(+)-(1<i>R</i>,5<i>S</i>,6<i>R</i>)-1-[3-(9,9-Dimethyl-4,4-dioxo-4λ^6^-thiatricyclo[6.1.1.0^2,6^]dec-2-en-5-yl)-2-<i>tert</i>-butyldimethylsilyloxy-4,6-dimethoxyphenyl]-3-methylbutan-1-one methyl <i>tert</i>-butyl ethersolvate at 133K
Bats, Jan W.; Berger, Bernd; Gerlach, Matthias; Reggelin, Michael; Acta Crystallographica Section C 55 (1999) IUC9900002–; doi:10.1107/S0108270199099837

data_2008186
_publ_section_title
;(+)-(1<i>R</i>,5<i>S</i>,6<i>R</i>)-1-[3-(9,9-Dimethyl-4,4-dioxo-4\l^6^-thiatricyclo[6.1.1.0^2,6^]dec-2-en-5-yl)-2-<i>tert</i>-butyldimethylsilyloxy-4,6-dimethoxyphenyl]-3-methylbutan-1-one
 methyl <i>tert</i>-butyl ethersolvate at 133K
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900002
_journal_paper_doi               10.1107/S0108270199099837
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          'C30 H46 O6 S Si, 0.5C5 H12 O'
_chemical_formula_moiety         'C30 H46 O6 S Si, 0.5C5 H12 O'
_chemical_formula_sum            'C32.5 H52 O6.5 S Si'
_chemical_formula_weight         606.89
_chemical_name_systematic
;(+)-(1R,5S,6R)-1-[3-(9,9-Dimethyl-4,4-dioxo-4\l^6^-thiatricyclo[6.1.1.0^2,6^]-
dec-2-en-5-yl)-2-tert-butyldimethylsilyloxy-4,6-dimethoxy-phenyl]-3-methyl-
butan-1-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'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.129(3)
_cell_length_b                   19.201(4)
_cell_length_c                   27.672(6)
_cell_measurement_reflns_used    134
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     6976(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995) '
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'CIF in SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS in SHELXTL (Sheldrick, 1996a)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type  'Siemens SMART'
_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  0.089
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            74444
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  540
_diffrn_standards_number         332
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   'empirical (SADABS; Sheldrick, 1996b)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.324
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_coef       0.00168(12)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         13583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.103
_refine_ls_R_factor_gt           0.061
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.03P)^2^+4.80P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.114
_reflns_number_gt                9906
_reflns_number_total             13583
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qa0081.cif
_cod_data_source_block           qa0081
_cod_original_formula_sum        'C32.50 H52 O6.50 S Si'
_cod_database_code               2008186