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#$Date: 2025-08-21 01:01:10 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/54/4325496.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4325496
loop_
_publ_author_name
'Timothy J. Boyle'
'Leigh Anna M. Ottley'
'Christopher A. Apblett'
'Constantine A. Stewart'
'Sarah M. Hoppe'
'Krista L. Hawthorne'
'Mark A. Rodriguez'
_publ_section_title
;
 Synthesis, Characterization, and Electrochemical Properties of a Series
 of Sterically Varied Iron(II) Alkoxide Precursors and Their Resultant
 Nanoparticles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6174
_journal_page_last               6182
_journal_paper_doi               10.1021/ic200423m
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C54 H39 Fe O3'
_chemical_formula_weight         791.70
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'P 3*'
_symmetry_space_group_name_H-M   'R 3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.2140(10)
_cell_angle_beta                 97.2140(10)
_cell_angle_gamma                97.2140(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5954(5)
_cell_length_b                   10.5954(5)
_cell_length_c                   10.5954(5)
_cell_measurement_reflns_used    4611
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.56
_cell_volume                     1158.57(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8490
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       cube
_exptl_crystal_F_000             413
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;

;
_refine_diff_density_max         3.783
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2807
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1312P)²+1.2125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.1914
_reflns_number_gt                2766
_reflns_number_total             2807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200423m_si_001_10.cif
_cod_data_source_block           9oc221s
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4325496
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'z, x, y'
'y, z, x'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.1968 1.1968 0.1968 0.0208(3) Uani 1 3 d S
O1 O 0.2383(3) 1.0373(3) 0.2120(3) 0.0286(7) Uani 1 1 d .
C7 C 0.3799(5) 1.0726(5) 0.4632(5) 0.0282(11) Uani 1 1 d .
C13 C 0.3081(5) 0.8971(4) -0.0071(5) 0.0281(11) Uani 1 1 d .
C1 C 0.3439(4) 0.9790(4) 0.2297(5) 0.0229(9) Uani 1 1 d .
C6 C 0.4162(4) 0.9919(4) 0.3532(4) 0.0231(9) Uani 1 1 d .
C3 C 0.4926(5) 0.8480(5) 0.1436(5) 0.0298(10) Uani 1 1 d .
H3 H 0.5186 0.7981 0.0731 0.036 Uiso 1 1 calc R
C11 C 0.2230(5) 1.1576(6) 0.5839(5) 0.0361(12) Uani 1 1 d .
H11 H 0.1359 1.1565 0.5973 0.043 Uiso 1 1 calc R
C2 C 0.3815(5) 0.9076(4) 0.1235(5) 0.0257(9) Uani 1 1 d .
C8 C 0.4749(5) 1.1564(5) 0.5451(5) 0.0353(11) Uani 1 1 d .
H8 H 0.5620 1.1564 0.5323 0.042 Uiso 1 1 calc R
C5 C 0.5253(5) 0.9293(5) 0.3672(5) 0.0290(10) Uani 1 1 d .
H5 H 0.5735 0.9344 0.4501 0.035 Uiso 1 1 calc R
C12 C 0.2529(5) 1.0742(5) 0.4857(5) 0.0318(11) Uani 1 1 d .
H12 H 0.1860 1.0165 0.4320 0.038 Uiso 1 1 calc R
C16 C 0.1743(8) 0.8746(6) -0.2552(6) 0.0506(16) Uani 1 1 d .
H16 H 0.1286 0.8681 -0.3393 0.061 Uiso 1 1 calc R
C10 C 0.3182(6) 1.2433(6) 0.6638(5) 0.0468(14) Uani 1 1 d .
H10 H 0.2961 1.3025 0.7296 0.056 Uiso 1 1 calc R
C4 C 0.5639(5) 0.8606(5) 0.2632(6) 0.0358(11) Uani 1 1 d .
H4 H 0.6400 0.8219 0.2743 0.043 Uiso 1 1 calc R
C9 C 0.4456(6) 1.2423(6) 0.6474(6) 0.0431(14) Uani 1 1 d .
H9 H 0.5122 1.2981 0.7036 0.052 Uiso 1 1 calc R
C18 C 0.1752(6) 0.8657(5) -0.0297(5) 0.0358(12) Uani 1 1 d .
