# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'UMCM_25NH2Br.cif' _publ_contact_author P.V.Dau _publ_contact_author_email pdau@ucsd.edu _publ_contact_author_name P.V.Dau loop_ _publ_author_name M.Kim J.A.Boissonnault C.A.Allen P.V.Dau S.M.Cohen data_UMCM_25NH2Br _database_code_depnum_ccdc_archive 'CCDC 863173' #TrackingRef '- Revised CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H17 Br N0 O13 Zn4' _chemical_formula_weight 1077.83 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' '-x, -y, -z' '-x+y, -x, -z-1/2' '-y, x-y, -z-1/2' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' _cell_length_a 41.285(8) _cell_length_b 41.285(8) _cell_length_c 17.489(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25815(8) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3138 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.8896 _exptl_absorpt_correction_T_max 0.9244 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 67885 _diffrn_reflns_av_R_equivalents 0.1998 _diffrn_reflns_av_sigmaI/netI 0.1546 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 20.84 _reflns_number_total 9420 _reflns_number_gt 4447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was not refined as anisotropy to be consistent due to some disorder atoms. SQUEEZE found 6269 electrons that can be accounted to chloroform and DMF molecules that are trapped in the pores.Nitrogen cant be located due to the Br disorders. The value of sine(theta_max)/wavelength is less than 0.550, this error is be due to the quality of the crystal. The neighbors of C018, C021, C026, C028 and C030 have high Ueq because of severe disorders. No atom was refined as aniso so there is no _atom_site_aniso_label. Amino groups cannot be located due to the disorder of halogen atoms. 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^)+(0.0843P)^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 'not measured' _refine_ls_number_reflns 9420 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1430 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.1991 _refine_ls_wR_factor_gt 0.1745 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 -0.006 -0.003 -0.008 20872 6296 ' ' _platon_squeeze_details ; ; _refinement_detail ; ; 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 O001 O 0.05872(18) 0.42706(18) 0.7500 0.0537(18) Uiso 1 2 d S . . O002 O 0.05676(15) 0.38600(14) 0.9054(3) 0.0695(15) Uiso 1 1 d . . . O003 O -0.01662(14) 0.35569(14) 0.8139(3) 0.0680(15) Uiso 1 1 d . . . O004 O 0.1472(2) 0.4742(3) 0.7500 0.097(3) Uiso 1 2 d S . . O005 O 0.1238(3) 0.5115(3) 0.7500 0.107(3) Uiso 1 2 d S . . C001 C 0.1510(4) 0.5044(4) 0.7500 0.086(4) Uiso 1 2 d S . . O006 O 0.11002(14) 0.40241(14) 0.8435(3) 0.0649(15) Uiso 1 1 d . . . O007 O 0.01609(16) 0.43294(17) 0.9000(3) 0.0866(18) Uiso 1 1 d . . . O008 O 0.04771(18) 0.48782(18) 0.8369(3) 0.102(2) Uiso 1 1 d . . . C002 C 0.0266(2) 0.4653(3) 0.8880(5) 0.078(3) Uiso 1 1 d . . . C003 C 0.0891(2) 0.3911(2) 0.8979(4) 0.067(2) Uiso 1 1 d . . . C004 C -0.0290(3) 0.3415(3) 0.7500 0.066(3) Uiso 1 2 d S . . C005 C -0.0645(4) 0.3055(4) 0.7500 0.083(4) Uiso 1 2 d S . . C006 C 0.1872(5) 0.5389(5) 0.7500 0.119(5) Uiso 1 2 d S . . C007 C 0.2183(9) 0.5352(8) 0.7500 0.230(11) Uiso 1 2 d S . . H007 H 0.2156 0.5114 0.7500 0.276 Uiso 1 2 calc SR . . C008 C 0.1050(3) 0.3842(2) 0.9730(5) 0.077(3) Uiso 1 1 d . . . C009 C 0.0812(3) 0.3664(3) 1.0307(5) 0.103(3) Uiso 1 1 d . . . H009 H 0.0557 0.3575 1.0250 0.124 Uiso 1 1 calc R . . C011 C 0.1350(3) 0.3758(2) 1.1087(5) 0.084(3) Uiso 1 1 d . . . C013 C 0.1425(3) 0.3958(3) 0.9742(5) 0.100(3) Uiso 1 1 d . . . H013 H 0.1569 0.4058 0.9304 0.120 Uiso 1 1 calc R . . C010 C 0.0966(3) 0.3613(3) 1.1045(5) 0.100(3) Uiso 1 1 d . . . H010 H 0.0810 0.3490 1.1458 0.120 Uiso 1 1 calc R . . C012 C 0.1591(3) 0.3926(3) 1.0422(6) 0.132(4) Uiso 1 1 d . . . H012 H 0.1846 0.4009 1.0445 0.159 Uiso 1 1 calc R . . C015 C 0.1518(3) 0.3718(2) 1.1798(5) 0.088(3) Uiso 1 1 d . . . C016 C 0.1347(4) 0.3729(3) 1.2500 0.091(4) Uiso 1 2 d S . . H016 H 0.1129 0.3742 1.2500 0.109 Uiso 1 2 calc SR . . C020 C 0.2609(8) 0.6014(8) 0.7500 0.177(8) Uiso 1 2 d S . . C018 C 0.2292(14) 0.6045(12) 0.7500 0.328(19) Uiso 1 2 d S . . H018 H 0.2313 0.6280 0.7500 0.394 Uiso 1 2 calc SR . . C021 C 0.2558(11) 0.5681(12) 0.7500 0.303(16) Uiso 1 2 d S . . H021 H 0.2765 0.5648 0.7500 0.364 Uiso 1 2 calc SR . . C023 C 0.3023(6) 0.6716(7) 0.7500 0.140(6) Uiso 1 2 d S . . H023 H 0.2816 0.6748 0.7500 0.168 Uiso 1 2 calc SR . . C022 C 0.2983(6) 0.6360(7) 0.7500 0.145(6) Uiso 1 2 d S . . C024 C -0.1321(4) 0.2358(4) 0.7500 0.097(4) Uiso 1 2 d S . . C025 C -0.1144(4) 0.2527(4) 0.8161(8) 0.191(6) Uiso 1 1 d . . . H025 H -0.1222 0.2399 0.8623 0.229 Uiso 1 1 calc R . . C026 C -0.0836(4) 0.2906(4) 0.8141(8) 0.189(6) Uiso 1 1 d . . . H026 H -0.0769 0.3049 0.8584 0.227 Uiso 1 1 calc R . . C027 C 0.0117(2) 0.4843(3) 0.9463(5) 0.081(3) Uiso 1 1 d . . . C028 C -0.0023(3) 0.4657(3) 1.0122(6) 0.110(3) Uiso 1 1 d . . . C029 C 0.0169(3) 0.5181(4) 0.9321(6) 0.134(4) Uiso 1 1 d . . . C030 C 0.1977(13) 0.5759(15) 0.7500 0.37(2) Uiso 1 2 d S . . H030 H 0.1779 0.5806 0.7500 0.446 Uiso 1 2 calc SR . . Zn3 Zn 0.10430(3) 0.42440(3) 0.7500 0.0487(4) Uiso 1 2 d S . . Zn2 Zn 0.07014(4) 0.47795(4) 0.7500 0.0633(4) Uiso 1 2 d S . . Zn1 Zn 0.02891(2) 0.40103(2) 0.83975(4) 0.0512(3) Uiso 1 1 d . . . Br1B Br 0.02447(17) 0.54289(17) 0.8369(3) 0.159(2) Uiso 0.25 1 d P . . Br2B Br -0.0366(7) 0.4140(8) 1.0139(14) 0.631(15) Uiso 0.25 1 d P . . C014 C 0.1841(3) 0.3704(2) 1.1815(5) 0.094(3) Uiso 1 1 d . . . H014 H 0.1962 0.3715 1.1360 0.113 Uiso 1 1 calc R . . C031 C 0.1990(4) 0.3675(4) 1.2500 0.099(4) Uiso 1 2 d S . . _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 O001 Zn2 1.909(6) . ? O001 Zn3 1.939(6) . ? O001 Zn1 1.952(4) . ? O001 Zn1 1.952(4) 12_557 ? O002 C003 1.251(8) . ? O002 Zn1 1.934(5) . ? O003 C004 1.247(6) . ? O003 Zn1 1.929(5) . ? O004 C001 1.178(14) . ? O004 Zn3 1.930(9) . ? O005 C001 1.296(14) . ? O005 Zn2 1.937(10) . ? C001 C006 1.460(18) . ? O006 C003 1.211(8) . ? O006 Zn3 1.941(5) . ? O007 C002 1.200(9) . ? O007 Zn1 1.956(6) . ? O008 C002 1.269(9) . ? O008 Zn2 1.927(6) . ? C002 C027 1.584(11) . ? C003 C008 1.556(10) . ? C004 O003 1.247(6) 12_557 ? C004 C005 1.477(15) . ? C005 C026 1.330(14) 12_557 ? C005 C026 1.331(14) . ? C006 C030 1.36(5) . ? C006 C007 1.37(3) . ? C007 C021 1.46(4) . ? C008 C009 1.341(10) . ? C008 C013 1.372(11) . ? C009 C010 1.498(11) . ? C011 C010 1.389(11) . ? C011 C012 1.462(12) . ? C011 C015 1.473(11) . ? C013 C012 1.411(11) . ? C015 C014 1.362(11) . ? C015 C016 1.428(10) . ? C016 C015 1.428(10) 12_558 ? C020 C021 1.28(4) . ? C020 C018 1.38(4) . ? C020 C022 1.49(2) . ? C018 C030 1.25(5) . ? C023 C022 1.364(19) 8_567 ? C023 C022 1.394(19) . ? C022 C023 1.364(19) 9_667 ? C024 C025 1.359(14) . ? C024 C025 1.359(14) 12_557 ? C024 C031 1.513(17) 2_554 ? C025 C026 1.441(17) . ? C027 C029 1.324(12) . ? C027 C028 1.344(10) . ? C028 C029 1.471(13) 7_567 ? C028 Br2B 1.88(3) . ? C029 C028 1.471(13) 7_567 ? C029 Br1B 1.898(12) . ? Zn3 O006 1.941(5) 12_557 ? Zn2 O008 1.927(6) 12_557 ? Zn1 Zn1 3.1393(16) 12_557 ? C014 C031 1.379(10) . ? C031 C014 1.379(10) 12_558 ? C031 C024 1.513(17) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Zn2 O001 Zn3 110.4(3) . . ? Zn2 O001 Zn1 110.3(2) . . ? Zn3 O001 Zn1 109.4(2) . . ? Zn2 O001 Zn1 110.3(2) . 12_557 ? Zn3 O001 Zn1 109.4(2) . 12_557 ? Zn1 O001 Zn1 107.0(3) . 12_557 ? C003 O002 Zn1 129.8(5) . . ? C004 O003 Zn1 129.6(6) . . ? C001 O004 Zn3 133.9(10) . . ? C001 O005 Zn2 130.5(10) . . ? O004 C001 O005 124.7(15) . . ? O004 C001 C006 124.1(16) . . ? O005 C001 C006 111.2(15) . . ? C003 O006 Zn3 127.8(5) . . ? C002 O007 Zn1 125.9(6) . . ? C002 O008 Zn2 128.9(6) . . ? O007 C002 O008 132.3(9) . . ? O007 C002 C027 115.1(8) . . ? O008 C002 C027 112.7(8) . . ? O006 C003 O002 130.0(8) . . ? O006 C003 C008 116.7(8) . . ? O002 C003 C008 113.1(7) . . ? O003 C004 O003 127.4(11) . 12_557 ? O003 C004 C005 116.1(6) . . ? O003 C004 C005 116.1(6) 12_557 . ? C026 C005 C026 114.7(18) 12_557 . ? C026 C005 C004 121.7(9) 12_557 . ? C026 C005 C004 121.7(9) . . ? C030 C006 C007 110(3) . . ? C030 C006 C001 134(3) . . ? C007 C006 C001 117(2) . . ? C006 C007 C021 121(3) . . ? C009 C008 C013 124.6(9) . . ? C009 C008 C003 118.4(9) . . ? C013 C008 C003 116.9(8) . . ? C008 C009 C010 118.7(9) . . ? C010 C011 C012 121.5(9) . . ? C010 C011 C015 119.8(9) . . ? C012 C011 C015 118.5(9) . . ? C008 C013 C012 119.7(10) . . ? C011 C010 C009 117.1(9) . . ? C013 C012 C011 117.9(10) . . ? C014 C015 C016 119.4(10) . . ? C014 C015 C011 123.3(9) . . ? C016 C015 C011 117.0(9) . . ? C015 C016 C015 118.6(13) . 12_558 ? C021 C020 C018 117(3) . . ? C021 C020 C022 124(4) . . ? C018 C020 C022 119(3) . . ? C030 C018 C020 120(5) . . ? C020 C021 C007 122(3) . . ? C022 C023 C022 118(3) 8_567 . ? C023 C022 C023 122(3) 9_667 . ? C023 C022 C020 116(3) 9_667 . ? C023 C022 C020 122(3) . . ? C025 C024 C025 116.5(19) . 