7'-Amino-1'<i>H</i>-spiro[cycloheptane-1,2'-pyrimido[4,5-<i>d</i>]pyrimidin]-4'(3'<i>H</i>)-one
Chen, Shu; Shi, Daxin; Liu, Mingxing; Li, Jiarong; Acta Crystallographica Section E 68 (2012) o2546–; doi:10.1107/S1600536812031492

data_2235771
_publ_section_title
;
 7'-Amino-1'<i>H</i>-spiro[cycloheptane-1,2'-pyrimido[4,5-<i>d</i>]pyrimidin]-4'(3'<i>H</i>)-one
;
_journal_coeditor_code           CV5317
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2546
_journal_paper_doi               10.1107/S1600536812031492
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C12 H17 N5 O'
_chemical_formula_moiety         'C12 H17 N5 O'
_chemical_formula_sum            'C12 H17 N5 O'
_chemical_formula_weight         247.31
_chemical_name_systematic
;
7'-Amino-1'<i>H</i>-spiro[cycloheptane-1,2'-pyrimido[4,5-<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 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 110.287(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.798(3)
_cell_length_b                   10.365(3)
_cell_length_c                   11.341(3)
_cell_measurement_reflns_used    4105
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.026
_cell_measurement_theta_min      1.965
_cell_volume                     1190.6(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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9163
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.215
_refine_ls_extinction_coef       0.0058(19)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0495P)^2^+0.9600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                3237
_reflns_number_total             3450
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv5317.cif
_cod_data_source_block           I
_cod_original_cell_volume        1190.5(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2235771
_cod_database_fobs_code          2235771