#------------------------------------------------------------------------------
#$Date: 2024-08-16 04:25:39 +0200 (Fri 16 de Aug de 2024) $
#$Revision: 294150 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/23/1572367.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1572367
loop_
_publ_author_name
'Pacoste, Laura'
'Ignat'ev, Vladislav Mikhailovich'
'Dominiak, Paulina Maria'
'Zou, Xiaodong'
_publ_section_title
;
 On the structure refinement of metal complexes against 3D electron
 diffraction data using multipolar scattering factors.
;
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524006730
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C15 H21 Fe O6'
_chemical_formula_sum            'C15 H21 Fe O6'
_chemical_formula_weight         353.172
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_audit_creation_date             2024-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.35(5)
_cell_length_b                   13.56(7)
_cell_length_c                   16.50(5)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      69.90
_cell_measurement_theta_min      2.70
_cell_volume                     3434(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.9205
_diffrn_measured_fraction_theta_max 0.9186
_diffrn_measurement_device_type
'ThermoFisher Scientific Titan Krios cryo-Transmission Electron Microscope'
_diffrn_measurement_method       β\
_diffrn_radiation_source         'Electron Schottky Gun'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.01967
_diffrn_reflns_av_R_equivalents  0.2170
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_Laue_measured_fraction_full 0.9205
_diffrn_reflns_Laue_measured_fraction_max 0.9186
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37312
_diffrn_reflns_point_group_measured_fraction_full 0.9205
_diffrn_reflns_point_group_measured_fraction_max 0.9186
_diffrn_reflns_theta_full        0.6634
_diffrn_reflns_theta_max         0.66
_diffrn_reflns_theta_min         0.07
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             542.168
_exptl_crystal_size_max          0.0005
_exptl_crystal_size_mid          0.0005
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.9448
_refine_diff_density_min         -1.1442
_refine_diff_density_rms         0.2843
_refine_ls_d_res_high            0.8494
_refine_ls_d_res_low             8.6530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.2359
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.2359
_refine_ls_R_factor_all          0.2275
_refine_ls_R_factor_gt           0.1934
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2139P)²+2.3800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4556
_refine_ls_wR_factor_ref         0.4745
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2007
_reflns_number_total             2687
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jf5002.cif
_cod_data_source_block           3DED_IAM_charged_Fe2
_cod_original_cell_volume        3434(23)
_cod_database_code               1572367
_diffrn_oxdiff_scatteringfactors_ed
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C010(H010), C012(H012), C013(H013)
2.b Idealised Me refined as rotating group:
 C007(H00a,H00b,H00c), C008(H00d,H00e,H00f), C009(H00g,H00h,H00i), C011(H01a,
 H01b,H01c), C014(H01d,H01e,H01f), C015(H01g,H01h,H01i)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y+1/2,-z+1/2
4 -x+1/2,-y,z+1/2
5 -x,-y,-z
6 -x-1/2,y-1/2,z
7 x,-y-1/2,z-1/2
8 x-1/2,y,-z-1/2
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_refinement_flags_posn
Fe01 Fe 0.64247(19) 0.7265(3) 0.74605(17) 0.0297(11) Uani 1.000000 .
O001 O 0.5950(6) 0.6579(10) 0.6464(5) 0.038(3) Uani 1.000000 .
O002 O 0.7007(6) 0.7987(9) 0.8352(5) 0.036(3) Uani 1.000000 .
O003 O 0.5714(5) 0.6406(9) 0.8208(5) 0.036(3) Uani 1.000000 .
O004 O 0.7066(5) 0.8174(8) 0.6690(5) 0.028(2) Uani 1.000000 .
O005 O 0.7381(5) 0.6245(9) 0.7533(5) 0.031(3) Uani 1.000000 .
O006 O 0.5423(5) 0.8248(9) 0.7483(5) 0.033(2) Uani 1.000000 .
C001 C 0.5960(7) 0.6880(11) 0.5735(6) 0.043(3) Uani 1.000000 .
C002 C 0.4974(6) 0.6531(10) 0.8511(6) 0.036(3) Uani 1.000000 .
