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_4076534
_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_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C27 H51 Cl3 N O P2 W'
_chemical_formula_sum            'C27 H51 Cl3 N O P2 W'
_chemical_formula_weight         757.86
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 126.2874(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   29.2304(8)
_cell_length_b                   14.9824(4)
_cell_length_c                   19.7839(5)
_cell_measurement_reflns_used    52894
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.00
_cell_volume                     6983.8(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      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0408
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55714
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.652
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3064.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.150
_refine_diff_density_max         3.980
_refine_diff_density_min         -0.948
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  6855 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     676
_refine_ls_number_reflns         15114
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[3.3000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                14592
_reflns_number_total             15114
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om300011z_si_001.cif
_cod_data_source_block           '[WCl3(tBuPNP)]'
_cod_original_cell_volume        6983.9(3)
_cod_database_code               4076534