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#$Date: 2024-07-05 19:05:07 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293023 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/55/7715527.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715527
loop_
_publ_author_name
'Koucký, Filip'
'Dobrovolná, Tereza'
'Kotek, Jan'
'Císařová, Ivana'
'Havlíčková, Jana'
'Liška, Alan'
'Kubíček, Vojtěch'
'Hermann, Petr'
_publ_section_title
;
 Transition metal complexes of the (2,2,2-trifluoroethyl)phosphinate NOTA
 analogue as potential contrast agents for ¹⁹F magnetic
 resonance imaging.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9267
_journal_page_last               9285
_journal_paper_doi               10.1039/d4dt00507d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C9 H9 F3 O3 S'
_chemical_formula_sum            'C9 H9 F3 O3 S'
_chemical_formula_weight         254.22
_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
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.944(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2859(4)
_cell_length_b                   11.5440(6)
_cell_length_c                   11.0029(5)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4906
_cell_measurement_theta_min      2.4639
_cell_volume                     1049.96(9)
_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-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 0.999
_diffrn_measurement_device       'Bruker D8 VENTURE'
_diffrn_measurement_device_type  'κ-geometry diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25026
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         2.464
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.92
_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    1.608
_exptl_crystal_description       prism
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0281
_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/[σ²(Fo²)+(0.0324P)²+0.5803P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2356
_reflns_number_total             2412
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00507d2.cif
_cod_data_source_block           cf3ch2ots
_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 7715524--7715535.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7715527
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.955
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.72410(3) 0.18280(3) 0.63996(3) 0.01673(10) Uani 1 1 d . . . . .
O1 O 0.72948(11) 0.32096(8) 0.65425(8) 0.01920(19) Uani 1 1 d . . . . .
O2 O 0.85940(11) 0.14878(8) 0.57487(9) 0.0230(2) Uani 1 1 d . . . . .
O3 O 0.70769(12) 0.14368(9) 0.76112(8) 0.0243(2) Uani 1 1 d . . . . .
C1 C 0.76786(17) 0.38408(11) 0.54744(12) 0.0231(3) Uani 1 1 d . . . . .
H11 H 0.6919 0.3632 0.4775 0.028 Uiso 1 1 calc R U . . .
H12 H 0.8793 0.3659 0.5263 0.028 Uiso 1 1 calc R U . . .
C2 C 0.75308(17) 0.51027(12) 0.57677(13) 0.0258(3) Uani 1 1 d . . . . .
F1 F 0.60504(11) 0.53934(9) 0.60611(9) 0.0389(2) Uani 1 1 d . . . . .
F2 F 0.85340(12) 0.54406(8) 0.66951(10) 0.0427(3) Uani 1 1 d . . . . .
F3 F 0.78620(15) 0.57263(8) 0.47965(10) 0.0490(3) Uani 1 1 d . . . . .
C3 C 0.54543(14) 0.15926(10) 0.54934(11) 0.0159(2) Uani 1 1 d . . . . .
C4 C 0.39863(15) 0.16319(11) 0.60375(11) 0.0189(2) Uani 1 1 d . . . . .
H41 H 0.3960 0.1736 0.6892 0.023 Uiso 1 1 calc R U . . .
C5 C 0.25667(15) 0.15157(11) 0.53079(12) 0.0212(3) Uani 1 1 d . . . . .
H51 H 0.1558 0.1538 0.5669 0.025 Uiso 1 1 calc R U . . .
C6 C 0.25933(15) 0.13663(11) 0.40497(12) 0.0205(3) Uani 1 1 d . . . . .
C7 C 0.40814(16) 0.12918(11) 0.35399(11) 0.0201(3) Uani 1 1 d . . . . .
H71 H 0.4112 0.1157 0.2690 0.024 Uiso 1 1 calc R U . . .
C8 C 0.55220(15) 0.14106(11) 0.42515(11) 0.0180(2) Uani 1 1 d . . . . .
H81 H 0.6533 0.1368 0.3895 0.022 Uiso 1 1 calc R U . . .
C9 C 0.10411(19) 0.12942(15) 0.32626(16) 0.0297(3) Uani 1 1 d . . . . .
