6-Acetoxymethyl-3-[(2-hydroxy-3-methoxybenzylidene)amino]-3,4,5,6-tetrahydro-2<i>H</i>-pyran-2,4,5-triyl triacetate
Wang, Yan Fei; Zhang, Shu-Hua; Chen, Zhen Feng; Liang, Hong; Acta Crystallographica Section E 66 (2010) o990–; doi:10.1107/S1600536810011475

data_2225699
_publ_section_title
;
 6-Acetoxymethyl-3-[(2-hydroxy-3-methoxybenzylidene)amino]-3,4,5,6-tetrahydro-2<i>H</i>-pyran-2,4,5-triyl
 triacetate
;
_journal_coeditor_code           SI2250
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o990
_journal_paper_doi               10.1107/S1600536810011475
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C22 H27 N O11'
_chemical_formula_moiety         'C22 H27 N O11'
_chemical_formula_sum            'C22 H27 N O11'
_chemical_formula_weight         481.45
_chemical_name_systematic
;
6-Acetoxymethyl-3-[(2-hydroxy-3-methoxybenzylidene)amino]-3,4,5,6-tetrahydro-
2<i>H</i>-pyran-2,4,5-triyl triacetate
;
_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           SHELXL-97
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.806(3)
_cell_length_b                   11.151(3)
_cell_length_c                   20.243(5)
_cell_measurement_reflns_used    1384
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.58
_cell_measurement_theta_min      2.62
_cell_volume                     2439.2(11)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
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_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12313
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
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_refine_diff_density_max         0.170
_refine_diff_density_min         -0.140
_refine_ls_extinction_coef       0.0074(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         2460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0823
_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
'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.1770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                1506
_reflns_number_total             2460
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            si2250.cif
_cod_data_source_block           I
_cod_database_code               2225699
_cod_database_fobs_code          2225699