# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1268 #================================================================= data_global # SUBMISSION DETAILS _publ_contact_author ; Dr. Michael Ward School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287655' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the five crystal structures in the paper 'Tetranuclear grid-like copper(II) complexes with pyrazolate bridges: syntheses, structures, magnetic and EPR spectroscopic properties.' by K. L. V. Mann, et al, submitted to Dalton Transactions for publication. ; #================================================================= data_/tintin3/people/karen/pop/sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H21 F12 N9 Ni O P2' _chemical_formula_weight 800.15 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 11.531(3) _cell_length_b 12.642(3) _cell_length_c 21.607(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.26(2) _cell_angle_gamma 90.00 _cell_volume 3130.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method ? _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19307 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7100 _reflns_number_observed 4106 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens 1995b)' _computing_cell_refinement 'SAINT (Siemens 1995b)' _computing_data_reduction 'SAINT (Siemens 1995b)' _computing_structure_solution 'SHELXTL (Siemens 1995a)' _computing_structure_refinement 'SHELXTL (Siemens 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens 1995a)' _computing_publication_material 'SHELXTL (Siemens 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+3.2831P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7100 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1255 _refine_ls_R_factor_obs 0.0615 _refine_ls_wR_factor_all 0.1646 _refine_ls_wR_factor_obs 0.1341 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.010 _refine_ls_restrained_S_obs 1.102 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.32710(5) 0.52393(4) 0.17516(2) 0.0233(2) Uani 1 d . . N11 N 0.2465(3) 0.4072(3) 0.1178(2) 0.0262(8) Uani 1 d . . N12 N 0.1543(3) 0.4003(3) 0.0740(2) 0.0325(9) Uani 1 d . . H12 H 0.0972(3) 0.4468(3) 0.0692(2) 0.039 Uiso 1 calc R . C13 C 0.1602(5) 0.3132(4) 0.0384(2) 0.0389(12) Uani 1 d . . H13 H 0.1047(5) 0.2916(4) 0.0051(2) 0.047 Uiso 1 calc R . C14 C 0.2625(4) 0.2612(4) 0.0595(2) 0.0369(12) Uani 1 d . . H14 H 0.2923(4) 0.1979(4) 0.0437(2) 0.044 Uiso 1 calc R . C15 C 0.3124(4) 0.3228(3) 0.1095(2) 0.0276(10) Uani 1 d . . N21 N 0.4456(3) 0.3951(3) 0.1899(2) 0.0274(8) Uani 1 d . . C22 C 0.4214(4) 0.3121(4) 0.1510(2) 0.0280(10) Uani 1 d . . C23 C 0.4939(4) 0.2250(4) 0.1513(2) 0.0412(12) Uani 1 d . . H23 H 0.4753(4) 0.1682(4) 0.1232(2) 0.049 Uiso 1 calc R . C24 C 0.5933(5) 0.2210(5) 0.1927(3) 0.0493(15) Uani 1 d . . H24 H 0.6443(5) 0.1619(5) 0.1936(3) 0.059 Uiso 1 calc R . C25 C 0.6169(4) 0.3044(4) 0.2325(2) 0.0439(13) Uani 1 d . . H25 H 0.6848(4) 0.3036(4) 0.2616(2) 0.053 Uiso 1 calc R . C26 C 0.5421(4) 0.3893(4) 0.2303(2) 0.0336(11) Uani 1 d . . H26 H 0.5595(4) 0.4461(4) 0.2586(2) 0.040 Uiso 1 calc R . N31 N 0.4181(3) 0.6120(3) 0.2442(2) 0.0263(8) Uani 1 d . . N32 N 0.5151(3) 0.6711(3) 0.2515(2) 0.0301(9) Uani 1 d . . H32 H 0.5541(3) 0.6913(3) 0.2207(2) 0.036 Uiso 1 calc R . C33 C 0.5454(4) 0.6958(4) 0.3112(2) 0.0361(12) Uani 1 d . . H33 H 0.6111(4) 0.7369(4) 0.3270(2) 0.043 Uiso 1 calc R . C34 C 0.4649(4) 0.6511(4) 0.3457(2) 0.0378(12) Uani 1 d . . H34 H 0.4625(4) 0.6549(4) 0.3894(2) 0.045 Uiso 1 calc R . C35 C 0.3866(4) 0.5985(4) 0.3013(2) 0.0268(10) Uani 1 d . . N41 N 0.2367(3) 0.4886(3) 0.2520(2) 0.0255(8) Uani 1 d . . C42 C 0.2841(4) 0.5316(3) 0.3067(2) 0.0260(9) Uani 1 d . . C43 C 0.2372(4) 0.5141(4) 0.3617(2) 0.0314(10) Uani 1 d . . H43 H 0.2737(4) 0.5427(4) 0.3996(2) 0.038 Uiso 1 calc R . C44 C 0.1371(4) 0.4549(4) 0.3615(2) 0.0378(12) Uani 1 d . . H44 H 0.1029(4) 0.4429(4) 0.3989(2) 0.045 Uiso 1 calc R . C45 C 0.0872(4) 0.4134(4) 0.3056(2) 0.0376(12) Uani 1 d . . H45 H 0.0168(4) 0.3739(4) 0.3040(2) 0.045 Uiso 1 calc R . C46 C 0.1405(4) 0.4296(4) 0.2524(2) 0.0322(11) Uani 1 d . . H46 H 0.1078(4) 0.3978(4) 0.2146(2) 0.039 Uiso 1 calc R . N51 N 0.4126(3) 0.5842(3) 0.1032(2) 0.0266(8) Uani 1 d . . N52 N 0.5116(3) 0.5662(3) 0.0775(2) 0.0332(9) Uani 1 d . . H52 H 0.5630(3) 0.5172(3) 0.0903(2) 0.040 Uiso 1 calc R . C53 C 0.5223(4) 0.6326(4) 0.0299(2) 0.0384(12) Uani 1 d . . H53 H 0.5855(4) 0.6348(4) 0.0052(2) 0.046 Uiso 1 calc R . C54 C 0.4257(5) 0.6968(4) 0.0232(2) 0.0415(13) Uani 1 d . . H54 H 0.4078(5) 0.7512(4) -0.0066(2) 0.050 Uiso 1 calc R . C55 C 0.3585(4) 0.6633(4) 0.0709(2) 0.0307(11) Uani 1 d . . N61 N 0.2129(3) 0.6472(3) 0.1398(2) 0.0294(9) Uani 1 d . . C62 C 0.2466(4) 0.6975(4) 0.0890(2) 0.0307(11) Uani 1 d . . C63 C 0.1815(5) 0.7758(4) 0.0574(2) 0.0383(12) Uani 1 d . . H63 H 0.2067(5) 0.8079(4) 0.0214(2) 0.046 Uiso 1 calc R . C64 C 0.0780(5) 0.8064(4) 0.0796(2) 0.0412(13) Uani 1 d . . H64 H 0.0320(5) 0.8614(4) 0.0595(2) 0.049 Uiso 1 calc R . C65 C 0.0428(4) 0.7564(4) 0.1310(2) 0.0395(12) Uani 1 d . . H65 H -0.0279(4) 0.7762(4) 0.1466(2) 0.047 Uiso 1 calc R . C66 C 0.1112(4) 0.6773(4) 0.1594(2) 0.0346(11) Uani 1 d . . H66 H 0.0854(4) 0.6424(4) 0.1944(2) 0.042 Uiso 1 calc R . P1 P 0.74019(13) -0.01722(11) 0.07324(6) 0.0407(3) Uani 1 d . . F1 F 0.8564(4) 0.0099(4) 0.0417(2) 0.117(2) Uani 1 d . . F2 F 0.7207(5) 0.1033(3) 0.0787(2) 0.112(2) Uani 1 d . . F3 F 0.6766(4) -0.0211(3) 0.0058(2) 0.0883(13) Uani 1 d . . F4 F 0.7749(4) -0.1397(3) 0.0690(2) 0.0839(13) Uani 1 d . . F5 F 0.8137(5) -0.0187(4) 0.1392(2) 0.113(2) Uani 1 d . . F6 F 0.6305(4) -0.0485(4) 0.1048(2) 0.110(2) Uani 1 d . . P2 P -0.16896(11) 0.47787(12) 0.09675(6) 0.0408(3) Uani 1 d . . F7 F -0.2789(3) 0.4444(4) 0.1311(2) 0.0828(13) Uani 1 d . . F8 F -0.0851(3) 0.4642(3) 0.1589(2) 0.0794(12) Uani 1 d . . F9 F -0.1917(3) 0.5989(3) 0.1123(2) 0.0717(11) Uani 1 d . . F10 F -0.2525(3) 0.4926(3) 0.03405(14) 0.0606(9) Uani 1 d . . F11 F -0.1446(4) 0.3590(3) 0.0792(2) 0.0827(12) Uani 1 d . . F12 F -0.0599(3) 0.5161(3) 0.0617(2) 0.0662(10) Uani 1 d . . O1 O 0.6532(3) 0.7400(3) 0.1620(2) 0.0438(9) Uani 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 Ni1 0.0246(3) 0.0253(3) 0.0201(3) -0.0003(2) 0.0031(2) -0.0007(3) N11 0.024(2) 0.032(2) 0.023(2) -0.003(2) 0.0028(15) -0.002(2) N12 0.029(2) 0.042(2) 0.026(2) 0.004(2) 0.000(2) 0.001(2) C13 0.048(3) 0.046(3) 0.023(2) -0.001(2) 0.003(2) -0.020(3) C14 0.050(3) 0.032(3) 0.031(3) -0.005(2) 0.015(2) -0.006(2) C15 0.032(3) 0.025(2) 0.028(2) -0.006(2) 0.011(2) -0.004(2) N21 0.027(2) 0.030(2) 0.025(2) 0.001(2) 0.005(2) 0.001(2) C22 0.027(2) 0.028(3) 0.030(2) 0.003(2) 0.009(2) 0.000(2) C23 0.039(3) 0.032(3) 0.055(3) -0.001(3) 0.015(2) 0.008(2) C24 0.044(3) 0.043(3) 0.063(4) 0.014(3) 0.016(3) 0.016(3) C25 0.032(3) 0.052(4) 0.048(3) 0.014(3) 0.005(2) 0.011(3) C26 0.031(3) 0.042(3) 0.027(2) 0.005(2) -0.001(2) 0.003(2) N31 0.028(2) 0.025(2) 0.026(2) -0.004(2) 0.002(2) -0.003(2) N32 0.033(2) 0.026(2) 0.032(2) -0.002(2) 0.007(2) -0.005(2) C33 0.029(3) 0.039(3) 0.040(3) -0.014(2) 0.001(2) -0.002(2) C34 0.036(3) 0.046(3) 0.030(3) -0.007(2) 0.000(2) 0.001(2) C35 0.025(2) 0.030(3) 0.025(2) -0.004(2) 0.001(2) 0.005(2) N41 0.027(2) 0.025(2) 0.024(2) 0.000(2) 0.0032(14) 0.000(2) C42 0.030(2) 0.025(2) 0.024(2) 0.001(2) 0.004(2) 0.008(2) C43 0.037(3) 0.031(3) 0.026(2) 0.000(2) 0.005(2) 0.006(2) C44 0.047(3) 0.037(3) 0.033(3) 0.005(2) 0.016(2) -0.001(2) C45 0.034(3) 0.037(3) 0.043(3) 0.003(2) 0.011(2) -0.010(2) C46 0.032(3) 0.033(3) 0.032(3) -0.007(2) 0.007(2) -0.005(2) N51 0.027(2) 0.028(2) 0.025(2) -0.001(2) 0.006(2) -0.003(2) N52 0.031(2) 0.039(2) 0.031(2) -0.002(2) 0.006(2) -0.001(2) C53 0.036(3) 0.049(3) 0.032(3) 0.004(2) 0.014(2) -0.005(2) C54 0.047(3) 0.043(3) 0.034(3) 0.009(2) 0.003(2) 0.000(3) C55 0.037(3) 0.028(3) 0.027(2) -0.001(2) 0.001(2) -0.004(2) N61 0.029(2) 0.030(2) 0.028(2) -0.006(2) 0.000(2) 0.004(2) C62 0.038(3) 0.025(2) 0.028(2) -0.004(2) -0.004(2) -0.006(2) C63 0.045(3) 0.031(3) 0.038(3) 0.003(2) 0.000(2) -0.002(2) C64 0.045(3) 0.031(3) 0.045(3) -0.002(2) -0.007(2) 0.000(2) C65 0.033(3) 0.037(3) 0.047(3) -0.010(2) 0.002(2) 0.006(2) C66 0.039(3) 0.035(3) 0.030(2) -0.002(2) 0.005(2) 0.002(2) P1 0.0572(9) 0.0366(8) 0.0288(7) 0.0020(6) 0.0064(6) -0.0015(7) F1 0.092(3) 0.132(4) 0.137(4) 0.071(3) 0.054(3) 0.016(3) F2 0.234(6) 0.041(2) 0.069(3) 0.009(2) 0.046(3) 0.032(3) F3 0.116(3) 0.101(3) 0.042(2) 0.003(2) -0.019(2) 0.016(3) F4 0.127(4) 0.060(2) 0.068(2) 0.008(2) 0.028(2) 0.030(2) F5 0.161(5) 0.097(3) 0.067(3) 0.025(2) -0.049(3) -0.044(3) F6 0.063(3) 0.146(4) 0.130(4) 0.069(3) 0.047(3) 0.024(3) P2 0.0321(7) 0.0471(8) 0.0430(8) 0.0087(7) 0.0028(6) 0.0028(7) F7 0.049(2) 0.125(4) 0.077(3) 0.057(2) 0.017(2) -0.001(2) F8 0.067(2) 0.113(3) 0.054(2) 0.012(2) -0.014(2) 0.017(2) F9 0.065(2) 0.062(2) 0.088(3) -0.017(2) 0.012(2) 0.014(2) F10 0.052(2) 0.076(2) 0.051(2) 0.018(2) -0.008(2) -0.010(2) F11 0.110(3) 0.048(2) 0.087(3) 0.008(2) -0.003(2) 0.012(2) F12 0.036(2) 0.077(3) 0.088(3) 0.025(2) 0.019(2) 0.012(2) O1 0.040(2) 0.049(2) 0.043(2) -0.003(2) 0.013(2) -0.010(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 Ni1 N31 2.056(4) . ? Ni1 N51 2.074(4) . ? Ni1 N11 2.080(4) . ? Ni1 N41 2.101(4) . ? Ni1 N61 2.127(4) . ? Ni1 N21 2.128(4) . ? N11 C15 1.334(6) . ? N11 N12 1.347(5) . ? N12 C13 1.349(6) . ? C13 C14 1.383(7) . ? C14 C15 1.402(6) . ? C15 C22 1.468(6) . ? N21 C26 1.339(6) . ? N21 C22 1.355(6) . ? C22 C23 1.383(6) . ? C23 C24 1.375(7) . ? C24 C25 1.369(8) . ? C25 C26 1.374(7) . ? N31 C35 1.333(5) . ? N31 N32 1.341(5) . ? N32 C33 1.336(6) . ? C33 C34 1.374(7) . ? C34 C35 1.410(6) . ? C35 C42 1.469(6) . ? N41 C46 1.337(6) . ? N41 C42 1.360(5) . ? C42 C43 1.377(6) . ? C43 C44 1.375(7) . ? C44 C45 1.382(7) . ? C45 C46 1.378(6) . ? N51 C55 1.335(6) . ? N51 N52 1.343(5) . ? N52 C53 1.345(6) . ? C53 C54 1.373(7) . ? C54 C55 1.419(7) . ? C55 C62 1.455(7) . ? N61 C66 1.345(6) . ? N61 C62 1.360(6) . ? C62 C63 1.377(7) . ? C63 C64 1.389(7) . ? C64 C65 1.377(7) . ? C65 C66 1.376(7) . ? P1 F2 1.546(4) . ? P1 F6 1.552(4) . ? P1 F3 1.560(4) . ? P1 F5 1.576(4) . ? P1 F4 1.605(4) . ? P1 F1 1.606(4) . ? P2 F8 1.577(3) . ? P2 F11 1.582(4) . ? P2 F10 1.585(3) . ? P2 F9 1.594(4) . ? P2 F7 1.594(3) . ? P2 F12 1.612(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Ni1 N51 95.66(14) . . ? N31 Ni1 N11 167.53(14) . . ? N51 Ni1 N11 91.82(14) . . ? N31 Ni1 N41 78.43(14) . . ? N51 Ni1 N41 170.72(14) . . ? N11 Ni1 N41 95.28(14) . . ? N31 Ni1 N61 96.36(14) . . ? N51 Ni1 N61 77.75(15) . . ? N11 Ni1 N61 94.96(14) . . ? N41 Ni1 N61 95.67(14) . . ? N31 Ni1 N21 92.15(14) . . ? N51 Ni1 N21 92.50(14) . . ? N11 Ni1 N21 77.54(14) . . ? N41 Ni1 N21 94.85(14) . . ? N61 Ni1 N21 167.60(14) . . ? C15 N11 N12 105.8(4) . . ? C15 N11 Ni1 115.1(3) . . ? N12 N11 Ni1 137.1(3) . . ? N11 N12 C13 111.6(4) . . ? N12 C13 C14 107.1(4) . . ? C13 C14 C15 104.7(4) . . ? N11 C15 C14 110.8(4) . . ? N11 C15 C22 117.0(4) . . ? C14 C15 C22 132.2(4) . . ? C26 N21 C22 117.6(4) . . ? C26 N21 Ni1 127.9(3) . . ? C22 N21 Ni1 114.5(3) . . ? N21 C22 C23 122.0(4) . . ? N21 C22 C15 114.4(4) . . ? C23 C22 C15 123.6(4) . . ? C24 C23 C22 119.6(5) . . ? C25 C24 C23 118.3(5) . . ? C24 C25 C26 119.9(5) . . ? N21 C26 C25 122.6(5) . . ? C35 N31 N32 105.7(3) . . ? C35 N31 Ni1 115.7(3) . . ? N32 N31 Ni1 137.7(3) . . ? C33 N32 N31 111.7(4) . . ? N32 C33 C34 107.9(4) . . ? C33 C34 C35 104.2(4) . . ? N31 C35 C34 110.5(4) . . ? N31 C35 C42 116.7(4) . . ? C34 C35 C42 132.8(4) . . ? C46 N41 C42 118.1(4) . . ? C46 N41 Ni1 127.4(3) . . ? C42 N41 Ni1 114.5(3) . . ? N41 C42 C43 121.9(4) . . ? N41 C42 C35 114.3(4) . . ? C43 C42 C35 123.7(4) . . ? C44 C43 C42 119.4(4) . . ? C43 C44 C45 118.7(4) . . ? C46 C45 C44 119.4(4) . . ? N41 C46 C45 122.3(4) . . ? C55 N51 N52 106.3(4) . . ? C55 N51 Ni1 115.8(3) . . ? N52 N51 Ni1 138.0(3) . . ? N51 N52 C53 111.3(4) . . ? N52 C53 C54 108.0(4) . . ? C53 C54 C55 104.4(4) . . ? N51 C55 C54 110.0(4) . . ? N51 C55 C62 117.3(4) . . ? C54 C55 C62 132.7(4) . . ? C66 N61 C62 117.2(4) . . ? C66 N61 Ni1 128.4(3) . . ? C62 N61 Ni1 114.4(3) . . ? N61 C62 C63 123.2(5) . . ? N61 C62 C55 114.7(4) . . ? C63 C62 C55 122.1(4) . . ? C62 C63 C64 118.1(5) . . ? C65 C64 C63 119.4(5) . . ? C66 C65 C64 119.3(5) . . ? N61 C66 C65 122.8(5) . . ? F2 P1 F6 94.9(3) . . ? F2 P1 F3 92.6(2) . . ? F6 P1 F3 94.6(3) . . ? F2 P1 F5 90.6(3) . . ? F6 P1 F5 89.0(3) . . ? F3 P1 F5 174.9(3) . . ? F2 P1 F4 173.9(3) . . ? F6 P1 F4 89.9(2) . . ? F3 P1 F4 90.6(2) . . ? F5 P1 F4 85.8(2) . . ? F2 P1 F1 87.5(3) . . ? F6 P1 F1 177.3(3) . . ? F3 P1 F1 86.5(3) . . ? F5 P1 F1 89.7(3) . . ? F4 P1 F1 87.6(2) . . ? F8 P2 F11 89.5(2) . . ? F8 P2 F10 179.4(2) . . ? F11 P2 F10 90.8(2) . . ? F8 P2 F9 91.4(2) . . ? F11 P2 F9 178.0(2) . . ? F10 P2 F9 88.2(2) . . ? F8 P2 F7 91.1(2) . . ? F11 P2 F7 91.8(2) . . ? F10 P2 F7 89.4(2) . . ? F9 P2 F7 90.0(2) . . ? F8 P2 F12 89.8(2) . . ? F11 P2 F12 90.2(2) . . ? F10 P2 F12 89.7(2) . . ? F9 P2 F12 88.0(2) . . ? F7 P2 F12 177.8(2) . . ? _refine_diff_density_max 0.990 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.091 #=END data_/tintin3/people/leigh/gnral/kzn/kzn _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H23 F12 N9 O P2 Zn' _chemical_formula_weight 808.82 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 11.5877(14) _cell_length_b 12.651(2) _cell_length_c 21.630(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.208(13) _cell_angle_gamma 90.00 _cell_volume 3152.