Carbon-chalcogen wires: alkynyltellurolatocarbynes.
Onn, Chee S.; Hill, Anthony F.; Chemical communications (Cambridge, England) 60 (2024) 3555–3558; doi:10.1039/d4cc00303a

data_7132795
_publ_section_title
;
 Carbon-chalcogen wires: alkynyltellurolatocarbynes.
;
_journal_issue                   26
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3555
_journal_page_last               3558
_journal_paper_doi               10.1039/d4cc00303a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C20 H28 Au B Cl4 N6 O2 S Te W, C H2 Cl2'
_chemical_formula_sum            'C21 H30 Au B Cl6 N6 O2 S Te W'
_chemical_formula_weight         1162.49
_chemical_name_common            'Thesis - Compound A.14 - CO19a'
_chemical_name_systematic        CO19a
_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   mixed
_audit_creation_date             2020-09-02
_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.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                89.093(4)
_cell_angle_beta                 89.186(3)
_cell_angle_gamma                77.275(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1523(4)
_cell_length_b                   11.1610(5)
_cell_length_c                   14.3505(6)
_cell_measurement_reflns_used    3688
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      70.7210
_cell_measurement_theta_min      4.0550
_cell_volume                     1742.02(13)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.959
_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    -54.00  27.00   1.00    5.50    --  -35.78  38.00-180.00   81
  2  \w    -85.00  29.00   1.00    5.50    --  -35.78   0.00 150.00  114
  3  \w    -55.00  26.00   1.00    5.50    --  -35.78  38.00  30.00   81
  4  \w     27.00  89.00   1.00    5.50    --   35.78-125.00 -90.00   62
  5  \w     27.00  87.00   1.00    5.50    --   35.78-125.00  90.00   60
  6  \w     44.00 106.00   1.00   35.00    --  105.15 -95.00 150.00   62
  7  \w     35.00 123.00   1.00   35.00    --  105.15 -30.00-180.00   88
  8  \w     35.00 125.00   1.00   35.00    --  105.15 -30.00  90.00   90
  9  \w     90.00 172.00   1.00   35.00    --  105.15  61.00 120.00   82
 10  \w     72.00 106.00   1.00   35.00    --  105.15 -95.00  60.00   34
 11  \w     76.00 109.00   1.00   35.00    --  105.15-111.00 -90.00   33
 12  \w     36.00 106.00   1.00   35.00    --  105.15 -95.00 -30.00   70
 13  \w    111.00 165.00   1.00   35.00    --  105.15  77.00 150.00   54
 14  \w     38.00 120.00   1.00   35.00    --  105.15 -61.00-180.00   82
 15  \w     39.00 122.00   1.00   35.00    --  105.15 -61.00   0.00   83
 16  \w     34.00 127.00   1.00   35.00    --  105.15 -15.00 -30.00   93
;
_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      -0.0544266000
_diffrn_orient_matrix_UB_12      0.1334094000
_diffrn_orient_matrix_UB_13      -0.0311096000
_diffrn_orient_matrix_UB_21      -0.0271312000
_diffrn_orient_matrix_UB_22      -0.0454926000
_diffrn_orient_matrix_UB_23      -0.0966091000
_diffrn_orient_matrix_UB_31      -0.1279055000
_diffrn_orient_matrix_UB_32      -0.0126335000
_diffrn_orient_matrix_UB_33      0.0350368000
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9740
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.039
_diffrn_reflns_theta_min         4.061
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53948
_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 light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_description       plate
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.043
_refine_diff_density_max         5.186
_refine_diff_density_min         -2.355
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6466
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0802P)^2^+23.9392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4649
_reflns_number_total             6466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00303a2.cif
_cod_data_source_block           co19_wtetms_aucl-forcehemisphere_scale
_cod_depositor_comments
'Adding full bibliography for 7132794--7132799.cif.'
_cod_database_code               7132795
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H30 B1 N6 S1 Te1 Cl6'
_chemical_oxdiff_usercomment     'D/H crude dirty'
_reflns_odcompleteness_completeness 99.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Restrained distances
 B1-H1
 1.15 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C3)
Uanis(Cl3) = Uanis(Cl4) = Uanis(Cl1) = Uanis(Cl2)
4.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C6(H6), C16(H16)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C),
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              99699
_shelx_hkl_checksum              89439
_ins_header
;
TITL CO_WTeTMS_AuCl-force hemisphere_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  11.152260  11.161028  14.350530  89.0934  89.1856  77.2752
ZERR    5.00   0.000396   0.000501   0.000635   0.0036   0.0033   0.0034
LATT  1
SFAC C H B N S Cl Te
UNIT 105.00 150.00 5.00 30.00 5.00 30.00 5.00
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 1.674
_oxdiff_exptl_absorpt_empirical_full_min 0.585