Spiro[cyclopentane-1,2'(1'<i>H</i>)-pyrido[2,3-<i>d</i>]pyrimidin]-4'(3'<i>H</i>)-one
Shi, Daxin; Yang, Liupan; Tang, Jianhong; Wang, Xiuzhen; Li, Jiarong; Acta Crystallographica Section E 66 (2010) o2301–; doi:10.1107/S1600536810027479

data_2227809
_publ_section_title
;
 Spiro[cyclopentane-1,2'(1'<i>H</i>)-pyrido[2,3-<i>d</i>]pyrimidin]-4'(3'<i>H</i>)-one
;
_journal_coeditor_code           LX2156
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2301
_journal_paper_doi               10.1107/S1600536810027479
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C11 H13 N3 O'
_chemical_formula_moiety         'C11 H13 N3 O'
_chemical_formula_sum            'C11 H13 N3 O'
_chemical_formula_weight         203.24
_chemical_name_systematic
;
Spiro[cyclopentane-1,2'(1'<i>H</i>)-pyrido[2,3-<i>d</i>]pyrimidin]-
4'(3'<i>H</i>)-one
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.4000(10)
_cell_length_b                   12.1650(15)
_cell_length_c                   15.370(2)
_cell_measurement_reflns_used    9441
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      35.60
_cell_measurement_theta_min      1.30
_cell_volume                     1944.6(4)
_computing_cell_refinement       'Crystal Clear-SM Expert (Rigaku/MSC, 2009)'
_computing_data_collection       'Crystal Clear-SM Expert (Rigaku/MSC, 2009)'
_computing_data_reduction        'Crystal Clear-SM Expert (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      113(2)
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite  multilayer'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21571
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_correction_T_min  0.9709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear-SM Expert; Rigaku/MSC, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0569P)^2^+0.6834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                2168
_reflns_number_total             2314
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            lx2156.cif
_cod_data_source_block           I
_cod_database_code               2227809
_cod_database_fobs_code          2227809