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_7133302
_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
'C74 H82 N12 Ni4 O10, 2(C F3 O3 S), [+ solvents]'
_chemical_formula_sum            'C76 H82 F6 N12 Ni4 O16 S2'
_chemical_formula_weight         1832.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 111.887(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1401(9)
_cell_length_b                   32.5762(9)
_cell_length_c                   17.5728(6)
_cell_measurement_reflns_used    17266
_cell_measurement_temperature    85
_cell_measurement_theta_max      66.5910
_cell_measurement_theta_min      2.7240
_cell_volume                     8573.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection
'DTREK_VERSION=d*TREK version 9.9.9.4 W9RSSI -- Aug 22 2012'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (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 0.998
_diffrn_measured_fraction_theta_max 0.984
_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   20.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00   20.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00   20.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00   20.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00   20.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00   20.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00   20.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00   20.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00   20.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00   20.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00   20.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00   20.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00   20.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00   20.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00   20.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00   20.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00   20.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00   20.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00   20.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00   20.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00   20.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00   20.00    --  -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      -0.0946573000
_diffrn_orient_matrix_UB_12      -0.0178358000
_diffrn_orient_matrix_UB_13      -0.0408539000
_diffrn_orient_matrix_UB_21      0.0149987000
_diffrn_orient_matrix_UB_22      -0.0265446000
_diffrn_orient_matrix_UB_23      0.0765467000
_diffrn_orient_matrix_UB_31      -0.0373243000
_diffrn_orient_matrix_UB_32      0.0348315000
_diffrn_orient_matrix_UB_33      0.0374178000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1640
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            117295
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.645
_diffrn_reflns_theta_min         2.713
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (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    1.420
_exptl_crystal_description       plate
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.272
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         15886
_refine_ls_number_restraints     503
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.1345
_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^)+(0.1748P)^2^+74.3771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3526
_refine_ls_wR_factor_ref         0.3756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11245
_reflns_number_total             15886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02241f2.cif
_cod_data_source_block           hl524
_cod_depositor_comments
'Adding full bibliography for 7133299--7133302.cif.'
_cod_database_code               7133302
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H45 F3 N6 Ni2 O8 S1'
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.52
_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, All O(H,H) groups
2. Restrained distances
 C76B-F4B = C76B-F5B = C76B-F6B
 1.33 with sigma of 0.02
 C76B-S2B
 1.82 with sigma of 0.02
 C75B-F1B = C75B-F2B = C75B-F3B
 1.33 with sigma of 0.02
 S2B-O14B = S2B-O16B = S2B-O15B
 1.44 with sigma of 0.02
 C76B-O14B
 2.58 with sigma of 0.04
 C76B-O16B
 2.56 with sigma of 0.04
 C76B-O15B