12_557 ? C025 C024 C031 121.7(9) . 2_554 ? C025 C024 C031 121.7(9) 12_557 2_554 ? C024 C025 C026 119.5(15) . . ? C005 C026 C025 121.3(15) . . ? C029 C027 C028 123.9(9) . . ? C029 C027 C002 120.1(10) . . ? C028 C027 C002 115.7(9) . . ? C027 C028 C029 117.8(10) . 7_567 ? C027 C028 Br2B 121.7(11) . . ? C029 C028 Br2B 105.1(12) 7_567 . ? C027 C029 C028 117.9(10) . 7_567 ? C027 C029 Br1B 129.0(10) . . ? C028 C029 Br1B 109.2(10) 7_567 . ? C018 C030 C006 131(5) . . ? O004 Zn3 O001 109.9(3) . . ? O004 Zn3 O006 103.7(2) . 12_557 ? O001 Zn3 O006 112.02(17) . 12_557 ? O004 Zn3 O006 103.7(2) . . ? O001 Zn3 O006 112.02(17) . . ? O006 Zn3 O006 114.8(3) 12_557 . ? O001 Zn2 O008 110.6(2) . 12_557 ? O001 Zn2 O008 110.6(2) . . ? O008 Zn2 O008 104.2(4) 12_557 . ? O001 Zn2 O005 110.6(3) . . ? O008 Zn2 O005 110.3(2) 12_557 . ? O008 Zn2 O005 110.3(2) . . ? O003 Zn1 O002 105.9(2) . . ? O003 Zn1 O001 112.7(2) . . ? O002 Zn1 O001 110.0(2) . . ? O003 Zn1 O007 108.6(2) . . ? O002 Zn1 O007 107.5(2) . . ? O001 Zn1 O007 111.8(3) . . ? O003 Zn1 Zn1 76.47(14) . 12_557 ? O002 Zn1 Zn1 126.44(15) . 12_557 ? O001 Zn1 Zn1 36.48(15) . 12_557 ? O007 Zn1 Zn1 122.63(16) . 12_557 ? C015 C014 C031 120.8(11) . . ? C014 C031 C014 120.6(14) . 12_558 ? C014 C031 C024 119.3(7) . 3 ? C014 C031 C024 119.3(7) 12_558 3 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.84 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.983 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.059 data_UMCM_25NH2Cl _database_code_depnum_ccdc_archive 'CCDC 863174' #TrackingRef '- Revised CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H17 Cl N0 O13 Zn4' _chemical_formula_weight 1026.49 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' Cl Cl 0.1484 0.1585 '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 ? _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 41.247(7) _cell_length_b 41.247(7) _cell_length_c 17.447(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25706(8) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9208 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 17.19 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3060 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.9175 _exptl_absorpt_correction_T_max 0.9439 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 63917 _diffrn_reflns_av_R_equivalents 0.1453 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 17.25 _reflns_number_total 5485 _reflns_number_gt 4114 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was not refined as anisotropy to be consistent due to some disorder atoms.SQUEEZE found 6615 electrons that can be accounted to chloroform and DMF molecules that are trapped in the pores. Nitrogen atom cannot be located due to the disorder of cloro atoms.The value of sine(theta_max)/wavelength is less than 0.550 is due to the weak diffraction of the crystal (poor quality crystal). The neighbors of O11b, C17 and C30 have high Ueq because of the disorders.2theta = 17.25 because of the weak diffraction. Amino groups cannot be located due to the disorder of halogen atoms. 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^)+(0.1818P)^2^+10.2198P] 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 'not measured' _refine_ls_number_reflns 5485 _refine_ls_number_parameters 140 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1271 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.2671 _refine_ls_wR_factor_gt 0.2456 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 -0.006 -0.005 -0.011 21194 6615 ' ' _platon_squeeze_details ; ; _refinement_detail ; ; 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 O3 O 0.40057(18) 0.11008(18) 0.6596(3) 0.054(2) Uiso 1 1 d . . . O2 O 0.38630(19) 0.0573(2) 0.5923(4) 0.070(2) Uiso 1 1 d . . . O4 O 0.42912(19) 0.0605(2) 0.7500 0.024(2) Uiso 1 2 d SD . . C7 C 0.3685(4) 0.1853(4) 0.3234(7) 0.095(4) Uiso 1 1 d . . . C3 C 0.3710(3) 0.1530(3) 0.3182(6) 0.059(3) Uiso 1 1 d . . . C2 C 0.3729(3) 0.1364(3) 0.3935(6) 0.065(3) Uiso 1 1 d . . . C1 C 0.3912(3) 0.0881(3) 0.6032(6) 0.055(3) Uiso 1 1 d . . . C6 C 0.3608(4) 0.0983(4) 0.3935(8) 0.114(5) Uiso 1 1 d . . . H6 H 0.3484 0.0833 0.3515 0.136 Uiso 1 1 calc R . . C4 C 0.3711(4) 0.1336(4) 0.2500 0.068(5) Uiso 1 2 d S . . C5 C 0.3884(3) 0.1606(4) 0.4584(7) 0.094(4) Uiso 1 1 d . . . H5 H 0.3955 0.1858 0.4579 0.113 Uiso 1 1 calc R . . O7 O 0.35864(18) -0.01423(19) 0.6862(4) 0.064(2) Uiso 1 1 d . . . O6 O 0.4309(3) 0.0152(2) 0.5969(5) 0.098(3) Uiso 1 1 d . . . O5 O 0.4863(3) 0.0457(3) 0.6649(5) 0.123(3) Uiso 1 1 d . . . C11 C 0.3418(4) -0.0279(4) 0.7500 0.056(4) Uiso 1 2 d S . . C20 C 0.3106(5) -0.0614(4) 0.7500 0.060(5) Uiso 1 2 d S . . C8 C 0.3825(3) 0.1057(3) 0.5289(5) 0.045(3) Uiso 1 1 d . . . C10 C 0.3916(3) 0.1411(4) 0.5261(7) 0.090(4) Uiso 1 1 d . . . H10 H 0.4009 0.1551 0.5707 0.108 Uiso 1 1 calc R . . C9 C 0.3686(4) 0.0817(4) 0.4644(7) 0.104(5) Uiso 1 1 d . . . H9 H 0.3645 0.0574 0.4653 0.125 Uiso 1 1 calc R . . C13 C 0.4826(4) 0.0130(4) 0.5554(8) 0.095(4) Uiso 1 1 d . . . C19 C 0.2376(5) -0.1287(5) 0.7500 0.094(6) Uiso 1 2 d S . . C15 C 0.5151(5) 0.0120(5) 0.5691(10) 0.143(6) Uiso 1 1 d . . . C12 C 0.4640(4) 0.0258(4) 0.6126(7) 0.089(4) Uiso 1 1 d . . . C14 C 0.4660(5) -0.0002(4) 0.4833(9) 0.139(6) Uiso 1 1 d . . . H14 H 0.4437 -0.0012 0.4700 0.167 Uiso 1 1 calc R . . C18 C 0.2020(5) -0.1695(5) 0.7500 0.093(6) Uiso 1 2 d S . . C16 C 0.2875(5) -0.0778(5) 0.6854(10) 0.142(6) Uiso 1 1 d . . . H16 H 0.2962 -0.0647 0.6397 0.171 Uiso 1 1 calc R . . C17 C 0.2519(7) -0.1128(7) 0.6811(13) 0.214(9) Uiso 1 1 d . . . H17 H 0.2399 -0.1232 0.6350 0.256 Uiso 1 1 calc R . . Cl1 Cl 0.5383(3) 0.0207(3) 0.6641(5) 0.147(3) Uiso 0.50 1 d P . . O10 O 0.4678(4) 0.1510(4) 0.7500 0.128(5) Uiso 1 2 d SD . . O11B O 0.5047(6) 0.1266(4) 0.7500 0.219(9) Uiso 1 2 d SD . . C28 C 0.4996(7) 0.1548(7) 0.7500 0.141(9) Uiso 1 2 d SD . . C30 C 0.5385(10) 0.1912(10) 0.7500 0.213(14) Uiso 1 2 d SD . . C35 C 0.6302(10) 0.3305(12) 0.7500 0.194(12) Uiso 1 2 d S . . H35 H 0.6068 0.3287 0.7500 0.232 Uiso 1 2 calc SR . . C34 C 0.6354(9) 0.2995(9) 0.7500 0.152(9) Uiso 1 2 d S . . C32 C 0.5648(9) 0.2547(9) 0.7500 0.205(13) Uiso 1 2 d SD . . H32 H 0.5627 0.2761 0.7500 0.246 Uiso 1 2 calc SR . . C31 C 0.5993(10) 0.2584(10) 0.7500 0.201(13) Uiso 1 2 d SD . . C33 C 0.5331(9) 0.2206(9) 0.7500 0.185(11) Uiso 1 2 d SD . . H33 H 0.5093 0.2178 0.7500 0.222 Uiso 1 2 calc SR . . Zn1 Zn 0.40274(3) 0.03060(3) 0.66032(6) 0.0482(6) Uiso 1 1 d . . . Zn2 Zn 0.42438(4) 0.10461(5) 0.7500 0.0437(7) Uiso 1 2 d S . . Zn3 Zn 0.48145(6) 0.07453(6) 0.7500 0.0795(8) Uiso 1 2 d SD . . _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 O3 C1 1.260(11) . ? O3 Zn2 1.930(6) . ? O2 C1 1.198(11) . ? O2 Zn1 1.955(7) . ? O4 Zn2 1.925(7) . ? O4 Zn3 1.935(7) . ? O4 Zn1 1.952(4) 10_557 ? O4 Zn1 1.952(4) . ? C7 C3 1.393(14) . ? C7 C18 1.430(14) 9_556 ? C3 C4 1.434(12) . ? C3 C2 1.502(13) . ? C2 C6 1.392(15) . ? C2 C5 1.432(14) . ? C1 C8 1.614(13) . ? C6 C9 1.520(17) . ? C4 C3 1.434(12) 10_556 ? C5 C10 1.470(15) . ? O7 C11 1.284(9) . ? O7 Zn1 1.889(7) . ? O6 C12 1.239(13) . ? O6 Zn1 1.929(9) . ? O5 C12 1.263(13) . ? O5 Zn3 1.973(10) . ? C11 O7 1.284(9) 10_557 ? C11 C20 1.338(18) . ? C20 C16 1.410(18) . ? C20 C16 1.410(18) 10_557 ? C8 C10 1.313(13) . ? C8 C9 1.417(14) . ? C13 C15 1.381(18) . ? C13 C14 1.405(17) . ? C13 C12 1.502(16) . ? C19 C17 1.35(2) 10_557 ? C19 C17 1.35(2) . ? C19 C18 1.59(2) . ? C15 C14 1.438(19) 7_656 ? C15 Cl1 1.858(18) . ? C14 C15 1.438(19) 7_656 ? C18 C7 1.430(14) 8_556 ? C18 C7 1.430(14) 5 ? C16 C17 1.46(2) . ? O10 C28 1.242(16) . ? O10 Zn2 1.853(15) . ? O11B C28 1.283(16) . ? O11B Zn3 1.864(15) . ? C28 C30 1.55(4) . ? C30 C33 1.335(18) . ? C35 C34 1.40(3) . ? C35 C34 1.40(3) 3_665 ? C34 C35 1.40(3) 2_655 ? C34 C31 1.60(4) . ? C32 C31 1.355(18) . ? C32 C33 1.361(18) . ? Zn1 Zn1 3.129(2) 10_557 ? Zn1 Zn2 3.1365(19) . ? Zn2 O3 1.930(6) 10_557 ? Zn2 Zn1 3.1366(19) 10_557 ? Zn3 O5 1.973(10) 10_557 ? 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 C1 O3 Zn2 123.0(7) . . ? C1 O2 Zn1 125.3(7) . . ? Zn2 O4 Zn3 110.0(4) . . ? Zn2 O4 Zn1 108.0(2) . 10_557 ? Zn3 O4 Zn1 112.0(2) . 10_557 ? Zn2 O4 Zn1 108.0(2) . . ? Zn3 O4 Zn1 112.0(2) . . ? Zn1 O4 Zn1 106.6(3) 10_557 . ? C3 C7 C18 111.9(12) . 9_556 ? C7 C3 C4 127.7(11) . . ? C7 C3 C2 115.2(10) . . ? C4 C3 C2 117.1(9) . . ? C6 C2 C5 124.8(11) . . ? C6 C2 C3 116.4(10) . . ? C5 C2 C3 118.7(10) . . ? O2 C1 O3 135.7(10) . . ? O2 C1 C8 113.2(9) . . ? O3 C1 C8 111.1(9) . . ? C2 C6 C9 118.0(13) . . ? C3 C4 C3 112.0(13) 10_556 . ? C2 C5 C10 112.6(11) . . ? C11 O7 Zn1 133.0(8) . . ? C12 O6 Zn1 119.8(9) . . ? C12 O5 Zn3 132.7(10) . . ? O7 C11 O7 120.3(14) . 10_557 ? O7 C11 C20 119.0(7) . . ? O7 C11 C20 119.0(7) 10_557 . ? C11 C20 C16 124.5(10) . . ? C11 C20 C16 124.5(10) . 10_557 ? C16 C20 C16 106.1(19) . 