Stereoselective synthesis of polyhydroxylated aminocyclohexanes.
Ahmad, Sajjad; Thomas, Lynne H.; Sutherland, Andrew; Organic & biomolecular chemistry 9 (2011) 2801–2808; doi:10.1039/c0ob00619j

data_7151731
_publ_section_title
;
 Stereoselective synthesis of polyhydroxylated aminocyclohexanes.
;
_journal_issue                   8
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2801
_journal_page_last               2808
_journal_paper_doi               10.1039/c0ob00619j
_journal_volume                  9
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_formula_sum            'C8 H12 Cl3 N O4'
_chemical_formula_weight         292.54
_chemical_name_systematic
;
(1S,2S,3S,4S)-1-(2?,2?,2?-trichloromethylcarbonylamino)-2,3,4-
trihydroxycyclohexane
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-08-12T11:31:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.296(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   39.705(2)
_cell_length_b                   5.8312(3)
_cell_length_c                   20.2162(14)
_cell_measurement_reflns_used    7537
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.27
_cell_measurement_theta_min      6.05
_cell_volume                     4679.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku R-axis/RAPID'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1025
_diffrn_reflns_av_unetI/netI     0.1599
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13482
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.3751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear 1.4.0 (Rigaku, 2008)'
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.76
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         9273
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1714
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+31.8892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                4852
_reflns_number_total             9273
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c0ob00619j.txt
_cod_data_source_block           sa188a
_cod_depositor_comments
;
 Removing the '_symmetry_space_group_name' data item since it was not found
 in the core CIF dictionary and the same information was already provided in
 the official space group data items. No information was lost by removing this
 data item.

 Antanas Vaitkus,
 2017-03-06
;
_cod_database_code               7151731