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 171(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method ? _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 171(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14695 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5537 _reflns_number_observed 4608 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens 1995b)' _computing_cell_refinement 'SAINT (Siemens 1995b)' _computing_data_reduction 'SAINT (Siemens 1995b)' _computing_structure_solution 'SHELXTL (Siemens 1995a)' _computing_structure_refinement 'SHELXTL (Siemens 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens 1995a)' _computing_publication_material 'SHELXTL (Siemens 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+9.7755P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5532 _refine_ls_number_parameters 469 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_obs 0.0603 _refine_ls_wR_factor_all 0.1699 _refine_ls_wR_factor_obs 0.1549 _refine_ls_goodness_of_fit_all 1.068 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.074 _refine_ls_restrained_S_obs 1.081 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.32095(4) 0.52700(4) 0.17633(2) 0.0290(2) Uani 1 d . . N11 N 0.2295(3) 0.4928(3) 0.2553(2) 0.0328(8) Uani 1 d . . C12 C 0.1323(4) 0.4341(4) 0.2559(2) 0.0426(12) Uani 1 d . . H12 H 0.1000(22) 0.4071(18) 0.2211(23) 0.051 Uiso 1 calc R . C13 C 0.0834(5) 0.4160(4) 0.3093(2) 0.0467(13) Uani 1 d . . H13 H 0.0292(45) 0.3856(26) 0.3083(3) 0.056 Uiso 1 calc R . C14 C 0.1341(5) 0.4538(4) 0.3647(3) 0.0490(13) Uani 1 d . . H14 H 0.0972(22) 0.4383(10) 0.4062(24) 0.059 Uiso 1 calc R . C15 C 0.2336(5) 0.5121(4) 0.3657(2) 0.0416(12) Uani 1 d . . H15 H 0.2681(24) 0.5364(17) 0.4006(24) 0.050 Uiso 1 calc R . C16 C 0.2787(4) 0.5317(4) 0.3100(2) 0.0335(10) Uani 1 d . . C17 C 0.3827(4) 0.5962(4) 0.3061(2) 0.0342(10) Uani 1 d . . C18 C 0.4609(5) 0.6461(5) 0.3514(3) 0.0500(14) Uani 1 d . . H18 H 0.4583(5) 0.6474(5) 0.3871(29) 0.060 Uiso 1 calc R . C19 C 0.5432(4) 0.6919(4) 0.3185(3) 0.0466(13) Uani 1 d . . H19 H 0.5969(42) 0.7242(26) 0.3323(11) 0.056 Uiso 1 calc R . N110 N 0.5136(3) 0.6706(3) 0.2586(2) 0.0386(10) Uani 1 d . . H110 H 0.5455(26) 0.6876(14) 0.2343(20) 0.046 Uiso 1 calc R . N111 N 0.4154(3) 0.6129(3) 0.2499(2) 0.0329(8) Uani 1 d . . N21 N 0.4431(3) 0.3935(3) 0.1894(2) 0.0337(8) Uani 1 d . . C22 C 0.5408(4) 0.3858(5) 0.2291(2) 0.0421(12) Uani 1 d . . H22 H 0.5577(13) 0.4352(37) 0.2532(18) 0.051 Uiso 1 calc R . C23 C 0.6127(5) 0.3009(5) 0.2314(3) 0.0562(15) Uani 1 d . . H23 H 0.6845(46) 0.2985(5) 0.2630(20) 0.067 Uiso 1 calc R . C24 C 0.5889(5) 0.2207(6) 0.1921(3) 0.062(2) Uani 1 d . . H24 H 0.6452(37) 0.1557(43) 0.1925(3) 0.074 Uiso 1 calc R . C25 C 0.4909(5) 0.2239(4) 0.1514(3) 0.0508(14) Uani 1 d . . H25 H 0.4739(13) 0.1714(39) 0.1256(19) 0.061 Uiso 1 calc R . C26 C 0.4179(4) 0.3111(4) 0.1511(2) 0.0365(10) Uani 1 d . . C27 C 0.3102(4) 0.3216(3) 0.1096(2) 0.0330(10) Uani 1 d . . C28 C 0.2650(5) 0.2601(4) 0.0586(2) 0.0448(13) Uani 1 d . . H28 H 0.2938(22) 0.2050(41) 0.0445(11) 0.054 Uiso 1 calc R . C29 C 0.1625(5) 0.3105(5) 0.0366(2) 0.0530(15) Uani 1 d . . H29 H 0.1143(35) 0.2911(15) 0.0045(23) 0.064 Uiso 1 calc R . N210 N 0.1498(4) 0.3959(4) 0.0740(2) 0.0413(10) Uani 1 d . . H210 H 0.0900(40) 0.4409(30) 0.0697(3) 0.050 Uiso 1 calc R . N211 N 0.2408(3) 0.4024(3) 0.1184(2) 0.0318(8) Uani 1 d . . N31 N 0.2053(3) 0.6529(3) 0.1372(2) 0.0375(9) Uani 1 d . . C32 C 0.1042(5) 0.6838(4) 0.1566(2) 0.0449(12) Uani 1 d . . H32 H 0.0800(18) 0.6538(21) 0.1882(22) 0.054 Uiso 1 calc R . C33 C 0.0388(4) 0.7630(4) 0.1264(2) 0.0454(13) Uani 1 d . . H33 H -0.0217(45) 0.7812(14) 0.1389(10) 0.054 Uiso 1 calc R . C34 C 0.0754(5) 0.8106(4) 0.0757(3) 0.0509(13) Uani 1 d . . H34 H 0.0234(30) 0.8733(35) 0.0517(14) 0.061 Uiso 1 calc R . C35 C 0.1774(5) 0.7799(4) 0.0546(3) 0.0496(13) Uani 1 d . . H35 H 0.2076(17) 0.8165(21) 0.0134(23) 0.059 Uiso 1 calc R . C36 C 0.2411(5) 0.7016(4) 0.0869(2) 0.0393(11) Uani 1 d . . C37 C 0.3527(4) 0.6675(4) 0.0693(2) 0.0398(11) Uani 1 d . . C38 C 0.4207(5) 0.6996(5) 0.0210(3) 0.060(2) Uani 1 d . . H38 H 0.4061(14) 0.7422(39) -0.0034(22) 0.071 Uiso 1 calc R . C39 C 0.5175(5) 0.6371(5) 0.0281(3) 0.0497(13) Uani 1 d . . H39 H 0.5779(41) 0.6387(5) 0.0045(16) 0.060 Uiso 1 calc R . N310 N 0.5063(4) 0.5730(4) 0.0766(2) 0.0444(10) Uani 1 d . . H310 H 0.5575(36) 0.5250(34) 0.0900(10) 0.053 Uiso 1 calc R . N311 N 0.4079(3) 0.5907(3) 0.1022(2) 0.0359(9) Uani 1 d . . P1 P 0.76222(13) 0.47816(11) 0.42458(6) 0.0453(3) Uani 1 d . . P2 P 0.82676(13) 0.47834(13) 0.09693(8) 0.0547(4) Uani 1 d . . F1 F 0.6521(5) 0.4969(5) 0.4620(3) 0.128(2) Uani 1 d . . F2 F 0.7348(5) 0.3535(3) 0.4292(2) 0.0962(15) Uani 1 d . . F3 F 0.8334(5) 0.4760(4) 0.4898(2) 0.100(2) Uani 1 d . . F4 F 0.7706(5) 0.6001(3) 0.4193(2) 0.109(2) Uani 1 d . . F5 F 0.6798(5) 0.4744(4) 0.3616(2) 0.106(2) Uani 1 d . . F6 F 0.8654(4) 0.4546(5) 0.3883(3) 0.125(2) Uani 1 d . . F7 F 0.8091(4) 0.5993(3) 0.1124(2) 0.0865(12) Uani 1 d . . F8 F 0.7153(3) 0.4484(4) 0.1304(2) 0.103(2) Uani 1 d . . F9 F 0.9094(4) 0.4603(4) 0.1585(2) 0.100(2) Uani 1 d . . F10 F 0.8459(5) 0.3610(3) 0.0782(2) 0.108(2) Uani 1 d . . F11 F 0.7449(3) 0.4976(3) 0.0345(2) 0.0785(12) Uani 1 d . . F12 F 0.9374(3) 0.5127(4) 0.0621(2) 0.0887(13) Uani 1 d . . O1 O 0.6531(4) 0.7347(3) 0.1685(2) 0.0598(11) Uani 1 d D . H2 H 0.7007(52) 0.6846(45) 0.1568(30) 0.072 Uiso 1 d D . H1 H 0.6544(57) 0.7946(42) 0.1470(29) 0.072 Uiso 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 Zn1 0.0317(3) 0.0314(3) 0.0242(3) -0.0004(2) 0.0035(2) 0.0003(2) N11 0.032(2) 0.038(2) 0.029(2) 0.001(2) 0.006(2) -0.001(2) C12 0.046(3) 0.045(3) 0.037(3) -0.008(2) 0.006(2) -0.006(2) C13 0.043(3) 0.049(3) 0.051(3) 0.000(2) 0.019(2) -0.015(2) C14 0.062(4) 0.043(3) 0.045(3) 0.001(2) 0.021(3) 0.004(3) C15 0.049(3) 0.046(3) 0.031(2) 0.000(2) 0.009(2) 0.007(2) C16 0.038(3) 0.032(2) 0.030(2) 0.002(2) 0.005(2) 0.012(2) C17 0.036(2) 0.035(2) 0.032(2) -0.007(2) 0.001(2) 0.007(2) C18 0.046(3) 0.066(4) 0.037(3) -0.013(3) 0.001(2) 0.005(3) C19 0.034(3) 0.050(3) 0.054(3) -0.018(3) -0.004(2) -0.003(2) N110 0.037(2) 0.035(2) 0.044(2) -0.004(2) 0.006(2) -0.002(2) N111 0.036(2) 0.032(2) 0.031(2) -0.004(2) 0.002(2) -0.003(2) N21 0.033(2) 0.034(2) 0.034(2) 0.002(2) 0.006(2) 0.001(2) C22 0.034(3) 0.052(3) 0.040(3) 0.006(2) -0.001(2) -0.003(2) C23 0.043(3) 0.068(4) 0.058(3) 0.018(3) 0.008(3) 0.011(3) C24 0.049(3) 0.064(4) 0.074(4) 0.006(3) 0.013(3) 0.012(3) C25 0.049(3) 0.040(3) 0.066(4) 0.001(3) 0.016(3) 0.005(2) C26 0.037(3) 0.035(2) 0.041(3) 0.004(2) 0.015(2) 0.001(2) C27 0.038(2) 0.030(2) 0.032(2) -0.002(2) 0.011(2) -0.006(2) C28 0.059(3) 0.037(3) 0.042(3) -0.008(2) 0.018(2) -0.010(2) C29 0.063(4) 0.063(4) 0.032(3) -0.001(2) 0.000(2) -0.030(3) N210 0.036(2) 0.052(3) 0.035(2) 0.005(2) -0.002(2) -0.004(2) N211 0.032(2) 0.036(2) 0.028(2) -0.002(2) 0.003(2) -0.004(2) N31 0.038(2) 0.038(2) 0.036(2) -0.006(2) 0.000(2) 0.004(2) C32 0.051(3) 0.045(3) 0.038(3) -0.003(2) 0.002(2) 0.008(2) C33 0.034(3) 0.048(3) 0.054(3) -0.010(2) 0.003(2) 0.008(2) C34 0.051(3) 0.041(3) 0.058(3) -0.003(3) -0.005(3) -0.001(3) C35 0.051(3) 0.042(3) 0.054(3) 0.004(2) -0.004(3) -0.001(2) C36 0.054(3) 0.028(2) 0.033(2) 0.000(2) -0.010(2) -0.008(2) C37 0.046(3) 0.042(3) 0.031(2) 0.002(2) 0.002(2) -0.012(2) C38 0.067(4) 0.057(4) 0.055(3) 0.014(3) 0.005(3) -0.001(3) C39 0.043(3) 0.059(3) 0.050(3) 0.012(3) 0.021(2) -0.001(3) N310 0.040(2) 0.053(3) 0.041(2) 0.001(2) 0.010(2) -0.001(2) N311 0.036(2) 0.039(2) 0.033(2) 0.001(2) 0.007(2) -0.008(2) P1 0.0588(9) 0.0443(8) 0.0330(7) -0.0033(6) 0.0056(6) 0.0016(6) P2 0.0427(8) 0.0541(9) 0.0660(10) 0.0114(7) -0.0001(7) 0.0020(7) F1 0.108(4) 0.151(5) 0.137(5) -0.066(4) 0.070(4) -0.031(4) F2 0.153(4) 0.064(3) 0.071(3) 0.004(2) 0.010(3) -0.024(3) F3 0.126(4) 0.111(4) 0.054(2) 0.000(2) -0.029(2) -0.019(3) F4 0.204(6) 0.048(2) 0.077(3) -0.009(2) 0.028(3) -0.021(3) F5 0.134(4) 0.094(3) 0.079(3) -0.021(2) -0.043(3) 0.026(3) F6 0.073(3) 0.175(6) 0.137(5) -0.067(4) 0.052(3) -0.022(3) F7 0.083(3) 0.068(3) 0.111(3) -0.012(2) 0.023(2) 0.013(2) F8 0.060(2) 0.148(4) 0.102(3) 0.073(3) 0.016(2) -0.003(3) F9 0.084(3) 0.133(4) 0.077(3) 0.003(3) -0.023(2) 0.026(3) F10 0.152(4) 0.061(3) 0.101(3) 0.003(2) -0.024(3) 0.017(3) F11 0.070(2) 0.086(3) 0.076(3) 0.027(2) -0.012(2) -0.005(2) F12 0.050(2) 0.107(3) 0.112(3) 0.025(3) 0.026(2) 0.021(2) O1 0.057(3) 0.056(3) 0.069(3) -0.001(2) 0.025(2) -0.006(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 Zn1 N111 2.129(4) . ? Zn1 N311 2.141(4) . ? Zn1 N11 2.149(4) . ? Zn1 N211 2.160(4) . ? Zn1 N31 2.192(4) . ? Zn1 N21 2.201(4) . ? N11 C16 1.349(6) . ? N11 C12 1.350(6) . ? C12 C13 1.361(7) . ? C13 C14 1.363(8) . ? C14 C15 1.367(8) . ? C15 C16 1.387(7) . ? C16 C17 1.465(7) . ? C17 N111 1.328(6) . ? C17 C18 1.411(7) . ? C18 C19 1.378(8) . ? C19 N110 1.330(7) . ? N110 N111 1.348(5) . ? N21 C26 1.343(6) . ? N21 C22 1.349(6) . ? C22 C23 1.357(8) . ? C23 C24 1.334(9) . ? C24 C25 1.360(8) . ? C25 C26 1.390(7) . ? C26 C27 1.463(7) . ? C27 N211 1.328(6) . ? C27 C28 1.404(7) . ? C28 C29 1.386(8) . ? C29 N210 1.367(7) . ? N210 N211 1.349(5) . ? N31 C32 1.344(6) . ? N31 C36 1.355(6) . ? C32 C33 1.377(7) . ? C33 C34 1.359(8) . ? C34 C35 1.368(8) . ? C35 C36 1.380(7) . ? C36 C37 1.452(7) . ? C37 N311 1.328(6) . ? C37 C38 1.435(8) . ? C38 C39 1.367(8) . ? C39 N310 1.345(7) . ? N310 N311 1.339(5) . ? P1 F6 1.528(4) . ? P1 F4 1.550(4) . ? P1 F3 1.556(4) . ? P1 F5 1.578(4) . ? P1 F1 1.601(5) . ? P1 F2 1.614(4) . ? P2 F10 1.561(5) . ? P2 F9 1.571(4) . ? P2 F11 1.584(4) . ? P2 F7 1.585(4) . ? P2 F8 1.593(4) . ? P2 F12 1.615(4) . ? 