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_1569341
_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         'C12 H6 F10 N2 Ni'
_chemical_formula_sum            'C12 H6 F10 N2 Ni'
_chemical_formula_weight         426.90
_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             2022-02-17
_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                 110.6460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.68610(10)
_cell_length_b                   13.95460(10)
_cell_length_c                   10.89740(10)
_cell_measurement_reflns_used    19599
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.2750
_cell_measurement_theta_min      3.2010
_cell_volume                     1378.36(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -40.00  77.00   0.50    0.50    --   49.60 -57.00 -60.00  234
  2  \w    -40.00  77.00   0.50    0.50    --   49.60 -57.00-180.00  234
  3  \w     24.00 139.00   0.50    0.50    --   49.60  38.00  60.00  230
  4  \w     21.00 136.00   0.50    0.50    --  110.20 -45.00 120.00  230
  5  \w     21.00 146.00   0.50    0.50    --  110.20 -82.00 -90.00  250
  6  \w     21.00 139.00   0.50    0.50    --  110.20 -61.00 -90.00  236
  7  \w     21.00 138.00   0.50    0.50    --  110.20 -30.00 -60.00  234
  8  \w     21.00 156.00   0.50    0.50    --  110.20 -15.00 -90.00  270
  9  \w     85.00 200.00   0.50    0.50    --  110.20  45.00 -30.00  230
 10  \w     83.00 200.00   0.50    0.50    --  110.20  30.00 -90.00  234
 11  \w     16.00 139.00   0.50    0.50    --   49.60  77.00  60.00  246
 12  \w     14.00 139.00   0.50    0.50    --   49.60  82.00 -60.00  250
 13  \w     14.00 139.00   0.50    0.50    --   49.60  82.00-120.00  250
 14  \w     22.00 139.00   0.50    0.50    --   49.60  57.00 150.00  234
 15  \w     83.00 200.00   0.50    0.50    --  110.20  30.00  60.00  234
 16  \w     65.00 200.00   0.50    0.50    --  110.20  15.00-180.00  270
 17  \w     21.00 146.00   0.50    0.50    --  110.20 -82.00  90.00  250
 18  \w     75.00 200.00   0.50    0.50    --  110.20  82.00-180.00  250
 19  \w     85.00 200.00   0.50    0.50    --  110.20  45.00  90.00  230
 20  \w     85.00 172.00   0.50    0.50    --  110.20  45.00   0.00  174
 21  \w     85.00 200.00   0.50    0.50    --  110.20  45.00 -60.00  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      -0.0722158000
_diffrn_orient_matrix_UB_12      -0.0991781000
_diffrn_orient_matrix_UB_13      -0.0068348000
_diffrn_orient_matrix_UB_21      -0.0742800000
_diffrn_orient_matrix_UB_22      0.0343943000
_diffrn_orient_matrix_UB_23      0.0960043000
_diffrn_orient_matrix_UB_31      -0.1347122000
_diffrn_orient_matrix_UB_32      0.0341423000
_diffrn_orient_matrix_UB_33      -0.1164979000
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23943
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.939
_diffrn_reflns_theta_min         5.263
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.241
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_description       irregular
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00124(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0360P)^2^+1.5566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2939
_reflns_number_total             2984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01861j3.cif
_cod_data_source_block           jk1094
_cod_database_code               1569341
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C20H12F10N4Ni1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12)
;
_shelx_res_checksum              35428
_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 2.507
_oxdiff_exptl_absorpt_empirical_full_min 0.508