# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_test _audit_creation_date 2013-06-26T13:50:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C82 H152 Cr7 F8 N O32 Zn' _chemical_formula_weight 2245.42 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system tetragonal _space_group_name_H-M_alt 'I 4' _space_group_name_Hall 'I 4' _space_group_IT_number 79 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 19.8766(5) _cell_length_b 19.8766(5) _cell_length_c 16.0127(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6326.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2354 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1666 _exptl_absorpt_correction_T_max 0.2850 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Prospector' _diffrn_measurement_method 'phi and omega scans;1 degree slicing' _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_unetI/netI 0.1024 _diffrn_reflns_number 9104 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 68.12 _diffrn_reflns_theta_full 68.12 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_point_group_measured_fraction_ful 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.986 _reflns_number_total 4355 _reflns_number_gt 3738 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX SERVER' _computing_cell_refinement 'Bruker APEX SERVER' _computing_data_reduction 'Bruker APEX SERVER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal contains solvent accessible voids (263 \%A^3^). However the descrete location of the solvent molecules could not be determined. The large number of restraints are a result of idealising the highly disordered ^t^butyl moieties of the bridging pivalate groups. ; _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^)+(0.1717P)^2^+194.7443P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4355 _refine_ls_number_parameters 304 _refine_ls_number_restraints 202 _refine_ls_R_factor_all 0.1539 _refine_ls_R_factor_gt 0.1434 _refine_ls_wR_factor_ref 0.3776 _refine_ls_wR_factor_gt 0.3702 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(10) _refine_diff_density_max 1.823 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.207 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.49733(12) 0.72097(11) 0.71563(19) 0.0305(6) Uani 0.13 1 d P . . C102 C 0.5 0.5 0.780(3) 0.061(11) Uani 1 4 d SDU . . H10A H 0.5158 0.5232 0.8288 0.092 Uiso 0.25 1 calc PR . . H10B H 0.5242 0.4585 0.7739 0.092 Uiso 0.25 1 calc PR . . H10C H 0.4528 0.4907 0.7858 0.092 Uiso 0.25 1 calc PR . . C101 C 0.5 0.5 0.633(3) 0.051(10) Uani 1 4 d SDU . . H10D H 0.5157 0.5231 0.5845 0.076 Uiso 0.25 1 calc PR . . H10E H 0.4528 0.4907 0.6278 0.076 Uiso 0.25 1 calc PR . . H10F H 0.5242 0.4585 0.6397 0.076 Uiso 0.25 1 calc PR . . Zn2 Zn 0.34149(11) 0.65484(11) 0.6899(2) 0.0305(6) Uani 0.13 1 d P . . C1 C 0.4194(9) 0.7025(7) 0.5486(13) 0.040(4) Uani 1 1 d DU . . C2 C 0.4368(9) 0.7067(9) 0.4543(13) 0.053(4) Uani 1 1 d DU . . C3 C 0.3773(10) 0.6899(10) 0.4052(11) 0.059(5) Uani 1 1 d DU . . H3A H 0.3427 0.7226 0.4156 0.089 Uiso 1 1 calc R . . H3B H 0.3614 0.6461 0.4208 0.089 Uiso 1 1 calc R . . H3C H 0.3886 0.6902 0.3469 0.089 Uiso 1 1 calc R . . C4 C 0.4943(10) 0.6589(13) 0.4400(14) 0.085(8) Uani 1 1 d DU . . H4A H 0.532 0.6722 0.4737 0.127 Uiso 1 1 calc R . . H4B H 0.5069 0.6598 0.3821 0.127 Uiso 1 1 calc R . . H4C H 0.4807 0.6142 0.455 0.127 Uiso 1 1 calc R . . C5 C 0.4594(13) 0.7783(11) 0.4380(16) 0.102(9) Uani 1 1 d DU . . H5A H 0.4225 0.8084 0.4472 0.153 Uiso 1 1 calc R . . H5B H 0.4746 0.7823 0.3814 0.153 Uiso 1 1 calc R . . H5C H 0.4956 0.7895 0.4753 0.153 Uiso 1 1 calc R . . C6 C 0.3695(12) 0.7969(9) 0.7384(13) 0.050(5) Uani 1 1 d U . . C7 C 0.3427(12) 0.8643(10) 0.7593(14) 0.067(5) Uani 1 1 d DU . . C8 C 0.2840(19) 0.854(2) 0.812(3) 0.163(14) Uani 1 1 d DU . . H8A H 0.298 0.8382 0.8655 0.244 Uiso 1 1 calc R . . H8B H 0.2547 0.822 0.7862 0.244 Uiso 1 1 calc R . . H8C H 0.2607 0.8963 0.8183 0.244 Uiso 1 1 calc R . . C9 C 0.3220(17) 0.8952(10) 0.6760(17) 0.107(10) Uani 1 1 d DU . . H9A H 0.3612 0.9012 0.6416 0.16 Uiso 1 1 calc R . . H9B H 0.301 0.938 0.6856 0.16 Uiso 1 1 calc R . . H9C H 0.2909 0.8658 0.6482 0.16 Uiso 1 1 calc R . . C10 C 0.3930(16) 0.9102(15) 0.803(2) 0.122(11) Uani 1 1 d DU . . H10G H 0.4095 0.8887 0.8521 0.183 Uiso 1 1 calc R . . H10H H 0.3713 0.9517 0.8173 0.183 Uiso 1 1 calc R . . H10I H 0.4298 0.9193 0.7655 0.183 Uiso 1 1 calc R . . C11 C 0.5881(10) 0.6986(10) 0.8459(12) 0.045(4) Uani 1 1 d U . . C12 C 0.6036(11) 0.6979(11) 0.9459(13) 0.067(5) Uani 1 1 d DU . . C13 C 0.5447(10) 0.7230(15) 0.9909(15) 0.083(8) Uani 1 1 d DU . . H13A H 0.5073 0.6935 0.9813 0.125 Uiso 1 1 calc R . . H13B H 0.5338 0.7673 0.9713 0.125 Uiso 1 1 calc R . . H13C H 0.5544 0.7247 1.0496 0.125 Uiso 1 1 calc R . . C14 C 0.6660(13) 0.7381(17) 0.962(2) 0.109(10) Uani 1 1 d DU . . H14A H 0.7028 0.719 0.9312 0.163 Uiso 1 1 calc R . . H14B H 0.6762 0.7373 1.0205 0.163 Uiso 1 1 calc R . . H14C H 0.659 0.7837 0.9442 0.163 Uiso 1 1 calc R . . C15 C 0.6134(19) 0.6244(13) 0.969(2) 0.116(11) Uani 1 1 d DU . . H15A H 0.5728 0.5999 0.9581 0.174 Uiso 1 1 calc R . . H15B H 0.6239 0.6212 1.0278 0.174 Uiso 1 1 calc R . . H15C H 0.6496 0.6058 0.9372 0.174 Uiso 1 1 calc R . . C16 C 0.6193(11) 0.8009(8) 0.6593(13) 0.048(4) Uani 1 1 d U . . C17 C 0.6449(10) 0.8698(9) 0.6368(14) 0.063(5) Uani 1 1 d DU . . C18 C 0.6967(16) 0.8860(12) 0.696(2) 0.122(11) Uani 1 1 d DU . . H18A H 0.7297 0.8508 0.697 0.183 Uiso 1 1 calc R . . H18B H 0.6771 0.8904 0.7508 0.183 Uiso 1 1 calc R . . H18C H 0.7178 0.9277 0.6808 0.183 Uiso 1 1 calc R . . C19 C 0.5904(15) 0.9220(13) 0.633(3) 0.115(11) Uani 1 1 d DU . . H19A H 0.559 0.9104 0.5896 0.173 Uiso 1 1 calc R . . H19B H 0.6099 0.9652 0.6209 0.173 Uiso 1 1 calc R . . H19C H 0.5674 0.9239 0.6855 0.173 Uiso 1 1 calc R . . C20 C 0.675(2) 0.8610(16) 0.5499(17) 0.133(12) Uani 1 1 d DU . . H20A H 0.71 0.8276 0.5519 0.199 Uiso 1 1 calc R . . H20B H 0.6938 0.903 0.5314 0.199 Uiso 1 1 calc R . . H20C H 0.6407 0.8469 0.5117 0.199 Uiso 1 1 calc R . . O1 O 0.3732(6) 0.6678(7) 0.5735(9) 0.045(3) Uani 1 1 d . . . O2 O 0.4638(6) 0.7337(6) 0.5952(8) 0.041(3) Uani 1 1 d . . . O3 O 0.3318(8) 0.7503(6) 0.7079(12) 0.066(5) Uani 1 1 d . . . O4 O 0.4327(6) 0.7866(7) 0.7579(10) 0.050(4) Uani 1 1 d . . . O5 O 0.5294(7) 0.7095(7) 0.8264(9) 0.046(3) Uani 1 1 d . . . O6 O 0.3084(6) 0.6388(6) 0.8029(8) 0.040(3) Uani 1 1 d . . . O7 O 0.5592(5) 0.7945(5) 0.6909(10) 0.046(3) Uani 1 1 d . . . O8 O 0.2490(5) 0.6554(6) 0.6453(9) 0.043(3) Uani 1 1 d . . . F1 F 0.4329(4) 0.6494(4) 0.7315(6) 0.0265(18) Uani 1 1 d . . . F2 F 0.5576(4) 0.6528(4) 0.6698(6) 0.0293(19) Uani 1 1 d . . . Cr1 Cr 0.49733(12) 0.72097(11) 0.71563(19) 0.0305(6) Uani 0.88 1 d P . . Cr2 Cr 0.34149(11) 0.65484(11) 0.6899(2) 0.0305(6) Uani 0.88 1 d P . . N1 N 0.511(4) 0.542(2) 0.706(2) 0.067(12) Uani 0.25 1 d PDU . . H1A H 0.4822 0.5769 0.7063 0.08 Uiso 0.25 1 calc PR . . H1B H 0.5533 0.5582 0.7063 0.08 Uiso 0.25 1 calc PR . . 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 0.0360(12) 0.0206(10) 0.0350(12) 0.0004(10) 0.0038(12) 0.0027(9) C102 0.059(15) 0.059(15) 0.07(3) 0 0 0 C101 0.038(11) 0.038(11) 0.08(3) 0 0 0 Zn2 0.0273(11) 0.0268(11) 0.0373(13) 0.0057(11) 0.0085(11) 0.0079(9) C1 0.060(10) 0.010(6) 0.050(9) 0.006(6) -0.015(8) -0.007(7) C2 0.065(10) 0.051(9) 0.044(9) 0.001(8) -0.004(8) -0.010(8) C3 0.070(13) 0.077(14) 0.031(10) 0.009(10) -0.002(9) -0.003(11) C4 0.062(13) 0.14(2) 0.048(13) -0.010(15) -0.018(11) 0.026(14) C5 0.12(2) 0.109(18) 0.072(17) 0.035(16) 0.001(16) -0.072(16) C6 0.073(11) 0.038(9) 0.040(9) 0.007(7) 0.017(9) 0.031(9) C7 0.087(11) 0.038(8) 0.077(11) -0.013(8) 0.000(9) 0.043(8) C8 0.19(3) 0.13(3) 0.17(3) -0.02(2) 0.08(3) 0.05(2) C9 0.17(2) 0.033(10) 0.12(2) -0.006(13) -0.066(19) 0.042(13) C10 0.16(2) 0.080(17) 0.13(3) -0.035(18) -0.04(2) 0.059(16) C11 0.052(10) 0.047(9) 0.036(9) -0.012(8) 0.009(8) -0.005(8) C12 0.081(12) 0.082(12) 0.038(10) -0.003(10) 0.017(9) -0.009(10) C13 0.057(13) 0.15(2) 0.045(12) -0.037(15) 0.006(10) -0.033(13) C14 0.080(17) 0.18(3) 0.069(18) -0.02(2) -0.003(15) -0.019(19) C15 0.17(3) 0.106(19) 0.067(18) 0.008(16) -0.02(2) 0.047(19) C16 0.083(12) 0.021(7) 0.040(9) -0.005(7) 0.002(9) -0.024(8) C17 0.081(12) 0.029(8) 0.080(12) 0.011(9) 0.003(10) -0.035(8) C18 0.18(2) 0.054(12) 0.13(2) 0.051(16) -0.07(2) -0.063(15) C19 0.15(2) 0.050(13) 0.15(3) 0.016(17) -0.03(2) -0.013(14) C20 0.21(3) 0.084(19) 0.10(2) 0.032(17) 0.05(2) -0.06(2) O1 0.030(6) 0.064(8) 0.042(7) 0.011(6) 0.002(5) -0.014(6) O2 0.035(6) 0.047(7) 0.040(7) 0.001(6) -0.003(5) -0.006(5) O3 0.078(9) 0.033(6) 0.088(13) -0.016(8) -0.005(10) 0.026(6) O4 0.044(7) 0.049(7) 0.057(8) -0.023(7) -0.001(6) 0.032(6) O5 0.040(7) 