Di- and tri-valent metal complexes with tris-amide-functionalised 1,4,7-triazacyclononane chelators
O’Callaghan, Charley; Greenacre, Victoria K.; Reid, Gillian; New Journal of Chemistry 49 (2025) 4061–4071; doi:10.1039/D4NJ05327C

data_7063641
_publ_section_title
;
 Di- and tri-valent metal complexes with tris-amide-functionalised
 1,4,7-triazacyclononane chelators
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4061
_journal_page_last               4071
_journal_paper_doi               10.1039/D4NJ05327C
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C30 H35 Co N6 O3, 2(N O3), 2(C1 H4 O1)'
_chemical_formula_sum            'C32 H43 Co N8 O11'
_chemical_formula_weight         774.67
_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   geom
_audit_creation_date             2024-10-29
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-25 deposited with the CCDC.	2025-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.185(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8001(2)
_cell_length_b                   17.3514(3)
_cell_length_c                   19.5643(3)
_cell_measurement_reflns_used    40647
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.3020
_cell_measurement_theta_min      1.8940
_cell_volume                     3644.95(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      0.00  56.00   0.50    1.11    --   11.49  57.00  60.00  112
  2  \w      0.00  56.00   0.50    1.11    --   11.49  57.00 150.00  112
  3  \w      0.00  56.00   0.50    1.11    --   11.49  57.00   0.00  112
  4  \w      8.00  89.00   0.50    1.11    --   11.49  22.00 -71.00  162
  5  \w      0.00  56.00   0.50    1.11    --   11.49  57.00 -90.00  112
  6  \w      8.00  65.00   0.50    1.11    --  -12.74  22.00 -71.00  114
  7  \w    -32.00  18.00   0.50    1.11    --  -12.74  77.00-120.00  100
  8  \w    -32.00  18.00   0.50    1.11    --  -12.74  77.00 150.00  100
  9  \w    -91.00 -14.00   0.50    1.11    --  -12.74 -22.00 122.00  154
 10  \w    -65.00 -14.00   0.50    1.11    --   11.49 -22.00 122.00  102
 11  \w    -66.00 -22.00   0.50    1.11    --   11.49 -19.00  60.00   88
 12  \w    -66.00 -22.00   0.50    1.11    --   11.49 -19.00-120.00   88
 13  \w    -66.00 -22.00   0.50    1.11    --   11.49 -19.00-180.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74317
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.897
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark pink'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         9423
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0885P)^2^+5.5085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8227
_reflns_number_total             9423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj05327c2.cif
_cod_data_source_block           gr_coc_(co(l1)(no3)2_reprocessed1(1)
_cod_depositor_comments
'Adding full bibliography for 7063640--7063645.cif.'
_cod_database_code               7063641
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O108-C101 \\sim O107-C102
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O107, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O107, H107, C102, H10A, H10B, H10C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O107)=Sof(H107)=Sof(C102)=Sof(H10A)=Sof(H10B)=Sof(H10C)=1-FVAR(1)
 Sof(O108)=Sof(H108)=Sof(C101)=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C15(H15A,H15B), C23(H23A,H23B)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C29(H29),
  C30(H30)
5.c Idealised Me refined as rotating group:
 C102(H10A,H10B,H10C), C101(H10D,H10E,H10F), C103(H10G,H10H,H10I)
5.d Idealised tetrahedral OH refined as rotating group:
 O107(H107), O108(H108), O109(H109)
;
_shelx_res_checksum              10915
_shelx_hkl_checksum              98097
_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
;