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_4080561
_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         'C38.50 H59 Cl11 P2 W2 Zr '
_chemical_formula_sum            'C38.5 H59 Cl11 P2 W2 Zr'
_chemical_formula_weight         1432.74
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.0210(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.1693(3)
_cell_length_b                   21.5637(8)
_cell_length_c                   27.9730(10)
_cell_measurement_reflns_used    22639
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4920.9(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_ambient_temperature      173.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.089
_diffrn_reflns_limit_h_max       9
_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       -36
_diffrn_reflns_number            37907
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    5.567
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2780.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.87
_refine_diff_density_min         -3.51
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  8907 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.026(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     1080
_refine_ls_number_reflns         20015
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.6630\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1403
_reflns_number_gt                13413
_reflns_number_total             20015
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om400088d_si_002.cif
_cod_data_source_block           '_1c'
_cod_original_formula_sum        'C38.50 H59 Cl11 P2 W2 Zr '
_cod_database_code               4080561