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_7134005
_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 Se3'
_chemical_formula_sum            'C48 H50 B2 Se3'
_chemical_formula_weight         885.38
_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                 95.4230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.83960(10)
_cell_length_b                   19.9939(2)
_cell_length_c                   16.8684(2)
_cell_measurement_reflns_used    16228
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.1970
_cell_measurement_theta_min      3.4010
_cell_volume                     4310.97(8)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    -70.00  21.00   1.00    0.10    --  -48.45  75.00 -32.00   91
  2  \w   -104.00 -26.00   1.00    0.10    --  -48.45 -75.00-159.00   78
  3  \w     50.00  75.00   1.00    0.10    --   48.45  75.00 -32.00   25
  4  \w      3.00  44.00   1.00    0.10    --   48.45 -75.00-159.00   41
  5  \w   -130.00 -67.00   1.00    0.40    --  -86.25 -75.00-159.00   63
  6  \w    -62.00 -14.00   1.00    0.40    --  -86.25  75.00 -32.00   48
  7  \w     55.00 128.00   1.00    0.40    --  106.49 -75.00-159.00   73
  8  \w     85.00 149.00   1.00    0.40    --  106.49  75.00 -32.00   64
  9  \w   -159.00 -83.00   1.00    0.40    --  -86.25 -99.00 -60.00   76
 10  \w     40.00 109.00   1.00    0.40    --  106.49 -99.00 120.00   69
 11  \w     34.00 117.00   1.00    0.40    --  106.49-125.00  90.00   83
 12  \w     35.00 107.00   1.00    0.40    --  106.49 -99.00-150.00   72
 13  \w     92.00 178.00   1.00    0.40    --  106.49 125.00 150.00   86
;
_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      0.0503196000
_diffrn_orient_matrix_UB_12      0.0065241000
_diffrn_orient_matrix_UB_13      0.0862560000
_diffrn_orient_matrix_UB_21      0.0580880000
_diffrn_orient_matrix_UB_22      0.0635366000
_diffrn_orient_matrix_UB_23      -0.0233290000
_diffrn_orient_matrix_UB_31      -0.0926770000
_diffrn_orient_matrix_UB_32      0.0431305000
_diffrn_orient_matrix_UB_33      0.0210734000
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25645
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56029
_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    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0194P)^2^+10.6202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6443
_reflns_number_total             7597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05240d2.cif
_cod_data_source_block           klb-32
_cod_depositor_comments
'Adding full bibliography for 7134004--7134007.cif.'
_cod_database_code               7134005
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SeCB
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.435
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C42(H42), C9(H9), C5(H5), C44(H44), C35(H35), C3(H3), C4(H4), C33(H33),
 C18(H18), C29(H29), C11(H11), C20(H20), C27(H27), C28(H28)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C48(H48A,H48B,
 H48C), C46(H46A,H46B,H46C), C37(H37A,H37B,H37C), C23(H23A,H23B,H23C), C47(H47A,
 H47B,H47C), C39(H39A,H39B,H39C), C24(H24A,H24B,H24C), C38(H38A,H38B,H38C),
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              9657
_shelx_hkl_checksum              57276
_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 1.702
_oxdiff_exptl_absorpt_empirical_full_min 0.570