Crystal structure of [(2<i>R</i>,3<i>R</i>,4<i>S</i>)-3,4-bis(acetyloxy)-5-iodo-3,4-dihydro-2<i>H</i>-pyran-2-yl]methyl acetate
Zukerman-Schpector, Julio; Caracelli, Ignez; Stefani, Hélio A.; Shamim, Anwar; Tiekink, Edward R.T.; Acta Crystallographica Section E 71 (2015) o53–o54; doi:10.1107/S205698901402564X

data_2240336
_publ_section_title
;
 Crystal structure of
 [(2<i>R</i>,3<i>R</i>,4<i>S</i>)-3,4-bis(acetyloxy)-5-iodo-3,4-dihydro-2<i>H</i>-pyran-2-yl]methyl
 acetate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o53
_journal_page_last               o54
_journal_paper_doi               10.1107/S205698901402564X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C12 H15 I O7'
_chemical_formula_moiety         'C12 H15 I O7'
_chemical_formula_sum            'C12 H15 I O7'
_chemical_formula_weight         398.14
_chemical_name_systematic
'[(2<i>R</i>,3<i>R</i>,4<i>S</i>)-3,4-Bis(acetyloxy)-5-iodo-3,4-dihydro-2<i>H</i>-pyran-2-yl]methyl acetate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9048(2)
_cell_length_b                   8.7521(2)
_cell_length_c                   22.7094(5)
_cell_measurement_reflns_used    3256
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.73
_cell_volume                     1571.12(6)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and  DIAMOND (Brandenburg,
2006)
;
_computing_publication_material
;
MarvinSketch (ChemAxon, 2010) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR (Burla <i>et al.</i>,  2014
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            6116
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.368
_diffrn_reflns_theta_min         1.793
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       irregular
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.578
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 925 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.000(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0299P)^2^+0.3563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                2456
_reflns_number_total             2818
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7323sup1.cif
_cod_data_source_block           I
_cod_database_code               2240336
_cod_database_fobs_code          2240336
_shelx_hkl_checksum              6411
_shelx_res_checksum              91954