Synthesis and Catalytic Activity of Molybdenum‒Dinitrogen Complexes Bearing Unsymmetric PNP-Type Pincer Ligands
Kinoshita, Eriko; Arashiba, Kazuya; Kuriyama, Shogo; Miyake, Yoshihiro; Shimazaki, Ryuji; Nakanishi, Haruyuki; Nishibayashi, Yoshiaki; Organometallics 31 (2012) 8437–; doi:10.1021/om301046t

data_4079734
_publ_section_title
;
 Synthesis and Catalytic Activity of Molybdenum--Dinitrogen Complexes
 Bearing Unsymmetric PNP-Type Pincer Ligands
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8437
_journal_paper_doi               10.1021/om301046t
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C42 H78 Mo2 N12 P4'
_chemical_formula_sum            'C42 H78 Mo2 N12 P4'
_chemical_formula_weight         1066.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.4060(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.4475(4)
_cell_length_b                   22.2321(7)
_cell_length_c                   19.5339(7)
_cell_measurement_reflns_used    26693
_cell_measurement_temperature    198
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.20
_cell_volume                     5404.1(3)
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0895
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51032
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2232.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.600
_refine_diff_density_min         -1.500
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     619
_refine_ls_number_reflns         12322
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[1.8000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                7621
_reflns_number_total             12322
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om301046t_si_002.cif
_cod_data_source_block           '[Mo(N2)2(3c)]2(mu-N2)'
_cod_original_cell_volume        5404.0(3)
_cod_database_code               4079734