Nickel-Catalyzed Dehydrogenative Zn–Zn Coupling to a Zn(I) Dimer and Its Reactivity
Rajput, Sagrika; PADHAN, SMRUTIRANI; M T, Nithya; Mukhopadhyay, Sayantan; Nembenna, Sharanappa; Chemical Communications  (2025) –; doi:10.1039/D5CC06233K

data_7135247
_publ_section_title
;
 Nickel-Catalyzed Dehydrogenative Zn--Zn Coupling to a Zn(I) Dimer and Its
 Reactivity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC06233K
_journal_year                    2025
_chemical_formula_moiety         'C56 H75 N5 Te Zn, 2(C6 H6)'
_chemical_formula_sum            'C68 H87 N5 Te Zn'
_chemical_formula_weight         1167.39
_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   geom
_audit_creation_date             2025-11-21
_audit_creation_method
;
Olex2 1.5-ac5-021
(compiled 2022.02.15 svn.rf212a0ae for Rigaku Oxford Diffraction, GUI svn.r6439)
;
_audit_update_record
;
2025-11-21 deposited with the CCDC.	2025-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                91.490(2)
_cell_angle_beta                 90.601(2)
_cell_angle_gamma                111.293(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3684(3)
_cell_length_b                   12.4059(3)
_cell_length_c                   21.7277(4)
_cell_measurement_reflns_used    48455
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      36.6800
_cell_measurement_theta_min      3.4260
_cell_volume                     3104.57(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-021 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-021 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     17.00  65.00   0.50    3.30    --   -0.82-148.00 -61.00   96
  2  \w    -12.00  62.00   0.50    3.30    --   -0.82  57.00   0.00  148
  3  \w    -70.00   5.00   0.50    3.30    --   -0.82 -19.00  60.00  150
  4  \w    -67.00   3.00   0.50    3.30    --   -0.82 -38.00   0.00  140
  5  \w      8.00  51.00   0.50    3.30    --   -0.82-127.00 161.74   86
  6  \w    -70.00  14.00   0.50    3.30    --   -0.82  -9.00 126.83  168
  7  \w    -23.00  69.00   0.50    3.30    --   -0.82   6.00 131.87  184
  8  \w     -4.00  65.00   0.50    3.30    --   -0.82  38.00 -30.00  138
  9  \w     20.00  89.00   0.50    3.30    --   20.00-152.00 -24.70  138
 10  \w     17.00  86.00   0.50    3.30    --   20.00-148.00  62.01  138
 11  \w     16.00  84.00   0.50    3.30    --   20.00-145.00-164.39  136
 12  \w    -49.00  24.00   0.50    3.30    --   20.00 -26.00 -98.48  146
 13  \w    -42.00  13.00   0.50    3.30    --   -0.82 -77.00-180.00  110
 14  \w    -15.00  34.00   0.50    3.30    --   -0.82 -99.00  30.00   98
 15  \w    -12.00  62.00   0.50    3.30    --   -0.82  57.00-180.00  148
 16  \w    -15.00  34.00   0.50    3.30    --   -0.82 -99.00-120.00   98
 17  \w    -24.00  21.00   0.50    3.30    --   -0.82  77.00  30.00   90
 18  \w     17.00  86.00   0.50    3.30    --   20.00-148.00 -77.15  138
 19  \w    -43.00  37.00   0.50    3.30    --   20.00 -67.00-154.63  160
 20  \w      8.00  71.00   0.50    3.30    --   20.00-127.00 112.90  126
 21  \w     -9.00  58.00   0.50    3.30    --   20.00-107.00 157.23  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            105632
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.321
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         11325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0384P)^2^+9.3437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9354
_reflns_number_total             11325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06233k2.cif
_cod_data_source_block           sn-sr-c9-dippteph_auto
_cod_database_code               7135247
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.841
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Te2) = Uanis(Te1)
2. Others
 Fixed Sof: Te1(0.8) Te2(0.2)
3.a Ternary CH refined with riding coordinates:
 C31(H31), C34(H34), C49(H49), C58(H58), C28(H28), C61(H61), C37(H37), C46(H46)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C13(H13), C12(H12), C44(H44), C11(H11), C26(H26), C43(H43),
 C56(H56), C24(H24), C25(H25), C42(H42), C6(H6), C54(H54), C7(H7), C67(H67),
 C5(H5A), C66(H66), C55(H55), C73(H73), C74(H74), C72(H72), C4(H4A), C71(H71),
 C8(H8), C68(H68), C75(H75), C64(H64), C65(H65), C70(H70), C69(H69)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C30(H30A,H30B,H30C), C51(H51A,H51B,H51C), C63(H63A,
 H63B,H63C), C48(H48A,H48B,H48C), C29(H29A,H29B,H29C), C47(H47A,H47B,H47C),
 C50(H50A,H50B,H50C), C62(H62A,H62B,H62C), C60(H60A,H60B,H60C), C38(H38A,H38B,
 H38C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              21500
_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
;