Catalytic Formation of Ammonia from Molecular Dinitrogen by Use of Dinitrogen-Bridged Dimolybdenum-Dinitrogen Complexes Bearing PNP-Pincer Ligands: Remarkable Effect of Substituent at PNP-Pincer Ligand.
Kuriyama, Shogo; Arashiba, Kazuya; Nakajima, Kazunari; Tanaka, Hiromasa; Kamaru, Nobuaki; Yoshizawa, Kazunari; Nishibayashi, Yoshiaki; Journal of the American Chemical Society 136 (2014) 9719–9731; doi:10.1021/ja5044243

data_4122100
_publ_section_title
;
 Catalytic Formation of Ammonia from Molecular Dinitrogen by Use of
 Dinitrogen-Bridged Dimolybdenum-Dinitrogen Complexes Bearing PNP-Pincer
 Ligands: Remarkable Effect of Substituent at PNP-Pincer Ligand.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9719
_journal_page_last               9731
_journal_paper_doi               10.1021/ja5044243
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C54 H104 Mo2 N12 O2 P4'
_chemical_formula_sum            'C54 H104 Mo2 N12 O2 P4'
_chemical_formula_weight         1269.27
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 111.7160(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   31.2829(12)
_cell_length_b                   10.0768(4)
_cell_length_c                   21.9085(7)
_cell_measurement_reflns_used    16626
_cell_measurement_temperature    183
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.06
_cell_volume                     6416.1(4)
_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    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      183
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0765
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25769
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2688.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.270
_refine_diff_density_min         -1.900
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7203
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[3.3300\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                5027
_reflns_number_total             7203
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja5044243_si_002.cif
_cod_data_source_block           '[Mo(N2)2(3f)]2(mu-N2)_(1f)'
_cod_depositor_comments
'Adding full bibliography for 4122097--4122101.cif.'
_cod_database_code               4122100