#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:46:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179127 $
#$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_paper_doi               10.1021/ic050171a
_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       'κ-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/[σ²(Fo²)+(0.0636P)²+0.0000P] where P=(Fo²+2Fc²)/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)
_cod_data_source_file            ic050171asi20050201_080716_1.cif
_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_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) . ?
