Alkynyltellurolato ligands including a solvatochromic rhenium(i) complex
Burt, Liam K.; Kirk, Ryan M.; Hill, Anthony F.; Chemical Communications 61 (2025) 6150–6153; doi:10.1039/D5CC00770D

data_7134337
_publ_section_title
;
 Alkynyltellurolato ligands including a solvatochromic rhenium(i) complex
;
_journal_issue                   33
_journal_name_full               'Chemical Communications'
_journal_page_first              6150
_journal_page_last               6153
_journal_paper_doi               10.1039/D5CC00770D
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C18 H17 N2 O3 Re Si Te'
_chemical_formula_sum            'C18 H17 N2 O3 Re Si Te'
_chemical_formula_weight         651.22
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-13
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-02-11 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                80.861(5)
_cell_angle_beta                 73.077(5)
_cell_angle_gamma                72.852(4)
_cell_formula_units_Z            1
_cell_length_a                   7.0960(3)
_cell_length_b                   7.1524(4)
_cell_length_c                   11.2227(7)
_cell_measurement_reflns_used    3526
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.1400
_cell_measurement_theta_min      4.0410
_cell_volume                     519.04(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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 (Sheldrick, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.869
_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    -14.00  80.00   1.00   40.00    --   12.89  77.00 -30.00   94
  2  \w     -4.00  80.00   1.00   40.00    --   12.89  57.00 120.00   84
  3  \w    -55.00  40.00   1.00   40.00    --   12.89 -77.00-150.00   95
  4  \w    -20.00  25.00   1.00   40.00    --  -13.91 -99.00 -30.00   45
  5  \w     34.00  85.00   1.00   40.00    --   12.89-178.00-180.00   51
  6  \w    -14.00  80.00   1.00   40.00    --   12.89  77.00-150.00   94
  7  \w    -55.00  40.00   1.00   40.00    --   12.89 -77.00  90.00   95
  8  \w    -20.00  52.00   1.00   40.00    --   12.89 -99.00 -60.00   72
  9  \w    -20.00  49.00   1.00   40.00    --   12.89 -99.00 150.00   69
 10  \w    -20.00  52.00   1.00   40.00    --   12.89 -99.00   0.00   72
;
_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      0.0816557000
_diffrn_orient_matrix_UB_12      -0.0840886000
_diffrn_orient_matrix_UB_13      0.0049230000
_diffrn_orient_matrix_UB_21      0.0201819000
_diffrn_orient_matrix_UB_22      -0.0109952000
_diffrn_orient_matrix_UB_23      -0.0645863000
_diffrn_orient_matrix_UB_31      0.0682207000
_diffrn_orient_matrix_UB_32      0.0603994000
_diffrn_orient_matrix_UB_33      -0.0140265000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7897
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.100
_diffrn_reflns_theta_min         3.657
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_description       plate
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.998
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.194
_refine_ls_abs_structure_details
;
 Flack x determined using 1699 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4099
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0069P)^2^+3.1520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.748
_reflns_number_gt                3993
_reflns_number_total             4099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00770d2.cif
_cod_data_source_block           liam2_scale
_cod_depositor_comments
'Adding full bibliography for 7134336--7134337.cif.'
_cod_database_code               7134337
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H17 N2 O3 Re1 Si1 Te1'
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.529
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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(O2) = Uanis(O3) = Uanis(O1)
Uanis(C7) = Uanis(C8) = Uanis(C6)
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              62567
_shelx_hkl_checksum              7688
_ins_header
;
TITL Liam2_scale in P1 
REM P1 (#1 in standard setting)
CELL 0.71073   7.096008   7.152444  11.222672  80.8612  73.0767  72.8523
ZERR    1.00   0.000346   0.000352   0.000725   0.0049   0.0051   0.0043
LATT -1
SFAC C H N O Si Te Re
UNIT 18.00 17.00 2.00 3.00 1.00 1.00 1.00
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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.918