Crystalline potassium boryl dithiolate and diselenolate.
Dai, Yuyang; Wang, Yu; Wang, Liliang; Qi, Fan; Li, Qianli; Kong, Lingbing; Chemical communications (Cambridge, England) 61 (2024) 169–172; doi:10.1039/d4cc05240d

data_7134007
_publ_section_title
;
 Crystalline potassium boryl dithiolate and diselenolate.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              169
_journal_page_last               172
_journal_paper_doi               10.1039/d4cc05240d
_journal_volume                  61
_journal_year                    2024
_chemical_formula_moiety         'C84 H99 B3 K6 O3 S6, C4 H8 O'
_chemical_formula_sum            'C88 H107 B3 K6 O4 S6'
_chemical_formula_weight         1688.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-14 deposited with the CCDC.	2024-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                88.753(3)
_cell_angle_beta                 70.986(3)
_cell_angle_gamma                68.924(3)
_cell_formula_units_Z            2
_cell_length_a                   14.8368(5)
_cell_length_b                   17.0181(6)
_cell_length_c                   20.5205(7)
_cell_measurement_reflns_used    6698
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      70.2080
_cell_measurement_theta_min      3.3860
_cell_volume                     4544.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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     24.00  73.00   1.00    2.56    --   48.20 -95.00 -16.00   49
  2  \w     -8.00  20.00   1.00    2.56    --   48.20 -95.00 -16.00   28
  3  \w    -43.00  25.00   1.00    2.56    --  -48.20  38.00   0.00   68
  4  \w    -43.00  25.00   1.00    2.56    --  -48.20  38.00-120.00   68
  5  \w    -76.00  24.00   1.00    2.56    --  -48.20  95.00  93.00  100
  6  \w   -120.00 -73.00   1.00    2.56    --  -48.20-125.00 150.00   47
  7  \w    -55.00 -28.00   1.00   10.00    --  -86.25  95.00  93.00   27
  8  \w   -154.00 -83.00   1.00   10.00    --  -86.25 -95.00 -16.00   71
  9  \w    153.00 178.00   1.00   10.00    --  106.49  38.00 -60.00   25
 10  \w    108.00 155.00   1.00   10.00    --  106.49  95.00  93.00   47
 11  \w     94.00 177.00   1.00   10.00    --  106.49  19.00  30.00   83
 12  \w     94.00 178.00   1.00   10.00    --  106.49  19.00  60.00   84
 13  \w     93.00 141.00   1.00   10.00    --  106.49  38.00 -60.00   48
 14  \w     94.00 178.00   1.00   10.00    --  106.49  38.00-120.00   84
 15  \w     93.00 174.00   1.00   10.00    --  106.49  38.00 -30.00   81
 16  \w     46.00 105.00   1.00   10.00    --  106.49 -95.00 -16.00   59
 17  \w     39.00 106.00   1.00   10.00    --  106.49 -99.00  60.00   67
 18  \w     34.00 105.00   1.00   10.00    --  106.49 -77.00 -30.00   71
 19  \w     35.00 106.00   1.00   10.00    --  106.49 -99.00 -90.00   71
 20  \w     34.00 105.00   1.00   10.00    --  106.49 -99.00-120.00   71
 21  \w     34.00 110.00   1.00   10.00    --  106.49-125.00-120.00   76
 22  \w     34.00  66.00   1.00   10.00    --  106.49 -57.00  90.00   32
 23  \w     34.00 106.00   1.00   10.00    --  106.49 -99.00 150.00   72
 24  \w     34.00 106.00   1.00   10.00    --  106.49 -99.00  90.00   72
 25  \w     34.00  66.00   1.00   10.00    --  106.49 -57.00 150.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0432562000
_diffrn_orient_matrix_UB_12      0.0011590000
_diffrn_orient_matrix_UB_13      0.0586351000
_diffrn_orient_matrix_UB_21      -0.0732141000
_diffrn_orient_matrix_UB_22      -0.0403772000
_diffrn_orient_matrix_UB_23      0.0455601000
_diffrn_orient_matrix_UB_31      0.0823356000
_diffrn_orient_matrix_UB_32      -0.0888345000
_diffrn_orient_matrix_UB_33      -0.0294318000
_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  0.0710
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44043
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.388
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1303
_refine_ls_number_reflns         15953
_refine_ls_number_restraints     1832
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0768
_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^)+(0.0574P)^2^+8.5460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11863
_reflns_number_total             15953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05240d2.cif
_cod_data_source_block           klb-72
_cod_depositor_comments
'Adding full bibliography for 7134004--7134007.cif.'
