Allowing the direct interaction of N-aryl α-diimines with a high valent metal chloride: one-pot WCl6-promoted formation of quinoxalinium salts
Bartalucci, Niccolò; Bortoluzzi, Marco; Funaioli, Tiziana; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton Trans.  (2017) –; doi:10.1039/C7DT03226A

data_7044297
_publ_section_title
;
 Allowing the direct interaction of N-aryl \a-diimines with a high valent
 metal chloride: one-pot WCl6-promoted formation of quinoxalinium salts
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03226A
_journal_year                    2017
_chemical_formula_sum            'C22 H28 Cl4 N2 W'
_chemical_formula_weight         646.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-22 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.770(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3214(13)
_cell_length_b                   12.5342(15)
_cell_length_c                   17.149(2)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.590
_cell_measurement_theta_min      2.4565
_cell_volume                     2353.1(5)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            25047
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.375
_exptl_absorpt_correction_T_max  0.3369
_exptl_absorpt_correction_T_min  0.1465
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1680 (selected reflections only, before parameter refinement)
 R(int) =  0.0948 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.945
_refine_diff_density_min         -3.493
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+122.6080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4141
_reflns_number_total             4578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03226a3.cif
_cod_data_source_block           4b
_cod_database_code               7044297
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.480
_shelx_estimated_absorpt_t_max   0.565
_shelx_res_checksum              67651