# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kumar Biradha' _publ_contact_author_email kbiradha@yahoo.com _publ_section_title ; Post-synthetic modification of isomorphic coordination layers: exchange dynamics of metal ions in single crystal to single crystal fashion ; loop_ _publ_author_name K.Biradha G.Mukherjee # Attachment '- kbga-r1.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 866718' #TrackingRef '- kbga-r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H48 F12 N6 O14 P2 Zn' _chemical_formula_weight 1512.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2940(17) _cell_length_b 19.025(3) _cell_length_c 16.509(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.204(5) _cell_angle_gamma 90.00 _cell_volume 3200.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6712 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 26.84 _exptl_crystal_description diamond _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41162 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.81 _reflns_number_total 6712 _reflns_number_gt 5201 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.061 0.300 0.166 52 5 ' ' 2 -0.062 0.800 0.334 52 5 ' ' 3 0.061 0.200 0.666 52 5 ' ' 4 -0.062 0.700 0.834 52 5 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6712 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.2308 _refine_ls_wR_factor_gt 0.2221 _refine_ls_goodness_of_fit_ref 1.679 _refine_ls_restrained_S_all 1.679 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.5000 0.5000 0.0000 0.0311(2) Uani 1 2 d S . . O1 O 0.6681(2) 0.59537(12) 0.35173(18) 0.0476(7) Uani 1 1 d . . . O1W O 1.6103(2) 0.46424(12) 0.11144(15) 0.0389(6) Uani 1 1 d . . . O2 O 0.6874(2) 0.34202(13) 0.38726(18) 0.0490(7) Uani 1 1 d . . . O3 O 0.9976(2) 0.46167(14) 0.25020(15) 0.0409(6) Uani 1 1 d . . . O16 O 0.4667(3) 0.57132(17) 0.2902(3) 0.0889(12) Uani 1 1 d . . . O21 O 0.8787(3) 0.4345(2) 0.13044(19) 0.0739(11) Uani 1 1 d . . . O31 O 0.4765(3) 0.35205(17) 0.3291(2) 0.0773(11) Uani 1 1 d . . . N11 N 0.4594(4) 0.82822(18) 0.3578(2) 0.0613(10) Uani 1 1 d . . . N21 N 1.3271(3) 0.47502(15) 0.05772(18) 0.0346(6) Uani 1 1 d . . . N31 N 0.5163(3) 0.10806(14) 0.44799(18) 0.0366(7) Uani 1 1 d . . . C1 C 0.7176(4) 0.52798(18) 0.3373(2) 0.0395(8) Uani 1 1 d . . . C2 C 0.8261(4) 0.52692(19) 0.2981(2) 0.0391(8) Uani 1 1 d . . . H2 H 0.8601 0.5681 0.2793 0.047 Uiso 1 1 calc R . . C3 C 0.8829(3) 0.46306(18) 0.2877(2) 0.0360(8) Uani 1 1 d . . . C4 C 0.8356(3) 0.40167(18) 0.3161(2) 0.0387(8) Uani 1 1 d . . . H4 H 0.8757 0.3587 0.3092 0.046 Uiso 1 1 calc R . . C5 C 0.7261(3) 0.40618(17) 0.3555(2) 0.0386(8) Uani 1 1 d . . . C6 C 0.6666(4) 0.46878(19) 0.3681(2) 0.0416(8) Uani 1 1 d . . . H6 H 0.5948 0.4711 0.3964 0.050 Uiso 1 1 calc R . . C11 C 0.5802(5) 0.8018(2) 0.3765(4) 0.0805(17) Uani 1 1 d . . . H11 H 0.6468 0.8326 0.3974 0.097 Uiso 1 1 calc R . . C12 C 0.6134(4) 0.7335(2) 0.3674(3) 0.0657(13) Uani 1 1 d . . . H12 H 0.6997 0.7187 0.3817 0.079 Uiso 1 1 calc R . . C13 C 0.5175(4) 0.68688(19) 0.3368(2) 0.0448(9) Uani 1 1 d . . . C14 C 0.3901(4) 0.7120(2) 0.3159(3) 0.0545(10) Uani 1 1 d . . . H14 H 0.3225 0.6821 0.2943 0.065 Uiso 1 1 calc R . . C15 C 0.3667(5) 0.7821(2) 0.3281(3) 0.0604(11) Uani 1 1 d . . . H15 H 0.2811 0.7985 0.3147 0.073 Uiso 1 1 calc R . . C16 C 0.5444(4) 0.6115(2) 0.3221(2) 0.0480(9) Uani 1 1 d . . . C21 C 1.3288(4) 0.4889(2) 0.1374(2) 0.0430(9) Uani 1 1 d . . . H21 H 1.4064 0.5056 0.1669 0.052 Uiso 1 1 calc R . . C22 C 1.2219(4) 0.4799(2) 0.1783(2) 0.0453(9) Uani 1 1 d . . . H22 H 1.2273 0.4900 0.2338 0.054 Uiso 1 1 calc R . . C23 C 1.1064(3) 0.45535(19) 0.1341(2) 0.0386(8) Uani 1 1 d . . . C24 C 1.1039(3) 0.4401(2) 0.0531(2) 0.0475(10) Uani 1 1 d . . . H24 H 1.0280 0.4224 0.0226 0.057 Uiso 1 1 calc R . . C25 C 1.2148(3) 0.4510(2) 0.0167(2) 0.0427(9) Uani 1 1 d . . . H25 H 1.2112 0.4413 -0.0388 0.051 Uiso 1 1 calc R . . C26 C 0.9819(3) 0.4487(2) 0.1704(2) 0.0430(9) Uani 1 1 d . . . C31 C 0.4195(4) 0.1428(2) 0.4033(3) 0.0466(9) Uani 1 1 d . . . H31 H 0.3402 0.1196 0.3884 0.056 Uiso 1 1 calc R . . C32 C 0.4299(4) 0.2120(2) 0.3773(3) 0.0513(10) Uani 1 1 d . . . H32 H 0.3586 0.2348 0.3476 0.062 Uiso 1 1 calc R . . C33 C 0.5492(4) 0.24600(19) 0.3969(2) 0.0426(9) Uani 1 1 d . . . C34 C 0.6516(4) 0.20959(19) 0.4419(3) 0.0462(9) Uani 1 1 d . . . H34 H 0.7333 0.2306 0.4558 0.055 Uiso 1 1 calc R . . C35 C 0.6301(4) 0.14180(19) 0.4655(3) 0.0465(9) Uani 1 1 d . . . H35 H 0.6997 0.1179 0.4956 0.056 Uiso 1 1 calc R . . C36 C 0.5627(4) 0.31906(19) 0.3673(3) 0.0463(9) Uani 1 1 d . . . C101 C 0.1066(7) 0.4232(4) 0.4758(4) 0.093(2) Uani 1 1 d . . . C102 C 0.2104(8) 0.4109(6) 0.4377(5) 0.130(3) Uani 1 1 d . . . H102 H 0.2400 0.3652 0.4320 0.157 Uiso 1 1 calc R . . C103 C 0.2739(9) 0.4674(7) 0.4064(5) 0.135(4) Uani 1 1 d . . . H103 H 0.3479 0.4584 0.3816 0.162 Uiso 1 1 calc R . . C104 C 0.2303(9) 0.5387(6) 0.4108(4) 0.124(3) Uani 1 1 d . . . H104 H 0.2761 0.5749 0.3896 0.149 Uiso 1 1 calc R . . C105 C 0.1205(7) 0.5531(5) 0.4463(4) 0.097(2) Uani 1 1 d . . . C106 C 0.0534(6) 0.4931(3) 0.4824(3) 0.0800(17) Uani 1 1 d . . . C107 C 0.0366(9) 0.3686(5) 0.5083(4) 0.113(2) Uani 1 1 d . . . H107 H 0.0644 0.3227 0.5020 0.136 Uiso 1 1 calc R . . C108 C 0.0683(9) 0.6213(4) 0.4521(5) 0.112(2) Uani 1 1 d . . . H108 H 0.1060 0.6593 0.4286 0.135 Uiso 1 1 calc R . . P1 P 0.00147(17) 0.17806(10) 0.33672(12) 0.0933(6) Uani 1 1 d . . . F100 F -0.0814(7) 0.1536(6) 0.4034(5) 0.271(5) Uani 1 1 d . . . F101 F 0.1099(7) 0.1908(4) 0.2834(5) 0.208(3) Uani 1 1 d . . . F102 F -0.0763(6) 0.1464(4) 0.2595(4) 0.212(3) Uani 1 1 d . . . F103 F 0.0994(7) 0.2042(4) 0.4094(5) 0.245(4) Uani 1 1 d . . . F104 F -0.0909(7) 0.2377(3) 0.3296(5) 0.240(4) Uani 1 1 d . . . F105 F 0.0687(5) 0.1027(2) 0.3533(3) 0.1404(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0229(3) 0.0275(3) 0.0450(4) -0.0041(2) 0.0117(2) -0.0018(2) O1 0.0396(14) 0.0258(12) 0.0786(19) -0.0090(12) 0.0132(13) 0.0016(10) O1W 0.0272(12) 0.0376(13) 0.0522(14) 0.0022(11) 0.0070(10) -0.0023(10) O2 0.0405(14) 0.0297(13) 0.0803(19) 0.0157(12) 0.0203(13) -0.0033(11) O3 0.0270(12) 0.0514(16) 0.0472(14) -0.0009(11) 0.0153(10) -0.0038(11) O16 0.073(2) 0.0487(18) 0.132(3) -0.038(2) -0.032(2) 0.0105(17) O21 0.0251(14) 0.141(3) 0.0574(18) -0.0213(19) 0.0130(13) -0.0147(17) O31 0.0512(18) 0.0502(18) 0.127(3) 0.0339(19) 0.0002(19) -0.0071(15) N11 0.066(2) 0.0392(19) 0.079(3) -0.0098(17) 0.0121(19) 0.0123(18) N21 0.0244(14) 0.0328(14) 0.0489(17) -0.0036(13) 0.0130(12) 0.0002(12) N31 0.0309(15) 0.0302(14) 0.0518(17) 0.0066(12) 0.0161(13) 0.0000(12) C1 0.0385(19) 0.0268(17) 0.055(2) -0.0072(15) 0.0130(16) -0.0015(15) C2 0.039(2) 0.0294(17) 0.051(2) 0.0063(15) 0.0159(16) -0.0042(15) C3 0.0268(17) 0.0396(19) 0.0436(18) -0.0011(15) 0.0118(14) -0.0041(14) C4 0.0316(18) 0.0313(17) 0.056(2) 0.0005(15) 0.0176(16) 0.0009(14) C5 0.0378(19) 0.0285(17) 0.053(2) 0.0043(14) 0.0189(16) -0.0040(14) C6 0.038(2) 0.038(2) 0.054(2) 0.0012(16) 