A dinuclear nickel peroxycarbonate complex: CO<sub>2</sub> addition promotes H<sub>2</sub>O<sub>2</sub> release.
Lillo, Hayley L.; Buss, Joshua A.; Chemical communications (Cambridge, England) 60 (2024) 8549–8552; doi:10.1039/d4cc02241f

data_7133299
_publ_section_title
;
 A dinuclear nickel peroxycarbonate complex: CO<sub>2</sub> addition
 promotes H<sub>2</sub>O<sub>2</sub> release.
;
_journal_issue                   65
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8549
_journal_page_last               8552
_journal_paper_doi               10.1039/d4cc02241f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C38 H39 F6 N6 Ni2 O7 S2, C H2 Cl2, C F3 O3 S'
_chemical_formula_sum            'C40 H41 Cl2 F9 N6 Ni2 O10 S3'
_chemical_formula_weight         1221.29
_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             2024-06-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.11800(10)
_cell_length_b                   20.66740(10)
_cell_length_c                   21.7121(2)
_cell_measurement_reflns_used    49765
_cell_measurement_temperature    85
_cell_measurement_theta_max      69.1270
_cell_measurement_theta_min      2.0720
_cell_volume                     4940.10(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      85
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_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   -110.00  70.00   1.00    1.00    --  -20.00   0.00-180.00  180
  2  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  \w    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  \w   -173.00-128.00   1.00    2.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    2.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    2.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    2.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    2.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    2.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    2.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    2.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    2.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    2.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    2.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    2.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    2.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    2.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    2.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    2.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    2.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    2.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    2.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    2.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    2.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    2.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0556175000
_diffrn_orient_matrix_UB_12      -0.0427697000
_diffrn_orient_matrix_UB_13      0.0548302000
_diffrn_orient_matrix_UB_21      0.0027440000
_diffrn_orient_matrix_UB_22      0.0585485000
_diffrn_orient_matrix_UB_23      0.0440367000
_diffrn_orient_matrix_UB_31      -0.1283962000
_diffrn_orient_matrix_UB_32      -0.0172347000
_diffrn_orient_matrix_UB_33      0.0137811000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73909
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.429
_diffrn_reflns_theta_min         2.966
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00202(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         9159
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0512P)^2^+6.7725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9031
_reflns_number_total             9159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02241f2.cif
_cod_data_source_block           cp125
_cod_depositor_comments
'Adding full bibliography for 7133299--7133302.cif.'
_cod_database_code               7133299
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H39CuF6N6NiO7S2
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.520
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.30
_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. Restrained distances
 Cl1-C40B \\sim Cl1-C40A
 with sigma of 0.02
 Cl2A-C40B \\sim Cl2B-C40A
 with sigma of 0.02
 Cl1-Cl2A \\sim Cl1-Cl2B
 with sigma of 0.02
 Cl1-C40A \\sim Cl1-C40B \\sim Cl2A-C40A \\sim Cl2B-C40B
 with sigma of 0.02
 Cl1-C40B \\sim Cl2A-C40A
 with sigma of 0.02
 Cl1-C40A \\sim Cl2B-C40B
 with sigma of 0.02
 Cl2B-C40B \\sim Cl1-C40B
 with sigma of 0.02
 Cl1-C40A \\sim Cl2A-C40A
 with sigma of 0.02
3. Rigid bond restraints
 C40B, Cl1, Cl2B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C40A \\sim Cl1 \\sim C40B \\sim Cl2A \\sim H40A \\sim H40B \\sim Cl2B \\sim
H40C \\sim H40D: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
5. Rigid body (RIGU) restrains
 C40B, Cl1, Cl2B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(Cl2B)=Sof(C40B)=Sof(H40C)=Sof(H40D)=1-FVAR(2)
 Sof(Cl2A)=Sof(C40A)=Sof(H40A)=Sof(H40B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C25(H25A,
 H25B), C31(H31A,H31B), C40A(H40A,H40B), C40B(H40C,H40D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
 C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36)
7.c Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C8B(H8BA,H8BB,
 H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F)
;
_shelx_res_checksum              72559
_shelx_hkl_checksum              2451
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.768
_oxdiff_exptl_absorpt_empirical_full_min 0.563