data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Bacchi, Alessia' _publ_contact_author_email alessia.bacchi@unipr.it _publ_section_title ; Diamondoid and square-grid networks based on bent wheel-and-axle diols ; loop_ _publ_author_name A.Bacchi M.Carcelli P.Pelagatti T.Chiodo ##################### # Adamantoid and square-grid networks: # from wheel-and-axle diols to bent-axle zinc complexes # A. Bacchi, M. Carcelli, T. Chiodo, P. Pelagatti # submitted to CrystEngComm ##################### data_1 _database_code_depnum_ccdc_archive 'CCDC 775954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 Cl2 N4 O2 Zn' _chemical_formula_weight 837.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P42 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' _cell_length_a 19.5952(16) _cell_length_b 19.5952(16) _cell_length_c 5.2472(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2014.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 4 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715575 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS procedure' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17512 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2896 _reflns_number_gt 2005 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^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 0.007(19) _refine_ls_number_reflns 2896 _refine_ls_number_parameters 356 _refine_ls_number_restraints 775 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.824 _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 -0.5000 0.0000 0.52347(16) 0.04637(19) Uani 1 2 d SU . . Cl1 Cl -0.42931(7) -0.07066(7) 0.7244(3) 0.0816(4) Uani 1 1 d U . . O1 O -0.83263(16) -0.33268(16) -1.1107(6) 0.0616(9) Uani 1 1 d DU . . H1O H -0.8613 -0.3579 -1.0468 0.100 Uiso 1 1 calc RD A 1 C61 C -0.6526(6) -0.1948(8) -0.248(3) 0.058(3) Uani 0.499(3) 1 d PU B 2 H61 H -0.6314 -0.2371 -0.2601 0.069 Uiso 0.499(3) 1 calc PR B 2 N21 N -0.7003(6) -0.1733(7) -0.379(3) 0.049(3) Uani 0.499(3) 1 d PU B 2 C6 C -0.6946(8) -0.1527(7) -0.245(3) 0.061(3) Uani 0.501(3) 1 d PU B 1 H6 H -0.7371 -0.1317 -0.2530 0.074 Uiso 0.501(3) 1 calc PR B 1 N2 N -0.6744(7) -0.1995(6) -0.381(3) 0.052(3) Uani 0.501(3) 1 d PU B 1 N1 N -0.55921(15) -0.05947(15) 0.2972(4) 0.0519(11) Uani 1 1 d GU B . C1 C -0.62153(16) -0.03478(15) 0.2105(7) 0.0829(16) Uani 1 1 d GU . . H1 H -0.6379 0.0069 0.2696 0.100 Uiso 1 1 calc R . . C2 C -0.65934(16) -0.0723(2) 0.0356(8) 0.116(2) Uani 1 1 d GU B . H2 H -0.7010 -0.0558 -0.0223 0.139 Uiso 1 1 calc R . . C3 C -0.6348(2) -0.1345(2) -0.0526(6) 0.115(2) Uani 1 1 d GU . . C4 C -0.5725(2) -0.15924(16) 0.0340(8) 0.118(2) Uani 1 1 d GU B . H4 H -0.5561 -0.2009 -0.0250 0.142 Uiso 1 1 calc R . . C5 C -0.53469(15) -0.12170(16) 0.2089(7) 0.0850(16) Uani 1 1 d GU . . H5 H -0.4930 -0.1382 0.2669 0.102 Uiso 1 1 calc R B . C7 C -0.7172(9) -0.2318(8) -0.566(4) 0.045(4) Uani 0.501(3) 1 d PGU B 1 C8 C -0.7767(8) -0.2028(7) -0.662(4) 0.043(3) Uani 0.501(3) 1 d PGU B 1 H8 H -0.7903 -0.1598 -0.6069 0.051 Uiso 0.501(3) 1 calc PR B 1 C9 C -0.8156(8) -0.2380(8) -0.840(5) 0.049(3) Uani 0.501(3) 1 d PGDU B 1 C10 C -0.7952(9) -0.3023(9) -0.922(5) 0.043(4) Uani 0.501(3) 1 d PGU B 1 C11 C -0.7358(9) -0.3313(7) -0.826(5) 0.042(3) Uani 0.501(3) 1 d PGDU B 1 C12 C -0.6968(8) -0.2961(7) -0.648(4) 0.052(4) Uani 0.501(3) 1 d PGU B 1 H12 H -0.6570 -0.3155 -0.5839 0.063 Uiso 0.501(3) 1 calc PR B 1 C13 C -0.8800(3) -0.2042(3) -0.9374(12) 0.041(3) Uani 0.501(3) 1 d PGDU B 1 C14 C -0.9416(3) -0.2385(2) -0.9088(12) 0.053(3) Uani 0.501(3) 1 d PGU B 1 H14 H -0.9423 -0.2825 -0.8420 0.064 Uiso 0.501(3) 1 calc PR B 1 C15 C -1.0023(2) -0.2072(3) -0.9799(14) 0.057(2) Uani 0.501(3) 1 d PGU B 1 H15 H -1.0436 -0.2301 -0.9607 0.068 Uiso 0.501(3) 1 calc PR B 1 C16 C -1.0014(3) -0.1414(3) -1.0796(14) 0.054(3) Uani 0.501(3) 1 d PGU B 1 H16 H -1.0420 -0.1204 -1.1272 0.065 Uiso 0.501(3) 1 calc PR B 1 C17 C -0.9398(3) -0.1071(2) -1.1082(12) 0.060(2) Uani 0.501(3) 1 d PGU B 1 H17 H -0.9392 -0.0632 -1.1750 0.072 Uiso 0.501(3) 1 calc PR B 1 C18 C -0.8791(3) -0.1385(3) -1.0371(11) 0.051(2) Uani 0.501(3) 1 d PGU B 1 H18 H -0.8379 -0.1156 -1.0563 0.061 Uiso 0.501(3) 1 calc PR B 1 C19 C -0.7109(3) -0.3999(3) -0.9096(12) 0.051(3) Uani 