# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dirk Volkmer' _publ_contact_author_email DIRK.VOLKMER@UNI-ULM.DE _publ_section_title ; A Cubic Coordination Framework Constructed from Benzobistriazolate Ligands and Zinc Ions Having Coordinatively Unsaturated Sites ; loop_ _publ_author_name 'Dirk Volkmer' 'Shyam Biswas' 'Stefanie Dehnen' 'Maciej Grzywa' 'Stefan Kaskel' 'Hari Nayek' ; I.Senkovska ; # Attachment 'MFU-4.cif' data_MFU-4 _database_code_depnum_ccdc_archive 'CCDC 723714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H6 Cl4 N18 Zn5, 3(C3 H7 N1 O1)' _chemical_formula_sum 'C27 H27 Cl4 N21 O3 Zn5' _chemical_formula_weight 1162.3612 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Fm-3m _symmetry_space_group_name_Hall '-F 4 2 3' 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, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'y, -x+1/2, z+1/2' '-y, x+1/2, z+1/2' 'x, z+1/2, -y+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'x, -z+1/2, y+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' '-z, y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, -z+1/2' '-y+1/2, -x, -z+1/2' 'y+1/2, -x, z+1/2' '-y+1/2, x, z+1/2' 'x+1/2, z, -y+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' 'y+1/2, -x+1/2, z' '-y+1/2, x+1/2, z' 'x+1/2, z+1/2, -y' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'x+1/2, -z+1/2, y' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' '-z+1/2, y+1/2, x' '-z+1/2, -y+1/2, -x' '-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, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-z, -x+1/2, -y+1/2' '-z, x+1/2, y+1/2' 'z, x+1/2, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' '-y, -x+1/2, z+1/2' 'y, x+1/2, z+1/2' '-y, x+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' '-x, -z+1/2, y+1/2' 'x, -z+1/2, -y+1/2' 'x, z+1/2, y+1/2' '-x, z+1/2, -y+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' 'z, -y+1/2, -x+1/2' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' '-z+1/2, -x, -y+1/2' '-z+1/2, x, y+1/2' 'z+1/2, x, -y+1/2' 'z+1/2, -x, y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/2, -z, x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' '-y+1/2, -x, z+1/2' 'y+1/2, x, z+1/2' '-y+1/2, x, -z+1/2' 'y+1/2, -x, -z+1/2' '-x+1/2, -z, y+1/2' 'x+1/2, -z, -y+1/2' 'x+1/2, z, y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' 'z+1/2, -y, -x+1/2' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/2, y' 'z+1/2, x+1/2, -y' 'z+1/2, -x+1/2, y' '-y+1/2, -z+1/2, -x' 'y+1/2, -z+1/2, x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' '-y+1/2, x+1/2, -z' 'y+1/2, -x+1/2, -z' '-x+1/2, -z+1/2, y' 'x+1/2, -z+1/2, -y' 'x+1/2, z+1/2, y' '-x+1/2, z+1/2, -y' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, -x' 'z+1/2, y+1/2, x' _cell_length_a 21.697(3) _cell_length_b 21.697(3) _cell_length_c 21.697(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10214(2) _cell_formula_units_Z 8 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description octahedral _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4624 _exptl_absorpt_coefficient_mu 2.573 _exptl_absorpt_correction_type 'semi-empirical from psi-scans' _exptl_absorpt_correction_T_min 