Crystal structure of 3R,4S,5R,6S,7R-5-amino-6-(tert-butyldimethylsiloxy)- 7-(tert-butyldimethylsiloxymethyl)-3-hydroxymethyl-2,2-dimethyloxepan- 4-ol, C~22~H~49~NO~5~Si~2~
Al-Harrasi, A.; Brüdgam, I.; Hartl, H.; Reißig, H.-U.; Zeitschrift für Kristallographie - New Crystal Structures 221 (2006) 131–132; doi:

data_8101884
_publ_section_title
;
Crystal structure of 3R,4S,5R,6S,7R-5-amino-6-(tert-butyldimethylsiloxy)-
7-(tert-butyldimethylsiloxymethyl)-3-hydroxymethyl-2,2-dimethyloxepan-
4-ol, C~22~H~49~NO~5~Si~2~
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              131
_journal_page_last               132
_journal_volume                  221
_journal_year                    2006
_chemical_formula_sum            'C22 H49 N O5 Si2'
_chemical_formula_weight         463.80
_chemical_name_systematic
; 
3S,4S,5R,6S,7R-5-amino-6-(tert-butyldimethylsiloxy)-7-(tert-
butyldimethylsiloxymethyl)-3-hydroxymethyl-2,2-dimethyloxepan-4-ol
;
_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                 98.015(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5288(18)
_cell_length_b                   8.1518(14)
_cell_length_c                   16.554(3)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      1.95
_cell_volume                     1406.9(4)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14327
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.95
_diffrn_standards_interval_time  '20 sec/frame'
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.237
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1021P)^2^+1.5029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1879
_reflns_number_gt                5259
_reflns_number_total             6461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1672.cff
_cod_data_source_block           orgal3nm
_cod_original_sg_symbol_H-M      P12(1)1
_cod_database_code               8101884