Crystal structures of 2-methyl-pyridinium hydrogen 2,3-bis-(4-methyl-benzo-yloxy)succinate and bis-[4-methyl-pyridinium hydrogen 2,3-bis-(4-methyl-benzo-yloxy)succinate] penta-hydrate.
Sivakumar, P.; Israel, S.; Chakkaravarthi, G.; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 1483–1487; doi:10.1107/S2056989017012981

data_2311427
_publ_section_title
;
 Crystal structures of 2-methyl-pyridinium hydrogen
 2,3-bis-(4-methyl-benzo-yloxy)succinate and bis-[4-methyl-pyridinium
 hydrogen 2,3-bis-(4-methyl-benzo-yloxy)succinate] penta-hydrate.
;
_journal_coeditor_code           ZS2388
_journal_issue                   'Pt 10'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1483
_journal_page_last               1487
_journal_paper_doi               10.1107/S2056989017012981
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C20 H17 O8 +, C6 H8 N-, 2.5H2 O'
_chemical_formula_moiety         'C20 H17 O8, C6 H8 N, 2.5(H2 O)'
_chemical_formula_sum            'C26 H30 N O10.5'
_chemical_formula_weight         524.51
_chemical_name_common
;
Bis-[4-methylpyridinium hydrogen 2,3-bis(4-methylbenzoyloxy)succinate]
pentahydrate
;
_chemical_name_systematic
;
Bis-[4-methylpyridinium hydrogen 2,3-bis(4-methylbenzoyloxy)succinate]
pentahydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                75.646(2)
_cell_angle_beta                 88.438(2)
_cell_angle_gamma                86.344(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5106(2)
_cell_length_b                   10.0155(3)
_cell_length_c                   18.5203(5)
_cell_measurement_reflns_used    9138
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      2.3
_cell_volume                     1346.81(7)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2016  (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2016 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26169
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.129
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       block
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.230
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2690 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.6(3)
_refine_ls_extinction_coef       0.032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2016 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         9433
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0673P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                6749
_reflns_number_total             9433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zs2388sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
;

2022-12-20
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C20 H17 O8), 2(C6 H8 N), 5(H2 O)'
_cod_original_formula_iupac      '2C20 H17 O8 +, 2C6 H8 N-, 5H2 O'
_cod_original_formula_sum        'C52 H60 N2 O21'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1049.02
_cod_database_code               2311427
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_checksum              56260
_shelx_res_checksum              17465