One-Electron Reduction Product of a Biphosphinine Derivative and of Its Ni(0) Complex: Crystal Structure, EPR/ENDOR, and DFT Investigations on (tmbp).- and [Ni(tmbp)2].-
Sylvie Choua; Helena Sidorenkova; Théo Berclaz; Michel Geoffroy; Patrick Rosa; Nicolas Mézailles; Louis Ricard; François Mathey; Pascal Le Floch; Journal of the American Chemical Society 122 (2000) 12227–12234; doi:10.1021/ja002125+

data_4116267
_publ_contact_author
;
Louis Ricard,
Labo DCPH,
Ecole Polytechnique
Route de Saclay
91128 Palaiseau
France
;
_publ_contact_author_email       ricard@neptune.polytechnique.fr
_publ_contact_author_fax         01-69-33-39-90
_publ_contact_author_phone       01-69-33-45-72
_publ_section_title
;
 One-Electron Reduction Product of a Biphosphinine Derivative and of Its
 Ni(0) Complex: Crystal Structure, EPR/ENDOR, and DFT Investigations on
 (tmbp).- and [Ni(tmbp)2].-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12227
_journal_page_last               12234
_journal_paper_doi               10.1021/ja002125+
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C30 H48 Li N2 O5 P2'
_chemical_formula_weight         585.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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             22-02-99
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.998(3)
_cell_angle_beta                 74.883(3)
_cell_angle_gamma                72.182(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5316(6)
_cell_length_b                   11.5497(5)
_cell_length_c                   13.0148(4)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1562.62(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full .945
_diffrn_measured_fraction_theta_max .945
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11139
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.9651
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       cube
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .449
_refine_diff_density_min         -.445
_refine_diff_density_rms         .135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         8644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.2259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                7067
_reflns_number_total             8644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0021252B.cif
_cod_data_source_block           tmbpli
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4116267