#------------------------------------------------------------------------------ #$Date: 2014-07-11 23:16:09 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308924.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308924 loop_ _publ_author_name 'Samuele Ciattini' 'Ferdinando Costantino' 'Pablo Lorenzo-Luis' 'Stefano Midollini' 'Annabella Orlandini' 'Alberto Vacca' _publ_contact_author 'Orlandini, Annabella' _publ_contact_author_email annabella.bianchi@iccom.cnr.it _publ_section_title ; Inorganic-Organic Hybrids Formed by P,P'-Diphenylmethylenediphosphinate, pcp2-, with the Cu2+ Ion. X-ray Crystal Structures of [Cu(pcp)(H2O)2].H2O and [Cu(pcp)(bipy)(H2O)] ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 4008 _journal_page_last 4016 _journal_volume 44 _journal_year 2005 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety '[Cu(pcp)(bipy)(H2O)]' _chemical_formula_structural 'C21 H18 CU1 N2 O4 P2' _chemical_formula_sum 'C23 H22 Cu N2 O5 P2' _chemical_formula_weight 531.91 _chemical_name_systematic ; P,P'-diphenylmethylenediphosphinate copper(II) Bipyridine aquo ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _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_date 2003-11-28T08:47:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 99.26(2) _cell_angle_beta 99.94(6) _cell_angle_gamma 102.10(5) _cell_formula_units_Z 2 _cell_length_a 7.135(9) _cell_length_b 10.870(2) _cell_length_c 16.271(5) _cell_measurement_reflns_used 0 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 0 _cell_measurement_theta_min 0 _cell_measurement_wavelength 0.71073 _cell_volume 1189.7(16) _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _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 CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_UB_11 -0.15657E-1 _diffrn_orient_matrix_UB_12 0.52855E-1 _diffrn_orient_matrix_UB_13 -0.44517E-1 _diffrn_orient_matrix_UB_21 0.12652E-1 _diffrn_orient_matrix_UB_22 0.77031E-1 _diffrn_orient_matrix_UB_23 0.45371E-1 _diffrn_orient_matrix_UB_31 0.145378 _diffrn_orient_matrix_UB_32 0.22717E-1 _diffrn_orient_matrix_UB_33 0.4969E-2 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0533 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3288 _diffrn_reflns_theta_full 22.97 _diffrn_reflns_theta_max 22.97 _diffrn_reflns_theta_min 2.56 _diffrn_source 'Enraf Nonius FR590' _diffrn_standards_decay_% 2 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_T_max 1.1466 _exptl_absorpt_correction_T_min 0.7904 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 546 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.385 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 386 _refine_ls_number_reflns 3288 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.071 _refine_ls_R_factor_gt 0.0414 _refine_ls_shift/su_max 0.879 _refine_ls_shift/su_mean 0.211 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.1063 _reflns_number_gt 2520 _reflns_number_total 3288 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic050171asi20050201_080716_1.cif _[local]_cod_data_source_block cu(pcp)(bipy)(H2O) _cod_database_code 4308924 #BEGIN Tags that were not found in dictionaries: _exptl_absorpt_factor_mur 0.054 _exptl_absorpt_correction_t_ave 0.9515 _diffrn_standards_decay_corr_max 1.053 _diffrn_standards_decay_corr_min 0.984 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.07736(7) 0.38802(5) 0.14550(3) 0.0355(2) Uani 1 1 d . . . P1 P 0.30829(16) 0.50611(10) 0.29047(7) 0.0349(3) Uani 1 1 d . . . P2 P 0.18746(16) 0.21458(10) 0.22439(8) 0.0372(3) Uani 1 1 d . . . O1 O 0.1219(4) 0.5119(3) 0.2325(2) 0.0470(8) Uani 1 1 d . . . O2 O 0.4915(4) 0.5389(3) 0.2586(2) 0.0493(8) Uani 1 1 d . . . O3 O 0.0124(4) 0.2376(3) 0.16758(19) 0.0460(8) Uani 1 1 d . . . O4 O 0.3533(5) 0.1904(3) 0.1844(2) 0.0522(9) Uani 1 1 d . . . O5 O -0.2937(6) 0.3652(5) 0.2246(3) 0.0616(10) Uani 1 1 d . . . N2 N -0.2364(5) 0.2873(3) 0.0308(2) 0.0376(9) Uani 1 1 d . . . N1 N -0.1433(5) 0.5321(3) 0.0919(2) 0.0377(9) Uani 1 1 d . . . C1 C 0.2697(8) 0.3480(4) 0.3150(3) 0.0406(11) Uani 1 1 d . . . C2 C -0.0909(6) 0.6569(4) 0.1296(3) 0.0417(11) Uani 1 1 d . . . C3 C -0.1309(7) 0.7503(5) 0.0871(3) 0.0451(12) Uani 1 1 d . . . C4 C -0.2280(7) 0.7169(5) 0.0027(3) 0.0488(13) Uani 1 1 d . . . C5 C -0.2824(6) 0.5896(5) -0.0358(3) 0.0412(11) Uani 1 1 d . . . C6 C -0.2405(5) 0.4981(4) 0.0099(3) 0.0344(10) Uani 1 1 d . . . C7 C -0.2940(6) 0.3581(4) -0.0254(3) 0.0363(10) Uani 1 1 d . . . C8 C -0.3939(6) 0.3022(5) -0.1082(3) 0.0446(12) Uani 1 1 d . . . C9 C -0.4341(7) 0.1699(5) -0.1327(3) 0.0536(14) Uani 1 1 d . . . C10 C -0.3763(8) 0.0984(5) -0.0767(4) 0.0534(13) Uani 1 1 d . . . C11 C -0.2773(7) 0.1593(5) 0.0051(3) 0.0455(12) Uani 1 1 d . . . C110 C 0.3290(7) 0.6147(4) 0.3894(3) 0.0437(11) Uani 1 1 d . . . C12 C 0.1749(10) 0.6133(6) 0.4288(4) 0.0647(15) Uani 1 1 d . . . C13 C 0.1974(15) 0.6996(8) 0.5060(5) 0.092(2) Uani 1 1 d . . . C14 C 0.3740(16) 0.7862(8) 0.5399(5) 0.096(3) Uani 1 1 d . . . C15 C 0.5279(15) 0.7878(7) 0.5023(5) 0.092(2) Uani 1 1 d . . . C16 C 0.5075(10) 0.7013(6) 0.4283(4) 0.0633(16) Uani 1 1 d . . . C21 C 0.0968(6) 0.0803(4) 0.2707(3) 0.0387(11) Uani 1 1 d . . . C22 C -0.0848(8) 0.0608(6) 0.2915(4) 0.0612(16) Uani 1 1 d . . . C23 C -0.1473(10) -0.0389(6) 0.3310(5) 0.080(2) Uani 1 1 d . . . C24 C -0.0286(11) -0.1198(6) 0.3494(4) 0.078(2) Uani 1 1 d . . . C25 C 0.1500(10) -0.1017(6) 0.3277(4) 0.0691(17) Uani 1 1 d . . . C26 C 0.2127(8) -0.0033(5) 0.2895(3) 0.0492(13) Uani 1 1 d . . . H2 H -0.020(7) 0.661(5) 0.189(3) 0.066(16) Uiso 1 1 d . . . H3 H -0.092(7) 0.829(5) 0.117(3) 0.047(14) Uiso 1 1 d . . . H4 H -0.253(7) 0.780(5) -0.029(3) 0.045(15) Uiso 1 1 d . . . H5 H -0.343(7) 0.557(5) -0.085(3) 0.050(16) Uiso 1 1 d . . . H8 H -0.426(7) 0.351(5) -0.148(3) 