Exploring transition metal fluoride chelates - synthesis, properties and prospects towards potential PET probes.
Blower, Philip J.; Levason, William; Luthra, Sajinder K.; McRobbie, Graeme; Monzittu, Francesco M.; Mules, Thomas O.; Reid, Gillian; Subhan, M. Nadeem; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6767–6776; doi:10.1039/c8dt03696a

data_7049843
_publ_section_title
;
 Exploring transition metal fluoride chelates - synthesis, properties and
 prospects towards potential PET probes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6767
_journal_page_last               6776
_journal_paper_doi               10.1039/c8dt03696a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C9 H20.75 Co F3 N3, 4(H2 O)'
_chemical_formula_sum            'C9 H28.75 Co F3 N3 O4'
_chemical_formula_weight         359.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-03 deposited with the CCDC.    2019-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.74923(7)
_cell_length_b                   13.14407(11)
_cell_length_c                   26.2569(3)
_cell_measurement_reflns_used    19978
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.4960
_cell_measurement_theta_min      3.1820
_cell_volume                     3019.56(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -54.00  70.00   0.50   10.00    --  -19.10  57.00  30.00  248
  2  \w   -108.00  16.00   0.50   10.00    --  -19.10 -57.00 -90.00  248
  3  \w   -108.00  14.00   0.50   10.00    --  -19.10 -38.00  30.00  244
  4  \w    -52.00  70.00   0.50   10.00    --  -19.10  38.00   0.00  244
  5  \w    -57.00 -30.00   0.50   10.00    --  -19.10  72.00 150.00   54
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0254037000
_diffrn_orient_matrix_UB_12      0.0169204000
_diffrn_orient_matrix_UB_13      0.0242176000
_diffrn_orient_matrix_UB_21      0.0757053000
_diffrn_orient_matrix_UB_22      -0.0148367000
_diffrn_orient_matrix_UB_23      -0.0062054000
_diffrn_orient_matrix_UB_31      0.0141540000
_diffrn_orient_matrix_UB_32      0.0490276000
_diffrn_orient_matrix_UB_33      -0.0102332000
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0104
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30727
_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         25.998
_diffrn_reflns_theta_min         2.902
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear purple'
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       block
_exptl_crystal_F_000             1518
_exptl_crystal_recrystallization_method MiTegen
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.380
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2973
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.328
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0333P)^2^+12.0373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2971
_reflns_number_total             2973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03696a2.cif
_cod_data_source_block           2017fmm-8148-32k
_cod_depositor_comments
'Adding full bibliography for 7049842--7049845.cif.'
_cod_original_cell_volume        3019.55(5)
_cod_database_code               7049843
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.932
_reflns_odcompleteness_completeness 97.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C11A)=Sof(H11A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=1-FVAR(3)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=FVAR(3)
4.a Free rotating group:
 O1(H1C,H1D), O2(H2C,H2D), O3(H3C,H3D), O4(H4C,H4D)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B), C1(H1A,H1B),
 C9A(H9AA,H9AB), C15A(H15A,H15B), C8A(H8AA,H8AB), C14A(H14A,H14B), C13A(H13A,
 H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C11A(H11A)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              82122
_olex2_exptl_crystal_mounting_method MiTegen
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.447
_oxdiff_exptl_absorpt_empirical_full_min 0.785