# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_MAF-4_293K _database_code_depnum_ccdc_archive 'CCDC 893937' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 N4.40 Zn' _chemical_formula_weight 233.17 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.039(3) _cell_length_b 17.039(3) _cell_length_c 17.039(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4946.6(13) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1426 _exptl_absorpt_coefficient_mu 1.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7482 _exptl_absorpt_correction_T_max 0.7580 _exptl_absorpt_process_details SADABS _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 CCD _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9551 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.94 _reflns_number_total 933 _reflns_number_gt 817 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0441P)^2^+0.0951P] 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 0.01(3) _refine_ls_number_reflns 933 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.2500 0.5000 0.0581(3) Uani 1 4 d S . . C1 C 0.12272(14) 0.12272(14) 0.5064(4) 0.0566(11) Uani 1 2 d S . . N1 N 0.08942(16) 0.18257(15) 0.46833(14) 0.0602(7) Uani 1 1 d . . . C2 C 0.1309(2) 0.1868(2) 0.39882(19) 0.0739(10) Uani 1 1 d . . . H2A H 0.1218 0.2225 0.3585 0.089 Uiso 1 1 calc R . . C3 C 0.0941(3) 0.0941(3) 0.5855(3) 0.0806(15) Uani 1 2 d S . . H3A H 0.1219 0.1211 0.6264 0.121 Uiso 1 2 calc SR . . H3B H 0.1034 0.0387 0.5899 0.121 Uiso 0.50 1 calc PR . . H3C H 0.0389 0.1044 0.5903 0.121 Uiso 0.50 1 calc PR . . N41 N 0.0000 0.0000 0.7490(12) 0.084(7) Uiso 0.24 4 d SP . . N31 N 0.2538(19) 0.2538(19) 0.2538(19) 0.090(9) Uiso 0.24 6 d SP . . 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 0.0598(3) 0.0546(4) 0.0598(3) 0.000 0.000 0.000 C1 0.0579(13) 0.0579(13) 0.054(3) -0.001(2) -0.001(2) 0.0007(17) N1 0.0664(16) 0.0580(14) 0.0561(15) 0.0053(11) 0.0028(12) 0.0067(13) C2 0.085(2) 0.078(2) 0.0591(19) 0.0164(17) 0.0108(18) 0.0134(18) C3 0.088(2) 0.088(2) 0.066(3) 0.016(2) 0.016(2) 0.015(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 Zn1 N1 1.983(2) 48 ? Zn1 N1 1.983(2) 3_556 ? Zn1 N1 1.983(2) . ? Zn1 N1 1.983(2) 46_455 ? C1 N1 1.335(4) . ? C1 N1 1.335(4) 13 ? C1 C3 1.512(8) . ? N1 C2 1.382(4) . ? C2 C2 1.346(7) 13 ? 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 109.61(8) 48 3_556 ? N1 Zn1 N1 109.61(8) 48 . ? N1 Zn1 N1 109.19(16) 3_556 . ? N1 Zn1 N1 109.19(16) 48 46_455 ? N1 Zn1 N1 109.61(8) 3_556 46_455 ? N1 Zn1 N1 109.61(8) . 46_455 ? N1 C1 N1 114.4(5) . 13 ? N1 C1 C3 122.8(3) . . ? N1 C1 C3 122.8(3) 13 . ? C1 N1 C2 103.8(4) . . ? C1 N1 Zn1 129.5(3) . . ? C2 N1 Zn1 126.6(2) . . ? C2 C2 N1 108.98(18) 13 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.198 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.056 data_MAF-4_113K _database_code_depnum_ccdc_archive 'CCDC 893938' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 N11 Zn' _chemical_formula_weight 325.64 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.086(2) _cell_length_b 17.086(2) _cell_length_c 17.086(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4987.7(11) _cell_formula_units_Z 12 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7456 _exptl_absorpt_correction_T_max 0.7555 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9596 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.93 _reflns_number_total 940 _reflns_number_gt 918 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0593P)^2^+5.2588P] 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 0.02(3) _refine_ls_number_reflns 940 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.2500 0.5000 0.0218(2) Uani 1 4 d S . . C1 C 0.12287(15) 0.12287(15) 0.5083(4) 0.0219(11) Uani 1 2 d S . . N1 N 0.09054(15) 0.18289(15) 0.46994(15) 0.0238(5) Uani 1 1 d . . . C2 C 0.13218(19) 0.1887(2) 0.40092(19) 0.0290(7) Uani 1 1 d . . . H2A H 0.1231 0.2256 0.3604 0.035 Uiso 1 1 calc R . . C3 C 0.0934(2) 0.0934(2) 0.5856(3) 0.0309(10) Uani 1 2 d S . . H3A H 0.1206 0.1206 0.6281 0.046 Uiso 1 2 calc SR . . H3B H 0.1032 0.0370 0.5896 0.046 Uiso 0.50 1 calc PR . . H3C H 0.0370 0.1032 0.5896 0.046 Uiso 0.50 1 calc PR . . N21 N 0.2872(7) 0.2872(7) 0.5220(9) 0.158(6) Uiso 0.93 2 d SP . . N22 N 0.3406(19) 0.2864(16) 0.484(2) 0.250(15) Uiso 0.47 1 d P . . N31 N 0.2076(7) 0.2076(7) 0.7924(7) 0.105(5) Uiso 1 6 d S . . N32 N 0.2404(6) 0.2404(6) 0.7596(6) 0.048(4) Uiso 0.50 6 d SP A 1 N32' N 0.1796(18) 0.1796(18) 0.8204(18) 0.156(17) Uiso 0.50 6 d SP A 2 N41 N 0.2517(10) 0.5000 0.5000 0.136(7) Uiso 0.80 4 d SP . . N42 N 0.267(5) 0.544(3) 0.456(3) 0.37(4) Uiso 0.40 2 d SP . . N51 N 0.456(3) 0.5000 0.5000 0.21(4) Uiso 0.33 4 d SP . . 