A tetraphenylborate-based anionic metal-organic framework as a versatile solid electrolyte for fast Li<sup>+</sup>, Na<sup>+</sup>, K<sup>+</sup>, Mg<sup>2+</sup>, Ca<sup>2+</sup>, and Zn<sup>2+</sup> transportation.
Xia, Qingchun; Han, Kaixin; Ma, Xuxiao; Qiu, Pengtao; Li, Zhiyong; Chen, Xuenian; Chemical science 15 (2024) 17579–17589; doi:10.1039/d4sc02861a

data_1572826
_publ_section_title
;
 A tetraphenylborate-based anionic metal-organic framework as a versatile
 solid electrolyte for fast Li<sup>+</sup>, Na<sup>+</sup>, K<sup>+</sup>,
 Mg<sup>2+</sup>, Ca<sup>2+</sup>, and Zn<sup>2+</sup> transportation.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              17579
_journal_page_last               17589
_journal_paper_doi               10.1039/d4sc02861a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C31.5 H23.5 B Er1.5 N O10.5'
_chemical_formula_sum            'C31.5 H23.5 B Er1.5 N O10.5'
_chemical_formula_weight         845.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-28 deposited with the CCDC.	2024-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.6786(5)
_cell_length_b                   24.8964(4)
_cell_length_c                   13.9814(3)
_cell_measurement_reflns_used    11715
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      70.7700
_cell_measurement_theta_min      4.4550
_cell_volume                     11375.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.974
_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    -19.00  25.00   1.00    3.00    --  -35.37  57.00 -30.00   44
  2  \w     24.00  86.00   1.00    3.00    --   35.37-125.00 150.00   62
  3  \w    -31.00  85.00   1.00    3.00    --   35.37   0.00-120.00  116
  4  \w     46.00 107.00   1.00   12.00    --  106.50-111.00 150.00   61
  5  \w     38.00 122.00   1.00   12.00    --  106.50 -45.00-120.00   84
  6  \w     37.00  63.00   1.00   12.00    --  106.50 -30.00 150.00   26
  7  \w     75.00 105.00   1.00   12.00    --  106.50 -95.00 -30.00   30
  8  \w     92.00 128.00   1.00   12.00    --  106.50 -30.00 150.00   36
  9  \w     87.00 133.00   1.00   12.00    --  106.50 -77.00   0.00   46
 10  \w     41.00  68.00   1.00   12.00    --  106.50 -77.00   0.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0213294000
_diffrn_orient_matrix_UB_12      0.0537974000
_diffrn_orient_matrix_UB_13      -0.0222012000
_diffrn_orient_matrix_UB_21      0.0011172000
_diffrn_orient_matrix_UB_22      0.0146640000
_diffrn_orient_matrix_UB_23      0.1071343000
_diffrn_orient_matrix_UB_31      0.0419971000
_diffrn_orient_matrix_UB_32      0.0267805000
_diffrn_orient_matrix_UB_33      -0.0138107000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25680
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.295
_diffrn_reflns_theta_min         3.438
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    0.988
_exptl_crystal_description       block
_exptl_crystal_F_000             3284
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         11018
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0631P)^2^+30.4995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8425
_reflns_number_total             11018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02861a2.cif
_cod_data_source_block           bairx2168c
_cod_depositor_comments
'Adding full bibliography for 1572825--1572826.cif.'
_cod_original_formula_sum        'C31.50 H23.50 B Er1.50 N O10.50'
_cod_database_code               1572826
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 O1 B1 Er1 Li1 N1'
_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
2. Restrained distances
 Er1-O6 \\sim Er2-O5
 with sigma of 0.01
3. Restrained planarity
 C29, C30, C31, N1, O6
 with sigma of 0.01
 C32, C33, C34, N2, O5
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31 \\sim N1 \\sim O6 \\sim C32 \\sim C33 \\sim C34 \\sim
N2 \\sim O5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C29, C30, C31, N1, O6, C32, C33, C34, N2, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Same fragment restrains
{C29, C30, C31, N1, O6} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C32, C33, C34, N2, O5}
7. Others
 Fixed Sof: C29(0.5) H29(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C31(0.5)
 H31A(0.5) H31B(0.5) H31C(0.5) N1(0.5) O6(0.5) C32(0.5) H32(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) N2(0.5)
 O5(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27),
  C35(H35), C29(H29), C32(H32)
8.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31399
_shelx_hkl_checksum              24674
_shelx_fab_checksum              95743
_olex2_date_sample_data_collection 2018-12-10
_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 1.346
_oxdiff_exptl_absorpt_empirical_full_min 0.347