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_1575802
_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         'C51 H73 N5 Zn'
_chemical_formula_sum            'C51 H73 N5 Zn'
_chemical_formula_weight         821.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 104.6932(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.02153(12)
_cell_length_b                   20.9515(2)
_cell_length_c                   21.7220(3)
_cell_measurement_reflns_used    25195
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.0400
_cell_measurement_theta_min      4.1350
_cell_volume                     4851.96(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.941
_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    -43.00  26.00   0.50    1.03    --  -38.50  46.00  84.00  138
  2  \w   -103.00 -34.00   0.50    1.03    --  -38.50 -46.00 -64.00  138
  3  \w    -16.00  53.00   0.50    1.03    --   48.56 -46.00 -64.00  138
  4  \w     44.00 113.00   0.50    1.03    --   48.56  46.00  84.00  138
  5  \w     97.00 166.00   0.50    2.36    --  101.38  46.00  84.00  138
  6  \w     37.00 106.00   0.50    2.36    --  101.38 -46.00 -64.00  138
  7  \w    -50.00  24.00   0.50    1.03    --  -38.50  57.00 -60.00  148
  8  \w     28.00 100.00   0.50    1.03    --   48.56-125.00-180.00  144
  9  \w     46.00  97.00   0.50    1.03    --   48.56  37.00-180.00  102
 10  \w    104.00 145.00   0.50    2.36    --  101.38  77.00 -30.00   82
 11  \w     35.00  66.00   0.50    2.36    --  101.38-111.00  60.00   62
 12  \w     72.00 108.00   0.50    2.36    --  101.38-105.00  -4.74   72
 13  \w     39.00  97.00   0.50    2.36    --  101.38-111.00-120.00  116
 14  \w     44.00 103.00   0.50    2.36    --  101.38 -45.00   0.00  118
 15  \w     98.00 162.00   0.50    2.36    --  101.38  45.00 120.00  128
 16  \w     61.00 115.00   0.50    2.36    --  101.38 178.00 -90.00  108
 17  \w     45.00 102.00   0.50    2.36    --  101.38 -30.00-120.00  114
 18  \w     83.00 109.00   0.50    2.36    --  101.38-111.00  60.00   52
 19  \w     33.00 105.00   0.50    2.36    --  101.38 -94.00 -90.00  144
 20  \w     49.00 109.00   0.50    2.36    --  101.38-111.00 -90.00  120
 21  \w    104.00 151.00   0.50    2.36    --  101.38 111.00   0.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0617271000
_diffrn_orient_matrix_UB_12      -0.0117626000
_diffrn_orient_matrix_UB_13      0.0551423000
_diffrn_orient_matrix_UB_21      -0.0078846000
_diffrn_orient_matrix_UB_22      0.0726074000
_diffrn_orient_matrix_UB_23      0.0097560000
_diffrn_orient_matrix_UB_31      -0.1304201000
_diffrn_orient_matrix_UB_32      0.0011020000
_diffrn_orient_matrix_UB_33      -0.0472674000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37847
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.540
_diffrn_reflns_theta_min         4.147
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+2.1680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8690
_reflns_number_total             9478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02907k2.cif
_cod_data_source_block           sn-rks-dippznme
_cod_depositor_comments
'Adding full bibliography for 1575802--1575808.cif.'
_cod_database_code               1575802
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C204 H284 N20 Zn4 '
_diffrn_oxdiff_digest_frames
;
01b992a137252f4aff2f13d9748568c891000356c25
;
_diffrn_oxdiff_digest_hkl
;
01571c49d658766da3f8fd1c76f5217a185e09
;
_reflns_odcompleteness_completeness 94.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C00G(H00G), C00L(H00L), C00M(H00M), C00N(H00N), C00Q(H00Q), C00V(H00V),
 C00X(H00X), C012(H012)
2.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W),
 C00Z(H00Z), C010(H010), C011(H011), C013(H013), C014(H014), C015(H015),
 C016(H016)
2.c Idealised Me refined as rotating group:
 C00O(H00A,H00B,H00C), C00Y(H00D,H00E,H00F), C017(H01A,H01B,H01C), C018(H01D,
 H01E,H01F), C019(H01G,H01H,H01I), C01A(H01J,H01K,H01L), C01B(H01M,H01N,H01O),
 C01C(H01P,H01Q,H01R), C01D(H01S,H01T,H01U), C01E(H01V,H01W,H01X), C01F(H01Y,H,
 HA), C01G(H01Z,HB,HC), C1(H1A,H1B,H1C), C01I(H01,HD,HE), C01J(H0AA,HF,HG),
 C01K(H1AA,HH,HI), C01L(H2AA,HJ,HK)
;
_shelx_res_checksum              38336
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.305
_oxdiff_exptl_absorpt_empirical_full_min 0.508