Physico-chemical study of new supramolecular-architectured hybrid organic–inorganic sulfates incorporating diammoniumdiphenylsulfone cations
Bouguerra, Manel; Mahroug, Adel; Wróbel, Agata; Trzybiński, Damian; Woźniak, Krzysztof; Belhouchet, Mohamed; RSC Advances 11 (2021) 26368–26378; doi:10.1039/D1RA03696C

data_7243336
_publ_section_title
;
 Physico-chemical study of new supramolecular-architectured hybrid
 organic--inorganic sulfates incorporating diammoniumdiphenylsulfone
 cations
;
_journal_issue                   42
_journal_name_full               'RSC Advances'
_journal_page_first              26368
_journal_page_last               26378
_journal_paper_doi               10.1039/D1RA03696C
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C12 H14 N2 O2 S, O4 S'
_chemical_formula_sum            'C12 H14 N2 O6 S2'
_chemical_formula_weight         346.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2021-04-26 deposited with the CCDC.	2021-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.307(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.1122(18)
_cell_length_b                   11.7047(5)
_cell_length_c                   8.0292(3)
_cell_measurement_reflns_used    2256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.7050
_cell_measurement_theta_min      2.9400
_cell_volume                     2812.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4391
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -8.00  41.00   1.00    1.00    --    0.00 -57.00 -60.00   49
  2  \w     32.00 126.00   1.00    2.50    --   55.02  45.00 -30.00   94
  3  \w    104.00 146.00   1.00    3.00    --  110.04  50.00 -90.00   42
  4  \w    120.00 160.00   1.00    3.00    --  110.04 111.00 -90.00   40
  5  \w     98.00 143.00   1.00    2.50    --   55.02 125.00-180.00   45
  6  \w     83.00 134.00   1.00    3.00    --  110.04 178.00 -90.00   51
  7  \w     64.00 174.00   1.00    3.00    --  110.04  38.00   0.00  110
  8  \w     58.00 115.00   1.00    3.00    --  110.04-111.00 120.00   57
  9  \w     55.00  96.00   1.00    3.00    --  110.04-111.00 -30.00   41
 10  \w     35.00 108.00   1.00    3.00    --  110.04-111.00-120.00   73
 11  \w     19.00  75.00   1.00    3.00    --  110.04 -50.00-150.00   56
 12  \w    -45.00  54.00   1.00    2.50    --   55.02 -77.00-120.00   99
 13  \w     27.00  54.00   1.00    3.00    --  110.04-111.00 120.00   27
 14  \w    -82.00 -30.00   1.00    1.00    --    0.00 -57.00 -60.00   52
 15  \w    -93.00 -39.00   1.00    2.50    --  -55.02 125.00 -60.00   54
 16  \w   -144.00 -93.00   1.00    2.50    --  -55.02 -94.00  30.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0195412000
_diffrn_orient_matrix_UB_12      -0.0091992000
_diffrn_orient_matrix_UB_13      0.1688875000
_diffrn_orient_matrix_UB_21      -0.0446404000
_diffrn_orient_matrix_UB_22      -0.0422781000
_diffrn_orient_matrix_UB_23      -0.0914369000
_diffrn_orient_matrix_UB_31      0.0166246000
_diffrn_orient_matrix_UB_32      -0.1243186000
_diffrn_orient_matrix_UB_33      0.0187585000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10170
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5010
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0625P)^2^+3.4906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3647
_reflns_number_total             5010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03696c2.cif
_cod_data_source_block           3-3
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C24 H28 N4 O12 S4'
_cod_original_formula_weight         692.74
_cod_original_formula_moiety         '2(C12 H14 N2 O2 S), 2(O4 S)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7243336
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H,H,H,H,H,H,H,H) groups
2. Restrained distances
 N16A-H16C
 0.87 with sigma of 0.01
 N16A-H16B
 0.87 with sigma of 0.01
 N16A-H16A
 0.87 with sigma of 0.01
 N17A-H17C
 0.87 with sigma of 0.01
 N17A-H17B
 0.87 with sigma of 0.01
 N17A-H17A
 0.87 with sigma of 0.01
 N17B-H17F
 0.87 with sigma of 0.01
 N17B-H17E
 0.87 with sigma of 0.01
 N17B-H17D
 0.87 with sigma of 0.01
 N16B-H16E
 0.87 with sigma of 0.01
 N16B-H16F
 0.87 with sigma of 0.01
 N16B-H16D
 0.87 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C6A(H6A),
 C6B(H6B), C9A(H9A), C9B(H9B), C11A(H11A), C11B(H11B), C12A(H12A), C12B(H12B),
 C13A(H13A), C13B(H13B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.761