Synthesis and electronic structure elucidation of bioinspired heterobimetallic nickel complexes.
Patterson, Claire R.; Oyala, Paul H.; Buss, Joshua A.; Chemical communications (Cambridge, England) 61 (2025) 12345–12348; doi:10.1039/d5cc03435c

data_7134943
_publ_section_title
;
 Synthesis and electronic structure elucidation of bioinspired
 heterobimetallic nickel complexes.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12345
_journal_page_last               12348
_journal_paper_doi               10.1039/d5cc03435c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C39 H42 F3 Li N7 Ni O4 S, C F3 O3 S'
_chemical_formula_sum            'C40 H42 F6 Li N7 Ni O7 S2'
_chemical_formula_weight         976.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-29
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.22 svn.r631f81ec for OlexSys, GUI svn.r7248)
;
_audit_update_record
;
2025-05-29 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.08910(10)
_cell_length_b                   19.17890(10)
_cell_length_c                   23.98280(10)
_cell_measurement_reflns_used    70105
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      69.3940
_cell_measurement_theta_min      3.2550
_cell_volume                     8780.29(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (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_temperature      153(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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   -110.00  70.00   1.00    1.00    --  -20.00   0.00-180.00  180
  2  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  \w    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  \w   -173.00-128.00   1.00    5.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    5.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    5.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    5.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    5.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    5.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    5.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    5.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    5.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    5.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    5.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    5.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    5.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    5.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    5.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    5.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    5.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    5.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    5.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    5.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    5.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    5.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0042331000
_diffrn_orient_matrix_UB_12      0.0388868000
_diffrn_orient_matrix_UB_13      -0.0561007000
_diffrn_orient_matrix_UB_21      0.0806042000
_diffrn_orient_matrix_UB_22      -0.0007808000
_diffrn_orient_matrix_UB_23      0.0035166000
_diffrn_orient_matrix_UB_31      0.0014437000
_diffrn_orient_matrix_UB_32      -0.0702764000
_diffrn_orient_matrix_UB_33      -0.0310575000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            125929
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.530
_diffrn_reflns_theta_min         2.950
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       block
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.373(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1235
_refine_ls_number_reflns         16349
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0424P)^2^+1.7916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                15890
_reflns_number_total             16349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03435c2.cif
_cod_data_source_block           cp124
_cod_database_code               7134943
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C37H39F3N6NiO4S
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.627(11)
 0.373(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O15-C81 \\sim O12-C80
 with sigma of 0.02
 F15-F13 \\sim F11-F12
 with sigma of 0.02
 O17-C81 \\sim O14-C80
 with sigma of 0.02
 F14-C81 \\sim F10-C80
 with sigma of 0.02
 F15-C81 \\sim F11-C80
 with sigma of 0.02
 O17-O15 \\sim O14-O12
 with sigma of 0.02
 F15-O15 \\sim F11-O12
 with sigma of 0.02
 O17-O16 \\sim O14-O13
 with sigma of 0.02
 S5-F14 \\sim S4-F10
 with sigma of 0.02
 S5-F15 \\sim S4-F11
 with sigma of 0.02
 F13-C81 \\sim F12-C80
 with sigma of 0.02
 S5-O17 \\sim S4-O14
 with sigma of 0.02
 S5-F13 \\sim S4-F12
 with sigma of 0.02
 S5-O15 \\sim S4-O12
 with sigma of 0.02
 O15-O16 \\sim O12-O13
 with sigma of 0.02
 S5-O16 \\sim S4-O13
 with sigma of 0.02
 S5-C81 \\sim S4-C80
 with sigma of 0.02
 O16-C81 \\sim O13-C80
 with sigma of 0.02
 F14-F15 \\sim F10-F11
 with sigma of 0.02
 F14-F13 \\sim F10-F12
 with sigma of 0.02
 F15-O17 \\sim F11-O14
 with sigma of 0.02
4. Rigid bond restraints
 S5, O17, O15, O16, C81, F13, F14, F15, S4, C80, F12, F10, F11, O14, O12, O13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Rigid body (RIGU) restrains
 O14, S5, O17, O15, O16, C81, F13, F14, F15, C80, S4, F12, F10, F11, O12, O13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C80)=Sof(S4)=Sof(O14)=Sof(O12)=Sof(O13)=Sof(F12)=Sof(F10)=Sof(F11)=1-
 FVAR(1)
 Sof(S5)=Sof(F14)=Sof(F15)=Sof(O17)=Sof(F13)=Sof(O15)=Sof(O16)=Sof(C81)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C65(H65A,H65B), C31(H31A,H31B), C51(H51A,H51B), C52(H52A,
 H52B), C71(H71A,H71B), C25(H25A,H25B), C64(H64A,H64B), C11(H11A,H11B),
 C58(H58A,H58B), C12(H12A,H12B), C18(H18A,H18B)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C43(H43), C57(H57), C36(H36), C30(H30), C17(H17), C73(H73), C56(H56),
 C70(H70), C33(H33), C29(H29), C23(H23), C20(H20), C3(H3), C54(H54), C63(H63),
 C55(H55), C61(H61), C69(H69), C14(H14), C22(H22), C15(H15), C16(H16), C74(H74),
  C34(H34), C60(H60), C67(H67), C35(H35), C76(H76), C45(H45), C21(H21),
 C68(H68), C62(H62), C28(H28), C27(H27), C75(H75)
7.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C79(H79A,H79B,H79C), C50(H50A,H50B,H50C), C8(H8A,H8B,
 H8C), C9(H9A,H9B,H9C), C39(H39A,H39B,H39C), C48(H48A,H48B,H48C), C10(H10A,H10B,
 H10C)
;
_shelx_res_checksum              46600
_shelx_hkl_checksum              6477
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.248
_oxdiff_exptl_absorpt_empirical_full_min 0.568