# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'SonBinh Nguyen' _publ_contact_author_email STN@NORTHWESTERN.EDU _publ_section_title ; Ligand-elaboration as a strategy for engendering structural diversity in porous metal-organic framework compounds ; loop_ _publ_author_name 'Sonbinh Nguyen' 'Tendai Gadzikwa' 'J Hupp' 'Bi-Shun Zeng.' # Attachment 'Compound_A_B_and_D.cif' data_CompoundA _database_code_depnum_ccdc_archive 'CCDC 661009' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CompoundA _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 N4 O6 Zn' _chemical_formula_weight 631.97 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.848(7) _cell_length_b 6.1751(15) _cell_length_c 17.144(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.838(4) _cell_angle_gamma 90.00 _cell_volume 3017.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5121 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.26 _exptl_crystal_description plate/needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.0105 _exptl_crystal_size_mid 0.0470 _exptl_crystal_size_max 0.1400 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method none _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7706 _exptl_absorpt_correction_T_max 0.9652 _exptl_absorpt_process_details 'XPREP in SHELXTL (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13047 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.79 _reflns_number_total 3627 _reflns_number_gt 2702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+9.4797P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3627 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1954 _refine_ls_wR_factor_gt 0.1839 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.58053(11) 0.2500 0.0263(2) Uani 1 2 d S . . O1 O 0.05052(9) 0.7815(5) 0.28562(17) 0.0347(7) Uani 1 1 d . . . O2 O 0.09814(10) 0.4992(6) 0.28341(19) 0.0394(7) Uani 1 1 d . . . N1 N 0.00242(11) 0.3769(6) 0.1567(2) 0.0300(8) Uani 1 1 d . . . C1 C 0.09076(13) 0.6879(7) 0.3001(2) 0.0287(9) Uani 1 1 d . . . C2 C 0.12947(13) 0.8256(7) 0.3446(2) 0.0290(9) Uani 1 1 d . . . C3 C 0.17461(14) 0.7380(8) 0.3648(3) 0.0348(10) Uani 1 1 d . . . H3 H 0.1812 0.5956 0.3486 0.042 Uiso 1 1 calc R . . C4 C 0.12019(14) 1.0322(8) 0.3682(2) 0.0336(10) Uani 1 1 d . . . H4 H 0.0897 1.0913 0.3538 0.040 Uiso 1 1 calc R . . C5 C 0.15499(15) 1.1555(8) 0.4129(3) 0.0367(10) Uani 1 1 d . . . H5 H 0.1480 1.2971 0.4294 0.044 Uiso 1 1 calc R . . C6 C 0.20925(14) 0.8610(8) 0.4084(3) 0.0392(11) Uani 1 1 d . . . H6 H 0.2399 0.8027 0.4218 0.047 Uiso 1 1 calc R . . C7 C 0.19981(14) 1.0714(8) 0.4333(3) 0.0379(10) Uani 1 1 d . . . C8 C 0.23547(15) 1.1960(9) 0.4803(3) 0.0420(11) Uani 1 1 d . . . C13 C 0.03001(16) 0.1996(8) 0.1635(2) 0.0397(11) Uani 1 1 d . . . H13 H 0.0507 0.1778 0.2115 0.048 Uiso 1 1 calc R . . C12 C -0.02629(13) 0.4042(7) 0.0883(2) 0.0309(9) Uani 1 1 d . . . H12 H -0.0461 0.5279 0.0823 0.037 Uiso 1 1 calc R . . C11 C -0.02842(14) 0.2614(7) 0.0264(2) 0.0306(9) Uani 1 1 d . . . H11 H -0.0495 0.2876 -0.0209 0.037 Uiso 1 1 calc R . . C10 C 0.02970(16) 0.0508(8) 0.1053(3) 0.0406(11) Uani 1 1 d . . . H10 H 0.0495 -0.0725 0.1134 0.049 Uiso 1 1 calc R . . C9 C 0.00009(13) 0.0788(7) 0.0329(2) 0.0279(8) Uani 1 1 d . . . O5 O 0.1206(2) 0.4702(12) 0.0431(4) 0.117(2) Uani 1 1 d . . . N3 N 0.1616(2) 0.2336(15) 0.1249(4) 0.097(2) Uani 1 1 d . . . C14 C 0.1338(2) 0.2828(13) 0.0605(4) 0.0673(17) Uani 1 1 d . . . H14 H 0.1229 0.1695 0.0248 0.081 Uiso 1 1 calc R . . C16 C 0.1805(4) 0.348(3) 0.1842(7) 0.190(8) Uani 1 1 d . . . H16A H 0.1746 0.5019 0.1728 0.285 Uiso 1 1 calc R . . H16B H 0.2144 0.3220 0.1939 0.285 Uiso 1 1 calc R . . H16C H 0.1670 0.3073 0.2312 0.285 Uiso 1 1 calc R . . C15 C 0.1702(4) -0.011(2) 0.1391(6) 0.145(5) Uani 1 1 d . . . H15A H 0.1992 -0.0535 0.1198 0.217 Uiso 1 1 calc R . . H15B H 0.1438 -0.0930 0.1108 0.217 Uiso 1 1 calc R . . H15C H 0.1732 -0.0416 0.1957 0.217 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0186(3) 0.0324(4) 0.0246(3) 0.000 -0.0067(2) 0.000 O1 0.0202(13) 0.0410(18) 0.0376(16) -0.0012(13) -0.0127(11) -0.0001(12) O2 0.0282(15) 0.0427(18) 0.0433(18) -0.0103(15) -0.0072(13) -0.0031(13) N1 0.0240(16) 0.037(2) 0.0271(17) -0.0014(14) -0.0037(13) -0.0015(13) C1 0.0244(19) 0.034(2) 0.0251(19) 0.0001(17) -0.0029(15) -0.0042(16) C2 0.0218(18) 0.037(2) 0.0261(19) 0.0003(17) -0.0037(15) -0.0034(16) C3 0.0241(19) 0.044(3) 0.035(2) -0.0080(19) -0.0005(16) 0.0002(17) C4 0.0245(19) 0.041(3) 0.031(2) -0.0037(18) -0.0076(16) -0.0017(17) C5 0.032(2) 0.034(2) 0.039(2) -0.0064(19) -0.0100(18) -0.0051(18) C6 0.0198(19) 0.052(3) 0.043(2) -0.005(2) -0.0032(17) 0.0003(18) C7 0.0266(19) 0.048(3) 0.036(2) -0.010(2) -0.0050(16) -0.012(2) C8 0.028(2) 0.055(3) 0.040(2) -0.008(2) -0.0050(18) -0.007(2) C13 0.043(2) 0.048(3) 0.022(2) -0.0023(19) -0.0139(17) 0.011(2) C12 0.0261(18) 0.036(2) 0.029(2) 0.0014(18) 0.0007(15) 0.0027(17) C11 0.0266(19) 0.044(3) 0.0183(18) 0.0023(17) -0.0049(14) 0.0036(17) C10 0.043(2) 0.044(3) 0.030(2) -0.004(2) -0.0124(18) 0.013(2) C9 0.0259(18) 0.035(2) 0.0218(18) 0.0014(17) -0.0009(14) -0.0020(17) O5 0.089(4) 0.138(6) 0.128(5) 0.075(5) 0.028(3) 0.045(4) N3 0.068(4) 0.169(8) 0.058(3) 0.029(4) 0.016(3) 0.032(4) C14 0.061(4) 0.084(5) 0.058(4) 0.008(3) 0.009(3) 0.007(3) C16 0.093(7) 0.37(2) 0.114(8) -0.131(12) 0.040(6) -0.047(10) C15 0.162(10) 0.172(10) 0.112(8) 0.086(8) 0.061(7) 0.088(9) _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 O1 1.940(3) . ? Zn1 O1 1.940(3) 2 ? Zn1 N1 2.044(4) . ? Zn1 N1 2.044(4) 2 ? O1 C1 1.286(5) . ? O2 C1 1.226(5) . ? N1 C12 1.338(5) . ? N1 C13 1.348(6) . ? C1 C2 1.513(5) . ? C2 C4 1.377(6) . ? C2 C3 1.403(6) . ? C3 C6 1.380(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 H4 0.9500 . ? C5 C7 1.388(6) . ? C5 H5 0.9500 . ? C6 C7 1.407(7) . ? C6 H6 0.9500 . ? C7 C8 1.430(6) . ? C8 C8 1.195(9) 7_576 ? C13 C10 1.355(6) . ? C13 H13 0.9500 . ? C12 C11 1.374(6) . ? C12 H12 0.9500 . ? C11 C9 1.390(6) . ? C11 H11 0.9500 . ? C10 C9 1.405(5) . ? C10 H10 0.9500 . ? C9 C9 1.489(8) 5 ? O5 C14 1.240(9) . ? N3 C16 1.289(12) . ? N3 C14 1.298(8) . ? N3 C15 1.544(14) . ? C14 H14 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 O1 Zn1 O1 100.47(18) . 2 ? O1 Zn1 N1 121.70(13) . . ? O1 Zn1 N1 105.15(13) 2 . ? O1 Zn1 N1 105.15(13) . 2 ? O1 Zn1 N1 121.69(13) 2 2 ? N1 Zn1 N1 104.1(2) . 2 ? C1 O1 Zn1 112.7(3) . . ? C12 N1 C13 117.1(4) . . ? C12 N1 Zn1 121.2(3) . . ? C13 N1 Zn1 121.5(3) . . ? O2 C1 O1 124.5(4) . . ? O2 C1 C2 120.7(4) . . ? O1 C1 C2 114.8(4) . . ? C4 C2 C3 120.0(4) . . ? C4 C2 C1 120.5(4) . . ? C3 C2 C1 119.5(4) . . ? C6 C3 C2 119.3(4) . . ? C6 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C2 C4 C5 120.8(4) . . ? C2 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C7 C5 C4 119.9(4) . . ? C7 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C3 C6 C7 121.0(4) . . ? C3 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C5 C7 C6 119.0(4) . . ? C5 C7 C8 120.1(4) . . ? C6 C7 C8 120.8(4) . . ? C8 C8 C7 178.5(7) 7_576 . ? N1 C13 C10 123.4(4) . . ? N1 C13 H13 118.3 . . ? C10 C13 H13 118.3 . . ? N1 C12 C11 123.0(4) . . ? N1 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C12 C11 C9 120.2(3) . . ? C12 C11 H11 119.9 . . ? C9 C11 H11 119.9 . . ? C13 C10 C9 120.1(4) . . ? C13 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C9 C10 116.2(4) . . ? C11 C9 C9 122.4(4) . 5 ? C10 C9 C9 121.3(5) . 5 ? C16 N3 C14 132.4(11) . . ? C16 N3 C15 111.9(11) . . ? C14 N3 C15 115.3(9) . . ? O5 C14 N3 123.3(8) . . ? O5 C14 H14 118.3 . . ? N3 C14 H14 118.3 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 28.79 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.209 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.115 #===END data_CompoundB _database_code_depnum_ccdc_archive 'CCDC 661010' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CompoundB _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H48 N3 O12 Zn3' _chemical_formula_weight 1307.21 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.792(2) _cell_length_b 27.979(3) _cell_length_c 14.0334(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.579(2) _cell_angle_gamma 90.00 _cell_volume 8539.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6087 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.16 _exptl_crystal_description columnar _exptl_crystal_colour yellow _exptl_crystal_size_max 0.081 _exptl_crystal_size_mid 0.039 _exptl_crystal_size_min 0.033 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2676 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7625 _exptl_absorpt_correction_T_max 0.9095 _exptl_absorpt_process_details 'XPREP in SHELXTL (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39097 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.75 _reflns_number_total 19772 _reflns_number_gt 11758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.587(13) _refine_ls_number_reflns 19772 _refine_ls_number_parameters 786 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7137(3) 0.9832(2) 0.6917(4) 0.0258(14) Uani 1 1 d . . . C2 C 0.7532(3) 1.0247(2) 0.6895(4) 0.0265(14) Uani 1 1 d . . . C3 C 0.7645(3) 1.0462(2) 0.5976(4) 0.0368(16) Uani 1 1 d . . . H3 H 0.7476 1.0321 0.5402 0.044 Uiso 1 1 calc R . . C4 C 0.7818(3) 1.04495(19) 0.7735(4) 0.0298(14) Uani 1 1 d . . . H4 H 0.7765 1.0307 0.8339 0.036 Uiso 1 1 calc R . . C5 C 0.8173(3) 1.0854(2) 0.7672(4) 0.0380(15) Uani 1 1 d . . . H5 H 0.8367 1.0986 0.8237 0.046 Uiso 1 1 calc R . . C6 C 0.8000(3) 1.0874(2) 0.5940(4) 0.0340(14) Uani 1 1 d . . . C7 C 0.8137(3) 1.1063(2) 0.4943(4) 0.0568(18) Uani 1 1 d . . . H7A H 0.7944 1.1377 0.4842 0.085 Uiso 1 1 calc R . . H7B H 0.7971 1.0840 0.4453 0.085 Uiso 1 1 calc R . . H7C H 0.8582 1.1093 0.4900 0.085 Uiso 1 1 calc R . . C8 C 0.8257(3) 1.1081(2) 0.6774(4) 0.0276(14) Uani 1 1 d . . . C9 C 0.8621(3) 1.1500(2) 0.6773(4) 0.0297(14) Uani 1 1 d . . . C10 C 0.8934(3) 1.1851(2) 0.6788(5) 0.0338(16) Uani 1 1 d . . . C11 C 0.9298(3) 1.2271(2) 0.6800(4) 0.0272(15) Uani 1 1 d . . . C12 C 0.9300(3) 1.2578(2) 0.6031(4) 0.0302(15) Uani 1 1 d . . . C13 C 0.8897(3) 1.2495(2) 0.5160(4) 0.0552(17) Uani 1 1 d . . . H13A H 0.9015 1.2196 0.4858 0.083 Uiso 1 1 calc R . . H13B H 0.8940 1.2761 0.4715 0.083 Uiso 1 1 calc R . . H13C H 0.8468 1.2474 0.5331 0.083 Uiso 1 1 calc R . . C14 C 0.9678(3) 1.2378(2) 0.7607(4) 0.0388(17) Uani 1 1 d . . . H14 H 0.9679 1.2173 0.8147 0.047 Uiso 1 1 calc R . . C15 C 1.0051(3) 1.2775(2) 0.7634(4) 0.0301(14) Uani 1 1 d . . . H15 H 1.0301 1.2843 0.8198 0.036 Uiso 1 1 calc R . . C16 C 0.9691(3) 1.2979(2) 0.6094(4) 0.0383(17) Uani 1 1 d . . . H16 H 0.9692 1.3194 0.5571 0.046 Uiso 1 1 calc R . . C17 C 1.0069(3) 1.30654(19) 0.6888(4) 0.0216(13) Uani 1 1 d . . . C18 C 1.0537(3) 1.34862(19) 0.6855(4) 0.0198(13) Uiso 1 1 d . . . C19 C 0.7121(3) 0.84915(19) 0.6749(5) 0.0269(14) Uani 1 1 d . . . C20 C 0.7569(3) 0.80696(19) 0.6721(4) 0.0253(13) Uani 1 1 d . . . C21 C 0.7658(3) 0.7848(2) 0.5936(5) 0.0439(18) Uani 1 1 d . . . H21 H 0.7436 0.7957 0.5372 0.053 Uiso 1 1 calc R . . C22 C 0.7833(3) 0.7901(2) 0.7547(4) 0.0387(16) Uani 1 1 d . . . H22 H 0.7762 0.8058 0.8130 0.046 Uiso 1 1 calc R . . C23 C 0.8216(3) 0.7490(2) 0.7555(5) 0.0479(18) Uani 1 1 d . . . H23 H 0.8397 0.7367 0.8138 0.057 Uiso 1 1 calc R . . C24 C 0.8054(3) 0.7461(2) 0.5851(5) 0.0436(17) Uani 1 1 d . . . C25 C 0.8104(5) 0.7213(4) 0.4870(7) 0.172(5) Uani 1 1 d . . . H25A H 0.7834 0.7375 0.4387 0.258 Uiso 1 1 calc R . . H25B H 0.7980 