Transition metal complexes of cyclam with two 2,2,2-trifluoroethylphosphinate pendant arms as probes for <sup>19</sup>F magnetic resonance imaging.
Koucký, Filip; Kotek, Jan; Císařová, Ivana; Havlíčková, Jana; Kubíček, Vojtěch; Hermann, Petr; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01420g

data_7713402
_publ_section_title
;
 Transition metal complexes of cyclam with two
 2,2,2-trifluoroethylphosphinate pendant arms as probes for <sup>19</sup>F
 magnetic resonance imaging.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01420g
_journal_year                    2023
_chemical_formula_moiety         'C30 H44 F6 N4 O4 P2, 6(C2 H F3 O2), 2(H2 O)'
_chemical_formula_sum            'C42 H54 F24 N4 O18 P2'
_chemical_formula_weight         1420.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.019(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3608(4)
_cell_length_b                   11.3394(4)
_cell_length_c                   21.7985(8)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      77.1933
_cell_measurement_theta_min      3.5758
_cell_volume                     3055.37(18)
_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_molecular_graphics    'shelXle (C.B. Huebschle, rev 1328)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55783
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.604
_diffrn_reflns_theta_min         3.576
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.943
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.76
_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    1.544
_exptl_crystal_description       bar
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         6464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+3.8655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2061
_refine_ls_wR_factor_ref         0.2216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5214
_reflns_number_total             6464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01420g2.cif
_cod_data_source_block           pf2b2cam2tfa2
_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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7713402
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.659
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              92672
_shelx_hkl_checksum              59231