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_7133301
_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_absolute_configuration syn
_chemical_formula_moiety         'C72 H82 N12 Ni4 O6, 2(C F3 O3 S), 3[C4H8O]'
_chemical_formula_sum            'C74 H82 F6 N12 Ni4 O12 S2'
_chemical_formula_weight         1744.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-19
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7338(4)
_cell_length_b                   18.9753(5)
_cell_length_c                   33.7970(12)
_cell_measurement_reflns_used    31537
_cell_measurement_temperature    85
_cell_measurement_theta_max      66.2850
_cell_measurement_theta_min      2.6130
_cell_volume                     8807.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    6.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    6.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    6.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    6.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    6.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    6.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    6.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    6.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    6.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    6.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    6.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    6.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    6.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    6.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    6.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    6.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    6.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    6.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    6.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    6.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    6.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    6.00    --  -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      -0.0227639000
_diffrn_orient_matrix_UB_12      0.0200708000
_diffrn_orient_matrix_UB_13      -0.0431867000
_diffrn_orient_matrix_UB_21      -0.1070717000
_diffrn_orient_matrix_UB_22      -0.0215799000
_diffrn_orient_matrix_UB_23      0.0061392000
_diffrn_orient_matrix_UB_31      -0.0242991000
_diffrn_orient_matrix_UB_32      0.0756557000
_diffrn_orient_matrix_UB_33      0.0132861000
_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  0.0849
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            130494
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.153
_diffrn_reflns_theta_min         2.615
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.316
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       plate
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_coef       0.00042(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   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         16461
_refine_ls_number_restraints     652
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0795
_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^)+(0.1177P)^2^+12.2463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2111
_refine_ls_wR_factor_ref         0.2216
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                14084
_reflns_number_total             16461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02241f2.cif
_cod_data_source_block           hll273
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'Syn' was changed
to 'syn' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133299--7133302.cif.
;
_cod_database_code               7133301
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C74H82F6N12Ni4O12S2
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.794
_reflns_odcompleteness_completeness 98.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.03
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.92(4)
 0.08(4)
2. 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 C(H,H,H,H) groups
3. Restrained distances
 C49A-F5A = C49A-F6A = C49A-F4A
 1.33 with sigma of 0.02
 C49A-S2A
 1.82 with sigma of 0.02
 S2A-O10A = S2A-O11A = S2A-O12A
 1.44 with sigma of 0.02
 O4-H4 = O5-H5 = O3-H3 = O2-H2
 0.99 with sigma of 0.02
 C49A-O12A
 2.57 with sigma of 0.04
 C49A-O10A
 2.58 with sigma of 0.04
 C49A-O11A
 2.56 with sigma of 0.04
 H4-Ni2
 2.5 with sigma of 0.04
 Ni3-H4
 2.5 with sigma of 0.04
 Ni3-H2
 2.45 with sigma of 0.04
 H2-Ni1
 2.45 with sigma of 0.04
 H5-Ni2
 2.35 with sigma of 0.04
 H5-Ni4
 2.35 with sigma of 0.04
 Ni1-H3
 2.45 with sigma of 0.04
 H3-Ni4
 2.45 with sigma of 0.04
 F2A-C48A \\sim F2B-C48B
 with sigma of 0.02
 F2A-F3A \\sim F2B-F3B
 with sigma of 0.04
 S1-O7 \\sim S1A-O7A
 with sigma of 0.02
 F1A-C48A \\sim F1B-C48B
 with sigma of 0.02
 F1A-F2A \\sim F1B-F2B
 with sigma of 0.04