0.81023 _exptl_absorpt_correction_T_max 0.85732 _exptl_absorpt_process_details XPREP _exptl_special_details ; North, A. C. T., Phillips, D. C. and Mathews, F. S. (1968) Acta. Cryst. A24, 351-359 ; _diffrn_ambient_temperature 103(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16467 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.60 _diffrn_reflns_theta_max 26.77 _reflns_number_total 542 _reflns_number_gt 505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE EXPOSE' _computing_cell_refinement 'STOE CELL' _computing_data_reduction 'STOE INTEGRATE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.4.2' _computing_publication_material 'DIAMOND 3.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+219.3190P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 542 _refine_ls_number_parameters 48 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1514 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _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 0.34584(4) 0.34584(4) 0.15416(4) 0.0259(5) Uani 1 6 d S . . Zn2 Zn 0.2500 0.2500 0.2500 0.0225(7) Uani 1 24 d S . . Cl1 Cl 0.40188(12) 0.40188(12) 0.09812(12) 0.0660(14) Uani 1 6 d S . . N1 N 0.3858(2) 0.28548(17) 0.21452(17) 0.0192(11) Uani 1 2 d S . . N2 N 0.3519(3) 0.2500 0.2500 0.0205(15) Uani 1 4 d S . . C1 C 0.4464(3) 0.2273(2) 0.2727(2) 0.0180(12) Uani 1 2 d S . . C2 C 0.5000 0.2007(3) 0.2993(3) 0.027(2) Uani 1 4 d S . . H2 H 0.5000 0.1704 0.3296 0.032 Uiso 1 4 calc SR . . C11 C 0.0000 0.4389(3) 0.0000(3) 0.08(5) Uiso 0.13 8 d SPR . . C22 C 0.0291 0.4189(3) 0.0812(3) 0.09(9) Uiso 0.05 2 d SPR . . C33 C 0.1121 0.3376(3) 0.1121(3) 0.07(6) Uiso 0.05 2 d SPR . . C44 C 0.0641 0.2839(3) 0.0641(3) 0.09(2) Uiso 0.19 2 d SPR . . C55 C 0.0760 0.3497(3) 0.0000(3) 0.08(5) Uiso 0.07 2 d SPR . . C66 C 0.0000 0.2134(3) 0.0000(3) 0.06(3) Uiso 0.20 8 d SPR . . C77 C 0.1468 0.3532(3) 0.0000(3) 0.10(8) Uiso 0.09 4 d SPR . . C88 C 0.0865 0.4135(3) 0.0000(3) 0.08(8) Uiso 0.07 4 d SPR . . C99 C 0.0000 0.1687(3) 0.0000(3) 0.07(4) Uiso 0.18 8 d SPR . . C111 C 0.0000 0.2090(3) 0.0884(3) 0.09(9) Uiso 0.05 2 d SPR . . C222 C 0.1113 0.2457(3) 0.0000(3) 0.07(6) Uiso 0.05 2 d SPR . . C333 C 0.1484 0.2970(3) 0.1484(3) 0.10(6) Uiso 0.08 2 d SPR . . O11 O 0.0852 0.3199(3) 0.0852(3) 0.086(18) Uiso 0.15 2 d SPR . . O22 O 0.0000 0.3733(3) 0.0000(3) 0.01(4) Uiso 0.03 8 d SPR . . O33 O 0.0000 0.1609(3) -0.0790(3) 0.11(18) Uiso 0.02 2 d SPR . . O44 O 0.1129 0.3067(3) 0.0000(3) 0.11(5) Uiso 0.07 2 d SPR . . N11 N 0.0324 0.4676(3) -0.0324(3) 0.09(5) Uiso 0.13 6 d SPR . . N22 N 0.1364 0.3636(3) 0.1364(3) 0.08(5) Uiso 0.10 6 d SPR . . N33 N 0.0447 0.2352(3) 0.0447(3) 0.11(6) Uiso 0.08 2 d SPR . . N44 N 0.0437 0.2583(3) 0.0000(3) 0.08(3) Uiso 0.09 2 d SPR . . 