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_7704399
_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 Fe2 Ni1 O16, 4(C3 H6 O), H2 O'
_chemical_formula_sum            'C24 H32 F18 Fe2 Ni O21'
_chemical_formula_weight         1168.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-04-23
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2020-04-23 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                92.6340(10)
_cell_angle_beta                 97.2410(10)
_cell_angle_gamma                111.9130(10)
_cell_formula_units_Z            2
_cell_length_a                   10.56550(10)
_cell_length_b                   11.5802(2)
_cell_length_c                   19.90320(10)
_cell_measurement_reflns_used    18978
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1320
_cell_measurement_theta_min      4.5140
_cell_volume                     2229.74(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_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    -22.00   4.00   0.50    0.14    --  -49.75  38.00  90.00   52
  2  \w    -31.00  21.00   0.50    0.14    --  -49.75  38.00  30.00  104
  3  \w    -46.00 -21.00   0.50    0.57    --  -84.25  96.00 -95.00   50
  4  \w    -72.00   8.00   0.50    0.14    --  -49.75  96.00 -95.00  160
  5  \w     -5.00  58.00   0.50    0.14    --   49.75 -96.00 155.00  126
  6  \w     43.00  71.00   0.50    0.57    --  105.75 -96.00 155.00   56
  7  \w     88.00 114.00   0.50    0.57    --  105.75 -77.00 150.00   52
  8  \w     72.00 106.00   0.50    0.57    --  105.75 -94.00  90.00   68
  9  \w     65.00 104.00   0.50    0.57    --  105.75 -94.00  60.00   78
 10  \w     76.00 106.00   0.50    0.57    --  105.75 -94.00   0.00   60
 11  \w     59.00 106.00   0.50    0.57    --  105.75 -94.00 -90.00   94
 12  \w     81.00 106.00   0.50    0.57    --  105.75 -94.00-150.00   50
 13  \w     38.00  94.00   0.50    0.57    --  105.75 -77.00 -90.00  112
 14  \w     41.00  72.00   0.50    0.57    --  105.75 -61.00 -90.00   62
 15  \w     46.00  76.00   0.50    0.57    --  105.75 -94.00-150.00   60
 16  \w     47.00  79.00   0.50    0.57    --  105.75 -61.00-150.00   64
 17  \w    103.00 175.00   0.50    0.57    --  105.75  15.00-120.00  144
 18  \w    106.00 167.00   0.50    0.57    --  105.75  96.00 -95.00  122
 19  \w    124.00 166.00   0.50    0.57    --  105.75  15.00  30.00   84
 20  \w    153.00 178.00   0.50    0.57    --  105.75  30.00 120.00   50
 21  \w    105.00 141.00   0.50    0.57    --  105.75  30.00 120.00   72
 22  \w    102.00 174.00   0.50    0.57    --  105.75  15.00   0.00  144
 23  \w     92.00 121.00   0.50    0.57    --  105.75  61.00-150.00   58
 24  \w     96.00 147.00   0.50    0.57    --  105.75  61.00-120.00  102
 25  \w    115.00 143.00   0.50    0.57    --  105.75  15.00-180.00   56
 26  \w     99.00 175.00   0.50    0.57    --  105.75  45.00-180.00  152
 27  \w    105.00 173.00   0.50    0.57    --  105.75  15.00 -90.00  136
 28  \w    101.00 126.00   0.50    0.57    --  105.75  15.00 -30.00   50
 29  \w     43.00  69.00   0.50    0.57    --  105.75 -61.00 -30.00   52
 30  \w     47.00 105.00   0.50    0.57    --  105.75 -94.00 -30.00  116
 31  \w     52.00 111.00   0.50    0.57    --  105.75-125.00  30.00  118
 32  \w     44.00  73.00   0.50    0.57    --  105.75-125.00 120.00   58
 33  \w     47.00 109.00   0.50    0.57    --  105.75-125.00 150.00  124
 34  \w     69.00 107.00   0.50    0.57    --  105.75-104.00 174.71   76
 35  \w     35.00  61.00   0.50    0.57    --  105.75 -77.00 150.00   52
 36  \w     43.00  88.00   0.50    0.57    --  105.75-125.00  90.00   90
 37  \w     34.00 104.00   0.50    0.57    --  105.75 -94.00  30.00  140
 38  \w     34.00  71.00   0.50    0.57    --  105.75 -61.00  60.00   74
 39  \w     35.00  60.00   0.50    0.57    --  105.75 -94.00   0.00   50
 40  \w     34.00  68.00   0.50    0.57    --  105.75 -61.00  30.00   68
 41  \w    -22.00   3.00   0.50    0.14    --   49.75 -19.00 150.00   50
 42  \w    -20.00  13.00   0.50    0.14    --   49.75 -19.00  60.00   66
 43  \w     -3.00  22.00   0.50    0.14    --  -49.75  19.00-150.00   50
 44  \w    -21.00  59.00   0.50    0.14    --   49.75 -57.00-180.00  160