0.052(8) 0.047(8) -0.014(6) 0.005(6) -0.003(6) O6 0.042(7) 0.045(7) 0.034(6) 0.000(6) 0.008(5) -0.007(5) O7 0.039(6) 0.028(5) 0.070(9) -0.014(6) 0.022(7) 0.005(4) O8 0.018(5) 0.042(6) 0.068(9) 0.024(6) 0.010(5) 0.013(5) F1 0.022(4) 0.019(3) 0.039(5) 0.004(4) 0.002(4) -0.004(3) F2 0.032(4) 0.017(3) 0.039(5) 0.005(3) 0.008(4) -0.005(3) Cr1 0.0360(12) 0.0206(10) 0.0350(12) 0.0004(10) 0.0038(12) 0.0027(9) Cr2 0.0273(11) 0.0268(11) 0.0373(13) 0.0057(11) 0.0085(11) 0.0079(9) N1 0.07(2) 0.05(2) 0.09(3) 0.016(19) 0.01(2) 0.02(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O5 1.899(15) . ? Zn1 F1 1.931(7) . ? Zn1 O4 1.951(11) . ? Zn1 O7 1.952(11) . ? Zn1 F2 1.951(8) . ? Zn1 O2 2.056(13) . ? C102 N1 1.46(2) . ? C102 H10A 0.96 . ? C102 H10B 0.96 . ? C102 H10C 0.96 . ? C101 N1 1.45(2) . ? C101 H10D 0.96 . ? C101 H10E 0.96 . ? C101 H10F 0.96 . ? Zn2 O6 1.952(13) . ? Zn2 O3 1.929(12) . ? Zn2 F1 1.938(8) . ? Zn2 F2 1.963(8) 3_655 ? Zn2 O8 1.972(12) . ? Zn2 O1 1.984(14) . ? C1 O1 1.22(2) . ? C1 O2 1.31(2) . ? C1 C2 1.55(3) . ? C2 C3 1.46(2) . ? C2 C4 1.50(2) . ? C2 C5 1.51(2) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? C6 O3 1.29(3) . ? C6 O4 1.31(3) . ? C6 C7 1.48(2) . ? C7 C8 1.45(2) . ? C7 C9 1.53(2) . ? C7 C10 1.52(2) . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 H10G 0.96 . ? C10 H10H 0.96 . ? C10 H10I 0.96 . ? C11 O6 1.23(2) 4_565 ? C11 O5 1.23(2) . ? C11 C12 1.63(3) . ? C12 C13 1.46(2) . ? C12 C14 1.50(2) . ? C12 C15 1.52(2) . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C16 O8 1.24(2) 4_565 ? C16 O7 1.30(2) . ? C16 C17 1.51(2) . ? C17 C18 1.44(2) . ? C17 C19 1.50(2) . ? C17 C20 1.53(2) . ? C18 H18A 0.96 . ? C18 H18B 0.96 . ? C18 H18C 0.96 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? O6 C11 1.23(2) 3_655 ? O8 C16 1.24(2) 3_655 ? F2 Cr2 1.963(8) 4_565 ? F2 Zn2 1.963(8) 4_565 ? N1 H1A 0.9 . ? N1 H1B 0.9 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 F1 90.6(5) . . ? O5 Zn1 O4 88.7(6) . . ? F1 Zn1 O4 90.6(5) . . ? O5 Zn1 O7 93.9(6) . . ? F1 Zn1 O7 175.4(6) . . ? O4 Zn1 O7 89.1(5) . . ? O5 Zn1 F2 93.6(5) . . ? F1 Zn1 F2 86.8(3) . . ? O4 Zn1 F2 176.6(5) . . ? O7 Zn1 F2 93.3(4) . . ? O5 Zn1 O2 179.3(5) . . ? F1 Zn1 O2 89.9(4) . . ? O4 Zn1 O2 91.7(6) . . ? O7 Zn1 O2 85.5(6) . . ? F2 Zn1 O2 86.0(5) . . ? N1 C102 H10A 109.5 . . ? N1 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? N1 C102 H10C 109.4 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? N1 C101 H10D 109.5 . . ? N1 C101 H10E 109.4 . . ? H10D C101 H10E 109.5 . . ? N1 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? O6 Zn2 O3 89.4(7) . . ? O6 Zn2 F1 89.3(5) . . ? O3 Zn2 F1 95.6(5) . . ? O6 Zn2 F2 90.6(5) . 3_655 ? O3 Zn2 F2 177.5(5) . 3_655 ? F1 Zn2 F2 87.0(3) . 3_655 ? O6 Zn2 O8 91.3(5) . . ? O3 Zn2 O8 87.5(6) . . ? F1 Zn2 O8 176.9(4) . . ? F2 Zn2 O8 90.0(4) 3_655 . ? O6 Zn2 O1 177.7(5) . . ? O3 Zn2 O1 92.5(7) . . ? F1 Zn2 O1 91.9(5) . . ? F2 Zn2 O1 87.5(5) 3_655 . ? O8 Zn2 O1 87.5(5) . . ? O1 C1 O2 126.2(19) . . ? O1 C1 C2 121.2(15) . . ? O2 C1 C2 112.2(15) . . ? C3 C2 C4 113.0(14) . . ? C3 C2 C5 111.3(14) . . ? C4 C2 C5 110.0(14) . . ? C3 C2 C1 109.4(14) . . ? C4 C2 C1 106.5(14) . . ? C5 C2 C1 106.5(14) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 122.5(14) . . ? O3 C6 C7 121.7(19) . . ? O4 C6 C7 116(2) . . ? C8 C7 C6 107(2) . . ? C8 C7 C9 110(2) . . ? C6 C7 C9 105.3(16) . . ? C8 C7 C10 110(2) . . ? C6 C7 C10 114.1(19) . . ? C9 C7 C10 109.4(18) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10G 109.5 . . ? C7 C10 H10H 109.5 . . ? H10G C10 H10H 109.5 . . ? C7 C10 H10I 109.5 . . ? H10G C10 H10I 109.5 . . ? H10H C10 H10I 109.5 . . ? O6 C11 O5 131(2) 4_565 . ? O6 C11 C12 113.2(18) 4_565 . ? O5 C11 C12 115.5(17) . . ? C13 C12 C14 113.4(18) . . ? C13 C12 C15 107.9(19) . . ? C14 C12 C15 111(2) . . ? C13 C12 C11 109.2(19) . . ? C14 C12 C11 108.7(19) . . ? C15 C12 C11 106.0(19) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O7 121.4(14) 4_565 . ? O8 C16 C17 119.2(18) 4_565 . ? O7 C16 C17 119.4(17) . . ? C18 C17 C19 112.9(19) . . ? C18 C17 C20 110(2) . . ? C19 C17 C20 109(2) . . ? C18 C17 C16 106.7(17) . . ? C19 C17 C16 113.2(19) . . ? C20 C17 C16 104.3(18) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1 O1 Zn2 128.4(13) . . ? C1 O2 Zn1 133.9(11) . . ? C6 O3 Zn2 134.9(12) . . ? C6 O4 Zn1 130.7(12) . . ? C11 O5 Zn1 125.3(13) . . ? C11 O6 Zn2 133.8(13) 3_655 . ? C16 O7 Zn1 136.8(10) . . ? C16 O8 Zn2 132.5(12) 3_655 . ? Zn2 F1 Zn1 122.3(4) . . ? Cr2 F2 Zn2 0.00(19) 4_565 4_565 ? Cr2 F2 Zn1 120.2(4) 4_565 . ? Zn2 F2 Zn1 120.2(4) 4_565 . ? C101 N1 C102 107(4) . . ? C101 N1 H1A 110.2 . . ? C102 N1 H1A 110.2 . . ? C101 N1 H1B 110.2 . . ? C102 N1 H1B 110.2 . . ? H1A N1 H1B 108.