Crystal structure of N-((2R*,4S*)-2-tert-butyl-5-methyl-4H-1,3-dioxin- 4-yl)-2-(trimethylsilyl)ethanesulfonamide, C~14~H~29~NO~4~Si
Tatarov, E.; Bruhn, C.; Frauenrath, H.; Zeitschrift für Kristallographie - New Crystal Structures 222 (2007) 139–140; doi:

data_8102104
_publ_section_title
;
Crystal structure of N-((2R*,4S*)-2-tert-butyl-5-methyl-4H-1,3-dioxin-
4-yl)-2-(trimethylsilyl)ethanesulfonamide, C~14~H~29~NO~4~Si
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              139
_journal_page_last               140
_journal_volume                  222
_journal_year                    2007
_chemical_formula_moiety         'C14 H29 N O4 S Si'
_chemical_formula_structural     C14H29NO4SSi
_chemical_formula_sum            'C14 H29 N O4 S Si'
_chemical_formula_weight         335.53
_chemical_name_systematic
;
N-(2-tert-butyl-5-methyl-4H-1,3-dioxin-4-yl)-2-(trimethylsilyl)-
ethanesulfonamide
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   35.939(2)
_cell_length_b                   10.4219(7)
_cell_length_c                   10.1829(8)
_cell_measurement_reflns_used    20863
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.26
_cell_volume                     3814.0(4)
_computing_cell_refinement       X-AREA
_computing_data_collection       X-AREA
_computing_data_reduction        X-AREA
_computing_molecular_graphics    ORTEP-3
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      '180 frames, detector distance = 130 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18573
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.26
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.50
_diffrn_source_voltage           50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9288
_exptl_absorpt_correction_T_min  0.8683
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-red ver. 1.06 (Stoe & Cie. 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                2419
_reflns_number_total             3454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1983.cff
_cod_data_source_block           i0255
_cod_original_formula_sum        'C14 H29 N1 O4 S1 Si1'
_cod_database_code               8102104