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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/7/71/55/7715524.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_7715524
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
'2(C15 H24 F9 Mn N3 O6 P3), H12 Mn O6, 18(H2 O)'
_chemical_formula_sum            'C30 H96 F18 Mn3 N6 O36 P6'
_chemical_formula_weight         1809.76
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.3178(3)
_cell_length_b                   17.3178(3)
_cell_length_c                   21.8650(7)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4647
_cell_measurement_theta_min      2.8717
_cell_volume                     5678.9(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12613
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         2.305
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.75
_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    1.588
_exptl_crystal_description       prism
_exptl_crystal_F_000             2799
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0340
_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)+(0.0703P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2770
_reflns_number_total             2890
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00507d2.cif
_cod_data_source_block           mnnotpf3
_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_cell_volume        5678.9(3)
_cod_database_code               7715524
_shelx_shelxl_version_number     2017/1
_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   0.718
_shelx_estimated_absorpt_t_max   0.887
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Mn1 Mn 0.666667 0.333333 0.56245(2) 0.01450(15) Uani 1 3 d S T P . .
N1 N 0.73576(12) 0.44343(13) 0.63714(8) 0.0165(4) Uani 1 1 d . . . . .
C2 C 0.80459(16) 0.42505(15) 0.66261(10) 0.0193(5) Uani 1 1 d . . . . .
H21 H 0.834657 0.465887 0.697349 0.023 Uiso 1 1 calc R U . . .
H22 H 0.850090 0.437539 0.630823 0.023 Uiso 1 1 calc R U . . .
C3 C 0.76586(16) 0.32903(16) 0.68445(10) 0.0203(5) Uani 1 1 d . . . . .
H31 H 0.815147 0.317806 0.694442 0.024 Uiso 1 1 calc R U . . .
H32 H 0.730772 0.320192 0.722173 0.024 Uiso 1 1 calc R U . . .
C4 C 0.77905(16) 0.53201(15) 0.60655(10) 0.0192(5) Uani 1 1 d . . . . .
H41 H 0.825099 0.577209 0.633822 0.023 Uiso 1 1 calc R U . . .
H42 H 0.733996 0.549953 0.598299 0.023 Uiso 1 1 calc R U . . .
P1 P 0.83064(4) 0.52717(4) 0.53439(3) 0.01723(15) Uani 1 1 d . . . . .
O11 O 0.77217(12) 0.43308(11) 0.51031(7) 0.0228(4) Uani 1 1 d . . . . .
O12 O 0.92688(12) 0.55521(14) 0.54262(8) 0.0282(4) Uani 1 1 d . . . . .
C5 C 0.81774(17) 0.60024(18) 0.48071(11) 0.0257(5) Uani 1 1 d . . . . .
H51 H 0.824350 0.583116 0.438664 0.031 Uiso 1 1 calc R U . . .
H52 H 0.756461 0.590291 0.484555 0.031 Uiso 1 1 calc R U . . .
C6 C 0.8821(2) 0.6973(2) 0.48908(14) 0.0355(6) Uani 1 1 d . . . . .
F61 F 0.88480(17) 0.72315(12) 0.54751(9) 0.0506(6) Uani 1 1 d . . . . .
F62 F 0.96511(14) 0.72002(13) 0.47258(11) 0.0541(6) Uani 1 1 d . . . . .
F63 F 0.85997(17) 0.74801(14) 0.45547(9) 0.0552(6) Uani 1 1 d . . . . .
Mn2 Mn 0.666667 0.333333 0.333333 0.01484(18) Uani 1 6 d S T P . .
O1W O 0.78380(12) 0.38574(15) 0.39148(8) 0.0267(4) Uani 1 1 d . . . . .
H11W H 0.784(2) 0.401(3) 0.4235(16) 0.031(9) Uiso 1 1 d . . . . .
H12W H 0.836(2) 0.392(2) 0.3838(15) 0.031(8) Uiso 1 1 d . . . . .
O2W O 0.94787(13) 0.40324(14) 0.36461(10) 0.0294(4) Uani 1 1 d . . . . .
H21W H 0.984(3) 0.408(3) 0.3946(18) 0.047(11) Uiso 1 1 d . . . . .
H22W H 0.946(3) 0.362(4) 0.342(2) 0.075(16) Uiso 1 1 d . . . . .
O3W O 1.06989(13) 0.61616(13) 0.46719(10) 0.0300(4) Uani 1 1 d . . . . .
H31W H 1.031(2) 0.600(2) 0.4937(14) 0.058(13) Uiso 1 1 d . . . . .
H32W H 1.100720 0.588838 0.469560 0.069 Uiso 1 1 d R U . . .
O4W O 0.91908(17) 0.24848(16) 0.31792(11) 0.0400(5) Uani 1 1 d . . . . .
H41W H 0.927654 0.251507 0.275647 0.048 Uiso 1 1 d R U . . .
H42W H 0.858(4) 0.206(4) 0.325(2) 0.075(15) Uiso 1 1 d . . . . .
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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
O11 Mn1 O11 93.64(6) 2_655 . ?
O11 Mn1 O11 93.64(6) 2_655 3_665 ?
O11 Mn1 O11 93.64(6) . 3_665 ?
O11 Mn1 N1 150.07(7) 2_655 3_665 ?
O11 Mn1 N1 115.85(7) . 3_665 ?
O11 Mn1 N1 80.16(6) 3_665 3_665 ?
O11 Mn1 N1 80.17(6) 2_655 2_655 ?
O11 Mn1 N1 150.07(7) . 2_655 ?