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 0.0259(5) 0.0259(5) 0.0259(5) -0.0042(3) -0.0042(3) 0.0042(3) Zn2 0.0225(7) 0.0225(7) 0.0225(7) 0.000 0.000 0.000 Cl1 0.0660(14) 0.0660(14) 0.0660(14) 0.0143(11) 0.0143(11) -0.0143(11) N1 0.016(2) 0.0209(16) 0.0209(16) 0.005(2) 0.0021(14) -0.0021(14) N2 0.023(4) 0.019(2) 0.019(2) -0.003(3) 0.000 0.000 C1 0.015(3) 0.0197(17) 0.0197(17) 0.005(2) 0.0017(16) -0.0017(16) C2 0.022(5) 0.029(3) 0.029(3) 0.008(4) 0.000 0.000 _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 2.045(6) 35 ? Zn1 N1 2.045(6) . ? Zn1 N1 2.045(6) 56 ? Zn1 Cl1 2.106(5) . ? Zn2 N2 2.212(7) 58 ? Zn2 N2 2.212(7) . ? Zn2 N2 2.212(7) 74 ? Zn2 N2 2.212(7) 5 ? Zn2 N2 2.212(7) 30 ? Zn2 N2 2.212(7) 9 ? N1 N2 1.314(6) . ? N1 C1 1.372(8) 28 ? N2 N1 1.314(6) 28 ? C1 N1 1.372(8) 28 ? C1 C1 1.395(12) 28 ? C1 C2 1.419(9) . ? C2 C1 1.419(9) 100_655 ? C2 H2 0.93 . ? C11 O22 1.4249 . ? C22 N11 1.498(10) 98 ? C22 C22 1.596(10) 30 ? C22 C22 1.596(10) 84 ? C22 C55 1.632(3) 23 ? C22 C55 1.631(3) 125 ? C33 C333 1.4199 . ? C33 C33 1.543(5) 84 ? C33 C33 1.543(5) 30 ? C44 N44 1.562(8) 23 ? C44 N44 1.5623 . ? C55 C88 1.4026 . ? C55 C77 1.5380 . ? C55 C22 1.631(3) 177 ? C55 C22 1.631(2) 84 ? C66 N44 1.3594 . ? C66 N44 1.359(5) 21 ? C66 N44 1.359(5) 23 ? C66 N44 1.3594 3 ? C66 N33 1.451(9) 98 ? C66 N33 1.4514 . ? C66 N33 1.451(9) 3 ? C66 N33 1.4515 100 ? C77 C55 1.537(7) 181 ? C88 C55 1.402(8) 181 ? C99 O33 1.7225 . ? C99 O33 1.722(7) 118 ? C99 O33 1.722(7) 21 ? C99 O33 1.722(14) 98 ? C111 N44 1.443(5) 23 ? C111 N33 1.4707 . ? C111 N33 1.4707 100 ? C222 O44 1.3251 . ? C222 N44 1.4918 . ? C222 N33 1.755(8) 98 ? C222 N33 1.7554 . ? C333 N22 1.4914 . ? C333 C333 1.674(5) 84 ? C333 C333 1.674(5) 30 ? O22 C55 1.727(7) 21 ? O22 C55 1.727(7) 23 ? O22 C55 1.7269 3 ? N11 N11 1.405(14) 99_565 ? N11 N11 1.407(14) 98 ? N11 N11 1.4069 100 ? N11 C22 1.497(15) 128_554 ? N11 C22 1.498(5) 177 ? N11 C22 1.498(10) 98 ? N22 C333 1.491(5) 84 ? N22 C333 1.4908 30 ? N33 C111 1.471(9) 21 ? N33 C222 1.7554(19) 23 ? N44 N44 1.3418 21 ? N44 N44 1.3418 23 ? N44 C111 1.443(5) 21 ? N44 C44 1.562(12) 98 ? 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 97.66(19) 35 . ? N1 Zn1 N1 97.66(19) 35 56 ? N1 Zn1 N1 97.66(19) . 56 ? N1 Zn1 Cl1 119.63(15) 35 . ? N1 Zn1 Cl1 119.63(15) . . ? N1 Zn1 Cl1 119.63(15) 56 . ? N2 Zn2 N2 90.0 58 . ? N2 Zn2 N2 90.000(1) 58 74 ? N2 Zn2 N2 180.0 . 74 ? N2 Zn2 N2 90.0 58 5 ? N2 Zn2 N2 90.000(1) . 5 ? N2 Zn2 N2 90.0 74 5 ? N2 Zn2 N2 90.0 58 30 ? N2 Zn2 N2 90.0 . 30 ? N2 Zn2 N2 90.000(1) 74 30 ? N2 Zn2 N2 180.000(1) 5 30 ? N2 Zn2 N2 180.0 58 9 ? N2 Zn2 N2 90.0 . 9 ? N2 Zn2 N2 90.0 74 9 ? N2 Zn2 N2 90.0 5 9 ? N2 Zn2 N2 90.0 30 9 ? N2 N1 C1 107.5(5) . 28 ? N2 N1 Zn1 120.9(4) . . ? C1 N1 Zn1 131.7(4) 28 . ? N1 N2 N1 111.9(7) 28 . ? N1 N2 Zn2 124.0(4) 28 . ? N1 N2 Zn2 124.0(4) . . ? N1 C1 C1 106.6(3) 28 28 ? N1 C1 C2 128.4(6) 28 . ? C1 C1 C2 125.0(4) 28 . ? C1 C2 C1 109.9(8) . 100_655 ? C1 C2 H2 125.0(3) . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 26.77 _diffrn_measured_fraction_theta_full 0.99 _refine_diff_density_max 0.977 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.113 # Attachment 'MFU-4_powder.cif' data_MFU-4_powder _database_code_depnum_ccdc_archive 'CCDC 723715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 Cl4 N18 Zn5' _chemical_formula_sum 'C18 Cl4 N18 Zn5' _chemical_formula_weight 937.03 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F m -3 m' _symmetry_space_group_name_Hall '-F 4 2 3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x,z 3 x,-y,-z 4 z,x,y 5 -x,-y,z 6 y,x,-z 7 -x,z,y 8 y,-x,z 