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C102 H10B F1 0.96 2.41 3.346(13) 166.6 2_665 C102 H10C F1 0.96 2.49 3.346(13) 148.4 3_655 C101 H10E F2 0.96 2.57 3.298(11) 132.3 3_655 N1 H1A F1 0.9 1.79 2.67(6) 165.9 . N1 H1B F1 0.9 1.96 2.82(7) 160.4 4_565 # END of CIF _database_code_depnum_ccdc_archive 'CCDC 954609' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_xrepw99_0m _audit_creation_date 2013-06-26T11:36:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C82 H152 F8 Ga7 N O32 Zn' _chemical_formula_weight 2369.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system tetragonal _space_group_name_H-M_alt 'I 4' _space_group_name_Hall 'I 4' _space_group_IT_number 79 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' 'y, -x, z' '-x, -y, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' _cell_length_a 19.8454(5) _cell_length_b 19.8454(5) _cell_length_c 15.8931(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6259.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5219 _exptl_absorpt_correction_T_max 0.6356 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Prospector' _diffrn_measurement_method 'phi and omega scans;1 degree slicing' _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_unetI/netI 0.0727 _diffrn_reflns_number 14378 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 68.24 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_ful 0.904 _diffrn_reflns_point_group_measured_fraction_max 0.902 _reflns_number_total 5191 _reflns_number_gt 4870 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX SERVER' _computing_cell_refinement 'Bruker APEX SERVER' _computing_data_reduction 'Bruker APEX SERVER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal contains solvent accessible voids (263 \%A^3^). However the descrete location of the solvent molecules could not be determined. The large number of restraints are a result of idealising the highly disordered ^t^butyl moieties of the bridging pivalate groups. ; _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^)+(0.0991P)^2^+96.6479P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00102(12) _refine_ls_number_reflns 5191 _refine_ls_number_parameters 361 _refine_ls_number_restraints 373 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.2638 _refine_ls_wR_factor_gt 0.2611 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(10) _refine_diff_density_max 1.507 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.193 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ga1 Ga 0.65261(7) 0.34102(7) 0.52635(11) 0.0420(4) Uani 0.88 1 d P . . Ga2 Ga 0.71971(6) 0.49574(7) 0.49744(11) 0.0411(4) Uani 0.88 1 d P . . Zn1 Zn 0.65261(7) 0.34102(7) 0.52635(11) 0.0420(4) Uani 0.13 1 d P . . Zn2 Zn 0.71971(6) 0.49574(7) 0.49744(11) 0.0411(4) Uani 0.13 1 d P . . F1 F 0.6478(3) 0.4316(3) 0.4816(5) 0.0429(16) Uani 1 1 d . . . F2 F 0.5556(3) 0.3478(3) 0.5425(4) 0.0434(16) Uani 1 1 d . . . O1 O 0.6529(5) 0.2494(4) 0.5696(7) 0.055(2) Uani 1 1 d . . . O2 O 0.5582(5) 0.2069(4) 0.5173(7) 0.057(2) Uani 1 1 d . . . O3 O 0.7332(5) 0.4624(5) 0.6153(6) 0.053(2) Uani 1 1 d . . . O4 O 0.6648(5) 0.3755(4) 0.6405(6) 0.053(2) Uani 1 1 d . . . O5 O 0.7482(4) 0.3320(5) 0.5047(8) 0.067(3) Uani 1 1 d . . . O6 O 0.7844(5) 0.4315(5) 0.4512(6) 0.057(2) Uani 1 1 d . . . O7 O 0.5289(5) 0.2962(5) 0.3838(7) 0.058(2) Uani 1 1 d . . . O8 O 0.6389(4) 0.3084(5) 0.4100(6) 0.051(2) Uani 1 1 d . . . C1 C 0.6155(8) 0.2005(6) 0.5517(8) 0.052(3) Uani 1 1 d U A . C2 C 0.6417(7) 0.1291(6) 0.5695(9) 0.063(4) Uani 1 1 d DU . . C3 C 0.6980(16) 0.1132(13) 0.517(2) 0.109(12) Uani 0.61(3) 1 d PDU A 1 H3A H 0.7348 0.1448 0.5283 0.164 Uiso 0.61(3) 1 calc PR A 1 H3B H 0.6846 0.1166 0.4578 0.164 Uiso 0.61(3) 1 calc PR A 1 H3C H 0.7131 0.0671 0.5289 0.164 Uiso 0.61(3) 1 calc PR A 1 C4 C 0.6554(16) 0.1313(14) 0.6622(13) 0.081(8) Uani 0.61(3) 1 d PDU A 1 H4A H 0.6139 0.1433 0.6921 0.122 Uiso 0.61(3) 1 calc PR A 1 H4B H 0.6902 0.1651 0.6738 0.122 Uiso 0.61(3) 1 calc PR A 1 H4C H 0.6709 0.087 