0.501(3) 1 d PGDU B 1 C20 C -0.7025(3) -0.4156(3) -1.1660(11) 0.060(3) Uani 0.501(3) 1 d PGU B 1 H20 H -0.7187 -0.3859 -1.2903 0.072 Uiso 0.501(3) 1 calc PR B 1 C21 C -0.6698(4) -0.4756(3) -1.2366(12) 0.072(3) Uani 0.501(3) 1 d PGU B 1 H21 H -0.6641 -0.4861 -1.4082 0.086 Uiso 0.501(3) 1 calc PR B 1 C22 C -0.6455(3) -0.5200(3) -1.0509(16) 0.075(4) Uani 0.501(3) 1 d PGU B 1 H22 H -0.6236 -0.5602 -1.0981 0.090 Uiso 0.501(3) 1 calc PR B 1 C23 C -0.6540(3) -0.5043(3) -0.7944(14) 0.064(3) Uani 0.501(3) 1 d PGU B 1 H23 H -0.6378 -0.5340 -0.6701 0.077 Uiso 0.501(3) 1 calc PR B 1 C24 C -0.6867(4) -0.4443(3) -0.7238(10) 0.060(3) Uani 0.501(3) 1 d PGU B 1 H24 H -0.6924 -0.4338 -0.5522 0.071 Uiso 0.501(3) 1 calc PR B 1 C71 C -0.7316(8) -0.2172(9) -0.564(4) 0.046(4) Uani 0.499(3) 1 d PGU B 2 C81 C -0.7956(7) -0.1965(8) -0.648(4) 0.051(4) Uani 0.499(3) 1 d PGU B 2 H81 H -0.8153 -0.1571 -0.5817 0.061 Uiso 0.499(3) 1 calc PR B 2 C91 C -0.8301(7) -0.2346(8) -0.830(5) 0.044(3) Uani 0.499(3) 1 d PGDU B 2 C101 C -0.8007(9) -0.2935(9) -0.928(5) 0.044(4) Uani 0.499(3) 1 d PGU B 2 C111 C -0.7367(9) -0.3143(7) -0.844(4) 0.044(4) Uani 0.499(3) 1 d PGDU B 2 C121 C -0.7021(7) -0.2762(8) -0.662(4) 0.042(3) Uani 0.499(3) 1 d PGU B 2 H121 H -0.6593 -0.2900 -0.6059 0.051 Uiso 0.499(3) 1 calc PR B 2 C131 C -0.8997(3) -0.2102(3) -0.9081(11) 0.049(3) Uani 0.499(3) 1 d PGDU B 2 C141 C -0.9440(3) -0.1859(4) -0.7223(10) 0.058(3) Uani 0.499(3) 1 d PGU B 2 H141 H -0.9333 -0.1912 -0.5507 0.070 Uiso 0.499(3) 1 calc PR B 2 C151 C -1.0044(3) -0.1537(3) -0.7928(14) 0.067(3) Uani 0.499(3) 1 d PGU B 2 H151 H -1.0340 -0.1374 -0.6685 0.081 Uiso 0.499(3) 1 calc PR B 2 C161 C -1.0204(3) -0.1458(3) -1.0492(16) 0.075(4) Uani 0.499(3) 1 d PGU B 2 H161 H -1.0607 -0.1243 -1.0964 0.090 Uiso 0.499(3) 1 calc PR B 2 C171 C -0.9760(3) -0.1701(4) -1.2351(12) 0.073(3) Uani 0.499(3) 1 d PGU B 2 H171 H -0.9867 -0.1648 -1.4066 0.088 Uiso 0.499(3) 1 calc PR B 2 C181 C -0.9157(3) -0.2023(3) -1.1645(10) 0.058(3) Uani 0.499(3) 1 d PGU B 2 H181 H -0.8861 -0.2186 -1.2889 0.069 Uiso 0.499(3) 1 calc PR B 2 C191 C -0.7043(3) -0.3803(2) -0.9372(12) 0.041(3) Uani 0.499(3) 1 d PGDU B 2 C201 C -0.7385(2) -0.4420(3) -0.9089(13) 0.056(3) Uani 0.499(3) 1 d PGU B 2 H201 H -0.7825 -0.4428 -0.8426 0.067 Uiso 0.499(3) 1 calc PR B 2 C211 C -0.7069(3) -0.5026(2) -0.9795(15) 0.059(3) Uani 0.499(3) 1 d PGU B 2 H211 H -0.7297 -0.5439 -0.9606 0.071 Uiso 0.499(3) 1 calc PR B 2 C221 C -0.6411(3) -0.5015(2) -1.0785(15) 0.055(3) Uani 0.499(3) 1 d PGU B 2 H221 H -0.6199 -0.5421 -1.1258 0.066 Uiso 0.499(3) 1 calc PR B 2 C231 C -0.6069(2) -0.4398(3) -1.1068(12) 0.058(2) Uani 0.499(3) 1 d PGU B 2 H231 H -0.5629 -0.4391 -1.1731 0.070 Uiso 0.499(3) 1 calc PR B 2 C241 C -0.6385(3) -0.3792(2) -1.0362(12) 0.050(2) Uani 0.499(3) 1 d PGU B 2 H241 H -0.6157 -0.3379 -1.0551 0.060 Uiso 0.499(3) 1 calc PR B 2 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 0.0487(5) 0.0481(5) 0.0424(3) 0.000 0.000 -0.0118(4) Cl1 0.0902(11) 0.0903(11) 0.0644(8) 0.0103(9) -0.0096(9) 0.0209(8) O1 0.059(2) 0.063(2) 0.063(2) -0.0193(18) -0.0147(18) -0.0092(17) C61 0.053(7) 0.055(6) 0.065(8) 0.024(5) -0.009(5) 0.003(6) N21 0.042(6) 0.050(7) 0.055(7) -0.002(5) 0.001(5) 0.008(4) C6 0.066(7) 0.062(8) 0.056(8) -0.012(5) 0.020(5) -0.010(6) N2 0.051(8) 0.049(6) 0.057(7) -0.005(6) -0.006(6) 0.001(5) N1 0.057(2) 0.056(2) 0.042(3) -0.0018(19) -0.0008(19) -0.0232(19) C1 0.077(3) 0.090(4) 0.081(4) 0.012(3) -0.027(3) -0.023(3) C2 0.116(4) 0.142(5) 0.090(4) 0.012(4) -0.058(4) -0.072(4) C3 0.148(5) 0.155(5) 0.040(3) -0.006(3) 0.000(3) -0.118(5) C4 0.137(5) 0.116(4) 0.101(5) -0.062(5) 0.013(4) -0.072(4) C5 0.093(4) 0.074(3) 0.088(4) -0.025(3) 0.010(4) -0.026(3) C7 0.036(7) 0.048(9) 0.052(7) -0.007(6) -0.006(6) -0.008(6) C8 0.042(8) 0.029(6) 0.057(8) -0.013(5) 0.003(6) 0.003(5) C9 0.047(6) 0.058(7) 0.042(7) -0.010(5) -0.004(6) 0.001(5) C10 0.053(8) 0.038(6) 0.038(8) -0.002(5) -0.004(6) -0.006(6) C11 0.035(6) 0.042(7) 0.051(7) -0.002(6) 0.002(4) -0.010(5) C12 0.049(7) 0.054(10) 0.054(8) -0.014(8) -0.004(5) 0.010(6) C13 0.042(4) 0.040(5) 0.041(6) -0.018(5) 0.008(4) -0.007(4) C14 0.048(5) 0.052(5) 0.059(7) -0.001(5) -0.001(5) -0.005(4) C15 0.038(4) 0.066(5) 0.066(7) -0.013(6) 