Traceless Solid-Phase Synthesis of Nitrogen-Containing Heterocycles and Their Biological Evaluations as Inhibitors of Neuronal Sodium Channels
Kong, Kah-Hoe; Chen, Yu; Ma, Xiang; Chui, Wai Keung; Lam, Yulin; Journal of Combinatorial Chemistry 6 (2004) 928–; doi:10.1021/cc049910t

data_1506799
_publ_section_title
;
 Traceless Solid-Phase Synthesis of Nitrogen-Containing Heterocycles and
 Their Biological Evaluations as Inhibitors of Neuronal Sodium Channels
;
_journal_issue                   6
_journal_name_full               'Journal of Combinatorial Chemistry'
_journal_page_first              928
_journal_paper_doi               10.1021/cc049910t
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C16 H14 N2 S'
_chemical_formula_weight         266.35
_chemical_name_systematic
; 
 4,6-Diphenyl-3,4-dihydro-1H-pyrimidine-2-thione  
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.6750(10)
_cell_angle_beta                 72.7560(10)
_cell_angle_gamma                65.3710(10)
_cell_formula_units_Z            6
_cell_length_a                   11.3899(8)
_cell_length_b                   12.0714(8)
_cell_length_c                   17.4959(11)
_cell_measurement_reflns_used    2527
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.02
_cell_measurement_theta_min      2.20
_cell_volume                     2078.9(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.1306
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28013
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  0.964544
_exptl_absorpt_correction_T_min  0.781511
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.740
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         10019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.740
_refine_ls_R_factor_all          0.1408
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0348P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                3841
_reflns_number_total             10019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cc049910tsi20040505_113933.cif
_cod_data_source_block           4,6-Diphenyl-3,4-dihydro-1H-pyrimidine-2-thione
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1506799