Two-coordinate Co and Ni complexes of a bulky imidazolin-2-iminato ligand and facile synthesis of heterobimetallic complexes.
Chen, Yu-Hsuan; Chen, Guan-Wen; Lee, Yi-Hui; Liu, Hsin-Kuan; Lin, Chun-Yi; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14448–14455; doi:10.1039/d5dt01455g

data_7719317
_publ_section_title
;
 Two-coordinate Co and Ni complexes of a bulky imidazolin-2-iminato ligand
 and facile synthesis of heterobimetallic complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14448
_journal_page_last               14455
_journal_paper_doi               10.1039/d5dt01455g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C54 H72 Cl2 Co Ge N6'
_chemical_formula_sum            'C54 H72 Cl2 Co Ge N6'
_chemical_formula_weight         1007.59
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3891(2)
_cell_length_b                   19.61330(10)
_cell_length_c                   12.14250(10)
_cell_measurement_reflns_used    20062
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.8560
_cell_measurement_theta_min      3.0040
_cell_volume                     5332.06(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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     43.00 107.00   0.50    0.19    --   56.39  15.00 -90.00  128
  2  \w     83.00 109.00   0.50    0.19    --   80.61  15.00 -90.00   52
  3  \w     51.00  76.00   0.50    0.19    --   80.61  15.00 -90.00   50
  4  \w     45.00 126.00   0.50    0.19    --   80.61  15.00 -60.00  162
  5  \w     47.00 110.00   0.50    0.19    --   80.61  15.00  30.00  126
  6  \w     16.00  42.00   0.50    0.19    --   56.39 -95.00 -30.00   52
  7  \w     28.00  57.00   0.50    0.19    --   69.64 -95.00-180.00   58
  8  \w     49.00  89.00   0.50    0.19    --   80.61-111.00-180.00   80
  9  \w     38.00  63.00   0.50    0.19    --   80.61 -95.00-120.00   50
 10  \w     38.00  73.00   0.50    0.19    --   80.61 -95.00-150.00   70
 11  \w     28.00  60.00   0.50    0.19    --   69.64 -95.00   0.00   64
 12  \w     36.00  74.00   0.50    0.19    --   80.61-111.00  30.00   76
 13  \w     28.00  54.00   0.50    0.19    --   56.39 -95.00  60.00   52
 14  \w     36.00  66.00   0.50    0.19    --   80.61-111.00 150.00   60
 15  \w     22.00  50.00   0.50    0.19    --   56.39 -95.00 120.00   56
 16  \w   -127.00-101.00   0.50    0.19    --  -76.67 -15.00-120.00   52
 17  \w   -126.00 -44.00   0.50    0.19    --  -76.67 -15.00  90.00  164
 18  \w   -127.00 -41.00   0.50    0.19    --  -76.67 -15.00 -30.00  172
 19  \w    -91.00 -35.00   0.50    0.19    --  -76.67 111.00-150.00  112
 20  \w    -46.00 -21.00   0.50    0.19    --  -59.22 112.00 143.00   50
 21  \w     13.00  38.00   0.50    0.19    --   56.15 -95.00 -30.00   50
 22  \w    -51.00 -25.00   0.50    0.19    --  -71.82 125.00  30.00   52
 23  \w    -58.00 -32.00   0.50    0.19    --  -76.67 111.00-150.00   52
 24  \w    -57.00 -31.00   0.50    0.19    --  -76.67 111.00 -90.00   52
 25  \w     38.00  63.00   0.50    0.19    --   80.61 -95.00-180.00   50
 26  \w     46.00  75.00   0.50    0.19    --   80.61 -95.00 -90.00   58
 27  \w     55.00  81.00   0.50    0.19    --   80.61 -95.00   0.00   52
 28  \w     56.00  82.00   0.50    0.19    --   80.61 -95.00  60.00   52
 29  \w     39.00  65.00   0.50    0.19    --   80.61 -95.00  90.00   52
 30  \w    -70.00 -45.00   0.50    0.19    --  -59.22 112.00 143.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0425827000
_diffrn_orient_matrix_UB_12      0.0142325000
_diffrn_orient_matrix_UB_13      0.0611132000
_diffrn_orient_matrix_UB_21      0.0059199000
_diffrn_orient_matrix_UB_22      -0.1235830000
_diffrn_orient_matrix_UB_23      0.0164326000
_diffrn_orient_matrix_UB_31      0.0537320000
_diffrn_orient_matrix_UB_32      0.0248792000
_diffrn_orient_matrix_UB_33      0.0465265000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            45096
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.307
_diffrn_reflns_theta_min         2.995
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.96a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             2124
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.753
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.493(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         9997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0606P)^2^+3.8778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.881
_reflns_number_gt                8855
_reflns_number_total             9997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01455g2.cif
_cod_data_source_block           240262lt_auto
_cod_depositor_comments
'Adding full bibliography for 7719316--7719320.cif.'
_cod_database_code               7719317
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O H Cl Co Ge'
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.543
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.507(5)
 0.493(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C37(H37), C40(H40), C49(H49), C52(H52)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C45(H45), C46(H46), C47(H47)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              62588
_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 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.786