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_4080566
_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         'C60 H55 B Cl2 F24 Mo P2 Zr'
_chemical_formula_sum            'C60 H55 B Cl2 F24 Mo P2 Zr'
_chemical_formula_weight         1562.88
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   33.5527(8)
_cell_length_b                   14.4432(3)
_cell_length_c                   12.7234(3)
_cell_measurement_reflns_used    49370
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.04
_cell_volume                     6165.9(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0310
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48889
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3128.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.170
_refine_diff_density_max         3.090
_refine_diff_density_min         -1.920
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  5641 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     856
_refine_ls_number_reflns         13002
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[10.6300\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                12669
_reflns_number_total             13002
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om400088d_si_002.cif
_cod_data_source_block           '_4a'
_cod_original_cell_volume        6165.8(3)
_cod_database_code               4080566