Activation of CN bonds by high-valent group 6 metal chlorides, including the conversion of an α-diimine into a functionalized imidazolium
Bartalucci, Niccolò; Bortoluzzi, Marco; Zacchini, Stefano; Pampaloni, Guido; Marchetti, Fabio; New Journal of Chemistry 42 (2018) 8503–; doi:10.1039/C8NJ00846A

data_7057308
_publ_section_title
;
 Activation of C&#xE001;N bonds by high-valent group 6 metal chlorides,
 including the conversion of an \a-diimine into a functionalized
 imidazolium
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8503
_journal_paper_doi               10.1039/C8NJ00846A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C28 H30 Cl6 N3 W'
_chemical_formula_weight         805.10
_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
;
2018-03-15 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.532(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3116(4)
_cell_length_b                   18.5141(9)
_cell_length_c                   22.4919(11)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1315
_cell_measurement_theta_min      2.382
_cell_volume                     3431.2(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0676
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            60561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.430
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.855
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3634
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1520 (selected reflections only, before parameter refinement)
 R(int) =  0.0726 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       prism
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.773
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         8263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0293P)^2^+4.2858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6907
_reflns_number_total             8263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00846a3.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7057306--7057308.cif.'
_cod_database_code               7057308
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.484
_shelx_estimated_absorpt_t_max   0.655
_shelx_res_checksum              87459
_shelx_fab_checksum              13294