0.6877 0.4917 0.258 Uiso 1 1 calc R . . H25C H 0.8530 0.7229 0.4686 0.258 Uiso 1 1 calc R . . C26 C 0.8319(3) 0.7275(2) 0.6702(6) 0.050(2) Uani 1 1 d . . . C27 C 0.8683(3) 0.6840(3) 0.6719(5) 0.0481(19) Uani 1 1 d . . . C28 C 0.8980(3) 0.6487(2) 0.6704(5) 0.0442(18) Uani 1 1 d . . . C29 C 0.9347(3) 0.6056(2) 0.6753(5) 0.0449(19) Uani 1 1 d . . . C30 C 0.9767(3) 0.5974(2) 0.7553(5) 0.071(3) Uani 1 1 d . . . H30 H 0.9796 0.6201 0.8057 0.085 Uiso 1 1 calc R . . C31 C 0.9291(3) 0.57211(19) 0.5997(4) 0.0362(15) Uani 1 1 d . . . C32 C 0.8826(3) 0.5785(2) 0.5163(5) 0.072(2) Uani 1 1 d . . . H32A H 0.8988 0.6010 0.4705 0.108 Uiso 1 1 calc R . . H32B H 0.8443 0.5911 0.5392 0.108 Uiso 1 1 calc R . . H32C H 0.8747 0.5476 0.4851 0.108 Uiso 1 1 calc R . . C33 C 0.9662(2) 0.53278(18) 0.6063(4) 0.0307(14) Uani 1 1 d . . . H33 H 0.9622 0.5095 0.5571 0.037 Uiso 1 1 calc R . . C34 C 1.0123(3) 0.5585(2) 0.7612(5) 0.065(2) Uani 1 1 d . . . H34 H 1.0389 0.5527 0.8163 0.077 Uiso 1 1 calc R . . C35 C 1.0096(3) 0.5253(2) 0.6815(4) 0.0327(16) Uani 1 1 d . . . C36 C 1.0486(3) 0.4821(2) 0.6859(5) 0.0264(14) Uani 1 1 d . . . C37 C 0.6785(2) 0.93422(18) 0.3947(3) 0.0401(13) Uani 1 1 d . . . H37 H 0.7134 0.9433 0.4344 0.048 Uiso 1 1 calc R . . C38 C 0.57673(18) 0.9138(2) 0.3794(2) 0.0300(9) Uani 1 1 d . . . H38 H 0.5388 0.9086 0.4077 0.036 Uiso 1 1 calc R . . C39 C 0.57751(19) 0.91266(19) 0.2820(3) 0.0327(10) Uani 1 1 d . . . H39 H 0.5412 0.9057 0.2436 0.039 Uiso 1 1 calc R . . C40 C 0.6833(2) 0.93429(18) 0.3005(3) 0.0444(14) Uani 1 1 d . . . H40 H 0.7209 0.9427 0.2742 0.053 Uiso 1 1 calc R . . C41 C 0.63192(19) 0.9218(2) 0.2409(3) 0.0309(13) Uani 1 1 d . . . C42 C 0.63607(18) 0.9189(3) 0.1344(3) 0.0283(10) Uani 1 1 d . . . C43 C 0.6009(2) 0.88503(18) 0.0807(3) 0.0392(13) Uani 1 1 d . . . H43 H 0.5758 0.8625 0.1107 0.047 Uiso 1 1 calc R . . C44 C 0.6719(2) 0.94905(19) 0.0850(3) 0.0406(13) Uani 1 1 d . . . H44 H 0.6969 0.9720 0.1188 0.049 Uiso 1 1 calc R . . C45 C 0.6723(2) 0.94666(17) -0.0130(3) 0.0351(12) Uani 1 1 d . . . H45 H 0.6978 0.9682 -0.0448 0.042 Uiso 1 1 calc R . . C46 C 0.6043(2) 0.88593(17) -0.0180(3) 0.0305(11) Uani 1 1 d . . . H46 H 0.5801 0.8636 -0.0550 0.037 Uiso 1 1 calc R . . C47 C 0.5813(3) 0.6517(2) 0.9958(4) 0.0293(15) Uani 1 1 d . . . C48 C 0.6215(3) 0.69363(19) 0.9992(4) 0.0268(14) Uani 1 1 d . . . C49 C 0.6305(3) 0.7196(2) 0.9112(4) 0.0344(15) Uani 1 1 d . . . H49 H 0.6126 0.7089 0.8516 0.041 Uiso 1 1 calc R . . C50 C 0.6529(3) 0.70820(19) 1.0852(4) 0.0285(13) Uani 1 1 d . . . H50 H 0.6490 0.6896 1.1411 0.034 Uiso 1 1 calc R . . C51 C 0.6887(3) 0.7483(2) 1.0904(4) 0.0358(15) Uani 1 1 d . . . C52 C 0.7202(3) 0.76499(16) 1.1829(3) 0.0438(15) Uani 1 1 d . . . H52A H 0.7066 0.7454 1.2355 0.066 Uiso 1 1 calc R . . H52B H 0.7098 0.7985 1.1938 0.066 Uiso 1 1 calc R . . H52C H 0.7649 0.7619 1.1796 0.066 Uiso 1 1 calc R . . C53 C 0.6666(3) 0.76086(19) 0.9182(4) 0.0291(14) Uani 1 1 d . . . H53 H 0.6702 0.7801 0.8631 0.035 Uiso 1 1 calc R . . C54 C 0.6968(3) 0.7742(2) 1.0022(4) 0.0307(15) Uani 1 1 d . . . C55 C 0.7374(3) 0.8159(2) 1.0073(5) 0.0355(16) Uani 1 1 d . . . C56 C 0.7705(3) 0.8492(2) 1.0086(4) 0.0346(15) Uani 1 1 d . . . C57 C 0.8091(3) 0.8917(2) 1.0034(5) 0.0313(15) Uani 1 1 d . . . C58 C 0.8168(2) 0.9130(2) 0.9173(4) 0.0285(12) Uani 1 1 d . . . H58 H 0.7973 0.9003 0.8604 0.034 Uiso 1 1 calc R . . C59 C 0.8355(3) 0.9096(2) 1.0887(4) 0.0361(15) Uani 1 1 d . . . C60 C 0.8297(3) 0.88537(18) 1.1817(3) 0.0505(16) Uani 1 1 d . . . H60A H 0.8543 0.9024 1.2317 0.076 Uiso 1 1 calc R . . H60B H 0.8444 0.8524 1.1776 0.076 Uiso 1 1 calc R . . H60C H 0.7864 0.8853 1.1972 0.076 Uiso 1 1 calc R . . C61 C 0.8709(3) 0.95171(19) 1.0786(4) 0.0324(14) Uani 1 1 d . . . H61 H 0.8904 0.9652 1.1348 0.039 Uiso 1 1 calc R . . C62 C 0.8529(3) 0.95274(19) 0.9140(4) 0.0341(15) Uani 1 1 d . . . H62 H 0.8605 0.9666 0.8541 0.041 Uiso 1 1 calc R . . C63 C 0.8787(3) 0.97312(19) 0.9979(4) 0.0275(14) Uani 1 1 d . . . C64 C 0.9219(3) 1.01584(19) 0.9929(4) 0.0222(13) Uani 1 1 d . . . C65 C 0.5193(2) 0.62009(17) 0.7028(3) 0.0352(12) Uani 1 1 d . . . H65 H 0.5340 0.6473 0.7377 0.042 Uiso 1 1 calc R . . C66 C 0.4758(3) 0.54419(17) 0.6989(3) 0.0485(16) Uani 1 1 d . . . H66 H 0.4596 0.5177 0.7314 0.058 Uiso 1 1 calc R . . C67 C 0.4770(3) 0.54254(16) 0.6019(3) 0.0449(15) Uani 1 1 d . . . H67 H 0.4625 0.5151 0.5674 0.054 Uiso 1 1 calc R . . C68 C 0.5212(2) 0.61986(17) 0.6065(3) 0.0363(13) Uani 1 1 d . . . H68 H 0.5378 0.6467 0.5757 0.044 Uiso 1 1 calc R . . C69 C 0.5001(2) 0.5825(2) 0.5532(3) 0.0291(11) Uani 1 1 d . . . N1 N 0.62721(15) 0.92202(17) 0.4364(2) 0.0230(9) Uani 1 1 d . . . N2 N 0.63929(13) 0.9161(2) -0.0638(2) 0.0208(7) Uani 1 1 d . . . N3 N 0.49699(16) 0.5826(2) 0.7508(2) 0.0264(9) Uani 1 1 d . . . O1 O 0.6909(2) 0.96703(14) 0.6152(3) 0.0398(11) Uani 1 1 d . . . O2 O 0.70161(18) 0.96658(12) 0.7729(3) 0.0252(9) Uani 1 1 d . . . O3 O 1.0643(2) 1.36414(13) 0.6081(3) 0.0352(11) Uani 1 1 d . . . O4 O 1.07323(18) 1.36315(12) 0.7678(3) 0.0279(10) Uani 1 1 d . . . O5 O 0.69155(19) 0.86454(13) 0.5976(3) 0.0349(11) Uani 1 1 d . . . O6 O 0.7014(2) 0.86468(13) 0.7564(3) 0.0341(11) Uani 1 1 d . . . O7 O 1.0604(2) 0.46413(13) 0.6044(3) 0.0325(10) Uani 1 1 d . . . O8 O 1.0730(2) 0.46706(13) 0.7633(3) 0.0358(11) Uani 1 1 d . . . O9 O 0.9375(2) 1.03540(13) 1.0701(3) 0.0336(11) Uani 1 1 d . . . O10 O 0.9337(2) 1.02888(13) 0.9103(3) 0.0382(11) Uani 1 1 d . . . O11 O 0.5566(2) 0.63819(13) 0.9163(3) 0.0368(11) Uani 1 1 d . . . O12 O 0.57095(18) 0.63130(12) 1.0762(3) 0.0284(10) Uani 1 1 d . . . Zn1 Zn 0.49488(2) 0.583849(16) 0.89522(3) 0.02080(11) Uani 1 1 d . . . Zn2 Zn 0.626475(19) 0.91633(2) 0.58075(3) 0.01980(11) Uani 1 1 d . . . Zn3 Zn 0.638692(19) 0.91555(2) 0.79079(3) 0.02012(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(3) 0.024(3) 0.022(3) -0.003(2) -0.003(2) 0.001(2) C2 0.029(3) 0.025(3) 0.026(3) 0.003(2) 0.000(2) -0.006(3) C3 0.043(4) 0.046(4) 0.021(3) -0.002(3) -0.004(3) -0.018(3) C4 0.050(4) 0.024(3) 0.013(2) -0.002(2) -0.011(2) -0.015(3) C5 0.042(4) 0.039(3) 0.031(3) 0.003(3) -0.010(2) -0.012(3) C6 0.038(3) 0.034(3) 0.030(3) 0.017(3) -0.003(2) -0.019(3) C7 0.053(4) 0.078(5) 0.039(3) 0.015(3) -0.004(3) -0.030(3) C8 0.024(3) 0.028(3) 0.031(3) 0.005(2) -0.001(2) -0.010(2) C9 0.030(3) 0.026(3) 0.033(3) 0.012(2) 0.002(3) -0.008(3) C10 0.037(4) 0.032(4) 0.031(3) 0.004(3) -0.006(3) 0.006(3) C11 0.029(3) 0.020(3) 0.032(3) 0.001(3) -0.004(3) -0.006(3) C12 0.042(4) 0.025(3) 0.022(3) 0.002(2) -0.007(3) -0.015(3) C13 0.080(5) 0.044(4) 0.040(3) 0.012(3) -0.012(3) -0.001(4) C14 0.063(5) 0.030(3) 0.023(3) 0.007(3) 0.002(3) -0.014(3) C15 0.029(3) 0.030(3) 0.031(3) -0.010(2) 0.001(2) -0.007(2) C16 0.054(4) 0.025(3) 0.036(4) 0.003(3) 0.006(3) -0.013(3) C17 0.015(3) 0.020(3) 0.029(3) -0.008(2) 0.004(2) -0.002(2) C19 0.022(3) 0.017(3) 0.043(4) 0.000(2) 0.005(3) -0.001(2) C20 0.029(3) 0.024(3) 0.024(3) 0.000(2) 0.005(2) 0.003(2) C21 0.034(4) 0.036(4) 0.061(5) -0.003(3) -0.004(3) 0.012(3) C22 0.045(4) 0.038(3) 0.033(3) -0.014(3) 0.002(3) 0.011(3) C23 0.062(4) 0.044(4) 0.037(3) -0.008(3) -0.005(3) 0.034(4) C24 0.047(4) 0.041(4) 0.043(4) 0.002(3) 0.004(3) 0.011(3) C25 0.223(13) 0.151(10) 0.148(10) 0.008(7) 0.064(9) 0.094(9) C26 0.037(4) 0.033(4) 0.082(5) -0.013(3) 0.007(4) 0.015(3) C27 0.054(5) 0.047(4) 0.044(4) 0.007(3) 0.006(3) 0.010(4) C28 0.046(4) 0.038(4) 0.049(4) -0.005(3) 0.000(3) 0.026(3) C29 0.039(4) 0.035(4) 0.058(4) 0.004(3) -0.011(3) 0.011(3) C30 0.078(6) 0.049(5) 0.079(6) -0.038(4) -0.041(4) 0.032(4) C31 0.044(4) 0.032(4) 0.033(3) -0.003(2) -0.001(3) 0.005(3) C32 0.066(4) 0.054(4) 0.090(5) -0.018(4) -0.042(4) 0.051(4) C33 0.031(3) 0.027(3) 0.032(3) -0.009(2) -0.011(3) 0.012(3) C34 0.076(5) 0.047(4) 0.064(5) -0.045(3) -0.047(4) 0.035(4) C35 0.043(4) 0.031(3) 0.024(3) -0.008(3) 0.002(3) 0.013(3) C36 0.020(3) 0.022(3) 0.037(3) -0.004(2) 0.002(2) 0.001(2) C37 0.036(3) 0.061(4) 0.023(2) -0.001(2) -0.005(2) -0.007(2) C38 0.027(2) 0.040(2) 0.024(2) 0.005(3) 0.0071(16) -0.004(3) C39 0.035(2) 0.041(3) 0.0212(19) -0.010(2) -0.0053(17) 0.004(3) C40 0.034(3) 0.072(4) 0.028(3) -0.003(2) 0.012(2) -0.016(3) C41 0.022(2) 0.053(4) 0.018(2) 0.020(3) 0.0021(17) -0.010(3) C42 0.023(2) 0.048(3) 0.0140(19) -0.014(3) -0.0012(16) 0.001(3) C43 0.053(4) 0.042(3) 0.023(3) -0.001(2) 0.012(2) -0.025(3) C44 0.038(3) 0.059(3) 0.024(3) -0.005(2) 0.003(2) -0.006(3) C45 0.035(3) 0.034(3) 0.036(3) -0.006(2) 0.008(2) -0.004(2) C46 0.041(3) 0.029(3) 0.021(2) -0.003(2) -0.003(2) -0.003(2) C47 0.027(3) 0.032(3) 0.029(3) 0.000(2) 0.000(2) 0.003(2) C48 0.041(4) 0.020(3) 0.019(3) 0.008(2) -0.002(3) -0.012(3) C49 0.049(4) 0.027(3) 0.025(3) 0.014(2) -0.012(3) -0.010(3) C50 0.036(3) 0.024(3) 0.024(3) 0.002(2) -0.009(2) -0.007(2) C51 0.037(3) 0.036(3) 0.033(3) 0.005(3) -0.005(2) -0.014(3) C52 0.071(4) 0.029(3) 0.029(3) -0.003(2) -0.017(3) -0.037(3) C53 0.027(3) 0.024(3) 0.037(3) 0.012(2) 0.003(2) -0.007(2) C54 0.039(4) 0.017(3) 0.036(3) 0.003(2) 0.003(3) -0.003(3) C55 0.034(4) 0.027(3) 0.045(4) 0.005(3) 0.007(3) -0.012(3) C56 0.040(4) 0.029(3) 0.034(3) -0.001(2) -0.001(3) -0.002(3) C57 0.035(4) 0.020(3) 0.039(3) 0.003(3) 0.004(3) -0.008(3) C58 0.031(3) 0.023(3) 0.030(3) -0.001(3) -0.009(2) -0.006(3) C59 0.042(3) 0.032(4) 0.034(3) 0.001(3) -0.001(2) -0.012(3) C60 0.083(4) 0.038(3) 0.030(3) 0.007(2) -0.003(3) -0.030(3) C61 0.047(4) 0.024(3) 0.025(3) 0.003(2) -0.011(3) -0.009(3) C62 0.037(4) 0.030(3) 0.036(3) 0.012(2) 0.004(3) 0.000(3) C63 0.025(3) 0.023(3) 0.035(4) -0.010(3) 0.003(3) -0.006(3) C64 0.023(3) 0.014(3) 0.030(3) 0.001(2) 0.007(2) 0.000(2) C65 0.054(3) 0.028(3) 0.024(3) -0.003(2) 0.002(2) -0.002(2) C66 0.097(5) 0.021(3) 0.027(3) 0.004(2) 0.007(3) -0.026(3) C67 0.099(5) 0.018(2) 0.018(2) -0.0042(19) 0.003(3) -0.016(3) C68 0.053(4) 0.031(3) 0.024(3) 0.009(2) 0.001(2) -0.015(2) C69 0.047(3) 0.021(2) 0.020(2) 0.009(3) 0.006(2) -0.003(3) N1 0.0227(18) 0.024(2) 0.0218(17) 0.005(2) -0.0021(14) -0.001(2) N2 0.0232(17) 0.0221(17) 0.0173(16) -0.003(2) 0.0021(13) 0.002(3) N3 0.031(2) 0.026(2) 0.022(2) 0.004(2) -0.0039(16) -0.006(2) O1 0.043(3) 0.043(3) 0.033(2) 0.004(2) -0.003(2) -0.017(2) O2 0.030(2) 0.026(2) 0.0199(19) 0.0027(15) 0.0016(16) -0.0086(17) O3 0.051(3) 0.023(2) 0.034(2) 0.0021(18) 0.013(2) -0.0106(19) O4 0.031(2) 0.025(2) 0.026(2) 0.0002(17) -0.0061(18) -0.0196(18) O5 0.038(2) 0.040(3) 0.025(2) 0.0002(18) -0.0078(18) 0.026(2) O6 0.044(3) 0.026(2) 0.033(2) -0.0077(17) 0.007(2) 0.0090(19) O7 0.039(3) 0.030(2) 0.028(2) 0.0025(17) -0.0031(18) 0.0119(18) O8 0.045(3) 0.026(2) 0.036(3) 0.0024(19) -0.003(2) 0.007(2) O9 0.044(3) 0.029(2) 0.028(2) -0.0066(18) 0.002(2) -0.0176(19) O10 0.044(3) 0.027(2) 0.044(3) 0.0029(18) 0.008(2) -0.0133(19) O11 0.044(3) 0.034(3) 0.032(2) -0.0026(19) 0.002(2) -0.004(2) O12 0.032(2) 0.026(2) 0.026(2) 0.0062(17) -0.0039(17) -0.0116(17) Zn1 0.0257(3) 0.0177(2) 0.0188(2) 0.0001(3) 0.0001(2) 0.0002(3) Zn2 0.0236(3) 0.0189(2) 0.0168(2) -0.0014(3) 0.00123(18) 0.0011(4) Zn3 0.0252(3) 0.0177(2) 0.0175(2) 0.0000(3) 0.00125(18) -0.0016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.240(7) . ? C1 O2 1.274(7) . ? C1 C2 1.447(8) . ? C2 C4 1.417(7) . ? C2 C3 1.458(8) . ? C3 C6 1.390(8) . ? C4 C5 1.378(8) . ? C5 C8 1.432(8) . ? C6 C8 1.392(8) . ? C6 C7 1.543(7) . ? C8 C9 1.416(8) . ? C9 C10 1.196(6) . ? C10 C11 1.416(8) . ? C11 C12 1.380(7) . ? C11 C14 1.394(8) . ? C12 C16 1.409(8) . ? C12 C13 1.478(8) . ? C14 C15 1.376(8) . ? C15 C17 1.328(8) . ? C16 C17 