0.6812 0.122 Uiso 0.61(3) 1 calc PR A 1 C5 C 0.5827(15) 0.0777(15) 0.555(3) 0.111(12) Uani 0.61(3) 1 d PDU A 1 H5A H 0.5449 0.089 0.5916 0.166 Uiso 0.61(3) 1 calc PR A 1 H5B H 0.5984 0.032 0.567 0.166 Uiso 0.61(3) 1 calc PR A 1 H5C H 0.568 0.0802 0.4957 0.166 Uiso 0.61(3) 1 calc PR A 1 C3B C 0.5961(19) 0.085(2) 0.614(3) 0.079(10) Uani 0.39(3) 1 d PDU A 2 H3B1 H 0.6177 0.0409 0.6224 0.119 Uiso 0.39(3) 1 calc PR A 2 H3B2 H 0.5549 0.0789 0.5808 0.119 Uiso 0.39(3) 1 calc PR A 2 H3B3 H 0.5848 0.1045 0.6687 0.119 Uiso 0.39(3) 1 calc PR A 2 C4B C 0.7122(14) 0.131(2) 0.603(3) 0.098(13) Uani 0.39(3) 1 d PDU A 2 H4B1 H 0.7382 0.165 0.571 0.147 Uiso 0.39(3) 1 calc PR A 2 H4B2 H 0.7333 0.0871 0.5961 0.147 Uiso 0.39(3) 1 calc PR A 2 H4B3 H 0.7114 0.1438 0.6622 0.147 Uiso 0.39(3) 1 calc PR A 2 C5B C 0.648(2) 0.0963(18) 0.4781(16) 0.071(9) Uani 0.39(3) 1 d PDU A 2 H5B1 H 0.6792 0.123 0.4439 0.107 Uiso 0.39(3) 1 calc PR A 2 H5B2 H 0.6036 0.0957 0.4511 0.107 Uiso 0.39(3) 1 calc PR A 2 H5B3 H 0.665 0.0501 0.4831 0.107 Uiso 0.39(3) 1 calc PR A 2 C6 C 0.5884(7) 0.3031(7) 0.3619(9) 0.054(3) Uani 1 1 d U . . C7 C 0.6053(8) 0.3019(8) 0.2650(10) 0.074(4) Uani 1 1 d DU . . C8 C 0.5468(9) 0.2803(11) 0.2156(12) 0.091(6) Uani 1 1 d DU . . H8A H 0.5098 0.3124 0.2235 0.136 Uiso 1 1 calc R . . H8B H 0.5324 0.2355 0.2343 0.136 Uiso 1 1 calc R . . H8C H 0.559 0.2785 0.1559 0.136 Uiso 1 1 calc R . . C9 C 0.6665(10) 0.2618(15) 0.2515(16) 0.145(10) Uani 1 1 d DU . . H9A H 0.6572 0.2145 0.2649 0.218 Uiso 1 1 calc R . . H9B H 0.7026 0.2785 0.2879 0.218 Uiso 1 1 calc R . . H9C H 0.6804 0.2655 0.1925 0.218 Uiso 1 1 calc R . . C10 C 0.6161(18) 0.3781(11) 0.2426(17) 0.171(12) Uani 1 1 d DU . . H10A H 0.5743 0.403 0.2531 0.257 Uiso 1 1 calc R . . H10B H 0.6285 0.3821 0.1832 0.257 Uiso 1 1 calc R . . H10C H 0.6523 0.3966 0.2776 0.257 Uiso 1 1 calc R . . C11 C 0.7949(7) 0.3684(8) 0.4740(9) 0.058(4) Uani 1 1 d U B . C12 C 0.8609(7) 0.3376(8) 0.4538(10) 0.082(5) Uani 1 1 d DU . . C13 C 0.8950(10) 0.3212(17) 0.5326(16) 0.096(9) Uani 0.59(2) 1 d PDU B 1 H13A H 0.9011 0.3624 0.5658 0.144 Uiso 0.59(2) 1 calc PR B 1 H13B H 0.9392 0.3014 0.5204 0.144 Uiso 0.59(2) 1 calc PR B 1 H13C H 0.8678 0.289 0.5645 0.144 Uiso 0.59(2) 1 calc PR B 1 C14 C 0.851(2) 0.2802(17) 0.395(3) 0.143(14) Uani 0.59(2) 1 d PDU B 1 H14A H 0.8281 0.2959 0.3445 0.215 Uiso 0.59(2) 1 calc PR B 1 H14B H 0.8238 0.2455 0.4229 0.215 Uiso 0.59(2) 1 calc PR B 1 H14C H 0.8951 0.2613 0.3801 0.215 Uiso 0.59(2) 1 calc PR B 1 C15 C 0.9072(12) 0.3912(14) 0.4087(19) 0.088(8) Uani 0.59(2) 1 d PDU B 1 H15A H 0.9122 0.4308 0.4449 0.131 Uiso 0.59(2) 1 calc PR B 1 H15B H 0.8865 0.4046 0.3553 0.131 Uiso 0.59(2) 1 calc PR B 1 H15C H 0.9516 0.3714 0.3978 0.131 Uiso 0.59(2) 1 calc PR B 1 C13B C 0.9146(17) 0.379(2) 0.483(3) 0.111(13) Uani 0.41(2) 1 d PDU B 2 H13D H 0.9578 0.3589 0.4673 0.166 Uiso 0.41(2) 1 calc PR B 2 H13E H 0.912 0.3834 0.5444 0.166 Uiso 0.41(2) 1 calc PR B 2 H13F H 0.9109 0.424 0.4574 0.166 Uiso 0.41(2) 1 calc PR B 2 C14B C 0.8610(17) 0.2640(12) 0.475(2) 0.084(11) Uani 0.41(2) 1 d PDU B 2 H14D H 0.8198 0.243 0.4535 0.126 Uiso 0.41(2) 1 calc PR B 2 H14E H 0.8627 0.2585 0.5365 0.126 Uiso 0.41(2) 1 calc PR B 2 H14F H 0.9004 0.2423 0.4498 0.126 Uiso 0.41(2) 1 calc PR B 2 C15B C 0.858(2) 0.340(2) 0.3544(14) 0.097(12) Uani 0.41(2) 1 d PDU B 2 H15D H 0.8229 0.309 0.3344 0.145 Uiso 0.41(2) 1 calc PR B 2 H15E H 0.9018 0.3254 0.3315 0.145 Uiso 0.41(2) 1 calc PR B 2 H15F H 0.8483 0.3856 0.3356 0.145 Uiso 0.41(2) 1 calc PR B 2 C16 C 0.6997(5) 0.4220(6) 0.6623(9) 0.046(3) Uani 1 1 d DU . . C17 C 0.7044(7) 0.4422(7) 0.7570(9) 0.069(4) Uani 1 1 d DU . . C18 C 0.6533(11) 0.4929(8) 0.7752(11) 0.128(9) Uani 1 1 d DU . . H18A H 0.6087 0.4752 0.7608 0.192 Uiso 1 1 calc R . . H18B H 0.6623 0.5335 0.7418 0.192 Uiso 1 1 calc R . . H18C H 0.6546 0.5043 0.8352 0.192 Uiso 1 1 calc R . . C19 C 0.7742(10) 0.4634(11) 0.7772(12) 0.139(10) Uani 1 1 d DU . . H19A H 0.8054 0.4265 0.7645 0.209 Uiso 1 1 calc R . . H19B H 0.7773 0.4748 0.8371 0.209 Uiso 1 1 calc R . . H19C H 0.7861 0.503 0.7434 0.209 Uiso 1 1 calc R . . C20 C 0.6886(7) 0.3769(8) 0.8080(9) 0.070(4) Uani 1 1 d DU . . H20A H 0.7228 0.3426 0.7955 0.104 Uiso 1 1 calc R . . H20B H 0.644 0.3599 0.7922 0.104 Uiso 1 1 calc R . . H20C H 0.6892 0.3872 0.8683 0.104 Uiso 1 1 calc R . . C101 C 0.5 0.5 0.583(2) 0.056(7) Uani 1 4 d SD . . H101 H 0.512 0.4723 0.6321 0.084 Uiso 0.25 1 calc PR . . H102 H 0.4515 0.5094 0.5842 0.084 Uiso 0.25 1 calc PR . . H103 H 0.525 0.5425 0.5854 0.084 Uiso 0.25 1 calc PR . . C102 C 0.5 0.5 0.430(2) 0.064(8) Uani 1 4 d SD . . H104 H 0.5117 0.472 0.3811 0.096 Uiso 0.25 1 calc PR . . H105 H 0.5254 0.5423 0.4274 0.096 Uiso 0.25 1 calc PR . . H106 H 0.4516 0.5098 0.4291 0.096 Uiso 0.25 1 calc PR . . N1 N 0.517(6) 0.464(3) 0.5068(18) 0.12(3) Uani 0.25 1 d PDU . . H1A H 0.4947 0.4235 0.5068 0.142 Uiso 0.25 1 calc PR . . H1B H 0.5624 0.4554 0.5068 0.142 Uiso 0.25 1 calc PR . . 