_cod_database_code               7134007
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SCB
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.365
_reflns_odcompleteness_completeness 98.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3B-C81A
 2.38 with sigma of 0.02
 C80B-C78B = C81A-C84A
 2.4 with sigma of 0.02
 O3A-C81A = O3B-C81B = O3A-C84B = O3B-C84A
 1.54 with sigma of 0.02
 C81B-C82B = C81A-C82A = C83A-C82B = C83B-C82A = C83A-C84B = C84A-C83B
 1.54 with sigma of 0.02
 O3B-C81B = O3A-C81A = O3B-C84B = O3A-C84A
 1.44 with sigma of 0.02
 C83B-O3A
 2.38 with sigma of 0.02
 O3B-C84B = O3B-C81B
 1.44 with sigma of 0.02
 C83B-C84B = C83B-C82B = C81B-C82B
 1.52 with sigma of 0.02
 C84B-C82B
 2.35 with sigma of 0.02
 O3A-C82A
 2.35 with sigma of 0.02
 C81A-C82A = C83A-C82A = C84A-C83A
 1.52 with sigma of 0.02
 C81A-C84A
 2.35 with sigma of 0.02
 C82B-O3B
 2.35 with sigma of 0.02
 C83B-C81B
 2.35 with sigma of 0.02
 O3A-C81A = O3A-C84A
 1.44 with sigma of 0.02
 C83B-O3B
 2.35 with sigma of 0.02
 C83A-C81A
 2.38 with sigma of 0.02
 O3A-C84A = O3A-C81A
 1.44 with sigma of 0.02
 C84A-C83A = C82A-C81A
 1.53 with sigma of 0.02
 C83A-C82A
 1.54 with sigma of 0.02
 O3A-C83A
 2.38 with sigma of 0.02
 C82A-O3A
 2.38 with sigma of 0.02
 C84A-C82A
 2.38 with sigma of 0.02
 C79A-C78A \\sim C79A-C80A \\sim C78A-C77A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.001 within 2A
C61 \\sim C81 \\sim C74 \\sim C60 \\sim C55 \\sim C75 \\sim C56 \\sim C62 \\sim
C80 \\sim C77 \\sim C57 \\sim C78 \\sim C79 \\sim C58 \\sim C59 \\sim C63 \\sim
C63B \\sim C63A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C63A) \\sim Ueq, Uanis(C63B) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C56) \\sim Ueq,
Uanis(C77) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C81) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C59)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C66) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C96) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Sof(O2B)=Sof(O3B)=Sof(C77B)=Sof(H77C)=Sof(H77D)=Sof(C78B)=Sof(H78C)=Sof(H78D)=
 Sof(C79B)=Sof(H79C)=Sof(H79D)=Sof(C80B)=Sof(H80C)=Sof(H80D)=Sof(C81B)=
 Sof(H81C)=Sof(H81D)=Sof(C82B)=Sof(H82C)=Sof(H82D)=Sof(C83B)=Sof(H83C)=
 Sof(H83D)=Sof(C84B)=Sof(H84C)=Sof(H84D)=1-FVAR(1)
 Sof(O2A)=Sof(O3A)=Sof(C77A)=Sof(H77A)=Sof(H77B)=Sof(C78A)=Sof(H78A)=Sof(H78B)=
 Sof(C79A)=Sof(H79A)=Sof(H79B)=Sof(C80A)=Sof(H80A)=Sof(H80B)=Sof(C81A)=
 Sof(H81A)=Sof(H81B)=Sof(C82A)=Sof(H82A)=Sof(H82B)=Sof(C83A)=Sof(H83A)=
 Sof(H83B)=Sof(C84A)=Sof(H84A)=Sof(H84B)=FVAR(1)
 Sof(C85B)=Sof(H85C)=Sof(H85D)=Sof(C86B)=Sof(H86C)=Sof(H86D)=Sof(C87B)=
