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_7049844
_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 H25 F3 Fe N3, 2(H2 O)'
_chemical_formula_sum            'C15 H29 F3 Fe N3 O2'
_chemical_formula_weight         396.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-13 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                   9.5216(3)
_cell_length_b                   12.4903(4)
_cell_length_c                   29.8518(9)
_cell_measurement_reflns_used    14028
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.5120
_cell_measurement_theta_min      2.2010
_cell_volume                     3550.20(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_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
_diffrn_detector                 CCD
_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    -84.00  61.00   0.50    5.00    --    5.00 -19.00  60.00  290
  2  \w    -96.00  24.00   0.50    5.00    --   -6.30 -57.00 -90.00  240
  3  \w    -96.00  28.00   0.50    5.00    --   -6.30 -70.00  60.00  248
  4  \w    -96.00  24.00   0.50    5.00    --   -6.30 -57.00-180.00  240
  5  \w    -84.00 -59.00   0.50    5.00    --    5.00 -38.00 -30.00   50
  6  \w    -37.00  83.00   0.50    5.00    --   -6.30  57.00-120.00  240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_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      0.0737634000
_diffrn_orient_matrix_UB_12      -0.0060118000
_diffrn_orient_matrix_UB_13      0.0021905000
_diffrn_orient_matrix_UB_21      0.0101537000
_diffrn_orient_matrix_UB_22      0.0506749000
_diffrn_orient_matrix_UB_23      -0.0102407000
_diffrn_orient_matrix_UB_31      -0.0027735000
_diffrn_orient_matrix_UB_32      0.0249193000
_diffrn_orient_matrix_UB_33      0.0213186000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            74969
_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         25.997
_diffrn_reflns_theta_min         1.767
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 2621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+1.5907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6541
_reflns_number_total             6982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03696a2.cif
_cod_data_source_block           2018fmm8148-39r
_cod_depositor_comments
'Adding full bibliography for 7049842--7049845.cif.'
_cod_database_code               7049844
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C15H27F3N3FeO
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.978
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Free rotating group:
 O4(H4C,H4D), O3(H3C,H3D), O1(H1C,H1D), O2(H2C,H2D)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C23(H23A,H23B), C18(H18A,H18B), C3(H3A,H3B), C8(H8A,H8B), C2(H2A,
 H2B), C20(H20A,H20B), C21(H21A,H21B), C5(H5A,H5B), C16(H16A,H16B), C4(H4A,H4B),
  C1(H1A,H1B), C19(H19A,H19B), C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C28(H28), C14(H14), C12(H12), C27(H27), C11(H11), C26(H26),
 C10(H10), C29(H29), C13(H13)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C7(H7A,H7B,H7C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              75789
_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 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.719