(5<i>S</i>,6<i>R</i>)-6-Bromo-6-methyl-5-phenyl-3,4,5,6-tetrahydro-2<i>H</i>-cyclopenta[<i>b</i>]pyran-7-one
Ieawsuwan, Winai; Bolte, Michael; Acta Crystallographica Section E 67 (2011) o2748–; doi:10.1107/S1600536811038232

data_2231859
_publ_section_title
;
 (5<i>S</i>,6<i>R</i>)-6-Bromo-6-methyl-5-phenyl-3,4,5,6-tetrahydro-2<i>H</i>-cyclopenta[<i>b</i>]pyran-7-one
;
_journal_coeditor_code           DS2143
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2748
_journal_paper_doi               10.1107/S1600536811038232
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C15 H15 Br O2'
_chemical_formula_moiety         'C15 H15 Br O2'
_chemical_formula_sum            'C15 H15 Br O2'
_chemical_formula_weight         307.18
_chemical_name_systematic
;
(5<i>S</i>,6<i>R</i>)-6-Bromo-6-methyl-5-phenyl-3,4,5,6-tetrahydro-2<i>H</i>-
cyclopenta[<i>b</i>]pyran-7-one
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2217(11)
_cell_length_b                   11.5041(12)
_cell_length_c                   12.9149(17)
_cell_measurement_reflns_used    7315
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.6
_cell_volume                     1370.1(3)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_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  0.0775
_diffrn_reflns_av_sigmaI/netI    0.1036
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11129
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.992
_exptl_absorpt_correction_T_max  0.9156
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.072
_refine_diff_density_min         -1.129
_refine_ls_abs_structure_details 'Flack  (1983), 1009 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0820
_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^)+(0.1273P)^2^+1.2132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2168
_reflns_number_gt                1849
_reflns_number_total             2407
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ds2143.cif
_cod_data_source_block           I
_cod_database_code               2231859
_cod_database_fobs_code          2231859