Synthesis of Bis(phosphinoferrocenyl) Copper Complexes from Zwitterionic Quinonoid Ligands and Their Structural and Redox Properties
Pierre Braunstein; Denis Bubrin; Biprajit Sarkar; Inorganic Chemistry 48 (2009) 2534–2540; doi:10.1021/ic802042w

data_4301706
_publ_contact_author_address
;
Institut Le Bel, rue Blaise Pascal, 67000 STRASBOURG, FRANCE
;
_publ_contact_author_email       braunst@chimie.u-strasbg.fr
_publ_contact_author_fax         0390241322
_publ_contact_author_name
;
Pierre Braunstein
;
_publ_contact_author_phone       0390241308
_publ_section_title
;
Synthesis of Bis(phosphinoferrocenyl) Copper Complexes from Zwitterionic
Quinonoid Ligands and Their Structural and Redox Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2534
_journal_page_last               2540
_journal_paper_doi               10.1021/ic802042w
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C36 H57 Cu Fe N2 O2 P2'
_chemical_formula_sum            'C36 H57 Cu Fe N2 O2 P2'
_chemical_formula_weight         731.17
_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_method           SHELXL-97
_cell_angle_alpha                92.505(2)
_cell_angle_beta                 105.466(2)
_cell_angle_gamma                97.362(2)
_cell_formula_units_Z            4
_cell_length_a                   11.5638(4)
_cell_length_b                   16.3723(7)
_cell_length_c                   20.7837(5)
_cell_measurement_reflns_used    4322
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.540
_cell_measurement_theta_min      0.998
_cell_volume                     3748.6(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.1216
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20834
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         14654
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                8449
_reflns_number_total             14654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802042w_si_004.cif
_cod_data_source_block           global
_cod_database_code               4301706