Absolute Configuration of (<i>S</i>)-(+)-[(Benzyloxymethyl)(<i>tert</i>-butyl)methylsilyl] Methyl Ketone
Bratovanov, S.; Linden, A.; Bienz, S.; Acta Crystallographica Section C 52 (1996) 1045–1047; doi:10.1107/S0108270195014338

data_2004670
_publ_section_title
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 Absolute Configuration of
 (<i>S</i>)-(+)-[(Benzyloxymethyl)(<i>tert</i>-butyl)methylsilyl]
 Methyl Ketone
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_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1045
_journal_page_last               1047
_journal_paper_doi               10.1107/S0108270195014338
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C30 H48 N2 O3 S Si'
_chemical_formula_sum            'C30 H48 N2 O3 S Si'
_chemical_formula_weight         544.87
_chemical_melting_point          365.5(15)
_chemical_name_systematic
;
(S)-(+)-[(benzyloxymethyl)(tert-butyl)methylsilyl] methyl ketone 2,4,6-
triisopropylphenylsulfonylhydrazone
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_cell_angle_alpha                97.24(1)
_cell_angle_beta                 105.824(8)
_cell_angle_gamma                93.82(1)
_cell_formula_units_Z            2
_cell_length_a                   10.890(1)
_cell_length_b                   17.714(3)
_cell_length_c                   8.940(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      18
_cell_volume                     1636.8(4)
_diffrn_ambient_temperature      243(2)
_diffrn_measurement_device       'Rigaku AFC-5R'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1165
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13818
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        insignificant
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details 'Flack (1983) parameter = -0.02(7)'
_refine_ls_abs_structure_Flack   -0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         13157
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.013
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_obs          0.0501
_refine_ls_shift/esd_max         0.30
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0712P)^2^ + 0.2780P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1446
_refine_ls_wR_factor_obs         0.1270
_reflns_number_observed          9678
_reflns_number_total             13158
_reflns_observed_criterion       F^2^>2\s(F^2^)
_cod_data_source_file            ab1320.cif
_cod_data_source_block           bz9501
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '364-367' was changed to '365.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_database_code               2004670