A new tetrakis-substituted pyrazine carboxylic acid, 3,3',3'',3'''-{[pyrazine-2,3,5,6-tetrayltetrakis(methylene)]tetrakis(sulfanediyl)}tetrapropionic acid: crystal structures of two triclinic polymorphs and of two potassium–organic frameworks
Pacifico, Jessica; Stoeckli-Evans, Helen; Acta Crystallographica Section E 77 (2021) 480–490; doi:10.1107/S2056989021003479

data_2243801
_publ_section_title
;
 A new tetrakis-substituted pyrazine carboxylic acid,
 3,3',3'',3'''-{[pyrazine-2,3,5,6-tetrayltetrakis(methylene)]tetrakis(sulfanediyl)}tetrapropionic
 acid: crystal structures of two triclinic polymorphs and of two
 potassium--organic frameworks
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              480
_journal_page_last               490
_journal_paper_doi               10.1107/S2056989021003479
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C20 H28 N2 O8 S4'
_chemical_formula_moiety         'C20 H28 N2 O8 S4'
_chemical_formula_sum            'C20 H28 N2 O8 S4'
_chemical_formula_weight         552.68
_chemical_name_systematic
'3,3',3'',3'''-{[Pyrazine-2,3,5,6-tetrayltetrakis(methylene))tetrakis(sulfanediyl]}tetrapropionic acid'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                96.96(3)
_cell_angle_beta                 97.14(3)
_cell_angle_gamma                100.72(3)
_cell_formula_units_Z            1
_cell_length_a                   4.9424(17)
_cell_length_b                   8.993(3)
_cell_length_c                   14.190(6)
_cell_measurement_reflns_used    5563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.35
_cell_volume                     608.1(4)
_computing_cell_refinement
;
X-Area (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED32 (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020) and Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
SHELXL-2018/3 (Sheldrick, 2015), PLATON (Spek, 2020) and
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\f + \w scans'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4152
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         2.331
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.6162
_exptl_absorpt_correction_T_min  0.1442
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>ShxAbs</i>; Spek, 2020)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plate
_exptl_crystal_F_000             290
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2201
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+0.4241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                1537
_reflns_number_total             2201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2656sup1.cif
_cod_data_source_block           H4L1B
_cod_database_code               2243801
_cod_database_fobs_code          2243801
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.978
_shelx_hkl_checksum              44838
_shelx_res_checksum              27304