[(2<i>R</i>,5<i>R</i>,6<i>S</i>,9<i>R</i>)-6-Isopropyl-9-methyl-1,4-dioxaspiro[4.5]decan-2-yl]methyl 4-bromobenzoate
Kiessling, Anthony; Zeller, Matthias; Acta Crystallographica Section E 67 (2011) o733–o734; doi:10.1107/S1600536811006428

data_2229526
_publ_section_title
;
 [(2<i>R</i>,5<i>R</i>,6<i>S</i>,9<i>R</i>)-6-Isopropyl-9-methyl-1,4-dioxaspiro[4.5]decan-2-yl]methyl
 4-bromobenzoate
;
_journal_coeditor_code           TK2718
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o733
_journal_page_last               o734
_journal_paper_doi               10.1107/S1600536811006428
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H27 Br O4'
_chemical_formula_moiety         'C20 H27 Br O4'
_chemical_formula_sum            'C20 H27 Br O4'
_chemical_formula_weight         411.33
_chemical_name_systematic
;
[(2<i>R</i>,5<i>R</i>,6<i>S</i>,9<i>R</i>)-6-Isopropyl-9-methyl-1,4-
dioxaspiro[4.5]decan-2-yl]methyl 4-bromobenzoate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 92.618(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.976(7)
_cell_length_b                   5.5763(9)
_cell_length_c                   16.072(3)
_cell_measurement_reflns_used    3693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.54
_cell_volume                     3847.6(11)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17537
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.158
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.000
_refine_diff_density_min         -0.753
_refine_ls_abs_structure_details 'Flack (1983), 3965 Friedel pairs'
_refine_ls_abs_structure_Flack   0.000(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9230
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                6765
_reflns_number_total             9230
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2718.cif
_cod_data_source_block           I
_cod_original_cell_volume        3847.5(11)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2229526
_cod_database_fobs_code          2229526