Synthesis and Reactivity of Tungsten− and Molybdenum−Dinitrogen Complexes Bearing Ferrocenyldiphosphines toward Protonolysis
Yuki, Masahiro; Miyake, Yoshihiro; Nishibayashi, Yoshiaki; Wakiji, Issei; Hidai, Masanobu; Organometallics 27 (2008) 3947–; doi:10.1021/om800327j

data_4071709
_publ_section_title
;
 Synthesis and Reactivity of Tungsten&#x2212; and
 Molybdenum&#x2212;Dinitrogen Complexes Bearing Ferrocenyldiphosphines
 toward Protonolysis
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3947
_journal_paper_doi               10.1021/om800327j
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C38 H58 F6 Fe2 N2 O6 P4 S2 W '
_chemical_formula_sum            'C38 H58 F6 Fe2 N2 O6 P4 S2 W'
_chemical_formula_weight         1236.44
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.0220(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.9906(5)
_cell_length_b                   14.3654(3)
_cell_length_c                   19.4780(5)
_cell_measurement_reflns_used    51161
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.0
_cell_volume                     4591.7(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42091
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    3.426
_exptl_absorpt_correction_T_max  0.504
_exptl_absorpt_correction_T_min  0.282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2480.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.57
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10463
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                8369
_reflns_number_total             10471
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om800327j-file003.cif
_cod_data_source_block           '_3-non-solvent'
_cod_original_formula_sum        'C38 H58 F6 Fe2 N2 O6 P4 S2 W '
_cod_database_code               4071709