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_7719319
_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         '3(C54 H72 Co N6)'
_chemical_formula_sum            'C162 H216 Co3 N18'
_chemical_formula_weight         2592.30
_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             2024-06-21
_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                   49.9427(5)
_cell_length_b                   15.8154(2)
_cell_length_c                   18.8866(2)
_cell_measurement_reflns_used    55828
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.7690
_cell_measurement_theta_min      2.9340
_cell_volume                     14917.8(3)
_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      99.99(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 0.975
_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    -58.00 -33.00   0.50    0.57    --  -59.24 -15.00 120.00   50
  2  \w    -99.00 -74.00   0.50    0.57    --  -59.24 -15.00 120.00   50
  3  \w   -126.00 -41.00   0.50    0.57    --  -75.92 -15.00  60.00  170
  4  \w    -77.00 -51.00   0.50    0.57    --  -75.92 -15.00   0.00   52
  5  \w   -117.00 -92.00   0.50    0.57    --  -75.92 -15.00   0.00   50
  6  \w   -125.00 -40.00   0.50    0.57    --  -75.92 -15.00 -60.00  170
  7  \w    -81.00 -56.00   0.50    0.57    --  -71.89 107.00 117.00   50
  8  \w    -91.00 -38.00   0.50    0.57    --  -75.92 111.00  90.00  106
  9  \w    -63.00 -35.00   0.50    0.57    --  -75.92 107.00 117.00   56
 10  \w    -94.00 -46.00   0.50    0.57    --  -71.89 125.00 150.00   96
 11  \w    -50.00 -24.00   0.50    0.57    --  -59.24 107.00 117.00   52
 12  \w     56.00  93.00   0.50    0.57    --   56.34  15.00 120.00   74
 13  \w     49.00  77.00   0.50    0.57    --   56.34  15.00  60.00   56
 14  \w     80.00 106.00   0.50    0.57    --   56.34  15.00  60.00   52
 15  \w     49.00 135.00   0.50    0.57    --   84.35  15.00 -30.00  172
 16  \w     21.00  57.00   0.50    0.57    --   56.34-125.00 -90.00   72
 17  \w     18.00  44.00   0.50    0.57    --   56.34 -95.00 -60.00   52
 18  \w     36.00  62.00   0.50    0.57    --   56.34-107.00  18.00   52
 19  \w     28.00  74.00   0.50    0.57    --   69.55-107.00  18.00   92
 20  \w     38.00  63.00   0.50    0.57    --   76.38-107.00  18.00   50
 21  \w     65.00  91.00   0.50    0.57    --   84.35 -95.00  60.00   52
 22  \w     35.00  80.00   0.50    0.57    --   76.38 -95.00  60.00   90
 23  \w     42.00  91.00   0.50    0.57    --   84.35 -95.00  30.00   98
 24  \w     41.00  87.00   0.50    0.57    --   84.35-107.00  18.00   92
 25  \w     42.00  92.00   0.50    0.57    --   84.35 -95.00  90.00  100
 26  \w     33.00  76.00   0.50    0.57    --   69.55 -95.00 -60.00   86
 27  \w     35.00  83.00   0.50    0.57    --   76.38 -95.00 -90.00   96
 28  \w     54.00  80.00   0.50    0.57    --   84.35 -95.00-150.00   52
 29  \w    -53.00 -27.00   0.50    0.57    --  -71.89 107.00 117.00   52
 30  \w     32.00  57.00   0.50    0.57    --   56.34-125.00 120.00   50
 31  \w    -55.00 -29.00   0.50    0.57    --  -71.89 125.00-120.00   52
 32  \w     93.00 119.00   0.50    0.57    --   76.38  15.00 -90.00   52
 33  \w     31.00  57.00   0.50    0.57    --   76.38-111.00  90.00   52
 34  \w     38.00  82.00   0.50    0.57    --   76.38 -95.00-120.00   88
 35  \w     43.00  78.00   0.50    0.57    --   76.38  15.00 -90.00   70
 36  \w     39.00  64.00   0.50    0.57    --   84.35-111.00 150.00   50
 37  \w     51.00  77.00   0.50    0.57    --   84.35 -95.00 -30.00   52
 38  \w     58.00  84.00   0.50    0.57    --   84.35 -95.00-150.00   52
 39  \w     31.00  56.00   0.50    0.57    --   69.55-107.00  18.00   50
 40  \w    -74.00 -48.00   0.50    0.57    --  -59.24 -15.00 -30.00   52
 41  \w    -61.00 -35.00   0.50    0.57    --  -76.68 111.00  90.00   52
 42  \w    -62.00 -36.00   0.50    0.57    --  -76.68 111.00-120.00   52
 43  \w     96.00 122.00   0.50    0.57    --   80.73  15.00-150.00   52
