Heterometallic trinuclear oxo-centered clusters as single-source precursors for synthesis of stoichiometric monodisperse transition metal ferrite nanocrystals.
Sanchez-Lievanos, Karla R; Tariq, Mehrin; Brennessel, William W.; Knowles, Kathryn E.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16348–16358; doi:10.1039/d0dt01369b

data_7704400
_publ_section_title
;
 Heterometallic trinuclear oxo-centered clusters as single-source
 precursors for synthesis of stoichiometric monodisperse transition metal
 ferrite nanocrystals.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16348
_journal_page_last               16358
_journal_paper_doi               10.1039/d0dt01369b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C12 H6 F18 Fe3 O16, 2.5(O), H2 O'
_chemical_formula_sum            'C12 H13 F18 Fe3 O19.5'
_chemical_formula_weight         978.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-04-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-04-14 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.8530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.7504(3)
_cell_length_b                   10.71550(10)
_cell_length_c                   16.4299(2)
_cell_measurement_reflns_used    17034
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      77.1590
_cell_measurement_theta_min      2.6180
_cell_volume                     5934.55(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.979
_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     60.00 121.00   0.50    0.41    --   49.87  23.00  74.00  122
  2  \w    107.00 156.00   0.50    1.63    --  105.75  30.00 120.00   98
  3  \w     92.00 153.00   0.50    1.63    --  105.75  61.00  90.00  122
  4  \w    101.00 161.00   0.50    1.63    --  105.75  23.00  74.00  120
  5  \w    107.00 133.00   0.50    1.63    --  105.75  15.00   0.00   52
  6  \w     99.00 176.00   0.50    1.63    --  105.75  45.00 -60.00  154
  7  \w    102.00 173.00   0.50    1.63    --  105.75  61.00   0.00  142
  8  \w     95.00 140.00   0.50    1.63    --  105.75 125.00 120.00   90
  9  \w    153.00 178.00   0.50    1.63    --  105.75 125.00 120.00   50
 10  \w    -19.00   6.00   0.50    0.41    --   49.87 -23.00 -91.00   50
 11  \w    -21.00  13.00   0.50    0.41    --   49.87 -19.00  90.00   68
 12  \w    -19.00  11.00   0.50    0.41    --   49.87 -19.00 120.00   60
 13  \w    -21.00   8.00   0.50    0.41    --   49.87 -19.00 150.00   58
 14  \w     53.00  96.00   0.50    1.63    --  105.75 -94.00 120.00   86
 15  \w     34.00 106.00   0.50    1.63    --  105.75 -94.00 150.00  144
 16  \w     40.00  71.00   0.50    1.63    --  105.75 -94.00  90.00   62
 17  \w     55.00  99.00   0.50    1.63    --  105.75 -94.00-150.00   88
 18  \w     39.00  65.00   0.50    1.63    --  105.75 -94.00-180.00   52
 19  \w     36.00  62.00   0.50    1.63    --  105.75 -61.00-180.00   52
 20  \w     37.00  63.00   0.50    1.63    --  105.75 -61.00-150.00   52
 21  \w     51.00  80.00   0.50    1.63    --  105.75 -61.00 -60.00   58
 22  \w     48.00  78.00   0.50    1.63    --  105.75 -61.00   0.00   60
 23  \w     37.00  64.00   0.50    1.63    --  105.75 -61.00 150.00   54
 24  \w     45.00  73.00   0.50    1.63    --  105.75 -61.00  90.00   56
 25  \w     -4.00  24.00   0.50    0.41    --  -49.87  19.00 -60.00   56
 26  \w    -33.00   8.00   0.50    0.41    --  -49.87  38.00-180.00   82
 27  \w     -5.00  20.00   0.50    0.41    --  -49.87  19.00-150.00   50
 28  \w    -12.00  23.00   0.50    0.41    --  -49.87  23.00  74.00   70
 29  \w    -44.00 -19.00   0.50    1.63    --  -84.25  45.00  30.00   50
 30  \w    -41.00 -12.00   0.50    1.63    --  -84.25  45.00-120.00   58
 31  \w    -98.00 -50.00   0.50    0.41    --  -49.87 -23.00 -91.00   96
 32  \w   -141.00-116.00   0.50    1.63    --  -84.25 -23.00 -91.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0432460000
_diffrn_orient_matrix_UB_12      0.0428577000
_diffrn_orient_matrix_UB_13      -0.0070959000
_diffrn_orient_matrix_UB_21      0.0065026000
_diffrn_orient_matrix_UB_22      -0.0065662000
_diffrn_orient_matrix_UB_23      0.0933466000
_diffrn_orient_matrix_UB_31      0.0132380000
_diffrn_orient_matrix_UB_32      -0.1371623000
_diffrn_orient_matrix_UB_33      -0.0066446000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26694
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.792
_diffrn_reflns_theta_min         2.622
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
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    2.191
_exptl_crystal_description       block
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.761
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6218
_refine_ls_number_restraints     590
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+13.2079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5776
_reflns_number_total             6218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01369b2.cif
_cod_data_source_block           knoks16
_cod_depositor_comments
'Adding full bibliography for 7704398--7704402.cif.'
_cod_original_formula_sum        'C12 H13 F18 Fe3 O19.50'
_cod_database_code               7704400
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.321
_shelx_estimated_absorpt_t_min   0.168
_diffrn_oxdiff_digest_frames
;
01c0e8682fc596e2f56ef3b6ce392f3df2000517da8
;
_diffrn_oxdiff_digest_hkl
;
01b6c31fbb17fffa75c514e5eb53b59b8d76d5
;
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C3-C4 \\sim C3-C4'
 with sigma of 0.01
 C4-F4 \\sim C4-F5 \\sim C4-F6 \\sim C4'-F4' \\sim C4'-F5' \\sim C4'-F6'
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4'-F5' \\sim F5'-F6' \\sim F6'-F4'
 with sigma of 0.02
 C7-C8 \\sim C7-C8'
 with sigma of 0.01
 C8-F10 \\sim C8-F11 \\sim C8-F12 \\sim C8'-F11' \\sim C8'-F12' \\sim C8'-F10'
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F11'-F12' \\sim F12'-F10' \\sim
F10'-F11'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
F11 \\sim F12': within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(O17) = Uanis(O17')
Uanis(O18) = Uanis(O18')
Uanis(O19) = Uanis(O19')
4. Rigid body (RIGU) restrains
 F10, F11, F12, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10', F11', F12', C8'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F5, F6, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4', F5', F6', C4'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(C4')=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4)=FVAR(1)
 Sof(F10')=Sof(F11')=Sof(F12')=Sof(C8')=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C8)=FVAR(2)
 Sof(O17')=1-FVAR(3)
 Sof(O17)=FVAR(3)
 Sof(O18')=1-FVAR(4)
 Sof(O18)=FVAR(4)
 Sof(O19')=0.5*(1-FVAR(6))
 Sof(O19)=0.5*FVAR(6)
6.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O20(H20A,H20B)
;
_shelx_res_checksum              79025
_olex2_submission_original_sample_id knoks16
_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 1.735
_oxdiff_exptl_absorpt_empirical_full_min 0.672