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 N111 Zn1 N311 97.00(14) . . ? N111 Zn1 N11 76.50(14) . . ? N311 Zn1 N11 169.49(15) . . ? N111 Zn1 N211 163.72(14) . . ? N311 Zn1 N211 92.76(14) . . ? N11 Zn1 N211 95.50(14) . . ? N111 Zn1 N31 99.27(14) . . ? N311 Zn1 N31 75.8(2) . . ? N11 Zn1 N31 96.86(15) . . ? N211 Zn1 N31 95.73(14) . . ? N111 Zn1 N21 91.38(14) . . ? N311 Zn1 N21 92.08(14) . . ? N11 Zn1 N21 96.28(14) . . ? N211 Zn1 N21 75.22(14) . . ? N31 Zn1 N21 164.71(14) . . ? C16 N11 C12 117.7(4) . . ? C16 N11 Zn1 115.2(3) . . ? C12 N11 Zn1 127.0(3) . . ? N11 C12 C13 121.7(5) . . ? C12 C13 C14 120.5(5) . . ? C13 C14 C15 119.1(5) . . ? C14 C15 C16 118.7(5) . . ? N11 C16 C15 122.2(5) . . ? N11 C16 C17 115.1(4) . . ? C15 C16 C17 122.6(4) . . ? N111 C17 C18 109.8(4) . . ? N111 C17 C16 117.3(4) . . ? C18 C17 C16 132.8(4) . . ? C19 C18 C17 105.0(5) . . ? N110 C19 C18 107.3(5) . . ? C19 N110 N111 111.8(4) . . ? C17 N111 N110 106.1(4) . . ? C17 N111 Zn1 115.3(3) . . ? N110 N111 Zn1 137.7(3) . . ? C26 N21 C22 116.6(4) . . ? C26 N21 Zn1 115.0(3) . . ? C22 N21 Zn1 128.4(3) . . ? N21 C22 C23 123.4(5) . . ? C24 C23 C22 119.7(6) . . ? C23 C24 C25 119.4(6) . . ? C24 C25 C26 119.5(6) . . ? N21 C26 C25 121.4(5) . . ? N21 C26 C27 115.0(4) . . ? C25 C26 C27 123.6(5) . . ? N211 C27 C28 111.1(4) . . ? N211 C27 C26 118.1(4) . . ? C28 C27 C26 130.8(5) . . ? C29 C28 C27 104.3(5) . . ? N210 C29 C28 107.7(5) . . ? N211 N210 C29 110.1(4) . . ? C27 N211 N210 106.8(4) . . ? C27 N211 Zn1 114.6(3) . . ? N210 N211 Zn1 135.3(3) . . ? C32 N31 C36 118.1(4) . . ? C32 N31 Zn1 127.5(4) . . ? C36 N31 Zn1 114.4(3) . . ? N31 C32 C33 121.1(5) . . ? C34 C33 C32 120.1(5) . . ? C33 C34 C35 119.9(5) . . ? C34 C35 C36 118.0(5) . . ? N31 C36 C35 122.6(5) . . ? N31 C36 C37 115.8(4) . . ? C35 C36 C37 121.6(5) . . ? N311 C37 C38 109.1(5) . . ? N311 C37 C36 117.9(4) . . ? C38 C37 C36 133.0(5) . . ? C39 C38 C37 105.2(5) . . ? N310 C39 C38 106.9(5) . . ? N311 N310 C39 112.4(5) . . ? C37 N311 N310 106.4(4) . . ? C37 N311 Zn1 116.0(3) . . ? N310 N311 Zn1 137.5(3) . . ? F6 P1 F4 95.6(3) . . ? F6 P1 F3 95.4(3) . . ? F4 P1 F3 93.1(3) . . ? F6 P1 F5 89.2(3) . . ? F4 P1 F5 90.1(3) . . ? F3 P1 F5 174.1(3) . . ? F6 P1 F1 177.2(3) . . ? F4 P1 F1 87.1(3) . . ? F3 P1 F1 85.3(3) . . ? F5 P1 F1 90.0(3) . . ? F6 P1 F2 90.7(3) . . ? F4 P1 F2 172.3(3) . . ? F3 P1 F2 90.9(3) . . ? F5 P1 F2 85.4(3) . . ? F1 P1 F2 86.6(3) . . ? F10 P2 F9 89.5(3) . . ? F10 P2 F11 90.8(3) . . ? F9 P2 F11 179.1(3) . . ? F10 P2 F7 176.9(3) . . ? F9 P2 F7 92.4(3) . . ? F11 P2 F7 87.3(2) . . ? F10 P2 F8 92.1(3) . . ? F9 P2 F8 91.7(3) . . ? F11 P2 F8 89.1(2) . . ? F7 P2 F8 90.2(3) . . ? F10 P2 F12 89.6(3) . . ? F9 P2 F12 89.6(3) . . ? F11 P2 F12 89.6(2) . . ? F7 P2 F12 88.0(2) . . ? F8 P2 F12 177.9(3) . . ? _refine_diff_density_max 1.405 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.092 #=END data_/tintin3/people/ward/claire/kcu/kcu _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H64 Cu4 F12 N22 O4 P2' _chemical_formula_weight 1701.43 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.410(2) _cell_length_b 13.282(3) _cell_length_c 14.170(2) _cell_angle_alpha 85.254(10) _cell_angle_beta 70.087(12) _cell_angle_gamma 68.15(2) _cell_volume 1707.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method ? _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.373 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8183 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5820 _reflns_number_observed 5409 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens 1995b)' _computing_cell_refinement 'SAINT (Siemens 1995b)' _computing_data_reduction 'SAINT (Siemens 1995b)' _computing_structure_solution 'SHELXTL (Siemens 1995a)' _computing_structure_refinement 'SHELXTL (Siemens 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens 1995a)' _computing_publication_material 'SHELXTL (Siemens 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+3.0096P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5820 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all 0.1056 _refine_ls_wR_factor_obs 0.0989 _refine_ls_goodness_of_fit_all 0.934 _refine_ls_goodness_of_fit_obs 0.910 _refine_ls_restrained_S_all 0.934 _refine_ls_restrained_S_obs 0.910 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.10679(3) -0.04038(2) 0.11565(2) 0.02062(11) Uani 1 d . . Cu2 Cu -0.24002(3) 0.22865(2) 0.13841(2) 0.02066(11) Uani 1 d . . N11 N 0.1055(3) -0.1823(2) 0.1865(2) 0.0245(5) Uani 1 d . . C12 C 0.2159(3) -0.2793(2) 0.1693(2) 0.0311(6) Uani 1 d . . H12 H 0.3073(3) -0.2867(2) 0.1190(2) 0.037 Uiso 1 calc R . C13 C 0.2015(4) -0.3684(2) 0.2218(3) 0.0355(7) Uani 1 d . . H13 H 0.2820(4) -0.4359(2) 0.2083(3) 0.043 Uiso 1 calc R . C14 C 0.0689(4) -0.3589(2) 0.2942(2) 0.0344(7) Uani 1 d . . H14 H 0.0569(4) -0.4197(2) 0.3311(2) 0.041 Uiso 1 calc R . C15 C -0.0465(3) -0.2594(2) 0.3123(2) 0.0303(6) Uani 1 d . . H15 H -0.1392(3) -0.2508(2) 0.3616(2) 0.036 Uiso 1 calc R . C16 C -0.0239(3) -0.1729(2) 0.2571(2) 0.0243(6) Uani 1 d . . C17 C -0.1359(3) -0.0641(2) 0.2695(2) 0.0235(5) Uani 1 d . . C18 C -0.2780(3) -0.0177(2) 0.3365(2) 0.0297(6) Uani 1 d . . H18 H -0.3306(3) -0.0510(2) 0.3895(2) 0.036 Uiso 1 calc R . C19 C -0.3248(3) 0.0880(2) 0.3079(2) 0.0282(6) Uani 1 d . . H19 H -0.4190(3) 0.1417(2) 0.3394(2) 0.034 Uiso 1 calc R . N110 N -0.2186(2) 0.1047(2) 0.2291(2) 0.0224(5) Uani 1 d . . N111 N -0.1009(2) 0.0099(2) 0.2052(2) 0.0215(5) Uani 1 d . . N21 N -0.2420(3) 0.3715(2) 0.0669(2) 0.0252(5) Uani 1 d . . C22 C -0.3554(3) 0.4664(2) 0.0784(2) 0.0344(7) Uani 1 d . . H22 H -0.4492(3) 0.4717(2) 0.1240(2) 0.041 Uiso 1 calc R . C23 C -0.3411(4) 0.5565(3) 0.0265(3) 0.0382(7) Uani 1 d . . H23 H -0.4237(4) 0.6223(3) 0.0361(3) 0.046 Uiso 1 calc R . C24 C -0.2052(4) 0.5494(2) -0.0393(2) 0.0341(7) Uani 1 d . . H24 H -0.1926(4) 0.6109(2) -0.0747(2) 0.041 Uiso 1 calc R . C25 C -0.0869(3) 0.4518(2) -0.0532(2) 0.0280(6) Uani 1 d . . H25 H 0.0075(3) 0.4445(2) -0.0992(2) 0.034 Uiso 1 calc R . C26 C -0.1105(3) 0.3646(2) 0.0022(2) 0.0234(5) Uani 1 d . . C27 C 0.0049(3) 0.2579(2) -0.0068(2) 0.0227(5) Uani 1 d . . C28 C 0.1485(3) 0.2127(2) -0.0709(2) 0.0287(6) Uani 1 d . . H28 H 0.2023(3) 0.2470(2) -0.1219(2) 0.034 Uiso 1 calc R . C29 C 0.1958(3) 0.1064(2) -0.0435(2) 0.0274(6) Uani 1 d . . H29 H 0.2909(3) 0.0535(2) -0.0741(2) 0.033 Uiso 1 calc R . N210 N 0.0878(2) 0.0884(2) 0.0327(2) 0.0218(5) Uani 1 d . . N211 N -0.0311(2) 0.1829(2) 0.0554(2) 0.0217(5) Uani 1 d . . N31 N -0.4574(2) 0.2996(2) 0.2225(2) 0.0216(5) Uani 1 d . . C32 C -0.5071(3) 0.3618(2) 0.3074(2) 0.0260(6) Uani 1 d . . H32 H -0.4405(3) 0.3841(2) 0.3242(2) 0.031 Uiso 1 calc R . C33 C -0.6510(3) 0.3942(2) 0.3708(2) 0.0292(6) Uani 1 d . . H33 H -0.6830(3) 0.4380(2) 0.4302(2) 0.035 Uiso 1 calc R . C34 C -0.7479(3) 0.3615(2) 0.3459(2) 0.0300(6) Uani 1 d . . H34 H -0.8471(3) 0.3814(2) 0.3889(2) 0.036 Uiso 1 calc R . C35 C -0.6986(3) 0.2999(2) 0.2580(2) 0.0259(6) Uani 1 d . . H35 H -0.7642(3) 0.2782(2) 0.2392(2) 0.031 Uiso 1 calc R . C36 C -0.5523(3) 0.2697(2) 0.1972(2) 0.0221(5) Uani 1 d . . C47 C 0.4903(3) -0.2034(2) -0.1036(2) 0.0217(5) Uani 1 d . . C48 C 0.5536(3) -0.1618(2) -0.0518(2) 0.0257(6) Uani 1 d . . H48 H 0.6535(3) -0.1693(2) -0.0702(2) 0.031 Uiso 1 calc R . C49 C 0.4382(3) -0.1071(2) 0.0320(2) 0.0252(6) Uani 1 d . . H49 H 0.4455(3) -0.0697(2) 0.0831(2) 0.030 Uiso 1 calc R . N410 N 0.3134(2) -0.1148(2) 0.0304(2) 0.0228(5) Uani 1 d . . N411 N 0.3453(2) -0.1744(2) -0.0528(2) 0.0222(5) Uani 1 d . . O51 O 0.1899(2) 0.0132(2) 0.2297(2) 0.0380(5) Uani 1 d . . C52 C 0.1040(4) 0.0653(3) 0.3078(2) 0.0370(7) Uani 1 d . . H52 H 0.0027(4) 0.0937(3) 0.3151(2) 0.044 Uiso 1 calc R . N53 N 0.1404(4) 0.0853(2) 0.3830(2) 0.0484(8) Uani 1 d . . C54 C 0.0277(7) 0.1426(4) 0.4755(3) 0.085(2) Uani 1 d . . H54A H 0.0410(28) 0.2093(18) 0.4868(17) 0.128 Uiso 1 calc R . H54B H 0.0358(30) 0.0960(13) 0.5322(6) 0.128 Uiso 1 calc R . H54C H -0.0696(7) 0.1610(30) 0.4698(13) 0.128 Uiso 1 calc R . C55 C 0.2942(5) 0.0486(4) 0.3768(4) 0.0641(12) Uani 1 d . . H55A H 0.3171(11) -0.0159(17) 0.4161(21) 0.096 Uiso 1 calc R . H55B H 0.3108(10) 0.1065(11) 0.4038(24) 0.096 Uiso 1 calc R . H55C H 0.3576(5) 0.0307(27) 0.3065(4) 0.096 Uiso 1 calc R . P1 P -0.17742(9) -0.55855(7) 0.33459(7) 0.0377(2) Uani 1 d . . F1 F -0.1755(3) -0.6753(2) 0.3179(3) 0.0881(10) Uani 1 d . . F6 F -0.1860(3) -0.4405(2) 0.3555(3) 0.0898(9) Uani 1 d . . F3 F -0.1094(3) -0.5999(3) 0.4222(2) 0.0868(10) Uani 1 d . . F4 F -0.0184(2) -0.5850(2) 0.2557(2) 0.0722(7) Uani 1 d . . F5 F -0.2490(3) -0.5162(3) 0.2498(2) 0.0759(8) Uani 1 d . . F2 F -0.3375(2) -0.5289(2) 0.4151(2) 0.0593(6) Uani 1 d . . C1 C 0.5487(6) -0.2289(4) 0.2800(3) 0.0707(13) Uani 1 d . . H1A H 0.4800(6) -0.1848(26) 0.2462(12) 0.106 Uiso 1 calc R . H1B H 0.6148(31) -0.2964(4) 0.2397(10) 0.106 Uiso 1 calc R . H1C H 0.6065(32) -0.1883(27) 0.2878(3) 0.106 Uiso 1 calc R . C2 C 0.3741(5) -0.3124(4) 0.3797(3) 0.0610(11) Uani 1 d . . H2A H 0.4325(8) -0.3806(13) 0.3389(20) 0.092 Uiso 1 calc R . H2B H 0.2970(22) -0.2678(11) 0.3526(23) 0.092 Uiso 1 calc R . H2C H 0.3290(28) -0.3284(24) 0.4492(4) 0.092 Uiso 1 calc R . N3 N 0.4681(3) -0.2542(2) 0.3772(2) 0.0389(6) Uani 1 d . . C4 C 0.4912(4) -0.2360(3) 0.4598(3) 0.0456(8) Uani 1 d . . H4 H 0.4380(4) -0.2587(3) 0.5210(3) 0.055 Uiso 1 calc R . O5 O 0.5749(3) -0.1925(2) 0.4646(2) 0.0485(6) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0173(2) 0.0211(2) 0.0224(2) 0.00110(12) -0.00656(13) -0.00603(13) Cu2 0.0146(2) 0.0215(2) 0.0240(2) 0.00310(13) -0.00541(13) -0.00599(13) N11 0.0236(12) 0.0235(12) 0.0279(12) 0.0025(9) -0.0118(10) -0.0077(10) C12 0.0255(15) 0.0281(15) 0.037(2) 0.0020(12) -0.0113(13) -0.0066(12) C13 0.033(2) 0.0261(15) 0.046(2) 0.0049(13) -0.0186(14) -0.0050(13) C14 0.039(2) 0.0235(14) 0.045(2) 0.0087(12) -0.0191(15) -0.0124(13) C15 0.029(2) 0.0289(15) 0.035(2) 0.0057(12) -0.0119(13) -0.0126(12) C16 0.0269(14) 0.0248(14) 0.0245(13) 0.0020(10) -0.0118(11) -0.0103(11) C17 0.0251(14) 0.0235(13) 0.0241(13) 0.0027(10) -0.0097(11) -0.0102(11) C18 0.0263(15) 0.0301(15) 0.0292(15) 0.0059(12) -0.0042(12) -0.0119(12) C19 0.0218(14) 0.0297(15) 0.0270(14) 0.0033(11) -0.0031(11) -0.0080(12) N110 0.0184(11) 0.0228(11) 0.0236(11) 0.0011(9) -0.0058(9) -0.0063(9) N111 0.0215(11) 0.0208(11) 0.0219(11) 0.0017(9) -0.0076(9) -0.0071(9) N21 0.0220(12) 0.0247(12) 0.0289(12) 0.0056(9) -0.0097(10) -0.0084(10) C22 0.0250(15) 0.031(2) 0.038(2) 0.0084(13) -0.0063(13) -0.0054(12) C23 0.034(2) 0.028(2) 0.043(2) 0.0102(13) -0.0123(14) -0.0038(13) C24 0.038(2) 0.029(2) 0.036(2) 0.0110(12) -0.0150(14) -0.0132(13) C25 0.0265(14) 0.0292(15) 0.0317(15) 0.0084(12) -0.0123(12) -0.0131(12) C26 0.0233(14) 0.0264(14) 0.0235(13) 0.0018(11) -0.0112(11) -0.0093(11) C27 0.0215(13) 0.0251(14) 0.0249(13) 0.0059(10) -0.0104(11) -0.0107(11) C28 0.0212(14) 0.0322(15) 0.0317(15) 0.0084(12) -0.0062(12) -0.0125(12) C29 0.0167(13) 0.0324(15) 0.0289(14) 0.0020(11) -0.0049(11) -0.0070(11) N210 0.0171(11) 0.0237(11) 0.0219(11) 0.0007(9) -0.0049(9) -0.0060(9) N211 0.0180(11) 0.0235(11) 0.0248(11) 0.0031(9) -0.0085(9) -0.0080(9) N31 0.0183(11) 0.0197(11) 0.0255(11) 0.0035(9) -0.0072(9) -0.0062(9) C32 0.0262(14) 0.0241(13) 0.0260(14) 0.0004(11) -0.0093(11) -0.0067(11) C33 0.030(2) 0.0248(14) 0.0260(14) -0.0023(11) -0.0079(12) -0.0032(12) C34 0.0185(13) 0.032(2) 0.0298(15) 0.0052(12) -0.0034(11) -0.0031(11) C35 0.0169(13) 0.0277(14) 0.0304(14) 0.0047(11) -0.0074(11) -0.0063(11) C36 0.0207(13) 0.0184(12) 0.0252(13) 0.0055(10) -0.0078(11) -0.0057(10) C47 0.0159(12) 0.0212(13) 0.0258(13) 0.0053(10) -0.0069(10) -0.0054(10) C48 0.0170(13) 0.0252(14) 0.034(2) 0.0027(11) -0.0096(11) -0.0068(11) C49 0.0262(14) 0.0242(13) 0.0306(14) 0.0019(11) -0.0148(12) -0.0106(11) N410 0.0216(11) 0.0223(11) 0.0253(12) 0.0003(9) -0.0094(9) -0.0073(9) N411 0.0171(11) 0.0230(11) 0.0240(11) 0.0007(9) -0.0059(9) -0.0054(9) O51 0.0336(12) 0.0478(13) 0.0331(12) -0.0095(10) -0.0131(10) -0.0114(10) C52 0.037(2) 0.040(2) 0.034(2) -0.0030(14) -0.0154(14) -0.0103(14) N53 0.068(2) 0.040(2) 0.040(2) -0.0042(12) -0.030(2) -0.0094(15) C54 0.109(4) 0.080(3) 0.046(2) -0.025(2) -0.030(3) -0.005(3) C55 0.080(3) 0.053(2) 0.079(3) 0.004(2) -0.061(3) -0.016(2) P1 0.0282(4) 0.0489(5) 0.0406(5) 0.0055(4) -0.0123(4) -0.0191(4) F1 0.060(2) 0.0432(14) 0.154(3) -0.016(2) -0.031(2) -0.0116(12) F6 0.076(2) 0.067(2) 0.142(3) -0.004(2) -0.031(2) -0.0457(15) F3 0.057(2) 0.145(3) 0.073(2) 0.040(2) -0.0400(14) -0.043(2) F4 0.0322(12) 0.105(2) 0.0625(15) 0.0112(14) -0.0028(11) -0.0197(12) F5 0.0559(15) 0.117(2) 0.0544(14) 0.0157(14) -0.0303(12) -0.0228(15) F2 0.0378(12) 0.081(2) 0.0556(13) -0.0102(11) -0.0054(10) -0.0243(11) C1 0.092(4) 0.072(3) 0.038(2) 0.002(2) 0.001(2) -0.040(3) C2 0.054(2) 0.079(3) 0.058(2) 0.008(2) -0.019(2) -0.034(2) N3 0.0380(15) 0.042(2) 0.0319(14) 0.0081(11) -0.0081(12) -0.0141(12) C4 0.044(2) 0.047(2) 0.042(2) 0.014(2) -0.012(2) -0.017(2) O5 0.053(2) 0.0515(15) 0.0485(14) 0.0070(11) -0.0142(12) -0.0301(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 Cu1 N410 1.977(2) . ? Cu1 N210 1.980(2) . ? Cu1 N111 1.982(2) . ? Cu1 N11 2.064(2) . ? Cu1 O51 2.339(2) . ? Cu2 N211 1.968(2) . ? Cu2 N110 1.996(2) . ? Cu2 N31 2.047(2) . ? Cu2 N21 2.073(2) . ? Cu2 N411 2.198(2) 2 ? N11 C12 1.341(4) . ? N11 C16 1.345(4) . ? C12 C13 1.373(4) . ? C13 C14 1.378(5) . ? C14 C15 1.386(4) . ? C15 C16 1.384(4) . ? C16 C17 1.458(4) . ? C17 N111 1.350(3) . ? C17 C18 1.390(4) . ? C18 C19 1.380(4) . ? C19 N110 1.349(4) . ? N110 N111 1.357(3) . ? N21 C26 1.337(4) . ? N21 C22 1.343(4) . ? C22 C23 1.380(4) . ? C23 C24 1.378(5) . ? C24 C25 1.387(4) . ? C25 C26 1.397(4) . ? C26 C27 1.458(4) . ? C27 N211 1.348(3) . ? C27 C28 1.385(4) . ? C28 C29 1.381(4) . ? C29 N210 1.348(4) . ? N210 N211 1.360(3) . ? N31 C32 1.349(4) . ? N31 C36 1.349(3) . ? C32 C33 1.380(4) . ? C33 C34 1.387(4) . ? C34 C35 1.381(4) . ? C35 C36 1.390(4) . ? C36 C47 1.463(4) 2 ? C47 N411 1.349(3) . ? C47 C48 1.394(4) . ? C47 C36 1.463(4) 2 ? C48 C49 1.379(4) . ? C49 N410 1.348(4) . ? N410 N411 1.349(3) . ? N411 Cu2 2.198(2) 2 ? O51 C52 1.222(4) . ? C52 N53 1.321(4) . ? N53 C54 1.459(5) . ? N53 C55 1.462(5) . ? P1 F4 1.577(2) . ? P1 F1 1.580(3) . ? P1 F5 1.582(2) . ? P1 F6 1.584(3) . ? P1 F2 1.589(2) . ? P1 F3 1.594(3) . ? C1 N3 1.435(5) . ? C2 N3 1.447(5) . ? N3 C4 1.329(5) . ? C4 O5 1.233(4) . ? 