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_7135246
_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         'C96 H118 N10 O2 Zn2, C6 H6'
_chemical_formula_sum            'C102 H124 N10 O2 Zn2'
_chemical_formula_weight         1652.84
_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                113.349(2)
_cell_angle_beta                 103.698(2)
_cell_angle_gamma                94.740(2)
_cell_formula_units_Z            1
_cell_length_a                   11.9496(3)
_cell_length_b                   13.6798(3)
_cell_length_c                   15.5151(3)
_cell_measurement_reflns_used    24666
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.7540
_cell_measurement_theta_min      3.5310
_cell_volume                     2217.57(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -33.00  30.00   0.50    5.65    --    3.35 -83.00 170.00  126
  2  \w    -33.00  22.00   0.50    5.65    --   -4.45 -83.00 170.00  110
  3  \w    -42.00  27.00   0.50    5.65    --    3.35 -77.00 -60.00  138
  4  \w     -8.00  66.00   0.50    5.65    --    3.35  57.00   0.00  148
  5  \w      0.00  70.00   0.50    5.65    --    3.35  38.00 -90.00  140
  6  \w     -8.00  62.00   0.50    5.65    --   -4.45  38.00 120.00  140
  7  \w    -42.00  19.00   0.50    5.65    --   -4.45 -77.00   0.00  122
  8  \w    -15.00  38.00   0.50    5.65    --    3.35 -99.00 -90.00  106
  9  \w    -74.00   1.00   0.50    5.65    --   -4.45 -19.00   0.00  150
 10  \w    -74.00  -7.00   0.50    5.65    --   -4.45   0.00  90.00  134
 11  \w    -71.00  -1.00   0.50    5.65    --   -4.45 -38.00  90.00  140
;
_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  0.0683
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43838
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.373
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69530
_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    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.084
_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     531
_refine_ls_number_reflns         8102
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0636P)^2^+3.9124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7262
_reflns_number_total             8102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06233k2.cif
_cod_data_source_block           sn-sr-c9-108_auto
_cod_original_cell_volume        2217.57(9)
_cod_database_code               7135246
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.890
_olex2_refinement_description
;
1. Rigid bond restraints
 Zn1, N2, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
Zn1 \\sim N2 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C44(H44A,H44B), C52(H52A,H52B), C36(H36A,H36B), C38(H38A,
 H38B), C40(H40A,H40B), C34(H34A,H34B), C42(H42A,H42B)
4.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N4(H4), C7(H7), C50(H50), C8(H8), C13(H13), C48(H48), C26(H26),
 C6(H6), C49(H49), C4(H4A), C24(H24), C12(H12), C32(H32), C25(H25), C57(H57),
 C31(H31), C11(H11), C5(H5A), C30(H30), C56(H56), C58(H58)
4.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C55(H55A,H55B,H55C), C39(H39A,H39B,
 H39C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C53(H53A,
 H53B,H53C)
;
_shelx_res_checksum              99635
_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
;