0.006(6) -0.004(4) C16 0.050(5) 0.065(7) 0.047(7) -0.017(6) -0.001(6) 0.020(5) C17 0.072(6) 0.053(5) 0.056(6) 0.001(5) 0.001(5) 0.009(4) C18 0.050(4) 0.053(5) 0.049(6) -0.006(4) 0.000(4) -0.005(4) C19 0.046(6) 0.055(6) 0.053(6) -0.010(4) 0.001(6) 0.001(5) C20 0.077(7) 0.054(5) 0.050(5) 0.000(4) -0.002(5) 0.003(5) C21 0.085(7) 0.059(6) 0.071(6) -0.015(5) 0.004(6) 0.016(6) C22 0.093(9) 0.050(6) 0.082(8) -0.009(5) 0.004(7) 0.001(6) C23 0.082(7) 0.044(6) 0.066(6) -0.006(5) -0.019(7) 0.005(5) C24 0.072(7) 0.056(6) 0.051(5) -0.007(4) -0.009(5) 0.003(5) C71 0.045(9) 0.037(7) 0.055(8) -0.008(6) -0.002(6) -0.002(6) C81 0.053(9) 0.044(7) 0.056(8) 0.003(5) -0.014(8) 0.009(5) C91 0.053(7) 0.027(6) 0.051(7) 0.003(5) -0.007(6) -0.002(5) C101 0.044(7) 0.042(7) 0.047(9) -0.001(6) -0.009(6) -0.005(5) C111 0.051(6) 0.041(6) 0.040(7) -0.005(6) -0.003(5) 0.001(5) C121 0.026(6) 0.041(8) 0.060(8) -0.002(6) -0.009(5) 0.000(5) C131 0.055(6) 0.042(6) 0.049(6) 0.003(5) -0.010(4) 0.002(5) C141 0.056(6) 0.074(7) 0.046(5) -0.005(5) -0.005(4) -0.002(5) C151 0.043(6) 0.088(8) 0.070(6) -0.022(7) -0.004(5) 0.006(5) C161 0.047(6) 0.093(9) 0.085(8) 0.004(7) -0.013(5) -0.002(6) C171 0.057(6) 0.095(8) 0.068(6) 0.001(6) -0.023(5) 0.009(6) C181 0.060(6) 0.072(6) 0.040(5) -0.004(5) -0.004(4) 0.008(5) C191 0.040(5) 0.041(4) 0.043(6) -0.002(4) -0.020(5) -0.006(4) C201 0.052(5) 0.043(4) 0.072(8) -0.007(5) 0.000(5) -0.002(4) C211 0.064(5) 0.042(4) 0.071(7) -0.005(6) -0.014(6) -0.001(4) C221 0.062(7) 0.046(5) 0.056(7) -0.004(6) -0.017(6) 0.022(5) C231 0.048(5) 0.069(6) 0.057(6) 0.000(5) -0.007(5) 0.013(4) C241 0.054(5) 0.043(4) 0.052(6) -0.006(4) -0.010(4) -0.004(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 Zn1 N1 2.028(2) . ? Zn1 N1 2.028(2) 2_455 ? Zn1 Cl1 2.2242(13) 2_455 ? Zn1 Cl1 2.2242(13) . ? O1 C10 1.369(13) . ? O1 C101 1.377(13) . ? C61 N21 1.234(19) . ? C61 C3 1.602(17) . ? N21 C71 1.436(16) . ? C6 N2 1.23(2) . ? C6 C3 1.586(17) . ? N2 C7 1.432(16) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C9 C13 1.514(10) . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C11 C19 1.495(10) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C71 C81 1.3900 . ? C71 C121 1.3900 . ? C81 C91 1.3900 . ? C91 C101 1.3900 . ? C91 C131 1.502(10) . ? C101 C111 1.3900 . ? C111 C121 1.3900 . ? C111 C191 1.521(9) . ? C131 C141 1.3900 . ? C131 C181 1.3900 . ? C141 C151 1.3900 . ? C151 C161 1.3900 . ? C161 C171 1.3900 . ? C171 C181 1.3900 . ? C191 C201 1.3900 . ? C191 C241 1.3900 . ? C201 C211 1.3900 . ? C211 C221 1.3900 . ? C221 C231 1.3900 . ? C231 C241 1.3900 . ? 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 N1 Zn1 N1 108.33(16) . 2_455 ? N1 Zn1 Cl1 106.20(11) . 2_455 ? N1 Zn1 Cl1 106.03(11) 2_455 2_455 ? N1 Zn1 Cl1 106.03(11) . . ? N1 Zn1 Cl1 106.20(11) 2_455 . ? Cl1 Zn1 Cl1 123.41(9) 2_455 . ? C10 O1 C101 8.6(12) . . ? N21 C61 C3 105.5(14) . . ? C61 N21 C71 119.6(16) . . ? N2 C6 C3 107.4(15) . . ? C6 N2 C7 122.4(17) . . ? C1 N1 C5 120.0 . . ? C1 N1 Zn1 119.61(19) . . ? C5 N1 Zn1 120.09(19) . . ? N1 C1 C2 120.0 . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 C6 141.1(6) . . ? C2 C3 C6 98.8(6) . . ? C4 C3 C61 98.2(5) . . ? C2 C3 C61 141.7(5) . . ? C6 C3 C61 42.9(5) . . ? C3 C4 C5 120.0 . . ? C4 C5 N1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 N2 123.8(10) . . ? C12 C7 N2 116.2(10) . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 C13 117.9(9) . . ? C10 C9 C13 122.1(9) . . ? O1 C10 C11 122.2(10) . . ? O1 C10 C9 117.6(10) . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 C19 122.3(10) . . ? C12 C11 C19 117.7(9) . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 C9 118.4(10) . . ? C18 C13 C9 121.4(9) . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 C11 121.4(10) . . ? C24 C19 C11 117.9(10) . