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_7127527
_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         '0.25(C48 H48 N4 O20 Pb4)'
_chemical_formula_sum            'C12 H12 N O5 Pb'
_chemical_formula_weight         457.42
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-04-07 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                111.886(4)
_cell_angle_beta                 101.798(3)
_cell_angle_gamma                103.943(4)
_cell_formula_units_Z            4
_cell_length_a                   10.4855(4)
_cell_length_b                   11.1137(5)
_cell_length_c                   12.4920(4)
_cell_measurement_reflns_used    4165
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      26.3440
_cell_measurement_theta_min      1.8610
_cell_volume                     1239.04(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -44.00 -18.00   1.00    1.00    --   -7.70  31.00  57.00   26
  2  \w    -95.00  28.00   1.00    1.00    --   -7.70 -31.00-102.00  123
  3  \w    -86.00  25.00   1.00    1.00    --   -7.70 -57.00  90.00  111
  4  \w    -94.00  16.00   1.00    1.00    --   -7.70 -57.00-180.00  110
  5  \w    -31.00  -2.00   1.00    1.00    --   -7.70 -57.00 -30.00   29
  6  \w      7.00  64.00   1.00    1.00    --   -7.70  31.00  57.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0730453000
_diffrn_orient_matrix_UB_12      0.0350721000
_diffrn_orient_matrix_UB_13      0.0240782000
_diffrn_orient_matrix_UB_21      0.0103087000
_diffrn_orient_matrix_UB_22      -0.0635949000
_diffrn_orient_matrix_UB_23      -0.0100969000
_diffrn_orient_matrix_UB_31      0.0015576000
_diffrn_orient_matrix_UB_32      -0.0105063000
_diffrn_orient_matrix_UB_33      -0.0592295000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24359
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         1.859
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.632
_exptl_absorpt_correction_T_max  0.513
_exptl_absorpt_correction_T_min  0.134
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.051
_refine_diff_density_max         5.219
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7619
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0681P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6439
_reflns_number_total             7619
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9588\% 
 around [0.70 0.71 -0.00] (reciprocal) or [0.67 0.66 0.33] (direct)
;
_cod_data_source_file            d0cc05270a2.cif
_cod_data_source_block           s5102r_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7127527--7127529.cif.'
_cod_original_cell_volume        1239.04(9)
_cod_database_code               7127527
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C24H24N2O10Pb2
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H15A(0.074) H15B(0.074) H15C(0.074) H18(0.019) H16A(0.087)
 H16B(0.087) H16C(0.087) H3(0.019) H22A(0.089) H22B(0.089) H22C(0.089)
 H23A(0.095) H23B(0.095) H23C(0.095) H8(0.021) H13(0.023) H17A(0.077)
 H17B(0.077) H17C(0.077) H11(0.02) H20(0.019) H24A(0.092) H24B(0.092)
 H24C(0.092)
 Fixed X: H15A(0.784876) H15B(0.883659) H15C(0.943435) H18(0.478257)
 H16A(0.854639) H16B(0.94824) H16C(0.787842) H3(0.483186) H22A(1.171925)
 H22B(1.074419) H22C(1.198234) H23A(1.101324) H23B(1.022972) H23C(1.177189) H8(-
 0.01195) H13(0.189088) H17A(0.726324) H17B(0.69605) H17C(0.847174) H11(-
 0.202544) H20(0.52252) H24A(0.846271) H24B(0.957124) H24C(0.804816)
 Fixed Y: H15A(0.671518) H15B(0.653881) H15C(0.706183) H18(0.304261)
 H16A(0.324932) H16B(0.451729) H16C(0.389358) H3(0.517815) H22A(1.431154)
 H22B(1.289287) H22C(1.294398) H23A(1.197432) H23B(1.285172) H23C(1.356598)
 H8(0.044165) H13(-0.001096) H17A(0.514736) H17B(0.595097) H17C(0.637333) H11(-
 0.001544) H20(0.703297) H24A(1.268427) H24B(1.418335) H24C(1.391949)
 Fixed Z: H15A(-0.046279) H15B(-0.125307) H15C(0.01611) H18(0.342286) H16A(-
 0.173167) H16B(-0.182128) H16C(-0.251974) H3(0.145171) H22A(0.398348)
 H22B(0.28802) H22C(0.38634) H23A(0.52411) H23B(0.595449) H23C(0.607737) H8(-
 0.345932) H13(-0.060347) H17A(0.147072) H17B(0.070668) H17C(0.156854) H11(-
 0.106915) H20(0.496339) H24A(0.244065) H24B(0.315858) H24C(0.31992)
;
_shelx_res_checksum              57236
_shelx_hkl_checksum              87953
_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 1.844
_oxdiff_exptl_absorpt_empirical_full_min 0.594
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2