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_7127689
_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)'
_chemical_formula_sum            'C16 H0 N11 O6 S2'
_chemical_formula_weight         506.39
_chemical_name_systematic        UPC-H8
_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     iterative
_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                 97.458(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6616(3)
_cell_length_b                   12.3127(4)
_cell_length_c                   22.5851(9)
_cell_measurement_reflns_used    3458
_cell_measurement_temperature    150(3)
_cell_measurement_theta_max      68.4150
_cell_measurement_theta_min      4.0930
_cell_volume                     2664.00(16)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_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 0.996
_diffrn_measured_fraction_theta_max 0.980
_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    -17.00  66.00   1.00    1.00    --    0.00  57.00  60.00   83
  2  \w    -61.00 -34.00   1.00    1.00    --    0.00 135.00-138.00   27
  3  \w     28.00 116.00   1.00    1.00    --   53.47  38.00-180.00   88
  4  \w     25.00  94.00   1.00    1.00    --   53.47-125.00 -90.00   69
  5  \w     38.00 123.00   1.00    1.00    --   53.47  57.00 -90.00   85
  6  \w     -6.00  50.00   1.00    1.00    --   53.47 -57.00 -60.00   56
  7  \w     35.00 107.00   1.00    1.29    --  106.95-111.00-120.00   72
  8  \w    140.00 175.00   1.00    1.29    --  106.95 111.00  30.00   35
  9  \w     85.00 177.00   1.00    1.29    --  106.95  25.00 -30.00   92
 10  \w     54.00 147.00   1.00    1.29    --  106.95 -25.00 120.00   93
 11  \w     59.00 151.00   1.00    1.29    --  106.95 178.00  90.00   92
 12  \w     53.00 107.00   1.00    1.29    --  106.95-111.00  60.00   54
 13  \w     36.00 131.00   1.00    1.29    --  106.95 -38.00  30.00   95
;
_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      0.0116941000
_diffrn_orient_matrix_UB_12      -0.0163385000
_diffrn_orient_matrix_UB_13      0.0681085000
_diffrn_orient_matrix_UB_21      0.0667359000
_diffrn_orient_matrix_UB_22      0.1132858000
_diffrn_orient_matrix_UB_23      0.0097281000
_diffrn_orient_matrix_UB_31      -0.1459305000
_diffrn_orient_matrix_UB_32      0.0503545000
_diffrn_orient_matrix_UB_33      0.0000707000
_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  0.0477
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9910
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.394
_diffrn_reflns_theta_min         3.948
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.268
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84232
_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    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+9.5553P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3949
_reflns_number_total             4988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05402j2.cif
_cod_data_source_block           UPC-H8
_cod_database_code               7127689
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N S'
_reflns_odcompleteness_completeness 99.80
_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
2.a Rotating group:
 N1(H1A,H1B), N5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C2(H2), C3(H3), C5(H5), C12(H12), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,
 H1CB,H1CC)
;
_shelx_res_checksum              54460
_shelx_hkl_checksum              31942
_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 1.866
_oxdiff_exptl_absorpt_empirical_full_min 0.374