<i>rac</i>-(1<i>S</i>*,4a<i>S</i>*,8a<i>S</i>*)-4a-Hydroxy-2-methylperhydrospiro[isoquinoline-4,1'-cyclohexan]-2'-one
Siaka, Sorho; Soldatenkov, Anatoly T.; Malkova, Anastasia V.; Soldatova, Svetlana A.; Khrustalev, Victor N.; Acta Crystallographica Section E 69 (2013) o628–; doi:10.1107/S1600536813007010

data_2237998
_publ_section_title
;
 <i>rac</i>-(1<i>S</i>*,4a<i>S</i>*,8a<i>S</i>*)-4a-Hydroxy-2-methylperhydrospiro[isoquinoline-4,1'-cyclohexan]-2'-one
;
_journal_coeditor_code           RK2397
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o628
_journal_paper_doi               10.1107/S1600536813007010
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C15 H25 N O2'
_chemical_formula_moiety         'C15 H25 N O2'
_chemical_formula_sum            'C15 H25 N O2'
_chemical_formula_weight         251.36
_chemical_melting_point_gt       437
_chemical_melting_point_lt       439
_chemical_name_systematic
;
<i>rac</i>-(1<i>S</i>*,4a<i>S</i>*,8a<i>S</i>*)-4a-Hydroxy-2-methylperhydrospiro[isoquinoline-4,1'-cyclohexan]-2'-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   calc
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8438(2)
_cell_length_b                   18.5756(7)
_cell_length_c                   12.2148(5)
_cell_measurement_reflns_used    6340
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.62
_cell_measurement_theta_min      2.19
_cell_volume                     1320.66(9)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2001)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2005)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2001)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXTL</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine--focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17142
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0368
_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^)+(0.055P)^2^+0.4P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                3221
_reflns_number_total             3852
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2397.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2237998
_cod_database_fobs_code          2237998