2-Amino-4-(2-chlorophenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4<i>H</i>-chromene-3-carbonitrile hemihydrate
Hu, Xiao-Lei; Wang, Zhong-Xia; Wang, Fang-Ming; Han, Guang-Fan; Acta Crystallographica Section E 68 (2012) o823–; doi:10.1107/S1600536812003807

data_2234038
_publ_section_title
;
 2-Amino-4-(2-chlorophenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4<i>H</i>-chromene-3-carbonitrile
 hemihydrate
;
_journal_coeditor_code           XU5439
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o823
_journal_paper_doi               10.1107/S1600536812003807
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C18 H17 Cl N2 O2, 0.5H2 O'
_chemical_formula_moiety         'C18 H17 Cl N2 O2, 0.5(H2 O)'
_chemical_formula_sum            'C18 H18 Cl N2 O2.5'
_chemical_formula_weight         337.80
_chemical_name_systematic
;
2-amino-4-(2-chlorophenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-
4<i>H</i>-chromene-3-carbonitrile hemihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 111.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   31.431(6)
_cell_length_b                   9.3230(19)
_cell_length_c                   25.079(5)
_cell_measurement_reflns_used    3715
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      23.87
_cell_measurement_theta_min      2.12
_cell_volume                     6850(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15314
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_correction_T_min  0.9452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.502
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0954P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1677
_reflns_number_gt                3806
_reflns_number_total             6243
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5439.cif
_cod_data_source_block           I
_cod_original_cell_volume        6850(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2234038
_cod_database_fobs_code          2234038