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_7704401
_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 Cu1 F18 Fe2 O16, 2.5(O), H2 O'
_chemical_formula_sum            'C12 H13 Cu F18 Fe2 O19.5'
_chemical_formula_weight         986.46
_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             2020-04-01
_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                 93.306(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.6407(8)
_cell_length_b                   10.6483(3)
_cell_length_c                   16.5280(4)
_cell_measurement_reflns_used    21331
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.3180
_cell_measurement_theta_min      2.6170
_cell_volume                     5910.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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      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 0.998
_diffrn_measured_fraction_theta_max 0.850
_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    -34.00   6.00   0.50    3.52    --  -12.20  83.00 -75.00   80
  2  \w    -59.00   0.00   0.50    3.52    --  -12.20 -38.00 120.00  118
  3  \w    -39.00  21.00   0.50    3.52    --   10.95 -83.00 164.00  120
  4  \w    -42.00 -17.00   0.50    3.52    --  -12.20 -83.00 164.00   50
  5  \w    -19.00  43.00   0.50    3.52    --   10.95 -99.00  60.00  124
  6  \w    -23.00  40.00   0.50    3.52    --   10.95 -99.00 -60.00  126
;
_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      0.0143712000
_diffrn_orient_matrix_UB_12      -0.0418398000
_diffrn_orient_matrix_UB_13      0.0178577000
_diffrn_orient_matrix_UB_21      -0.0154478000
_diffrn_orient_matrix_UB_22      -0.0408195000
_diffrn_orient_matrix_UB_23      0.0110544000
_diffrn_orient_matrix_UB_31      0.0008829000
_diffrn_orient_matrix_UB_32      -0.0320272000
_diffrn_orient_matrix_UB_33      -0.0374890000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32063
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         33.171
_diffrn_reflns_theta_min         2.469
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         9615
_refine_ls_number_restraints     519
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0212P)^2^+27.5714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8563
_reflns_number_total             9615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01369b2.cif
_cod_data_source_block           knoks12mo
_cod_depositor_comments
'Adding full bibliography for 7704398--7704402.cif.'
_cod_original_cell_volume        5910.7(2)
_cod_original_formula_sum        'C12 H13 Cu F18 Fe2 O19.50'
_cod_database_code               7704401
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.570
_diffrn_oxdiff_digest_frames
;
0169c4662de78dfbc0b470ebd54fcc273100027a225
;
_diffrn_oxdiff_digest_hkl
;
01090b1ff4100f1db79b3b52b9387a100181a5
;
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{Fe1, Cu1}
{Fe2, Cu2}
{Fe3, Cu3}
3. 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' \\sim C7-C8" \\sim C7-C8Z
 with sigma of 0.01
 C8-F10 \\sim C8-F11 \\sim C8-F12 \\sim C8'-F11' \\sim C8'-F12' \\sim C8'-F10'
\\sim C8"-F10" \\sim C8"-
 F11" \\sim C8"-F12" \\sim C8Z-F10Z \\sim C8Z-F11Z \\sim C8Z-F12Z
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F11'-F12' \\sim F12'-F10' \\sim
F10'-F11' \\sim F10"-F11" ~
 F11"-F12" \\sim F12"-F10" \\sim F10Z-F11Z \\sim F11Z-F12Z \\sim F12Z-F10Z
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
F12 \\sim F12Z: 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')
Uanis(Fe1) = Uanis(Cu1)
Uanis(Fe2) = Uanis(Cu2)
Uanis(Fe3) = Uanis(Cu3)
5. Rigid body (RIGU) restrains
 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
 C8, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8', F10', F11', F12'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8", F10", F11", F12"
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8Z, F10Z, F11Z, F12Z
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Fe1)+Sof(Cu1)]+1*[Sof(Fe2)+Sof(Cu2)]+1*[Sof(Fe3)+Sof(Cu3)]=2 with esd
 of 0.0001
 1*[Sof(C8)+Sof(F10)+Sof(F11)+Sof(F12)]+1*[Sof(C8')+Sof(F12')+Sof(F10')+
 Sof(F11')]+1*[Sof(C8")+Sof(F10")+Sof(F11")+Sof(F12")]+1*[Sof(C8Z)+Sof(F10Z)+
 Sof(F11Z)+Sof(F12Z)]=1 with esd of 0.0001
 Sof(C4')=Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(1)
 Sof(C4)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(O17')=1-FVAR(2)
 Sof(O17)=FVAR(2)
 Sof(O18')=1-FVAR(3)
 Sof(O18)=FVAR(3)
 Sof(O19')=0.5*(1-FVAR(5))
 Sof(O19)=0.5*FVAR(5)
 Sof(Cu1)=1-FVAR(5)
 Sof(Fe1)=FVAR(5)
 Sof(Cu2)=1-FVAR(6)
 Sof(Fe2)=FVAR(6)
 Sof(Cu3)=1-FVAR(7)
 Sof(Fe3)=FVAR(7)
 Sof(C8)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(8)
 Sof(C8')=Sof(F12')=Sof(F10')=Sof(F11')=FVAR(9)
 Sof(C8")=Sof(F10")=Sof(F11")=Sof(F12")=FVAR(10)
 Sof(C8Z)=Sof(F10Z)=Sof(F11Z)=Sof(F12Z)=FVAR(11)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O20(H20A,H20B)
;
_shelx_res_checksum              19989
_olex2_submission_original_sample_id knoks12mo
_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 1.414
_oxdiff_exptl_absorpt_empirical_full_min 0.817