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_4122097
_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         'C64 H104 Mo2 N12 P4 '
_chemical_formula_sum            'C64 H104 Mo2 N12 P4'
_chemical_formula_weight         1357.38
_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                96.7468(12)
_cell_angle_beta                 101.4347(8)
_cell_angle_gamma                96.4981(12)
_cell_formula_units_Z            2
_cell_length_a                   12.5589(3)
_cell_length_b                   14.6629(5)
_cell_length_c                   20.7661(5)
_cell_measurement_reflns_used    37692
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3685.45(18)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.055
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58815
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1432.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.45
_refine_diff_density_min         -1.71
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     828
_refine_ls_number_reflns         16473
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[2.9000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                9911
_reflns_number_total             16473
_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(3b)]2(mu-N2)_(1b)'
_cod_depositor_comments
'Adding full bibliography for 4122097--4122101.cif.'
_cod_original_cell_volume        3685.46(18)
_cod_original_formula_sum        'C64 H104 Mo2 N12 P4 '
_cod_database_code               4122097