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C81 C71 C121 120.0 . . ? C81 C71 N21 115.1(10) . . ? C121 C71 N21 124.9(10) . . ? C71 C81 C91 120.0 . . ? C101 C91 C81 120.0 . . ? C101 C91 C131 122.7(10) . . ? C81 C91 C131 117.3(10) . . ? O1 C101 C111 117.9(9) . . ? O1 C101 C91 122.1(9) . . ? C111 C101 C91 120.0 . . ? C121 C111 C101 120.0 . . ? C121 C111 C191 118.4(9) . . ? C101 C111 C191 121.6(9) . . ? C111 C121 C71 120.0 . . ? C141 C131 C181 120.0 . . ? C141 C131 C91 119.0(10) . . ? C181 C131 C91 120.3(10) . . ? C151 C141 C131 120.0 . . ? C141 C151 C161 120.0 . . ? C171 C161 C151 120.0 . . ? C161 C171 C181 120.0 . . ? C171 C181 C131 120.0 . . ? C201 C191 C241 120.0 . . ? C201 C191 C111 120.3(9) . . ? C241 C191 C111 119.5(9) . . ? C191 C201 C211 120.0 . . ? C221 C211 C201 120.0 . . ? C231 C221 C211 120.0 . . ? C241 C231 C221 120.0 . . ? C231 C241 C191 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.313 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.042 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 775955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 Br2 N4 O2 Zn' _chemical_formula_weight 926.00 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' Br Br -0.2901 2.4595 '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 tetragonal _symmetry_space_group_name_H-M P42 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' _cell_length_a 19.589(7) _cell_length_b 19.589(7) _cell_length_c 5.149(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1975.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 4 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 2.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.542584 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS procedure' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9820 _diffrn_reflns_av_R_equivalents 0.1168 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 18.98 _reflns_number_total 1582 _reflns_number_gt 1112 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^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 0.13(3) _refine_ls_number_reflns 1582 _refine_ls_number_parameters 356 _refine_ls_number_restraints 769 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.751 _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 0.5000 0.0000 -0.5205(4) 0.0389(5) Uani 1 2 d SU . . Br Br 0.42460(6) 0.07535(6) -0.7327(2) 0.0672(5) Uani 1 1 d U . . O1 O 0.8273(4) 0.3276(4) 1.1430(13) 0.051(2) Uani 1 1 d DU . . H1O H 0.8554 0.3522 1.0713 0.100 Uiso 1 1 calc RD A 1 C61 C 0.6521(14) 0.1953(17) 0.242(6) 0.051(6) Uani 0.498(6) 1 d PU B 2 H61 H 0.6327 0.2387 0.2415 0.062 Uiso 0.498(6) 1 calc PR B 2 N21 N 0.6985(10) 0.1721(12) 0.397(5) 0.025(5) Uani 0.498(6) 1 d PU B 2 C6 C 0.6943(17) 0.1535(14) 0.235(6) 0.050(6) Uani 0.502(6) 1 d PU B 1 H6 H 0.7380 0.1352 0.2293 0.060 Uiso 0.502(6) 1 calc PR B 1 N2 N 0.6730(13) 0.1988(11) 0.395(5) 0.033(6) Uani 0.502(6) 1 d PU B 1 N1 N 0.5603(4) 0.0605(3) -0.2979(14) 0.045(3) Uani 1 1 d GU B . C1 C 0.6227(4) 0.0358(3) -0.2101(19) 0.075(4) Uani 1 1 d GU . . H1 H 0.6391 -0.0058 -0.2708 0.090 Uiso 1 1 calc R . . C2 C 0.6605(4) 0.0732(5) -0.031(2) 0.096(4) Uani 1 1 d GU B . H2 H 0.7022 0.0567 0.0273 0.115 Uiso 1 1 calc R . . C3 C 0.6359(5) 0.1354(5) 0.0593(14) 0.085(4) Uani 1 1 d GU . . C4 C 0.5735(5) 0.1601(4) -0.029(2) 0.098(4) Uani 1 1 d GU B . H4 H 0.5571 0.2016 0.0322 0.118 Uiso 1 1 calc R . . C5 C 0.5357(3) 0.1226(4) -0.207(2) 0.078(4) Uani 1 1 d GU . . H5 H 0.4940 0.1392 -0.2659 0.094 Uiso 1 1 calc R B . C7 C 0.7187(14) 0.2325(11) 0.566(6) 0.032(6) Uani 0.502(6) 1 d PGU B 1 C8 C 0.7758(14) 0.2006(12) 0.671(7) 0.034(6) Uani 0.502(6) 1 d PGU B 1 H8 H 0.7897 0.1584 0.6078 0.040 Uiso 0.502(6) 1 calc PR B 1 C9 C 0.8120(12) 0.2318(14) 0.871(7) 0.032(5) Uani 0.502(6) 1 d PGDU B 1 C10 C 0.7911(15) 0.2949(14) 0.965(7) 0.035(5) Uani 0.502(6) 1 d PGU B 1 C11 C 0.7341(15) 0.3268(11) 0.860(7) 0.039(5) Uani 0.502(6) 1 d PGDU B 1 C12 C 0.6979(12) 0.2956(10) 0.661(7) 0.035(7) Uani 0.502(6) 1 d PGU B 1 H12 H 0.6597 0.3170 0.5904 0.041 Uiso 0.502(6) 1 calc PR B 1 C13 C 0.8782(6) 0.2004(7) 0.963(3) 0.031(5) Uani 0.502(6) 1 d PGDU B 1 C14 C 0.9397(7) 0.2347(6) 0.928(3) 0.043(5) Uani 0.502(6) 1 d PGU B 1 H14 H 0.9400 0.2785 0.8588 0.051 Uiso 0.502(6) 1 calc PR B 1 C15 C 1.0007(6) 0.2034(7) 0.998(3) 0.040(5) Uani 0.502(6) 1 d PGU B 1 H15 H 1.0418 0.2263 0.9751 0.048 Uiso 0.502(6) 1 calc PR B 1 C16 C 1.0002(6) 0.1379(8) 1.102(3) 0.047(6) Uani 0.502(6) 1 d PGU B 1 H16 H 1.0411 0.1170 1.1485 0.057 Uiso 0.502(6) 1 calc PR B 1 C17 C 0.9387(8) 0.1037(6) 1.136(3) 0.043(5) Uani 0.502(6) 1 d PGU B 1 H17 H 0.9384 0.0599 1.2056 0.052 Uiso 0.502(6) 1 calc PR B 1 C18 C 0.8777(6) 0.1349(7) 1.067(3) 