 2.57 with sigma of 0.04
 C75B-F1B \\sim C75A-F1A
 with sigma of 0.02
 C75B-F2B \\sim C75A-F2A
 with sigma of 0.02
 C75B-F3B \\sim C75A-F3A
 with sigma of 0.02
 C9A-C7 \\sim C8B-C7 \\sim C8A-C7 \\sim C7-C10B \\sim C7-C10A \\sim C9B-C7
 with sigma of 0.02
 S1-O11B \\sim S1A-O11A
 with sigma of 0.02
 F1B-F2B \\sim F1A-F2A
 with sigma of 0.04
 F1B-F3B \\sim F1A-F3A
 with sigma of 0.04
 C8A-C9A \\sim C8A-C10A \\sim C9A-C10A
 with sigma of 0.02
 F2B-F3B \\sim F2A-F3A
 with sigma of 0.04
 C8B-C9B \\sim C8B-C10B \\sim C9B-C10B
 with sigma of 0.02
 C75B-F1B \\sim C75B-F2B \\sim C75B-F3B
 with sigma of 0.02
 F1B-F2B \\sim F2B-F3B \\sim F3B-F1B
 with sigma of 0.04
 F3B-C75B \\sim F1B-C75B \\sim F2B-C75B \\sim F1A-C75A \\sim F2A-C75A \\sim
F3A-C75A
 with sigma of 0.02
 S1A-C75A \\sim S1-C75B
 with sigma of 0.02
 S1A-O12A \\sim S1A-O13A \\sim S1A-O11A \\sim S1-O11B \\sim S1-O13B \\sim
S1-O12B
 with sigma of 0.02
 C76B-F4B \\sim C76B-F5B \\sim C76B-F6B
 with sigma of 0.02
 F4B-F5B \\sim F5B-F6B \\sim F6B-F4B
 with sigma of 0.04
 S2B-F4B \\sim S2B-F5B \\sim S2B-F6B
 with sigma of 0.04
 S2B-O14B \\sim S2B-O16B \\sim S2B-O15B
 with sigma of 0.02
 O14B-O16B \\sim O16B-O15B \\sim O14B-O15B
 with sigma of 0.04
 C76B-O14B \\sim C76B-O16B \\sim C76B-O15B
 with sigma of 0.04
 C76B-F4B \\sim C76A-F5A
 with sigma of 0.02
 C76B-F5B \\sim C76A-F6A
 with sigma of 0.02
 C76B-F6B \\sim C76A-F4A
 with sigma of 0.02
 C76B-S2B \\sim C76A-S2A
 with sigma of 0.02
 S2B-O14B \\sim S2A-O16A
 with sigma of 0.02
 S2B-O16B \\sim S2A-O15A
 with sigma of 0.02
 S2B-O15B \\sim S2A-O14A
 with sigma of 0.02
 C76B-O14B \\sim C76A-O16A
 with sigma of 0.04
 C76B-O16B \\sim C76A-O15A
 with sigma of 0.04
 C76B-O15B \\sim C76A-O14A
 with sigma of 0.04
 F4B-F5B \\sim F5A-F6A
 with sigma of 0.04
 F4B-F6B \\sim F5A-F4A
 with sigma of 0.04
 F4B-S2B \\sim F5A-S2A
 with sigma of 0.04
 F5B-F6B \\sim F6A-F4A
 with sigma of 0.04
 F5B-S2B \\sim F6A-S2A
 with sigma of 0.04
 F6B-S2B \\sim F4A-S2A
 with sigma of 0.04
 O14B-O16B \\sim O16A-O15A
 with sigma of 0.04
 O14B-O15B \\sim O16A-O14A
 with sigma of 0.04
 O16B-O15B \\sim O15A-O14A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S1 \\sim F1B \\sim F2B \\sim F3B \\sim O11B \\sim O12B \\sim O13B \\sim C75B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
S2B \\sim F4B \\sim F5B \\sim F6B \\sim O14B \\sim O15B \\sim O16B \\sim C76B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 S1, F1B, F2B, F3B, O11B, O12B, O13B, C75B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1A, F1A, F2A, F3A, O11A, O12A, O13A, C75A, S1, F1B, F2B, F3B, O11B, O12B,
 O13B, C75B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2B, F4B, F5B, F6B, O14B, O15B, O16B, C76B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2A, S2B, F4A, F4B, F5A, F5B, F6A, F6B, O14A, O14B, O15A, O15B, O16A, O16B,
 C76A, C76B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7, C8A, C9A, C10A, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(C10B)=Sof(H10F)=Sof(H10G)=Sof(H10H)=1-FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(H10E)=FVAR(1)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O11A)=Sof(O12A)=Sof(O13A)=Sof(C75A)=1-
 FVAR(2)
 Sof(S1)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O11B)=Sof(O12B)=Sof(O13B)=Sof(C75B)=
 FVAR(2)
 Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O14A)=Sof(O15A)=Sof(O16A)=Sof(C76A)=1-
 FVAR(3)
 Sof(S2B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O14B)=Sof(O15B)=Sof(O16B)=Sof(C76B)=
 FVAR(3)
6.a Rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C25(H25A,
 H25B), C31(H31A,H31B), C49(H49A,H49B), C50(H50A,H50B), C56(H56A,H56B),
 C62(H62A,H62B), C63(H63A,H63B), C69(H69A,H69B)
6.c 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), C41(H41), C43(H43), C52(H52), C53(H53), C54(H54),
 C55(H55), C58(H58), C59(H59), C60(H60), C61(H61), C65(H65), C66(H66), C67(H67),
  C68(H68), C71(H71), C72(H72), C73(H73), C74(H74)
6.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C8A(H8AA,H8AB,
 H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10C,H10D,H10E), C8B(H8BA,H8BB,H8BC),
 C9B(H9BA,H9BB,H9BC), C10B(H10F,H10G,H10H)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35808
_shelx_hkl_checksum              32214
_shelx_fab_checksum              1595
_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 2.048
_oxdiff_exptl_absorpt_empirical_full_min 0.528