0.0210(17) 0.0004(16) C11 0.064(3) 0.041(2) 0.130(5) -0.027(3) -0.006(3) -0.001(2) C12 0.044(2) 0.040(2) 0.110(4) -0.014(2) 0.004(2) 0.0070(19) C13 0.048(2) 0.0326(18) 0.053(2) -0.0071(16) 0.0061(17) 0.0059(16) C14 0.046(2) 0.043(2) 0.071(3) -0.0008(19) -0.0011(19) 0.0033(18) C15 0.054(3) 0.049(2) 0.078(3) -0.002(2) 0.007(2) 0.015(2) C16 0.054(2) 0.038(2) 0.051(2) -0.0056(17) 0.0051(18) 0.0017(18) C21 0.0281(18) 0.055(2) 0.047(2) -0.0137(16) 0.0114(16) -0.0094(15) C22 0.0327(19) 0.061(2) 0.044(2) -0.0106(17) 0.0126(16) -0.0087(17) C23 0.0245(17) 0.046(2) 0.048(2) -0.0027(16) 0.0131(14) -0.0012(14) C24 0.0261(18) 0.070(3) 0.047(2) -0.0093(18) 0.0068(15) -0.0085(17) C25 0.0323(19) 0.053(2) 0.044(2) -0.0074(16) 0.0102(15) -0.0019(16) C26 0.0244(17) 0.055(2) 0.052(2) -0.0021(17) 0.0113(16) -0.0019(15) C31 0.0324(18) 0.040(2) 0.069(3) 0.0115(18) 0.0127(17) -0.0067(16) C32 0.040(2) 0.039(2) 0.073(3) 0.0137(19) 0.0068(19) 0.0005(17) C33 0.038(2) 0.0349(18) 0.060(2) 0.0061(16) 0.0240(17) 0.0004(15) C34 0.0347(19) 0.040(2) 0.067(2) 0.0069(18) 0.0160(17) -0.0071(16) C35 0.0350(19) 0.0340(19) 0.072(3) 0.0081(17) 0.0136(18) -0.0003(15) C36 0.044(2) 0.0332(19) 0.065(2) 0.0081(17) 0.0205(19) -0.0028(16) C101 0.082(4) 0.108(5) 0.081(4) -0.020(4) -0.017(3) 0.013(4) C102 0.101(6) 0.215(11) 0.073(5) -0.029(5) 0.004(4) 0.038(6) C103 0.099(6) 0.208(12) 0.094(6) -0.021(7) 0.006(5) 0.042(7) C104 0.103(6) 0.186(10) 0.080(5) 0.003(5) 0.002(4) -0.019(6) C105 0.073(4) 0.146(7) 0.066(3) -0.006(4) -0.005(3) -0.005(4) C106 0.071(4) 0.108(5) 0.057(3) -0.015(3) -0.006(3) 0.004(3) C107 0.114(6) 0.130(7) 0.088(5) -0.008(4) -0.014(4) -0.010(6) C108 0.133(7) 0.098(5) 0.096(5) 0.003(4) -0.018(5) -0.022(5) P1 0.0757(10) 0.0954(12) 0.1080(12) -0.0252(10) 0.0099(9) 0.0345(9) F100 0.190(6) 0.380(12) 0.279(9) 0.127(8) 0.156(7) 0.132(7) F101 0.213(6) 0.189(6) 0.227(7) 0.032(5) 0.047(5) -0.078(5) F102 0.190(5) 0.236(7) 0.173(5) -0.065(5) -0.103(4) 0.075(5) F103 0.201(6) 0.257(8) 0.265(8) -0.169(7) -0.004(6) -0.014(6) F104 0.260(8) 0.128(4) 0.339(9) 0.014(5) 0.066(7) 0.134(5) F105 0.184(4) 0.130(4) 0.100(3) -0.007(2) -0.006(3) 0.055(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 Zn1 O1W 2.131(2) 3_865 ? Zn1 O1W 2.131(2) . ? Zn1 N21 2.188(3) . ? Zn1 N21 2.188(3) 3_865 ? Zn1 N31 2.243(3) 2_755 ? Zn1 N31 2.243(3) 4_665 ? O1 C16 1.333(5) . ? O1 C1 1.412(4) . ? O2 C36 1.351(5) . ? O2 C5 1.408(4) . ? O3 C26 1.327(4) . ? O3 C3 1.410(4) . ? O16 C16 1.176(5) . ? O21 C26 1.198(4) . ? O31 C36 1.191(5) . ? N11 C11 1.336(6) . ? N11 C15 1.337(6) . ? N21 C25 1.334(4) . ? N21 C21 1.339(5) . ? N31 C31 1.329(5) . ? N31 C35 1.331(4) . ? N31 Zn1 2.243(3) 2_745 ? C1 C6 1.371(5) . ? C1 C2 1.368(5) . ? C2 C3 1.370(5) . ? C2 H2 0.9300 . ? C3 C4 1.374(5) . ? C4 C5 1.382(5) . ? C4 H4 0.9300 . ? C5 C6 1.369(5) . ? C6 H6 0.9300 . ? C11 C12 1.357(6) . ? C11 H11 0.9300 . ? C12 C13 1.369(6) . ? C12 H12 0.9300 . ? C13 C14 1.392(6) . ? C13 C16 1.487(5) . ? C14 C15 1.375(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C21 C22 1.381(5) . ? C21 H21 0.9300 . ? C22 C23 1.384(5) . ? C22 H22 0.9300 . ? C23 C24 1.365(5) . ? C23 C26 1.496(5) . ? C24 C25 1.379(5) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C31 C32 1.393(5) . ? C31 H31 0.9300 . ? C32 C33 1.384(5) . ? C32 H32 0.9300 . ? C33 C34 1.385(5) . ? C33 C36 1.486(5) . ? C34 C35 1.374(5) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C101 C102 1.336(10) . ? C101 C107 1.413(10) . ? C101 C106 1.449(9) . ? C102 C103 1.394(13) . ? C102 H102 0.9300 . ? C103 C104 1.434(13) . ? C103 H103 0.9300 . ? C104 C105 1.374(11) . ? C104 H104 0.9300 . ? C105 C108 1.413(11) . ? C105 C106 1.501(10) . ? C106 C106 1.341(13) 3_566 ? C107 C108 1.354(10) 3_566 ? C107 H107 0.9300 . ? C108 C107 1.354(10) 3_566 ? C108 H108 0.9300 . ? P1 F104 1.474(5) . ? P1 F101 1.536(7) . ? P1 F102 1.528(5) . ? P1 F103 1.535(6) . ? P1 F100 1.557(6) . ? P1 F105 1.598(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 O1W Zn1 O1W 180.0 3_865 . ? O1W Zn1 N21 94.54(10) 3_865 . ? O1W Zn1 N21 85.46(10) . . ? O1W Zn1 N21 85.46(10) 3_865 3_865 ? O1W Zn1 N21 94.54(10) . 3_865 ? N21 Zn1 N21 180.0 . 3_865 ? O1W Zn1 N31 88.75(10) 3_865 2_755 ? O1W Zn1 N31 91.25(10) . 2_755 ? N21 Zn1 N31 85.55(10) . 2_755 ? N21 Zn1 N31 94.45(10) 3_865 2_755 ? O1W Zn1 N31 91.25(10) 3_865 4_665 ? O1W Zn1 N31 88.75(10) . 4_665 ? N21 Zn1 N31 94.45(10) . 4_665 ? N21 Zn1 N31 85.55(10) 3_865 4_665 ? N31 Zn1 N31 180.0 2_755 4_665 ? C16 O1 C1 119.7(3) . . ? C36 O2 C5 119.9(3) . . ? C26 O3 C3 116.6(3) . . ? C11 N11 C15 115.5(4) . . ? C25 N21 C21 117.1(3) . . ? C25 N21 Zn1 123.6(2) . . ? C21 N21 Zn1 119.2(2) . . ? C31 N31 C35 116.6(3) . . ? C31 N31 Zn1 125.3(2) . 2_745 ? C35 N31 Zn1 118.1(2) . 2_745 ? C6 C1 C2 123.0(3) . . ? C6 C1 O1 121.1(3) . . ? C2 C1 O1 115.6(3) . . ? C1 C2 C3 117.7(3) . . ? C1 C2 H2 121.2 . . ? C3 C2 H2 121.2 . . ? C4 C3 C2 122.2(3) . . ? C4 C3 O3 119.6(3) . . ? C2 C3 O3 118.1(3) . . ? C3 C4 C5 117.4(3) . . ? C3 C4 H4 121.3 . . ? C5 C4 H4 121.3 . . ? C6 C5 C4 122.6(3) . . ? C6 C5 O2 122.8(3) . . ? C4 C5 O2 114.5(3) . . ? C1 C6 C5 117.1(3) . . ? C1 C6 H6 121.4 . . ? C5 C6 H6 121.4 . . ? N11 C11 C12 125.2(4) . . ? N11 C11 H11 117.4 . . ? C12 C11 H11 117.4 . . ? C13 C12 C11 118.8(4) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 118.2(4) . . ? C12 C13 C16 122.9(4) . . ? C14 C13 C16 118.8(4) . . ? C15 C14 C13 118.4(4) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? N11 C15 C14 124.0(4) . . ? N11 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? O16 C16 O1 124.6(4) . . ? O16 C16 C13 124.7(4) . . ? O1 C16 C13 110.7(3) . . ? N21 C21 C22 123.8(3) . . ? N21 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C21 C22 C23 117.9(3) . . ? C21 C22 H22 121.0 . . ? C23 C22 H22 121.0 . . ? C24 C23 C22 118.8(3) . . ? C24 C23 C26 118.6(3) . . ? C22 C23 C26 122.5(3) . . ? C23 C24 C25 119.6(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N21 C25 C24 122.8(3) . . ? N21 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? O21 C26 O3 124.2(3) . . ? O21 C26 C23 122.7(4) . . ? O3 C26 C23 113.1(3) . . ? N31 C31 C32 123.8(3) . . ? N31 C31 H31 118.1 . . ? C32 C31 H31 118.1 . . ? C33 C32 C31 118.3(4) . . ? C33 C32 H32 120.9 . . ? C31 C32 H32 120.9 . . ? C34 C33 C32 118.2(3) . . ? C34 C33 C36 123.0(3) . . ? C32 C33 C36 118.8(3) . . ? C35 C34 C33 118.7(3) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? N31 C35 C34 124.3(4) . . ? N31 C35 H35 117.9 . . ? C34 C35 H35 117.9 . . ? O31 C36 O2 124.7(3) . . ? O31 C36 C33 124.7(4) . . ? O2 C36 C33 110.6(3) . . ? C102 C101 C107 122.4(9) . . ? C102 C101 C106 122.2(9) . . ? C107 C101 C106 115.3(7) . . ? C101 C102 C103 119.2(10) . . ? C101 C102 H102 120.4 . . ? C103 C102 H102 120.4 . . ? C102 C103 C104 123.0(9) . . ? C102 C103 H103 118.5 . . ? C104 C103 H103 118.5 . . ? C105 C104 C103 119.5(9) . . ? C105 C104 H104 120.3 . . ? C103 C104 H104 120.3 . . ? C104 C105 C108 123.8(9) . . ? C104 C105 C106 118.1(8) . . ? C108 C105 C106 118.1(7) . . ? C106 C106 C101 123.7(8) 3_566 . ? C106 C106 C105 118.4(8) 3_566 . ? C101 C106 C105 117.9(6) . . ? C108 C107 C101 124.4(9) 3_566 . ? C108 C107 H107 117.8 3_566 . ? C101 C107 H107 117.8 . . ? C107 C108 C105 120.0(9) 3_566 . ? C107 C108 H108 120.0 3_566 . ? C105 C108 H108 120.0 . . ? F104 P1 F101 110.2(4) . . ? F104 P1 F102 88.9(4) . . ? F101 P1 F102 85.5(4) . . ? F104 P1 F103 99.1(4) . . ? F101 P1 F103 87.0(4) . . ? F102 P1 F103 170.5(4) . . ? F104 P1 F100 82.7(4) . . ? F101 P1 F100 165.6(4) . . ? F102 P1 F100 101.4(5) . . ? F103 P1 F100 84.8(5) . . ? F104 P1 F105 164.2(4) . . ? F101 P1 F105 84.7(3) . . ? F102 P1 F105 87.3(3) . . ? F103 P1 F105 86.3(4) . . ? F100 P1 F105 83.