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_4069607
_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         'C44 H54 N4 P4 Ru W '
_chemical_formula_sum            'C44 H54 N4 P4 Ru W'
_chemical_formula_weight         1047.75
_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                 99.581(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.4793(7)
_cell_length_b                   19.8614(12)
_cell_length_c                   20.6273(13)
_cell_measurement_reflns_used    12780
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.3
_cell_volume                     4233.3(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.118
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30497
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_exptl_absorpt_coefficient_mu    3.263
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.322
_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    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2096.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.71
_refine_diff_density_min         -1.86
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7461
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.7000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                4011
_reflns_number_total             7470
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om900298g_si_001.cif
_cod_data_source_block           '_WRu_compound_1'
_cod_original_cell_volume        4233.4(5)
_cod_original_formula_sum        'C44 H54 N4 P4 Ru W '
_cod_database_code               4069607