Finding a mononuclear cobalt(iii)-peroxo complex with 1,4,7,10-tetraazacyclododecane, an intermediate for dioxygen reduction
Zhang, Yan; Qi, Xiao-Fang; Li, Can-Hao; Zhan, Shu-Zhong; New Journal of Chemistry 47 (2023) 21648–21653; doi:10.1039/D3NJ04108E

data_7062880
_publ_section_title
;
 Finding a mononuclear cobalt(iii)-peroxo complex with
 1,4,7,10-tetraazacyclododecane, an intermediate for dioxygen reduction
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21648
_journal_page_last               21653
_journal_paper_doi               10.1039/D3NJ04108E
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H41 Co2 N8 O3, 3(Cl), H2 O'
_chemical_formula_sum            'C16 H43 Cl3 Co2 N8 O4'
_chemical_formula_weight         635.79
_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             2023-03-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-06-28 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7998(3)
_cell_length_b                   12.8690(5)
_cell_length_c                   23.2104(6)
_cell_measurement_reflns_used    5348
_cell_measurement_temperature    99.98(11)
_cell_measurement_theta_max      74.8250
_cell_measurement_theta_min      3.8120
_cell_volume                     2628.45(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      99.98(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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     33.00  65.00   0.50    2.04    --    0.00  42.00 156.00   64
  2  \w    -29.00  -4.00   0.50    2.04    --    0.00 -79.00-170.00   50
  3  \w    112.00 137.00   0.50    8.15    --  101.30  79.00 -45.00   50
  4  \w     46.00  72.00   0.50    8.15    --  101.30 -42.00   4.00   52
  5  \w     49.00  74.00   0.50    8.15    --  101.30 -79.00-170.00   50
  6  \w    134.00 159.00   0.50    8.15    --  101.30  42.00 156.00   50
  7  \w     17.00  46.00   0.50    2.04    --    0.00  77.00  30.00   58
  8  \w    -28.00   7.00   0.50    2.04    --    0.00  77.00   0.00   70
  9  \w    -32.00  -6.00   0.50    2.04    --    0.00  79.00  42.60   52
 10  \w    -19.00  35.00   0.50    2.04    --    0.00  82.00 150.00  108
 11  \w     11.00  36.00   0.50    2.04    --    0.00  77.00   0.00   50
 12  \w     79.00 188.00   0.50    8.15    --  101.30  38.00 -60.00  218
 13  \w     14.00  55.00   0.50    8.15    --  101.30 -57.00 -60.00   82
 14  \w    104.00 133.00   0.50    8.15    --  101.30 -77.00 120.00   58
 15  \w     18.00  45.00   0.50    8.15    --  101.30 -77.00 120.00   54
 16  \w     69.00 128.00   0.50    8.15    --  101.30 -57.00 -60.00  118
 17  \w    165.00 190.00   0.50    8.15    --  101.30  82.00  60.00   50
 18  \w    148.00 191.00   0.50    8.15    --  101.30  82.00  30.00   86
 19  \w     83.00 157.00   0.50    8.15    --  101.30  82.00  60.00  148
 20  \w    154.00 180.00   0.50    8.15    --  101.30  79.00 -45.00   52
 21  \w    119.00 150.00   0.50    8.15    --  101.30  38.00  30.00   62
 22  \w    161.00 187.00   0.50    8.15    --  101.30  38.00  30.00   52
 23  \w     84.00 116.00   0.50    8.15    --  101.30  38.00  30.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0451740000
_diffrn_orient_matrix_UB_12      0.0098709000
_diffrn_orient_matrix_UB_13      -0.0638384000
_diffrn_orient_matrix_UB_21      0.1415340000
_diffrn_orient_matrix_UB_22      0.0629818000
_diffrn_orient_matrix_UB_23      0.0174760000
_diffrn_orient_matrix_UB_31      0.0923982000
_diffrn_orient_matrix_UB_32      -0.1014601000
_diffrn_orient_matrix_UB_33      0.0046701000
_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  0.0583
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14760
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.103
_diffrn_reflns_theta_min         3.809
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    13.025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.496(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5216
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0618
_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^)+(0.1110P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.916
_reflns_number_gt                4464
_reflns_number_total             5216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04108e2.cif
_cod_data_source_block           co
_cod_depositor_comments
'Adding full bibliography for 7062879--7062880.cif.'
_cod_database_code               7062880
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.304
_shelx_estimated_absorpt_t_min   0.191
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.504(8)
 0.496(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O1-H1
 0.85 with sigma of 0.02
 Co2-H1 \\sim H1-Co1
 with sigma of 0.02
4.a Free rotating group:
 O1W(H1WB,H1WA)
4.b Ternary CH refined with riding coordinates:
 N1(H1A), N6(H6), N5(H5), N3(H3), N2(H2), N7(H7), N4(H4), N8(H8)
4.c Secondary CH2 refined with riding coordinates:
 C14(H14B,H14A), C1(H1C,H1B), C7(H7B,H7A), C8(H8A,H8B), C5(H5A,H5B), C9(H9A,
 H9B), C10(H10B,H10A), C15(H15A,H15B), C12(H12B,H12A), C16(H16A,H16B), C6(H6B,
 H6A), C11(H11A,H11B), C13(H13B,H13A), C2(H2A,H2B), C4(H4B,H4A), C3(H3B,H3A)
;
_shelx_res_checksum              7054
_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 3.192
_oxdiff_exptl_absorpt_empirical_full_min 0.415