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

data_7132794
_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         'C29 H43 B N6 O2 Si Te W'
_chemical_formula_sum            'C29 H43 B N6 O2 Si Te W'
_chemical_formula_weight         858.04
_chemical_name_common            'Thesis - Compound A.4 - CO32'
_chemical_name_systematic        CO32
_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             2020-01-07
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-21 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                84.687(4)
_cell_angle_beta                 87.521(4)
_cell_angle_gamma                75.938(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6281(5)
_cell_length_b                   11.0432(6)
_cell_length_c                   15.1354(7)
_cell_measurement_reflns_used    3943
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.0230
_cell_measurement_theta_min      4.8050
_cell_volume                     1715.38(15)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -29.00  12.00   1.00    3.85    --   35.53 -57.00  30.00   41
  2  \w    -30.00  52.00   1.00    3.85    --   35.53 -57.00 -60.00   82
  3  \w     23.00  81.00   1.00    3.85    --   35.53-125.00  60.00   58
  4  \w     15.00  52.00   1.00    3.85    --   35.53 -57.00  30.00   37
  5  \w     18.00 104.00   1.00    3.85    --   35.53  38.00-150.00   86
  6  \w    -36.00  58.00   1.00    3.85    --   35.53 -19.00  30.00   94
  7  \w     32.00  87.00   1.00    3.85    --   35.53-125.00-180.00   55
  8  \w      2.00  73.00   1.00    3.85    --   35.53 -99.00 -90.00   71
  9  \w     81.00 125.00   1.00   15.40    --  108.91 -45.00  90.00   44
 10  \w     41.00  74.00   1.00   15.40    --  108.91 -45.00-180.00   33
 11  \w     45.00 133.00   1.00   15.40    --  108.91 -77.00 -30.00   88
 12  \w     87.00 121.00   1.00   15.40    --  108.91 -45.00-180.00   34
 13  \w     83.00 139.00   1.00   15.40    --  108.91  77.00  30.00   56
 14  \w    100.00 153.00   1.00   15.40    --  108.91 111.00-150.00   53
 15  \w     42.00 113.00   1.00   15.40    --  108.91-111.00 -30.00   71
 16  \w     64.00 113.00   1.00   15.40    --  108.91-111.00 120.00   49
 17  \w     40.00 107.00   1.00   15.40    --  108.91 -45.00  60.00   67
 18  \w     93.00 151.00   1.00   15.40    --  108.91  45.00 -90.00   58
 19  \w     40.00 121.00   1.00   15.40    --  108.91 -45.00 -90.00   81
 20  \w     45.00 132.00   1.00   15.40    --  108.91 -77.00 150.00   87
 21  \w     55.00 169.00   1.00   15.40    --  108.91   0.00-150.00  114
;
_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      0.0214549000
_diffrn_orient_matrix_UB_12      0.1019472000
_diffrn_orient_matrix_UB_13      -0.0716691000
_diffrn_orient_matrix_UB_21      -0.0931253000
_diffrn_orient_matrix_UB_22      -0.0379333000
_diffrn_orient_matrix_UB_23      -0.0614494000
_diffrn_orient_matrix_UB_31      -0.1149219000
_diffrn_orient_matrix_UB_32      0.0948655000
_diffrn_orient_matrix_UB_33      0.0392714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10111
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         4.142
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69076
_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    1.661
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.056
_refine_diff_density_max         2.410
_refine_diff_density_min         -1.601
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0819P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4666
_reflns_number_total             6019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00303a2.cif
_cod_data_source_block           co32a_co_wtetips_scale
_cod_depositor_comments
'Adding full bibliography for 7132794--7132799.cif.'
_cod_database_code               7132794
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H31 Au1 B1 Cl1 N6 O2 W1'
_chemical_oxdiff_usercomment     'chloroform ethanol or hexane'
_reflns_odcompleteness_completeness 99.36
_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. Uiso/Uaniso restraints and constraints
Uanis(C25) = Uanis(C26)
Uanis(C29) = Uanis(C28)
Uanis(C22) = Uanis(C23)
3.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C27(H27)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C18(H18), C8(H8)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C11(H11A,H11B,
 H11C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C29(H29A,H29B,H29C), C25(H25A,
 H25B,H25C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C),
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              5581
_shelx_hkl_checksum              13838
_ins_header
;
TITL CO_WTeTIPS_scale in P1 
REM P1 (#1 in standard setting)
CELL 1.54184  10.628083  11.043199  15.135361  84.6872  87.5214  75.9377
ZERR    2.00   0.000548   0.000566   0.000735   0.0041   0.0041   0.0045
LATT -1
SFAC C H B N O Cl W Au
UNIT 48.00 62.00 2.00 12.00 4.00 2.00 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 1.744
_oxdiff_exptl_absorpt_empirical_full_min 0.732