2,2,5,7,8-Pentamethylchroman-6-yl 2,3,4,6-tetra-<i>O</i>-acetyl-α-<small>D</small>-glucopyranoside from synchrotron data
Brzezinski, Krzysztof; Wałejko, Piotr; Baj, Aneta; Witkowski, Stanisław; Dauter, Zbigniew; Acta Crystallographica Section E 67 (2011) o718–; doi:10.1107/S160053681100626X

data_2229383
_publ_section_title
;
 2,2,5,7,8-Pentamethylchroman-6-yl
 2,3,4,6-tetra-<i>O</i>-acetyl-\a-<small>D</small>-glucopyranoside from
 synchrotron data
;
_journal_coeditor_code           GK2341
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o718
_journal_paper_doi               10.1107/S160053681100626X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C28 H38 O11'
_chemical_formula_moiety         'C28 H38 O11'
_chemical_formula_sum            'C28 H38 O11'
_chemical_formula_weight         550.58
_chemical_name_systematic
;
2,2,5,7,8-Pentamethylchroman-6-yl
2,3,4,6-tetra-<i>O</i>-acetyl-\a-D-glucopyranoside
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                85.74(5)
_cell_angle_beta                 89.13(5)
_cell_angle_gamma                88.16(5)
_cell_formula_units_Z            2
_cell_length_a                   8.660(10)
_cell_length_b                   11.300(10)
_cell_length_c                   14.550(10)
_cell_measurement_reflns_used    5956
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.55
_cell_measurement_theta_min      1.50
_cell_volume                     1419(2)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'NECAT APS beamline software'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PyMOL (DeLano, 2002)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Mar Research MAR315 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Si111 double crystal'
_diffrn_radiation_source         'NECAT 24ID-C synchrotron beamline APS, USA'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.59040
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8538
_diffrn_reflns_theta_full        22.55
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski <i>et al.</i>, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         5956
_refine_ls_number_restraints     752
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0671P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                5260
_reflns_number_total             5956
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2341.cif
_cod_data_source_block           I
_cod_database_code               2229383
_cod_database_fobs_code          2229383