1.365(8) . ? C17 C18 1.560(7) . ? C18 O3 1.205(6) . ? C18 O4 1.273(6) . ? C19 O5 1.226(7) . ? C19 O6 1.259(7) . ? C19 C20 1.533(7) . ? C20 C21 1.290(8) . ? C20 C22 1.347(8) . ? C21 C24 1.394(8) . ? C22 C23 1.420(8) . ? C23 C26 1.371(9) . ? C24 C26 1.396(9) . ? C24 C25 1.552(11) . ? C26 C27 1.452(9) . ? C27 C28 1.181(7) . ? C28 C29 1.446(8) . ? C29 C31 1.414(8) . ? C29 C30 1.423(9) . ? C30 C34 1.336(8) . ? C31 C33 1.366(7) . ? C31 C32 1.510(8) . ? C33 C35 1.388(8) . ? C34 C35 1.453(8) . ? C35 C36 1.476(8) . ? C36 O8 1.251(7) . ? C36 O7 1.289(7) . ? C37 C40 1.332(6) . ? C37 N1 1.338(5) . ? C38 N1 1.339(5) . ? C38 C39 1.368(5) . ? C39 C41 1.375(5) . ? C40 C41 1.398(6) . ? C41 C42 1.506(5) . ? C42 C44 1.366(7) . ? C42 C43 1.408(7) . ? C43 C46 1.392(6) . ? C44 C45 1.378(6) . ? C45 N2 1.301(6) . ? C46 N2 1.330(6) . ? C47 O11 1.266(7) . ? C47 O12 1.296(7) . ? C47 C48 1.465(8) . ? C48 C50 1.409(7) . ? C48 C49 1.456(7) . ? C49 C53 1.396(7) . ? C50 C51 1.367(7) . ? C51 C54 1.453(8) . ? C51 C52 1.505(7) . ? C53 C54 1.366(8) . ? C54 C55 1.463(8) . ? C55 C56 1.178(6) . ? C56 C57 1.462(8) . ? C57 C58 1.367(8) . ? C57 C59 1.390(8) . ? C58 C62 1.363(7) . ? C59 C61 1.419(8) . ? C59 C60 1.484(8) . ? C61 C63 1.301(8) . ? C62 C63 1.396(8) . ? C63 C64 1.526(7) . ? C64 O9 1.243(7) . ? C64 O10 1.257(7) . ? C65 N3 1.353(6) . ? C65 C68 1.355(6) . ? C66 N3 1.362(6) . ? C66 C67 1.365(6) . ? C67 C69 1.418(7) . ? C68 C69 1.349(7) . ? C69 C69 1.494(8) 2_656 ? N1 Zn2 2.033(3) . ? N2 Zn3 2.040(3) 1_554 ? N3 Zn1 2.031(3) . ? O1 Zn2 2.032(4) . ? O2 Zn3 2.006(4) . ? O3 Zn2 2.044(4) 3 ? O4 Zn3 2.057(3) 3 ? O5 Zn2 2.031(4) . ? O6 Zn3 2.052(4) . ? O7 Zn2 2.007(4) 3_545 ? O8 Zn3 2.051(4) 3_545 ? O9 Zn1 2.039(4) 4_657 ? O10 Zn1 2.055(4) 3 ? O11 Zn1 2.039(4) . ? O12 Zn1 2.013(4) 2_657 ? Zn1 O12 2.013(4) 2_657 ? Zn1 O9 2.039(4) 4_647 ? Zn1 O10 2.055(4) 3_445 ? Zn1 Zn1 2.9354(10) 2_657 ? Zn2 O7 2.007(4) 3_455 ? Zn2 O3 2.044(4) 3_445 ? Zn2 Zn3 2.9430(7) . ? Zn3 N2 2.040(3) 1_556 ? Zn3 O8 2.051(4) 3_455 ? Zn3 O4 2.057(4) 3_445 ? 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 O1 C1 O2 123.1(6) . . ? O1 C1 C2 118.8(5) . . ? O2 C1 C2 118.0(5) . . ? C4 C2 C1 122.3(5) . . ? C4 C2 C3 118.8(5) . . ? C1 C2 C3 118.9(5) . . ? C6 C3 C2 120.0(5) . . ? C5 C4 C2 119.6(5) . . ? C4 C5 C8 121.6(5) . . ? C3 C6 C8 120.6(5) . . ? C3 C6 C7 117.2(5) . . ? C8 C6 C7 122.0(5) . . ? C6 C8 C9 122.6(5) . . ? C6 C8 C5 119.3(5) . . ? C9 C8 C5 118.0(5) . . ? C10 C9 C8 178.8(6) . . ? C9 C10 C11 179.2(6) . . ? C12 C11 C14 118.1(6) . . ? C12 C11 C10 122.4(6) . . ? C14 C11 C10 119.5(6) . . ? C11 C12 C16 118.6(6) . . ? C11 C12 C13 121.2(5) . . ? C16 C12 C13 120.2(5) . . ? C15 C14 C11 121.1(6) . . ? C17 C15 C14 121.2(6) . . ? C17 C16 C12 121.6(6) . . ? C15 C17 C16 119.3(6) . . ? C15 C17 C18 122.5(5) . . ? C16 C17 C18 118.1(5) . . ? O3 C18 O4 129.1(5) . . ? O3 C18 C17 117.5(5) . . ? O4 C18 C17 113.3(5) . . ? O5 C19 O6 127.2(5) . . ? O5 C19 C20 116.5(5) . . ? O6 C19 C20 116.3(5) . . ? C21 C20 C22 119.2(6) . . ? C21 C20 C19 121.4(6) . . ? C22 C20 C19 119.2(5) . . ? C20 C21 C24 124.9(7) . . ? C20 C22 C23 120.7(6) . . ? C26 C23 C22 118.4(6) . . ? C21 C24 C26 116.3(6) . . ? C21 C24 C25 120.1(7) . . ? C26 C24 C25 122.9(7) . . ? C23 C26 C24 120.1(6) . . ? C23 C26 C27 118.2(7) . . ? C24 C26 C27 121.7(7) . . ? C28 C27 C26 178.0(7) . . ? C27 C28 C29 176.3(7) . . ? C31 C29 C30 120.5(6) . . ? C31 C29 C28 119.7(6) . . ? C30 C29 C28 119.8(6) . . ? C34 C30 C29 121.5(6) . . ? C33 C31 C29 117.3(5) . . ? C33 C31 C32 121.0(5) . . ? C29 C31 C32 121.7(5) . . ? C31 C33 C35 123.1(5) . . ? C30 C34 C35 118.6(6) . . ? C33 C35 C34 118.7(5) . . ? C33 C35 C36 121.2(5) . . ? C34 C35 C36 119.8(6) . . ? O8 C36 O7 122.8(5) . . ? O8 C36 C35 121.5(6) . . ? O7 C36 C35 115.3(6) . . ? C40 C37 N1 123.6(4) . . ? N1 C38 C39 122.7(4) . . ? C38 C39 C41 118.7(4) . . ? C37 C40 C41 118.9(4) . . ? C39 C41 C40 118.3(4) . . ? C39 C41 C42 120.9(4) . . ? C40 C41 C42 120.7(4) . . ? C44 C42 C43 117.0(4) . . ? C44 C42 C41 122.8(4) . . ? C43 C42 C41 120.2(4) . . ? C46 C43 C42 117.3(4) . . ? C42 C44 C45 121.0(5) . . ? N2 C45 C44 122.8(5) . . ? N2 C46 C43 124.0(4) . . ? O11 C47 O12 123.3(6) . . ? O11 C47 C48 119.2(6) . . ? O12 C47 C48 117.4(5) . . ? C50 C48 C49 119.8(5) . . ? C50 C48 C47 121.1(5) . . ? C49 C48 C47 119.0(5) . . ? C53 C49 C48 117.3(5) . . ? C51 C50 C48 121.9(6) . . ? C50 C51 C54 117.6(5) . . ? C50 C51 C52 121.9(5) . . ? C54 C51 C52 120.5(5) . . ? C54 C53 C49 121.7(5) . . ? C53 C54 C51 121.4(5) . . ? C53 C54 C55 121.2(6) . . ? C51 C54 C55 117.4(6) . . ? C56 C55 C54 177.9(6) . . ? C55 C56 C57 175.7(6) . . ? C58 C57 C59 122.4(6) . . ? C58 C57 C56 120.2(6) . . ? C59 C57 C56 117.4(6) . . ? C62 C58 C57 119.3(5) . . ? C57 C59 C61 114.4(6) . . ? C57 C59 C60 122.6(6) . . ? C61 C59 C60 123.0(5) . . ? C63 C61 C59 124.7(6) . . ? C58 C62 C63 120.5(6) . . ? C61 C63 C62 118.6(6) . . ? C61 C63 C64 121.0(6) . . ? C62 C63 C64 119.9(6) . . ? O9 C64 O10 128.0(5) . . ? O9 C64 C63 116.1(5) . . ? O10 C64 C63 115.6(5) . . ? N3 C65 C68 121.8(4) . . ? N3 C66 C67 122.2(4) . . ? C66 C67 C69 118.9(4) . . ? C69 C68 C65 121.7(4) . . ? C68 C69 C67 117.6(4) . . ? C68 C69 C69 122.3(3) . 2_656 ? C67 C69 C69 120.1(3) . 2_656 ? C37 N1 C38 117.3(3) . . ? C37 N1 Zn2 121.0(3) . . ? C38 N1 Zn2 121.7(3) . . ? C45 N2 C46 117.8(4) . . ? C45 N2 Zn3 121.5(3) . 1_554 ? C46 N2 Zn3 120.7(3) . 1_554 ? C65 N3 C66 117.8(4) . . ? C65 N3 Zn1 120.9(4) . . ? C66 N3 Zn1 121.3(3) . . ? C1 O1 Zn2 134.0(4) . . ? C1 O2 Zn3 123.6(4) . . ? C18 O3 Zn2 126.4(4) . 3 ? C18 O4 Zn3 124.0(4) . 3 ? C19 O5 Zn2 124.6(4) . . ? C19 O6 Zn3 128.1(4) . . ? C36 O7 Zn2 126.2(4) . 3_545 ? C36 O8 Zn3 130.8(4) . 3_545 ? C64 O9 Zn1 130.9(4) . 4_657 ? C64 O10 Zn1 118.9(4) . 3 ? C47 O11 Zn1 126.2(4) . . ? C47 O12 Zn1 128.9(4) . 2_657 ? O12 Zn1 N3 105.75(17) 2_657 . ? O12 Zn1 O9 154.73(15) 2_657 4_647 ? N3 Zn1 O9 99.52(17) . 4_647 ? O12 Zn1 O11 87.18(17) 2_657 . ? N3 Zn1 O11 95.84(18) . . ? O9 Zn1 O11 90.07(14) 4_647 . ? O12 Zn1 O10 89.90(14) 2_657 3_445 ? N3 Zn1 O10 98.34(19) . 3_445 ? O9 Zn1 O10 86.65(18) 4_647 3_445 ? O11 Zn1 O10 165.79(17) . 3_445 ? O12 Zn1 Zn1 79.10(11) 2_657 2_657 ? N3 Zn1 Zn1 174.26(11) . 2_657 ? O9 Zn1 Zn1 75.66(11) 4_647 2_657 ? O11 Zn1 Zn1 81.18(12) . 2_657 ? O10 Zn1 Zn1 84.61(13) 3_445 2_657 ? O7 Zn2 O5 163.48(16) 3_455 . ? O7 Zn2 O1 89.26(18) 3_455 . ? O5 Zn2 O1 90.20(12) . . ? O7 Zn2 N1 99.38(16) 3_455 . ? O5 Zn2 N1 97.05(16) . . ? O1 Zn2 N1 97.72(16) . . ? O7 Zn2 O3 87.40(12) 3_455 3_445 ? O5 Zn2 O3 86.24(19) . 3_445 ? O1 Zn2 O3 155.44(16) . 3_445 ? N1 Zn2 O3 106.83(17) . 3_445 ? O7 Zn2 Zn3 81.97(12) 3_455 . ? O5 Zn2 Zn3 81.92(11) . . ? O1 Zn2 Zn3 75.45(12) . . ? N1 Zn2 Zn3 173.06(11) . . ? O3 Zn2 Zn3 79.99(12) 3_445 . ? O2 Zn3 N2 99.08(17) . 1_556 ? O2 Zn3 O8 87.19(18) . 3_455 ? N2 Zn3 O8 98.27(17) 1_556 3_455 ? O2 Zn3 O6 89.64(11) . . ? N2 Zn3 O6 106.13(17) 1_556 . ? O8 Zn3 O6 155.58(16) 3_455 . ? O2 Zn3 O4 163.83(15) . 3_445 ? N2 Zn3 O4 97.09(17) 1_556 3_445 ? O8 Zn3 O4 90.12(11) 3_455 3_445 ? O6 Zn3 O4 86.24(17) . 3_445 ? O2 Zn3 Zn2 83.65(10) . . ? N2 Zn3 Zn2 175.11(9) 1_556 . ? O8 Zn3 Zn2 77.74(12) 3_455 . ? O6 Zn3 Zn2 77.85(11) . . ? O4 Zn3 Zn2 80.20(11) 3_445 . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.085 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.081 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 1 0.401 0.105 -0.055 3441.1 820.8 2 0.000 0.277 0.000 35.4 -2.5 3 0.500 0.777 0.000 35.4 -2.5 _platon_squeeze_details ; ? ; #===END # The data for C were poor, and all the disorder could not be satisfactorily # modeled, resulting in lack of convergence. As no other suitable single # crystals could be grown, the available data was used, solving only the zinc # corners anisotropically. The hyrdrogen atoms of the disordered pyridine # groups were not included. data_CompoundC _database_code_depnum_ccdc_archive 'CCDC 661011' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CompoundC _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H72 N4 O24 Zn4' _chemical_formula_weight 1879.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.909(16) _cell_length_b 27.458(16) _cell_length_c 14.013(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.183(17) _cell_angle_gamma 90.00 _cell_volume 8417(10) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6066 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.08 _exptl_crystal_description needle _exptl_crystal_colour light _exptl_crystal_size_max 0.071 _exptl_crystal_size_mid 0.044 _exptl_crystal_size_min 0.0135 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8500 _exptl_absorpt_correction_T_max 0.9684 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39326 _diffrn_reflns_av_R_equivalents 0.1299 _diffrn_reflns_av_sigmaI/netI 0.2730 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.96 _reflns_number_total 19782 _reflns_number_gt 6673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1387P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(3) _refine_ls_number_reflns 19782 _refine_ls_number_parameters 298 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.2053 _refine_ls_R_factor_gt 0.1142 _refine_ls_wR_factor_ref 0.3222 _refine_ls_wR_factor_gt 0.2882 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 5.598 _refine_ls_shift/su_mean 0.249 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 C5 C 0.6262(3) 0.9709(4) 0.2625(5) 0.0236(17) Uiso 1 1 d D . . C6 C 0.6278(3) 0.9685(4) 0.1555(5) 0.0225(19) Uiso 1 1 d D A . C11 C 1.0358(5) 0.5310(4) 0.7027(8) 0.045(3) Uiso 1 1 d . . . C12 C 0.9863(4) 0.5673(3) 0.7004(7) 0.041(3) Uiso 1 1 d D . . C13 C 0.9763(5) 0.5960(4) 0.7837(9) 0.053(3) Uiso 1 1 d D . . H13 H 0.9986 0.5882 0.8418 0.063 Uiso 1 1 calc R . . C14 C 0.9537(4) 0.5784(3) 0.6143(8) 0.046(3) Uiso 1 1 d D . . H14 H 0.9595 0.5596 0.5587 0.055 Uiso 1 1 calc R . . C15 C 0.9354(5) 0.6348(4) 0.7831(9) 0.066(4) Uiso 1 1 d D . . H15 H 0.9294 0.6533 0.8390 0.079 Uiso 1 1 calc R . . C16 C 0.9115(5) 0.6182(5) 0.6103(11) 0.085(5) Uiso 1 1 d D . . C17 C 0.9041(5) 0.6450(4) 0.6971(10) 0.071(4) Uiso 1 1 d D . . C18 C 0.8652(7) 0.6842(6) 0.7020(12) 0.109(6) Uiso 1 1 d D . . C19 C 0.8310(10) 0.7172(9) 0.7036(19) 0.181(10) Uiso 1 1 d D . . C20 C 0.8013(5) 0.7653(5) 0.7024(12) 0.089(5) Uiso 1 1 d D . . C21 C 0.7838(5) 0.7836(5) 0.7948(13) 0.099(5) Uiso 1 1 d D . . H21 H 0.7951 0.7666 0.8521 0.119 Uiso 1 1 calc R . . C22 C 0.7840(5) 0.7913(5) 0.6188(10) 0.075(4) Uiso 1 1 d D . . C23 C 0.7492(5) 0.8273(4) 0.7968(10) 0.069(4) Uiso 1 1 d D . . H23 H 0.7373 0.8398 0.8561 0.082 Uiso 1 1 calc R . . C24 C 0.7505(4) 0.8339(4) 0.6239(9) 0.060(3) Uiso 1 1 d D . . H24 H 0.7390 0.8512 0.5670 0.072 Uiso 1 1 calc R . . C25 C 0.7330(4) 0.8519(4) 0.7135(9) 0.059(3) Uiso 1 1 d D . . C26 C 0.6967(4) 0.8982(4) 0.7132(8) 0.043(3) Uiso 1 1 d D A . C27 C 0.8092(8) 0.7744(6) 0.5216(12) 0.109(6) Uiso 1 1 d D . . H27A H 0.8543 0.7773 0.5234 0.131 Uiso 1 1 calc R . . H27B H 0.7977 0.7402 0.5075 0.131 Uiso 1 1 calc R . . C28 C 0.8753(7) 0.6305(6) 0.5165(12) 0.119(6) Uiso 1 1 d D . . H28A H 0.8786 0.6027 0.4722 0.143 Uiso 1 1 calc R . . H28B H 0.8316 0.6339 0.5301 0.143 Uiso 1 1 calc R . . C29 C 0.7197(6) 1.0275(5) 0.7115(9) 0.064(4) Uiso 1 1 d . A . C30 C 0.7625(5) 1.0725(4) 0.7188(9) 0.054(3) Uiso 1 1 d D . . C31 C 0.7841(6) 1.0888(5) 0.8088(11) 0.081(4) Uiso 1 1 d D . . H31 H 0.7707 1.0743 0.8656 0.098 Uiso 1 1 calc R . . C32 C 0.7787(6) 1.0909(5) 0.6354(11) 0.084(5) Uiso 1 1 d D . . H32 H 0.7615 1.0778 0.5771 0.101 