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_4071706
_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         'C46 H76 Fe2 N4 O2.50 P4 W '
_chemical_formula_sum            'C46 H76 Fe2 N4 O2.5 P4 W'
_chemical_formula_weight         1144.57
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 116.4261(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.7672(9)
_cell_length_b                   13.9265(6)
_cell_length_c                   21.5321(10)
_cell_measurement_reflns_used    16714
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     4502.6(4)
_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    'DIRDIF99 (PATTY)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.056
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21335
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    3.374
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.263
_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-yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2344.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.66
_refine_diff_density_min         -0.81
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5155
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0007Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                4394
_reflns_number_total             5159
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om800327j-file003.cif
_cod_data_source_block           '_cis-1'
_cod_original_formula_sum        'C46 H76 Fe2 N4 O2.50 P4 W '
_cod_database_code               4071706