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 0.0221(2) 0.0212(3) 0.0221(2) 0.000 0.000 0.000 C1 0.0215(10) 0.0215(10) 0.023(3) -0.0008(14) -0.0008(14) -0.0022(13) N1 0.0252(13) 0.0226(13) 0.0236(12) 0.0001(9) 0.0028(10) 0.0024(10) C2 0.0337(18) 0.0281(17) 0.0253(16) 0.0081(13) 0.0033(13) 0.0061(14) C3 0.0351(15) 0.0351(15) 0.022(2) 0.0068(15) 0.0068(15) 0.010(2) _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 1.993(2) 48 ? Zn1 N1 1.993(2) 46_455 ? Zn1 N1 1.993(2) . ? Zn1 N1 1.993(2) 3_556 ? C1 N1 1.337(4) . ? C1 N1 1.337(4) 13 ? C1 C3 1.501(8) . ? N1 C2 1.381(4) . ? C2 C2 1.365(6) 13 ? N21 N22 1.12(3) 13 ? N21 N22 1.12(3) . ? N22 N22 1.31(6) 13 ? N31 N32' 0.83(5) . ? N31 N32 0.97(2) . ? N41 N42 1.11(7) . ? N41 N42 1.11(7) 4_566 ? N51 N51 1.06(8) 6_566 ? N51 N51 1.06(8) 9 ? N51 N51 1.06(8) 10_656 ? N51 N51 1.06(8) 5 ? N51 N51 1.50(11) 2_665 ? 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 109.75(15) 48 46_455 ? N1 Zn1 N1 109.33(8) 48 . ? N1 Zn1 N1 109.33(8) 46_455 . ? N1 Zn1 N1 109.33(8) 48 3_556 ? N1 Zn1 N1 109.33(8) 46_455 3_556 ? N1 Zn1 N1 109.75(15) . 3_556 ? N1 C1 N1 113.2(5) . 13 ? N1 C1 C3 123.4(2) . . ? N1 C1 C3 123.4(2) 13 . ? C1 N1 C2 105.1(3) . . ? C1 N1 Zn1 129.5(3) . . ? C2 N1 Zn1 125.4(2) . . ? C2 C2 N1 108.29(17) 13 . ? N22 N21 N22 71(3) 13 . ? N21 N22 N22 54.3(17) . 13 ? N32' N31 N32 180(6) . . ? N42 N41 N42 152(9) . 4_566 ? N51 N51 N51 60.000(13) 6_566 9 ? N51 N51 N51 60.000(13) 6_566 10_656 ? N51 N51 N51 90.00(2) 9 10_656 ? N51 N51 N51 90.000(19) 6_566 5 ? N51 N51 N51 60.000(7) 9 5 ? N51 N51 N51 60.000(6) 10_656 5 ? N51 N51 N51 45.000(4) 6_566 2_665 ? N51 N51 N51 45.0 9 2_665 ? N51 N51 N51 45.0 10_656 2_665 ? N51 N51 N51 45.000(4) 5 2_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.495 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.077 data_MAF-4_111K _database_code_depnum_ccdc_archive 'CCDC 893939' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 N11.64 Zn' _chemical_formula_weight 334.61 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.120(2) _cell_length_b 17.120(2) _cell_length_c 17.120(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5018.1(12) _cell_formula_units_Z 12 _cell_measurement_temperature 111(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2034 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7464 _exptl_absorpt_correction_T_max 0.7563 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 111(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7912 _diffrn_reflns_av_R_equivalents 0.1309 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 954 _reflns_number_gt 924 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0805P)^2^+25.5610P] 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 0.04(6) _refine_ls_number_reflns 954 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1586 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.2500 0.5000 0.0183(4) Uani 1 4 d S . . C1 C 0.1270(3) 0.1270(3) 0.5093(8) 0.024(2) Uani 1 2 d S . . N1 N 0.0890(3) 0.1819(3) 0.4679(3) 0.0218(11) Uani 1 1 d . . . C2 C 0.1208(7) 0.1755(7) 0.3956(5) 0.072(3) Uani 1 1 d . . . H2A H 0.1060 0.2058 0.3515 0.087 Uiso 1 1 calc R . . C3 C 0.1091(12) 0.1091(12) 0.5925(9) 0.122(10) Uani 1 2 d S . . H3A H 0.1416 0.1416 0.6265 0.182 Uiso 1 2 calc SR . . H3B H 0.1199 0.0538 0.6029 0.182 Uiso 0.50 1 calc PR . . H3C H 0.0538 0.1199 0.6029 0.182 Uiso 0.50 1 calc PR . . N11 N 0.0000 0.0000 0.5267(15) 0.050(10) Uiso 0.37(4) 4 d SP . . N21 N 0.2745(13) 0.2745(13) 0.4810(17) 0.073(8) Uiso 0.50 2 d SP A 1 N22 N 0.2814(16) 0.2814(16) 0.418(2) 0.094(10) Uiso 0.50 2 d SP A 1 N31 N 0.285(2) 0.285(2) 0.715(2) 0.09(2) Uiso 0.50 6 d SP B 1 N32 N 0.306(3) 0.306(3) 0.694(3) 0.077(16) Uiso 0.50 6 d SP B 1 N21' N 0.290(3) 0.290(3) 0.549(3) 0.128(18) Uiso 0.50 2 d SP C 2 N22' N 0.287(3) 0.337(4) 0.525(3) 0.13(2) Uiso 0.25 1 d P C 2 N31' N 0.179(4) 0.179(4) 0.821(4) 0.14(4) Uiso 0.50 6 d SP D 2 N32' N 0.156(5) 0.156(5) 0.844(5) 0.20(6) Uiso 0.50 6 d SP D 2 N41 N 0.254(2) 0.5000 0.5000 0.150(14) Uiso 0.80 4 d SP . . N42 N 0.282(6) 0.539(4) 0.461(4) 0.27(6) Uiso 0.40 2 d SP . . N51 N 0.479(5) 0.479(5) 0.479(5) 0.21(9) Uiso 0.50 6 d SP . . 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 0.0187(4) 0.0174(6) 0.0187(4) 0.000 0.000 0.000 C1 0.027(2) 0.027(2) 0.017(6) -0.005(3) -0.005(3) 0.008(3) N1 0.024(3) 0.021(2) 0.020(2) 0.0023(18) 0.0014(19) 0.002(2) C2 0.089(7) 0.098(8) 0.030(4) 0.018(5) 0.030(4) 0.066(7) C3 0.156(15) 0.156(15) 0.053(9) 0.054(10) 0.054(10) 0.146(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 1.997(5) 48 ? Zn1 N1 1.997(5) 3_556 ? Zn1 N1 1.997(5) . ? Zn1 N1 1.997(5) 46_455 ? C1 N1 1.346(8) 13 ? C1 N1 1.346(8) . ? C1 C3 1.489(18) . ? N1 C2 1.356(9) . ? C2 C2 1.325(18) 13 ? N11 N11 0.92(5) 3_556 ? N21 N22 1.09(5) . ? N31 N32 0.60(9) . ? N21' N22' 0.89(6) . ? N21' N22' 0.89(6) 13 ? N22' N22' 1.22(11) 13 ? N31' N32' 0.67(19) . ? N41 N42 1.06(10) . ? N41 N42 1.06(10) 4_566 ? N42 N42 1.9(2) 4_566 ? N51 N51 1.0(2) 4_566 ? N51 N51 1.0(2) 2_665 ? N51 N51 1.0(2) 3_656 ? 