Solid state transformations of different stoichiometric forms of an organic salt formed from 5-sulfosalicylic acid and hexamethylenetetramine upon dehydration and rehydration
Fu, Qiang; Xu, Xi-kun; Liu, Bao-kai; Guo, Fang; CrystEngComm 20 (2018) 1844–; doi:10.1039/C8CE00022K

data_7230187
_publ_section_title
;
 Solid state transformations of different stoichiometric forms of an
 organic salt formed from 5-sulfosalicylic acid and hexamethylenetetramine
 upon dehydration and rehydration
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1844
_journal_paper_doi               10.1039/C8CE00022K
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C7 H4 O6 S, 2(C6 H13 N4)'
_chemical_formula_sum            'C19 H30 N8 O6 S'
_chemical_formula_weight         498.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-11-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-11-23 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8939(7)
_cell_length_b                   12.2771(9)
_cell_length_c                   16.6849(13)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    222(2)
_cell_measurement_theta_max      28.257
_cell_measurement_theta_min      2.952
_cell_volume                     2231.5(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      222.14
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12193
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         2.952
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1549 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0193P)^2^+2.4291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                4463
_reflns_number_total             5461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00022k2.cif
_cod_data_source_block           1_2
_cod_depositor_comments
'Adding full bibliography for 7230185--7230188.cif.'
_cod_database_code               7230187
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C12(H12A,H12B), C15(H15A,H15B), C17(H17A,H17B), C10(H10A,
 H10B), C9(H9A,H9B), C16(H16A,H16B), C13(H13A,H13B), C18(H18A,H18B), C11(H11A,
 H11B), C8(H8A,H8B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3A), C4(H4)
;
_shelx_res_checksum              22801
_olex2_submission_special_instructions 'No special instructions were received'