0.040(5) Uani 0.502(6) 1 d PGU B 1 H18 H 0.8366 0.1120 1.0894 0.047 Uiso 0.502(6) 1 calc PR B 1 C19 C 0.7113(7) 0.3981(6) 0.927(3) 0.030(5) Uani 0.502(6) 1 d PGDU B 1 C20 C 0.7014(7) 0.4123(6) 1.188(3) 0.036(5) Uani 0.502(6) 1 d PGU B 1 H20 H 0.7167 0.3819 1.3140 0.043 Uiso 0.502(6) 1 calc PR B 1 C21 C 0.6685(7) 0.4722(7) 1.262(3) 0.055(5) Uani 0.502(6) 1 d PGU B 1 H21 H 0.6619 0.4817 1.4376 0.066 Uiso 0.502(6) 1 calc PR B 1 C22 C 0.6456(7) 0.5177(6) 1.075(4) 0.048(6) Uani 0.502(6) 1 d PGU B 1 H22 H 0.6236 0.5577 1.1243 0.058 Uiso 0.502(6) 1 calc PR B 1 C23 C 0.6555(7) 0.5034(7) 0.813(3) 0.053(5) Uani 0.502(6) 1 d PGU B 1 H23 H 0.6401 0.5339 0.6874 0.063 Uiso 0.502(6) 1 calc PR B 1 C24 C 0.6883(7) 0.4436(7) 0.739(2) 0.042(5) Uani 0.502(6) 1 d PGU B 1 H24 H 0.6949 0.4341 0.5638 0.051 Uiso 0.502(6) 1 calc PR B 1 C71 C 0.7273(13) 0.2137(11) 0.594(6) 0.032(5) Uani 0.498(6) 1 d PGU B 2 C81 C 0.7921(13) 0.1943(13) 0.676(7) 0.035(6) Uani 0.498(6) 1 d PGU B 2 H81 H 0.8114 0.1541 0.6136 0.042 Uiso 0.498(6) 1 calc PR B 2 C91 C 0.8280(11) 0.2350(15) 0.850(7) 0.035(5) Uani 0.498(6) 1 d PGDU B 2 C101 C 0.7990(14) 0.2950(14) 0.942(7) 0.034(5) Uani 0.498(6) 1 d PGU B 2 C111 C 0.7342(13) 0.3144(12) 0.861(7) 0.040(5) Uani 0.498(6) 1 d PGDU B 2 C121 C 0.6983(10) 0.2738(11) 0.687(6) 0.024(6) Uani 0.498(6) 1 d PGU B 2 H121 H 0.6550 0.2868 0.6322 0.029 Uiso 0.498(6) 1 calc PR B 2 C131 C 0.8983(6) 0.2098(7) 0.928(3) 0.033(5) Uani 0.498(6) 1 d PGDU B 2 C141 C 0.9438(7) 0.1874(7) 0.739(2) 0.039(5) Uani 0.498(6) 1 d PGU B 2 H141 H 0.9338 0.1940 0.5644 0.047 Uiso 0.498(6) 1 calc PR B 2 C151 C 1.0040(7) 0.1552(7) 0.812(3) 0.047(5) Uani 0.498(6) 1 d PGU B 2 H151 H 1.0344 0.1402 0.6852 0.057 Uiso 0.498(6) 1 calc PR B 2 C161 C 1.0189(6) 0.1454(7) 1.073(3) 0.044(6) Uani 0.498(6) 1 d PGU B 2 H161 H 1.0592 0.1238 1.1214 0.053 Uiso 0.498(6) 1 calc PR B 2 C171 C 0.9735(7) 0.1678(7) 1.262(3) 0.051(5) Uani 0.498(6) 1 d PGU B 2 H171 H 0.9834 0.1613 1.4368 0.061 Uiso 0.498(6) 1 calc PR B 2 C181 C 0.9132(6) 0.2000(7) 1.190(3) 0.038(5) Uani 0.498(6) 1 d PGU B 2 H181 H 0.8828 0.2150 1.3160 0.046 Uiso 0.498(6) 1 calc PR B 2 C191 C 0.6996(7) 0.3781(6) 0.963(3) 0.030(5) Uani 0.498(6) 1 d PGDU B 2 C201 C 0.7345(6) 0.4394(8) 0.933(3) 0.041(5) Uani 0.498(6) 1 d PGU B 2 H201 H 0.7786 0.4395 0.8658 0.050 Uiso 0.498(6) 1 calc PR B 2 C211 C 0.7035(8) 0.5005(6) 1.003(3) 0.051(5) Uani 0.498(6) 1 d PGU B 2 H211 H 0.7268 0.5415 0.9825 0.062 Uiso 0.498(6) 1 calc PR B 2 C221 C 0.6376(8) 0.5004(6) 1.103(3) 0.050(6) Uani 0.498(6) 1 d PGU B 2 H221 H 0.6169 0.5413 1.1500 0.060 Uiso 0.498(6) 1 calc PR B 2 C231 C 0.6028(6) 0.4391(8) 1.134(3) 0.042(5) Uani 0.498(6) 1 d PGU B 2 H231 H 0.5587 0.4390 1.2009 0.050 Uiso 0.498(6) 1 calc PR B 2 C241 C 0.6338(7) 0.3780(6) 1.064(3) 0.035(5) Uani 0.498(6) 1 d PGU B 2 H241 H 0.6104 0.3370 1.0842 0.042 Uiso 0.498(6) 1 calc PR B 2 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 0.0355(13) 0.0363(13) 0.0451(10) 0.000 0.000 -0.0078(12) Br 0.0723(11) 0.0741(11) 0.0552(7) 0.0051(10) -0.0032(10) 0.0285(9) O1 0.050(5) 0.050(5) 0.053(6) -0.017(4) -0.009(4) -0.017(4) C61 0.067(14) 0.072(12) 0.015(13) 0.028(9) -0.008(9) -0.012(11) N21 0.020(11) 0.032(13) 0.022(11) 0.006(9) 0.011(8) -0.004(9) C6 0.079(13) 0.056(14) 0.013(14) 0.002(9) 0.019(9) -0.012(11) N2 0.050(13) 0.021(12) 0.027(12) 0.011(9) -0.015(9) 0.014(9) N1 0.046(6) 0.045(6) 0.046(7) 0.007(5) 0.005(4) -0.031(5) C1 0.090(9) 0.052(7) 0.083(9) 0.020(7) -0.050(8) -0.026(6) C2 0.099(9) 0.097(10) 0.091(10) 0.003(8) -0.044(9) -0.062(7) C3 0.113(10) 0.120(10) 0.021(8) 0.002(7) 0.003(7) -0.080(8) C4 0.094(10) 0.104(10) 0.097(10) -0.045(9) 0.003(8) -0.059(7) C5 0.067(8) 0.082(9) 0.087(9) -0.041(8) 0.009(8) -0.025(6) C7 0.036(11) 0.022(12) 0.038(12) 0.009(9) -0.011(8) 0.010(9) C8 0.044(12) 0.004(10) 0.053(12) 0.005(9) -0.021(9) 0.007(9) C9 0.027(9) 0.032(9) 0.038(11) 0.000(7) -0.002(9) -0.005(8) C10 0.027(11) 0.023(9) 0.056(12) -0.001(8) -0.008(9) -0.012(7) C11 0.026(9) 0.039(9) 0.052(10) -0.007(8) 0.003(7) 0.002(8) C12 0.014(11) 0.030(13) 0.060(14) -0.006(12) -0.004(9) 0.008(10) C13 0.029(7) 0.035(9) 0.029(11) -0.008(9) -0.003(8) -0.004(7) C14 0.030(8) 0.043(11) 0.056(13) -0.016(10) -0.006(11) -0.006(8) C15 0.027(8) 