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_1550176
_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         'C23 H22 Ba2 O16, 3(H2 O), 0.5(C3 H7 N O)'
_chemical_formula_sum            'C24.5 H31.5 Ba2 N0.5 O19.5'
_chemical_formula_weight         919.68
_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                83.592(2)
_cell_angle_beta                 85.579(2)
_cell_angle_gamma                82.416(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3111(3)
_cell_length_b                   12.4288(4)
_cell_length_c                   14.3649(4)
_cell_measurement_reflns_used    11929
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.6544859544
_cell_measurement_theta_min      1.37578559545
_cell_volume                     1634.27(9)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.4.5-g37e56cb3-release'
_computing_data_reduction
'aimless (Evans, P. R. and Murshudov, G. N., 2013) ccp4 (Winn, M. D. et al., 2011) DIALS 1.4.5-g37e56cb3-release pointless (Evans, P., 2006) XIA2 0.5.179-gfd2bada8-dials-1.4 (Winter, G., 2010)'
_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      120
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Pilatus M2'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24057
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.837
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.993784511169
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'CCP4 7.0.027: AIMLESS, version 0.5.31 : 12/12/16 Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       needle
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.532
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8090
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0529
_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          0.1540
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6290
_reflns_number_total             8090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03022g2.cif
_cod_data_source_block           shelxt_a
_cod_original_cell_volume        1634.26(6)
_cod_original_formula_sum        'C24.50 H31.50 Ba2 N0.50 O19.50'
_cod_database_code               1550176
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.340
_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
 C26-C25
 2.4 with sigma of 0.02
 C26-C24
 2.4 with sigma of 0.02
 C24-C26
 2.4 with sigma of 0.02
 O19-C24
 1.2 with sigma of 0.02
 N1AA-C24 = N1AA-C26 = N1AA-C25
 1.4 with sigma of 0.02
 O19-N1AA
 2.3 with sigma of 0.002
 O9-H9
 0.85 with sigma of 0.002
 O8-H8
 0.85 with sigma of 0.002
 C26-C25 \\sim C25-C24
 with sigma of 0.002
 N1AA-C26 \\sim N1AA-C25 \\sim N1AA-C24
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O18 \\sim O17: within 2A with sigma of 0.0002 and sigma for terminal atoms of
0.0004
O4 \\sim O3: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C26 \\sim O19 \\sim N1AA \\sim C24 \\sim C25: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 C26, O19, N1AA, C24, C25
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: H8(0.5) H9(0.5) O4(0.5) H4A(0.5) H4B(0.5) C26(0.5) H26A(0.5)
 H26B(0.5) H26C(0.5) O19(0.5) N1AA(0.5) O3AA(0.5) H3AA(0.5) H3AB(0.5) O4AA(0.5)
 H4AA(0.5) H4AB(0.5) O3(0.5) H3A(0.5) H3B(0.5) C24(0.5) H24(0.5) C25(0.5)
 H25A(0.5) H25B(0.5) H25C(0.5) O18(0.5) H18A(0.5) H18B(0.5) O17(0.5) H17A(0.5)
 H17B(0.5)
6.a Riding coordinates:
 O8(H8), O9(H9), O11(H11A,H11B), O13(H13A,H13B), O12(H12A,H12B), O2(H2A,H2B),
 O15(H15A,H15B), O4(H4A,H4B), O16(H16A,H16B), O3AA(H3AA,H3AB), O4AA(H4AA,H4AB),
 O3(H3A,H3B), O18(H18A,H18B), O17(H17A,H17B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C19(H19), C18(H18), C11(H11), C12(H12), C14(H14), C21(H21),
 C22(H22), C24(H24)
6.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              52281
_olex2_submission_special_instructions 'No special instructions were received'