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 109.94(14) 48 3_556 ? N1 Zn1 N1 109.94(14) 48 . ? N1 Zn1 N1 108.5(3) 3_556 . ? N1 Zn1 N1 108.5(3) 48 46_455 ? N1 Zn1 N1 109.94(14) 3_556 46_455 ? N1 Zn1 N1 109.94(14) . 46_455 ? N1 C1 N1 113.3(11) 13 . ? N1 C1 C3 123.3(5) 13 . ? N1 C1 C3 123.3(5) . . ? C1 N1 C2 103.4(7) . . ? C1 N1 Zn1 129.1(6) . . ? C2 N1 Zn1 127.2(5) . . ? C2 C2 N1 109.9(4) 13 . ? N22' N21' N22' 86(10) . 13 ? N21' N22' N22' 47(5) . 13 ? N42 N41 N42 128(10) . 4_566 ? N41 N42 N42 26(6) . 4_566 ? N51 N51 N51 60.00(2) 4_566 2_665 ? N51 N51 N51 60.000(11) 4_566 3_656 ? N51 N51 N51 60.000(2) 2_665 3_656 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.652 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.120 data_MAF-4_109K _database_code_depnum_ccdc_archive 'CCDC 893940' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 N12.67 Zn' _chemical_formula_weight 348.99 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.1236(19) _cell_length_b 17.1236(19) _cell_length_c 17.1236(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5020.9(10) _cell_formula_units_Z 12 _cell_measurement_temperature 109(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7458 _exptl_absorpt_correction_T_max 0.7557 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 109(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9702 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.99 _reflns_number_total 956 _reflns_number_gt 946 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0538P)^2^+2.5610P] 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 0.00(2) _refine_ls_number_reflns 956 _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.2500 0.5000 0.01364(17) Uani 1 4 d S . . C1 C 0.13224(12) 0.13224(12) 0.5099(3) 0.0158(8) Uani 1 2 d S . . N1 N 0.08842(12) 0.18104(11) 0.46698(11) 0.0148(4) Uani 1 1 d . . . C2 C 0.11003(16) 0.16618(17) 0.39089(15) 0.0193(5) Uani 1 1 d . . . H2A H 0.0892 0.1910 0.3459 0.023 Uiso 1 1 calc R . . C3 C 0.12615(17) 0.12615(17) 0.5978(3) 0.0216(8) Uani 1 2 d S . . H3A H 0.1629 0.1627 0.6220 0.032 Uiso 1 2 calc SR . . H3B H 0.1388 0.0728 0.6141 0.032 Uiso 0.50 1 calc PR . . H3C H 0.0728 0.1390 0.6142 0.032 Uiso 0.50 1 calc PR . . N11 N 0.0000 0.0000 0.4694(4) 0.064(2) Uani 1 4 d S . . N21 N 0.2730(2) 0.2730(2) 0.4729(3) 0.0539(13) Uani 1 2 d S . . N22 N 0.2822(3) 0.2822(3) 0.4222(4) 0.087(2) Uani 1 2 d S . . N31 N 0.3076(6) 0.3076(6) 0.6924(6) 0.110(4) Uiso 1 6 d S . . N32 N 0.3356(7) 0.3356(7) 0.6644(7) 0.147(7) Uiso 1 6 d S . . N41 N 0.2513(4) 0.5149(5) 0.4851(5) 0.128(4) Uiso 1 2 d S . . N51 N 0.4721(17) 0.5279(17) 0.5279(17) 0.24(4) Uiso 0.50 6 d SP . . 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 0.01385(19) 0.0132(2) 0.01385(19) 0.000 0.000 0.000 C1 0.0152(8) 0.0152(8) 0.017(2) -0.0009(10) -0.0009(10) -0.0013(10) N1 0.0161(10) 0.0139(10) 0.0142(9) -0.0008(7) 0.0018(8) 0.0025(8) C2 0.0194(13) 0.0211(13) 0.0174(13) -0.0020(11) 0.0012(10) 0.0058(12) C3 0.0225(13) 0.0225(13) 0.020(2) 0.0028(11) 0.0028(11) 0.0100(19) N11 0.0361(16) 0.0361(16) 0.121(6) 0.000 0.000 0.010(6) N21 0.0506(18) 0.0506(18) 0.060(3) 0.0001(17) 0.0001(17) 0.002(2) N22 0.087(3) 0.087(3) 0.087(5) 0.031(3) 0.031(3) 0.020(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 2.002(2) 48 ? Zn1 N1 2.002(2) 3_556 ? Zn1 N1 2.002(2) . ? Zn1 N1 2.002(2) 46_455 ? C1 N1 1.342(3) 13 ? C1 N1 1.342(3) . ? C1 C3 1.513(6) . ? N1 C2 1.378(3) . ? C2 C2 1.360(6) 13 ? N11 N11 1.047(13) 3_556 ? N21 N22 0.896(7) . ? N31 N32 0.83(2) . ? N41 N41 0.72(2) 4_566 ? N51 N51 1.35(8) 4_566 ? N51 N51 1.35(8) 2_665 ? N51 N51 1.35(8) 3_656 ? 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 110.37(6) 48 3_556 ? N1 Zn1 N1 110.37(6) 48 . ? N1 Zn1 N1 107.70(11) 3_556 . ? N1 Zn1 N1 107.70(11) 48 46_455 ? N1 Zn1 N1 110.37(6) 3_556 46_455 ? N1 Zn1 N1 110.37(6) . 46_455 ? N1 C1 N1 113.4(4) 13 . ? N1 C1 C3 123.32(19) 13 . ? N1 C1 C3 123.32(19) . . ? C1 N1 C2 104.6(2) . . ? C1 N1 Zn1 129.5(2) . . ? C2 N1 Zn1 125.39(17) . . ? C2 C2 N1 108.69(14) 13 . ? N51 N51 N51 60.000(1) 4_566 2_665 ? N51 N51 N51 60.000(3) 4_566 3_656 ? N51 N51 N51 60.000(4) 2_665 3_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.944 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.066 data_MAF-4_100K _database_code_depnum_ccdc_archive 'CCDC 893941' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 N12.67 Zn' _chemical_formula_weight 348.99 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.133(2) _cell_length_b 17.133(2) _cell_length_c 17.133(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5029.3(12) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7462 _exptl_absorpt_correction_T_max 0.7561 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9751 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.98 _reflns_number_total 955 _reflns_number_gt 941 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0505P)^2^+3.5610P] 