10'-Chloro-3',4'-dihydro-2'<i>H</i>-spiro[cyclopropane-1,7'(6'<i>H</i>)-pyrimido[2,1-<i>a</i>]isoquinolin]-6'-one
Okuda, Kensuke; Hirota, Takashi; Nishina, Yuta; Ishida, Hiroyuki; Acta Crystallographica Section E 68 (2012) o3252–; doi:10.1107/S1600536812044261

data_2236186
_publ_section_title
;
 10'-Chloro-3',4'-dihydro-2'<i>H</i>-spiro[cyclopropane-1,7'(6'<i>H</i>)-pyrimido[2,1-<i>a</i>]isoquinolin]-6'-one
;
_journal_coeditor_code           FF2085
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3252
_journal_paper_doi               10.1107/S1600536812044261
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C14 H13 Cl N2 O'
_chemical_formula_moiety         'C14 H13 Cl N2 O'
_chemical_formula_sum            'C14 H13 Cl N2 O'
_chemical_formula_weight         260.72
_chemical_name_systematic
;
10'-Chloro-3',4'-dihydro-2'<i>H</i>-spiro[cyclopropane-
1,7'(6'<i>H</i>)-pyrimido[2,1-<i>a</i>]isoquinolin]-6'-one
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.8746(5)
_cell_length_b                   13.3273(7)
_cell_length_c                   9.8331(6)
_cell_measurement_reflns_used    15021
_cell_measurement_temperature    180.0(10)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.1
_cell_volume                     1163.00(11)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku/MSC, 2004)'
_computing_data_collection       'PROCESS-AUTO (Rigaku/MSC, 2004)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPIDII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17373
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(NUMABS; Higashi, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             544.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.152
_refine_ls_abs_structure_details 'Flack (1983), 1571 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3359
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0483P)^2^+0.1225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                3095
_reflns_number_total             3359
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ff2085.cif
_cod_data_source_block           I
_cod_original_cell_volume        1163.01(11)
_cod_database_code               2236186
_cod_database_fobs_code          2236186