Extraordinary kinetic inertness of lanthanide(iii) complexes of pyridine-rigidified 18-membered hexaazamacrocycles with four acetate pendant arms.
Faltejsek, Jan; Urbanovský, Peter; Kubíček, Vojtěch; Havlíčková, Jana; Císařová, Ivana; Kotek, Jan; Hermann, Petr; Chemical science 16 (2025) 12558–12567; doi:10.1039/d5sc01893e

data_1574757
_publ_section_title
;
 Extraordinary kinetic inertness of lanthanide(iii) complexes of
 pyridine-rigidified 18-membered hexaazamacrocycles with four acetate
 pendant arms.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              12558
_journal_page_last               12567
_journal_paper_doi               10.1039/d5sc01893e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C26 H54 N6 O18 Pr2, 6(Cl), 9(H2 O)'
_chemical_formula_sum            'C26 H72 Cl6 N6 O27 Pr2'
_chemical_formula_weight         1395.41
_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-2017/1
_audit_update_record
;
2025-02-10 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                94.789(2)
_cell_angle_beta                 109.861(2)
_cell_angle_gamma                99.596(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9445(6)
_cell_length_b                   11.2448(5)
_cell_length_c                   13.1854(8)
_cell_measurement_reflns_used    5855
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.4777
_cell_measurement_theta_min      2.2262
_cell_volume                     1351.64(13)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0836
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_min         2.226
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.161
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.87
_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    1.714
_exptl_crystal_description       plate
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.059
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.988
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6196
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0743P)^2^+1.4087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4985
_reflns_number_total             6196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01893e2.cif
_cod_data_source_block           haf12pr_stop_maly
_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 1574757--1574764.cif.
;
_cod_database_code               1574757
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.883
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              16937