9 -x,y,-z 10 -z,-x,y 11 -y,-x,-z 12 x,-z,y 13 z,-x,-y 14 x,z,-y 15 -z,x,-y 16 -x,-z,-y 17 z,-y,x 18 y,z,x 19 -z,y,x 20 -y,-z,x 21 z,y,-x 22 -y,z,-x 23 -z,-y,-x 24 y,-z,-x 25 -x,-y,-z 26 y,-x,-z 27 -x,y,z 28 -z,-x,-y 29 x,y,-z 30 -y,-x,z 31 x,-z,-y 32 -y,x,-z 33 x,-y,z 34 z,x,-y 35 y,x,z 36 -x,z,-y 37 -z,x,y 38 -x,-z,y 39 z,-x,y 40 x,z,y 41 -z,y,-x 42 -y,-z,-x 43 z,-y,-x 44 y,z,-x 45 -z,-y,x 46 y,-z,x 47 z,y,x 48 -y,z,x 49 x,1/2+y,1/2+z 50 -y,1/2+x,1/2+z 51 x,1/2-y,1/2-z 52 z,1/2+x,1/2+y 53 -x,1/2-y,1/2+z 54 y,1/2+x,1/2-z 55 -x,1/2+z,1/2+y 56 y,1/2-x,1/2+z 57 -x,1/2+y,1/2-z 58 -z,1/2-x,1/2+y 59 -y,1/2-x,1/2-z 60 x,1/2-z,1/2+y 61 z,1/2-x,1/2-y 62 x,1/2+z,1/2-y 63 -z,1/2+x,1/2-y 64 -x,1/2-z,1/2-y 65 z,1/2-y,1/2+x 66 y,1/2+z,1/2+x 67 -z,1/2+y,1/2+x 68 -y,1/2-z,1/2+x 69 z,1/2+y,1/2-x 70 -y,1/2+z,1/2-x 71 -z,1/2-y,1/2-x 72 y,1/2-z,1/2-x 73 -x,1/2-y,1/2-z 74 y,1/2-x,1/2-z 75 -x,1/2+y,1/2+z 76 -z,1/2-x,1/2-y 77 x,1/2+y,1/2-z 78 -y,1/2-x,1/2+z 79 x,1/2-z,1/2-y 80 -y,1/2+x,1/2-z 81 x,1/2-y,1/2+z 82 z,1/2+x,1/2-y 83 y,1/2+x,1/2+z 84 -x,1/2+z,1/2-y 85 -z,1/2+x,1/2+y 86 -x,1/2-z,1/2+y 87 z,1/2-x,1/2+y 88 x,1/2+z,1/2+y 89 -z,1/2+y,1/2-x 90 -y,1/2-z,1/2-x 91 z,1/2-y,1/2-x 92 y,1/2+z,1/2-x 93 -z,1/2-y,1/2+x 94 y,1/2-z,1/2+x 95 z,1/2+y,1/2+x 96 -y,1/2+z,1/2+x 97 1/2+x,y,1/2+z 98 1/2-y,x,1/2+z 99 1/2+x,-y,1/2-z 100 1/2+z,x,1/2+y 101 1/2-x,-y,1/2+z 102 1/2+y,x,1/2-z 103 1/2-x,z,1/2+y 104 1/2+y,-x,1/2+z 105 1/2-x,y,1/2-z 106 1/2-z,-x,1/2+y 107 1/2-y,-x,1/2-z 108 1/2+x,-z,1/2+y 109 1/2+z,-x,1/2-y 110 1/2+x,z,1/2-y 111 1/2-z,x,1/2-y 112 1/2-x,-z,1/2-y 113 1/2+z,-y,1/2+x 114 1/2+y,z,1/2+x 115 1/2-z,y,1/2+x 116 1/2-y,-z,1/2+x 117 1/2+z,y,1/2-x 118 1/2-y,z,1/2-x 119 1/2-z,-y,1/2-x 120 1/2+y,-z,1/2-x 121 1/2-x,-y,1/2-z 122 1/2+y,-x,1/2-z 123 1/2-x,y,1/2+z 124 1/2-z,-x,1/2-y 125 1/2+x,y,1/2-z 126 1/2-y,-x,1/2+z 127 1/2+x,-z,1/2-y 128 1/2-y,x,1/2-z 129 1/2+x,-y,1/2+z 130 1/2+z,x,1/2-y 131 1/2+y,x,1/2+z 132 1/2-x,z,1/2-y 133 1/2-z,x,1/2+y 134 1/2-x,-z,1/2+y 135 1/2+z,-x,1/2+y 136 1/2+x,z,1/2+y 137 1/2-z,y,1/2-x 138 1/2-y,-z,1/2-x 139 1/2+z,-y,1/2-x 140 1/2+y,z,1/2-x 141 1/2-z,-y,1/2+x 142 1/2+y,-z,1/2+x 143 1/2+z,y,1/2+x 144 1/2-y,z,1/2+x 145 1/2+x,1/2+y,z 146 1/2-y,1/2+x,z 147 1/2+x,1/2-y,-z 148 1/2+z,1/2+x,y 149 1/2-x,1/2-y,z 150 1/2+y,1/2+x,-z 151 1/2-x,1/2+z,y 152 1/2+y,1/2-x,z 153 1/2-x,1/2+y,-z 154 1/2-z,1/2-x,y 155 1/2-y,1/2-x,-z 156 1/2+x,1/2-z,y 157 1/2+z,1/2-x,-y 158 1/2+x,1/2+z,-y 159 1/2-z,1/2+x,-y 160 1/2-x,1/2-z,-y 161 1/2+z,1/2-y,x 162 1/2+y,1/2+z,x 163 1/2-z,1/2+y,x 164 1/2-y,1/2-z,x 165 1/2+z,1/2+y,-x 166 1/2-y,1/2+z,-x 167 1/2-z,1/2-y,-x 168 1/2+y,1/2-z,-x 169 1/2-x,1/2-y,-z 170 1/2+y,1/2-x,-z 171 1/2-x,1/2+y,z 172 1/2-z,1/2-x,-y 173 1/2+x,1/2+y,-z 174 1/2-y,1/2-x,z 175 1/2+x,1/2-z,-y 176 1/2-y,1/2+x,-z 177 1/2+x,1/2-y,z 178 1/2+z,1/2+x,-y 179 1/2+y,1/2+x,z 180 1/2-x,1/2+z,-y 181 1/2-z,1/2+x,y 182 1/2-x,1/2-z,y 183 1/2+z,1/2-x,y 184 1/2+x,1/2+z,y 185 1/2-z,1/2+y,-x 186 1/2-y,1/2-z,-x 187 1/2+z,1/2-y,-x 188 1/2+y,1/2+z,-x 189 1/2-z,1/2-y,x 190 1/2+y,1/2-z,x 191 1/2+z,1/2+y,x 192 1/2-y,1/2+z,x _cell_length_a 21.6265(9) _cell_length_b 21.6265(9) _cell_length_c 21.6265(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10114.