#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2203263.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_2203263 loop_ _publ_author_name 'Goreshnik, Evgeny' 'Schollmeyer, Dieter' 'Mys'kiv, Marian' _publ_section_title ; Bis(2-methylbenzimidazole-\kN^1^)copper(I) dichlorocuprate(I) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m279 _journal_page_last m281 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Cu (C8 H8 N2)2] [Cu Cl2]' _chemical_formula_moiety 'C16 H16 Cu N4 1+, Cl2 Cu 1-' _chemical_formula_sum 'C16 H16 Cl2 Cu2 N4' _chemical_formula_weight 462.31 _chemical_name_systematic ; ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 112.628(10) _cell_angle_beta 98.786(11) _cell_angle_gamma 103.832(11) _cell_formula_units_Z 1 _cell_length_a 7.2510(10) _cell_length_b 7.4873(10) _cell_length_c 9.7058(13) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 73 _cell_measurement_theta_min 65 _cell_volume 454.32(12) _computing_cell_refinement 'CAD4- Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CORINC (Dr\"ager & Gattow, 1971)' _computing_molecular_graphics 'DIAMIND (Bergerhoff, 1996)' _computing_publication_material 'enCIFer (CCDC, 2002)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf--Nonius CAD-4' _diffrn_measurement_method \q/2\w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 1986 _diffrn_reflns_theta_full 73.95 _diffrn_reflns_theta_max 73.95 _diffrn_reflns_theta_min 5.13 _diffrn_standards_decay_% 3 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.626 _exptl_absorpt_correction_T_max 0.3991 _exptl_absorpt_correction_T_min 0.2118 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(de Meulanear & Tompa, 1965)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_meas 1.7 _exptl_crystal_density_method 'flotation in chloroform--bromoform' _exptl_crystal_description block _exptl_crystal_F_000 232 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.544 _refine_diff_density_min -0.481 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 1835 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.129 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0440 _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^)+(0.0731P)^2^+0.1751P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1217 _refine_ls_wR_factor_ref 0.1245 _reflns_number_gt 1676 _reflns_number_total 1835 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6405.cif _[local]_cod_data_source_block I _cod_original_cell_volume 454.32(11) _cod_database_code 2203263 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 0.0000 0.5000 0.5000 0.0496(2) Uani d S 1 Cu Cu2 0.0000 1.0000 0.0000 0.0655(2) Uani d S 1 Cu Cl1 0.19627(14) 1.23371(13) 0.20890(10) 0.0753(3) Uani d . 1 Cl N1 0.1253(3) 0.7437(3) 0.4913(2) 0.0433(4) Uani d . 1 N C2 0.1003(4) 0.7854(4) 0.3706(3) 0.0428(5) Uani d . 1 C N3 0.2082(3) 0.9796(3) 0.4082(2) 0.0449(5) Uani d . 1 N H3 0.2024 1.0414 0.3436 0.064(9) Uiso d R 1 H C4 0.3110(4) 1.0710(4) 0.5622(3) 0.0428(5) Uani d . 1 C C5 0.4421(4) 1.2658(4) 0.6577(4) 0.0518(6) Uani d . 1 C H5 0.4701 1.3767 0.6312 0.056(9) Uiso d R 1 H C6 0.5184(4) 1.3077(5) 0.8095(4) 0.0584(7) Uani d . 1 C H6 0.6048 1.4442 0.8828 0.076(11) Uiso d R 1 H C7 0.4662(5) 1.1588(5) 0.8637(4) 0.0622(7) Uani d . 1 C H7 0.5226 1.2119 0.9809 0.070(10) Uiso d R 1 H C8 0.3363(5) 0.9661(5) 0.7684(3) 0.0556(6) Uani d . 