10_557 ? C10 C8 C9 122.6(11) . . ? C10 C8 C1 121.8(10) . . ? C9 C8 C1 115.3(9) . . ? C8 C10 C5 125.6(12) . . ? C8 C9 C6 115.8(12) . . ? C15 C13 C14 115.8(14) . . ? C15 C13 C12 124.5(15) . . ? C14 C13 C12 119.6(15) . . ? C17 C19 C17 125(3) 10_557 . ? C17 C19 C18 117.4(14) 10_557 . ? C17 C19 C18 117.4(14) . . ? C13 C15 C14 126.9(15) . 7_656 ? C13 C15 Cl1 124.2(14) . . ? C14 C15 Cl1 108.5(14) 7_656 . ? O6 C12 O5 134.5(14) . . ? O6 C12 C13 113.3(13) . . ? O5 C12 C13 112.2(13) . . ? C13 C14 C15 117.3(15) . 7_656 ? C7 C18 C7 127.2(18) 8_556 5 ? C7 C18 C19 115.3(9) 8_556 . ? C7 C18 C19 115.3(9) 5 . ? C20 C16 C17 128.3(19) . . ? C19 C17 C16 114(2) . . ? C28 O10 Zn2 123.2(16) . . ? C28 O11B Zn3 145(2) . . ? O10 C28 O11B 122(3) . . ? O10 C28 C30 130(2) . . ? O11B C28 C30 109(2) . . ? C33 C30 C28 108(3) . . ? C34 C35 C34 113(4) . 3_665 ? C35 C34 C35 127(4) . 2_655 ? C35 C34 C31 119(4) . . ? C35 C34 C31 114(4) 2_655 . ? C31 C32 C33 122(4) . . ? C32 C31 C34 119(3) . . ? C30 C33 C32 115(4) . . ? O7 Zn1 O6 105.0(3) . . ? O7 Zn1 O4 112.8(3) . . ? O6 Zn1 O4 115.5(3) . . ? O7 Zn1 O2 105.1(3) . . ? O6 Zn1 O2 105.9(3) . . ? O4 Zn1 O2 111.8(3) . . ? O7 Zn1 Zn1 76.2(2) . 10_557 ? O6 Zn1 Zn1 125.0(3) . 10_557 ? O4 Zn1 Zn1 36.72(17) . 10_557 ? O2 Zn1 Zn1 127.3(2) . 10_557 ? O7 Zn1 Zn2 120.0(2) . . ? O6 Zn1 Zn2 133.0(3) . . ? O4 Zn1 Zn2 35.7(2) . . ? O2 Zn1 Zn2 76.4(2) . . ? Zn1 Zn1 Zn2 60.08(3) 10_557 . ? O10 Zn2 O4 118.2(5) . . ? O10 Zn2 O3 99.5(3) . 10_557 ? O4 Zn2 O3 114.1(2) . 10_557 ? O10 Zn2 O3 99.5(3) . . ? O4 Zn2 O3 114.1(2) . . ? O3 Zn2 O3 109.6(4) 10_557 . ? O10 Zn2 Zn1 131.4(4) . . ? O4 Zn2 Zn1 36.29(11) . . ? O3 Zn2 Zn1 127.4(2) 10_557 . ? O3 Zn2 Zn1 78.0(2) . . ? O10 Zn2 Zn1 131.4(4) . 10_557 ? O4 Zn2 Zn1 36.29(11) . 10_557 ? O3 Zn2 Zn1 78.0(2) 10_557 10_557 ? O3 Zn2 Zn1 127.4(2) . 10_557 ? Zn1 Zn2 Zn1 59.84(5) . 10_557 ? O11B Zn3 O4 101.5(7) . . ? O11B Zn3 O5 123.0(4) . 10_557 ? O4 Zn3 O5 104.6(3) . 10_557 ? O11B Zn3 O5 123.1(4) . . ? O4 Zn3 O5 104.6(3) . . ? O5 Zn3 O5 97.6(6) 10_557 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 17.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.182 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.076 data_UMCM_25NH2I _database_code_depnum_ccdc_archive 'CCDC 863175' #TrackingRef '- Revised CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.50 H18 I N0 O13 Zn4' _chemical_formula_weight 1136.96 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 41.345(2) _cell_length_b 41.345(2) _cell_length_c 17.5177(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25932(2) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.37 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.8967 _exptl_absorpt_correction_T_max 0.9294 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 119356 _diffrn_reflns_av_R_equivalents 0.1503 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.37 _reflns_number_total 16412 _reflns_number_gt 8786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was not refined as anisotropy to be consistent due to some disorder atoms. SQUEEZE found 6329 electrons that can be accounted to chloroform or DMF molecules. No hydrogen atom was added to C19 and C20 due to the disorder/ distortion of the ring. The neighbors of C24 has high Ueq probably due to the disorder. Amino groups cannot be located due to the disorder of halogen atoms. 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^)+(0.2000P)^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 'not measured' _refine_ls_number_reflns 16412 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.2640 _refine_ls_wR_factor_gt 0.2308 _refine_ls_goodness_of_fit_ref 0.775 _refine_ls_restrained_S_all 0.775 _refine_ls_shift/su_max 0.115 _refine_ls_shift/su_mean 0.090 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 -0.006 -0.005 -0.006 20831 6329 ' ' _platon_squeeze_details ; ; _refinement_detail ; ; 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 O1 O 0.36835(10) 0.42662(10) 0.2500 0.0338(9) Uiso 1 2 d S . . O6 O 0.29263(10) 0.40217(10) 0.3428(2) 0.0607(9) Uiso 1 1 d . . . O7 O 0.32976(10) 0.38640(9) 0.4059(2) 0.0594(9) Uiso 1 1 d . . . O5 O 0.32808(16) 0.47507(16) 0.2500 0.0723(15) Uiso 1 2 d S . . O2 O 0.43963(11) 0.48742(11) 0.3390(2) 0.0709(11) Uiso 1 1 d . . . O4 O 0.38937(15) 0.51194(15) 0.2500 0.0671(14) Uiso 1 2 d S . . O8 O 0.37328(10) 0.35602(10) 0.3134(2) 0.0622(10) Uiso 1 1 d . . . O3 O 0.41604(10) 0.43346(11) 0.3999(2) 0.0705(11) Uiso 1 1 d . . . C3 C 0.3719(2) 0.3063(2) 0.2500 0.068(2) Uiso 1 2 d S . . C1 C 0.30222(14) 0.39200(14) 0.4008(3) 0.0510(12) Uiso 1 1 d . . . C2 C 0.37259(19) 0.34170(19) 0.2500 0.0500(17) Uiso 1 2 d S . . C13 C 0.3565(2) 0.5069(2) 0.2500 0.0500(17) Uiso 1 2 d S . . C11 C 0.47108(14) 0.48441(15) 0.4458(3) 0.0556(13) Uiso 1 1 d . . . C14 C 0.3517(2) 0.5379(2) 0.2500 0.0581(19) Uiso 1 2 d S . . C10 C 0.43919(15) 0.46664(16) 0.3896(3) 0.0597(14) Uiso 1 1 d . . . C8 C 0.22062(17) 0.37289(17) 0.6802(4) 0.0732(17) Uiso 1 1 d . . . C4 C 0.28006(15) 0.38554(15) 0.4728(3) 0.0584(14) Uiso 1 1 d . . . C5 C 0.28432(17) 0.36700(17) 0.5310(4) 0.0790(18) Uiso 1 1 d . . . H5 H 0.3001 0.3566 0.5252 0.095 Uiso 1 1 calc R . . C6 C 0.26477(19) 0.36253(19) 0.6045(4) 0.089(2) Uiso 1 1 d . . . H6 H 0.2685 0.3503 0.6466 0.107 Uiso 1 1 calc R . . C9 C 0.2378(3) 0.3728(2) 0.7500 0.082(3) Uiso 1 2 d S . . H9 H 0.2608 0.3728 0.7500 0.098 Uiso 1 2 calc SR . . C12 C 0.4706(2) 0.4635(2) 0.5029(5) 0.103(2) Uiso 1 1 d . . . C7 C 0.24058(18) 0.37687(17) 0.6097(4) 0.0752(17) Uiso 1 1 d . . . C15 C 0.5001(2) 0.5210(2) 0.4364(5) 0.117(3) Uiso 1 1 d . . . C23 C 0.18650(18) 0.36940(17) 0.6810(4) 0.0770(17) Uiso 1 1 d . . . H23 H 0.1740 0.3665 0.6338 0.092 Uiso 1 1 calc R . . C21 C 0.1328(3) 0.3704(3) 0.7500 0.078(3) Uiso 1 2 d S . . C22 C 0.1680(3) 0.3699(2) 0.7500 0.077(2) Uiso 1 2 d S . . C18 C 0.25382(17) 0.39541(17) 0.4777(4) 0.0790(18) Uiso 1 1 d . . . H18 H 0.2485 0.4055 0.4339 0.095 Uiso 1 1 calc R . . C17 C 0.2344(2) 0.39147(18) 0.5433(4) 0.089(2) Uiso 1 1 d . . . H17 H 0.2161 0.3989 0.5437 0.107 Uiso 1 1 calc R . . C20 C 0.3669(3) 0.2533(3) 0.3163(6) 0.059(3) Uiso 0.50 1 d P . . C16 C 0.3791(4) 0.5712(4) 0.2500 0.133(5) Uiso 1 2 d S . . H16 H 0.4036 0.5745 0.2500 0.160 Uiso 1 2 calc SR . . I1 I 0.50858(11) 0.56011(12) 0.3536(2) 0.1155(12) Uiso 0.15 1 d P . . I2 I 0.4245(3) 0.4183(3) 0.5627(6) 0.285(4) Uiso 0.15 1 d P . . C26 C 0.3423(3) 0.6024(3) 0.2500 0.089(3) Uiso 1 2 d S . . C27 C 0.3378(3) 0.6364(3) 0.2500 0.075(2) Uiso 1 2 d S . . C28 C 0.3692(3) 0.6714(3) 0.2500 0.085(3) Uiso 1 2 d S . . H28 H 0.3936 0.6745 0.2500 0.103 Uiso 1 2 calc SR . . C25 C 0.3158(6) 0.5664(6) 0.2500 0.199(8) Uiso 1 2 d S . . H25 H 0.2909 0.5620 0.2500 0.239 Uiso 1 2 calc SR . . C24 C 0.3186(6) 0.5362(6) 0.2500 0.210(8) Uiso 1 2 d S . . H24 H 0.2964 0.5124 0.2500 0.252 Uiso 1 2 calc SR . . C29 C 0.3756(5) 0.6058(5) 0.2500 0.160(6) Uiso 1 2 d S . . H29 H 0.3973 0.6299 0.2500 0.192 Uiso 1 2 calc SR . . C19 C 0.3725(3) 0.2892(3) 0.3177(7) 0.086(3) Uiso 0.60 1 d P . . Zn2 Zn 0.371820(14) 0.400836(14) 0.34007(3) 0.03702(17) Uiso 1 1 d . . . Zn3 Zn 0.40753(2) 0.47751(2) 0.2500 0.0404(2) Uiso 1 2 d S . . Zn1 Zn 0.320104(19) 0.424654(19) 0.2500 0.0370(2) Uiso 1 2 d S . . _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 O1 Zn3 1.909(4) . ? O1 Zn2 1.949(2) 10_556 ? O1 Zn2 1.949(2) . ? O1 Zn1 1.955(4) . ? O6 C1 1.238(6) . ? O6 Zn1 1.934(4) . ? O7 C1 1.274(5) . ? O7 Zn2 1.916(4) . ? O5 C13 1.252(8) . ? O5 Zn1 1.941(6) . ? O2 C10 1.229(6) . ? O2 Zn3 1.954(4) . ? O4 C13 1.267(8) . ? O4 Zn3 1.913(5) . ? O8 C2 1.252(5) . ? O8 Zn2 1.941(3) . ? O3 C10 1.232(6) . ? O3 Zn2 1.947(4) . ? C3 C19 1.387(12) . ? C3 C19 1.387(12) 10_556 ? C3 C2 1.450(10) . ? C1 C4 1.502(7) . ? C2 O8 1.252(5) 10_556 ? C13 C14 1.394(10) . ? C11 C12 1.316(9) . ? C11 C15 1.393(9) . ? C11 C10 1.509(7) . ? C14 C16 1.272(14) . ? C14 C24 1.34(2) . ? C8 C23 1.344(8) . ? C8 C9 1.416(8) . ? C8 C7 1.447(8) . ? C4 C5 1.340(8) . ? C4 C18 1.340(7) . ? C5 C6 1.481(9) . ? C6 C7 1.397(8) . ? C9 C8 1.416(8) 10_557 ? C12 C15 1.494(11) 7_666 ? C12 I2 2.161(12) . ? C7 C17 1.391(8) . ? C15 C12 1.494(11) 7_666 ? C15 I1 2.066(10) . ? C23 C22 1.436(8) . ? C21 C20 1.374(11) 9_556 ? C21 C20 1.374(11) 6 ? C21 C22 1.466(12) . ? C22 C23 1.436(8) 10_557 ? C18 C17 1.364(9) . ? C20 C21 1.374(11) 8_556 ? C20 C19 1.381(14) . ? C16 C29 1.510(18) . ? I1 I2 2.853(11) 7_666 ? I2 I1 2.853(11) 7_666 ? C26 C29 1.313(15) . ? C26 C25 1.335(19) . ? C26 C27 1.509(13) . ? C27 C28 1.372(11) 3_565 ? C27 C28 1.379(11) . ? C28 C27 1.372(11) 2_665 ? C25 C24 1.31(2) . ? Zn2 Zn2 3.1557(10) 10_556 ? Zn3 O2 1.953(4) 10_556 ? Zn3 Zn1 3.1531(10) . ? Zn1 O6 1.934(4) 10_556 ? 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 Zn3 O1 Zn2 110.41(13) . 