 0.0360(11) 0.0404(11) 0.0040(9) -0.0042(9) -0.0154(9) O2 0.0214(9) 0.0362(11) 0.0286(10) -0.0092(8) -0.0048(7) -0.0072(8) O3 0.0155(8) 0.0306(10) 0.0360(11) 0.0054(8) -0.0036(7) -0.0062(7) O4 0.0219(9) 0.0292(10) 0.0330(10) -0.0034(8) -0.0048(8) -0.0049(7) O5 0.0169(8) 0.0189(8) 0.0222(8) 0.0011(7) -0.0036(6) 0.0002(6) O6 0.0211(9) 0.0175(9) 0.0322(10) 0.0019(7) -0.0027(7) 0.0030(7) O7 0.0255(9) 0.0256(9) 0.0182(8) 0.0016(7) -0.0007(7) 0.0093(7) O8 0.0310(10) 0.0282(10) 0.0242(9) 0.0003(8) 0.0030(8) 0.0114(8) O9 0.0311(10) 0.0272(10) 0.0224(9) -0.0057(7) 0.0072(8) -0.0073(7) O10 0.0321(10) 0.0309(10) 0.0265(10) -0.0044(8) 0.0047(8) -0.0125(8) O11 0.0169(8) 0.0281(10) 0.0298(10) -0.0005(8) -0.0015(7) 0.0018(7) O12 0.0182(8) 0.0270(9) 0.0244(9) 0.0021(7) 0.0004(7) 0.0065(7) O13 0.0578(13) 0.0323(11) 0.0223(10) -0.0036(8) 0.0017(9) 0.0059(10) O14 0.0559(15) 0.0500(14) 0.0426(13) -0.0002(11) 0.0032(11) -0.0006(11) O15 0.0610(16) 0.0642(17) 0.0509(15) 0.0025(13) 0.0063(12) -0.0042(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.385(3) . ? C1 C6 1.398(3) . ? C1 H1 0.9500 . ? C2 C3 1.399(3) . ? C2 H2 0.9500 . ? C3 C4 1.388(3) . ? C3 C15 1.500(3) . ? C4 C5 1.392(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.552(3) . ? C7 C17 1.544(3) . ? C7 C8 1.546(3) . ? C7 C16 1.547(3) . ? C8 C13 1.392(3) . ? C8 C9 1.396(3) . ? C9 C10 1.392(3) . ? C9 H9 0.9500 . ? C10 C11 1.386(3) . ? C10 H10 0.9500 . ? C11 C12 1.393(3) . ? C11 C14 1.503(3) . ? C12 C13 1.384(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O12 1.246(3) . ? C14 O11 1.281(3) . ? C15 O10 1.223(3) . ? C15 O9 1.310(3) . ? C16 F11 1.336(3) . ? C16 F12 1.341(3) . ? C16 F13 1.347(3) . ? C17 F15 1.338(3) . ? C17 F16 1.343(3) . ? C17 F14 1.347(3) . ? C18 C33 1.543(3) . ? C18 C31 1.546(3) . ? C18 C20 1.547(3) . ? C18 C34 1.551(3) . ? C19 C24 1.384(3) . ? C19 C20 1.396(3) . ? C19 H19 0.9500 . ? C20 C21 1.397(3) . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C24 1.396(3) . ? C23 C25 1.508(3) . ? C24 H24 0.9500 . ? C25 O4 1.244(3) . ? C25 O3 1.276(3) . ? C26 C27 1.390(3) . ? C26 C31 1.392(3) . ? C26 H26 0.9500 . ? C27 C28 1.393(3) . ? C27 H27 0.9500 . ? C28 C29 1.393(3) . ? C28 C32 1.505(3) . ? C29 C30 1.394(3) . ? C29 H29 0.9500 . ? C30 C31 1.397(3) . ? C30 H30 0.9500 . ? C32 O6 1.235(3) . ? C32 O5 1.297(3) . ? C33 F10 1.336(3) . ? C33 F9 1.341(3) . ? C33 F18 1.346(3) . ? C34 F17 1.333(3) . ? C34 F8 1.340(3) . ? C34 F7 1.343(3) . ? C35 C40 1.387(3) . ? C35 C36 1.395(4) . ? C35 C51 1.499(3) . ? C36 C37 1.389(3) . ? C36 H36 0.9500 . ? C37 C38 1.399(3) . ? C37 H37 0.9500 . ? C38 C39 1.398(3) . ? C38 C47 1.545(3) . ? C39 C40 1.375(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.384(3) . ? C41 C46 1.398(3) . ? C41 H41 0.9500 . ? C42 C43 1.395(3) . ? C42 H42 0.9500 . ? C43 C44 1.390(3) . ? C43 C50 1.496(3) . ? C44 C45 1.394(3) . ? C44 H44 0.9500 . ? C45 C46 1.396(3) . ? C45 H45 0.9500 . ? C46 C47 1.546(3) . ? C47 C48 1.549(3) . ? C47 C49 1.552(3) . ? C48 F3 1.339(3) . ? C48 F1 1.340(3) . ? C48 F2 1.343(3) . ? C49 F6 1.336(3) . ? C49 F4 1.342(3) . ? C49 F5 1.342(3) . ? C50 O8 1.216(3) . ? C50 O7 1.322(3) . ? C51 O1 1.215(3) . ? C51 O2 1.321(3) . ? C52 N2 1.325(3) . ? C52 C75 1.404(4) . ? C52 H52 0.9500 . ? C53 N2 1.360(3) . ? C53 C54 1.404(3) . ? C53 C59 1.426(3) . ? C54 C55 1.414(4) . ? C54 C56 1.428(4) . ? C55 C75 1.363(4) . ? C55 H55 0.9500 . ? C56 C57 1.354(4) . ? C56 H56 0.9500 . ? C57 C58 1.434(4) . ? C57 H57 0.9500 . ? C58 C59 1.404(3) . ? C58 C62 1.409(4) . ? C59 N1 1.364(3) . ? C60 N1 1.331(3) . ? C60 C61 1.401(4) . ? C60 H60 0.9500 . ? C61 C62 1.376(4) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 N3 1.332(3) . ? C63 C64 1.402(4) . ? C63 H63 0.9500 . ? C64 C65 1.364(4) . ? C64 H64 0.9500 . ? C65 C66 1.410(4) . ? C65 H65 0.9500 . ? C66 C67 1.413(3) . ? C66 C68 1.439(4) . ? C67 N3 1.360(3) . ? C67 C71 1.445(3) . ? C68 C69 1.352(4) . ? C68 H68 0.9500 . ? C69 C70 1.440(4) . ? C69 H69 0.9500 . ? C70 C74 1.405(4) . ? C70 C71 1.408(3) . ? C71 N4 1.364(3) . ? C72 N4 1.337(3) . ? C72 C73 1.400(4) . ? C72 H72 0.9500 . ? C73 C74 1.373(4) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C78 O15 1.276(11) . ? C78 O14 1.621(11) . ? C78 H78 0.9500 . ? Cu1 O5 1.9837(16) . ? Cu1 N1 2.014(2) . ? Cu1 N4 2.029(2) . ? Cu1 N2 2.039(2) . ? Cu1 N3 2.272(2) . ? O2 H2A 0.8400 . ? O3 H3A 0.8400 . ? O7 H7A 0.8400 . ? O9 H9A 0.8400 . ? O13 H13A 0.9482 . ? O13 H13B 0.8895 . ? 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 C2 C1 C6 120.8(2) . . ? C2 C1 H1 119.6 . . ? C6 C1 H1 119.6 . . ? C1 C2 C3 120.4(2) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 118.8(2) . . ? C4 C3 C15 119.9(2) . . ? C2 C3 C15 121.3(2) . . ? C3 C4 C5 120.9(2) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 120.4(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 118.6(2) . . ? C5 C6 C7 123.5(2) . . ? C1 C6 C7 117.8(2) . . ? C17 C7 C8 106.29(18) . . ? C17 C7 C16 108.53(19) . . ? C8 C7 C16 112.10(19) . . ? C17 C7 C6 112.59(19) . . ? C8 C7 C6 110.79(19) . . ? C16 C7 C6 106.62(18) . . ? C13 C8 C9 118.6(2) . . ? C13 C8 C7 117.5(2) . . ? C9 C8 C7 123.8(2) . . ? C10 C9 C8 120.5(2) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.3(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 119.3(2) . . ? C10 C11 C14 121.5(2) . . ? C12 C11 C14 119.2(2) . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 120.8(2) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? O12 C14 O11 126.0(2) . . ? O12 C14 C11 118.7(2) . . ? O11 C14 C11 115.4(2) . . ? O10 C15 O9 124.5(2) . . ? O10 C15 C3 121.8(2) . . ? O9 C15 C3 113.7(2) . . ? F11 C16 F12 106.97(19) . . ? F11 C16 F13 107.03(19) . . ? F12 C16 F13 106.38(19) . . ? F11 C16 C7 111.07(19) . . ? F12 C16 C7 111.73(19) . . ? F13 C16 C7 113.29(19) . . ? F15 C17 F16 107.11(19) . . ? F15 C17 F14 106.15(19) . . ? F16 C17 F14 106.51(19) . . ? F15 C17 C7 111.4(2) . . ? F16 C17 C7 113.21(19) . . ? F14 C17 C7 112.0(2) . . ? C33 C18 C31 112.77(19) . . ? C33 C18 C20 105.77(18) . . ? C31 C18 C20 111.73(18) . . ? C33 C18 C34 107.7(2) . . ? C31 C18 C34 105.81(18) . . ? C20 C18 C34 113.11(19) . . ? C24 C19 C20 120.8(2) . . ? C24 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 118.7(2) . . ? C19 C20 C18 117.0(2) . . ? C21 C20 C18 124.1(2) . . ? C22 C21 C20 120.3(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.9(2) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C24 118.9(2) . . ? C22 C23 C25 120.7(2) . . ? C24 C23 C25 120.3(2) . . ? C19 C24 C23 120.4(2) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? O4 C25 O3 125.7(2) . . ? O4 C25 C23 119.9(2) . . ? O3 C25 C23 114.4(2) . . ? C27 C26 C31 120.5(2) . . ? C27 C26 H26 119.7 . . ? C31 C26 H26 119.7 . . ? C26 C27 C28 120.9(2) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C29 118.8(2) . . ? C27 C28 C32 118.9(2) . . ? C29 C28 C32 122.3(2) . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C31 120.8(2) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C26 C31 C30 118.6(2) . . ? C26 C31 C18 117.2(2) . . ? C30 C31 C18 124.1(2) . . ? O6 C32 O5 122.8(2) . . ? O6 C32 C28 120.2(2) . . ? O5 C32 C28 116.9(2) . . ? F10 C33 F9 106.6(2) . . ? F10 C33 F18 107.0(2) . . ? F9 C33 F18 106.87(19) . . ? F10 C33 C18 111.3(2) . . ? F9 C33 C18 111.9(2) . . ? F18 C33 C18 112.7(2) . . ? F17 C34 F8 107.2(2) . . ? F17 C34 F7 107.1(2) . . ? F8 C34 F7 106.6(2) . . ? F17 C34 C18 111.2(2) . . ? F8 C34 C18 111.2(2) . . ? F7 C34 C18 113.2(2) . . ? C40 C35 C36 119.3(2) . . ? C40 C35 C51 118.6(2) . . ? C36 C35 C51 122.2(2) . . ? C37 C36 C35 119.9(2) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 120.8(2) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C39 C38 C37 118.3(2) . . ? C39 C38 C47 117.5(2) . . ? C37 C38 C47 124.0(2) . . ? C40 C39 C38 120.8(2) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C35 120.8(2) . . ? C39 C40 H40 119.6 . . ? C35 C40 H40 119.6 . . ? C42 C41 C46 121.1(2) . . ? C42 C41 H41 119.5 . . ? C46 C41 H41 119.5 . . ? C41 C42 C43 120.1(2) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.3(2) . . ? C44 C43 C50 121.6(2) . . ? C42 C43 C50 119.0(2) . . ? C43 C44 C45 120.5(2) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C46 120.5(2) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C41 118.5(2) . . ? C45 C46 C47 123.9(2) . . ? C41 C46 C47 117.5(2) . . ? C38 C47 C46 111.50(19) . . ? C38 C47 C48 113.22(19) . . ? C46 C47 C48 106.05(18) . . ? C38 C47 C49 106.14(18) . . ? C46 C47 C49 111.93(19) . . ? C48 C47 C49 108.0(2) . . ? F3 C48 F1 107.0(2) . . ? F3 C48 F2 106.8(2) . . ? F1 C48 F2 106.5(2) . . ? F3 C48 C47 111.4(2) . . ? F1 C48 C47 113.2(2) . . ? F2 C48 C47 111.6(2) . . ? F6 C49 F4 107.0(2) . . ? F6 C49 F5 106.6(2) . . ? F4 C49 F5 106.86(19) . . ? F6 C49 C47 111.48(19) . . ? F4 C49 C47 113.0(2) . . ? F5 C49 C47 111.5(2) . . ? O8 C50 O7 124.0(2) . . ? O8 C50 C43 122.3(2) . . ? O7 C50 C43 113.7(2) . . ? O1 C51 O2 124.0(2) . . ? O1 C51 C35 122.1(2) . . ? O2 C51 C35 113.8(2) . . ? N2 C52 C75 122.5(3) . . ? N2 C52 H52 118.8 . . ? C75 C52 H52 118.8 . . ? N2 C53 C54 123.7(2) . . ? N2 C53 C59 116.4(2) . . ? C54 C53 C59 119.9(2) . . ? C53 C54 C55 116.7(2) . . ? C53 C54 C56 118.9(2) . . ? C55 C54 C56 124.3(2) . . ? C75 C55 C54 119.4(2) . . ? C75 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C57 C56 C54 121.1(2) . . ? C57 C56 H56 119.5 . . ? C54 C56 H56 119.5 . . ? C56 C57 C58 121.2(2) . . ? C56 C57 H57 119.4 . . ? C58 C57 H57 119.4 . . ? C59 C58 C62 116.9(2) . . ? C59 C58 C57 118.5(2) . . ? C62 C58 C57 124.6(2) . . ? N1 C59 C58 123.2(2) . . ? N1 C59 C53 116.5(2) . . ? C58 C59 C53 120.3(2) . . ? N1 C60 C61 122.2(2) . . ? N1 C60 H60 118.9 . . ? C61 C60 H60 118.9 . . ? C62 C61 C60 119.7(2) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? C61 C62 C58 119.6(2) . . ? C61 C62 H62 120.2 . . ? C58 C62 H62 120.2 . . ? N3 C63 C64 123.1(2) . . ? N3 C63 H63 118.4 . . ? C64 C63 H63 118.4 . . ? C65 C64 C63 119.8(2) . . ? C65 C64 H64 120.1 . . ? C63 C64 H64 120.1 . . ? C64 C65 C66 119.2(2) . . ? C64 C65 H65 120.4 . . ? C66 C65 H65 120.4 . . ? C65 C66 C67 117.3(2) . . ? C65 C66 C68 123.3(2) . . ? C67 C66 C68 119.4(2) . . ? N3 C67 C66 123.2(2) . . ? N3 C67 C71 117.6(2) . . ? C66 C67 C71 119.2(2) . . ? C69 C68 C66 121.1(2) . . ? C69 C68 H68 119.4 . . ? C66 C68 H68 119.4 . . ? C68 C69 C70 121.0(2) . . ? C68 C69 H69 119.5 . . ? C70 C69 H69 119.5 . . ? C74 C70 C71 117.7(2) . . ? C74 C70 C69 123.1(2) . . ? C71 C70 C69 119.2(2) . . ? N4 C71 C70 122.4(2) . . ? N4 C71 C67 117.7(2) . . ? C70 C71 C67 120.0(2) . . ? N4 C72 C73 122.9(2) . . ? N4 C72 H72 118.5 . . ? C73 C72 H72 118.5 . . ? C74 C73 C72 119.0(2) . . ? C74 C73 H73 120.5 . . ? C72 C73 H73 120.5 . . ? C73 C74 C70 119.8(2) . . ? C73 C74 H74 120.1 . . ? C70 C74 H74 120.1 . . ? C55 C75 C52 119.9(3) . . ? C55 C75 H75 120.0 . . ? C52 C75 H75 120.0 . . ? O15 C78 O14 139.7(11) . . ? O15 C78 H78 110.1 . . ? O14 C78 H78 110.1 . . ? O5 Cu1 N1 91.51(8) . . ? O5 Cu1 N4 91.79(8) . . ? N1 Cu1 N4 172.14(8) . . ? O5 Cu1 N2 165.93(8) . . ? N1 Cu1 N2 81.27(8) . . ? N4 Cu1 N2 93.96(8) . . ? O5 Cu1 N3 98.89(7) . . ? N1 Cu1 N3 108.70(8) . . ? N4 Cu1 N3 77.81(8) . . ? N2 Cu1 N3 94.87(8) . . ? C60 N1 C59 118.4(2) . . ? C60 N1 Cu1 128.39(17) . . ? C59 N1 Cu1 113.21(15) . . ? C52 N2 C53 117.9(2) . . ? C52 N2 Cu1 129.51(19) . . ? C53 N2 Cu1 112.60(15) . . ? C63 N3 C67 117.4(2) . . ? C63 N3 Cu1 133.00(17) . . ? C67 N3 Cu1 109.56(15) . . ? C72 N4 C71 118.2(2) . . ? C72 N4 Cu1 124.42(17) . . ? C71 N4 Cu1 117.38(16) . . ? C51 O2 H2A 109.5 . . ? C25 O3 H3A 109.5 . . ? C32 O5 Cu1 105.30(14) . . ? C50 O7 H7A 109.5 . . ? C15 O9 H9A 109.5 . . ? H13A O13 H13B 83.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.6(4) . . . . ? C1 C2 C3 C4 1.8(3) . . . . ? C1 C2 C3 C15 -177.8(2) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C15 C3 C4 C5 178.6(2) . . . . ? C3 C4 C5 C6 -1.2(4) . . . . ? C4 C5 C6 C1 2.4(3) . . . . ? C4 C5 C6 C7 -177.0(2) . . . . ? C2 C1 C6 C5 -1.5(3) . . . . ? C2 C1 C6 C7 178.0(2) . . . . ? C5 C6 C7 C17 14.7(3) . . . . ? C1 C6 C7 C17 -164.8(2) . . . . ? C5 C6 C7 C8 133.6(2) . . . . ? C1 C6 C7 C8 -45.9(3) . . . . ? C5 C6 C7 C16 -104.2(2) . . . . ? C1 C6 C7 C16 76.3(2) . . . . ? C17 C7 C8 C13 83.5(2) . . . . ? C16 C7 C8 C13 -158.0(2) . . . . ? C6 C7 C8 C13 -39.1(3) . . . . ? C17 C7 C8 C9 -92.0(3) . . . . ? C16 C7 C8 C9 26.4(3) . . . . ? C6 C7 C8 C9 145.4(2) . . . . ? C13 C8 C9 C10 -0.4(4) . . . . ? C7 C8 C9 C10 175.1(2) . . . . ? C8 C9 C10 C11 0.0(4) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C9 C10 C11 C14 -177.2(2) . . . . ? C10 C11 C12 C13 -0.7(4) . . . . ? C14 C11 C12 C13 177.1(2) . . . . ? C11 C12 C13 C8 0.3(4) . . . . ? C9 C8 C13 C12 0.2(4) . . . . ? C7 C8 C13 C12 -175.5(2) . . . . ? C10 C11 C14 O12 -174.0(2) . . . . ? C12 C11 C14 O12 8.2(3) . . . . ? C10 C11 C14 O11 6.9(3) . . . . ? C12 C11 C14 O11 -170.9(2) . . . . ? C4 C3 C15 O10 -2.3(4) . . . . ? C2 C3 C15 O10 177.3(2) . . . . ? C4 C3 C15 O9 177.7(2) . . . . ? C2 C3 C15 O9 -2.8(3) . . . . ? C17 C7 C16 F11 167.26(18) . . . . ? C8 C7 C16 F11 50.2(3) . . . . ? C6 C7 C16 F11 -71.2(2) . . . . ? C17 C7 C16 F12 -73.4(2) . . . . ? C8 C7 C16 F12 169.54(19) . . . . ? C6 C7 C16 F12 48.1(3) . . . . ? C17 C7 C16 F13 46.8(3) . . . . ? C8 C7 C16 F13 -70.3(3) . . . . ? C6 C7 C16 F13 168.28(19) . . . . ? C8 C7 C17 F15 -68.3(2) . . . . ? C16 C7 C17 F15 170.91(18) . . . . ? C6 C7 C17 F15 53.1(3) . . . . ? C8 C7 C17 F16 170.87(19) . . . . ? C16 C7 C17 F16 50.1(3) . . . . ? C6 C7 C17 F16 -67.7(3) . . . . ? C8 C7 C17 F14 50.4(2) . . . . ? C16 C7 C17 F14 -70.4(2) . . . . ? C6 C7 C17 F14 171.87(18) . . . . ? C24 C19 C20 C21 1.1(4) . . . . ? C24 C19 C20 C18 -173.8(2) . . . . ? C33 C18 C20 C19 76.7(2) . . . . ? C31 C18 C20 C19 -46.3(3) . . . . ? C34 C18 C20 C19 -165.6(2) . . . . ? C33 C18 C20 C21 -97.9(3) . . . . ? C31 C18 C20 C21 139.0(2) . . . . ? C34 C18 C20 C21 19.8(3) . . . . ? C19 C20 