(+)-Methyl (4<i>R</i>,5<i>S</i>)-4-[(<i>R</i>)-1-hydroxybut-3-enyl]-5-2,2-dimethyl-trichloroacetamido-1,3-dioxane-5-carboxylate
Ohba, Shigeru; Sato, Hideyuki; Iida, Masatoshi; Chida, Noritaka; Acta Crystallographica Section E 59 (2003) o1259–o1260; doi:10.1107/S160053680301691X

data_2202695
_publ_section_title
;(+)-Methyl
 (4<i>R</i>,5<i>S</i>)-4-[(<i>R</i>)-1-hydroxybut-3-enyl]-5-2,2-dimethyl-trichloroacetamido-1,3-dioxane-5-carboxylate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1259
_journal_page_last               o1260
_journal_paper_doi               10.1107/S160053680301691X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C14 H20 Cl3 N O6'
_chemical_formula_moiety         'C14 H20 Cl3 N O6'
_chemical_formula_sum            'C14 H20 Cl3 N O6'
_chemical_formula_weight         404.67
_chemical_melting_point          .371E-305
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1926(8)
_cell_length_b                   9.1926(8)
_cell_length_c                   22.724(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297
_cell_measurement_theta_max      10.8
_cell_measurement_theta_min      10.1
_cell_volume                     1920.3(3)
_computing_cell_refinement
;
WinAFC Diffractometer Control Software
;
_computing_data_collection
;
WinAFC Diffractometer Control Software (Rigaku, 1999)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation, 2001)
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 1997)
;
_computing_structure_solution
;
SIR92 (Altomare et al., 1994)
;
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3009
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_standards_decay_%        13.3
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.51
_refine_ls_abs_structure_details 'Flack (1983), 140 Friedel pairs'
_refine_ls_abs_structure_Flack   0.16(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2388
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.0110
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0963P)^2^+1.4164P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1708
_reflns_number_gt                1963
_reflns_number_total             2388
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6093.cif
_cod_data_source_block           I
_cod_original_cell_volume        1920.2(3)
_cod_database_code               2202695
_cod_database_fobs_code          2202695