 Sof(H87C)=Sof(H87D)=Sof(C88B)=Sof(H88C)=Sof(H88D)=1-FVAR(2)
 Sof(C85A)=Sof(H85A)=Sof(H85B)=Sof(C86A)=Sof(H86A)=Sof(H86B)=Sof(C87A)=
 Sof(H87A)=Sof(H87B)=Sof(C88A)=Sof(H88A)=Sof(H88B)=FVAR(2)
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(H73C)=Sof(H73D)=Sof(H76C)=Sof(H76D)=
 Sof(C63B)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C74B)=Sof(H74C)=Sof(H74D)=
 Sof(C75B)=Sof(H75C)=Sof(H75D)=Sof(C74)=Sof(C63)=Sof(H63)=Sof(C58)=Sof(C57)=
 Sof(H57)=Sof(C56)=Sof(C55)=Sof(C88)=Sof(H88)=Sof(C90)=Sof(C89)=Sof(H89)=
 Sof(C92)=Sof(C93)=Sof(H93)=Sof(C91)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C96)=Sof(C50)=Sof(C51)=Sof(C68)=
 Sof(H68)=Sof(C67)=Sof(C54)=Sof(H54)=1-FVAR(3)
 Sof(C60)=Sof(C59)=Sof(H59)=Sof(C79)=Sof(C78)=Sof(H78)=Sof(C77)=Sof(C75)=
 Sof(C66)=Sof(H66)=Sof(C65)=Sof(C64)=Sof(C69)=Sof(C94)=Sof(H94)=Sof(C53)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=
 Sof(H73A)=Sof(H73B)=Sof(H76A)=Sof(H76B)=Sof(C63A)=Sof(H63A)=Sof(H63B)=
 Sof(H63C)=Sof(C74A)=Sof(H74A)=Sof(H74B)=Sof(C75A)=Sof(H75A)=Sof(H75B)=Sof(C80)=
 Sof(H80E)=Sof(H80F)=Sof(H80G)=Sof(C81)=Sof(H81E)=Sof(H81F)=Sof(H81G)=Sof(C83)=
 Sof(H83)=Sof(C84)=Sof(H84)=Sof(C85)=Sof(H85)=Sof(C82)=Sof(C86)=Sof(C87)=
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C73(H73C,H73D), C73(H73A,H73B), C76(H76C,H76D), C76(H76A,H76B), C74A(H74A,
 H74B), C75A(H75A,H75B), C77A(H77A,H77B), C78A(H78A,H78B), C79A(H79A,H79B),
 C80A(H80A,H80B), C81A(H81A,H81B), C82A(H82A,H82B), C83A(H83A,H83B), C84A(H84A,
 H84B), C74B(H74C,H74D), C75B(H75C,H75D), C77B(H77C,H77D), C78B(H78C,H78D),
 C79B(H79C,H79D), C80B(H80C,H80D), C81B(H81C,H81D), C82B(H82C,H82D), C83B(H83C,
 H83D), C84B(H84C,H84D), C85A(H85A,H85B), C86A(H86A,H86B), C87A(H87A,H87B),
 C88A(H88A,H88B), C85B(H85C,H85D), C86B(H86C,H86D), C87B(H87C,H87D), C88B(H88C,
 H88D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20), C27(H27),
 C28(H28), C29(H29), C33(H33), C35(H35), C42(H42), C44(H44), C59(H59), C78(H78),
  C66(H66), C94(H94), C63(H63), C57(H57), C83(H83), C84(H84), C85(H85),
 C88(H88), C89(H89), C93(H93), C68(H68), C54(H54)
5.c Fitted hexagon refined as free rotating group:
 C60(C59,C79,C78,C77,C75), C66(C65,C64,C69,C94,C53), C74(C63,C58,C57,C56,C55),
 C96(C50,C51,C68,C67,C54)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C70(H70A,H70B,
 H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C63A(H63A,H63B,H63C),
 C63B(H63D,H63E,H63F), C80(H80E,H80F,H80G), C81(H81E,H81F,H81G), C95(H95A,H95B,
 H95C), C52(H52A,H52B,H52C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              71833
_shelx_hkl_checksum              4781
_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 1.858
_oxdiff_exptl_absorpt_empirical_full_min 0.754