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 -0.04(2) _refine_ls_number_reflns 955 _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.2500 0.5000 0.01390(19) Uani 1 4 d S . . C1 C 0.13219(15) 0.13219(15) 0.5100(3) 0.0155(9) Uani 1 2 d S . . N1 N 0.08872(13) 0.18114(13) 0.46686(13) 0.0140(5) Uani 1 1 d . . . C2 C 0.10990(18) 0.1661(2) 0.39069(17) 0.0184(6) Uani 1 1 d . . . H2A H 0.0888 0.1908 0.3458 0.022 Uiso 1 1 calc R . . C3 C 0.1260(2) 0.1260(2) 0.5978(3) 0.0218(9) Uani 1 2 d S . . H3A H 0.1626 0.1626 0.6221 0.033 Uiso 1 2 calc SR . . H3B H 0.1387 0.0727 0.6141 0.033 Uiso 0.50 1 calc PR . . H3C H 0.0727 0.1387 0.6141 0.033 Uiso 0.50 1 calc PR . . N11 N 0.0000 0.0000 0.4693(4) 0.060(2) Uani 1 4 d S . . N21 N 0.2730(3) 0.2730(3) 0.4724(4) 0.0510(14) Uani 1 2 d S . . N22 N 0.2827(4) 0.2827(4) 0.4222(5) 0.088(3) Uani 1 2 d S . . N31 N 0.3078(6) 0.3078(6) 0.6922(6) 0.109(5) Uiso 1 6 d S . . N32 N 0.3356(7) 0.3356(7) 0.6644(7) 0.136(7) Uiso 1 6 d S . . N41 N 0.2510(4) 0.5146(5) 0.4854(5) 0.124(4) Uiso 1 2 d S . . N51 N 0.4729(18) 0.5271(18) 0.5271(18) 0.23(4) Uiso 0.50 6 d SP . . 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 0.0142(2) 0.0134(3) 0.0142(2) 0.000 0.000 0.000 C1 0.0163(10) 0.0163(10) 0.014(3) -0.0030(12) -0.0030(12) -0.0010(12) N1 0.0150(11) 0.0132(11) 0.0138(10) -0.0002(8) 0.0002(9) 0.0017(9) C2 0.0193(15) 0.0223(16) 0.0137(15) -0.0026(12) 0.0003(11) 0.0046(14) C3 0.0221(15) 0.0221(15) 0.021(3) 0.0013(13) 0.0013(13) 0.010(2) N11 0.0337(17) 0.0337(17) 0.113(6) 0.000 0.000 0.012(6) N21 0.0448(19) 0.0448(19) 0.063(4) -0.0013(18) -0.0013(18) 0.003(2) N22 0.087(4) 0.087(4) 0.089(6) 0.034(4) 0.034(4) 0.023(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 2.006(2) 48 ? Zn1 N1 2.006(2) 3_556 ? Zn1 N1 2.006(2) 46_455 ? Zn1 N1 2.006(2) . ? C1 N1 1.343(4) 13 ? C1 N1 1.343(4) . ? C1 C3 1.512(7) . ? N1 C2 1.379(4) . ? C2 C2 1.362(6) 13 ? N11 N11 1.053(13) 3_556 ? N21 N22 0.892(7) . ? N31 N32 0.82(2) . ? N41 N41 0.71(2) 4_566 ? N51 N51 1.31(9) 4_566 ? N51 N51 1.31(9) 2_665 ? N51 N51 1.31(9) 3_656 ? 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 110.23(6) 48 3_556 ? N1 Zn1 N1 107.96(13) 48 46_455 ? N1 Zn1 N1 110.23(6) 3_556 46_455 ? N1 Zn1 N1 110.23(6) 48 . ? N1 Zn1 N1 107.96(13) 3_556 . ? N1 Zn1 N1 110.23(6) 46_455 . ? N1 C1 N1 113.0(4) 13 . ? N1 C1 C3 123.5(2) 13 . ? N1 C1 C3 123.5(2) . . ? C1 N1 C2 105.0(3) . . ? C1 N1 Zn1 129.2(2) . . ? C2 N1 Zn1 125.24(19) . . ? C2 C2 N1 108.54(16) 13 . ? N51 N51 N51 60.000(1) 4_566 2_665 ? N51 N51 N51 60.000(3) 4_566 3_656 ? N51 N51 N51 60.000(4) 2_665 3_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.373 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.072 data_MAF-7_293K _database_code_depnum_ccdc_archive 'CCDC 893942' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 N6.40 Zn' _chemical_formula_weight 235.16 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.019(3) _cell_length_b 17.019(3) _cell_length_c 17.019(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4929.2(13) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1426 _exptl_absorpt_coefficient_mu 1.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6577 _exptl_absorpt_correction_T_max 0.7470 _exptl_absorpt_process_details SADABS _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 CCD _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9424 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.98 _reflns_number_total 920 _reflns_number_gt 792 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0413P)^2^+1.5320P] 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 0.02(3) _refine_ls_number_reflns 920 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.2500 0.5000 0.0677(2) Uani 1 4 d S . . C1 C 0.12383(15) 0.12383(15) 0.5118(3) 0.0694(13) Uani 1 2 d S A . N1 N 0.09052(15) 0.18223(14) 0.47247(13) 0.0712(7) Uani 1 1 d . . . C2 C 0.1300(2) 0.1849(2) 0.40233(19) 0.0966(10) Uani 0.50 1 d P A 1 H2A H 0.1198 0.2197 0.3614 0.116 Uiso 0.50 1 calc PR A 1 N2 N 0.1300(2) 0.1849(2) 0.40233(19) 0.0966(10) Uani 0.50 1 d P A 2 C3 C 0.0987(3) 0.0987(3) 0.5930(3) 0.116(2) Uani 1 2 d S . . H3A H 0.1284 0.1271 0.6315 0.174 Uiso 1 2 calc SR A . H3B H 0.1079 0.0434 0.5992 0.174 Uiso 0.50 1 calc PR . . H3C H 0.0437 0.1095 0.5998 0.174 Uiso 0.50 1 calc PR . . N41 N 0.0000 0.0000 0.7495(12) 0.098(7) Uiso 0.24 4 d SP . . N31 N 0.248(2) 0.248(2) 0.248(2) 0.096(8) Uiso 0.24 6 d SP . . 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 0.0713(3) 0.0606(3) 0.0713(3) 0.000 0.000 0.000 C1 0.0715(13) 0.0715(13) 0.065(4) 0.0007(15) 0.0007(15) 0.0024(18) N1 0.0769(15) 0.0671(13) 0.0696(18) 0.0024(11) 0.0039(11) 0.0066(12) C2 0.109(2) 0.100(2) 0.081(2) 0.0239(17) 0.0202(18) 0.0216(18) N2 0.109(2) 0.100(2) 0.081(2) 0.0239(17) 0.0202(18) 0.0216(18) C3 0.130(3) 0.130(3) 0.087(3) 0.034(3) 0.034(3) 0.044(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 1.981(2) 3_556 ? Zn1 N1 1.981(2) 48 ? Zn1 N1 1.981(2) . ? Zn1 N1 1.981(2) 46_455 ? C1 N1 1.326(3) . ? C1 N1 1.326(3) 13 ? C1 C3 1.508(7) . ? N1 C2 1.370(4) . ? C2 C2 1.323(6) 13 ? 