6-Methoxy-2-phenyl-4,4a,6,7,8,8a-hexahydro-2<i>H</i>-pyrano[3,2-<i>d</i>][1,3]dioxine-7,8-diyl bis(4-methylbenzene-1-sulfonate)
Wardell, James L.; Tiekink, Edward R. T.; Acta Crystallographica Section E 68 (2012) o758–; doi:10.1107/S1600536812006186

data_2233850
_publ_section_title
;
 6-Methoxy-2-phenyl-4,4a,6,7,8,8a-hexahydro-2<i>H</i>-pyrano[3,2-<i>d</i>][1,3]dioxine-7,8-diyl
 bis(4-methylbenzene-1-sulfonate)
;
_journal_coeditor_code           HB6633
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o758
_journal_paper_doi               10.1107/S1600536812006186
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C28 H30 O10 S2'
_chemical_formula_moiety         'C28 H30 O10 S2'
_chemical_formula_sum            'C28 H30 O10 S2'
_chemical_formula_weight         590.64
_chemical_name_systematic
;
6-Methoxy-2-phenyl-4,4a,6,7,8,8a-hexahydro-2<i>H</i>-
pyrano[3,2-<i>d</i>][1,3]dioxine-7,8-diyl bis(4-methylbenzene-1-sulfonate)
;
_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                   5.7031(16)
_cell_length_b                   17.020(5)
_cell_length_c                   28.084(8)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.4
_cell_volume                     2726.0(14)
_computing_cell_refinement       'CrystalClear-SM Expert (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert (Rigaku, 2011)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Rigaku AFC12 (Right): Kappa three-circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            25991
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear-SM Expert; Rigaku, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.384
_refine_ls_abs_structure_details 'Flack (1983), with 2656 Friedel pairs'
_refine_ls_abs_structure_Flack   0.21(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0820
_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^)+(0.0335P)^2^+1.4810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                5326
_reflns_number_total             6262
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6633.cif
_cod_data_source_block           I
_cod_database_code               2233850
_cod_database_fobs_code          2233850