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_4122099
_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         'C60 H118 Mo2 N12 P4 '
_chemical_formula_sum            'C60 H118 Mo2 N12 P4'
_chemical_formula_weight         1323.45
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.7381(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   24.7796(9)
_cell_length_b                   21.6001(9)
_cell_length_c                   13.6238(6)
_cell_measurement_reflns_used    16348
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     7083.4(5)
_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    SHELXS97
_diffrn_ambient_temperature      173.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.040
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33451
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2824.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     423
_refine_ls_number_reflns         8033
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[3.1000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                5358
_reflns_number_total             8033
_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(3e)]2(mu-N2)_(1e)'
_cod_depositor_comments
'Adding full bibliography for 4122097--4122101.cif.'
_cod_original_formula_sum        'C60 H118 Mo2 N12 P4 '
_cod_database_code               4122099