10_556 ? Zn3 O1 Zn2 110.41(13) . . ? Zn2 O1 Zn2 108.09(18) 10_556 . ? Zn3 O1 Zn1 109.37(18) . . ? Zn2 O1 Zn1 109.26(13) 10_556 . ? Zn2 O1 Zn1 109.26(13) . . ? C1 O6 Zn1 130.0(3) . . ? C1 O7 Zn2 131.0(3) . . ? C13 O5 Zn1 134.0(5) . . ? C10 O2 Zn3 131.2(4) . . ? C13 O4 Zn3 131.7(5) . . ? C2 O8 Zn2 131.3(4) . . ? C10 O3 Zn2 129.1(4) . . ? C19 C3 C19 117.5(12) . 10_556 ? C19 C3 C2 121.2(6) . . ? C19 C3 C2 121.2(6) 10_556 . ? O6 C1 O7 125.9(5) . . ? O6 C1 C4 118.6(5) . . ? O7 C1 C4 115.5(5) . . ? O8 C2 O8 125.0(7) . 10_556 ? O8 C2 C3 117.5(3) . . ? O8 C2 C3 117.5(3) 10_556 . ? O4 C13 O5 122.6(7) . . ? O4 C13 C14 119.0(7) . . ? O5 C13 C14 118.4(7) . . ? C12 C11 C15 121.7(6) . . ? C12 C11 C10 117.0(6) . . ? C15 C11 C10 121.3(6) . . ? C16 C14 C24 113.3(13) . . ? C16 C14 C13 122.2(10) . . ? C24 C14 C13 124.4(12) . . ? O3 C10 O2 128.0(6) . . ? O3 C10 C11 116.8(5) . . ? O2 C10 C11 115.2(5) . . ? C23 C8 C9 119.4(7) . . ? C23 C8 C7 122.0(6) . . ? C9 C8 C7 118.6(6) . . ? C5 C4 C18 118.9(6) . . ? C5 C4 C1 119.9(5) . . ? C18 C4 C1 121.0(5) . . ? C4 C5 C6 120.9(6) . . ? C7 C6 C5 117.8(7) . . ? C8 C9 C8 119.6(9) 10_557 . ? C11 C12 C15 121.2(7) . 7_666 ? C11 C12 I2 130.7(6) . . ? C15 C12 I2 101.6(6) 7_666 . ? C6 C7 C17 116.9(7) . . ? C6 C7 C8 119.8(6) . . ? C17 C7 C8 123.0(6) . . ? C11 C15 C12 117.0(7) . 7_666 ? C11 C15 I1 130.6(6) . . ? C12 C15 I1 112.4(6) 7_666 . ? C8 C23 C22 123.1(7) . . ? C20 C21 C20 115.5(11) 9_556 6 ? C20 C21 C22 121.6(6) 9_556 . ? C20 C21 C22 121.6(6) 6 . ? C23 C22 C23 114.6(8) . 10_557 ? C23 C22 C21 122.7(4) . . ? C23 C22 C21 122.7(4) 10_557 . ? C4 C18 C17 122.3(7) . . ? C18 C17 C7 122.2(7) . . ? C21 C20 C19 121.4(11) 8_556 . ? C14 C16 C29 124.6(13) . . ? C15 I1 I2 69.1(3) . 7_666 ? C12 I2 I1 71.3(4) . 7_666 ? C29 C26 C25 110.7(15) . . ? C29 C26 C27 120.7(12) . . ? C25 C26 C27 128.5(14) . . ? C28 C27 C28 123.2(11) 3_565 . ? C28 C27 C26 117.7(10) 3_565 . ? C28 C27 C26 119.1(10) . . ? C27 C28 C27 116.8(11) 2_665 . ? C24 C25 C26 130(2) . . ? C25 C24 C14 122(2) . . ? C26 C29 C16 119.4(14) . . ? C3 C19 C20 119.7(11) . . ? O7 Zn2 O8 107.70(15) . . ? O7 Zn2 O3 106.47(16) . . ? O8 Zn2 O3 108.91(16) . . ? O7 Zn2 O1 110.73(15) . . ? O8 Zn2 O1 111.91(15) . . ? O3 Zn2 O1 110.91(16) . . ? O7 Zn2 Zn2 127.00(11) . 10_556 ? O8 Zn2 Zn2 76.07(12) . 10_556 ? O3 Zn2 Zn2 122.53(12) . 10_556 ? O1 Zn2 Zn2 35.95(9) . 10_556 ? O1 Zn3 O4 112.8(2) . . ? O1 Zn3 O2 110.14(13) . 10_556 ? O4 Zn3 O2 108.80(14) . 10_556 ? O1 Zn3 O2 110.14(13) . . ? O4 Zn3 O2 108.80(15) . . ? O2 Zn3 O2 105.9(2) 10_556 . ? O1 Zn3 Zn1 35.80(11) . . ? O4 Zn3 Zn1 77.01(16) . . ? O2 Zn3 Zn1 124.64(12) 10_556 . ? O2 Zn3 Zn1 124.64(12) . . ? O6 Zn1 O6 114.4(2) . 10_556 ? O6 Zn1 O5 105.07(13) . . ? O6 Zn1 O5 105.07(13) 10_556 . ? O6 Zn1 O1 111.21(12) . . ? O6 Zn1 O1 111.21(12) 10_556 . ? O5 Zn1 O1 109.5(2) . . ? O6 Zn1 Zn3 121.83(11) . . ? O6 Zn1 Zn3 121.84(11) 10_556 . ? O5 Zn1 Zn3 74.65(17) . . ? O1 Zn1 Zn3 34.83(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.293 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.089 data_UMCM_Br _database_code_depnum_ccdc_archive 'CCDC 863176' #TrackingRef '- Revised CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H0 Br0.50 O13 Zn4' _chemical_formula_weight 1037.88 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' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 41.336(3) _cell_length_b 41.336(3) _cell_length_c 17.554(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25976(5) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9952 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 17.04 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3033 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.9051 _exptl_absorpt_correction_T_max 0.9353 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 306780 _diffrn_reflns_av_R_equivalents 0.1426 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.44 _reflns_number_total 16515 _reflns_number_gt 11001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was not refined as anisotropy to be consistent due to some disorder atoms. Squeez found 6187 electrons that can be accounted to chloroform and DMF molecules. No hydrogen was added to C7 c8 c10 and C11 due to disorder/distortion of the ring. 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^)+(0.1189P)^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 'not measured' _refine_ls_number_reflns 16515 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1190 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.1895 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.006 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 -0.007 -0.003 -0.005 20408 6187 ' ' _platon_squeeze_details ; ; _refinement_detail ; ; 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 0.028878(11) 0.400711(11) 0.66021(2) 0.03503(14) Uiso 1 1 d . . . Zn2 Zn 0.069414(17) 0.477786(17) 0.7500 0.03887(17) Uiso 1 2 d S . . Zn3 Zn 0.104463(16) 0.425117(16) 0.7500 0.03562(17) Uiso 1 2 d S . . O1 O 0.05793(9) 0.42665(9) 0.7500 0.0302(7) Uiso 1 2 d S . . O2 O 0.11006(8) 0.40353(8) 0.65719(16) 0.0584(8) Uiso 1 1 d . . . O3 O 0.05669(8) 0.38653(8) 0.59412(17) 0.0582(8) Uiso 1 1 d . . . O4 O 0.04743(8) 0.48773(9) 0.66194(17) 0.0613(8) Uiso 1 1 d . . . O5 O 0.01674(8) 0.43346(8) 0.60177(17) 0.0613(8) Uiso 1 1 d . . . O6 O 0.14645(14) 0.47583(14) 0.7500 0.0754(13) Uiso 1 2 d S . . O7 O 0.12177(13) 0.51259(12) 0.7500 0.0655(12) Uiso 1 2 d S . . O8 O -0.01683(8) 0.35645(8) 0.68629(17) 0.0593(8) Uiso 1 1 d . . . C1 C 0.02755(12) 0.46736(12) 0.6104(2) 0.0541(11) Uiso 1 1 d . . . C2 C 0.01281(12) 0.48387(12) 0.5537(2) 0.0539(11) Uiso 1 1 d . . . C3B C 0.0141(3) 0.5181(3) 0.5712(6) 0.058(3) Uiso 0.50 1 d P . 2 C4A C 0.0003(3) 0.4671(3) 0.4820(6) 0.064(3) Uiso 0.50 1 d P . 2 Br1 Br 0.0276(2) 0.5444(2) 0.6684(4) 0.0643(19) Uiso 0.06 1 d P A 2 Br3 Br -0.0041(3) 0.4206(3) 0.4421(5) 0.079(2) Uiso 0.06 1 d P B 2 C3A C 0.0283(3) 0.5216(3) 0.5484(6) 0.065(3) Uiso 0.50 1 d P . 1 C4B C -0.0148(3) 0.4618(3) 0.5031(6) 0.060(3) Uiso 0.50 1 d P . 1 Br2 Br -0.0433(3) 0.4072(3) 0.4935(7) 0.103(3) Uiso 0.06 1 d P C 1 Br4 Br 0.0568(3) 0.5604(3) 0.6365(6) 0.089(3) Uiso 0.06 1 d P D 1 C5 C 0.14954(17) 0.50753(17) 0.7500 0.0520(15) Uiso 1 2 d S . . C12 C 0.2978(2) 0.6358(2) 0.7500 0.076(2) Uiso 1 2 d S . . C13 C 0.3028(2) 0.6723(2) 0.7500 0.077(2) Uiso 1 2 d S . . H13 H 0.2818 0.6758 0.7500 0.092 Uiso 1 2 calc SR . . C14 C 0.09000(12) 0.39234(11) 0.5986(2) 0.0493(10) Uiso 1 1 d . . . C15 C 0.10570(12) 0.38596(12) 0.5281(2) 0.0526(11) Uiso 1 1 d . . . C16 C 0.14287(15) 0.39694(14) 0.5248(3) 0.0752(14) Uiso 1 1 d . . . H16 H 0.1582 0.4070 0.5686 0.090 Uiso 1 1 calc R . . C17 C 0.15849(16) 0.39317(15) 0.4552(3) 0.0834(16) Uiso 1 1 d . . . H17 H 0.1844 0.4012 0.4526 0.100 Uiso 1 1 calc R . . C18 C 0.13654(14) 0.37807(14) 0.3922(3) 0.0685(13) Uiso 1 1 d . . . C19 C 0.09894(16) 0.36516(16) 0.3984(3) 0.0849(16) Uiso 1 1 d . . . H19 H 0.0832 0.3534 0.3558 0.102 Uiso 1 1 calc R . . C20 C 0.08315(16) 0.36910(15) 0.4672(3) 0.0811(15) Uiso 1 1 d . . . H20 H 0.0571 0.3600 0.4707 0.097 Uiso 1 1 calc R . . C21 C 0.15308(14) 0.37488(14) 0.3200(3) 0.0698(14) Uiso 1 1 d . . . C22 C 0.1363(2) 0.3760(2) 0.2500 0.073(2) Uiso 1 2 d S . . H22 H 0.1140 0.3774 0.2500 0.088 Uiso 1 2 calc SR . . C23 C 0.18564(14) 0.37275(13) 0.3192(3) 0.0677(13) Uiso 1 1 d . . . H23 H 0.1969 0.3721 0.3659 0.081 Uiso 1 1 calc R . . C24 C -0.03091(15) 0.34212(16) 0.7500 0.0442(13) Uiso 1 2 d S . . C25 C -0.06582(17) 0.30577(17) 0.7500 0.0529(15) Uiso 1 2 d S . . C26A C -0.0766(3) 0.2818(2) 0.6889(5) 0.057(2) Uiso 0.50 1 d P E 2 H26A H -0.0606 0.2885 0.6458 0.068 Uiso 0.50 1 calc PR E 2 C26B C -0.1093(2) 0.2487(2) 0.6882(5) 0.054(2) Uiso 0.50 1 d P E 2 H26B H -0.1157 0.2329 0.6450 0.064 Uiso 0.50 1 calc PR E 2 C27A C -0.0892(2) 0.2956(2) 0.6862(5) 0.050(2) Uiso 0.50 1 d P E 1 H27A H -0.0822 0.3119 0.6435 0.060 Uiso 0.50 1 calc PR E 1 C27B C -0.1224(2) 0.2622(2) 0.6850(5) 0.050(2) Uiso 0.50 1 d P E 1 H27B H -0.1379 0.2552 0.6411 0.060 Uiso 0.50 1 calc PR E 1 C28 C -0.13363(19) 0.23786(19) 0.7500 0.0627(17) Uiso 1 2 d S . . C29 C 0.20196(19) 0.37159(19) 0.2500 0.0638(17) Uiso 1 2 d S . . C6 C 0.18745(19) 0.54042(19) 0.7500 0.0648(18) Uiso 1 2 d S . . C9 C 0.2587(2) 0.6023(2) 0.7500 0.084(2) Uiso 1 2 d S . . C7 C 0.1925(4) 0.5748(4) 0.7500 0.058(3) Uiso 0.50 2 d SP . . C8 C 0.2270(4) 0.6045(4) 0.7500 0.071(4) Uiso 0.50 2 d SP . . C11 C 0.2180(4) 0.5377(4) 0.7193(7) 0.037(3) Uiso 0.25 1 d P . . C10 C 0.2511(3) 0.5679(3) 0.7182(6) 0.078(3) Uiso 0.50 1 d P . . _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 O8 1.916(3) . ? Zn1 O3 1.920(3) . ? Zn1 O1 1.9466(19) . ? Zn1 O5 1.954(3) . ? Zn1 Zn1 3.1525(10) 10_557 ? Zn2 O7 1.908(5) . ? Zn2 O1 1.921(3) . ? Zn2 O4 1.938(3) 10_557 ? Zn2 O4 1.939(3) . ? Zn3 O2 1.926(3) . ? Zn3 O2 1.926(3) 10_557 ? Zn3 O6 1.941(5) . ? Zn3 O1 1.956(3) . ? O1 Zn1 1.9465(19) 10_557 ? O2 C14 1.255(5) . ? O3 C14 1.276(5) . ? O4 C1 1.229(5) . ? O5 C1 1.249(5) . ? O6 C5 1.251(7) . ? O7 