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_7062879
_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_formula_moiety         'C8 H20 Cl2 Co N4, Cl'
_chemical_formula_sum            'C8 H20 Cl3 Co N4'
_chemical_formula_weight         337.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2f7fjn
_audit_creation_date             2023-06-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_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                   14.5774(8)
_cell_length_b                   7.4338(3)
_cell_length_c                   12.8552(7)
_cell_measurement_reflns_used    2224
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5290
_cell_measurement_theta_min      4.1250
_cell_volume                     1393.06(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -15.00  41.00   1.00    5.00    --   15.49 -99.00 -90.00   56
  2  \w    -23.00   3.00   1.00    5.00    --  -16.28 -99.00 -60.00   26
  3  \w     32.00  88.00   1.00    5.00    --   15.49-178.00  60.00   56
  4  \w    -13.00  23.00   1.00    5.00    --  -16.28 -99.00  90.00   36
  5  \w     34.00  83.00   1.00    5.00    --   15.49  57.00-180.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0475329000
_diffrn_orient_matrix_UB_12      0.0137499000
_diffrn_orient_matrix_UB_13      0.0085495000
_diffrn_orient_matrix_UB_21      -0.0052644000
_diffrn_orient_matrix_UB_22      -0.0925274000
_diffrn_orient_matrix_UB_23      0.0121304000
_diffrn_orient_matrix_UB_31      0.0088253000
_diffrn_orient_matrix_UB_32      0.0188166000
_diffrn_orient_matrix_UB_33      0.0531731000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5469
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.017
_diffrn_reflns_theta_max         25.017
_diffrn_reflns_theta_min         3.461
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.788
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2224
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0439P)^2^+0.5923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    0.808
_reflns_Friedel_fraction_max     0.808
_reflns_number_gt                2036
_reflns_number_total             2224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04108e2.cif
_cod_data_source_block           exp_9472
_cod_depositor_comments
'Adding full bibliography for 7062879--7062880.cif.'
_cod_database_code               7062879
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.716
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58(4)
 0.42(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
3.a Ternary CH refined with riding coordinates:
 N11(H11), N28(H28), N27(H27), N17(H17)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C23(H23A,H23B), C18(H18A,H18B), C10(H10A,H10B), C12(H12A,H12B),
 C20(H20A,H20B), C26(H26A,H26B), C33(H33A,H33B)
;
_shelx_res_checksum              20494
_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 1.127
_oxdiff_exptl_absorpt_empirical_full_min 0.875