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_4002892
_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         'C16 H10 F24 Fe3 O20, 2(C2 H F3 O2)'
_chemical_formula_sum            'C20 H12 F30 Fe3 O24'
_chemical_formula_weight         1373.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                84.900(14)
_cell_angle_beta                 71.634(14)
_cell_angle_gamma                81.897(14)
_cell_formula_units_Z            1
_cell_length_a                   9.201(5)
_cell_length_b                   10.484(6)
_cell_length_c                   12.232(6)
_cell_measurement_reflns_used    516
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      24.358
_cell_measurement_theta_min      2.349
_cell_volume                     1107.4(10)
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (2016)'
_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      250
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.955
_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_unetI/netI     0.1362
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4731
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.538
_diffrn_reflns_theta_min         1.756
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.823759
_exptl_absorpt_correction_T_min  0.509163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1070 before and 0.0471 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1025 before and 0.0406 after correction.
 The Ratio of minimum to maximum transmission is 0.62.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 22822 reflections, Rint = 0.1168
 (4853 with I > 3sig(I), Rint = 0.0904)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_preparation       'FeCl3 + TFA, reflux, 26h, add H2O after 2h'
_exptl_crystal_recrystallization_method
'crystallized from a THF/toluene mixture'
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         4731
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0841P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2405
_reflns_number_total             4731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b04382_si_005.cif
_cod_data_source_block           p_1_twin
_cod_depositor_comments
'Adding full bibliography for 4002891--4002892.cif.'
_cod_original_cell_volume        1107.5(10)
_cod_database_code               4002892
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.714(10)
 0.286(10)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Shared sites
{C6B, C6}
4. Restrained distances
 O1-H1B = O1-H1A
 0.958 with sigma of 0.001
 H1B-H1A
 1.515 with sigma of 0.001
 O7-H1B
 1.732 with sigma of 0.02
 C6B-C5 \\sim C6A-C5 \\sim C5-C6
 with sigma of 0.001
 F9-F7 \\sim F9-F8 \\sim F7-F8
 with sigma of 0.001
 F8A-F7A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.001
 F8B-F7B \\sim F8B-F9B \\sim F7B-F9B
 with sigma of 0.001
 F7A-C6A \\sim F8A-C6A \\sim F9A-C6A
 with sigma of 0.001
 F8-C6B \\sim F9-C6B \\sim F7-C6B
 with sigma of 0.001
 F7B-C6 \\sim F9B-C6 \\sim F8B-C6
 with sigma of 0.001
 C4A-C3 \\sim C4-C3 \\sim C4B-C3
 with sigma of 0.001
 F6B-C4B \\sim F5B-C4B \\sim F4B-C4B
 with sigma of 0.001
 F6A-C4A \\sim F5A-C4A \\sim F4A-C4A
 with sigma of 0.001
 C4-F5 \\sim C4-F4 \\sim C4-F6
 with sigma of 0.001
 F6A-F4A \\sim F6A-F5A \\sim F4A-F5A \\sim F6B-F4B \\sim F6B-F5B \\sim F4B-F5B
\\sim F5-F4 \\sim F5-F6 ~
 F4-F6
 with sigma of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(C6B) = Uanis(C6A) = Uanis(C6)
Uanis(C4A) = Uanis(C4) = Uanis(C4B)
Uanis(F5B) = Uanis(F5A)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 1*[Sof(F4)+Sof(F5)+Sof(F6)+Sof(C4)]+1*[Sof(F4A)+Sof(F5A)+Sof(F6A)+Sof(C4A)]+1*
 [Sof(F4B)+Sof(F5B)+Sof(F6B)+Sof(C4B)]=1 with esd of 0.001
 1*[Sof(F7)+Sof(F8)+Sof(F9)+Sof(C6B)]+1*[Sof(F7A)+Sof(F8A)+Sof(F9A)+Sof(C6A)]+
 1*[Sof(F7B)+Sof(F8B)+Sof(F9B)+Sof(C6)]=1 with esd of 0.001
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(C4A)=FVAR(2)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(C4B)=FVAR(3)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C6B)=FVAR(4)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(C6A)=FVAR(5)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(C6)=FVAR(6)
8.a Rotating group:
 O10(H10A,H10B)
8.b Idealised tetrahedral OH refined as rotating group:
 O9(H9), O11(H11)
;
_shelx_res_checksum              65010
_shelx_hkl_checksum              1343
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'