C5 1.265(7) . ? O8 C24 1.263(4) . ? C1 C2 1.498(6) . ? C2 C3A 1.362(11) . ? C2 C4B 1.371(11) . ? C2 C4A 1.403(11) . ? C2 C3B 1.422(11) . ? C3B C4A 1.404(13) 7_566 ? C3B Br1 1.948(13) . ? C4A C3B 1.404(13) 7_566 ? C4A Br3 1.968(14) . ? C3A C4B 1.407(14) 7_566 ? C3A Br4 2.112(15) . ? C4B C3A 1.407(14) 7_566 ? C4B Br2 1.964(15) . ? C5 C6 1.474(9) . ? C12 C13 1.357(9) 2_665 ? C12 C13 1.416(9) . ? C12 C9 1.516(11) . ? C13 C12 1.357(9) 3_565 ? C14 C15 1.482(6) . ? C15 C20 1.359(7) . ? C15 C16 1.369(6) . ? C16 C17 1.426(7) . ? C17 C18 1.368(7) . ? C18 C19 1.372(7) . ? C18 C21 1.476(7) . ? C19 C20 1.421(7) . ? C21 C23 1.392(7) . ? C21 C22 1.424(6) . ? C22 C21 1.424(6) 10_556 ? C23 C29 1.402(6) . ? C24 O8 1.263(4) 10_557 ? C24 C25 1.474(8) . ? C25 C26A 1.375(9) 10_557 ? C25 C26A 1.375(9) . ? C25 C27A 1.401(9) 10_557 ? C25 C27A 1.401(9) . ? C26A C26B 1.361(11) . ? C26B C28 1.391(9) . ? C27A C27B 1.377(11) . ? C27B C28 1.435(9) . ? C28 C26B 1.391(9) 10_557 ? C28 C27B 1.435(9) 10_557 ? C28 C29 1.486(9) 9_556 ? C29 C23 1.402(6) 10_556 ? C29 C28 1.486(9) 8_556 ? C6 C7 1.329(14) . ? C6 C11 1.427(15) . ? C6 C11 1.427(15) 10_557 ? C9 C8 1.359(15) . ? C9 C10 1.409(11) 10_557 ? C9 C10 1.409(11) . ? C7 C8 1.339(18) . ? C11 C11 1.08(3) 10_557 ? C11 C10 1.314(16) . ? C11 C10 1.712(16) 10_557 ? C10 C10 1.12(2) 10_557 ? C10 C11 1.712(16) 10_557 ? 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 O8 Zn1 O3 107.95(13) . . ? O8 Zn1 O1 112.01(12) . . ? O3 Zn1 O1 111.02(12) . . ? O8 Zn1 O5 108.35(13) . . ? O3 Zn1 O5 107.15(13) . . ? O1 Zn1 O5 110.18(13) . . ? O8 Zn1 Zn1 76.17(9) . 10_557 ? O3 Zn1 Zn1 127.18(9) . 10_557 ? O1 Zn1 Zn1 35.93(8) . 10_557 ? O5 Zn1 Zn1 121.67(9) . 10_557 ? O7 Zn2 O1 113.12(17) . . ? O7 Zn2 O4 108.39(12) . 10_557 ? O1 Zn2 O4 110.44(10) . 10_557 ? O7 Zn2 O4 108.39(12) . . ? O1 Zn2 O4 110.44(10) . . ? O4 Zn2 O4 105.77(18) 10_557 . ? O2 Zn3 O2 115.51(18) . 10_557 ? O2 Zn3 O6 104.52(12) . . ? O2 Zn3 O6 104.52(12) 10_557 . ? O2 Zn3 O1 111.27(10) . . ? O2 Zn3 O1 111.28(10) 10_557 . ? O6 Zn3 O1 109.12(17) . . ? Zn2 O1 Zn1 110.55(10) . 10_557 ? Zn2 O1 Zn1 110.55(10) . . ? Zn1 O1 Zn1 108.15(15) 10_557 . ? Zn2 O1 Zn3 109.26(15) . . ? Zn1 O1 Zn3 109.15(10) 10_557 . ? Zn1 O1 Zn3 109.15(10) . . ? C14 O2 Zn3 130.8(3) . . ? C14 O3 Zn1 131.3(3) . . ? C1 O4 Zn2 131.7(3) . . ? C1 O5 Zn1 130.0(3) . . ? C5 O6 Zn3 134.3(4) . . ? C5 O7 Zn2 131.0(4) . . ? C24 O8 Zn1 131.5(3) . . ? O4 C1 O5 126.8(4) . . ? O4 C1 C2 117.5(4) . . ? O5 C1 C2 115.6(4) . . ? C3A C2 C4B 118.4(7) . . ? C3A C2 C4A 110.5(7) . . ? C4B C2 C4A 27.6(5) . . ? C3A C2 C3B 27.5(5) . . ? C4B C2 C3B 114.0(7) . . ? C4A C2 C3B 120.4(7) . . ? C3A C2 C1 120.1(6) . . ? C4B C2 C1 121.4(6) . . ? C4A C2 C1 120.2(6) . . ? C3B C2 C1 119.2(5) . . ? C4A C3B C2 118.4(8) 7_566 . ? C4A C3B Br1 113.9(8) 7_566 . ? C2 C3B Br1 127.1(7) . . ? C3B C4A C2 120.9(9) 7_566 . ? C3B C4A Br3 109.7(8) 7_566 . ? C2 C4A Br3 129.2(7) . . ? C2 C3A C4B 121.8(9) . 7_566 ? C2 C3A Br4 125.7(7) . . ? C4B C3A Br4 107.9(8) 7_566 . ? C2 C4B C3A 119.6(9) . 7_566 ? C2 C4B Br2 129.9(8) . . ? C3A C4B Br2 110.4(8) 7_566 . ? O6 C5 O7 123.1(6) . . ? O6 C5 C6 118.1(6) . . ? O7 C5 C6 118.8(6) . . ? C13 C12 C13 120.7(9) 2_665 . ? C13 C12 C9 119.7(8) 2_665 . ? C13 C12 C9 119.6(8) . . ? C12 C13 C12 119.3(9) 3_565 . ? O2 C14 O3 124.9(4) . . ? O2 C14 C15 118.9(4) . . ? O3 C14 C15 116.2(4) . . ? C20 C15 C16 120.3(5) . . ? C20 C15 C14 119.9(4) . . ? C16 C15 C14 119.7(4) . . ? C15 C16 C17 119.7(5) . . ? C18 C17 C16 120.6(5) . . ? C17 C18 C19 118.5(5) . . ? C17 C18 C21 120.2(5) . . ? C19 C18 C21 121.2(5) . . ? C18 C19 C20 121.2(6) . . ? C15 C20 C19 119.4(5) . . ? C23 C21 C22 119.7(5) . . ? C23 C21 C18 121.4(5) . . ? C22 C21 C18 118.8(5) . . ? C21 C22 C21 119.4(7) 10_556 . ? C21 C23 C29 120.5(5) . . ? O8 C24 O8 124.6(5) 10_557 . ? O8 C24 C25 117.7(3) 10_557 . ? O8 C24 C25 117.7(3) . . ? C26A C25 C26A 102.6(9) 10_557 . ? C26A C25 C27A 40.0(4) 10_557 10_557 ? C26A C25 C27A 118.8(7) . 10_557 ? C26A C25 C27A 118.8(7) 10_557 . ? C26A C25 C27A 40.0(4) . . ? C27A C25 C27A 106.3(8) 10_557 . ? C26A C25 C24 122.3(5) 10_557 . ? C26A C25 C24 122.3(5) . . ? C27A C25 C24 118.9(5) 10_557 . ? C27A C25 C24 118.9(5) . . ? C26B C26A C25 122.1(8) . . ? C26A C26B C28 120.9(8) . . ? C27B C27A C25 120.3(8) . . ? C27A C27B C28 120.1(8) . . ? C26B C28 C26B 102.5(9) 10_557 . ? C26B C28 C27B 117.7(7) 10_557 . ? C26B C28 C27B 39.2(4) . . ? C26B C28 C27B 39.2(4) 10_557 10_557 ? C26B C28 C27B 117.7(7) . 10_557 ? C27B C28 C27B 105.3(8) . 10_557 ? C26B C28 C29 121.6(5) 10_557 9_556 ? C26B C28 C29 121.6(5) . 9_556 ? C27B C28 C29 120.7(5) . 9_556 ? C27B C28 C29 120.7(5) 10_557 9_556 ? C23 C29 C23 120.1(7) . 10_556 ? C23 C29 C28 119.9(3) . 8_556 ? C23 C29 C28 119.9(3) 10_556 8_556 ? C7 C6 C11 114.3(9) . . ? C7 C6 C11 114.3(9) . 10_557 ? C11 C6 C11 44.4(11) . 10_557 ? C7 C6 C5 120.8(8) . . ? C11 C6 C5 120.0(8) . . ? C11 C6 C5 120.0(8) 10_557 . ? C8 C9 C10 109.5(9) . 10_557 ? C8 C9 C10 109.5(9) . . ? C10 C9 C10 46.7(8) 10_557 . ? C8 C9 C12 124.1(9) . . ? C10 C9 C12 121.3(8) 10_557 . ? C10 C9 C12 121.3(8) . . ? C6 C7 C8 120.5(12) . . ? C9 C8 C7 123.8(13) . . ? C11 C11 C10 90.9(7) 10_557 . ? C11 C11 C6 67.8(5) 10_557 . ? C10 C11 C6 118.3(11) . . ? C11 C11 C10 50.1(6) 10_557 10_557 ? C10 C11 C10 40.8(8) . 10_557 ? C6 C11 C10 96.7(9) . 10_557 ? C10 C10 C11 89.1(7) 10_557 . ? C10 C10 C9 66.6(4) 10_557 . ? C11 C10 C9 123.5(11) . . ? C10 C10 C11 50.1(5) 10_557 10_557 ? C11 C10 C11 39.0(10) . 10_557 ? C9 C10 C11 100.0(8) . 10_557 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.094 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.069 data_UMCM_Dioxole _database_code_depnum_ccdc_archive 'CCDC 863177' #TrackingRef '- Revised CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H0 O13 Zn4' _chemical_formula_weight 997.92 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' O O 0.0106 0.0060 '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 ? _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 41.367(4) _cell_length_b 41.367(4) _cell_length_c 17.5389(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25992(4) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.9204 _exptl_absorpt_correction_T_max 0.9459 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 239509 _diffrn_reflns_av_R_equivalents 0.1256 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.37 _reflns_number_total 16465 _reflns_number_gt 10021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was not refined as anisotropy to be consistent due to some disorder atoms. SQUEEZE found 6181 electrons that can be accounted for chloroform or DMF molecules. Due to bad disorders, only one oxygen (O10) of the dioxole can be clearly located. Other carbon atoms belonged to the BDC ligand also have disorder. Zn3 was refined as anisotropy because there is a huge eletron density close to Zn3 if Zn3 was refined isotropy. The neighbors of C17, C19, C27 have high Ueq because of the disorders. 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^)+(0.2000P)^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 'not measured' _refine_ls_number_reflns 16465 _refine_ls_number_parameters 149 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.2385 _refine_ls_wR_factor_gt 0.1981 _refine_ls_goodness_of_fit_ref 0.780 _refine_ls_restrained_S_all 0.781 _refine_ls_shift/su_max 0.110 _refine_ls_shift/su_mean 0.068 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 -0.006 -0.004 -0.010 21487 6181 ' ' _platon_squeeze_details ; ; _refinement_detail ; ; 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 O6 O 0.36811(8) 0.42618(9) 0.2500 0.0321(7) Uiso 1 2 d S . . O3 O 0.29306(8) 0.40329(8) 0.34316(17) 0.0604(8) Uiso 1 1 d . . . O4 O 0.32986(8) 0.38715(8) 0.40714(17) 0.0600(8) Uiso 1 1 d . . . O2 O 0.32915(13) 0.47571(13) 0.2500 0.0705(12) Uiso 1 2 d S . . O1 O 0.38980(14) 0.51216(13) 0.2500 0.0763(13) Uiso 1 2 d S . . O5 O 0.37307(8) 0.35645(8) 0.31307(17) 0.0612(8) Uiso 1 1 d . . . O8 O 0.44058(10) 0.48789(9) 0.33765(19) 0.0744(9) Uiso 1 1 d . . . O7 O 0.41669(9) 0.43314(9) 0.39781(18) 0.0684(9) Uiso 1 1 d . . . C14 C 0.37324(15) 0.34216(15) 0.2500 0.0423(13) Uiso 1 2 d S . . C12 C 0.37218(18) 0.30685(18) 0.2500 0.0583(16) Uiso 1 2 d S . . C3 C 0.30209(11) 0.39265(11) 0.4022(2) 0.0501(10) Uiso 1 1 d . . . C1 C 0.35767(17) 0.50707(16) 0.2500 0.0501(14) Uiso 1 2 d S . . C4 C 0.28087(13) 0.38668(13) 0.4721(3) 0.0615(12) Uiso 1 1 d . . . C2 C 0.43997(14) 0.46734(15) 0.3880(3) 0.0714(14) Uiso 1 1 d D . . C10 C 0.22146(15) 0.37416(15) 0.6789(3) 0.0794(15) Uiso 1 1 d . . . C9 C 0.26572(16) 0.36568(16) 0.6013(4) 0.0884(17) Uiso 1 1 d . . . H9 H 0.2697 0.3541 0.6428 0.106 Uiso 1 1 calc R . . C11 C 0.2397(2) 0.3750(2) 0.7500 0.083(2) Uiso 1 2 d S . . C8 C 0.24141(14) 0.37833(14) 0.6079(3) 0.0679(13) Uiso 1 1 d . . . C13 C 0.3531(2) 0.5396(2) 0.2500 0.0679(18) Uiso 1 2 d SD . . C7 C 0.23487(17) 