#------------------------------------------------------------------------------ #$Date: 2008-06-20 14:44:24 +0100 (Fri, 20 Jun 2008) $ #$Revision: 397 $ #$URL: svn://www.crystallography.net/cod/cif/2/2103782.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_2103782 loop_ _publ_author_name 'Clemente, Dore Augusto' 'Marzotto, Armando' _publ_section_title ; 22 Space-group changes ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 43 _journal_page_last 50 _journal_volume 59 _journal_year 2003 _chemical_formula_moiety 'C10 H20 Cl2 Cu N2 O4' _chemical_formula_sum 'C10 H20 Cl2 Cu N2 O4' _chemical_formula_weight 366.72 _chemical_name_systematic ; bis(Chloroacetato)-(N,N,N',N'-tetramethylethylenediamine) copper(ii) ; _space_group_IT_number 20 _symmetry_space_group_name_Hall 'C 2c 2' _symmetry_space_group_name_H-M 'C 2 2 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.002(3) _cell_length_b 11.400(5) _cell_length_c 14.846(7) _cell_measurement_temperature 293(2) _cell_volume 1523.5(11) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.338 _diffrn_measured_fraction_theta_max 0.338 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0060 _diffrn_reflns_av_sigmaI/netI 0.0927 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 8366 _diffrn_reflns_theta_full 45.64 _diffrn_reflns_theta_max 45.64 _diffrn_reflns_theta_min 2.74 _exptl_absorpt_coefficient_mu 1.794 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _refine_diff_density_max 0.104 _refine_diff_density_min -0.155 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.252 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 2103 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.252 _refine_ls_R_factor_all 0.0061 _refine_ls_R_factor_gt 0.0061 _refine_ls_shift/su_max 1.279 _refine_ls_shift/su_mean 0.016 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0422 _reflns_number_gt 2095 _reflns_number_total 2103 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file an0613.cif _[local]_cod_data_source_block claecu loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 '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' 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' 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_type_symbol Cu1 0.00000 0.103000(12) 0.25000 0.02000(4) Uiso d S 1 Cu N1 -0.14260(7) -0.02670(6) 0.21200(5) 0.02000(11) Uiso d . 1 N C1 -0.08360(8) -0.13590(7) 0.25390(7) 0.02000(12) Uiso d . 1 C H1 -0.1257(15) -0.2107(12) 0.2215(9) 0.020(3) Uiso d . 1 H H2 -0.1210(14) -0.1400(12) 0.3165(10) 0.020(3) Uiso d . 1 H C3 -0.15370(7) -0.04170(8) 0.11320(6) 0.02000(13) Uiso d . 1 C H5 -0.1915(15) 0.0310(11) 0.0870(8) 0.020(3) Uiso d . 1 H H6 -0.2118(13) -0.1108(11) 0.1010(9) 0.020(3) Uiso d . 1 H H7 -0.0608(14) -0.0527(11) 0.0830(9) 0.020(3) Uiso d . 1 H C4 -0.29120(8) 0.00080(7) 0.24880(6) 0.02000(13) Uiso d . 1 C H8 -0.3248(14) 0.0767(12) 0.2150(8) 0.020(3) Uiso d . 1 H H9 -0.3630(14) -0.0630(12) 0.2350(9) 0.020(3) Uiso d . 1 H H10 -0.2898(13) 0.0178(11) 0.3085(9) 0.020(3) Uiso d . 1 H O1 -0.10440(6) 0.22160(5) 0.17640(4) 0.02000(10) Uiso d . 1 O C7 -0.02140(7) 0.23430(7) 0.10700(6) 0.02000(12) Uiso d . 1 C C8 -0.08500(8) 0.32340(8) 0.04060(6) 0.02000(12) Uiso d . 1 C H17 -0.1833(13) 0.3037(12) 0.0180(8) 0.020(3) Uiso d . 1 H H18 -0.0920(12) 0.3990(13) 0.0710(8) 0.020(3) Uiso d . 1 H Cl1 0.025500(18) 0.341600(17) -0.057800(12) 0.02000(4) Uiso d . 1 Cl O2 0.09550(6) 0.18120(6) 0.09410(4) 0.02000(11) Uiso d . 1 O loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Cu1 O1 4 1.9761(8) Cu1 O1 . 1.9762(8) Cu1 N1 . 2.0377(9) Cu1 N1 4 2.0377(9) N1 C4 . 1.4786(11) N1 C3 . 1.4801(14) N1 C1 . 1.4895(12) C1 C1 4 1.5096(15) O1 C7 . 1.2809(10) C7 O2 . 1.2290(9) C7 C8 . 1.5268(12) C8 Cl1 . 1.7795(11) 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 O1 Cu1 O1 4 . 93.66(5) O1 Cu1 N1 4 . 161.64(3) O1 Cu1 N1 . . 92.51(4) O1 Cu1 N1 4 4 92.51(4) O1 Cu1 N1 . 4 161.64(3) N1 Cu1 N1 . 4 86.96(5) C4 N1 C3 . . 109.24(6) C4 N1 C1 . . 110.21(7) C3 N1 C1 . . 109.96(7) C4 N1 Cu1 . . 108.29(6) C3 N1 Cu1 . . 113.62(5) C1 N1 Cu1 . . 105.44(6) N1 C1 C1 . 4 108.87(6) C7 O1 Cu1 . . 104.16(5) O2 C7 O1 . . 124.69(8) O2 C7 C8 . . 123.24(8) O1 C7 C8 . . 112.07(6) C7 C8 Cl1 . . 113.45(6)