Synthesis and characterization of tetrapodal nickel complexes with adaptable ligand binding geometries.
Cho, Hsien-Liang; Gullett, Kelly L.; Fout, Alison R.; Chemical communications (Cambridge, England) 60 (2024) 10564–10567; doi:10.1039/d4cc03186e

data_7133681
_publ_section_title
;
 Synthesis and characterization of tetrapodal nickel complexes with
 adaptable ligand binding geometries.
;
_journal_issue                   76
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10564
_journal_page_last               10567
_journal_paper_doi               10.1039/d4cc03186e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C42 H47 F3 N7 Ni O3 S, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C45 H50 F6 N8 Ni O6 S2'
_chemical_formula_weight         1035.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.22020(10)
_cell_length_b                   21.21480(10)
_cell_length_c                   24.43120(10)
_cell_measurement_reflns_used    62870
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.6750
_cell_measurement_theta_min      2.3720
_cell_volume                     9443.58(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.103a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.103a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.103a (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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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     43.00 113.00   0.50    1.00    --  113.25-127.00 157.00  140
  2  \w     42.00 106.00   0.50    1.00    --  113.25 -95.00  30.00  128
  3  \w     44.00 111.00   0.50    1.00    --  113.25-125.00-120.00  134
  4  \w     44.00 111.00   0.50    1.00    --  113.25-125.00-180.00  134
  5  \w     42.00  75.00   0.50    1.00    --  113.25 -61.00-120.00   66
  6  \w     42.00  75.00   0.50    1.00    --  113.25 -61.00-150.00   66
  7  \w     42.00  75.00   0.50    1.00    --  113.25 -61.00 -90.00   66
  8  \w     42.00  75.00   0.50    1.00    --  113.25 -61.00 -30.00   66
  9  \w     42.00  75.00   0.50    1.00    --  113.25 -61.00  30.00   66
 10  \w    -27.00  12.00   0.50    0.16    --   47.72 -19.00 150.00   78
 11  \w    -27.00  12.00   0.50    0.16    --   47.72 -19.00  90.00   78
 12  \w     42.00  75.00   0.50    1.00    --  113.25 -61.00  60.00   66
 13  \w     42.00  75.00   0.50    1.00    --  113.25 -61.00  90.00   66
 14  \w    101.00 178.00   0.50    1.00    --  113.25  30.00  60.00  154
 15  \w     36.00 121.00   0.50    0.16    --   47.72  38.00  30.00  170
 16  \w    101.00 178.00   0.50    1.00    --  113.25  45.00-120.00  154
 17  \w    110.00 178.00   0.50    1.00    --  113.25  77.00-180.00  136
 18  \w     36.00 107.00   0.50    0.16    --   47.72  38.00-180.00  142
 19  \w    -87.00 -21.00   0.50    1.00    --  -91.75 127.00-127.00  132
 20  \w    -82.00 -22.00   0.50    1.00    --  -91.75 110.00 151.00  120
 21  \w    -49.00 -20.00   0.50    1.00    --  -91.75  45.00 150.00   58
 22  \w    -39.00  25.00   0.50    0.16    --  -47.72  38.00  90.00  128
 23  \w    -39.00  25.00   0.50    0.16    --  -47.72  38.00 -30.00  128
 24  \w   -166.00 -78.00   0.50    1.00    --  -91.75 -17.00-143.00  176
 25  \w   -119.00 -60.00   0.50    0.16    --  -47.72-144.00 -11.00  118
 26  \w   -118.00 -72.00   0.50    0.16    --  -47.72-127.00 157.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0094971000
_diffrn_orient_matrix_UB_12      -0.0699659000
_diffrn_orient_matrix_UB_13      -0.0152374000
_diffrn_orient_matrix_UB_21      -0.0159171000
_diffrn_orient_matrix_UB_22      -0.0188394000
_diffrn_orient_matrix_UB_23      0.0597439000
_diffrn_orient_matrix_UB_31      -0.0825065000
_diffrn_orient_matrix_UB_32      -0.0044872000
_diffrn_orient_matrix_UB_33      -0.0132651000
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            91427
_diffrn_reflns_theta_full        80.08
_diffrn_reflns_theta_max         80.08
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.103a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+10.9702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                9744
_reflns_number_total             10166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4cc03186e2.cif
_cod_data_source_block           hlc_qpniotf2_mecn_ether_20240131_auto
_cod_depositor_comments
'Adding full bibliography for 7133679--7133683.cif.'
_cod_original_cell_volume        9443.59(8)
_cod_database_code               7133681
_chemical_oxdiff_formula         CHNiNOSF
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F5)=Sof(F6)=Sof(F4)=Sof(O9)=Sof(O8)=Sof(O7)=1-FVAR(1)
 Sof(F8)=Sof(F9)=Sof(F7)=Sof(O4)=Sof(O5)=Sof(O6)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C25(H25), C36(H36)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C41(H41A,H41B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,
 H40B), C27(H27A,H27B), C30(H30A,H30B), C29(H29A,H29B), C26(H26A,H26B),
 C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 N7(H7), N5(H5), C22(H22), C21(H21), C35(H35), C1(H1), C16(H16), C24(H24),
 C33(H33), C32(H32), C14(H14), C3(H3), C10(H10), C4(H4), C15(H15), C12(H12),
 C2(H2), C11(H11), C9(H9)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C44(H44A,H44B,H44C)
;
_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 1.238
_oxdiff_exptl_absorpt_empirical_full_min 0.680