Enhanced proton conductivity in a flexible metal-organic framework promoted by single-crystal-to-single-crystal transformation.
Chen, Xi; Zhang, Zhongyue; Chen, Jin; Sapchenko, Sergei; Han, Xue; da-Silva, Ivan; Li, Ming; Vitorica-Yrezabal, Inigo J; Whitehead, George; Tang, Chiu C.; Awaga, Kunio; Yang, Sihai; Schröder, Martin; Chemical communications (Cambridge, England) 57 (2021) 65–68; doi:10.1039/d0cc05270a

data_7127528
_publ_section_title
;
 Enhanced proton conductivity in a flexible metal-organic framework
 promoted by single-crystal-to-single-crystal transformation.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              65
_journal_page_last               68
_journal_paper_doi               10.1039/d0cc05270a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C16 H8 O9 Pb2'
_chemical_formula_sum            'C16 H8 O9 Pb2'
_chemical_formula_weight         758.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-07 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                81.482(17)
_cell_angle_beta                 74.95(2)
_cell_angle_gamma                73.334(18)
_cell_formula_units_Z            2
_cell_length_a                   7.3121(17)
_cell_length_b                   9.4816(17)
_cell_length_c                   11.803(3)
_cell_measurement_reflns_used    757
_cell_measurement_temperature    99.8(8)
_cell_measurement_theta_max      70.0930
_cell_measurement_theta_min      5.9750
_cell_volume                     754.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.8(8)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.911
_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    -27.00  28.00   1.00    1.00    --    5.00 -66.00-103.00   55
  2  \w    -80.00   2.00   1.00    1.00    --  -44.10  66.00  31.00   82
  3  \w   -112.00 -80.00   1.00    1.00    --  -44.10 -66.00-103.00   32
  4  \w   -143.00 -77.00   1.00    1.00    -- -107.20  66.00  31.00   66
  5  \w    -76.00 -30.00   1.00    1.00    -- -107.20  66.00  31.00   46
  6  \w   -159.00 -99.00   1.00    1.00    -- -107.20 -66.00-103.00   60
  7  \w     -8.00  19.00   1.00    1.00    --    5.00  66.00  31.00   27
  8  \w    -37.00  41.00   1.00    1.00    --  -44.10  76.00-180.00   78
  9  \w    -78.00 -40.00   1.00    1.00    --  -44.10  76.00-180.00   38
 10  \w    -75.00  39.00   1.00    1.00    --  -44.10  76.00  90.00  114
 11  \w    -77.00 -15.00   1.00    1.00    --  -44.10 -66.00-103.00   62
 12  \w    -69.00 -35.00   1.00    1.00    -- -107.20  76.00-150.00   34
 13  \w   -106.00 -72.00   1.00    1.00    -- -107.20  76.00-150.00   34
 14  \w   -146.00 -98.00   1.00    1.00    -- -107.20  38.00-120.00   48
 15  \w    -47.00 -20.00   1.00    1.00    -- -107.20  76.00 -60.00   27
 16  \w   -112.00 -70.00   1.00    1.00    -- -107.20  76.00 -60.00   42
 17  \w   -195.00 -95.00   1.00    1.00    -- -107.20 -19.00  60.00  100
 18  \w    -94.00 -18.00   1.00    1.00    -- -107.20 -19.00  60.00   76
 19  \w   -147.00 -47.00   1.00    1.00    -- -107.20  76.00-180.00  100
 20  \w   -148.00-107.00   1.00    1.00    -- -107.20  76.00-150.00   41
 21  \w   -131.00 -21.00   1.00    1.00    -- -107.20  76.00  30.00  110
 22  \w    -82.00 -18.00   1.00    1.00    -- -107.20  38.00  30.00   64
 23  \w   -139.00-103.00   1.00    1.00    -- -107.20  38.00  30.00   36
 24  \w    -97.00 -18.00   1.00    1.00    -- -107.20  38.00-120.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5354
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.946
_diffrn_reflns_theta_min         3.891
_exptl_absorpt_coefficient_mu    43.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.338
_exptl_crystal_description       needle
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.031
_refine_diff_density_max         10.433
_refine_diff_density_min         -5.235
_refine_diff_density_rms         0.633
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2797
_refine_ls_wR_factor_ref         0.3038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3809
_reflns_number_total             5354
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9275\% 
 around [0.33 0.88 0.33] (reciprocal) or [0.26 0.96 0.09] (direct)
;
_cod_data_source_file            d0cc05270a2.cif
_cod_data_source_block           rms139_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7127527--7127529.cif.'
_cod_database_code               7127528
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.346
_shelx_estimated_absorpt_t_min   0.034
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.442(3)
 0.558(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Rigid body (RIGU) restrains
 C14, Pb01, O00M, C00E, C004, O006, C00D, C00O, C00V, C00F, C00Q, C005, C00R,
 C00S, O00C, O00L, C00J, C00W, Pb02, C003, C00K, C00N, O00B, O00P, O008, O009
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Rotating group:
 O4(H4A,H4B)
4.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00K(H00K), C00R(H00R), C00S(H00S), C14(H14)
;
_shelx_res_checksum              74199
_shelx_hkl_checksum              9027
_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
;