Oxygen transfer reactivity mediated by nickel perfluoroalkyl complexes using molecular oxygen as a terminal oxidant
Deolka, Shubham; Govindarajan, R.; Khaskin, Eugene; Vasylevskyi, Serhii; Bahri, Janet; Fayzullin, Robert R.; Roy, Michael C.; Khusnutdinova, Julia R.; Chemical Science 14 (2023) 7026–7035; doi:10.1039/D3SC01861J

data_1569337
_publ_section_title
;
 Oxygen transfer reactivity mediated by nickel perfluoroalkyl complexes
 using molecular oxygen as a terminal oxidant
;
_journal_issue                   25
_journal_name_full               'Chemical Science'
_journal_page_first              7026
_journal_page_last               7035
_journal_paper_doi               10.1039/D3SC01861J
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C24 H20 F10 N4 Ni'
_chemical_formula_sum            'C24 H20 F10 N4 Ni'
_chemical_formula_weight         613.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-02-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-02-14 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.067(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6069(3)
_cell_length_b                   10.0489(2)
_cell_length_c                   11.2681(3)
_cell_measurement_reflns_used    6084
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.0730
_cell_measurement_theta_min      5.9260
_cell_volume                     1189.16(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_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     16.00 139.00   0.50    1.23    --   49.60  77.00 120.00  246
  2  \w     24.00 139.00   0.50    1.23    --   49.60  38.00  90.00  230
  3  \w     24.00 139.00   0.50    1.23    --   49.60  38.00-150.00  230
  4  \w     21.00 139.00   0.50    4.91    --  110.20 -61.00  60.00  236
  5  \w     85.00 200.00   0.50    4.91    --  110.20  45.00 150.00  230
  6  \w     85.00 200.00   0.50    4.91    --  110.20  45.00  90.00  230
  7  \w     75.00 200.00   0.50    4.91    --  110.20  82.00-180.00  250
  8  \w     21.00 144.00   0.50    4.91    --  110.20 -77.00  60.00  246
  9  \w     83.00 200.00   0.50    4.91    --  110.20  30.00 150.00  234
 10  \w     85.00 200.00   0.50    4.91    --  110.20  45.00 120.00  230
 11  \w    -40.00  85.00   0.50    1.23    --   49.60 -82.00-120.00  250
 12  \w     14.00 139.00   0.50    1.23    --   49.60  82.00-120.00  250
 13  \w     22.00 106.00   0.50    1.23    --   49.60  57.00   0.00  168
 14  \w     24.00 139.00   0.50    1.23    --   49.60  38.00 -30.00  230
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0830221000
_diffrn_orient_matrix_UB_12      -0.0496328000
_diffrn_orient_matrix_UB_13      -0.0926710000
_diffrn_orient_matrix_UB_21      0.0754483000
_diffrn_orient_matrix_UB_22      0.1313747000
_diffrn_orient_matrix_UB_23      0.0128834000
_diffrn_orient_matrix_UB_31      0.0943193000
_diffrn_orient_matrix_UB_32      -0.0615506000
_diffrn_orient_matrix_UB_33      0.1017311000
_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  0.0762
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11676
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.503
_diffrn_reflns_theta_min         5.364
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1273P)^2^+0.1818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2169
_reflns_number_total             2506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01861j3.cif
_cod_data_source_block           jk2000_s
_cod_database_code               1569337
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C20H20N4F10Ni1
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.639
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              49586
_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 3.486
_oxdiff_exptl_absorpt_empirical_full_min 0.494