C21 C22 0.7(3) . . . . ? C18 C20 C21 C22 175.3(2) . . . . ? C20 C21 C22 C23 -1.8(4) . . . . ? C21 C22 C23 C24 1.0(4) . . . . ? C21 C22 C23 C25 -176.1(2) . . . . ? C20 C19 C24 C23 -1.9(4) . . . . ? C22 C23 C24 C19 0.9(4) . . . . ? C25 C23 C24 C19 177.9(2) . . . . ? C22 C23 C25 O4 -6.6(4) . . . . ? C24 C23 C25 O4 176.4(2) . . . . ? C22 C23 C25 O3 171.6(2) . . . . ? C24 C23 C25 O3 -5.4(3) . . . . ? C31 C26 C27 C28 -0.9(4) . . . . ? C26 C27 C28 C29 -1.9(4) . . . . ? C26 C27 C28 C32 175.5(2) . . . . ? C27 C28 C29 C30 2.9(3) . . . . ? C32 C28 C29 C30 -174.4(2) . . . . ? C28 C29 C30 C31 -1.0(3) . . . . ? C27 C26 C31 C30 2.8(3) . . . . ? C27 C26 C31 C18 -173.2(2) . . . . ? C29 C30 C31 C26 -1.8(3) . . . . ? C29 C30 C31 C18 173.9(2) . . . . ? C33 C18 C31 C26 -168.2(2) . . . . ? C20 C18 C31 C26 -49.2(3) . . . . ? C34 C18 C31 C26 74.3(2) . . . . ? C33 C18 C31 C30 16.1(3) . . . . ? C20 C18 C31 C30 135.0(2) . . . . ? C34 C18 C31 C30 -101.4(3) . . . . ? C27 C28 C32 O6 14.7(3) . . . . ? C29 C28 C32 O6 -168.0(2) . . . . ? C27 C28 C32 O5 -163.0(2) . . . . ? C29 C28 C32 O5 14.3(3) . . . . ? C31 C18 C33 F10 52.0(3) . . . . ? C20 C18 C33 F10 -70.4(2) . . . . ? C34 C18 C33 F10 168.38(18) . . . . ? C31 C18 C33 F9 171.20(19) . . . . ? C20 C18 C33 F9 48.8(3) . . . . ? C34 C18 C33 F9 -72.4(2) . . . . ? C31 C18 C33 F18 -68.3(3) . . . . ? C20 C18 C33 F18 169.31(19) . . . . ? C34 C18 C33 F18 48.1(3) . . . . ? C33 C18 C34 F17 -74.9(2) . . . . ? C31 C18 C34 F17 45.9(3) . . . . ? C20 C18 C34 F17 168.5(2) . . . . ? C33 C18 C34 F8 165.70(19) . . . . ? C31 C18 C34 F8 -73.4(2) . . . . ? C20 C18 C34 F8 49.2(3) . . . . ? C33 C18 C34 F7 45.7(3) . . . . ? C31 C18 C34 F7 166.5(2) . . . . ? C20 C18 C34 F7 -70.8(3) . . . . ? C40 C35 C36 C37 1.9(4) . . . . ? C51 C35 C36 C37 -178.2(2) . . . . ? C35 C36 C37 C38 -1.2(4) . . . . ? C36 C37 C38 C39 -0.7(4) . . . . ? C36 C37 C38 C47 173.9(2) . . . . ? C37 C38 C39 C40 1.8(4) . . . . ? C47 C38 C39 C40 -173.1(2) . . . . ? C38 C39 C40 C35 -1.0(4) . . . . ? C36 C35 C40 C39 -0.9(4) . . . . ? C51 C35 C40 C39 179.3(2) . . . . ? C46 C41 C42 C43 -3.0(4) . . . . ? C41 C42 C43 C44 -0.7(4) . . . . ? C41 C42 C43 C50 175.2(2) . . . . ? C42 C43 C44 C45 3.4(4) . . . . ? C50 C43 C44 C45 -172.3(2) . . . . ? C43 C44 C45 C46 -2.6(4) . . . . ? C44 C45 C46 C41 -1.0(3) . . . . ? C44 C45 C46 C47 175.7(2) . . . . ? C42 C41 C46 C45 3.8(4) . . . . ? C42 C41 C46 C47 -173.2(2) . . . . ? C39 C38 C47 C46 -43.9(3) . . . . ? C37 C38 C47 C46 141.5(2) . . . . ? C39 C38 C47 C48 -163.4(2) . . . . ? C37 C38 C47 C48 22.0(3) . . . . ? C39 C38 C47 C49 78.2(3) . . . . ? C37 C38 C47 C49 -96.3(3) . . . . ? C45 C46 C47 C38 131.9(2) . . . . ? C41 C46 C47 C38 -51.4(3) . . . . ? C45 C46 C47 C48 -104.5(3) . . . . ? C41 C46 C47 C48 72.3(3) . . . . ? C45 C46 C47 C49 13.1(3) . . . . ? C41 C46 C47 C49 -170.1(2) . . . . ? C38 C47 C48 F3 49.3(3) . . . . ? C46 C47 C48 F3 -73.3(2) . . . . ? C49 C47 C48 F3 166.53(19) . . . . ? C38 C47 C48 F1 -71.4(3) . . . . ? C46 C47 C48 F1 166.02(19) . . . . ? C49 C47 C48 F1 45.8(3) . . . . ? C38 C47 C48 F2 168.5(2) . . . . ? C46 C47 C48 F2 45.9(3) . . . . ? C49 C47 C48 F2 -74.2(2) . . . . ? C38 C47 C49 F6 -68.1(2) . . . . ? C46 C47 C49 F6 53.7(2) . . . . ? C48 C47 C49 F6 170.15(18) . . . . ? C38 C47 C49 F4 171.36(19) . . . . ? C46 C47 C49 F4 -66.8(3) . . . . ? C48 C47 C49 F4 49.6(3) . . . . ? C38 C47 C49 F5 50.9(2) . . . . ? C46 C47 C49 F5 172.80(19) . . . . ? C48 C47 C49 F5 -70.8(2) . . . . ? C44 C43 C50 O8 160.2(2) . . . . ? C42 C43 C50 O8 -15.5(4) . . . . ? C44 C43 C50 O7 -17.7(3) . . . . ? C42 C43 C50 O7 166.5(2) . . . . ? C40 C35 C51 O1 -9.1(4) . . . . ? C36 C35 C51 O1 171.1(3) . . . . ? C40 C35 C51 O2 171.4(2) . . . . ? C36 C35 C51 O2 -8.5(3) . . . . ? N2 C53 C54 C55 -0.9(4) . . . . ? C59 C53 C54 C55 178.9(2) . . . . ? N2 C53 C54 C56 178.8(2) . . . . ? C59 C53 C54 C56 -1.4(3) . . . . ? C53 C54 C55 C75 0.3(4) . . . . ? C56 C54 C55 C75 -179.4(3) . . . . ? C53 C54 C56 C57 0.3(4) . . . . ? C55 C54 C56 C57 180.0(2) . . . . ? C54 C56 C57 C58 0.8(4) . . . . ? C56 C57 C58 C59 -0.8(4) . . . . ? C56 C57 C58 C62 177.7(2) . . . . ? C62 C58 C59 N1 0.7(3) . . . . ? C57 C58 C59 N1 179.3(2) . . . . ? C62 C58 C59 C53 -179.0(2) . . . . ? C57 C58 C59 C53 -0.4(3) . . . . ? N2 C53 C59 N1 1.6(3) . . . . ? C54 C53 C59 N1 -178.2(2) . . . . ? N2 C53 C59 C58 -178.7(2) . . . . ? C54 C53 C59 C58 1.5(3) . . . . ? N1 C60 C61 C62 0.9(4) . . . . ? C60 C61 C62 C58 0.1(4) . . . . ? C59 C58 C62 C61 -0.8(3) . . . . ? C57 C58 C62 C61 -179.3(2) . . . . ? N3 C63 C64 C65 -1.4(4) . . . . ? C63 C64 C65 C66 0.5(4) . . . . ? C64 C65 C66 C67 1.1(3) . . . . ? C64 C65 C66 C68 179.7(2) . . . . ? C65 C66 C67 N3 -2.0(3) . . . . ? C68 C66 C67 N3 179.3(2) . . . . ? C65 C66 C67 C71 177.5(2) . . . . ? C68 C66 C67 C71 -1.2(3) . . . . ? C65 C66 C68 C69 -176.9(2) . . . . ? C67 C66 C68 C69 1.6(4) . . . . ? C66 C68 C69 C70 -0.5(4) . . . . ? C68 C69 C70 C74 178.7(2) . . . . ? C68 C69 C70 C71 -1.2(4) . . . . ? C74 C70 C71 N4 0.5(3) . . . . ? C69 C70 C71 N4 -179.5(2) . . . . ? C74 C70 C71 C67 -178.3(2) . . . . ? C69 C70 C71 C67 1.6(3) . . . . ? N3 C67 C71 N4 0.2(3) . . . . ? C66 C67 C71 N4 -179.3(2) . . . . ? N3 C67 C71 C70 179.1(2) . . . . ? C66 C67 C71 C70 -0.5(3) . . . . ? N4 C72 C73 C74 0.4(4) . . . . ? C72 C73 C74 C70 0.2(4) . . . . ? C71 C70 C74 C73 -0.7(3) . . . . ? C69 C70 C74 C73 179.4(2) . . . . ? C54 C55 C75 C52 0.1(4) . . . . ? N2 C52 C75 C55 0.0(5) . . . . ? C61 C60 N1 C59 -1.0(3) . . . . ? C61 C60 N1 Cu1 -178.76(18) . . . . ? C58 C59 N1 C60 0.2(3) . . . . ? C53 C59 N1 C60 179.9(2) . . . . ? C58 C59 N1 Cu1 178.32(18) . . . . ? C53 C59 N1 Cu1 -2.0(3) . . . . ? O5 Cu1 N1 C60 11.4(2) . . . . ? N4 Cu1 N1 C60 126.2(5) . . . . ? N2 Cu1 N1 C60 179.2(2) . . . . ? N3 Cu1 N1 C60 -88.5(2) . . . . ? O5 Cu1 N1 C59 -166.48(16) . . . . ? N4 Cu1 N1 C59 -51.6(6) . . . . ? N2 Cu1 N1 C59 1.39(16) . . . . ? N3 Cu1 N1 C59 93.60(16) . . . . ? C75 C52 N2 C53 -0.5(4) . . . . ? C75 C52 N2 Cu1 -178.6(2) . . . . ? C54 C53 N2 C52 1.0(4) . . . . ? C59 C53 N2 C52 -178.8(2) . . . . ? C54 C53 N2 Cu1 179.44(18) . . . . ? C59 C53 N2 Cu1 -0.4(3) . . . . ? O5 Cu1 N2 C52 -122.6(3) . . . . ? N1 Cu1 N2 C52 177.6(3) . . . . ? N4 Cu1 N2 C52 -8.6(2) . . . . ? N3 Cu1 N2 C52 69.4(2) . . . . ? O5 Cu1 N2 C53 59.3(4) . . . . ? N1 Cu1 N2 C53 -0.54(16) . . . . ? N4 Cu1 N2 C53 173.17(16) . . . . ? N3 Cu1 N2 C53 -108.75(16) . . . . ? C64 C63 N3 C67 0.6(4) . . . . ? C64 C63 N3 Cu1 -177.52(18) . . . . ? C66 C67 N3 C63 1.1(3) . . . . ? C71 C67 N3 C63 -178.4(2) . . . . ? C66 C67 N3 Cu1 179.69(17) . . . . ? C71 C67 N3 Cu1 0.2(2) . . . . ? O5 Cu1 N3 C63 -92.2(2) . . . . ? N1 Cu1 N3 C63 2.5(2) . . . . ? N4 Cu1 N3 C63 177.9(2) . . . . ? N2 Cu1 N3 C63 84.9(2) . . . . ? O5 Cu1 N3 C67 89.60(15) . . . . ? N1 Cu1 N3 C67 -175.75(14) . . . . ? N4 Cu1 N3 C67 -0.32(15) . . . . ? N2 Cu1 N3 C67 -93.33(16) . . . . ? C73 C72 N4 C71 -0.5(4) . . . . ? C73 C72 N4 Cu1 178.82(19) . . . . ? C70 C71 N4 C72 0.0(3) . . . . ? C67 C71 N4 C72 178.9(2) . . . . ? C70 C71 N4 Cu1 -179.35(17) . . . . ? C67 C71 N4 Cu1 -0.5(3) . . . . ? O5 Cu1 N4 C72 82.4(2) . . . . ? N1 Cu1 N4 C72 -32.4(7) . . . . ? N2 Cu1 N4 C72 -84.7(2) . . . . ? N3 Cu1 N4 C72 -178.9(2) . . . . ? O5 Cu1 N4 C71 -98.27(17) . . . . ? N1 Cu1 N4 C71 146.9(5) . . . . ? N2 Cu1 N4 C71 94.58(17) . . . . ? N3 Cu1 N4 C71 0.44(16) . . . . ? O6 C32 O5 Cu1 -3.3(3) . . . . ? C28 C32 O5 Cu1 174.37(16) . . . . ? N1 Cu1 O5 C32 89.77(15) . . . . ? N4 Cu1 O5 C32 -83.10(15) . . . . ? N2 Cu1 O5 C32 31.1(4) . . . . ? N3 Cu1 O5 C32 -161.04(15) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.185 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.078 data_F-MOF2 _database_code_depnum_ccdc_archive 'CCDC 745104' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'F-MOF 2' _chemical_melting_point ? _chemical_formula_moiety 'C27 H18 Cu F6 N2 O5' _chemical_formula_sum 'C27 H18 Cu F6 N2 O5' _chemical_formula_weight 627.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/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 7.7882(11) _cell_length_b 28.449(4) _cell_length_c 10.7928(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.520(2) _cell_angle_gamma 90.00 _cell_volume 2391.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7524 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.96 _exptl_crystal_description cubic _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8397 _exptl_absorpt_correction_T_max 0.9061 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'phi and omega scans' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24548 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4722 _reflns_number_gt 4009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^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 4722 _refine_ls_number_parameters 371 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0437(3) 0.41314(9) 1.2705(2) 0.0134(5) Uani 1 1 d . . . C2 C 1.0148(3) 0.33795(9) 1.1458(2) 0.0135(5) Uani 1 1 d . . . H2 H 1.1231 0.3447 1.1100 0.016 Uiso 1 1 calc R . . C3 C 0.9509(3) 0.36749(9) 1.2369(2) 0.0128(5) Uani 1 1 d . . . C4 C 0.7979(3) 0.35549(8) 1.2934(2) 0.0136(5) Uani 1 1 d . . . H4 H 0.7580 0.3736 1.3612 0.016 Uiso 1 1 calc R . . C5 C 0.7021(3) 0.31726(8) 1.2521(2) 0.0136(5) Uani 1 1 d . . . H5 H 0.5954 0.3103 1.2899 0.016 Uiso 1 1 calc R . . C6 C 0.7612(3) 0.28913(8) 1.1560(2) 0.0125(5) Uani 1 1 d . . . C7 C 0.6512(3) 0.25039(8) 1.0931(2) 0.0127(5) Uani 1 1 d . . . C8 C 0.8440(3) 0.18600(9) 1.1750(2) 0.0153(5) Uani 1 1 d . . . H8 H 0.8474 0.2029 1.2509 0.018 Uiso 1 1 calc R . . C9 C 0.7525(3) 0.20446(8) 1.0739(2) 0.0124(5) Uani 1 1 d . . . C10 C 0.7518(3) 0.17885(8) 0.9631(2) 0.0139(5) Uani 1 1 d . . . H10 H 0.6879 0.1901 0.8939 0.017 Uiso 1 1 calc R . . C11 C 0.8434(3) 0.13728(9) 0.9535(2) 0.0136(5) Uani 1 1 d . . . H11 H 0.8455 0.1212 0.8764 0.016 Uiso 1 1 calc R . . C12 C 0.9324(3) 0.11865(8) 1.0547(2) 0.0122(5) Uani 1 1 d . . . C13 C 0.9299(3) 0.14344(9) 1.1662(2) 0.0155(5) Uani 1 1 d . . . H13 H 0.9877 0.1310 1.2368 0.019 Uiso 1 1 calc R . . C14 C 0.4905(3) 0.23806(9) 1.1695(2) 0.0165(5) Uani 1 1 d . . . C15 C 0.5858(3) 0.27203(9) 0.9691(2) 0.0163(5) Uani 1 1 d . . . C16 C 1.0645(3) 0.06403(8) 0.6608(2) 0.0144(5) Uani 1 1 d . . . H16 H 1.0069 0.0822 0.7214 0.017 Uiso 1 1 calc R . . C17 C 1.0397(3) 0.07464(9) 0.5365(2) 0.0157(5) Uani 1 1 d . . . H17 H 0.9663 0.0998 0.5123 0.019 Uiso 1 1 calc R . . C18 C 1.1234(3) 0.04803(9) 0.4481(2) 0.0163(5) Uani 1 1 d . . . H18 H 1.1100 0.0551 0.3626 0.020 Uiso 1 1 calc R . . C19 C 1.2269(3) 0.01108(9) 0.4858(2) 0.0155(5) Uani 1 1 d . . . H19 H 1.2846 -0.0078 0.4266 0.019 Uiso 1 1 calc R . . C20 C 1.2448(3) 0.00210(9) 0.6119(2) 0.0128(5) Uani 1 1 d . . . C21 C 1.3489(3) -0.03714(8) 0.6633(2) 0.0125(5) Uani 1 1 d . . . C22 C 1.4244(3) -0.07182(9) 0.5911(2) 0.0169(5) Uani 1 1 d . . . H22 H 1.4053 -0.0727 0.5041 0.020 Uiso 1 1 calc R . . C23 C 1.5276(3) -0.10501(9) 0.6483(2) 0.0187(6) Uani 1 1 d . . . H23 H 1.5810 -0.1290 0.6010 0.022 Uiso 1 1 calc R . . C24 C 1.5523(3) -0.10290(9) 0.7755(2) 0.0175(6) Uani 1 1 d . . . H24 H 1.6272 -0.1245 0.8159 0.021 Uiso 1 1 calc R . . C25 C 1.4672(3) -0.06917(9) 0.8426(2) 0.0154(5) Uani 1 1 d . . . H25 H 1.4799 -0.0688 0.9302 0.019 Uiso 1 1 calc R . . C26 C 1.0282(3) 0.07275(9) 1.0443(2) 0.0129(5) Uani 1 1 d . . . C28 C 0.9233(3) 0.29874(8) 1.1062(2) 0.0134(5) Uani 1 1 d . . . H28 H 0.9704 0.2785 1.0454 0.016 Uiso 1 1 calc R . . Cu1 Cu 1.23162(4) 0.013470(10) 0.87352(3) 0.01162(11) Uani 1 1 d . . . F1 F 0.37729(18) 0.27349(5) 1.17872(14) 0.0198(3) Uani 1 1 d . . . F2 F 0.40323(19) 0.20198(5) 1.11881(15) 0.0231(4) Uani 1 1 d . . . F3 F 0.53342(18) 0.22494(5) 1.28508(13) 0.0196(3) Uani 1 1 d . . . F4 F 0.51446(19) 0.31446(5) 0.98585(13) 0.0203(3) Uani 1 1 d . . . F5 F 0.71229(18) 0.27788(5) 0.88833(13) 0.0192(3) Uani 1 1 d . . . F6 F 0.46531(19) 0.24532(5) 0.91314(14) 0.0201(3) Uani 1 1 d . . . N1 N 1.3662(2) -0.03668(7) 0.78767(19) 0.0120(4) Uani 1 1 d . . . N2 N 1.1673(3) 0.02896(7) 0.69793(19) 0.0121(4) Uani 1 1 d . . . O1 O 0.9833(2) 0.43662(6) 1.36171(15) 0.0149(4) Uani 1 1 d . . . O2 O 1.1701(2) 0.42456(6) 1.20804(16) 0.0181(4) Uani 1 1 d . . . O3 O 1.2794(2) -0.00915(6) 1.04036(15) 0.0166(4) Uani 1 1 d . . . H3A H 1.2133 0.0042 1.0904 0.025 Uiso 1 1 calc RD . . H3B H 1.3528 -0.0278 1.0791 0.025 Uiso 1 1 d RD . . O4 O 1.0824(2) 0.06310(6) 0.93588(15) 0.0131(4) Uani 1 1 d . . . O5 O 1.0483(2) 0.04797(6) 1.13894(15) 0.0171(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0135(12) 0.0139(13) 0.0126(12) 0.0032(10) -0.0082(10) 0.0019(10) C2 0.0111(12) 0.0163(13) 0.0132(12) 0.0028(10) -0.0014(10) -0.0003(10) C3 0.0125(12) 0.0134(12) 0.0123(12) 0.0015(10) -0.0060(10) 0.0031(10) C4 0.0153(12) 0.0119(12) 0.0137(12) -0.0016(10) -0.0036(10) 0.0031(10) C5 0.0125(12) 0.0122(12) 0.0161(12) -0.0008(10) -0.0008(10) 0.0015(10) C6 0.0149(12) 0.0092(12) 0.0134(12) 0.0007(10) -0.0051(10) 0.0004(10) C7 0.0135(12) 0.0113(12) 0.0132(12) -0.0016(10) -0.0042(10) 0.0002(10) C8 0.0168(13) 0.0150(13) 0.0141(12) -0.0040(10) -0.0056(10) 0.0014(10) C9 0.0121(12) 0.0094(12) 0.0156(12) -0.0013(10) -0.0025(10) -0.0015(10) C10 0.0140(12) 0.0135(12) 0.0141(12) 0.0000(10) -0.0055(10) 0.0006(10) C11 0.0150(12) 0.0132(13) 0.0125(12) -0.0031(10) -0.0032(10) -0.0011(10) C12 0.0104(12) 0.0115(12) 0.0148(12) 0.0003(10) -0.0010(10) -0.0008(10) C13 0.0166(13) 0.0157(13) 0.0142(12) 0.0012(10) -0.0048(10) 0.0010(10) C14 0.0142(13) 0.0127(12) 0.0224(14) -0.0018(10) -0.0038(11) -0.0001(10) C15 0.0184(13) 0.0119(13) 0.0185(13) -0.0006(10) -0.0076(11) 0.0028(10) C16 0.0125(12) 0.0142(13) 0.0166(13) -0.0008(10) -0.0036(10) -0.0013(10) C17 0.0155(13) 0.0118(12) 0.0197(13) 0.0030(10) -0.0067(10) -0.0013(10) C18 0.0156(13) 0.0197(13) 0.0133(12) 0.0023(10) -0.0049(10) -0.0055(11) C19 0.0148(12) 0.0168(13) 0.0147(13) -0.0025(10) -0.0024(10) -0.0026(10) C20 0.0098(12) 0.0134(12) 0.0151(13) -0.0003(10) -0.0031(10) -0.0032(10) C21 0.0090(11) 0.0144(12) 0.0140(12) -0.0001(10) -0.0006(10) -0.0020(10) C22 0.0168(13) 0.0185(13) 0.0154(12) -0.0022(11) -0.0011(10) -0.0008(11) C23 0.0178(13) 0.0160(13) 0.0222(14) -0.0046(11) 0.0022(11) 0.0016(11) C24 0.0160(13) 0.0122(13) 0.0242(14) 0.0020(10) -0.0032(11) 0.0012(10) C25 0.0150(12) 0.0167(13) 0.0145(12) 0.0021(10) -0.0044(10) -0.0004(10) C26 0.0096(12) 0.0137(12) 0.0153(12) -0.0017(10) -0.0035(10) -0.0031(10) C28 0.0136(12) 0.0139(12) 0.0126(12) -0.0010(10) -0.0020(10) 0.0032(10) Cu1 0.01208(17) 0.01260(18) 0.01013(17) -0.00009(11) -0.00272(12) 0.00266(12) F1 0.0120(7) 0.0173(8) 0.0302(9) -0.0003(7) 0.0005(6) 0.0024(6) F2 0.0194(8) 0.0173(8) 0.0326(9) -0.0040(7) -0.0034(7) -0.0069(6) F3 0.0195(8) 0.0204(8) 0.0188(8) 0.0039(6) 0.0008(6) 0.0006(6) F4 0.0256(8) 0.0135(7) 0.0218(8) 0.0000(6) -0.0072(7) 0.0070(6) F5 0.0233(8) 0.0191(8) 0.0153(8) 0.0019(6) -0.0018(6) 0.0017(6) F6 0.0194(8) 0.0173(8) 0.0233(8) -0.0009(6) -0.0141(7) 0.0000(6) N1 0.0094(10) 0.0130(10) 0.0136(10) -0.0001(8) -0.0017(8) -0.0024(8) N2 0.0101(10) 0.0137(11) 0.0124(10) -0.0012(8) -0.0025(8) -0.0011(8) O1 0.0142(9) 0.0148(9) 0.0157(9) -0.0034(7) -0.0058(7) -0.0003(7) O2 0.0178(9) 0.0208(10) 0.0157(9) 0.0006(8) -0.0015(8) -0.0063(8) O3 0.0175(9) 0.0200(10) 0.0123(9) 0.0013(7) -0.0014(7) 0.0084(7) O4 0.0139(9) 0.0142(9) 0.0111(8) 0.0005(7) -0.0003(7) 0.0021(7) O5 0.0221(10) 0.0173(9) 0.0118(9) 0.0013(7) -0.0015(7) 0.0060(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.241(3) . ? C1 O1 1.282(3) . ? C1 C3 1.528(3) . ? C2 C3 1.389(3) . ? C2 C28 1.389(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C4 C5 1.390(3) . ? C4 H4 0.9500 . ? C5 C6 1.392(3) . ? C5 H5 0.9500 . ? C6 C28 1.404(3) . ? C6 C7 1.549(3) . ? C7 C9 1.541(3) . ? C7 C14 1.546(4) . ? C7 C15 1.555(3) . ? C8 C13 1.387(3) . ? C8 C9 1.400(3) . ? C8 H8 0.9500 . ? C9 C10 1.400(3) . