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_4337850
_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 H22 Cl6 N W'
_chemical_formula_weight         684.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7496(16)
_cell_length_b                   15.1195(17)
_cell_length_c                   10.8580(12)
_cell_measurement_reflns_used    9290
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.730
_cell_measurement_theta_min      4.3095
_cell_volume                     2421.4(5)
_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 (Johnson, 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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16322
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    5.442
_exptl_absorpt_correction_T_max  0.3945
_exptl_absorpt_correction_T_min  0.3319
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1448 (selected reflections only, before parameter refinement)
 R(int) = 0.0688 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.897
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.036(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0269P)^2^+0.2494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0627
_reflns_number_gt                4573
_reflns_number_total             4738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5001683_si_003.cif
_cod_data_source_block           pna21
_cod_depositor_comments
'Adding full bibliography for 4337849--4337850.cif.'
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4337850