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_7719614
_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         'C16 H26 Cd N4 O8, H2 O'
_chemical_formula_sum            'C16 H28 Cd N4 O9'
_chemical_formula_weight         532.82
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'Intrinsic Phasing'
_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                90
_cell_angle_beta                 95.702(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8060(4)
_cell_length_b                   11.3430(5)
_cell_length_c                   25.0311(13)
_cell_measurement_reflns_used    9702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2583
_cell_measurement_theta_min      3.0406
_cell_volume                     1922.85(17)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'Bruker Instrument Service v8.5.5.6'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            PhotonIII_C14
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 180.0; len= 180.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 287.7; len= 232.5; end= 520.2 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg omega=   0.867 deg chi= -24.000 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 301.3; len= 126.5; end= 427.8 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=  28.097 deg phi= 187.118 deg chi=  51.790 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 122.5; end= 127.5 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg phi= 360.000 deg chi= -44.500 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start= 295.7; len= 216.5; end= 512.2 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg omega=   3.974 deg chi= -44.500 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start= 360.0; len= 310.0; end= 670.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg omega= 271.837 deg chi=  24.000 deg] 
measure for 5.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
;
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'flat graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            55773
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_min         1.973
_diffrn_source                   'sealed tube'
_diffrn_source_current           1.599
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.79
_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            colourless
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_recrystallization_method
'Vapour diffusion of acetone into an aqueous solution'
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+1.7872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4681
_reflns_number_total             4759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01880c2.cif
_cod_data_source_block           mo_jo_cddota_2
_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_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7719614
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.790
_shelx_estimated_absorpt_t_max   0.865
_exptl_bruker_absorpt_correction_t_ratio 0.9411
_bruker_diffrn_measurement_temperature_device Cryostream
_diffrn_measurement_bruker_total_exposure_time 10620.0
_diffrn_reflns_bruker_av_norm_i  17146.038
_diffrn_reflns_bruker_number_gt  78200
_computing_bruker_data_scaling   'SADABS-2016/2 - Bruker AXS area detector'
_shelx_res_checksum              34616
_shelx_hkl_checksum              6593