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.393(3) . ? C11 H11 0.9500 . ? C12 C13 1.395(3) . ? C12 C26 1.509(3) . ? C13 H13 0.9500 . ? C14 F3 1.342(3) . ? C14 F1 1.343(3) . ? C14 F2 1.345(3) . ? C15 F5 1.331(3) . ? C15 F4 1.342(3) . ? C15 F6 1.346(3) . ? C16 N2 1.338(3) . ? C16 C17 1.387(3) . ? C16 H16 0.9500 . ? C17 C18 1.386(4) . ? C17 H17 0.9500 . ? C18 C19 1.383(4) . ? C18 H18 0.9500 . ? C19 C20 1.391(3) . ? C19 H19 0.9500 . ? C20 N2 1.349(3) . ? C20 C21 1.485(3) . ? C21 N1 1.347(3) . ? C21 C22 1.391(3) . ? C22 C23 1.382(4) . ? C22 H22 0.9500 . ? C23 C24 1.385(4) . ? C23 H23 0.9500 . ? C24 C25 1.376(4) . ? C24 H24 0.9500 . ? C25 N1 1.347(3) . ? C25 H25 0.9500 . ? C26 O5 1.249(3) . ? C26 O4 1.278(3) . ? C28 H28 0.9500 . ? Cu1 O3 1.9449(17) . ? Cu1 O4 1.9522(16) . ? Cu1 N1 2.003(2) . ? Cu1 N2 2.005(2) . ? Cu1 O1 2.4246(17) 4_665 ? O1 Cu1 2.4247(17) 4_566 ? O3 H3A 0.8400 . ? O3 H3B 0.8816 . ? 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 O2 C1 O1 125.4(2) . . ? O2 C1 C3 118.0(2) . . ? O1 C1 C3 116.7(2) . . ? C3 C2 C28 121.2(2) . . ? C3 C2 H2 119.4 . . ? C28 C2 H2 119.4 . . ? C4 C3 C2 118.5(2) . . ? C4 C3 C1 120.7(2) . . ? C2 C3 C1 120.7(2) . . ? C3 C4 C5 120.9(2) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C28 118.6(2) . . ? C5 C6 C7 123.4(2) . . ? C28 C6 C7 117.8(2) . . ? C9 C7 C14 107.30(19) . . ? C9 C7 C6 112.36(19) . . ? C14 C7 C6 112.0(2) . . ? C9 C7 C15 112.6(2) . . ? C14 C7 C15 106.8(2) . . ? C6 C7 C15 105.72(19) . . ? C13 C8 C9 121.1(2) . . ? C13 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 117.9(2) . . ? C10 C9 C7 123.9(2) . . ? C8 C9 C7 118.1(2) . . ? C11 C10 C9 120.7(2) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 121.2(2) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C13 118.2(2) . . ? C11 C12 C26 120.9(2) . . ? C13 C12 C26 120.8(2) . . ? C8 C13 C12 120.8(2) . . ? C8 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? F3 C14 F1 107.3(2) . . ? F3 C14 F2 106.7(2) . . ? F1 C14 F2 105.85(19) . . ? F3 C14 C7 111.3(2) . . ? F1 C14 C7 113.9(2) . . ? F2 C14 C7 111.4(2) . . ? F5 C15 F4 106.6(2) . . ? F5 C15 F6 107.1(2) . . ? F4 C15 F6 106.30(19) . . ? F5 C15 C7 112.0(2) . . ? F4 C15 C7 111.9(2) . . ? F6 C15 C7 112.6(2) . . ? N2 C16 C17 122.0(2) . . ? N2 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 119.0(2) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 119.3(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 118.7(2) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? N2 C20 C19 121.9(2) . . ? N2 C20 C21 114.5(2) . . ? C19 C20 C21 123.6(2) . . ? N1 C21 C22 121.7(2) . . ? N1 C21 C20 114.5(2) . . ? C22 C21 C20 123.8(2) . . ? C23 C22 C21 118.8(2) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 119.2(2) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 119.2(2) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? N1 C25 C24 121.9(2) . . ? N1 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? O5 C26 O4 126.0(2) . . ? O5 C26 C12 119.1(2) . . ? O4 C26 C12 114.9(2) . . ? C2 C28 C6 120.0(2) . . ? C2 C28 H28 120.0 . . ? C6 C28 H28 120.0 . . ? O3 Cu1 O4 91.70(7) . . ? O3 Cu1 N1 95.51(8) . . ? O4 Cu1 N1 172.09(7) . . ? O3 Cu1 N2 172.72(8) . . ? O4 Cu1 N2 91.29(7) . . ? N1 Cu1 N2 81.18(8) . . ? O3 Cu1 O1 95.42(7) . 4_665 ? O4 Cu1 O1 94.51(7) . 4_665 ? N1 Cu1 O1 88.06(7) . 4_665 ? N2 Cu1 O1 90.97(7) . 4_665 ? C25 N1 C21 119.0(2) . . ? C25 N1 Cu1 126.23(17) . . ? C21 N1 Cu1 114.81(16) . . ? C16 N2 C20 119.1(2) . . ? C16 N2 Cu1 126.21(17) . . ? C20 N2 Cu1 114.62(16) . . ? C1 O1 Cu1 130.37(15) . 4_566 ? Cu1 O3 H3A 109.5 . . ? Cu1 O3 H3B 139.1 . . ? H3A O3 H3B 111.3 . . ? C26 O4 Cu1 132.37(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C28 C2 C3 C4 3.9(4) . . . . ? C28 C2 C3 C1 -173.8(2) . . . . ? O2 C1 C3 C4 -172.5(2) . . . . ? O1 C1 C3 C4 7.3(3) . . . . ? O2 C1 C3 C2 5.1(3) . . . . ? O1 C1 C3 C2 -175.0(2) . . . . ? C2 C3 C4 C5 -6.0(4) . . . . ? C1 C3 C4 C5 171.7(2) . . . . ? C3 C4 C5 C6 2.4(4) . . . . ? C4 C5 C6 C28 3.3(4) . . . . ? C4 C5 C6 C7 -171.3(2) . . . . ? C5 C6 C7 C9 -135.6(2) . . . . ? C28 C6 C7 C9 49.9(3) . . . . ? C5 C6 C7 C14 -14.7(3) . . . . ? C28 C6 C7 C14 170.7(2) . . . . ? C5 C6 C7 C15 101.3(3) . . . . ? C28 C6 C7 C15 -73.3(3) . . . . ? C13 C8 C9 C10 -0.6(4) . . . . ? C13 C8 C9 C7 176.3(2) . . . . ? C14 C7 C9 C10 102.7(3) . . . . ? C6 C7 C9 C10 -133.7(2) . . . . ? C15 C7 C9 C10 -14.5(3) . . . . ? C14 C7 C9 C8 -74.0(3) . . . . ? C6 C7 C9 C8 49.5(3) . . . . ? C15 C7 C9 C8 168.8(2) . . . . ? C8 C9 C10 C11 -1.9(4) . . . . ? C7 C9 C10 C11 -178.7(2) . . . . ? C9 C10 C11 C12 2.9(4) . . . . ? C10 C11 C12 C13 -1.2(4) . . . . ? C10 C11 C12 C26 178.5(2) . . . . ? C9 C8 C13 C12 2.3(4) . . . . ? C11 C12 C13 C8 -1.4(4) . . . . ? C26 C12 C13 C8 179.0(2) . . . . ? C9 C7 C14 F3 67.4(2) . . . . ? C6 C7 C14 F3 -56.4(3) . . . . ? C15 C7 C14 F3 -171.71(19) . . . . ? C9 C7 C14 F1 -171.16(19) . . . . ? C6 C7 C14 F1 65.1(3) . . . . ? C15 C7 C14 F1 -50.2(3) . . . . ? C9 C7 C14 F2 -51.5(3) . . . . ? C6 C7 C14 F2 -175.31(19) . . . . ? C15 C7 C14 F2 69.4(2) . . . . ? C9 C7 C15 F5 -53.6(3) . . . . ? C14 C7 C15 F5 -171.08(19) . . . . ? C6 C7 C15 F5 69.5(2) . . . . ? C9 C7 C15 F4 -173.2(2) . . . . ? C14 C7 C15 F4 69.3(2) . . . . ? C6 C7 C15 F4 -50.1(3) . . . . ? C9 C7 C15 F6 67.2(3) . . . . ? C14 C7 C15 F6 -50.3(3) . . . . ? C6 C7 C15 F6 -169.8(2) . . . . ? N2 C16 C17 C18 0.2(4) . . . . ? C16 C17 C18 C19 1.2(4) . . . . ? C17 C18 C19 C20 -0.6(4) . . . . ? C18 C19 C20 N2 -1.5(4) . . . . ? C18 C19 C20 C21 178.6(2) . . . . ? N2 C20 C21 N1 -7.3(3) . . . . ? C19 C20 C21 N1 172.7(2) . . . . ? N2 C20 C21 C22 173.0(2) . . . . ? C19 C20 C21 C22 -7.0(4) . . . . ? N1 C21 C22 C23 -3.7(4) . . . . ? C20 C21 C22 C23 176.0(2) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? C22 C23 C24 C25 3.0(4) . . . . ? C23 C24 C25 N1 -3.1(4) . . . . ? C11 C12 C26 O5 -152.2(2) . . . . ? C13 C12 C26 O5 27.4(3) . . . . ? C11 C12 C26 O4 28.0(3) . . . . ? C13 C12 C26 O4 -152.4(2) . . . . ? C3 C2 C28 C6 1.7(4) . . . . ? C5 C6 C28 C2 -5.3(4) . . . . ? C7 C6 C28 C2 169.5(2) . . . . ? C24 C25 N1 C21 -0.3(4) . . . . ? C24 C25 N1 Cu1 178.76(18) . . . . ? C22 C21 N1 C25 3.8(3) . . . . ? C20 C21 N1 C25 -175.9(2) . . . . ? C22 C21 N1 Cu1 -175.41(18) . . . . ? C20 C21 N1 Cu1 4.9(3) . . . . ? O3 Cu1 N1 C25 -7.0(2) . . . . ? O4 Cu1 N1 C25 -162.6(5) . . . . ? N2 Cu1 N1 C25 179.6(2) . . . . ? O1 Cu1 N1 C25 88.3(2) 4_665 . . . ? O3 Cu1 N1 C21 172.14(17) . . . . ? O4 Cu1 N1 C21 16.5(6) . . . . ? N2 Cu1 N1 C21 -1.32(16) . . . . ? O1 Cu1 N1 C21 -92.60(16) 4_665 . . . ? C17 C16 N2 C20 -2.2(4) . . . . ? C17 C16 N2 Cu1 174.07(18) . . . . ? C19 C20 N2 C16 2.9(3) . . . . ? C21 C20 N2 C16 -177.2(2) . . . . ? C19 C20 N2 Cu1 -173.84(19) . . . . ? C21 C20 N2 Cu1 6.1(3) . . . . ? O3 Cu1 N2 C16 117.3(6) . . . . ? O4 Cu1 N2 C16 3.2(2) . . . . ? N1 Cu1 N2 C16 -179.2(2) . . . . ? O1 Cu1 N2 C16 -91.4(2) 4_665 . . . ? O3 Cu1 N2 C20 -66.3(7) . . . . ? O4 Cu1 N2 C20 179.58(17) . . . . ? N1 Cu1 N2 C20 -2.84(17) . . . . ? O1 Cu1 N2 C20 85.05(17) 4_665 . . . ? O2 C1 O1 Cu1 103.6(3) . . . 4_566 ? C3 C1 O1 Cu1 -76.3(3) . . . 4_566 ? O5 C26 O4 Cu1 -7.6(4) . . . . ? C12 C26 O4 Cu1 172.23(15) . . . . ? O3 Cu1 O4 C26 -5.7(2) . . . . ? N1 Cu1 O4 C26 150.0(5) . . . . ? N2 Cu1 O4 C26 167.7(2) . . . . ? O1 Cu1 O4 C26 -101.2(2) 4_665 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.730 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.097 data_F-MOF3 _database_code_depnum_ccdc_archive 'CCDC 745105' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'F-MOF 3' _chemical_melting_point ? _chemical_formula_moiety 'C75 H48 Cu2 F18 N4 O12, C17 H10 F6 O4, 2(O)' _chemical_formula_sum 'C92 H58 Cu2 F24 N4 O18 ' _chemical_formula_weight 2090.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 51.500(14) _cell_length_b 11.992(3) _cell_length_c 14.114(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8717(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8882 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.39 _exptl_crystal_description Cubic _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8873 _exptl_absorpt_correction_T_max 0.9301 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 92999 _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -65 _diffrn_reflns_limit_h_max 65 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9518 _reflns_number_gt 8080 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+7.9267P] 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 9518 _refine_ls_number_parameters 635 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.09994(5) 0.5185(2) 0.08586(19) 0.0166(6) Uani 1 1 d . . . C2 C 0.08387(5) 0.4913(2) -0.00069(19) 0.0149(5) Uani 1 1 d . . . C3 C 0.06292(5) 0.4182(2) 0.00690(19) 0.0165(5) Uani 1 1 d . . . H3 H 0.0586 0.3871 0.0668 0.020 Uiso 1 1 calc R . . C4 C 0.04836(5) 0.3905(2) -0.07256(19) 0.0169(6) Uani 1 1 d . . . H4 H 0.0340 0.3415 -0.0664 0.020 Uiso 1 1 calc R . . C5 C 0.05469(5) 0.4338(2) -0.16125(18) 0.0155(5) Uani 1 1 d . . . C6 C 0.07519(5) 0.5100(2) -0.16760(19) 0.0173(6) Uani 1 1 d . . . H6 H 0.0794 0.5425 -0.2271 0.021 Uiso 1 1 calc R . . C7 C 0.08945(5) 0.5385(2) -0.08821(19) 0.0172(6) Uani 1 1 d . . . H7 H 0.1032 0.5909 -0.0936 0.021 Uiso 1 1 calc R . . C8 C 0.03920(5) 0.4067(2) -0.25231(18) 0.0155(5) Uani 1 1 d . . . C9 C 0.05700(5) 0.3868(2) -0.33881(18) 0.0151(5) Uani 1 1 d . . . C10 C 0.08065(5) 0.3312(2) -0.32513(19) 0.0169(6) Uani 1 1 d . . . H10 H 0.0861 0.3128 -0.2627 0.020 Uiso 1 1 calc R . . C11 C 0.09617(5) 0.3027(2) -0.40093(19) 0.0175(6) Uani 1 1 d . . . H11 H 0.1121 0.2650 -0.3904 0.021 Uiso 1 1 calc R . . C12 C 0.08854(5) 0.3290(2) -0.49293(19) 0.0174(6) Uani 1 1 d . . . C13 C 0.06502(5) 0.3843(2) -0.50727(19) 0.0179(6) Uani 1 1 d . . . H13 H 0.0597 0.4023 -0.5699 0.022 Uiso 1 1 calc R . . C14 C 0.04934(5) 0.4134(2) -0.43106(19) 0.0176(6) Uani 1 1 d . . . H14 H 0.0334 0.4514 -0.4417 0.021 Uiso 1 1 calc R . . C15 C 0.02024(6) 0.5057(2) -0.2675(2) 0.0220(6) Uani 1 1 d . . . C16 C 0.02284(5) 0.2991(2) -0.24259(19) 0.0188(6) Uani 1 1 d . . . C17 C 0.15893(6) 0.3213(3) 0.2194(2) 0.0216(6) Uani 1 1 d . . . C18 C 0.18178(5) 0.3028(2) 0.15345(19) 0.0185(6) Uani 1 1 d . . . C19 C 0.20047(5) 0.2231(2) 0.17656(19) 0.0172(6) Uani 1 1 d . . . H19 H 0.1983 0.1786 0.2317 0.021 Uiso 1 1 calc R . . C20 C 0.22220(5) 0.2083(2) 0.11953(19) 0.0155(5) Uani 1 1 d . . . H20 H 0.2348 0.1540 0.1363 0.019 Uiso 1 1 calc R . . C21 C 0.22568(5) 0.2722(2) 0.03815(18) 0.0159(5) Uani 1 1 d . . . C22 C 0.20652(6) 0.3492(3) 0.0138(2) 0.0231(6) Uani 1 1 d . . . H22 H 0.2082 0.3915 -0.0428 0.028 Uiso 1 1 calc R . . C23 C 0.18495(6) 0.3647(3) 0.0719(2) 0.0245(7) Uani 1 1 d . . . H23 H 0.1722 0.4186 0.0550 0.029 Uiso 1 1 calc R . . C24 C 0.2500 0.2500 -0.0235(3) 0.0168(8) Uani 1 2 d S . . C25 C 0.24304(5) 0.1498(2) -0.08815(19) 0.0173(6) Uani 1 1 d . . . C26 C 0.12271(5) 0.5584(2) 0.4579(2) 0.0171(6) Uani 1 1 d . . . C27 C 0.09734(5) 0.6015(2) 0.42508(19) 0.0173(6) Uani 1 1 d . . . C28 C 0.08065(5) 0.6651(2) 0.4810(2) 0.0192(6) Uani 1 1 d . . . H28 H 0.0853 0.6828 0.5444 0.023 Uiso 1 1 calc R . . C29 C 0.05719(6) 0.7026(2) 0.4438(2) 0.0209(6) Uani 1 1 d . . . C30 C 0.05144(6) 0.6731(3) 0.3507(2) 0.0241(6) Uani 1 1 d . . . H30 H 0.0356 0.6966 0.3228 0.029 Uiso 1 1 calc R . . C31 C 0.06872(6) 0.6100(3) 0.2989(2) 0.0237(6) Uani 1 1 d . . . H31 H 0.0645 0.5907 0.2354 0.028 Uiso 1 1 calc R . . C32 C 0.03874(6) 0.7711(3) 0.5012(2) 0.0282(7) Uani 1 1 d . . . H32A H 0.0360 0.8433 0.4701 0.042 Uiso 1 1 calc R . . H32B H 0.0460 0.7831 0.5646 0.042 Uiso 1 1 calc R . . H32C H 0.0221 0.7319 0.5065 0.042 Uiso 1 1 calc R . . C33 C 0.13087(6) 0.5653(2) 0.5512(2) 0.0210(6) Uani 1 1 d . . . H33 H 0.1200 0.5984 0.5976 0.025 Uiso 1 1 calc R . . C34 C 0.15506(6) 0.5236(2) 0.5766(2) 0.0235(6) Uani 1 1 d . . . C35 C 0.17054(6) 0.4801(2) 0.5053(2) 0.0240(6) Uani 