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_7134946
_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
'C40 H45 N6 Ni2 O5, C32 H12 B F24, 0.75[C4H10O]'
_chemical_formula_sum            'C75 H64.5 B F24 N6 Ni2 O5.75'
_chemical_formula_weight         1726.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-28
_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                80.2090(10)
_cell_angle_beta                 80.1190(10)
_cell_angle_gamma                75.3510(10)
_cell_formula_units_Z            4
_cell_length_a                   12.9520(2)
_cell_length_b                   17.1844(3)
_cell_length_c                   35.8757(4)
_cell_measurement_reflns_used    36757
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      69.3270
_cell_measurement_theta_min      2.6710
_cell_volume                     7543.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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 0.973
_diffrn_measured_fraction_theta_max 0.959
_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    3.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    3.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    3.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    3.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    3.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    3.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    3.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    3.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    3.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    3.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    3.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    3.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    3.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    3.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    3.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    3.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    3.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    3.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    3.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    3.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    3.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    3.00    --  -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      0.0816637000
_diffrn_orient_matrix_UB_12      0.0514727000
_diffrn_orient_matrix_UB_13      -0.0184613000
_diffrn_orient_matrix_UB_21      -0.0931835000
_diffrn_orient_matrix_UB_22      0.0716355000
_diffrn_orient_matrix_UB_23      -0.0109569000
_diffrn_orient_matrix_UB_31      -0.0064975000
_diffrn_orient_matrix_UB_32      0.0309732000
_diffrn_orient_matrix_UB_33      0.0383825000
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            112794
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.569
_diffrn_reflns_theta_min         2.681
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       needle
_exptl_crystal_F_000             3518
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2075
_refine_ls_number_reflns         27204
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0533P)^2^+4.2504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22981
_reflns_number_total             27204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03435c2.cif
_cod_data_source_block           hll3157
_cod_original_formula_sum        'C75 H64.50 B F24 N6 Ni2 O5.75'
_cod_database_code               7134946
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C72H57BF24N6Ni2O5
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. 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
2. Restrained distances
 F58-C144 \\sim F54-C144
 with sigma of 0.02
 F56-C144 \\sim F55-C144
 with sigma of 0.02
 F57-C144 \\sim F52-C144
 with sigma of 0.02
 F43-C136 \\sim F46-C136
 with sigma of 0.02
 F45-C136 \\sim F48-C136
 with sigma of 0.02
 F44-C136 \\sim F47-C136
 with sigma of 0.02
 F23-C112 \\sim F27-C112
 with sigma of 0.02
 F22-C112 \\sim F26-C112
 with sigma of 0.02
 F24-C112 \\sim F25-C112
 with sigma of 0.02
3. Rigid bond restraints
 F58, F56, F57, C144, F55, F54, F52, C141
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F43, F45, F44, C136, F47, F48, F46, C131
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F23, F22, F24, C112, F25, F27, F26, C110
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
F58 \\sim F56 \\sim F57 \\sim C144 \\sim F55 \\sim F54 \\sim F52 \\sim C141:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
F43 \\sim F45 \\sim F44 \\sim C136 \\sim F47 \\sim F48 \\sim F46 \\sim C131:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
F23 \\sim F22 \\sim F24 \\sim C112 \\sim F25 \\sim F27 \\sim F26 \\sim C110:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
5. Others
 Sof(F55)=Sof(F54)=Sof(F52)=1-FVAR(1)
 Sof(F58)=Sof(F56)=Sof(F57)=FVAR(1)
 Sof(F47)=Sof(F48)=Sof(F46)=1-FVAR(2)
 Sof(F43)=Sof(F45)=Sof(F44)=FVAR(2)
 Sof(F25)=Sof(F27)=Sof(F26)=1-FVAR(3)
 Sof(F23)=Sof(F22)=Sof(F24)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C52(H52A,H52B), C71(H71A,H71B), C11(H11A,H11B), C64(H64A,
 H64B), C12(H12A,H12B), C18(H18A,H18B), C51(H51A,H51B), C65(H65A,H65B),
 C25(H25A,H25B), C31(H31A,H31B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C86(H86), C84(H84), C82(H82), C94(H94), C98(H98), C109(H109), C102(H102),
 C140(H140), C43(H43), C100(H100), C45(H45), C106(H106), C134(H134), C90(H90),
 C70(H70), C60(H60), C61(H61), C63(H63), C122(H122), C114(H114), C142(H142),
 C138(H138), C118(H118), C92(H92), C76(H76), C62(H62), C108(H108), C126(H126),
 C57(H57), C14(H14), C116(H116), C17(H17), C56(H56), C29(H29), C3(H3),
 C130(H130), C27(H27), C30(H30), C54(H54), C67(H67), C69(H69), C16(H16),
 C124(H124), C5(H5), C55(H55), C23(H23), C73(H73), C15(H15), C68(H68), C28(H28),
  C20(H20), C132(H132), C33(H33), C75(H75), C74(H74), C36(H36), C22(H22),
 C21(H21), C35(H35), C34(H34)
6.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C78(H78A,H78B,H78C), C80(H80A,H80B,
 H80C), C48(H48A,H48B,H48C), C38(H38A,H38B,H38C), C9(H9A,H9B,H9C), C40(H40A,
 H40B,H40C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16587
_shelx_hkl_checksum              17767
_shelx_fab_checksum              52471
_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 1.909
_oxdiff_exptl_absorpt_empirical_full_min 0.579