Synthesis and Structures of Tungsten (1-Pyridinio)imido Complexes and Their Facile N-N Bond Cleavage1
Hiroshige Ishino; Shin'ichi Tokunaga; Hidetake Seino; Youichi Ishii; Masanobu Hidai; Inorganic Chemistry 38 (1999) 2489–2496; doi:10.1021/ic981116n

data_4322027
_publ_contact_author
;
    Masanobu Hidai
 Department of Chemistry and Biotechnology, Graduate School of Engineering,
The University of Tokyo, Hongo, Bunkyo-ku, Tokyo 113-8656, Japan
;
_publ_contact_author_fax         ' +81-3-5800-6945 '
_publ_contact_author_phone       ' +81-3-5800-6945 ext 7261 '
_publ_section_title
;
 Synthesis and Structures of Tungsten (1-Pyridinio)imido Complexes and
 Their Facile N-N Bond Cleavage1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2489
_journal_page_last               2496
_journal_paper_doi               10.1021/ic981116n
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C23 H29 Cl3 N2 O6 P2 W'
_chemical_formula_weight         781.65
_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'
_audit_creation_date             'Mon Aug 17 14:04:23 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                98.640(10)
_cell_angle_beta                 96.330(9)
_cell_angle_gamma                96.472(9)
_cell_formula_units_Z            2
_cell_length_a                   10.068(1)
_cell_length_b                   10.756(1)
_cell_length_c                   14.323(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.6
_cell_volume                     1510.9(3)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.08616
_diffrn_orient_matrix_UB_12      -0.03665
_diffrn_orient_matrix_UB_13      0.01150
_diffrn_orient_matrix_UB_21      0.05233
_diffrn_orient_matrix_UB_22      0.08496
_diffrn_orient_matrix_UB_23      0.00072
_diffrn_orient_matrix_UB_31      -0.00141
_diffrn_orient_matrix_UB_32      0.02095
_diffrn_orient_matrix_UB_33      0.07028
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7273
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -0.69
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.237
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             768.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.48
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.014
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5741
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.2300
_refine_ls_shift/su_mean         0.0080
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0289
_refine_ls_wR_factor_ref         0.0289
_reflns_number_gt                5741
_reflns_number_total             6907
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic981116n_2.cif
_cod_data_source_block           '[WCl2(NNC5H4OMe-4)(CO)(PMe2Ph)2][ClO4]'
_cod_original_cell_volume        1510.7(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C23 H29 Cl3 N2 O6 P2 W '
_cod_database_code               4322027