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_1569344
_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         'C18 H13 F18 N3 Ni2, C H2 Cl2'
_chemical_formula_sum            'C19 H15 Cl2 F18 N3 Ni2'
_chemical_formula_weight         815.66
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-20
_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                 101.679(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5628(5)
_cell_length_b                   13.9251(7)
_cell_length_c                   17.4612(7)
_cell_measurement_reflns_used    3611
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.0930
_cell_measurement_theta_min      4.2260
_cell_volume                     2753.3(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.970
_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     24.00 139.00   1.00   50.00    --   49.60  38.00-180.00  115
  2  \w    -40.00  75.00   1.00   50.00    --   49.60 -38.00-150.00  115
  3  \w    -40.00  77.00   1.00   50.00    --   49.60 -57.00 -60.00  117
  4  \w     21.00 146.00   1.00   50.00    --  110.20 -82.00 -90.00  125
  5  \w     83.00 200.00   1.00   50.00    --  110.20  30.00 150.00  117
  6  \w     21.00 138.00   1.00   50.00    --  110.20 -30.00-150.00  117
  7  \w     21.00 156.00   1.00   50.00    --  110.20 -15.00-180.00  135
  8  \w     21.00 146.00   1.00   50.00    --  110.20 -82.00-150.00  125
  9  \w     82.00 200.00   1.00   50.00    --  110.20  61.00-180.00  118
 10  \w     21.00 139.00   1.00   50.00    --  110.20 -61.00 -90.00  118
 11  \w     21.00 144.00   1.00   50.00    --  110.20 -77.00  30.00  123
 12  \w     24.00 139.00   1.00   50.00    --   49.60  38.00  60.00  115
 13  \w     22.00 103.00   1.00   50.00    --   49.60  57.00 -60.00   81
;
_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      -0.1325817000
_diffrn_orient_matrix_UB_12      0.0053824000
_diffrn_orient_matrix_UB_13      0.0015400000
_diffrn_orient_matrix_UB_21      0.0294785000
_diffrn_orient_matrix_UB_22      -0.0051488000
_diffrn_orient_matrix_UB_23      0.0899739000
_diffrn_orient_matrix_UB_31      0.0078231000
_diffrn_orient_matrix_UB_32      0.1103960000
_diffrn_orient_matrix_UB_33      0.0042015000
_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  0.0972
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27772
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.211
_diffrn_reflns_theta_min         4.094
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52403
_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    1.968
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1497P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3801
_reflns_number_total             5833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01861j3.cif
_cod_data_source_block           jk1313
_cod_database_code               1569344
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C10H14N4Ni2F6O4
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.699
_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.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C14(H14), C13(H13)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              17825
_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 1.476
_oxdiff_exptl_absorpt_empirical_full_min 0.707