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_4076533
_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         'C26 H52 Mo N5 P3 '
_chemical_formula_sum            'C26 H52 Mo N5 P3'
_chemical_formula_weight         623.59
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 106.435(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.8589(8)
_cell_length_b                   20.7314(18)
_cell_length_c                   17.8396(17)
_cell_measurement_reflns_used    14598
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3142.5(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 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.090
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19707
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1320.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5487
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0006Fo^2^ + 0.1600\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                2339
_reflns_number_total             5487
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om300011z_si_001.cif
_cod_data_source_block           trans-[Mo(N2)2(tBuPNP)(PMe3)]
_cod_original_formula_sum        'C26 H52 Mo N5 P3 '
_cod_database_code               4076533