5,5'-(Ethyne-1,2-diyl)diisophthalic acid dimethyl sulfoxide tetrasolvate
Münch, Alexander S.; Katzsch, Felix; Weber, Edwin; Mertens, Florian O. R. L.; Acta Crystallographica Section E 69 (2013) o908–o909; doi:10.1107/S1600536813013068

data_2238002
_publ_section_title
;
 5,5'-(Ethyne-1,2-diyl)diisophthalic acid dimethyl sulfoxide tetrasolvate
;
_journal_coeditor_code           RK2402
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o908
_journal_page_last               o909
_journal_paper_doi               10.1107/S1600536813013068
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C18 H10 O8, 4C2 H6 O S'
_chemical_formula_moiety         'C18 H10 O8, 4(C2 H6 O S)'
_chemical_formula_sum            'C26 H34 O12 S4'
_chemical_formula_weight         666.81
_chemical_melting_point_gt       623
_chemical_name_systematic
;
5,5'-(Ethyne-1,2-diyl)diisophthalic acid dimethyl sulfoxide tetrasolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 95.9700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1406(2)
_cell_length_b                   8.7328(2)
_cell_length_c                   21.4351(5)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      49.59
_cell_measurement_theta_min      2.52
_cell_volume                     1515.56(6)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2007)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2007)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2007)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20635
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.8770
_exptl_absorpt_correction_T_min  0.8065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.277
_refine_ls_extinction_coef       0.0065(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0228P)^2^+1.1796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                2567
_reflns_number_total             2666
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2402.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               2238002
_cod_database_fobs_code          2238002