0.065(16) Uiso 1 1 d . . . H9 H -0.497(7) 0.124(5) -0.190(3) 0.055(15) Uiso 1 1 d . . . H10 H -0.381(7) 0.018(5) -0.089(3) 0.048(14) Uiso 1 1 d . . . H11 H -0.233(7) 0.116(5) 0.048(3) 0.054(15) Uiso 1 1 d . . . H110 H 0.181(7) 0.341(4) 0.351(3) 0.044(13) Uiso 1 1 d . . . H120 H 0.380(7) 0.343(4) 0.353(3) 0.045(14) Uiso 1 1 d . . . H12 H 0.058(6) 0.565(4) 0.403(2) 0.019(11) Uiso 1 1 d . . . H13 H 0.102(8) 0.693(5) 0.525(4) 0.067(19) Uiso 1 1 d . . . H14 H 0.380(11) 0.840(7) 0.595(5) 0.12(3) Uiso 1 1 d . . . H15 H 0.638(12) 0.855(8) 0.526(5) 0.14(3) Uiso 1 1 d . . . H16 H 0.592(9) 0.696(6) 0.400(4) 0.07(2) Uiso 1 1 d . . . H22 H -0.158(7) 0.105(5) 0.280(3) 0.043(15) Uiso 1 1 d . . . H23 H -0.263(10) -0.064(6) 0.339(4) 0.11(2) Uiso 1 1 d . . . H24 H -0.077(7) -0.194(5) 0.367(3) 0.070(15) Uiso 1 1 d . . . H25 H 0.209(8) -0.149(5) 0.342(4) 0.074(18) Uiso 1 1 d . . . H26 H 0.315(7) 0.012(4) 0.271(3) 0.040(13) Uiso 1 1 d . . . H51 H -0.383(9) 0.310(6) 0.214(4) 0.05(2) Uiso 1 1 d . . . H52 H -0.340(10) 0.435(7) 0.232(4) 0.11(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0295(3) 0.0338(3) 0.0404(3) 0.0074(2) 0.0040(2) 0.0043(2) P1 0.0344(6) 0.0303(6) 0.0362(7) 0.0069(5) 0.0030(5) 0.0032(5) P2 0.0384(6) 0.0291(6) 0.0436(7) 0.0081(5) 0.0092(5) 0.0064(5) O1 0.0465(19) 0.0305(16) 0.055(2) 0.0072(14) -0.0072(15) 0.0046(14) O2 0.0472(19) 0.0433(18) 0.058(2) 0.0121(16) 0.0172(16) 0.0054(15) O3 0.0518(19) 0.0340(17) 0.0482(19) 0.0065(14) 0.0002(15) 0.0118(14) O4 0.0478(19) 0.0419(19) 0.069(2) 0.0076(16) 0.0261(17) 0.0066(15) O5 0.042(2) 0.062(3) 0.085(3) 0.013(2) 0.032(2) 0.008(2) N2 0.033(2) 0.034(2) 0.041(2) 0.0044(17) 0.0076(17) 0.0014(16) N1 0.0267(19) 0.039(2) 0.046(2) 0.0049(18) 0.0082(17) 0.0081(16) C1 0.045(3) 0.031(2) 0.043(3) 0.008(2) 0.006(3) 0.006(2) C2 0.036(2) 0.039(3) 0.052(3) 0.009(2) 0.009(2) 0.013(2) C3 0.040(3) 0.035(3) 0.059(3) 0.008(2) 0.010(2) 0.008(2) C4 0.047(3) 0.056(3) 0.056(3) 0.024(3) 0.023(3) 0.021(3) C5 0.029(2) 0.053(3) 0.042(3) 0.011(3) 0.008(2) 0.010(2) C6 0.018(2) 0.043(3) 0.043(3) 0.010(2) 0.0094(19) 0.0061(18) C7 0.021(2) 0.042(3) 0.045(3) 0.008(2) 0.010(2) 0.0017(19) C8 0.031(2) 0.058(3) 0.040(3) 0.006(3) 0.007(2) 0.003(2) C9 0.044(3) 0.065(4) 0.038(3) -0.009(3) 0.004(2) 0.002(3) C10 0.051(3) 0.039(3) 0.057(3) -0.006(3) 0.008(3) -0.001(2) C11 0.039(3) 0.042(3) 0.050(3) 0.008(3) 0.007(2) 0.002(2) C110 0.056(3) 0.033(3) 0.043(3) 0.013(2) 0.007(2) 0.010(2) C12 0.071(4) 0.053(4) 0.071(4) 0.010(3) 0.024(4) 0.014(3) C13 0.127(7) 0.092(5) 0.083(5) 0.023(4) 0.058(5) 0.051(5) C14 0.139(8) 0.085(6) 0.056(5) -0.007(4) 0.002(5) 0.038(6) C15 0.117(6) 0.065(5) 0.065(5) -0.016(4) -0.013(5) 0.011(4) C16 0.071(4) 0.054(4) 0.053(4) 0.006(3) -0.005(3) 0.008(3) C21 0.039(3) 0.032(2) 0.043(3) 0.007(2) 0.006(2) 0.005(2) C22 0.049(3) 0.059(4) 0.087(5) 0.034(3) 0.021(3) 0.016(3) C23 0.069(4) 0.071(4) 0.106(5) 0.046(4) 0.028(4) 