Twist and sliding dynamics between interpenetrated frames in Ti-MOF revealing high proton conductivity
Cao, Jing; Ma, Wenjie; Lyu, Kangjie; Zhuang, Lin; Cong, Hengjiang; Deng, Hexiang; Chemical Science 11 (2020) 3978–3985; doi:10.1039/C9SC06500H

data_1557627
_publ_section_title
;
 Twist and sliding dynamics between interpenetrated frames in Ti-MOF
 revealing high proton conductivity
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              3978
_journal_page_last               3985
_journal_paper_doi               10.1039/C9SC06500H
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         '0.04(C84 H36 N12 O24 Ti4)'
_chemical_formula_sum            'C3.5 H1.5 N0.5 O Ti0.17'
_chemical_formula_weight         74.54
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-10 deposited with the CCDC.	2020-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            48
_cell_length_a                   21.1222(4)
_cell_length_b                   21.1222(4)
_cell_length_c                   21.1222(4)
_cell_measurement_reflns_used    4198
_cell_measurement_temperature    249.99(10)
_cell_measurement_theta_max      42.8080
_cell_measurement_theta_min      2.9120
_cell_volume                     9423.6(3)
_computing_cell_refinement
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_collection
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_reduction
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      249.99(10)
_diffrn_detector                 'Hybrid Pixel Counting (HPC) detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HyPix-6000HE'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -32.00  94.00   0.50   60.00    --    5.00  38.00-120.00  252
  2  \w    -90.00  33.00   0.50   60.00    --  -56.20  57.00 -60.00  246
  3  \w   -146.00 -96.00   0.50   60.00    --  -56.20 -38.00 -60.00  100
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from \w-scans and \phi-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0101795000
_diffrn_orient_matrix_UB_12      0.0722148000
_diffrn_orient_matrix_UB_13      -0.0026532000
_diffrn_orient_matrix_UB_21      0.0657653000
_diffrn_orient_matrix_UB_22      0.0080837000
_diffrn_orient_matrix_UB_23      -0.0305399000
_diffrn_orient_matrix_UB_31      -0.0300866000
_diffrn_orient_matrix_UB_32      -0.0067972000
_diffrn_orient_matrix_UB_33      -0.0660218000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'VariMax VHF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11570
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        44.287
_diffrn_reflns_theta_max         44.287
_diffrn_reflns_theta_min         3.624
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.534
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1231
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.495
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.1083
_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          0.3521
_refine_ls_wR_factor_ref         0.3639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                885
_reflns_number_total             1231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06500h2.cif
_cod_data_source_block           MOF-217-250K
_cod_depositor_comments
;Adding full bibliography for 1557626--1557628.cif.

 Adding full bibliography for 1557626--1557628.cif.
;
_cod_original_cell_volume        9423.6(5)
_cod_original_formula_sum        'C3.50 H1.50 N0.50 O Ti0.17'
_cod_database_code               1557627
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'H C N O Ti'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C5(H5)
;
_shelx_res_checksum              55465
_shelx_fab_checksum              79821
_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 1.607
_oxdiff_exptl_absorpt_empirical_full_min 0.668