0.39352(16) 0.5442(4) 0.0927(17) Uiso 1 1 d . . . H7 H 0.2173 0.4013 0.5465 0.111 Uiso 1 1 calc R . . C6 C 0.25395(15) 0.39759(15) 0.4762(3) 0.0810(15) Uiso 1 1 d . . . H6 H 0.2488 0.4076 0.4335 0.097 Uiso 1 1 calc R . . C5 C 0.28511(16) 0.36964(15) 0.5328(3) 0.0860(16) Uiso 1 1 d . . . H5 H 0.3013 0.3602 0.5298 0.103 Uiso 1 1 calc R . . C15 C 0.37236(14) 0.18549(14) 0.3213(3) 0.0717(14) Uiso 1 1 d . . . C16 C 0.3710(2) 0.2021(2) 0.2500 0.080(2) Uiso 1 2 d S . . C20 C 0.3423(2) 0.6024(2) 0.2500 0.080(2) Uiso 1 2 d SD . . C22 C 0.3675(2) 0.6713(2) 0.2500 0.088(2) Uiso 1 2 d S . . H22 H 0.3914 0.6745 0.2500 0.105 Uiso 1 2 calc SR . . C21 C 0.3381(2) 0.6358(2) 0.2500 0.080(2) Uiso 1 2 d S . . C23 C 0.4722(2) 0.4853(2) 0.4470(5) 0.119(2) Uiso 1 1 d D . . C18 C 0.3813(3) 0.5743(3) 0.2500 0.132(4) Uiso 1 2 d SD . . H18 H 0.4056 0.5785 0.2500 0.159 Uiso 1 2 calc SR . . C19 C 0.3757(4) 0.6038(4) 0.2500 0.164(5) Uiso 1 2 d SD . . H19 H 0.3969 0.6274 0.2500 0.197 Uiso 1 2 calc SR . . C17 C 0.3190(4) 0.5355(4) 0.2500 0.179(6) Uiso 1 2 d SD . . H17 H 0.2976 0.5121 0.2500 0.215 Uiso 1 2 calc SR . . C26 C 0.3723(2) 0.2900(2) 0.3143(5) 0.140(3) Uiso 1 1 d . . . H26 H 0.3729 0.3009 0.3610 0.168 Uiso 1 1 calc R . . C27 C 0.3715(3) 0.2546(3) 0.3118(6) 0.161(3) Uiso 1 1 d . . . H27 H 0.3717 0.2436 0.3578 0.193 Uiso 1 1 calc R . . C28 C 0.3166(4) 0.5698(4) 0.2500 0.156(5) Uiso 1 2 d SD . . H28 H 0.2926 0.5664 0.2500 0.187 Uiso 1 2 calc SR . . C29 C 0.37063(19) 0.2375(2) 0.2500 0.0659(18) Uiso 1 2 d S . . C24 C 0.4686(4) 0.4715(4) 0.5137(7) 0.105(4) Uiso 0.50 1 d PD . . H24 H 0.4481 0.4477 0.5201 0.127 Uiso 0.50 1 calc PR . . C25 C 0.5068(4) 0.5119(4) 0.4150(9) 0.117(5) Uiso 0.50 1 d PD . . O10 O 0.5176(6) 0.5231(6) 0.3372(11) 0.143(8) Uiso 0.25 1 d PD . . Zn1 Zn 0.371745(12) 0.400891(12) 0.33981(2) 0.03782(15) Uiso 1 1 d . . . Zn2 Zn 0.320469(16) 0.425235(16) 0.2500 0.03683(18) Uiso 1 2 d S . . Zn3 Zn 0.408216(17) 0.477692(17) 0.2500 0.0466(2) Uani 1 2 d S . . 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 Zn3 0.0309(3) 0.0410(4) 0.0676(5) 0.000 0.000 0.0177(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 O6 Zn1 1.9379(18) 10_556 ? O6 Zn1 1.9379(18) . ? O6 Zn3 1.939(3) . ? O6 Zn2 1.951(3) . ? O3 C3 1.253(5) . ? O3 Zn2 1.937(3) . ? O4 C3 1.281(5) . ? O4 Zn1 1.933(3) . ? O2 C1 1.243(7) . ? O2 Zn2 1.934(5) . ? O1 C1 1.237(7) . ? O1 Zn3 1.924(5) . ? O5 C14 1.256(4) . ? O5 Zn1 1.924(3) . ? O8 C2 1.217(6) . ? O8 Zn3 1.941(3) . ? O7 C2 1.263(6) . ? O7 Zn1 1.947(3) . ? C14 O5 1.256(4) 10_556 ? C14 C12 1.439(8) . ? C12 C26 1.327(9) 10_556 ? C12 C26 1.327(9) . ? C3 C4 1.455(6) . ? C1 C13 1.451(9) . ? C4 C5 1.337(7) . ? C4 C6 1.397(6) . ? C2 C23 1.552(9) . ? C10 C15 1.395(7) 9_556 ? C10 C11 1.449(7) . ? C10 C8 1.455(7) . ? C9 C8 1.351(7) . ? C9 C5 1.407(7) . ? C11 C10 1.449(7) 10_557 ? C8 C7 1.374(7) . ? C13 C18 1.322(12) . ? C13 C17 1.336(15) . ? C7 C6 1.394(8) . ? C15 C10 1.395(7) 8_556 ? C15 C16 1.442(6) . ? C16 C29 1.474(10) . ? C16 C15 1.442(6) 10_556 ? C20 C28 1.230(13) . ? C20 C19 1.356(14) . ? C20 C21 1.476(11) . ? C22 C21 1.359(10) . ? C22 C21 1.356(10) 2_665 ? C21 C22 1.356(10) 3_565 ? C23 C24 1.278(11) . ? C23 C25 1.413(15) . ? C18 C19 1.351(15) . ? C17 C28 1.468(16) . ? C26 C27 1.449(10) . ? C27 C29 1.283(9) . ? C29 C27 1.283(9) 10_556 ? C24 C25 1.539(18) 7_666 ? C25 O10 1.438(15) . ? C25 C24 1.539(18) 7_666 ? Zn1 Zn1 3.1502(9) 10_556 ? Zn2 O3 1.937(3) 10_556 ? Zn3 O8 1.941(3) 10_556 ? 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 Zn1 O6 Zn1 108.74(15) 10_556 . ? Zn1 O6 Zn3 109.79(10) 10_556 . ? Zn1 O6 Zn3 109.79(10) . . ? Zn1 O6 Zn2 109.84(10) 10_556 . ? Zn1 O6 Zn2 109.84(10) . . ? Zn3 O6 Zn2 108.83(15) . . ? C3 O3 Zn2 130.9(3) . . ? C3 O4 Zn1 131.2(3) . . ? C1 O2 Zn2 133.9(4) . . ? C1 O1 Zn3 131.6(4) . . ? C14 O5 Zn1 132.4(3) . . ? C2 O8 Zn3 130.7(4) . . ? C2 O7 Zn1 128.9(3) . . ? O5 C14 O5 123.5(5) . 10_556 ? O5 C14 C12 118.2(3) . . ? O5 C14 C12 118.2(3) 10_556 . ? C26 C12 C26 116.4(10) 10_556 . ? C26 C12 C14 121.8(5) 10_556 . ? C26 C12 C14 121.8(5) . . ? O3 C3 O4 124.7(4) . . ? O3 C3 C4 119.7(4) . . ? O4 C3 C4 115.6(4) . . ? O1 C1 O2 123.8(6) . . ? O1 C1 C13 118.0(6) . . ? O2 C1 C13 118.2(6) . . ? C5 C4 C6 117.7(5) . . ? C5 C4 C3 122.3(5) . . ? C6 C4 C3 120.0(4) . . ? O8 C2 O7 128.2(5) . . ? O8 C2 C23 115.9(5) . . ? O7 C2 C23 115.9(5) . . ? C15 C10 C11 120.7(6) 9_556 . ? C15 C10 C8 120.6(5) 9_556 . ? C11 C10 C8 118.4(5) . . ? C8 C9 C5 121.3(6) . . ? C10 C11 C10 118.8(7) 10_557 . ? C9 C8 C7 117.5(5) . . ? C9 C8 C10 121.0(5) . . ? C7 C8 C10 121.4(5) . . ? C18 C13 C17 116.2(11) . . ? C18 C13 C1 123.6(8) . . ? C17 C13 C1 120.2(9) . . ? C8 C7 C6 121.5(6) . . ? C7 C6 C4 120.0(5) . . ? C4 C5 C9 121.6(5) . . ? C10 C15 C16 119.7(5) 8_556 . ? C29 C16 C15 119.8(3) . . ? C29 C16 C15 119.8(3) . 10_556 ? C15 C16 C15 120.4(7) . 10_556 ? C28 C20 C19 110.6(11) . . ? C28 C20 C21 125.9(10) . . ? C19 C20 C21 123.5(10) . . ? C21 C22 C21 124.3(9) . 2_665 ? C22 C21 C22 115.7(9) . 3_565 ? C22 C21 C20 123.6(8) . . ? C22 C21 C20 120.8(8) 3_565 . ? C24 C23 C25 123.8(11) . . ? C24 C23 C2 121.1(9) . . ? C25 C23 C2 113.7(9) . . ? C13 C18 C19 121.5(12) . . ? C18 C19 C20 126.3(13) . . ? C13 C17 C28 117.0(13) . . ? C12 C26 C27 120.1(9) . . ? C29 C27 C26 124.2(10) . . ? C20 C28 C17 128.3(14) . . ? C27 C29 C27 115.2(11) . 10_556 ? C27 C29 C16 122.4(6) . . ? C27 C29 C16 122.4(6) 10_556 . ? C23 C24 C25 129.8(12) . 7_666 ? O10 C25 C23 131.0(16) . . ? O10 C25 C24 126.7(16) . 7_666 ? C23 C25 C24 102.2(11) . 7_666 ? O5 Zn1 O6 111.39(12) . . ? O5 Zn1 O4 108.51(13) . . ? O6 Zn1 O4 110.81(12) . . ? O5 Zn1 O7 107.95(13) . . ? O6 Zn1 O7 111.11(13) . . ? O4 Zn1 O7 106.91(13) . . ? O5 Zn1 Zn1 75.90(9) . 10_556 ? O6 Zn1 Zn1 35.63(7) . 10_556 ? O4 Zn1 Zn1 127.66(9) . 10_556 ? O7 Zn1 Zn1 121.50(9) . 10_556 ? O3 Zn2 O3 115.08(18) . 10_556 ? O3 Zn2 O2 104.79(11) . . ? O3 Zn2 O2 104.79(11) 10_556 . ? O3 Zn2 O6 110.98(10) . . ? O3 Zn2 O6 110.98(10) 10_556 . ? O2 Zn2 O6 109.75(16) . . ? O1 Zn3 O8 108.94(13) . 10_556 ? O1 Zn3 O8 108.94(13) . . ? O8 Zn3 O8 104.7(2) 10_556 . ? O1 Zn3 O6 112.11(17) . . ? O8 Zn3 O6 110.92(12) 10_556 . ? O8 Zn3 O6 110.92(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.007 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.066 data_UMCM_OAllyl _database_code_depnum_ccdc_archive 'CCDC 863178' #TrackingRef '- Revised CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H0 O15 Zn4' _chemical_formula_weight 1053.94 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' O O 0.0106 0.0060 '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 ? _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 41.351(4) _cell_length_b 41.351(4) _cell_length_c 17.5266(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25953(4) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9960 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.33 _exptl_crystal_description needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.7652 _exptl_absorpt_correction_T_max 0.9456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 16412 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.37 _reflns_number_total 16412 _reflns_number_gt 9344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was not refined as anisotropy to be consistent due to some disorder atoms. No hydrogen atom was added to C15 and C16 due to the bad distortion/ disorder. SQUEEZE found 6588 electrons that can be accounted to the chlorofom and DMF molecules. The neighbors of C16 and C9 have high Ueq becaus of the disorders. 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^)+(0.2000P)^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 'not measured' _refine_ls_number_reflns 16412 _refine_ls_number_parameters 156 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1960 _refine_ls_wR_factor_gt 0.1790 _refine_ls_goodness_of_fit_ref 0.624 _refine_ls_restrained_S_all 0.624 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 -0.006 -0.005 -0.007 21239 6588 ' ' _platon_squeeze_details ; ; _refine_detail ; ; 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 0.400668(9) 0.028778(9) 0.339847(18) 0.03762(12) Uiso 1 1 d . . . Zn2 Zn 0.477432(14) 0.069213(14) 0.2500 0.04320(15) Uiso 1 2 d S . . Zn3 Zn 0.424957(13) 0.104418(13) 0.2500 0.03887(14) Uiso 1 2 d S . . O1 O 0.42660(7) 0.05810(7) 0.2500 0.0340(6) Uiso 1 2 d S . . O2 O 0.35595(7) -0.01651(7) 0.31301(14) 0.0622(6) Uiso 1 1 d . . . O3 O 0.43300(7) 0.01646(7) 0.39771(14) 0.0666(7) Uiso 1 1 d . . . O4 O 0.48785(7) 0.04751(7) 0.33825(14) 0.0679(7) Uiso 1 1 d . . . O5 O 0.4235(6) -0.0285(6) 0.5156(14) 0.643(13) Uiso 1 1 d . . . O6 O 0.51252(10) 0.12197(10) 0.2500 0.0713(10) Uiso 1 2 d S . . O7 O 0.47618(12) 0.14687(11) 0.2500 0.0822(11) Uiso 1 2 d S . . O8 O 0.40331(7) 0.11012(7) 0.34323(13) 0.0608(6) Uiso 1 1 d . . . O9 O 0.38618(7) 0.05655(7) 0.40573(13) 0.0623(6) Uiso 1 1 d . . . C1 C 0.34098(13) -0.03075(12) 