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_4080560
_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_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C38.25 H58.50 Cl10.50 Hf Mo2 P2'
_chemical_formula_sum            'C38.25 H58.5 Cl10.5 Hf Mo2 P2'
_chemical_formula_weight         1322.96
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.9040(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.1877(3)
_cell_length_b                   21.5572(6)
_cell_length_c                   27.9565(7)
_cell_measurement_reflns_used    36674
_cell_measurement_temperature    198
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.07
_cell_volume                     4928.1(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID 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      198
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43452
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.259
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2610.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         5.250
_refine_diff_density_min         -5.920
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  9616 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.058(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         20902
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[4.7800\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1943
_reflns_number_gt                17763
_reflns_number_total             20902
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om400088d_si_002.cif
_cod_data_source_block           '_1b'
_cod_original_formula_sum        'C38.25 H58.50 Cl10.50 Hf Mo2 P2'
_cod_database_code               4080560