Metal-metalloid bond containing complexes of the bulky organotellurium ligand: applications in catalysis of C–O coupling and aldehyde to amide transformation reactions
Oswal, Preeti; Arora, Aayushi; Purohit, Suraj; Bahuguna, Anurag; Sharma, Pankaj; Roy, Jiben; Kumar, Arun; New Journal of Chemistry 47 (2023) 4346–4354; doi:10.1039/D2NJ04408K

data_7062238
_publ_section_title
;
 Metal-metalloid bond containing complexes of the bulky organotellurium
 ligand: applications in catalysis of C--O coupling and aldehyde to amide
 transformation reactions
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4346
_journal_page_last               4354
_journal_paper_doi               10.1039/D2NJ04408K
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C23 H19 Cl2.356 N O Pd Te'
_chemical_formula_sum            'C23 H19 Cl2.34 N O Pd Te'
_chemical_formula_weight         642.43
_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   geom
_audit_creation_date             2022-12-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-03 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.843(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5904(8)
_cell_length_b                   12.0469(6)
_cell_length_c                   15.6608(9)
_cell_measurement_reflns_used    2230
_cell_measurement_temperature    150.0(4)
_cell_measurement_theta_max      27.1630
_cell_measurement_theta_min      2.4880
_cell_volume                     2092.9(2)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0(4)
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.884
_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     39.00  93.00   1.00   15.00    --   26.84 178.00-180.00   54
  2  \w     -9.00 102.00   1.00   15.00    --   26.84  57.00   0.00  111
  3  \w     48.00 116.00   1.00   15.00    --   26.84 178.00 -60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7189
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.155
_diffrn_reflns_theta_min         1.942
_exptl_absorpt_coefficient_mu    2.568
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.831
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.039
_exptl_crystal_description       needle
_exptl_crystal_F_000             1239
_exptl_crystal_recrystallization_method
'Crystals were grown by slow evaporation of solvents from the solution of compound in acetonitrile and ether at room temperature'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.620
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4530
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0556P)^2^+7.3632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3350
_reflns_number_total             4530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04408k2.cif
_cod_data_source_block           atepd_lt_mo
_cod_depositor_comments
'Adding full bibliography for 7062238--7062239.cif.'
_cod_database_code               7062238
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1-Cl2_$1
 2.3 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
;
_shelx_res_checksum              11848
_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
;