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Zn1 N21 C25 33.9(3) 3_865 . . . ? O1W Zn1 N21 C25 -146.1(3) . . . . ? N31 Zn1 N21 C25 122.3(3) 2_755 . . . ? N31 Zn1 N21 C25 -57.7(3) 4_665 . . . ? O1W Zn1 N21 C21 -141.1(3) 3_865 . . . ? O1W Zn1 N21 C21 38.9(3) . . . . ? N31 Zn1 N21 C21 -52.7(3) 2_755 . . . ? N31 Zn1 N21 C21 127.3(3) 4_665 . . . ? C16 O1 C1 C6 -64.0(5) . . . . ? C16 O1 C1 C2 122.2(4) . . . . ? C6 C1 C2 C3 2.0(6) . . . . ? O1 C1 C2 C3 175.7(3) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C1 C2 C3 O3 -177.7(3) . . . . ? C26 O3 C3 C4 87.0(4) . . . . ? C26 O3 C3 C2 -96.2(4) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? O3 C3 C4 C5 177.4(3) . . . . ? C3 C4 C5 C6 -1.4(6) . . . . ? C3 C4 C5 O2 -176.5(3) . . . . ? C36 O2 C5 C6 58.5(5) . . . . ? C36 O2 C5 C4 -126.4(4) . . . . ? C2 C1 C6 C5 -2.6(6) . . . . ? O1 C1 C6 C5 -175.9(3) . . . . ? C4 C5 C6 C1 2.2(6) . . . . ? O2 C5 C6 C1 176.9(3) . . . . ? C15 N11 C11 C12 0.0(9) . . . . ? N11 C11 C12 C13 0.0(10) . . . . ? C11 C12 C13 C14 0.4(8) . . . . ? C11 C12 C13 C16 178.0(5) . . . . ? C12 C13 C14 C15 -0.9(7) . . . . ? C16 C13 C14 C15 -178.5(4) . . . . ? C11 N11 C15 C14 -0.5(7) . . . . ? C13 C14 C15 N11 0.9(7) . . . . ? C1 O1 C16 O16 7.5(7) . . . . ? C1 O1 C16 C13 -174.1(3) . . . . ? C12 C13 C16 O16 -173.9(5) . . . . ? C14 C13 C16 O16 3.6(7) . . . . ? C12 C13 C16 O1 7.6(6) . . . . ? C14 C13 C16 O1 -174.9(4) . . . . ? C25 N21 C21 C22 -0.1(6) . . . . ? Zn1 N21 C21 C22 175.2(3) . . . . ? N21 C21 C22 C23 -0.3(6) . . . . ? C21 C22 C23 C24 1.1(6) . . . . ? C21 C22 C23 C26 -175.4(4) . . . . ? C22 C23 C24 C25 -1.6(6) . . . . ? C26 C23 C24 C25 175.0(4) . . . . ? C21 N21 C25 C24 -0.4(6) . . . . ? Zn1 N21 C25 C24 -175.5(3) . . . . ? C23 C24 C25 N21 1.3(6) . . . . ? C3 O3 C26 O21 -4.3(6) . . . . ? C3 O3 C26 C23 174.2(3) . . . . ? C24 C23 C26 O21 -4.4(6) . . . . ? C22 C23 C26 O21 172.1(4) . . . . ? C24 C23 C26 O3 177.0(3) . . . . ? C22 C23 C26 O3 -6.5(5) . . . . ? C35 N31 C31 C32 -2.6(6) . . . . ? Zn1 N31 C31 C32 174.7(3) 2_745 . . . ? N31 C31 C32 C33 2.1(7) . . . . ? C31 C32 C33 C34 -0.5(6) . . . . ? C31 C32 C33 C36 178.1(4) . . . . ? C32 C33 C34 C35 -0.4(6) . . . . ? C36 C33 C34 C35 -179.0(4) . . . . ? C31 N31 C35 C34 1.5(6) . . . . ? Zn1 N31 C35 C34 -176.0(3) 2_745 . . . ? C33 C34 C35 N31 0.0(6) . . . . ? C5 O2 C36 O31 -6.6(6) . . . . ? C5 O2 C36 C33 171.3(3) . . . . ? C34 C33 C36 O31 -179.3(5) . . . . ? C32 C33 C36 O31 2.1(7) . . . . ? C34 C33 C36 O2 2.7(5) . . . . ? C32 C33 C36 O2 -175.8(3) . . . . ? C107 C101 C102 C103 179.4(7) . . . . ? C106 C101 C102 C103 3.0(10) . . . . ? C101 C102 C103 C104 -2.1(12) . . . . ? C102 C103 C104 C105 -0.7(11) . . . . ? C103 C104 C105 C108 -178.7(6) . . . . ? C103 C104 C105 C106 2.4(9) . . . . ? C102 C101 C106 C106 177.4(7) . . . 3_566 ? C107 C101 C106 C106 0.9(10) . . . 3_566 ? C102 C101 C106 C105 -1.3(9) . . . . ? C107 C101 C106 C105 -177.8(5) . . . . ? C104 C105 C106 C106 179.7(6) . . . 3_566 ? C108 C105 C106 C106 0.7(10) . . . 3_566 ? C104 C105 C106 C101 -1.5(8) . . . . ? C108 C105 C106 C101 179.5(5) . . . . ? C102 C101 C107 C108 179.4(7) . . . 3_566 ? C106 C101 C107 C108 -4.0(10) . . . 3_566 ? C104 C105 C108 C107 -176.7(6) . . . 3_566 ? C106 C105 C108 C107 2.2(9) . . . 3_566 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.81 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.419 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.094 data_3a _database_code_depnum_ccdc_archive 'CCDC 866719' #TrackingRef '- kbga-r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H48 Cu F12 N6 O16 P2' _chemical_formula_weight 1510.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.224(2) _cell_length_b 18.934(4) _cell_length_c 16.667(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.438(7) _cell_angle_gamma 90.00 _cell_volume 3205.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5798 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 25.50 _exptl_crystal_description blocks _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1538 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-2 CCD' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37242 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5798 _reflns_number_gt 3962 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.433 0.705 0.332 51 4 ' ' 2 0.433 0.795 0.832 51 4 ' ' 3 0.567 0.205 0.168 51 4 ' ' 4 0.567 0.295 0.668 51 4 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5798 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2229 _refine_ls_wR_factor_gt 0.2109 _refine_ls_goodness_of_fit_ref 1.407 _refine_ls_restrained_S_all 1.407 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.0000 0.0364(3) Uani 1 2 d S . . P100 P -0.4976(2) 0.16930(11) -0.15927(13) 0.0929(6) Uani 1 1 d . . . F100 F -0.5809(7) 0.1415(5) -0.0915(5) 0.234(4) Uani 1 1 d . . . F101 F -0.5730(6) 0.1334(4) -0.2350(4) 0.198(3) Uani 1 1 d . . . F102 F -0.5889(8) 0.2301(3) -0.1675(5) 0.224(3) Uani 1 1 d . . . F104 F -0.3897(9) 0.1849(5) -0.2117(5) 0.230(4) Uani 1 1 d . . . F105 F -0.4249(6) 0.0946(3) -0.1445(3) 0.1453(19) Uani 1 1 d . . . F103 F -0.4022(7) 0.1941(3) -0.0843(4) 0.188(3) Uani 1 1 d . . . O1W O 0.1249(3) 0.03594(16) 0.12385(19) 0.0502(8) Uani 1 1 d . . . O1 O -0.8087(3) 0.16322(16) 0.3937(2) 0.0541(8) Uani 1 1 d . . . O2 O -0.8313(3) -0.09019(15) 0.3543(2) 0.0558(9) Uani 1 1 d . . . O3 O -0.4939(3) 0.04368(16) 0.25345(18) 0.0461(8) Uani 1 1 d . . . C1 C -0.7683(4) 0.0995(2) 0.3605(3) 0.0447(11) Uani 1 1 d . . . C2 C -0.8292(4) 0.0368(2) 0.3730(3) 0.0470(11) Uani 1 1 d . . . H2 H -0.9023 0.0345 0.4015 0.056 Uiso 1 1 calc R . . C3 C -0.7778(5) -0.0226(2) 0.3416(3) 0.0452(11) Uani 1 1 d . . . C4 C -0.6682(4) -0.0218(2) 0.3022(3) 0.0439(11) Uani 1 1 d . . . H4 H -0.6344 -0.0632 0.2827 0.053 Uiso 1 1 calc R . . C5 C -0.6090(4) 0.0426(2) 0.2921(3) 0.0424(10) Uani 1 1 d . . . C6 C -0.6581(4) 0.1041(2) 0.3213(3) 0.0417(10) Uani 1 1 d . . . H6 H -0.6175 0.1473 0.3145 0.050 Uiso 1 1 calc R . . O11 O -1.0182(4) 0.1545(2) 0.3362(3) 0.0908(14) Uani 1 1 d . . . N11 N -0.9817(3) 0.39775(18) 0.4560(2) 0.0414(9) Uani 1 1 d . . . C11 C -0.8688(5) 0.3636(2) 0.4756(3) 0.0517(12) Uani 1 1 d . . . H11 H -0.8011 0.3867 0.5072 0.062 Uiso 1 1 calc R . . C12 C -0.8482(4) 0.2954(2) 0.4509(3) 0.0504(12) Uani 1 1 d . . . H12 H -0.7678 0.2734 0.4657 0.061 Uiso 1 1 calc R . . C13 C -0.9462(5) 0.2603(2) 0.4045(3) 0.0471(11) Uani 1 1 d . . . C14 C -1.0642(5) 0.2960(3) 0.3829(3) 0.0582(13) Uani 1 1 d . . . H14 H -1.1333 0.2743 0.3512 0.070 Uiso 1 1 calc R . . C15 C -1.0757(5) 0.3644(2) 0.4097(3) 0.0529(12) Uani 1 1 d . . . H15 H -1.1538 0.3884 0.3944 0.063 Uiso 1 1 calc R . . C16 C -0.9317(5) 0.1872(3) 0.3736(3) 0.0551(13) Uani 1 1 d . . . O21 O -1.0261(5) -0.0645(2) 0.2901(3) 0.1110(18) Uani 1 1 d . . . N21 N -1.0444(6) -0.3234(2) 0.3519(3) 0.0743(14) Uani 1 1 d . . . C21 C -0.9268(7) -0.2990(3) 0.3720(4) 0.0854(19) Uani 1 1 d . . . H21 H -0.8629 -0.3312 0.3927 0.103 Uiso 1 1 calc R . . C22 C -0.8882(6) -0.2298(3) 0.3655(4) 0.0703(15) Uani 1 1 d . . . H22 H -0.8022 -0.2156 0.3818 0.084 Uiso 1 1 calc R . . C23 C -0.9827(5) -0.1824(3) 0.3337(3) 0.0548(12) Uani 1 1 d . . . C24 C -1.1083(6) -0.2066(3) 0.3118(4) 0.0702(15) Uani 1 1 d . . . H24 H -1.1741 -0.1759 0.2904 0.084 Uiso 1 1 calc R . . C25 C -1.1351(7) -0.2766(3) 0.3219(4) 0.0757(17) Uani 1 1 d . . . H25 H -1.2205 -0.2925 0.3072 0.091 Uiso 1 1 calc R . . C26 C -0.9506(6) -0.1057(3) 0.3227(3) 0.0573(13) Uani 1 1 d . . . O31 O -0.6085(3) 0.0757(3) 0.1376(2) 0.0836(13) Uani 1 1 d . . . N31 N -0.1625(3) 0.02422(18) 0.0579(2) 0.0379(8) Uani 1 1 d . . . C31 C -0.1600(4) 0.0146(2) 0.1372(3) 0.0469(11) Uani 1 1 d . . . H31 H -0.0818 -0.0005 0.1660 0.056 Uiso 1 1 calc R . . C32 C -0.2668(4) 0.0256(3) 0.1786(3) 0.0467(11) Uani 1 1 d . . . H32 H -0.2606 0.0181 0.2340 0.056 Uiso 1 1 calc R . . C33 C -0.3826(4) 0.0478(2) 0.1373(3) 0.0442(11) Uani 1 1 d . . . C34 C -0.3852(4) 0.0593(3) 0.0553(3) 0.0496(12) Uani 1 1 d . . . H34 H -0.4613 0.0758 0.0255 0.059 Uiso 1 1 calc R . . C35 C -0.2754(4) 0.0461(3) 0.0185(3) 0.0492(12) Uani 1 1 d . . . H35 H -0.2796 0.0528 -0.0370 0.059 Uiso 1 1 calc R . . C36 C -0.5073(4) 0.0580(3) 0.1745(3) 0.0496(12) Uani 1 1 d . . . C1A C -0.6019(11) -0.0800(6) -0.4804(6) 0.146(4) Uiso 1 1 d . . . C2A C -0.5514(9) -0.0113(5) -0.4849(5) 0.116(3) Uiso 1 1 d . . . C3A C -0.6171(12) 0.0539(6) -0.4420(7) 0.145(3) Uiso 1 1 d . . . C4A C -0.7235(12) 0.0376(7) -0.4095(7) 0.157(4) Uiso 1 1 d . . . H4A H -0.7727 0.0718 -0.3863 0.189 Uiso 1 1 calc R . . C5A C -0.7612(15) -0.0356(8) -0.4113(9) 0.192(5) Uiso 1 1 d . . . H5A H -0.8375 -0.0442 -0.3873 0.231 Uiso 1 1 calc R . . C6A C -0.7135(12) -0.0893(7) -0.4378(7) 0.161(4) Uiso 1 1 d . . . H6A H -0.7488 -0.1338 -0.4304 0.194 Uiso 1 1 calc R . . C7A C -0.5412(12) -0.1351(7) -0.5120(6) 0.157(4) Uiso 1 1 d . . . H7A H -0.5713 -0.1811 -0.5078 0.189 Uiso 1 1 calc R . . C8A C -0.5724(10) 0.1191(6) -0.4476(6) 0.132(3) Uiso 1 1 d . . . H8A H -0.6159 0.1558 -0.4247 0.158 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0264(4) 0.0318(4) 0.0541(5) 0.0073(3) 0.0179(3) 0.0022(3) P100 0.0799(12) 0.0973(14) 0.1020(14) -0.0186(11) 0.0121(11) 0.0252(11) F100 0.178(6) 0.311(11) 0.234(7) 0.092(7) 0.117(6) 0.093(7) F101 0.181(6) 0.210(7) 0.182(5) -0.063(5) -0.079(5) 0.073(5) F102 0.264(8) 0.125(4) 0.286(8) -0.022(5) 0.041(7) 0.120(5) F104 0.250(8) 0.230(8) 0.221(7) 0.037(6) 0.075(7) -0.106(7) F105 0.173(5) 0.152(5) 0.106(3) -0.010(3) -0.006(3) 0.054(4) F103 0.215(7) 0.147(5) 0.193(6) -0.055(4) -0.021(5) -0.004(5) O1W 0.0361(17) 0.0506(19) 0.065(2) -0.0073(15) 0.0117(15) -0.0028(14) O1 0.0440(19) 0.0388(17) 0.083(2) -0.0148(15) 0.0237(16) 0.0058(14) O2 0.050(2) 0.0342(17) 0.085(2) 0.0080(15) 0.0144(18) -0.0013(15) O3 0.0332(16) 0.058(2) 0.0498(18) 0.0029(14) 0.0175(13) 0.0079(14) C1 0.046(3) 0.034(2) 0.057(3) -0.0052(19) 0.014(2) 0.010(2) C2 0.041(3) 0.042(3) 0.064(3) 0.004(2) 0.030(2) 0.004(2) C3 0.046(3) 0.033(2) 0.059(3) 0.006(2) 0.018(2) 0.003(2) C4 0.045(3) 0.034(2) 0.056(3) -0.0053(19) 0.018(2) 0.0075(19) C5 0.031(2) 0.053(3) 0.044(2) 0.000(2) 0.0115(19) 0.006(2) C6 0.034(2) 0.038(2) 0.056(3) 0.0012(19) 0.014(2) 0.0001(19) O11 0.067(3) 0.059(2) 0.143(4) -0.044(3) -0.007(3) 0.016(2) N11 0.0291(19) 0.039(2) 0.059(2) -0.0049(17) 0.0191(17) 0.0001(16) C11 0.036(3) 0.043(3) 0.077(3) -0.009(2) 0.013(2) 0.006(2) C12 0.035(2) 0.047(3) 0.072(3) -0.005(2) 0.018(2) 0.010(2) C13 0.044(3) 0.037(2) 0.064(3) -0.008(2) 0.023(2) 0.003(2) C14 0.047(3) 0.047(3) 0.082(4) -0.021(2) 0.011(3) -0.004(2) C15 0.040(3) 0.040(3) 0.080(3) -0.010(2) 0.013(2) 0.008(2) C16 0.047(3) 0.040(3) 0.081(4) -0.011(2) 0.024(3) 0.004(2) O21 0.109(4) 0.050(2) 0.159(4) 0.033(3) -0.052(3) -0.016(2) N21 0.086(4) 0.050(3) 0.090(3) 0.004(2) 0.021(3) -0.019(3) C21 0.089(5) 0.042(3) 0.126(5) 0.022(3) 0.013(4) 0.007(3) C22 0.062(3) 0.044(3) 0.103(4) 0.011(3) 0.002(3) -0.004(3) C23 0.059(3) 0.044(3) 0.062(3) 0.004(2) 0.008(2) -0.005(2) C24 0.075(4) 0.054(3) 0.080(4) 0.006(3) 0.001(3) -0.004(3) C25 0.080(4) 0.056(4) 0.090(4) 0.001(3) 0.005(3) -0.023(3) C26 0.068(4) 0.043(3) 0.060(3) 0.016(2) 0.003(3) 0.002(3) O31 0.030(2) 0.153(4) 0.070(2) 0.029(2) 0.0150(17) 0.018(2) N31 0.0265(18) 0.0354(18) 0.054(2) 0.0066(16) 0.0166(16) 0.0003(14) C31 0.034(2) 0.053(3) 0.055(3) 0.013(2) 0.013(2) 0.007(2) C32 0.036(3) 0.058(3) 0.047(3) 0.009(2) 0.010(2) 0.007(2) C33 0.032(2) 0.048(3) 0.054(3) 0.002(2) 0.014(2) -0.0051(19) C34 0.021(2) 0.079(3) 0.049(3) 0.008(2) 0.0051(19) 0.006(2) C35 0.035(3) 0.060(3) 0.052(3) 0.004(2) 0.008(2) -0.002(2) C36 0.027(3) 0.059(3) 0.066(3) 0.003(2) 0.016(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N31 2.065(3) 3 ? Cu1 N31 2.065(3) . ? Cu1 N11 2.086(3) 4_665 ? Cu1 N11 2.086(3) 2_445 ? Cu1 O1W 2.401(3) . ? Cu1 O1W 2.401(3) 3 ? P100 F102 1.479(5) . ? P100 F104 1.511(7) . ? P100 F101 1.559(6) . ? P100 F103 1.568(6) . ? P100 F100 1.579(7) . ? P100 F105 1.604(5) . ? O1 C16 1.343(6) . ? O1 C1 1.408(5) . ? O2 C26 1.307(6) . ? O2 C3 1.416(5) . ? O3 C36 1.335(5) . ? O3 C5 1.404(5) . ? C1 C2 1.368(6) . ? C1 C6 1.367(6) . ? C2 C3 1.369(6) . ? C3 C4 1.361(6) . ? C4 C5 1.379(6) . ? C5 C6 1.378(6) . ? O11 C16 1.196(6) . ? N11 C15 1.323(6) . ? N11 C11 1.332(6) . ? N11 Cu1 2.086(3) 2_455 ? C11 C12 1.378(6) . ? C12 C13 1.368(7) . ? C13 C14 1.394(7) . ? C13 C16 1.490(6) . ? C14 C15 1.379(6) . ? O21 C26 1.186(6) . ? N21 C21 1.296(8) . ? N21 C25 1.338(8) . ? C21 C22 1.377(8) . ? C22 C23 1.381(7) . ? C23 C24 1.374(7) . ? C23 C26 1.503(7) . ? C24 C25 1.367(8) . ? O31 C36 1.191(5) . ? N31 C35 1.329(5) . ? N31 C31 1.332(5) . ? C31 C32 1.371(6) . ? C32 C33 1.367(6) . ? C33 C34 1.380(6) . ? C33 C36 1.492(6) . ? C34 C35 1.361(6) . ? C1A C7A 1.350(13) . ? C1A C2A 1.405(13) . ? C1A C6A 1.420(14) . ? C2A C2A 1.288(17) 3_454 ? C2A C3A 1.611(14) . ? C3A C4A 1.304(14) . ? C3A C8A 1.323(13) . ? C4A C5A 1.439(17) . ? C5A C6A 1.231(15) . ? C7A C8A 1.438(13) 3_454 ? C8A C7A 1.438(13) 3_454 ? 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 N31 180.0 3 . ? N31 Cu1 N11 86.17(13) 3 4_665 ? N31 Cu1 N11 93.83(13) . 4_665 ? N31 Cu1 N11 93.83(13) 3 2_445 ? N31 Cu1 N11 86.17(13) . 2_445 ? N11 Cu1 N11 180.00 4_665 2_445 ? N31 Cu1 O1W 94.96(12) 3 . ? N31 Cu1 O1W 85.04(12) . . ? N11 Cu1 O1W 88.80(13) 4_665 . ? N11 Cu1 O1W 91.20(13) 2_445 . ? N31 Cu1 O1W 85.04(12) 3 3 ? N31 Cu1 O1W 94.96(12) . 