#------------------------------------------------------------------------------ #$Date: 2012-02-26 23:34:47 +0200 (Sun, 26 Feb 2012) $ #$Revision: 35909 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/55/7015590.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7015590 loop_ _publ_author_name 'Liu, Ying-Ya' 'Grzywa, Maciej' 'Tonigold, Markus' 'Sastre, German' 'Sch\"uttrigkeit, Tanja' 'Leeson, Nicholas S.' 'Volkmer, Dirk' _publ_section_title ; Photophysical properties of Kuratowski-type coordination compounds [M(II)Zn(4)Cl(4)(Me(2)bta)(6)] (M(II) = Zn or Ru) featuring long-lived excited electronic states. ; _journal_issue 22 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 5926 _journal_page_last 5938 _journal_volume 40 _journal_year 2011 _chemical_formula_moiety 'C12 H12 Cl4 N18 Zn5' _chemical_formula_sum 'C12 H12 Cl4 N18 Zn5' _chemical_formula_weight 877.04 _space_group_IT_number 88 _symmetry_cell_setting tetragonal _symmetry_Int_Tables_number 88 _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method shelxl-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.937(3) _cell_length_b 14.937(3) _cell_length_c 12.059(3) _cell_measurement_reflns_used 13772 _cell_measurement_temperature 220(2) _cell_measurement_theta_max 25.80 _cell_measurement_theta_min 2.17 _cell_volume 2690.5(10) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 220(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type mok\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 13772 _diffrn_reflns_theta_full 25.80 _diffrn_reflns_theta_max 25.80 _diffrn_reflns_theta_min 2.17 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'STOE IPDS' _exptl_absorpt_coefficient_mu 4.833 _exptl_absorpt_correction_T_max 0.6184 _exptl_absorpt_correction_T_min 0.2610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1712 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.446 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 89 _refine_ls_number_reflns 1300 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0225 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(fo^2^)+(0.0221p)^2^+4.7530p] where p=(fo^2^+2fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.0495 _reflns_number_gt 1113 _reflns_number_total 1300 _reflns_threshold_expression >2sigma(i) _[local]_cod_data_source_file c0dt01750g.txt _[local]_cod_data_source_block lin739 _[local]_cod_cif_authors_sg_H-M 'I 41/a' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_structure_factor_coef' value 'fsqd' changed to 'Fsqd' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_atom_site_adp_type' value 'uani' changed to 'Uani' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (11 times). '_atom_site_adp_type' value 'uiso' changed to 'Uiso' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (3 times). Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_database_code 7015590 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 zn 0.5000 0.7500 0.1250 0.01643(14) Uani 1 4 d S . . Zn2 zn 0.680260(18) 0.821942(19) -0.04521(3) 0.02202(12) Uani 1 1 d . . . Cl1 cl 0.79087(5) 0.86593(5) -0.14618(7) 0.0389(2) Uani 1 1 d . . . N1 n 0.5000 0.7500 -0.0549(2) 0.0206(6) Uani 1 2 d S . . N2 n 0.56780(13) 0.77574(13) -0.11948(18) 0.0204(4) Uani 1 1 d . . . N3 n 0.44423(13) 0.61550(13) 0.12251(18) 0.0202(4) Uani 1 1 d . . . N4 n 0.62222(14) 0.91226(14) 0.05805(18) 0.0224(5) Uani 1 1 d . . . N5 n 0.70270(13) 0.72227(14) 0.06555(18) 0.0213(5) Uani 1 1 d . . . C1 c 0.54293(17) 0.76649(17) -0.2257(2) 0.0246(6) Uani 1 1 d . . . H1 h 0.5777 0.7801 -0.2885 0.030 Uiso 1 1 calc R . . C2 c 0.63676(18) 0.99906(17) 0.0790(2) 0.0281(6) Uani 1 1 d . . . H2 h 0.6801 1.0356 0.0453 0.034 Uiso 1 1 calc R . . C3 c 0.77453(17) 0.67324(18) 0.0915(2) 0.0269(6) Uani 1 1 d . . . H3 h 0.8321 0.6790 0.0607 0.032 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 0.01622(18) 0.01622(18) 0.0168(3) 0.000 0.000 0.000 zn2 0.01934(17) 0.02339(17) 0.02333(18) 0.00190(12) 0.00526(12) -0.00177(12) cl1 0.0290(4) 0.0424(4) 0.0452(5) 0.0105(3) 0.0177(3) -0.0015(3) N1 0.0176(14) 0.0224(15) 0.0219(16) 0.000 0.000 -0.0043(12) N2 0.0199(10) 0.0210(10) 0.0203(11) 0.0014(9) 0.0051(9) -0.0012(8) N3 0.0193(10) 0.0192(10) 0.0222(11) 0.0022(9) -0.0044(9) 0.0008(8) N4 0.0216(11) 0.0229(11) 0.0225(12) 0.0018(9) 0.0043(9) -0.0015(8) N5 0.0201(10) 0.0217(11) 0.0222(12) 0.0010(9) 0.0043(9) -0.0029(9) C1 0.0330(14) 0.0242(13) 0.0165(13) 0.0011(10) 0.0021(11) 0.0064(11) C2 0.0291(14) 0.0205(13) 0.0348(16) 0.0030(11) -0.0005(12) -0.0082(11) C3 0.0164(12) 0.0303(14) 0.0340(16) -0.0027(12) 0.0019(11) 0.0006(11) 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' cl cl 0.1484 0.1585 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 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 180.0 15_565 . ? n1 zn1 n3 89.21(6) 15_565 12_766 ? n1 zn1 n3 90.79(6) . 12_766 ? n1 zn1 n3 90.79(6) 15_565 6_564 ? n1 zn1 n3 89.21(6) . 6_564 ? n3 zn1 n3 90.011(2) 12_766 6_564 ? n1 zn1 n3 90.79(6) 15_565 . ? n1 zn1 n3 89.21(6) . . ? n3 zn1 n3 90.011(2) 12_766 . ? n3 zn1 n3 178.42(12) 6_564 . ? n1 zn1 n3 89.21(6) 15_565 15_565 ? n1 zn1 n3 90.79(6) . 15_565 ? n3 zn1 n3 178.42(12) 12_766 15_565 ? n3 zn1 n3 90.011(2) 6_564 15_565 ? n3 zn1 n3 90.011(2) . 15_565 ? n2 zn2 n5 100.26(8) . . ? n2 zn2 n4 98.25(8) . . ? n5 zn2 n4 98.89(9) . . ? n2 zn2 cl1 119.34(7) . . ? n5 zn2 cl1 117.98(6) . . ? n4 zn2 cl1 118.12(6) . . ? n2 n1 n2 108.6(3) . 6_564 ? n2 n1 zn1 125.72(14) . . ? n2 n1 zn1 125.72(14) 6_564 . ? n1 n2 c1 108.5(2) . . ? n1 n2 zn2 118.01(17) . . ? c1 n2 zn2 133.43(17) . . ? n4 n3 n5 108.96(19) 6_564 15_565 ? n4 n3 zn1 125.66(15) 6_564 . ? n5 n3 zn1 125.36(15) 15_565 . ? n3 n4 c2 108.3(2) 6_564 . ? n3 n4 zn2 118.10(15) 6_564 . ? c2 n4 zn2 133.63(18) . . ? n3 n5 c3 108.1(2) 12_766 . ? n3 n5 zn2 118.31(15) 12_766 . ? c3 n5 zn2 133.57(18) . . ? n2 c1 c1 107.19(14) . 6_564 ? n4 c2 c3 107.2(2) . 12_766 ? n5 c3 c2 107.5(2) . 15_565 ? 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 2.169(3) 15_565 ? Zn1 N1 2.169(3) . ? Zn1 N3 2.175(2) 12_766 ? Zn1 N3 2.175(2) 6_564 ? Zn1 N3 2.175(2) . ? Zn1 N3 2.175(2) 15_565 ? Zn2 N2 2.025(2) . ? Zn2 N5 2.028(2) . ? Zn2 N4 2.030(2) . ? Zn2 Cl1 2.1551(8) . ? N1 N2 1.334(3) . ? N1 N2 1.334(3) 6_564 ? N2 C1 1.341(3) . ? N3 N4 1.327(3) 6_564 ? N3 N5 1.331(3) 15_565 ? N4 N3 1.327(3) 6_564 ? N4 C2 1.339(3) . ? N5 C3 1.336(3) . ? C1 C1 1.374(5) 6_564 ? C2 C3 1.367(4) 12_766 ?