Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 207 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Alessia Bacchi' _publ_contact_author_address ; Department of General Chemistry University of Parma Parma I-43100 ITALY ; _publ_contact_author_email ALESSIA.BACCHI@UNIPR.IT _publ_section_title ; Unusual hydrogen bonded (OH)4 tetrahedral nests organize zinc(II) coordination complexes in a non covalent diamandoid network ; loop_ _publ_author_name 'Alessia Bacchi' 'Elsa Bosetti' 'Mauro Carcelli' data_zncl2 _database_code_depnum_ccdc_archive 'CCDC 623768' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Cl2 N2 O2 Zn' _chemical_formula_weight 658.89 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' Cl Cl 0.1484 0.1585 '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 Tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' 'y+1/2, x+1/2, z+1/2' _cell_length_a 15.748(3) _cell_length_b 15.748(3) _cell_length_c 12.706(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3151.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 5 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Philips PW1100 diffractometer' _diffrn_measurement_method '\q/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2582 _diffrn_reflns_av_R_equivalents 0.1006 _diffrn_reflns_av_sigmaI/netI 0.1298 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 23.55 _reflns_number_total 1332 _reflns_number_gt 742 _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^)+(0.0512P)^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 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 0.49(6) _refine_ls_number_reflns 1332 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _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 Zn Zn 0.0000 0.5000 0.17036(14) 0.0482(5) Uani 1 2 d S . . Cl Cl 0.06840(16) 0.40336(16) 0.0736(2) 0.0520(8) Uani 1 1 d . . . N N -0.0854(5) 0.4404(5) 0.2671(7) 0.037(2) Uani 1 1 d . . . O O -0.3303(5) 0.2652(6) 0.3533(6) 0.044(2) Uani 1 1 d . . . C1 C -0.2683(6) 0.2854(6) 0.4323(9) 0.038(3) Uani 1 1 d . . . C2 C -0.2040(7) 0.3399(6) 0.3752(8) 0.036(3) Uani 1 1 d . . . C3 C -0.2267(7) 0.3943(7) 0.2970(8) 0.043(3) Uani 1 1 d . . . H3 H -0.2836 0.3984 0.2783 0.052 Uiso 1 1 calc R . . C4 C -0.1674(7) 0.4441(7) 0.2440(9) 0.048(3) Uani 1 1 d . . . H4 H -0.1858 0.4806 0.1912 0.058 Uiso 1 1 calc R . . C5 C -0.0613(7) 0.3893(6) 0.3484(9) 0.046(3) Uani 1 1 d . . . H5 H -0.0045 0.3891 0.3688 0.055 Uiso 1 1 calc R . . C6 C -0.1165(6) 0.3389(6) 0.4007(8) 0.045(3) Uani 1 1 d . . . H6 H -0.0969 0.3033 0.4537 0.054 Uiso 1 1 calc R . . C7 C -0.2301(6) 0.2014(7) 0.4715(8) 0.036(3) Uani 1 1 d . . . C8 C -0.2001(7) 0.1431(7) 0.3994(9) 0.045(3) Uani 1 1 d . . . H8 H -0.2008 0.1565 0.3281 0.054 Uiso 1 1 calc R . . C9 C -0.1686(7) 0.0645(7) 0.4318(10) 0.051(3) Uani 1 1 d . . . H9 H -0.1495 0.0258 0.3817 0.061 Uiso 1 1 calc R . . C10 