Tribenzylamine C-H Activation and Intermolecular Hydrogen Transfer Promoted by WCl6.
Bortoluzzi, Marco; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Inorganic chemistry 53 (2014) 3832–; doi:10.1021/ic5001683

data_4337849
_publ_section_title
;
 Tribenzylamine C-H Activation and Intermolecular Hydrogen Transfer
 Promoted by WCl6.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3832
_journal_paper_doi               10.1021/ic5001683
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C21 H20 Cl6 N W'
_chemical_formula_weight         682.93
_chemical_name_systematic
; 
 ? 
;
_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                69.140(3)
_cell_angle_beta                 85.436(3)
_cell_angle_gamma                85.915(3)
_cell_formula_units_Z            2
_cell_length_a                   10.288(3)
_cell_length_b                   10.937(3)
_cell_length_c                   11.342(3)
_cell_measurement_reflns_used    2674
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.846
_cell_measurement_theta_min      2.231
_cell_volume                     1187.5(6)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Jonson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11628
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    5.548
_exptl_absorpt_correction_T_max  0.5805
_exptl_absorpt_correction_T_min  0.4187
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.0980 (selected reflections only, before parameter refinement)
 R(int) = 0.0475 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.369
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                3384
_reflns_number_total             4478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5001683_si_002.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 4337849--4337850.cif.'
_cod_original_cell_volume        1187.5(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4337849