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 N410 Cu1 N210 91.57(9) . . ? N410 Cu1 N111 170.61(9) . . ? N210 Cu1 N111 96.64(9) . . ? N410 Cu1 N11 90.51(9) . . ? N210 Cu1 N11 168.85(9) . . ? N111 Cu1 N11 80.57(9) . . ? N410 Cu1 O51 89.00(9) . . ? N210 Cu1 O51 98.09(9) . . ? N111 Cu1 O51 94.35(9) . . ? N11 Cu1 O51 92.90(9) . . ? N211 Cu2 N110 96.60(9) . . ? N211 Cu2 N31 171.35(9) . . ? N110 Cu2 N31 90.31(9) . . ? N211 Cu2 N21 80.72(9) . . ? N110 Cu2 N21 165.66(9) . . ? N31 Cu2 N21 91.31(9) . . ? N211 Cu2 N411 105.84(9) . 2 ? N110 Cu2 N411 96.37(9) . 2 ? N31 Cu2 N411 78.44(9) . 2 ? N21 Cu2 N411 97.92(9) . 2 ? C12 N11 C16 118.5(2) . . ? C12 N11 Cu1 127.7(2) . . ? C16 N11 Cu1 113.8(2) . . ? N11 C12 C13 122.3(3) . . ? C12 C13 C14 119.3(3) . . ? C13 C14 C15 119.1(3) . . ? C16 C15 C14 118.5(3) . . ? N11 C16 C15 122.3(3) . . ? N11 C16 C17 113.8(2) . . ? C15 C16 C17 123.9(3) . . ? N111 C17 C18 110.2(2) . . ? N111 C17 C16 117.0(2) . . ? C18 C17 C16 132.7(2) . . ? C19 C18 C17 103.6(2) . . ? N110 C19 C18 110.7(3) . . ? C19 N110 N111 107.6(2) . . ? C19 N110 Cu2 127.5(2) . . ? N111 N110 Cu2 123.1(2) . . ? C17 N111 N110 107.8(2) . . ? C17 N111 Cu1 114.4(2) . . ? N110 N111 Cu1 137.3(2) . . ? C26 N21 C22 118.3(2) . . ? C26 N21 Cu2 113.2(2) . . ? C22 N21 Cu2 128.5(2) . . ? N21 C22 C23 122.6(3) . . ? C24 C23 C22 118.9(3) . . ? C23 C24 C25 119.4(3) . . ? C24 C25 C26 118.1(3) . . ? N21 C26 C25 122.6(3) . . ? N21 C26 C27 114.3(2) . . ? C25 C26 C27 123.0(2) . . ? N211 C27 C28 110.0(2) . . ? N211 C27 C26 116.8(2) . . ? C28 C27 C26 133.2(2) . . ? C29 C28 C27 104.1(2) . . ? N210 C29 C28 110.4(2) . . ? C29 N210 N211 107.5(2) . . ? C29 N210 Cu1 126.9(2) . . ? N211 N210 Cu1 124.6(2) . . ? C27 N211 N210 108.0(2) . . ? C27 N211 Cu2 114.8(2) . . ? N210 N211 Cu2 136.5(2) . . ? C32 N31 C36 119.0(2) . . ? C32 N31 Cu2 124.0(2) . . ? C36 N31 Cu2 116.4(2) . . ? N31 C32 C33 122.5(3) . . ? C32 C33 C34 118.5(3) . . ? C35 C34 C33 119.3(3) . . ? C34 C35 C36 119.5(3) . . ? N31 C36 C35 121.2(2) . . ? N31 C36 C47 115.6(2) . 2 ? C35 C36 C47 123.2(2) . 2 ? N411 C47 C48 109.6(2) . . ? N411 C47 C36 118.3(2) . 2 ? C48 C47 C36 132.2(2) . 2 ? C49 C48 C47 104.4(2) . . ? N410 C49 C48 109.7(2) . . ? C49 N410 N411 108.5(2) . . ? C49 N410 Cu1 130.7(2) . . ? N411 N410 Cu1 120.2(2) . . ? N410 N411 C47 107.9(2) . . ? N410 N411 Cu2 141.6(2) . 2 ? C47 N411 Cu2 110.3(2) . 2 ? C52 O51 Cu1 121.3(2) . . ? O51 C52 N53 125.5(3) . . ? C52 N53 C54 120.7(4) . . ? C52 N53 C55 121.1(3) . . ? C54 N53 C55 118.2(4) . . ? F4 P1 F1 92.5(2) . . ? F4 P1 F5 91.22(14) . . ? F1 P1 F5 89.4(2) . . ? F4 P1 F6 90.1(2) . . ? F1 P1 F6 177.4(2) . . ? F5 P1 F6 91.0(2) . . ? F4 P1 F2 178.4(2) . . ? F1 P1 F2 89.12(15) . . ? F5 P1 F2 89.07(14) . . ? F6 P1 F2 88.3(2) . . ? F4 P1 F3 90.19(15) . . ? F1 P1 F3 90.9(2) . . ? F5 P1 F3 178.5(2) . . ? F6 P1 F3 88.7(2) . . ? F2 P1 F3 89.51(14) . . ? C4 N3 C1 121.5(3) . . ? C4 N3 C2 121.3(3) . . ? C1 N3 C2 116.8(3) . . ? O5 C4 N3 126.2(3) . . ? _refine_diff_density_max 0.703 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.071 #=END data_/tintin3/people/elia/two/two _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H52 Cu4 F12 N18 O4 P2' _chemical_formula_weight 1537.2 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.888(2) _cell_length_b 12.739(2) _cell_length_c 13.050(2) _cell_angle_alpha 116.745(8) _cell_angle_beta 101.313(11) _cell_angle_gamma 102.246(13) _cell_volume 1488.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.857 _exptl_crystal_density_method ? _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.56 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15396 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.66 _reflns_number_total 6727 _reflns_number_observed 4647 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens 1995b)' _computing_cell_refinement 'SAINT (Siemens 1995b)' _computing_data_reduction 'SAINT (Siemens 1995b)' _computing_structure_solution 'SHELXTL (Siemens 1995a)' _computing_structure_refinement 'SHELXTL (Siemens 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens 1995a)' _computing_publication_material 'SHELXTL (Siemens 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0492P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6727 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_obs 0.0380 _refine_ls_wR_factor_all 0.0943 _refine_ls_wR_factor_obs 0.0903 _refine_ls_goodness_of_fit_all 0.903 _refine_ls_goodness_of_fit_obs 1.058 _refine_ls_restrained_S_all 0.903 _refine_ls_restrained_S_obs 1.058 _refine_ls_shift/esd_max -0.183 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 1.52318(3) 1.78505(3) 0.12456(3) 0.01943(10) Uani 1 d . . Cu2 Cu 1.38859(3) 1.47727(3) 0.13239(3) 0.02116(10) Uani 1 d . . O1 O 1.2301(2) 1.3400(2) 0.1554(2) 0.0352(5) Uani 1 d . . H1 H 1.2008(46) 1.3765(43) 0.1981(41) 0.083(18) Uiso 1 d . . C1 C 1.1205(4) 1.2492(3) 0.0488(3) 0.0491(10) Uani 1 d . . H1A H 1.0593(12) 1.1987(15) 0.0687(5) 0.074 Uiso 1 calc R . H1B H 1.1529(4) 1.1947(14) -0.0125(8) 0.074 Uiso 1 calc R . H1C H 1.0735(14) 1.2912(3) 0.0166(12) 0.074 Uiso 1 calc R . N11 N 1.3445(2) 1.6978(2) 0.1509(2) 0.0206(5) Uani 1 d . . N12 N 1.2865(2) 1.5936(2) 0.1528(2) 0.0221(5) Uani 1 d . . C13 C 1.1641(3) 1.5903(3) 0.1577(2) 0.0250(6) Uani 1 d . . H13 H 1.1030(3) 1.5265(3) 0.1599(2) 0.030 Uiso 1 calc R . C14 C 1.1392(3) 1.6935(3) 0.1592(2) 0.0236(6) Uani 1 d . . H14 H 1.0610(3) 1.7147(3) 0.1628(2) 0.028 Uiso 1 calc R . C15 C 1.2565(3) 1.7590(2) 0.1540(2) 0.0191(6) Uani 1 d . . N21 N 1.4205(2) 1.9086(2) 0.1436(2) 0.0209(5) Uani 1 d . . C22 C 1.2961(3) 1.8744(3) 0.1507(2) 0.0204(6) Uani 1 d . . C23 C 1.2132(3) 1.9438(3) 0.1505(2) 0.0240(6) Uani 1 d . . H23 H 1.1273(3) 1.9192(3) 0.1563(2) 0.029 Uiso 1 calc R . C24 C 1.2562(3) 2.0490(3) 0.1417(3) 0.0280(6) Uani 1 d . . H24 H 1.1997(3) 2.0960(3) 0.1397(3) 0.034 Uiso 1 calc R . C25 C 1.3834(3) 2.0847(3) 0.1359(3) 0.0264(6) Uani 1 d . . H25 H 1.4155(3) 2.1571(3) 0.1309(3) 0.032 Uiso 1 calc R . C26 C 1.4625(3) 2.0127(3) 0.1376(2) 0.0244(6) Uani 1 d . . H26 H 1.5497(3) 2.0376(3) 0.1344(2) 0.029 Uiso 1 calc R . N31 N 1.6536(2) 1.6982(2) 0.1285(2) 0.0204(5) Uani 1 d . . N32 N 1.6789(2) 1.5983(2) 0.0466(2) 0.0230(5) Uani 1 d . . C33 C 1.7744(3) 1.5771(3) 0.1113(3) 0.0262(6) Uani 1 d . . H33 H 1.8100(3) 1.5124(3) 0.0767(3) 0.031 Uiso 1 calc R . C34 C 1.8128(3) 1.6627(3) 0.2341(3) 0.0267(6) Uani 1 d . . H34 H 1.8774(3) 1.6690(3) 0.2992(3) 0.032 Uiso 1 calc R . C35 C 1.7348(3) 1.7374(3) 0.2405(2) 0.0229(6) Uani 1 d . . N41 N 1.6303(2) 1.8889(2) 0.3096(2) 0.0237(5) Uani 1 d . . C42 C 1.7253(3) 1.8457(3) 0.3422(2) 0.0237(6) Uani 1 d . . C43 C 1.8071(3) 1.9013(3) 0.4624(3) 0.0341(7) Uani 1 d . . H43 H 1.8726(3) 1.8690(3) 0.4834(3) 0.041 Uiso 1 calc R . C44 C 1.7901(4) 2.0054(3) 0.5509(3) 0.0403(8) Uani 1 d . . H44 H 1.8458(4) 2.0467(3) 0.6334(3) 0.048 Uiso 1 calc R . C45 C 1.6919(3) 2.0485(3) 0.5182(3) 0.0380(8) Uani 1 d . . H45 H 1.6785(3) 2.1188(3) 0.5779(3) 0.046 Uiso 1 calc R . C46 C 1.6134(3) 1.9877(3) 0.3973(3) 0.0303(7) Uani 1 d . . H46 H 1.5451(3) 2.0168(3) 0.3752(3) 0.036 Uiso 1 calc R . N51 N 1.5189(2) 1.3908(2) 0.1381(2) 0.0198(5) Uani 1 d . . N52 N 1.5532(2) 1.2977(2) 0.0564(2) 0.0210(5) Uani 1 d . . C53 C 1.6537(3) 1.2817(3) 0.1213(2) 0.0251(6) Uani 1 d . . H53 H 1.6970(3) 1.2236(3) 0.0870(2) 0.030 Uiso 1 calc R . C54 C 1.6840(3) 1.3623(3) 0.2450(3) 0.0264(6) Uani 1 d . . H54 H 1.7490(3) 1.3700(3) 0.3107(3) 0.032 Uiso 1 calc R . C55 C 1.5976(3) 1.4289(3) 0.2507(2) 0.0217(6) Uani 1 d . . N61 N 1.4828(2) 1.5712(2) 0.3191(2) 0.0258(5) Uani 1 d . . C62 C 1.5784(3) 1.5296(3) 0.3526(2) 0.0240(6) Uani 1 d . . C63 C 1.6498(3) 1.5783(3) 0.4743(3) 0.0352(7) Uani 1 d . . H63 H 1.7180(3) 1.5490(3) 0.4962(3) 0.042 Uiso 1 calc R . C64 C 1.6191(4) 1.6712(3) 0.5635(3) 0.0422(8) Uani 1 d . . H64 H 1.6654(4) 1.7053(3) 0.6473(3) 0.051 Uiso 1 calc R . C65 C 1.5207(4) 1.7131(3) 0.5286(3) 0.0447(9) Uani 1 d . . H65 H 1.4986(4) 1.7764(3) 0.5880(3) 0.054 Uiso 1 calc R . C66 C 1.4549(3) 1.6616(3) 0.4061(3) 0.0369(8) Uani 1 d . . H66 H 1.3877(3) 1.6909(3) 0.3824(3) 0.044 Uiso 1 calc R . P1 P 2.08632(10) 1.88670(11) 0.73333(10) 0.0502(3) Uani 1 d . . F11 F 2.2183(14) 1.9890(13) 0.8354(10) 0.123(5) Uani 0.449(10) d P . F11' F 2.2328(7) 1.9806(8) 0.8166(9) 0.079(3) Uani 0.551(10) d P . F12 F 1.9267(7) 1.8151(7) 0.6726(7) 0.053(2) Uani 0.449(10) d P . F12' F 1.9702(11) 1.7677(11) 0.6230(11) 0.151(5) Uani 0.551(10) d P . F13 F 2.2003(10) 1.8351(7) 0.6636(8) 0.095(4) Uani 0.449(10) d P . F13' F 2.1067(10) 1.8535(6) 0.6141(6) 0.100(3) Uani 0.551(10) d P . F14 F 2.0464(9) 2.0061(8) 0.7345(8) 0.052(2) Uani 0.449(10) d P . F14' F 2.0781(10) 1.9739(15) 0.6868(16) 0.185(7) Uani 0.551(10) d P . F15 F 2.0546(9) 1.9353(9) 0.8625(6) 0.069(3) Uani 0.449(10) d P . F15' F 2.0059(13) 1.9234(11) 0.8093(17) 0.183(6) Uani 0.551(10) d P . F16 F 2.1105(17) 1.7785(19) 0.7329(17) 0.106(5) Uani 0.449(10) d P . F16' F 2.1093(11) 1.7856(13) 0.7774(12) 0.083(3) Uani 0.551(10) d P . O2 O 1.8946(3) 1.5552(3) 0.6752(3) 0.0705(9) Uani 1 d . . H2 H 1.9758(75) 1.6306(72) 0.7085(68) 0.203(35) Uiso 1 d . . C2 C 1.9186(5) 1.4452(5) 0.6013(4) 0.0723(13) Uani 1 d . . H2A H 1.9202(30) 1.4404(15) 0.5245(12) 0.108 Uiso 1 calc R . H2B H 1.8475(16) 1.3719(5) 0.5844(23) 0.108 Uiso 1 calc R . H2C H 2.0046(14) 1.4471(13) 0.6438(12) 0.108 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0193(2) 0.0236(2) 0.0192(2) 0.0113(2) 0.00919(14) 0.01112(15) Cu2 0.0230(2) 0.0226(2) 0.0208(2) 0.0110(2) 0.00903(15) 0.01186(15) O1 0.0335(13) 0.0358(14) 0.0364(13) 0.0191(12) 0.0133(11) 0.0091(11) C1 0.049(2) 0.041(2) 0.049(2) 0.027(2) 0.005(2) 0.000(2) N11 0.0201(12) 0.0245(13) 0.0203(12) 0.0113(10) 0.0095(10) 0.0110(10) N12 0.0251(12) 0.0228(13) 0.0220(12) 0.0122(10) 0.0105(10) 0.0103(10) C13 0.0247(15) 0.028(2) 0.028(2) 0.0170(13) 0.0129(13) 0.0114(13) C14 0.0206(14) 0.029(2) 0.0267(15) 0.0157(13) 0.0104(12) 0.0127(12) C15 0.0202(14) 0.0232(14) 0.0145(13) 0.0084(12) 0.0076(11) 0.0100(12) N21 0.0222(12) 0.0238(12) 0.0198(11) 0.0109(10) 0.0105(10) 0.0109(10) C22 0.0221(14) 0.0243(15) 0.0151(13) 0.0088(12) 0.0082(11) 0.0099(12) C23 0.0220(14) 0.027(2) 0.0247(14) 0.0129(13) 0.0100(12) 0.0111(12) C24 0.031(2) 0.029(2) 0.029(2) 0.0143(14) 0.0110(14) 0.0180(14) C25 0.031(2) 0.025(2) 0.030(2) 0.0172(13) 0.0134(14) 0.0116(13) C26 0.027(2) 0.0242(15) 0.0243(15) 0.0128(13) 0.0130(13) 0.0072(13) N31 0.0225(12) 0.0224(12) 0.0189(11) 0.0102(10) 0.0092(10) 0.0111(10) N32 0.0247(12) 0.0243(13) 0.0242(12) 0.0124(11) 0.0093(11) 0.0150(11) C33 