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_7062239
_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         'C33 H33 Cl N Ru Te, F6 P, C2 H3 N'
_chemical_formula_sum            'C35 H36 Cl F6 N2 P Ru Te'
_chemical_formula_weight         893.774
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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                110.209(5)
_cell_angle_beta                 92.595(4)
_cell_angle_gamma                101.402(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9686(5)
_cell_length_b                   11.5281(6)
_cell_length_c                   15.8156(9)
_cell_measurement_reflns_used    4128
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5030
_cell_measurement_theta_min      2.2010
_cell_volume                     1825.61(18)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9809
_diffrn_measured_fraction_theta_max 0.8508
_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    -52.00  66.00   1.00   17.93    --   26.84 -77.00 -90.00  118
  2  \w    -53.00  66.00   1.00   17.93    --   26.84 -77.00  30.00  119
  3  \w    -52.00  66.00   1.00   17.93    --   26.84 -77.00 150.00  118
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.9809
_diffrn_reflns_Laue_measured_fraction_max 0.8508
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10206
_diffrn_reflns_point_group_measured_fraction_full 0.9809
_diffrn_reflns_point_group_measured_fraction_max 0.8508
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86482
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             881.756
_refine_diff_density_max         1.6586
_refine_diff_density_min         -0.5959
_refine_diff_density_rms         0.1285
_refine_ls_d_res_high            0.7486
_refine_ls_d_res_low             10.5346
_refine_ls_goodness_of_fit_ref   1.0771
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7763
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.0475
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+1.5717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6033
_reflns_number_total             7763
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj04408k2.cif
_cod_data_source_block           Ru_Te_Rt_Mo
_cod_depositor_comments
'Adding full bibliography for 7062238--7062239.cif.'
_cod_database_code               7062239
_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. Rigid bond restraints
 P1, F1, F2, F3, F4, F5, F6, F2A, F1A, F5A, F3A, F6A, F4A
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
 N2, C34, C35, C34A, C35A
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
3. Uiso/Uaniso restraints and constraints
P1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F2A \\sim F1A
\\sim F5A \\sim F3A \\sim F6A \\sim F4A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
N2 \\sim C34 \\sim C35 \\sim C34A \\sim C35A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{P1, F1, F2, F3, F4, F5, F6, F2A, F1A, F5A, F3A, F6A, F4A} sigma for 1-2: 0.01,
1-3: 0.02
as in
{P1, F1, F2, F3, F4, F5, F6, F2A, F1A, F5A, F3A, F6A, F4A}
{N2, C34, C35, C34A, C35A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{N2, C34, C35, C34A, C35A}
5. Others
 Sof(F2A)=Sof(F1A)=Sof(F5A)=Sof(F3A)=Sof(F6A)=Sof(F4A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(C34A)=Sof(C35A)=Sof(H35d)=Sof(H35e)=Sof(H35f)=1-FVAR(2)
 Sof(C34)=Sof(C35)=Sof(H35a)=Sof(H35b)=Sof(H35c)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C8(H8a,H8b)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C25(H25), C26(H26),
 C28(H28), C29(H29), C21(H21), C22(H22), C9(H9), C14(H14), C15(H15), C17(H17),
 C19(H19), C20(H20), C2(H2)
6.d Idealised Me refined with fixed occupancy and ADP/Uiso:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c)
6.e Idealised Me refined as rotating group:
 C30(H30a,H30b,H30c), C35(H35a,H35b,H35c), C35A(H35d,H35e,H35f)
;
_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
;