1 1 d . . . H35 H 0.1876 0.4544 0.5191 0.029 Uiso 1 1 calc R . . C36 C 0.16102(5) 0.4744(2) 0.4136(2) 0.0212(6) Uani 1 1 d . . . H36 H 0.1717 0.4434 0.3657 0.025 Uiso 1 1 calc R . . C37 C 0.16337(7) 0.5244(3) 0.6790(2) 0.0329(8) Uani 1 1 d . . . H37A H 0.1600 0.4511 0.7071 0.049 Uiso 1 1 calc R . . H37B H 0.1535 0.5814 0.7134 0.049 Uiso 1 1 calc R . . H37C H 0.1820 0.5413 0.6830 0.049 Uiso 1 1 calc R . . C38 C 0.15525(6) 0.8042(2) 0.4067(2) 0.0189(6) Uani 1 1 d . . . C39 C 0.18003(5) 0.7833(2) 0.35507(19) 0.0179(6) Uani 1 1 d . . . C40 C 0.20262(5) 0.8407(2) 0.37852(19) 0.0195(6) Uani 1 1 d . . . H40 H 0.2027 0.8905 0.4308 0.023 Uiso 1 1 calc R . . C41 C 0.18026(6) 0.7103(2) 0.2789(2) 0.0219(6) Uani 1 1 d . . . H41 H 0.1650 0.6702 0.2630 0.026 Uiso 1 1 calc R . . C42 C 0.22496(5) 0.8252(2) 0.32586(19) 0.0195(6) Uani 1 1 d . . . H42 H 0.2403 0.8643 0.3427 0.023 Uiso 1 1 calc R . . C43 C 0.20260(6) 0.6953(2) 0.2260(2) 0.0201(6) Uani 1 1 d . . . H43 H 0.2025 0.6452 0.1738 0.024 Uiso 1 1 calc R . . C44 C 0.22524(5) 0.7533(2) 0.24873(18) 0.0170(6) Uani 1 1 d . . . C45 C 0.2500 0.7500 0.1873(3) 0.0193(8) Uani 1 2 d S . . C46 C 0.25145(6) 0.6457(3) 0.1234(2) 0.0264(7) Uani 1 1 d . . . C48 C 0.10422(5) 0.3025(2) 0.4217(2) 0.0184(6) Uani 1 1 d . . . Cu1 Cu 0.117670(6) 0.47964(3) 0.26928(2) 0.01697(10) Uani 1 1 d . . . F1 F 0.24730(4) 0.55272(15) 0.17339(13) 0.0329(4) Uani 1 1 d . . . F2 F 0.23413(4) 0.64721(17) 0.05282(12) 0.0361(5) Uani 1 1 d . . . F3 F 0.27485(3) 0.63472(17) 0.08314(13) 0.0354(5) Uani 1 1 d . . . F4 F 0.00835(3) 0.53484(15) -0.18697(12) 0.0299(4) Uani 1 1 d . . . F5 F 0.00140(3) 0.48467(14) -0.33068(12) 0.0262(4) Uani 1 1 d . . . F6 F 0.03305(4) 0.59588(13) -0.29861(12) 0.0272(4) Uani 1 1 d . . . F7 F 0.01289(3) 0.26694(13) -0.32606(11) 0.0225(4) Uani 1 1 d . . . F8 F 0.00259(3) 0.31022(15) -0.18299(12) 0.0258(4) Uani 1 1 d . . . F9 F 0.03735(3) 0.21469(13) -0.21075(12) 0.0227(4) Uani 1 1 d . . . F10 F 0.21971(3) 0.16155(13) -0.12797(11) 0.0222(4) Uani 1 1 d . . . F11 F 0.24232(3) 0.05470(13) -0.03811(11) 0.0224(4) Uani 1 1 d . . . F12 F 0.26004(3) 0.13403(13) -0.15940(11) 0.0223(4) Uani 1 1 d . . . N1 N 0.09133(4) 0.5749(2) 0.33501(16) 0.0189(5) Uani 1 1 d . . . N2 N 0.13731(4) 0.51087(18) 0.38980(16) 0.0169(5) Uani 1 1 d . . . O1 O 0.09547(4) 0.46078(16) 0.15910(13) 0.0180(4) Uani 1 1 d . . . O2 O 0.11626(4) 0.59644(17) 0.08287(13) 0.0218(4) Uani 1 1 d . . . O3 O 0.14678(4) 0.41221(18) 0.20462(14) 0.0255(5) Uani 1 1 d . . . O4 O 0.15446(4) 0.25147(18) 0.28219(15) 0.0265(5) Uani 1 1 d . . . O5 O 0.13435(4) 0.77499(16) 0.37492(15) 0.0245(5) Uani 1 1 d . . . O6 O 0.15815(4) 0.85837(19) 0.48716(15) 0.0281(5) Uani 1 1 d . . . H6A H 0.1435 0.8687 0.5122 0.042 Uiso 1 1 calc R . . O8 O 0.10588(6) 0.7770(2) 0.20406(19) 0.0489(7) Uani 1 1 d . . . O18 O 0.12658(4) 0.25154(17) 0.43754(14) 0.0252(5) Uani 1 1 d . . . O19 O 0.09727(4) 0.32996(17) 0.34218(13) 0.0218(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0139(13) 0.0200(14) 0.0159(13) -0.0037(11) 0.0014(10) 0.0054(11) C2 0.0150(13) 0.0141(13) 0.0157(13) -0.0039(10) -0.0004(10) 0.0035(10) C3 0.0171(14) 0.0170(13) 0.0153(13) 0.0007(11) 0.0021(10) 0.0021(11) C4 0.0155(13) 0.0151(13) 0.0203(14) 0.0016(11) 0.0008(11) -0.0012(10) C5 0.0167(13) 0.0144(13) 0.0154(13) -0.0022(10) 0.0000(11) 0.0027(10) C6 0.0198(14) 0.0164(13) 0.0157(13) 0.0012(11) 0.0023(11) -0.0012(11) C7 0.0168(14) 0.0150(13) 0.0197(14) -0.0017(11) 0.0022(11) -0.0028(10) C8 0.0159(13) 0.0141(13) 0.0166(13) 0.0002(10) -0.0013(10) -0.0005(10) C9 0.0156(13) 0.0148(13) 0.0150(13) -0.0020(10) -0.0007(10) -0.0032(10) C10 0.0201(14) 0.0153(13) 0.0154(13) 0.0013(11) -0.0026(11) 0.0005(11) C11 0.0169(14) 0.0143(13) 0.0215(14) -0.0008(11) 0.0001(11) -0.0001(11) C12 0.0202(14) 0.0161(13) 0.0159(13) -0.0014(11) -0.0001(11) -0.0062(11) C13 0.0213(15) 0.0183(14) 0.0142(13) 0.0019(11) -0.0028(11) -0.0055(11) C14 0.0168(14) 0.0169(13) 0.0192(14) 0.0011(11) -0.0024(11) -0.0013(11) C15 0.0236(15) 0.0227(15) 0.0198(14) -0.0004(12) -0.0034(12) 0.0038(12) C16 0.0174(14) 0.0217(14) 0.0173(14) 0.0003(11) -0.0007(11) -0.0010(11) C17 0.0185(14) 0.0293(16) 0.0171(14) -0.0086(13) -0.0028(11) 0.0034(12) C18 0.0147(13) 0.0259(15) 0.0148(13) -0.0048(11) -0.0009(11) 0.0018(11) C19 0.0183(14) 0.0196(14) 0.0138(13) -0.0022(11) -0.0023(11) -0.0008(11) C20 0.0115(13) 0.0162(13) 0.0189(13) -0.0039(11) -0.0020(10) 0.0029(10) C21 0.0134(13) 0.0203(14) 0.0139(13) -0.0040(11) -0.0012(10) 0.0019(11) C22 0.0228(15) 0.0296(16) 0.0168(14) 0.0051(12) -0.0007(11) 0.0094(12) C23 0.0230(15) 0.0295(16) 0.0210(15) -0.0005(12) -0.0011(12) 0.0123(13) C24 0.019(2) 0.0171(19) 0.0139(18) 0.000 0.000 0.0039(15) C25 0.0176(14) 0.0193(14) 0.0149(13) 0.0001(11) 0.0010(11) -0.0007(11) C26 0.0171(14) 0.0145(13) 0.0198(14) 0.0001(11) -0.0010(11) -0.0021(11) C27 0.0149(13) 0.0171(13) 0.0198(14) -0.0010(11) 0.0003(11) -0.0024(10) C28 0.0189(14) 0.0195(14) 0.0192(14) -0.0035(11) 0.0012(11) -0.0035(11) C29 0.0175(14) 0.0160(13) 0.0293(16) -0.0003(12) 0.0047(12) -0.0011(11) C30 0.0146(14) 0.0279(16) 0.0297(16) -0.0009(13) -0.0015(12) 0.0054(12) C31 0.0170(15) 0.0313(17) 0.0227(15) -0.0043(13) -0.0043(12) 0.0029(12) C32 0.0226(16) 0.0282(17) 0.0339(18) -0.0056(14) 0.0063(13) 0.0025(13) C33 0.0253(16) 0.0180(14) 0.0197(14) -0.0017(11) -0.0025(12) -0.0028(12) C34 0.0296(16) 0.0168(14) 0.0240(15) 0.0003(12) -0.0086(13) -0.0033(12) C35 0.0196(15) 0.0219(15) 0.0305(16) -0.0017(13) -0.0100(13) 0.0021(12) C36 0.0168(14) 0.0199(14) 0.0270(15) -0.0040(12) -0.0029(12) 0.0008(11) C37 0.039(2) 0.0337(18) 0.0263(17) -0.0042(14) -0.0153(14) 0.0056(15) C38 0.0218(15) 0.0144(13) 0.0206(14) 0.0036(11) 0.0022(11) 0.0016(11) C39 0.0178(14) 0.0187(14) 0.0172(14) 0.0062(11) -0.0007(11) 0.0022(11) C40 0.0210(15) 0.0215(14) 0.0159(13) -0.0020(11) -0.0018(11) 0.0025(11) C41 0.0224(15) 0.0175(14) 0.0259(15) 0.0006(12) 0.0000(12) -0.0030(11) C42 0.0167(14) 0.0230(15) 0.0187(14) -0.0001(12) -0.0017(11) -0.0001(11) C43 0.0233(15) 0.0181(14) 0.0190(14) -0.0035(11) -0.0023(12) 0.0017(11) C44 0.0173(14) 0.0193(13) 0.0146(13) 0.0043(11) -0.0014(10) 0.0045(11) C45 0.017(2) 0.027(2) 0.0143(19) 0.000 0.000 0.0038(16) C46 0.0168(15) 0.0400(19) 0.0225(15) -0.0106(14) -0.0004(12) 0.0050(13) C48 0.0185(14) 0.0155(13) 0.0212(15) -0.0029(11) 0.0013(11) -0.0062(11) Cu1 0.01379(18) 0.02215(18) 0.01498(17) -0.00311(14) -0.00126(13) 0.00398(13) F1 0.0345(11) 0.0243(9) 0.0399(11) -0.0120(8) -0.0053(9) 0.0052(8) F2 0.0249(10) 0.0610(13) 0.0225(9) -0.0177(9) -0.0086(8) 0.0079(9) F3 0.0204(9) 0.0561(13) 0.0296(10) -0.0209(9) 0.0009(8) 0.0087(9) F4 0.0295(10) 0.0341(10) 0.0260(9) -0.0055(8) 0.0002(8) 0.0146(8) F5 0.0213(9) 0.0304(9) 0.0269(9) -0.0018(7) -0.0065(7) 0.0064(7) F6 0.0367(10) 0.0151(8) 0.0297(9) 0.0022(7) -0.0064(8) 0.0028(7) F7 0.0211(9) 0.0245(9) 0.0218(8) -0.0026(7) -0.0045(7) -0.0059(7) F8 0.0181(9) 0.0351(10) 0.0241(9) -0.0017(8) 0.0036(7) -0.0056(7) F9 0.0266(9) 0.0154(8) 0.0260(9) 0.0035(7) -0.0028(7) -0.0033(7) F10 0.0212(9) 0.0244(9) 0.0212(8) -0.0024(7) -0.0053(7) -0.0016(7) F11 0.0277(9) 0.0164(8) 0.0230(9) 0.0011(7) 0.0010(7) 0.0001(7) F12 0.0254(9) 0.0257(9) 0.0157(8) -0.0047(7) 0.0041(7) 0.0002(7) N1 0.0152(12) 0.0223(12) 0.0192(12) -0.0035(10) -0.0019(9) 0.0032(9) N2 0.0154(11) 0.0149(11) 0.0203(12) -0.0010(9) -0.0024(9) -0.0007(9) O1 0.0171(10) 0.0236(10) 0.0133(9) 0.0001(8) -0.0002(8) 0.0006(8) O2 0.0192(10) 0.0283(11) 0.0178(10) -0.0038(9) 0.0005(8) -0.0070(9) O3 0.0191(11) 0.0370(12) 0.0204(10) -0.0015(9) 0.0022(8) 0.0121(9) O4 0.0250(11) 0.0285(11) 0.0262(11) -0.0026(9) 0.0088(9) 0.0020(9) O5 0.0179(10) 0.0209(11) 0.0348(12) -0.0030(9) 0.0022(9) -0.0022(8) O6 0.0186(11) 0.0429(13) 0.0229(11) -0.0045(10) 0.0037(9) 0.0036(10) O8 0.0601(18) 0.0409(16) 0.0456(16) 0.0041(12) 0.0033(14) -0.0015(13) O18 0.0251(11) 0.0271(11) 0.0234(11) 0.0010(9) 0.0035(9) 0.0021(9) O19 0.0237(11) 0.0274(11) 0.0144(10) -0.0031(8) 0.0011(8) -0.0048(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.257(3) . ? C1 O1 1.266(3) . ? C1 C2 1.511(4) . ? C2 C7 1.389(4) . ? C2 C3 1.395(4) . ? C3 C4 1.389(4) . ? C4 C5 1.394(4) . ? C5 C6 1.399(4) . ? C5 C8 1.547(4) . ? C6 C7 1.383(4) . ? C8 C9 1.545(4) . ? C8 C16 1.547(4) . ? C8 C15 1.552(4) . ? C9 C14 1.398(4) . ? C9 C10 1.402(4) . ? C10 C11 1.378(4) . ? C11 C12 1.393(4) . ? C12 C13 1.396(4) . ? C12 C48 1.485(4) 1_554 ? C13 C14 1.390(4) . ? C15 F4 1.337(3) . ? C15 F6 1.341(3) . ? C15 F5 1.342(3) . ? C16 F9 1.336(3) . ? C16 F7 1.341(3) . ? C16 F8 1.346(3) . ? C17 O4 1.240(4) . ? C17 O3 1.275(4) . ? C17 C18 1.517(4) . ? C18 C23 1.380(4) . ? C18 C19 1.395(4) . ? C19 C20 1.390(4) . ? C20 C21 1.392(4) . ? C21 C22 1.395(4) . ? C21 C24 1.548(3) . ? C22 C23 1.393(4) . ? C24 C21 1.548(3) 2 ? C24 C25 1.551(3) . ? C24 C25 1.551(3) 2 ? C25 F10 1.334(3) . ? C25 F11 1.342(3) . ? C25 F12 1.347(3) . ? C26 N2 1.347(4) . ? C26 C33 1.385(4) . ? C26 C27 1.480(4) . ? C27 N1 1.347(3) . ? C27 C28 1.394(4) . ? C28 C29 1.392(4) . ? C29 C30 1.392(4) . ? C29 C32 1.495(4) . ? C30 C31 1.379(4) . ? C31 N1 1.339(4) . ? C33 C34 1.390(4) . ? C34 C35 1.386(4) . ? C34 C37 1.507(4) . ? C35 C36 1.385(4) . ? C36 N2 1.340(4) . ? C38 O5 1.217(3) . ? C38 O6 1.317(3) . ? C38 C39 1.490(4) . ? C39 C41 1.386(4) . ? C39 C40 1.392(4) . ? C40 C42 1.382(4) . ? C41 C43 1.384(4) . ? C42 C44 1.389(4) . ? C43 C44 1.395(4) . ? C44 C45 1.542(3) . ? C45 C44 1.542(3) 2_565 ? C45 C46 1.545(4) 2_565 ? C45 C46 1.545(4) . ? C46 F1 1.336(4) . ? C46 F2 1.337(3) . ? C46 F3 1.339(3) . ? C48 O19 1.224(3) . ? C48 O18 1.323(4) . ? C48 C12 1.485(4) 1_556 ? Cu1 O3 1.932(2) . ? Cu1 O1 1.9434(19) . ? Cu1 N1 2.001(2) . ? Cu1 N2 2.014(2) . ? Cu1 O19 2.321(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.8(2) . . ? O2 C1 C2 120.0(2) . . ? O1 C1 C2 116.3(2) . . ? C7 C2 C3 119.0(2) . . ? C7 C2 C1 121.2(2) . . ? C3 C2 C1 119.8(2) . . ? C4 C3 C2 120.4(2) . . ? C3 C4 C5 120.6(2) . . ? C4 C5 C6 118.5(2) . . ? C4 C5 C8 123.2(2) . . ? C6 C5 C8 118.2(2) . . ? C7 C6 C5 120.7(3) . . ? C6 C7 C2 120.6(2) . . ? C9 C8 C5 112.5(2) . . ? C9 C8 C16 105.3(2) . . ? C5 C8 C16 112.5(2) . . ? C9 C8 C15 112.5(2) . . ? C5 C8 C15 106.2(2) . . ? C16 C8 C15 107.9(2) . . ? C14 C9 C10 118.8(2) . . ? C14 C9 C8 122.2(2) . . ? C10 C9 C8 118.7(2) . . ? C11 C10 C9 121.0(2) . . ? C10 C11 C12 120.3(3) . . ? C11 C12 C13 119.2(3) . . ? C11 C12 C48 123.7(3) . 1_554 ? C13 C12 C48 117.1(2) . 1_554 ? C14 C13 C12 120.8(2) . . ? C13 C14 C9 120.0(3) . . ? F4 C15 F6 107.0(2) . . ? F4 C15 F5 106.4(2) . . ? F6 C15 F5 106.8(2) . . ? F4 C15 C8 111.8(2) . . ? F6 C15 C8 110.6(2) . . ? F5 C15 C8 113.8(2) . . ? F9 C16 F7 106.9(2) . . ? F9 C16 F8 107.3(2) . . ? F7 C16 F8 106.4(2) . . ? F9 C16 C8 110.9(2) . . ? F7 C16 C8 111.7(2) . . ? F8 C16 C8 113.2(2) . . ? O4 C17 O3 127.1(3) . . ? O4 C17 C18 118.9(3) . . ? O3 C17 C18 113.9(3) . . ? C23 C18 C19 118.8(3) . . ? C23 C18 C17 121.7(3) . . ? C19 C18 C17 119.5(3) . . ? C20 C19 C18 120.5(3) . . ? C19 C20 C21 120.8(2) . . ? C20 C21 C22 118.4(2) . . ? C20 C21 C24 118.3(2) . . ? C22 C21 C24 123.2(2) . . ? C23 C22 C21 120.5(3) . . ? C18 C23 C22 120.9(3) . . ? C21 C24 C21 111.6(3) . 2 ? C21 C24 C25 106.05(14) . . ? C21 C24 C25 112.63(14) 2 . ? C21 C24 C25 112.63(14) . 2 ? C21 C24 C25 106.04(14) 2 2 ? C25 C24 C25 107.9(3) . 2 ? F10 C25 F11 106.7(2) . . ? F10 C25 F12 106.6(2) . . ? F11 C25 F12 107.0(2) . . ? F10 C25 C24 112.0(2) . . ? F11 C25 C24 110.8(2) . . ? F12 C25 C24 113.4(2) . . ? N2 C26 C33 122.3(3) . . ? N2 C26 C27 114.7(2) . . ? C33 C26 C27 123.0(3) . . ? N1 C27 C28 121.5(3) . . ? N1 C27 C26 114.5(2) . . ? C28 C27 C26 124.0(2) . . ? C29 C28 C27 119.9(3) . . ? C28 C29 C30 117.3(3) . . ? C28 C29 C32 121.6(3) . . ? C30 C29 C32 121.0(3) . . ? C31 C30 C29 120.2(3) . . ? N1 C31 C30 122.1(3) . . ? C26 C33 C34 119.7(3) . . ? C35 C34 C33 117.6(3) . . ? C35 C34 C37 122.4(3) . . ? C33 C34 C37 120.0(3) . . ? C36 C35 C34 119.5(3) . . ? N2 C36 C35 122.8(3) . . ? O5 C38 O6 124.0(3) . . ? O5 C38 C39 121.9(3) . . ? O6 C38 C39 114.0(2) . . ? C41 C39 C40 119.3(3) . . ? C41 C39 C38 119.5(3) . . ? C40 C39 C38 121.1(3) . . ? C42 C40 C39 120.1(3) . . ? C43 C41 C39 120.5(3) . . ? C40 C42 C44 120.9(3) . . ? C41 C43 C44 120.4(3) . . ? C42 C44 C43 118.8(3) . . ? C42 C44 C45 117.7(2) . . ? C43 C44 C45 123.3(2) . . ? C44 C45 C44 111.6(3) . 2_565 ? C44 C45 C46 105.52(15) . 2_565 ? C44 C45 C46 112.90(16) 2_565 2_565 ? C44 C45 C46 112.90(16) . . ? C44 C45 C46 105.52(15) 2_565 . ? C46 C45 C46 108.5(3) 2_565 . ? F1 C46 F2 107.4(3) . . ? F1 C46 F3 106.6(2) . . ? F2 C46 F3 106.6(2) . . ? F1 C46 C45 111.1(2) . . ? F2 C46 C45 113.1(2) . . ? F3 C46 C45 111.8(2) . . ? O19 C48 O18 122.3(3) . . ? O19 C48 C12 121.9(3) . 1_556 ? O18 C48 C12 115.8(2) . 1_556 ? O3 Cu1 O1 91.72(8) . . ? O3 Cu1 N1 169.60(10) . . ? O1 Cu1 N1 92.20(9) . . ? O3 Cu1 N2 95.00(9) . . ? O1 Cu1 N2 173.15(9) . . ? N1 Cu1 N2 80.95(9) . . ? O3 Cu1 O19 103.71(8) . . ? O1 Cu1 O19 89.90(8) . . ? N1 Cu1 O19 85.93(9) . . ? N2 Cu1 O19 89.81(8) . . ? C31 N1 C27 119.0(2) . . ? C31 N1 Cu1 126.3(2) . . ? C27 N1 Cu1 114.66(18) . . ? C36 N2 C26 117.9(2) . . ? C36 N2 Cu1 127.5(2) . . ? C26 N2 Cu1 113.65(18) . . ? C1 O1 Cu1 118.87(17) . . ? C17 O3 Cu1 131.4(2) . . ? C48 O19 Cu1 118.84(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 10.2(4) . . . . ? O1 C1 C2 C7 -171.2(2) . . . . ? O2 C1 C2 C3 -169.4(2) . . . . ? O1 C1 C2 C3 9.2(4) . . . . ? C7 C2 C3 C4 1.9(4) . . . . ? C1 C2 C3 C4 -178.5(2) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C3 C4 C5 C6 -3.1(4) . . . . ? C3 C4 C5 C8 -179.7(2) . . . . ? C4 C5 C6 C7 2.3(4) . . . . ? C8 C5 C6 C7 179.0(2) . . . . ? C5 C6 C7 C2 0.6(4) . . . . ? C3 C2 C7 C6 -2.7(4) . . . . ? C1 C2 C7 C6 177.7(2) . . . . ? C4 C5 C8 C9 -138.7(3) . . . . ? C6 C5 C8 C9 44.8(3) . . . . ? C4 C5 C8 C16 -20.0(4) . . . . ? C6 C5 C8 C16 163.5(2) . . . . ? C4 C5 C8 C15 97.8(3) . . . . ? C6 C5 C8 C15 -78.7(3) . . . . ? C5 C8 C9 C14 -148.7(2) . . . . ? C16 C8 C9 C14 88.5(3) . . . . ? C15 C8 C9 C14 -28.8(3) . . . . ? C5 C8 C9 C10 37.1(3) . . . . ? C16 C8 C9 C10 -85.8(3) . . . . ? C15 C8 C9 C10 157.0(2) . . . . ? C14 C9 C10 C11 -0.2(4) . . . . ? C8 C9 C10 C11 174.3(2) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C10 C11 C12 C13 0.0(4) . . . . ? C10 C11 C12 C48 179.3(3) . . . 