Single-crystal-to-single-crystal transformation and proton conductivity of three hydrogen-bonded organic frameworks.
Wang, Yijie; Zhang, Minghui; Yang, Qianqian; Yin, Jianbo; Liu, Di; Shang, Yanxue; Kang, Zixi; Wang, Rongming; Sun, Daofeng; Jiang, Jianzhuang; Chemical communications (Cambridge, England) 56 (2020) 15529–15532; doi:10.1039/d0cc05402j

data_7127690
_publ_section_title
;
 Single-crystal-to-single-crystal transformation and proton conductivity
 of three hydrogen-bonded organic frameworks.
;
_journal_issue                   99
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15529
_journal_page_last               15532
_journal_paper_doi               10.1039/d0cc05402j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C14 H12 N2 O6 S2, 2(C4 H12 N), 2(H2 O)'
_chemical_formula_sum            'C22 H44 N4 O10 S2'
_chemical_formula_weight         588.73
_chemical_name_systematic        UPC-H9
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2020-02-15
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-02-15 deposited with the CCDC.	2020-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.51(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2723(18)
_cell_length_b                   18.109(3)
_cell_length_c                   14.821(3)
_cell_measurement_reflns_used    852
_cell_measurement_temperature    150(3)
_cell_measurement_theta_max      62.8060
_cell_measurement_theta_min      4.2730
_cell_volume                     2833.6(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.935
_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    -45.00  18.00   1.00   10.00    --    0.00 102.00 -62.00   63
  2  \w    -22.00  69.00   1.00   10.00    --    0.00  57.00 120.00   91
  3  \w    -16.00  75.00   1.00   25.00    --   53.47 -57.00-180.00   91
  4  \w     38.00 120.00   1.00   25.00    --   53.47  38.00 150.00   82
  5  \w     80.00 116.00   1.00   25.00    --   53.47  57.00-120.00   36
  6  \w     94.00 123.00   1.00   25.00    --   53.47  57.00 -30.00   29
  7  \w     33.00  80.00   1.00   25.00    --   53.47  57.00 -30.00   47
  8  \w     32.00 119.00   1.00   25.00    --   53.47  57.00  30.00   87
  9  \w     89.00 174.00   1.00    5.00    --  106.95  38.00  60.00   85
 10  \w     55.00 111.00   1.00    5.00    --  106.95 -50.00  30.00   56
 11  \w     83.00 158.00   1.00    5.00    --  106.95  63.00 150.00   75
 12  \w     43.00 127.00   1.00    5.00    --  106.95 -50.00-120.00   84
 13  \w    126.00 160.00   1.00    5.00    --  106.95 111.00 150.00   34
 14  \w     93.00 170.00   1.00    5.00    --  106.95  38.00 120.00   77
 15  \w     36.00 137.00   1.00    5.00    --  106.95 -91.00  60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1074628000
_diffrn_orient_matrix_UB_12      0.0565125000
_diffrn_orient_matrix_UB_13      -0.0415072000
_diffrn_orient_matrix_UB_21      0.0153884000
_diffrn_orient_matrix_UB_22      -0.0057368000
_diffrn_orient_matrix_UB_23      -0.0990849000
_diffrn_orient_matrix_UB_31      -0.0976545000
_diffrn_orient_matrix_UB_32      -0.0631824000
_diffrn_orient_matrix_UB_33      -0.0281243000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1740
_diffrn_reflns_av_unetI/netI     0.3005
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10380
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.667
_diffrn_reflns_theta_min         4.013
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.213
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.3541
_refine_ls_R_factor_gt           0.1129
_refine_ls_shift/su_max          1.658
_refine_ls_shift/su_mean         0.120
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1515P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2491
_refine_ls_wR_factor_ref         0.3817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1246
_reflns_number_total             5083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05402j2.cif
_cod_data_source_block           UPC-H9
_cod_database_code               7127690
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N S'
_reflns_odcompleteness_completeness 97.93
_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 N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5d,H5e), O9(H9a,H9b)
2.b Rotating group:
 N22(H22a,H22b), N35(H35a,H35b)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C20(H20), C34(H34)
2.d Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C5(H5a,H5b,H5c), C10(H10a,H10b,H10c), C4(H4a,H4b,H4c),
 C11(H11a,H11b,H11c), C17(H17a,H17b,H17c), C23(H23a,H23b,H23c), C18(H18a,H18b,
 H18c)
;
_shelx_res_checksum              5683
_shelx_hkl_checksum              85159
_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 39.673
_oxdiff_exptl_absorpt_empirical_full_min 0.565