0.030(2) 0.028(2) 0.029(2) 0.0164(14) 0.0118(13) 0.0170(13) C34 0.0240(15) 0.035(2) 0.027(2) 0.0182(14) 0.0081(13) 0.0149(13) C35 0.0218(14) 0.028(2) 0.0227(14) 0.0152(13) 0.0075(12) 0.0113(12) N41 0.0238(13) 0.0260(13) 0.0212(12) 0.0106(11) 0.0100(10) 0.0098(11) C42 0.0246(15) 0.029(2) 0.0215(14) 0.0146(13) 0.0101(12) 0.0104(13) C43 0.039(2) 0.044(2) 0.022(2) 0.0153(15) 0.0093(14) 0.023(2) C44 0.047(2) 0.048(2) 0.020(2) 0.013(2) 0.009(2) 0.019(2) C45 0.047(2) 0.039(2) 0.024(2) 0.0095(15) 0.014(2) 0.021(2) C46 0.034(2) 0.035(2) 0.025(2) 0.0131(14) 0.0140(14) 0.0196(15) N51 0.0212(12) 0.0223(12) 0.0181(11) 0.0106(10) 0.0083(10) 0.0098(10) N52 0.0218(12) 0.0237(12) 0.0225(12) 0.0122(10) 0.0104(10) 0.0132(10) C53 0.027(2) 0.029(2) 0.0257(15) 0.0150(13) 0.0113(13) 0.0170(13) C54 0.027(2) 0.033(2) 0.0226(15) 0.0153(14) 0.0076(13) 0.0158(14) C55 0.0211(14) 0.0234(15) 0.0211(14) 0.0121(12) 0.0071(12) 0.0069(12) N61 0.0307(14) 0.0234(13) 0.0222(12) 0.0094(11) 0.0084(11) 0.0132(11) C62 0.0260(15) 0.0215(15) 0.0219(14) 0.0090(12) 0.0081(12) 0.0083(12) C63 0.041(2) 0.038(2) 0.023(2) 0.0111(15) 0.0073(15) 0.019(2) C64 0.056(2) 0.040(2) 0.022(2) 0.0086(15) 0.008(2) 0.024(2) C65 0.062(2) 0.039(2) 0.024(2) 0.006(2) 0.013(2) 0.029(2) C66 0.045(2) 0.037(2) 0.026(2) 0.0100(15) 0.011(2) 0.026(2) P1 0.0369(5) 0.0669(7) 0.0601(7) 0.0466(6) 0.0135(5) 0.0118(5) F11 0.098(10) 0.146(10) 0.043(5) -0.011(5) 0.003(5) 0.048(7) F11' 0.018(3) 0.108(6) 0.150(8) 0.105(7) 0.016(4) 0.010(3) F12 0.035(3) 0.047(4) 0.065(4) 0.024(3) 0.009(3) 0.013(3) F12' 0.099(7) 0.127(8) 0.146(9) 0.082(8) -0.046(6) -0.056(6) F13 0.099(7) 0.091(5) 0.094(5) 0.033(4) 0.069(5) 0.030(4) F13' 0.168(8) 0.113(5) 0.096(5) 0.069(4) 0.108(6) 0.092(5) F14 0.052(5) 0.057(4) 0.067(4) 0.040(3) 0.029(3) 0.025(4) F14' 0.053(5) 0.247(15) 0.307(16) 0.260(14) -0.037(8) -0.037(7) F15 0.082(5) 0.081(5) 0.035(3) 0.037(3) 0.016(3) -0.003(4) F15' 0.170(11) 0.176(11) 0.392(19) 0.197(14) 0.243(13) 0.143(10) F16 0.114(7) 0.154(8) 0.207(15) 0.164(10) 0.114(9) 0.112(7) F16' 0.056(4) 0.111(5) 0.152(8) 0.115(6) 0.040(5) 0.040(4) O2 0.084(2) 0.065(2) 0.089(2) 0.044(2) 0.062(2) 0.032(2) C2 0.088(4) 0.097(4) 0.080(3) 0.061(3) 0.053(3) 0.059(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N31 1.983(2) . ? Cu1 N52 1.999(2) 2_885 ? Cu1 N21 2.072(2) . ? Cu1 N41 2.076(2) . ? Cu1 N11 2.196(2) . ? Cu2 N51 1.982(2) . ? Cu2 N32 1.982(2) 2_885 ? Cu2 N12 1.991(2) . ? Cu2 N61 2.072(2) . ? Cu2 O1 2.349(2) . ? O1 C1 1.419(4) . ? N11 C15 1.352(3) . ? N11 N12 1.357(3) . ? N12 C13 1.340(3) . ? C13 C14 1.390(4) . ? C14 C15 1.402(4) . ? C15 C22 1.464(4) . ? N21 C26 1.350(3) . ? N21 C22 1.366(3) . ? C22 C23 1.393(4) . ? C23 C24 1.385(4) . ? C24 C25 1.391(4) . ? C25 C26 1.390(4) . ? N31 C35 1.347(3) . ? N31 N32 1.370(3) . ? N32 C33 1.359(3) . ? N32 Cu2 1.982(2) 2_885 ? C33 C34 1.379(4) . ? C34 C35 1.390(4) . ? C35 C42 1.464(4) . ? N41 C46 1.346(3) . ? N41 C42 1.353(3) . ? C42 C43 1.393(4) . ? C43 C44 1.392(4) . ? C44 C45 1.380(5) . ? C45 C46 1.383(4) . ? N51 C55 1.348(3) . ? N51 N52 1.374(3) . ? N52 C53 1.358(3) . ? N52 Cu1 1.999(2) 2_885 ? C53 C54 1.387(4) . ? C54 C55 1.386(4) . ? C55 C62 1.465(4) . ? N61 C66 1.347(4) . ? N61 C62 1.350(4) . ? C62 C63 1.390(4) . ? C63 C64 1.396(4) . ? C64 C65 1.382(5) . ? C65 C66 1.380(4) . ? P1 F15' 1.438(8) . ? P1 F16 1.45(2) . ? P1 F13' 1.494(5) . ? P1 F14' 1.496(9) . ? P1 F11 1.558(13) . ? P1 F12' 1.574(8) . ? P1 F11' 1.580(7) . ? P1 F12 1.617(7) . ? P1 F15 1.650(7) . ? P1 F14 1.663(9) . ? P1 F16' 1.673(11) . ? P1 F13 1.746(8) . ? O2 C2 1.414(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Cu1 N52 97.23(9) . 2_885 ? N31 Cu1 N21 168.30(9) . . ? N52 Cu1 N21 89.67(9) 2_885 . ? N31 Cu1 N41 80.49(9) . . ? N52 Cu1 N41 170.12(9) 2_885 . ? N21 Cu1 N41 91.11(9) . . ? N31 Cu1 N11 110.40(9) . . ? N52 Cu1 N11 96.73(9) 2_885 . ? N21 Cu1 N11 77.96(8) . . ? N41 Cu1 N11 93.06(8) . . ? N51 Cu2 N32 97.34(9) . 2_885 ? N51 Cu2 N12 168.89(9) . . ? N32 Cu2 N12 90.39(9) 2_885 . ? N51 Cu2 N61 80.60(9) . . ? N32 Cu2 N61 172.00(9) 2_885 . ? N12 Cu2 N61 90.65(9) . . ? N51 Cu2 O1 92.80(9) . . ? N32 Cu2 O1 100.28(9) 2_885 . ? N12 Cu2 O1 93.66(9) . . ? N61 Cu2 O1 87.57(9) . . ? C1 O1 Cu2 116.0(2) . . ? C15 N11 N12 108.0(2) . . ? C15 N11 Cu1 111.5(2) . . ? N12 N11 Cu1 140.0(2) . . ? C13 N12 N11 108.3(2) . . ? C13 N12 Cu2 135.2(2) . . ? N11 N12 Cu2 116.2(2) . . ? N12 C13 C14 110.3(2) . . ? C13 C14 C15 103.8(2) . . ? N11 C15 C14 109.5(2) . . ? N11 C15 C22 118.2(2) . . ? C14 C15 C22 132.4(2) . . ? C26 N21 C22 118.6(2) . . ? C26 N21 Cu1 124.5(2) . . ? C22 N21 Cu1 116.6(2) . . ? N21 C22 C23 121.2(2) . . ? N21 C22 C15 115.3(2) . . ? C23 C22 C15 123.5(2) . . ? C24 C23 C22 119.8(3) . . ? C23 C24 C25 119.1(3) . . ? C26 C25 C24 118.8(3) . . ? N21 C26 C25 122.6(3) . . ? C35 N31 N32 107.7(2) . . ? C35 N31 Cu1 115.1(2) . . ? N32 N31 Cu1 136.9(2) . . ? C33 N32 N31 107.2(2) . . ? C33 N32 Cu2 127.1(2) . 2_885 ? N31 N32 Cu2 124.8(2) . 2_885 ? N32 C33 C34 110.6(3) . . ? C33 C34 C35 103.9(2) . . ? N31 C35 C34 110.5(2) . . ? N31 C35 C42 116.6(2) . . ? C34 C35 C42 132.8(3) . . ? C46 N41 C42 118.5(2) . . ? C46 N41 Cu1 128.2(2) . . ? C42 N41 Cu1 113.3(2) . . ? N41 C42 C43 122.3(3) . . ? N41 C42 C35 114.2(2) . . ? C43 C42 C35 123.5(3) . . ? C44 C43 C42 118.1(3) . . ? C45 C44 C43 119.7(3) . . ? C44 C45 C46 118.9(3) . . ? N41 C46 C45 122.4(3) . . ? C55 N51 N52 107.5(2) . . ? C55 N51 Cu2 115.1(2) . . ? N52 N51 Cu2 137.4(2) . . ? C53 N52 N51 107.5(2) . . ? C53 N52 Cu1 127.6(2) . 2_885 ? N51 N52 Cu1 124.7(2) . 2_885 ? N52 C53 C54 110.2(2) . . ? C55 C54 C53 104.1(2) . . ? N51 C55 C54 110.7(2) . . ? N51 C55 C62 116.6(2) . . ? C54 C55 C62 132.7(3) . . ? C66 N61 C62 118.9(3) . . ? C66 N61 Cu2 127.7(2) . . ? C62 N61 Cu2 113.4(2) . . ? N61 C62 C63 121.9(3) . . ? N61 C62 C55 114.2(2) . . ? C63 C62 C55 123.9(3) . . ? C62 C63 C64 118.6(3) . . ? C65 C64 C63 119.3(3) . . ? C66 C65 C64 119.1(3) . . ? N61 C66 C65 122.3(3) . . ? F15' P1 F16 106.7(6) . . ? F15' P1 F13' 148.5(10) . . ? F16 P1 F13' 93.8(7) . . ? F15' P1 F14' 96.5(8) . . ? F16 P1 F14' 155.6(9) . . ? F13' P1 F14' 61.8(9) . . ? F15' P1 F11 93.6(9) . . ? F16 P1 F11 98.0(10) . . ? F13' P1 F11 107.2(6) . . ? F14' P1 F11 88.0(7) . . ? F15' P1 F12' 95.2(6) . . ? F16 P1 F12' 73.3(9) . . ? F13' P1 F12' 67.5(7) . . ? F14' P1 F12' 97.3(6) . . ? F11 P1 F12' 169.1(9) . . ? F15' P1 F11' 104.9(9) . . ? F16 P1 F11' 95.3(9) . . ? F13' P1 F11' 96.6(5) . . ? F14' P1 F11' 86.0(4) . . ? F11 P1 F11' 11.3(7) . . ? F12' P1 F11' 159.2(8) . . ? F15' P1 F12 62.1(7) . . ? F16 P1 F12 92.6(8) . . ? F13' P1 F12 93.9(5) . . ? F14' P1 F12 91.4(4) . . ? F11 P1 F12 155.5(6) . . ? F12' P1 F12 34.5(5) . . ? F11' P1 F12 166.4(5) . . ? F15' P1 F15 25.6(8) . . ? F16 P1 F15 93.1(7) . . ? F13' P1 F15 172.7(5) . . ? F14' P1 F15 111.3(9) . . ? F11 P1 F15 73.8(6) . . ? F12' P1 F15 112.7(6) . . ? F11' P1 F15 84.8(5) . . ? F12 P1 F15 83.7(4) . . ? F15' P1 F14 69.5(5) . . ? F16 P1 F14 175.3(7) . . ? F13' P1 F14 88.6(4) . . ? F14' P1 F14 27.5(8) . . ? F11 P1 F14 85.1(7) . . ? F12' P1 F14 104.0(6) . . ? F11' P1 F14 88.4(4) . . ? F12 P1 F14 83.2(4) . . ? F15 P1 F14 84.3(4) . . ? F15' P1 F16' 90.3(6) . . ? F16 P1 F16' 18.6(10) . . ? F13' P1 F16' 112.4(6) . . ? F14' P1 F16' 173.1(8) . . ? F11 P1 F16' 90.5(7) . . ? F12' P1 F16' 83.1(6) . . ? F11' P1 F16' 91.2(5) . . ? F12 P1 F16' 92.8(5) . . ? F15 P1 F16' 74.6(6) . . ? F14 P1 F16' 158.9(5) . . ? F15' P1 F13 167.9(9) . . ? F16 P1 F13 63.8(7) . . ? F13' P1 F13 43.4(3) . . ? F14' P1 F13 94.1(10) . . ? F11 P1 F13 80.9(5) . . ? F12' P1 F13 89.2(8) . . ? F11' P1 F13 70.0(4) . . ? F12 P1 F13 123.6(4) . . ? F15 P1 F13 143.0(6) . . ? F14 P1 F13 120.4(4) . . ? F16' P1 F13 79.1(6) . . ? _refine_diff_density_max 0.725 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.095 #=END data_/tintin3/people/elia/zoa/zoa _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C82 H106 Cu4 F24 N26 O10 P4' _chemical_formula_weight 2449.97 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 19.567(2) _cell_length_b 26.313(3) _cell_length_c 20.033(3) _cell_angle_alpha 90.0 _cell_angle_beta 91.441(10) _cell_angle_gamma 90.0 _cell_volume 10310.8(25) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method ? _exptl_crystal_F_000 5008 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type ? 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63226 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.1153 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.48 _reflns_number_total 23223 _reflns_number_observed 11581 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens 1995b)' _computing_cell_refinement 'SAINT (Siemens 1995b)' _computing_data_reduction 'SAINT (Siemens 1995b)' _computing_structure_solution 'SHELXTL (Siemens 1995a)' _computing_structure_refinement 'SHELXTL (Siemens 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens 1995a)' _computing_publication_material 'SHELXTL (Siemens 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+21.6564P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23223 _refine_ls_number_parameters 1445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1739 _refine_ls_R_factor_obs 0.0792 _refine_ls_wR_factor_all 0.2000 _refine_ls_wR_factor_obs 0.1606 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.214 _refine_ls_restrained_S_all 1.040 _refine_ls_restrained_S_obs 1.214 _refine_ls_shift/esd_max -2.414 _refine_ls_shift/esd_mean 0.030 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.04538(3) 0.27798(3) 0.74865(4) 0.0323(2) Uani 1 d . . Cu2 Cu 0.18108(3) 0.28159(3) 0.55170(4) 0.0301(2) Uani 1 d . . Cu3 Cu 0.22029(3) 0.21761(3) 0.72149(4) 0.0316(2) Uani 1 d . . Cu4 Cu 0.01542(3) 0.20398(3) 0.58228(4) 0.0303(2) Uani 1 d . . N11 N 0.0281(2) 0.2998(2) 0.6540(2) 0.0300(11) Uani 1 d . . N12 N 0.0188(2) 0.2775(2) 0.5930(2) 0.0282(10) Uani 1 d . . C13 C 0.0063(3) 0.3146(2) 0.5476(3) 0.0325(14) Uani 1 d . . H13 H -0.0023(3) 0.3094(2) 0.5012(3) 0.039 Uiso 1 calc R . C14 C 0.0080(3) 0.3613(2) 0.5792(3) 0.0291(13) Uani 1 d . . H14 H 0.0010(3) 0.3937(2) 0.5593(3) 0.035 Uiso 1 calc R . C15 C 0.0218(3) 0.3511(2) 0.6455(3) 0.0298(13) Uani 1 d . . N21 N 0.0484(2) 0.3519(2) 0.7593(3) 0.0352(12) Uani 1 d . . C22 C 0.0366(3) 0.3814(2) 0.7048(3) 0.0318(14) Uani 1 d . . C23 C 0.0421(3) 0.4335(2) 0.7092(3) 0.041(2) Uani 1 d . . H23 H 0.0327(3) 0.4546(2) 0.6715(3) 0.049 Uiso 1 calc R . C24 C 0.0618(4) 0.4542(3) 0.7703(4) 0.058(2) Uani 1 d . . H24 H 0.0656(4) 0.4901(3) 0.7748(4) 0.070 Uiso 1 calc R . C25 C 0.0763(4) 0.4231(3) 0.8257(4) 0.058(2) Uani 1 d . . H25 H 0.0902(4) 0.4374(3) 0.8674(4) 0.070 Uiso 1 calc R . C26 C 0.0698(3) 0.3708(3) 0.8182(3) 0.042(2) Uani 1 d . . N31 N 0.0796(2) 0.2832(2) 0.8459(3) 0.0400(13) Uani 1 d . . C32 C 0.0860(3) 0.3311(3) 0.8683(3) 0.045(2) Uani 1 d . . C33 C 0.1076(4) 0.3409(3) 0.9331(4) 0.063(2) Uani 1 d . . H33 H 0.1135(4) 0.3747(3) 0.9487(4) 0.076 Uiso 1 calc R . C34 C 0.1208(4) 0.2992(4) 0.9753(4) 0.068(2) Uani 1 d . . H34 H 0.1342(4) 0.3048(4) 1.0207(4) 0.081 Uiso 1 calc R . C35 C 0.1145(3) 0.2514(3) 0.9520(4) 0.055(2) Uani 1 d . . H35 H 0.1244(3) 0.2230(3) 0.9799(4) 0.066 Uiso 1 calc R . C36 C 0.0934(3) 0.2448(3) 0.8869(3) 0.048(2) Uani 1 d . . H36 H 0.0884(3) 0.2112(3) 0.8704(3) 0.057 Uiso 1 calc R . N41 N 0.1934(2) 0.3093(2) 0.6448(2) 0.0299(11) Uani 1 d . . N42 N 0.2048(2) 0.2901(2) 0.7073(2) 0.0315(11) Uani 1 d . . C43 C 0.2161(3) 0.3299(2) 0.7483(3) 0.0377(15) Uani 1 d . . H43 H 0.2265(3) 0.3270(2) 0.7947(3) 0.045 Uiso 1 calc R . C44 C 0.2107(3) 0.3750(2) 0.7147(3) 0.038(2) Uani 1 d . . H44 H 0.2158(3) 0.4085(2) 0.7319(3) 0.045 Uiso 1 calc R . C45 C 0.1961(3) 0.3602(2) 0.6493(3) 0.0324(14) Uani 1 d . . N51 N 0.1727(2) 0.3544(2) 0.5346(3) 0.0329(12) Uani 1 d . . C52 C 0.1800(3) 0.3870(2) 0.5859(3) 0.0351(14) Uani 1 d . . C53 C 0.1676(3) 0.4384(2) 0.5771(4) 0.042(2) Uani 1 d . . H53 H 0.1730(3) 0.4617(2) 0.6131(4) 0.051 Uiso 1 calc R . C54 C 0.1471(4) 0.4547(3) 0.5140(4) 0.055(2) Uani 1 d . . H54 H 0.1383(4) 0.4898(3) 0.5066(4) 0.066 Uiso 1 calc R . C55 C 