6'-Bromo-1'<i>H</i>-spiro[cyclohexane-1,2'-pyrido[2,3-<i>d</i>]pyrimidin]-4'(3'<i>H</i>)-one
Yang, Liupan; Shi, Daxin; Chen, Shu; Chai, Hongxin; Li, Jiarong; Acta Crystallographica Section E 68 (2012) o178–; doi:10.1107/S1600536811052299

data_2233207
_publ_section_title
;
 6'-Bromo-1'<i>H</i>-spiro[cyclohexane-1,2'-pyrido[2,3-<i>d</i>]pyrimidin]-4'(3'<i>H</i>)-one
;
_journal_coeditor_code           IS5001
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o178
_journal_paper_doi               10.1107/S1600536811052299
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C12 H14 Br N3 O'
_chemical_formula_moiety         'C12 H14 Br N3 O'
_chemical_formula_sum            'C12 H14 Br N3 O'
_chemical_formula_weight         296.17
_chemical_name_systematic
;6'-Bromo-1'<i>H</i>-spiro[cyclohexane-1,2'-pyrido[2,3-
<i>d</i>]pyrimidin]-4'(3'<i>H</i>)-one
;
_space_group_IT_number           14
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.951(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.591(3)
_cell_length_b                   12.359(3)
_cell_length_c                   9.116(3)
_cell_measurement_reflns_used    3621
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.122
_cell_measurement_theta_min      2.547
_cell_volume                     1181.8(6)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2009)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2009)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2009)'
_computing_molecular_graphics    'CrystalStructure (Rigaku/MSC, 2009)'
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2009)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC10/Saturn724+'
_diffrn_measurement_method       '\f and \w 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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10128
_diffrn_reflns_theta_full        29.10
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.465
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku/MSC, 2009)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.664
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0295P)^2^+0.1260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                2283
_reflns_number_total             3160
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            is5001.cif
_cod_data_source_block           I
_cod_original_cell_volume        1181.7(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2233207
_cod_database_fobs_code          2233207