3-<i>tert</i>-Butyl-2-oxo-1-oxaspiro[4.5]dec-3-en-4-yl 4-chlorobenzoate
Wang, Zong-cheng; Cheng, Jing-li; Zhao, Jin-hao; Yu, Feng; Acta Crystallographica Section E 67 (2011) o2804–; doi:10.1107/S1600536811034684

data_2232056
_publ_section_title
;
 3-<i>tert</i>-Butyl-2-oxo-1-oxaspiro[4.5]dec-3-en-4-yl 4-chlorobenzoate
;
_journal_coeditor_code           SI2372
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2804
_journal_paper_doi               10.1107/S1600536811034684
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H23 Cl O4'
_chemical_formula_moiety         'C20 H23 Cl O4'
_chemical_formula_sum            'C20 H23 Cl O4'
_chemical_formula_weight         362.83
_chemical_name_systematic
;
3-<i>tert</i>-Butyl-2-oxo-1-oxaspiro[4.5]dec-3-en-4-yl 4-chlorobenzoate
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            32
_cell_length_a                   36.8219(15)
_cell_length_b                   15.9526(7)
_cell_length_c                   25.9325(9)
_cell_measurement_reflns_used    23569
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     15232.9(11)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_reduction
'CrystalStructure (Rigaku Americas & Rigaku, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rolling anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35855
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.8956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             6144
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.316
_refine_ls_abs_structure_details 'Flack (1983), 4227 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8661
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0399P)^2^+3.4469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                5087
_reflns_number_total             8661
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2372.cif
_cod_data_source_block           I
_cod_database_code               2232056
_cod_database_fobs_code          2232056