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_7127688
_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            'C22 H36 N4 O6 S2'
_chemical_formula_weight         516.67
_chemical_name_systematic        UPC-H7
_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   geom
_audit_creation_date             2020-02-02
_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                 96.082(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7754(3)
_cell_length_b                   12.5427(4)
_cell_length_c                   22.3714(7)
_cell_measurement_reflns_used    5036
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.8950
_cell_measurement_theta_min      3.9930
_cell_volume                     2727.52(15)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9950
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.162
_diffrn_reflns_theta_min         3.974
_exptl_absorpt_coefficient_mu    2.120
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0761P)^2^+4.7934P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.1996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4410
_reflns_number_total             5070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05402j2.cif
_cod_data_source_block           UPC-H7
_cod_database_code               7127688
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.676
_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 Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C18(H18A,
 H18B,H18C)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C13(H13), C7(H7), C8(H8), C10(H10), C2(H2), C11(H11), C3(H3)
2.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B)
;
_shelx_res_checksum              72614
_shelx_hkl_checksum              71007
_olex2_submission_special_instructions 'No special instructions were received'