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_7135240
_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         'C42 H55 N5 S6 Zn'
_chemical_formula_sum            'C42 H55 N5 S6 Zn'
_chemical_formula_weight         887.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-10-20
_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                90
_cell_angle_beta                 92.938(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7048(9)
_cell_length_b                   14.9584(7)
_cell_length_c                   17.0574(9)
_cell_measurement_reflns_used    12045
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9450
_cell_measurement_theta_min      3.5100
_cell_volume                     4256.7(4)
_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      100.00(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_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    -14.00  69.00   0.50    1.90    --   -0.82  10.00 -68.00  166
  2  \w    -69.00   1.00   0.50    1.90    --   -0.82 -10.00 117.00  140
  3  \w    -15.00  34.00   0.50    1.90    --   -0.82 -99.00-180.00   98
  4  \w    -12.00  53.00   0.50    1.90    --   -0.82  57.00 -30.00  130
;
_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  0.0775
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32590
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.505
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70081
_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    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+3.5887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5904
_reflns_number_total             7726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06233k2.cif
_cod_data_source_block           sn-sr-c9-zn-s_auto
_cod_original_cell_volume        4256.6(4)
_cod_database_code               7135240
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.839
_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.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C31(H31A,H31B), C27(H27A,H27B), C29(H29A,H29B), C51(H51A,
 H51B), C43(H43A,H43B), C53(H53A,H53B), C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N5(H5), C12(H12), C25(H25), C23(H23), C11(H11), C10(H10),
 C49(H49), C24(H24), C47(H47), C39(H39), C38(H38), C37(H37), C48(H48)
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C54(H54A,H54B,H54C), C30(H30A,H30B,H30C), C28(H28A,H28B,
 H28C), C44(H44A,H44B,H44C), C32(H32A,H32B,H32C), C52(H52A,H52B,H52C), C42(H42A,
 H42B,H42C)
;
_shelx_res_checksum              76163
_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
;