Synthesis and Characterization of a Coupled Binuclear CuI/CuIII Complex
Jesús García-López; Víctor Yañez-Rodríguez; Laura Roces; Santiago García-Granda; Ana Martínez; Alfredo Guevara-García; German R. Castro; Félix Jiménez-Villacorta; María J. Iglesias; Fernando López Ortiz; Journal of the American Chemical Society 132 (2010) 10665–10667; doi:10.1021/ja1034667

data_4102805
_publ_section_title
;
 Synthesis and Characterization of a Coupled Binuclear CuI/CuIII Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10665
_journal_page_last               10667
_journal_paper_doi               10.1021/ja1034667
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H32 Cu2 N2 O4 P2, C H Cl3'
_chemical_formula_sum            'C33 H33 Cl3 Cu2 N2 O4 P2'
_chemical_formula_weight         816.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-02-02T21:56:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7699(1)
_cell_length_b                   13.8445(1)
_cell_length_c                   19.5705(1)
_cell_measurement_reflns_used    13606
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.6923
_cell_measurement_theta_min      3.1861
_cell_volume                     3459.93(4)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.264
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\o scans'
_diffrn_orient_matrix_UB_11      0.0748894882
_diffrn_orient_matrix_UB_12      -0.0459244745
_diffrn_orient_matrix_UB_13      0.0523990827
_diffrn_orient_matrix_UB_21      0.0586733524
_diffrn_orient_matrix_UB_22      0.0964705523
_diffrn_orient_matrix_UB_23      0.0070802889
_diffrn_orient_matrix_UB_31      -0.074192523
_diffrn_orient_matrix_UB_32      0.0299395997
_diffrn_orient_matrix_UB_33      0.0580011026
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17788
_diffrn_reflns_theta_full        73.89
_diffrn_reflns_theta_max         73.89
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    4.852
_exptl_absorpt_correction_T_max  0.8424
_exptl_absorpt_correction_T_min  0.6858
_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            yellow
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.653(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+1.1418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                6267
_reflns_number_total             6735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1034667_si_002.cif
_cod_data_source_block           CuCu
_cod_original_sg_symbol_Hall     'P 2ac 2ac'
_cod_database_code               4102805