Synthesis, Structure, and Reactivity of Group VI Metal Complexes Bearing Group IV Metallocenyldiphosphine Moieties and a Pentamethylcyclopentadienyl Ligand
Miyazaki, Takamasa; Tanabe, Yoshiaki; Yuki, Masahiro; Miyake, Yoshihiro; Nishibayashi, Yoshiaki; Organometallics 32 (2013) 2007–; doi:10.1021/om400088d

data_4080565
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Group VI Metal Complexes Bearing
 Group IV Metallocenyldiphosphine Moieties and a
 Pentamethylcyclopentadienyl Ligand
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2007
_journal_paper_doi               10.1021/om400088d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C31.50 H47 Cl3 P2 W Zr'
_chemical_formula_sum            'C31.5 H47 Cl3 P2 W Zr'
_chemical_formula_weight         869.09
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                101.389(2)
_cell_angle_beta                 100.6910(19)
_cell_angle_gamma                103.736(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2774(6)
_cell_length_b                   11.3357(6)
_cell_length_c                   15.0666(10)
_cell_measurement_reflns_used    10146
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      3.00
_cell_volume                     1620.96(17)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.143
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13363
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.238
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             862.00
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         4.060
_refine_diff_density_min         -4.890
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     336
_refine_ls_number_reflns         7114
_refine_ls_R_factor_gt           0.1058
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[3.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1937
_reflns_number_gt                3589
_reflns_number_total             7114
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om400088d_si_002.cif
_cod_data_source_block           '_3c'
_cod_original_cell_volume        1620.98(17)
_cod_original_formula_sum        'C31.50 H47 Cl3 P2 W Zr'
_cod_database_code               4080565