0.047(10) 0.045(12) -0.014(10) -0.008(10) -0.008(9) C16 0.043(9) 0.049(11) 0.050(13) -0.012(10) 0.015(12) 0.015(9) C17 0.050(11) 0.042(11) 0.039(12) 0.002(10) 0.016(11) 0.014(8) C18 0.047(9) 0.037(10) 0.035(12) -0.005(9) -0.004(10) 0.002(8) C19 0.017(11) 0.038(9) 0.035(9) 0.001(8) 0.001(10) -0.003(8) C20 0.035(11) 0.040(10) 0.033(8) -0.004(8) -0.007(10) 0.005(9) C21 0.069(13) 0.041(11) 0.057(9) -0.007(9) -0.004(12) 0.013(9) C22 0.055(14) 0.020(11) 0.069(11) -0.003(9) -0.006(12) -0.004(10) C23 0.067(13) 0.030(10) 0.061(9) 0.000(10) -0.021(12) -0.009(9) C24 0.049(13) 0.040(10) 0.037(9) 0.013(9) 0.000(12) -0.008(9) C71 0.037(11) 0.026(12) 0.034(11) 0.003(10) -0.007(8) 0.008(9) C81 0.040(12) 0.017(11) 0.049(13) 0.000(9) -0.017(10) 0.012(9) C91 0.035(9) 0.027(9) 0.044(11) 0.003(7) -0.002(8) -0.008(8) C101 0.023(9) 0.032(10) 0.048(11) -0.007(9) -0.003(9) -0.013(8) C111 0.033(9) 0.037(9) 0.051(12) -0.010(9) -0.003(7) -0.002(8) C121 0.010(9) 0.027(12) 0.036(13) 0.002(10) -0.001(8) 0.001(9) C131 0.037(9) 0.028(10) 0.032(8) -0.008(10) -0.003(8) -0.008(8) C141 0.040(10) 0.048(13) 0.028(9) -0.004(12) 0.000(9) -0.003(9) C151 0.035(10) 0.060(13) 0.046(9) -0.017(12) -0.011(10) 0.002(9) C161 0.029(11) 0.050(14) 0.053(10) -0.004(11) -0.008(9) 0.000(10) C171 0.042(11) 0.062(13) 0.048(9) -0.008(12) -0.006(9) 0.003(9) C181 0.043(10) 0.044(12) 0.027(8) -0.003(10) 0.002(8) 0.001(9) C191 0.025(9) 0.035(8) 0.031(11) -0.009(9) -0.010(9) -0.007(7) C201 0.032(10) 0.036(8) 0.056(13) -0.005(11) -0.013(10) -0.004(8) C211 0.053(11) 0.031(8) 0.069(13) -0.007(11) -0.010(11) -0.004(9) C221 0.052(11) 0.033(9) 0.065(13) 0.008(12) -0.012(10) 0.016(9) C231 0.041(12) 0.049(11) 0.035(12) 0.000(11) -0.002(10) 0.009(8) C241 0.043(10) 0.036(9) 0.025(12) 0.002(10) 0.003(9) -0.002(8) _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 N1 2.028(5) . ? Zn1 N1 2.028(5) 2_655 ? Zn1 Br 2.3568(17) . ? Zn1 Br 2.3568(17) 2_655 ? O1 C10 1.323(19) . ? O1 C101 1.33(2) . ? C61 N21 1.29(4) . ? C61 C3 1.54(3) . ? N21 C71 1.42(3) . ? C6 N2 1.28(4) . ? C6 C3 1.50(3) . ? N2 C7 1.42(3) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C9 C13 1.512(13) . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C11 C19 1.505(13) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C71 C81 1.3900 . ? C71 C121 1.3900 . ? C81 C91 1.3900 . ? C91 C101 1.3900 . ? C91 C131 1.518(13) . ? C101 C111 1.3900 . ? C111 C121 1.3900 . ? C111 C191 1.515(14) . ? C131 C141 1.3900 . ? C131 C181 1.3900 . ? C141 C151 1.3900 . ? C151 C161 1.3900 . ? C161 C171 1.3900 . ? C171 C181 1.3900 . ? C191 C201 1.3900 . ? C191 C241 1.3900 . ? C201 C211 1.3900 . ? C211 C221 1.3900 . ? C221 C231 1.3900 . ? C231 C241 1.3900 . ? 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 N1 Zn1 N1 111.2(4) . 2_655 ? N1 Zn1 Br 105.1(2) . . ? N1 Zn1 Br 105.2(2) 2_655 . ? N1 Zn1 Br 105.2(2) . 2_655 ? N1 Zn1 Br 105.1(2) 2_655 2_655 ? Br Zn1 Br 124.76(11) . 2_655 ? C10 O1 C101 8(3) . . ? N21 C61 C3 105(3) . . ? C61 N21 C71 121(3) . . ? N2 C6 C3 108(3) . . ? C6 N2 C7 121(3) . . ? C1 N1 C5 120.0 . . ? C1 N1 Zn1 119.5(5) . . ? C5 N1 Zn1 120.0(5) . . ? N1 C1 C2 120.0 . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 C6 141.5(13) . . ? C2 C3 C6 98.5(13) . . ? C4 C3 C61 96.5(13) . . ? C2 C3 C61 143.5(13) . . ? C6 C3 C61 45.0(13) . . ? C3 C4 C5 120.0 . . ? C4 C5 N1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 N2 122.6(15) . . ? C12 C7 N2 116.5(16) . . ? C7 C8 C9 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 C13 120.3(16) . . ? C8 C9 C13 119.4(16) . . ? O1 C10 C11 118.8(17) . . ? O1 C10 C9 121.0(17) . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 C19 124.6(16) . . ? C12 C11 C19 115.1(17) . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 C9 120.5(17) . . ? C18 C13 C9 119.4(16) . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 C11 116.6(17) . . ? C24 C19 C11 122.2(16) . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C81 C71 C121 120.0 . . ? C81 C71 N21 114.9(16) . . ? C121 C71 N21 124.8(16) . . ? C71 C81 C91 120.0 . . ? C101 C91 C81 120.0 . . ? C101 C91 C131 123.6(16) . . ? C81 C91 C131 116.4(16) . . ? O1 C101 C91 120.1(16) . . ? O1 C101 C111 118.8(17) . . ? C91 C101 C111 120.0 . . ? C121 C111 C101 120.0 . . ? C121 C111 C191 118.1(16) . . ? C101 C111 C191 121.9(16) . . ? C111 C121 C71 120.0 . . ? C141 C131 C181 120.0 . . ? C141 C131 C91 119.8(16) . . ? C181 C131 C91 119.5(17) . . ? C131 C141 C151 120.0 . . ? C161 C151 C141 120.0 . . ? C151 C161 C171 120.0 . . ? C181 C171 C161 120.0 . . ? C171 C181 C131 120.0 . . ? C201 C191 C241 120.0 . . ? C201 C191 C111 116.9(17) . . ? C241 C191 C111 122.9(16) . . ? C191 C201 C211 120.0 . . ? C201 C211 C221 120.0 . . ? C211 C221 C231 120.0 . . ? C241 C231 C221 120.0 . . ? C231 C241 C191 120.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 18.98 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.630 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.069 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 775956' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 I2 N4 O2 Zn' _chemical_formula_weight 1019.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 18.90370(10) _cell_length_b 18.90370(10) _cell_length_c 11.8392(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4230.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 4 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 2.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6147 _exptl_absorpt_correction_T_max 0.7450 _exptl_absorpt_process_details 'SADABS procedure' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42634 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.28 _reflns_number_total 3429 _reflns_number_gt 2682 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.2867P] 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 mixed _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 0.00 _refine_ls_number_reflns 3429 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.5000 0.0000 -0.45378(8) 0.0479(2) Uani 1 2 d S . . I1 I 0.60318(2) 0.063380(19) -0.54905(4) 0.06504(13) Uani 1 1 d . . . O1 O 0.7936(3) -0.3702(2) 0.2928(4) 0.0664(12) Uani 1 1 d . . . H1O H 0.835(3) -0.363(3) 0.292(5) 0.06(2) Uiso 1 1 d . . . N1 N 0.5456(2) -0.0748(2) -0.3493(4) 0.0483(11) Uani 1 1 d . . . N2 N 0.6784(2) -0.2003(2) -0.0451(5) 0.0680(13) Uani 1 1 d . . . C1 C 0.5307(3) -0.1436(3) -0.3541(5) 0.0604(16) Uani 1 1 d . . . H1 H 0.4986 -0.1592 -0.4082 0.072 Uiso 1 1 calc R . . C2 C 0.5603(3) -0.1926(3) -0.2828(5) 0.0627(16) Uani 1 1 d . . . H2 H 0.5489 -0.2402 -0.2897 0.075 Uiso 1 1 calc R . . C3 C 0.6067(3) -0.1707(3) -0.2019(5) 0.0532(14) Uani 1 1 d . . . C4 C 0.6222(3) -0.1001(3) -0.1959(5) 0.0658(18) Uani 1 1 d . . . H4 H 0.6533 -0.0835 -0.1410 0.079 Uiso 1 1 calc R . . C5 C 0.5916(3) -0.0532(3) -0.2716(5) 0.0648(17) Uani 1 1 d . . . H5 H 0.6035 -0.0055 -0.2680 0.078 Uiso 1 1 calc R . . C6 C 0.6380(3) -0.2208(3) -0.1194(5) 0.0644(17) Uani 1 1 d . . . H6 H 0.6268 -0.2686 -0.1241 0.077 Uiso 1 1 calc R . . C7 C 0.7058(3) -0.2474(3) 0.0382(6) 0.0593(14) Uani 1 1 d . . . C8 C 0.7703(3) -0.2290(3) 0.0842(4) 0.0611(16) Uani 1 1 d . . . H8 H 0.7925 -0.1881 0.0586 0.073 Uiso 1 1 calc R . . C9 C 0.8034(3) -0.2689(3) 0.1667(5) 0.0554(15) Uani 1 1 d . . . C10 C 0.7668(3) -0.3283(3) 0.2096(5) 0.0566(16) Uani 1 1 d . . . C11 C 0.7005(3) -0.3476(3) 0.1664(5) 0.0546(16) Uani 1 1 d . . . C12 C 0.6720(3) -0.3073(3) 0.0790(5) 0.0626(17) Uani 1 1 d . . . H12 H 0.6291 -0.3210 0.0472 0.075 Uiso 1 1 calc R . . C13 C 0.8768(3) -0.2507(3) 0.2014(5) 0.0597(16) Uani 1 1 d . . . C14 C 0.9265(4) -0.2377(3) 0.1167(6) 0.0681(17) Uani 1 1 d . . . H14 H 0.9134 -0.2416 0.0412 0.082 Uiso 1 1 calc R . . C15 C 0.9943(4) -0.2194(4) 0.1439(7) 0.087(2) Uani 1 1 d . . . H15 H 1.0264 -0.2090 0.0867 0.104 Uiso 1 1 calc R . . C16 C 1.0156(4) -0.2161(4) 0.2545(8) 0.096(2) Uani 1 1 d . . . H16 H 1.0622 -0.2046 0.2721 0.116 Uiso 1 1 calc R . . C17 C 0.9682(5) -0.2298(4) 0.3386(7) 0.095(2) Uani 1 1 d . . . H17 H 0.9830 -0.2281 0.4135 0.114 Uiso 1 1 calc R . . C18 C 0.8985(4) -0.2461(3) 0.3139(6) 0.0737(18) Uani 1 1 d . . . H18 H 0.8663 -0.2539 0.3719 0.088 Uiso 1 1 calc R . . C19 C 0.6622(3) -0.4110(3) 0.2087(5) 0.0614(17) Uani 1 1 d . . . C20 C 0.6511(3) -0.4222(4) 0.3222(5) 0.0713(19) Uani 1 1 d . . . H20 H 0.6691 -0.3899 0.3741 0.086 Uiso 1 1 calc R . . C21 C 0.6139(4) -0.4804(5) 0.3607(7) 0.093(2) Uani 1 1 d . . . H21 H 0.6056 -0.4859 0.4376 0.112 Uiso 1 1 calc R . . C22 C 0.5894(4) -0.5292(5) 