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_7134006
_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         'C32 H41 B K2 O2 Se3'
_chemical_formula_sum            'C32 H41 B K2 O2 Se3'
_chemical_formula_weight         783.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 95.480(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7889(3)
_cell_length_b                   12.3813(4)
_cell_length_c                   22.4926(6)
_cell_measurement_reflns_used    7755
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.2040
_cell_measurement_theta_min      3.7870
_cell_volume                     3545.27(17)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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    103.00 177.00   1.00    1.20    --  106.49  57.00 150.00   74
  2  \w     92.00 118.00   1.00    1.20    --  106.49  57.00   0.00   26
  3  \w    132.00 177.00   1.00    1.20    --  106.49  57.00   0.00   45
  4  \w     95.00 171.00   1.00    1.20    --  106.49 125.00 -90.00   76
  5  \w     97.00 140.00   1.00    1.20    --  106.49 141.00-119.00   43
  6  \w     35.00  66.00   1.00    1.20    --  106.49 -57.00 -60.00   31
  7  \w     66.00 114.00   1.00    1.20    --  106.49-129.00  -5.00   48
  8  \w     71.00  96.00   1.00    0.19    --   48.45-129.00  -5.00   25
  9  \w     34.00 105.00   1.00    1.20    --  106.49 -99.00-150.00   71
 10  \w     82.00 123.00   1.00    1.20    --  106.49-141.00-177.00   41
 11  \w     39.00 106.00   1.00    1.20    --  106.49 -99.00-180.00   67
 12  \w     50.00  75.00   1.00    0.19    --   48.45-141.00-177.00   25
 13  \w    -27.00  27.00   1.00    0.19    --  -48.45  19.00  90.00   54
 14  \w    -68.00 -42.00   1.00    0.19    --  -48.45 129.00  68.00   26
 15  \w    -76.00 -51.00   1.00    1.20    --  -86.25 129.00  68.00   25
 16  \w    -77.00 -22.00   1.00    1.20    --  -86.25 141.00-119.00   55
 17  \w    -43.00  22.00   1.00    0.19    --  -48.45  38.00-150.00   65
 18  \w   -115.00 -84.00   1.00    1.20    --  -86.25-129.00  -5.00   31
 19  \w   -110.00 -71.00   1.00    0.19    --  -48.45-129.00  -5.00   39
 20  \w   -117.00 -63.00   1.00    0.19    --  -48.45-141.00-177.00   54
;
_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      -0.0536745000
_diffrn_orient_matrix_UB_12      0.1063902000
_diffrn_orient_matrix_UB_13      -0.0213434000
_diffrn_orient_matrix_UB_21      0.0936993000
_diffrn_orient_matrix_UB_22      0.0642150000
_diffrn_orient_matrix_UB_23      0.0302116000
_diffrn_orient_matrix_UB_31      0.0546367000
_diffrn_orient_matrix_UB_32      -0.0056829000
_diffrn_orient_matrix_UB_33      -0.0580422000
_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  0.0747
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20480
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.065
_diffrn_reflns_theta_max         67.065
_diffrn_reflns_theta_min         3.827
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65309
_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    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6220
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0516P)^2^+6.7910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5035
_reflns_number_total             6220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05240d2.cif
_cod_data_source_block           klb-78
_cod_depositor_comments
'Adding full bibliography for 7134004--7134007.cif.'
_cod_database_code               7134006
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SeCB
_shelx_estimated_absorpt_t_max   0.376
_shelx_estimated_absorpt_t_min   0.195
_reflns_odcompleteness_completeness 98.36
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O2A \\sim C29A \\sim C31A \\sim C32A \\sim O2 \\sim C29 \\sim C30 \\sim C31
\\sim C32: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Se3 \\sim Se3A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C30 \\sim C30A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O2) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C31A) \\sim Ueq,
Uanis(C32A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(C29A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Se3) \\sim Ueq, Uanis(Se3A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=
 Sof(H32A)=Sof(H32B)=Sof(O2A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=1-FVAR(1)
 Sof(O2)=Sof(C29)=Sof(H29C)=Sof(H29D)=Sof(C30)=Sof(H30C)=Sof(H30D)=Sof(C31)=
 Sof(H31C)=Sof(H31D)=Sof(C32)=Sof(H32C)=Sof(H32D)=FVAR(1)
 Sof(Se3A)=1-FVAR(2)
 Sof(Se3)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C30A(H30A,
 H30B), C31A(H31A,H31B), C32A(H32A,H32B), C29A(H29A,H29B), C29(H29C,H29D),
 C30(H30C,H30D), C31(H31C,H31D), C32(H32C,H32D)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20)
4.c Fitted pentagon refined as free rotating group:
 C30A(C31A,C32A,O2A,C29A)
4.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)
;
_shelx_res_checksum              30245
_shelx_hkl_checksum              65345
_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 1.845
_oxdiff_exptl_absorpt_empirical_full_min 0.334