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

data_7132796
_publ_section_title
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 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         'C58 H86 B2 Cl4 Cu4 N12 O4 Si2 Te2 W2, C6 H14'
_chemical_formula_sum            'C64 H100 B2 Cl4 Cu4 N12 O4 Si2 Te2 W2'
_chemical_formula_weight         2198.21
_chemical_name_common            'Thesis - Compound A.15 - CO194'
_chemical_name_systematic        CO194
_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             2020-02-02
_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                90
_cell_angle_beta                 102.630(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9539(2)
_cell_length_b                   18.7716(4)
_cell_length_c                   20.4333(4)
_cell_measurement_reflns_used    5265
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      70.8320
_cell_measurement_theta_min      4.7470
_cell_volume                     4099.87(14)
_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 (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      150.01(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    -24.00  32.00   1.00    1.00    --  -36.03  77.00 -30.00   56
  2  \w    -31.00  65.00   1.00    1.00    --   36.03 -19.00-150.00   96
  3  \w     35.00  89.00   1.00    1.00    --   36.03-125.00 -30.00   54
  4  \w      8.00  49.00   1.00    1.00    --   36.03 -57.00   0.00   41
  5  \w    104.00 175.00   1.00   15.00    --  105.15 111.00-180.00   71
  6  \w     43.00 109.00   1.00   15.00    --  105.15-111.00 120.00   66
  7  \w     36.00 106.00   1.00   15.00    --  105.15 -95.00 -90.00   70
  8  \w     35.00 127.00   1.00   15.00    --  105.15 -30.00-180.00   92
  9  \w     84.00 175.00   1.00   15.00    --  105.15  30.00-180.00   91
 10  \w     55.00 123.00   1.00   15.00    --  105.15 -45.00-120.00   68
;
_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      0.0644192000
_diffrn_orient_matrix_UB_12      -0.0708920000
_diffrn_orient_matrix_UB_13      -0.0100818000
_diffrn_orient_matrix_UB_21      0.0931595000
_diffrn_orient_matrix_UB_22      0.0402860000
_diffrn_orient_matrix_UB_23      -0.0330669000
_diffrn_orient_matrix_UB_31      0.0891257000
_diffrn_orient_matrix_UB_32      0.0090130000
_diffrn_orient_matrix_UB_33      0.0691275000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13081
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         4.244
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.541
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90222
_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    1.781
_exptl_crystal_description       plate
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.061
_refine_diff_density_max         2.005
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0457P)^2^+3.9490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5956
_reflns_number_total             7171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00303a2.cif
_cod_data_source_block           co194_tetips_cucl_scale
_cod_depositor_comments
'Adding full bibliography for 7132794--7132799.cif.'
_cod_database_code               7132796
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H43 B1 N6 O2 Te1 Si1 W1 Cu2 Cl2'
_chemical_oxdiff_usercomment     'D/E slow evap 0.84'
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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.a Ternary CH refined with riding coordinates:
 C12(H12), C6(H6), C9(H9)
3.b Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C2A(H2AA,H2AB)
3.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C27(H27), C22(H22)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C19(H19A,H19B,
 H19C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C), C14(H14A,H14B,H14C), C24(H24A,
 H24B,H24C), C8(H8A,H8B,H8C), C1A(H1AA,H1AB,H1AC), C11(H11A,H11B,H11C),
 C10(H10A,H10B,H10C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              9523
_shelx_hkl_checksum              46622
_ins_header
;
TITL CO_TeTIPS_CuCl_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.953928  18.771622  20.433281  90.0000 102.6295  90.0000
ZERR    4.00   0.000238   0.000356   0.000420   0.0000   0.0022   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O Si Cl Cu Te W
UNIT 116.00 172.00 4.00 24.00 8.00 4.00 8.00 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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.792