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_4071710
_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         'C45 H73 F6 Fe2 N2 O7 P4 S2 W '
_chemical_formula_sum            'C45 H73 F6 Fe2 N2 O7 P4 S2 W'
_chemical_formula_weight         1351.63
_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                77.6402(10)
_cell_angle_beta                 78.9330(14)
_cell_angle_gamma                83.6774(14)
_cell_formula_units_Z            2
_cell_length_a                   10.9423(5)
_cell_length_b                   11.2199(4)
_cell_length_c                   23.4042(8)
_cell_measurement_reflns_used    22957
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     2747.42(19)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27049
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1370.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.43
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     695
_refine_ls_number_reflns         12359
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.9800\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                10467
_reflns_number_total             12359
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om800327j-file003.cif
_cod_data_source_block           '_3-thf-0.5hexane'
_cod_original_cell_volume        2747.44(18)
_cod_original_formula_sum        'C45 H73 F6 Fe2 N2 O7 P4 S2 W '
_cod_database_code               4071710