1 C H8 0.3075 0.8392 0.8006 0.112(17) Uiso d R 1 H C9 0.2578(3) 0.9216(4) 0.6142(3) 0.0421(5) Uani d . 1 C C10 -0.0267(5) 0.6406(5) 0.2116(3) 0.0562(7) Uani d . 1 C H10A -0.0189 0.7080 0.1451 0.138(13) Uiso calc R 1 H H10B -0.1609 0.5957 0.2147 0.138(13) Uiso calc R 1 H H10C 0.0178 0.5245 0.1721 0.138(13) 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 Cu1 0.0509(3) 0.0363(3) 0.0598(4) 0.0041(2) 0.0099(2) 0.0273(3) Cu2 0.0808(5) 0.0524(4) 0.0686(4) 0.0163(3) 0.0163(3) 0.0366(3) Cl1 0.0943(6) 0.0544(4) 0.0730(5) 0.0051(4) 0.0105(4) 0.0396(4) N1 0.0470(11) 0.0349(10) 0.0474(11) 0.0085(8) 0.0125(8) 0.0206(9) C2 0.0460(12) 0.0371(11) 0.0460(12) 0.0127(10) 0.0136(10) 0.0190(10) N3 0.0551(11) 0.0386(10) 0.0468(11) 0.0143(9) 0.0157(9) 0.0246(9) C4 0.0446(12) 0.0386(12) 0.0484(13) 0.0124(10) 0.0175(10) 0.0214(10) C5 0.0508(14) 0.0364(12) 0.0652(17) 0.0078(10) 0.0212(12) 0.0213(12) C6 0.0499(14) 0.0460(14) 0.0599(16) 0.0054(11) 0.0116(12) 0.0111(13) C7 0.0583(16) 0.0665(19) 0.0491(15) 0.0125(14) 0.0056(12) 0.0207(14) C8 0.0614(16) 0.0548(16) 0.0511(14) 0.0115(12) 0.0115(12) 0.0297(13) C9 0.0433(12) 0.0361(11) 0.0466(12) 0.0087(9) 0.0130(9) 0.0201(10) C10 0.0628(16) 0.0497(15) 0.0462(14) 0.0154(12) 0.0065(12) 0.0158(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 Cu1 N1 2_566 . 180.0 yes Cl1 Cu2 Cl1 . 2_575 180.0 yes C2 N1 C9 . . 106.0(2) yes C2 N1 Cu1 . . 127.52(17) no C9 N1 Cu1 . . 126.39(17) no N1 C2 N3 . . 111.4(2) yes N1 C2 C10 . . 125.8(2) yes N3 C2 C10 . . 122.8(2) yes C2 N3 C4 . . 108.4(2) yes C2 N3 H3 . . 124.7 no C4 N3 H3 . . 126.6 no N3 C4 C5 . . 131.9(2) yes N3 C4 C9 . . 105.3(2) yes C5 C4 C9 . . 122.8(2) yes C6 C5 C4 . . 116.7(3) yes C6 C5 H5 . . 117.2 no C4 C5 H5 . . 125.6 no C5 C6 C7 . . 121.2(3) yes C5 C6 H6 . . 120.1 no C7 C6 H6 . . 118.6 no C8 C7 C6 . . 121.8(3) yes C8 C7 H7 . . 124.0 no C6 C7 H7 . . 114.0 no C7 C8 C9 . . 117.6(3) yes C7 C8 H8 . . 124.2 no C9 C8 H8 . . 117.6 no N1 C9 C4 . . 108.9(2) yes N1 C9 C8 . . 131.1(2) yes C4 C9 C8 . . 120.0(2) yes C2 C10 H10A . . 109.5 no C2 C10 H10B . . 109.5 no H10A C10 H10B . . 109.5 no C2 C10 H10C . . 109.5 no H10A C10 H10C . . 109.5 no H10B C10 H10C . . 109.5 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 N1 2_566 1.874(2) yes Cu1 N1 . 1.874(2) yes Cu2 Cl1 . 2.0967(10) yes Cu2 Cl1 2_575 2.0967(10) yes N1 C2 . 1.321(3) yes N1 C9 . 1.391(3) yes C2 N3 . 1.349(3) yes C2 C10 . 1.486(4) yes N3 C4 . 1.373(3) yes N3 H3 . 0.9140 no C4 C5 . 1.385(4) yes C4 C9 . 1.393(3) yes C5 C6 . 1.373(4) yes C5 H5 . 0.9467 no C6 C7 . 1.405(5) yes C6 H6 . 0.9702 no C7 C8 . 1.372(5) yes C7 H7 . 1.0251 no C8 C9 . 1.393(4) yes C8 H8 . 1.0947 no C10 H10A . 0.9600 no C10 H10B . 0.9600 no C10 H10C . 0.9600 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N3 H3 Cl1 0.91 2.29 3.199(2) 173 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag C9 N1 C2 N3 -0.2(3) yes Cu1 N1 C2 N3 177.16(16) no C9 N1 C2 C10 179.0(2) yes Cu1 N1 C2 C10 -3.6(4) no N1 C2 N3 C4 0.3(3) yes C10 C2 N3 C4 -178.9(2) yes C2 N3 C4 C5 179.7(3) yes C2 N3 C4 C9 -0.3(3) yes N3 C4 C5 C6 179.5(3) yes C9 C4 C5 C6 -0.4(4) yes C4 C5 C6 C7 0.4(4) yes C5 C6 C7 C8 -0.5(5) yes C6 C7 C8 C9 0.5(5) yes C2 N1 C9 C4 0.0(3) yes Cu1 N1 C9 C4 -177.40(17) no C2 N1 C9 C8 179.6(3) no Cu1 N1 C9 C8 2.3(4) no N3 C4 C9 N1 0.2(3) yes C5 C4 C9 N1 -179.8(2) yes N3 C4 C9 C8 -179.5(2) yes C5 C4 C9 C8 0.5(4) yes C7 C8 C9 N1 179.9(3) yes C7 C8 C9 C4 -0.5(4) yes