Uiso 1 1 calc R . . C33 C 0.8248(7) 1.1261(6) 0.8122(16) 0.130(7) Uiso 1 1 d D . . C34 C 0.8204(7) 1.1288(6) 0.6334(14) 0.116(6) Uiso 1 1 d D . . H34 H 0.8328 1.1423 0.5751 0.139 Uiso 1 1 calc R . . C35 C 0.8424(6) 1.1456(5) 0.7196(13) 0.098(5) Uiso 1 1 d D . . C36 C 0.8877(8) 1.1873(7) 0.7268(15) 0.124(7) Uiso 1 1 d D . . C37 C 0.9250(8) 1.2215(7) 0.7304(15) 0.134(7) Uiso 1 1 d D . . C38 C 0.9541(5) 1.2674(5) 0.7260(12) 0.086(5) Uiso 1 1 d D . . C39 C 0.9699(7) 1.2920(7) 0.8059(17) 0.140(8) Uiso 1 1 d D . . C40 C 0.9743(10) 1.2853(11) 0.633(3) 0.234(14) Uiso 1 1 d D . . H40 H 0.9633 1.2681 0.5761 0.281 Uiso 1 1 calc R . . C41 C 1.0057(5) 1.3349(5) 0.8022(11) 0.081(5) Uiso 1 1 d D . . H41 H 1.0172 1.3524 0.8588 0.097 Uiso 1 1 calc R . . C42 C 1.0063(6) 1.3238(6) 0.6301(12) 0.095(5) Uiso 1 1 d D . . H42 H 1.0190 1.3347 0.5700 0.114 Uiso 1 1 calc R . . C43 C 1.0238(4) 1.3509(4) 0.7128(8) 0.043(3) Uiso 1 1 d D . . C44 C 1.0599(5) 1.3949(4) 0.7077(8) 0.049(3) Uiso 1 1 d . . . C45 C 0.977(3) 1.272(2) 0.918(3) 0.41(4) Uiso 1 1 d D . . H45A H 0.9666 1.2375 0.9231 0.496 Uiso 1 1 calc R . . H45B H 1.0184 1.2782 0.9472 0.496 Uiso 1 1 calc R . . C46 C 0.850(8) 1.151(5) 0.914(3) 1.9(3) Uiso 1 1 d D . . H46A H 0.8938 1.1432 0.9264 2.313 Uiso 1 1 calc R . . H46B H 0.8458 1.1869 0.9097 2.313 Uiso 1 1 calc R . . C1A C 0.6650(13) 0.9905(8) 0.424(2) 0.018(8) Uiso 0.313(14) 1 d PD A 1 C2A C 0.6769(15) 0.9951(10) 0.318(3) 0.019(10) Uiso 0.313(14) 1 d PD A 1 C3A C 0.589(2) 0.9546(11) 0.305(4) 0.072(18) Uiso 0.313(14) 1 d PD A 1 C4A C 0.5748(10) 0.9488(8) 0.4007(16) 0.000(6) Uiso 0.313(14) 1 d PD A 1 C7A C 0.6803(8) 0.9721(7) 0.1098(12) 0.063(6) Uiso 0.555(12) 1 d PD A 3 C8A C 0.6790(7) 0.9756(7) 0.0090(11) 0.050(5) Uiso 0.555(12) 1 d PD A 3 C9A C 0.5735(7) 0.9687(6) 0.0051(10) 0.038(4) Uiso 0.555(12) 1 d PD A 3 C10A C 0.5695(8) 0.9658(6) 0.1011(12) 0.057(6) Uiso 0.555(12) 1 d PD A 3 C1B C 0.6758(7) 0.9510(5) 0.4143(13) 0.039(5) Uiso 0.687(14) 1 d PD A 2 C2B C 0.6738(9) 0.9517(6) 0.3194(18) 0.055(7) Uiso 0.687(14) 1 d PD A 2 C3B C 0.5774(8) 0.9917(5) 0.3104(12) 0.030(5) Uiso 0.687(14) 1 d PD A 2 C4B C 0.5829(8) 0.9894(5) 0.4142(14) 0.050(6) Uiso 0.687(14) 1 d PD A 2 C7B C 0.6536(8) 1.0119(8) 0.1086(16) 0.053(8) Uiso 0.445(12) 1 d PD A 4 C8B C 0.6510(7) 1.0112(8) 0.0105(14) 0.038(6) Uiso 0.445(12) 1 d PD A 4 C9B C 0.6045(8) 0.9367(9) 0.0064(17) 0.059(8) Uiso 0.445(12) 1 d PD A 4 C10B C 0.6040(8) 0.9323(9) 0.1031(17) 0.058(8) Uiso 0.445(12) 1 d PD A 4 N1 N 0.6245(3) 0.9722(4) 0.4591(4) 0.0247(14) Uiso 1 1 d D . . N2 N 0.6272(3) 0.9737(4) -0.0409(4) 0.0296(15) Uiso 1 1 d D . . O1 O 0.6933(3) 0.9276(3) 0.6352(6) 0.047(2) Uiso 1 1 d . . . O2 O 0.6789(4) 1.0294(3) 0.6358(6) 0.056(3) Uiso 1 1 d . . . O3 O 1.0705(3) 0.5326(3) 0.6307(6) 0.050(2) Uiso 1 1 d . . . O4 O 1.0522(3) 1.4292(3) 0.6201(5) 0.046(2) Uiso 1 1 d . . . O5 O 1.0726(4) 0.5290(3) 0.7824(6) 0.056(3) Uiso 1 1 d . . . O6 O 0.6829(3) 1.0317(3) 0.7926(5) 0.049(2) Uiso 1 1 d . . . O7 O 0.7014(4) 0.9300(3) 0.7972(6) 0.068(3) Uiso 1 1 d . . . O8 O 1.0557(3) 1.4268(3) 0.7866(6) 0.052(2) Uiso 1 1 d . . . O9 O 0.7815(9) 0.8066(8) 0.4518(16) 0.226(8) Uiso 1 1 d D . . H9 H 0.8038 0.8089 0.4053 0.339 Uiso 1 1 calc R . . O10 O 0.8923(6) 0.6698(5) 0.4735(11) 0.141(5) Uiso 1 1 d D . . H10 H 0.9300 0.6685 0.4660 0.212 Uiso 1 1 calc R . . O11 O 0.934(3) 1.301(3) 0.960(7) 0.77(5) Uiso 1 1 d D . . H11 H 0.9214 1.3229 0.9214 1.156 Uiso 1 1 calc R . . O12 O 0.8152(17) 1.1328(11) 0.992(3) 0.362(15) Uiso 1 1 d D . . H12 H 0.7798 1.1446 0.9874 0.542 Uiso 1 1 calc R . . Zn1 Zn 0.62357(5) 0.97348(8) 0.60536(5) 0.0314(3) Uani 1 1 d . . . Zn2 Zn 0.62848(5) 0.97292(8) 0.81429(5) 0.0324(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0645(8) 0.0261(5) 0.0041(4) -0.0020(10) 0.0066(4) 0.0004(11) Zn2 0.0646(8) 0.0283(5) 0.0048(4) -0.0009(11) 0.0062(4) 0.0050(12) _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 C5 C3A 1.12(5) . ? C5 C2B 1.38(2) . ? C5 C2A 1.48(4) . ? C5 C3B 1.414(19) . ? C5 C6 1.503(9) . ? C6 C7A 1.351(18) . ? C6 C7B 1.49(2) . ? C6 C10A 1.452(18) . ? C6 C10B 1.33(3) . ? C11 O5 1.341(13) . ? C11 O3 1.299(12) . ? C11 C12 1.471(14) . ? C12 C14 1.402(14) . ? C12 C13 1.436(14) . ? C13 C15 1.391(15) . ? C14 C16 1.430(17) . ? C15 C17 1.382(17) . ? C16 C17 1.437(18) . ? C16 C28 1.535(17) . ? C17 C18 1.38(2) . ? C18 C19 1.18(3) . ? C19 C20 1.47(3) . ? C20 C22 1.406(19) . ? C20 C21 1.46(2) . ? C21 C23 1.421(18) . ? C22 C24 1.386(16) . ? C22 C27 1.567(17) . ? C23 C25 1.376(16) . ? C24 C25 1.421(16) . ? C25 C26 1.502(15) . ? C26 O1 1.357(12) . ? C26 O7 1.463(13) . ? C27 O9 1.429(18) . ? C28 O10 1.300(14) . ? C29 O2 1.350(15) . ? C29 O6 1.433(14) . ? C29 C30 1.551(16) . ? C30 C32 1.339(17) . ? C30 C31 1.395(17) . ? C31 C33 1.36(2) . ? C32 C34 1.39(2) . ? C33 C35 1.48(2) . ? C33 C46 1.65(4) . ? C34 C35 1.36(2) . ? C35 C36 1.51(2) . ? C36 C37 1.25(2) . ? C37 C38 1.42(2) . ? C38 C39 1.34(2) . ? C38 C40 1.48(3) . ? C39 C41 1.42(2) . ? C39 C45 1.66(3) . ? C40 C42 1.27(3) . ? C41 C43 1.405(17) . ? C42 C43 1.411(18) . ? C43 C44 1.448(15) . ? C44 O8 1.419(13) . ? C44 O4 1.549(13) . ? C45 O11 1.38(5) . ? C46 O12 1.45(4) . ? C1A N1 1.15(3) . ? C1A C2A 1.53(5) . ? C3A C4A 1.41(6) . ? C4A N1 1.47(2) . ? C7A C8A 1.414(19) . ? C8A N2 1.300(16) . ? C9A N2 1.379(15) . ? C9A C10A 1.355(19) . ? C1B N1 1.441(18) . ? C1B C2B 1.33(3) . ? C3B C4B 1.45(2) . ? C4B N1 1.177(18) . ? C7B C8B 1.37(2) . ? C8B N2 1.34(2) . ? C9B N2 1.32(3) . ? C9B C10B 1.36(2) . ? N1 Zn1 2.051(6) . ? N2 Zn2 2.032(6) 1_554 ? O1 Zn1 2.007(8) . ? O2 Zn1 1.988(8) . ? O3 Zn1 2.038(8) 3_545 ? O4 Zn1 2.000(7) 3 ? O5 Zn2 2.001(8) 3_545 ? O6 Zn2 2.041(8) . ? O7 Zn2 2.010(9) . ? O8 Zn2 2.055(8) 3 ? Zn1 O4 2.000(7) 3_445 ? Zn1 O3 2.038(8) 3_455 ? Zn1 Zn2 2.924(2) . ? Zn2 O8 2.055(8) 3_445 ? Zn2 N2 2.032(6) 1_556 ? Zn2 O5 2.001(8) 3_455 ? 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 C3A C5 C2B 95(2) . . ? C3A C5 C2A 116(3) . . ? C2B C5 C2A 49.3(8) . . ? C3A C5 C3B 47.6(9) . . ? C2B C5 C3B 116.5(13) . . ? C2A C5 C3B 97.7(13) . . ? C3A C5 C6 125(3) . . ? C2B C5 C6 120.0(11) . . ? C2A C5 C6 119.1(15) . . ? C3B C5 C6 123.5(9) . . ? C7A C6 C7B 51.5(8) . . ? C7A C6 C10A 120.1(11) . . ? C7B C6 C10A 98.8(10) . . ? C7A C6 C10B 96.4(11) . . ? C7B C6 C10B 120.2(14) . . ? C10A C6 C10B 50.5(8) . . ? C7A C6 C5 122.5(9) . . ? C7B C6 C5 115.8(12) . . ? C10A C6 C5 117.2(8) . . ? C10B C6 C5 123.8(13) . . ? O5 C11 O3 107.3(10) . . ? O5 C11 C12 117.1(10) . . ? O3 C11 C12 115.0(9) . . ? C14 C12 C13 119.1(10) . . ? C14 C12 C11 120.5(10) . . ? C13 C12 C11 119.9(10) . . ? C15 C13 C12 122.8(12) . . ? C16 C14 C12 119.9(11) . . ? C17 C15 C13 116.7(13) . . ? C14 C16 C17 117.4(13) . . ? C14 C16 C28 120.2(14) . . ? C17 C16 C28 122.4(15) . . ? C15 C17 C18 113.2(14) . . ? C15 C17 C16 124.1(14) . . ? C18 C17 C16 122.7(15) . . ? C19 C18 C17 178(2) . . ? C18 C19 C20 166.5(8) . . ? C22 C20 C21 119.5(16) . . ? C22 C20 C19 124.2(17) . . ? C21 C20 C19 115.9(17) . . ? C23 C21 C20 118.4(16) . . ? C20 C22 C24 120.3(13) . . ? C20 C22 C27 118.9(14) . . ? C24 C22 C27 120.5(13) . . ? C25 C23 C21 120.6(14) . . ? C22 C24 C25 120.5(13) . . ? C24 C25 C23 120.7(13) . . ? C24 C25 C26 117.4(11) . . ? C23 C25 C26 121.9(12) . . ? O1 C26 O7 107.0(8) . . ? O1 C26 C25 120.7(9) . . ? O7 C26 C25 119.3(9) . . ? O9 C27 C22 104.8(16) . . ? O10 C28 C16 115.6(12) . . ? O2 C29 O6 104.0(10) . . ? O2 C29 C30 113.2(10) . . ? O6 C29 C30 104.3(10) . . ? C32 C30 C31 125.2(14) . . ? C32 C30 C29 115.5(12) . . ? C31 C30 C29 119.2(12) . . ? C30 C31 C33 117.6(16) . . ? C30 C32 C34 120.4(16) . . ? C31 C33 C35 116.5(19) . . ? C31 C33 C46 122(2) . . ? C35 C33 C46 121(2) . . ? C35 C34 C32 116.0(18) . . ? C34 C35 C33 124.3(19) . . ? C34 C35 C36 121.0(18) . . ? C33 C35 C36 114.7(17) . . ? C37 C36 C35 178(2) . . ? C36 C37 C38 165.2(10) . . ? C39 C38 C40 120(2) . . ? C39 C38 C37 120.6(19) . . ? C40 C38 C37 119(2) . . ? C38 C39 C41 120(2) . . ? C38 C39 C45 129(3) . . ? C41 C39 C45 106(3) . . ? C42 C40 C38 120(3) . . ? C43 C41 C39 118.5(16) . . ? C40 C42 C43 122(2) . . ? C41 C43 C42 119.3(14) . . ? C41 C43 C44 119.1(11) . . ? C42 C43 C44 121.6(12) . . ? O8 C44 O4 103.5(9) . . ? O8 C44 C43 114.7(9) . . ? O4 C44 C43 120.7(9) . . ? O11 C45 C39 101(5) . . ? O12 C46 C33 110(4) . . ? N1 C1A C2A 129(3) . . ? C1A C2A C5 108(3) . . ? C5 C3A C4A 139(5) . . ? N1 C4A C3A 106(3) . . ? C6 C7A C8A 120.5(14) . . ? N2 C8A C7A 120.2(14) . . ? N2 C9A C10A 125.0(13) . . ? C9A C10A C6 114.5(13) . . ? N1 C1B C2B 116.6(16) . . ? C5 C2B C1B 124.5(18) . . ? C4B C3B C5 115.8(14) . . ? N1 C4B C3B 124.9(16) . . ? C8B C7B C6 115.9(19) . . ? C7B C8B N2 122.6(19) . . ? N2 C9B C10B 126(2) . . ? C9B C10B C6 117(2) . . ? C4B N1 C1B 121.9(12) . . ? C4B N1 C1A 100.9(14) . . ? C1B N1 C1A 49.7(8) . . ? C4B N1 C4A 49.6(7) . . ? C1B N1 C4A 98.8(9) . . ? C1A N1 C4A 121.3(18) . . ? C4B N1 Zn1 118.5(10) . . ? C1B N1 Zn1 119.6(8) . . ? C1A N1 Zn1 117.7(16) . . ? C4A N1 Zn1 121.0(9) . . ? C9B N2 C8A 95.8(11) . . ? C9B N2 C9A 48.5(8) . . ? C8A N2 C9A 119.6(10) . . ? C9B N2 C8B 117.7(14) . . ? C8A N2 C8B 51.8(8) . . ? C9A N2 C8B 98.1(10) . . ? C9B N2 Zn2 121.2(12) . 1_554 ? C8A N2 Zn2 118.5(8) . 1_554 ? C9A N2 Zn2 121.7(7) . 1_554 ? C8B N2 Zn2 121.1(10) . 1_554 ? C26 O1 Zn1 123.2(7) . . ? C29 O2 Zn1 120.6(8) . . ? C11 O3 Zn1 118.3(7) . 3_545 ? C44 O4 Zn1 113.6(6) . 3 ? C11 O5 Zn2 123.4(7) . 3_545 ? C29 O6 Zn2 114.4(7) . . ? C26 O7 Zn2 115.1(6) . . ? C44 O8 Zn2 116.4(7) . 3 ? O1 Zn1 O4 100.8(3) . 3_445 ? O1 Zn1 O3 154.0(3) . 3_455 ? O4 Zn1 O3 90.5(3) 3_445 3_455 ? O1 Zn1 O2 89.5(3) . . ? O4 Zn1 O2 156.7(3) 3_445 . ? O3 Zn1 O2 72.3(3) 3_455 . ? O1 Zn1 N1 98.5(3) . . ? O4 Zn1 N1 98.3(3) 3_445 . ? O3 Zn1 N1 103.0(3) 3_455 . ? O2 Zn1 N1 100.8(4) . . ? O1 Zn1 Zn2 78.6(2) . . ? O4 Zn1 Zn2 83.1(2) 3_445 . ? O3 Zn1 Zn2 79.6(2) 3_455 . ? O2 Zn1 Zn2 78.5(3) . . ? N1 Zn1 Zn2 177.0(2) . . ? O8 Zn2 O7 103.3(4) 3_445 . ? O8 Zn2 O6 155.9(3) 3_445 . ? O7 Zn2 O6 88.4(4) . . ? O8 Zn2 N2 98.1(3) 3_445 1_556 ? O7 Zn2 N2 100.4(3) . 1_556 ? O6 Zn2 N2 100.4(4) . 1_556 ? O8 Zn2 O5 88.4(3) 3_445 3_455 ? O7 Zn2 O5 154.8(4) . 3_455 ? O6 Zn2 O5 73.4(3) . 3_455 ? N2 Zn2 O5 99.9(4) 1_556 3_455 ? O8 Zn2 Zn1 80.2(2) 3_445 . ? O7 Zn2 Zn1 82.5(3) . . ? O6 Zn2 Zn1 80.5(2) . . ? N2 Zn2 Zn1 177.0(2) 1_556 . ? O5 Zn2 Zn1 77.5(2) 3_455 . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 28.96 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.710 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.164 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 1 0.005 -0.003 -0.009 4911.9 -19.2 _platon_squeeze_details ; ? ; #===END data_CompoundD _database_code_depnum_ccdc_archive 'CCDC 661012' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CompoundD _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H60 Br12 N6 O24 Zn6' _chemical_formula_weight 3392.94 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.0828(9) _cell_length_b 28.2518(18) _cell_length_c 21.4518(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.5600(10) _cell_angle_gamma 90.00 _cell_volume 8518.