#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/82/2008269.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_2008269 loop_ _publ_author_name 'Jin, Qiong-Hua' 'Wang, Yu-Xian' 'Xin, Xiu-Lan' _publ_section_title Di-\m-iodo-1:2\k^4^I-bis(quinoline)-1\kN,2\kN-bis(triphenylphosphine)-1\kP,2\kP-dicopper(I) _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 341 _journal_page_last 343 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Cu2 I2 (C9 H7 N)2 (C18 H15 P)2]' _chemical_formula_moiety 'C27 H22 Cu I N P' _chemical_formula_sum 'C54 H44 Cu2 I2 N2 P2' _chemical_formula_weight 1163.74 _chemical_name_systematic ; (triphenylphosphine)-1\kP,2\kP-dicopper(I) Di(triphenylphosphine) Diquinoline Bis(\m-Iodine) Dicopper ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 107.896(10) _cell_angle_beta 107.812(14) _cell_angle_gamma 96.383(11) _cell_formula_units_Z 1 _cell_length_a 9.304(2) _cell_length_b 10.9792(13) _cell_length_c 13.685(3) _cell_measurement_reflns_used 30 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14.75 _cell_measurement_theta_min 5.62 _cell_volume 1233.6(4) _diffrn_ambient_temperature 293(2) _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method \q-2\q _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 0.018 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5134 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_min 1.68 _diffrn_standards_decay_% 2.43 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.215 _exptl_absorpt_correction_T_max 0.671 _exptl_absorpt_correction_T_min 0.487 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(XEMP; Siemens, 1991)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 576 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.591 _refine_diff_density_min -0.487 _refine_ls_extinction_coef 0.0140(6) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 282 _refine_ls_number_reflns 4263 _refine_ls_R_factor_gt 0.029 _refine_ls_shift/su_max -0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0392P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref 0.065 _reflns_number_observed 3444 _reflns_number_total 4263 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file jz1317.cif _[local]_cod_data_source_block jz1317 _cod_original_cell_volume 1233.7(4) _cod_database_code 2008269 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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol I 0.63205(3) 0.84967(2) 0.97179(2) 0.04574(11) Uani d . 1 . I Cu 0.41755(5) 0.92229(4) 1.05457(3) 0.04233(13) Uani d . 1 . Cu P 0.48402(10) 0.96179(8) 1.23555(7) 0.0363(2) Uani d . 1 . P N 0.2087(3) 0.7866(3) 0.9491(2) 0.0415(7) Uani d . 1 . N C1 0.6513(4) 1.0940(3) 1.3344(3) 0.0407(8) Uani d . 1 . C C2 0.7004(5) 1.1955(4) 1.3032(4) 0.0600(11) Uani d . 1 . C H2 0.6518(5) 1.1928(4) 1.2320(4) 0.094(16) Uiso calc R 1 . H C3 0.8207(5) 1.3000(4) 1.3771(4) 0.0784(14) Uani d . 1 . C H3 0.8524(5) 1.3676(4) 1.3554(4) 0.092(16) Uiso calc R 1 . H C4 0.8947(5) 1.3050(4) 1.4832(4) 0.0751(13) Uani d . 1 . C H4 0.9746(5) 1.3763(4) 1.5333(4) 0.087(14) Uiso calc R 1 . H C5 0.8490(5) 1.2043(4) 1.5134(3) 0.0658(11) Uani d . 1 . C H5 0.8996(5) 1.2066(4) 1.5842(3) 0.087(15) Uiso calc R 1 . H C6 0.7285(4) 1.0987(4) 1.4402(3) 0.0518(9) Uani d . 