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_4071708
_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         'C36 H56 Fe2 Mo N4 P4 '
_chemical_formula_sum            'C36 H56 Fe2 Mo N4 P4'
_chemical_formula_weight         876.39
_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'
_cell_angle_alpha                68.4688(18)
_cell_angle_beta                 75.0902(17)
_cell_angle_gamma                75.3883(8)
_cell_formula_units_Z            2
_cell_length_a                   10.3341(3)
_cell_length_b                   12.9756(4)
_cell_length_c                   16.0505(4)
_cell_measurement_reflns_used    15238
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.3
_cell_volume                     1904.58(10)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.024
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17543
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             908.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8455
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0013Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                7649
_reflns_number_total             8462
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om800327j-file003.cif
_cod_data_source_block           '_trans-2'
_cod_original_cell_volume        1904.58(9)
_cod_original_formula_sum        'C36 H56 Fe2 Mo N4 P4 '
_cod_database_code               4071708