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_4002891
_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 H12 F24 Fe4 O24, 2(H2 O)'
_chemical_formula_sum            'C16 H16 F24 Fe4 O26'
_chemical_formula_weight         1303.78
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2017-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9152(9)
_cell_length_b                   8.3225(5)
_cell_length_c                   19.2599(13)
_cell_measurement_reflns_used    5796
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      26.378
_cell_measurement_theta_min      2.178
_cell_volume                     2010.2(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      102.06
_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 0.997
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26832
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.548
_diffrn_reflns_theta_min         1.726
_exptl_absorpt_coefficient_mu    1.615
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0772 before and 0.0562 after correction. The Ratio of minimum to maximum transmission is 0.8927. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_preparation       'FeCl3 + TFA, reflux, 26h, add H2O after 2h'
_exptl_crystal_recrystallization_method
'Dissolved in toluene at 60 degree C, cool down, kept at air for 1 week'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4183
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0474P)^2^+1.3192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3494
_reflns_number_total             4183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b04382_si_006.cif
_cod_data_source_block           fe4o
_cod_depositor_comments
'Adding full bibliography for 4002891--4002892.cif.'
_cod_database_code               4002891
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H13A(0.068) H13B(0.068)
;
_shelx_res_checksum              51309
_shelx_hkl_checksum              57825
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_original_sample_id Fe4O2TFA
_olex2_submission_special_instructions 'No special instructions were received'