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_1550177
_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         'C26.5 H25.5 Ba2 N1.5 O11'
_chemical_formula_sum            'C26.5 H25.5 Ba2 N1.5 O11'
_chemical_formula_weight         815.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 92.3020(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.44352(15)
_cell_length_b                   17.2735(2)
_cell_length_c                   14.1871(2)
_cell_measurement_reflns_used    11144
_cell_measurement_temperature    120.03(10)
_cell_measurement_theta_max      73.2550
_cell_measurement_theta_min      4.0120
_cell_volume                     2802.10(6)
_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)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 4.2207
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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    -50.00  29.00   1.00    1.00    --  -42.37  38.00-150.00   79
  2  \w   -124.00 -79.00   1.00    1.00    --  -42.37 -99.00-180.00   45
  3  \w   -124.00 -79.00   1.00    1.00    --  -42.37 -99.00-120.00   45
  4  \w     17.00 112.00   1.00    1.00    --   42.37  57.00-120.00   95
  5  \w     30.00  91.00   1.00    3.00    --  103.32 -30.00-120.00   61
  6  \w     30.00  91.00   1.00    3.00    --  103.32 -30.00   0.00   61
  7  \w     20.00 108.00   1.00    3.00    --  103.32 -94.00-180.00   88
  8  \w     33.00  98.00   1.00    3.00    --  103.32 -45.00  60.00   65
  9  \w     79.00 174.00   1.00    3.00    --  103.32  45.00  60.00   95
 10  \w     20.00 108.00   1.00    3.00    --  103.32 -94.00-120.00   88
 11  \w     33.00  98.00   1.00    3.00    --  103.32 -45.00 -60.00   65
 12  \w     33.00  98.00   1.00    3.00    --  103.32 -45.00 150.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15093
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.464
_diffrn_reflns_theta_min         3.866
_exptl_absorpt_coefficient_mu    22.270
_exptl_absorpt_correction_T_max  0.432
_exptl_absorpt_correction_T_min  0.055
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.933
_exptl_crystal_description       plate
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.437
_refine_diff_density_min         -2.632
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5518
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5254
_reflns_number_total             5518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03022g2.cif
_cod_data_source_block           baprrf
_cod_original_cell_volume        2802.08(7)
_cod_original_formula_sum        'C26.50 H25.50 Ba2 N1.50 O11'
_cod_database_code               1550177
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Others
 Fixed Sof: O10(0.5) H10A(0.5) H10B(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) N1(0.5) C23(0.5) H23(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 O9(0.5)
 Fixed Uiso: H8A(0.041) H8B(0.041) H17(0.019) H6(0.022) H13(0.017) H18(0.019)
 H20(0.019) H5(0.019) H10(0.018) H7(0.02) H21(0.018) H11(0.017) H14(0.019)
 H1A(0.027) H1B(0.027) H27A(0.059) H27B(0.059) H27C(0.059) H28A(0.067)
 H28B(0.067) H28C(0.067) H26(0.055) H10A(0.065) H10B(0.065) H25A(0.182)
 H25B(0.182) H25C(0.182) H23(0.081) H24A(0.096) H24B(0.096) H24C(0.096)
 Fixed X: H8A(0.6868) H8B(0.6509) H17(0.902) H6(1.1273) H13(0.7949)
 H18(0.8109) H20(0.6155) H5(1.0311) H10(0.6857) H7(1.0209) H21(0.6939)
 H11(0.5963) H14(0.8852) H1A(0.5284) H1B(0.5719) H27A(1.0777) H27B(1.0112)
 H27C(1.1249) H28A(1.098) H28B(0.9764) H28C(1.068) H26(0.8267) H10A(0.1774)
 H10B(0.2122) H25A(0.1898) H25B(0.0739) H25C(0.0839) H23(0.1185) H24A(-0.076)
 H24B(-0.0947) H24C(-0.1047)
 Fixed Y: H8A(0.6295) H8B(0.7067) H17(0.8539) H6(0.6435) H13(0.3256)
 H18(0.9742) H20(0.8892) H5(0.7608) H10(0.5517) H7(0.5321) H21(0.7659)
 H11(0.4349) H14(0.4427) H1A(0.4238) H1B(0.4324) H27A(0.2513) H27B(0.2674)
 H27C(0.2134) H28A(0.075) H28B(0.0543) H28C(0.1101) H26(0.1151) H10A(0.6425)
 H10B(0.6681) H25A(0.4711) H25B(0.4473) H25C(0.4301) H23(0.6469) H24A(0.609)
 H24B(0.5229) H24C(0.5401)
 Fixed Z: H8A(0.5441) H8B(0.559) H17(0.1682) H6(0.2692) H13(0.2533)
 H18(0.1816) H20(0.3907) H5(0.2879) H10(0.0906) H7(0.2301) H21(0.3665)
 H11(0.0514) H14(0.2944) H1A(0.2902) H1B(0.2959) H27A(0.5457) H27B(0.4462)
 H27C(0.4516) H28A(0.5058) H28B(0.5517) H28C(0.6064) H26(0.4762) H10A(0.4204)
 H10B(0.5111) H25A(0.5266) H25B(0.5791) H25C(0.4689) H23(0.4653) H24A(0.4705)
 H24B(0.4312) H24C(0.5414)
;
_shelx_res_checksum              57036
_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
;