The chemistry of high valent tungsten chlorides with N-substituted ureas, including urea self-protonation reactions triggered by WCl6
Bortoluzzi, Marco; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; New J. Chem. 40 (2016) 8271–; doi:10.1039/C6NJ01822J

data_7055722
_publ_section_title
;
 The chemistry of high valent tungsten chlorides with N-substituted ureas,
 including urea self-protonation reactions triggered by WCl6
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              8271
_journal_paper_doi               10.1039/C6NJ01822J
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C10 H25 Cl6 N4 O2 W'
_chemical_formula_weight         629.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-11 deposited with the CCDC.
2016-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.100(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8051(16)
_cell_length_b                   13.364(2)
_cell_length_c                   9.6474(17)
_cell_measurement_reflns_used    6589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9195
_cell_measurement_theta_min      2.2085
_cell_volume                     1085.0(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10402
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    6.072
_exptl_absorpt_correction_T_max  0.5294
_exptl_absorpt_correction_T_min  0.4433
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1347 (selected reflections only, before parameter refinement)
 R(int) =  0.0302 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.577
_refine_diff_density_min         -2.509
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2352
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+10.4459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                2040
_reflns_number_total             2352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj01822j2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7055722--7055727.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7055722