0.002(3) C24 0.085(5) 0.053(4) 0.097(5) 0.041(4) 0.016(4) 0.002(3) C25 0.078(4) 0.048(3) 0.086(5) 0.029(3) 0.008(3) 0.022(3) C26 0.057(3) 0.039(3) 0.050(3) 0.009(2) 0.008(3) 0.011(2) 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 0 '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' O O 0.0106 0.006 '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' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 5 0 4 -4 0 -1 4 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O3 96.54(14) . . ? O1 Cu1 N1 89.51(14) . . ? O3 Cu1 N1 163.68(14) . . ? O1 Cu1 N2 161.72(14) . . ? O3 Cu1 N2 89.99(14) . . ? N1 Cu1 N2 79.98(15) . . ? O1 Cu1 O5 94.89(17) . . ? O3 Cu1 O5 94.20(17) . . ? N1 Cu1 O5 100.39(16) . . ? N2 Cu1 O5 101.66(17) . . ? O2 P1 O1 116.3(2) . . ? O2 P1 C110 109.7(2) . . ? O1 P1 C110 106.1(2) . . ? O2 P1 C1 111.2(2) . . ? O1 P1 C1 107.3(2) . . ? C110 P1 C1 105.5(2) . . ? O4 P2 O3 117.3(2) . . ? O4 P2 C21 109.4(2) . . ? O3 P2 C21 106.9(2) . . ? O4 P2 C1 111.6(2) . . ? O3 P2 C1 107.3(2) . . ? C21 P2 C1 103.3(2) . . ? P1 O1 Cu1 134.30(19) . . ? P2 O3 Cu1 135.23(19) . . ? C11 N2 C7 118.8(4) . . ? C11 N2 Cu1 125.5(3) . . ? C7 N2 Cu1 115.6(3) . . ? C2 N1 C6 118.6(4) . . ? C2 N1 Cu1 125.6(3) . . ? C6 N1 Cu1 115.7(3) . . ? P1 C1 P2 115.9(3) . . ? N1 C2 C3 122.1(5) . . ? C2 C3 C4 119.9(5) . . ? C5 C4 C3 118.2(5) . . ? C4 C5 C6 120.0(5) . . ? N1 C6 C5 121.2(4) . . ? N1 C6 C7 114.4(4) . . ? C5 C6 C7 124.4(4) . . ? N2 C7 C8 121.8(4) . . ? N2 C7 C6 114.1(4) . . ? C8 C7 C6 124.1(4) . . ? C7 C8 C9 118.0(5) . . ? C10 C9 C8 120.4(5) . . ? C9 C10 C11 119.1(5) . . ? N2 C11 C10 121.8(5) . . ? C12 C110 C16 118.5(5) . . ? C12 C110 P1 121.9(4) . . ? C16 C110 P1 119.6(4) . . ? C110 C12 C13 120.0(7) . . ? C14 C13 C12 119.1(8) . . ? C15 C14 C13 121.5(7) . . ? C14 C15 C16 119.3(8) . . ? C15 C16 C110 121.5(8) . . ? C22 C21 C26 118.3(5) . . ? C22 C21 P2 121.3(4) . . ? C26 C21 P2 120.3(4) . . ? C21 C22 C23 120.4(6) . . ? C24 C23 C22 120.0(7) . . ? C25 C24 C23 119.6(6) . . ? C26 C25 C24 120.6(6) . . ? C25 C26 C21 121.1(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.931(3) . ? Cu1 O3 1.939(3) . ? Cu1 N1 2.010(4) . ? Cu1 N2 2.016(4) . ? Cu1 O5 2.174(4) . ? P1 O2 1.484(4) . ? P1 O1 1.511(3) . ? P1 C110 1.800(5) . ? P1 C1 1.803(4) . ? P2 O4 1.495(4) . ? P2 O3 1.512(3) . ? P2 C21 1.801(4) . ? P2 C1 1.810(5) . ? N2 C11 1.340(6) . ? N2 C7 1.351(5) . ? N1 C2 1.341(6) . ? N1 C6 1.347(6) . ? C2 C3 1.368(7) . ? C3 C4 1.378(7) . ? C4 C5 1.367(7) . ? C5 C6 1.385(6) . ? C6 C7 1.479(6) . ? C7 C8 1.384(6) . ? C8 C9 1.383(7) . ? C9 C10 1.355(8) . ? C10 C11 1.380(7) . ? C110 C12 1.363(7) . ? C110 C16 1.391(8) . ? C12 C13 1.404(9) . ? C13 C14 1.369(11) . ? C14 C15 1.344(11) . ? C15 C16 1.369(9) . ? C21 C22 1.377(7) . ? C21 C26 1.386(7) . ? C22 C23 1.381(8) . ? C23 C24 1.375(9) . ? C24 C25 1.363(9) . ? C25 C26 1.356(8) . ? _journal_paper_doi 10.1021/ic050171a