#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202400.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_2202400 loop_ _publ_author_name 'Ana Mar\'ia Atria' . 'Piedad Cort\'es' . 'Mar\'ia Teresa Garland' . 'Ricardo Baggio' . _publ_section_title ; [Cu(2-Me-imidH)~4~Cl]Cl: a conflict between high symmetry and packing efficiency ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1075 _journal_page_last m1077 _journal_paper_doi 10.1107/S1600536803024553 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Cu Cl (C4 H6 N2)4] Cl' _chemical_formula_moiety 'C16 H24 Cl Cu N8 1+, Cl 1-' _chemical_formula_sum 'C16 H24 Cl2 Cu N8' _chemical_formula_weight 462.87 _chemical_name_systematic ; Chlorotetrakis(2-methylimidazole)copper(II) chloride ; _space_group_IT_number 104 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P 4 -2n' _symmetry_space_group_name_H-M 'P 4 n c' _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 9.8106(12) _cell_length_b 9.8106(12) _cell_length_c 10.8547(19) _cell_measurement_reflns_used 134 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.86 _cell_measurement_theta_min 3.10 _cell_volume 1044.7(3) _computing_cell_refinement SMART-NT _computing_data_collection 'SMART-NT (Bruker, 2001)' _computing_data_reduction 'SAINT-NT(Bruker, 2001)' _computing_molecular_graphics 'XP in SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 3889 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.80 _diffrn_standards_decay_% <2 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '[SADABS (Sheldrick, 1996) in SAINT-NT (Bruker, 2000)]' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plates _exptl_crystal_F_000 478 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.565 _refine_diff_density_min -0.328 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 64 _refine_ls_number_reflns 896 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.926 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0408 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0382P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.0853 _reflns_number_gt 670 _reflns_number_total 896 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt6371.cif _cod_data_source_block I _cod_database_code 2202400 _cod_database_fobs_code 2202400 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, 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 -0.5000 0.5000 1.09269(8) 0.0315(3) Uani d S 1 . . Cu Cl1 -0.5000 0.5000 0.8507(2) 0.0489(7) Uani d S 1 . . Cl Cl2 -0.5000 0.5000 1.4710(3) 0.0442(5) Uani d S 1 . . Cl N1 -0.3846(3) 0.3318(3) 1.1221(4) 0.0322(10) Uani d . 1 . . N C1 -0.4137(6) 0.2365(5) 1.2110(6) 0.0484(16) Uani d . 1 . . C H1A -0.4877 0.2407 1.2645 0.058 Uiso calc R 1 . . H C2 -0.3208(6) 0.1369(6) 1.2097(7) 0.0585(19) Uani d . 1 . . C H2A -0.3170 0.0608 1.2607 0.070 Uiso calc R 1 . . H N2 -0.2334(4) 0.1708(4) 1.1185(6) 0.0558(14) Uani d . 1 . . N H2B -0.1637 0.1235 1.0963 0.067 Uiso calc R 1 . . H C3 -0.2717(5) 0.2890(4) 1.0680(4) 0.0376(13) Uani d . 1 . . C C4 -0.1958(5) 0.3576(5) 0.9678(7) 0.0611(17) Uani d . 1 . . C H4A -0.2406 0.4413 0.9467 0.092 Uiso calc R 1 . . H H4B -0.1928 0.2992 0.8969 0.092 Uiso calc R 1 . . H H4C -0.1046 0.3767 0.9948 0.092 Uiso calc R 1 . . H 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 0.0258(4) 0.0258(4) 0.0431(7) 0.000 0.000 0.000 Cl1 0.0521(10) 0.0521(10) 0.0425(17) 0.000 0.000 0.000 Cl2 0.0382(7) 0.0382(7) 0.0562(15) 0.000 0.000 0.000 N1 0.0302(19) 0.0268(18) 0.040(3) -0.0019(17) 0.0052(19) 0.0055(19) C1 0.039(3) 0.044(3) 0.062(4) 0.007(3) 0.003(3) 0.014(3) C2 0.056(4) 0.049(4) 0.071(5) 0.007(3) -0.004(4) 0.027(4) N2 0.039(2) 0.038(2) 0.089(5) 0.017(2) 0.002(3) 0.004(3) C3 0.037(3) 0.033(3) 0.043(4) -0.002(2) 0.000(2) -0.003(2) C4 0.052(3) 0.064(4) 0.068(5) 0.012(3) 0.020(5) 0.005(5) 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' Cu Cu 0.3201 1.2651 '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 N1 Cu N1 4_455 3_565 161.9(2) ? N1 Cu N1 4_455 . 88.58(4) ? N1 Cu N1 3_565 . 88.58(4) y N1 Cu N1 4_455 2_465 88.58(4) ? N1 Cu N1 3_565 2_465 88.58(4) ? N1 Cu N1 . 2_465 161.9(2) ? N1 Cu Cl1 4_455 . 99.06(12) ? N1 Cu Cl1 3_565 . 99.06(12) ? N1 Cu Cl1 . . 99.06(12) y N1 Cu Cl1 2_465 . 99.06(12) ? C3 N1 C1 . . 105.7(4) ? C3 N1 Cu . . 131.0(3) ? C1 N1 Cu . . 123.3(3) ? C2 C1 N1 . . 110.4(6) ? C2 C1 H1A . . 124.8 ? N1 C1 H1A . . 124.8 ? C1 C2 N2 . . 105.1(6) ? C1 C2 H2A . . 127.4 ? N2 C2 H2A . . 127.4 ? C3 N2 C2 . . 109.6(4) ? C3 N2 H2B . . 125.2 ? C2 N2 H2B . . 125.2 ? N1 C3 N2 . . 109.2(4) ? N1 C3 C4 . . 127.2(4) ? N2 C3 C4 . . 123.7(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 ? 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 N1 4_455 2.027(3) ? Cu N1 3_565 2.027(3) ? Cu N1 . 2.027(3) y Cu N1 2_465 2.027(3) ? Cu Cl1 . 2.627(3) y N1 C3 . 1.322(5) y N1 C1 . 1.374(6) y C1 C2 . 1.337(7) y C1 H1A . 0.9300 ? C2 N2 . 1.351(7) y C2 H2A . 0.9300 ? N2 C3 . 1.337(6) y N2 H2B . 0.8600 ? C3 C4 . 1.480(7) y C4 H4A . 0.9600 ? C4 H4B . 0.9600 ? C4 H4C . 0.9600 ? 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 N2 H2B Cl2 5_554 0.86 2.43 3.258(5) 162