0.2500 0.0465(10) Uiso 1 2 d S . . C2 C 0.30494(14) -0.06543(14) 0.2500 0.0559(12) Uiso 1 2 d S . . C3A C 0.2817(2) -0.0757(2) 0.3121(4) 0.062(2) Uiso 0.542(7) 1 d P A 1 H3A H 0.2892 -0.0608 0.3555 0.075 Uiso 0.542(7) 1 calc PR A 1 C3B C 0.2951(2) -0.0882(2) 0.3140(4) 0.050(2) Uiso 0.458(7) 1 d P A 2 H3B H 0.3105 -0.0807 0.3567 0.060 Uiso 0.458(7) 1 calc PR A 2 C4A C 0.2470(2) -0.1083(2) 0.3108(4) 0.071(2) Uiso 0.542(7) 1 d P A 1 H4A H 0.2309 -0.1137 0.3519 0.085 Uiso 0.542(7) 1 calc PR A 1 C4B C 0.2621(3) -0.1221(3) 0.3137(5) 0.072(3) Uiso 0.458(7) 1 d P A 2 H4B H 0.2565 -0.1384 0.3547 0.086 Uiso 0.458(7) 1 calc PR A 2 C5 C 0.23587(16) -0.13281(16) 0.2500 0.0686(14) Uiso 1 2 d S . . C6 C 0.46706(11) 0.02695(10) 0.3899(2) 0.0626(9) Uiso 1 1 d . . . C7 C 0.48443(10) 0.01349(10) 0.4472(2) 0.0621(9) Uiso 1 1 d . . . C8 C 0.52061(14) 0.02396(14) 0.4429(3) 0.0974(14) Uiso 1 1 d . . . H8 H 0.5351 0.0396 0.4036 0.117 Uiso 1 1 calc R . . C9 C 0.46265(16) -0.01140(15) 0.5020(3) 0.1011(15) Uiso 1 1 d . . . C10 C 0.50758(13) 0.15013(13) 0.2500 0.0506(11) Uiso 1 2 d SD . . C11 C 0.54017(15) 0.18722(15) 0.2500 0.0626(13) Uiso 1 2 d SD . . C12 C 0.5743(3) 0.1925(3) 0.2500 0.130(3) Uiso 1 2 d S . . H12 H 0.5779 0.1721 0.2500 0.156 Uiso 1 2 calc SR . . C13 C 0.6041(3) 0.2273(3) 0.2500 0.147(3) Uiso 1 2 d S . . H13 H 0.6276 0.2294 0.2500 0.176 Uiso 1 2 calc SR . . C14 C 0.60284(19) 0.25935(19) 0.2500 0.0826(17) Uiso 1 2 d SD . . C17 C 0.63604(18) 0.29747(18) 0.2500 0.0792(17) Uiso 1 2 d SD . . C18 C 0.67103(18) 0.30168(18) 0.2500 0.0803(17) Uiso 1 2 d S . . C19 C 0.39152(10) 0.08955(10) 0.40199(19) 0.0551(8) Uiso 1 1 d . . . C20 C 0.38447(10) 0.10474(11) 0.4719(2) 0.0627(9) Uiso 1 1 d . . . C21 C 0.39655(12) 0.14368(12) 0.4759(3) 0.0819(12) Uiso 1 1 d . . . H21 H 0.4063 0.1589 0.4332 0.098 Uiso 1 1 calc R . . C22 C 0.39338(12) 0.15844(14) 0.5449(3) 0.0868(13) Uiso 1 1 d . . . H22 H 0.4031 0.1841 0.5494 0.104 Uiso 1 1 calc R . . C23 C 0.37601(12) 0.13559(12) 0.6069(2) 0.0731(11) Uiso 1 1 d . . . C24 C 0.36295(13) 0.09773(13) 0.6021(3) 0.0850(13) Uiso 1 1 d . . . H24 H 0.3518 0.0825 0.6442 0.102 Uiso 1 1 calc R . . C25 C 0.36650(12) 0.08214(13) 0.5332(3) 0.0841(12) Uiso 1 1 d . . . H25 H 0.3566 0.0565 0.5293 0.101 Uiso 1 1 calc R . . C26 C 0.37329(13) 0.15220(13) 0.6788(3) 0.0804(12) Uiso 1 1 d . . . C27 C 0.37033(12) 0.18437(12) 0.6797(2) 0.0777(11) Uiso 1 1 d . . . C28 C 0.20092(16) -0.16793(17) 0.2500 0.0724(15) Uiso 1 2 d S A . C29 C 0.37412(17) 0.13473(17) 0.7500 0.0773(16) Uiso 1 2 d S . . C16 C 0.5369(3) 0.2174(3) 0.2887(6) 0.233(5) Uiso 1 1 d D . . C15 C 0.5707(4) 0.2548(4) 0.2500 0.168(4) Uiso 1 2 d SD . . _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 O2 1.919(2) . ? Zn1 O9 1.923(2) . ? Zn1 O3 1.938(3) . ? Zn1 O1 1.9493(15) . ? Zn1 Zn1 3.1494(7) 10_556 ? Zn2 O1 1.914(3) . ? Zn2 O6 1.923(4) . ? Zn2 O4 1.942(3) . ? Zn2 O4 1.942(3) 10_556 ? Zn3 O8 1.933(2) . ? Zn3 O8 1.933(2) 10_556 ? Zn3 O1 1.950(3) . ? Zn3 O7 1.962(4) . ? O1 Zn1 1.9492(15) 10_556 ? O2 C1 1.259(3) . ? O3 C6 1.257(4) . ? O4 C6 1.245(4) . ? O5 C9 1.42(2) . ? O6 C10 1.279(5) . ? O7 C10 1.237(5) . ? O8 C19 1.268(4) . ? O9 C19 1.270(4) . ? C1 O2 1.259(3) 10_556 ? C1 C2 1.463(7) . ? C2 C3A 1.370(8) . ? C2 C3A 1.370(8) 10_556 ? C2 C3B 1.389(8) 10_556 ? C2 C3B 1.389(8) . ? C3A C4A 1.395(9) . ? C3B C4B 1.383(11) . ? C4A C5 1.381(8) . ? C4B C5 1.463(10) . ? C5 C4A 1.381(8) 10_556 ? C5 C28 1.449(8) . ? C5 C4B 1.463(10) 10_556 ? C6 C7 1.494(5) . ? C7 C8 1.336(6) . ? C7 C9 1.367(6) . ? C8 C9 1.429(7) 7_656 ? C9 C8 1.429(7) 7_656 ? C10 C11 1.450(7) . ? C11 C12 1.317(10) . ? C11 C16 1.486(10) . ? C11 C16 1.486(10) 10_556 ? C12 C13 1.346(11) . ? C13 C14 1.353(11) . ? C14 C15 1.245(12) . ? C14 C17 1.485(9) . ? C17 C18 1.368(8) . ? C17 C18 1.427(8) 3_665 ? C18 C17 1.427(8) 2_655 ? C19 C20 1.472(5) . ? C20 C25 1.373(6) . ? C20 C21 1.429(5) . ? C21 C22 1.389(6) . ? C22 C23 1.383(6) . ? C23 C24 1.380(6) . ? C23 C26 1.466(6) . ? C24 C25 1.410(6) . ? C26 C27 1.395(6) . ? C26 C29 1.451(5) . ? C27 C28 1.426(5) 9_556 ? C28 C27 1.426(5) 5_554 ? C28 C27 1.426(5) 8_556 ? C29 C26 1.451(5) 10_557 ? C16 C16 1.36(2) 10_556 ? C16 C15 1.626(12) . ? C15 C16 1.626(12) 10_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O9 107.09(10) . . ? O2 Zn1 O3 109.05(10) . . ? O9 Zn1 O3 107.73(11) . . ? O2 Zn1 O1 111.77(9) . . ? O9 Zn1 O1 110.63(10) . . ? O3 Zn1 O1 110.42(10) . . ? O2 Zn1 Zn1 75.82(7) . 10_556 ? O9 Zn1 Zn1 126.90(7) . 10_556 ? O3 Zn1 Zn1 121.56(7) . 10_556 ? O1 Zn1 Zn1 36.11(6) . 10_556 ? O1 Zn2 O6 112.80(14) . . ? O1 Zn2 O4 111.10(9) . . ? O6 Zn2 O4 107.96(10) . . ? O1 Zn2 O4 111.10(9) . 10_556 ? O6 Zn2 O4 107.96(10) . 10_556 ? O4 Zn2 O4 105.60(15) . 10_556 ? O8 Zn3 O8 115.37(15) . 10_556 ? O8 Zn3 O1 111.43(8) . . ? O8 Zn3 O1 111.44(8) 10_556 . ? O8 Zn3 O7 104.45(9) . . ? O8 Zn3 O7 104.45(9) 10_556 . ? O1 Zn3 O7 109.05(14) . . ? Zn2 O1 Zn1 110.24(9) . 10_556 ? Zn2 O1 Zn1 110.24(9) . . ? Zn1 O1 Zn1 107.77(12) 10_556 . ? Zn2 O1 Zn3 109.73(12) . . ? Zn1 O1 Zn3 109.41(8) 10_556 . ? Zn1 O1 Zn3 109.41(8) . . ? C1 O2 Zn1 132.8(3) . . ? C6 O3 Zn1 130.8(2) . . ? C6 O4 Zn2 131.1(3) . . ? C10 O6 Zn2 131.3(3) . . ? C10 O7 Zn3 134.6(4) . . ? C19 O8 Zn3 130.6(2) . . ? C19 O9 Zn1 132.2(2) . . ? O2 C1 O2 122.6(4) . 10_556 ? O2 C1 C2 118.7(2) . . ? O2 C1 C2 118.7(2) 10_556 . ? C3A C2 C3A 105.1(7) . 10_556 ? C3A C2 C3B 120.6(5) . 10_556 ? C3A C2 C3B 39.2(3) 10_556 10_556 ? C3A C2 C3B 39.2(3) . . ? C3A C2 C3B 120.6(5) 10_556 . ? C3B C2 C3B 107.8(7) 10_556 . ? C3A C2 C1 121.1(4) . . ? C3A C2 C1 121.1(4) 10_556 . ? C3B C2 C1 118.3(4) 10_556 . ? C3B C2 C1 118.3(4) . . ? C2 C3A C4A 120.7(7) . . ? C4B C3B C2 119.4(7) . . ? C3A C4A C5 121.7(7) . . ? C3B C4B C5 121.0(8) . . ? C4A C5 C4A 101.0(7) . 10_556 ? C4A C5 C28 122.3(4) . . ? C4A C5 C28 122.3(4) 10_556 . ? C4A C5 C4B 116.3(6) . 10_556 ? C4A C5 C4B 42.6(4) 10_556 10_556 ? C28 C5 C4B 121.4(5) . 10_556 ? C4A C5 C4B 42.7(4) . . ? C4A C5 C4B 116.3(6) 10_556 . ? C28 C5 C4B 121.4(5) . . ? C4B C5 C4B 99.6(8) 10_556 . ? O4 C6 O3 125.9(4) . . ? O4 C6 C7 116.5(3) . . ? O3 C6 C7 117.6(3) . . ? C8 C7 C9 119.6(4) . . ? C8 C7 C6 120.7(4) . . ? C9 C7 C6 119.6(4) . . ? C7 C8 C9 120.8(5) . 7_656 ? O5 C9 C7 130.4(11) . . ? O5 C9 C8 110.1(11) . 7_656 ? C7 C9 C8 119.5(5) . 7_656 ? O7 C10 O6 122.5(5) . . ? O7 C10 C11 119.0(5) . . ? O6 C10 C11 118.4(4) . . ? C12 C11 C10 121.9(6) . . ? C12 C11 C16 113.6(7) . . ? C10 C11 C16 117.6(6) . . ? C12 C11 C16 113.6(7) . 10_556 ? C10 C11 C16 117.5(6) . 10_556 ? C16 C11 C16 54.3(8) . 10_556 ? C11 C12 C13 120.8(9) . . ? C14 C13 C12 125.6(10) . . ? C15 C14 C13 114.5(9) . . ? C15 C14 C17 120.6(8) . . ? C13 C14 C17 124.9(8) . . ? C18 C17 C18 121.4(7) . 3_665 ? C18 C17 C14 119.5(6) . . ? C18 C17 C14 119.1(6) 3_665 . ? C17 C18 C17 118.6(7) . 2_655 ? O9 C19 O8 124.4(3) . . ? O9 C19 C20 116.8(3) . . ? O8 C19 C20 118.8(3) . . ? C25 C20 C21 119.6(4) . . ? C25 C20 C19 121.1(4) . . ? C21 C20 C19 119.3(3) . . ? C22 C21 C20 118.7(4) . . ? C23 C22 C21 121.0(4) . . ? C22 C23 C24 120.1(4) . . ? C22 C23 C26 119.4(4) . . ? C24 C23 C26 120.4(4) . . ? C23 C24 C25 120.0(4) . . ? C20 C25 C24 120.2(4) . . ? C27 C26 C29 120.0(4) . . ? C27 C26 C23 121.3(4) . . ? C29 C26 C23 118.6(4) . . ? C26 C27 C28 120.8(4) . 9_556 ? C27 C28 C27 119.7(6) 5_554 8_556 ? C27 C28 C5 120.1(3) 5_554 . ? C27 C28 C5 120.1(3) 8_556 . ? C26 C29 C26 118.6(6) 10_557 . ? C16 C16 C11 62.9(4) 10_556 . ? C16 C16 C15 65.4(4) 10_556 . ? C11 C16 C15 102.3(8) . . ? C14 C15 C16 119.2(9) . 10_556 ? C14 C15 C16 119.2(9) . . ? C16 C15 C16 49.2(8) 10_556 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.869 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.063 data_UMCM_OBnB(OH)2 _database_code_depnum_ccdc_archive 'CCDC 863179' #TrackingRef '- Revised CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H0 O14 Zn4' _chemical_formula_weight 1037.94 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' O O 0.0106 0.0060 '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 ? _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 41.283(3) _cell_length_b 41.283(3) _cell_length_c 17.5145(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25850(3) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3048 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.9198 _exptl_absorpt_correction_T_max 0.9455 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 118497 _diffrn_reflns_av_R_equivalents 0.0944 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.39 _reflns_number_total 16408 _reflns_number_gt 9408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was not refined as anisotropy to be consistent due to some disorder atoms. SQUEEZE found 6956 electrons that can be accounted for chloroform and DMF molecules. No hydrogen was added to C22 C23 C24 and C30 due to the disorder/ distortion of the ring. 