Crystal structure of 3S,4'S,6'S-2-benzyl-3-[(tert-butyl-dimethyl-siloxy)- (2',2'-dimethyl-1,3-dioxolan-4'-yl)-6'-methyl]-4-[2-(trimethylsilyl) ethoxy]-3.6-dihydro-2H-1,2-oxazine, C~28~H~49~NO~5~Si~2~
Al-Harrasi, A.; Brüdgam, I.; Hartl, H.; Reißig, H.-U.; Zeitschrift für Kristallographie - New Crystal Structures 221 (2006) 12–14; doi:

data_8101883
_publ_section_title
;
Crystal structure of 3S,4'S,6'S-2-benzyl-3-[(tert-butyl-dimethyl-siloxy)-
(2',2'-dimethyl-1,3-dioxolan-4'-yl)-6'-methyl]-4-[2-(trimethylsilyl)
ethoxy]-3.6-dihydro-2H-1,2-oxazine, C~28~H~49~NO~5~Si~2~
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              12
_journal_page_last               14
_journal_volume                  221
_journal_year                    2006
_chemical_formula_sum            'C28 H49 N O5 Si2'
_chemical_formula_weight         535.86
_chemical_name_systematic
;3S,4'S,6'S-2-benzyl-3-[(tert-butyldimethylsiloxy)-(2',2'-dimethyl-1,3-dioxolan-
4'-yl)-6'-methyl]-4-[2-(trimethylsilyl)ethoxy]-3.6-dihydro-2H-1,2-oxazine
;
_space_group_IT_number           4
_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                 102.978(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.325(3)
_cell_length_b                   11.850(2)
_cell_length_c                   19.459(4)
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      1.61
_cell_volume                     3218.8(11)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'phi/omega, Delta(omega) = 0.3\%'
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0936
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22282
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.61
_diffrn_standards_interval_count '20 sec frame'
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          .65
_exptl_crystal_size_mid          .13
_exptl_crystal_size_min          .05
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         14174
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                8416
_reflns_number_total             14174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1671.cff
_cod_data_source_block           orgal2a
_cod_original_cell_volume        3218.7(12)
_cod_original_sg_symbol_H-M      P12(1)1
_cod_database_code               8101883