#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/23/2012399.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012399 loop_ _publ_author_name 'Tian-Huey Lu' 'Yung-Jan Lin' 'Hung Luh' 'Fen-Ling Liao' 'Chung-Sun Chung' _publ_section_title ; A linear cyclic oximate-bridged tetracopper(II) complex ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1398 _journal_page_last 1399 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu4 (C6 H12 N8 O)4] (Cl O4)4, 0.6H2 O' _chemical_formula_moiety 'C24 H48 Cu4 N12 O4 4+, 4Cl O4 -, 0.6H2 O' _chemical_formula_sum 'C24 H50 Cl4 Cu4 N12 O20.6' _chemical_formula_weight 1232.32 _chemical_name_systematic ; ? ; _space_group_IT_number 86 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4bc' _symmetry_space_group_name_H-M 'P 42/n :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 2 _cell_length_a 12.440(3) _cell_length_b 12.440 _cell_length_c 14.851(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.31 _cell_measurement_theta_min 5.35 _cell_volume 2298.2(12) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'NRCVAX (Gabe et al., 1989)' _computing_molecular_graphics NRCVAX _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) and NRCVAX' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0000 _diffrn_reflns_av_sigmaI/netI .0456 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3349 _diffrn_reflns_theta_full 29.98 _diffrn_reflns_theta_max 29.98 _diffrn_reflns_theta_min 2.14 _diffrn_standards_decay_% 3 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.146 _exptl_absorpt_correction_T_max .54 _exptl_absorpt_correction_T_min .37 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour Black _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'square bipyramidal' _exptl_crystal_F_000 1260 _exptl_crystal_size_max .47 _exptl_crystal_size_mid .34 _exptl_crystal_size_min .29 _refine_diff_density_max 1.310 _refine_diff_density_min -.737 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 153 _refine_ls_number_reflns 3349 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all .1249 _refine_ls_R_factor_gt .0660 _refine_ls_shift/su_max .031 _refine_ls_shift/su_mean .019 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .1653 _refine_ls_wR_factor_ref .1834 _reflns_number_gt 1710 _reflns_number_total 3349 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ta1319.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 42/n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012399 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu .57965(4) .75901(4) .19143(3) .0455(2) Uani d . 1 . . Cu Cl .36504(11) -.05427(12) .27656(10) .0689(4) Uani d . 1 . . Cl O1 .6149(3) .7823(2) .31724(18) .0464(7) Uani d . 1 . . O O2 .4544(3) -.0699(4) .2175(3) .0825(12) Uani d . 1 . . O O3 .3256(6) -.1522(5) .3059(5) .174(3) Uani d . 1 . . O O4 .2841(4) .0031(6) .2328(4) .149(2) Uani d . 1 . . O O5 .3975(5) .0029(6) .3523(4) .139(2) Uani d . 1 . . O OW .7500 .7500 .6558(15) .221(14) Uani d SP .30(3) . . O N1 .4520(3) .6624(3) .2065(3) .0566(10) Uani d . 1 . . N H1A .4722 .5996 .2314 .068 Uiso calc R 1 . . H H1B .4031 .6936 .2428 .068 Uiso calc R 1 . . H N2 .5295(3) .7720(3) .0683(3) .0552(10) Uani d . 1 . . N N3 .6919(3) .8554(3) .1407(2) .0423(8) Uani d . 1 . . N C1 .4056(6) .6438(6) .1174(4) .103(3) Uani d . 1 . . C H2A .4331 .5760 .0947 .123 Uiso calc R 1 . . H H2B .3284 .6361 .1241 .123 Uiso calc R 1 . . H C2 .4252(5) .7224(6) .0538(4) .087(2) Uani d . 1 . . C H3A .3696 .7769 .0572 .104 Uiso calc R 1 . . H H3B .4230 .6909 -.0059 .104 Uiso calc R 1 . . H C3 .5803(4) .8361(4) .0179(3) .0574(12) Uani d . 