3 ? N11 Cu1 O1W 91.20(13) 4_665 3 ? N11 Cu1 O1W 88.80(13) 2_445 3 ? O1W Cu1 O1W 180.0 . 3 ? F102 P100 F104 106.8(5) . . ? F102 P100 F101 90.9(4) . . ? F104 P100 F101 86.8(5) . . ? F102 P100 F103 99.8(4) . . ? F104 P100 F103 88.4(5) . . ? F101 P100 F103 169.2(4) . . ? F102 P100 F100 86.6(4) . . ? F104 P100 F100 165.0(5) . . ? F101 P100 F100 100.2(5) . . ? F103 P100 F100 82.4(4) . . ? F102 P100 F105 167.9(5) . . ? F104 P100 F105 84.6(4) . . ? F101 P100 F105 85.3(3) . . ? F103 P100 F105 84.5(3) . . ? F100 P100 F105 82.8(4) . . ? C16 O1 C1 119.9(4) . . ? C26 O2 C3 120.1(4) . . ? C36 O3 C5 117.2(3) . . ? C2 C1 C6 122.8(4) . . ? C2 C1 O1 121.7(4) . . ? C6 C1 O1 115.3(4) . . ? C3 C2 C1 117.0(4) . . ? C4 C3 C2 123.1(4) . . ? C4 C3 O2 115.8(4) . . ? C2 C3 O2 120.9(4) . . ? C3 C4 C5 117.8(4) . . ? C6 C5 C4 121.5(4) . . ? C6 C5 O3 120.4(4) . . ? C4 C5 O3 118.1(4) . . ? C1 C6 C5 117.9(4) . . ? C15 N11 C11 117.7(4) . . ? C15 N11 Cu1 124.0(3) . 2_455 ? C11 N11 Cu1 118.3(3) . 2_455 ? N11 C11 C12 122.6(5) . . ? C13 C12 C11 119.8(4) . . ? C12 C13 C14 117.9(4) . . ? C12 C13 C16 123.5(4) . . ? C14 C13 C16 118.6(5) . . ? C15 C14 C13 118.3(5) . . ? N11 C15 C14 123.7(4) . . ? O11 C16 O1 124.9(4) . . ? O11 C16 C13 124.3(5) . . ? O1 C16 C13 110.8(4) . . ? C21 N21 C25 116.5(5) . . ? N21 C21 C22 125.7(6) . . ? C21 C22 C23 117.1(5) . . ? C24 C23 C22 118.5(5) . . ? C24 C23 C26 120.0(5) . . ? C22 C23 C26 121.4(5) . . ? C25 C24 C23 119.0(6) . . ? N21 C25 C24 123.2(6) . . ? O21 C26 O2 124.5(5) . . ? O21 C26 C23 123.5(5) . . ? O2 C26 C23 112.0(4) . . ? C35 N31 C31 116.9(4) . . ? C35 N31 Cu1 122.6(3) . . ? C31 N31 Cu1 120.4(3) . . ? N31 C31 C32 123.4(4) . . ? C33 C32 C31 119.1(4) . . ? C32 C33 C34 117.8(4) . . ? C32 C33 C36 124.2(4) . . ? C34 C33 C36 118.0(4) . . ? C35 C34 C33 119.5(4) . . ? N31 C35 C34 123.3(4) . . ? O31 C36 O3 123.6(4) . . ? O31 C36 C33 123.7(4) . . ? O3 C36 C33 112.7(4) . . ? C7A C1A C2A 120.4(11) . . ? C7A C1A C6A 122.0(12) . . ? C2A C1A C6A 117.5(11) . . ? C2A C2A C1A 130.5(13) 3_454 . ? C2A C2A C3A 108.6(11) 3_454 . ? C1A C2A C3A 120.8(9) . . ? C4A C3A C8A 124.1(12) . . ? C4A C3A C2A 114.3(11) . . ? C8A C3A C2A 121.2(11) . . ? C3A C4A C5A 117.0(12) . . ? C6A C5A C4A 133.4(15) . . ? C5A C6A C1A 116.8(14) . . ? C1A C7A C8A 116.8(12) . 3_454 ? C3A C8A C7A 122.2(12) . 3_454 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.063 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.092 data_3b _database_code_depnum_ccdc_archive 'CCDC 866720' #TrackingRef '- kbga-r1.cif' #'-sr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H48 Cu F12 N6 O16 P2' _chemical_formula_weight 1510.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.213(3) _cell_length_b 18.938(5) _cell_length_c 16.619(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.744(9) _cell_angle_gamma 90.00 _cell_volume 3192.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5928 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 25.50 _exptl_crystal_description blocks _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1538 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-2 CCD' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38489 _diffrn_reflns_av_R_equivalents 0.1711 _diffrn_reflns_av_sigmaI/netI 0.1360 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5928 _reflns_number_gt 2957 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1454P)^2^+3.3154P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5928 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1858 _refine_ls_R_factor_gt 0.1113 _refine_ls_wR_factor_ref 0.2936 _refine_ls_wR_factor_gt 0.2564 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.0000 0.0347(4) Uani 1 2 d S . . P100 P -0.4981(3) 0.16948(18) -0.1603(2) 0.0923(10) Uani 1 1 d . . . F100 F -0.5847(11) 0.1415(8) -0.0959(8) 0.251(7) Uani 1 1 d . . . F101 F -0.5739(10) 0.1349(6) -0.2350(6) 0.209(5) Uani 1 1 d . . . F102 F -0.5875(12) 0.2313(5) -0.1695(8) 0.235(6) Uani 1 1 d . . . F104 F -0.3949(13) 0.1881(7) -0.2128(8) 0.239(6) Uani 1 1 d . . . F105 F -0.4262(8) 0.0948(4) -0.1449(4) 0.139(3) Uani 1 1 d . . . F103 F -0.4017(11) 0.1946(6) -0.0866(7) 0.196(4) Uani 1 1 d . . . O1W O 0.1251(4) 0.0358(2) 0.1235(3) 0.0438(12) Uani 1 1 d . . . O1 O -0.8090(5) 0.1632(2) 0.3935(3) 0.0518(14) Uani 1 1 d . . . O2 O -0.8299(5) -0.0903(2) 0.3549(3) 0.0514(14) Uani 1 1 d . . . O3 O -0.4927(4) 0.0437(3) 0.2535(3) 0.0428(12) Uani 1 1 d . . . C1 C -0.7687(7) 0.0997(4) 0.3602(5) 0.0433(18) Uani 1 1 d . . . C2 C -0.8303(7) 0.0367(4) 0.3716(5) 0.0464(19) Uani 1 1 d . . . H2 H -0.9051 0.0347 0.3985 0.056 Uiso 1 1 calc R . . C3 C -0.7778(7) -0.0231(3) 0.3422(5) 0.0407(18) Uani 1 1 d . . . C4 C -0.6673(7) -0.0218(4) 0.3017(4) 0.0385(17) Uani 1 1 d . . . H4 H -0.6338 -0.0630 0.2816 0.046 Uiso 1 1 calc R . . C5 C -0.6089(6) 0.0418(4) 0.2924(4) 0.0393(18) Uani 1 1 d . . . C6 C -0.6571(6) 0.1042(4) 0.3216(4) 0.0405(18) Uani 1 1 d . . . H6 H -0.6156 0.1473 0.3153 0.049 Uiso 1 1 calc R . . O11 O -1.0197(6) 0.1539(3) 0.3360(5) 0.085(2) Uani 1 1 d . . . N11 N -0.9818(5) 0.3977(3) 0.4552(4) 0.0393(14) Uani 1 1 d . . . C11 C -0.8695(7) 0.3633(4) 0.4763(5) 0.0447(19) Uani 1 1 d . . . H11 H -0.8025 0.3863 0.5089 0.054 Uiso 1 1 calc R . . C12 C -0.8476(7) 0.2946(4) 0.4518(5) 0.0444(19) Uani 1 1 d . . . H12 H -0.7675 0.2724 0.4676 0.053 Uiso 1 1 calc R . . C13 C -0.9456(7) 0.2602(4) 0.4042(4) 0.0404(18) Uani 1 1 d . . . C14 C -1.0653(7) 0.2960(4) 0.3820(5) 0.053(2) Uani 1 1 d . . . H14 H -1.1348 0.2739 0.3505 0.064 Uiso 1 1 calc R . . C15 C -1.0770(7) 0.3644(4) 0.4081(5) 0.049(2) Uani 1 1 d . . . H15 H -1.1551 0.3885 0.3922 0.059 Uiso 1 1 calc R . . C16 C -0.9326(8) 0.1861(4) 0.3738(5) 0.049(2) Uani 1 1 d . . . O21 O -1.0276(7) -0.0650(4) 0.2900(5) 0.105(3) Uani 1 1 d . . . N21 N -1.0449(8) -0.3230(4) 0.3519(5) 0.069(2) Uani 1 1 d . . . C21 C -0.9253(11) -0.3001(5) 0.3712(7) 0.080(3) Uani 1 1 d . . . H21 H -0.8605 -0.3327 0.3895 0.097 Uiso 1 1 calc R . . C22 C -0.8882(9) -0.2289(4) 0.3661(6) 0.067(3) Uani 1 1 d . . . H22 H -0.8029 -0.2140 0.3838 0.080 Uiso 1 1 calc R . . C23 C -0.9831(8) -0.1824(4) 0.3340(5) 0.0468(19) Uani 1 1 d . . . C24 C -1.1096(9) -0.2071(4) 0.3115(6) 0.065(2) Uani 1 1 d . . . H24 H -1.1753 -0.1765 0.2891 0.077 Uiso 1 1 calc R . . C25 C -1.1364(10) -0.2750(5) 0.3222(6) 0.070(3) Uani 1 1 d . . . H25 H -1.2227 -0.2904 0.3085 0.084 Uiso 1 1 calc R . . C26 C -0.9498(9) -0.1061(4) 0.3227(5) 0.052(2) Uani 1 1 d . . . O31 O -0.6080(5) 0.0759(4) 0.1374(4) 0.083(2) Uani 1 1 d . . . N31 N -0.1620(5) 0.0243(3) 0.0576(4) 0.0356(14) Uani 1 1 d . . . C31 C -0.1608(7) 0.0143(4) 0.1376(5) 0.0435(19) Uani 1 1 d . . . H31 H -0.0828 -0.0011 0.1669 0.052 Uiso 1 1 calc R . . C32 C -0.2666(7) 0.0252(4) 0.1786(5) 0.0446(19) Uani 1 1 d . . . H32 H -0.2606 0.0168 0.2340 0.054 Uiso 1 1 calc R . . C33 C -0.3821(6) 0.0488(4) 0.1373(4) 0.0363(17) Uani 1 1 d . . . C34 C -0.3862(6) 