Thermal fragmentation of spirodithiohydantoins: A novel route to NHCs
Jishkariani, Davit; Hall, C. Dennis; Oliferenko, Alexander; Tomlin, Blake J.; Steel, Peter J.; Katritzky, Alan R.; RSC Adv. 3 (2013) 1669–; doi:10.1039/C2RA22487A

data_7238777
_publ_section_title
;
 Thermal fragmentation of spirodithiohydantoins: A novel route to NHCs
;
_journal_issue                   6
_journal_name_full               'RSC Adv.'
_journal_page_first              1669
_journal_paper_doi               10.1039/C2RA22487A
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C18 H19 N3 S'
_chemical_formula_sum            'C18 H19 N3 S'
_chemical_formula_weight         309.42
_chemical_name_common            D469
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0394(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.86514(13)
_cell_length_b                   14.6361(3)
_cell_length_c                   18.7566(3)
_cell_measurement_reflns_used    4832
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      73.7333
_cell_measurement_theta_min      3.0168
_cell_volume                     1606.12(5)
_computing_cell_refinement
;
'Mon Jul 30 16:40:32 2012'
;
_computing_data_collection
;
'Mon Jul 30 16:40:32 2012'
;
_computing_data_reduction
;
'Mon Jul 30 16:40:32 2012'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10315
_diffrn_reflns_theta_full        67.46
_diffrn_reflns_theta_max         67.46
_diffrn_reflns_theta_min         3.83
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Mon Jul 30 16:40:32 2012'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0480P)^2^+0.6550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                2446
_reflns_number_total             2883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra22487a.txt
_cod_data_source_block           d469
_cod_database_code               7238777