0.1393(4) 0.4210(3) 0.4619(4) 0.051(2) Uani 1 d . . H55 H 0.1254(4) 0.4326(3) 0.4188(4) 0.061 Uiso 1 calc R . C56 C 0.1519(3) 0.3701(2) 0.4730(3) 0.0372(15) Uani 1 d . . N61 N 0.1476(2) 0.2806(2) 0.4540(2) 0.0336(11) Uani 1 d . . C62 C 0.1413(3) 0.3270(2) 0.4259(3) 0.0380(15) Uani 1 d . . C63 C 0.1254(3) 0.3325(3) 0.3580(3) 0.049(2) Uani 1 d . . H63 H 0.1223(3) 0.3654(3) 0.3386(3) 0.059 Uiso 1 calc R . C64 C 0.1144(3) 0.2899(3) 0.3197(3) 0.051(2) Uani 1 d . . H64 H 0.1031(3) 0.2932(3) 0.2735(3) 0.061 Uiso 1 calc R . C65 C 0.1196(3) 0.2428(3) 0.3481(3) 0.042(2) Uani 1 d . . H65 H 0.1128(3) 0.2130(3) 0.3219(3) 0.050 Uiso 1 calc R . C66 C 0.1353(3) 0.2394(3) 0.4164(3) 0.040(2) Uani 1 d . . H66 H 0.1372(3) 0.2068(3) 0.4368(3) 0.047 Uiso 1 calc R . N71 N 0.1138(2) 0.1845(2) 0.5707(2) 0.0302(11) Uani 1 d . . N72 N 0.1753(2) 0.2082(2) 0.5649(2) 0.0301(11) Uani 1 d . . C73 C 0.2237(3) 0.1721(2) 0.5571(3) 0.0363(15) Uani 1 d . . H73 H 0.2710(3) 0.1786(2) 0.5517(3) 0.044 Uiso 1 calc R . C74 C 0.1940(3) 0.1242(2) 0.5581(3) 0.0341(14) Uani 1 d . . H74 H 0.2159(3) 0.0922(2) 0.5535(3) 0.041 Uiso 1 calc R . C75 C 0.1246(3) 0.1335(2) 0.5672(3) 0.0322(14) Uani 1 d . . N81 N 0.0085(2) 0.1297(2) 0.5849(2) 0.0334(11) Uani 1 d . . C82 C 0.0649(3) 0.1016(2) 0.5749(3) 0.0324(14) Uani 1 d . . C83 C 0.0613(3) 0.0491(2) 0.5767(3) 0.041(2) Uani 1 d . . H83 H 0.1008(3) 0.0290(2) 0.5699(3) 0.050 Uiso 1 calc R . C84 C -0.0010(4) 0.0265(2) 0.5888(4) 0.050(2) Uani 1 d . . H84 H -0.0045(4) -0.0095(2) 0.5889(4) 0.060 Uiso 1 calc R . C85 C -0.0579(3) 0.0555(2) 0.6007(4) 0.049(2) Uani 1 d . . H85 H -0.1003(3) 0.0399(2) 0.6101(4) 0.059 Uiso 1 calc R . C86 C -0.0522(3) 0.1085(2) 0.5986(3) 0.0375(15) Uani 1 d . . N91 N -0.0827(2) 0.1949(2) 0.6125(2) 0.0331(11) Uani 1 d . . C92 C -0.1054(3) 0.1463(2) 0.6117(3) 0.0372(15) Uani 1 d . . C93 C -0.1735(3) 0.1351(3) 0.6251(4) 0.052(2) Uani 1 d . . H93 H -0.1892(3) 0.1009(3) 0.6235(4) 0.062 Uiso 1 calc R . C94 C -0.2178(3) 0.1739(3) 0.6406(4) 0.053(2) Uani 1 d . . H94 H -0.2642(3) 0.1668(3) 0.6498(4) 0.064 Uiso 1 calc R . C95 C -0.1939(3) 0.2228(3) 0.6425(3) 0.050(2) Uani 1 d . . H95 H -0.2234(3) 0.2500(3) 0.6537(3) 0.060 Uiso 1 calc R . C96 C -0.1263(3) 0.2324(2) 0.6280(3) 0.040(2) Uani 1 d . . H96 H -0.1103(3) 0.2665(2) 0.6289(3) 0.048 Uiso 1 calc R . N101 N 0.1268(2) 0.1876(2) 0.7324(2) 0.0329(12) Uani 1 d . . N102 N 0.0625(2) 0.2054(2) 0.7393(2) 0.0337(12) Uani 1 d . . C103 C 0.0213(3) 0.1650(2) 0.7500(3) 0.039(2) Uani 1 d . . H103 H -0.0265(3) 0.1670(2) 0.7571(3) 0.047 Uiso 1 calc R . C104 C 0.0583(3) 0.1209(2) 0.7490(3) 0.042(2) Uani 1 d . . H104 H 0.0422(3) 0.0871(2) 0.7547(3) 0.050 Uiso 1 calc R . C105 C 0.1250(3) 0.1367(2) 0.7378(3) 0.0365(15) Uani 1 d . . N111 N 0.2420(2) 0.1451(2) 0.7203(2) 0.0342(12) Uani 1 d . . C112 C 0.1907(3) 0.1111(2) 0.7281(3) 0.0386(15) Uani 1 d . . C113 C 0.2043(3) 0.0594(2) 0.7234(3) 0.046(2) Uani 1 d . . H113 H 0.1691(3) 0.0351(2) 0.7290(3) 0.055 Uiso 1 calc R . C114 C 0.2701(3) 0.0441(2) 0.7104(3) 0.046(2) Uani 1 d . . H114 H 0.2802(3) 0.0088(2) 0.7080(3) 0.055 Uiso 1 calc R . C115 C 0.3218(3) 0.0793(2) 0.7007(3) 0.045(2) Uani 1 d . . H115 H 0.3669(3) 0.0687(2) 0.6909(3) 0.054 Uiso 1 calc R . C116 C 0.3054(3) 0.1305(2) 0.7057(3) 0.0349(14) Uani 1 d . . N121 N 0.3201(2) 0.2198(2) 0.6917(2) 0.0355(12) Uani 1 d . . C122 C 0.3517(3) 0.1739(2) 0.6916(3) 0.0370(15) Uani 1 d . . C123 C 0.4203(3) 0.1698(3) 0.6785(3) 0.047(2) Uani 1 d . . H123 H 0.4425(3) 0.1377(3) 0.6802(3) 0.057 Uiso 1 calc R . C124 C 0.4561(3) 0.2131(3) 0.6628(4) 0.053(2) Uani 1 d . . H124 H 0.5034(3) 0.2109(3) 0.6535(4) 0.063 Uiso 1 calc R . C125 C 0.4240(3) 0.2591(3) 0.6606(3) 0.044(2) Uani 1 d . . H125 H 0.4482(3) 0.2891(3) 0.6492(3) 0.052 Uiso 1 calc R . C126 C 0.3557(3) 0.2610(2) 0.6752(3) 0.0379(15) Uani 1 d . . H126 H 0.3330(3) 0.2929(2) 0.6735(3) 0.045 Uiso 1 calc R . O1 O -0.0629(2) 0.2646(2) 0.7783(2) 0.0432(11) Uani 1 d . . N1 N -0.1608(2) 0.2832(2) 0.8314(3) 0.0427(13) Uani 1 d . . C1 C -0.0995(3) 0.2938(3) 0.8082(3) 0.042(2) Uani 1 d . . H1 H -0.0826(3) 0.3273(3) 0.8155(3) 0.050 Uiso 1 calc R . C10 C -0.2016(4) 0.3210(3) 0.8668(5) 0.084(3) Uani 1 d . . H10A H -0.2071(26) 0.3101(12) 0.9132(9) 0.126 Uiso 1 calc R . H10B H -0.2467(12) 0.3241(17) 0.8448(18) 0.126 Uiso 1 calc R . H10C H -0.1783(16) 0.3540(6) 0.8662(27) 0.126 Uiso 1 calc R . C11 C -0.1913(3) 0.2336(2) 0.8228(4) 0.051(2) Uani 1 d . . H11A H -0.2311(14) 0.2361(4) 0.7923(17) 0.077 Uiso 1 calc R . H11B H -0.2057(21) 0.2207(7) 0.8661(5) 0.077 Uiso 1 calc R . H11C H -0.1577(8) 0.2102(5) 0.8040(21) 0.077 Uiso 1 calc R . O2 O 0.2920(2) 0.2750(2) 0.5222(2) 0.0413(10) Uani 1 d . . N2 N 0.3955(3) 0.3041(3) 0.4884(3) 0.059(2) Uani 1 d . . C2 C 0.3308(3) 0.3098(3) 0.5086(3) 0.052(2) Uani 1 d . . H2 H 0.3140(3) 0.3435(3) 0.5127(3) 0.062 Uiso 1 calc R . C20 C 0.4371(4) 0.3482(4) 0.4732(6) 0.115(4) Uani 1 d . . H20A H 0.4518(33) 0.3461(15) 0.4269(13) 0.173 Uiso 1 calc R . H20B H 0.4773(22) 0.3489(17) 0.5033(26) 0.173 Uiso 1 calc R . H20C H 0.4102(14) 0.3792(4) 0.4791(39) 0.173 Uiso 1 calc R . C21 C 0.4258(4) 0.2547(4) 0.4829(4) 0.077(3) Uani 1 d . . H21A H 0.4674(16) 0.2532(8) 0.5110(22) 0.116 Uiso 1 calc R . H21B H 0.4373(26) 0.2483(9) 0.4363(6) 0.116 Uiso 1 calc R . H21C H 0.3934(12) 0.2289(4) 0.4976(27) 0.116 Uiso 1 calc R . O3 O 0.2496(2) 0.2333(2) 0.8278(2) 0.0429(11) Uani 1 d . . N3 N 0.2854(2) 0.2118(2) 0.9325(3) 0.0436(14) Uani 1 d . . C3 C 0.2630(3) 0.2015(3) 0.8718(3) 0.0384(15) Uani 1 d . . H3 H 0.2565(3) 0.1667(3) 0.8607(3) 0.046 Uiso 1 calc R . C30 C 0.2963(4) 0.2644(3) 0.9537(4) 0.062(2) Uani 1 d . . H30A H 0.3445(6) 0.2693(6) 0.9666(24) 0.092 Uiso 1 calc R . H30B H 0.2677(19) 0.2718(6) 0.9919(16) 0.092 Uiso 1 calc R . H30C H 0.2841(24) 0.2874(3) 0.9168(9) 0.092 Uiso 1 calc R . C31 C 0.3021(4) 0.1722(3) 0.9810(4) 0.064(2) Uani 1 d . . H31A H 0.2758(19) 0.1776(11) 1.0214(10) 0.096 Uiso 1 calc R . H31B H 0.3510(6) 0.1733(12) 0.9924(19) 0.096 Uiso 1 calc R . H31C H 0.2905(23) 0.1389(3) 0.9619(10) 0.096 Uiso 1 calc R . O4 O -0.0175(2) 0.2156(2) 0.4762(2) 0.0381(10) Uani 1 d . . N4 N -0.0513(2) 0.1958(2) 0.3698(3) 0.0382(12) Uani 1 d . . C4 C -0.0301(3) 0.1842(2) 0.4319(3) 0.0359(14) Uani 1 d . . H4 H -0.0245(3) 0.1493(2) 0.4427(3) 0.043 Uiso 1 calc R . C40 C -0.0668(4) 0.1564(3) 0.3208(4) 0.066(2) Uani 1 d . . H40A H -0.0354(17) 0.1594(12) 0.2836(12) 0.099 Uiso 1 calc R . H40B H -0.1140(9) 0.1604(12) 0.3041(18) 0.099 Uiso 1 calc R . H40C H -0.0613(25) 0.1229(3) 0.3417(7) 0.099 Uiso 1 calc R . C41 C -0.0619(3) 0.2478(3) 0.3483(3) 0.049(2) Uani 1 d . . H41A H -0.1093(7) 0.2520(5) 0.3321(20) 0.074 Uiso 1 calc R . H41B H -0.0307(16) 0.2557(6) 0.3123(15) 0.074 Uiso 1 calc R . H41C H -0.0531(21) 0.2708(3) 0.3860(6) 0.074 Uiso 1 calc R . P1 P 0.06194(10) 0.57991(7) 0.62566(10) 0.0486(5) Uani 1 d . . F11 F 0.0135(2) 0.5348(2) 0.6014(3) 0.089(2) Uani 1 d . . F12 F 0.0143(2) 0.6202(2) 0.5889(2) 0.0854(15) Uani 1 d . . F13 F 0.1114(2) 0.62438(15) 0.6493(2) 0.0742(13) Uani 1 d . . F14 F 0.1111(2) 0.5389(2) 0.6610(3) 0.085(2) Uani 1 d . . F15 F 0.0217(3) 0.5854(2) 0.6915(3) 0.113(2) Uani 1 d . . F16 F 0.1044(3) 0.5737(2) 0.5592(3) 0.095(2) Uani 1 d . . P2 P 0.12654(8) 0.19679(7) 0.14948(9) 0.0404(4) Uani 1 d . . F21 F 0.0710(2) 0.1939(2) 0.2064(2) 0.0573(11) Uani 1 d . . F22 F 0.0660(2) 0.1971(2) 0.0937(2) 0.0587(11) Uani 1 d . . F23 F 0.1820(2) 0.2004(2) 0.0924(2) 0.0608(11) Uani 1 d . . F24 F 0.1864(2) 0.19712(15) 0.2051(2) 0.0540(10) Uani 1 d . . F25 F 0.1240(2) 0.25734(14) 0.1526(2) 0.0614(11) Uani 1 d . . F26 F 0.1301(2) 0.1363(2) 0.1466(2) 0.0702(12) Uani 1 d . . P3 P 0.1799(3) 0.92670(11) 0.1850(2) 0.1109(12) Uani 1 d . . F31 F 0.2339(5) 0.8790(6) 0.2158(5) 0.113(4) Uani 0.71(3) d P . F31' F 0.2325(9) 0.9180(17) 0.2144(20) 0.137(15) Uani 0.29(3) d P . F32 F 0.2586(16) 0.9547(8) 0.1727(8) 0.211(11) Uani 0.71(3) d P . F32' F 0.2081(23) 0.9808(15) 0.1746(24) 0.143(18) Uani 0.29(3) d P . F33 F 0.1476(15) 0.9728(7) 0.1589(9) 0.191(12) Uani 0.71(3) d P . F33' F 0.1009(24) 0.9475(18) 0.1446(21) 0.158(19) Uani 0.29(3) d P . F34 F 0.1871(18) 0.9471(5) 0.2588(6) 0.191(11) Uani 0.71(3) d P . F34' F 0.1335(21) 0.9527(16) 0.2441(18) 0.139(15) Uani 0.29(3) d P . F35 F 0.1267(3) 0.8868(2) 0.1962(4) 0.142(3) Uani 1 d . . F36 F 0.1970(4) 0.9041(3) 0.1146(3) 0.142(3) Uani 1 d . . P4 P 0.21438(10) 0.93341(7) 0.56786(11) 0.0526(5) Uani 1 d . . F41 F 0.2198(10) 0.9934(4) 0.5537(13) 0.088(7) Uani 0.49(3) d P . F41' F 0.1907(10) 0.9726(8) 0.5149(9) 0.095(8) Uani 0.51(3) d P . F42 F 0.1407(8) 0.9328(10) 0.5392(11) 0.146(10) Uani 0.49(3) d P . F42' F 0.1534(9) 0.8977(10) 0.5424(7) 0.103(8) Uani 0.51(3) d P . F43 F 0.2044(14) 0.8785(6) 0.5888(19) 0.148(13) Uani 0.49(3) d P . F43' F 0.2409(14) 0.8897(9) 0.6141(8) 0.117(10) Uani 0.51(3) d P . F44 F 0.2811(10) 0.9371(9) 0.6066(14) 0.125(10) Uani 0.49(3) d P . F44' F 0.2800(11) 0.9653(10) 0.5899(12) 0.121(10) Uani 0.51(3) d P . F45 F 0.1731(3) 0.9539(2) 0.6295(3) 0.098(2) Uani 1 d . . F46 F 0.2574(3) 0.9139(2) 0.5070(3) 0.110(2) Uani 1 d . . C131 C -0.1366(8) 0.4455(6) 0.7203(10) 0.149(7) Uani 1 d . . H131 H -0.1284(8) 0.4808(6) 0.7142(10) 0.178 Uiso 1 calc R . O131 O -0.1246(4) 0.4289(4) 0.7785(5) 0.141(4) Uani 1 d . . N131 N -0.1579(5) 0.4219(3) 0.6695(5) 0.094(3) Uani 1 d . . C132 C -0.1703(6) 0.3709(4) 0.6705(6) 0.122(4) Uani 1 d . . H13A H -0.1388(29) 0.3535(5) 0.6409(33) 0.183 Uiso 1 calc R . H13B H -0.2175(14) 0.3644(5) 0.6553(41) 0.183 Uiso 1 calc R . H13C H -0.1636(42) 0.3580(7) 0.7162(10) 0.183 Uiso 1 calc R . C133 C -0.1672(16) 0.4463(7) 0.6096(9) 0.419(24) Uani 1 d . . H13D H -0.1897(197) 0.4232(51) 0.5774(60) 0.629 Uiso 1 calc R . H13E H -0.1228(20) 0.4567(141) 0.5927(102) 0.629 Uiso 1 calc R . H13F H -0.1959(172) 0.4764(87) 0.6157(41) 0.629 Uiso 1 calc R . N141 N 0.1573(5) 0.0526(3) 0.9614(4) 0.098(3) Uani 1 d . . O141 O 0.1347(5) 0.1318(3) 0.9252(5) 0.150(4) Uani 1 d . . C141 C 0.1323(6) 0.0999(6) 0.9693(6) 0.117(4) Uani 1 d . . H141 H 0.1121(6) 0.1087(6) 1.0104(6) 0.140 Uiso 1 calc R . C142 C 0.1558(9) 0.0128(6) 1.0103(8) 0.233(9) Uani 1 d . . H14A H 0.1701(84) -0.0192(14) 0.9899(24) 0.350 Uiso 1 calc R . H14B H 0.1093(21) 0.0092(44) 1.0266(63) 0.350 Uiso 1 calc R . H14C H 0.1871(66) 0.0212(31) 1.0476(40) 0.350 Uiso 1 calc R . C143 C 0.1899(8) 0.0427(5) 0.9002(7) 0.164(6) Uani 1 d . . H14D H 0.1647(33) 0.0161(30) 0.8757(26) 0.246 Uiso 1 calc R . H14E H 0.2369(19) 0.0313(40) 0.9094(7) 0.246 Uiso 1 calc R . H14F H 0.1905(51) 0.0738(12) 0.8733(24) 0.246 Uiso 1 calc R . N151 N 0.0834(3) 0.4221(3) 0.1522(5) 0.091(3) Uani 1 d . . O151 O -0.0258(3) 0.4512(2) 0.1335(3) 0.080(2) Uani 1 d . . C151 C 0.0311(6) 0.4520(4) 0.1640(7) 0.113(4) Uani 1 d . . H151 H 0.0369(6) 0.4764(4) 0.1987(7) 0.136 Uiso 1 calc R . C152 C 0.0796(6) 0.3870(4) 0.0978(5) 0.108(4) Uani 1 d . . H15A H 0.0858(37) 0.3523(4) 0.1148(7) 0.162 Uiso 1 calc R . H15B H 0.1157(24) 0.3948(18) 0.0663(19) 0.162 Uiso 1 calc R . H15C H 0.0349(15) 0.3899(20) 0.0751(22) 0.162 Uiso 1 calc R . C153 C 0.1434(7) 0.4214(5) 0.1926(7) 0.155(6) Uani 1 d . . H15D H 0.1826(10) 0.4307(39) 0.1657(15) 0.232 Uiso 1 calc R . H15E H 0.1503(30) 0.3872(12) 0.2110(43) 0.232 Uiso 1 calc R . H15F H 0.1389(23) 0.4458(30) 0.2293(32) 0.232 Uiso 1 calc R . N161 N 0.0529(5) 0.9403(4) 0.8168(6) 0.112(3) Uani 1 d . . C161 C 0.1140(7) 0.9192(7) 0.8193(9) 0.163(7) Uani 1 d . . H161 H 0.1466(7) 0.9233(7) 0.7854(9) 0.196 Uiso 1 calc R . O161 O 0.1255(6) 0.8916(5) 0.8742(5) 0.185(5) Uani 1 d . . C162 C 0.0069(9) 0.9498(10) 0.8646(9) 0.319(16) Uani 1 d . . H16A H -0.0392(15) 0.9503(105) 0.8444(25) 0.478 Uiso 1 calc R . H16B H 0.0169(85) 0.9828(47) 0.8853(94) 0.478 Uiso 1 calc R . H16C H 0.0097(98) 0.9231(56) 0.8986(72) 0.478 Uiso 1 calc R . C163 C 0.0328(8) 0.9665(5) 0.7539(9) 0.197(8) Uani 1 d . . H16D H 0.0080(63) 0.9978(28) 0.7643(10) 0.296 Uiso 1 calc R . H16E H 0.0032(60) 0.9442(21) 0.7267(33) 0.296 Uiso 1 calc R . H16F H 0.0738(10) 0.9750(48) 0.7291(34) 0.296 Uiso 1 calc R . N171 N 0.1731(3) 0.0645(2) 0.3537(4) 