0.0594(4) 0.0567(5) 0.049(2) Uani 1 1 d . . . H34 H -0.4631 0.0757 0.0271 0.058 Uiso 1 1 calc R . . C35 C -0.2753(7) 0.0458(4) 0.0182(5) 0.0426(18) Uani 1 1 d . . . H35 H -0.2808 0.0520 -0.0376 0.051 Uiso 1 1 calc R . . C36 C -0.5075(7) 0.0580(4) 0.1752(5) 0.0458(19) Uani 1 1 d . . . C100 C -0.4485(13) 0.0109(8) 0.4854(8) 0.113(4) Uiso 1 1 d . . . C101 C -0.5714(13) 0.1205(8) 0.5556(8) 0.120(4) Uiso 1 1 d . . . H101 H -0.6134 0.1564 0.5809 0.143 Uiso 1 1 calc R . . C102 C -0.3845(16) -0.0546(9) 0.4425(9) 0.132(5) Uiso 1 1 d . . . C103 C -0.3973(18) 0.0796(10) 0.4795(10) 0.150(6) Uiso 1 1 d . . . C104 C -0.4550(16) 0.1366(9) 0.5132(10) 0.145(5) Uiso 1 1 d . . . H104 H -0.4229 0.1823 0.5096 0.174 Uiso 1 1 calc R . . C105 C -0.2837(19) -0.0373(10) 0.4097(11) 0.164(7) Uiso 1 1 d . . . H105 H -0.2381 -0.0713 0.3838 0.197 Uiso 1 1 calc R . . C106 C -0.238(2) 0.0367(11) 0.4123(12) 0.180(7) Uiso 1 1 d . . . H106 H -0.1590 0.0440 0.3911 0.216 Uiso 1 1 calc R . . C107 C -0.2884(18) 0.0915(11) 0.4383(11) 0.169(7) Uiso 1 1 d . . . H107 H -0.2553 0.1365 0.4306 0.202 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0291(6) 0.0280(7) 0.0487(8) 0.0071(6) 0.0125(5) 0.0019(5) P100 0.081(2) 0.093(2) 0.102(2) -0.0180(19) 0.006(2) 0.0293(18) F100 0.178(10) 0.334(16) 0.272(13) 0.086(12) 0.153(10) 0.096(10) F101 0.201(9) 0.214(10) 0.180(9) -0.056(8) -0.114(8) 0.082(8) F102 0.280(13) 0.127(8) 0.300(14) 0.011(8) 0.049(11) 0.143(9) F104 0.244(12) 0.265(14) 0.218(12) 0.046(10) 0.074(10) -0.118(11) F105 0.169(7) 0.153(7) 0.089(5) -0.005(5) -0.003(5) 0.061(6) F103 0.208(10) 0.173(9) 0.196(10) -0.055(8) -0.030(8) -0.012(8) O1W 0.037(3) 0.043(3) 0.052(3) -0.005(2) 0.007(2) 0.000(2) O1 0.044(3) 0.032(3) 0.082(4) -0.013(3) 0.020(3) 0.006(2) O2 0.047(3) 0.030(3) 0.077(4) 0.007(3) 0.010(3) -0.001(2) O3 0.032(3) 0.051(3) 0.048(3) 0.006(3) 0.012(2) 0.007(2) C1 0.048(4) 0.026(4) 0.058(5) -0.004(3) 0.013(4) 0.006(3) C2 0.046(4) 0.039(5) 0.058(5) 0.000(4) 0.021(4) 0.008(4) C3 0.045(4) 0.022(4) 0.057(5) 0.007(3) 0.017(4) 0.006(3) C4 0.038(4) 0.032(4) 0.046(4) -0.008(3) 0.008(3) 0.006(3) C5 0.030(4) 0.044(5) 0.046(5) 0.012(4) 0.012(3) 0.006(3) C6 0.035(4) 0.034(4) 0.054(5) -0.001(3) 0.010(3) 0.000(3) O11 0.065(4) 0.052(4) 0.136(6) -0.042(4) -0.001(4) 0.013(3) N11 0.030(3) 0.039(4) 0.051(4) -0.002(3) 0.011(3) 0.003(3) C11 0.033(4) 0.037(4) 0.063(5) -0.011(4) 0.002(4) 0.003(3) C12 0.040(4) 0.040(4) 0.054(5) -0.005(4) 0.008(4) 0.010(3) C13 0.041(4) 0.035(4) 0.046(5) -0.006(3) 0.007(3) 0.001(3) C14 0.042(4) 0.041(5) 0.077(6) -0.017(4) 0.011(4) 0.003(4) C15 0.039(4) 0.035(4) 0.074(6) -0.007(4) 0.007(4) 0.007(3) C16 0.049(5) 0.029(4) 0.073(6) -0.005(4) 0.016(4) 0.006(4) O21 0.103(5) 0.058(4) 0.137(7) 0.034(4) -0.051(5) -0.016(4) N21 0.080(6) 0.044(5) 0.085(6) 0.003(4) 0.017(5) -0.020(4) C21 0.087(7) 0.031(5) 0.121(9) 0.017(5) 0.003(6) 0.009(5) C22 0.062(6) 0.034(5) 0.103(8) 0.016(5) 0.007(5) -0.005(4) C23 0.066(5) 0.031(4) 0.042(5) 0.006(3) 0.000(4) -0.008(4) C24 0.078(7) 0.040(5) 0.075(6) 0.007(4) 0.001(5) -0.007(4) C25 0.070(6) 0.064(7) 0.073(7) -0.003(5) -0.002(5) -0.013(5) C26 0.064(6) 0.039(5) 0.051(5) 0.012(4) -0.007(4) 0.003(4) O31 0.026(3) 0.159(7) 0.065(4) 0.035(4) 0.008(3) 0.020(4) N31 0.033(3) 0.026(3) 0.048(4) 0.003(3) 0.006(3) -0.002(2) C31 0.028(4) 0.049(5) 0.053(5) 0.012(4) 0.005(3) 0.008(3) C32 0.036(4) 0.056(5) 0.043(4) 0.007(4) 0.006(3) 0.004(3) C33 0.025(3) 0.049(5) 0.036(4) 0.000(3) 0.005(3) -0.001(3) C34 0.019(4) 0.071(6) 0.056(5) 0.011(4) 0.003(3) 0.008(3) C35 0.036(4) 0.051(5) 0.041(4) 0.004(4) 0.005(3) -0.003(3) C36 0.031(4) 0.056(5) 0.050(5) 0.002(4) 0.004(4) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N31 2.059(5) 3 ? Cu1 N31 2.059(5) . ? Cu1 N11 2.092(6) 4_665 ? Cu1 N11 2.092(6) 2_445 ? Cu1 O1W 2.385(5) . ? Cu1 O1W 2.385(5) 3 ? P100 F102 1.482(8) . ? P100 F104 1.487(10) . ? P100 F101 1.531(9) . ? P100 F103 1.553(9) . ? P100 F100 1.560(10) . ? P100 F105 1.600(7) . ? O1 C16 1.340(9) . ? O1 C1 1.406(8) . ? O2 C26 1.312(9) . ? O2 C3 1.405(8) . ? O3 C36 1.321(9) . ? O3 C5 1.418(7) . ? C1 C2 1.373(10) . ? C1 C6 1.375(9) . ? C2 C3 1.367(9) . ? C3 C4 1.380(9) . ? C4 C5 1.361(9) . ? C5 C6 1.389(10) . ? O11 C16 1.195(9) . ? N11 C15 1.333(9) . ? N11 C11 1.330(8) . ? N11 Cu1 2.092(6) 2_455 ? C11 C12 1.387(10) . ? C12 C13 1.367(10) . ? C13 C14 1.409(10) . ? C13 C16 1.501(10) . ? C14 C15 1.376(10) . ? O21 C26 1.196(9) . ? N21 C21 1.301(11) . ? N21 C25 1.354(11) . ? C21 C22 1.405(11) . ? C22 C23 1.371(11) . ? C23 C24 1.383(11) . ? C23 C26 1.503(10) . ? C24 C25 1.332(12) . ? O31 C36 1.188(8) . ? N31 C35 1.326(9) . ? N31 C31 1.342(9) . ? C31 C32 1.359(9) . ? C32 C33 1.369(10) . ? C33 C34 1.349(10) . ? C33 C36 1.502(9) . ? C34 C35 1.389(9) . ? C100 C100 1.28(2) 3_456 ? C100 C103 1.411(19) . ? C100 C102 1.607(19) . ? C101 C102 1.328(18) 3_456 ? C101 C104 1.483(18) . ? C102 C105 1.26(2) . ? C102 C101 1.328(18) 3_456 ? C103 C104 1.38(2) . ? C103 C107 1.39(2) . ? C105 C106 1.48(2) . ? C106 C107 1.26(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 N31 Cu1 N31 180.0 3 . ? N31 Cu1 N11 86.1(2) 3 4_665 ? N31 Cu1 N11 93.9(2) . 4_665 ? N31 Cu1 N11 93.9(2) 3 2_445 ? N31 Cu1 N11 86.1(2) . 2_445 ? N11 Cu1 N11 180.0 4_665 2_445 ? N31 Cu1 O1W 94.87(19) 3 . ? N31 Cu1 O1W 85.13(19) . . ? N11 Cu1 O1W 89.0(2) 4_665 . ? N11 Cu1 O1W 91.0(2) 2_445 . ? N31 Cu1 O1W 85.13(19) 3 3 ? N31 Cu1 O1W 94.87(19) . 3 ? N11 Cu1 O1W 91.0(2) 4_665 3 ? N11 Cu1 O1W 89.0(2) 2_445 3 ? O1W Cu1 O1W 180.0 . 3 ? F102 P100 F104 102.9(8) . . ? F102 P100 F101 90.4(6) . . ? F104 P100 F101 87.2(7) . . ? F102 P100 F103 99.5(7) . . ? F104 P100 F103 87.9(7) . . ? F101 P100 F103 169.7(6) . . ? F102 P100 F100 86.9(7) . . ? F104 P100 F100 169.0(7) . . ? F101 P100 F100 97.9(8) . . ? F103 P100 F100 85.5(7) . . ? F102 P100 F105 168.6(7) . . ? F104 P100 F105 87.7(6) . . ? F101 P100 F105 86.0(5) . . ? F103 P100 F105 84.7(5) . . ? F100 P100 F105 82.9(6) . . ? C16 O1 C1 119.5(6) . . ? C26 O2 C3 119.7(6) . . ? C36 O3 C5 116.7(5) . . ? C2 C1 C6 122.5(6) . . ? C2 C1 O1 121.9(6) . . ? C6 C1 O1 115.3(6) . . ? C1 C2 C3 117.7(7) . . ? C4 C3 C2 122.5(7) . . ? C4 C3 O2 115.8(6) . . ? C2 C3 O2 121.6(6) . . ? C5 C4 C3 117.7(6) . . ? C4 C5 C6 122.4(6) . . ? C4 C5 O3 118.4(6) . . ? C6 C5 O3 119.1(6) . . ? C1 C6 C5 117.1(6) . . ? C15 N11 C11 118.1(6) . . ? C15 N11 Cu1 123.9(5) . 2_455 ? C11 N11 Cu1 118.0(5) . 2_455 ? N11 C11 C12 123.0(7) . . ? C13 C12 C11 119.0(7) . . ? C12 C13 C14 118.4(7) . . ? C12 C13 C16 123.6(7) . . ? C14 C13 C16 118.0(7) . . ? C15 C14 C13 118.4(7) . . ? N11 C15 C14 123.1(7) . . ? O11 C16 O1 125.8(7) . . ? O11 C16 C13 124.4(7) . . ? O1 C16 C13 109.8(7) . . ? C21 N21 C25 117.0(8) . . ? N21 C21 C22 123.9(9) . . ? C23 C22 C21 117.1(8) . . ? C22 C23 C24 118.9(7) . . ? C22 C23 C26 120.4(7) . . ? C24 C23 C26 120.6(7) . . ? C25 C24 C23 119.4(9) . . ? C24 C25 N21 123.5(9) . . ? O21 C26 O2 125.2(8) . . ? O21 C26 C23 122.3(8) . . ? O2 C26 C23 112.5(7) . . ? C35 N31 C31 116.1(6) . . ? C35 N31 Cu1 122.7(5) . . ? C31 N31 Cu1 121.0(5) . . ? N31 C31 C32 124.0(7) . . ? C31 C32 C33 119.2(7) . . ? C34 C33 C32 118.1(6) . . ? C34 C33 C36 118.1(6) . . ? C32 C33 C36 123.7(7) . . ? C33 C34 C35 119.9(6) . . ? N31 C35 C34 122.7(7) . . ? O31 C36 O3 124.8(7) . . ? O31 C36 C33 122.6(7) . . ? O3 C36 C33 112.6(6) . . ? C100 C100 C103 131(2) 3_456 . ? C100 C100 C102 108.4(17) 3_456 . ? C103 C100 C102 120.5(13) . . ? C102 C101 C104 119.8(15) 3_456 . ? C105 C102 C101 123.4(18) . 