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 623(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.2303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3619 _exptl_absorpt_coefficient_mu 4.933 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details '(Jana2000; Petricek, Dusek & Palatinus, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 623(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type "Philips X'Pert PRO" _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _pd_meas_number_of_points 3748 _pd_meas_2theta_range_min 5.020 _pd_meas_2theta_range_max 79.960 _pd_meas_2theta_range_inc 0.02 _reflns_number_total ? _reflns_number_gt ? _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Diffractometer software' _computing_cell_refinement PROSZKI _computing_data_reduction ? _computing_structure_solution EXPO2004 _computing_structure_refinement Jana200 _computing_molecular_graphics 'Mercury 1.4.2' _computing_publication_material 'DIAMOND 3.0' _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. ; _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr 'March & Dollase' _pd_proc_ls_prof_R_factor 0.0903 _pd_proc_ls_prof_wR_factor 0.1367 _pd_proc_ls_prof_wR_expected 0.0357 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'calc w=1/[\s(Y\i)]' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns ? _refine_ls_number_parameters ? _refine_ls_number_restraints ? _refine_ls_shift/su_max 0.0474 _refine_ls_shift/su_mean 0.0231 _refine_ls_R_factor_gt 0.1062 _refine_ls_wR_factor_gt 0.0881 _refine_ls_R_factor_all 0.1400 _refine_ls_wR_factor_ref 0.0881 _refine_ls_goodness_of_fit_ref ? _refine_ls_restrained_S_all ? _pd_proc_2theta_range_min 5.02 _pd_proc_2theta_range_max 79.96 _pd_proc_2theta_range_inc 0.02 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 0.2500 0.2500 0.2500 0.128(4) Uiso 1 8 d . . . Zn2 Zn 0.3443(2) 0.3443(2) 0.3443(2) 0.128(4) Uiso 1 32 d . . . Cl Cl 0.4062(4) 0.4062(4) 0.4062(4) 0.09(1) Uiso 1 32 d . . . N1 N 0.2881(5) 0.3816(7) 0.2881(5) 0.16(2) Uiso 1 96 d . . . N2 N 0.25 0.3559(9) 0.25 0.16(2) Uiso 1 48 d . . . C1 C 0.2998(10) 0.5 0.2998(10) 0.14(2) Uiso 1 48 d . . . C2 C 0.2752(8) 0.4461(8) 0.2752(8) 0.14(2) Uiso 1 96 d . . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 N2 . . 2.289(20) yes Zn1 N2 . 74_555 2.289(20) yes Zn1 N2 . 51_555 2.289(20) yes Zn1 N2 . 4_555 2.289(20) yes Zn1 N2 . 174_555 2.289(20) yes Zn1 N2 . 79_555 2.289(20) yes Zn2 Cl . . 2.319(10) yes Zn2 N1 . . 1.896(13) yes Zn2 N1 . 4_555 1.896(13) yes Zn2 N1 . 35_555 1.896(13) yes Zn2 N2 . . 2.893(5) yes Zn2 N2 . 74_555 2.893(5) yes Zn2 N2 . 4_555 2.893(5) yes N1 N1 . 4_555 2.858(19) yes N1 N1 . 105_555 2.332(15) yes N1 N1 . 35_555 2.858(19) yes N1 N2 . . 1.292(14) yes N1 C1 . . 2.584(15) yes N1 C2 . . 1.45(2) yes N1 C2 . 105_555 2.38(2) yes N2 C2 . . 2.10(3) yes N2 C2 . 105_555 2.10(3) yes C1 C2 . . 1.39(2) yes C1 C2 . 33_565 1.39(2) yes C2 C2 . 105_555 1.54(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 Zn1 N2 . . 74_555 90 yes N2 Zn1 N2 . . 51_555 180 yes N2 Zn1 N2 . . 4_555 90 yes N2 Zn1 N2 . . 174_555 90 yes N2 Zn1 N2 . . 79_555 90 yes N2 Zn1 N2 74_555 . . 90 yes N2 Zn1 N2 74_555 . 