1 . . C C4 .5456(6) .8705(6) -.0739(4) .103(3) Uani d . 1 . . C H4A .4747 .8435 -.0857 .123 Uiso calc R 1 . . H H4B .5947 .8426 -.1179 .123 Uiso calc R 1 . . H H4C .5449 .9476 -.0770 .123 Uiso calc R 1 . . H C5 .7629(5) .9393(5) .0051(4) .0780(18) Uani d . 1 . . C H5A .7460 1.0145 .0068 .094 Uiso calc R 1 . . H H5B .7630 .9149 -.0563 .094 Uiso calc R 1 . . H H5C .8327 .9278 .0310 .094 Uiso calc R 1 . . H C6 .6812(4) .8782(4) .0573(3) .0487(11) Uani d . 1 . . C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu .0509(3) .0544(4) .0312(3) -.0061(2) -.0043(2) .0055(2) Cl .0638(8) .0758(9) .0669(8) .0017(7) .0049(7) -.0011(7) O1 .0584(18) .0494(17) .0315(14) .0025(13) -.0040(13) .0049(12) O2 .081(3) .090(3) .076(3) .015(2) .023(2) .014(2) O3 .171(7) .103(4) .249(9) -.026(4) .125(6) -.014(5) O4 .092(4) .259(8) .094(4) .063(5) -.003(3) .014(5) O5 .119(4) .217(7) .081(3) -.030(5) .003(3) -.062(4) OW .25(3) .18(2) .23(2) -.080(17) .000 .000 N1 .063(2) .058(2) .049(2) -.0108(19) -.0078(18) .0078(18) N2 .060(2) .067(3) .039(2) -.011(2) -.0141(17) .0044(18) N3 .050(2) .0439(18) .0328(17) -.0005(15) -.0055(15) .0037(14) C1 .103(5) .139(6) .066(4) -.059(5) -.027(4) .013(4) C2 .075(4) .128(6) .058(3) -.041(4) -.021(3) .017(4) C3 .077(3) .060(3) .035(2) -.007(2) -.012(2) .005(2) C4 .123(6) .139(6) .046(3) -.038(5) -.034(4) .032(4) C5 .096(4) .097(4) .041(3) -.031(3) -.003(3) .019(3) C6 .063(3) .052(3) .032(2) -.005(2) -.0030(19) .0029(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu N2 . 1.939(4) y Cu O1 . 1.941(3) y Cu N3 . 1.989(3) y Cu N1 . 2.004(4) y Cl O3 . 1.383(6) ? Cl O5 . 1.391(5) ? Cl O4 . 1.395(6) ? Cl O2 . 1.429(4) ? O1 N3 8_756 1.339(4) ? N1 C1 . 1.462(7) ? N1 H1A . .9000 ? N1 H1B . .9000 ? N2 C3 . 1.264(6) ? N2 C2 . 1.452(6) ? N3 C6 . 1.278(5) ? N3 O1 6_576 1.339(4) ? C1 C2 . 1.382(8) ? C1 H2A . .9700 ? C1 H2B . .9700 ? C2 H3A . .9700 ? C2 H3B . .9700 ? C3 C6 . 1.480(6) ? C3 C4 . 1.492(6) ? C4 H4A . .9600 ? C4 H4B . .9600 ? C4 H4C . .9600 ? C5 C6 . 1.487(7) ? C5 H5A . .9600 ? C5 H5B . .9600 ? C5 H5C . .9600 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 Cu O1 . . 165.50(16) y N2 Cu N3 . . 79.54(15) y O1 Cu N3 . . 96.66(15) y N2 Cu N1 . . 84.26(16) y O1 Cu N1 . . 99.28(16) y N3 Cu N1 . . 163.78(15) y O3 Cl O5 . . 107.4(5) ? O3 Cl O4 . . 110.0(4) ? O5 Cl O4 . . 108.9(4) ? O3 Cl O2 . . 110.4(3) ? O5 Cl O2 . . 109.9(3) ? O4 Cl O2 . . 110.2(3) ? N3 O1 Cu 8_756 . 112.7(2) ? C1 N1 Cu . . 107.9(3) ? C1 N1 H1A . . 110.1 ? Cu N1 H1A . . 110.1 ? C1 N1 H1B . . 110.2 ? Cu N1 H1B . . 110.1 ? H1A N1 H1B . . 108.4 ? C3 N2 C2 . . 128.8(4) ? C3 N2 Cu . . 116.8(3) ? C2 N2 Cu . . 113.1(3) ? C6 N3 O1 . 6_576 118.6(3) ? C6 N3 Cu . . 115.3(3) ? O1 N3 Cu 6_576 . 125.4(2) ? C2 C1 N1 . . 115.9(5) ? C2 C1 H2A . . 108.3 ? N1 C1 H2A . . 108.3 ? C2 C1 H2B . . 108.3 ? N1 C1 H2B . . 108.3 ? H2A C1 H2B . . 107.4 ? C1 C2 N2 . . 110.9(5) ? C1 C2 H3A . . 109.5 ? N2 C2 H3A . . 109.4 ? C1 C2 H3B . . 109.4 ? N2 C2 H3B . . 109.5 ? H3A C2 H3B . . 108.0 ? N2 C3 C6 . . 114.4(4) ? N2 C3 C4 . . 125.3(5) ? C6 C3 C4 . . 120.3(5) ? C3 C4 H4A . . 109.5 ? C3 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? C3 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? C6 C5 H5A . . 109.5 ? C6 C5 H5B . . 109.5 ? H5A C5 H5B . . 109.5 ? C6 C5 H5C . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? N3 C6 C3 . . 113.1(4) ? N3 C6 C5 . . 123.2(4) ? C3 C6 C5 . . 123.7(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O2 8_656 .90 2.305 3.181(6) 164.2 yes N1 H1B O3 1_565 .90 2.343 3.158(8) 150.5 yes OW (H) O4 2_655 . . 3.305(10) . yes _journal_paper_doi 10.1107/S0108270101016456