1_554 ? C11 C12 C13 C14 0.2(4) . . . . ? C48 C12 C13 C14 -179.2(2) 1_554 . . . ? C12 C13 C14 C9 -0.3(4) . . . . ? C10 C9 C14 C13 0.3(4) . . . . ? C8 C9 C14 C13 -174.0(2) . . . . ? C9 C8 C15 F4 -168.7(2) . . . . ? C5 C8 C15 F4 -45.2(3) . . . . ? C16 C8 C15 F4 75.5(3) . . . . ? C9 C8 C15 F6 -49.6(3) . . . . ? C5 C8 C15 F6 73.9(3) . . . . ? C16 C8 C15 F6 -165.3(2) . . . . ? C9 C8 C15 F5 70.7(3) . . . . ? C5 C8 C15 F5 -165.8(2) . . . . ? C16 C8 C15 F5 -45.0(3) . . . . ? C9 C8 C16 F9 72.1(3) . . . . ? C5 C8 C16 F9 -50.8(3) . . . . ? C15 C8 C16 F9 -167.6(2) . . . . ? C9 C8 C16 F7 -47.1(3) . . . . ? C5 C8 C16 F7 -170.0(2) . . . . ? C15 C8 C16 F7 73.2(3) . . . . ? C9 C8 C16 F8 -167.2(2) . . . . ? C5 C8 C16 F8 69.9(3) . . . . ? C15 C8 C16 F8 -46.8(3) . . . . ? O4 C17 C18 C23 167.5(3) . . . . ? O3 C17 C18 C23 -14.8(4) . . . . ? O4 C17 C18 C19 -14.0(4) . . . . ? O3 C17 C18 C19 163.7(3) . . . . ? C23 C18 C19 C20 1.5(4) . . . . ? C17 C18 C19 C20 -177.0(2) . . . . ? C18 C19 C20 C21 -0.3(4) . . . . ? C19 C20 C21 C22 -1.7(4) . . . . ? C19 C20 C21 C24 -178.8(2) . . . . ? C20 C21 C22 C23 2.5(4) . . . . ? C24 C21 C22 C23 179.4(3) . . . . ? C19 C18 C23 C22 -0.7(4) . . . . ? C17 C18 C23 C22 177.8(3) . . . . ? C21 C22 C23 C18 -1.3(5) . . . . ? C20 C21 C24 C21 -39.88(18) . . . 2 ? C22 C21 C24 C21 143.2(3) . . . 2 ? C20 C21 C24 C25 83.1(3) . . . . ? C22 C21 C24 C25 -93.8(3) . . . . ? C20 C21 C24 C25 -159.0(2) . . . 2 ? C22 C21 C24 C25 24.0(4) . . . 2 ? C21 C24 C25 F10 46.5(3) . . . . ? C21 C24 C25 F10 168.8(2) 2 . . . ? C25 C24 C25 F10 -74.44(18) 2 . . . ? C21 C24 C25 F11 -72.5(2) . . . . ? C21 C24 C25 F11 49.9(3) 2 . . . ? C25 C24 C25 F11 166.6(2) 2 . . . ? C21 C24 C25 F12 167.2(2) . . . . ? C21 C24 C25 F12 -70.4(3) 2 . . . ? C25 C24 C25 F12 46.27(15) 2 . . . ? N2 C26 C27 N1 7.6(4) . . . . ? C33 C26 C27 N1 -171.9(3) . . . . ? N2 C26 C27 C28 -172.1(3) . . . . ? C33 C26 C27 C28 8.4(4) . . . . ? N1 C27 C28 C29 -0.1(4) . . . . ? C26 C27 C28 C29 179.6(3) . . . . ? C27 C28 C29 C30 0.5(4) . . . . ? C27 C28 C29 C32 -179.9(3) . . . . ? C28 C29 C30 C31 -0.5(4) . . . . ? C32 C29 C30 C31 179.9(3) . . . . ? C29 C30 C31 N1 0.0(5) . . . . ? N2 C26 C33 C34 1.0(4) . . . . ? C27 C26 C33 C34 -179.6(3) . . . . ? C26 C33 C34 C35 2.4(4) . . . . ? C26 C33 C34 C37 -176.2(3) . . . . ? C33 C34 C35 C36 -3.3(4) . . . . ? C37 C34 C35 C36 175.3(3) . . . . ? C34 C35 C36 N2 0.9(4) . . . . ? O5 C38 C39 C41 -13.0(4) . . . . ? O6 C38 C39 C41 168.4(2) . . . . ? O5 C38 C39 C40 163.2(3) . . . . ? O6 C38 C39 C40 -15.4(4) . . . . ? C41 C39 C40 C42 0.4(4) . . . . ? C38 C39 C40 C42 -175.9(3) . . . . ? C40 C39 C41 C43 -0.7(4) . . . . ? C38 C39 C41 C43 175.6(3) . . . . ? C39 C40 C42 C44 0.5(4) . . . . ? C39 C41 C43 C44 0.2(4) . . . . ? C40 C42 C44 C43 -1.0(4) . . . . ? C40 C42 C44 C45 173.7(2) . . . . ? C41 C43 C44 C42 0.7(4) . . . . ? C41 C43 C44 C45 -173.7(2) . . . . ? C42 C44 C45 C44 44.47(19) . . . 2_565 ? C43 C44 C45 C44 -141.1(3) . . . 2_565 ? C42 C44 C45 C46 -78.5(3) . . . 2_565 ? C43 C44 C45 C46 95.9(3) . . . 2_565 ? C42 C44 C45 C46 163.2(3) . . . . ? C43 C44 C45 C46 -22.5(4) . . . . ? C44 C45 C46 F1 -50.5(3) . . . . ? C44 C45 C46 F1 71.7(3) 2_565 . . . ? C46 C45 C46 F1 -167.1(3) 2_565 . . . ? C44 C45 C46 F2 70.3(3) . . . . ? C44 C45 C46 F2 -167.5(2) 2_565 . . . ? C46 C45 C46 F2 -46.29(19) 2_565 . . . ? C44 C45 C46 F3 -169.4(2) . . . . ? C44 C45 C46 F3 -47.2(3) 2_565 . . . ? C46 C45 C46 F3 74.0(2) 2_565 . . . ? C30 C31 N1 C27 0.4(4) . . . . ? C30 C31 N1 Cu1 178.2(2) . . . . ? C28 C27 N1 C31 -0.4(4) . . . . ? C26 C27 N1 C31 179.9(3) . . . . ? C28 C27 N1 Cu1 -178.4(2) . . . . ? C26 C27 N1 Cu1 1.8(3) . . . . ? O3 Cu1 N1 C31 107.5(5) . . . . ? O1 Cu1 N1 C31 -4.6(3) . . . . ? N2 Cu1 N1 C31 175.2(3) . . . . ? O19 Cu1 N1 C31 -94.3(3) . . . . ? O3 Cu1 N1 C27 -74.6(6) . . . . ? O1 Cu1 N1 C27 173.3(2) . . . . ? N2 Cu1 N1 C27 -6.87(19) . . . . ? O19 Cu1 N1 C27 83.6(2) . . . . ? C35 C36 N2 C26 2.4(4) . . . . ? C35 C36 N2 Cu1 -165.6(2) . . . . ? C33 C26 N2 C36 -3.4(4) . . . . ? C27 C26 N2 C36 177.1(2) . . . . ? C33 C26 N2 Cu1 166.3(2) . . . . ? C27 C26 N2 Cu1 -13.2(3) . . . . ? O3 Cu1 N2 C36 -10.1(2) . . . . ? O1 Cu1 N2 C36 -179(9) . . . . ? N1 Cu1 N2 C36 179.6(3) . . . . ? O19 Cu1 N2 C36 93.7(2) . . . . ? O3 Cu1 N2 C26 -178.56(19) . . . . ? O1 Cu1 N2 C26 12.8(8) . . . . ? N1 Cu1 N2 C26 11.10(19) . . . . ? O19 Cu1 N2 C26 -74.81(19) . . . . ? O2 C1 O1 Cu1 -7.8(3) . . . . ? C2 C1 O1 Cu1 173.68(16) . . . . ? O3 Cu1 O1 C1 -69.1(2) . . . . ? N1 Cu1 O1 C1 101.3(2) . . . . ? N2 Cu1 O1 C1 99.6(7) . . . . ? O19 Cu1 O1 C1 -172.80(19) . . . . ? O4 C17 O3 Cu1 0.2(5) . . . . ? C18 C17 O3 Cu1 -177.24(18) . . . . ? O1 Cu1 O3 C17 -113.6(3) . . . . ? N1 Cu1 O3 C17 134.3(5) . . . . ? N2 Cu1 O3 C17 67.7(3) . . . . ? O19 Cu1 O3 C17 -23.3(3) . . . . ? O18 C48 O19 Cu1 -72.7(3) . . . . ? C12 C48 O19 Cu1 104.5(3) 1_556 . . . ? O3 Cu1 O19 C48 88.6(2) . . . . ? O1 Cu1 O19 C48 -179.6(2) . . . . ? N1 Cu1 O19 C48 -87.4(2) . . . . ? N2 Cu1 O19 C48 -6.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.708 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.086 data_F-MOF4 _database_code_depnum_ccdc_archive 'CCDC 745106' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'F-MOF 4' _chemical_melting_point ? _chemical_formula_moiety '2(C23 H15 Cu F6 N O4), 0.82(C6 H6 N), 3(C3 H7 N O)' _chemical_formula_sum 'C59.94 H55.94 Cu2 F12 N5.82 O11' _chemical_formula_weight 1389.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.643(8) _cell_length_b 11.004(3) _cell_length_c 24.351(7) _cell_angle_alpha 90.00 _cell_angle_beta 115.518(5) _cell_angle_gamma 90.00 _cell_volume 6201(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5776 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.36 _exptl_crystal_description Cubic _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2842 _exptl_absorpt_coefficient_mu 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8588 _exptl_absorpt_correction_T_max 0.8716 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'phi and omega scans' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44864 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 26.06 _reflns_number_total 12226 _reflns_number_gt 7364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^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 12226 _refine_ls_number_parameters 804 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0990 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.43389(16) 0.9521(3) 0.38938(17) 0.0145(8) Uani 1 1 d . . . C2 C 0.39531(15) 0.9138(3) 0.32562(17) 0.0145(8) Uani 1 1 d . . . C3 C 0.34683(16) 0.9811(3) 0.28998(18) 0.0209(9) Uani 1 1 d . . . H3 H 0.3385 1.0518 0.3056 0.025 Uiso 1 1 calc R . . C4 C 0.31041(16) 0.9447(3) 0.23119(17) 0.0200(9) Uani 1 1 d . . . H4 H 0.2779 0.9908 0.2081 0.024 Uiso 1 1 calc R . . C5 C 0.32203(15) 0.8396(3) 0.20637(17) 0.0149(8) Uani 1 1 d . . . C6 C 0.37094(16) 0.7718(3) 0.24347(17) 0.0179(9) Uani 1 1 d . . . H6 H 0.3793 0.7004 0.2284 0.021 Uiso 1 1 calc R . . C7 C 0.40676(16) 0.8083(3) 0.30142(17) 0.0170(9) Uani 1 1 d . . . H7 H 0.4391 0.7619 0.3248 0.020 Uiso 1 1 calc R . . C8 C 0.28279(15) 0.7908(3) 0.14247(17) 0.0172(9) Uani 1 1 d . . . C9 C 0.31887(15) 0.7327(3) 0.11239(16) 0.0149(8) Uani 1 1 d . . . C10 C 0.30530(16) 0.6225(3) 0.08120(17) 0.0193(9) Uani 1 1 d . . . H10 H 0.2726 0.5799 0.0773 0.023 Uiso 1 1 calc R . . C11 C 0.34030(16) 0.5760(3) 0.05590(17) 0.0187(9) Uani 1 1 d . . . H11 H 0.3313 0.5016 0.0358 0.022 Uiso 1 1 calc R . . C12 C 0.38877(16) 0.6399(3) 0.06031(17) 0.0168(9) Uani 1 1 d . . . C13 C 0.40194(16) 0.7504(3) 0.09053(16) 0.0162(9) Uani 1 1 d . . . H13 H 0.4340 0.7941 0.0934 0.019 Uiso 1 1 calc R . . C14 C 0.36759(16) 0.7957(3) 0.11639(17) 0.0190(9) Uani 1 1 d . . . H14 H 0.3771 0.8696 0.1369 0.023 Uiso 1 1 calc R . . C15 C 0.42827(16) 0.5876(3) 0.03451(17) 0.0158(9) Uani 1 1 d . . . C16 C 0.21461(16) 0.6860(3) 0.36079(17) 0.0180(9) Uani 1 1 d . . . C17 C 0.24630(18) 0.5821(4) 0.40465(19) 0.0272(11) Uani 1 1 d . . . C18 C 0.25989(17) 0.7679(4) 0.3529(2) 0.0273(10) Uani 1 1 d . . . C19 C 0.17983(16) 0.7542(3) 0.38996(17) 0.0179(9) Uani 1 1 d . . . C20 C 0.12887(15) 0.7000(3) 0.38525(17) 0.0175(9) Uani 1 1 d . . . H20 H 0.1168 0.6270 0.3644 0.021 Uiso 1 1 calc R . . C21 C 0.09632(16) 0.7534(3) 0.41116(17) 0.0190(9) Uani 1 1 d . . . H21 H 0.0629 0.7152 0.4084 0.023 Uiso 1 1 calc R . . C22 C 0.11291(15) 0.8636(3) 0.44129(17) 0.0145(8) Uani 1 1 d . . . C23 C 0.16302(16) 0.9183(4) 0.44600(17) 0.0207(9) Uani 1 1 d . . . H23 H 0.1741 0.9929 0.4656 0.025 Uiso 1 1 calc R . . C24 C 0.19717(17) 0.8627(4) 0.42157(18) 0.0223(10) Uani 1 1 d . . . H24 H 0.2318 0.8985 0.4265 0.027 Uiso 1 1 calc R . . C25 C 0.07475(15) 0.9206(3) 0.46711(17) 0.0168(9) Uani 1 1 d . . . C26 C 0.17448(15) 0.6402(3) 0.29655(17) 0.0152(8) Uani 1 1 d . . . C27 C 0.12882(16) 0.7159(3) 0.25917(17) 0.0173(9) Uani 1 1 d . . . H27 H 0.1228 0.7894 0.2744 0.021 Uiso 1 1 calc R . . C28 C 0.09286(15) 0.6831(3) 0.20038(17) 0.0148(8) Uani 1 1 d . . . H28 H 0.0623 0.7336 0.1767 0.018 Uiso 1 1 calc R . . C29 C 0.10181(15) 0.5747(3) 0.17596(17) 0.0152(9) Uani 1 1 d . . . C30 C 0.14644(16) 0.4985(3) 0.21256(17) 0.0193(9) Uani 1 1 d . . . H30 H 0.1523 0.4252 0.1971 0.023 Uiso 1 1 calc R . . C31 C 0.18246(16) 0.5311(3) 0.27228(18) 0.0206(9) Uani 1 1 d . . . H31 H 0.2122 0.4793 0.2963 0.025 Uiso 1 1 calc R . . C32 C 0.06461(16) 0.5432(3) 0.11114(18) 0.0168(9) Uani 1 1 d . . . C33 C 0.44352(15) 1.3688(3) 0.45117(17) 0.0159(9) Uani 1 1 d . . . H33 H 0.4595 1.3462 0.4249 0.019 Uiso 1 1 calc R . . C34 C 0.41579(16) 1.3167(3) 0.52567(18) 0.0208(9) Uani 1 1 d . . . H34 H 0.4115 1.2582 0.5510 0.025 Uiso 1 1 calc R . . C35 C 0.39828(17) 1.4345(4) 0.52848(19) 0.0282(10) Uani 1 1 d . . . H35 H 0.3829 1.4552 0.5555 0.034 Uiso 1 1 calc R . . C36 C 0.40415(17) 1.5205(4) 0.49035(19) 0.0262(10) Uani 1 1 d . . . H36 H 0.3932 1.6004 0.4920 0.031 Uiso 1 1 calc R . . C37 C 0.42624(16) 1.4884(3) 0.44978(18) 0.0209(9) Uani 1 1 d . . . C38 C 0.43039(18) 1.5776(4) 0.4051(2) 0.0304(11) Uani 1 1 d . . . H38A H 0.3936 1.5837 0.3704 0.046 Uiso 1 1 calc R . . H38B H 0.4589 1.5501 0.3922 0.046 Uiso 1 1 calc R . . H38C H 0.4413 1.6558 0.4241 0.046 Uiso 1 1 calc R . . C39 C 0.06986(15) 0.1502(3) 0.06772(18) 0.0181(9) Uani 1 1 d . . . H39 H 0.0728 0.1947 0.1014 0.022 Uiso 1 1 calc R . . C40 C 0.08198(16) 0.0267(3) 0.0753(2) 0.0246(10) Uani 1 1 d . . . C41 C 0.07748(17) -0.0370(4) 0.0248(2) 0.0308(11) Uani 1 1 d . . . H41 H 0.0848 -0.1201 0.0274 0.037 Uiso 1 1 calc R . . C42 C 0.06193(18) 0.0232(4) -0.0299(2) 0.0370(12) Uani 1 1 d . . . H42 H 0.0593 -0.0185 -0.0642 0.044 Uiso 1 1 calc R . . C43 C 0.05036(17) 0.1458(4) -0.0328(2) 0.0269(10) Uani 1 1 d . . . H43 H 0.0394 0.1860 -0.0697 0.032 Uiso 1 1 calc R . . C44 C 0.09784(19) -0.0316(4) 0.1360(2) 0.0413(13) Uani 1 1 d . . . H44A H 0.0646 -0.0333 0.1445 0.062 Uiso 1 1 calc R . . H44B H 0.1281 0.0144 0.1669 0.062 Uiso 1 1 calc R . . H44C H 0.1110 -0.1130 0.1354 0.062 Uiso 1 1 calc R . . C45 C 0.4347(5) 0.1288(11) 0.2006(6) 0.175(5) Uiso 0.824(4) 1 d P . . H45A H 0.3948 0.1052 0.1808 0.263 Uiso 0.824(4) 1 calc PR . . H45B H 0.4551 0.0749 0.2341 0.263 Uiso 0.824(4) 1 calc PR . . H45C H 0.4513 0.1245 0.1721 0.263 Uiso 0.824(4) 1 calc PR . . C47 C 0.4392(3) 0.2593(7) 0.2244(4) 0.075(2) Uiso 0.824(4) 1 d PD . . C48 C 0.4401(3) 0.3606(8) 0.1900(4) 0.095(3) Uiso 0.824(4) 1 d PD . . H47 H 0.4293 0.3498 0.1487 0.114 Uiso 0.824(4) 1 calc PR . . C49 C 0.4553(5) 0.4697(12) 0.2129(6) 0.160(5) Uiso 0.824(4) 1 d PD . . H48 H 0.4548 0.5376 0.1899 0.192 Uiso 0.824(4) 1 calc PR . . C50 C 0.4756(6) 0.4733(14) 0.2868(8) 0.203(6) Uiso 0.824(4) 1 d PD . . C46 C 0.4514(3) 0.2637(8) 0.2853(4) 0.094(3) Uiso 0.824(4) 1 d PD . . H50 H 0.4511 0.1949 0.3073 0.112 Uiso 0.824(4) 1 calc PR . . N21 N 0.4640(3) 0.3752(7) 0.3105(3) 0.095(2) Uiso 0.824(4) 1 d PD . . C51 C 0.1981(3) 0.2267(6) 0.0126(3) 0.086(2) Uani 1 1 d . . . H51A H 0.2215 0.2084 -0.0082 0.128 Uiso 1 1 calc R . . H51B H 0.1681 0.2826 -0.0113 0.128 Uiso 1 1 calc R . . H51C H 0.1810 0.1532 0.0185 0.128 Uiso 1 1 calc R . . C52 C 0.2050(2) 0.3105(5) 0.1095(3) 0.0683(18) Uani 1 1 d . . . H52A H 0.1893 0.2372 0.1178 0.102 Uiso 1 1 calc R . . H52B H 0.1742 0.3665 0.0880 0.102 Uiso 1 1 calc R . . H52C H 0.2315 0.3465 0.1471 0.102 Uiso 1 1 calc R . . C53 C 0.2901(3) 0.2923(5) 0.0937(4) 0.090(3) Uani 1 1 d . . . H53 H 0.3113 0.3182 0.1336 0.108 Uiso 1 1 calc R . . C54 C 0.0538(2) 0.2450(5) 0.2182(2) 0.0605(16) Uani 1 1 d . . . H54A H 0.0324 0.1702 0.2093 0.091 Uiso 1 1 calc R . . H54B H 0.0928 0.2290 0.2245 0.091 Uiso 1 1 calc R . . H54C H 0.0360 0.3001 0.1846 0.091 Uiso 1 1 calc R . . C55 C 0.0803(3) 0.2288(9) 0.3293(3) 0.162(5) Uani 1 1 d . . . H55A H 0.0708 0.2645 0.3598 0.243 Uiso 1 1 calc R . . H55B H 0.1215 0.2282 0.3435 0.243 Uiso 1 1 calc R . . H55C H 0.0660 0.1470 0.3215 0.243 Uiso 1 1 calc R . . C56 C 0.0304(3) 0.4046(6) 0.2736(3) 0.074(2) Uani 1 1 d . . . H56 H 0.0135 0.4454 0.2366 0.089 Uiso 1 1 calc R . . C57 C 0.3126(2) 0.2944(4) 0.3187(3) 0.0606(17) Uani 1 1 d . . . H57A H 0.3492 0.2542 0.3316 0.091 Uiso 1 1 calc R . . H57B H 0.3181 0.3723 0.3382 0.091 Uiso 1 1 calc R . . H57C H 0.2957 0.3053 0.2754 0.091 Uiso 1 1 calc R . . C58 C 0.2930(2) 0.1860(5) 0.3983(2) 0.0675(19) Uani 1 1 d . . . H58A H 0.2631 0.1402 0.4025 0.101 Uiso 1 1 calc R . . H58B H 0.3012 0.2577 0.4231 0.101 Uiso 1 1 calc R . . H58C