 44  \w     49.00  91.00   0.50    0.57    --   80.73-111.00-120.00   84
 45  \w     40.00  65.00   0.50    0.57    --   80.73-107.00  18.00   50
 46  \w     34.00  60.00   0.50    0.57    --   56.34 -95.00 -90.00   52
 47  \w     57.00  83.00   0.50    0.57    --   80.73 -95.00-120.00   52
 48  \w    -68.00 -43.00   0.50    0.57    --  -59.24 107.00 117.00   50
 49  \w     34.00  60.00   0.50    0.57    --   56.34 -95.00 -90.00   52
;
_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      -0.0251435000
_diffrn_orient_matrix_UB_12      0.0296061000
_diffrn_orient_matrix_UB_13      0.0440724000
_diffrn_orient_matrix_UB_21      0.0055394000
_diffrn_orient_matrix_UB_22      0.0733795000
_diffrn_orient_matrix_UB_23      -0.0388307000
_diffrn_orient_matrix_UB_31      -0.0170304000
_diffrn_orient_matrix_UB_32      -0.0198630000
_diffrn_orient_matrix_UB_33      -0.0776696000
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            199019
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.974
_diffrn_reflns_theta_min         2.931
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.004
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68053
_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            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             5580
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.354
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.442(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1697
_refine_ls_number_reflns         28392
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0575
_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^)+(0.1124P)^2^+3.0754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.947
_reflns_Friedel_fraction_max     0.870
_reflns_number_gt                22711
_reflns_number_total             28392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01455g2.cif
_cod_data_source_block           231108lt_auto
_cod_depositor_comments
'Adding full bibliography for 7719316--7719320.cif.'
_cod_database_code               7719319
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C H N O '
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55753
 0.44247
2.a Ternary CH refined with riding coordinates:
 C51(H51), C54(H54), C58(H58), C61(H61), C171(H171), C174(H174), C178(H178),
 C181(H181), C81(H81), C84(H84), C88(H88), C91(H91), C141(H141), C144(H144),
 C148(H148), C151(H151), C21(H21), C24(H24), C28(H28), C31(H31), C111(H111),
 C114(H114), C118(H118), C121(H121)
2.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C47(H47), C48(H48),
 C49(H49), C156(H156), C157(H157), C158(H158), C161(H161), C162(H162),
 C167(H167), C168(H168), C169(H169), C66(H66), C67(H67), C68(H68), C71(H71),
 C72(H72), C77(H77), C78(H78), C79(H79), C126(H126), C127(H127), C128(H128),
 C131(H131), C132(H132), C137(H137), C138(H138), C139(H139), C6(H6), C7(H7),
 C8(H8), C11(H11), C12(H12), C17(H17), C18(H18), C19(H19), C96(H96), C97(H97),
 C98(H98), C101(H101), C102(H102), C107(H107), C108(H108), C109(H109)
2.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C172(H17G,H17H,H17I), C173(H17A,H17B,H17C), C175(H17M,H17N,H17O),
 C176(H17J,H17K,H17L), C179(H17D,H17E,H17F), C180(H18A,H18B,H18C), C182(H18G,
 H18H,H18I), C183(H18D,H18E,H18F), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C),
 C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C89(H89A,H89B,H89C), C90(H90A,H90B,
 H90C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C142(H14J,H14K,H14L),
 C143(H14A,H14B,H14C), C145(H14G,H14H,H14I), C146(H14D,H14E,H14F), C149(H14M,
 H14N,H14O), C150(H15G,H15H,H15I), C152(H15D,H15E,H15F), C153(H15A,H15B,H15C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C112(H11G,H11H,H11I), C113(H11A,H11B,H11C), C115(H11M,H11N,H11O),
 C116(H11J,H11K,H11L), C119(H11D,H11E,H11F), C120(H12D,H12E,H12F), C122(H12G,
 H12H,H12I), C123(H12A,H12B,H12C)
;
_shelx_res_checksum              46227
_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 1.287
_oxdiff_exptl_absorpt_empirical_full_min 0.811