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7377 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.46 _exptl_crystal_description columnar _exptl_crystal_colour yellow _exptl_crystal_size_max 0.136 _exptl_crystal_size_mid 0.053 _exptl_crystal_size_min 0.037 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3300 _exptl_absorpt_coefficient_mu 3.699 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2513 _exptl_absorpt_correction_T_max 0.6164 _exptl_absorpt_process_details 'XPREP in SHELXTL (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80578 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.99 _reflns_number_total 38211 _reflns_number_gt 22525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.176(9) _refine_ls_number_reflns 38211 _refine_ls_number_parameters 1565 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br -0.20603(6) 0.48588(3) 0.41373(5) 0.0413(3) Uani 1 1 d . . . Br2 Br -0.20835(7) 0.36988(4) 0.51811(6) 0.0652(4) Uani 1 1 d . . . Br3 Br 0.20991(6) 0.48732(4) 0.07944(6) 0.0630(4) Uani 1 1 d . . . Br4 Br 0.20497(6) 0.36691(3) -0.01405(4) 0.0300(2) Uani 1 1 d . . . Br5 Br 0.90353(8) 0.33211(6) 1.10764(8) 0.0994(6) Uani 1 1 d . . . Br6 Br 0.50127(7) 0.20802(5) 1.16053(7) 0.0821(5) Uani 1 1 d . . . Br7 Br 0.48700(6) 0.33894(4) 0.64070(5) 0.0449(3) Uani 1 1 d . . . Br8 Br 0.48154(6) 0.20481(4) 0.57568(5) 0.0453(3) Uani 1 1 d . . . Br9 Br 0.50148(6) 0.85108(4) 1.12121(5) 0.0496(3) Uani 1 1 d . . . Br10 Br 0.48688(7) 0.72450(5) 1.03889(7) 0.0749(5) Uani 1 1 d . . . Br11 Br 0.46688(13) 0.81103(9) 0.54778(13) 0.1565(11) Uani 1 1 d . . . Br12 Br 0.51179(9) 0.67973(4) 0.61208(6) 0.0655(4) Uani 1 1 d . . . C3 C 1.3935(7) 0.4838(4) 0.9132(6) 0.066(4) Uani 1 1 d . A . H3 H 1.4300 0.4620 0.9384 0.079 Uiso 1 1 calc R . . C4 C 1.2969(7) 0.4808(5) 0.9167(8) 0.089(5) Uani 1 1 d . A . H4 H 1.2691 0.4583 0.9429 0.106 Uiso 1 1 calc R . . C5 C 1.2435(5) 0.5109(3) 0.8814(4) 0.0266(19) Uani 1 1 d . . . C6 C 1.1361(5) 0.5100(4) 0.8806(4) 0.032(2) Uani 1 1 d . A . C7 C 1.0916(6) 0.5460(3) 0.9178(4) 0.037(2) Uani 1 1 d . . . H7 H 1.1287 0.5689 0.9406 0.045 Uiso 1 1 calc R A . C8 C 1.0851(6) 0.4806(3) 0.8471(4) 0.032(2) Uani 1 1 d . . . H8 H 1.1139 0.4579 0.8216 0.039 Uiso 1 1 calc R A . C9 C 0.9851(6) 0.4829(3) 0.8494(4) 0.033(2) Uani 1 1 d . A . H9 H 0.9478 0.4605 0.8258 0.039 Uiso 1 1 calc R . . C10 C 0.9942(6) 0.5457(3) 0.9186(4) 0.031(2) Uani 1 1 d . A . H10 H 0.9640 0.5675 0.9448 0.038 Uiso 1 1 calc R . . C11 C -0.0055(5) 0.2572(3) -0.1680(4) 0.0135(16) Uani 1 1 d . . . C12 C 0.6883(5) 0.4507(3) 0.9683(4) 0.0188(17) Uani 1 1 d . A . C13 C 0.6919(5) 0.4093(3) 1.0141(4) 0.0207(18) Uani 1 1 d . . . C14 C 0.6056(6) 0.3889(3) 1.0281(4) 0.032(2) Uani 1 1 d . . . H14 H 0.5464 0.4024 1.0136 0.038 Uiso 1 1 calc R . . C15 C 0.7769(6) 0.3944(3) 1.0399(4) 0.027(2) Uani 1 1 d . . . H15 H 0.8333 0.4113 1.0323 0.032 Uiso 1 1 calc R . . C16 C 0.7808(6) 0.3557(3) 1.0762(5) 0.039(2) Uani 1 1 d . . . C17 C 0.6098(6) 0.3482(3) 1.0638(4) 0.030(2) Uani 1 1 d . . . H17 H 0.5533 0.3312 1.0709 0.037 Uiso 1 1 calc R . . C18 C 0.6983(5) 0.3320(3) 1.0894(4) 0.029(2) Uani 1 1 d . . . C19 C 0.6998(7) 0.2892(4) 1.1297(5) 0.044(3) Uani 1 1 d . . . C20 C 0.6988(7) 0.2521(3) 1.1567(5) 0.044(3) Uani 1 1 d . . . C21 C 0.6999(6) 0.2099(4) 1.1931(5) 0.038(2) Uani 1 1 d . . . C22 C 0.7813(7) 0.1919(4) 1.2234(5) 0.051(3) Uani 1 1 d . . . H22 H 0.8397 0.2083 1.2199 0.061 Uiso 1 1 calc R . . C23 C 0.6143(7) 0.1846(3) 1.1981(5) 0.042(3) Uani 1 1 d . . . C24 C 0.7813(6) 0.1511(3) 1.2586(4) 0.028(2) Uani 1 1 d . . . H24 H 0.8392 0.1393 1.2777 0.033 Uiso 1 1 calc R . . C25 C 0.6113(6) 0.1445(3) 1.2352(4) 0.030(2) Uani 1 1 d . . . H25 H 0.5527 0.1287 1.2400 0.035 Uiso 1 1 calc R . . C26 C 0.6967(6) 0.1273(3) 1.2660(4) 0.0205(18) Uani 1 1 d . . . C27 C 0.6945(5) 0.0848(3) 1.3042(4) 0.0177(17) Uani 1 1 d . . . C28 C 0.6907(6) 0.4477(3) 0.8019(4) 0.0189(17) Uani 1 1 d . A . C29 C 0.6889(5) 0.4057(3) 0.7574(4) 0.0175(17) Uani 1 1 d . . . C30 C 0.6074(6) 0.3944(3) 0.7234(4) 0.0229(19) Uani 1 1 d . . . H30 H 0.5527 0.4138 0.7257 0.028 Uiso 1 1 calc R . . C31 C 0.7688(6) 0.3778(3) 0.7519(4) 0.0215(18) Uani 1 1 d . . . H31 H 0.8266 0.3865 0.7741 0.026 Uiso 1 1 calc R . . C32 C 0.7673(5) 0.3385(3) 0.7159(4) 0.0230(18) Uani 1 1 d . . . H32 H 0.8224 0.3193 0.7143 0.028 Uiso 1 1 calc R . . C33 C 0.6039(5) 0.3544(3) 0.6853(4) 0.026(2) Uani 1 1 d . . . C34 C 0.6826(5) 0.3264(3) 0.6805(4) 0.0228(19) Uani 1 1 d . . . C35 C 0.6798(6) 0.2838(3) 0.6423(4) 0.028(2) Uani 1 1 d . . . C36 C 0.6810(6) 0.2481(3) 0.6136(4) 0.0229(18) Uani 1 1 d . . . C37 C 0.6841(5) 0.2051(3) 0.5788(4) 0.0172(16) Uani 1 1 d . . . C38 C 0.6003(6) 0.1800(3) 0.5562(4) 0.029(2) Uani 1 1 d . . . C39 C 0.7746(5) 0.1863(3) 0.5660(4) 0.0209(17) Uani 1 1 d . . . H39 H 0.8312 0.2017 0.5816 0.025 Uiso 1 1 calc R . . C40 C 0.7796(5) 0.1453(3) 0.5304(4) 0.0201(18) Uani 1 1 d . . . H40 H 0.8397 0.1328 0.5211 0.024 Uiso 1 1 calc R . . C41 C 0.6052(6) 0.1401(3) 0.5231(4) 0.0238(19) Uani 1 1 d . . . H41 H 0.5484 0.1240 0.5098 0.029 Uiso 1 1 calc R . . C42 C 0.6938(5) 0.1218(3) 0.5077(4) 0.0190(17) Uani 1 1 d . . . C43 C 0.6977(5) 0.0791(3) 0.4659(4) 0.0150(16) Uani 1 1 d . . . C44 C 0.6949(6) 0.9505(3) 1.2978(4) 0.0195(18) Uani 1 1 d . . . C45 C 0.6933(5) 0.9096(2) 1.2528(3) 0.0129(15) Uani 1 1 d . . . C46 C 0.6157(5) 0.9007(3) 1.2122(4) 0.0209(18) Uani 1 1 d . . . H46 H 0.5646 0.9227 1.2097 0.025 Uiso 1 1 calc R . . C47 C 0.7705(6) 0.8799(3) 1.2532(4) 0.0248(19) Uani 1 1 d . . . H47 H 0.8261 0.8870 1.2788 0.030 Uiso 1 1 calc R . . C48 C 0.7677(5) 0.8389(3) 1.2159(3) 0.0170(16) Uani 1 1 d . . . H48 H 0.8202 0.8178 1.2180 0.020 Uiso 1 1 calc R . . C49 C 0.6103(5) 0.8619(3) 1.1761(4) 0.0167(17) Uani 1 1 d . . . C50 C 0.6877(5) 0.8290(3) 1.1754(4) 0.0216(18) Uani 1 1 d . . . C51 C 0.6831(5) 0.7876(3) 1.1384(4) 0.0200(17) Uani 1 1 d . . . C52 C 0.6813(5) 0.7535(3) 1.1070(4) 0.0229(18) Uani 1 1 d D . . C53 C 0.6844(5) 0.7118(3) 1.0693(3) 0.0197(17) Uiso 1 1 d D . . C54 C 0.6064(6) 0.6925(3) 1.0356(4) 0.035(2) Uani 1 1 d D . . C55 C 0.7720(5) 0.6880(3) 1.0654(4) 0.0207(17) Uani 1 1 d D . . H55 H 0.8285 0.6999 1.0864 0.025 Uiso 1 1 calc R . . C56 C 0.7736(5) 0.6458(3) 1.0291(4) 0.0217(18) Uani 1 1 d . . . H56 H 0.8319 0.6290 1.0281 0.026 Uiso 1 1 calc R . . C57 C 0.6086(6) 0.6523(3) 1.0000(4) 0.029(2) Uani 1 1 d . . . H57 H 0.5525 0.6408 0.9783 0.035 Uiso 1 1 calc R . . C58 C 0.6970(5) 0.6283(3) 0.9962(4) 0.0180(17) Uani 1 1 d . . . C59 C 0.6991(5) 0.5840(3) 0.9603(4) 0.0156(16) Uani 1 1 d . A . C60 C 0.6860(6) 0.9480(3) 0.4639(4) 0.0226(19) Uani 1 1 d . . . C61 C 0.6825(6) 0.9083(3) 0.5108(4) 0.0236(19) Uani 1 1 d . . . C62 C 0.5955(6) 0.8840(3) 0.5174(5) 0.035(2) Uani 1 1 d . . . H62 H 0.5402 0.8933 0.4928 0.042 Uiso 1 1 calc R . . C63 C 0.7611(6) 0.8928(3) 0.5475(4) 0.035(2) Uani 1 1 d . . . H63 H 0.8206 0.9080 0.5436 0.042 Uiso 1 1 calc R . . C64 C 0.7556(7) 0.8571(3) 0.5884(5) 0.041(3) Uani 1 1 d . . . H64 H 0.8093 0.8486 0.6150 0.050 Uiso 1 1 calc R . . C65 C 0.5905(7) 0.8481(3) 0.5576(5) 0.047(3) Uani 1 1 d . . . C66 C 0.6666(7) 0.8316(3) 0.5913(4) 0.033(2) Uani 1 1 d . . . C67 C 0.6662(7) 0.7901(3) 0.6319(5) 0.039(2) Uani 1 1 d . . . C68 C 0.6614(6) 0.7545(3) 0.6618(5) 0.035(2) Uani 1 1 d . . . C69 C 0.6647(6) 0.7118(3) 0.6956(4) 0.033(2) Uani 1 1 d . . . C70 C 0.6020(7) 0.6735(4) 0.6796(5) 0.042(3) Uani 1 1 d . . . C71 C 0.7304(7) 0.7044(4) 0.7468(5) 0.050(3) Uani 1 1 d . . . H71 H 0.7713 0.7296 0.7604 0.060 Uiso 1 1 calc R . . C72 C 0.7371(7) 0.6611(3) 0.7784(5) 0.043(3) Uani 1 1 d . . . H72 H 0.7853 0.6565 0.8109 0.051 Uiso 1 1 calc R . . C73 C 0.6078(6) 0.6314(3) 0.7128(4) 0.030(2) Uani 1 1 d . . . H73 H 0.5653 0.6064 0.7011 0.035 Uiso 1 1 calc R . . C74 C 0.6735(5) 0.6248(3) 0.7625(4) 0.0199(18) Uani 1 1 d . . . C75 C 0.6765(5) 0.5807(3) 0.8001(4) 0.0175(17) Uani 1 1 d . A . C76 C 1.4054(7) 0.0310(4) 1.4314(5) 0.052(3) Uani 1 1 d . . . H76 H 1.4459 0.0393 1.4667 0.062 Uiso 1 1 calc R . . C77 C 1.3877(5) 0.0089(3) 1.3278(4) 0.0239(18) Uani 1 1 d . . . H77 H 1.4153 0.0019 1.2895 0.029 Uiso 1 1 calc R . . C78 C 1.2913(5) 0.0095(3) 1.3296(4) 0.0261(19) Uani 1 1 d . . . H78 H 1.2528 0.0048 1.2921 0.031 Uiso 1 1 calc R . . C79 C 1.3064(6) 0.0326(4) 1.4355(5) 0.052(3) Uani 1 1 d . . . H79 H 1.2793 0.0443 1.4719 0.063 Uiso 1 1 calc R . . C80 C 1.2490(5) 0.0167(3) 1.3845(4) 0.030(2) Uani 1 1 d D . . C81 C 1.1417(5) 0.0147(3) 1.3868(3) 0.0199(17) Uiso 1 1 d D . . C82 C 1.0902(5) -0.0175(3) 1.3528(4) 0.027(2) Uani 1 1 d D . . H82 H 1.1211 -0.0398 1.3279 0.033 Uiso 1 1 calc R . . C83 C 1.0954(5) 0.0466(3) 1.4258(4) 0.0267(19) Uani 1 1 d D . . H83 H 1.1304 0.0686 1.4516 0.032 Uiso 1 1 calc R . . C84 C 0.9960(5) 0.0445(3) 1.4250(4) 0.0226(18) Uani 1 1 d . . . H84 H 0.9640 0.0658 1.4507 0.027 Uiso 1 1 calc R . . C85 C 0.9922(5) -0.0178(3) 1.3545(4) 0.0191(17) Uani 1 1 d . . . H85 H 0.9565 -0.0406 1.3305 0.023 Uiso 1 1 calc R . . C86 C 0.0158(5) 0.6224(3) 0.3287(4) 0.0199(18) Uani 1 1 d . . . C87 C 0.0080(6) 0.5772(3) 0.3674(4) 0.0204(18) Uani 1 1 d . . . C88 C -0.0804(5) 0.5567(3) 0.3744(4) 0.027(2) Uani 1 1 d . . . H88 H -0.1364 0.5719 0.3575 0.032 Uiso 1 1 calc R . . C89 C 0.0910(6) 0.5565(3) 0.3938(4) 0.025(2) Uani 1 1 d . . . H89 H 0.1516 0.5705 0.3893 0.030 Uiso 1 1 calc R . . C90 C -0.0873(6) 0.5136(3) 0.4064(4) 0.0239(19) Uani 1 1 d . . . C91 C 0.0817(5) 0.5152(3) 0.4264(4) 0.025(2) Uani 1 1 d . . . H91 H 0.1381 0.5003 0.4433 0.031 Uiso 1 1 calc R . . C92 C -0.0029(5) 0.4941(3) 0.4363(4) 0.0250(19) Uani 1 1 d . . . C93 C -0.0084(6) 0.4511(3) 0.4723(4) 0.030(2) Uani 1 1 d . . . C94 C -0.0098(6) 0.4178(3) 0.5055(4) 0.0244(19) Uani 1 1 d . . . C95 C -0.0097(6) 0.3781(3) 0.5444(4) 0.032(2) Uani 1 1 d . . . C96 C -0.0913(6) 0.3530(3) 0.5555(4) 0.028(2) Uani 1 1 d . . . C97 C 0.0769(6) 0.3629(3) 0.5746(4) 0.034(2) Uani 1 1 d . . . H97 H 0.1335 0.3796 0.5670 0.041 Uiso 1 1 calc R . . C98 C 0.0826(6) 0.3235(3) 0.6159(4) 0.028(2) Uani 1 1 d . . . H98 H 0.1410 0.3150 0.6376 0.034 Uiso 1 1 calc R . . C99 C -0.0869(6) 0.3109(3) 0.5945(4) 0.030(2) Uani 1 1 d . . . H99 H -0.1428 0.2930 0.6000 0.036 Uiso 1 1 calc R . . C100 C -0.0011(5) 0.2973(3) 0.6235(4) 0.0183(17) Uani 1 1 d . . . C101 C 0.0007(5) 0.2561(3) 0.6687(4) 0.0171(17) Uani 1 1 d . . . C102 C -0.0067(6) 0.6218(3) 0.1703(4) 0.0193(18) Uani 1 1 d . . . C103 C -0.0016(6) 0.5780(3) 0.1315(4) 0.0208(18) Uani 1 1 d . . . C104 C -0.0836(5) 0.5565(3) 0.1070(4) 0.0200(17) Uani 1 1 d . . . H104 H -0.1440 0.5694 0.1147 0.024 Uiso 1 1 calc R . . C105 C 0.0864(6) 0.5584(3) 0.1229(4) 0.034(2) Uani 1 1 d . . . H105 H 0.1431 0.5729 0.1399 0.041 Uiso 1 1 calc R . . C106 C 0.0900(6) 0.5162(3) 0.0881(5) 0.031(2) Uani 1 1 d . . . C107 C -0.0777(5) 0.5166(3) 0.0714(4) 0.0218(18) Uani 1 1 d . . . H107 H -0.1345 0.5029 0.0530 0.026 Uiso 1 1 calc R . . C108 C 0.0064(5) 0.4960(3) 0.0616(4) 0.0223(18) Uani 1 1 d . . . C109 C 0.0128(5) 0.4530(3) 0.0225(4) 0.0220(18) Uani 1 1 d . . . C110 C 0.0136(5) 0.4206(3) -0.0103(4) 0.0216(18) Uani 1 1 d . . . C111 C 0.0083(5) 0.3792(3) -0.0498(4) 0.0210(18) Uani 1 1 d . . . C112 C -0.0788(5) 0.3675(3) -0.0823(4) 0.0221(18) Uani 1 1 d . . . H112 H -0.1334 0.3868 -0.0791 0.027 Uiso 1 1 calc R . . C113 C 0.0885(5) 0.3501(3) -0.0570(4) 0.0222(18) Uani 1 1 d . . . C114 C 0.0859(5) 0.3114(3) -0.0944(4) 0.0189(17) Uani 1 1 d . . . H114 H 0.1416 0.2931 -0.0992 0.023 Uiso 1 1 calc R . . C115 C -0.0828(5) 0.3268(3) -0.1191(4) 0.0215(18) Uani 1 1 d . . . H115 H -0.1420 0.3182 -0.1397 0.026 Uiso 1 1 calc R . . C116 C -0.0043(5) 0.2985(3) -0.1271(4) 0.0181(17) Uani 1 1 d . . . C117 C 0.2986(5) 0.7256(3) 0.2243(4) 0.0251(19) Uani 1 1 d . . . H117 H 0.2622 0.7514 0.2075 0.030 Uiso 1 1 calc R . . C118 C 0.3040(5) 0.6522(3) 0.2738(4) 0.0209(17) Uani 1 1 d . . . H118 H 0.2718 0.6271 0.2929 0.025 Uiso 1 1 calc R . . C119 C 0.3943(5) 0.7255(3) 0.2221(4) 