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 109.82(7) 3_556 48 ? N1 Zn1 N1 108.78(15) 3_556 . ? N1 Zn1 N1 109.82(8) 48 . ? N1 Zn1 N1 109.82(7) 3_556 46_455 ? N1 Zn1 N1 108.78(15) 48 46_455 ? N1 Zn1 N1 109.82(7) . 46_455 ? N1 C1 N1 112.7(4) . 13 ? N1 C1 C3 123.6(2) . . ? N1 C1 C3 123.6(2) 13 . ? C1 N1 C2 104.8(3) . . ? C1 N1 Zn1 130.5(2) . . ? C2 N1 Zn1 124.6(2) . . ? C2 C2 N1 108.82(17) 13 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.192 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.057 data_MAF-7_118K _database_code_depnum_ccdc_archive 'CCDC 893943' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 N13 Zn' _chemical_formula_weight 327.62 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.0641(19) _cell_length_b 17.0641(19) _cell_length_c 17.0641(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4968.8(10) _cell_formula_units_Z 12 _cell_measurement_temperature 118(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 1.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6544 _exptl_absorpt_correction_T_max 0.7443 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 118(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9494 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.97 _reflns_number_total 925 _reflns_number_gt 916 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0651P)^2^+4.1328P] 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 -0.02(3) _refine_ls_number_reflns 925 _refine_ls_number_parameters 50 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.040 _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 0.2500 0.5000 0.0253(2) Uani 1 4 d S . . N1 N 0.09156(14) 0.18273(13) 0.47405(13) 0.0279(5) Uani 1 1 d . . . C1 C 0.12360(14) 0.12360(14) 0.5133(3) 0.0273(11) Uani 1 2 d S A . C2 C 0.13249(17) 0.18773(19) 0.40546(17) 0.0407(7) Uani 0.50 1 d P A 1 H2A H 0.1232 0.2244 0.3646 0.049 Uiso 0.50 1 calc PR A 1 N2 N 0.13249(17) 0.18773(19) 0.40546(17) 0.0407(7) Uani 0.50 1 d P A 2 C3 C 0.0974(3) 0.0974(3) 0.5930(3) 0.0468(12) Uani 1 2 d S . . H3A H 0.1263 0.1264 0.6332 0.070 Uiso 1 2 calc SR A . H3B H 0.1075 0.0412 0.5989 0.070 Uiso 0.50 1 calc PR . . H3C H 0.0411 0.1074 0.5989 0.070 Uiso 0.50 1 calc PR . . N21 N 0.2782(6) 0.2782(6) 0.5402(9) 0.145(5) Uiso 1 2 d S . . N22 N 0.2670(12) 0.3160(14) 0.510(2) 0.207(10) Uiso 0.50 1 d P . . N31 N 0.2039(10) 0.2039(10) 0.7961(10) 0.138(7) Uiso 1 6 d S . . N32 N 0.2356(8) 0.2356(8) 0.7644(8) 0.074(6) Uiso 0.50 6 d SP . . N32' N 0.181(3) 0.181(3) 0.819(3) 0.24(4) Uiso 0.50 6 d SP . . N41 N 0.2585(14) 0.5000 0.5000 0.182(9) Uiso 0.83 4 d SPD . . N42 N 0.323(3) 0.5000 0.5000 0.53(4) Uiso 0.83 4 d SPD . . 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 0.0264(2) 0.0232(3) 0.0264(2) 0.000 0.000 0.000 N1 0.0285(12) 0.0259(11) 0.0293(12) 0.0002(8) 0.0018(8) 0.0029(9) C1 0.0275(10) 0.0275(10) 0.027(3) 0.0009(10) 0.0009(10) -0.0008(13) C2 0.0423(16) 0.0461(17) 0.0336(15) 0.0105(13) 0.0094(12) 0.0074(13) N2 0.0423(16) 0.0461(17) 0.0336(15) 0.0105(13) 0.0094(12) 0.0074(13) C3 0.0537(18) 0.0537(18) 0.033(2) 0.0155(17) 0.0155(17) 0.020(2) _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 1.989(2) 48 ? Zn1 N1 1.989(2) 3_556 ? Zn1 N1 1.989(2) . ? Zn1 N1 1.989(2) 46_455 ? N1 C1 1.329(3) . ? N1 C2 1.366(4) . ? C1 N1 1.329(3) 13 ? C1 C3 1.499(6) . ? C2 C2 1.333(6) 13 ? N21 N22 0.85(3) . ? N21 N22 0.85(3) 13 ? N22 N22 1.18(4) 13 ? N31 N32' 0.67(9) . ? N31 N32 0.94(3) . ? N32 N32' 1.61(8) . ? N41 N42 1.10(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 109.46(7) 48 3_556 ? N1 Zn1 N1 109.46(7) 48 . ? N1 Zn1 N1 109.49(14) 3_556 . ? N1 Zn1 N1 109.49(14) 48 46_455 ? N1 Zn1 N1 109.46(7) 3_556 46_455 ? N1 Zn1 N1 109.46(7) . 46_455 ? C1 N1 C2 105.6(2) . . ? C1 N1 Zn1 130.5(2) . . ? C2 N1 Zn1 123.82(19) . . ? N1 C1 N1 111.7(3) . 13 ? N1 C1 C3 124.13(17) . . ? N1 C1 C3 124.13(17) 13 . ? C2 C2 N1 108.51(16) 13 . ? N22 N21 N22 88(4) . 13 ? N21 N22 N22 46(2) . 13 ? N32' N31 N32 180(10) . . ? N31 N32 N32' 0(4) . . ? N31 N32' N32 0(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.497 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.073 data_MAF-7_115K _database_code_depnum_ccdc_archive 'CCDC 893944' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 N14.67 Zn' _chemical_formula_weight 350.97 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.082(2) _cell_length_b 17.082(2) _cell_length_c 17.082(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4984.5(10) _cell_formula_units_Z 12 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6539 _exptl_absorpt_correction_T_max 0.7438 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9551 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.94 _reflns_number_total 928 _reflns_number_gt 920 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0637P)^2^+18.6295P] 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 0.02(4) _refine_ls_number_reflns 928 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.2500 0.5000 0.0175(3) Uani 1 4 d S . . C1 C 0.1325(2) 0.1325(2) 0.5135(4) 0.0229(15) Uani 1 2 d S A . N1 N 0.08906(19) 0.18066(18) 0.46998(18) 0.0203(7) Uani 1 1 d . . . C2 C 0.1100(3) 0.1649(3) 0.3945(3) 0.0360(11) Uani 0.50 1 d P A 1 H2A H 0.0887 0.1893 0.3492 0.043 Uiso 0.50 1 calc PR A 1 N2 N 0.1100(3) 0.1649(3) 0.3945(3) 0.0360(11) Uani 0.50 1 d P A 2 C3 C 0.1307(4) 0.1307(4) 0.6012(5) 0.0388(19) Uani 1 2 d S . . H3A H 0.1682 0.1688 0.6220 0.058 Uiso 1 2 calc SR A . H3B H 0.1447 0.0782 0.6196 0.058 Uiso 0.50 1 calc PR . . H3C H 0.0779 0.1439 0.6196 0.058 Uiso 0.50 1 calc PR . . N11 N 0.0000 0.0000 0.4681(7) 0.089(5) Uani 1 4 d S . . N21 N 0.2722(6) 0.2722(6) 0.4779(15) 0.118(9) Uani 1 2 d S . . N22 N 0.2912(9) 0.2912(9) 0.443(2) 0.183(12) Uani 1 2 d S . . N33 N 0.2653(11) 0.2653(11) 0.7347(11) 0.053(8) Uiso 0.40 6 d SP . . N31 N 0.2981(12) 0.2981(12) 0.7019(12) 0.122(10) Uiso 1 6 d S . . N32 N 0.320(3) 0.320(3) 0.680(3) 0.19(3) Uiso 0.60 6 d SP . . N41 N 0.2498(8) 0.5139(13) 0.4861(13) 0.197(10) Uiso 1 2 d S . . N51 N 0.425(5) 0.575(5) 0.425(5) 0.18(5) Uiso 0.25 6 d SP . . N52 N 0.460(5) 0.540(5) 0.460(5) 0.26(12) Uiso 0.25 6 d SP . . 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 0.0182(3) 0.0162(4) 0.0182(3) 0.000 0.000 0.000 C1 0.0230(15) 0.0230(15) 0.023(5) 0.0010(15) 0.0010(15) 0.0021(18) N1 0.0210(16) 0.0170(15) 0.0231(15) -0.0010(11) 0.0026(12) 0.0014(13) C2 0.038(3) 0.043(3) 0.026(2) 0.002(2) 0.0035(18) 0.015(2) N2 0.038(3) 0.043(3) 0.026(2) 0.002(2) 0.0035(18) 0.015(2) C3 0.046(3) 0.046(3) 0.025(4) 0.004(2) 0.004(2) 0.023(4) N11 0.055(3) 0.055(3) 0.158(14) 0.000 0.000 -0.017(12) N21 0.070(5) 0.070(5) 0.21(3) 0.008(8) 0.008(8) -0.010(6) N22 0.126(11) 0.126(11) 0.30(3) 0.031(11) 0.031(11) -0.031(13) _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 1.995(3) 46_455 ? Zn1 N1 1.995(3) 3_556 ? Zn1 N1 1.995(3) 48 ? Zn1 N1 1.995(3) . ? C1 N1 1.334(5) 13 ? C1 N1 1.334(5) . ? C1 C3 1.500(10) . ? N1 C2 1.366(6) . ? C2 C2 1.326(10) 13 ? N11 N11 1.09(2) 3_556 ? N21 N22 0.75(3) . ? N33 N31 0.97(4) . ? N33 N32 1.62(8) . ? N31 N32 0.65(8) . ? N41 N41 0.67(7) 4_566 ? N51 N52 1.1(2) . ? 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 110.64(9) 46_455 3_556 ? N1 Zn1 N1 107.16(18) 46_455 48 ? N1 Zn1 N1 110.64(9) 3_556 48 ? N1 Zn1 N1 110.64(9) 46_455 . ? N1 Zn1 N1 107.16(18) 3_556 . ? N1 Zn1 N1 110.64(9) 48 . ? N1 C1 N1 112.1(5) 13 . ? N1 C1 C3 123.9(3) 13 . ? N1 C1 C3 123.9(3) . . ? C1 N1 C2 105.0(4) . . ? C1 N1 Zn1 130.3(3) . . ? C2 N1 Zn1 124.0(3) . . ? C2 C2 N1 109.0(2) 13 . ? N31 N33 N32 0(3) . . ? N32 N31 N33 180(10) . . ? N31 N32 N33 0(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.496 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.090 data_MAF-7_100K1 _database_code_depnum_ccdc_archive 'CCDC 893945' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 N13 Zn' _chemical_formula_weight 327.62 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.0550(8) _cell_length_b 17.0550(8) _cell_length_c 17.0550(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4960.8(4) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 1.497 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6540 _exptl_absorpt_correction_T_max 0.7440 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18359 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.98 _reflns_number_total 940 _reflns_number_gt 939 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0743P)^2^+15.4830P] 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 0.00(4) _refine_ls_number_reflns 940 _refine_ls_number_parameters 50 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.078 _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 0.2500 0.5000 0.0226(3) Uani 1 4 d S . . N1 N 0.0912(2) 0.18242(19) 0.47293(19) 0.0264(7) Uani 1 1 d . . . C1 C 0.1252(2) 0.1252(2) 0.5130(4) 0.0316(18) Uani 1 2 d S A . C2 C 0.1310(3) 0.1858(3) 0.4046(3) 0.0519(13) Uani 0.50 1 d P A 1 H2A H 0.1212 0.2217 0.3632 0.062 Uiso 0.50 1 calc PR A 1 N2 N 0.1310(3) 0.1858(3) 0.4046(3) 0.0519(13) Uani 0.50 1 d P A 2 C3 C 0.0979(5) 0.0979(5) 0.5931(4) 0.059(2) Uani 1 2 d S . . H3A H 0.1268 0.1264 0.6339 0.089 Uiso 1 2 calc SR A . H3B H 0.1077 0.0416 0.5985 0.089 Uiso 0.50 1 calc PR . . H3C H 0.0417 0.1083 0.5988 0.089 Uiso 0.50 1 calc PR . . N21 N 0.2783(9) 0.2783(9) 0.5315(11) 0.139(6) Uiso 1 2 d S . . N22 N 0.272(2) 0.327(3) 0.521(3) 0.26(2) Uiso 0.50 1 d P . . N31 N 0.2069(13) 0.2069(13) 0.7931(13) 0.124(9) Uiso 1 6 d S . . N32 N 0.2362(11) 0.2362(11) 0.7638(11) 0.067(8) Uiso 0.50 6 d SP . . N32' N 0.182(3) 0.182(3) 0.818(3) 0.19(3) Uiso 0.50 6 d SP . . N41 N 0.259(2) 0.5000 0.5000 0.204(15) Uiso 0.83 4 d SPD . . N42 N 0.324(4) 0.5000 0.5000 0.57(7) Uiso 0.83 4 d SPD . . 