3_456 ? C105 C102 C100 112.7(16) . . ? C101 C102 C100 123.9(15) 3_456 . ? C104 C103 C107 118.5(19) . . ? C104 C103 C100 120.9(17) . . ? C107 C103 C100 120.6(17) . . ? C103 C104 C101 115.9(16) . . ? C102 C105 C106 120(2) . . ? C107 C106 C105 131(2) . . ? C106 C107 C103 115(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.023 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.102 data_4a _database_code_depnum_ccdc_archive 'CCDC 866721' #TrackingRef '- kbga-r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H48 Cd F12 N6 O16 P2' _chemical_formula_weight 1559.42 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.484(3) _cell_length_b 19.181(5) _cell_length_c 16.381(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.553(8) _cell_angle_gamma 90.00 _cell_volume 3248.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5657 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.0 _exptl_crystal_description Blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-2 CCD' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38016 _diffrn_reflns_av_R_equivalents 0.1673 _diffrn_reflns_av_sigmaI/netI 0.1280 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5667 _reflns_number_gt 2850 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.021 0.406 0.012 7 1 ' ' 2 0.021 0.094 0.512 7 1 ' ' 3 0.438 0.698 0.339 52 7 ' ' 4 0.438 0.802 0.839 52 7 ' ' 5 0.562 0.199 0.161 52 7 ' ' 6 0.562 0.301 0.661 52 7 ' ' 7 0.979 0.906 0.488 7 1 ' ' 8 0.979 0.594 0.988 7 1 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1454P)^2^+3.3154P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5667 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1635 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2370 _refine_ls_wR_factor_gt 0.1824 _refine_ls_goodness_of_fit_ref 0.851 _refine_ls_restrained_S_all 0.851 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.0427(3) Uani 1 2 d S . . P100 P -0.4951(4) 0.3163(2) 0.3326(3) 0.1183(15) Uani 1 1 d . . . F100 F -0.5861(14) 0.3297(14) 0.3896(13) 0.386(13) Uani 1 1 d . . . F101 F -0.5712(11) 0.3466(9) 0.2578(8) 0.261(8) Uani 1 1 d . . . F102 F -0.557(2) 0.2519(7) 0.3218(10) 0.417(16) Uani 1 1 d . . . F104 F -0.3852(13) 0.3075(7) 0.2805(9) 0.228(6) Uani 1 1 d . . . F105 F -0.4399(11) 0.3910(5) 0.3512(5) 0.184(4) Uani 1 1 d . . . F103 F -0.3963(12) 0.2943(7) 0.4093(9) 0.235(6) Uani 1 1 d . . . O1W O 0.1138(5) 0.0404(3) 0.1234(3) 0.0541(15) Uani 1 1 d . . . O1 O -0.8126(5) 0.1555(3) 0.3844(4) 0.0576(16) Uani 1 1 d . . . O2 O -0.8284(5) -0.0961(3) 0.3453(4) 0.0575(16) Uani 1 1 d . . . O3 O -0.5041(5) 0.0384(3) 0.2514(4) 0.0526(15) Uani 1 1 d . . . C1 C -0.7737(8) 0.0919(4) 0.3535(5) 0.051(2) Uani 1 1 d . . . C2 C -0.8323(8) 0.0300(4) 0.3642(5) 0.050(2) Uani 1 1 d . . . H2 H -0.9041 0.0274 0.3907 0.060 Uiso 1 1 calc R . . C3 C -0.7797(8) -0.0289(4) 0.3337(5) 0.046(2) Uani 1 1 d . . . C4 C -0.6729(8) -0.0271(4) 0.2943(5) 0.051(2) Uani 1 1 d . . . H4 H -0.6410 -0.0673 0.2732 0.061 Uiso 1 1 calc R . . C5 C -0.6168(7) 0.0361(5) 0.2877(5) 0.049(2) Uani 1 1 d . . . C6 C -0.6649(7) 0.0976(4) 0.3157(5) 0.048(2) Uani 1 1 d . . . H6 H -0.6262 0.1405 0.3093 0.058 Uiso 1 1 calc R . . O11 O -1.0224(7) 0.1419(4) 0.3339(6) 0.099(3) Uani 1 1 d . . . N11 N -0.9803(7) 0.3859(3) 0.4468(4) 0.0510(18) Uani 1 1 d . . . C11 C -0.8672(8) 0.3543(5) 0.4614(6) 0.061(2) Uani 1 1 d . . . H11 H -0.7970 0.3791 0.4893 0.073 Uiso 1 1 calc R . . C12 C -0.8463(9) 0.2866(4) 0.4380(6) 0.064(3) Uani 1 1 d . . . H12 H -0.7642 0.2670 0.4499 0.076 Uiso 1 1 calc R . . C13 C -0.9483(8) 0.2488(4) 0.3970(6) 0.052(2) Uani 1 1 d . . . C14 C -1.0688(8) 0.2806(4) 0.3799(6) 0.063(3) Uani 1 1 d . . . H14 H -1.1406 0.2568 0.3526 0.076 Uiso 1 1 calc R . . C15 C -1.0783(9) 0.3496(4) 0.4051(6) 0.059(2) Uani 1 1 d . . . H15 H -1.1581 0.3717 0.3920 0.071 Uiso 1 1 calc R . . C16 C -0.9343(9) 0.1764(5) 0.3691(6) 0.057(2) Uani 1 1 d . . . O21 O -1.0331(7) -0.0684(4) 0.2939(6) 0.103(3) Uani 1 1 d . . . N21 N -1.0438(10) -0.3245(5) 0.3523(6) 0.088(3) Uani 1 1 d . . . C21 C -0.9229(12) -0.3007(6) 0.3707(8) 0.100(4) Uani 1 1 d . . . H21 H -0.8587 -0.3324 0.3916 0.120 Uiso 1 1 calc R . . C22 C -0.8854(11) -0.2314(5) 0.3610(7) 0.084(3) Uani 1 1 d . . . H22 H -0.7992 -0.2177 0.3728 0.100 Uiso 1 1 calc R . . C23 C -0.9803(9) -0.1857(5) 0.3339(6) 0.055(2) Uani 1 1 d . . . C24 C -1.1077(10) -0.2073(5) 0.3139(6) 0.072(3) Uani 1 1 d . . . H24 H -1.1729 -0.1761 0.2932 0.087 Uiso 1 1 calc R . . C25 C -1.1347(11) -0.2771(6) 0.3260(7) 0.078(3) Uani 1 1 d . . . H25 H -1.2206 -0.2916 0.3152 0.093 Uiso 1 1 calc R . . C26 C -0.9529(10) -0.1115(5) 0.3214(6) 0.063(3) Uani 1 1 d . . . O31 O -0.6218(6) 0.0681(5) 0.1305(4) 0.091(2) Uani 1 1 d . . . N31 N -0.1829(6) 0.0266(3) 0.0596(5) 0.0467(17) Uani 1 1 d . . . C31 C -0.1810(8) 0.0117(5) 0.1391(7) 0.067(3) Uani 1 1 d . . . H31 H -0.1045 -0.0055 0.1692 0.080 Uiso 1 1 calc R . . C32 C -0.2854(8) 0.0203(5) 0.1800(6) 0.063(3) Uani 1 1 d . . . H32 H -0.2790 0.0094 0.2358 0.076 Uiso 1 1 calc R . . C33 C -0.3993(7) 0.0453(4) 0.1353(6) 0.050(2) Uani 1 1 d . . . C34 C -0.4005(8) 0.0624(5) 0.0560(6) 0.065(3) Uani 1 1 d . . . H34 H -0.4739 0.0825 0.0253 0.078 Uiso 1 1 calc R . . C35 C -0.2921(8) 0.0502(5) 0.0197(6) 0.063(3) Uani 1 1 d . . . H35 H -0.2979 0.0594 -0.0365 0.076 Uiso 1 1 calc R . . C36 C -0.5215(8) 0.0515(5) 0.1714(6) 0.054(2) Uani 1 1 d . . . C105 C -0.4429(11) 0.0041(8) 0.4826(7) 0.086(3) Uani 1 1 d . . . C106 C -0.3816(15) -0.0523(11) 0.4508(9) 0.110(5) Uani 1 1 d . . . C104 C -0.3915(14) 0.0742(9) 0.4779(9) 0.105(4) Uani 1 1 d . . . C108 C -0.4581(18) 0.1279(8) 0.5108(9) 0.116(5) Uani 1 1 d . . . H108 H -0.4265 0.1729 0.5067 0.140 Uiso 1 1 calc R . . C102 C -0.2216(17) 0.0282(16) 0.4113(11) 0.163(10) Uani 1 1 d . . . H102 H -0.1467 0.0349 0.3888 0.196 Uiso 1 1 calc R . . C107 C -0.4357(19) -0.1213(11) 0.4519(10) 0.129(6) Uani 1 1 d . . . H107 H -0.4001 -0.1593 0.4284 0.155 Uiso 1 1 calc R . . C103 C -0.2824(18) 0.0831(14) 0.4415(10) 0.163(9) Uani 1 1 d . . . H103 H -0.2497 0.1278 0.4375 0.195 Uiso 1 1 calc R . . C101 C -0.2759(18) -0.0404(12) 0.4150(10) 0.141(7) Uani 1 1 d . . . H101 H -0.2373 -0.0777 0.3922 0.169 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0351(4) 0.0326(4) 0.0650(6) 0.0058(5) 0.0224(4) 0.0000(4) P100 0.083(2) 0.122(3) 0.143(4) 0.048(3) 0.001(3) -0.046(2) F100 0.167(12) 0.60(4) 0.44(3) 0.06(3) 0.201(16) -0.081(17) F101 0.170(10) 0.38(2) 0.197(11) 0.093(12) -0.084(9) -0.052(11) F102 0.75(4) 0.164(12) 0.303(19) 