51_555 90 yes N2 Zn1 N2 74_555 . 4_555 90 yes N2 Zn1 N2 74_555 . 174_555 180 yes N2 Zn1 N2 74_555 . 79_555 90 yes N2 Zn1 N2 51_555 . . 180 yes N2 Zn1 N2 51_555 . 74_555 90 yes N2 Zn1 N2 51_555 . 4_555 90 yes N2 Zn1 N2 51_555 . 174_555 90 yes N2 Zn1 N2 51_555 . 79_555 90 yes N2 Zn1 N2 4_555 . . 90 yes N2 Zn1 N2 4_555 . 74_555 90 yes N2 Zn1 N2 4_555 . 51_555 90 yes N2 Zn1 N2 4_555 . 174_555 90 yes N2 Zn1 N2 4_555 . 79_555 180 yes N2 Zn1 N2 174_555 . . 90 yes N2 Zn1 N2 174_555 . 74_555 180 yes N2 Zn1 N2 174_555 . 51_555 90 yes N2 Zn1 N2 174_555 . 4_555 90 yes N2 Zn1 N2 174_555 . 79_555 90 yes N2 Zn1 N2 79_555 . . 90 yes N2 Zn1 N2 79_555 . 74_555 90 yes N2 Zn1 N2 79_555 . 51_555 90 yes N2 Zn1 N2 79_555 . 4_555 180 yes N2 Zn1 N2 79_555 . 174_555 90 yes Cl Zn2 N1 . . . 119.5(5) yes Cl Zn2 N1 . . 4_555 119.5(5) yes Cl Zn2 N1 . . 35_555 119.5(5) yes Cl Zn2 N2 . . . 139.7(5) yes Cl Zn2 N2 . . 74_555 139.7(5) yes Cl Zn2 N2 . . 4_555 139.7(5) yes N1 Zn2 N1 . . 4_555 97.8(6) yes N1 Zn2 N1 . . 35_555 97.8(6) yes N1 Zn2 N2 . . . 20.2(6) yes N1 Zn2 N2 . . 74_555 84.5(5) yes N1 Zn2 N2 . . 4_555 84.5(5) yes N1 Zn2 N1 4_555 . . 97.8(6) yes N1 Zn2 N1 4_555 . 35_555 97.8(6) yes N1 Zn2 N2 4_555 . . 84.5(5) yes N1 Zn2 N2 4_555 . 74_555 84.5(5) yes N1 Zn2 N2 4_555 . 4_555 20.2(6) yes N1 Zn2 N1 35_555 . . 97.8(6) yes N1 Zn2 N1 35_555 . 4_555 97.8(6) yes N1 Zn2 N2 35_555 . . 84.5(5) yes N1 Zn2 N2 35_555 . 74_555 20.2(6) yes N1 Zn2 N2 35_555 . 4_555 84.5(5) yes N2 Zn2 N2 . . 74_555 68.1(4) yes N2 Zn2 N2 . . 4_555 68.1(4) yes N2 Zn2 N2 74_555 . . 68.1(4) yes N2 Zn2 N2 74_555 . 4_555 68.1(4) yes N2 Zn2 N2 4_555 . . 68.1(4) yes N2 Zn2 N2 4_555 . 74_555 68.1(4) yes Zn2 N1 N1 . . 105_555 154.8(9) yes Zn2 N1 N2 . . . 129.3(13) yes Zn2 N1 C1 . . . 107.3(7) yes Zn2 N1 C2 . . . 131.1(11) yes Zn2 N1 C2 . . 105_555 169.4(9) yes N1 N1 N1 4_555 . 105_555 120.0(7) yes N1 N1 N1 4_555 . 35_555 60.0(4) yes N1 N1 N2 4_555 . . 98.5(10) yes N1 N1 C1 4_555 . . 129.2(7) yes N1 N1 C2 4_555 . . 144.8(10) yes N1 N1 C2 4_555 . 105_555 145.0(7) yes N1 N1 N1 105_555 . 4_555 120.0(7) yes N1 N1 N1 105_555 . 35_555 120.0(7) yes N1 N1 C1 105_555 . . 97.9(8) yes N1 N1 C2 105_555 . . 74.1(9) yes N1 N1 N1 35_555 . 4_555 60.0(4) yes N1 N1 N1 35_555 . 105_555 120.0(7) yes N1 N1 N2 35_555 . . 98.5(10) yes N1 N1 C1 35_555 . . 129.2(7) yes N1 N1 C2 35_555 . . 144.8(10) yes N1 N1 C2 35_555 . 105_555 145.0(7) yes N2 N1 C1 . . . 123.4(12) yes N2 N1 C2 . . . 99.6(13) yes N2 N1 C2 . . 105_555 61.2(10) yes C1 N1 C2 . . 105_555 62.1(7) yes Zn1 N2 Zn2 . . . 85.0(4) yes Zn1 N2 Zn2 . . 128_555 85.0(4) yes Zn1 N2 N1 . . . 115.5(10) yes Zn1 N2 N1 . . 105_555 115.5(10) yes Zn1 N2 C2 . . . 158.5(5) yes Zn1 N2 C2 . . 105_555 158.5(5) yes Zn2 N2 Zn2 . . 128_555 170.0(8) yes Zn2 N2 N1 . . 105_555 159.5(13) yes Zn2 N2 C2 . . . 73.5(5) yes Zn2 N2 C2 . . 105_555 116.5(8) yes Zn2 N2 Zn2 128_555 . . 170.0(8) yes Zn2 N2 N1 128_555 . . 159.5(13) yes Zn2 N2 C2 128_555 . . 116.5(8) yes Zn2 N2 C2 128_555 . 105_555 73.5(5) yes N1 N2 N1 . . 105_555 129.0(18) yes N1 N2 C2 . . 105_555 86.0(13) yes N1 N2 N1 105_555 . . 129.0(18) yes N1 N2 C2 105_555 . . 86.0(13) yes N1 C1 N1 . . 33_565 164.2(10) yes N1 C1 C2 . . 