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

data_7132797
_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         'C24 H27 B N8 O2 Te W'
_chemical_formula_sum            'C24 H27 B N8 O2 Te W'
_chemical_formula_weight         781.79
_chemical_name_common            'Thesis - Compound A.10 - CO47'
_chemical_name_systematic        CO47
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 99.742(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9095(2)
_cell_length_b                   18.2594(4)
_cell_length_c                   9.7522(3)
_cell_measurement_reflns_used    8512
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.5190
_cell_measurement_theta_min      4.8510
_cell_volume                     1388.13(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -105.00 -34.00   1.00    2.04    --  -37.04 -77.00  90.00   71
  2  \w    -27.00  81.00   1.00    2.04    --   37.04 -11.00 -85.00  108
  3  \w     80.00 105.00   1.00    2.04    --   37.04  77.00-120.00   25
  4  \w      1.00  28.00   1.00    2.04    --   37.04 -99.00-120.00   27
  5  \w    -30.00  54.00   1.00    2.04    --   37.04 -57.00-120.00   84
  6  \w     22.00  54.00   1.00    2.04    --   37.04 -57.00 -90.00   32
  7  \w    -20.00   5.00   1.00    2.04    --   37.04 -57.00 -90.00   25
  8  \w     -7.00  46.00   1.00    2.04    --   37.04 -57.00 120.00   53
  9  \w     34.00  89.00   1.00    2.04    --   37.04-125.00  60.00   55
 10  \w      2.00  54.00   1.00    2.04    --   37.04 -99.00 120.00   52
 11  \w     31.00  90.00   1.00    2.04    --   37.04-125.00-120.00   59
 12  \w     25.00  52.00   1.00    2.04    --   37.04  77.00-120.00   27
 13  \w     44.00 136.00   1.00    8.18    --  111.00 -25.00 -60.00   92
 14  \w     80.00 109.00   1.00    8.18    --  111.00-111.00 120.00   29
 15  \w     49.00  86.00   1.00    8.18    --  111.00-111.00 -60.00   37
 16  \w     43.00  68.00   1.00    8.18    --  111.00-111.00 120.00   25
 17  \w     55.00 105.00   1.00    8.18    --  111.00 -50.00  30.00   50
 18  \w     57.00  84.00   1.00    8.18    --  111.00 -25.00  60.00   27
 19  \w    136.00 177.00   1.00    8.18    --  111.00  64.00-120.00   41
 20  \w     51.00 111.00   1.00    8.18    --  111.00-111.00 -30.00   60
 21  \w    101.00 162.00   1.00    8.18    --  111.00 111.00 -30.00   61
 22  \w     42.00  68.00   1.00    8.18    --  111.00 -92.00  30.00   26
 23  \w     43.00  68.00   1.00    8.18    --  111.00 -92.00 150.00   25
 24  \w     76.00 102.00   1.00    8.18    --  111.00-111.00  90.00   26
 25  \w     92.00 128.00   1.00    8.18    --  111.00 -64.00  60.00   36
 26  \w     78.00 105.00   1.00    8.18    --  111.00-111.00-180.00   27
 27  \w    125.00 151.00   1.00    8.18    --  111.00  64.00-180.00   26
 28  \w    120.00 146.00   1.00    8.18    --  111.00  77.00  30.00   26
 29  \w     88.00 113.00   1.00    8.18    --  111.00-111.00  60.00   25
 30  \w     99.00 124.00   1.00    8.18    --  111.00  50.00 -60.00   25
 31  \w     47.00 130.00   1.00    8.18    --  111.00 -25.00 150.00   83
 32  \w     92.00 117.00   1.00    8.18    --  111.00  64.00-120.00   25
 33  \w     80.00 113.00   1.00    8.18    --  111.00-111.00 -90.00   33
 34  \w     89.00 128.00   1.00    8.18    --  111.00 -64.00 150.00   39
 35  \w    101.00 154.00   1.00    8.18    --  111.00  64.00 -30.00   53
 36  \w     71.00  97.00   1.00    8.18    --  111.00 -92.00 -30.00   26
 37  \w     83.00 113.00   1.00    8.18    --  111.00-111.00-150.00   30
 38  \w     41.00  68.00   1.00    8.18    --  111.00-111.00  60.00   27
 39  \w     64.00 107.00   1.00    8.18    --  111.00-111.00  30.00   43
 40  \w     47.00  98.00   1.00    8.18    --  111.00 -64.00  30.00   51
 41  \w     84.00 110.00   1.00    8.18    --  111.00 -50.00 150.00   26
