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_7135242
_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         'C84 H110 N10 O2 Zn2, 2(C6 H6)'
_chemical_formula_sum            'C96 H122 N10 O2 Zn2'
_chemical_formula_weight         1578.77
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-10-06
_audit_creation_method
;
Olex2 1.5-ac5-021
(compiled 2022.02.15 svn.rf212a0ae for Rigaku Oxford Diffraction, GUI svn.r6439)
;
_audit_update_record
;
2025-10-20 deposited with the CCDC.	2025-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                106.138(3)
_cell_angle_beta                 108.774(3)
_cell_angle_gamma                91.802(3)
_cell_formula_units_Z            1
_cell_length_a                   12.0595(4)
_cell_length_b                   12.8394(4)
_cell_length_c                   15.0633(5)
_cell_measurement_reflns_used    16006
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.9380
_cell_measurement_theta_min      3.5490
_cell_volume                     2102.42(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
'olex2.solve 1.5-ac5-021 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -13.00  38.00   0.50    9.56    --    1.08-102.00  -9.00  102
  2  \w    -13.00  34.00   0.50    9.56    --   -2.25-102.00  -9.00   94
  3  \w     -5.00  64.00   0.50    9.56    --   -2.25  37.00-150.00  138
  4  \w     -5.00  64.00   0.50    9.56    --   -2.25  37.00 -30.00  138
  5  \w    -42.00  21.00   0.50    9.56    --   -2.25 -77.00-150.00  126
  6  \w     -5.00  64.00   0.50    9.56    --   -2.25  37.00  90.00  138
  7  \w    -68.00   3.00   0.50    9.56    --    1.08 -19.00   0.00  142
  8  \w    -25.00  21.00   0.50    9.56    --   -2.25  77.00 150.00   92
  9  \w    -25.00  21.00   0.50    9.56    --   -2.25  77.00  30.00   92
;
_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  0.0659
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31839
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.333
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54786
_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    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_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         -0.843
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7674
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0889P)^2^+1.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6393
_reflns_number_total             7674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06233k2.cif
_cod_data_source_block           sn-sr-c8-znoh_auto
_cod_database_code               7135242
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.885
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.8 with sigma of 0.02
3. Rigid bond restraints
 C3, C8, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C4) = Uanis(C8)
5.a Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C46(H46a,H46b), C24(H24a,H24b), C26(H26a,H26b), C38(H38a,
 H38b), C48(H48a,H48b), C22(H22a,H22b), C36(H36a,H36b)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C7(H7), C19(H19), C20(H20), C44(H44), C18(H18), C5(H5a),
 C43(H43), C34(H34), C42(H42), C53(H53), C6(H6), C33(H33), C52(H52), C51(H51),
 C50(H50), C54(H54), C55(H55), C32(H32)
5.c Idealised Me refined as rotating group:
 C49(H49a,H49b,H49c), C25(H25a,H25b,H25c), C47(H47a,H47b,H47c), C29(H29a,H29b,
 H29c), C39(H39a,H39b,H39c), C27(H27a,H27b,H27c), C23(H23a,H23b,H23c), C37(H37a,
 H37b,H37c)
;
_shelx_res_checksum              38146
_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
;