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_7049842
_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         'C9.01 H21 F3 Mn N3, 4(H2 O)'
_chemical_formula_sum            'C9 H29 F3 Mn N3 O4'
_chemical_formula_weight         355.29
_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
_audit_creation_date             2017-11-27
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.9041(2)
_cell_length_b                   13.2669(3)
_cell_length_c                   26.9700(6)
_cell_measurement_reflns_used    9349
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.0460
_cell_measurement_theta_min      3.1240
_cell_volume                     3185.96(12)
_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_temperature      100.0
_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   -109.00  15.00   1.00   15.00    --  -19.30 -37.00 -30.00  124
  2  \w    -55.00  70.00   1.00   15.00    --  -19.30  57.00  30.00  125
  3  \w    -58.00  70.00   1.00   15.00    --  -19.30  72.00-150.00  128
  4  \w    -58.00 -33.00   1.00   15.00    --  -19.30  72.00  90.00   25
  5  \w   -109.00  19.00   1.00   15.00    --  -19.30 -72.00 150.00  128
;
_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      0.0236169000
_diffrn_orient_matrix_UB_12      -0.0453201000
_diffrn_orient_matrix_UB_13      0.0115545000
_diffrn_orient_matrix_UB_21      0.0716796000
_diffrn_orient_matrix_UB_22      0.0215369000
_diffrn_orient_matrix_UB_23      0.0044619000
_diffrn_orient_matrix_UB_31      -0.0254950000
_diffrn_orient_matrix_UB_32      0.0184547000
_diffrn_orient_matrix_UB_33      0.0232005000
_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  0.0584
_diffrn_reflns_av_unetI/netI     0.0288
_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       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32812
_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         25.996
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74356
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.353
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0236P)^2^+7.1874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3023
_reflns_number_total             3124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03696a2.cif
_cod_data_source_block           fmm_tm52017k
_cod_depositor_comments
'Adding full bibliography for 7049842--7049845.cif.'
_cod_database_code               7049842
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C9H25MnF3N3O2
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.949
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. 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
4. Others
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H4AA)=Sof(H4AB)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(3)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=FVAR(3)
5.a Free rotating group:
 O4(H4C,H4D), O2(H2C,H2D), O3(H3C,H3D), O1(H1C,H1D)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2A,H2B), C4(H4A,H4B), C1(H1A,H1B), C3(H3A,H3B), C6(H6A,H6B),
 C6A(H6AA,H6AB), C1A(H1AA,H1AB), C2A(H2AA,H2AB), C4A(H4AA,H4AB), C3A(H3AA,H3AB),
  C5A(H5AA,H5AB)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              9683
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.777