0.061(2) Uani 1 d . . O171 O 0.0766(3) 0.1011(3) 0.3922(4) 0.106(2) Uani 1 d . . C171 C 0.1288(6) 0.0761(4) 0.3999(5) 0.083(3) Uani 1 d . . H171 H 0.1386(6) 0.0638(4) 0.4437(5) 0.100 Uiso 1 calc R . C172 C 0.2315(5) 0.0330(4) 0.3693(5) 0.096(3) Uani 1 d . . H17A H 0.2735(5) 0.0522(9) 0.3617(34) 0.144 Uiso 1 calc R . H17B H 0.2303(19) 0.0028(14) 0.3405(24) 0.144 Uiso 1 calc R . H17C H 0.2303(19) 0.0225(21) 0.4161(10) 0.144 Uiso 1 calc R . C173 C 0.1654(5) 0.0805(4) 0.2854(5) 0.095(3) Uani 1 d . . H17D H 0.1619(33) 0.0505(4) 0.2564(5) 0.143 Uiso 1 calc R . H17E H 0.2052(16) 0.1007(21) 0.2731(11) 0.143 Uiso 1 calc R . H17F H 0.1239(18) 0.1011(20) 0.2800(8) 0.143 Uiso 1 calc R . N181 N 0.0970(4) 0.5621(3) 0.0200(4) 0.090(2) Uani 1 d . . C181 C 0.0572(5) 0.5768(4) 0.0719(5) 0.087(3) Uani 1 d . . H181 H 0.0365(5) 0.5538(4) 0.1018(5) 0.104 Uiso 1 calc R . O181 O 0.0511(9) 0.6246(7) 0.0753(12) 0.378(12) Uani 1 d . . C182 C 0.1050(7) 0.5064(5) 0.0092(8) 0.170(6) Uani 1 d . . H18A H 0.1281(56) 0.5005(5) -0.0329(30) 0.254 Uiso 1 calc R . H18B H 0.0599(8) 0.4903(8) 0.0074(63) 0.254 Uiso 1 calc R . H18C H 0.1324(54) 0.4918(9) 0.0461(32) 0.254 Uiso 1 calc R . C183 C 0.1261(5) 0.6046(8) -0.0249(5) 0.252(12) Uani 1 d . . H18D H 0.0883(7) 0.6222(50) -0.0482(76) 0.378 Uiso 1 calc R . H18E H 0.1564(79) 0.5895(12) -0.0576(64) 0.378 Uiso 1 calc R . H18F H 0.1518(86) 0.6290(42) 0.0029(12) 0.378 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0266(4) 0.0420(4) 0.0283(4) 0.0066(4) 0.0016(3) -0.0023(3) Cu2 0.0282(4) 0.0353(4) 0.0267(4) -0.0012(3) 0.0030(3) 0.0020(3) Cu3 0.0265(4) 0.0405(4) 0.0278(4) 0.0012(4) 0.0009(3) -0.0004(3) Cu4 0.0280(4) 0.0332(4) 0.0297(4) 0.0033(3) 0.0024(3) 0.0018(3) N11 0.025(2) 0.032(3) 0.034(3) 0.006(2) 0.003(2) 0.000(2) N12 0.030(2) 0.032(2) 0.023(3) 0.001(2) 0.004(2) 0.002(2) C13 0.037(3) 0.038(3) 0.022(3) 0.000(3) 0.003(3) 0.006(3) C14 0.032(3) 0.033(3) 0.023(3) 0.011(3) 0.007(2) 0.004(2) C15 0.025(3) 0.036(3) 0.029(3) 0.003(3) 0.010(2) 0.003(2) N21 0.030(3) 0.045(3) 0.031(3) 0.002(3) 0.003(2) -0.004(2) C22 0.024(3) 0.036(3) 0.036(4) 0.004(3) 0.007(3) -0.005(2) C23 0.041(4) 0.043(4) 0.039(4) 0.001(3) 0.008(3) -0.005(3) C24 0.057(5) 0.045(4) 0.072(6) -0.007(4) 0.012(4) -0.019(3) C25 0.057(5) 0.067(5) 0.050(5) -0.010(4) -0.003(4) -0.021(4) C26 0.036(3) 0.052(4) 0.037(4) 0.002(3) -0.001(3) -0.022(3) N31 0.030(3) 0.057(3) 0.033(3) 0.006(3) 0.001(2) -0.007(2) C32 0.029(3) 0.075(5) 0.030(4) 0.000(4) 0.001(3) -0.018(3) C33 0.062(5) 0.077(6) 0.050(5) -0.007(5) -0.007(4) -0.023(4) C34 0.057(5) 0.114(7) 0.032(4) 0.012(5) -0.014(4) -0.012(5) C35 0.043(4) 0.080(6) 0.042(5) 0.015(4) -0.007(3) -0.005(4) C36 0.030(3) 0.075(5) 0.039(4) 0.020(4) 0.004(3) -0.001(3) N41 0.026(2) 0.038(3) 0.026(3) 0.002(2) 0.005(2) -0.002(2) N42 0.030(3) 0.038(3) 0.027(3) -0.001(2) 0.008(2) -0.004(2) C43 0.030(3) 0.045(4) 0.038(4) -0.007(3) 0.001(3) -0.005(3) C44 0.033(3) 0.041(4) 0.039(4) -0.011(3) 0.011(3) -0.006(3) C45 0.024(3) 0.038(3) 0.035(4) 0.001(3) 0.009(3) -0.004(2) N51 0.029(3) 0.033(3) 0.037(3) 0.001(2) 0.010(2) 0.002(2) C52 0.029(3) 0.037(3) 0.040(4) 0.003(3) 0.010(3) -0.005(3) C53 0.053(4) 0.031(3) 0.044(4) -0.001(3) 0.016(3) -0.002(3) C54 0.069(5) 0.033(4) 0.063(6) 0.007(4) 0.015(4) 0.005(3) C55 0.070(5) 0.047(4) 0.037(4) 0.014(4) 0.011(4) 0.008(4) C56 0.040(3) 0.042(4) 0.030(4) 0.006(3) 0.009(3) 0.003(3) N61 0.024(2) 0.046(3) 0.030(3) -0.001(3) 0.005(2) 0.002(2) C62 0.034(3) 0.051(4) 0.029(4) 0.004(3) 0.008(3) 0.007(3) C63 0.060(4) 0.060(5) 0.029(4) 0.005(4) 0.005(3) 0.012(4) C64 0.056(4) 0.071(5) 0.027(4) -0.007(4) -0.001(3) 0.012(4) C65 0.039(4) 0.059(4) 0.027(4) -0.007(3) 0.007(3) 0.007(3) C66 0.034(3) 0.051(4) 0.033(4) -0.007(3) 0.001(3) 0.003(3) N71 0.027(3) 0.037(3) 0.026(3) -0.001(2) 0.000(2) 0.003(2) N72 0.030(2) 0.036(3) 0.025(3) 0.006(2) 0.001(2) 0.004(2) C73 0.030(3) 0.043(4) 0.037(4) -0.003(3) -0.001(3) 0.004(3) C74 0.033(3) 0.039(3) 0.030(4) -0.006(3) -0.001(3) 0.007(3) C75 0.038(3) 0.035(3) 0.024(3) 0.001(3) -0.002(3) 0.004(3) N81 0.041(3) 0.032(3) 0.026(3) 0.006(2) 0.001(2) -0.002(2) C82 0.044(4) 0.033(3) 0.020(3) 0.002(3) -0.003(3) 0.000(3) C83 0.052(4) 0.034(3) 0.038(4) -0.001(3) -0.004(3) 0.006(3) C84 0.063(5) 0.031(3) 0.055(5) 0.005(3) -0.003(4) -0.001(3) C85 0.049(4) 0.046(4) 0.053(5) 0.007(4) -0.001(3) -0.011(3) C86 0.037(3) 0.043(4) 0.032(4) 0.007(3) -0.002(3) -0.001(3) N91 0.027(3) 0.042(3) 0.030(3) 0.004(2) -0.001(2) 0.000(2) C92 0.037(3) 0.047(4) 0.028(4) 0.008(3) -0.005(3) -0.003(3) C93 0.043(4) 0.054(4) 0.058(5) 0.005(4) 0.003(4) -0.011(3) C94 0.040(4) 0.069(5) 0.052(5) 0.008(4) 0.012(3) -0.008(4) C95 0.032(3) 0.071(5) 0.047(4) 0.006(4) 0.008(3) 0.011(3) C96 0.035(3) 0.049(4) 0.037(4) 0.006(3) 0.001(3) 0.003(3) N101 0.028(3) 0.038(3) 0.033(3) 0.003(2) 0.001(2) 0.004(2) N102 0.026(2) 0.041(3) 0.034(3) 0.010(2) 0.001(2) -0.001(2) C103 0.030(3) 0.048(4) 0.041(4) 0.008(3) 0.003(3) -0.004(3) C104 0.037(4) 0.041(4) 0.048(4) 0.014(3) -0.003(3) -0.009(3) C105 0.039(3) 0.043(4) 0.027(4) 0.003(3) -0.004(3) 0.000(3) N111 0.034(3) 0.041(3) 0.028(3) -0.001(2) 0.001(2) 0.002(2) C112 0.039(4) 0.047(4) 0.030(4) 0.005(3) -0.003(3) 0.003(3) C113 0.055(4) 0.036(4) 0.046(4) 0.005(3) -0.004(3) -0.001(3) C114 0.055(4) 0.042(4) 0.040(4) 0.000(3) 0.000(3) 0.013(3) C115 0.040(4) 0.050(4) 0.045(4) -0.003(3) -0.004(3) 0.014(3) C116 0.034(3) 0.049(4) 0.021(3) -0.004(3) -0.002(3) 0.007(3) N121 0.030(3) 0.051(3) 0.025(3) -0.007(3) -0.002(2) 0.001(2) C122 0.033(3) 0.048(4) 0.029(4) -0.009(3) -0.003(3) 0.001(3) C123 0.040(4) 0.058(4) 0.044(4) -0.015(4) 0.003(3) 0.016(3) C124 0.030(3) 0.073(5) 0.055(5) -0.012(4) 0.010(3) -0.008(3) C125 0.034(4) 0.058(4) 0.038(4) -0.008(3) 0.002(3) -0.006(3) C126 0.034(3) 0.052(4) 0.028(4) 0.000(3) 0.003(3) -0.002(3) O1 0.030(2) 0.057(3) 0.042(3) 0.003(2) 0.010(2) -0.003(2) N1 0.034(3) 0.052(3) 0.042(3) -0.001(3) 0.008(2) -0.002(2) C1 0.033(3) 0.050(4) 0.042(4) 0.011(3) 0.000(3) -0.010(3) C10 0.053(5) 0.073(6) 0.128(9) -0.028(6) 0.038(5) -0.005(4) C11 0.042(4) 0.054(4) 0.059(5) 0.004(4) 0.017(3) -0.012(3) O2 0.031(2) 0.053(3) 0.040(3) -0.007(2) 0.008(2) -0.002(2) N2 0.031(3) 0.094(5) 0.052(4) 0.021(4) 0.008(3) -0.005(3) C2 0.035(4) 0.079(5) 0.042(4) 0.010(4) 0.001(3) 0.004(4) C20 0.055(6) 0.144(9) 0.147(11) 0.080(8) 0.013(6) -0.021(6) C21 0.042(5) 0.125(8) 0.064(6) -0.036(6) 0.008(4) 0.002(5) O3 0.042(2) 0.056(3) 0.030(3) 0.001(2) -0.006(2) -0.002(2) N3 0.037(3) 0.061(4) 0.033(3) 0.001(3) 0.000(2) 0.005(3) C3 0.031(3) 0.057(4) 0.028(4) -0.010(3) 0.003(3) -0.003(3) C30 0.056(5) 0.083(6) 0.046(5) -0.019(4) -0.003(4) -0.009(4) C31 0.060(5) 0.096(6) 0.036(4) 0.009(4) 0.004(4) 0.024(4) O4 0.042(2) 0.046(2) 0.025(2) 0.001(2) -0.004(2) 0.004(2) N4 0.040(3) 0.047(3) 0.027(3) 0.000(3) -0.003(2) 0.000(2) C4 0.035(3) 0.040(3) 0.033(4) 0.003(3) -0.004(3) 0.002(3) C40 0.096(6) 0.069(5) 0.033(4) -0.007(4) -0.014(4) -0.015(4) C41 0.046(4) 0.063(5) 0.038(4) 0.008(4) -0.002(3) 0.010(3) P1 0.0607(12) 0.0434(10) 0.0416(12) 0.0068(9) -0.0022(9) 0.0017(9) F11 0.100(4) 0.072(3) 0.091(4) 0.020(3) -0.044(3) -0.027(3) F12 0.102(4) 0.077(3) 0.076(4) 0.022(3) -0.024(3) 0.021(3) F13 0.099(3) 0.052(2) 0.071(3) 0.001(2) -0.012(3) -0.014(2) F14 0.090(3) 0.057(3) 0.106(4) 0.012(3) -0.037(3) 0.004(2) F15 0.140(5) 0.130(5) 0.070(4) 0.018(4) 0.050(4) 0.002(4) F16 0.132(4) 0.077(3) 0.078(4) -0.019(3) 0.041(3) -0.007(3) P2 0.0360(9) 0.0572(11) 0.0281(9) -0.0023(9) 0.0014(7) 0.0046(8) F21 0.041(2) 0.098(3) 0.034(2) 0.003(2) 0.008(2) -0.006(2) F22 0.040(2) 0.101(3) 0.035(2) 0.007(2) -0.007(2) 0.002(2) F23 0.043(2) 0.103(3) 0.037(2) -0.003(2) 0.008(2) 0.008(2) F24 0.040(2) 0.080(3) 0.041(2) 0.002(2) -0.006(2) 0.003(2) F25 0.061(3) 0.054(2) 0.069(3) 0.003(2) 0.002(2) 0.009(2) F26 0.084(3) 0.060(3) 0.066(3) -0.009(2) -0.004(2) 0.001(2) P3 0.200(4) 0.071(2) 0.062(2) 0.005(2) 0.011(2) -0.038(2) F31 0.144(9) 0.090(9) 0.106(8) 0.009(6) -0.005(6) -0.032(6) F31' 0.021(10) 0.130(34) 0.259(38) -0.037(29) -0.025(14) -0.019(12) F32 0.318(27) 0.175(16) 0.143(12) 0.000(12) 0.048(15) -0.165(18) F32' 0.161(37) 0.105(24) 0.166(34) -0.017(22) 0.089(33) -0.040(26) F33 0.299(32) 0.156(19) 0.119(15) 0.077(14) 0.042(20) 0.092(21) F33' 0.183(37) 0.174(38) 0.114(23) -0.016(24) -0.041(24) 0.117(29) F34 0.440(34) 0.079(7) 0.053(7) 0.008(6) -0.009(14) -0.045(14) F34' 0.193(33) 0.164(29) 0.061(21) -0.051(19) 0.033(19) -0.001(23) F35 0.137(6) 0.119(5) 0.173(7) 0.009(5) 0.048(5) -0.022(4) F36 0.164(6) 0.182(7) 0.080(5) -0.032(5) 0.029(4) -0.031(5) P4 0.0525(11) 0.0468(11) 0.0580(14) 0.0042(10) -0.0086(10) 0.0045(9) F41 0.101(12) 0.032(6) 0.132(17) 0.014(7) 0.031(11) 0.007(6) F41' 0.113(12) 0.093(13) 0.081(10) 0.058(9) 0.024(8) 0.047(11) F42 0.090(10) 0.117(15) 0.227(22) -0.048(15) -0.097(12) 0.002(11) F42' 0.109(12) 0.125(17) 0.075(9) -0.021(10) 0.012(8) -0.053(12) F43 0.166(25) 0.030(7) 0.251(36) 0.016(13) 0.061(21) 0.002(11) F43' 0.171(21) 0.120(20) 0.061(9) 0.046(11) -0.003(10) 0.069(15) F44 0.064(11) 0.112(17) 0.196(21) -0.049(15) -0.066(12) 0.035(12) F44' 0.090(14) 0.144(19) 0.131(15) -0.070(15) 0.043(12) -0.064(14) F45 0.102(4) 0.086(4) 0.107(5) -0.006(3) 0.042(3) 0.010(3) F46 0.127(5) 0.127(5) 0.078(4) -0.026(4) 0.018(3) 0.015(4) C131 0.149(14) 0.126(12) 0.176(17) -0.065(14) 0.086(14) -0.017(10) O131 0.075(5) 0.211(11) 0.136(8) -0.068(8) 0.001(6) 0.004(5) N131 0.142(8) 0.058(5) 0.083(7) 0.006(5) 0.038(6) 0.020(5) C132 0.129(10) 0.105(9) 0.133(11) -0.002(8) 0.007(8) -0.037(7) C133 0.865(63) 0.245(22) 0.156(18) 0.132(17) 0.182(28) 0.354(33) N141 0.139(8) 0.084(6) 0.071(6) 0.010(5) 0.015(5) 0.026(5) O141 0.193(9) 0.122(7) 0.132(8) 0.057(6) -0.038(7) -0.006(6) C141 0.107(9) 0.159(13) 0.085(9) -0.006(9) 0.010(7) 0.018(9) C142 0.315(24) 0.205(17) 0.180(17) 0.141(15) 0.023(16) 0.004(16) C143 0.226(16) 0.158(13) 0.110(11) -0.029(10) 0.044(11) 0.027(11) N151 0.046(4) 0.087(5) 0.140(8) -0.078(5) 0.006(4) 0.004(4) O151 0.055(4) 0.095(4) 0.090(5) 0.009(4) 0.009(3) 0.001(3) C151 0.099(8) 0.061(6) 0.182(14) -0.007(7) 0.038(9) -0.007(6) C152 0.143(10) 0.101(8) 0.083(8) -0.015(7) 0.047(7) -0.007(7) C153 0.142(12) 0.155(12) 0.166(14) -0.050(11) -0.018(11) 0.041(9) N161 0.066(6) 0.114(7) 0.156(10) 0.014(7) 0.002(6) 0.000(5) C161 0.100(11) 0.216(18) 0.173(17) -0.104(15) -0.018(11) 0.001(11) O161 0.187(10) 0.249(13) 0.116(8) -0.008(9) -0.014(8) 0.087(9) C162 0.169(17) 0.642(50) 0.151(17) 0.018(23) 0.103(15) -0.019(22) C163 0.233(19) 0.099(10) 0.255(22) 0.024(12) -0.082(17) -0.004(10) N171 0.068(4) 0.052(4) 0.064(5) -0.004(4) 0.005(4) -0.004(3) O171 0.086(5) 0.122(6) 0.110(6) -0.013(5) 0.004(4) 0.043(4) C171 0.105(8) 0.080(7) 0.064(7) -0.012(5) 0.002(6) -0.007(6) C172 0.082(7) 0.099(7) 0.107(9) 0.031(7) 0.003(6) -0.004(6) C173 0.137(9) 0.093(7) 0.056(6) 0.007(6) -0.014(6) -0.007(6) N181 0.070(5) 0.100(6) 0.100(7) -0.019(5) -0.004(5) 0.004(4) C181 0.102(8) 0.090(7) 0.070(7) -0.012(6) 0.046(6) -0.004(6) O181 0.267(19) 0.299(21) 0.571(37) -0.097(23) 0.078(20) -0.010(16) C182 0.169(13) 0.117(10) 0.223(18) -0.045(11) 0.001(12) 0.056(9) C183 0.077(8) 0.642(36) 0.037(6) 0.035(12) 0.005(5) -0.169(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N102 1.948(5) . ? Cu1 N21 1.956(5) . ? Cu1 N11 2.002(5) . ? Cu1 N31 2.049(5) . ? Cu1 O1 2.243(4) . ? Cu2 N72 1.952(4) . ? Cu2 N51 1.953(5) . ? Cu2 N41 2.012(5) . ? Cu2 N61 2.049(5) . ? Cu2 O2 2.270(4) . ? Cu3 N42 1.952(5) . ? Cu3 N111 1.955(5) . ? Cu3 N101 2.009(5) . ? Cu3 N121 2.056(5) . ? Cu3 O3 2.230(4) . ? Cu4 N12 1.949(5) . ? Cu4 N81 1.961(5) . ? Cu4 N71 2.011(4) . ? Cu4 N91 2.041(4) . ? Cu4 O4 2.226(4) . ? N11 N12 1.365(6) . ? N11 C15 1.365(7) . ? N12 C13 1.353(7) . ? C13 C14 1.381(8) . ? C14 C15 1.375(8) . ? C15 C22 1.453(8) . ? N21 C26 1.338(8) . ? N21 C22 1.354(7) . ? C22 C23 1.379(8) . ? C23 C24 1.387(9) . ? C24 C25 1.401(10) . ? C25 C26 1.390(9) . ? C26 C32 1.479(9) . ? N31 C36 1.325(8) . ? N31 C32 1.341(8) . ? C32 C33 1.380(9) . ? C33 C34 1.405(10) . ? C34 C35 1.346(11) . ? C35 C36 1.368(9) . ? N41 C45 1.345(7) . ? N41 N42 1.361(6) . ? N42 C43 