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 0.0236(3) 0.0207(4) 0.0236(3) 0.000 0.000 0.000 N1 0.0270(17) 0.0248(16) 0.0275(16) 0.0028(11) 0.0020(12) 0.0030(13) C1 0.0318(16) 0.0318(16) 0.031(5) 0.0014(17) 0.0014(17) 0.003(2) C2 0.056(3) 0.065(3) 0.035(2) 0.017(2) 0.016(2) 0.018(2) N2 0.056(3) 0.065(3) 0.035(2) 0.017(2) 0.016(2) 0.018(2) C3 0.071(3) 0.071(3) 0.036(4) 0.018(3) 0.018(3) 0.039(5) _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 1.991(3) 3_556 ? Zn1 N1 1.991(3) 48 ? Zn1 N1 1.991(3) . ? Zn1 N1 1.991(3) 46_455 ? N1 C1 1.325(5) . ? N1 C2 1.349(6) . ? C1 N1 1.325(5) 13 ? C1 C3 1.516(9) . ? C2 C2 1.321(10) 13 ? N21 N22 0.85(5) . ? N21 N22 0.85(5) 13 ? N22 N22 1.32(9) 13 ? N31 N32' 0.73(9) . ? N31 N32 0.87(4) . ? N32 N32' 1.59(9) . ? N41 N42 1.11(5) . ? 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 109.58(10) 3_556 48 ? N1 Zn1 N1 109.25(19) 3_556 . ? N1 Zn1 N1 109.58(10) 48 . ? N1 Zn1 N1 109.58(10) 3_556 46_455 ? N1 Zn1 N1 109.25(19) 48 46_455 ? N1 Zn1 N1 109.58(10) . 46_455 ? C1 N1 C2 104.9(4) . . ? C1 N1 Zn1 130.4(3) . . ? C2 N1 Zn1 124.6(3) . . ? N1 C1 N1 112.2(6) 13 . ? N1 C1 C3 123.9(3) 13 . ? N1 C1 C3 123.9(3) . . ? C2 C2 N1 109.0(2) 13 . ? N22 N21 N22 101(6) . 13 ? N21 N22 N22 39(3) . 13 ? N32' N31 N32 180(10) . . ? N31 N32 N32' 0(2) . . ? N31 N32' N32 0(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.860 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.104 data_MAF-7_100K2 _database_code_depnum_ccdc_archive 'CCDC 893946' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 N13.91 Zn' _chemical_formula_weight 340.43 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.0659(12) _cell_length_b 17.0659(12) _cell_length_c 17.0659(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4970.4(6) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2057 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6537 _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5676 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.96 _reflns_number_total 901 _reflns_number_gt 896 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1048P)^2^+15.3600P] 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 0.06(6) _refine_ls_number_reflns 901 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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 0.2500 0.5000 0.0211(4) Uani 1 4 d S . . C1 C 0.1277(3) 0.1277(3) 0.5138(6) 0.031(3) Uani 1 2 d S A . N1 N 0.0906(3) 0.1822(3) 0.4724(3) 0.0245(10) Uani 1 1 d . . . C2 C 0.1252(6) 0.1805(7) 0.4013(5) 0.082(4) Uani 0.50 1 d P A 1 H2A H 0.1124 0.2134 0.3583 0.098 Uiso 0.50 1 calc PR A 1 N2 N 0.1252(6) 0.1805(7) 0.4013(5) 0.082(4) Uani 0.50 1 d P A 2 C3 C 0.1038(11) 0.1038(11) 0.5941(7) 0.105(8) Uani 1 2 d S . . H3A H 0.1342 0.1334 0.6328 0.158 Uiso 1 2 calc SR A . H3B H 0.1135 0.0476 0.6011 0.158 Uiso 0.50 1 calc PR . . H3C H 0.0478 0.1146 0.6015 0.158 Uiso 0.50 1 calc PR . . N11 N 0.0000 0.0000 0.476(3) 0.065(19) Uiso 0.25(4) 4 d SP . . N21 N 0.2774(17) 0.2774(17) 0.520(3) 0.163(14) Uiso 1 2 d S . . N22 N 0.273(4) 0.305(4) 0.550(3) 0.22(3) Uiso 0.50 1 d P . . N31 N 0.2849(18) 0.2849(18) 0.2849(18) 0.135(14) Uiso 1 6 d S . . N32 N 0.313(2) 0.313(2) 0.313(2) 0.21(3) Uiso 1 6 d S . . N41 N 0.246(5) 0.5000 0.5000 0.29(4) Uiso 1 4 d S . . N42 N 0.308(10) 0.5000 0.5000 0.58(10) Uiso 1 4 d S . . N51 N 0.531(10) 0.469(10) 0.469(10) 0.4(3) Uiso 0.50 6 d SP . . 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 0.0221(5) 0.0191(5) 0.0221(5) 0.000 0.000 0.000 C1 0.032(2) 0.032(2) 0.028(8) -0.001(2) -0.001(2) 0.007(3) N1 0.026(2) 0.022(2) 0.026(2) 0.0029(16) 0.0030(17) 0.0007(19) C2 0.082(6) 0.121(9) 0.043(4) 0.040(5) 0.035(4) 0.060(6) N2 0.082(6) 0.121(9) 0.043(4) 0.040(5) 0.035(4) 0.060(6) C3 0.141(12) 0.141(12) 0.035(6) 0.026(7) 0.026(7) 0.123(14) _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 1.987(5) 48 ? Zn1 N1 1.987(5) 3_556 ? Zn1 N1 1.987(5) 46_455 ? Zn1 N1 1.987(5) . ? C1 N1 1.330(7) . ? C1 N1 1.330(7) 13 ? C1 C3 1.487(16) . ? N1 C2 1.349(9) . ? C2 C2 1.335(17) 13 ? N11 N11 0.81(9) 3_556 ? N21 N22 0.70(7) 13 ? N21 N22 0.70(7) . ? N22 N22 0.75(15) 13 ? N31 N32 0.84(7) . ? N41 N42 1.06(16) . ? N51 N51 1.5(5) 4_566 ? N51 N51 1.5(5) 2_665 ? N51 N51 1.5(5) 3_656 ? 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 109.79(14) 48 3_556 ? N1 Zn1 N1 108.8(3) 48 46_455 ? N1 Zn1 N1 109.79(14) 3_556 46_455 ? N1 Zn1 N1 109.79(14) 48 . ? N1 Zn1 N1 108.8(3) 3_556 . ? N1 Zn1 N1 109.79(14) 46_455 . ? N1 C1 N1 112.6(8) . 13 ? N1 C1 C3 123.5(4) . . ? N1 C1 C3 123.5(4) 13 . ? C1 N1 C2 104.7(6) . . ? C1 N1 Zn1 130.6(5) . . ? C2 N1 Zn1 124.5(5) . . ? C2 C2 N1 109.0(4) 13 . ? N22 N21 N22 65(10) 13 . ? N21 N22 N22 58(6) . 