H 0.3273 0.1372 0.4112 0.101 Uiso 1 1 calc R . . C59 C 0.2240(2) 0.1802(4) 0.2920(3) 0.0443(13) Uani 1 1 d . . . H59 H 0.2017 0.1305 0.3043 0.053 Uiso 1 1 calc R . . C60 C 0.24057(16) 0.7013(4) 0.15090(19) 0.0226(10) Uani 1 1 d . . . C61 C 0.24681(17) 0.8939(4) 0.09848(19) 0.0245(10) Uani 1 1 d . . . Cu1 Cu 0.473028(18) 1.10608(4) 0.49159(2) 0.01242(13) Uani 1 1 d . . . Cu2 Cu 0.026190(18) 0.39320(4) 0.00674(2) 0.01246(13) Uani 1 1 d . . . F1 F 0.27408(10) 0.6207(2) 0.46198(10) 0.0363(7) Uani 1 1 d . . . F2 F 0.20979(10) 0.4946(2) 0.40406(10) 0.0318(6) Uani 1 1 d . . . F3 F 0.28630(10) 0.5280(2) 0.39048(10) 0.0363(7) Uani 1 1 d . . . F4 F 0.30381(9) 0.8003(2) 0.40649(11) 0.0358(7) Uani 1 1 d . . . F5 F 0.28376(9) 0.7140(2) 0.32013(10) 0.0326(6) Uani 1 1 d . . . F6 F 0.23592(10) 0.8717(2) 0.32393(11) 0.0300(6) Uani 1 1 d . . . F24 F 0.20652(9) 0.9414(2) 0.11357(10) 0.0294(6) Uani 1 1 d . . . F25 F 0.21911(9) 0.8533(2) 0.04143(10) 0.0292(6) Uani 1 1 d . . . F26 F 0.28069(9) 0.9858(2) 0.09773(10) 0.0274(6) Uani 1 1 d . . . F30 F 0.26871(9) 0.6007(2) 0.18030(10) 0.0272(6) Uani 1 1 d . . . F31 F 0.19761(9) 0.6644(2) 0.09807(10) 0.0314(6) Uani 1 1 d . . . F32 F 0.21556(9) 0.7494(2) 0.18374(10) 0.0277(6) Uani 1 1 d . . . N1 N 0.05435(13) 0.2086(3) 0.01532(14) 0.0167(7) Uani 1 1 d . . . N5 N 0.43864(12) 1.2838(3) 0.48800(14) 0.0144(7) Uani 1 1 d . . . N10 N 0.0541(2) 0.2996(5) 0.2734(2) 0.0639(14) Uani 1 1 d . . . N11 N 0.27423(16) 0.2205(3) 0.3353(2) 0.0428(11) Uani 1 1 d . . . N13 N 0.2348(2) 0.2826(3) 0.0730(2) 0.0502(12) Uani 1 1 d . . . O1 O 0.08299(10) 1.0310(2) 0.48287(12) 0.0207(6) Uani 1 1 d . . . O2 O 0.03707(11) 0.8530(2) 0.47044(12) 0.0226(7) Uani 1 1 d . . . O3 O 0.07285(11) 0.4424(2) 0.09139(11) 0.0204(6) Uani 1 1 d . . . O4 O 0.02723(11) 0.6203(2) 0.08007(12) 0.0207(6) Uani 1 1 d . . . O5 O 0.47246(11) 0.8780(2) 0.42160(12) 0.0206(6) Uani 1 1 d . . . O6 O 0.42503(11) 1.0549(2) 0.40710(12) 0.0234(7) Uani 1 1 d . . . O7 O 0.46651(11) 0.6561(2) 0.03328(12) 0.0212(6) Uani 1 1 d . . . O8 O 0.41949(10) 0.4782(2) 0.01680(12) 0.0217(6) Uani 1 1 d . . . O10 O 0.3161(2) 0.2680(4) 0.0618(3) 0.130(2) Uani 1 1 d . . . O11 O 0.0279(2) 0.4553(5) 0.3174(2) 0.0985(16) Uani 1 1 d . . . O9A O 0.20511(15) 0.2034(3) 0.23760(18) 0.0591(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(2) 0.017(2) 0.014(2) -0.0001(18) 0.0106(18) -0.0031(17) C2 0.017(2) 0.014(2) 0.014(2) 0.0001(17) 0.0076(18) -0.0008(16) C3 0.024(2) 0.019(2) 0.020(2) -0.0043(18) 0.009(2) 0.0042(18) C4 0.019(2) 0.022(2) 0.015(2) -0.0020(18) 0.0032(19) 0.0074(17) C5 0.017(2) 0.017(2) 0.014(2) -0.0011(17) 0.0101(18) -0.0023(16) C6 0.023(2) 0.015(2) 0.016(2) -0.0003(18) 0.0095(19) 0.0029(17) C7 0.020(2) 0.017(2) 0.013(2) 0.0024(17) 0.0064(19) 0.0024(17) C8 0.014(2) 0.025(2) 0.012(2) -0.0028(18) 0.0055(18) 0.0003(17) C9 0.016(2) 0.020(2) 0.008(2) -0.0002(17) 0.0049(17) 0.0052(16) C10 0.0124(19) 0.025(2) 0.017(2) -0.0058(18) 0.0027(18) -0.0055(17) C11 0.024(2) 0.015(2) 0.016(2) -0.0056(17) 0.0077(19) -0.0001(17) C12 0.020(2) 0.018(2) 0.011(2) 0.0028(17) 0.0054(18) 0.0048(17) C13 0.018(2) 0.017(2) 0.013(2) 0.0020(17) 0.0059(18) -0.0016(17) C14 0.027(2) 0.013(2) 0.019(2) -0.0014(18) 0.012(2) 0.0021(17) C15 0.018(2) 0.016(2) 0.011(2) 0.0020(17) 0.0035(18) 0.0057(17) C16 0.017(2) 0.024(2) 0.012(2) -0.0025(18) 0.0050(18) 0.0015(17) C17 0.025(2) 0.043(3) 0.012(2) 0.000(2) 0.007(2) 0.016(2) C18 0.018(2) 0.043(3) 0.020(3) -0.013(2) 0.008(2) 0.003(2) C19 0.018(2) 0.022(2) 0.014(2) -0.0008(18) 0.0066(19) 0.0029(17) C20 0.021(2) 0.016(2) 0.014(2) -0.0026(17) 0.0064(19) -0.0002(17) C21 0.017(2) 0.019(2) 0.022(2) 0.0027(18) 0.0096(19) -0.0006(17) C22 0.018(2) 0.015(2) 0.012(2) 0.0029(17) 0.0074(18) 0.0063(16) C23 0.024(2) 0.023(2) 0.015(2) -0.0049(18) 0.008(2) -0.0021(18) C24 0.019(2) 0.030(2) 0.019(2) -0.0040(19) 0.009(2) -0.0031(18) C25 0.017(2) 0.017(2) 0.015(2) 0.0032(18) 0.0054(19) 0.0037(17) C26 0.016(2) 0.021(2) 0.009(2) -0.0032(17) 0.0067(18) -0.0016(16) C27 0.022(2) 0.015(2) 0.016(2) -0.0035(18) 0.0097(19) 0.0007(17) C28 0.015(2) 0.015(2) 0.014(2) 0.0009(17) 0.0065(18) -0.0009(16) C29 0.017(2) 0.015(2) 0.014(2) 0.0024(17) 0.0068(18) -0.0017(16) C30 0.027(2) 0.018(2) 0.014(2) -0.0039(18) 0.0094(19) 0.0049(18) C31 0.021(2) 0.024(2) 0.018(2) 0.0016(19) 0.0089(19) 0.0088(17) C32 0.017(2) 0.019(2) 0.017(2) 0.0002(19) 0.0091(19) -0.0036(17) C33 0.0135(19) 0.017(2) 0.013(2) -0.0039(17) 0.0010(18) -0.0035(16) C34 0.023(2) 0.020(2) 0.022(2) 0.0038(18) 0.011(2) 0.0039(17) C35 0.031(2) 0.031(3) 0.024(3) -0.008(2) 0.014(2) 0.008(2) C36 0.025(2) 0.014(2) 0.030(3) -0.007(2) 0.003(2) 0.0062(18) C37 0.017(2) 0.014(2) 0.018(2) -0.0022(18) -0.0050(18) 0.0002(17) C38 0.029(2) 0.018(2) 0.038(3) 0.007(2) 0.009(2) 0.0002(19) C39 0.0096(19) 0.019(2) 0.024(2) -0.0011(19) 0.0055(18) -0.0012(16) C40 0.018(2) 0.016(2) 0.040(3) 0.010(2) 0.012(2) 0.0037(17) C41 0.021(2) 0.014(2) 0.054(3) -0.005(2) 0.012(2) 0.0010(18) C42 0.033(3) 0.027(3) 0.046(3) -0.013(2) 0.012(3) 0.007(2) C43 0.023(2) 0.027(2) 0.029(3) -0.006(2) 0.010(2) 0.0038(19) C44 0.040(3) 0.031(3) 0.061(4) 0.026(3) 0.029(3) 0.014(2) C51 0.115(6) 0.065(5) 0.068(5) -0.005(4) 0.032(5) 0.014(4) C52 0.050(4) 0.083(5) 0.084(5) -0.014(4) 0.039(4) -0.006(3) C53 0.084(5) 0.052(4) 0.188(8) -0.032(4) 0.109(6) -0.022(3) C54 0.057(4) 0.074(4) 0.057(4) -0.014(3) 0.031(3) -0.003(3) C55 0.147(8) 0.286(13) 0.054(5) 0.050(7) 0.045(6) 0.149(8) C56 0.079(5) 0.085(5) 0.072(5) -0.014(4) 0.046(4) -0.004(4) C57 0.041(3) 0.041(3) 0.093(5) -0.032(3) 0.023(3) -0.006(3) C58 0.049(4) 0.088(5) 0.038(4) -0.025(3) -0.007(3) 0.018(3) C59 0.033(3) 0.037(3) 0.050(4) -0.003(3) 0.006(3) 0.008(2) C60 0.017(2) 0.032(3) 0.021(2) -0.009(2) 0.010(2) -0.0051(19) C61 0.020(2) 0.035(3) 0.020(2) -0.004(2) 0.009(2) 0.0056(19) Cu1 0.0154(2) 0.0107(2) 0.0116(3) -0.0004(2) 0.0062(2) -0.00014(19) Cu2 0.0154(3) 0.0108(2) 0.0124(3) -0.0003(2) 0.0072(2) -0.00066(19) F1 0.0329(14) 0.0559(17) 0.0138(14) -0.0030(12) 0.0042(12) 0.0213(12) F2 0.0377(15) 0.0299(14) 0.0260(15) 0.0068(11) 0.0121(13) 0.0134(12) F3 0.0276(13) 0.0561(17) 0.0191(14) -0.0067(12) 0.0043(12) 0.0249(12) F4 0.0163(12) 0.0613(18) 0.0264(15) -0.0202(13) 0.0061(12) -0.0067(12) F5 0.0241(13) 0.0539(17) 0.0268(15) -0.0144(12) 0.0177(12) -0.0013(12) F6 0.0324(14) 0.0332(15) 0.0308(15) -0.0057(12) 0.0197(13) -0.0081(11) F24 0.0189(12) 0.0476(15) 0.0199(14) -0.0023(12) 0.0068(11) 0.0134(11) F25 0.0269(13) 0.0427(15) 0.0123(13) -0.0044(11) 0.0029(11) 0.0078(11) F26 0.0293(13) 0.0271(14) 0.0271(15) 0.0058(11) 0.0135(12) 0.0070(11) F30 0.0311(13) 0.0247(13) 0.0290(15) -0.0018(11) 0.0159(12) -0.0065(11) F31 0.0214(13) 0.0476(16) 0.0257(15) -0.0168(12) 0.0104(12) -0.0123(11) F32 0.0260(13) 0.0408(15) 0.0245(14) -0.0098(11) 0.0186(12) -0.0071(11) N1 0.0186(17) 0.0150(17) 0.0175(19) 0.0003(15) 0.0085(16) -0.0002(14) N5 0.0134(16) 0.0120(16) 0.0166(19) 0.0003(14) 0.0053(15) 0.0017(13) N10 0.050(3) 0.098(4) 0.045(3) -0.003(3) 0.022(3) 0.014(3) N11 0.025(2) 0.041(3) 0.051(3) -0.018(2) 0.005(2) 0.0067(19) N13 0.064(3) 0.030(2) 0.069(4) -0.005(2) 0.041(3) -0.009(2) O1 0.0225(15) 0.0194(15) 0.0245(17) -0.0067(13) 0.0143(14) -0.0013(12) O2 0.0258(15) 0.0152(14) 0.0366(19) 0.0002(13) 0.0227(15) 0.0005(12) O3 0.0282(16) 0.0167(15) 0.0134(16) 0.0002(12) 0.0061(13) 0.0045(12) O4 0.0250(15) 0.0173(15) 0.0152(16) -0.0033(12) 0.0042(13) 0.0040(12) O5 0.0251(15) 0.0165(15) 0.0156(16) 0.0012(12) 0.0045(13) 0.0059(12) O6 0.0287(16) 0.0176(15) 0.0169(16) -0.0059(13) 0.0032(14) 0.0064(12) O7 0.0263(15) 0.0157(14) 0.0312(18) -0.0033(13) 0.0217(14) -0.0023(12) O8 0.0222(15) 0.0173(15) 0.0306(18) -0.0056(13) 0.0161(14) 0.0004(12) O10 0.133(4) 0.074(3) 0.260(7) -0.042(4) 0.157(5) -0.026(3) O11 0.104(4) 0.121(4) 0.085(4) -0.040(3) 0.054(3) -0.012(3) O9A 0.048(2) 0.060(3) 0.049(3) -0.003(2) 0.001(2) -0.0041(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O5 1.261(4) . ? C1 O6 1.266(4) . ? C1 C2 1.498(5) . ? C2 C3 1.385(5) . ? C2 C7 1.389(5) . ? C3 C4 1.389(5) . ? C3 H3 0.9300 . ? C4 C5 1.395(5) . ? C4 H4 0.9300 . ? C5 C6 1.403(5) . ? C5 C8 1.540(5) . ? C6 C7 1.371(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C60 1.541(5) . ? C8 C9 1.544(5) . ? C8 C61 1.561(5) . ? C9 C10 1.393(5) . ? C9 C14 1.395(5) . ? C10 C11 1.387(5) . ? C10 H10 0.9300 . ? C11 C12 1.391(5) . ? C11 H11 0.9300 . ? C12 C13 1.386(5) . ? C12 C15 1.517(5) . ? C13 C14 1.378(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O7 1.247(4) . ? C15 O8 1.266(4) . ? C16 C17 1.537(5) . ? C16 C26 1.541(5) . ? C16 C18 1.546(5) . ? C16 C19 1.552(5) . ? C17 F1 1.334(4) . ? C17 F2 1.339(5) . ? C17 F3 1.353(4) . ? C18 F5 1.335(4) . ? C18 F6 1.344(5) . ? C18 F4 1.354(4) . ? C19 C24 1.385(5) . ? C19 C20 1.396(5) . ? C20 C21 1.376(5) . ? C20 H20 0.9300 . ? C21 C22 1.386(5) . ? C21 H21 0.9300 . ? C22 C23 1.378(5) . ? C22 C25 1.509(5) . ? C23 C24 1.395(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O2 1.250(4) . ? C25 O1 1.264(4) . ? C26 C31 1.392(5) . ? C26 C27 1.405(5) . ? C27 C28 1.376(5) . ? C27 H27 0.9300 . ? C28 C29 1.395(5) . ? C28 H28 0.9300 . ? C29 C30 1.388(5) . ? C29 C32 1.491(5) . ? C30 C31 1.392(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 O4 1.259(4) . ? C32 O3 1.263(4) . ? C33 N5 1.339(4) . ? C33 C37 1.384(5) . ? C33 H33 0.9300 . ? C34 N5 1.334(4) . ? C34 C35 1.384(5) . ? C34 H34 0.9300 . ? C35 C36 1.379(6) . ? C35 H35 0.9300 . ? C36 C37 1.380(5) . ? C36 H36 0.9300 . ? C37 C38 1.503(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N1 1.327(5) . ? C39 C40 1.389(5) . ? C39 H39 0.9300 . ? C40 C41 1.376(6) . ? C40 C44 1.497(6) . ? C41 C42 1.383(6) . ? C41 H41 0.9300 . ? C42 C43 1.377(5) . ? C42 H42 0.9300 . ? C43 N1 1.325(5) . ? C43 H43 0.9300 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C47 1.535(12) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C47 C46 1.379(10) . ? C47 C48 1.399(10) . ? C48 C49 1.311(12) . ? C48 H47 0.9300 . ? C49 C50 1.645(16) . ? C49 H48 0.9300 . ? C50 N21 1.316(15) . ? C46 N21 1.347(10) . ? C46 H50 0.9300 . ? C51 N13 1.496(7) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 N13 1.432(6) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 O10 1.251(7) . ? C53 N13 1.289(7) . ? C53 H53 0.9300 . ? C54 N10 1.470(6) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N10 1.458(8) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 O11 1.229(7) . ? C56 N10 1.306(7) . ? C56 H56 0.9300 . ? C57 N11 1.460(6) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 N11 1.448(6) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 O9A 1.226(6) . ? C59 N11 1.340(6) . ? C59 H59 0.9300 . ? C60 F32 1.332(4) . ? C60 F31 1.347(4) . ? C60 F30 1.347(4) . ? C61 F25 1.335(4) . ? C61 F26 1.338(4) . ? C61 F24 1.343(4) . ? Cu1 O8 1.962(2) 4_576 ? Cu1 O7 1.970(2) 2_655 ? Cu1 O6 1.971(3) . ? Cu1 O5 1.977(3) 3_676 ? Cu1 N5 2.131(3) . ? Cu1 Cu1 2.6539(10) 3_676 ? Cu2 O3 1.962(3) . ? Cu2 O4 1.968(3) 3_565 ? Cu2 O1 1.971(2) 4_575 ? Cu2 O2 1.978(2) 2_545 ? Cu2 N1 2.136(3) . ? Cu2 Cu2 2.6564(10) 3_565 ? O1 Cu2 1.971(2) 4_576 ? O2 Cu2 1.978(2) 2 ? O4 Cu2 1.968(3) 3_565 ? O5 Cu1 1.977(3) 3_676 ? O7 Cu1 1.970(2) 2_645 ? O8 Cu1 1.962(2) 4_575 ? 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 O5 C1 O6 125.0(4) . . ? O5 C1 C2 117.0(3) . . ? O6 C1 C2 118.0(3) . . ? C3 C2 C7 118.6(4) . . ? C3 C2 C1 120.8(3) . . ? C7 C2 C1 120.6(3) . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 120.8(4) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 117.4(3) . . ? C4 C5 C8 123.9(3) . . ? C6 C5 C8 118.6(3) . . ? C7 C6 C5 121.6(3) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C2 120.7(4) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? C5 C8 C60 106.2(3) . . ? C5 C8 C9 111.0(3) . . ? C60 C8 C9 113.4(3) . . ? C5 C8 C61 112.1(3) . . ? C60 C8 C61 108.3(3) . . ? C9 C8 C61 105.9(3) . . ? C10 C9 C14 118.5(3) . . ? C10 C9 C8 124.0(3) . . ? C14 C9 C8 117.6(3) . . ? C11 C10 C9 120.4(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 119.3(3) . . ? C13 C12 C15 120.0(3) . . ? C11 C12 C15 120.7(3) . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 121.2(4) . . ? C13 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? O7 C15 O8 126.4(3) . . ? O7 C15 C12 116.9(3) . . ? O8 C15 C12 116.7(3) . . ? C17 C16 C26 112.6(3) . . ? C17 C16 C18 108.6(3) . . ? C26 C16 C18 105.8(3) . . ? C17 C16 C19 106.1(3) . . ? C26 C16 C19 111.0(3) . . ? C18 C16 C19 112.7(3) . . ? F1 C17 F2 107.2(3) . . ? F1 C17 F3 106.6(3) . . ? F2 C17 F3 106.5(3) . . ? F1 C17 C16 112.0(3) . . ? F2 C17 C16 111.7(3) . . ? F3 C17 C16 112.5(3) . . ? F5 C18 F6 106.7(3) . . ? F5 C18 F4 106.7(3) . . ? F6 C18 F4 106.5(3) . . ? F5 C18 C16 112.2(3) . . ? F6 C18 C16 111.2(3) . . ? F4 C18 C16 113.0(3) . . ? C24 C19 C20 118.6(3) . . ? C24 C19 C16 124.1(3) . . ? C20 C19 C16 117.3(3) . . ? C21 C20 C19 120.7(4) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.3(3) . . ? C23 C22 C25 122.2(3) . . ? C21 C22 C25 118.6(3) . . ? C22 C23 C24 120.5(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 120.3(4) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? O2 C25 O1 125.8(3) . . ? O2 C25 C22 116.0(3) . . ? O1 C25 C22 118.2(3) . . ? C31 C26 C27 118.0(3) . . ? C31 C26 C16 123.9(3) . . ? C27 C26 C16 118.0(3) . . ? C28 C27 C26 121.1(3) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.6(3) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 118.9(4) . . ? C30 C29 C32 120.9(3) . . ? C28 C29 C32 120.1(3) . . ? C29 C30 C31 120.5(3) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C26 C31 C30 120.9(4) . . ? C26 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? O4 C32 O3 124.9(4) . . ? O4 C32 C29 117.0(3) . . ? O3 C32 C29 118.1(3) . . ? N5 C33 C37 124.0(4) . . ? N5 C33 H33 118.0 . . ? C37 C33 H33 118.0 . . ? N5 C34 C35 122.4(4) . . ? N5 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C36 C35 C34 118.6(4) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C35 C36 C37 120.3(4) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C33 116.8(4) . . ? C36 C37 C38 122.1(4) . . ? C33 C37 C38 121.1(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 C40 123.9(4) . . ? N1 C39 H39 118.0 . . ? C40 C39 H39 118.0 . . ? C41 C40 C39 116.9(4) . . ? C41 C40 C44 123.1(4) . . ? C39 C40 C44 120.0(4) . . ? C40 C41 C42 119.7(4) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 118.9(4) . . ? C43 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? N1 C43 C42 122.3(4) . . ? N1 C43 H43 118.9 . . ? C42 C43 H43 118.9 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 H45A 109.5 . . ? C47 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C47 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 C47 C48 124.1(9) . . ? C46 C47 C45 112.6(8) . . ? C48 C47 C45 122.5(9) . . ? C49 C48 C47 123.7(11) . . ? C49 C48 H47 118.2 . . ? C47 C48 H47 118.2 . . ? C48 C49 C50 112.5(12) . . ? C48 C49 H48 123.8 . . ? C50 C49 H48 123.8 . . ? N21 C50 C49 115.8(13) . . ? N21 C46 C47 114.9(8) . . ? N21 C46 H50 122.6 . . ? C47 C46 H50 122.6 . . ? C50 N21 C46 127.0(11) . . ? N13 C51 H51A 109.5 . . ? N13 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N13 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N13 C52 H52A 109.5 . . ? N13 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N13 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O10 C53 N13 122.0(8) . . ? O10 C53 H53 119.0 . . ? N13 C53 H53 119.0 . . ? N10 C54 H54A 109.5 . . ? N10 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N10 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N10 C55 H55A 109.5 . . ? N10 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N10 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O11 C56 N10 127.1(7) . . ? O11 C56 H56 116.5 . . ? N10 C56 H56 116.5 . . ? N11 C57 H57A 109.5 . . ? N11 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N11 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N11 C58 H58A 109.5 . . ? N11 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N11 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O9A C59 N11 125.5(5) . . ? O9A C59 H59 117.3 . . ? N11 C59 H59 117.3 . . ? F32 C60 F31 106.6(3) . . ? F32 C60 F30 107.1(3) . . ? F31 C60 F30 106.9(3) . . ? F32 C60 C8 112.0(3) . . ? F31 C60 C8 113.5(3) . . ? F30 C60 C8 110.5(3) . . ? F25 C61 F26 107.2(3) . . ? F25 C61 F24 106.7(3) . . ? F26 C61 F24 106.9(3) . . ? F25 C61 C8 111.3(3) . . ? F26 C61 C8 111.3(3) . . ? F24 C61 C8 113.1(3) . . ? O8 Cu1 O7 167.87(10) 4_576 2_655 ? O8 Cu1 O6 89.15(12) 4_576 . ? O7 Cu1 O6 88.80(11) 2_655 . ? O8 Cu1 O5 88.57(11) 4_576 3_676 ? O7 Cu1 O5 90.94(11) 2_655 3_676 ? O6 Cu1 O5 167.89(10) . 3_676 ? O8 Cu1 N5 96.52(11) 4_576 . ? O7 Cu1 N5 95.60(11) 2_655 . ? O6 Cu1 N5 99.10(11) . . ? O5 Cu1 N5 92.97(11) 3_676 . ? O8 Cu1 Cu1 85.66(8) 4_576 3_676 ? O7 Cu1 Cu1 82.31(8) 2_655 3_676 ? O6 Cu1 Cu1 87.66(8) . 3_676 ? O5 Cu1 Cu1 80.31(7) 3_676 3_676 ? N5 Cu1 Cu1 172.90(9) . 3_676 ? O3 Cu2 O4 167.64(10) . 3_565 ? O3 Cu2 O1 89.96(11) . 4_575 ? O4 Cu2 O1 88.62(11) 3_565 4_575 ? O3 Cu2 O2 88.25(11) . 2_545 ? O4 Cu2 O2 90.53(11) 3_565 2_545 ? O1 Cu2 O2 167.74(10) 4_575 2_545 ? O3 Cu2 N1 97.59(11) . . ? O4 Cu2 N1 94.75(11) 3_565 . ? O1 Cu2 N1 99.78(11) 4_575 . ? O2 Cu2 N1 92.48(11) 2_545 . ? O3 Cu2 Cu2 86.15(8) . 3_565 ? O4 Cu2 Cu2 81.55(7) 3_565 3_565 ? O1 Cu2 Cu2 89.28(8) 4_575 3_565 ? O2 Cu2 Cu2 78.50(8) 2_545 3_565 ? N1 Cu2 Cu2 170.16(8) . 3_565 ? C43 N1 C39 118.3(3) . . ? C43 N1 Cu2 121.0(3) . . ? C39 N1 Cu2 120.2(3) . . ? C34 N5 C33 117.8(3) . . ? C34 N5 Cu1 121.1(2) . . ? C33 N5 Cu1 120.8(2) . . ? C56 N10 C55 119.9(6) . . ? C56 N10 C54 123.1(5) . . ? C55 N10 C54 117.0(5) . . ? C59 N11 C58 121.0(5) . . ? C59 N11 C57 120.0(5) . . ? C58 N11 C57 118.9(4) . . ? C53 N13 C52 122.1(6) . . ? C53 N13 C51 122.6(5) . . ? C52 N13 C51 114.9(5) . . ? C25 O1 Cu2 116.6(2) . 4_576 ? C25 O2 Cu2 129.4(2) . 2 ? C32 O3 Cu2 121.1(2) . . ? C32 O4 Cu2 126.3(2) . 3_565 ? C1 O5 Cu1 127.7(2) . 3_676 ? C1 O6 Cu1 119.2(2) . . ? C15 O7 Cu1 124.7(2) . 2_645 ? C15 O8 Cu1 120.7(2) . 4_575 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 C1 C2 C3 170.6(3) . . . . ? O6 C1 C2 C3 -8.5(5) . . . . ? O5 C1 C2 C7 -7.9(5) . . . . ? O6 C1 C2 C7 172.9(3) . . . . ? C7 C2 C3 C4 -0.3(6) . . . . ? C1 C2 C3 C4 -178.9(3) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C3 C4 C5 C6 1.3(5) . . . . ? C3 C4 C5 C8 177.9(3) . . . . ? C4 C5 C6 C7 -1.3(5) . . . . ? C8 C5 C6 C7 -178.1(3) . . . . ? C5 C6 C7 C2 0.6(6) . . . . ? C3 C2 C7 C6 0.2(5) . . . . ? C1 C2 C7 C6 178.8(3) . . . . ? C4 C5 C8 C60 -91.6(4) . . . . ? C6 C5 C8 C60 84.9(4) . . . . ? C4 C5 C8 C9 144.6(4) . . . . ? C6 C5 C8 C9 -38.8(4) . . . . ? C4 C5 C8 C61 26.5(5) . . . . ? C6 C5 C8 C61 -156.9(3) . . . . ? C5 C8 C9 C10 135.8(4) . . . . ? C60 C8 C9 C10 16.3(5) . . . . ? C61 C8 C9 C10 -102.4(4) . . . . ? C5 C8 C9 C14 -45.0(4) . . . . ? C60 C8 C9 C14 -164.4(3) . . . . ? C61 C8 C9 C14 76.9(4) . . . . ? C14 C9 C10 C11 1.3(6) . . . . ? C8 C9 C10 C11 -179.5(3) . . . . ? C9 C10 C11 C12 -1.2(6) . . . . ? C10 C11 C12 C13 0.3(6) . . . . ? C10 C11 C12 C15 178.0(3) . . . . ? C11 C12 C13 C14 0.6(6) . . . . ? C15 C12 C13 C14 -177.1(3) . . . . ? C12 C13 C14 C9 -0.6(6) . . . . ? C10 C9 C14 C13 -0.4(6) . . . . ? C8 C9 C14 C13 -179.7(3) . . . . ? C13 C12 C15 O7 -11.1(5) . . . . ? C11 C12 C15 O7 171.2(3) . . . . ? C13 C12 C15 O8 168.3(3) . . . . ? C11 C12 C15 O8 -9.4(5) . . . . ? C26 C16 C17 F1 -170.7(3) . . . . ? C18 C16 C17 F1 72.4(4) . . . . ? C19 C16 C17 F1 -49.1(4) . . . . ? C26 C16 C17 F2 -50.4(4) . . . . ? C18 C16 C17 F2 -167.3(3) . . . . ? C19 C16 C17 F2 71.2(4) . . . . ? C26 C16 C17 F3 69.3(4) . . . . ? C18 C16 C17 F3 -47.6(4) . . . . ? C19 C16 C17 F3 -169.0(3) . . . . ? C17 C16 C18 F5 71.6(4) . . . . ? C26 C16 C18 F5 -49.6(4) . . . . ? C19 C16 C18 F5 -171.1(3) . . . . ? C17 C16 C18 F6 -168.9(3) . . . . ? C26 C16 C18 F6 69.9(4) . . . . ? C19 C16 C18 F6 -51.6(4) . . . . ? C17 C16 C18 F4 -49.2(4) . . . . ? C26 C16 C18 F4 -170.3(3) . . . . ? C19 C16 C18 F4 68.1(4) . . . . ? C17 C16 C19 C24 101.0(4) . . . . ? C26 C16 C19 C24 -136.3(4) . . . . ? C18 C16 C19 C24 -17.8(5) . . . . ? C17 C16 C19 C20 -77.0(4) . . . . ? C26 C16 C19 C20 45.7(5) . . . . ? C18 C16 C19 C20 164.2(3) . . . . ? C24 C19 C20 C21 0.3(6) . . . . ? C16 C19 C20 C21 178.5(3) . . . . ? C19 C20 C21 C22 1.5(6) . . . . ? C20 C21 C22 C23 -1.2(6) . . . . ? C20 C21 C22 C25 177.9(3) . . . . ? C21 C22 C23 C24 -1.0(6) . . . . ? C25 C22 C23 C24 179.9(3) . . . . ? C20 C19 C24 C23 -2.5(6) . . . . ? C16 C19 C24 C23 179.5(3) . . . . ? C22 C23 C24 C19 2.8(6) . . . . ? C23 C22 C25 O2 -166.8(4) . . . . ? C21 C22 C25 O2 14.2(5) . . . . ? C23 C22 C25 O1 13.8(5) . . . . ? C21 C22 C25 O1 -165.3(4) . . . . ? C17 C16 C26 C31 -25.5(5) . . . . ? C18 C16 C26 C31 93.0(4) . . . . ? C19 C16 C26 C31 -144.4(4) . . . . ? C17 C16 C26 C27 157.7(3) . . . . ? C18 C16 C26 C27 -83.7(4) . . . . ? C19 C16 C26 C27 38.9(4) . . . . ? C31 C26 C27 C28 0.2(5) . . . . ? C16 C26 C27 C28 177.1(3) . . . . ? C26 C27 C28 C29 -1.5(5) . . . . ? C27 C28 C29 C30 2.1(5) . . . . ? C27 C28 C29 C32 -176.6(3) . . . . ? C28 C29 C30 C31 -1.4(5) . . . . ? C32 C29 C30 C31 177.3(3) . . . . ? C27 C26 C31 C30 0.5(5) . . . . ? C16 C26 C31 C30 -176.3(3) . . . . ? C29 C30 C31 C26 0.1(6) . . . . ? C30 C29 C32 O4 -176.1(3) . . . . ? C28 C29 C32 O4 2.6(5) . . . . ? C30 C29 C32 O3 3.6(5) . . . . ? C28 C29 C32 O3 -177.6(3) . . . . ? N5 C34 C35 C36 0.8(6) . . . . ? C34 C35 C36 C37 1.0(6) . . . . ? C35 C36 C37 C33 -2.1(6) . . . . ? C35 C36 C37 C38 176.6(4) . . . . ? N5 C33 C37 C36 1.7(6) . . . . ? N5 C33 C37 C38 -177.0(3) . . . . ? N1 C39 C40 C41 0.2(6) . . . . ? N1 C39 C40 C44 -178.6(3) . . . . ? C39 C40 C41 C42 0.5(6) . . . . ? C44 C40 C41 C42 179.2(4) . . . . ? C40 C41 C42 C43 -1.0(6) . . . . ? C41 C42 C43 N1 0.9(6) . . . . ? C46 C47 C48 C49 3.3(13) . . . . ? C45 C47 C48 C49 -165.8(10) . . . . ? C47 C48 C49 C50 2.1(15) . . . . ? C48 C49 C50 N21 -11.9(17) . . . . ? C48 C47 C46 N21 0.9(10) . . . . ? C45 C47 C46 N21 171.0(8) . . . . ? C49 C50 N21 C46 18.2(18) . . . . ? C47 C46 N21 C50 -12.9(15) . . . . ? C5 C8 C60 F32 49.8(4) . . . . ? C9 C8 C60 F32 172.0(3) . . . . ? C61 C8 C60 F32 -70.8(4) . . . . ? C5 C8 C60 F31 170.5(3) . . . . ? C9 C8 C60 F31 -67.2(4) . . . . ? C61 C8 C60 F31 50.0(4) . . . . ? C5 C8 C60 F30 -69.5(4) . . . . ? C9 C8 C60 F30 52.7(4) . . . . ? C61 C8 C60 F30 170.0(3) . . . . ? C5 C8 C61 F25 171.5(3) . . . . ? C60 C8 C61 F25 -71.6(4) . . . . ? C9 C8 C61 F25 50.3(4) . . . . ? C5 C8 C61 F26 52.0(4) . . . . ? C60 C8 C61 F26 168.8(3) . . . . ? C9 C8 C61 F26 -69.2(4) . . . . ? C5 C8 C61 F24 -68.3(4) . . . . ? C60 C8 C61 F24 48.5(4) . . . . ? C9 C8 C61 F24 170.5(3) . . . . ? C42 C43 N1 C39 -0.3(6) . . . . ? C42 C43 N1 Cu2 -172.4(3) . . . . ? C40 C39 N1 C43 -0.3(5) . . . . ? C40 C39 N1 Cu2 171.9(3) . . . . ? O3 Cu2 N1 C43 -157.4(3) . . . . ? O4 Cu2 N1 C43 23.3(3) 3_565 . . . ? O1 Cu2 N1 C43 -66.1(3) 4_575 . . . ? O2 Cu2 N1 C43 114.0(3) 2_545 . . . ? Cu2 Cu2 N1 C43 90.7(6) 3_565 . . . ? O3 Cu2 N1 C39 30.6(3) . . . . ? O4 Cu2 N1 C39 -148.7(3) 3_565 . . . ? O1 Cu2 N1 C39 121.9(3) 4_575 . . . ? O2 Cu2 N1 C39 -58.0(3) 2_545 . . . ? Cu2 Cu2 N1 C39 -81.3(6) 3_565 . . . ? C35 C34 N5 C33 -1.2(6) . . . . ? C35 C34 N5 Cu1 173.6(3) . . . . ? C37 C33 N5 C34 -0.1(5) . . . . ? C37 C33 N5 Cu1 -174.9(3) . . . . ? O8 Cu1 N5 C34 32.2(3) 4_576 . . . ? O7 Cu1 N5 C34 -148.0(3) 2_655 . . . ? O6 Cu1 N5 C34 122.3(3) . . . . ? O5 Cu1 N5 C34 -56.8(3) 3_676 . . . ? Cu1 Cu1 N5 C34 -75.4(8) 3_676 . . . ? O8 Cu1 N5 C33 -153.2(3) 4_576 . . . ? O7 Cu1 N5 C33 26.6(3) 2_655 . . . ? O6 Cu1 N5 C33 -63.1(3) . . . . ? O5 Cu1 N5 C33 117.9(3) 3_676 . . . ? Cu1 Cu1 N5 C33 99.2(7) 3_676 . . . ? O11 C56 N10 C55 1.3(11) . . . . ? O11 C56 N10 C54 178.7(6) . . . . ? O9A C59 N11 C58 -179.0(5) . . . . ? O9A C59 N11 C57 -2.8(7) . . . . ? O10 C53 N13 C52 -180.0(5) . . . . ? O10 C53 N13 C51 8.1(9) . . . . ? O2 C25 O1 Cu2 -6.7(5) . . . 4_576 ? C22 C25 O1 Cu2 172.7(2) . . . 4_576 ? O1 C25 O2 Cu2 6.1(6) . . . 2 ? C22 C25 O2 Cu2 -173.3(2) . . . 2 ? O4 C32 O3 Cu2 -0.2(5) . . . . ? C29 C32 O3 Cu2 -179.9(2) . . . . ? O4 Cu2 O3 C32 7.1(7) 3_565 . . . ? O1 Cu2 O3 C32 90.5(3) 4_575 . . . ? O2 Cu2 O3 C32 -77.4(3) 2_545 . . . ? N1 Cu2 O3 C32 -169.7(3) . . . . ? Cu2 Cu2 O3 C32 1.2(3) 3_565 . . . ? O3 C32 O4 Cu2 -1.7(5) . . . 3_565 ? C29 C32 O4 Cu2 178.0(2) . . . 3_565 ? O6 C1 O5 Cu1 3.4(5) . . . 3_676 ? C2 C1 O5 Cu1 -175.6(2) . . . 3_676 ? O5 C1 O6 Cu1 -1.3(5) . . . . ? C2 C1 O6 Cu1 177.8(2) . . . . ? O8 Cu1 O6 C1 -86.3(3) 4_576 . . . ? O7 Cu1 O6 C1 81.7(3) 2_655 . . . ? O5 Cu1 O6 C1 -7.2(7) 3_676 . . . ? N5 Cu1 O6 C1 177.2(3) . . . . ? Cu1 Cu1 O6 C1 -0.6(3) 3_676 . . . ? O8 C15 O7 Cu1 -4.6(6) . . . 2_645 ? C12 C15 O7 Cu1 174.7(2) . . . 2_645 ? O7 C15 O8 Cu1 6.6(5) . . . 4_575 ? C12 C15 O8 Cu1 -172.7(2) . . . 4_575 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.762 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.087 data_F-MOF5 _database_code_depnum_ccdc_archive 'CCDC 745107' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'F-MOF 5' _chemical_melting_point ? _chemical_formula_moiety '2(C29 H16 Cu F6 N2 O4), C2 N O2, 2(C)' _chemical_formula_sum 'C62 H32 Cu2 F12 N5 O10 ' _chemical_formula_weight 1362.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbcn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.389(7) _cell_length_b 13.157(6) _cell_length_c 26.553(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5726(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3235 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 18.78 _exptl_crystal_description Cubic _exptl_crystal_colour Blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8355 _exptl_absorpt_correction_T_max 0.8624 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60708 _diffrn_reflns_av_R_equivalents 0.1260 _diffrn_reflns_av_sigmaI/netI 0.0884 _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 -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6252 _reflns_number_gt 3032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^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 6252 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1255 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1688(3) 0.8553(4) 0.0443(2) 0.0636(14) Uani 1 1 d . . . H1 H 0.1976 0.8345 0.0726 0.076 Uiso 1 1 calc R . . C2 C 0.1358(4) 0.7814(4) 0.0122(2) 0.0719(16) Uani 1 1 d . . . H2 H 0.1428 0.7127 0.0192 0.086 Uiso 1 1 calc R . . C3 C 0.0932(3) 0.8113(4) -0.0294(2) 0.0712(16) Uani 1 1 d . . . H3 H 0.0708 0.7627 -0.0507 0.085 Uiso 1 1 calc R . . C4 C 0.0831(3) 0.9137(4) -0.04015(19) 0.0558(13) Uani 1 1 d . . . C5 C 0.1177(3) 0.9829(4) -0.00633(16) 0.0449(11) Uani 1 1 d . . . C6 C 0.0385(3) 0.9535(5) -0.0826(2) 0.0688(16) Uani 1 1 d . . . H6 H 0.0146 0.9088 -0.1054 0.083 Uiso 1 1 calc R . . C7 C 0.0310(3) 1.0541(5) -0.0897(2) 0.0691(16) Uani 1 1 d . . . H7 H 0.0018 1.0776 -0.1174 0.083 Uiso 1 1 calc R . . C8 C 0.0663(3) 1.1255(4) -0.05644(18) 0.0549(13) Uani 1 1 d . . . C9 C 0.1089(3) 1.0894(3) -0.01430(16) 0.0421(11) Uani 1 1 d . . . C10 C 0.0631(3) 1.2328(5) -0.0616(2) 0.0717(17) Uani 1 1 d . . . H10 H 0.0363 1.2615 -0.0890 0.086 Uiso 1 1 calc R . . C11 C 0.0989(4) 1.2940(4) -0.0268(2) 0.0726(16) Uani 1 1 d . . . H11 H 0.0975 1.3642 -0.0307 0.087 Uiso 1 1 calc R . . C12 C 0.1374(3) 1.2513(4) 0.0145(2) 0.0602(14) Uani 1 1 d . . . H12 H 0.1598 1.2940 0.0387 0.072 Uiso 1 1 calc R . . C13 C 0.3551(3) 1.0050(3) 0.07794(19) 0.0477(12) Uani 1 1 d . . . C14 C 0.4363(3) 0.9770(3) 0.10149(17) 0.0432(11) Uani 1 1 d . . . C15 C 0.4471(3) 0.9754(4) 0.15359(18) 0.0541(13) Uani 1 1 d . . . H15 H 0.4028 0.9858 0.1749 0.065 Uiso 1 1 calc R . . C16 C 0.5230(3) 0.9587(4) 0.17334(17) 0.0545(13) Uani 1 1 d . . . H16 H 0.5293 0.9591 