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_7243337
_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           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 106.322(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6218(4)
_cell_length_b                   9.6697(4)
_cell_length_c                   14.1442(5)
_cell_measurement_reflns_used    4901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.4460
_cell_measurement_theta_min      3.2530
_cell_volume                     1394.20(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     32.00 143.00   1.00    1.00    --   55.02  45.00  90.00  111
  2  \w    101.00 177.00   1.00    1.00    --  110.04 111.00   0.00   76
  3  \w    105.00 176.00   1.00    1.00    --  110.04  71.00  94.67   71
  4  \w    103.00 177.00   1.00    1.00    --  110.04  77.00  60.00   74
  5  \w     68.00  95.00   1.00    1.00    --  110.04  50.00  90.00   27
  6  \w     69.00 166.00   1.00    1.00    --  110.04  77.00 120.00   97
  7  \w     69.00  96.00   1.00    1.00    --  110.04  54.00 176.20   27
  8  \w     69.00 174.00   1.00    1.00    --  110.04  77.00 150.00  105
  9  \w     70.00  96.00   1.00    1.00    --  110.04  50.00  60.00   26
 10  \w     66.00  98.00   1.00    1.00    --  110.04  63.00 120.00   32
 11  \w     67.00  93.00   1.00    1.00    --  110.04  77.00  60.00   26
 12  \w     66.00  98.00   1.00    1.00    --  110.04  63.00  60.00   32
 13  \w     67.00  94.00   1.00    1.00    --  110.04  75.00 114.05   27
 14  \w     67.00  93.00   1.00    1.00    --  110.04  63.00  90.00   26
 15  \w     67.00  93.00   1.00    1.00    --  110.04  77.00  90.00   26
 16  \w     69.00  95.00   1.00    1.00    --  110.04  72.00 143.12   26
 17  \w     68.00  95.00   1.00    1.00    --  110.04  63.00 150.00   27
 18  \w     67.00  93.00   1.00    1.00    --  110.04  71.00  94.67   26
 19  \w     61.00 148.00   1.00    1.00    --   55.02  61.00 150.00   87
 20  \w     21.00  49.00   1.00    1.00    --    0.00 -99.00 -60.00   28
 21  \w      1.00  47.00   1.00    1.00    --    0.00 -99.00-150.00   46
 22  \w     66.00 169.00   1.00    1.00    --  110.04  63.00-120.00  103
 23  \w     92.00 178.00   1.00    1.00    --  110.04  77.00-180.00   86
 24  \w     85.00 111.00   1.00    1.00    --   55.02  77.00-180.00   26
 25  \w     75.00 100.00   1.00    1.00    --  110.04  50.00-180.00   25
 26  \w     14.00  40.00   1.00    1.00    --   55.02  77.00-180.00   26
 27  \w      6.00  31.00   1.00    1.00    --    0.00  57.00-180.00   25
 28  \w     44.00  69.00   1.00    1.00    --    0.00  57.00-180.00   25
 29  \w    -38.00  -6.00   1.00    1.00    --    0.00  57.00-180.00   32
 30  \w      3.00 104.00   1.00    1.00    --   55.02 -94.00 -30.00  101
 31  \w     19.00 115.00   1.00    1.00    --  110.04-111.00-180.00   96
 32  \w     12.00  56.00   1.00    1.00    --   55.02  61.00 150.00   44
 33  \w    -91.00 -15.00   1.00    1.00    --  -55.02  30.00 150.00   76
 34  \w   -116.00 -78.00   1.00    1.00    --  -55.02-125.00 120.00   38
 35  \w     59.00 133.00   1.00    1.00    --  110.04 178.00-150.00   74
;
_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      -0.1128765000
_diffrn_orient_matrix_UB_12      -0.0122688000
_diffrn_orient_matrix_UB_13      0.0481304000
_diffrn_orient_matrix_UB_21      0.0890424000
_diffrn_orient_matrix_UB_22      0.0607281000
_diffrn_orient_matrix_UB_23      0.0963306000
_diffrn_orient_matrix_UB_31      -0.0463328000
_diffrn_orient_matrix_UB_32      0.1468257000
_diffrn_orient_matrix_UB_33      -0.0358461000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10111
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.055
_diffrn_reflns_theta_max         67.055
_diffrn_reflns_theta_min         3.256
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.787
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 1932 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4882
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0565P)^2^+0.1645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                4521
_reflns_number_total             4882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03696c2.cif
_cod_data_source_block           Manel-4-4
_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            2
_cod_original_cell_volume        1394.20(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7243337
_reflns_odcompleteness_completeness 99.96
_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
 N17A-H17E
 0.87 with sigma of 0.02
 N16A-H16E
 0.87 with sigma of 0.01
 N16A-H16E
 0.87 with sigma of 0.01
 N16A-H16D
 0.87 with sigma of 0.01
 N16A-H16F
 0.87 with sigma of 0.01
 N16B-H16B
 0.87 with sigma of 0.01
 N16B-H16A
 0.87 with sigma of 0.01
 N16B-H16C
 0.87 with sigma of 0.01
 N17A-H17F
 0.87 with sigma of 0.01
 N17A-H17D
 0.87 with sigma of 0.01
 N17A-H17E
 0.87 with sigma of 0.01
 N17B-H17C
 0.87 with sigma of 0.01
 N17B-H17A
 0.87 with sigma of 0.01
 N17B-H17B
 0.87 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B), C9B(H9B), C10B(H10B), C12B(H12B),
 C13B(H13B), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C9A(H9A), C10A(H10A),
 C12A(H12A), C13A(H13A)
;
_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 1.706
_oxdiff_exptl_absorpt_empirical_full_min 0.598