 45  \w     34.00  76.00   0.50    0.57    --  105.75 -61.00-180.00   84
 46  \w     41.00 106.00   0.50    0.57    --  105.75 -94.00-180.00  130
 47  \w     45.00  82.00   0.50    0.57    --  105.75-125.00-180.00   74
 48  \w    -21.00  42.00   0.50    0.14    --   49.75 -38.00-150.00  126
 49  \w   -113.00 -80.00   0.50    0.14    --  -49.75-125.00 -60.00   66
 50  \w   -153.00-116.00   0.50    0.57    --  -84.25 -45.00   0.00   74
 51  \w   -124.00 -90.00   0.50    0.57    --  -84.25 -96.00 155.00   68
;
_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      0.0968565000
_diffrn_orient_matrix_UB_12      0.0805487000
_diffrn_orient_matrix_UB_13      0.0636276000
_diffrn_orient_matrix_UB_21      -0.1255337000
_diffrn_orient_matrix_UB_22      -0.0197708000
_diffrn_orient_matrix_UB_23      0.0365695000
_diffrn_orient_matrix_UB_31      0.0128525000
_diffrn_orient_matrix_UB_32      -0.1178767000
_diffrn_orient_matrix_UB_33      0.0276566000
_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  0.0731
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37017
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.059
_diffrn_reflns_theta_min         4.136
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.614
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         9354
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0980P)^2^+0.6801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8318
_reflns_number_total             9354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01369b2.cif
_cod_data_source_block           knoks17
_cod_depositor_comments
'Adding full bibliography for 7704398--7704402.cif.'
_cod_database_code               7704399
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.166
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{Ni1, Fe1}
{Ni2, Fe2}
{Ni3, Fe3}
3. Restrained distances
 C1-C2 \\sim C1-C2'
 with sigma of 0.01
 C2-F1 \\sim C2-F2 \\sim C2-F3 \\sim C2'-F1' \\sim C2'-F2' \\sim C2'-F3'
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1'-F2' \\sim F2'-F3' \\sim F3'-F1'
 with sigma of 0.02
 C19-O19 \\sim C19'-O19' \\sim C22-O21 \\sim C22'-O21'
 with sigma of 0.01
 C19-C20 \\sim C19-C21 \\sim C19'-C20' \\sim C19'-C21' \\sim C22-C23 \\sim
C22-C24 \\sim C22'-C23' ~
 C22'-C24'
 with sigma of 0.01
 O19-C20 \\sim O19-C21 \\sim O19'-C20' \\sim O19'-C21' \\sim O21-C23 \\sim
O21-C24 \\sim O21'-C23' ~
 O21'-C24'
 with sigma of 0.02
 C20-C21 \\sim C20'-C21' \\sim C23-C24 \\sim C23'-C24'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1A
Uanis(Ni1) = Uanis(Fe1)
Uanis(Ni2) = Uanis(Fe2)
Uanis(Ni3) = Uanis(Fe3)
5. Rigid body (RIGU) restrains
 F1, F2, F3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1', F2', F3', C2'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19, C19, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19', C19', C20', C21'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21', C22', C23', C24'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Ni1)+Sof(Fe1)]+1*[Sof(Ni2)+Sof(Fe2)]+1*[Sof(Ni3)+Sof(Fe3)]=2 with esd
 of 0.0001
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(C2')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C2)=FVAR(1)
 Sof(O19')=Sof(C19')=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21')=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(O20')=Sof(H20I)=Sof(H20J)=Sof(O21')=
 Sof(C22')=Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24')=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(O19)=Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(O20)=Sof(H20G)=Sof(H20H)=Sof(O21)=Sof(C22)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Sof(Ni1)=1-FVAR(3)
 Sof(Fe1)=FVAR(3)
 Sof(Ni2)=1-FVAR(4)
 Sof(Fe2)=FVAR(4)
 Sof(Ni3)=1-FVAR(5)
 Sof(Fe3)=FVAR(5)
7.a Riding coordinates:
 O1(H1A,H1B), O20(H20G,H20H), O20'(H20I,H20J)
7.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C20'(H20D,H20E,H20F),
 C21'(H21D,H21E,H21F), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C23'(H23D,H23E,
 H23F), C24'(H24D,H24E,H24F)
;
_shelx_res_checksum              33823
_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 2.728
_oxdiff_exptl_absorpt_empirical_full_min 0.401