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_1575806
_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 H71 N5 Zn'
_chemical_formula_sum            'C50 H71 N5 Zn'
_chemical_formula_weight         807.55
_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'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     direct
_audit_creation_date             2023-02-19
_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                 127.917(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.6965(13)
_cell_length_b                   10.7068(3)
_cell_length_c                   19.6795(9)
_cell_measurement_reflns_used    16811
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.8990
_cell_measurement_theta_min      3.6640
_cell_volume                     4603.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_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    -65.00  11.00   0.50   27.25    --    4.39 -18.00-114.00  152
  2  \w    -74.00   1.00   0.50   27.25    --   -5.01 -18.00-114.00  150
  3  \w    -42.00  18.00   0.50   27.25    --   -5.01 -77.00 -30.00  120
  4  \w    -27.00  12.00   0.50   27.25    --   -5.01  77.00  90.00   78
  5  \w    -14.00  11.00   0.50   27.25    --   -5.01  77.00  60.00   50
  6  \w     -9.00  55.00   0.50   27.25    --   -5.01  19.00  30.00  128
  7  \w    -14.00  30.00   0.50   27.25    --   -5.01 -99.00-150.00   88
  8  \w    -15.00  10.00   0.50   27.25    --   -5.01 -99.00 150.00   50
;
_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      -0.0067100000
_diffrn_orient_matrix_UB_12      -0.0295902000
_diffrn_orient_matrix_UB_13      0.0255291000
_diffrn_orient_matrix_UB_21      0.0039704000
_diffrn_orient_matrix_UB_22      -0.0593054000
_diffrn_orient_matrix_UB_23      -0.0120970000
_diffrn_orient_matrix_UB_31      0.0315177000
_diffrn_orient_matrix_UB_32      0.0011172000
_diffrn_orient_matrix_UB_33      0.0358839000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28337
_diffrn_reflns_theta_full        26.3719
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.66
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.1650
_exptl_crystal_description       block
_exptl_crystal_F_000             1745.7437
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.9310
_refine_diff_density_min         -0.5309
_refine_diff_density_rms         0.0614
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             5.5636
_refine_ls_goodness_of_fit_ref   1.0302
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0302
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0510P)^2^+7.4426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              27
_reflns_limit_h_min              -34
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                4360
_reflns_number_total             4712
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02907k2.cif
_cod_data_source_block           SN_RKS_DippZnH
_cod_depositor_comments
'Adding full bibliography for 1575802--1575808.cif.'
_cod_original_cell_volume        4603.9(6)
_cod_database_code               1575806
_chemical_oxdiff_formula         'C200 H284 N20 Zn4 '
_diffrn_oxdiff_digest_frames
;
0171ea77b87adbd7f8d75d34947587742500025c0bf
;
_diffrn_oxdiff_digest_hkl
;
01dd84f7ef528a0f823c3e1699d9218636acc4
;
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_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:
 C24(H24), C27(H27), C15(H15), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C6(H6), C4(H4), C22(H22), C20(H20), C21(H21), C5(H5)
2.c Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C29(H29a,H29b,H29c), C16(H16a,H16b,H16c), C28(H28a,H28b,
 H28c), C26(H26a,H26b,H26c), C14(H14a,H14b,H14c), C13(H13a,H13b,H13c), C25(H25a,
 H25b,H25c)
;
_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 1.816
_oxdiff_exptl_absorpt_empirical_full_min 0.358