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_7063640
_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         'C18 H24 Ga N4 O5, N O3, 1.5[H2O]'
_chemical_formula_sum            'C18 H27 Ga N5 O9.5'
_chemical_formula_weight         535.166
_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             2025-01-31
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-04 deposited with the CCDC.	2025-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.467(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7590(5)
_cell_length_b                   20.1534(14)
_cell_length_c                   12.8678(6)
_cell_measurement_reflns_used    8637
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.4910
_cell_measurement_theta_min      1.9300
_cell_volume                     2154.5(2)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9923
_diffrn_measured_fraction_theta_max 0.9863
_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  -9.00   0.50   15.00    --  -14.16 122.00 -38.00   94
  2  \w    -56.00  -3.00   0.50   15.00    --  -14.16 -57.00-180.00  106
  3  \w    -92.00 -17.00   0.50   15.00    --  -14.16 -19.00 -90.00  150
  4  \w     21.00  64.00   0.50   15.00    --  -14.16  19.00-150.00   86
  5  \w     21.00  64.00   0.50   15.00    --  -14.16  19.00 120.00   86
  6  \w      6.00  62.00   0.50   15.00    --   17.44  57.00 -60.00  112
  7  \w      6.00  62.00   0.50   15.00    --   17.44  57.00   0.00  112
  8  \w      6.00  62.00   0.50   15.00    --   17.44  57.00  30.00  112
  9  \w      0.00  47.00   0.50   15.00    --   17.44 -99.00-180.00   94
 10  \w     21.00  46.00   0.50   15.00    --  -14.16  19.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0735143000
_diffrn_orient_matrix_UB_12      -0.0063715000
_diffrn_orient_matrix_UB_13      0.0420876000
_diffrn_orient_matrix_UB_21      0.0145443000
_diffrn_orient_matrix_UB_22      0.0345834000
_diffrn_orient_matrix_UB_23      0.0068687000
_diffrn_orient_matrix_UB_31      -0.0409911000
_diffrn_orient_matrix_UB_32      0.0007909000
_diffrn_orient_matrix_UB_33      0.0395020000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.9923
_diffrn_reflns_Laue_measured_fraction_max 0.9863
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20958
_diffrn_reflns_point_group_measured_fraction_full 0.9923
_diffrn_reflns_point_group_measured_fraction_max 0.9863
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75172
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       plate
_exptl_crystal_F_000             1110.005
_exptl_crystal_recrystallization_method
'Vapour diffusion of diethyl ether into a methanol solution containing sample'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.3153
_refine_diff_density_min         -1.3892
_refine_diff_density_rms         0.1540
_refine_ls_d_res_high            0.7401
_refine_ls_d_res_low             10.0767
_refine_ls_goodness_of_fit_ref   1.0413
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     566
_refine_ls_restrained_S_all      0.9868
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+1.2748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -11
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              -7
_reflns_number_gt                3940
_reflns_number_total             5491
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4nj05327c2.cif
_cod_data_source_block           GaL1NO3_reprocessed2
_cod_depositor_comments
'Adding full bibliography for 7063640--7063645.cif.'
_cod_original_formula_sum        'C18 H27 Ga1 N5 O9.5'
_cod_database_code               7063640
_chemical_oxdiff_formula         GaC18H28N7O6
_olex2_refinement_description
;
1. Restrained distances
 N5-O6 = N5-O7 = N5-O8
 1.24 with sigma of 0.02
 N5-O8
 1.24 with sigma of 0.001
 C18-H18
 1.08 with sigma of 0.02
 C1-H1b
 1.08 with sigma of 0.02
 O8-N5 \\sim O6-O7
 with sigma of 0.02
 O6-O7 \\sim O6-O8 \\sim O7-O8
 with sigma of 0.04
 N5-O6 \\sim N5-O7 \\sim N5-O8
 with sigma of 0.02
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_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:   1
   DATE:           2025-01-31_19-29-41
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 60 electrons were 
found in a volume of 188\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[H2O] per Asymmetric Unit 
which account for 60 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 4.229
_oxdiff_exptl_absorpt_empirical_full_min 0.355