Bulky bis-guanidine ligand-based neutral and cationic zinc alkyl, halide, and hydride complexes: synthesis, characterization, and catalytic application.
Sahoo, Rajata Kumar; Mukhopadhyay, Sayantan; Rajput, Sagrika; Jana, Achintya; Nembenna, Sharanappa; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15554–15560; doi:10.1039/d4dt02907k

data_1575808
_publ_section_title
;
 Bulky bis-guanidine ligand-based neutral and cationic zinc alkyl, halide,
 and hydride complexes: synthesis, characterization, and catalytic
 application.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15554
_journal_page_last               15560
_journal_paper_doi               10.1039/d4dt02907k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C52 H75 N5 Zn'
_chemical_formula_sum            'C52 H75 N5 Zn'
_chemical_formula_weight         835.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2023-04-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2023-09-03 deposited with the CCDC.	2025-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                91.713(1)
_cell_angle_beta                 104.010(1)
_cell_angle_gamma                115.085(1)
_cell_formula_units_Z            2
_cell_length_a                   10.7771(1)
_cell_length_b                   12.0104(2)
_cell_length_c                   21.3556(2)
_cell_measurement_reflns_used    24561
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.4480
_cell_measurement_theta_min      4.0990
_cell_volume                     2401.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9969
_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    -32.00  25.00   0.50    1.00    --    0.00  95.00  13.00  114
  2  \w    101.00 162.00   0.50    4.00    --   94.37  95.00  13.00  122
  3  \w     27.00 110.00   0.50    4.00    --   94.37 -95.00 -96.00  166
  4  \w    -61.00  10.00   0.50    1.00    --    0.00 -57.00-150.00  142
  5  \w    -65.00   1.00   0.50    1.00    --    0.00 -37.00 150.00  132
  6  \w     -1.00  65.00   0.50    1.00    --    0.00  37.00 -90.00  132
  7  \w     -1.00  65.00   0.50    1.00    --    0.00  37.00 -30.00  132
  8  \w     33.00 106.00   0.50    4.00    --   94.37 -61.00 120.00  146
  9  \w     28.00  95.00   0.50    4.00    --   94.37 -30.00-150.00  134
 10  \w     93.00 162.00   0.50    4.00    --   94.37  15.00-180.00  138
 11  \w     31.00  97.00   0.50    4.00    --   94.37 -45.00-120.00  132
 12  \w     31.00  97.00   0.50    4.00    --   94.37 -45.00 -30.00  132
 13  \w     33.00 106.00   0.50    4.00    --   94.37 -61.00  60.00  146
 14  \w     92.00 157.00   0.50    4.00    --   94.37  45.00-150.00  130
 15  \w     27.00  96.00   0.50    4.00    --   94.37 -15.00-120.00  138
 16  \w     31.00 117.00   0.50    4.00    --   94.37-125.00 -90.00  172
 17  \w     27.00 109.00   0.50    4.00    --   94.37 -94.00   0.00  164
 18  \w     94.00 161.00   0.50    4.00    --   94.37  30.00  90.00  134
 19  \w     32.00 116.00   0.50    4.00    --   94.37 -77.00   0.00  168
 20  \w     31.00  97.00   0.50    4.00    --   94.37 -45.00 120.00  132
 21  \w     31.00 117.00   0.50    4.00    --   94.37-125.00 150.00  172
 22  \w     27.00  96.00   0.50    4.00    --   94.37 -15.00 -60.00  138
 23  \w     31.00 117.00   0.50    4.00    --   94.37-125.00 -60.00  172
 24  \w     28.00  95.00   0.50    4.00    --   94.37 -30.00  30.00  134
 25  \w     94.00 158.00   0.50    4.00    --   94.37 125.00  60.00  128
 26  \w     72.00 157.00   0.50    4.00    --   94.37  77.00  90.00  170
 27  \w    -10.00  61.00   0.50    1.00    --    0.00  57.00  60.00  142
 28  \w     -1.00  65.00   0.50    1.00    --    0.00  37.00-150.00  132
 29  \w    -62.00  22.00   0.50    1.00    --    0.00 -77.00   0.00  168
 30  \w    -22.00  58.00   0.50    1.00    --    0.00  77.00  60.00  160
 31  \w     -1.00  65.00   0.50    1.00    --    0.00  37.00 150.00  132
;
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34581
_diffrn_reflns_theta_full        68.2513
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1556
_exptl_crystal_description       block
_exptl_crystal_F_000             903.0405
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.3921
_refine_diff_density_min         -0.9235
_refine_diff_density_rms         0.1175
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             10.7532
_refine_ls_goodness_of_fit_ref   1.0385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    115
_refine_ls_number_parameters     540
_refine_ls_number_reflns         8766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0385
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+7.2195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1774
_refine_ls_wR_factor_ref         0.1805
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7906
_reflns_number_total             8766
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02907k2.cif
_cod_data_source_block           SN-RKS-ZnEt
_cod_depositor_comments
'Adding full bibliography for 1575802--1575808.cif.'
_cod_database_code               1575808
_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 Ternary CH refined with riding coordinates:
 C23(H23), C35(H35), C47(H47), C38(H38), C26(H26), C12(H12), C50(H50), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N4(H4), C45(H45), C21(H21), C19(H19), C5(H5a), C43(H43), C44(H44),
 C20(H20), C7(H7), C32(H32), C31(H31), C6(H6), C33(H33)
2.d Idealised Me refined as rotating group:
 C48(H48a,H48b,H48c), C37(H37a,H37b,H37c), C49(H49a,H49b,H49c), C36(H36a,H36b,
 H36c), C51(H51a,H51b,H51c), C52(H52a,H52b,H52c), C28(H28a,H28b,H28c), C27(H27a,
 H27b,H27c), C2(H2a,H2b,H2c), C11(H11a,H11b,H11c), C24(H24a,H24b,H24c),
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C39(H39a,H39b,H39c), C40(H40a,H40b,
 H40c), C25(H25a,H25b,H25c), C10(H10a,H10b,H10c)
;
_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
;