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_7135241
_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 S Zn, C6 H6'
_chemical_formula_sum            'C62 H81 N5 S Zn'
_chemical_formula_weight         993.74
_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
_atom_sites_solution_primary     iterative
_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                100.512(2)
_cell_angle_beta                 92.232(2)
_cell_angle_gamma                96.334(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5911(3)
_cell_length_b                   14.3769(4)
_cell_length_c                   15.0900(3)
_cell_measurement_reflns_used    27596
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.6650
_cell_measurement_theta_min      2.9850
_cell_volume                     2876.10(12)
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10137
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.911
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.812
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         10137
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1216P)^2^+14.1164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2664
_refine_ls_wR_factor_ref         0.2699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9702
_reflns_number_total             10137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06233k2.cif
_cod_data_source_block           sn-sr-c8-121_auto
_cod_database_code               7135241
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90979
 0.09021
2. Uiso/Uaniso restraints and constraints
C6 \\sim C5 \\sim C4 \\sim C9 \\sim C8 \\sim C7 \\sim C8A \\sim C7A \\sim C6A
\\sim C5A \\sim C4A \\sim C9A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
3. Others
 Sof(C8A)=Sof(H8AA)=Sof(C7A)=Sof(H7AA)=Sof(C6A)=Sof(H6AA)=Sof(C5A)=Sof(H5AA)=
 Sof(C4A)=Sof(H4AA)=Sof(C9A)=Sof(H9AA)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(C5)=Sof(H5A)=Sof(C4)=Sof(H4A)=Sof(C9)=Sof(H9A)=Sof(C8)=
 Sof(H8A)=Sof(C7)=Sof(H7A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C00E(H00E), C00P(H00P), C00R(H00R), C00S(H00S), C011(H011), C013(H013),
 C018(H018), C01K(H2)
4.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C00D(H00D), C00K(H00K), C00L(H00L), C00N(H00N), C00Q(H00Q),
 C00V(H00V), C00X(H00X), C016(H016), C019(H019), C01B(H01S), C01C(H01T),
 C01E(H01X), C01F(H01Y), C01G(H01Z), C01H(H01), C01L(H3), C01N(H7), C6(H6A),
 C5(H5A), C4(H4A), C9(H9A), C8(H8A), C7(H7A), C8A(H8AA), C7A(H7AA), C6A(H6AA),
 C5A(H5AA), C4A(H4AA), C9A(H9AA)
4.c Fitted hexagon refined as free rotating group:
 C6(C5,C4,C9,C8,C7), C8A(C7A,C6A,C5A,C4A,C9A)
4.d Idealised Me refined as rotating group:
 C00O(H00A,H00B,H00C), C00W(H00F,H00G,H00H), C00Z(H00I,H00J,H00M), C010(H01A,
 H01B,H01C), C012(H01D,H01E,H01F), C014(H01G,H01H,H01I), C015(H01J,H01K,H01L),
 C017(H01M,H01N,H01O), C01A(H01P,H01Q,H01R), C01D(H01U,H01V,H01W), C01I(H1,H,
 HA), C01M(H6,HB,HC), C01O(H8,HD,HE), C01P(H9,HF,HG), C01Q(H10,HH,HI), C01R(H11,
 HJ,HK)
;
_shelx_res_checksum              37055
_olex2_submission_special_instructions 'No special instructions were received'