Methyl 2,3-di-<i>O</i>-acetyl-4-<i>O</i>-levulinoyl-1-<i>O</i>-(2,2,2-trichloro-2-iminoethyl)-<small>L</small>-idopyranosiduronate
Cai, Chao; Wei, Guohua; Du, Yuguo; Acta Crystallographica Section E 66 (2010) o949–; doi:10.1107/S1600536810010895

data_2225464
_publ_section_title
;
 Methyl
 2,3-di-<i>O</i>-acetyl-4-<i>O</i>-levulinoyl-1-<i>O</i>-(2,2,2-trichloro-2-iminoethyl)-<small>L</small>-idopyranosiduronate
;
_journal_coeditor_code           BT5207
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o949
_journal_paper_doi               10.1107/S1600536810010895
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C18 H22 Cl3 N O11'
_chemical_formula_moiety         'C18 H22 Cl3 N O11'
_chemical_formula_sum            'C18 H22 Cl3 N O11'
_chemical_formula_weight         534.72
_chemical_name_systematic
;
Methyl 2,3-di-<i>O</i>-acetyl-4-<i>O</i>-levulinoyl-1-<i>O</i>-(2,2,2-trichloro-
2-iminoethyl)-L-idopyranosiduronate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0498(10)
_cell_length_b                   9.7560(11)
_cell_length_c                   26.570(3)
_cell_measurement_reflns_used    1098
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.17
_cell_volume                     2345.9(5)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2001)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2001)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP area-detector'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16340
_diffrn_reflns_theta_full        68.21
_diffrn_reflns_theta_max         68.21
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.3953
_exptl_absorpt_correction_T_min  0.2862
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.483
_refine_ls_abs_structure_details 'Flack (1983), 1804  Friedel pairs'
_refine_ls_abs_structure_Flack   0.023(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+1.8534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                3893
_reflns_number_total             4259
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5207.cif
_cod_data_source_block           I
_cod_original_cell_volume        2345.8(4)
_cod_database_code               2225464
_cod_database_fobs_code          2225464