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_1575803
_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         'C50 H70 I N5 Zn'
_chemical_formula_sum            'C50 H70 I N5 Zn'
_chemical_formula_weight         933.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-02-16
_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                90
_cell_angle_beta                 104.4850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.16000(10)
_cell_length_b                   21.0258(2)
_cell_length_c                   21.7420(3)
_cell_measurement_reflns_used    12675
_cell_measurement_temperature    100
_cell_measurement_theta_max      76.1780
_cell_measurement_theta_min      4.2150
_cell_volume                     4939.55(10)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -35.00  19.00   0.50    1.00    --    0.00 100.00 147.00  108
  2  \w    101.00 170.00   0.50    4.00    --  102.08 100.00 147.00  138
  3  \w     34.00 110.00   0.50    4.00    --  102.08-100.00  41.00  152
  4  \w    -22.00  62.00   0.50    1.00    --    0.00  77.00-120.00  168
  5  \w     -1.00  65.00   0.50    1.00    --    0.00  37.00   0.00  132
  6  \w    -61.00  10.00   0.50    1.00    --    0.00 -57.00  30.00  142
  7  \w     36.00 103.00   0.50    4.00    --  102.08 -30.00 -30.00  134
  8  \w    101.00 169.00   0.50    4.00    --  102.08  30.00 150.00  136
  9  \w     36.00 103.00   0.50    4.00    --  102.08 -30.00-180.00  134
 10  \w     36.00 103.00   0.50    4.00    --  102.08 -30.00-120.00  134
 11  \w     40.00 114.00   0.50    4.00    --  102.08 -61.00  90.00  148
 12  \w     39.00 118.00   0.50    4.00    --  102.08-125.00-120.00  158
 13  \w    100.00 170.00   0.50    4.00    --  102.08  15.00  30.00  140
 14  \w     34.00 104.00   0.50    4.00    --  102.08 -94.00-180.00  140
 15  \w    100.00 162.00   0.50    4.00    --  102.08  45.00 120.00  124
 16  \w    107.00 165.00   0.50    4.00    --  102.08  45.00-150.00  116
 17  \w     41.00 105.00   0.50    4.00    --  102.08 -45.00-180.00  128
;
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18195
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         4.200
_exptl_absorpt_coefficient_mu    5.863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43257
_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            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.115
_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     267
_refine_ls_number_reflns         4537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0825P)^2^+3.8167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4282
_reflns_number_total             4537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02907k2.cif
_cod_data_source_block           sn-rks-196
_cod_depositor_comments
'Adding full bibliography for 1575802--1575808.cif.'
_cod_database_code               1575803
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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:
 C10(H10), C20(H20), C7(H7), C23(H23)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C3(H3A), C4(H4), C5(H5), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C11(H11A,H11B,
 H11C), C25(H25A,H25B,H25C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C21(H21A,
 H21B,H21C)
;
_shelx_res_checksum              91313
_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
;