1 . C H6 0.6992(4) 1.0306(4) 1.4620(3) 0.055(11) Uiso calc R 1 . H C7 0.3244(4) 1.0044(3) 1.2809(3) 0.0366(7) Uani d . 1 . C C8 0.3425(4) 1.1053(4) 1.3770(3) 0.0520(9) Uani d . 1 . C H8 0.4407(4) 1.1572(4) 1.4224(3) 0.050(10) Uiso calc R 1 . H C9 0.2165(4) 1.1294(4) 1.4060(3) 0.0618(11) Uani d . 1 . C H9 0.2303(4) 1.1971(4) 1.4711(3) 0.065(12) Uiso calc R 1 . H C10 0.0713(4) 1.0547(4) 1.3399(3) 0.0579(10) Uani d . 1 . C H10 -0.0135(4) 1.0715(4) 1.3600(3) 0.052(10) Uiso calc R 1 . H C11 0.0507(4) 0.9546(4) 1.2436(3) 0.0518(9) Uani d . 1 . C H11 -0.0479(4) 0.9033(4) 1.1984(3) 0.059(11) Uiso calc R 1 . H C12 0.1749(4) 0.9309(3) 1.2146(3) 0.0460(9) Uani d . 1 . C H12 0.1597(4) 0.8639(3) 1.1488(3) 0.057(11) Uiso calc R 1 . H C13 0.5204(4) 0.8202(3) 1.2762(3) 0.0390(8) Uani d . 1 . C C14 0.4363(4) 0.7659(3) 1.3261(3) 0.0463(9) Uani d . 1 . C H14 0.3616(4) 0.8060(3) 1.3464(3) 0.037(9) Uiso calc R 1 . H C15 0.4613(5) 0.6534(4) 1.3463(3) 0.0586(11) Uani d . 1 . C H15 0.4027(5) 0.6175(4) 1.3791(3) 0.058(12) Uiso calc R 1 . H C16 0.5718(6) 0.5940(4) 1.3183(4) 0.0712(13) Uani d . 1 . C H16 0.5884(6) 0.5179(4) 1.3321(4) 0.065(12) Uiso calc R 1 . H C17 0.6579(6) 0.6466(4) 1.2701(4) 0.0691(12) Uani d . 1 . C H17 0.7329(6) 0.6059(4) 1.2508(4) 0.074(13) Uiso calc R 1 . H C18 0.6344(5) 0.7602(4) 1.2496(3) 0.0548(10) Uani d . 1 . C H18 0.6949(5) 0.7964(4) 1.2181(3) 0.062(12) Uiso calc R 1 . H C19 0.0906(4) 0.8264(4) 0.8957(3) 0.0553(10) Uani d . 1 . C H19 0.1062(4) 0.9139(4) 0.9018(3) 0.070(12) Uiso calc R 1 . H C20 -0.0558(5) 0.7456(4) 0.8311(4) 0.0670(12) Uani d . 1 . C H20 -0.1349(5) 0.7793(4) 0.7957(4) 0.074(13) Uiso calc R 1 . H C21 -0.0816(5) 0.6185(4) 0.8203(3) 0.0649(12) Uani d . 1 . C H21 -0.1788(5) 0.5634(4) 0.7772(3) 0.085(14) Uiso calc R 1 . H C22 0.0387(4) 0.5693(4) 0.8742(3) 0.0494(9) Uani d . 1 . C C23 0.0197(5) 0.4381(4) 0.8711(3) 0.0617(11) Uani d . 1 . C H23 -0.0748(5) 0.3787(4) 0.8279(3) 0.070(13) Uiso calc R 1 . H C24 0.1370(5) 0.3986(4) 0.9300(4) 0.0633(11) Uani d . 1 . C H24 0.1219(5) 0.3127(4) 0.9283(4) 0.079(13) Uiso calc R 1 . H C25 0.2805(5) 0.4846(3) 0.9934(3) 0.0546(10) Uani d . 1 . C H25 0.3605(5) 0.4556(3) 1.0334(3) 0.065(12) Uiso calc R 1 . H C26 0.3049(4) 0.6110(3) 0.9974(3) 0.0468(9) Uani d . 1 . C H26 0.4019(4) 0.6673(3) 1.0385(3) 0.037(9) Uiso calc R 1 . H C27 0.1826(4) 0.6566(3) 0.9390(3) 0.0387(8) Uani d . 1 . C 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 I 0.0467(2) 0.04117(15) 0.0572(2) 0.01886(11) 0.02001(12) 0.02389(11) Cu 0.0430(3) 0.0402(2) 0.0388(2) 0.0087(2) 0.0081(2) 0.0144(2) P 0.0319(5) 0.0375(5) 0.0355(5) 0.0063(4) 0.0094(4) 0.0113(4) N 0.037(2) 0.043(2) 0.041(2) 0.0068(13) 0.0085(13) 0.0160(13) C1 0.031(2) 0.044(2) 0.042(2) 0.0058(15) 0.010(2) 0.012(2) C2 0.048(2) 0.054(2) 0.066(3) 0.001(2) 0.006(2) 0.024(2) C3 0.059(3) 0.052(2) 0.099(4) -0.012(2) 0.004(3) 0.027(3) C4 0.055(3) 0.054(3) 0.074(3) -0.012(2) 0.002(2) -0.005(2) C5 0.049(2) 0.081(3) 0.045(3) 0.004(2) 0.006(2) 0.008(2) C6 0.041(2) 0.061(2) 0.045(2) 0.001(2) 0.013(2) 0.014(2) C7 0.034(2) 0.038(2) 0.036(2) 0.0083(15) 0.0100(15) 0.0140(15) C8 0.037(2) 0.058(2) 0.044(2) 0.011(2) 0.006(2) 0.005(2) C9 0.048(2) 0.073(3) 0.046(2) 0.018(2) 0.014(2) -0.002(2) C10 0.042(2) 0.076(3) 0.066(3) 0.027(2) 0.028(2) 0.025(2) C11 0.029(2) 0.054(2) 0.065(3) 0.006(2) 0.014(2) 