(±)-Methyl 1-oxo-1<i>H</i>-spiro[benzo[<i>c</i>]pyran-3(4<i>H</i>),1'-cyclohexane]-4-carboxylate
Öztürk Yıldırım, Sema; Akkurt, Mehmet; Bogdanov, Milen G.; Kandinska, Meglena I.; Kazak, Canan; Acta Crystallographica Section E 63 (2007) o1321–o1323; doi:10.1107/S1600536807006861

data_2212666
_publ_section_title
;(+-)-Methyl
 1-oxo-1<i>H</i>-spiro[benzo[<i>c</i>]pyran-3(4<i>H</i>),1'-cyclohexane]-4-carboxylate
;
_journal_coeditor_code           PR2001
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1321
_journal_page_last               o1323
_journal_paper_doi               10.1107/S1600536807006861
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C16 H18 O4'
_chemical_formula_moiety         'C16 H18 O4'
_chemical_formula_sum            'C16 H18 O4'
_chemical_formula_weight         274.30
_chemical_name_systematic
;
(+-)-Methyl
1-oxo-1<i>H</i>-spiro[benzo[c]pyran-3(4H),1'-cyclohexane]-4-carboxylate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 95.573(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2647(9)
_cell_length_b                   14.0850(11)
_cell_length_c                   12.1150(14)
_cell_measurement_reflns_used    15642
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.22
_cell_volume                     1403.6(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22061
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        27.26
_diffrn_reflns_theta_max         27.26
_diffrn_reflns_theta_min         2.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.097
_refine_diff_density_min         -0.102
_refine_ls_extinction_coef       0.0126(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.845
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                1558
_reflns_number_total             3125
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pr2001.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212666
_cod_database_fobs_code          2212666