0.0234(18) Uani 1 1 d . . . H119 H 0.4238 0.7518 0.2035 0.028 Uiso 1 1 calc R . . C120 C 0.4020(5) 0.6502(3) 0.2705(4) 0.029(2) Uani 1 1 d . . . H120 H 0.4355 0.6227 0.2849 0.034 Uiso 1 1 calc R . . C121 C 0.4526(5) 0.6883(3) 0.2463(3) 0.0161(16) Uani 1 1 d . . . C122 C 0.5558(5) 0.6882(3) 0.2434(4) 0.0200(17) Uani 1 1 d . . . C123 C 0.6089(5) 0.7253(3) 0.2696(4) 0.0246(19) Uani 1 1 d . . . H123 H 0.5781 0.7515 0.2875 0.030 Uiso 1 1 calc R . . C124 C 0.6059(5) 0.6503(3) 0.2189(4) 0.0258(19) Uani 1 1 d . . . H124 H 0.5736 0.6232 0.2021 0.031 Uiso 1 1 calc R . . C125 C 0.7018(5) 0.6536(3) 0.2202(4) 0.0220(18) Uani 1 1 d . . . H125 H 0.7358 0.6284 0.2023 0.026 Uiso 1 1 calc R . . C126 C 0.7053(5) 0.7239(3) 0.2696(4) 0.0163(16) Uani 1 1 d . . . H126 H 0.7410 0.7491 0.2887 0.020 Uiso 1 1 calc R . . C1A C 1.3830(9) 0.5269(5) 0.8326(7) 0.038(3) Uani 0.680(10) 1 d P A 1 H1A H 1.4119 0.5391 0.7971 0.045 Uiso 0.680(10) 1 calc PR A 1 C2A C 1.2887(8) 0.5261(5) 0.8309(6) 0.036(3) Uani 0.680(10) 1 d P A 1 H2A H 1.2527 0.5360 0.7943 0.044 Uiso 0.680(10) 1 calc PR A 1 C1B C 1.3899(18) 0.5532(12) 0.8679(15) 0.038(3) Uani 0.320(10) 1 d P A 2 H1B H 1.4220 0.5799 0.8526 0.045 Uiso 0.320(10) 1 calc PR A 2 C2B C 1.2932(17) 0.5565(12) 0.8769(13) 0.036(3) Uani 0.320(10) 1 d P A 2 H2B H 1.2615 0.5860 0.8799 0.044 Uiso 0.320(10) 1 calc PR A 2 N1 N 0.2551(4) 0.6887(2) 0.2504(3) 0.0135(13) Uani 1 1 d . . . N2 N 0.7510(4) 0.6892(2) 0.2444(3) 0.0162(13) Uani 1 1 d . . . N3 N 0.9395(4) 0.5149(2) 0.8828(3) 0.0184(14) Uani 1 1 d . . . N4 N 1.4409(4) 0.5119(2) 0.8807(3) 0.0205(15) Uani 1 1 d . . . N5 N 1.4440(4) 0.0180(2) 1.3781(3) 0.0194(15) Uani 1 1 d . . . N6 N 0.9444(4) 0.0142(2) 1.3902(3) 0.0166(14) Uani 1 1 d . . . O1 O 0.0939(4) 0.63560(18) 0.3132(3) 0.0236(13) Uani 1 1 d . . . O2 O -0.0628(4) 0.6420(2) 0.3129(3) 0.0260(13) Uani 1 1 d . . . O3 O 0.0802(4) 0.24501(18) 0.6944(3) 0.0219(13) Uani 1 1 d . . . O4 O -0.0772(3) 0.23669(18) 0.6766(2) 0.0181(12) Uani 1 1 d . . . O5 O 0.0704(4) 0.6427(2) 0.1845(3) 0.0242(13) Uani 1 1 d . . . O6 O -0.0871(4) 0.63524(18) 0.1854(3) 0.0229(13) Uani 1 1 d . . . O7 O 0.0703(4) 0.23572(17) -0.1773(3) 0.0211(13) Uani 1 1 d . . . O8 O -0.0857(4) 0.24546(19) -0.1943(3) 0.0220(13) Uani 1 1 d . . . O9 O 0.7690(4) 0.46543(18) 0.9507(3) 0.0213(12) Uani 1 1 d . . . O10 O 0.6089(3) 0.46760(19) 0.9498(3) 0.0225(13) Uani 1 1 d . . . O11 O 0.7716(4) 0.06441(19) 1.3228(3) 0.0233(13) Uani 1 1 d . . . O12 O 0.6136(4) 0.0698(2) 1.3167(3) 0.0291(15) Uani 1 1 d . . . O13 O 0.7710(4) 0.46256(19) 0.8210(3) 0.0230(13) Uani 1 1 d . . . O14 O 0.6125(4) 0.46221(19) 0.8174(3) 0.0223(13) Uani 1 1 d . . . O15 O 0.7800(4) 0.06588(18) 0.4532(2) 0.0199(12) Uani 1 1 d . . . O16 O 0.6227(4) 0.05993(19) 0.4485(3) 0.0237(13) Uani 1 1 d . . . O17 O 0.7728(4) 0.96173(19) 1.3242(3) 0.0221(12) Uani 1 1 d . . . O18 O 0.6147(4) 0.96969(19) 1.3053(3) 0.0230(13) Uani 1 1 d . . . O19 O 0.7810(3) 0.56698(18) 0.9523(3) 0.0191(12) Uani 1 1 d . . . O20 O 0.6209(3) 0.56841(19) 0.9366(3) 0.0221(13) Uani 1 1 d . . . O22 O 0.7663(4) 0.9648(2) 0.4570(3) 0.0233(13) Uani 1 1 d . . . O23 O 0.6101(4) 0.9608(2) 0.4371(3) 0.0257(13) Uani 1 1 d . . . O24 O 0.7551(3) 0.56604(19) 0.8237(3) 0.0210(12) Uani 1 1 d . . . O25 O 0.5963(4) 0.56181(18) 0.8066(2) 0.0197(12) Uani 1 1 d . . . Zn1 Zn 0.10907(5) 0.69002(3) 0.25478(4) 0.01161(17) Uani 1 1 d . . . Zn2 Zn -0.10358(5) 0.68975(3) 0.24534(4) 0.01049(17) Uani 1 1 d . . . Zn3 Zn 0.79563(5) 0.51537(3) 0.88692(4) 0.01131(18) Uani 1 1 d . . . Zn4 Zn 0.58353(5) 0.51406(3) 0.87850(4) 0.01087(18) Uani 1 1 d . . . Zn5 Zn 0.79904(5) 0.01343(3) 1.39022(4) 0.01174(18) Uani 1 1 d . . . Zn6 Zn 0.58784(5) 0.01537(3) 1.37646(4) 0.01126(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0232(4) 0.0359(5) 0.0652(7) 0.0270(5) 0.0061(4) -0.0043(4) Br2 0.0246(5) 0.0761(8) 0.0936(9) 0.0663(7) -0.0062(5) 0.0066(5) Br3 0.0189(5) 0.0578(7) 0.1111(10) -0.0575(7) -0.0040(5) 0.0109(5) Br4 0.0205(4) 0.0259(5) 0.0421(5) -0.0152(4) -0.0089(4) -0.0020(3) Br5 0.0306(6) 0.1128(12) 0.1542(15) 0.1007(12) 0.0022(7) 0.0140(7) Br6 0.0255(5) 0.0947(10) 0.1253(12) 0.0839(10) -0.0018(6) 0.0069(6) Br7 0.0210(4) 0.0460(6) 0.0656(7) -0.0339(5) -0.0135(4) 0.0055(4) Br8 0.0185(4) 0.0491(6) 0.0691(7) -0.0364(6) 0.0095(4) 0.0034(4) Br9 0.0301(5) 0.0444(6) 0.0707(8) -0.0377(6) -0.0276(5) 0.0162(4) Br10 0.0183(5) 0.0663(8) 0.1380(12) -0.0765(8) -0.0112(6) 0.0140(5) Br11 0.0815(12) 0.163(2) 0.220(2) 0.1036(19) -0.0269(13) -0.0468(12) Br12 0.0778(8) 0.0519(7) 0.0618(8) 0.0316(6) -0.0368(6) -0.0154(6) C3 0.028(5) 0.059(8) 0.109(10) 0.056(7) 0.002(6) 0.003(5) C4 0.023(5) 0.070(9) 0.176(15) 0.056(10) 0.024(7) 0.005(6) C5 0.009(4) 0.040(5) 0.032(5) -0.002(4) 0.002(3) 0.000(4) C6 0.013(4) 0.054(6) 0.032(5) 0.012(5) 0.011(3) 0.008(4) C7 0.033(5) 0.042(6) 0.036(6) -0.012(5) -0.001(4) -0.007(4) C8 0.020(4) 0.026(5) 0.051(6) -0.015(4) 0.012(4) -0.009(4) C9 0.027(5) 0.026(5) 0.045(6) -0.012(4) -0.003(4) 0.002(4) C10 0.027(5) 0.032(5) 0.035(5) -0.003(4) 0.005(4) -0.004(4) C11 0.009(3) 0.013(4) 0.019(4) 0.002(3) 0.004(3) 0.002(3) C12 0.020(4) 0.014(4) 0.023(5) -0.001(3) 0.006(3) 0.005(3) C13 0.023(4) 0.026(5) 0.014(4) 0.010(3) 0.010(3) -0.006(3) C14 0.025(4) 0.030(5) 0.039(6) 0.010(4) 0.006(4) 0.008(4) C15 0.018(4) 0.022(4) 0.040(5) 0.022(4) 0.002(4) 0.005(3) C16 0.024(5) 0.037(6) 0.057(7) 0.019(5) -0.001(4) 0.003(4) C17 0.036(5) 0.023(5) 0.034(5) 0.007(4) 0.014(4) -0.007(4) C18 0.017(4) 0.026(5) 0.042(6) 0.017(4) -0.003(4) -0.004(4) C19 0.034(5) 0.047(6) 0.051(7) 0.012(5) 0.008(5) -0.011(5) C20 0.056(7) 0.023(5) 0.052(7) 0.013(5) 0.010(5) 0.001(5) C21 0.032(5) 0.041(6) 0.043(6) 0.021(5) 0.013(4) -0.004(4) C22 0.039(6) 0.038(6) 0.073(8) 0.027(6) -0.015(5) -0.008(5) C23 0.044(6) 0.036(6) 0.046(6) 0.028(5) 0.006(5) 0.005(5) C24 0.019(4) 0.024(5) 0.039(5) 0.006(4) -0.005(4) -0.003(3) C25 0.020(4) 0.022(5) 0.049(6) 0.008(4) 0.011(4) -0.002(3) C26 0.022(4) 0.015(4) 0.025(5) 0.010(4) 0.005(3) 0.004(3) C27 0.014(4) 0.022(4) 0.018(4) 0.001(3) 0.008(3) -0.004(3) C28 0.027(4) 0.015(4) 0.015(4) -0.003(3) 0.000(3) 0.001(3) C29 0.019(4) 0.021(4) 0.013(4) -0.014(3) 0.004(3) 0.001(3) C30 0.023(4) 0.020(4) 0.026(5) -0.020(4) 0.007(3) -0.008(3) C31 0.024(4) 0.017(4) 0.025(5) -0.004(3) 0.007(3) 0.009(3) C32 0.015(4) 0.018(4) 0.035(5) -0.010(4) -0.007(3) 0.003(3) C33 0.014(4) 0.025(5) 0.038(5) -0.013(4) 0.000(3) -0.001(3) C34 0.020(4) 0.023(5) 0.026(5) -0.009(4) 0.001(3) 0.000(3) C35 0.021(4) 0.032(5) 0.030(5) -0.012(4) 0.006(4) 0.002(4) C36 0.023(4) 0.023(4) 0.022(5) -0.014(4) -0.005(3) -0.004(3) C37 0.012(3) 0.015(4) 0.025(4) -0.011(3) 0.006(3) 0.006(3) C38 0.024(4) 0.032(5) 0.029(5) -0.009(4) -0.001(4) 0.007(4) C39 0.022(4) 0.015(4) 0.025(4) -0.008(3) -0.005(3) 0.000(3) C40 0.014(4) 0.017(4) 0.029(5) -0.007(4) 0.000(3) 0.005(3) C41 0.018(4) 0.028(5) 0.025(5) -0.007(4) -0.001(3) 0.006(3) C42 0.011(4) 0.013(4) 0.032(5) 0.004(4) -0.002(3) 0.001(3) C43 0.011(4) 0.017(4) 0.017(4) -0.007(3) 0.001(3) 0.000(3) C44 0.024(4) 0.007(4) 0.027(5) -0.007(3) 0.002(3) -0.007(3) C45 0.013(3) 0.010(4) 0.015(4) -0.010(3) 0.001(3) 0.000(3) C46 0.009(4) 0.024(5) 0.029(5) -0.005(4) -0.002(3) 0.009(3) C47 0.025(4) 0.020(4) 0.029(5) -0.016(4) -0.002(4) 0.006(3) C48 0.018(4) 0.015(4) 0.018(4) -0.010(3) 0.000(3) -0.005(3) C49 0.015(4) 0.012(4) 0.023(4) -0.009(3) -0.002(3) -0.001(3) C50 0.022(4) 0.015(4) 0.027(5) -0.010(4) -0.002(3) 0.004(3) C51 0.021(4) 0.017(4) 0.022(4) -0.011(4) 0.004(3) 0.000(3) C52 0.022(4) 0.018(4) 0.029(5) -0.002(4) 0.002(3) -0.005(3) C54 0.037(5) 0.025(5) 0.041(6) -0.017(4) 0.002(4) 0.006(4) C55 0.013(4) 0.014(4) 0.033(5) -0.001(4) -0.014(3) -0.003(3) C56 0.017(4) 0.023(4) 0.025(5) -0.007(4) 0.003(3) 0.003(3) C57 0.027(4) 0.014(4) 0.046(6) -0.023(4) -0.002(4) 0.000(3) C58 0.018(4) 0.019(4) 0.017(4) -0.002(3) 0.001(3) 0.000(3) C59 0.023(4) 0.009(4) 0.015(4) -0.002(3) 0.008(3) 0.002(3) C60 0.026(4) 0.022(5) 0.020(5) 0.003(4) 0.003(4) 0.003(4) C61 0.028(4) 0.022(5) 0.021(5) 0.010(4) 0.005(4) -0.005(3) C62 0.023(4) 0.039(6) 0.045(6) 0.006(5) 0.008(4) -0.004(4) C63 0.025(5) 0.034(5) 0.046(6) 0.003(5) 0.002(4) -0.009(4) C64 0.052(6) 0.024(5) 0.045(6) 0.024(5) -0.017(5) 0.008(4) C65 0.044(6) 0.033(6) 0.069(8) 0.022(5) 0.031(5) 0.006(5) C66 0.057(6) 0.019(5) 0.025(5) 0.004(4) 0.013(4) 0.001(4) C67 0.048(6) 0.027(5) 0.043(6) 0.007(5) 0.003(5) -0.005(4) C68 0.030(5) 0.031(5) 0.045(6) 0.007(5) 0.003(4) -0.003(4) C69 0.032(5) 0.031(5) 0.036(5) 0.018(4) -0.004(4) 0.000(4) C70 0.045(6) 0.041(6) 0.038(6) 0.018(5) -0.008(5) -0.001(5) C71 0.060(7) 0.034(5) 0.053(7) 0.009(5) -0.025(5) -0.017(5) C72 0.046(6) 0.018(5) 0.062(7) 0.020(5) -0.014(5) -0.005(4) C73 0.031(5) 0.019(5) 0.040(6) 0.013(4) 0.010(4) -0.003(4) C74 0.009(3) 0.020(4) 0.031(5) -0.005(4) 0.001(3) -0.001(3) C75 0.013(4) 0.023(4) 0.017(4) 0.005(3) 0.008(3) 0.002(3) C76 0.037(6) 0.083(9) 0.034(6) -0.006(6) -0.001(5) 0.000(6) C77 0.019(4) 0.034(5) 0.018(4) 0.000(4) -0.001(3) 0.000(4) C78 0.016(4) 0.038(5) 0.024(5) -0.005(4) -0.001(3) 0.000(4) C79 0.020(5) 0.084(8) 0.054(7) -0.013(6) 0.007(5) 0.008(5) C80 0.016(4) 0.035(5) 0.038(6) -0.005(4) -0.007(4) -0.014(4) C82 0.018(4) 0.030(5) 0.035(5) -0.017(4) 0.009(3) 0.005(3) C83 0.023(4) 0.027(5) 0.030(5) -0.012(4) 0.001(3) -0.004(4) C84 0.018(4) 0.029(5) 0.021(4) -0.011(4) 0.002(3) -0.015(3) C85 0.015(4) 0.016(4) 0.025(4) -0.007(3) -0.004(3) -0.002(3) C86 0.014(4) 0.016(4) 0.028(5) 0.003(4) -0.003(3) 0.002(3) C87 0.026(4) 0.008(4) 0.025(5) 0.004(3) -0.010(3) -0.003(3) C88 0.012(4) 0.035(5) 0.033(5) 0.007(4) -0.002(3) 0.000(3) C89 0.021(4) 0.015(4) 0.038(5) 0.002(4) -0.014(4) 0.001(3) C90 0.026(4) 0.021(4) 0.025(5) 0.004(4) 0.008(3) 0.001(4) C91 0.018(4) 0.036(5) 0.021(5) 0.008(4) -0.006(3) 0.002(4) C92 0.021(4) 0.019(4) 0.035(5) 0.013(4) -0.004(4) -0.002(3) C93 0.026(5) 0.028(5) 0.035(6) 0.012(4) 0.007(4) -0.005(4) C94 0.027(4) 0.018(4) 0.027(5) 0.006(4) -0.005(4) 0.001(3) C95 0.037(5) 0.024(5) 0.036(6) 0.013(4) 0.002(4) 0.000(4) C96 0.029(4) 0.019(4) 0.035(5) 0.014(4) -0.009(4) 0.002(4) C97 0.024(4) 0.033(5) 0.044(6) 0.007(5) -0.011(4) -0.011(4) C98 0.019(4) 0.023(5) 0.042(6) 0.008(4) 0.002(4) -0.002(3) C99 0.022(4) 0.034(5) 0.035(5) 0.015(4) 0.004(4) -0.009(4) C100 0.020(4) 0.006(4) 0.029(5) 0.008(3) -0.003(3) 0.003(3) C101 0.017(4) 0.016(4) 0.018(4) 0.011(3) -0.001(3) -0.009(3) C102 0.028(5) 0.017(4) 0.013(4) 0.002(3) -0.004(3) -0.003(3) C103 0.023(4) 0.015(4) 0.024(5) -0.008(3) 0.002(3) 0.008(3) C104 0.019(4) 0.009(4) 0.031(5) -0.007(3) -0.003(3) 0.003(3) C105 0.021(4) 0.028(5) 0.052(6) -0.032(4) -0.004(4) 0.004(4) C106 0.017(4) 0.027(5) 0.049(6) -0.019(4) 0.005(4) 0.006(4) C107 0.015(4) 0.021(5) 0.029(5) -0.004(4) -0.001(3) 0.003(3) C108 0.018(4) 0.013(4) 0.036(5) -0.004(4) 0.001(3) -0.003(3) C109 0.010(4) 0.016(4) 0.040(5) -0.008(4) 0.005(3) -0.001(3) C110 0.015(4) 0.024(5) 0.027(5) -0.003(4) 0.000(3) 0.006(3) C111 0.021(4) 0.014(4) 0.028(5) -0.007(3) 0.002(3) -0.004(3) C112 0.023(4) 0.017(4) 0.027(5) -0.010(4) 0.001(3) 0.006(3) C113 0.023(4) 0.022(4) 0.021(4) -0.003(4) 0.000(3) 0.000(3) C114 0.013(4) 0.019(4) 0.024(5) -0.001(3) 0.005(3) 0.004(3) C115 0.010(3) 0.032(5) 0.022(4) -0.014(4) -0.001(3) -0.007(3) C116 0.023(4) 0.013(4) 0.018(4) 0.000(3) 0.000(3) 0.000(3) C117 0.011(4) 0.027(5) 0.037(5) 0.002(4) -0.001(3) 0.002(3) C118 0.028(4) 0.011(4) 0.024(4) 0.005(3) 0.006(3) -0.001(3) C119 0.020(4) 0.024(4) 0.026(5) 0.009(4) 0.005(3) -0.002(3) C120 0.008(4) 0.029(5) 0.049(6) 0.015(4) 