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_4331634
_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         'C70 H58 Cl2 Mo N2 O1.50 P4 '
_chemical_formula_sum            'C70 H58 Cl2 Mo N2 O1.5 P4'
_chemical_formula_weight         1241.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.8563(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.6171(3)
_cell_length_b                   11.3510(2)
_cell_length_c                   30.2636(7)
_cell_measurement_reflns_used    17114
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     6258.9(2)
_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    SIR2004
_diffrn_ambient_temperature      173.1
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.043
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            46204
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             2560.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.69
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     773
_refine_ls_number_reflns         12126
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0019Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                12083
_reflns_number_total             14165
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic301577a_si_002_3.cif
_cod_data_source_block           1Xy
_cod_original_formula_sum        'C70 H58 Cl2 Mo N2 O1.50 P4 '
_cod_database_code               4331634