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_7044298
_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            'C24 H31 Cl8 N2 W'
_chemical_formula_weight         814.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                80.107(2)
_cell_angle_beta                 77.8480(10)
_cell_angle_gamma                89.233(2)
_cell_formula_units_Z            4
_cell_length_a                   9.9556(3)
_cell_length_b                   13.4893(4)
_cell_length_c                   23.5871(7)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.090
_cell_measurement_theta_min      2.452
_cell_volume                     3049.73(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.983
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54541
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.533
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.506
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4603
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1333 (selected reflections only, before parameter refinement)
 R(int) =  0.0500 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       prism
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.059
_refine_diff_density_min         -2.923
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         14465
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+34.4160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12637
_reflns_number_total             14465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03226a3.cif
_cod_data_source_block           1a
_cod_database_code               7044298
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.614
_shelx_res_checksum              50478