121_565 109.1(8) yes N1 C1 C2 . . 105_555 55.1(5) yes N1 C1 C2 . . 33_565 139.3(14) yes N1 C1 N1 33_565 . . 164.2(10) yes N1 C1 C2 33_565 . . 139.3(14) yes N1 C1 C2 33_565 . 121_565 55.1(5) yes N1 C1 C2 33_565 . 105_555 109.1(8) yes C2 C1 C2 . . 121_565 84.1(13) yes C2 C1 C2 . . 33_565 114.3(18) yes C2 C1 C2 121_565 . . 84.1(13) yes C2 C1 C2 121_565 . 105_555 54.0(7) yes C2 C1 C2 105_555 . 121_565 54.0(7) yes C2 C1 C2 105_555 . 33_565 84.1(13) yes C2 C1 C2 33_565 . . 114.3(18) yes C2 C1 C2 33_565 . 105_555 84.1(13) yes N1 C2 N1 . . 105_555 70.1(9) yes N1 C2 C1 . . . 131.3(15) yes N1 C2 C1 . . 121_565 132.9(11) yes N1 C2 C2 . . 121_565 162.5(12) yes N1 C2 C2 . . 105_555 105.9(13) yes N1 C2 C2 . . 33_565 164.1(13) yes N1 C2 N1 105_555 . . 70.1(9) yes N1 C2 C1 105_555 . . 158.6(14) yes N1 C2 C1 105_555 . 121_565 62.7(6) yes N1 C2 C2 105_555 . 121_565 92.4(7) yes N1 C2 C2 105_555 . 33_565 125.8(9) yes N2 C2 C1 . . . 168.7(14) yes N2 C2 C1 . . 121_565 95.5(7) yes N2 C2 C2 . . 121_565 125.1(8) yes N2 C2 C2 . . 105_555 68.5(9) yes N2 C2 C2 . . 33_565 158.5(10) yes C1 C2 C1 . . 121_565 95.9(12) yes C1 C2 C2 . . 121_565 66.2(11) yes C1 C2 C2 . . 105_555 122.8(15) yes C1 C2 C1 121_565 . . 95.9(12) yes C1 C2 C2 121_565 . 33_565 63.0(6) yes C2 C2 C2 121_565 . 105_555 56.6(9) yes C2 C2 C2 105_555 . 121_565 56.6(9) yes C2 C2 C2 105_555 . 33_565 90 yes C2 C2 C2 33_565 . 105_555 90 yes #END # Attachment 'bis686.cif' data_bis686 _database_code_depnum_ccdc_archive 'CCDC 723716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H1 Cl1 N3 Zn1, (C4 H9 N1 O1)' _chemical_formula_sum 'C7 H10 Cl1 N4 O1 Zn1' _chemical_formula_weight 267.01 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.812(2) _cell_length_b 8.6012(17) _cell_length_c 12.571(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.91(3) _cell_angle_gamma 90.00 _cell_volume 1053.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block-shaped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 2.558 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11882 _diffrn_reflns_av_R_equivalents 0.1948 _diffrn_reflns_av_sigmaI/netI 0.1163 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.95 _reflns_number_total 1920 _reflns_number_gt 1126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE EXPOSE' _computing_cell_refinement 'STOE CELL' _computing_data_reduction 'STOE INTEGRATE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.4.2' _computing_publication_material 'DIAMOND 3.0' _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^)+(0.0911P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1920 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _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 0.67061(9) 0.09534(9) 0.19691(6) 0.0364(3) Uani 1 1 d . . . Cl2 Cl 0.8786(2) 0.1417(3) 0.27857(18) 0.0649(6) Uani 1 1 d . . . N1 N 0.5650(6) -0.0228(7) 0.2964(4) 0.0364(14) Uani 1 1 d . . . N2 N 0.5024(6) -0.1554(7) 0.2659(4) 0.0379(14) Uani 1 1 d . . . N3 N 0.5614(6) 0.2861(7) 0.1565(4) 0.0365(14) Uani 1 1 d . . . O1 O 0.6913(6) -0.0082(6) 0.0608(4) 0.0522(14) Uani 1 1 d . . . C1 C 0.5397(8) 0.3848(7) 0.0687(5) 0.0337(15) Uani 1 1 d . . . C2 C 0.5418(7) 