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_4331636
_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 Mo N6 P4 C3 O'
_chemical_formula_sum            'C67 H58 Mo N6 O P4'
_chemical_formula_weight         1183.07
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   14.7122(6)
_cell_length_b                   23.2371(6)
_cell_length_c                   18.0126(6)
_cell_measurement_reflns_used    16779
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.12
_cell_volume                     6157.9(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45970
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             2472.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7049
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0605P)^2^+5.2255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                6373
_reflns_number_total             7049
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic301577a_si_002_4.cif
_cod_data_source_block           2Xy
_cod_database_code               4331636