C -0.1656(8) 0.0437(7) 0.5358(9) 0.055(4) Uani 1 1 d . . . H10 H -0.1454 -0.0089 0.5579 0.066 Uiso 1 1 calc R . . C11 C -0.1938(8) 0.1035(7) 0.6075(9) 0.059(4) Uani 1 1 d . . . H11 H -0.1906 0.0909 0.6789 0.071 Uiso 1 1 calc R . . C12 C -0.2259(7) 0.1795(6) 0.5778(9) 0.048(3) Uani 1 1 d . . . H12 H -0.2453 0.2173 0.6286 0.058 Uiso 1 1 calc R . . C13 C -0.3093(7) 0.3382(7) 0.5207(8) 0.037(3) Uani 1 1 d . . . C14 C -0.2617(7) 0.3890(6) 0.5853(9) 0.042(3) Uani 1 1 d . . . H14 H -0.2029 0.3900 0.5778 0.050 Uiso 1 1 calc R . . C15 C -0.3001(8) 0.4392(7) 0.6624(10) 0.053(3) Uani 1 1 d . . . H15 H -0.2672 0.4740 0.7052 0.064 Uiso 1 1 calc R . . C16 C -0.3852(8) 0.4372(8) 0.6746(10) 0.059(3) Uani 1 1 d . . . H16 H -0.4107 0.4699 0.7267 0.070 Uiso 1 1 calc R . . C17 C -0.4340(7) 0.3873(9) 0.6109(9) 0.065(4) Uani 1 1 d . . . H17 H -0.4927 0.3876 0.6181 0.078 Uiso 1 1 calc R . . C18 C -0.3963(8) 0.3367(7) 0.5362(9) 0.054(4) Uani 1 1 d . . . H18 H -0.4298 0.3009 0.4954 0.065 Uiso 1 1 calc R . . H1O H -0.361(7) 0.236(7) 0.375(10) 0.07(5) Uiso 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 Zn 0.0464(14) 0.0477(14) 0.0506(9) 0.000 0.000 -0.0042(10) Cl 0.0531(18) 0.0452(16) 0.0576(17) -0.0077(17) 0.0009(18) 0.0132(14) N 0.028(5) 0.042(5) 0.042(5) 0.000(5) -0.003(5) -0.018(4) O 0.039(5) 0.060(6) 0.034(5) 0.007(4) -0.005(4) -0.015(5) C1 0.043(6) 0.038(6) 0.034(6) 0.009(6) -0.005(6) -0.006(5) C2 0.044(7) 0.033(6) 0.032(6) 0.002(5) -0.002(5) -0.007(5) C3 0.037(7) 0.048(7) 0.045(7) 0.012(6) -0.016(6) -0.004(6) C4 0.054(8) 0.046(7) 0.044(7) 0.015(7) -0.006(7) -0.003(7) C5 0.031(6) 0.048(7) 0.058(8) -0.004(7) -0.010(6) -0.006(5) C6 0.047(7) 0.048(7) 0.039(8) 0.007(6) -0.011(6) -0.008(5) C7 0.031(6) 0.038(7) 0.038(7) -0.003(6) -0.002(5) -0.012(6) C8 0.047(7) 0.054(8) 0.033(7) 0.002(6) 0.012(6) 0.005(6) C9 0.059(8) 0.042(7) 0.051(8) -0.009(7) 0.005(7) -0.002(6) C10 0.068(9) 0.035(7) 0.062(9) 0.017(7) 0.001(8) -0.002(6) C11 0.100(10) 0.049(8) 0.027(7) 0.015(6) 0.002(7) -0.011(8) C12 0.074(8) 0.029(6) 0.042(7) 0.003(7) -0.002(8) -0.003(6) C13 0.044(7) 0.038(7) 0.030(7) 0.011(6) -0.005(6) -0.002(6) C14 0.048(7) 0.042(7) 0.036(7) 0.001(7) -0.004(7) 0.007(6) C15 0.070(9) 0.040(7) 0.050(7) -0.001(7) -0.006(8) -0.003(6) C16 0.064(9) 0.062(9) 0.050(8) 0.005(8) 0.012(8) 0.014(7) C17 0.029(6) 0.108(11) 0.058(9) -0.010(9) 0.006(7) -0.005(8) C18 0.052(8) 0.059(8) 0.050(8) -0.016(7) 0.003(7) -0.014(7) _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 Zn N 2.050(8) 3_565 ? Zn N 2.050(8) . ? Zn Cl 2.233(3) . ? Zn Cl 2.233(3) 3_565 ? N C4 1.326(11) . ? N C5 1.363(12) . ? O C1 1.436(12) . ? C1 C2 1.513(13) . ? C1 C7 1.536(12) . ? C1 C13 1.539(14) . ? C2 C3 1.360(13) . ? C2 C6 1.415(13) . ? C3 C4 1.392(14) . ? C5 C6 1.352(14) . ? C7 C8 1.380(13) . ? C7 C12 1.396(14) . ? C8 C9 1.396(14) . ? C9 C10 1.363(14) . ? C10 C11 1.383(14) . ? C11 C12 1.353(14) . ? C13 C14 1.370(12) . ? C13 C18 1.384(14) . ? C14 C15 1.398(14) . ? C15 C16 1.348(15) . ? C16 C17 1.365(15) . ? C17 C18 1.374(15) . ? 