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 Ga1 0.0381(7) 0.0372(7) 0.0506(8) -0.0104(6) -0.0089(7) 0.0098(5) Ga2 0.0264(6) 0.0488(8) 0.0482(8) -0.0069(7) 0.0001(6) 0.0022(5) Zn1 0.0381(7) 0.0372(7) 0.0506(8) -0.0104(6) -0.0089(7) 0.0098(5) Zn2 0.0264(6) 0.0488(8) 0.0482(8) -0.0069(7) 0.0001(6) 0.0022(5) F1 0.031(3) 0.034(3) 0.064(5) -0.011(3) -0.003(3) 0.000(2) F2 0.049(4) 0.031(3) 0.050(4) -0.008(3) -0.009(3) 0.013(3) O1 0.049(5) 0.039(5) 0.079(7) -0.010(4) -0.026(5) 0.015(4) O2 0.059(5) 0.044(4) 0.068(7) -0.014(4) -0.012(5) -0.012(4) O3 0.051(5) 0.052(5) 0.055(5) -0.004(4) -0.009(4) -0.004(4) O4 0.066(6) 0.035(4) 0.059(6) 0.000(4) -0.015(5) -0.001(4) O5 0.038(4) 0.073(6) 0.089(8) -0.013(6) -0.005(5) 0.015(4) O6 0.050(5) 0.056(6) 0.063(6) -0.008(4) 0.008(4) 0.028(4) O7 0.056(6) 0.055(6) 0.064(6) -0.013(5) -0.010(5) 0.001(4) O8 0.048(5) 0.054(5) 0.051(5) -0.017(4) -0.005(4) -0.001(4) C1 0.070(8) 0.029(5) 0.055(8) -0.018(5) -0.003(6) 0.021(5) C2 0.068(8) 0.034(6) 0.087(9) 0.004(6) -0.015(7) 0.023(6) C3 0.15(2) 0.054(14) 0.13(2) 0.055(16) 0.07(2) 0.046(14) C4 0.09(2) 0.064(16) 0.092(14) 0.016(13) -0.010(14) 0.018(14) C5 0.12(2) 0.064(15) 0.14(3) 0.01(2) -0.03(2) -0.025(16) C3B 0.092(17) 0.068(15) 0.079(16) 0.014(14) -0.009(14) 0.017(13) C4B 0.078(17) 0.09(3) 0.12(3) 0.01(2) -0.03(2) 0.038(17) C5B 0.086(17) 0.039(14) 0.089(14) -0.009(12) 0.005(13) 0.035(13) C6 0.052(8) 0.053(8) 0.057(7) -0.006(6) 0.001(6) 0.010(6) C7 0.075(10) 0.092(11) 0.056(8) -0.016(8) -0.010(7) -0.006(8) C8 0.079(11) 0.133(17) 0.060(10) -0.025(11) -0.017(9) 0.022(10) C9 0.068(12) 0.29(3) 0.082(15) -0.039(19) -0.003(11) 0.031(17) C10 0.28(4) 0.148(17) 0.082(17) 0.032(16) 0.01(2) -0.095(18) C11 0.039(6) 0.084(10) 0.050(7) -0.006(6) -0.002(5) 0.040(7) C12 0.041(7) 0.100(11) 0.106(11) 0.005(9) 0.010(7) 0.051(7) C13 0.017(9) 0.13(2) 0.14(2) 0.055(17) -0.007(13) 0.023(11) C14 0.13(3) 0.13(2) 0.17(3) -0.06(2) 0.03(2) 0.05(2) C15 0.047(13) 0.14(2) 0.075(18) 0.009(15) 0.015(12) 0.050(12) C13B 0.062(15) 0.15(3) 0.12(3) 0.00(3) 0.02(2) 0.041(17) C14B 0.067(19) 0.114(17) 0.07(2) 0.008(18) 0.019(18) 0.078(15) C15B 0.08(2) 0.12(3) 0.090(16) 0.011(18) 0.052(17) 0.05(2) C16 0.027(5) 0.049(7) 0.063(7) 0.000(6) -0.003(5) 0.004(5) C17 0.085(10) 0.074(9) 0.049(8) 0.004(7) -0.007(7) -0.023(8) C18 0.27(3) 0.071(12) 0.047(9) -0.005(9) 0.012(15) 0.045(15) C19 0.180(17) 0.16(2) 0.079(14) 0.016(14) -0.038(15) -0.119(16) C20 0.066(10) 0.078(10) 0.065(9) 0.023(8) -0.018(8) -0.006(8) C101 0.051(10) 0.051(10) 0.064(18) 0 0 0 C102 0.066(13) 0.066(13) 0.060(19) 0 0 0 N1 0.12(3) 0.12(3) 0.12(3) 0.002(10) -0.004(10) -0.007(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ga1 F1 1.935(7) . ? Ga1 O5 1.936(9) . ? Ga1 O1 1.943(9) . ? Ga1 F2 1.947(7) . ? Ga1 O4 1.953(10) . ? Ga1 O8 1.978(9) . ? Ga2 F2 1.928(7) 2_655 ? Ga2 F1 1.929(6) . ? Ga2 O2 1.939(9) 2_655 ? Ga2 O7 1.948(11) 2_655 ? Ga2 O6 1.953(8) . ? Ga2 O3 2.005(10) . ? F2 Zn2 1.928(7) 3_565 ? F2 Ga2 1.928(7) 3_565 ? O1 C1 1.254(16) . ? O2 C1 1.268(17) . ? O2 Zn2 1.939(9) 3_565 ? O2 Ga2 1.939(9) 3_565 ? O3 C16 1.280(16) . ? O4 C16 1.206(15) . ? O5 C11 1.273(19) . ? O6 C11 1.319(18) . ? O7 C6 1.237(17) . ? O7 Zn2 1.948(11) 3_565 ? O7 Ga2 1.948(11) 3_565 ? O8 C6 1.265(17) . ? C1 C2 1.537(16) . ? C2 C3 1.428(18) . ? C2 C3B 1.447(19) . ? C2 C4B 1.495(19) . ? C2 C4 1.498(19) . ? C2 C5 1.571(18) . ? C2 C5B 1.597(19) . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? C5B H5B1 0.98 . ? C5B H5B2 0.98 . ? C5B H5B3 0.98 . ? C6 C7 1.58(2) . ? C7 C8 1.466(17) . ? C7 C9 1.469(18) . ? C7 C10 1.567(18) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.481(16) . ? C12 C13B 1.425(19) . ? C12 C13 1.460(18) . ? C12 C14 1.483(19) . ? C12 C14B 1.500(19) . ? C12 C15 1.578(19) . ? C12 C15B 1.582(19) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C13B H13D 0.98 . ? C13B H13E 0.98 . ? C13B H13F 0.98 . ? C14B H14D 0.98 . ? C14B H14E 0.98 . ? C14B H14F 0.98 . ? C15B H15D 0.98 . ? C15B H15E 0.98 . ? C15B H15F 0.98 . ? C16 C17 1.56(2) . ? C17 C18 1.458(17) . ? C17 C19 1.484(17) . ? C17 C20 1.559(16) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C101 N1 1.45(2) . ? C101 H101 0.98 . ? C101 H102 0.98 . ? C101 H103 0.98 . ? C102 N1 1.45(2) . ? C102 H104 0.98 . ? C102 H105 0.98 . ? C102 H106 0.98 . ? N1 H1A 0.92 . ? N1 H1B 0.92 . ? 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 F1 Ga1 O5 93.9(4) . . ? F1 Ga1 O1 177.2(3) . . ? O5 Ga1 O1 88.5(4) . . ? F1 Ga1 F2 86.3(3) . . ? O5 Ga1 F2 177.0(4) . . ? O1 Ga1 F2 91.2(3) . . ? F1 Ga1 O4 91.3(3) . . ? O5 Ga1 O4 94.4(5) . . ? O1 Ga1 O4 90.0(4) . . ? F2 Ga1 O4 88.6(4) . . ? F1 Ga1 O8 87.3(4) . . ? O5 Ga1 O8 86.4(4) . . ? O1 Ga1 O8 91.4(4) . . ? F2 Ga1 O8 90.5(3) . . ? O4 Ga1 O8 178.4(4) . . ? F2 Ga2 F1 86.7(2) 2_655 . ? F2 Ga2 O2 93.9(3) 2_655 2_655 ? F1 Ga2 O2 177.7(4) . 2_655 ? F2 Ga2 O7 91.3(4) 2_655 2_655 ? F1 Ga2 O7 89.0(4) . 2_655 ? O2 Ga2 O7 93.2(4) 2_655 2_655 ? F2 Ga2 O6 177.0(4) 2_655 . ? F1 Ga2 O6 90.3(4) . . ? O2 Ga2 O6 89.2(4) 2_655 . ? O7 Ga2 O6 88.8(4) 2_655 . ? F2 Ga2 O3 87.1(4) 2_655 . ? F1 Ga2 O3 90.2(4) . . ? O2 Ga2 O3 87.7(4) 2_655 . ? O7 Ga2 O3 178.2(4) 2_655 . ? O6 Ga2 O3 92.8(4) . . ? Ga2 F1 Ga1 121.9(3) . . ? Zn2 F2 Ga2 0.00(9) 3_565 3_565 ? Zn2 F2 Ga1 120.9(3) 3_565 . ? Ga2 F2 Ga1 120.9(3) 3_565 . ? C1 O1 Ga1 129.9(9) . . ? C1 O2 Zn2 135.9(7) . 3_565 ? C1 O2 Ga2 135.9(7) . 3_565 ? Zn2 O2 Ga2 0.00(12) 3_565 3_565 ? C16 O3 Ga2 133.0(8) . . ? C16 O4 Ga1 127.4(10) . . ? C11 O5 Ga1 136.8(9) . . ? C11 O6 Ga2 128.3(9) . . ? C6 O7 Zn2 126.9(10) . 3_565 ? C6 O7 Ga2 126.9(10) . 3_565 ? Zn2 O7 Ga2 0.00(11) 3_565 3_565 ? C6 O8 Ga1 134.5(9) . . ? O1 C1 O2 123.5(11) . . ? O1 C1 C2 118.1(12) . . ? O2 C1 C2 118.3(12) . . ? C3 C2 C3B 130(2) . . ? C3 C2 C4B 59(2) . . ? C3B C2 C4B 116(2) . . ? C3 C2 C4 116.1(18) . . ? C3B C2 C4 70(2) . . ? C4B C2 C4 59(2) . . ? C3 C2 C1 111.2(14) . . ? C3B C2 C1 116(2) . . ? C4B C2 C1 111(2) . . ? C4 C2 C1 102.4(14) . . ? C3 C2 C5 110.5(18) . . ? C3B C2 C5 38.0(19) . . ? C4B C2 C5 141(2) . . ? C4 C2 C5 107.6(16) . . ? C1 C2 C5 108.6(17) . . ? C3 C2 C5B 47.0(18) . . ? C3B C2 C5B 104.2(19) . . ? C4B C2 C5B 105.1(18) . . ? C4 C2 C5B 153.2(18) . . ? C1 C2 C5B 103.5(15) . . ? C5 C2 C5B 70(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C3B H3B1 109.5 . . ? C2 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2 C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2 C4B H4B1 109.5 . . ? C2 C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C2 C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C2 C5B H5B1 109.5 . . ? C2 C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C2 C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? O7 C6 O8 126.5(14) . . ? O7 C6 C7 118.4(13) . . ? O8 C6 C7 115.0(12) . . ? C8 C7 C9 114.6(14) . . ? C8 C7 C10 105.6(16) . . ? C9 C7 C10 112.1(17) . . ? C8 C7 C6 111.1(14) . . ? C9 C7 C6 109.1(14) . . ? C10 C7 C6 103.7(14) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 121.9(10) . . ? O5 C11 C12 119.5(14) . . ? O6 C11 C12 118.2(14) . . ? C13B C12 C13 60(2) . . ? C13B C12 C11 111(2) . . ? C13 C12 C11 108.5(14) . . ? C13B C12 C14 138(3) . . ? C13 C12 C14 115.3(19) . . ? C11 C12 C14 109.7(19) . . ? C13B C12 C14B 119(2) . . ? C13 C12 C14B 66(2) . . ? C11 C12 C14B 110.7(16) . . ? C14 C12 C14B 52.7(19) . . ? C13B C12 C15 47(2) . . ? C13 C12 C15 105.7(15) . . ? C11 C12 C15 109.5(14) . . ? C14 C12 C15 108.0(18) . . ? C14B C12 C15 139.4(17) . . ? C13B C12 C15B 110(2) . . ? C13 C12 C15B 151(2) . . ? C11 C12 C15B 100.1(17) . . ? C14 C12 C15B 52(2) . . ? C14B C12 C15B 104.5(18) . . ? C15 C12 C15B 63.2(19) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C13B H13D 109.5 . . ? C12 C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C12 C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12 C14B H14D 109.5 . . ? C12 C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12 C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C12 C15B H15D 109.5 . . ? C12 C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C12 C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? O4 C16 O3 127.5(14) . . ? O4 C16 C17 120.5(12) . . ? O3 C16 C17 