Modulating proton diffusion and conductivity in metal-organic frameworks by incorporation of accessible free carboxylic acid groups
Rought, Peter; Marsh, Christopher; Pili, Simona; Silverwood, Ian Philip; Garcia Sakai, Victoria; Li, Ming; Brown, Martyn; Argent, Stephen; Vitorica-Yrzebal, Inigo; Whitehead, George F. S.; Warren, Mark R.; Yang, Sihai; Schroder, Martin; Chemical Science  (2019) –; doi:10.1039/C8SC03022G

data_1550175
_publ_section_title
;
 Modulating proton diffusion and conductivity in metal-organic frameworks
 by incorporation of accessible free carboxylic acid groups
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03022G
_journal_year                    2019
_chemical_formula_moiety         'C25 H21 Ba N O10'
_chemical_formula_sum            'C25 H21 Ba N O10'
_chemical_formula_weight         632.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-06-15 deposited with the CCDC.
2018-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                114.960(4)
_cell_angle_beta                 94.483(3)
_cell_angle_gamma                104.346(4)
_cell_formula_units_Z            2
_cell_length_a                   7.9225(3)
_cell_length_b                   12.5631(6)
_cell_length_c                   14.0398(5)
_cell_measurement_reflns_used    6646
_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      28.9480
_cell_measurement_theta_min      3.7570
_cell_volume                     1200.53(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.834
_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     16.00  51.00   1.00    1.00    --  -17.92  57.00   0.00   35
  2  \w     47.00  73.00   1.00    1.00    --   19.02  19.00 120.00   26
  3  \w     -8.00  81.00   1.00    1.00    --   19.02  77.00  90.00   89
  4  \w    -31.00  11.00   1.00    1.00    --  -17.92 -77.00 120.00   42
  5  \w    -50.00  46.00   1.00    1.00    --   19.02 -77.00 -30.00   96
  6  \w     52.00  78.00   1.00    1.00    --   19.02-178.00 -90.00   26
  7  \w    -86.00  -7.00   1.00    1.00    --  -17.92 -57.00-150.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.342
_diffrn_reflns_theta_min         3.273
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.750
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0382P)^2^+1.6124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5035
_reflns_number_total             5491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03022g2.cif
_cod_data_source_block           ams27
_cod_original_cell_volume        1200.53(9)
_cod_database_code               1550175
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.452
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B
 0.85 with sigma of 0.02
 H3A-H3B
 1.34 with sigma of 0.04
 Ba1-H3A \\sim Ba1-H3B
 with sigma of 0.02
3.a Riding coordinates:
 O3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C3(H3), C13(H13), C10(H10), C6(H6), C11(H11), C14(H14),
 C18(H18), C17(H17), C23(H23)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
3.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O7(H7)
;
_shelx_res_checksum              73625
_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
;