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 N Zn N 106.3(5) 3_565 . ? N Zn Cl 109.0(3) 3_565 . ? N Zn Cl 109.5(3) . . ? N Zn Cl 109.5(3) 3_565 3_565 ? N Zn Cl 109.0(3) . 3_565 ? Cl Zn Cl 113.21(17) . 3_565 ? C4 N C5 117.8(9) . . ? C4 N Zn 119.1(8) . . ? C5 N Zn 122.8(7) . . ? O C1 C2 104.2(9) . . ? O C1 C7 107.6(8) . . ? C2 C1 C7 112.4(8) . . ? O C1 C13 110.2(8) . . ? C2 C1 C13 109.0(8) . . ? C7 C1 C13 113.2(9) . . ? C3 C2 C6 115.5(10) . . ? C3 C2 C1 122.1(10) . . ? C6 C2 C1 122.4(9) . . ? C2 C3 C4 122.2(10) . . ? N C4 C3 121.4(10) . . ? C6 C5 N 122.6(10) . . ? C5 C6 C2 120.5(10) . . ? C8 C7 C12 117.5(10) . . ? C8 C7 C1 119.5(9) . . ? C12 C7 C1 123.0(10) . . ? C7 C8 C9 121.1(11) . . ? C10 C9 C8 120.8(12) . . ? C9 C10 C11 117.6(11) . . ? C12 C11 C10 122.6(11) . . ? C11 C12 C7 120.4(11) . . ? C14 C13 C18 117.8(11) . . ? C14 C13 C1 121.5(10) . . ? C18 C13 C1 120.7(10) . . ? C13 C14 C15 120.9(11) . . ? C16 C15 C14 119.9(12) . . ? C15 C16 C17 120.3(13) . . ? C16 C17 C18 120.0(12) . . ? C17 C18 C13 121.0(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.55 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.266 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.064 #===END data_znbr2 _database_code_depnum_ccdc_archive 'CCDC 623769' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Br2 N2 O2 Zn' _chemical_formula_weight 747.81 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 tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' 'y+1/2, x+1/2, z+1/2' _cell_length_a 15.9400(10) _cell_length_b 15.9400(10) _cell_length_c 12.604(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3202(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 3.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.518 _exptl_absorpt_correction_T_max 0.696 _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 'Bruker AXS CCD 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 22605 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 21.97 _reflns_number_total 1958 _reflns_number_gt 1774 _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^)+(0.0256P)^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 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 0.156(9) _refine_ls_number_reflns 1958 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0415 _refine_ls_wR_factor_gt 0.0404 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 Zn1 Zn 0.0000 0.5000 0.83071(4) 0.03644(14) Uani 1 2 d S . . Br1 Br -0.10008(2) 0.56984(2) 0.93653(3) 0.05339(12) Uani 1 1 d . . . N1 N 0.05789(16) 0.58444(15) 0.7330(2) 0.0374(7) Uani 1 1 d . . . O1 O 0.23059(16) 0.82504(15) 0.6490(2) 0.0467(7) Uani 1 1 d . . . C1 C 0.21138(18) 0.76475(18) 0.5673(3) 0.0380(8) Uani 1 1 d . . . C2 C 0.15707(19) 