#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/32/2013221.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_2013221 loop_ _publ_author_name 'Clarke, Rachael' 'Latham, Kay' 'Rix, Colin' 'White, Jonathan' _publ_section_title ; Two polymorphs of bis(1,10-phenanthroline-\k^2^N,N')copper(I) iodide ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m7 _journal_page_last m9 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Cu (C12 H8 N2)2] I' _chemical_formula_moiety 'C24 H16 Cu N4 + , I -' _chemical_formula_sum 'C24 H16 Cu I N4' _chemical_formula_weight 550.85 _chemical_melting_point 'decomposition, greater than 373K' _chemical_name_systematic ; bis(1,10-phenanthroline-\k^2^N,N')copper(I) iodide ; _space_group_IT_number 50 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ab 2b' _symmetry_space_group_name_H-M 'P b a n :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.215(4) _cell_length_b 7.458(2) _cell_length_c 9.493(3) _cell_measurement_reflns_used 1677 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.74 _cell_measurement_theta_min 2.87 _cell_volume 1006.4(5) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_molecular_graphics 'SHELXTL and ZORTEP (Zsolnai, 1994)' _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 2001)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.027 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 5578 _diffrn_reflns_theta_full 27.54 _diffrn_reflns_theta_max 27.54 _diffrn_reflns_theta_min 2.15 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.638 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 540 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.20 _refine_diff_density_min -0.32 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.241 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 70 _refine_ls_number_reflns 1178 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.241 _refine_ls_R_factor_all 0.060 _refine_ls_R_factor_gt 0.046 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.9045P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.113 _refine_ls_wR_factor_ref 0.119 _reflns_number_gt 892 _reflns_number_total 1178 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ta1392.cif _[local]_cod_data_source_block Ia _[local]_cod_cif_authors_sg_H-M 'P b a n' _cod_database_code 2013221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x, -y+1/2, -z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x, y-1/2, z' 'x-1/2, -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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C1 0.8560(4) 0.1123(7) 0.7455(4) 0.0689(13) Uani d . 1 . . C H1 0.7983 0.0838 0.7049 0.083 Uiso calc R 1 . . H C2 0.9359(4) 0.0860(7) 0.6671(5) 0.0799(15) Uani d . 1 . . C H2 0.9320 0.0455 0.5747 0.096 Uiso calc R 1 . . H C3 1.0205(4) 0.1201(7) 0.7270(6) 0.0795(16) Uani d . 1 . . C H3 1.0756 0.1007 0.6762 0.095 Uiso calc R 1 . . H C4 1.0249(3) 0.1829(7) 0.8618(5) 0.0652(12) Uani d . 1 . . C C5 0.9408(3) 0.2126(5) 0.9312(4) 0.0493(9) Uani d . 1 . . C C6 1.1094(4) 0.2177(7) 0.9354(7) 0.0838(17) Uani d . 1 . . C H6 1.1666 0.1943 0.8915 0.101 Uiso calc R 1 . . H N 0.8564(2) 0.1751(5) 0.8739(3) 0.0555(8) Uani d . 1 . . N Cu 0.7500 0.2500 1.0000 0.0667(3) Uani d S 1 . . Cu I 0.7500 0.7500 0.5000 0.0654(3) Uani d S 1 . . I 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 C1 0.071(3) 0.087(4) 0.049(2) -0.009(3) 0.004(2) -0.011(2) C2 0.086(4) 0.097(4) 0.057(2) -0.006(3) 0.022(3) -0.016(2) C3 0.078(4) 0.076(4) 0.084(3) 0.000(3) 0.040(3) -0.006(3) C4 0.053(3) 0.064(3) 0.078(3) -0.001(2) 0.019(2) 0.004(2) C5 0.050(2) 0.044(2) 0.054(2) -0.0001(16) 0.0047(18) 0.0048(16) C6 0.048(3) 0.075(4) 0.129(5) 0.000(2) 0.015(3) -0.009(3) N 0.0498(19) 0.075(2) 0.0418(15) -0.0039(17) 0.0028(15) -0.0053(16) Cu 0.0445(6) 0.1076(9) 0.0480(5) 0.000 0.000 0.000 I 0.0415(3) 0.0977(5) 0.0571(4) 0.000 0.000 0.000 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 C1 N . 1.306(5) yes C1 C2 . 1.372(6) ? C1 H1 . 0.9300 ? C2 C3 . 1.355(7) ? C2 H2 . 0.9300 ? C3 C4 . 1.365(7) ? C3 H3 . 0.9300 ? C4 C5 . 1.383(6) ? C4 C6 . 1.414(7) ? C5 N . 1.347(5) yes C6 H6 . 0.9300 ? N Cu . 2.008(3) yes 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 N C1 C2 . . 123.6(5) yes N C1 H1 . . 118.2 ? C2 C1 H1 . . 118.2 ? C3 C2 C1 . . 118.8(4) ? C3 C2 H2 . . 120.6 ? C1 C2 H2 . . 120.6 ? C2 C3 C4 . . 119.9(5) ? C2 C3 H3 . . 120.1 ? C4 C3 H3 . . 120.1 ? C3 C4 C5 . . 117.6(5) ? C3 C4 C6 . . 124.4(5) ? C5 C4 C6 . . 118.0(5) ? N C5 C4 . . 123.0(4) yes N C5 C5 . 3_557 116.9(2) yes C4 C5 C5 . 3_557 120.1(3) yes C6 C6 C4 3_557 . 121.8(3) yes C6 C6 H6 3_557 . 119.1 ? C4 C6 H6 . . 119.1 ? C1 N C5 . . 117.1(4) yes C1 N Cu . . 130.8(3) yes C5 N Cu . . 111.9(3) yes N Cu N 3_557 2_655 147.7(2) ? N Cu N 3_557 4_657 106.80(19) ? N Cu N 2_655 4_657 82.28(19) ? N Cu N 3_557 . 82.28(19) yes N Cu N 2_655 . 106.80(19) yes N Cu N 4_657 . 147.7(2) yes 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion N C1 C2 C3 . . 2.6(8) C1 C2 C3 C4 . . -1.3(8) C2 C3 C4 C5 . . -1.3(7) C2 C3 C4 C6 . . 178.0(5) C3 C4 C5 N . . 2.9(7) C6 C4 C5 N . . -176.4(4) C3 C4 C5 C5 . 3_557 -176.5(5) C6 C4 C5 C5 . 3_557 4.2(7) C3 C4 C6 C6 . 3_557 178.4(7) C5 C4 C6 C6 . 3_557 -2.3(10) C2 C1 N C5 . . -1.1(7) C2 C1 N Cu . . 172.3(4) C4 C5 N C1 . . -1.8(6) C5 C5 N C1 3_557 . 177.6(4) C4 C5 N Cu . . -176.4(3) C5 C5 N Cu 3_557 . 3.0(5) C1 N Cu N . 3_557 -174.7(5) C5 N Cu N . 3_557 -1.07(19) C1 N Cu N . 2_655 -26.5(4) C5 N Cu N . 2_655 147.1(3) C1 N Cu N . 4_657 75.9(4) C5 N Cu N . 4_657 -110.4(3) _cod_database_fobs_code 2013221