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)]
Samuele Ciattini; Ferdinando Costantino; Pablo Lorenzo-Luis; Stefano Midollini; Annabella Orlandini; Alberto Vacca; Inorganic Chemistry 44 (2005) 4008–4016; doi:10.1021/ic050171a

data_4308924
_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       '\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)
_cod_data_source_file            ic050171asi20050201_080716_1.cif
_cod_data_source_block           cu(pcp)(bipy)(H2O)
_cod_database_code               4308924
_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