0.003(3) -0.002(3) C121 0.010(3) 0.011(4) 0.027(4) -0.008(3) 0.004(3) -0.002(3) C122 0.004(3) 0.014(4) 0.042(5) -0.005(4) 0.006(3) 0.001(3) C123 0.007(3) 0.021(4) 0.045(5) -0.004(4) -0.004(3) -0.005(3) C124 0.023(4) 0.018(4) 0.037(5) -0.010(4) 0.011(4) -0.007(3) C125 0.008(3) 0.021(4) 0.037(5) -0.004(4) 0.002(3) 0.006(3) C126 0.007(3) 0.013(4) 0.030(4) 0.000(3) 0.008(3) 0.001(3) C1A 0.017(5) 0.054(10) 0.042(9) 0.005(6) 0.001(6) 0.002(6) C2A 0.012(5) 0.064(10) 0.031(7) 0.014(6) -0.011(5) 0.008(6) C1B 0.017(5) 0.054(10) 0.042(9) 0.005(6) 0.001(6) 0.002(6) C2B 0.012(5) 0.064(10) 0.031(7) 0.014(6) -0.011(5) 0.008(6) N1 0.004(3) 0.016(3) 0.020(3) 0.001(3) -0.003(2) 0.004(2) N2 0.010(3) 0.017(3) 0.022(3) 0.008(3) 0.002(2) 0.007(3) N3 0.002(3) 0.021(4) 0.031(4) 0.000(3) -0.004(2) 0.000(3) N4 0.015(3) 0.026(4) 0.020(4) 0.009(3) -0.002(3) 0.000(3) N5 0.006(3) 0.028(4) 0.024(4) -0.002(3) 0.002(3) -0.001(3) N6 0.014(3) 0.017(3) 0.019(4) -0.005(3) 0.000(2) -0.008(3) O1 0.018(3) 0.015(3) 0.037(4) 0.001(3) -0.001(2) 0.000(2) O2 0.019(3) 0.026(3) 0.033(3) 0.011(3) 0.002(2) 0.002(2) O3 0.017(3) 0.016(3) 0.032(3) 0.013(2) -0.002(2) 0.005(2) O4 0.017(3) 0.017(3) 0.020(3) 0.011(2) 0.003(2) -0.004(2) O5 0.019(3) 0.028(3) 0.025(3) -0.015(3) -0.005(2) 0.008(2) O6 0.026(3) 0.012(3) 0.032(3) -0.010(2) 0.009(3) 0.000(2) O7 0.019(3) 0.010(3) 0.033(3) -0.003(2) -0.006(2) 0.005(2) O8 0.020(3) 0.023(3) 0.023(3) -0.012(2) -0.008(2) 0.009(2) O9 0.018(3) 0.012(3) 0.034(3) 0.002(2) 0.003(2) -0.004(2) O10 0.011(2) 0.022(3) 0.035(3) 0.012(3) 0.000(2) 0.002(2) O11 0.021(3) 0.016(3) 0.033(3) 0.009(2) 0.000(2) 0.011(2) O12 0.022(3) 0.020(3) 0.048(4) 0.014(3) 0.020(3) 0.002(2) O13 0.024(3) 0.019(3) 0.025(3) -0.012(2) -0.003(2) 0.004(2) O14 0.016(3) 0.018(3) 0.033(3) -0.013(3) 0.003(2) 0.001(2) O15 0.019(3) 0.020(3) 0.021(3) -0.013(2) 0.006(2) 0.004(2) O16 0.013(3) 0.024(3) 0.034(3) -0.011(3) -0.003(2) 0.001(2) O17 0.017(3) 0.022(3) 0.028(3) -0.009(3) 0.005(2) 0.000(2) O18 0.020(3) 0.020(3) 0.029(3) -0.011(3) -0.001(2) 0.001(2) O19 0.015(3) 0.015(3) 0.027(3) -0.006(2) -0.001(2) 0.004(2) O20 0.012(3) 0.023(3) 0.032(3) -0.016(3) 0.001(2) -0.001(2) O22 0.018(3) 0.026(3) 0.026(3) 0.009(3) 0.004(2) -0.008(2) O23 0.022(3) 0.023(3) 0.033(4) 0.011(3) 0.007(3) -0.006(2) O24 0.015(3) 0.020(3) 0.028(3) 0.007(2) 0.002(2) 0.002(2) O25 0.019(3) 0.019(3) 0.021(3) 0.014(2) 0.003(2) 0.000(2) Zn1 0.0067(4) 0.0100(4) 0.0183(4) 0.0002(4) 0.0021(3) -0.0001(3) Zn2 0.0053(3) 0.0080(4) 0.0182(4) 0.0001(4) 0.0005(3) -0.0003(3) Zn3 0.0064(4) 0.0084(4) 0.0190(5) -0.0007(4) 0.0004(3) -0.0001(3) Zn4 0.0065(4) 0.0099(4) 0.0161(5) -0.0022(3) 0.0004(3) -0.0003(3) Zn5 0.0073(4) 0.0099(4) 0.0182(5) -0.0025(4) 0.0018(3) -0.0006(3) Zn6 0.0054(4) 0.0106(4) 0.0179(5) -0.0016(3) 0.0015(3) -0.0006(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 Br1 C90 1.862(8) . ? Br2 C96 1.851(8) . ? Br3 C106 1.895(8) . ? Br4 C113 1.891(8) . ? Br5 C16 1.934(9) . ? Br6 C23 1.859(9) . ? Br7 C33 1.903(8) . ? Br8 C38 1.884(8) . ? Br9 C49 1.898(7) . ? Br10 C54 1.916(9) . ? Br11 C65 2.031(11) . ? Br12 C70 1.875(9) . ? C3 N4 1.271(11) . ? C3 C4 1.369(13) . ? C3 H3 0.9500 . ? C4 C5 1.339(14) . ? C4 H4 0.9500 . ? C5 C2A 1.358(15) . ? C5 C2B 1.47(3) . ? C5 C6 1.512(10) . ? C6 C8 1.289(12) . ? C6 C7 1.457(13) . ? C7 C10 1.373(12) . ? C7 H7 0.9500 . ? C8 C9 1.414(11) . ? C8 H8 0.9500 . ? C9 N3 1.340(10) . ? C9 H9 0.9500 . ? C10 N3 1.366(10) . ? C10 H10 0.9500 . ? C11 O7 1.254(8) . ? C11 O8 1.275(8) . ? C11 C116 1.459(10) . ? C12 O10 1.256(9) . ? C12 O9 1.289(9) . ? C12 C13 1.527(11) . ? C13 C15 1.353(11) . ? C13 C14 1.396(11) . ? C14 C17 1.381(12) . ? C14 H14 0.9500 . ? C15 C16 1.342(12) . ? C15 H15 0.9500 . ? C16 C18 1.385(12) . ? C17 C18 1.407(11) . ? C17 H17 0.9500 . ? C18 C19 1.487(13) . ? C19 C20 1.197(13) . ? C20 C21 1.424(13) . ? C21 C22 1.380(13) . ? C21 C23 1.412(13) . ? C22 C24 1.379(12) . ? C22 H22 0.9500 . ? C23 C25 1.388(12) . ? C24 C26 1.386(11) . ? C24 H24 0.9500 . ? C25 C26 1.422(11) . ? C25 H25 0.9500 . ? C26 C27 1.456(11) . ? C27 O12 1.260(9) . ? C27 O11 1.270(9) . ? C28 O14 1.239(9) . ? C28 O13 1.250(9) . ? C28 C29 1.522(10) . ? C29 C30 1.359(10) . ? C29 C31 1.385(10) . ? C30 C33 1.395(11) . ? C30 H30 0.9500 . ? C31 C32 1.351(11) . ? C31 H31 0.9500 . ? C32 C34 1.415(10) . ? C32 H32 0.9500 . ? C33 C34 1.372(11) . ? C34 C35 1.456(12) . ? C35 C36 1.181(11) . ? C36 C37 1.429(11) . ? C37 C39 1.423(10) . ? C37 C38 1.434(11) . ? C38 C41 1.336(11) . ? C39 C40 1.392(10) . ? C39 H39 0.9500 . ? C40 C42 1.438(10) . ? C40 H40 0.9500 . ? C41 C42 1.409(10) . ? C41 H41 0.9500 . ? C42 C43 1.506(11) . ? C43 O16 1.224(8) . ? C43 O15 1.262(8) . ? C44 O17 1.244(9) . ? C44 O18 1.272(9) . ? C44 C45 1.504(10) . ? C45 C47 1.373(10) . ? C45 C46 1.378(10) . ? C46 C49 1.343(10) . ? C46 H46 0.9500 . ? C47 C48 1.406(10) . ? C47 H47 0.9500 . ? C48 C50 1.407(10) . ? C48 H48 0.9500 . ? C49 C50 1.434(10) . ? C50 C51 1.411(11) . ? C51 C52 1.177(11) . ? C52 C53 1.429(11) . ? C53 C54 1.389(11) . ? C53 C55 1.412(10) . ? C54 C57 1.369(11) . ? C55 C56 1.426(10) . ? C55 H55 0.9500 . ? C56 C58 1.345(10) . ? C56 H56 0.9500 . ? C57 C58 1.425(11) . ? C57 H57 0.9500 . ? C58 C59 1.471(10) . ? C59 O20 1.262(9) . ? C59 O19 1.272(9) . ? C60 O23 1.236(9) . ? C60 O22 1.246(9) . ? C60 C61 1.509(11) . ? C61 C63 1.388(12) . ? C61 C62 1.419(11) . ? C62 C65 1.336(13) . ? C62 H62 0.9500 . ? C63 C64 1.343(12) . ? C63 H63 0.9500 . ? C64 C66 1.450(13) . ? C64 H64 0.9500 . ? C65 C66 1.338(13) . ? C66 C67 1.462(12) . ? C67 C68 1.197(12) . ? C68 C69 1.407(12) . ? C69 C71 1.407(12) . ? C69 C70 1.426(13) . ? C70 C73 1.384(12) . ? C71 C72 1.399(13) . ? C71 H71 0.9500 . ? C72 C74 1.390(11) . ? C72 H72 0.9500 . ? C73 C74 1.381(12) . ? C73 H73 0.9500 . ? C74 C75 1.484(11) . ? C75 O24 1.258(9) . ? C75 O25 1.264(9) . ? C76 N5 1.346(12) . ? C76 C79 1.403(13) . ? C76 H76 0.9500 . ? C77 N5 1.325(9) . ? C77 C78 1.361(10) . ? C77 H77 0.9500 . ? C78 C80 1.368(12) . ? C78 H78 0.9500 . ? C79 C80 1.394(13) . ? C79 H79 0.9500 . ? C80 C81 1.515(10) . ? C81 C82 1.348(11) . ? C81 C83 1.417(11) . ? C82 C85 1.383(10) . ? C82 H82 0.9500 . ? C83 C84 1.400(10) . ? C83 H83 0.9500 . ? C84 N6 1.322(9) . ? C84 H84 0.9500 . ? C85 N6 1.385(9) . ? C85 H85 0.9500 . ? C86 O1 1.227(9) . ? C86 O2 1.265(9) . ? C86 C87 1.530(11) . ? C87 C88 1.391(10) . ? C87 C89 1.395(10) . ? C88 C90 1.402(11) . ? C88 H88 0.9500 . ? C89 C91 1.372(11) . ? C89 H89 0.9500 . ? C90 C92 1.426(11) . ? C91 C92 1.361(11) . ? C91 H91 0.9500 . ? C92 C93 1.445(11) . ? C93 C94 1.181(11) . ? C94 C95 1.397(11) . ? C95 C96 1.384(12) . ? C95 C97 1.412(12) . ? C96 C99 1.451(11) . ? C97 C98 1.422(12) . ? C97 H97 0.9500 . ? C98 C100 1.409(10) . ? C98 H98 0.9500 . ? C99 C100 1.380(10) . ? C99 H99 0.9500 . ? C100 C101 1.514(10) . ? C101 O4 1.247(8) . ? C101 O3 1.257(8) . ? C102 O6 1.256(9) . ? C102 O5 1.257(9) . ? C102 C103 1.494(11) . ? C103 C104 1.381(10) . ? C103 C105 1.381(10) . ? C104 C107 1.368(10) . ? C104 H104 0.9500 . ? C105 C106 1.410(11) . ? C105 H105 0.9500 . ? C106 C108 1.396(11) . ? C107 C108 1.347(10) . ? C107 H107 0.9500 . ? C108 C109 1.482(11) . ? C109 C110 1.156(11) . ? C110 C111 1.444(11) . ? C111 C113 1.411(11) . ? C111 C112 1.412(10) . ? C112 C115 1.393(10) . ? C112 H112 0.9500 . ? C113 C114 1.356(11) . ? C114 C116 1.458(10) . ? C114 H114 0.9500 . ? C115 C116 1.384(10) . ? C115 H115 0.9500 . ? C117 N1 1.347(10) . ? C117 C119 1.352(10) . ? C117 H117 0.9500 . ? C118 N1 1.322(9) . ? C118 C120 1.387(10) . ? C118 H118 0.9500 . ? C119 C121 1.412(10) . ? C119 H119 0.9500 . ? C120 C121 1.408(10) . ? C120 H120 0.9500 . ? C121 C122 1.458(9) . ? C122 C123 1.388(10) . ? C122 C124 1.403(10) . ? C123 C126 1.358(9) . ? C123 H123 0.9500 . ? C124 C125 1.352(10) . ? C124 H124 0.9500 . ? C125 N2 1.312(10) . ? C125 H125 0.9500 . ? C126 N2 1.306(9) . ? C126 H126 0.9500 . ? C1A C2A 1.328(16) . ? C1A N4 1.343(15) . ? C1A H1A 0.9500 . ? C2A H2A 0.9500 . ? C1B N4 1.39(3) . ? C1B C2B 1.39(3) . ? C1B H1B 0.9500 . ? C2B H2B 0.9500 . ? N1 Zn1 2.065(5) . ? N2 Zn2 2.047(5) 1_655 ? N3 Zn3 2.034(5) . ? N4 Zn4 2.013(6) 1_655 ? N5 Zn6 2.030(6) 1_655 ? N6 Zn5 2.048(6) . ? O1 Zn1 2.004(6) . ? O2 Zn2 2.036(5) . ? O3 Zn2 2.040(5) 2_546 ? O4 Zn1 2.047(5) 2_546 ? O5 Zn1 2.062(5) . ? O6 Zn2 2.029(5) . ? O7 Zn2 2.031(5) 2_545 ? O8 Zn1 2.047(5) 2_545 ? O9 Zn3 2.016(5) . ? O10 Zn4 2.031(5) . ? O11 Zn5 2.060(5) . ? O12 Zn6 2.048(5) . ? O13 Zn3 2.070(5) . ? O14 Zn4 2.025(5) . ? O15 Zn5 2.035(5) 1_554 ? O16 Zn6 2.030(5) 1_554 ? O17 Zn5 2.052(5) 1_565 ? O18 Zn6 2.051(5) 1_565 ? O19 Zn3 2.043(5) . ? O20 Zn4 2.026(5) . ? O22 Zn5 2.057(5) 1_564 ? O23 Zn6 2.028(5) 1_564 ? O24 Zn3 2.030(5) . ? O25 Zn4 2.065(5) . ? Zn1 O4 2.047(5) 2_556 ? Zn1 O8 2.047(5) 2 ? Zn1 Zn2 2.9891(11) . ? Zn2 O7 2.031(5) 2 ? Zn2 O3 2.040(5) 2_556 ? Zn2 N2 2.047(6) 1_455 ? Zn3 Zn4 2.9814(10) . ? Zn4 N4 2.013(6) 1_455 ? Zn5 O15 2.035(5) 1_556 ? Zn5 O17 2.052(5) 1_545 ? Zn5 O22 2.057(5) 1_546 ? Zn5 Zn6 2.9711(11) . ? Zn6 O23 2.028(5) 1_546 ? Zn6 N5 2.030(6) 1_455 ? Zn6 O16 2.030(5) 1_556 ? Zn6 O18 2.051(5) 1_545 ? 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 N4 C3 C4 128.8(10) . . ? N4 C3 H3 115.6 . . ? C4 C3 H3 115.6 . . ? C5 C4 C3 117.0(11) . . ? C5 C4 H4 121.5 . . ? C3 C4 H4 121.5 . . ? C4 C5 C2A 112.1(9) . . ? C4 C5 C2B 110.0(12) . . ? C2A C5 C2B 54.9(13) . . ? C4 C5 C6 121.4(8) . . ? C2A C5 C6 121.0(8) . . ? C2B C5 C6 119.6(12) . . ? C8 C6 C7 120.7(7) . . ? C8 C6 C5 122.7(8) . . ? C7 C6 C5 116.5(8) . . ? C10 C7 C6 117.9(8) . . ? C10 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C6 C8 C9 118.2(8) . . ? C6 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? N3 C9 C8 124.2(8) . . ? N3 C9 H9 117.9 . . ? C8 C9 H9 117.9 . . ? N3 C10 C7 121.6(8) . . ? N3 C10 H10 119.2 . . ? C7 C10 H10 119.2 . . ? O7 C11 O8 122.9(7) . . ? O7 C11 C116 120.3(6) . . ? O8 C11 C116 116.8(6) . . ? O10 C12 O9 124.6(7) . . ? O10 C12 C13 119.2(7) . . ? O9 C12 C13 116.2(6) . . ? C15 C13 C14 123.0(7) . . ? C15 C13 C12 119.7(7) . . ? C14 C13 C12 117.4(7) . . ? C17 C14 C13 117.0(8) . . ? C17 C14 H14 121.5 . . ? C13 C14 H14 121.5 . . ? C16 C15 C13 119.6(8) . . ? C16 C15 H15 120.2 . . ? C13 C15 H15 120.2 . . ? C15 C16 C18 120.5(8) . . ? C15 C16 Br5 119.2(7) . . ? C18 C16 Br5 120.3(7) . . ? C14 C17 C18 119.6(8) . . ? C14 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C16 C18 C17 119.8(8) . . ? C16 C18 C19 122.1(8) . . ? C17 C18 C19 118.1(7) . . ? C20 C19 C18 173.3(12) . . ? C19 C20 C21 175.4(12) . . ? C22 C21 C23 117.8(9) . . ? C22 C21 C20 123.2(9) . . ? C23 C21 C20 118.9(9) . . ? C24 C22 C21 122.6(9) . . ? C24 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? C25 C23 C21 120.8(9) . . ? C25 C23 Br6 118.9(7) . . ? C21 C23 Br6 120.0(7) . . ? C22 C24 C26 119.8(8) . . ? C22 C24 H24 120.1 . . ? C26 C24 H24 120.1 . . ? C23 C25 C26 119.5(8) . . ? C23 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C24 C26 C25 119.3(7) . . ? C24 C26 C27 120.9(7) . . ? C25 C26 C27 119.8(7) . . ? O12 C27 O11 123.2(7) . . ? O12 C27 C26 116.6(7) . . ? O11 C27 C26 120.1(7) . . ? O14 C28 O13 127.0(7) . . ? O14 C28 C29 116.4(7) . . ? O13 C28 C29 116.5(7) . . ? C30 C29 C31 119.0(7) . . ? C30 C29 C28 120.0(7) . . ? C31 C29 C28 121.1(7) . . ? C29 C30 C33 120.2(7) . . ? C29 C30 H30 119.9 . . ? C33 C30 H30 119.9 . . ? C32 C31 C29 122.2(8) . . ? C32 C31 H31 118.9 . . ? C29 C31 H31 118.9 . . ? C31 C32 C34 119.3(7) . . ? C31 C32 H32 120.4 . . ? C34 C32 H32 120.4 . . ? C34 C33 C30 120.8(7) . . ? C34 C33 Br7 120.5(6) . . ? C30 