The synthesis of a monodisperse quaternary ferrite (FeCoCrO<sub>4</sub>) from the hot injection thermolysis of the single source precursor [CrCoFeO(O<sub>2</sub>C<sup>t</sup>Bu)<sub>6</sub>(HO<sub>2</sub>C<sup>t</sup>Bu)<sub>3</sub>].
Abdulwahab, Khadijat O.; Malik, Mohammad A.; O'Brien, Paul; Vitorica-Yrezabal, Iñigo J; Timco, Grigore A.; Tuna, Floriana; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 376–381; doi:10.1039/c7dt03302h

data_7045008
_publ_section_title
;
 The synthesis of a monodisperse quaternary ferrite (FeCoCrO<sub>4</sub>)
 from the hot injection thermolysis of the single source precursor
 [CrCoFeO(O<sub>2</sub>C<sup>t</sup>Bu)<sub>6</sub>(HO<sub>2</sub>C<sup>t</sup>Bu)<sub>3</sub>].
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              376
_journal_page_last               381
_journal_paper_doi               10.1039/c7dt03302h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C45 H81 Co Cr Fe O19'
_chemical_formula_sum            'C45 H84 Co Cr Fe O19'
_chemical_formula_weight         1095.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2544(14)
_cell_length_b                   20.0328(11)
_cell_length_c                   16.9685(9)
_cell_measurement_reflns_used    4928
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      25.2680
_cell_measurement_theta_min      3.7590
_cell_volume                     6205.2(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_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      240.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -25.00  30.00   1.00   15.00    --  -12.00 -99.00 120.00   55
  2  \w    -30.00  49.00   1.00   15.00    --  -12.00  57.00  60.00   79
  3  \w    -45.00  44.00   1.00   15.00    --  -12.00  77.00 -60.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0057715000
_diffrn_orient_matrix_UB_12      -0.0348072000
_diffrn_orient_matrix_UB_13      0.0044883000
_diffrn_orient_matrix_UB_21      -0.0367125000
_diffrn_orient_matrix_UB_22      -0.0061012000
_diffrn_orient_matrix_UB_23      -0.0116462000
_diffrn_orient_matrix_UB_31      0.0113239000
_diffrn_orient_matrix_UB_32      -0.0021446000
_diffrn_orient_matrix_UB_33      -0.0399055000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17211
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       plate
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         3371
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0676
_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^)+(0.1207P)^2^+10.6540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2439
_reflns_number_total             3371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03302h2.cif
_cod_data_source_block           orepw1950
_cod_depositor_comments          'Adding full bibliography for 7045008.cif.'
_cod_original_cell_volume        6205.1(7)
_cod_database_code               7045008
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Cr7NiCuF20O34N2C80H180
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Cr02, Fe02, Co02}
{Cr01, Fe01, Co01}
3. Restrained distances
 C16-C17
 2.4 with sigma of 0.02
 C30-C27 = C28-C27 = C29-C27
 1.54 with sigma of 0.02
 C29-C30
 2.4 with sigma of 0.002
 C30-C28
 2.4 with sigma of 0.002
 C28-C29
 2.4 with sigma of 0.002
 C11-C9
 2.4 with sigma of 0.02
 C9-C10
 2.4 with sigma of 0.02
 C10-C11
 2.4 with sigma of 0.02
 C17-C15
 1.54 with sigma of 0.02
 C16-C15
 1.54 with sigma of 0.02
 C14_$2-C15
 1.54 with sigma of 0.02
 C8-C6 \\sim C10-C4 \\sim C7-C8 \\sim C9-C4 \\sim C11-C4 \\sim C8-C5 \\sim
C4-C3 \\sim C8-C3
 with sigma of 0.002
 O13_$1-C14_$2 \\sim O13_$2-C14_$2
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C22 \\sim C21 \\sim C20: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C16 \\sim C15 \\sim C17: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C27 \\sim C29 \\sim C30 \\sim C28: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Cr02) = Uanis(Fe02) = Uanis(Co02)
Uanis(Cr01) = Uanis(Fe01) = Uanis(Co01)
5. Rigid body (RIGU) restrains
 C9, C11, C10, C4, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O25, C7, C6, C5, C8, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O25, C24, O23, O26, C29, C27, C30, C28
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O12, C14, O13, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, C20, C21, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C22, C21, C19, O18
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Others
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C8)=1-FVAR(1)
 Sof(C4)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
 Fixed Sof: Co02(0.16667) Co01(0.08333) Fe02(0.16667) Fe01(0.08333)
 Cr02(0.16667) Cr01(0.08333) H21A(0.5) H21B(0.5) H21C(0.5) C14(0.25) C24(0.5)
 C17(0.25) H17A(0.25) H17B(0.25) H17C(0.25) O25(0.25) O13(0.25) O26(0.25)
 C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
 C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
7.a Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C10(H10A,H10B,
 H10C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C30(H30A,H30B,H30C), C29(H29A,
 H29B,H29C), C16(H16A,H16B,H16C), C28(H28A,H28B,H28C), C7(H7A,H7B,H7C), C6(H6A,
 H6B,H6C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              98447
_olex2_date_sample_data_collection 2016-07-20
_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 2.427
_oxdiff_exptl_absorpt_empirical_full_min 0.705