0.2870(8) 0.101(3) Uani 1 1 d . . . H22 H 0.5661 -0.5694 0.3130 0.121 Uiso 1 1 calc R . . C23 C 0.5994(4) -0.5189(4) 0.1733(7) 0.099(2) Uani 1 1 d . . . H23 H 0.5816 -0.5516 0.1219 0.118 Uiso 1 1 calc R . . C24 C 0.6355(4) -0.4607(4) 0.1350(6) 0.083(2) Uani 1 1 d . . . H24 H 0.6420 -0.4546 0.0578 0.099 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 0.0571(5) 0.0437(5) 0.0430(4) 0.000 0.000 -0.0041(4) I1 0.0714(3) 0.0619(2) 0.0618(2) 0.0013(2) 0.0150(2) -0.01174(19) O1 0.060(3) 0.073(3) 0.067(3) 0.016(2) -0.006(3) 0.009(3) N1 0.058(3) 0.045(3) 0.042(3) 0.000(2) -0.002(2) -0.004(2) N2 0.061(3) 0.081(3) 0.062(3) 0.008(3) -0.008(3) 0.007(3) C1 0.074(4) 0.049(4) 0.058(4) -0.002(3) -0.011(3) -0.005(3) C2 0.077(4) 0.044(3) 0.067(4) 0.004(3) -0.006(4) -0.008(3) C3 0.051(3) 0.051(4) 0.057(4) 0.013(3) 0.002(3) 0.003(3) C4 0.068(4) 0.076(5) 0.054(4) 0.002(4) -0.015(3) -0.013(4) C5 0.079(4) 0.056(4) 0.059(4) 0.012(3) -0.015(4) -0.018(3) C6 0.073(4) 0.060(4) 0.060(4) 0.009(3) -0.002(4) 0.003(3) C7 0.058(4) 0.066(4) 0.053(4) 0.011(4) -0.001(3) 0.014(3) C8 0.064(4) 0.054(4) 0.066(4) 0.005(3) 0.001(3) 0.011(3) C9 0.058(4) 0.054(4) 0.053(4) -0.001(3) 0.003(3) 0.012(3) C10 0.062(4) 0.064(4) 0.044(3) 0.001(3) -0.001(3) 0.021(4) C11 0.050(4) 0.068(4) 0.046(3) 0.004(3) 0.003(3) 0.018(3) C12 0.051(4) 0.075(4) 0.061(4) 0.002(3) 0.000(3) 0.009(3) C13 0.064(4) 0.048(4) 0.068(4) 0.000(3) -0.011(4) 0.010(3) C14 0.066(5) 0.060(4) 0.078(4) 0.006(3) -0.003(4) -0.009(3) C15 0.082(5) 0.074(5) 0.104(6) 0.013(4) -0.010(5) -0.014(4) C16 0.086(6) 0.074(5) 0.129(7) 0.010(5) -0.032(6) -0.017(4) C17 0.108(7) 0.081(5) 0.094(6) -0.014(5) -0.041(5) 0.001(5) C18 0.082(5) 0.070(5) 0.069(5) -0.005(3) -0.005(4) 0.011(4) C19 0.047(3) 0.077(5) 0.061(4) 0.005(4) 0.004(3) 0.008(3) C20 0.064(4) 0.085(5) 0.065(5) 0.014(4) 0.003(3) 0.003(4) C21 0.078(5) 0.118(7) 0.084(6) 0.031(5) 0.015(4) 0.009(5) C22 0.080(6) 0.087(6) 0.135(8) 0.021(6) 0.014(6) -0.005(5) C23 0.074(5) 0.095(6) 0.127(7) -0.008(6) 0.006(5) -0.012(5) C24 0.073(5) 0.098(6) 0.077(5) -0.001(5) 0.008(4) -0.004(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 Zn1 N1 2.067(4) 2_655 ? Zn1 N1 2.067(4) . ? Zn1 I1 2.5520(5) 2_655 ? Zn1 I1 2.5520(5) . ? O1 C10 1.361(7) . ? N1 C1 1.332(7) . ? N1 C5 1.330(6) . ? N2 C6 1.228(7) . ? N2 C7 1.425(7) . ? C1 C2 1.372(8) . ? C2 C3 1.362(8) . ? C3 C4 1.369(8) . ? C3 C6 1.483(8) . ? C4 C5 1.387(7) . ? C7 C8 1.381(8) . ? C7 C12 1.387(8) . ? C8 C9 1.383(7) . ? C9 C10 1.414(8) . ? C9 C13 1.487(8) . ? C10 C11 1.402(8) . ? C11 C12 1.392(8) . ? C11 C19 1.488(8) . ? C13 C18 1.397(8) . ? C13 C14 1.396(8) . ? C14 C15 1.366(9) . ? C15 C16 1.372(9) . ? C16 C17 1.364(10) . ? C17 C18 1.385(10) . ? C19 C20 1.376(8) . ? C19 C24 1.377(9) . ? C20 C21 1.384(10) . ? C21 C22 1.352(10) . ? C22 C23 1.374(10) . ? C23 C24 1.372(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 106.5(3) 2_655 . ? N1 Zn1 I1 105.49(13) 2_655 2_655 ? N1 Zn1 I1 105.19(13) . 2_655 ? N1 Zn1 I1 105.19(13) 2_655 . ? N1 Zn1 I1 105.49(13) . . ? I1 Zn1 I1 127.54(4) 2_655 . ? C1 N1 C5 117.9(5) . . ? C1 N1 Zn1 123.7(4) . . ? C5 N1 Zn1 118.4(4) . . ? C6 N2 C7 121.6(5) . . ? N1 C1 C2 123.1(6) . . ? C3 C2 C1 119.4(5) . . ? C2 C3 C4 118.0(5) . . ? C2 C3 C6 121.7(5) . . ? C4 C3 C6 120.2(6) . . ? C3 C4 C5 120.0(5) . . ? N1 C5 C4 121.6(5) . . ? N2 C6 C3 121.3(6) . . ? C8 C7 C12 118.3(6) . . ? C8 C7 N2 115.9(5) . . ? C12 C7 N2 125.8(6) . . ? C7 C8 C9 122.8(6) . . ? C8 C9 C10 117.7(6) . . ? C8 C9 C13 119.4(6) . . ? C10 C9 C13 122.7(5) . . ? O1 C10 C11 116.4(6) . . ? O1 C10 C9 122.7(6) . . ? C11 C10 C9 120.8(5) . . ? C12 C11 C10 118.4(6) . . ? C12 C11 C19 120.1(6) . . ? C10 C11 C19 121.4(5) . . ? C7 C12 C11 121.8(6) . . ? C18 C13 C14 118.4(6) . . ? C18 C13 C9 123.6(6) . . ? C14 C13 C9 118.1(6) . . ? C15 C14 C13 120.5(6) . . ? C14 C15 C16 120.8(8) . . ? C17 C16 C15 119.7(8) . . ? C16 C17 C18 120.8(7) . . ? C17 C18 C13 119.7(7) . . ? C20 C19 C24 117.3(6) . . ? C20 C19 C11 121.8(6) . . ? C24 C19 C11 120.9(6) . . ? C19 C20 C21 121.4(7) . . ? C22 C21 C20 120.3(8) . . ? C21 C22 C23 119.2(8) . . ? C22 C23 C24 120.4(8) . . ? C23 C24 C19 121.3(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.338 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.053