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_7134004
_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         'C48 H50 B2 S3'
_chemical_formula_sum            'C48 H50 B2 S3'
_chemical_formula_weight         744.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 95.1670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6674(2)
_cell_length_b                   20.0273(4)
_cell_length_c                   16.7069(3)
_cell_measurement_reflns_used    12041
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.4770
_cell_measurement_theta_min      3.4300
_cell_volume                     4221.21(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -95.00 -44.00   1.00    0.45    --  -48.45-166.00 -37.00   51
  2  \w    -86.00  -3.00   1.00    0.45    --  -48.45 116.00-161.00   83
  3  \w     34.00  59.00   1.00    0.45    --   48.45-116.00 109.00   25
  4  \w     63.00  88.00   1.00    0.45    --   48.45-166.00 -37.00   25
  5  \w   -142.00-117.00   1.00    2.00    --  -86.25-116.00 109.00   25
  6  \w    -74.00 -49.00   1.00    2.00    --  -86.25 116.00-161.00   25
  7  \w   -118.00 -93.00   1.00    2.00    --  -86.25-166.00 -37.00   25
  8  \w    -87.00 -31.00   1.00    2.00    --  -86.25 166.00 -15.00   56
  9  \w     95.00 120.00   1.00    2.00    --  100.87-166.00 -37.00   25
 10  \w     67.00 158.00   1.00    2.00    --  100.87 166.00 -15.00   91
 11  \w     31.00 112.00   1.00    2.00    --  100.87-116.00 109.00   81
 12  \w   -120.00 -70.00   1.00    0.45    --  -48.45-125.00 -30.00   50
 13  \w   -117.00 -70.00   1.00    0.45    --  -48.45-125.00 150.00   47
 14  \w   -159.00 -84.00   1.00    2.00    --  -86.25 -99.00 150.00   75
 15  \w     32.00 108.00   1.00    2.00    --  100.87 -57.00 120.00   76
 16  \w    101.00 171.00   1.00    2.00    --  100.87  57.00 -90.00   70
 17  \w     89.00 170.00   1.00    2.00    --  100.87  19.00 150.00   81
 18  \w     32.00 107.00   1.00    2.00    --  100.87 -99.00 -30.00   75
;
_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      0.0533419000
_diffrn_orient_matrix_UB_12      0.0681418000
_diffrn_orient_matrix_UB_13      0.0183069000
_diffrn_orient_matrix_UB_21      0.1098003000
_diffrn_orient_matrix_UB_22      -0.0335578000
_diffrn_orient_matrix_UB_23      0.0042834000
_diffrn_orient_matrix_UB_31      0.0046572000
_diffrn_orient_matrix_UB_32      0.0122181000
_diffrn_orient_matrix_UB_33      -0.0906135000
_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  0.0680
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29111
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1484P)^2^+0.9805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5942
_reflns_number_total             7446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05240d2.cif
_cod_data_source_block           klb-31
_cod_depositor_comments
'Adding full bibliography for 7134004--7134007.cif.'
_cod_database_code               7134004
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SCNB
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.609
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     65.72
_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.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C42(H42), C35(H35), C9(H9), C44(H44), C27(H27),
 C33(H33), C11(H11), C18(H18), C20(H20), C29(H29), C28(H28)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C37(H37A,H37B,H37C), C23(H23A,H23B,H23C), C22(H22A,H22B,
 H22C), C38(H38A,H38B,H38C), C48(H48A,H48B,H48C), C13(H13A,H13B,H13C), C47(H47A,
 H47B,H47C), C15(H15A,H15B,H15C), C46(H46A,H46B,H46C), C39(H39A,H39B,H39C),
 C24(H24A,H24B,H24C)
;
_shelx_res_checksum              1629
_shelx_hkl_checksum              81582
_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 2.681
_oxdiff_exptl_absorpt_empirical_full_min 0.245