Incisive analysis of hydrogen-bonded supramolecular architectures in designer polycyclitols: observation of some interesting self-assembly patterns
Rashid, Showkat; Husain, Ahmad; Bhat, Bilal A.; Mehta, Goverdhan; CrystEngComm 26 (2024) 1952–1961; doi:10.1039/D4CE00010B

data_7248189
_publ_section_title
;
 Incisive analysis of hydrogen-bonded supramolecular architectures in
 designer polycyclitols: observation of some interesting self-assembly
 patterns
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              1952
_journal_page_last               1961
_journal_paper_doi               10.1039/D4CE00010B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C11 H10 O6, H2 O'
_chemical_formula_sum            'C11 H12 O7'
_chemical_formula_weight         256.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-30 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.584(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.5680(2)
_cell_length_b                   27.9778(8)
_cell_length_c                   12.4818(4)
_cell_measurement_reflns_used    9649
_cell_measurement_temperature    295.5(2)
_cell_measurement_theta_max      26.7560
_cell_measurement_theta_min      2.1780
_cell_volume                     2291.30(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.5(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_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    -43.00  17.00   0.50   24.66    --  -15.60 -86.00  56.00  120
  2  \w     14.00  49.00   0.50   24.66    --   16.22 -86.00  56.00   70
  3  \w    -38.00   2.00   0.50   24.66    --   16.22 -86.00  56.00   80
  4  \w    -17.00  20.00   0.50   24.66    --  -15.60 -94.00 -30.00   74
  5  \w    -37.00  15.00   0.50   24.66    --  -15.60 -94.00 -60.00  104
  6  \w     28.00  53.00   0.50   24.66    --   16.22 -94.00 -90.00   50
  7  \w    -19.00   8.00   0.50   24.66    --  -15.60 -30.00 -60.00   54
  8  \w    -33.00  19.00   0.50   24.66    --   16.22 -94.00 -90.00  104
  9  \w    -36.00   9.00   0.50   24.66    --  -15.60 -94.00-150.00   90
 10  \w    -67.00 -33.00   0.50   24.66    --  -15.60 -30.00 -60.00   68
 11  \w    -85.00  -2.00   0.50   24.66    --  -15.60 -45.00 -60.00  166
 12  \w      3.00  89.00   0.50   24.66    --   16.22  30.00-150.00  172
 13  \w    -47.00   9.00   0.50   24.66    --  -15.60  86.00 174.00  112
 14  \w    -10.00  15.00   0.50   24.66    --   16.22  86.00 174.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0426118000
_diffrn_orient_matrix_UB_12      0.0095972000
_diffrn_orient_matrix_UB_13      -0.0465741000
_diffrn_orient_matrix_UB_21      -0.0364432000
_diffrn_orient_matrix_UB_22      -0.0199789000
_diffrn_orient_matrix_UB_23      -0.0301363000
_diffrn_orient_matrix_UB_31      -0.0924285000
_diffrn_orient_matrix_UB_32      0.0122994000
_diffrn_orient_matrix_UB_33      -0.0126270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20101
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.281
_diffrn_reflns_theta_min         2.188
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0668P)^2^+0.0191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3398
_reflns_number_total             4879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00010b2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7248187--7248191.cif.'
_cod_database_code               7248189
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H O'
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O14(H14A,H14B), O13(H13A,H13B)
2.b Ternary CH refined with riding coordinates:
 C1(H1A), C19(H19), C12(H12), C8(H8), C2(H2A), C7(H7), C18(H18), C13(H13)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C15(H15), C6(H6), C3(H3), C14(H14), C16(H16), C17(H17)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O7(H7A), O2(H2), O8(H8A)
;
_shelx_res_checksum              5179
_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 2.990
_oxdiff_exptl_absorpt_empirical_full_min 0.350