(3<i>R</i>,4<i>S</i>,5<i>R</i>)-Methyl 3,5-bis[(<i>tert</i>-butyldimethylsilyl)oxy]-4-methoxycyclohex-1-enecarboxylate
Liu, Ri; Shi, Yu; Xu, Chun-Xiu; Li, Yi-Liang; Acta Crystallographica Section E 69 (2013) o632–; doi:10.1107/S1600536813007551

data_2238063
_publ_section_title
;
 (3<i>R</i>,4<i>S</i>,5<i>R</i>)-Methyl
 3,5-bis[(<i>tert</i>-butyldimethylsilyl)oxy]-4-methoxycyclohex-1-enecarboxylate
;
_journal_coeditor_code           VM2187
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o632
_journal_paper_doi               10.1107/S1600536813007551
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C21 H42 O5 Si2'
_chemical_formula_moiety         'C21 H42 O5 Si2'
_chemical_formula_sum            'C21 H42 O5 Si2'
_chemical_formula_weight         430.72
_chemical_name_systematic
'Methyl (3<i>R</i>,4<i>S</i>,5<i>R</i>)-3,5-bis[(<i>tert</i>-butyldimethylsilyl)oxy]-4-methoxycyclohex-1-enecarboxylate'
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.997(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.760(5)
_cell_length_b                   8.321(4)
_cell_length_c                   14.601(7)
_cell_measurement_reflns_used    4632
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.9
_cell_volume                     1291.2(11)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.22
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.1005
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13589
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_correction_T_min  0.9682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.285
_refine_ls_abs_structure_details 'Flack (1983), 2745 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.04(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         6015
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                4456
_reflns_number_total             6015
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            vm2187.cif
_cod_data_source_block           I
_cod_original_cell_volume        1291.3(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2238063
_cod_database_fobs_code          2238063