#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/52/2005282.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_2005282 loop_ _publ_author_name 'Jackson, G. E.' 'Voy\'e, A.' 'Bourne, S. A.' _publ_section_title ; Bis[5,5-dichloro-4,6-dioxo-3,7-diaza-1,9-nonanediylbis(dimethylammonium)] Tetrachlorohexa-\m-chloro-\m~4~-oxo-tetracuprate(II) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1907 _journal_page_last 1908 _journal_paper_doi 10.1107/S0108270196002764 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '(C11 H24 Cl2 N4 O2)2 [Cu4 O Cl10]' _chemical_formula_moiety '2C11 H24 Cl2 N4 O2 , Cu4 O Cl10' _chemical_formula_sum 'C22 H48 Cl14 Cu4 N8 O5' _chemical_formula_weight 1255.2 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 99.61(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.405(2) _cell_length_b 15.805(2) _cell_length_c 20.644(5) _cell_measurement_reflns_used 24 _cell_measurement_temperature 293 _cell_measurement_theta_max 17 _cell_measurement_theta_min 16 _cell_volume 4634.1(14) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1988)' _computing_data_reduction 'CAD-4 Software' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1994)' _computing_structure_refinement 'SHELX76 (Sheldrick, 1978)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3708 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 5.5 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.66 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_type 'empirical, \y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_meas ? _exptl_crystal_description prism _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _refine_diff_density_max 1.28 _refine_diff_density_min 0.59 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_hydrogen_treatment 'H atoms: see text' _refine_ls_number_parameters 255 _refine_ls_number_reflns 3209 _refine_ls_R_factor_obs 0.049 _refine_ls_shift/esd_max 0.05 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1.538/[\s^2^(F)+0.001163F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.059 _reflns_number_observed 3209 _reflns_number_total 3658 _reflns_observed_criterion I>2\s(I) _cod_data_source_file na1210.cif _cod_data_source_block na1210a _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value ' 1.538/[\s^2^(F)+0.001163F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1.538/[\s^2^(F)+0.001163F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 4634(2) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2005282 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,1/2+z -x,-y,-z -x,y,1/2-z 1/2+x,1/2+y,z 1/2+x,1/2-y,1/2+z 1/2-x,1/2-y,-z 1/2-x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Cu1 .54254(1) .31763(1) .32472(2) .0422(1) Cu2 .60272(1) .45752(2) .23377(1) .0407(1) Cl1 .7270(1) .5321(1) .2110(1) .050(1) Cl2 .5832(1) .2355(1) .4133(1) .061(1) Cl3 .6871(1) .3956(1) .3315(1) .062(1) Cl4 .5738(1) .3980(1) .1250(1) .063(1) Cl5 .5 .5766(1) .25 .066(1) Cl6 .5 .2062(1) .25 .083(1) Cl7 .9781(1) .5144(1) .1685(1) .079(1) Cl8 1.0194(2) .4155(2) .0584(1) .094(1) O1A .5 .3880(3) .25 .031(1) C1 .6646(6) .7016(5) .0872(4) .074(3) C2 .5269(5) .6098(5) .0717(5) .078(3) N1 .6317(4) .6139(3) .0762(3) .053(2) C3 .6571(4) .5711(4) .0160(3) .053(2) C4 .7571(5) .5816(4) .0065(3) .053(2) N2 .8284(3) .5468(3) .0590(2) .045(2) C5 .8453(4) .4640(4) .0629(3) .049(2) O1 .7989(4) .4101(3) .0325(3) .078(2) C6 .9356(4) .4365(4) .1103(3) .053(2) O2 .9742(5) .2961(4) .1473(4) .109(3) C7 .9198(5) .3529(4) .1475(3) .054(2) N3 .8530(4) .3566(3) .1831(3) .062(2) C8 .8328(5) .2853(4) .2246(3) .061(2) C9 .7464(6) .2400(5) .2027(5) .080(3) N4 .7386(6) .1960(6) .1395(5) .121(5) C10 .6533(9) .152(1) .123(1) .33(2) C11 .809(1) .153(2) .1239(8) .24(1) H11 .7318(2) .70343(5) .0900(1) ? H12 .6479(2) .72225(5) .1275(1) ? H13 .6356(2) .73639(6) .0513(1) ? H21 .5063(2) .5523(1) .0645(2) ? H22 .4975(2) .6443(1) .0358(2) ? H23 .5098(2) .6302(1) .1119(2) ? H1N .6597(1) .5807(2) .1146(2) ? H31 .64401(4) .51110(7) .01858(8) ? H32 .61642(4) .59318(7) -.02248(9) ? H41 .76453(5) .55475(9) -.0345(1) ? H42 .76946(5) .64151(9) .0023(1) ? H2N .8595(2) .5803(1) .0875(2) ? H3N .8198(1) .4020(2) .1823(2) ? H81 .88458(5) .24545(6) .22788(7) ? H82 .83126(5) .30672(6) .26844(7) ? H91 .69464(6) .27982(4) .19992(6) ? H92 .73837(6) .19864(5) .23604(6) ? H4N .7319(3) .2426(2) .1078(1) ? 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 Cu1 O1A Cu2 . . 108.76(3) yes Cu1 O1A Cu2 . 4_655 110.09(3) yes Cl2 Cu1 Cl6 . . 96.07(6) yes Cl2 Cu1 Cl4 . 4_655 93.36(8) yes Cl2 Cu1 Cl3 . . 98.24(6) yes Cl4 Cu1 O1A 4_655 . 83.71(5) yes Cl6 Cu1 O1A . . 83.91(2) yes Cl3 Cu1 O1A . . 84.64(5) yes Cl2 Cu1 O1A . . 176.51(6) yes Cu1 Cl3 Cu2 . . 81.18(5) yes Cu2 Cl5 Cu2 . 4_655 79.70(3) yes N2 C5 C6 . . 116.0(5) yes N2 C5 O1 . . 126.1(6) yes O1 C5 C6 . . 117.9(6) yes Cl8 C6 C7 . . 107.9(4) yes Cu1 O1A Cu1 . 4_655 109.10(8) yes Cu2 O1A Cu2 . 4_655 110.08(5) yes Cl1 Cu2 Cl5 . . 98.35(6) yes Cl1 Cu2 Cl4 . . 91.74(7) yes Cl1 Cu2 Cl3 . . 94.59(6) yes Cl4 Cu2 O1A . . 85.48(5) yes Cl5 Cu2 O1A . . 85.11(3) yes Cl3 Cu2 O1A . . 85.16(4) yes Cl1 Cu2 O1A . . 176.25(5) yes Cu2 Cl4 Cu1 . 4_655 80.36(6) yes Cu1 Cl6 Cu1 . 4_655 83.13(2) yes C6 C7 N3 . . 114.8(5) yes O2 C7 N3 . . 125.6(7) yes C6 C7 O2 . . 119.0(6) yes C5 C6 C7 . . 111.8(5) yes Cl3 Cu1 Cl6 . . 123.30(10) no Cl4 Cu1 Cl6 4_655 . 122.70(10) no Cl3 Cu1 Cl4 4_655 . 110.80(10) no Cl3 Cu2 Cl5 . . 115.70(10) no Cl4 Cu2 Cl5 . . 114.50(10) no Cl3 Cu2 Cl4 . . 127.80(10) no C1 N1 C2 . . 110.2(5) no C2 N1 C3 . . 108.0(6) no C1 N1 C3 . . 115.6(5) no N1 C3 C4 . . 115.4(5) no C3 C4 N2 . . 115.6(5) no C4 N2 C5 . . 120.7(5) no Cl8 C6 C5 . . 104.7(4) no Cl7 C6 C5 . . 113.1(4) no Cl7 C6 Cl8 . . 110.4(4) no C10 N4 C11 . . 111.1(4) no C9 N4 C10 . . 113.0(10) no C9 N4 C11 . . 121.4(11) no C8 C9 N4 . . 116.7(7) no N3 C8 C9 . . 116.2(6) no C7 N3 C8 . . 121.9(6) no Cl7 C6 C7 . . 108.6(4) no 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 Cu1 Cl2 . 2.239(2) yes Cu1 O1A . 1.917(3) yes Cu1 Cl3 . 2.404(2) yes Cu1 Cl4 4_655 2.466(2) yes Cu1 Cl6 . 2.3530(10) yes N2 C5 . 1.331(8) yes C5 C6 . 1.554(8) yes C5 O1 . 1.194(8) yes Cl7 C6 . 1.758(6) yes Cu2 Cl1 . 2.257(2) yes Cu2 O1A . 1.917(3) yes Cu2 Cl3 4_655 2.386(2) yes Cu2 Cl4 . 2.404(2) yes Cu2 Cl5 . 2.4520(10) yes C7 N3 . 1.306(10) yes C6 C7 . 1.564(9) yes O2 C7 . 1.192(10) yes C6 Cl8 . 1.774(7) yes C1 N1 . 1.470(9) no C2 N1 . 1.498(9) no N1 C3 . 1.513(9) no C3 C4 . 1.495(10) no C4 N2 . 1.470(7) no N4 C11 . 1.30(2) no N4 C10 . 1.405(17) no C9 N4 . 1.466(14) no C8 C9 . 1.442(11) no N3 C8 . 1.473(9) no