Ethyl 5-chloromethyl-2-methylsulfanyl-7-phenyl-4,7-dihydro-1,2,4-triazolo[1,5-<i>a</i>]pyrimidine-6-carboxylate
Dan-Dan Song; Qiong Chen; Acta Crystallographica Section E 64 (2008) o45–o45; doi:10.1107/S1600536807062629

data_2217120
_publ_section_title
;Ethyl
 5-chloromethyl-2-methylsulfanyl-7-phenyl-4,7-dihydro-1,2,4-triazolo[1,5-<i>a</i>]pyrimidine-6-carboxylate
;
_journal_coeditor_code           HK2399
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o45
_journal_page_last               o45
_journal_paper_doi               10.1107/S1600536807062629
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C16 H17 Cl N4 O2 S'
_chemical_formula_moiety         'C16 H17 Cl N4 O2 S'
_chemical_formula_sum            'C16 H17 Cl N4 O2 S'
_chemical_formula_weight         364.85
_chemical_name_systematic
;
Ethyl 5-chloromethyl-2-methylsulfanyl-7-phenyl-4,7-dihydro-
1,2,4-triazolo[1,5-a]pyrimidine-6-carboxylate
;
_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                106.022(2)
_cell_angle_beta                 102.631(2)
_cell_angle_gamma                109.919(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9280(8)
_cell_length_b                   9.8217(9)
_cell_length_c                   11.3775(10)
_cell_measurement_reflns_used    1660
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      22.49
_cell_measurement_theta_min      2.39
_cell_volume                     845.85(13)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
'Bruker SMART 4K CCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6662
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.418
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0839P)^2^P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1555
_reflns_number_gt                2295
_reflns_number_total             3281
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2399.cif
_cod_data_source_block           I
_cod_database_code               2217120
_cod_database_fobs_code          2217120