DOTA complexes with divalent zinc, cadmium and mercury: X-ray and solid-state NMR studies and solution isomerism.
Obuch, Jakub; Císařová, Ivana; Brus, Jiří; Hermann, Petr; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16535–16549; doi:10.1039/d5dt01880c

data_7719617
_publ_section_title
;
 DOTA complexes with divalent zinc, cadmium and mercury: X-ray and
 solid-state NMR studies and solution isomerism.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16535
_journal_page_last               16549
_journal_paper_doi               10.1039/d5dt01880c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C32 H58 Ba2 Cd2 N8 O21, 18(H2 O), H1.50 O0.75, 0.5(H O0.50)'
_chemical_formula_sum            'C32 H96 Ba2 Cd2 N8 O40'
_chemical_formula_weight         1732.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-07-30 deposited with the CCDC.	2025-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                107.257(2)
_cell_angle_beta                 106.919(2)
_cell_angle_gamma                108.312(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6753(8)
_cell_length_b                   15.6300(9)
_cell_length_c                   16.8570(10)
_cell_measurement_reflns_used    9382
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      59.99
_cell_measurement_theta_min      5.093
_cell_volume                     3175.1(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            163298
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.011
_diffrn_reflns_theta_min         2.193
_exptl_absorpt_coefficient_mu    1.987
_exptl_absorpt_correction_T_max  0.6850
_exptl_absorpt_correction_T_min  0.6000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.205
_exptl_transmission_factor_max   0.6850
_exptl_transmission_factor_min   0.6000
_refine_diff_density_max         2.244
_refine_diff_density_min         -1.708
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00102(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         18462
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+5.1951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18111
_reflns_number_total             18462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01880c2.cif
_cod_data_source_block           mo_jo_bacddota
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7719614--7719618.cif.
;
_cod_database_code               7719617
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.601
_shelx_estimated_absorpt_t_max   0.686
_shelx_res_checksum              75866
_shelx_hkl_checksum              75505