0.69949(19) 0.6242(2) 0.0345(8) Uani 1 1 d . . . C3 C 0.15950(19) 0.6152(2) 0.6013(3) 0.0421(9) Uani 1 1 d . . . H3 H 0.1952 0.5955 0.5485 0.050 Uiso 1 1 calc R . . C4 C 0.1094(2) 0.5599(2) 0.6562(3) 0.0444(8) Uani 1 1 d . . . H4 H 0.1118 0.5032 0.6389 0.053 Uiso 1 1 calc R . . C5 C 0.0538(2) 0.6664(2) 0.7536(3) 0.0470(9) Uani 1 1 d . . . H5 H 0.0167 0.6848 0.8056 0.056 Uiso 1 1 calc R . . C6 C 0.1011(2) 0.7243(2) 0.7020(3) 0.0456(10) Uani 1 1 d . . . H6 H 0.0959 0.7808 0.7190 0.055 Uiso 1 1 calc R . . C7 C 0.15918(19) 0.8063(2) 0.4794(2) 0.0358(8) Uani 1 1 d . . . C8 C 0.1084(2) 0.7599(2) 0.4136(3) 0.0449(9) Uani 1 1 d . . . H8 H 0.1065 0.7019 0.4210 0.054 Uiso 1 1 calc R . . C9 C 0.0600(2) 0.7983(2) 0.3370(3) 0.0530(9) Uani 1 1 d . . . H9 H 0.0271 0.7657 0.2922 0.064 Uiso 1 1 calc R . . C10 C 0.0598(2) 0.8833(2) 0.3256(3) 0.0569(10) Uani 1 1 d . . . H10 H 0.0258 0.9088 0.2752 0.068 Uiso 1 1 calc R . . C11 C 0.1107(3) 0.9305(2) 0.3902(3) 0.0621(11) Uani 1 1 d . . . H11 H 0.1119 0.9885 0.3827 0.075 Uiso 1 1 calc R . . C12 C 0.1601(2) 0.8923(2) 0.4660(3) 0.0549(10) Uani 1 1 d . . . H12 H 0.1945 0.9250 0.5088 0.066 Uiso 1 1 calc R . . C13 C 0.2942(2) 0.72675(19) 0.5274(2) 0.0385(9) Uani 1 1 d . . . C14 C 0.3520(2) 0.69840(19) 0.6010(3) 0.0458(9) Uani 1 1 d . . . H14 H 0.3385 0.7002 0.6727 0.055 Uiso 1 1 calc R . . C15 C 0.4287(2) 0.6677(2) 0.5708(3) 0.0537(9) Uani 1 1 d . . . H15 H 0.4664 0.6486 0.6218 0.064 Uiso 1 1 calc R . . C16 C 0.4499(2) 0.6653(2) 0.4655(3) 0.0587(11) Uani 1 1 d . . . H16 H 0.5025 0.6460 0.4447 0.070 Uiso 1 1 calc R . . C17 C 0.3933(2) 0.6914(2) 0.3913(3) 0.0616(11) Uani 1 1 d . . . H17 H 0.4069 0.6881 0.3197 0.074 Uiso 1 1 calc R . . C18 C 0.3154(2) 0.7230(2) 0.4218(3) 0.0492(9) Uani 1 1 d . . . H18 H 0.2776 0.7415 0.3706 0.059 Uiso 1 1 calc R . . H100 H 0.2685(19) 0.849(2) 0.629(3) 0.042(12) Uiso 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 0.0323(3) 0.0323(3) 0.0447(3) 0.000 0.000 -0.0046(2) Br1 0.0418(2) 0.0526(2) 0.0658(2) -0.0020(2) 0.0048(2) 0.01167(16) N1 0.0384(16) 0.0326(18) 0.0411(16) -0.0016(13) 0.0013(14) -0.0045(13) O1 0.0500(16) 0.0475(16) 0.0425(16) -0.0083(13) 0.0060(14) -0.0208(14) C1 0.0415(18) 0.0350(18) 0.0375(19) -0.0072(19) 0.0007(19) -0.0085(15) C2 0.0356(19) 0.033(2) 0.0344(19) -0.0004(15) -0.0020(16) -0.0061(15) C3 0.042(2) 0.043(2) 0.041(2) -0.0087(17) 0.0107(16) -0.0063(16) C4 0.050(2) 0.036(2) 0.048(2) -0.0073(18) 0.002(2) -0.0070(18) C5 0.045(2) 0.043(2) 0.053(2) 0.0000(18) 0.0172(19) -0.0014(18) C6 0.048(2) 0.031(2) 0.058(2) -0.0030(17) 0.016(2) -0.0027(19) C7 0.0349(19) 0.037(2) 0.035(2) 0.0007(16) 0.0061(16) -0.0046(17) C8 0.0458(19) 0.0387(19) 0.050(3) -0.007(2) -0.004(2) -0.0005(17) C9 0.044(2) 0.064(3) 0.051(2) -0.008(2) -0.006(2) -0.001(2) C10 0.053(2) 0.066(3) 0.052(2) 0.010(2) 0.002(2) 0.012(2) C11 0.081(3) 0.039(2) 0.067(3) 0.006(2) -0.003(2) 