 S1-F2A \\sim S1A-F2B
 with sigma of 0.04
 S1-F3A \\sim S1A-F3B
 with sigma of 0.04
 F1A-F3A \\sim F1B-F3B
 with sigma of 0.04
 F3A-C48A \\sim F3B-C48B
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 O7-O9 \\sim O7A-O9A
 with sigma of 0.04
 O7-C48A \\sim O7A-C48B
 with sigma of 0.04
 O8-O9 \\sim O8A-O9A
 with sigma of 0.04
 O8-C48A \\sim O8A-C48B
 with sigma of 0.04
 S1-O8 \\sim S1A-O8A
 with sigma of 0.02
 S1-O9 \\sim S1A-O9A
 with sigma of 0.04
 O9-C48A \\sim O9A-C48B
 with sigma of 0.04
 S1-F1A \\sim S1A-F1B
 with sigma of 0.04
 S1-C48A \\sim S1A-C48B
 with sigma of 0.02
 C40-C43A \\sim C40-C43B
 with sigma of 0.02
 S2A-O10A \\sim S2A-O11A \\sim S2A-O12A
 with sigma of 0.02
 O10A-O11A \\sim O11A-O12A \\sim O10A-O12A
 with sigma of 0.04
 C49A-F5A \\sim C49A-F6A \\sim C49A-F4A
 with sigma of 0.02
 C43A-C46A \\sim C43B-C45B
 with sigma of 0.02
 C49A-O10A \\sim C49A-O11A \\sim C49A-O12A
 with sigma of 0.04
 F5A-F6A \\sim F6A-F4A \\sim F4A-F5A
 with sigma of 0.04
 S2A-F5A \\sim S2A-F6A \\sim S2A-F4A
 with sigma of 0.04
 C43A-C45A \\sim C43B-C44B
 with sigma of 0.02
 S2A-O12A \\sim S2B-O12B
 with sigma of 0.02
 C49A-O12A \\sim C43-O12B
 with sigma of 0.04
 O10A-O12A \\sim O10B-O12B
 with sigma of 0.04
 O11A-O12A \\sim O11B-O12B
 with sigma of 0.04
 C49A-F5A \\sim C43-F4B
 with sigma of 0.02
 C49A-F6A \\sim C43-F5B
 with sigma of 0.02
 C49A-F4A \\sim C43-F6B
 with sigma of 0.02
 C49A-S2A \\sim C43-S2B
 with sigma of 0.02
 S2A-O10A \\sim S2B-O10B
 with sigma of 0.02
 C43A-C44A \\sim C43B-C46B
 with sigma of 0.02
 S2A-O11A \\sim S2B-O11B
 with sigma of 0.02
 C49A-O10A \\sim C43-O10B
 with sigma of 0.04
 C49A-O11A \\sim C43-O11B
 with sigma of 0.04
 F5A-F6A \\sim F4B-F5B
 with sigma of 0.04
 F5A-F4A \\sim F4B-F6B
 with sigma of 0.04
 C40-C46A \\sim C40-C45B
 with sigma of 0.04
 F5A-S2A \\sim F4B-S2B
 with sigma of 0.04
 F6A-F4A \\sim F5B-F6B
 with sigma of 0.04
 F6A-S2A \\sim F5B-S2B
 with sigma of 0.04
 F4A-S2A \\sim F6B-S2B
 with sigma of 0.04
 O10A-O11A \\sim O10B-O11B
 with sigma of 0.04
 C40-C45A \\sim C40-C44B
 with sigma of 0.04
 C40-C44A \\sim C40-C46B
 with sigma of 0.04
 C46A-C45A \\sim C45B-C44B
 with sigma of 0.04
 C46A-C44A \\sim C45B-C46B
 with sigma of 0.04
 C45A-C44A \\sim C44B-C46B
 with sigma of 0.04
4. Restrained angles
 Ni2-O5-H5
 fixed at 120 with sigma of 0.02
 Ni2-O4-H4
 fixed at 120 with sigma of 0.02
5. Rigid bond restraints
 S1A, S1, O7, O8, O9, C48A, F1A, F2A, F3A, F2B, F3B, C48B, O7A, O8A, O9A, F1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2A, F4A, F5A, F6A, O10A, O11A, O12A, C49A, S2B, F4B, F5B, F6B, O10B, O11B,
 O12B, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
S2A \\sim F4A \\sim F5A \\sim F6A \\sim O10A \\sim O11A \\sim O12A \\sim C49A
\\sim S2B \\sim F4B \\sim F5B \\sim F6B \\sim O10B \\sim O11B \\sim O12B \\sim
C43: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
7. Rigid body (RIGU) restrains
 S1A, S1, O7, O8, O9, C48A, F1A, F2A, F3A, O8A, O7A, C48B, F1B, F2B, F3B, O9A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2A, F4A, F5A, F6A, O10A, O11A, O12A, C49A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2A, F4A, F5A, F6A, O10A, O11A, O12A, C49A, S2B, F4B, F5B, F6B, O10B, O11B,
 O12B, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C43A, C44A, H44A, H44B, H44C, C45A, H45A, H45B, H45C, C46A, H46A, H46B, H46C,
 C43B, C44B, C45B, H45D, H45E, H45F, C46B, H46D, H46E, H46F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Sof(C43B)=Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45B)=Sof(H45D)=
 Sof(H45E)=Sof(H45F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45A)=Sof(H45A)=
 Sof(H45B)=Sof(H45C)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
 Sof(S2B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=Sof(C43)=1-
 FVAR(2)
 Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(C49A)=
 FVAR(2)
 Sof(S1A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(C48B)=1-
 FVAR(3)
 Sof(S1)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C48A)=FVAR(3)
9.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), C47(H47A,H47B), C48(H48A,H48B), C54(H54A,H54B),
 C60(H60A,H60B), C61(H61A,H61B), C67(H67A,H67B)
9.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5A), 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), C39(H39), C41(H41), C50(H50), C51(H51), C52(H52),
 C53(H53), C56(H56), C57(H57), C58(H58), C59(H59), C63(H63), C64(H64), C65(H65),
  C66(H66), C69(H69), C70(H70), C71(H71), C72(H72)
9.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C44A(H44A,H44B,H44C),
 C45A(H45A,H45B,H45C), C46A(H46A,H46B,H46C), C44B(H44D,H44E,H44F), C45B(H45D,
 H45E,H45F), C46B(H46D,H46E,H46F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45256
_shelx_hkl_checksum              12019
_shelx_fab_checksum              15293
_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 2.122
_oxdiff_exptl_absorpt_empirical_full_min 0.523