1.345(7) . ? C43 C44 1.368(8) . ? C44 C45 1.389(8) . ? C45 C52 1.480(8) . ? N51 C52 1.345(7) . ? N51 C56 1.353(8) . ? C52 C53 1.385(8) . ? C53 C54 1.384(9) . ? C54 C55 1.375(9) . ? C55 C56 1.380(8) . ? C56 C62 1.486(9) . ? N61 C66 1.338(7) . ? N61 C62 1.350(7) . ? C62 C63 1.395(9) . ? C63 C64 1.373(9) . ? C64 C65 1.367(9) . ? C65 C66 1.399(9) . ? N71 C75 1.361(7) . ? N71 N72 1.363(6) . ? N72 C73 1.354(7) . ? C73 C74 1.389(8) . ? C74 C75 1.397(8) . ? C75 C82 1.450(8) . ? N81 C82 1.346(7) . ? N81 C86 1.348(7) . ? C82 C83 1.383(8) . ? C83 C84 1.382(9) . ? C84 C85 1.376(9) . ? C85 C86 1.398(8) . ? C86 C92 1.469(8) . ? N91 C96 1.347(7) . ? N91 C92 1.355(7) . ? C92 C93 1.397(8) . ? C93 C94 1.379(9) . ? C94 C95 1.371(9) . ? C95 C96 1.383(8) . ? N101 C105 1.344(7) . ? N101 N102 1.353(6) . ? N102 C103 1.356(7) . ? C103 C104 1.368(8) . ? C104 C105 1.395(8) . ? C105 C112 1.469(8) . ? N111 C116 1.339(7) . ? N111 C112 1.356(7) . ? C112 C113 1.391(8) . ? C113 C114 1.380(9) . ? C114 C115 1.388(9) . ? C115 C116 1.390(8) . ? C116 C122 1.490(8) . ? N121 C126 1.335(7) . ? N121 C122 1.357(7) . ? C122 C123 1.378(8) . ? C123 C124 1.378(9) . ? C124 C125 1.363(9) . ? C125 C126 1.377(8) . ? O1 C1 1.219(7) . ? N1 C1 1.328(7) . ? N1 C11 1.444(8) . ? N1 C10 1.470(8) . ? O2 C2 1.225(8) . ? N2 C2 1.346(8) . ? N2 C21 1.434(10) . ? N2 C20 1.454(10) . ? O3 C3 1.240(7) . ? N3 C3 1.309(8) . ? N3 C31 1.458(8) . ? N3 C30 1.461(8) . ? O4 C4 1.234(7) . ? N4 C4 1.336(7) . ? N4 C41 1.448(8) . ? N4 C40 1.453(8) . ? P1 F15 1.560(5) . ? P1 F12 1.581(4) . ? P1 F13 1.584(4) . ? P1 F11 1.588(5) . ? P1 F16 1.596(5) . ? P1 F14 1.598(4) . ? P2 F26 1.593(4) . ? P2 F25 1.595(4) . ? P2 F21 1.596(4) . ? P2 F24 1.597(4) . ? P2 F23 1.599(4) . ? P2 F22 1.607(4) . ? P3 F31' 1.20(3) . ? P3 F33 1.458(15) . ? P3 F35 1.499(7) . ? P3 F34 1.576(14) . ? P3 F36 1.574(7) . ? P3 F32' 1.54(4) . ? P3 F34' 1.66(3) . ? P3 F32 1.73(2) . ? P3 F31 1.74(2) . ? P3 F33' 1.81(4) . ? P4 F44 1.50(2) . ? P4 F43 1.52(2) . ? P4 F42 1.539(14) . ? P4 F41' 1.542(10) . ? P4 F43' 1.556(15) . ? P4 F46 1.583(6) . ? P4 F45 1.587(5) . ? P4 F44' 1.59(2) . ? P4 F42' 1.593(13) . ? P4 F41 1.607(10) . ? C131 N131 1.26(2) . ? C131 O131 1.26(2) . ? N131 C132 1.364(11) . ? N131 C133 1.37(2) . ? N141 C141 1.349(14) . ? N141 C143 1.421(13) . ? N141 C142 1.434(13) . ? O141 C141 1.220(13) . ? N151 C151 1.318(11) . ? N151 C153 1.409(13) . ? N151 C152 1.429(11) . ? O151 C151 1.257(12) . ? N161 C161 1.317(15) . ? N161 C162 1.35(2) . ? N161 C163 1.48(2) . ? C161 O161 1.33(2) . ? N171 C171 1.321(11) . ? N171 C173 1.437(10) . ? N171 C172 1.438(10) . ? O171 C171 1.221(10) . ? N181 C181 1.371(11) . ? N181 C182 1.491(13) . ? N181 C183 1.55(2) . ? C181 O181 1.27(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 N102 Cu1 N21 168.4(2) . . ? N102 Cu1 N11 102.5(2) . . ? N21 Cu1 N11 79.7(2) . . ? N102 Cu1 N31 96.0(2) . . ? N21 Cu1 N31 79.7(2) . . ? N11 Cu1 N31 157.6(2) . . ? N102 Cu1 O1 92.1(2) . . ? N21 Cu1 O1 98.8(2) . . ? N11 Cu1 O1 99.1(2) . . ? N31 Cu1 O1 92.7(2) . . ? N72 Cu2 N51 171.6(2) . . ? N72 Cu2 N41 103.8(2) . . ? N51 Cu2 N41 79.4(2) . . ? N72 Cu2 N61 95.6(2) . . ? N51 Cu2 N61 79.7(2) . . ? N41 Cu2 N61 156.8(2) . . ? N72 Cu2 O2 91.1(2) . . ? N51 Cu2 O2 96.1(2) . . ? N41 Cu2 O2 100.2(2) . . ? N61 Cu2 O2 92.0(2) . . ? N42 Cu3 N111 170.2(2) . . ? N42 Cu3 N101 105.2(2) . . ? N111 Cu3 N101 79.4(2) . . ? N42 Cu3 N121 94.3(2) . . ? N111 Cu3 N121 79.4(2) . . ? N101 Cu3 N121 156.4(2) . . ? N42 Cu3 O3 89.6(2) . . ? N111 Cu3 O3 98.1(2) . . ? N101 Cu3 O3 100.5(2) . . ? N121 Cu3 O3 92.8(2) . . ? N12 Cu4 N81 171.9(2) . . ? N12 Cu4 N71 103.6(2) . . ? N81 Cu4 N71 79.4(2) . . ? N12 Cu4 N91 96.5(2) . . ? N81 Cu4 N91 79.0(2) . . ? N71 Cu4 N91 156.1(2) . . ? N12 Cu4 O4 88.7(2) . . ? N81 Cu4 O4 98.3(2) . . ? N71 Cu4 O4 100.4(2) . . ? N91 Cu4 O4 92.8(2) . . ? N12 N11 C15 107.7(5) . . ? N12 N11 Cu1 137.8(4) . . ? C15 N11 Cu1 114.5(4) . . ? C13 N12 N11 108.1(4) . . ? C13 N12 Cu4 129.6(4) . . ? N11 N12 Cu4 122.0(4) . . ? N12 C13 C14 109.3(5) . . ? C15 C14 C13 105.8(5) . . ? N11 C15 C14 109.1(5) . . ? N11 C15 C22 115.1(5) . . ? C14 C15 C22 135.5(5) . . ? C26 N21 C22 122.7(5) . . ? C26 N21 Cu1 118.3(4) . . ? C22 N21 Cu1 118.6(4) . . ? N21 C22 C23 120.5(6) . . ? N21 C22 C15 111.8(5) . . ? C23 C22 C15 127.6(6) . . ? C22 C23 C24 117.8(6) . . ? C23 C24 C25 121.1(7) . . ? C26 C25 C24 118.4(7) . . ? N21 C26 C25 119.4(6) . . ? N21 C26 C32 113.1(6) . . ? C25 C26 C32 127.5(6) . . ? C36 N31 C32 119.5(6) . . ? C36 N31 Cu1 126.5(5) . . ? C32 N31 Cu1 114.0(4) . . ? N31 C32 C33 120.9(7) . . ? N31 C32 C26 114.8(6) . . ? C33 C32 C26 124.2(7) . . ? C32 C33 C34 117.9(7) . . ? C35 C34 C33 120.4(7) . . ? C34 C35 C36 118.1(7) . . ? N31 C36 C35 123.1(7) . . ? C45 N41 N42 107.6(5) . . ? C45 N41 Cu2 115.2(4) . . ? N42 N41 Cu2 137.0(4) . . ? C43 N42 N41 107.1(5) . . ? C43 N42 Cu3 130.4(4) . . ? N41 N42 Cu3 121.1(4) . . ? N42 C43 C44 111.4(6) . . ? C43 C44 C45 103.4(5) . . ? N41 C45 C44 110.4(6) . . ? N41 C45 C52 114.3(5) . . ? C44 C45 C52 135.2(6) . . ? C52 N51 C56 121.8(5) . . ? C52 N51 Cu2 119.0(4) . . ? C56 N51 Cu2 118.8(4) . . ? N51 C52 C53 120.7(6) . . ? N51 C52 C45 111.6(5) . . ? C53 C52 C45 127.5(6) . . ? C54 C53 C52 117.7(6) . . ? C55 C54 C53 121.2(6) . . ? C54 C55 C56 119.2(7) . . ? N51 C56 C55 119.5(6) . . ? N51 C56 C62 112.4(5) . . ? C55 C56 C62 128.0(6) . . ? C66 N61 C62 119.1(5) . . ? C66 N61 Cu2 126.6(4) . . ? C62 N61 Cu2 114.2(4) . . ? N61 C62 C63 121.1(6) . . ? N61 C62 C56 114.6(5) . . ? C63 C62 C56 124.3(6) . . ? C64 C63 C62 119.2(7) . . ? C65 C64 C63 120.0(6) . . ? C64 C65 C66 118.5(6) . . ? N61 C66 C65 122.0(6) . . ? C75 N71 N72 108.0(4) . . ? C75 N71 Cu4 114.0(4) . . ? N72 N71 Cu4 138.0(4) . . ? C73 N72 N71 108.1(4) . . ? C73 N72 Cu2 129.5(4) . . ? N71 N72 Cu2 121.3(3) . . ? N72 C73 C74 109.9(5) . . ? C73 C74 C75 104.6(5) . . ? N71 C75 C74 109.4(5) . . ? N71 C75 C82 116.1(5) . . ? C74 C75 C82 134.5(5) . . ? C82 N81 C86 122.2(5) . . ? C82 N81 Cu4 119.1(4) . . ? C86 N81 Cu4 118.7(4) . . ? N81 C82 C83 120.1(5) . . ? N81 C82 C75 111.3(5) . . ? C83 C82 C75 128.5(6) . . ? C84 C83 C82 118.7(6) . . ? C85 C84 C83 120.8(6) . . ? C84 C85 C86 118.9(6) . . ? N81 C86 C85 119.3(6) . . ? N81 C86 C92 112.9(5) . . ? C85 C86 C92 127.8(6) . . ? C96 N91 C92 119.0(5) . . ? C96 N91 Cu4 126.1(4) . . ? C92 N91 Cu4 114.7(4) . . ? N91 C92 C93 120.8(6) . . ? N91 C92 C86 114.1(5) . . ? C93 C92 C86 125.1(6) . . ? C94 C93 C92 119.7(6) . . ? C95 C94 C93 119.0(6) . . ? C94 C95 C96 119.6(6) . . ? N91 C96 C95 122.0(6) . . ? C105 N101 N102 108.1(5) . . ? C105 N101 Cu3 115.2(4) . . ? N102 N101 Cu3 136.6(4) . . ? N101 N102 C103 107.6(5) . . ? N101 N102 Cu1 120.8(4) . . ? C103 N102 Cu1 130.5(4) . . ? N102 C103 C104 110.3(5) . . ? C103 C104 C105 104.3(5) . . ? N101 C105 C104 109.7(5) . . ? N101 C105 C112 115.0(5) . . ? C104 C105 C112 135.3(6) . . ? C116 N111 C112 121.9(5) . . ? C116 N111 Cu3 119.0(4) . . ? C112 N111 Cu3 118.7(4) . . ? N111 C112 C113 119.6(6) . . ? N111 C112 C105 111.4(5) . . ? C113 C112 C105 128.9(6) . . ? C114 C113 C112 118.7(6) . . ? C113 C114 C115 121.2(6) . . ? C114 C115 C116 117.8(6) . . ? N111 C116 C115 120.7(6) . . ? N111 C116 C122 113.1(5) . . ? C115 C116 C122 126.0(6) . . ? C126 N121 C122 118.7(5) . . ? C126 N121 Cu3 126.9(4) . . ? C122 N121 Cu3 114.4(4) . . ? N121 C122 C123 121.2(6) . . ? N121 C122 C116 113.7(5) . . ? C123 C122 C116 125.1(6) . . ? C122 C123 C124 118.8(6) . . ? C125 C124 C123 120.3(6) . . ? C124 C125 C126 118.3(6) . . ? N121 C126 C125 122.6(6) . . ? C1 O1 Cu1 126.9(4) . . ? C1 N1 C11 121.5(6) . . ? C1 N1 C10 122.3(6) . . ? C11 N1 C10 116.2(5) . . ? O1 C1 N1 125.9(6) . . ? C2 O2 Cu2 127.1(4) . . ? C2 N2 C21 121.2(7) . . ? C2 N2 C20 120.6(7) . . ? C21 N2 C20 118.1(6) . . ? O2 C2 N2 125.2(7) . . ? C3 O3 Cu3 126.8(4) . . ? C3 N3 C31 122.2(6) . . ? C3 N3 C30 120.7(6) . . ? C31 N3 C30 117.1(6) . . ? O3 C3 N3 125.4(6) . . ? C4 O4 Cu4 130.0(4) . . ? C4 N4 C41 122.1(5) . . ? C4 N4 C40 121.4(6) . . ? C41 N4 C40 116.5(5) . . ? O4 C4 N4 124.7(6) . . ? F15 P1 F12 91.5(3) . . ? F15 P1 F13 89.8(3) . . ? F12 P1 F13 89.6(3) . . ? F15 P1 F11 91.0(3) . . ? F12 P1 F11 91.0(3) . . ? F13 P1 F11 178.9(3) . . ? F15 P1 F16 178.8(3) . . ? F12 P1 F16 89.6(3) . . ? F13 P1 F16 89.9(3) . . ? F11 P1 F16 89.3(3) . . ? F15 P1 F14 89.9(3) . . ? F12 P1 F14 178.5(3) . . ? F13 P1 F14 90.5(2) . . ? F11 P1 F14 88.8(2) . . ? F16 P1 F14 89.0(3) . . ? F26 P2 F25 179.2(2) . . ? F26 P2 F21 90.6(2) . . ? F25 P2 F21 89.9(2) . . ? F26 P2 F24 89.9(2) . . ? F25 P2 F24 89.4(2) . . ? F21 P2 F24 90.2(2) . . ? F26 P2 F23 90.1(2) . . ? F25 P2 F23 89.5(2) . . ? F21 P2 F23 179.4(3) . . ? F24 P2 F23 90.0(2) . . ? F26 P2 F22 90.7(2) . . ? F25 P2 F22 90.0(2) . . ? F21 P2 F22 89.6(2) . . ? F24 P2 F22 179.4(2) . . ? F23 P2 F22 90.2(2) . . ? F31' P3 F33 134.1(20) . . ? F31' P3 F35 112.6(21) . . ? F33 P3 F35 109.8(14) . . ? F31' P3 F34 63.0(16) . . ? F33 P3 F34 94.6(10) . . ? F35 P3 F34 98.2(9) . . ? F31' P3 F36 99.7(20) . . ? F33 P3 F36 95.5(8) . . ? F35 P3 F36 92.0(4) . . ? F34 P3 F36 162.3(14) . . ? F31' P3 F32' 86.3(25) . . ? F33 P3 F32' 48.6(16) . . ? F35 P3 F32' 156.7(19) . . ? F34 P3 F32' 77.8(19) . . ? F36 P3 F32' 98.3(16) . . ? F31' P3 F34' 101.9(21) . . ? F33 P3 F34' 70.9(18) . . ? F35 P3 F34' 77.6(15) . . ? F34 P3 F34' 39.4(12) . . ? F36 P3 F34' 158.2(17) . . ? F32' P3 F34' 85.4(21) . . ? F31' P3 F32 52.7(19) . . ? F33 P3 F32 88.5(10) . . ? F35 P3 F32 160.7(11) . . ? F34 P3 F32 86.0(11) . . ? F36 P3 F32 79.9(8) . . ? F32' P3 F32 42.7(13) . . ? F34' P3 F32 115.5(15) . . ? F31' P3 F31 35.0(20) . . ? F33 P3 F31 168.2(13) . . ? F35 P3 F31 82.0(5) . . ? F34 P3 F31 82.7(9) . . ? F36 P3 F31 84.5(5) . . ? F32' P3 F31 119.7(20) . . ? F34' P3 F31 112.4(17) . . ? F32 P3 F31 79.8(9) . . ? F31' P3 F33' 173.1(22) . . ? F33 P3 F33' 39.8(14) . . ? F35 P3 F33' 71.9(19) . . ? F34 P3 F33' 111.8(18) . . ? F36 P3 F33' 85.1(14) . . ? F32' P3 F33' 88.0(21) . . ? F34' P3 F33' 73.6(22) . . ? F32 P3 F33' 124.1(17) . . ? F31 P3 F33' 151.4(16) . . ? F44 P4 F43 92.0(12) . . ? F44 P4 F42 170.3(14) . . ? F43 P4 F42 88.2(11) . . ? F44 P4 F41' 123.6(11) . . ? F43 P4 F41' 142.0(13) . . ? F42 P4 F41' 59.2(9) . . ? F44 P4 F43' 57.9(10) . . ? F43 P4 F43' 34.5(10) . . ? F42 P4 F43' 120.7(11) . . ? F41' P4 F43' 173.0(10) . . ? F44 P4 F46 87.0(10) . . ? F43 P4 F46 88.7(11) . . ? F42 P4 F46 102.7(9) . . ? F41' P4 F46 81.0(6) . . ? F43' P4 F46 92.5(8) . . ? F44 P4 F45 91.6(10) . . ? F43 P4 F45 92.1(11) . . ? F42 P4 F45 78.7(9) . . ? F41' P4 F45 99.1(6) . . ? F43' P4 F45 87.5(8) . . ? F46 P4 F45 178.4(3) . . ? F44 P4 F44' 30.4(10) . . ? F43 P4 F44' 122.3(13) . . ? F42 P4 F44' 148.6(10) . . ? F41' P4 F44' 93.7(10) . . ? F43' P4 F44' 88.2(11) . . ? F46 P4 F44' 86.8(7) . . ? F45 P4 F44' 91.6(7) . . ? F44 P4 F42' 146.7(11) . . ? F43 P4 F42' 55.0(10) . . ? F42 P4 F42' 35.6(7) . . ? F41' P4 F42' 88.0(10) . . ? F43' P4 F42' 89.5(10) . . ? F46 P4 F42' 88.3(7) . . ? F45 P4 F42' 93.3(7) . . ? F44' P4 F42' 174.4(9) . . ? F44 P4 F41 88.2(9) . . ? F43 P4 F41 173.0(12) . . ? F42 P4 F41 90.5(9) . . ? F41' P4 F41 40.7(6) . . ? F43' P4 F41 143.9(11) . . ? F46 P4 F41 98.3(7) . . ? F45 P4 F41 80.9(7) . . ? F44' P4 F41 58.3(9) . . ? F42' P4 F41 125.1(10) . . ? N131 C131 O131 128.8(17) . . ? C131 N131 C132 122.1(12) . . ? C131 N131 C133 120.8(16) . . ? C132 N131 C133 117.1(15) . . ? C141 N141 C143 116.3(10) . . ? C141 N141 C142 125.5(12) . . ? C143 N141 C142 118.2(11) . . ? O141 C141 N141 121.9(12) . . ? C151 N151 C153 123.0(10) . . ? C151 N151 C152 119.8(10) . . ? C153 N151 C152 117.2(8) . . ? O151 C151 N151 125.8(11) . . ? C161 N161 C162 132.0(16) . . ? C161 N161 C163 116.8(14) . . ? C162 N161 C163 110.3(13) . . ? N161 C161 O161 113.3(16) . . ? C171 N171 C173 123.0(8) . . ? C171 N171 C172 120.9(8) . . ? C173 N171 C172 116.0(8) . . ? O171 C171 N171 126.7(10) . . ? C181 N181 C182 116.8(10) . . ? C181 N181 C183 117.4(10) . . ? C182 N181 C183 125.7(11) . . ? O181 C181 N181 112.1(13) . . ? _refine_diff_density_max 1.005 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.096 #=END