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

data_7132799
_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         'C26 H27 B N6 O2 Te W'
_chemical_formula_sum            'C26 H27 B N6 O2 Te W'
_chemical_formula_weight         777.79
_chemical_name_common            'Thesis - Compound A.8 - CO5'
_chemical_name_systematic        CO5
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 117.804(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.5319(5)
_cell_length_b                   14.2779(2)
_cell_length_c                   21.6073(4)
_cell_measurement_reflns_used    39264
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.5650
_cell_measurement_theta_min      3.9270
_cell_volume                     5602.9(2)
_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      150.01(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 0.990
_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      8.00 108.00   1.00    6.50    --   37.06  19.00-120.00  100
  2  \w    -30.00  64.00   1.00    6.50    --   37.06 -77.00 -60.00   94
  3  \w      1.00  76.00   1.00    6.50    --   37.06 -99.00  60.00   75
  4  \w    -30.00  54.00   1.00    6.50    --   37.06 -57.00   0.00   84
  5  \w     23.00  90.00   1.00    6.50    --   37.06-125.00-180.00   67
  6  \w     23.00  90.00   1.00    6.50    --   37.06-125.00 -90.00   67
  7  \w      8.00 108.00   1.00    6.50    --   37.06  19.00 150.00  100
  8  \w     41.00 132.00   1.00   10.00    --  111.00 -30.00  90.00   91
  9  \w     41.00 113.00   1.00   10.00    --  111.00-111.00   0.00   72
 10  \w     93.00 178.00   1.00   10.00    --  111.00  61.00 150.00   85
 11  \w     43.00 128.00   1.00   10.00    --  111.00 -45.00   0.00   85
 12  \w     42.00 110.00   1.00   10.00    --  111.00 -95.00  30.00   68
 13  \w     41.00 113.00   1.00   10.00    --  111.00-111.00-180.00   72
 14  \w     94.00 178.00   1.00   10.00    --  111.00  45.00 -90.00   84
 15  \w     40.00 149.00   1.00   10.00    --  111.00 -15.00 -60.00  109
 16  \w     41.00 132.00   1.00   10.00    --  111.00 -30.00-150.00   91
 17  \w     93.00 178.00   1.00   10.00    --  111.00  61.00  30.00   85
 18  \w     42.00 110.00   1.00   10.00    --  111.00 -95.00  90.00   68
 19  \w     43.00 138.00   1.00   10.00    --  111.00 -77.00-180.00   95
 20  \w     20.00 104.00   1.00    6.50    --   37.06  57.00 -90.00   84
 21  \w     10.00 105.00   1.00    6.50    --   37.06  77.00  60.00   95
 22  \w     20.00 104.00   1.00    6.50    --   37.06  57.00   0.00   84
 23  \w    -32.00  56.00   1.00    6.50    --   37.06 -38.00  60.00   88
 24  \w     10.00 105.00   1.00    6.50    --   37.06  77.00-180.00   95
 25  \w    -34.00  66.00   1.00    6.50    --   37.06 -19.00 120.00  100
 26  \w     73.00 178.00   1.00   10.00    --  111.00  15.00 120.00  105
 27  \w     73.00 178.00   1.00   10.00    --  111.00  15.00-120.00  105
 28  \w     73.00 178.00   1.00   10.00    --  111.00  15.00   0.00  105
;
_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      0.0008555000
_diffrn_orient_matrix_UB_12      0.0067734000
_diffrn_orient_matrix_UB_13      -0.0707584000
_diffrn_orient_matrix_UB_21      0.0600902000
_diffrn_orient_matrix_UB_22      0.0758813000
_diffrn_orient_matrix_UB_23      0.0304462000
_diffrn_orient_matrix_UB_31      0.0598591000
_diffrn_orient_matrix_UB_32      -0.0764143000
_diffrn_orient_matrix_UB_33      0.0237502000
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60406
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.875
_diffrn_reflns_theta_min         3.864
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16582
_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    1.844
_exptl_crystal_description       plate
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.078
_refine_diff_density_max         2.632
_refine_diff_density_min         -2.118
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         11248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0720P)^2^+47.7809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10540
_reflns_number_total             11248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00303a2.cif
_cod_data_source_block           co5_co_wteph_scale
_cod_depositor_comments
'Adding full bibliography for 7132794--7132799.cif.'
_cod_database_code               7132799
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C26 H27 B1 N6 O2 Te1 W1'
_chemical_oxdiff_usercomment     'DCM hexane, orange'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Others
 Fixed Sof: Te1(0.75) Te0A(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C8(H8), C13(H13), C8A(H8A), C18A(H18A), C13A(H13A), C26(H26),
 C26A(H26A), C25(H25), C22(H22), C25A(H25A), C24(H24), C22A(H22A), C23(H23),
 C23A(H23A), C24A(H24A)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15A(H15D,H15E,H15F), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C20(H20A,H20B,H20C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), C20A(H20D,
 H20E,H20F), C16A(H16D,H16E,H16F), C11A(H11D,H11E,H11F), C6A(H6AA,H6AB,H6AC),
 C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              67399
_shelx_hkl_checksum              57679
_ins_header
;
TITL CO_WTePh_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  20.531887  14.277892  21.607287  90.0000 117.8040  90.0000
ZERR   16.00   0.000459   0.000218   0.000443   0.0000   0.0028   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O Te W
UNIT 416.00 432.00 16.00 96.00 32.00 16.00 16.00
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 3.913
_oxdiff_exptl_absorpt_empirical_full_min 0.631