111.9(11) . . ? C18 C17 C19 114.2(12) . . ? C18 C17 C20 109.4(11) . . ? C19 C17 C20 108.1(11) . . ? C18 C17 C16 109.1(11) . . ? C19 C17 C16 109.7(12) . . ? C20 C17 C16 106.1(11) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C101 H101 109.5 . . ? N1 C101 H102 109.5 . . ? H101 C101 H102 109.5 . . ? N1 C101 H103 109.5 . . ? H101 C101 H103 109.5 . . ? H102 C101 H103 109.5 . . ? N1 C102 H104 109.5 . . ? N1 C102 H105 109.5 . . ? H104 C102 H105 109.5 . . ? N1 C102 H106 109.5 . . ? H104 C102 H106 109.5 . . ? H105 C102 H106 109.5 . . ? C101 N1 C102 114(4) . . ? C101 N1 H1A 108.6 . . ? C102 N1 H1A 108.6 . . ? C101 N1 H1B 108.6 . . ? C102 N1 H1B 108.6 . . ? H1A N1 H1B 107.6 . . ? 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 F2 Ga2 F1 Ga1 -126.2(5) 2_655 . . . ? O2 Ga2 F1 Ga1 -23(9) 2_655 . . . ? O7 Ga2 F1 Ga1 142.4(5) 2_655 . . . ? O6 Ga2 F1 Ga1 53.6(5) . . . . ? O3 Ga2 F1 Ga1 -39.1(5) . . . . ? O5 Ga1 F1 Ga2 -37.0(5) . . . . ? O1 Ga1 F1 Ga2 174(8) . . . . ? F2 Ga1 F1 Ga2 146.0(4) . . . . ? O4 Ga1 F1 Ga2 57.5(5) . . . . ? O8 Ga1 F1 Ga2 -123.2(5) . . . . ? F1 Ga1 F2 Zn2 126.6(4) . . . 3_565 ? O5 Ga1 F2 Zn2 32(8) . . . 3_565 ? O1 Ga1 F2 Zn2 -52.1(5) . . . 3_565 ? O4 Ga1 F2 Zn2 -142.0(5) . . . 3_565 ? O8 Ga1 F2 Zn2 39.3(5) . . . 3_565 ? F1 Ga1 F2 Ga2 126.6(4) . . . 3_565 ? O5 Ga1 F2 Ga2 32(8) . . . 3_565 ? O1 Ga1 F2 Ga2 -52.1(5) . . . 3_565 ? O4 Ga1 F2 Ga2 -142.0(5) . . . 3_565 ? O8 Ga1 F2 Ga2 39.3(5) . . . 3_565 ? F1 Ga1 O1 C1 20(9) . . . . ? O5 Ga1 O1 C1 -129.2(12) . . . . ? F2 Ga1 O1 C1 47.7(12) . . . . ? O4 Ga1 O1 C1 136.4(12) . . . . ? O8 Ga1 O1 C1 -42.8(12) . . . . ? F2 Ga2 O3 C16 77.6(12) 2_655 . . . ? F1 Ga2 O3 C16 -9.0(12) . . . . ? O2 Ga2 O3 C16 171.6(12) 2_655 . . . ? O7 Ga2 O3 C16 52(14) 2_655 . . . ? O6 Ga2 O3 C16 -99.4(12) . . . . ? F1 Ga1 O4 C16 -42.0(10) . . . . ? O5 Ga1 O4 C16 52.0(11) . . . . ? O1 Ga1 O4 C16 140.5(11) . . . . ? F2 Ga1 O4 C16 -128.3(10) . . . . ? O8 Ga1 O4 C16 -69(16) . . . . ? F1 Ga1 O5 C11 0.6(15) . . . . ? O1 Ga1 O5 C11 179.2(15) . . . . ? F2 Ga1 O5 C11 95(7) . . . . ? O4 Ga1 O5 C11 -90.9(15) . . . . ? O8 Ga1 O5 C11 87.7(16) . . . . ? F2 Ga2 O6 C11 -50(8) 2_655 . . . ? F1 Ga2 O6 C11 -52.6(12) . . . . ? O2 Ga2 O6 C11 125.2(12) 2_655 . . . ? O7 Ga2 O6 C11 -141.5(12) 2_655 . . . ? O3 Ga2 O6 C11 37.6(12) . . . . ? F1 Ga1 O8 C6 -77.7(13) . . . . ? O5 Ga1 O8 C6 -171.9(14) . . . . ? O1 Ga1 O8 C6 99.8(14) . . . . ? F2 Ga1 O8 C6 8.6(13) . . . . ? O4 Ga1 O8 C6 -50(16) . . . . ? Ga1 O1 C1 O2 -20(2) . . . . ? Ga1 O1 C1 C2 157.9(10) . . . . ? Zn2 O2 C1 O1 -14(2) 3_565 . . . ? Ga2 O2 C1 O1 -14(2) 3_565 . . . ? Zn2 O2 C1 C2 167.9(10) 3_565 . . . ? Ga2 O2 C1 C2 167.9(10) 3_565 . . . ? O1 C1 C2 C3 -66(2) . . . . ? O2 C1 C2 C3 111(2) . . . . ? O1 C1 C2 C3B 131(2) . . . . ? O2 C1 C2 C3B -51(3) . . . . ? O1 C1 C2 C4B -3(3) . . . . ? O2 C1 C2 C4B 175(2) . . . . ? O1 C1 C2 C4 58.2(19) . . . . ? O2 C1 C2 C4 -124.0(17) . . . . ? O1 C1 C2 C5 171.8(19) . . . . ? O2 C1 C2 C5 -10(2) . . . . ? O1 C1 C2 C5B -115(2) . . . . ? O2 C1 C2 C5B 63(2) . . . . ? Zn2 O7 C6 O8 -8(2) 3_565 . . . ? Ga2 O7 C6 O8 -8(2) 3_565 . . . ? Zn2 O7 C6 C7 168.7(10) 3_565 . . . ? Ga2 O7 C6 C7 168.7(10) 3_565 . . . ? Ga1 O8 C6 O7 -27(2) . . . . ? Ga1 O8 C6 C7 156.4(10) . . . . ? O7 C6 C7 C8 -10(2) . . . . ? O8 C6 C7 C8 166.9(14) . . . . ? O7 C6 C7 C9 -137.6(17) . . . . ? O8 C6 C7 C9 39.6(19) . . . . ? O7 C6 C7 C10 102.7(19) . . . . ? O8 C6 C7 C10 -80.0(18) . . . . ? Ga1 O5 C11 O6 4(2) . . . . ? Ga1 O5 C11 C12 -168.8(11) . . . . ? Ga2 O6 C11 O5 29(2) . . . . ? Ga2 O6 C11 C12 -157.6(11) . . . . ? O5 C11 C12 C13B -135(3) . . . . ? O6 C11 C12 C13B 52(3) . . . . ? O5 C11 C12 C13 -71(2) . . . . ? O6 C11 C12 C13 116.3(18) . . . . ? O5 C11 C12 C14 56(2) . . . . ? O6 C11 C12 C14 -117(2) . . . . ? O5 C11 C12 C14B 0(2) . . . . ? O6 C11 C12 C14B -173.5(19) . . . . ? O5 C11 C12 C15 174.5(17) . . . . ? O6 C11 C12 C15 1(2) . . . . ? O5 C11 C12 C15B 110(2) . . . . ? O6 C11 C12 C15B -64(2) . . . . ? Ga1 O4 C16 O3 5.2(18) . . . . ? Ga1 O4 C16 C17 -179.0(9) . . . . ? Ga2 O3 C16 O4 29(2) . . . . ? Ga2 O3 C16 C17 -147.3(10) . . . . ? O4 C16 C17 C18 -91.5(15) . . . . ? O3 C16 C17 C18 84.9(14) . . . . ? O4 C16 C17 C19 142.8(13) . . . . ? O3 C16 C17 C19 -40.8(15) . . . . ? O4 C16 C17 C20 26.3(15) . . . . ? O3 C16 C17 C20 -157.4(11) . . . . ? # END of CIF _database_code_depnum_ccdc_archive 'CCDC 954610'