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_7063644
_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         'C24 H48 Cu N6 O3, 2(N O3)'
_chemical_formula_sum            'C24 H48 Cu N8 O9'
_chemical_formula_weight         656.243
_chemical_name_systematic
'[Cu(1,4,7-tris-isopropylacrylamide-1,4,7-triazacyclononane)][NO3]2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2024-10-21
_audit_creation_method
;
Olex2 1.5-alpha
(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                 103.813(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4229(3)
_cell_length_b                   10.9307(2)
_cell_length_c                   17.9733(3)
_cell_measurement_reflns_used    47310
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.5450
_cell_measurement_theta_min      2.1800
_cell_volume                     3133.15(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9147
_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    -56.00   1.00   0.50    0.17    --  -10.97 -57.00 150.00  114
  2  \w    -50.00  -7.00   0.50    0.17    --  -10.97 119.00 105.63   86
  3  \w    -40.00   9.00   0.50    0.17    --  -10.97  95.00  11.59   98
  4  \w    -40.00   9.00   0.50    0.17    --  -10.97  95.00-126.82   98
  5  \w    -44.00   3.00   0.50    0.17    --  -10.97 104.00-148.78   94
  6  \w    -35.00  15.00   0.50    0.17    --  -10.97  87.00-178.02  100
  7  \w    -11.00  15.00   0.50    0.17    --   13.47  87.00 -28.30   52
  8  \w     -9.00  19.00   0.50    0.17    --   13.47  82.00-119.49   56
  9  \w    -22.00  62.00   0.50    0.17    --  -10.97  57.00 -60.00  168
 10  \w    -31.00   0.00   0.50    0.17    --  -10.97  77.00   0.00   62
 11  \w     21.00  67.00   0.50    0.17    --  -10.97  19.00 -30.00   92
 12  \w     21.00  67.00   0.50    0.17    --  -10.97  19.00  90.00   92
 13  \w     21.00  67.00   0.50    0.17    --  -10.97  19.00 150.00   92
 14  \w      2.00  62.00   0.50    0.17    --   13.47  57.00 120.00  120
 15  \w      2.00  62.00   0.50    0.17    --   13.47  57.00  60.00  120
 16  \w      2.00  62.00   0.50    0.17    --   13.47  57.00   0.00  120
 17  \w     21.00  92.00   0.50    0.17    --   13.47  19.00 -60.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.9998
_diffrn_reflns_Laue_measured_fraction_max 0.9147
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            85801
_diffrn_reflns_point_group_measured_fraction_full 0.9998
_diffrn_reflns_point_group_measured_fraction_max 0.9147
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.36
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.94a (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    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             1398.432
_exptl_crystal_recrystallization_method
'Vapour diffusion of diethyl ether into a methanol solutuion containing sample'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.9475
_refine_diff_density_min         -0.9090
_refine_diff_density_rms         0.0658
_refine_ls_d_res_high            0.6639
_refine_ls_d_res_low             10.5821
_refine_ls_goodness_of_fit_ref   1.0630
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     811
_refine_ls_number_reflns         10252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0630
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+0.8296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0559
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -24
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -15
_reflns_number_gt                8432
_reflns_number_total             10252
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4nj05327c2.cif
_cod_data_source_block           GR_CBG_[Cu(L2)][NO3]2_auto
_cod_depositor_comments
'Adding full bibliography for 7063640--7063645.cif.'
_cod_database_code               7063644
_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
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   2
   DATE:           2024-10-21_16-27-48
;
_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
;