C003 C 0.4700(5) 0.8212(9) 0.7857(6) 0.029(3) Uani 1.000000 .
C004 C 0.8067(7) 0.6255(9) 0.7964(6) 0.035(3) Uani 1.000000 .
C005 C 0.6939(6) 0.8324(10) 0.5921(6) 0.038(3) Uani 1.000000 .
C006 C 0.7765(6) 0.7857(10) 0.8653(6) 0.037(3) Uani 1.000000 .
C007 C 0.5494(8) 0.6211(13) 0.5120(6) 0.074(5) Uani 1.000000 .
H00a H 0.4808(10) 0.619(4) 0.526(2) 0.111(8) Uiso 1.000000 GR
H00b H 0.559(3) 0.650(3) 0.4518(8) 0.111(8) Uiso 1.000000 GR
H00c H 0.576(3) 0.5477(16) 0.516(2) 0.111(8) Uiso 1.000000 GR
C008 C 0.8669(7) 0.5380(11) 0.7900(8) 0.055(4) Uani 1.000000 .
H00d H 0.859(2) 0.504(2) 0.7316(13) 0.083(6) Uiso 1.000000 GR
H00e H 0.9333(7) 0.5621(12) 0.797(3) 0.083(6) Uiso 1.000000 GR
H00f H 0.8515(19) 0.4858(18) 0.8370(18) 0.083(6) Uiso 1.000000 GR
C009 C 0.4641(7) 0.5743(13) 0.9047(6) 0.062(4) Uani 1.000000 .
H00g H 0.3972(12) 0.590(2) 0.920(2) 0.093(7) Uiso 1.000000 GR
H00h H 0.468(3) 0.5045(14) 0.8738(12) 0.093(7) Uiso 1.000000 GR
H00i H 0.503(2) 0.572(3) 0.9591(14) 0.093(7) Uiso 1.000000 GR
C010 C 0.6408(8) 0.7700(12) 0.5433(6) 0.057(4) Uani 1.000000 .
H010 H 0.6348(8) 0.7869(12) 0.4794(6) 0.069(5) Uiso 1.000000 R
C011 C 0.7431(8) 0.9120(13) 0.5533(7) 0.066(5) Uani 1.000000 .
H01a H 0.7080(18) 0.938(3) 0.501(2) 0.100(7) Uiso 1.000000 GR
H01b H 0.752(3) 0.9717(19) 0.5956(13) 0.100(7) Uiso 1.000000 GR
H01c H 0.8059(15) 0.8847(15) 0.535(3) 0.100(7) Uiso 1.000000 GR
C012 C 0.4442(6) 0.7380(10) 0.8360(6) 0.043(3) Uani 1.000000 .
H012 H 0.3804(6) 0.7404(10) 0.8641(6) 0.051(4) Uiso 1.000000 R
C013 C 0.8302(7) 0.7058(11) 0.8497(6) 0.048(4) Uani 1.000000 .
H013 H 0.8933(7) 0.7034(11) 0.8791(6) 0.057(5) Uiso 1.000000 R
C014 C 0.8097(7) 0.8686(14) 0.9218(8) 0.086(7) Uani 1.000000 .
H01d H 0.8738(19) 0.850(3) 0.943(3) 0.128(10) Uiso 1.000000 GR
H01e H 0.812(4) 0.9370(16) 0.8888(13) 0.128(10) Uiso 1.000000 GR
H01f H 0.766(2) 0.876(4) 0.973(2) 0.128(10) Uiso 1.000000 GR
C015 C 0.4100(6) 0.9053(11) 0.7766(7) 0.047(3) Uani 1.000000 .
