Synthesis of K[B3H7NH2BH2NH2B3H7] for K-ion solid-state electrolyte
Chen, Xi-Meng; Jia, Si-Han; Kang, Jiaxin; Zhang, Yichun; Ma, Yubin; Ma, Yi-ming; Jiang, Xin; Yu, Xing-Chao; Qiu, Pengtao; Chen, Xuenian; Chemical Communications  (2022) –; doi:10.1039/D2CC00408A

data_7129776
_publ_section_title
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 Synthesis of K[B3H7NH2BH2NH2B3H7] for K-ion solid-state electrolyte
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00408A
_journal_year                    2022
_chemical_formula_moiety         'C24 H88 B14 K2 N4 O12'
_chemical_formula_sum            'C24 H88 B14 K2 N4 O12'
_chemical_formula_weight         854.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-11-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-18 deposited with the CCDC.	2022-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.294(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5487(3)
_cell_length_b                   9.1479(2)
_cell_length_c                   34.5522(7)
_cell_measurement_reflns_used    5954
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.2780
_cell_measurement_theta_min      5.5270
_cell_volume                     5208.40(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.968
_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    -65.00  28.00   1.00    4.83    --  -35.62  20.00  58.00   93
  2  \w   -106.00 -50.00   1.00    4.83    --  -35.62 -20.00-108.00   56
  3  \w    -10.00  15.00   1.00    4.83    --   35.62 -20.00-108.00   25
  4  \w     33.00  59.00   1.00    4.83    --   35.62  20.00  58.00   26
  5  \w     82.00 108.00   1.00   19.30    --  107.12 -20.00-108.00   26
  6  \w    113.00 177.00   1.00   19.30    --  107.12  20.00  58.00   64
  7  \w     22.00 100.00   1.00    4.83    --   35.62  57.00-120.00   78
  8  \w     64.00 100.00   1.00    4.83    --   35.62 178.00-180.00   36
  9  \w     78.00 107.00   1.00    4.83    --   35.62-178.00-120.00   29
 10  \w     57.00  85.00   1.00    4.83    --   35.62 178.00-120.00   28
 11  \w     49.00  75.00   1.00   19.30    --  107.12 -61.00 120.00   26
 12  \w     83.00 113.00   1.00   19.30    --  107.12-111.00  90.00   30
 13  \w     37.00  63.00   1.00   19.30    --  107.12-111.00  90.00   26
 14  \w     69.00 178.00   1.00   19.30    --  107.12  15.00   0.00  109
 15  \w    140.00 176.00   1.00   19.30    --  107.12 111.00  60.00   36
 16  \w     37.00 112.00   1.00   19.30    --  107.12-111.00 -90.00   75
 17  \w    102.00 136.00   1.00   19.30    --  107.12 111.00  60.00   34
 18  \w     97.00 123.00   1.00   19.30    --  107.12 -61.00 120.00   26
 19  \w     45.00 108.00   1.00   19.30    --  107.12 -77.00 -30.00   63
 20  \w     37.00  66.00   1.00   19.30    --  107.12-111.00 -60.00   29
;
_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      0.0251389000
_diffrn_orient_matrix_UB_12      -0.0404314000
_diffrn_orient_matrix_UB_13      -0.0404870000
_diffrn_orient_matrix_UB_21      -0.0886649000
_diffrn_orient_matrix_UB_22      0.0175868000
_diffrn_orient_matrix_UB_23      -0.0173091000
_diffrn_orient_matrix_UB_31      0.0158808000
_diffrn_orient_matrix_UB_32      0.1624157000
_diffrn_orient_matrix_UB_33      -0.0082306000
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            10316
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.498
_diffrn_reflns_theta_min         5.003
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.992
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4924
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0844P)^2^+1.6958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4179
_reflns_number_total             4924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00408a2.cif
_cod_data_source_block           20210708-jsh_pl
_cod_database_code               7129776
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 B1 N1 K1 O1'
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.961
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 B2-H3D
 2 with sigma of 0.02
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56916
_shelx_fab_checksum              62492
_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 2.847
_oxdiff_exptl_absorpt_empirical_full_min 0.583