Electronic Properties of 4,4',5,5'-Tetramethyl-2,2'-biphosphinine (tmbp) in the Redox Series fac-[Mn(Br)(CO)3(tmbp)], [Mn(CO)3(tmbp)]2, and [Mn(CO)3(tmbp)]-: Crystallographic, Spectroelectrochemical, and DFT Computational Study
František Hartl; Taasje Mahabiersing; Pascal Le Floch; Francois Mathey; Louis Ricard; Patrick Rosa; Stanislav Záliš; Inorganic Chemistry 42 (2003) 4442–4455; doi:10.1021/ic0206894

data_4313855
_publ_contact_author_address
;
    Labo DCPH,
    Ecole Polytechnique
    Route de Saclay
    91128 Palaiseau
    France
;
_publ_contact_author_email       louis.ricard@polytechnique.fr
_publ_contact_author_fax         01-69-33-39-90
_publ_contact_author_name        'Louis Ricard'
_publ_contact_author_phone       01-69-33-45-72
_publ_section_title
;
 Electronic Properties of 4,4',5,5'-Tetramethyl-2,2'-biphosphinine (tmbp)
 in the Redox Series fac-[Mn(Br)(CO)3(tmbp)], [Mn(CO)3(tmbp)]2, and
 [Mn(CO)3(tmbp)]-: Crystallographic, Spectroelectrochemical, and DFT
 Computational Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4442
_journal_page_last               4455
_journal_paper_doi               10.1021/ic0206894
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C25 H36 Mn Na O5 P2'
_chemical_formula_weight         556.41
_chemical_name_systematic
;
  ?
;
_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_method           SHELXL-97
_cell_angle_alpha                96.830(5)
_cell_angle_beta                 90.140(5)
_cell_angle_gamma                103.770(5)
_cell_formula_units_Z            2
_cell_length_a                   9.024(5)
_cell_length_b                   10.130(5)
_cell_length_c                   15.833(5)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.0
_cell_volume                     1395.1(11)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9407
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.9392
_exptl_absorpt_correction_T_min  0.8943
_exptl_absorpt_correction_type   'multiple scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6345
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0585P)^2^+0.3694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                4643
_reflns_number_total             6345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206894_3.cif
_cod_data_source_block           mnna;compound4
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4313855