trans-W(Cmesityl)(dmpe)2H: Revealing a Highly Polar W-H Bond and H-Mobility in Liquid and Solid State
Fenglou Zou; Franck Furno; Thomas Fox; Helmut W. Schmalle; Heinz Berke; Jürgen Eckert; Zema Chowdhury; Peter Burger; Journal of the American Chemical Society 129 (2007) 7195–7205; doi:10.1021/ja069140k

data_4109467
_publ_section_title
;
 trans-W(Cmesityl)(dmpe)2H: Revealing a Highly Polar W-H Bond and
 H-Mobility in Liquid and Solid State
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7195
_journal_page_last               7205
_journal_paper_doi               10.1021/ja069140k
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C22 H44 P4 W'
_chemical_formula_sum            'C22 H44 P4 W'
_chemical_formula_weight         616.30
_chemical_name_systematic
; 
 [Trans-hydrido-(2,3,5-trimethylphenylcarbyne)-
 bis(1,2-dimethylphosphino)ethane]tungsten
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.376(10)
_cell_angle_beta                 67.246(9)
_cell_angle_gamma                66.989(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0806(9)
_cell_length_b                   12.6747(12)
_cell_length_c                   12.8077(10)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.30
_cell_volume                     1371.3(2)
_computing_cell_refinement       'Stoe IPDS software'
_computing_data_collection       'Stoe IPDS software'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    'PLATON, PLUTON (Spek, 1990, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_sigmaI/netI    0.1667
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10799
_diffrn_reflns_theta_full        25.88
_diffrn_reflns_theta_max         25.88
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ' image'
_diffrn_standards_interval_time  9.0
_diffrn_standards_number         '50 to 200'
_exptl_absorpt_coefficient_mu    4.451
_exptl_absorpt_correction_T_max  0.9027
_exptl_absorpt_correction_T_min  0.7612
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Coppens et al. 1965'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       needle
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.793
_refine_diff_density_min         -1.708
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                3247
_reflns_number_total             4983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja069140ksi20070110_035822.cif
_cod_data_source_block           fen192
_cod_database_code               4109467