0.0060(8) 0.4015(4) 0.0350(16) Uani 1 1 d . . . C3 C 0.5853(8) 0.3725(8) -0.0317(5) 0.0374(17) Uani 1 1 d . . . H3 H 0.6392 0.2910 -0.0514 0.045 Uiso 1 1 calc R . . C4 C 0.7606(8) -0.1288(9) 0.0464(5) 0.048(2) Uani 1 1 d . . . N4 N 0.8231(8) -0.1420(8) -0.0385(5) 0.0530(18) Uani 1 1 d . . . C5 C 0.9023(11) -0.2792(11) -0.0609(7) 0.073(3) Uani 1 1 d . . . H5A H 0.9398 -0.2649 -0.1273 0.109 Uiso 1 1 calc R . . H5B H 0.8435 -0.3688 -0.0662 0.109 Uiso 1 1 calc R . . H5C H 0.9755 -0.2943 -0.0040 0.109 Uiso 1 1 calc R . . C6 C 0.7704(10) -0.2565(11) 0.1281(6) 0.063(2) Uani 1 1 d . . . H6A H 0.8256 -0.3395 0.1054 0.095 Uiso 1 1 calc R . . H6B H 0.6801 -0.2948 0.1354 0.095 Uiso 1 1 calc R . . H6C H 0.8118 -0.2170 0.1958 0.095 Uiso 1 1 calc R . . C7 C 0.8149(13) -0.0148(12) -0.1154(7) 0.085(3) Uani 1 1 d . . . H7A H 0.8662 -0.0411 -0.1732 0.128 Uiso 1 1 calc R . . H7B H 0.8524 0.0778 -0.0806 0.128 Uiso 1 1 calc R . . H7C H 0.7207 0.0029 -0.1430 0.128 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0435(6) 0.0388(5) 0.0278(4) 0.0026(3) 0.0079(3) 0.0023(4) Cl2 0.0501(15) 0.0764(16) 0.0666(13) 0.0022(11) -0.0001(10) -0.0068(11) N1 0.040(4) 0.043(3) 0.028(3) 0.006(2) 0.012(2) -0.005(3) N2 0.050(4) 0.038(3) 0.028(3) 0.002(2) 0.011(2) -0.009(3) N3 0.038(4) 0.043(3) 0.029(3) 0.004(2) 0.008(2) 0.007(3) O1 0.068(4) 0.053(3) 0.036(3) -0.001(2) 0.008(2) 0.018(3) C1 0.041(4) 0.037(4) 0.024(3) 0.000(3) 0.005(3) 0.006(3) C2 0.042(5) 0.042(4) 0.022(3) 0.000(3) 0.007(3) 0.000(3) C3 0.042(5) 0.035(4) 0.035(3) -0.002(3) 0.005(3) 0.010(3) C4 0.046(6) 0.063(6) 0.035(4) -0.004(3) 0.004(3) 0.004(4) N4 0.065(5) 0.058(4) 0.037(3) -0.007(3) 0.009(3) 0.010(3) C5 0.093(9) 0.071(6) 0.057(5) -0.003(4) 0.018(5) 0.030(6) C6 0.063(7) 0.074(6) 0.054(5) 0.011(4) 0.015(4) 0.010(5) C7 0.139(11) 0.075(7) 0.046(5) 0.011(5) 0.027(5) 0.019(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.961(5) . ? Zn1 N3 1.992(6) . ? Zn1 N1 1.995(5) . ? Zn1 Cl2 2.207(3) . ? N1 N2 1.330(8) . ? N1 C2 1.390(8) . ? N2 N3 1.320(7) 2_645 ? N3 N2 1.320(7) 2_655 ? N3 C1 1.388(8) . ? O1 C4 1.265(9) . ? C1 C3 1.392(9) . ? C1 C2 1.393(9) 2_655 ? C2 C3 1.377(9) 4_566 ? C2 C1 1.393(9) 2_645 ? C3 C2 1.377(9) 4_565 ? C4 N4 1.299(9) . ? C4 C6 1.498(11) . ? N4 C7 1.456(11) . ? N4 C5 1.459(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N3 105.1(2) . . ? O1 Zn1 N1 115.6(2) . . ? N3 Zn1 N1 106.0(2) . . ? O1 Zn1 Cl2 107.51(19) . . ? N3 Zn1 Cl2 114.11(19) . . ? N1 Zn1 Cl2 108.73(19) . . ? N2 N1 C2 107.7(5) . . ? N2 N1 Zn1 120.9(4) . . ? C2 N1 Zn1 131.5(5) . . ? N3 N2 N1 111.0(5) 2_645 . ? N2 N3 C1 108.3(5) 2_655 . ? N2 N3 Zn1 114.5(4) 2_655 . ? C1 N3 Zn1 137.1(4) . . ? C4 O1 Zn1 127.7(4) . . ? N3 C1 C3 129.7(6) . . ? N3 C1 C2 106.3(5) . 2_655 ? C3 C1 C2 123.9(6) . 2_655 ? C3 C2 N1 129.9(6) 4_566 . ? C3 C2 C1 123.4(6) 4_566 2_645 ? N1 C2 C1 106.7(5) . 2_645 ? C2 C3 C1 112.7(6) 4_565 . ? O1 C4 N4 120.3(7) . . ? O1 C4 C6 119.6(7) . . ? N4 C4 C6 120.1(7) . . ? C4 N4 C7 119.1(7) . . ? C4 N4 C5 123.0(7) . . ? C7 N4 C5 117.9(7) . . ? _diffrn_measured_fraction_theta_max 0.99 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.919 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.138