C33 Br7 118.7(6) . . ? C33 C34 C32 118.5(7) . . ? C33 C34 C35 121.7(7) . . ? C32 C34 C35 119.7(7) . . ? C36 C35 C34 176.3(10) . . ? C35 C36 C37 179.1(9) . . ? C39 C37 C36 118.3(7) . . ? C39 C37 C38 118.6(7) . . ? C36 C37 C38 123.1(7) . . ? C41 C38 C37 121.8(7) . . ? C41 C38 Br8 120.5(6) . . ? C37 C38 Br8 117.7(6) . . ? C40 C39 C37 119.4(7) . . ? C40 C39 H39 120.3 . . ? C37 C39 H39 120.3 . . ? C39 C40 C42 120.1(7) . . ? C39 C40 H40 119.9 . . ? C42 C40 H40 119.9 . . ? C38 C41 C42 120.8(8) . . ? C38 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C41 C42 C40 119.2(7) . . ? C41 C42 C43 120.0(7) . . ? C40 C42 C43 120.8(6) . . ? O16 C43 O15 126.2(7) . . ? O16 C43 C42 118.1(6) . . ? O15 C43 C42 115.6(6) . . ? O17 C44 O18 126.7(7) . . ? O17 C44 C45 117.8(7) . . ? O18 C44 C45 115.5(6) . . ? C47 C45 C46 119.3(7) . . ? C47 C45 C44 119.0(7) . . ? C46 C45 C44 121.7(7) . . ? C49 C46 C45 121.9(7) . . ? C49 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C45 C47 C48 120.4(7) . . ? C45 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C50 C48 C47 120.6(7) . . ? C50 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C46 C49 C50 121.3(7) . . ? C46 C49 Br9 120.3(6) . . ? C50 C49 Br9 118.3(6) . . ? C48 C50 C51 121.3(7) . . ? C48 C50 C49 116.4(7) . . ? C51 C50 C49 122.3(7) . . ? C52 C51 C50 178.4(9) . . ? C51 C52 C53 177.0(9) . . ? C54 C53 C55 116.6(7) . . ? C54 C53 C52 124.5(7) . . ? C55 C53 C52 118.9(7) . . ? C57 C54 C53 124.8(8) . . ? C57 C54 Br10 117.5(7) . . ? C53 C54 Br10 117.6(6) . . ? C53 C55 C56 118.3(7) . . ? C53 C55 H55 120.8 . . ? C56 C55 H55 120.8 . . ? C58 C56 C55 123.7(7) . . ? C58 C56 H56 118.2 . . ? C55 C56 H56 118.2 . . ? C54 C57 C58 118.5(8) . . ? C54 C57 H57 120.7 . . ? C58 C57 H57 120.7 . . ? C56 C58 C57 118.0(7) . . ? C56 C58 C59 123.1(7) . . ? C57 C58 C59 118.8(7) . . ? O20 C59 O19 126.1(7) . . ? O20 C59 C58 117.6(6) . . ? O19 C59 C58 116.1(7) . . ? O23 C60 O22 126.7(8) . . ? O23 C60 C61 117.8(7) . . ? O22 C60 C61 115.5(7) . . ? C63 C61 C62 117.0(8) . . ? C63 C61 C60 123.6(7) . . ? C62 C61 C60 119.3(8) . . ? C65 C62 C61 120.8(9) . . ? C65 C62 H62 119.6 . . ? C61 C62 H62 119.6 . . ? C64 C63 C61 122.0(8) . . ? C64 C63 H63 119.0 . . ? C61 C63 H63 119.0 . . ? C63 C64 C66 119.1(8) . . ? C63 C64 H64 120.5 . . ? C66 C64 H64 120.5 . . ? C62 C65 C66 122.7(9) . . ? C62 C65 Br11 113.8(8) . . ? C66 C65 Br11 121.9(7) . . ? C65 C66 C64 118.0(8) . . ? C65 C66 C67 124.7(9) . . ? C64 C66 C67 117.3(8) . . ? C68 C67 C66 175.1(11) . . ? C67 C68 C69 174.6(10) . . ? C68 C69 C71 121.9(9) . . ? C68 C69 C70 121.9(8) . . ? C71 C69 C70 116.3(8) . . ? C73 C70 C69 120.8(8) . . ? C73 C70 Br12 119.6(8) . . ? C69 C70 Br12 119.6(7) . . ? C72 C71 C69 121.9(9) . . ? C72 C71 H71 119.0 . . ? C69 C71 H71 119.0 . . ? C74 C72 C71 120.2(9) . . ? C74 C72 H72 119.9 . . ? C71 C72 H72 119.9 . . ? C74 C73 C70 121.9(9) . . ? C74 C73 H73 119.0 . . ? C70 C73 H73 119.0 . . ? C73 C74 C72 118.7(8) . . ? C73 C74 C75 121.9(7) . . ? C72 C74 C75 119.4(7) . . ? O24 C75 O25 126.0(7) . . ? O24 C75 C74 119.2(7) . . ? O25 C75 C74 114.8(7) . . ? N5 C76 C79 121.2(9) . . ? N5 C76 H76 119.4 . . ? C79 C76 H76 119.4 . . ? N5 C77 C78 121.5(8) . . ? N5 C77 H77 119.3 . . ? C78 C77 H77 119.3 . . ? C77 C78 C80 121.0(8) . . ? C77 C78 H78 119.5 . . ? C80 C78 H78 119.5 . . ? C80 C79 C76 118.0(9) . . ? C80 C79 H79 121.0 . . ? C76 C79 H79 121.0 . . ? C78 C80 C79 117.5(8) . . ? C78 C80 C81 120.7(7) . . ? C79 C80 C81 121.1(8) . . ? C82 C81 C83 119.7(7) . . ? C82 C81 C80 120.7(7) . . ? C83 C81 C80 119.5(7) . . ? C81 C82 C85 119.6(7) . . ? C81 C82 H82 120.2 . . ? C85 C82 H82 120.2 . . ? C84 C83 C81 117.5(7) . . ? C84 C83 H83 121.3 . . ? C81 C83 H83 121.3 . . ? N6 C84 C83 123.3(7) . . ? N6 C84 H84 118.3 . . ? C83 C84 H84 118.3 . . ? C82 C85 N6 122.0(7) . . ? C82 C85 H85 119.0 . . ? N6 C85 H85 119.0 . . ? O1 C86 O2 125.4(7) . . ? O1 C86 C87 119.7(7) . . ? O2 C86 C87 114.9(7) . . ? C88 C87 C89 121.0(7) . . ? C88 C87 C86 120.1(7) . . ? C89 C87 C86 118.9(7) . . ? C87 C88 C90 120.3(7) . . ? C87 C88 H88 119.8 . . ? C90 C88 H88 119.8 . . ? C91 C89 C87 117.4(8) . . ? C91 C89 H89 121.3 . . ? C87 C89 H89 121.3 . . ? C88 C90 C92 118.3(7) . . ? C88 C90 Br1 119.8(6) . . ? C92 C90 Br1 121.8(6) . . ? C92 C91 C89 124.3(8) . . ? C92 C91 H91 117.8 . . ? C89 C91 H91 117.8 . . ? C91 C92 C90 118.3(7) . . ? C91 C92 C93 121.8(7) . . ? C90 C92 C93 119.7(7) . . ? C94 C93 C92 174.9(10) . . ? C93 C94 C95 178.8(10) . . ? C96 C95 C94 123.0(8) . . ? C96 C95 C97 117.8(8) . . ? C94 C95 C97 119.2(8) . . ? C95 C96 C99 120.9(7) . . ? C95 C96 Br2 121.3(6) . . ? C99 C96 Br2 117.8(6) . . ? C95 C97 C98 122.6(8) . . ? C95 C97 H97 118.7 . . ? C98 C97 H97 118.7 . . ? C100 C98 C97 117.9(7) . . ? C100 C98 H98 121.1 . . ? C97 C98 H98 121.1 . . ? C100 C99 C96 119.5(7) . . ? C100 C99 H99 120.2 . . ? C96 C99 H99 120.2 . . ? C99 C100 C98 121.1(7) . . ? C99 C100 C101 118.9(7) . . ? C98 C100 C101 119.8(7) . . ? O4 C101 O3 126.7(7) . . ? O4 C101 C100 116.4(6) . . ? O3 C101 C100 116.9(6) . . ? O6 C102 O5 124.9(7) . . ? O6 C102 C103 118.0(7) . . ? O5 C102 C103 117.0(7) . . ? C104 C103 C105 120.6(7) . . ? C104 C103 C102 120.5(7) . . ? C105 C103 C102 118.8(7) . . ? C107 C104 C103 119.8(7) . . ? C107 C104 H104 120.1 . . ? C103 C104 H104 120.1 . . ? C103 C105 C106 118.2(7) . . ? C103 C105 H105 120.9 . . ? C106 C105 H105 120.9 . . ? C108 C106 C105 120.3(7) . . ? C108 C106 Br3 121.3(6) . . ? C105 C106 Br3 118.5(6) . . ? C108 C107 C104 121.8(7) . . ? C108 C107 H107 119.1 . . ? C104 C107 H107 119.1 . . ? C107 C108 C106 119.2(7) . . ? C107 C108 C109 121.7(7) . . ? C106 C108 C109 119.0(7) . . ? C110 C109 C108 176.1(9) . . ? C109 C110 C111 176.1(9) . . ? C113 C111 C112 119.1(7) . . ? C113 C111 C110 121.5(7) . . ? C112 C111 C110 119.4(7) . . ? C115 C112 C111 118.4(7) . . ? C115 C112 H112 120.8 . . ? C111 C112 H112 120.8 . . ? C114 C113 C111 122.7(7) . . ? C114 C113 Br4 118.7(6) . . ? C111 C113 Br4 118.5(6) . . ? C113 C114 C116 118.5(7) . . ? C113 C114 H114 120.8 . . ? C116 C114 H114 120.8 . . ? C116 C115 C112 122.8(7) . . ? C116 C115 H115 118.6 . . ? C112 C115 H115 118.6 . . ? C115 C116 C114 118.3(7) . . ? C115 C116 C11 123.8(7) . . ? C114 C116 C11 117.8(7) . . ? N1 C117 C119 119.6(7) . . ? N1 C117 H117 120.2 . . ? C119 C117 H117 120.2 . . ? N1 C118 C120 120.6(7) . . ? N1 C118 H118 119.7 . . ? C120 C118 H118 119.7 . . ? C117 C119 C121 123.1(7) . . ? C117 C119 H119 118.5 . . ? C121 C119 H119 118.5 . . ? C118 C120 C121 121.0(7) . . ? C118 C120 H120 119.5 . . ? C121 C120 H120 119.5 . . ? C120 C121 C119 114.1(6) . . ? C120 C121 C122 122.8(7) . . ? C119 C121 C122 123.0(7) . . ? C123 C122 C124 117.3(6) . . ? C123 C122 C121 119.6(7) . . ? C124 C122 C121 123.0(6) . . ? C126 C123 C122 119.4(8) . . ? C126 C123 H123 120.3 . . ? C122 C123 H123 120.3 . . ? C125 C124 C122 117.7(7) . . ? C125 C124 H124 121.1 . . ? C122 C124 H124 121.1 . . ? N2 C125 C124 124.2(7) . . ? N2 C125 H125 117.9 . . ? C124 C125 H125 117.9 . . ? N2 C126 C123 122.7(7) . . ? N2 C126 H126 118.6 . . ? C123 C126 H126 118.6 . . ? C2A C1A N4 125.1(13) . . ? C2A C1A H1A 117.5 . . ? N4 C1A H1A 117.5 . . ? C1A C2A C5 120.0(12) . . ? C1A C2A H2A 120.0 . . ? C5 C2A H2A 120.0 . . ? N4 C1B C2B 122(3) . . ? N4 C1B H1B 119.1 . . ? C2B C1B H1B 119.1 . . ? C1B C2B C5 115(3) . . ? C1B C2B H2B 122.5 . . ? C5 C2B H2B 122.5 . . ? C118 N1 C117 121.4(6) . . ? C118 N1 Zn1 119.6(5) . . ? C117 N1 Zn1 119.0(5) . . ? C126 N2 C125 118.6(6) . . ? C126 N2 Zn2 120.6(5) . 1_655 ? C125 N2 Zn2 120.8(5) . 1_655 ? C9 N3 C10 117.3(6) . . ? C9 N3 Zn3 122.6(5) . . ? C10 N3 Zn3 120.0(5) . . ? C3 N4 C1A 107.7(9) . . ? C3 N4 C1B 110.4(14) . . ? C1A N4 C1B 45.6(13) . . ? C3 N4 Zn4 126.2(6) . 1_655 ? C1A N4 Zn4 122.1(7) . 1_655 ? C1B N4 Zn4 118.3(13) . 1_655 ? C77 N5 C76 119.5(7) . . ? C77 N5 Zn6 121.7(5) . 1_655 ? C76 N5 Zn6 118.8(6) . 1_655 ? C84 N6 C85 117.7(6) . . ? C84 N6 Zn5 121.4(5) . . ? C85 N6 Zn5 120.9(5) . . ? C86 O1 Zn1 122.3(5) . . ? C86 O2 Zn2 133.2(5) . . ? C101 O3 Zn2 125.0(5) . 2_546 ? C101 O4 Zn1 127.9(5) . 2_546 ? C102 O5 Zn1 131.9(5) . . ? C102 O6 Zn2 122.3(5) . . ? C11 O7 Zn2 131.3(5) . 2_545 ? C11 O8 Zn1 125.7(5) . 2_545 ? C12 O9 Zn3 129.0(5) . . ? C12 O10 Zn4 126.5(5) . . ? C27 O11 Zn5 131.0(5) . . ? C27 O12 Zn6 125.6(5) . . ? C28 O13 Zn3 125.1(5) . . ? C28 O14 Zn4 129.1(5) . . ? C43 O15 Zn5 121.2(5) . 1_554 ? C43 O16 Zn6 132.0(5) . 1_554 ? C44 O17 Zn5 127.7(5) . 1_565 ? C44 O18 Zn6 124.7(5) . 1_565 ? C59 O19 Zn3 119.6(5) . . ? C59 O20 Zn4 134.4(5) . . ? C60 O22 Zn5 125.6(5) . 1_564 ? C60 O23 Zn6 128.1(5) . 1_564 ? C75 O24 Zn3 134.7(5) . . ? C75 O25 Zn4 118.5(5) . . ? O1 Zn1 O4 90.4(2) . 2_556 ? O1 Zn1 O8 164.6(2) . 2 ? O4 Zn1 O8 85.9(2) 2_556 2 ? O1 Zn1 O5 85.8(2) . . ? O4 Zn1 O5 152.0(2) 2_556 . ? O8 Zn1 O5 90.4(2) 2 . ? O1 Zn1 N1 99.2(2) . . ? O4 Zn1 N1 107.9(2) 2_556 . ? O8 Zn1 N1 96.1(2) 2 . ? O5 Zn1 N1 100.0(2) . . ? O1 Zn1 Zn2 83.98(15) . . ? O4 Zn1 Zn2 77.69(14) 2_556 . ? O8 Zn1 Zn2 80.67(14) 2 . ? O5 Zn1 Zn2 74.36(15) . . ? N1 Zn1 Zn2 173.40(17) . . ? O6 Zn2 O7 89.3(2) . 2 ? O6 Zn2 O2 84.9(2) . . ? O7 Zn2 O2 150.2(2) 2 . ? O6 Zn2 O3 164.1(2) . 2_556 ? O7 Zn2 O3 86.0(2) 2 2_556 ? O2 Zn2 O3 91.6(2) . 2_556 ? O6 Zn2 N2 98.2(2) . 1_455 ? O7 Zn2 N2 105.9(2) 2 1_455 ? O2 Zn2 N2 103.9(2) . 1_455 ? O3 Zn2 N2 97.7(2) 2_556 1_455 ? O6 Zn2 Zn1 83.76(16) . . ? O7 Zn2 Zn1 76.81(14) 2 . ? O2 Zn2 Zn1 73.52(15) . . ? O3 Zn2 Zn1 80.43(14) 2_556 . ? N2 Zn2 Zn1 176.66(17) 1_455 . ? O9 Zn3 O24 152.9(2) . . ? O9 Zn3 N3 104.6(2) . . ? O24 Zn3 N3 102.4(2) . . ? O9 Zn3 O19 90.1(2) . . ? O24 Zn3 O19 85.4(2) . . ? N3 Zn3 O19 100.2(2) . . ? O9 Zn3 O13 85.9(2) . . ? O24 Zn3 O13 91.3(2) . . ? N3 Zn3 O13 95.2(2) . . ? O19 Zn3 O13 164.6(2) . . ? O9 Zn3 Zn4 78.72(15) . . ? O24 Zn3 Zn4 74.29(14) . . ? N3 Zn3 Zn4 173.97(19) . . ? O19 Zn3 Zn4 84.68(14) . . ? O13 Zn3 Zn4 79.91(15) . . ? N4 Zn4 O14 103.6(3) 1_455 . ? N4 Zn4 O20 103.3(2) 1_455 . ? O14 Zn4 O20 153.1(2) . . ? N4 Zn4 O10 95.3(2) 1_455 . ? O14 Zn4 O10 89.3(2) . . ? O20 Zn4 O10 90.0(2) . . ? N4 Zn4 O25 99.8(2) 1_455 . ? O14 Zn4 O25 87.6(2) . . ? O20 Zn4 O25 86.2(2) . . ? O10 Zn4 O25 164.9(2) . . ? N4 Zn4 Zn3 175.07(19) 1_455 . ? O14 Zn4 Zn3 78.86(14) . . ? O20 Zn4 Zn3 74.46(14) . . ? O10 Zn4 Zn3 80.41(14) . . ? O25 Zn4 Zn3 84.48(14) . . ? O15 Zn5 N6 99.5(2) 1_556 . ? O15 Zn5 O17 162.1(2) 1_556 1_545 ? N6 Zn5 O17 98.3(2) . 1_545 ? O15 Zn5 O22 88.8(2) 1_556 1_546 ? N6 Zn5 O22 105.9(2) . 1_546 ? O17 Zn5 O22 88.1(2) 1_545 1_546 ? O15 Zn5 O11 86.0(2) 1_556 . ? N6 Zn5 O11 97.9(2) . . ? O17 Zn5 O11 89.7(2) 1_545 . ? O22 Zn5 O11 156.2(2) 1_546 . ? O15 Zn5 Zn6 83.10(15) 1_556 . ? N6 Zn5 Zn6 174.08(18) . . ? O17 Zn5 Zn6 78.96(14) 1_545 . ? O22 Zn5 Zn6 79.37(15) 1_546 . ? O11 Zn5 Zn6 76.95(15) . . ? O23 Zn6 N5 97.5(2) 1_546 1_455 ? O23 Zn6 O16 87.9(2) 1_546 1_556 ? N5 Zn6 O16 99.1(2) 1_455 1_556 ? O23 Zn6 O12 160.9(2) 1_546 . ? N5 Zn6 O12 101.5(2) 1_455 . ? O16 Zn6 O12 88.1(3) 1_556 . ? O23 Zn6 O18 88.3(2) 1_546 1_545 ? N5 Zn6 O18 105.5(2) 1_455 1_545 ? O16 Zn6 O18 155.4(2) 1_556 1_545 ? O12 Zn6 O18 87.6(2) . 1_545 ? O23 Zn6 Zn5 78.95(15) 1_546 . ? N5 Zn6 Zn5 173.22(19) 1_455 . ? O16 Zn6 Zn5 75.09(14) 1_556 . ? O12 Zn6 Zn5 82.02(16) . . ? O18 Zn6 Zn5 80.36(15) 1_545 . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 5.481 _refine_diff_density_min -2.042 _refine_diff_density_rms 0.167 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 1 -0.267 0.032 0.597 3292.6 823.0 2 0.498 0.877 0.246 26.6 0.5 3 0.501 0.377 0.754 26.6 0.6 _platon_squeeze_details ; ? ;