H01g H 0.4245(18) 0.944(2) 0.7212(14) 0.070(5) Uiso 1.000000 GR
H01h H 0.3439(6) 0.8788(11) 0.775(2) 0.070(5) Uiso 1.000000 GR
H01i H 0.4178(18) 0.9547(18) 0.8272(14) 0.070(5) Uiso 1.000000 GR
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00000 0.00000 0.60000 0.13600 0.54700 1.22500 40.93800 0.37400 3.27800
13.01300 0.00000 'Custom 4-Gaussian' custom
Fe 0.00000 0.00000 43.68700 1.29200 3.02900 9.66200 581.14100 0.86100 9.42100
106.74600 0.00000 'Custom 4-Gaussian' custom
H 0.00000 0.00000 0.12900 0.03600 0.12700 0.23600 37.73700 0.55300 3.77200
13.51800 0.00000 'Custom 4-Gaussian' custom
O 0.00000 0.00000 -16.47700 -3.90400 1.06800 0.24600 916.12900 177.36500 5.24500
0.53600 0.00000 'Custom 4-Gaussian' custom
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
_geom_angle_publ_flag
O002 Fe01 O001 173.1(4) . . ?
O003 Fe01 O001 92.1(4) . . ?
O003 Fe01 O002 94.3(4) . . ?
O004 Fe01 O001 86.8(4) . . ?
O004 Fe01 O002 86.9(4) . . ?
O004 Fe01 O003 176.3(4) . . ?
O005 Fe01 O001 89.7(4) . . ?
O005 Fe01 O002 88.1(4) . . ?
O005 Fe01 O003 87.8(4) . . ?
O005 Fe01 O004 95.8(4) . . ?
O006 Fe01 O001 92.5(4) . . ?
O006 Fe01 O002 90.2(5) . . ?
O006 Fe01 O003 87.6(4) . . ?
O006 Fe01 O004 88.9(4) . . ?
O006 Fe01 O005 175.0(4) . . ?
C001 O001 Fe01 128.1(10) . . ?
C006 O002 Fe01 129.2(9) . . ?
C002 O003 Fe01 131.0(10) . . ?
C005 O004 Fe01 129.5(7) . . ?
C004 O005 Fe01 128.8(9) . . ?
C003 O006 Fe01 130.0(9) . . ?
C007 C001 O001 115.5(12) . . ?
C010 C001 O001 126.7(11) . . ?
C010 C001 C007 117.5(10) . . ?
C009 C002 O003 117.0(11) . . ?
C012 C002 O003 123.8(11) . . ?
C012 C002 C009 119.2(9) . . ?
C012 C003 O006 123.0(10) . . ?
C015 C003 O006 117.8(10) . . ?
C015 C003 C012 119.2(8) . . ?
C008 C004 O005 117.3(10) . . ?
C013 C004 O005 123.8(11) . . ?
C013 C004 C008 118.9(9) . . ?
C010 C005 O004 123.0(11) . . ?
C011 C005 O004 117.7(10) . . ?
C011 C005 C010 119.1(10) . . ?
C013 C006 O002 125.3(11) . . ?
C014 C006 O002 115.7(11) . . ?
C014 C006 C013 118.9(9) . . ?
H00a C007 C001 109.5 . . ?
H00b C007 C001 109.5 . . ?
H00b C007 H00a 109.5 . . ?
H00c C007 C001 109.5 . . ?
H00c C007 H00a 109.5 . . ?
H00c C007 H00b 109.5 . . ?
H00d C008 C004 109.5 . . ?
H00e C008 C004 109.5 . . ?
H00e C008 H00d 109.5 . . ?
H00f C008 C004 109.5 . . ?
H00f C008 H00d 109.5 . . ?
H00f C008 H00e 109.5 . . ?
H00g C009 C002 109.5 . . ?
H00h C009 C002 109.5 . . ?
H00h C009 H00g 109.5 . . ?
H00i C009 C002 109.5 . . ?
H00i C009 H00g 109.5 . . ?
H00i C009 H00h 109.5 . . ?
C005 C010 C001 123.6(10) . . ?
H010 C010 C001 118.2(6) . . ?
H010 C010 C005 118.2(7) . . ?
H01a C011 C005 109.5 . . ?
H01b C011 C005 109.5 . . ?
H01b C011 H01a 109.5 . . ?
H01c C011 C005 109.5 . . ?
H01c C011 H01a 109.5 . . ?
H01c C011 H01b 109.5 . . ?