0.003(2) C12 0.063(2) 0.044(2) 0.058(3) -0.001(2) -0.010(2) -0.009(2) C13 0.0342(19) 0.037(2) 0.045(2) 0.0029(17) 0.0050(18) -0.0127(16) C14 0.049(2) 0.044(2) 0.044(2) 0.0081(17) -0.0017(19) -0.0071(19) C15 0.043(2) 0.052(2) 0.066(3) 0.008(2) -0.014(2) 0.0000(18) C16 0.035(2) 0.064(3) 0.077(3) 0.003(2) 0.013(2) 0.0002(19) C17 0.047(2) 0.087(3) 0.051(3) 0.003(2) 0.011(2) 0.005(2) C18 0.038(2) 0.070(2) 0.039(2) -0.001(2) 0.002(2) -0.0034(17) _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 2.044(3) 3_565 ? Zn1 N1 2.044(3) . ? Zn1 Br1 2.3586(7) . ? Zn1 Br1 2.3586(7) 3_565 ? N1 C4 1.329(4) . ? N1 C5 1.334(4) . ? O1 C1 1.441(4) . ? C1 C2 1.531(4) . ? C1 C13 1.537(4) . ? C1 C7 1.536(4) . ? C2 C6 1.383(4) . ? C2 C3 1.374(4) . ? C3 C4 1.376(4) . ? C5 C6 1.357(4) . ? C7 C12 1.382(4) . ? C7 C8 1.374(4) . ? C8 C9 1.379(5) . ? C9 C10 1.361(5) . ? C10 C11 1.374(5) . ? C11 C12 1.379(5) . ? C13 C18 1.375(4) . ? C13 C14 1.383(4) . ? C14 C15 1.371(4) . ? C15 C16 1.371(5) . ? C16 C17 1.364(5) . ? C17 C18 1.395(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 105.93(16) 3_565 . ? N1 Zn1 Br1 110.24(7) 3_565 . ? N1 Zn1 Br1 109.58(8) . . ? N1 Zn1 Br1 109.58(8) 3_565 3_565 ? N1 Zn1 Br1 110.24(7) . 3_565 ? Br1 Zn1 Br1 111.13(5) . 3_565 ? C4 N1 C5 117.4(3) . . ? C4 N1 Zn1 121.6(2) . . ? C5 N1 Zn1 120.4(2) . . ? O1 C1 C2 103.8(3) . . ? O1 C1 C13 108.3(2) . . ? C2 C1 C13 111.8(2) . . ? O1 C1 C7 110.1(2) . . ? C2 C1 C7 108.9(2) . . ? C13 C1 C7 113.5(3) . . ? C6 C2 C3 116.5(3) . . ? C6 C2 C1 120.2(3) . . ? C3 C2 C1 123.4(3) . . ? C4 C3 C2 120.3(3) . . ? N1 C4 C3 122.4(3) . . ? N1 C5 C6 123.0(3) . . ? C5 C6 C2 120.3(3) . . ? C12 C7 C8 117.8(3) . . ? C12 C7 C1 120.7(3) . . ? C8 C7 C1 121.5(3) . . ? C9 C8 C7 120.9(3) . . ? C10 C9 C8 121.1(3) . . ? C9 C10 C11 118.8(4) . . ? C10 C11 C12 120.3(4) . . ? C7 C12 C11 121.1(3) . . ? C18 C13 C14 118.2(3) . . ? C18 C13 C1 123.0(3) . . ? C14 C13 C1 118.8(3) . . ? C15 C14 C13 121.6(3) . . ? C14 C15 C16 119.9(3) . . ? C17 C16 C15 119.5(3) . . ? C16 C17 C18 120.7(4) . . ? C13 C18 C17 120.0(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.249 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.035 #===END data_zni2bis _database_code_depnum_ccdc_archive 'CCDC 623770' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 I2 N2 O2 Zn' _chemical_formula_weight 841.79 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' I I -0.4742 1.8119 '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 tetragonal _symmetry_space_group_name_H-M 'I -42 d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, -z+1/4' '-x, -y, z' '-x, y+1/2, -z+1/4' '-y+1/2, -x, z+3/4' '-y, x, -z' 'y, -x, -z' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1, -z+3/4' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1, -z+3/4' '-y+1, -x+1/2, z+5/4' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'y+1, x+1/2, z+5/4' _cell_length_a 21.9230(10) _cell_length_b 21.9230(10) _cell_length_c 14.7289(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7079.