Preparation, Characterization, and Reactivity of Dinitrogen Molybdenum Complexes with Bis(diphenylphosphino)amine Derivative Ligands that Form a Unique 4-Membered P-N-P Chelate Ring
Takahiko Ogawa; Yuji Kajita; Yuko Wasada-Tsutsui; Hiroaki Wasada; Hideki Masuda; Inorganic Chemistry 52 (2013) 182–195; doi:10.1021/ic301577a

data_4331632
_publ_contact_author_address
'gokiso-cho, showa-ku, nagoya 466-8555, Japan'
_publ_contact_author_email       masuda.hideki@nitech.ac.jp
_publ_contact_author_fax         +81-52-735-5209
_publ_contact_author_name        'Hideki Masuda'
_publ_contact_author_phone       +81-52-735-5228
_publ_section_title
;
 Preparation, Characterization, and Reactivity of Dinitrogen Molybdenum
 Complexes with Bis(diphenylphosphino)amine Derivative Ligands that Form a
 Unique 4-Membered P-N-P Chelate Ring
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              182
_journal_page_last               195
_journal_paper_doi               10.1021/ic301577a
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C64 H58 Cl2 Mo N2 O P4 '
_chemical_formula_sum            'C64 H58 Cl2 Mo N2 O P4'
_chemical_formula_weight         1161.92
_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                89.589(4)
_cell_angle_beta                 79.536(4)
_cell_angle_gamma                74.163(3)
_cell_formula_units_Z            2
_cell_length_a                   11.57560(10)
_cell_length_b                   12.6994(2)
_cell_length_c                   20.0643(5)
_cell_measurement_reflns_used    6975
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2787.56(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      173.1
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22279
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.895
_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    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             1200.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.37
_refine_diff_density_min         -1.92
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     725
_refine_ls_number_reflns         17090
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.0015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0024Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                16950
_reflns_number_total             12196
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic301577a_si_002_2.cif
_cod_data_source_block           1Ph
_cod_original_cell_volume        2787.56(9)
_cod_original_formula_sum        'C64 H58 Cl2 Mo N2 O P4 '
_cod_database_code               4331632