0.2081 0.065 Uiso 1 1 calc R . . C17 C 0.5909(3) 0.9412(3) 0.14321(16) 0.0410(11) Uani 1 1 d . . . C18 C 0.5789(3) 0.9414(3) 0.09129(16) 0.0455(11) Uani 1 1 d . . . H18 H 0.6227 0.9300 0.0698 0.055 Uiso 1 1 calc R . . C19 C 0.5025(3) 0.9583(3) 0.07168(17) 0.0462(11) Uani 1 1 d . . . H19 H 0.4957 0.9570 0.0369 0.055 Uiso 1 1 calc R . . C20 C 0.6755(3) 0.9303(3) 0.16799(16) 0.0425(11) Uani 1 1 d . . . C21 C 0.6728(3) 0.8687(3) 0.21721(16) 0.0420(11) Uani 1 1 d . . . C22 C 0.7203(3) 0.8908(4) 0.25885(18) 0.0547(13) Uani 1 1 d . . . H22 H 0.7532 0.9485 0.2585 0.066 Uiso 1 1 calc R . . C23 C 0.7200(3) 0.8294(4) 0.30091(18) 0.0600(14) Uani 1 1 d . . . H23 H 0.7527 0.8464 0.3283 0.072 Uiso 1 1 calc R . . C24 C 0.6721(3) 0.7434(4) 0.30313(16) 0.0482(12) Uani 1 1 d . . . C25 C 0.6241(3) 0.7211(4) 0.26204(18) 0.0592(14) Uani 1 1 d . . . H25 H 0.5908 0.6638 0.2628 0.071 Uiso 1 1 calc R . . C26 C 0.6245(3) 0.7820(4) 0.21994(18) 0.0556(13) Uani 1 1 d . . . H26 H 0.5917 0.7648 0.1927 0.067 Uiso 1 1 calc R . . C27 C 0.7065(4) 1.0399(5) 0.1766(2) 0.0701(16) Uani 1 1 d . . . C28 C 0.7354(3) 0.8736(5) 0.1333(2) 0.0687(16) Uani 1 1 d . . . C29 C 0.1716(3) 1.1729(4) 0.15184(19) 0.0573(13) Uani 1 1 d . . . Cu1 Cu 0.20434(3) 1.07325(4) 0.07364(2) 0.0476(2) Uani 1 1 d . . . F1 F 0.6678(2) 1.0847(2) 0.21382(15) 0.0914(11) Uani 1 1 d . . . F2 F 0.7865(2) 1.0429(3) 0.18639(13) 0.0970(12) Uani 1 1 d . . . F3 F 0.6954(2) 1.0969(3) 0.13540(14) 0.1061(14) Uani 1 1 d . . . F4 F 0.75757(19) 0.9290(3) 0.09300(12) 0.1000(13) Uani 1 1 d . . . F5 F 0.80413(17) 0.8481(3) 0.15725(12) 0.0914(11) Uani 1 1 d . . . F6 F 0.7038(2) 0.7867(3) 0.11621(11) 0.0825(10) Uani 1 1 d . . . N1 N 0.1601(2) 0.9543(3) 0.03539(14) 0.0464(9) Uani 1 1 d . . . N2 N 0.1433(2) 1.1511(3) 0.02051(14) 0.0469(9) Uani 1 1 d . . . O1 O 0.29320(19) 1.0012(3) 0.10718(12) 0.0587(9) Uani 1 1 d . . . O2 O 0.3521(2) 1.0302(3) 0.03339(13) 0.0654(10) Uani 1 1 d . . . O3 O 0.2208(2) 1.1945(2) 0.11588(12) 0.0583(9) Uani 1 1 d . . . O4 O 0.1271(2) 1.0976(3) 0.15084(14) 0.0758(11) Uani 1 1 d . . . N3 N 0.5000 0.301(2) 0.2500 0.290(10) Uiso 1 2 d S . . O5 O 0.5675(7) 0.2587(9) 0.3252(4) 0.279(5) Uiso 1 1 d . . . C33 C 0.5285(13) 0.2425(16) 0.2850(9) 0.329(11) Uiso 1 1 d . . . C31 C 0.5360(9) 0.4386(11) 0.2457(7) 0.256(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.061(3) 0.057(3) 0.073(4) 0.006(3) 0.008(3) 0.012(3) C2 0.079(4) 0.042(3) 0.095(5) -0.002(3) 0.014(4) -0.002(3) C3 0.067(4) 0.063(4) 0.084(4) -0.025(3) 0.008(3) -0.005(3) C4 0.043(3) 0.066(4) 0.058(3) -0.017(3) 0.006(2) -0.007(3) C5 0.032(2) 0.060(3) 0.043(3) -0.006(2) 0.004(2) 0.002(2) C6 0.050(3) 0.103(5) 0.053(3) -0.021(3) -0.002(3) -0.009(3) C7 0.053(3) 0.108(5) 0.047(3) -0.005(3) -0.005(3) 0.009(3) C8 0.044(3) 0.078(4) 0.043(3) 0.004(3) 0.009(2) 0.006(3) C9 0.035(2) 0.049(3) 0.042(3) 0.002(2) 0.004(2) 0.008(2) C10 0.067(4) 0.090(5) 0.059(4) 0.026(3) 0.000(3) 0.027(3) C11 0.081(4) 0.055(4) 0.082(4) 0.008(3) 0.002(4) 0.015(3) C12 0.067(4) 0.046(3) 0.068(4) 0.001(3) 0.000(3) 0.005(3) C13 0.047(3) 0.041(3) 0.055(3) 0.003(2) -0.008(3) 0.004(2) C14 0.044(3) 0.038(3) 0.048(3) 0.007(2) -0.003(2) -0.003(2) C15 0.039(3) 0.077(4) 0.046(3) 0.003(3) 0.003(2) 0.007(2) C16 0.051(3) 0.078(4) 0.034(3) 0.004(2) 0.001(2) 0.006(3) C17 0.044(3) 0.037(3) 0.042(3) 0.006(2) 0.004(2) 0.002(2) C18 0.051(3) 0.049(3) 0.036(2) 0.009(2) 0.008(2) 0.005(2) C19 0.051(3) 0.053(3) 0.035(2) 0.010(2) 0.000(2) 0.001(2) C20 0.037(2) 0.050(3) 0.041(3) 0.007(2) 0.002(2) -0.001(2) C21 0.038(2) 0.049(3) 0.038(3) 0.004(2) 0.002(2) 0.000(2) C22 0.056(3) 0.059(3) 0.049(3) 0.007(3) -0.006(2) -0.008(2) C23 0.066(3) 0.070(4) 0.044(3) 0.001(3) -0.013(2) -0.010(3) C24 0.047(3) 0.059(3) 0.039(3) 0.007(2) 0.000(2) 0.004(2) C25 0.061(3) 0.058(3) 0.059(3) 0.013(3) -0.004(3) -0.009(3) C26 0.061(3) 0.056(3) 0.050(3) 0.008(2) -0.014(2) -0.006(3) C27 0.070(4) 0.069(4) 0.071(4) 0.026(3) -0.019(3) -0.025(3) C28 0.044(3) 0.113(5) 0.049(3) 0.019(3) 0.002(3) 0.012(3) C29 0.050(3) 0.073(4) 0.049(3) -0.010(3) -0.005(3) 0.008(3) Cu1 0.0465(4) 0.0530(4) 0.0434(4) -0.0044(3) -0.0047(3) 0.0062(3) F1 0.116(3) 0.054(2) 0.104(3) -0.0124(19) -0.026(2) -0.0033(19) F2 0.075(2) 0.113(3) 0.103(3) 0.034(2) -0.026(2) -0.047(2) F3 0.121(3) 0.086(2) 0.111(3) 0.055(2) -0.044(2) -0.049(2) F4 0.058(2) 0.175(4) 0.067(2) 0.041(2) 0.0218(18) 0.009(2) F5 0.0483(19) 0.157(3) 0.068(2) 0.012(2) 0.0009(16) 0.032(2) F6 0.084(2) 0.100(3) 0.064(2) -0.0188(19) -0.0050(17) 0.041(2) N1 0.046(2) 0.045(2) 0.048(2) 0.0003(18) 0.0006(19) 0.0069(18) N2 0.043(2) 0.050(2) 0.047(2) -0.0041(19) -0.0004(18) 0.0048(19) O1 0.045(2) 0.077(2) 0.054(2) 0.0082(18) -0.0065(17) 0.0087(18) O2 0.061(2) 0.082(3) 0.053(2) 0.0218(19) -0.0059(18) 0.0110(19) O3 0.069(2) 0.064(2) 0.0419(19) -0.0096(17) 0.0044(17) -0.0028(17) O4 0.065(2) 0.088(3) 0.074(3) -0.029(2) 0.008(2) -0.023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.332(6) . ? C1 C2 1.401(7) . ? C2 C3 1.364(7) . ? C3 C4 1.388(7) . ? C4 C5 1.399(6) . ? C4 C6 1.441(7) . ? C5 N1 1.361(5) . ? C5 C9 1.424(6) . ? C6 C7 1.343(7) . ? C7 C8 1.413(7) . ? C8 C9 1.402(6) . ? C8 C10 1.420(7) . ? C9 N2 1.353(5) . ? C10 C11 1.358(8) . ? C11 C12 1.384(7) . ? C12 N2 1.332(6) . ? C13 O2 1.229(5) . ? C13 O1 1.279(5) . ? C13 C14 1.515(6) . ? C14 C19 1.366(6) . ? C14 C15 1.395(6) . ? C15 C16 1.367(6) . ? C16 C17 1.391(6) . ? C17 C18 1.393(6) . ? C17 C20 1.540(6) . ? C18 C19 1.373(6) . ? C20 C21 1.539(6) . ? C20 C28 1.540(7) . ? C20 C27 1.546(7) . ? C21 C22 1.383(6) . ? C21 C26 1.390(6) . ? C22 C23 1.379(6) . ? C23 C24 1.378(6) . ? C24 C25 1.378(6) . ? C24 C29 1.514(6) 6_656 ? C25 C26 1.376(6) . ? C27 F1 1.314(7) . ? C27 F2 1.336(6) . ? C27 F3 1.339(6) . ? C28 F6 1.334(7) . ? C28 F5 1.337(5) . ? C28 F4 1.345(6) . ? C29 O4 1.230(6) . ? C29 O3 1.281(6) . ? C29 C24 1.513(6) 6_566 ? C29 Cu1 2.514(5) . ? Cu1 O1 1.952(3) . ? Cu1 O3 1.968(3) . ? Cu1 N1 2.001(4) . ? Cu1 N2 2.010(4) . ? Cu1 O4 2.430(4) . ? N3 C33 1.29(2) 3_655 ? N3 C33 1.29(2) . ? N3 C31 1.91(2) . ? N3 C31 1.91(2) 3_655 ? O5 C33 1.26(2) . ? C31 C31 1.20(3) 3_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.0(5) . . ? C3 C2 C1 119.3(5) . . ? C2 C3 C4 120.5(5) . . ? C3 C4 C5 116.8(5) . . ? C3 C4 C6 125.0(5) . . ? C5 C4 C6 118.1(5) . . ? N1 C5 C4 123.4(5) . . ? N1 C5 C9 116.4(4) . . ? C4 C5 C9 120.2(4) . . ? C7 C6 C4 121.0(5) . . ? C6 C7 C8 122.0(5) . . ? C9 C8 C7 118.6(5) . . ? C9 C8 C10 115.6(5) . . ? C7 C8 C10 125.9(5) . . ? N2 C9 C8 123.3(4) . . ? N2 C9 C5 116.5(4) . . ? C8 C9 C5 120.1(4) . . ? C11 C10 C8 120.6(5) . . ? C10 C11 C12 119.6(5) . . ? N2 C12 C11 122.0(5) . . ? O2 C13 O1 124.2(4) . . ? O2 C13 C14 119.9(4) . . ? O1 C13 C14 115.9(4) . . ? C19 C14 C15 118.1(4) . . ? C19 C14 C13 120.2(4) . . ? C15 C14 C13 121.6(4) . . ? C16 C15 C14 119.9(4) . . ? C15 C16 C17 122.3(4) . . ? C16 C17 C18 117.1(4) . . ? C16 C17 C20 119.3(4) . . ? C18 C17 C20 123.4(4) . . ? C19 C18 C17 120.3(4) . . ? C14 C19 C18 122.3(4) . . ? C21 C20 C28 105.7(4) . . ? C21 C20 C17 112.7(3) . . ? C28 C20 C17 111.3(4) . . ? C21 C20 C27 112.0(4) . . ? C28 C20 C27 109.3(5) . . ? C17 C20 C27 105.9(4) . . ? C22 C21 C26 116.8(4) . . ? C22 C21 C20 123.5(4) . . ? C26 C21 C20 119.5(4) . . ? C23 C22 C21 121.5(5) . . ? C24 C23 C22 121.2(5) . . ? C25 C24 C23 117.9(4) . . ? C25 C24 C29 119.5(5) . 6_656 ? C23 C24 C29 122.7(5) . 6_656 ? C26 C25 C24 121.1(5) . . ? C25 C26 C21 121.6(5) . . ? F1 C27 F2 108.3(5) . . ? F1 C27 F3 107.3(5) . . ? F2 C27 F3 106.0(5) . . ? F1 C27 C20 111.7(5) . . ? F2 C27 C20 112.3(5) . . ? F3 C27 C20 110.9(5) . . ? F6 C28 F5 105.9(5) . . ? F6 C28 F4 107.4(5) . . ? F5 C28 F4 106.7(4) . . ? F6 C28 C20 111.8(4) . . ? F5 C28 C20 112.0(4) . . ? F4 C28 C20 112.7(5) . . ? O4 C29 O3 122.3(5) . . ? O4 C29 C24 120.9(5) . 6_566 ? O3 C29 C24 116.7(5) . 6_566 ? O4 C29 Cu1 71.8(3) . . ? O3 C29 Cu1 50.6(2) . . ? C24 C29 Cu1 166.2(4) 6_566 . ? O1 Cu1 O3 91.79(14) . . ? O1 Cu1 N1 97.01(15) . . ? O3 Cu1 N1 166.50(15) . . ? O1 Cu1 N2 159.85(15) . . ? O3 Cu1 N2 93.18(15) . . ? N1 Cu1 N2 82.05(16) . . ? O1 Cu1 O4 93.89(14) . . ? O3 Cu1 O4 58.92(13) . . ? N1 Cu1 O4 110.06(14) . . ? N2 Cu1 O4 105.39(15) . . ? O1 Cu1 C29 92.04(15) . . ? O3 Cu1 C29 30.21(15) . . ? N1 Cu1 C29 138.59(17) . . ? N2 Cu1 C29 101.98(16) . . ? O4 Cu1 C29 28.75(14) . . ? C1 N1 C5 118.0(4) . . ? C1 N1 Cu1 129.5(4) . . ? C5 N1 Cu1 112.5(3) . . ? C12 N2 C9 118.8(4) . . ? C12 N2 Cu1 128.7(3) . . ? C9 N2 Cu1 112.4(3) . . ? C13 O1 Cu1 107.2(3) . . ? C29 O3 Cu1 99.2(3) . . ? C29 O4 Cu1 79.4(3) . . ? C33 N3 C33 107(3) 3_655 . ? C33 N3 C31 129.1(16) 3_655 . ? C33 N3 C31 119.5(15) . . ? C33 N3 C31 119.5(15) 3_655 3_655 ? C33 N3 C31 129.1(16) . 3_655 ? C31 N3 C31 36.6(10) . 3_655 ? O5 C33 N3 134(2) . . ? C31 C31 N3 71.7(5) 3_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.2(8) . . . . ? C1 C2 C3 C4 0.5(8) . . . . ? C2 C3 C4 C5 -0.6(8) . . . . ? C2 C3 C4 C6 -179.2(5) . . . . ? C3 C4 C5 N1 0.4(7) . . . . ? C6 C4 C5 N1 179.1(4) . . . . ? C3 C4 C5 C9 -179.0(4) . . . . ? C6 C4 C5 C9 -0.3(7) . . . . ? C3 C4 C6 C7 179.2(5) . . . . ? C5 C4 C6 C7 0.6(8) . . . . ? C4 C6 C7 C8 0.1(8) . . . . ? C6 C7 C8 C9 -1.1(8) . . . . ? C6 C7 C8 C10 178.5(5) . . . . ? C7 C8 C9 N2 -178.4(4) . . . . ? C10 C8 C9 N2 1.9(6) . . . . ? C7 C8 C9 C5 1.4(7) . . . . ? C10 C8 C9 C5 -178.3(4) . . . . ? N1 C5 C9 N2 -0.4(6) . . . . ? C4 C5 C9 N2 179.1(4) . . . . ? N1 C5 C9 C8 179.8(4) . . . . ? C4 C5 C9 C8 -0.7(6) . . . . ? C9 C8 C10 C11 -0.9(7) . . . . ? C7 C8 C10 C11 179.5(5) . . . . ? C8 C10 C11 C12 -1.2(8) . . . . ? C10 C11 C12 N2 2.5(8) . . . . ? O2 C13 C14 C19 -14.1(7) . . . . ? O1 C13 C14 C19 166.5(4) . . . . ? O2 C13 C14 C15 162.0(5) . . . . ? O1 C13 C14 C15 -17.5(6) . . . . ? C19 C14 C15 C16 2.0(7) . . . . ? C13 C14 C15 C16 -174.1(4) . . . . ? C14 C15 C16 C17 -1.1(8) . . . . ? C15 C16 C17 C18 0.1(7) . . . . ? C15 C16 C17 C20 175.8(4) . . . . ? C16 C17 C18 C19 0.0(6) . . . . ? C20 C17 C18 C19 -175.5(4) . . . . ? C15 C14 C19 C18 -2.0(7) . . . . ? C13 C14 C19 C18 174.2(4) . . . . ? C17 C18 C19 C14 1.0(7) . . . . ? C16 C17 C20 C21 40.3(6) . . . . ? C18 C17 C20 C21 -144.3(4) . . . . ? C16 C17 C20 C28 158.9(4) . . . . ? C18 C17 C20 C28 -25.7(6) . . . . ? C16 C17 C20 C27 -82.5(5) . . . . ? C18 C17 C20 C27 92.9(5) . . . . ? C28 C20 C21 C22 95.2(5) . . . . ? C17 C20 C21 C22 -143.1(4) . . . . ? C27 C20 C21 C22 -23.8(6) . . . . ? C28 C20 C21 C26 -80.6(5) . . . . ? C17 C20 C21 C26 41.2(6) . . . . ? C27 C20 C21 C26 160.4(5) . . . . ? C26 C21 C22 C23 0.4(7) . . . . ? C20 C21 C22 C23 -175.5(4) . . . . ? C21 C22 C23 C24 -0.1(8) . . . . ? C22 C23 C24 C25 -0.4(8) . . . . ? C22 C23 C24 C29 178.6(5) . . . 6_656 ? C23 C24 C25 C26 0.7(7) . . . . ? C29 C24 C25 C26 -178.3(5) 6_656 . . . ? C24 C25 C26 C21 -0.4(8) . . . . ? C22 C21 C26 C25 -0.1(7) . . . . ? C20 C21 C26 C25 175.9(4) . . . . ? C21 C20 C27 F1 -49.9(6) . . . . ? C28 C20 C27 F1 -166.7(4) . . . . ? C17 C20 C27 F1 73.3(5) . . . . ? C21 C20 C27 F2 72.1(6) . . . . ? C28 C20 C27 F2 -44.8(6) . . . . ? C17 C20 C27 F2 -164.7(4) . . . . ? C21 C20 C27 F3 -169.5(4) . . . . ? C28 C20 C27 F3 73.6(6) . . . . ? C17 C20 C27 F3 -46.3(6) . . . . ? C21 C20 C28 F6 72.1(5) . . . . ? C17 C20 C28 F6 -50.6(5) . . . . ? C27 C20 C28 F6 -167.1(4) . . . . ? C21 C20 C28 F5 -46.5(6) . . . . ? C17 C20 C28 F5 -169.2(4) . . . . ? C27 C20 C28 F5 74.2(6) . . . . ? C21 C20 C28 F4 -166.8(4) . . . . ? C17 C20 C28 F4 70.5(6) . . . . ? C27 C20 C28 F4 -46.0(6) . . . . ? O4 C29 Cu1 O1 -94.4(3) . . . . ? O3 C29 Cu1 O1 90.0(3) . . . . ? C24 C29 Cu1 O1 64.8(15) 6_566 . . . ? O4 C29 Cu1 O3 175.6(5) . . . . ? C24 C29 Cu1 O3 -25.2(14) 6_566 . . . ? O4 C29 Cu1 N1 8.6(4) . . . . ? O3 C29 Cu1 N1 -167.0(3) . . . . ? C24 C29 Cu1 N1 167.8(14) 6_566 . . . ? O4 C29 Cu1 N2 100.2(3) . . . . ? O3 C29 Cu1 N2 -75.4(3) . . . . ? C24 C29 Cu1 N2 -100.6(15) 6_566 . . . ? O3 C29 Cu1 O4 -175.6(5) . . . . ? C24 C29 Cu1 O4 159.2(17) 6_566 . . . ? C2 C1 N1 C5 0.0(7) . . . . ? C2 C1 N1 Cu1 -177.6(4) . . . . ? C4 C5 N1 C1 -0.1(6) . . . . ? C9 C5 N1 C1 179.3(4) . . . . ? C4 C5 N1 Cu1 177.9(3) . . . . ? C9 C5 N1 Cu1 -2.7(5) . . . . ? O1 Cu1 N1 C1 21.4(4) . . . . ? O3 Cu1 N1 C1 -108.9(7) . . . . ? N2 Cu1 N1 C1 -178.9(4) . . . . ? O4 Cu1 N1 C1 -75.4(4) . . . . ? C29 Cu1 N1 C1 -79.8(5) . . . . ? O1 Cu1 N1 C5 -156.3(3) . . . . ? O3 Cu1 N1 C5 73.4(7) . . . . ? N2 Cu1 N1 C5 3.4(3) . . . . ? O4 Cu1 N1 C5 106.9(3) . . . . ? C29 Cu1 N1 C5 102.5(3) . . . . ? C11 C12 N2 C9 -1.5(7) . . . . ? C11 C12 N2 Cu1 174.0(4) . . . . ? C8 C9 N2 C12 -0.8(6) . . . . ? C5 C9 N2 C12 179.4(4) . . . . ? C8 C9 N2 Cu1 -177.0(3) . . . . ? C5 C9 N2 Cu1 3.2(5) . . . . ? O1 Cu1 N2 C12 -90.6(6) . . . . ? O3 Cu1 N2 C12 13.4(4) . . . . ? N1 Cu1 N2 C12 -179.3(4) . . . . ? O4 Cu1 N2 C12 72.0(4) . . . . ? C29 Cu1 N2 C12 42.6(4) . . . . ? O1 Cu1 N2 C9 85.1(5) . . . . ? O3 Cu1 N2 C9 -170.9(3) . . . . ? N1 Cu1 N2 C9 -3.6(3) . . . . ? O4 Cu1 N2 C9 -112.3(3) . . . . ? C29 Cu1 N2 C9 -141.7(3) . . . . ? O2 C13 O1 Cu1 -14.0(6) . . . . ? C14 C13 O1 Cu1 165.5(3) . . . . ? O3 Cu1 O1 C13 -101.8(3) . . . . ? N1 Cu1 O1 C13 88.4(3) . . . . ? N2 Cu1 O1 C13 2.4(6) . . . . ? O4 Cu1 O1 C13 -160.8(3) . . . . ? C29 Cu1 O1 C13 -132.1(3) . . . . ? O4 C29 O3 Cu1 -4.9(6) . . . . ? C24 C29 O3 Cu1 173.5(3) 6_566 . . . ? O1 Cu1 O3 C29 -91.0(3) . . . . ? N1 Cu1 O3 C29 39.8(8) . . . . ? N2 Cu1 O3 C29 108.5(3) . . . . ? O4 Cu1 O3 C29 2.5(3) . . . . ? O3 C29 O4 Cu1 4.0(5) . . . . ? C24 C29 O4 Cu1 -174.3(5) 6_566 . . . ? O1 Cu1 O4 C29 87.2(3) . . . . ? O3 Cu1 O4 C29 -2.6(3) . . . . ? N1 Cu1 O4 C29 -173.9(3) . . . . ? N2 Cu1 O4 C29 -86.9(3) . . . . ? C33 N3 C33 O5 174(3) 3_655 . . . ? C31 N3 C33 O5 14(3) . . . . ? C31 N3 C33 O5 -29(3) 3_655 . . . ? C33 N3 C31 C31 88(2) 3_655 . . 3_655 ? C33 N3 C31 C31 -117(2) . . . 3_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.749 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.089