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_1569339
_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         'C28 H22 F12 N4 Ni2 O9'
_chemical_formula_sum            'C28 H22 F12 N4 Ni2 O9'
_chemical_formula_weight         903.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-14 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.582(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0089(5)
_cell_length_b                   9.68800(10)
_cell_length_c                   20.2007(6)
_cell_measurement_reflns_used    12265
_cell_measurement_temperature    100
_cell_measurement_theta_max      77.0880
_cell_measurement_theta_min      4.3910
_cell_volume                     3438.62(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.974
_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    4.99    --   49.60  77.00 -90.00  246
  2  \w     22.00 139.00   0.50    4.99    --   49.60  57.00 120.00  234
  3  \w     85.00 200.00   0.50   19.96    --  110.20  45.00  30.00  230
  4  \w     21.00 139.00   0.50   19.96    --  110.20 -61.00  90.00  236
  5  \w     21.00 200.00   0.50   19.96    --  110.20   0.00  90.00  358
  6  \w     21.00 136.00   0.50   19.96    --  110.20 -45.00  30.00  230
  7  \w     21.00 136.00   0.50   19.96    --  110.20 -45.00-150.00  230
  8  \w    -40.00  85.00   0.50    4.99    --   49.60 -82.00  30.00  250
  9  \w     14.00 139.00   0.50    4.99    --   49.60  82.00   0.00  250
 10  \w     22.00 139.00   0.50    4.99    --   49.60  57.00-150.00  234
 11  \w     21.00 146.00   0.50   19.96    --  110.20 -82.00 -30.00  250
 12  \w     83.00 200.00   0.50   19.96    --  110.20  30.00 -90.00  234
 13  \w     21.00 146.00   0.50   19.96    --  110.20 -82.00-180.00  250
 14  \w     85.00 158.00   0.50   19.96    --  110.20  45.00-150.00  146
 15  \w     83.00 200.00   0.50   19.96    --  110.20  30.00-180.00  234
;
_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      -0.0011833000
_diffrn_orient_matrix_UB_12      0.1463665000
_diffrn_orient_matrix_UB_13      0.0292638000
_diffrn_orient_matrix_UB_21      0.0781373000
_diffrn_orient_matrix_UB_22      -0.0265491000
_diffrn_orient_matrix_UB_23      0.0692068000
_diffrn_orient_matrix_UB_31      0.0396764000
_diffrn_orient_matrix_UB_32      0.0563557000
_diffrn_orient_matrix_UB_33      -0.0435814000
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.869
_diffrn_reflns_theta_min         4.986
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       needle
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0536P)^2^+4.8334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3475
_reflns_number_total             3660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01861j3.cif
_cod_data_source_block           jk1300a
_cod_original_cell_volume        3438.62(16)
_cod_database_code               1569339
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C16F15H12N2O1Ni1
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.695
_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:
 C3(H3), C7(H7), C12(H12), C14(H14)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              59341
_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 1.501
_oxdiff_exptl_absorpt_empirical_full_min 0.567