H18 H 0.1291 0.8533 0.0402 0.043 Uiso 1 1 calc R
C15 C 0.3022(8) 0.9053(6) -0.2347(6) 0.0504(17) Uani 1 1 d .
H15 H 0.3466 0.9200 -0.3052 0.060 Uiso 1 1 calc R
C14 C 0.3716(6) 0.9163(5) -0.1127(5) 0.0357(12) Uani 1 1 d .
H14 H 0.4626 0.9368 -0.1009 0.043 Uiso 1 1 calc R
C17 C 0.1088(6) 0.8522(6) -0.1534(6) 0.0447(14) Uani 1 1 d .
H17 H 0.0183 0.8276 -0.1681 0.054 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Fe1 O1 111.48(10) 3_465 2_564
O1 Fe1 O1 111.48(10) 3_465 .
O1 Fe1 O1 111.48(10) 2_564 .
C1 O1 Fe1 139.2(3) . .
C8 C7 C12 117.6(5) . .
C8 C7 C6 119.0(5) . .
C12 C7 C6 123.4(5) . .
C18 C13 C14 117.6(5) . .
C18 C13 C2 121.7(5) . .
C14 C13 C2 120.6(5) . .
O1 C1 C2 119.0(4) . .
O1 C1 C6 120.1(4) . .
C2 C1 C6 120.9(4) . .
C5 C6 C1 118.1(4) . .
C5 C6 C7 121.2(4) . .
C1 C6 C7 120.6(4) . .
C4 C3 C2 121.3(4) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C12 C11 C10 120.9(5) . .
C12 C11 H11 119.6 . .
C10 C11 H11 119.6 . .
C1 C2 C3 118.2(4) . .
C1 C2 C13 121.0(4) . .
C3 C2 C13 120.7(4) . .
C7 C8 C9 121.8(5) . .
C7 C8 H8 119.1 . .
C9 C8 H8 119.1 . .
C4 C5 C6 121.3(5) . .
C4 C5 H5 119.3 . .
C6 C5 H5 119.3 . .
C11 C12 C7 121.3(5) . .
C11 C12 H12 119.4 . .
C7 C12 H12 119.4 . .
C15 C16 C17 119.7(6) . .
C15 C16 H16 120.1 . .
C17 C16 H16 120.1 . .
C9 C10 C11 119.8(5) . .
C9 C10 H10 120.1 . .
C11 C10 H10 120.1 . .
C3 C4 C5 120.1(5) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
C10 C9 C8 118.7(5) . .
C10 C9 H9 120.7 . .
C8 C9 H9 120.7 . .
C13 C18 C17 120.7(5) . .
C13 C18 H18 119.7 . .
C17 C18 H18 119.7 . .
C16 C15 C14 121.5(6) . .
C16 C15 H15 119.3 . .
C14 C15 H15 119.3 . .
C15 C14 C13 120.3(6) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C16 C17 C18 120.1(6) . .
C16 C17 H17 119.9 . .
C18 C17 H17 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.820(3) 3_465
Fe1 O1 1.820(3) 2_564
Fe1 O1 1.820(3) .
O1 C1 1.349(5) .
C7 C8 1.385(8) .
C7 C12 1.397(8) .
C7 C6 1.477(7) .
C13 C18 1.389(8) .
C13 C14 1.400(7) .
C13 C2 1.484(7) .
C1 C2 1.405(7) .
C1 C6 1.412(6) .
C6 C5 1.405(6) .
C3 C4 1.374(8) .
C3 C2 1.409(7) .
C3 H3 0.9500 .
C11 C12 1.374(8) .
C11 C10 1.386(9) .
C11 H11 0.9500 .
C8 C9 1.416(8) .
C8 H8 0.9500 .
C5 C4 1.377(8) .
C5 H5 0.9500 .
C12 H12 0.9500 .
C16 C15 1.337(10) .
C16 C17 1.382(10) .
C16 H16 0.9500 .
C10 C9 1.384(9) .
C10 H10 0.9500 .
C4 H4 0.9500 .
C9 H9 0.9500 .
C18 C17 1.389(8) .
C18 H18 0.9500 .
C15 C14 1.388(9) .
C15 H15 0.9500 .
C14 H14 0.9500 .
C17 H17 0.9500 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.649 0.649 0.649 188.2 -2.3
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139135850
