Synthesis and Protonolysis of Tungsten− and Molybdenum−Dinitrogen Complexes Bearing Ruthenocenyldiphosphines
Yuki, Masahiro; Midorikawa, Tatsuya; Miyake, Yoshihiro; Nishibayashi, Yoshiaki; Organometallics 28 (2009) 4741–; doi:10.1021/om900298g

data_4069608
_publ_section_title
;
 Synthesis and Protonolysis of Tungsten&#x2212; and
 Molybdenum&#x2212;Dinitrogen Complexes Bearing Ruthenocenyldiphosphines
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4741
_journal_paper_doi               10.1021/om900298g
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C40 H46 Mo N4 P4 Ru '
_chemical_formula_sum            'C40 H46 Mo N4 P4 Ru'
_chemical_formula_weight         903.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 104.0972(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.9067(5)
_cell_length_b                   22.0993(7)
_cell_length_c                   14.0746(6)
_cell_measurement_reflns_used    24253
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     3893.6(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.053
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37334
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.669
_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
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1840.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.97
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     497
_refine_ls_number_reflns         8861
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                5723
_reflns_number_total             8861
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om900298g_si_001.cif
_cod_data_source_block           '_MoRu_compond_7'
_cod_original_cell_volume        3893.6(2)
_cod_original_formula_sum        'C40 H46 Mo N4 P4 Ru '
_cod_database_code               4069608