Synthesis of Group IV (Zr, Hf)−Group VIII (Fe, Ru) Heterobimetallic Complexes Bearing Metallocenyl Diphosphine Moieties and Their Application to Catalytic Dehydrogenation of Amine−Boranes
Miyazaki, Takamasa; Tanabe, Yoshiaki; Yuki, Masahiro; Miyake, Yoshihiro; Nishibayashi, Yoshiaki; Organometallics 30 (2011) 2394–; doi:10.1021/om200127r

data_4064474
_publ_section_title
;
 Synthesis of Group IV (Zr, Hf)&#x2212;Group VIII (Fe, Ru)
 Heterobimetallic Complexes Bearing Metallocenyl Diphosphine Moieties and
 Their Application to Catalytic Dehydrogenation of Amine&#x2212;Boranes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2394
_journal_paper_doi               10.1021/om200127r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C37 H52 Cl3 Hf P2 Ru '
_chemical_formula_sum            'C37 H52 Cl3 Hf P2 Ru'
_chemical_formula_weight         944.68
_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'
_cell_angle_alpha                80.0785(14)
_cell_angle_beta                 74.0762(15)
_cell_angle_gamma                69.2253(12)
_cell_formula_units_Z            2
_cell_length_a                   10.0997(5)
_cell_length_b                   13.8189(5)
_cell_length_c                   15.2016(8)
_cell_measurement_reflns_used    17496
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1900.93(15)
_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    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      173.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.041
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18591
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    3.441
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_correction_T_min  0.193
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             942.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         3.72
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     390
_refine_ls_number_reflns         8598
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[3.9600\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                7963
_reflns_number_total             8598
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om200127r_si_002.cif
_cod_data_source_block           '_3b'
_cod_original_cell_volume        1900.92(15)
_cod_original_formula_sum        'C37 H52 Cl3 Hf P2 Ru '
_cod_database_code               4064474