13 ? N51 N51 N51 60.00(2) 4_566 2_665 ? N51 N51 N51 60.000(15) 4_566 3_656 ? N51 N51 N51 60.000(15) 2_665 3_656 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.933 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.121 data_MAF-7_100K3 _database_code_depnum_ccdc_archive 'CCDC 893947' #TrackingRef '12888_web_deposit_cif_file_0_Jie-PengZhang_1343360197.data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 N14.67 Zn' _chemical_formula_weight 350.97 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+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+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 17.0797(19) _cell_length_b 17.0797(19) _cell_length_c 17.0797(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4982.4(10) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6538 _exptl_absorpt_correction_T_max 0.7438 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9588 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.94 _reflns_number_total 927 _reflns_number_gt 919 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0477P)^2^+5.1328P] 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 0.00(2) _refine_ls_number_reflns 927 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.2500 0.5000 0.01517(18) Uani 1 4 d S . . C1 C 0.13384(13) 0.13384(13) 0.5133(2) 0.0167(9) Uani 1 2 d S A . N1 N 0.08880(12) 0.18037(12) 0.46941(12) 0.0165(5) Uani 1 1 d . . . C2 C 0.10816(16) 0.16326(18) 0.39342(15) 0.0241(6) Uani 0.50 1 d P A 1 H2A H 0.0859 0.1868 0.3482 0.029 Uiso 0.50 1 calc PR A 1 N2 N 0.10816(16) 0.16326(18) 0.39342(15) 0.0241(6) Uani 0.50 1 d P A 2 C3 C 0.13121(19) 0.13121(19) 0.6014(3) 0.0243(10) Uani 1 2 d S . . H3A H 0.1688 0.1689 0.6228 0.036 Uiso 1 2 calc SR A . H3B H 0.1447 0.0784 0.6194 0.036 Uiso 0.50 1 calc PR . . H3C H 0.0784 0.1446 0.6194 0.036 Uiso 0.50 1 calc PR . . N11 N 0.0000 0.0000 0.4699(3) 0.0577(17) Uani 1 4 d S . . N21 N 0.2715(3) 0.2715(3) 0.4773(6) 0.090(4) Uani 1 2 d S . . N22 N 0.2910(5) 0.2910(5) 0.4414(10) 0.159(6) Uani 1 2 d S . . N33 N 0.2640(6) 0.2640(6) 0.7360(6) 0.069(5) Uiso 0.60 6 d SP . . N31 N 0.2981(5) 0.2981(5) 0.7019(5) 0.090(4) Uiso 1 6 d S . . N32 N 0.3251(13) 0.3251(13) 0.6749(13) 0.095(10) Uiso 0.40 6 d SP . . N41 N 0.2455(4) 0.5136(6) 0.4864(6) 0.136(4) Uiso 1 2 d S . . N51 N 0.449(3) 0.551(3) 0.449(3) 0.19(4) Uiso 0.25 6 d SP . . N52 N 0.455(4) 0.5000 0.5000 0.17(5) Uiso 0.17 4 d SP . . 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 0.0157(2) 0.0141(3) 0.0157(2) 0.000 0.000 0.000 C1 0.0160(9) 0.0160(9) 0.018(3) -0.0001(9) -0.0001(9) -0.0021(11) N1 0.0167(10) 0.0166(10) 0.0164(9) -0.0014(8) 0.0013(8) 0.0019(8) C2 0.0265(15) 0.0288(14) 0.0169(13) -0.0022(11) -0.0003(10) 0.0030(12) N2 0.0265(15) 0.0288(14) 0.0169(13) -0.0022(11) -0.0003(10) 0.0030(12) C3 0.0293(15) 0.0293(15) 0.014(2) 0.0024(12) 0.0024(12) 0.006(2) N11 0.0358(14) 0.0358(14) 0.102(5) 0.000 0.000 -0.001(6) N21 0.049(2) 0.049(2) 0.172(13) 0.011(3) 0.011(3) -0.004(3) N22 0.120(6) 0.120(6) 0.236(15) 0.042(6) 0.042(6) -0.012(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 1.997(2) 3_556 ? Zn1 N1 1.997(2) 48 ? Zn1 N1 1.997(2) 46_455 ? Zn1 N1 1.997(2) . ? C1 N1 1.336(3) 13 ? C1 N1 1.336(3) . ? C1 C3 1.507(6) . ? N1 C2 1.371(3) . ? C2 C2 1.331(6) 13 ? N11 N11 1.028(12) 3_556 ? N21 N22 0.772(13) . ? N33 N31 1.007(19) . ? N33 N32 1.81(4) . ? N31 N32 0.80(4) . ? N41 N41 0.66(3) 4_566 ? N51 N52 1.23(8) 6_566 ? N51 N52 1.23(8) . ? N51 N52 1.23(8) 9 ? N52 N52 1.10(9) 9 ? N52 N52 1.10(9) 6_566 ? N52 N52 1.10(9) 10_656 ? N52 N52 1.10(9) 5 ? N52 N51 1.23(8) 4_566 ? N52 N52 1.55(13) 2_665 ? 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 110.77(6) 3_556 48 ? N1 Zn1 N1 110.77(6) 3_556 46_455 ? N1 Zn1 N1 106.90(12) 48 46_455 ? N1 Zn1 N1 106.90(12) 3_556 . ? N1 Zn1 N1 110.77(6) 48 . ? N1 Zn1 N1 110.77(6) 46_455 . ? N1 C1 N1 111.8(3) 13 . ? N1 C1 C3 124.11(16) 13 . ? N1 C1 C3 124.11(16) . . ? C1 N1 C2 105.4(2) . . ? C1 N1 Zn1 130.17(19) . . ? C2 N1 Zn1 123.90(18) . . ? C2 C2 N1 108.73(15) 13 . ? N31 N33 N32 0.0(9) . . ? N32 N31 N33 180(4) . . ? N31 N32 N33 0(2) . . ? N52 N51 N52 53(6) 6_566 . ? N52 N51 N52 53(6) 6_566 9 ? N52 N51 N52 53(6) . 9 ? N52 N52 N52 60.00(2) 9 6_566 ? N52 N52 N52 90.00(2) 9 10_656 ? N52 N52 N52 60.000(14) 6_566 10_656 ? N52 N52 N52 60.000(7) 9 5 ? N52 N52 N52 90.00(2) 6_566 5 ? N52 N52 N52 60.000(7) 10_656 5 ? N52 N52 N51 63(3) 9 . ? N52 N52 N51 63(3) 6_566 . ? N52 N52 N51 123(3) 10_656 . ? N52 N52 N51 123(3) 5 . ? N52 N52 N51 123(3) 9 4_566 ? N52 N52 N51 123(3) 6_566 4_566 ? N52 N52 N51 63(3) 10_656 4_566 ? N52 N52 N51 63(3) 5 4_566 ? N51 N52 N51 172(8) . 4_566 ? N52 N52 N52 45.000(16) 9 2_665 ? N52 N52 N52 45.000(4) 6_566 2_665 ? N52 N52 N52 45.0 10_656 2_665 ? N52 N52 N52 45.000(4) 5 2_665 ? N51 N52 N52 94(4) . 2_665 ? N51 N52 N52 94(4) 4_566 2_665 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.588 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.068