H91 H 0.092(6) 0.199(4) 0.283(5) 0.032(15) Uiso 0.50(9) 1 d . . P A 1
H92 H 0.021(6) 0.116(5) 0.365(4) 0.034(14) Uiso 0.50(9) 1 d . . P A 1
H93 H 0.110(5) 0.065(5) 0.266(4) 0.031(14) Uiso 0.50(9) 1 d . . P A 1
H94 H 0.125(6) 0.116(6) 0.248(5) 0.051(16) Uiso 0.50(9) 1 d . . P A 2
H95 H 0.035(6) 0.204(4) 0.332(4) 0.028(15) Uiso 0.50(9) 1 d . . P A 2
H96 H 0.032(6) 0.071(5) 0.363(4) 0.035(15) Uiso 0.50(9) 1 d . . P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 S1 O2 120.80(6) . . ?
O3 S1 O1 103.17(5) . . ?
O2 S1 O1 107.80(5) . . ?
O3 S1 C3 110.69(6) . . ?
O2 S1 C3 109.56(6) . . ?
O1 S1 C3 103.14(5) . . ?
C1 O1 S1 115.50(8) . . ?
O1 C1 C2 106.91(10) . . ?
O1 C1 H11 110.3 . . ?
C2 C1 H11 110.3 . . ?
O1 C1 H12 110.3 . . ?
C2 C1 H12 110.3 . . ?
H11 C1 H12 108.6 . . ?
F2 C2 F3 107.74(12) . . ?
F2 C2 F1 106.11(12) . . ?
F3 C2 F1 107.58(12) . . ?
F2 C2 C1 113.22(12) . . ?
F3 C2 C1 109.15(12) . . ?
F1 C2 C1 112.77(12) . . ?
C8 C3 C4 121.59(11) . . ?
C8 C3 S1 119.68(9) . . ?
C4 C3 S1 118.69(9) . . ?
C5 C4 C3 118.69(11) . . ?
C5 C4 H41 120.7 . . ?
C3 C4 H41 120.7 . . ?
C4 C5 C6 121.06(11) . . ?
C4 C5 H51 119.5 . . ?
C6 C5 H51 119.5 . . ?
C7 C6 C5 118.81(11) . . ?
C7 C6 C9 120.74(13) . . ?
C5 C6 C9 120.45(13) . . ?
C8 C7 C6 121.17(11) . . ?
C8 C7 H71 119.4 . . ?
C6 C7 H71 119.4 . . ?
C3 C8 C7 118.61(11) . . ?
C3 C8 H81 120.7 . . ?
C7 C8 H81 120.7 . . ?
C6 C9 H91 108(2) . . ?
C6 C9 H92 114(3) . . ?
H91 C9 H92 110(4) . . ?
C6 C9 H93 110(2) . . ?
H91 C9 H93 108(3) . . ?
H92 C9 H93 106(4) . . ?
C6 C9 H94 110(3) . . ?
C6 C9 H95 112(2) . . ?
H94 C9 H95 110(4) . . ?
C6 C9 H96 108(3) . . ?
H94 C9 H96 115(4) . . ?
H95 C9 H96 101(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.4228(9) . ?
S1 O2 1.4264(9) . ?
S1 O1 1.6029(9) . ?
S1 C3 1.7483(12) . ?
O1 C1 1.4369(15) . ?
C1 C2 1.4989(19) . ?
C1 H11 0.9900 . ?
C1 H12 0.9900 . ?
C2 F2 1.3295(16) . ?
C2 F3 1.3325(17) . ?
C2 F1 1.3326(17) . ?
C3 C8 1.3875(16) . ?
C3 C4 1.3929(16) . ?
C4 C5 1.3843(18) . ?
C4 H41 0.9500 . ?
C5 C6 1.3967(18) . ?
C5 H51 0.9500 . ?
C6 C7 1.3920(18) . ?
C6 C9 1.5026(18) . ?
C7 C8 1.3886(17) . ?
C7 H71 0.9500 . ?
C8 H81 0.9500 . ?
C9 H91 0.93(5) . ?
C9 H92 0.85(5) . ?
C9 H93 1.01(5) . ?
C9 H94 0.90(6) . ?
C9 H95 1.04(5) . ?
C9 H96 1.01(5) . ?
