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_7049845
_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         'C15 H11 F3 Fe N3, 3(H2 O)'
_chemical_formula_sum            'C15 H17 F3 Fe N3 O3'
_chemical_formula_weight         400.16
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-03-27
_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                 102.155(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6981(2)
_cell_length_b                   25.5075(5)
_cell_length_c                   7.4413(2)
_cell_measurement_reflns_used    19525
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.0170
_cell_measurement_theta_min      2.3740
_cell_volume                     1613.96(7)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -107.00  20.00   0.50    1.00    --  -17.30 -57.00  90.00  254
  2  \w    -55.00  72.00   0.50    1.00    --  -17.30  57.00  90.00  254
  3  \w   -107.00  23.00   0.50    1.00    --  -17.30 -70.00  60.00  260
  4  \w   -107.00  72.00   0.50    1.00    --  -17.30   0.00  60.00  358
  5  \w    -55.00  72.00   0.50    1.00    --  -17.30  57.00  30.00  254
  6  \w   -107.00  23.00   0.50    1.00    --  -17.30 -70.00 -90.00  260
  7  \w    -58.00  20.00   0.50    1.00    --  -17.30  70.00-120.00  156
  8  \w    -55.00  72.00   0.50    1.00    --  -17.30  57.00-180.00  254
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0799396000
_diffrn_orient_matrix_UB_12      -0.0050763000
_diffrn_orient_matrix_UB_13      -0.0406901000
_diffrn_orient_matrix_UB_21      0.0129525000
_diffrn_orient_matrix_UB_22      -0.0272210000
_diffrn_orient_matrix_UB_23      0.0159386000
_diffrn_orient_matrix_UB_31      -0.0200074000
_diffrn_orient_matrix_UB_32      0.0026021000
_diffrn_orient_matrix_UB_33      0.0871530000
_diffrn_radiation_collimation    'Confocal mirrors, VHF 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  0.0274
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            34245
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.395
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71336
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0206
_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^)+(0.0286P)^2^+0.9964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2971
_reflns_number_total             3177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03696a2.cif
_cod_data_source_block           2018fmmtmfefter
_cod_depositor_comments
'Adding full bibliography for 7049842--7049845.cif.'
_cod_database_code               7049845
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C15H11N3F3Fe
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.930
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O3(H3A,H3B), O2(H2A,H2B), O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C9(H9), C15(H15), C12(H12), C8(H8), C14(H14), C4(H4),
 C1(H1), C3(H3), C2(H2)
;
_shelx_res_checksum              35897
_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 2.029
_oxdiff_exptl_absorpt_empirical_full_min 0.615