C003 C012 C002 124.5(8) . . ?
H012 C012 C002 117.7(6) . . ?
H012 C012 C003 117.7(6) . . ?
C006 C013 C004 123.6(9) . . ?
H013 C013 C004 118.2(6) . . ?
H013 C013 C006 118.2(6) . . ?
H01d C014 C006 109.5 . . ?
H01e C014 C006 109.5 . . ?
H01e C014 H01d 109.5 . . ?
H01f C014 C006 109.5 . . ?
H01f C014 H01d 109.5 . . ?
H01f C014 H01e 109.5 . . ?
H01g C015 C003 109.5 . . ?
H01h C015 C003 109.5 . . ?
H01h C015 H01g 109.5 . . ?
H01i C015 C003 109.5 . . ?
H01i C015 H01g 109.5 . . ?
H01i C015 H01h 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 O001 2.024(11) . ?
Fe01 O002 1.980(10) . ?
Fe01 O003 2.017(11) . ?
Fe01 O004 2.025(10) . ?
Fe01 O005 2.021(12) . ?
Fe01 O006 2.035(12) . ?
O001 C001 1.270(14) . ?
O002 C006 1.277(13) . ?
O003 C002 1.253(12) . ?
O004 C005 1.299(13) . ?
O005 C004 1.271(13) . ?
O006 C003 1.271(12) . ?
C001 C007 1.538(16) . ?
C001 C010 1.399(19) . ?
C002 C009 1.478(18) . ?
C002 C012 1.432(17) . ?
C003 C012 1.456(17) . ?
C003 C015 1.474(17) . ?
C004 C008 1.507(17) . ?
C004 C013 1.446(17) . ?
C005 C010 1.424(17) . ?
C005 C011 1.465(18) . ?
C006 C013 1.385(17) . ?
C006 C014 1.547(18) . ?
C007 H00a 1.0770 . ?
C007 H00b 1.0770 . ?
C007 H00c 1.0770 . ?
C008 H00d 1.0770 . ?
C008 H00e 1.0770 . ?
C008 H00f 1.0770 . ?
C009 H00g 1.0770 . ?
C009 H00h 1.0770 . ?
C009 H00i 1.0770 . ?
C010 H010 1.0830 . ?
C011 H01a 1.0770 . ?
C011 H01b 1.0770 . ?
C011 H01c 1.0770 . ?
C012 H012 1.0830 . ?
C013 H013 1.0830 . ?
C014 H01d 1.0770 . ?
C014 H01e 1.0770 . ?
C014 H01f 1.0770 . ?
C015 H01g 1.0770 . ?
C015 H01h 1.0770 . ?
C015 H01i 1.0770 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 O001 C001 C007 -176.5(10) . . . . ?
Fe01 O001 C001 C010 9.4(13) . . . . ?
Fe01 O002 C006 C013 -11.0(13) . . . . ?
Fe01 O002 C006 C014 167.5(11) . . . . ?
Fe01 O003 C002 C009 -179.6(10) . . . . ?
Fe01 O003 C002 C012 0.9(11) . . . . ?
Fe01 O004 C005 C010 -13.3(12) . . . . ?
Fe01 O004 C005 C011 172.5(11) . . . . ?
Fe01 O005 C004 C008 179.5(9) . . . . ?
Fe01 O005 C004 C013 -1.4(12) . . . . ?
Fe01 O006 C003 C012 -1.5(12) . . . . ?
Fe01 O006 C003 C015 179.0(9) . . . . ?
O001 C001 C010 C005 0.6(16) . . . . ?
O002 C006 C013 C004 -0.0(14) . . . . ?
O003 C002 C012 C003 -1.6(14) . . . . ?
O004 C005 C010 C001 1.3(14) . . . . ?
O005 C004 C013 C006 6.4(13) . . . . ?
O006 C003 C012 C002 1.9(13) . . . . ?
C001 C010 C005 C011 175.5(13) . . . . ?
C002 C012 C003 C015 -178.5(11) . . . . ?
C004 C013 C006 C014 -178.5(13) . . . . ?
