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_4080559
_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         'C38.375 H58.75 Cl10.75 Mo2 P2 Zr'
_chemical_formula_sum            'C38.375 H58.75 Cl10.75 Mo2 P2 Zr'
_chemical_formula_weight         1246.30
_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                 92.9124(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.1657(3)
_cell_length_b                   21.5200(9)
_cell_length_c                   27.9068(10)
_cell_measurement_reflns_used    28735
_cell_measurement_temperature    198
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.08
_cell_volume                     4897.6(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  0.1197
_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       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            39651
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2503.00
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.730
_refine_diff_density_min         -3.590
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  9217 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1044
_refine_ls_number_reflns         20466
_refine_ls_R_factor_gt           0.1283
_refine_ls_shift/su_max          0.150
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[2.2000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                11002
_reflns_number_total             20466
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om400088d_si_002.cif
_cod_data_source_block           '_1a'
_cod_depositor_comments
;

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         2492.61
_cod_original_formula_moiety         'C76.75 H117.50 Cl21.50 Mo4 P4 Zr2'
_cod_original_formula_units_Z            2
_cod_original_formula_sum        'C76.75 H117.50 Cl21.50 Mo4 P4 Zr2'
_cod_database_code               4080559