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_4313854
_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            'C34 H32 Mn2 O6 P4'
_chemical_formula_weight         770.36
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(10)
_cell_angle_beta                 118.7330(10)
_cell_angle_gamma                90.0000(10)
_cell_formula_units_Z            4
_cell_length_a                   22.3415(9)
_cell_length_b                   10.6463(3)
_cell_length_c                   16.0877(7)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      3.0
_cell_volume                     3355.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      1500(1)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10854
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.9252
_exptl_absorpt_correction_T_min  0.8269
_exptl_absorpt_correction_type   'multiple scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0431P)^2^+1.2609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                4221
_reflns_number_total             4815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206894_2.cif
_cod_data_source_block           mnmn;compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4313854