Synthesis and Protonation of Molybdenum– and Tungsten–Dinitrogen Complexes Bearing PNP-Type Pincer Ligands
Arashiba, Kazuya; Sasaki, Kouitsu; Kuriyama, Shogo; Miyake, Yoshihiro; Nakanishi, Haruyuki; Nishibayashi, Yoshiaki; Organometallics 31 (2012) 2035–; doi:10.1021/om300011z

data_4076535
_publ_section_title
;
 Synthesis and Protonation of Molybdenum-- and Tungsten--Dinitrogen
 Complexes Bearing PNP-Type Pincer Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              2035
_journal_paper_doi               10.1021/om300011z
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C31 H54 N5 P3 W'
_chemical_formula_sum            'C31 H54 N5 P3 W'
_chemical_formula_weight         773.57
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                73.1991(12)
_cell_angle_beta                 79.6971(15)
_cell_angle_gamma                69.3292(14)
_cell_formula_units_Z            2
_cell_length_a                   10.6999(6)
_cell_length_b                   13.0508(6)
_cell_length_c                   13.9197(7)
_cell_measurement_reflns_used    14518
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.01
_cell_volume                     1734.60(15)
_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    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0460
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16878
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.500
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             788.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.150
_refine_diff_density_min         -1.980
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7815
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[1.4500\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                6652
_reflns_number_total             7815
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om300011z_si_001.cif
_cod_data_source_block           trans-[W(N2)2(tBuPNP)(PMe2Ph)]
_cod_original_cell_volume        1734.60(16)
_cod_database_code               4076535