0.017(11) -0.01(2) -0.31(2) F104 0.216(13) 0.213(13) 0.270(15) -0.041(11) 0.081(11) 0.060(10) F105 0.260(12) 0.152(8) 0.130(7) 0.001(6) 0.005(8) -0.081(8) F103 0.212(13) 0.215(13) 0.260(14) 0.108(11) -0.013(11) -0.006(10) O1W 0.043(3) 0.053(4) 0.068(4) -0.004(3) 0.014(3) 0.006(3) O1 0.046(3) 0.045(4) 0.088(5) -0.013(3) 0.029(3) 0.007(3) O2 0.045(3) 0.034(3) 0.098(5) 0.007(3) 0.025(3) -0.002(3) O3 0.039(3) 0.062(4) 0.061(4) 0.003(3) 0.020(3) 0.006(3) C1 0.041(5) 0.045(5) 0.072(6) 0.001(4) 0.023(4) 0.008(4) C2 0.047(5) 0.045(5) 0.066(6) 0.003(4) 0.032(4) 0.003(4) C3 0.054(5) 0.035(4) 0.053(5) -0.001(4) 0.018(4) 0.000(4) C4 0.049(5) 0.038(4) 0.068(6) -0.008(4) 0.020(5) 0.004(4) C5 0.035(4) 0.052(5) 0.063(6) 0.002(4) 0.016(4) -0.006(4) C6 0.037(4) 0.035(5) 0.079(6) -0.008(4) 0.025(4) 0.001(3) O11 0.056(4) 0.056(5) 0.183(8) -0.054(5) 0.013(5) 0.014(4) N11 0.050(4) 0.040(4) 0.066(5) -0.011(4) 0.019(4) -0.003(3) C11 0.039(5) 0.053(6) 0.095(7) -0.008(5) 0.024(5) 0.004(4) C12 0.046(5) 0.046(6) 0.103(8) -0.009(5) 0.024(5) 0.009(4) C13 0.040(5) 0.038(5) 0.082(6) -0.013(4) 0.024(4) 0.007(4) C14 0.039(5) 0.048(6) 0.107(8) -0.018(5) 0.027(5) 0.002(4) C15 0.056(6) 0.039(5) 0.083(7) -0.009(5) 0.016(5) 0.014(4) C16 0.048(5) 0.051(6) 0.075(7) -0.006(5) 0.018(5) 0.001(5) O21 0.072(5) 0.061(5) 0.168(8) 0.030(5) -0.008(5) -0.013(4) N21 0.100(8) 0.059(6) 0.103(7) 0.012(5) 0.013(6) -0.020(6) C21 0.089(9) 0.050(7) 0.152(12) 0.037(7) -0.005(8) -0.004(6) C22 0.067(7) 0.045(6) 0.134(10) 0.015(6) 0.001(7) -0.009(5) C23 0.059(6) 0.044(5) 0.060(6) 0.004(5) 0.004(5) -0.008(5) C24 0.075(7) 0.054(6) 0.087(8) -0.001(5) 0.010(6) -0.009(5) C25 0.080(7) 0.063(7) 0.088(8) 0.002(6) 0.005(6) -0.026(6) C26 0.072(7) 0.034(5) 0.081(7) 0.021(5) 0.009(5) 0.007(5) O31 0.041(4) 0.160(8) 0.076(5) 0.027(5) 0.024(4) 0.026(4) N31 0.031(4) 0.048(4) 0.065(5) 0.009(3) 0.020(3) 0.005(3) C31 0.035(4) 0.083(8) 0.087(7) 0.019(6) 0.021(4) 0.007(4) C32 0.049(5) 0.081(7) 0.065(6) 0.011(5) 0.022(5) 0.010(5) C33 0.035(5) 0.049(5) 0.070(6) 0.001(4) 0.024(4) 0.004(4) C34 0.042(5) 0.093(8) 0.066(7) 0.012(5) 0.023(5) 0.008(5) C35 0.048(6) 0.089(7) 0.058(6) 0.005(5) 0.024(5) -0.006(5) C36 0.039(5) 0.064(6) 0.061(7) 0.003(5) 0.015(5) 0.013(4) C105 0.071(7) 0.110(10) 0.075(7) -0.008(8) 0.004(6) -0.001(9) C106 0.093(11) 0.153(16) 0.079(9) 0.012(10) 0.000(8) 0.037(11) C104 0.084(10) 0.132(14) 0.090(10) 0.020(9) -0.009(8) -0.006(9) C108 0.149(15) 0.078(10) 0.113(12) 0.002(8) -0.006(11) 0.005(10) C102 0.081(12) 0.31(3) 0.098(13) 0.010(16) 0.025(9) -0.020(16) C107 0.129(14) 0.142(17) 0.113(13) -0.002(11) 0.011(10) 0.026(12) C103 0.107(14) 0.28(3) 0.097(13) 0.044(15) 0.018(10) -0.041(16) C101 0.109(14) 0.22(2) 0.097(12) -0.042(13) 0.031(10) 0.013(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 Cd1 O1W 2.304(6) 3 ? Cd1 O1W 2.304(6) . ? Cd1 N31 2.347(6) 3 ? Cd1 N31 2.347(6) . ? Cd1 N11 2.377(6) 2_445 ? Cd1 N11 2.377(6) 4_665 ? P100 F102 1.392(9) . ? P100 F100 1.464(15) . ? P100 F101 1.468(11) . ? P100 F104 1.553(12) . ? P100 F103 1.548(12) . ? P100 F105 1.556(10) . ? O1 C16 1.321(10) . ? O1 C1 1.407(9) . ? O2 C26 1.332(11) . ? O2 C3 1.412(9) . ? O3 C36 1.316(10) . ? O3 C5 1.410(9) . ? C1 C2 1.361(11) . ? C1 C6 1.391(10) . ? C2 C3 1.386(11) . ? C3 C4 1.383(11) . ? C4 C5 1.359(11) . ? C5 C6 1.391(11) . ? O11 C16 1.202(10) . ? N11 C11 1.318(10) . ? N11 C15 1.332(10) . ? N11 Cd1 2.377(6) 2_455 ? C11 C12 1.381(12) . ? C12 C13 1.373(12) . ? C13 C14 1.388(11) . ? C13 C16 1.478(12) . ? C14 C15 1.395(11) . ? O21 C26 1.212(10) . ? N21 C21 1.334(13) . ? N21 C25 1.336(13) . ? C21 C22 1.402(13) . ? C22 C23 1.344(13) . ? C23 C24 1.384(12) . ? C23 C26 1.475(12) . ? C24 C25 1.389(13) . ? O31 C36 1.193(10) . ? N31 C35 1.303(10) . ? N31 C31 1.330(11) . ? C31 C32 1.385(12) . ? C32 C33 1.379(12) . ? C33 C34 1.337(11) . ? C33 C36 1.502(11) . ? C34 C35 1.387(11) . ? C105 C106 1.403(19) . ? C105 C105 1.42(2) 3_456 ? C105 C104 1.456(18) . ? C106 C101 1.36(2) . ? C106 C107 1.44(2) . ? C104 C103 1.38(2) . ? C104 C108 1.401(19) . ? C108 C107 1.36(2) 3_456 ? C102 C103 1.37(3) . ? C102 C101 1.44(3) . ? C107 C108 1.36(2) 3_456 ? 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 O1W Cd1 O1W 180.0 3 . ? O1W Cd1 N31 84.4(2) 3 3 ? O1W Cd1 N31 95.6(2) . 3 ? O1W Cd1 N31 95.6(2) 3 . ? O1W Cd1 N31 84.4(2) . . ? N31 Cd1 N31 180.0 3 . ? O1W Cd1 N11 87.0(2) 3 2_445 ? O1W Cd1 N11 93.0(2) . 2_445 ? N31 Cd1 N11 94.6(2) 3 2_445 ? N31 Cd1 N11 85.4(2) . 2_445 ? O1W Cd1 N11 93.0(2) 3 4_665 ? O1W Cd1 N11 87.0(2) . 4_665 ? N31 Cd1 N11 85.4(2) 3 4_665 ? N31 Cd1 N11 94.6(2) . 4_665 ? N11 Cd1 N11 180.0 2_445 4_665 ? F102 P100 F100 84.2(12) . . ? F102 P100 F101 93.9(10) . . ? F100 P100 F101 98.1(11) . . ? F102 P100 F104 101.9(13) . . ? F100 P100 F104 172.4(11) . . ? F101 P100 F104 86.2(8) . . ? F102 P100 F103 95.5(10) . . ? F100 P100 F103 87.2(10) . . ? F101 P100 F103 169.6(7) . . ? F104 P100 F103 87.6(8) . . ? F102 P100 F105 172.6(13) . . ? F100 P100 F105 88.5(11) . . ? F101 P100 F105 86.1(7) . . ? F104 P100 F105 85.5(7) . . ? F103 P100 F105 85.1(6) . . ? C16 O1 C1 121.5(7) . . ? C26 O2 C3 121.4(7) . . ? C36 O3 C5 116.0(6) . . ? C2 C1 C6 123.2(7) . . ? C2 C1 O1 123.1(7) . . ? C6 C1 O1 113.6(7) . . ? C1 C2 C3 116.7(7) . . ? C2 C3 C4 123.3(8) . . ? C2 C3 O2 121.5(7) . . ? C4 C3 O2 115.1(7) . . ? C5 C4 C3 117.0(7) . . ? C4 C5 C6 123.0(7) . . ? C4 C5 O3 117.8(7) . . ? C6 C5 O3 119.1(7) . . ? C5 C6 C1 116.7(7) . . ? C11 N11 C15 116.5(7) . . ? C11 N11 Cd1 119.2(6) . 2_455 ? C15 N11 Cd1 124.2(5) . 2_455 ? N11 C11 C12 124.2(9) . . ? C13 C12 C11 119.1(8) . . ? C12 C13 C14 118.4(8) . . ? C12 C13 C16 122.6(8) . . ? C14 C13 C16 119.0(8) . . ? C13 C14 C15 117.7(8) . . ? N11 C15 C14 124.1(8) . . ? O11 C16 O1 124.4(9) . . ? O11 C16 C13 123.9(8) . . ? O1 C16 C13 111.6(8) . . ? C21 N21 C25 116.1(9) . . ? N21 C21 C22 125.0(10) . . ? C23 C22 C21 116.7(10) . . ? C22 C23 C24 121.0(9) . . ? C22 C23 C26 121.6(9) . . ? C24 C23 C26 117.3(9) . . ? C23 C24 C25 117.8(10) . . ? N21 C25 C24 123.3(10) . . ? O21 C26 O2 123.0(8) . . ? O21 C26 C23 124.9(9) . . ? O2 C26 C23 112.1(8) . . ? C35 N31 C31 115.8(7) . . ? C35 N31 Cd1 125.3(6) . . ? C31 N31 Cd1 118.7(5) . . ? N31 C31 C32 124.3(8) . . ? C33 C32 C31 118.0(9) . . ? C34 C33 C32 117.9(8) . . ? C34 C33 C36 119.5(8) . . ? C32 C33 C36 122.6(8) . . ? C33 C34 C35 119.9(9) . . ? N31 C35 C34 124.0(9) . . ? O31 C36 O3 125.0(8) . . ? O31 C36 C33 122.0(9) . . ? O3 C36 C33 113.0(7) . . ? C106 C105 C105 122.2(18) . 3_456 ? C106 C105 C104 119.8(14) . . ? C105 C105 C104 118.0(17) 3_456 . ? C101 C106 C105 119.2(18) . . ? C101 C106 C107 120.8(19) . . ? C105 C106 C107 119.9(16) . . ? C103 C104 C108 125(2) . . ? C103 C104 C105 118.4(17) . . ? C108 C104 C105 116.5(14) . . ? C107 C108 C104 126.9(16) 3_456 . ? C103 C102 C101 118.6(18) . . ? C108 C107 C106 116.4(16) 3_456 . ? C102 C103 C104 122(2) . . ? C106 C101 C102 122.0(19) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.592 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.089