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_7135244
_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 Se Zn, 1(C7 H8)'
_chemical_formula_sum            'C63 H83 N5 Se Zn'
_chemical_formula_weight         1054.67
_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                99.880(3)
_cell_angle_beta                 92.266(2)
_cell_angle_gamma                96.260(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6388(3)
_cell_length_b                   14.3737(5)
_cell_length_c                   15.1130(4)
_cell_measurement_reflns_used    21638
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.6970
_cell_measurement_theta_min      3.7950
_cell_volume                     2896.27(15)
_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      100.01(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     22.00  72.00   0.50    3.18    --    3.35-155.00-135.00  100
  2  \w      2.00  49.00   0.50    3.18    --    3.35-120.00  22.00   94
  3  \w    -65.00   9.00   0.50    3.18    --    3.35 -19.00  60.00  148
  4  \w     -8.00  66.00   0.50    3.18    --    3.35  57.00-120.00  148
  5  \w    -15.00  30.00   0.50    3.18    --   -4.60 -99.00  90.00   90
  6  \w    -42.00  19.00   0.50    3.18    --   -4.60 -77.00 -60.00  122
  7  \w    -16.00  58.00   0.50    3.18    --   -4.60  57.00-150.00  148
  8  \w    -65.00   9.00   0.50    3.18    --    3.35 -19.00 120.00  148
  9  \w    -67.00   7.00   0.50    3.18    --   -4.60 -57.00  30.00  148
;
_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_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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            10198
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.205
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63618
_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    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.797
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         10198
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0407P)^2^+14.3074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8932
_reflns_number_total             10198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06233k2.cif
_cod_data_source_block           sn-sr-c9-dep_auto
_cod_database_code               7135244
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.811
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93403
 0.06597
2. Restrained distances
 C4-C51 \\sim C4A-C51A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C51A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C4, C5, C6, C31, C32, C38, C51, C51A, C4A, C5A, C6A, C31A, C32A, C38A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C4A)=Sof(C5A)=Sof(H5AA)=Sof(C6A)=
 Sof(H6A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C38A)=Sof(H38A)=1-FVAR(1)
 Sof(C4)=Sof(C5)=Sof(H5A)=Sof(C6)=Sof(H6)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=
 Sof(C38)=Sof(H38)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C45(H45), C61(H61), C48(H48), C58(H58), C25(H25), C13(H13), C28(H28),
 C16(H16), C38A(H38A)
6.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C56(H56), C43(H43), C11(H11), C54(H54), C42(H42), C41(H41),
 C22(H22), C23(H23), C55(H55), C37(H37), C9(H9), C10(H10), C21(H21), C36(H36),
 C35(H35), C33(H33), C34(H34), C5(H5A), C6(H6), C31(H31), C32(H32), C38(H38),
 C5A(H5AA), C6A(H6A), C31A(H31A), C32A(H32A)
6.c Fitted hexagon refined as free rotating group:
 C4(C5,C6,C31,C32,C38), C4A(C5A,C6A,C31A,C32A,C38A)
6.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C27(H27A,H27B,
 H27C), C62(H62A,H62B,H62C), C47(H47A,H47B,H47C), C60(H60A,H60B,H60C), C15(H15A,
 H15B,H15C), C46(H46A,H46B,H46C), C59(H59A,H59B,H59C), C14(H14A,H14B,H14C),
 C26(H26A,H26B,H26C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C17(H17A,H17B,H17C), C51(H51A,H51B,H51C), C51A(H51D,H51E,H51F)
;
_shelx_res_checksum              25718
_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
;