0.015(2) C12 0.039(2) 0.045(2) 0.044(2) 0.005(2) 0.010(2) 0.008(2) C13 0.034(2) 0.044(2) 0.032(2) 0.007(2) 0.0061(15) 0.0104(15) C14 0.040(2) 0.047(2) 0.044(2) 0.003(2) 0.008(2) 0.016(2) C15 0.062(3) 0.049(2) 0.055(2) -0.002(2) 0.008(2) 0.024(2) C16 0.092(4) 0.048(2) 0.063(3) 0.021(2) 0.008(3) 0.023(2) C17 0.084(3) 0.074(3) 0.061(3) 0.047(3) 0.029(3) 0.028(2) C18 0.059(2) 0.064(2) 0.050(2) 0.025(2) 0.021(2) 0.027(2) C19 0.044(2) 0.051(2) 0.062(3) 0.004(2) 0.003(2) 0.026(2) C20 0.044(2) 0.076(3) 0.076(3) 0.012(2) 0.001(2) 0.042(2) C21 0.037(2) 0.069(3) 0.070(3) -0.008(2) -0.002(2) 0.028(2) C22 0.042(2) 0.051(2) 0.049(2) 0.007(2) 0.011(2) 0.017(2) C23 0.054(3) 0.041(2) 0.070(3) -0.003(2) 0.010(2) 0.011(2) C24 0.072(3) 0.034(2) 0.077(3) 0.007(2) 0.025(2) 0.016(2) C25 0.058(2) 0.037(2) 0.061(2) 0.016(2) 0.014(2) 0.013(2) C26 0.042(2) 0.042(2) 0.045(2) 0.008(2) 0.007(2) 0.008(2) C27 0.040(2) 0.035(2) 0.035(2) 0.0039(15) 0.011(2) 0.0080(14) 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 I Cu . 2.6617(6) yes I Cu 2_677 2.7059(5) yes Cu N . 2.097(3) yes Cu P . 2.2466(11) yes P C7 . 1.830(3) no P C1 . 1.834(3) no P C13 . 1.837(3) no N C19 . 1.321(4) no N C27 . 1.377(4) no C1 C2 . 1.387(5) no C1 C6 . 1.388(5) no C2 C3 . 1.377(6) no C3 C4 . 1.384(6) no C4 C5 . 1.360(6) no C5 C6 . 1.384(5) no C7 C8 . 1.384(5) no C7 C12 . 1.392(5) no C8 C9 . 1.375(5) no C9 C10 . 1.367(5) no C10 C11 . 1.375(5) no C11 C12 . 1.358(5) no C13 C14 . 1.383(5) no C13 C18 . 1.392(5) no C14 C15 . 1.376(5) no C15 C16 . 1.365(6) no C16 C17 . 1.366(6) no C17 C18 . 1.387(5) no C19 C20 . 1.391(5) no C20 C21 . 1.342(5) no C21 C22 . 1.400(5) no C22 C27 . 1.401(5) no C22 C23 . 1.417(5) no C23 C24 . 1.345(6) no C24 C25 . 1.391(5) no C25 C26 . 1.363(5) no C26 C27 . 1.416(5) no 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' P P 0.1023 0.0942 '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_3 _geom_angle _geom_angle_publ_flag Cu I Cu 2_677 71.70(2) yes N Cu P . 117.20(8) yes N Cu I . 106.25(8) yes P Cu I . 114.70(3) yes N Cu I 2_677 103.46(7) yes P Cu I 2_677 106.07(3) yes I Cu I 2_677 108.30(2) yes C7 P C1 . 103.54(15) no C7 P C13 . 102.98(15) no C1 P C13 . 103.25(15) no C7 P Cu . 110.35(11) no C1 P Cu . 119.78(12) no C13 P Cu . 115.09(11) no C19 N C27 . 116.8(3) no C19 N Cu . 120.2(2) no C27 N Cu . 122.8(2) no C2 C1 C6 . 118.5(3) no C2 C1 P . 118.9(3) no C6 C1 P . 122.6(3) no C3 C2 C1 . 120.6(4) no C2 C3 C4 . 120.4(4) no C5 C4 C3 . 119.2(4) no C4 C5 C6 . 121.2(4) no C5 C6 C1 . 120.0(4) no C8 C7 C12 . 117.7(3) no C8 C7 P . 124.2(3) no C12 C7 P . 118.1(3) no C9 C8 C7 . 120.5(3) no C10 C9 C8 . 120.6(4) no C9 C10 C11 . 119.8(4) no C12 C11 C10 . 119.7(3) no C11 C12 C7 . 121.7(3) no C14 C13 C18 . 118.4(3) no C14 C13 P . 123.9(3) no C18 C13 P . 117.6(3) no C15 C14 C13 . 120.8(4) no C16 C15 C14 . 120.4(4) no C15 C16 C17 . 119.9(4) no C16 C17 C18 . 120.5(4) no C17 C18 C13 . 119.9(4) no N C19 C20 . 124.2(3) no C21 C20 C19 . 119.2(4) no C20 C21 C22 . 119.8(4) no C21 C22 C27 . 117.9(3) no C21 C22 C23 . 123.3(4) no C27 C22 C23 . 118.6(3) no C24 C23 C22 . 120.6(4) no C23 C24 C25 . 120.9(4) no C26 C25 C24 . 120.6(4) no C25 C26 C27 . 119.9(3) no N C27 C22 . 122.1(3) no N C27 C26 . 118.5(3) no C22 C27 C26 . 119.4(3) no _journal_paper_doi 10.1107/S010827019801333X