5'-Methylsulfanyl-4'-oxo-7'-phenyl-3',4'-dihydro-1'<i>H</i>-spiro[cyclohexane-1,2'-quinazoline]-8'-carbonitrile dimethylformamide monosolvate
Liu, Xuan; Shi, Daxin; Tang, Jianhong; Yang, Deli; Li, Jiarong; Acta Crystallographica Section E 67 (2011) o2016–; doi:10.1107/S1600536811026948

data_2230984
_publ_section_title
;
 5'-Methylsulfanyl-4'-oxo-7'-phenyl-3',4'-dihydro-1'<i>H</i>-spiro[cyclohexane-1,2'-quinazoline]-8'-carbonitrile
 dimethylformamide monosolvate
;
_journal_coeditor_code           AA2012
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2016
_journal_paper_doi               10.1107/S1600536811026948
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H21 N3 O S, C3 H7 N O'
_chemical_formula_moiety         'C21 H21 N3 O S, C3 H7 N O'
_chemical_formula_sum            'C24 H28 N4 O2 S'
_chemical_formula_weight         436.56
_chemical_name_systematic
;
5'-Methylsulfanyl-4'-oxo-7'-phenyl-3',4'-dihydro-1'<i>H</i>-
spiro[cyclohexane-1,2'-quinazoline]-8'-carbonitrile dimethylformamide
monosolvate
;
_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                95.092(3)
_cell_angle_beta                 98.156(4)
_cell_angle_gamma                109.833(3)
_cell_formula_units_Z            2
_cell_length_a                   9.415(3)
_cell_length_b                   10.615(3)
_cell_length_c                   12.037(3)
_cell_measurement_reflns_used    3507
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.117
_cell_measurement_theta_min      2.488
_cell_volume                     1108.0(5)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku AFC10/Saturn724+'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11758
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.9788
_exptl_absorpt_correction_T_min  0.9473
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0568P)^2^+0.1600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                4274
_reflns_number_total             5754
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            aa2012.cif
_cod_data_source_block           I
_cod_original_cell_volume        1108.0(6)
_cod_database_code               2230984
_cod_database_fobs_code          2230984