O11 Mn1 N1 115.85(7) 3_665 2_655 ?
N1 Mn1 N1 76.49(7) 3_665 2_655 ?
O11 Mn1 N1 115.85(7) 2_655 . ?
O11 Mn1 N1 80.17(6) . . ?
O11 Mn1 N1 150.07(7) 3_665 . ?
N1 Mn1 N1 76.48(7) 3_665 . ?
N1 Mn1 N1 76.49(7) 2_655 . ?
C2 N1 C4 110.16(18) . . ?
C2 N1 C3 112.19(17) . 2_655 ?
C4 N1 C3 111.32(18) . 2_655 ?
C2 N1 Mn1 103.03(13) . . ?
C4 N1 Mn1 108.41(12) . . ?
C3 N1 Mn1 111.38(14) 2_655 . ?
N1 C2 C3 112.82(19) . . ?
N1 C2 H21 109.0 . . ?
C3 C2 H21 109.0 . . ?
N1 C2 H22 109.0 . . ?
C3 C2 H22 109.0 . . ?
H21 C2 H22 107.8 . . ?
N1 C3 C2 111.55(17) 3_665 . ?
N1 C3 H31 109.3 3_665 . ?
C2 C3 H31 109.3 . . ?
N1 C3 H32 109.3 3_665 . ?
C2 C3 H32 109.3 . . ?
H31 C3 H32 108.0 . . ?
N1 C4 P1 110.19(14) . . ?
N1 C4 H41 109.6 . . ?
P1 C4 H41 109.6 . . ?
N1 C4 H42 109.6 . . ?
P1 C4 H42 109.6 . . ?
H41 C4 H42 108.1 . . ?
O12 P1 O11 115.28(12) . . ?
O12 P1 C5 110.87(12) . . ?
O11 P1 C5 105.94(12) . . ?
O12 P1 C4 111.75(11) . . ?
O11 P1 C4 105.56(10) . . ?
C5 P1 C4 106.90(11) . . ?
P1 O11 Mn1 122.01(9) . . ?
C6 C5 P1 114.94(19) . . ?
C6 C5 H51 108.5 . . ?
P1 C5 H51 108.5 . . ?
C6 C5 H52 108.5 . . ?
P1 C5 H52 108.5 . . ?
H51 C5 H52 107.5 . . ?
F62 C6 F63 106.1(2) . . ?
F62 C6 F61 107.8(3) . . ?
F63 C6 F61 106.0(2) . . ?
F62 C6 C5 112.8(3) . . ?
F63 C6 C5 111.9(3) . . ?
F61 C6 C5 111.9(2) . . ?
O1W Mn2 O1W 180.0 . 16_655 ?
O1W Mn2 O1W 89.18(7) . 3_665 ?
O1W Mn2 O1W 90.82(7) 16_655 3_665 ?
O1W Mn2 O1W 90.82(7) . 18_545 ?
O1W Mn2 O1W 89.18(7) 16_655 18_545 ?
O1W Mn2 O1W 180.0 3_665 18_545 ?
O1W Mn2 O1W 89.18(7) . 2_655 ?
O1W Mn2 O1W 90.82(7) 16_655 2_655 ?
O1W Mn2 O1W 89.18(7) 3_665 2_655 ?
O1W Mn2 O1W 90.82(7) 18_545 2_655 ?
O1W Mn2 O1W 90.82(7) . 17 ?
O1W Mn2 O1W 89.18(7) 16_655 17 ?
O1W Mn2 O1W 90.82(7) 3_665 17 ?
O1W Mn2 O1W 89.18(7) 18_545 17 ?
O1W Mn2 O1W 180.00(7) 2_655 17 ?
Mn2 O1W H11W 123(3) . . ?
Mn2 O1W H12W 129(2) . . ?
H11W O1W H12W 108(3) . . ?
H21W O2W H22W 104(4) . . ?
H31W O3W H32W 112.6 . . ?
H41W O4W H42W 106.8 . . ?
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
Mn1 O11 2.1131(16) 2_655 ?
Mn1 O11 2.1132(17) . ?
Mn1 O11 2.1132(16) 3_665 ?
Mn1 N1 2.3351(18) 3_665 ?
Mn1 N1 2.3351(18) 2_655 ?
Mn1 N1 2.3351(18) . ?
N1 C2 1.487(3) . ?
N1 C4 1.488(3) . ?
N1 C3 1.488(3) 2_655 ?
C2 C3 1.526(3) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
C4 P1 1.836(2) . ?
C4 H41 0.9900 . ?
C4 H42 0.9900 . ?
P1 O12 1.4955(18) . ?
P1 O11 1.5190(17) . ?
P1 C5 1.820(3) . ?
C5 C6 1.492(4) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 F62 1.336(4) . ?
C6 F63 1.340(4) . ?
C6 F61 1.347(4) . ?
Mn2 O1W 2.1712(17) . ?
Mn2 O1W 2.1712(17) 16_655 ?
Mn2 O1W 2.1712(17) 3_665 ?
Mn2 O1W 2.1712(17) 18_545 ?
Mn2 O1W 2.1712(17) 2_655 ?
Mn2 O1W 2.1713(17) 17 ?
O1W H11W 0.75(4) . ?
O1W H12W 0.87(4) . ?
O2W H21W 0.88(4) . ?
O2W H22W 0.86(5) . ?
O3W H31W 0.82(3) . ?
O3W H32W 0.8742 . ?
O4W H41W 0.9335 . ?
O4W H42W 0.96(5) . ?