 42  \w     88.00 136.00   1.00    8.18    --  111.00 -25.00   0.00   48
 43  \w     61.00  87.00   1.00    8.18    --  111.00 -12.00  90.00   26
 44  \w    118.00 144.00   1.00    8.18    --  111.00 -12.00  90.00   26
 45  \w     44.00  70.00   1.00    8.18    --  111.00 -92.00   0.00   26
 46  \w     66.00  91.00   1.00    8.18    --  111.00 -92.00  90.00   25
 47  \w    142.00 176.00   1.00    8.18    --  111.00  50.00 -60.00   34
 48  \w     58.00  94.00   1.00    8.18    --  111.00-111.00-120.00   36
 49  \w     51.00 114.00   1.00    8.18    --  111.00 -50.00-120.00   63
 50  \w     96.00 123.00   1.00    8.18    --  111.00  50.00 -30.00   27
 51  \w     97.00 131.00   1.00    8.18    --  111.00 -72.00 106.36   34
 52  \w     42.00  82.00   1.00    8.18    --  111.00 -38.00 120.00   40
 53  \w    103.00 128.00   1.00    8.18    --  111.00 178.00   0.00   25
 54  \w     93.00 128.00   1.00    8.18    --  111.00 -77.00 -90.00   35
 55  \w    102.00 127.00   1.00    8.18    --  111.00 -77.00 -60.00   25
 56  \w     45.00  74.00   1.00    8.18    --  111.00 -72.00 106.36   29
;
_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      0.0666128000
_diffrn_orient_matrix_UB_12      -0.0137078000
_diffrn_orient_matrix_UB_13      -0.1373887000
_diffrn_orient_matrix_UB_21      -0.1858420000
_diffrn_orient_matrix_UB_22      -0.0013055000
_diffrn_orient_matrix_UB_23      -0.0791256000
_diffrn_orient_matrix_UB_31      0.0080530000
_diffrn_orient_matrix_UB_32      0.0832437000
_diffrn_orient_matrix_UB_33      -0.0237237000
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14026
_diffrn_reflns_point_group_measured_fraction_full 0.723
_diffrn_reflns_point_group_measured_fraction_max 0.722
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         4.600
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (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    1.870
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.706
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.191
_refine_ls_abs_structure_details
;
 Flack x determined using 957 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.503(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3673
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0951P)^2^+4.5224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.398
_reflns_Friedel_fraction_full    0.427
_reflns_Friedel_fraction_max     0.426
_reflns_number_gt                3584
_reflns_number_total             3673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00303a2.cif
_cod_data_source_block           co47_co_wte_imidazole_scale
_cod_depositor_comments
'Adding full bibliography for 7132794--7132799.cif.'
_cod_database_code               7132797
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H27 B1 N8 O2 Te1 W1'
_chemical_oxdiff_usercomment     'DCM ethanol'
_shelx_estimated_absorpt_t_max   0.572
_shelx_estimated_absorpt_t_min   0.172
_reflns_odcompleteness_completeness 98.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C3)
Uanis(C23) = Uanis(C22)
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C13(H13), C8(H8), C23(H23), C22(H22)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C10(H10A,H10B,
 H10C), C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              44492
_shelx_hkl_checksum              38096
_ins_header
;
TITL CO_WTe_imidazole_scale in P2(1) 
REM P2(1) (#4 in standard setting)
CELL 1.54184   7.909495  18.259374   9.752195  90.0000  99.7417  90.0000
ZERR    2.00   0.000207   0.000385   0.000264   0.0000   0.0025   0.0000
LATT -1
SYMM -x, y+1/2,-z 
SFAC C H B N O Te W
UNIT 48.00 54.00 2.00 16.00 4.00 2.00 2.00
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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.577
_oxdiff_exptl_absorpt_empirical_full_min 0.715