An orthorhombic polymorph of 3-oxapentane-1,5-diyl bis(<i>p</i>-toluenesulfonate)
Andrey A. Yakovenko; Jose B. Gallegos; Robert D. Long; Tatiana V. Timofeeva; Mikhail Yu. Antipin; Acta Crystallographica Section E 62 (2006) o2484–o2486; doi:10.1107/S1600536806018782

data_2209188
_publ_section_title
;
 An orthorhombic polymorph of 3-oxapentane-1,5-diyl
 bis(<i>p</i>-toluenesulfonate)
;
_journal_coeditor_code           HB2051
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2484
_journal_page_last               o2486
_journal_paper_doi               10.1107/S1600536806018782
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C18 H22 O7 S2'
_chemical_formula_moiety         'C18 H22 O7 S2'
_chemical_formula_sum            'C18 H22 O7 S2'
_chemical_formula_weight         414.48
_chemical_name_systematic
;
3-oxapentane-1,5-diyl bis(p-toluenesulfonate)
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.914(2)
_cell_length_b                   5.6447(6)
_cell_length_c                   15.4723(15)
_cell_measurement_reflns_used    5696
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.63
_cell_volume                     1913.9(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    SHELXTL-NT
_computing_publication_material  SHELXTL-NT
_computing_structure_refinement  SHELXTL-NT
_computing_structure_solution    'SHELXTL-NT (Sheldrick, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17461
_diffrn_reflns_theta_full        29.49
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.01P)^2^+2.05P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                2462
_reflns_number_total             2621
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2051.cif
_cod_data_source_block           I
_cod_database_code               2209188
_cod_database_fobs_code          2209188