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_4003119
_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         'C14 H4 F21 Fe3 O17, C2 H F3 O2'
_chemical_formula_sum            'C16 H5 F24 Fe3 O19'
_chemical_formula_weight         1124.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.855(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2131(19)
_cell_length_b                   15.207(2)
_cell_length_c                   20.901(4)
_cell_measurement_reflns_used    6546
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      25.173
_cell_measurement_theta_min      2.197
_cell_volume                     3715.1(10)
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_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      250.0
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type
'Bruker SMART Platform with a Apex I-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  Parallel,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  0.0360
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25309
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.983
_diffrn_reflns_theta_min         1.682
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.7242
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0601 before and 0.0458 after correction. The Ratio of minimum to maximum transmission is 0.7903. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2188
_exptl_crystal_recrystallization_method
'crystallized from synthesis solution under N2-atmosphere'
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         7200
_refine_ls_number_restraints     846
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0593P)^2^+1.8466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5415
_reflns_number_total             7200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b04382_si_002.cif
_cod_data_source_block           p21n_new_anis
_cod_original_cell_volume        3715.1(11)
_cod_database_code               4003119
_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
 F10-F12 \\sim F12-F11 \\sim F11-F10
 with sigma of 0.001
 F21A-F19A \\sim F19A-F20A \\sim F20A-F21A
 with sigma of 0.001
 F19-F20 \\sim F20-F21 \\sim F21-F19
 with sigma of 0.001
 F21-C14 \\sim F19-C14 \\sim F20-C14
 with sigma of 0.001
 F23A-F24A \\sim F24A-F22A \\sim F22A-F23A
 with sigma of 0.001
 F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.001
 F3-F2 \\sim F2-F1 \\sim F1-F3
 with sigma of 0.001
 F1-C2 \\sim F1A-C2 \\sim F3-C2 \\sim F3A-C2 \\sim F2A-C2 \\sim F2-C2
 with sigma of 0.001
 F10A-F12A \\sim F12A-F11A \\sim F11A-F10A
 with sigma of 0.001
 F12A-C8 \\sim F12-C8 \\sim F11A-C8 \\sim F11-C8 \\sim F10A-C8 \\sim F10-C8
 with sigma of 0.001
 F23-F22 \\sim F22-F24 \\sim F24-F23
 with sigma of 0.001
 F24-C16 \\sim F23A-C16 \\sim F23-C16 \\sim F22A-C16 \\sim F22-C16 \\sim
F24A-C16
 with sigma of 0.001
 F15A-F13A \\sim F13A-F14A \\sim F14A-F15A
 with sigma of 0.001
 F15-F13 \\sim F13-F14 \\sim F14-F15
 with sigma of 0.001
 C10-C9 \\sim C10A-C9
 with sigma of 0.001
 F14A-C10A \\sim F13-C10 \\sim F13A-C10A \\sim F14-C10 \\sim F15A-C10A \\sim
F15-C10
 with sigma of 0.001
 F4-F6 \\sim F6-F5 \\sim F5-F4
 with sigma of 0.001
 C4-C3 \\sim C4A-C3
 with sigma of 0.001
 F18A-F17A \\sim F17A-F16A \\sim F16A-F18A
 with sigma of 0.001
 F9-F8 \\sim F8-F7 \\sim F7-F9
 with sigma of 0.001
 C6A-C5 \\sim C6-C5
 with sigma of 0.001
 F18-F16 \\sim F16-F17 \\sim F17-F18
 with sigma of 0.001
 F18A-C12A \\sim F17A-C12A \\sim F16A-C12A \\sim F16-C12 \\sim F18-C12 \\sim
F17-C12
 with sigma of 0.001
 C12A-C11 \\sim C12-C11
 with sigma of 0.001
 F5A-F6A \\sim F6A-F4A \\sim F4A-F5A
 with sigma of 0.001
 F4A-C4A \\sim F6-C4 \\sim F6A-C4A \\sim F5-C4 \\sim F5A-C4A \\sim F4-C4
 with sigma of 0.001
 F7A-F9A \\sim F9A-F8A \\sim F8A-F7A
 with sigma of 0.001
 F9-C6 \\sim F8-C6 \\sim F8A-C6A \\sim F7-C6 \\sim F7A-C6A \\sim F9A-C6A
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F14A) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F15A) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C10) = Uanis(C10A)
Uanis(C4) = Uanis(C4A)
Uanis(C6) = Uanis(C6A)
Uanis(C12A) = Uanis(C12)
4. 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
5. Others
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(C6A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C6)=FVAR(2)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(C10A)=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(C10)=FVAR(3)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=Sof(C12A)=1-FVAR(4)
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(C12)=FVAR(4)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(5)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(5)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(C4A)=1-FVAR(6)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4)=FVAR(6)
 Sof(F1)=Sof(F2)=Sof(F3)=1-FVAR(7)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(7)
 Sof(F22)=Sof(F23)=Sof(F24)=1-FVAR(8)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=FVAR(8)
6.a Rotating group:
 O18(H18A,H18B), O19(H19A,H19B)
;
_shelx_res_checksum              86555
_shelx_hkl_checksum              30381
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'