Popcorn-Shaped Fe <sub> <i>x</i> </sub> O (Wüstite) Nanoparticles from a Single-Source Precursor: Colloidal Synthesis and Magnetic Properties.
Guntlin, Christoph P.; Ochsenbein, Stefan T.; Wörle, Michael; Erni, Rolf; Kravchyk, Kostiantyn V.; Kovalenko, Maksym V.; Chemistry of materials : a publication of the American Chemical Society 30 (2018) 1249–1256; doi:10.1021/acs.chemmater.7b04382

data_4003120
_publ_section_title
;
 Popcorn-Shaped Fe <sub> <i>x</i> </sub> O (W\"ustite) Nanoparticles from
 a Single-Source Precursor: Colloidal Synthesis and Magnetic Properties.
;
_journal_issue                   4
_journal_name_full
'Chemistry of materials : a publication of the American Chemical Society'
_journal_page_first              1249
_journal_page_last               1256
_journal_paper_doi               10.1021/acs.chemmater.7b04382
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'C12 H6 F18 Fe3 O16, Cl4 Fe'
_chemical_formula_sum            'C12 H6 Cl4 F18 Fe4 O16'
_chemical_formula_weight         1113.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.9420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5360(7)
_cell_length_b                   15.0772(7)
_cell_length_c                   17.4768(8)
_cell_measurement_reflns_used    7864
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.201
_cell_measurement_theta_min      2.479
_cell_volume                     3352.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52179
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.364
_diffrn_reflns_theta_min         1.600
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.179
_exptl_absorpt_correction_T_max  0.7565
_exptl_absorpt_correction_T_min  0.6768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0791 before and 0.0568 after correction. The Ratio of minimum to maximum transmission is 0.8946. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2160
_exptl_crystal_preparation
'FeCL3 + TFA, reflux, add water after 2h, then 60 degree, 24h'
_exptl_crystal_recrystallization_method
'Dissolve powder in TFA, heat to 50 degree, slowly cool down, 1 day'
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         8306
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0460P)^2^+1.4332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6681
_reflns_number_total             8306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b04382_si_004.cif
_cod_data_source_block           fe3o_26_0m
_cod_database_code               4003120
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C4-C3 \\sim C4A-C3 \\sim C4AA-C3
 with sigma of 0.001
 F5A-F6A \\sim F5A-F4A \\sim F4A-F6A \\sim F6-F5 \\sim F6-F4 \\sim F4-F5 \\sim
F6AA-F5AA \\sim F6AA-F4AA ~
 F4AA-F5AA
 with sigma of 0.001
 C4A-F5A \\sim C4A-F6A \\sim C4A-F4A \\sim F6-C4 \\sim F5-C4A \\sim F4-C4 \\sim
C4AA-F6AA \\sim C4AA-F5AA
 \\sim C4AA-F4AA
 with sigma of 0.001
 O4-H4B \\sim O4-H4A
 with sigma of 0.002
3. Rigid bond restraints
 F4AA, F5AA, F6AA, C4AA, F6, F6A, F4, F4A, F5, C4, F5A, C4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F6A) = Uanis(F6)
Uanis(C4A) = Uanis(C4) = Uanis(C4AA)
Uanis(F4) = Uanis(F4A)
Uanis(F4AA) = Uanis(F4A) = Uanis(F4)
5. Rigid body (RIGU) restrains
 O7, O8, C3, F5AA, F6AA, C4AA, F6, F6A, F4, F4A, F5, C4, F5A, C4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(F6)+Sof(F4)+Sof(F5)+Sof(C4)]+1*[Sof(F4AA)+Sof(F5AA)+Sof(F6AA)+
 Sof(C4AA)]+1*[Sof(F6A)+Sof(F4A)+Sof(F5A)+Sof(C4A)]=1 with esd of 0.001
 Sof(F6)=Sof(F4)=Sof(F5)=Sof(C4)=FVAR(1)
 Sof(F4AA)=Sof(F5AA)=Sof(F6AA)=Sof(C4AA)=FVAR(2)
 Sof(F6A)=Sof(F4A)=Sof(F5A)=Sof(C4A)=FVAR(3)
7.a Rotating group:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A)
;
_shelx_res_checksum              98336
_shelx_hkl_checksum              74293
_olex2_exptl_crystal_mounting_method Tip-mounted
_olex2_submission_original_sample_id Fe3OTFAFeCl4
_olex2_submission_special_instructions 'No special instructions were received'