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 2.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.884 _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 'BRUKER AXS CCD 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 23425 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 21.27 _reflns_number_total 1984 _reflns_number_gt 1784 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(10) _refine_ls_number_reflns 1984 _refine_ls_number_parameters 160 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0989 _refine_ls_wR_factor_ref 0.2922 _refine_ls_wR_factor_gt 0.2787 _refine_ls_goodness_of_fit_ref 1.403 _refine_ls_restrained_S_all 1.408 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.005 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 Zn Zn -0.09404(14) 0.2500 0.1250 0.0676(9) Uani 1 2 d S . . O1 O 0.0411(7) 0.0452(7) 0.4203(11) 0.086(4) Uani 1 1 d U . . H1 H 0.0606 0.0179 0.4450 0.129 Uiso 1 1 calc R . . I1 I -0.15340(7) 0.31774(7) 0.23548(10) 0.0904(7) Uani 1 1 d . . . C1 C 0.0827(8) 0.0842(8) 0.3672(12) 0.059(4) Uani 1 1 d U . . C2 C 0.0409(5) 0.1257(5) 0.3057(9) 0.051(4) Uani 1 1 d GU . . C3 C 0.0542(6) 0.1870(6) 0.2919(11) 0.130(9) Uani 1 1 d GU . . H3 H 0.0885 0.2043 0.3187 0.156 Uiso 1 1 calc R . . C4 C 0.0161(7) 0.2225(4) 0.2379(12) 0.132(9) Uani 1 1 d GU . . H4 H 0.0250 0.2635 0.2286 0.159 Uiso 1 1 calc R . . N1 N -0.0351(5) 0.1967(5) 0.1978(9) 0.067(4) Uani 1 1 d GU . . C5 C -0.0484(7) 0.1354(6) 0.2116(12) 0.142(10) Uani 1 1 d GU . . H5 H -0.0827 0.1182 0.1848 0.171 Uiso 1 1 calc R . . C6 C -0.0104(7) 0.0999(4) 0.2656(13) 0.117(7) Uani 1 1 d GU . . H6 H -0.0193 0.0589 0.2748 0.140 Uiso 1 1 calc R . . C7 C 0.1230(7) 0.1206(7) 0.4290(10) 0.066(4) Uani 1 1 d GU . . C8 C 0.1369(11) 0.1818(7) 0.4152(17) 0.173(12) Uani 1 1 d GU . . H8 H 0.1149 0.2045 0.3732 0.208 Uiso 1 1 calc R . . C9 C 0.1838(14) 0.2090(8) 0.464(2) 0.194(14) Uani 1 1 d GU . . H9 H 0.1931 0.2499 0.4550 0.233 Uiso 1 1 calc R . . C10 C 0.2167(11) 0.1750(11) 0.5270(18) 0.175(12) Uani 1 1 d GU . . H10 H 0.2481 0.1932 0.5598 0.210 Uiso 1 1 calc R . . C11 C 0.2028(9) 0.1139(11) 0.5408(14) 0.145(10) Uani 1 1 d GU . . H11 H 0.2249 0.0911 0.5828 0.173 Uiso 1 1 calc R . . C12 C 0.1560(9) 0.0867(7) 0.4918(13) 0.131(8) Uani 1 1 d GU . . H12 H 0.1467 0.0457 0.5010 0.158 Uiso 1 1 calc R . . C13 C 0.1152(7) 0.0411(6) 0.3151(11) 0.081(6) Uani 1 1 d GU . . C14 C 0.1394(11) -0.0100(9) 0.3578(12) 0.127(9) Uani 1 1 d GU . . H14 H 0.1309 -0.0175 0.4186 0.153 Uiso 1 1 calc R . . C15 C 0.1765(13) -0.0500(10) 0.3095(19) 0.184(13) Uani 1 1 d GU . . H15 H 0.1927 -0.0842 0.3380 0.220 Uiso 1 1 calc R . . C16 C 0.1892(13) -0.0389(11) 0.219(2) 0.201(14) Uani 1 1 d GU . . H16 H 0.2140 -0.0656 0.1862 0.241 Uiso 1 