Spodium bonding in bis(alkynyl)mecurials.
Onn, Chee S.; Hill, Anthony F.; Ward, Jas S.; Chemical communications (Cambridge, England) 60 (2024) 2552–2555; doi:10.1039/d3cc06027f

data_7132793
_publ_section_title
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 Spodium bonding in bis(alkynyl)mecurials.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2552
_journal_page_last               2555
_journal_paper_doi               10.1039/d3cc06027f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C20 H23 B N6 O2 Se W'
_chemical_formula_sum            'C20 H23 B N6 O2 Se W'
_chemical_formula_weight         653.06
_chemical_name_common            'Thesis - Compound 2.8 - CO12 xrd'
_chemical_name_systematic        CO12
_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   mixed
_audit_creation_date             2020-08-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-21 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.415(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9715(3)
_cell_length_b                   18.2689(6)
_cell_length_c                   19.7379(8)
_cell_measurement_reflns_used    4240
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.6830
_cell_measurement_theta_min      4.5710
_cell_volume                     2817.58(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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   17.50    --  -36.03  19.00 -90.00   93
  2  \w    -52.00  31.00   1.00   17.50    --  -36.03  57.00 -30.00   83
  3  \w    -84.00  -9.00   1.00   17.50    --  -36.03 125.00 -30.00   75
  4  \w     90.00 173.00   1.00   64.00    --  105.15  45.00 -90.00   83
  5  \w    103.00 154.00   1.00   64.00    --  105.15  77.00 -60.00   51
  6  \w     51.00 123.00   1.00   64.00    --  105.15 -61.00 -60.00   72
  7  \w    106.00 173.00   1.00   64.00    --  105.15  77.00-150.00   67
  8  \w     50.00 123.00   1.00   64.00    --  105.15 -45.00 120.00   73
  9  \w     35.00 106.00   1.00   64.00    --  105.15-111.00-180.00   71
;
_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      0.1885915000
_diffrn_orient_matrix_UB_12      0.0245712000
_diffrn_orient_matrix_UB_13      0.0125895000
_diffrn_orient_matrix_UB_21      -0.0308009000
_diffrn_orient_matrix_UB_22      0.0353671000
_diffrn_orient_matrix_UB_23      -0.0722242000
_diffrn_orient_matrix_UB_31      -0.0487699000
_diffrn_orient_matrix_UB_32      0.0724886000
_diffrn_orient_matrix_UB_33      0.0309888000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8595
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         4.571
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale orange'
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.190
_refine_diff_density_min         -2.346
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4934
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0981
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+123.2290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4260
_reflns_number_total             4934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06027f2.cif
_cod_data_source_block           co12_co_wseh_scale
_cod_database_code               7132793
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H23 B1 N6 O2 Se1 W1'
_chemical_oxdiff_usercomment     'D/H vap diff'
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Restrained distances
 B1-H6
 1.15 with sigma of 0.02
3. Rigid bond restraints
 C4, C5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C19, C18, C17
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C4 \\sim C5: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C19 \\sim C18 \\sim C17: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C18(H18)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C10(H10A,H10B,
 H10C), C15(H15A,H15B,H15C), C20(H20A,H20B,H20C)
5.c :
 C5(H5)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 198 electrons were 
found in a volume of 626 Ang^3^ in 1 void per unit cell. 
This is consistent with the presence of 1[C6H14] per 
Asymmetric Unit which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37044
_shelx_hkl_checksum              83822
_shelx_fab_checksum              35210
_ins_header
;
TITL CO_WSeH_scale in P2(1) 
REM P2(1) (#4 in standard setting)
CELL 1.54184   7.971494  18.268932  19.737925  90.0000 101.4153  90.0000
ZERR    4.00   0.000256   0.000608   0.000770   0.0000   0.0034   0.0000
LATT -1
SYMM -x, y+1/2,-z 
SFAC C H B N O Se W
UNIT 80.00 92.00 4.00 24.00 8.00 4.00 4.00
TREF
HKLF 4
END
;
_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 1.382
_oxdiff_exptl_absorpt_empirical_full_min 0.768