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^)+(0.2000P)^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 'not measured' _refine_ls_number_reflns 16408 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.1933 _refine_ls_goodness_of_fit_ref 0.709 _refine_ls_restrained_S_all 0.709 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.039 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 -0.006 -0.004 -0.010 21183 6956 ' ' _platon_squeeze_details ; ; _refinement_detail ; ; 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 O1 O 0.05775(8) 0.42573(8) 0.2500 0.0295(7) Uiso 1 2 d S . . O5 O 0.10913(8) 0.40208(8) 0.34315(16) 0.0585(7) Uiso 1 1 d . . . O3 O 0.04813(8) 0.48802(8) 0.33831(16) 0.0579(7) Uiso 1 1 d . . . O4 O 0.05659(7) 0.38619(7) 0.40698(16) 0.0557(7) Uiso 1 1 d . . . O6 O 0.12263(11) 0.51184(11) 0.2500 0.0618(11) Uiso 1 2 d S . . O7 O 0.14649(12) 0.47485(12) 0.2500 0.0701(12) Uiso 1 2 d S . . O2 O 0.01627(7) 0.43302(8) 0.39771(16) 0.0582(8) Uiso 1 1 d . . . O8 O -0.01694(7) 0.35603(7) 0.31382(16) 0.0561(7) Uiso 1 1 d . . . C14 C -0.03096(15) 0.34112(15) 0.2500 0.0443(13) Uiso 1 2 d S . . C15 C -0.06616(16) 0.30489(16) 0.2500 0.0543(15) Uiso 1 2 d S . . C8 C 0.14969(15) 0.50679(15) 0.2500 0.0452(13) Uiso 1 2 d S . . C1 C 0.08936(11) 0.39191(11) 0.4027(2) 0.0485(10) Uiso 1 1 d . . . C10 C 0.02728(11) 0.46731(11) 0.3886(2) 0.0505(10) Uiso 1 1 d . . . C11 C 0.01312(11) 0.48435(11) 0.4468(2) 0.0531(10) Uiso 1 1 d . . . C2 C 0.10508(12) 0.38536(12) 0.4725(3) 0.0595(11) Uiso 1 1 d . . . C13 C -0.01381(13) 0.46099(13) 0.4993(3) 0.0682(13) Uiso 1 1 d . . . C7 C 0.13506(19) 0.37440(18) 0.7500 0.0721(19) Uiso 1 2 d S . . H7 H 0.1127 0.3756 0.7500 0.087 Uiso 1 2 calc SR . . C6 C 0.15197(15) 0.37348(14) 0.6807(3) 0.0793(15) Uiso 1 1 d . . . C4 C 0.09795(15) 0.36349(15) 0.6019(3) 0.0850(16) Uiso 1 1 d . . . H4 H 0.0820 0.3511 0.6440 0.102 Uiso 1 1 calc R . . C12 C 0.02610(13) 0.52144(13) 0.4456(3) 0.0673(12) Uiso 1 1 d . . . C5 C 0.13520(14) 0.37656(13) 0.6083(3) 0.0713(13) Uiso 1 1 d . . . C3 C 0.08244(16) 0.36816(14) 0.5325(3) 0.0873(16) Uiso 1 1 d . . . H3 H 0.0564 0.3592 0.5287 0.105 Uiso 1 1 calc R . . C18 C -0.18675(13) 0.18442(13) 0.3187(3) 0.0686(13) Uiso 1 1 d . . . H18 H -0.1751 0.1953 0.3660 0.082 Uiso 1 1 calc R . . C29 C -0.13328(18) 0.23648(18) 0.2500 0.0632(17) Uiso 1 2 d S . . C19 C -0.1681(2) 0.20183(19) 0.2500 0.0726(19) Uiso 1 2 d S . . C25 C 0.29721(19) 0.63551(19) 0.2500 0.0705(19) Uiso 1 2 d S . . C16 C 0.14223(15) 0.39628(14) 0.4764(3) 0.0814(15) Uiso 1 1 d . . . H16 H 0.1576 0.4062 0.4325 0.098 Uiso 1 1 calc R . . C26 C 0.32902(19) 0.6319(2) 0.2500 0.0740(19) Uiso 1 2 d S . . H26 H 0.3258 0.6075 0.2500 0.089 Uiso 1 2 calc SR . . C17 C 0.15741(16) 0.39289(15) 0.5442(3) 0.0898(16) Uiso 1 1 d . . . H17 H 0.1835 0.4019 0.5471 0.108 Uiso 1 1 calc R . . C27 C -0.0815(3) 0.2864(3) 0.3134(7) 0.086(3) Uiso 0.50 1 d P . . H27 H -0.0693 0.2963 0.3607 0.103 Uiso 1 1 calc R . . C28 C -0.1147(2) 0.2532(2) 0.3126(6) 0.065(2) Uiso 0.50 1 d P . . H28 H -0.1249 0.2414 0.3601 0.078 Uiso 1 1 calc R . . O10 O -0.0299(4) 0.4236(4) 0.5035(8) 0.088(4) Uiso 0.25 1 d P . . O9 O 0.0534(4) 0.5456(4) 0.3919(7) 0.075(4) Uiso 0.25 1 d P . . C9 C 0.18705(17) 0.53875(18) 0.2500 0.0593(16) Uiso 1 2 d S . . C21 C 0.2602(2) 0.6018(2) 0.2500 0.0711(19) Uiso 1 2 d S . . C24 C 0.2302(3) 0.6050(3) 0.2500 0.118(3) Uiso 1 2 d S . . C30 C 0.1934(3) 0.5742(3) 0.2500 0.136(4) Uiso 1 2 d S . . C23 C 0.2172(3) 0.5371(2) 0.2829(5) 0.069(3) Uiso 0.50 1 d P . . C22 C 0.2526(3) 0.5690(3) 0.2842(5) 0.072(3) Uiso 0.50 1 d P . . Zn1 Zn 0.028507(10) 0.400508(10) 0.33967(2) 0.03199(14) Uiso 1 1 d . . . Zn2 Zn 0.104219(15) 0.424425(15) 0.2500 0.03250(16) Uiso 1 2 d S . . Zn3 Zn 0.069387(15) 0.477271(15) 0.2500 0.03474(17) Uiso 1 2 d S . . _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 O1 Zn1 1.9367(17) . ? O1 Zn1 1.9368(17) 10_556 ? O1 Zn2 1.946(3) . ? O1 Zn3 1.933(3) . ? O5 C1 1.259(4) . ? O5 Zn2 1.934(3) . ? O3 C10 1.229(4) . ? O3 Zn3 1.936(3) . ? O4 C1 1.254(4) . ? O4 Zn1 1.941(3) . ? O6 C8 1.234(6) . ? O6 Zn3 1.932(4) . ? O7 C8 1.258(6) . ? O7 Zn2 1.935(4) . ? O2 C10 1.262(4) . ? O2 Zn1 1.941(3) . ? O8 C14 1.268(3) . ? O8 Zn1 1.911(3) . ? C14 O8 1.268(3) 10_556 ? C14 C15 1.475(8) . ? C15 C27 1.317(11) . ? C15 C27 1.317(11) 10_556 ? C8 C9 1.444(8) . ? C1 C2 1.472(6) . ? C10 C11 1.513(5) . ? C11 C12 1.346(6) . ? C11 C13 1.392(6) . ? C2 C3 1.349(6) . ? C2 C16 1.367(6) . ? C13 O10 1.343(14) . ? C13 C12 1.443(6) 7_566 ? C7 C6 1.410(6) 10_557 ? C7 C6 1.410(6) . ? C6 C18 1.390(6) 8_556 ? C6 C5 1.481(7) . ? C4 C5 1.356(6) . ? C4 C3 1.432(7) . ? C12 C13 1.443(6) 7_566 ? C12 O9 1.424(13) . ? C5 C17 1.392(7) . ? C18 C6 1.390(6) 9_556 ? C18 C19 1.416(6) . ? C29 C28 1.318(9) . ? C29 C28 1.318(9) 10_556 ? C29 C19 1.433(9) . ? C19 C18 1.416(6) 10_556 ? C25 C26 1.362(8) 3_565 ? C25 C26 1.394(8) . ? C25 C21 1.466(9) . ? C16 C17 1.381(7) . ? C26 C25 1.362(9) 2_665 ? C27 C28 1.369(12) . ? C9 C30 1.352(11) . ? C9 C23 1.404(10) . ? C9 C23 1.404(10) 10_556 ? C21 C24 1.310(11) . ? C21 C22 1.365(10) . ? C21 C22 1.365(10) 10_556 ? C24 C30 1.411(13) . ? C23 C23 1.154(17) 10_556 ? C23 C22 1.393(12) . ? C23 C22 1.822(12) 10_556 ? C22 C22 1.196(17) 10_556 ? C22 C23 1.822(12) 10_556 ? Zn1 Zn1 3.1412(8) 10_556 ? Zn2 O5 1.934(3) 10_556 ? Zn2 Zn3 3.1567(8) . ? Zn3 O3 1.936(3) 10_556 ? 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 Zn1 O1 Zn1 108.38(14) . 10_556 ? Zn1 O1 Zn2 110.07(10) . . ? Zn1 O1 Zn2 110.07(10) 10_556 . ? Zn1 O1 Zn3 109.68(10) . . ? Zn1 O1 Zn3 109.68(10) 10_556 . ? Zn2 O1 Zn3 108.93(14) . . ? C1 O5 Zn2 130.7(3) . . ? C10 O3 Zn3 130.7(3) . . ? C1 O4 Zn1 131.2(3) . . ? C8 O6 Zn3 131.8(4) . . ? C8 O7 Zn2 133.9(4) . . ? C10 O2 Zn1 129.5(3) . . ? C14 O8 Zn1 131.8(3) . . ? O8 C14 O8 123.7(5) . 10_556 ? O8 C14 C15 118.1(3) . . ? O8 C14 C15 118.1(3) 10_556 . ? C27 C15 C27 114.9(12) . 10_556 ? C27 C15 C14 122.2(6) . . ? C27 C15 C14 122.2(6) 10_556 . ? O6 C8 O7 123.2(5) . . ? O6 C8 C9 119.3(5) . . ? O7 C8 C9 117.5(5) . . ? O4 C1 O5 124.8(4) . . ? O4 C1 C2 116.7(4) . . ? O5 C1 C2 118.5(4) . . ? O3 C10 O2 127.3(4) . . ? O3 C10 C11 117.3(4) . . ? O2 C10 C11 115.4(4) . . ? C12 C11 C13 121.6(4) . . ? C12 C11 C10 119.4(4) . . ? C13 C11 C10 118.9(4) . . ? C3 C2 C16 120.1(5) . . ? C3 C2 C1 119.4(4) . . ? C16 C2 C1 120.4(4) . . ? O10 C13 C11 126.7(7) . . ? O10 C13 C12 116.4(7) . 7_566 ? C11 C13 C12 116.9(4) . 7_566 ? C6 C7 C6 118.8(7) 10_557 . ? C18 C6 C7 120.2(5) 8_556 . ? C18 C6 C5 121.4(5) 8_556 . ? C7 C6 C5 118.4(5) . . ? C5 C4 C3 120.7(5) . . ? C11 C12 C13 121.4(4) . 7_566 ? C11 C12 O9 122.1(7) . . ? C13 C12 O9 116.4(6) 7_566 . ? C4 C5 C17 117.9(5) . . ? C4 C5 C6 121.5(5) . . ? C17 C5 C6 120.6(5) . . ? C2 C3 C4 119.6(5) . . ? C6 C18 C19 122.2(5) 9_556 . ? C28 C29 C28 112.5(10) . 10_556 ? C28 C29 C19 123.6(5) . . ? C28 C29 C19 123.6(5) 10_556 . ? C29 C19 C18 121.7(3) . . ? C29 C19 C18 121.7(3) . 10_556 ? C18 C19 C18 116.4(6) . 10_556 ? C26 C25 C26 116.7(8) 3_565 . ? C26 C25 C21 124.0(7) 3_565 . ? C26 C25 C21 119.3(7) . . ? C17 C16 C2 120.1(5) . . ? C25 C26 C25 123.3(8) 2_665 . ? C16 C17 C5 121.3(5) . . ? C15 C27 C28 121.5(11) . . ? C29 C28 C27 124.2(10) . . ? C30 C9 C23 110.8(7) . . ? C30 C9 C23 110.8(7) . 10_556 ? C23 C9 C23 48.5(7) . 10_556 ? C30 C9 C8 122.0(7) . . ? C23 C9 C8 121.6(6) . . ? C23 C9 C8 121.6(6) 10_556 . ? C24 C21 C22 110.0(7) . . ? C24 C21 C22 110.0(7) . 10_556 ? C22 C21 C22 52.0(8) . 10_556 ? C24 C21 C25 119.5(8) . . ? C22 C21 C25 123.7(7) . . ? C22 C21 C25 123.7(7) 10_556 . ? C21 C24 C30 123.6(10) . . ? C24 C30 C9 121.0(10) . . ? C23 C23 C22 90.9(5) 10_556 . ? C23 C23 C9 65.7(4) 10_556 . ? C22 C23 C9 119.8(8) . . ? C23 C23 C22 49.8(4) 10_556 10_556 ? C22 C23 C22 41.0(6) . 10_556 ? C9 C23 C22 96.3(6) . 10_556 ? C22 C22 C21 64.0(4) 10_556 . ? C22 C22 C23 89.1(5) 10_556 . ? C21 C22 C23 122.8(9) . . ? C22 C22 C23 49.8(4) 10_556 10_556 ? C21 C22 C23 97.8(6) . 10_556 ? C23 C22 C23 39.3(6) . 10_556 ? O8 Zn1 O1 111.90(11) . . ? O8 Zn1 O4 107.47(11) . . ? O1 Zn1 O4 110.46(11) . . ? O8 Zn1 O2 108.57(11) . . ? O1 Zn1 O2 111.15(12) . . ? O4 Zn1 O2 107.10(12) . . ? O8 Zn1 Zn1 76.29(8) . 10_556 ? O1 Zn1 Zn1 35.81(7) . 10_556 ? O4 Zn1 Zn1 127.39(8) . 10_556 ? O2 Zn1 Zn1 121.58(8) . 10_556 ? O7 Zn2 O5 105.06(10) . . ? O7 Zn2 O5 105.06(10) . 10_556 ? O5 Zn2 O5 115.03(17) . 10_556 ? O7 Zn2 O1 109.97(15) . . ? O5 Zn2 O1 110.67(9) . . ? O5 Zn2 O1 110.68(9) 10_556 . ? O7 Zn2 Zn3 74.57(13) . . ? O5 Zn2 Zn3 121.48(8) . . ? O5 Zn2 Zn3 121.48(8) 10_556 . ? O1 Zn2 Zn3 35.40(8) . . ? O3 Zn3 O3 106.05(17) . 10_556 ? O3 Zn3 O6 108.02(11) . . ? O3 Zn3 O6 108.02(11) 10_556 . ? O3 Zn3 O1 111.14(10) . . ? O3 Zn3 O1 111.14(10) 10_556 . ? O6 Zn3 O1 112.21(15) . . ? O3 Zn3 Zn2 125.00(8) . . ? O3 Zn3 Zn2 125.01(8) 10_556 . ? O6 Zn3 Zn2 76.54(12) . . ? O1 Zn3 Zn2 35.67(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.161 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.069