1 calc R . . C17 C 0.1650(15) 0.0122(12) 0.1759(14) 0.197(14) Uani 1 1 d GU . . H17 H 0.1735 0.0197 0.1150 0.236 Uiso 1 1 calc R . . C18 C 0.1279(11) 0.0522(8) 0.2241(12) 0.152(10) Uani 1 1 d GU . . H18 H 0.1117 0.0864 0.1956 0.182 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 Zn 0.0793(18) 0.0637(17) 0.0598(18) 0.0217(13) 0.000 0.000 O1 0.097(9) 0.079(8) 0.083(9) 0.044(7) -0.002(8) -0.024(7) I1 0.1013(11) 0.0912(10) 0.0788(10) 0.0093(7) 0.0165(7) 0.0058(7) C1 0.055(8) 0.062(8) 0.061(9) 0.026(8) 0.000(7) -0.005(7) C2 0.071(9) 0.049(8) 0.034(7) 0.026(6) -0.006(7) -0.012(7) C3 0.128(17) 0.15(2) 0.110(18) 0.065(16) -0.004(15) -0.017(16) C4 0.110(16) 0.143(19) 0.15(2) 0.048(18) 0.005(17) 0.023(15) N1 0.091(10) 0.059(8) 0.049(7) 0.019(6) -0.006(7) -0.004(7) C5 0.142(19) 0.16(2) 0.126(19) 0.065(17) -0.012(16) -0.043(17) C6 0.106(15) 0.112(16) 0.132(18) 0.021(16) -0.015(15) 0.001(14) C7 0.074(10) 0.063(9) 0.060(10) 0.017(8) -0.022(8) -0.014(8) C8 0.19(2) 0.18(2) 0.15(2) 0.02(2) -0.06(2) -0.06(2) C9 0.22(3) 0.17(2) 0.19(3) -0.01(2) -0.07(2) -0.09(2) C10 0.21(3) 0.15(2) 0.16(2) 0.02(2) -0.08(2) -0.06(2) C11 0.15(2) 0.18(2) 0.105(18) 0.014(18) -0.015(16) -0.054(19) C12 0.142(19) 0.15(2) 0.100(17) 0.019(17) -0.001(16) -0.022(17) C13 0.090(11) 0.056(9) 0.097(13) 0.021(10) -0.036(11) -0.030(9) C14 0.15(2) 0.135(18) 0.099(16) 0.027(16) -0.017(16) 0.034(17) C15 0.20(3) 0.15(2) 0.20(3) 0.03(2) 0.00(3) 0.10(2) C16 0.23(3) 0.16(2) 0.22(3) 0.06(2) 0.06(3) 0.12(2) C17 0.25(3) 0.16(2) 0.18(3) 0.01(2) 0.09(2) 0.06(2) C18 0.18(2) 0.121(18) 0.15(2) 0.032(19) 0.04(2) -0.002(18) _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 Zn N1 2.045(16) 2 ? Zn N1 2.045(8) . ? Zn I1 2.559(2) 2 ? Zn I1 2.559(2) . ? O1 C1 1.48(2) . ? C1 C13 1.41(2) . ? C1 C7 1.50(2) . ? C1 C2 1.578(19) . ? C2 C3 1.3900 . ? C2 C6 1.3900 . ? C3 C4 1.3900 . ? C4 N1 1.3900 . ? N1 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 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 Zn N1 101.7(11) 2 . ? N1 Zn I1 108.6(11) 2 2 ? N1 Zn I1 108.9(4) . 2 ? N1 Zn I1 108.9(10) 2 . ? N1 Zn I1 108.6(4) . . ? I1 Zn I1 118.86(14) 2 . ? C13 C1 O1 102.2(14) . . ? C13 C1 C7 113.0(14) . . ? O1 C1 C7 110.6(14) . . ? C13 C1 C2 111.6(14) . . ? O1 C1 C2 106.2(12) . . ? C7 C1 C2 112.6(13) . . ? C3 C2 C6 120.0 . . ? C3 C2 C1 121.4(9) . . ? C6 C2 C1 118.6(9) . . ? C4 C3 C2 120.0 . . ? C3 C4 N1 120.0 . . ? C5 N1 C4 120.0 . . ? C5 N1 Zn 119.8(7) . . ? C4 N1 Zn 120.1(7) . . ? N1 C5 C6 120.0 . . ? C5 C6 C2 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 C1 123.7(12) . . ? C12 C7 C1 115.1(12) . . ? C7 C8 C9 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C12 C11 C10 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 C1 119.2(13) . . ? C18 C13 C1 120.5(13) . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.611 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.264