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_1575807
_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 H76 N5 Zn, B C24 F20, C H Cl3'
_chemical_formula_sum            'C77 H77 B Cl3 F20 N5 Zn'
_chemical_formula_weight         1634.96
_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             2024-09-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-05 deposited with the CCDC.	2025-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                76.126(2)
_cell_angle_beta                 73.337(2)
_cell_angle_gamma                78.115(2)
_cell_formula_units_Z            2
_cell_length_a                   16.1606(4)
_cell_length_b                   17.0908(3)
_cell_length_c                   17.4475(3)
_cell_measurement_reflns_used    17336
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.932
_cell_measurement_theta_min      3.423
_cell_volume                     4432.88(17)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61141
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.932
_diffrn_reflns_theta_min         3.423
_exptl_absorpt_coefficient_mu    1.933
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.327
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.646
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         17308
_refine_ls_number_restraints     666
_refine_ls_restrained_S_all      1.630
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.1232
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3766
_refine_ls_wR_factor_ref         0.3906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13701
_reflns_number_total             17308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02907k2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1575802--1575808.cif.'
_cod_database_code               1575807
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: -0.6(9)
 1.6(9)
2. 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
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24), C33(H33), C36(H36), C46(H46), C49(H49),
 C77(H77)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C17(H17), C18(H18), C19(H19), C29(H29), C30(H30), C31(H31),
 C42(H42), C43(H43), C44(H44), C52(H52), N3(H3), N4(H4), N5(H5A)
4.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42902
_shelx_fab_checksum              38293
_olex2_submission_special_instructions 'No special instructions were received'