# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1861919'
loop_
_audit_author_name
_audit_author_address
'Jiong-Peng Zhao'
;Tianjin University Of Technology
China
;
_audit_update_record             
;
2018-08-14 deposited with the CCDC.	2019-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H9 Fe3 O16, H2 O, C H2 O2'
_chemical_formula_sum            'C8 H13 Fe3 O19'
_chemical_formula_weight         580.73
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Fe Fe 0.3463 0.8444 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   17.062(3)
_cell_length_b                   6.8226(15)
_cell_length_c                   16.186(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.84(2)
_cell_angle_gamma                90
_cell_volume                     1850.6(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    720
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2720
_cell_measurement_theta_min      2.5790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2920
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.431
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00 120.00   1.00   20.00    --   30.00  54.00   0.00  195
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0374429000
_diffrn_orient_matrix_UB_12      0.0130073000
_diffrn_orient_matrix_UB_13      -0.0122203000
_diffrn_orient_matrix_UB_21      0.0195488000
_diffrn_orient_matrix_UB_22      -0.0118916000
_diffrn_orient_matrix_UB_23      0.0424155000
_diffrn_orient_matrix_UB_31      0.0024797000
_diffrn_orient_matrix_UB_32      -0.1024897000
_diffrn_orient_matrix_UB_33      -0.0065287000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1477
_reflns_number_total             1845
_reflns_odcompleteness_completeness 83.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.93
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.214
_refine_ls_abs_structure_details 
;
 Flack x determined using 148 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_coef       0.0073(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         1845
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0545
_refine_ls_restrained_S_all      1.070
_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/[σ²(Fo²)+(0.0748P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1519
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.82(10)
 0.18(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3.a Free rotating group:
 O18(H18A,H18B)
3.b Rotating group:
 O00B(H00A,H00B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C2(H2), C1(H1), C6(H6), C5(H5), C4(H4), C8(H8)
3.d Idealised tetrahedral OH refined as rotating group:
 O16(H16)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.65680(14) 0.5372(3) 0.38964(14) 0.0242(6) Uani 1 1 d . . . . .
Fe2 Fe 0.47654(13) 0.7135(3) 0.39511(13) 0.0228(6) Uani 1 1 d . . . . .
Fe3 Fe 0.62089(14) 0.7421(3) 0.56567(14) 0.0250(6) Uani 1 1 d . . . . .
O14 O 0.3586(7) 0.7657(17) 0.3363(7) 0.030(3) Uani 1 1 d . . . . .
O12 O 0.4298(7) 0.6150(17) 0.4950(7) 0.035(3) Uani 1 1 d . . . . .
O7 O 0.7209(7) 0.8728(18) 0.5435(8) 0.036(3) Uani 1 1 d . . . . .
O2 O 0.4575(7) 0.4451(17) 0.3383(7) 0.030(3) Uani 1 1 d . . . . .
O15 O 0.2398(7) 0.8965(19) 0.3310(7) 0.035(3) Uani 1 1 d . . . . .
O10 O 0.4762(8) 0.9948(16) 0.4351(7) 0.035(3) Uani 1 1 d . . . . .
O1 O 0.5840(6) 0.6618(14) 0.4509(7) 0.022(2) Uani 1 1 d . . . . .
O00B O 0.6682(9) 0.8280(18) 0.6897(7) 0.038(3) Uani 1 1 d . . . . .
H00A H 0.653284 0.944733 0.697690 0.057 Uiso 1 1 d GR . . . .
H00B H 0.719007 0.823776 0.698033 0.057 Uiso 1 1 d GR . . . .
O8 O 0.6975(8) 0.3437(17) 0.4832(8) 0.036(3) Uani 1 1 d . . . . .
O11 O 0.5701(8) 1.0108(17) 0.5527(7) 0.034(3) Uani 1 1 d . . . . .
O4 O 0.5057(7) 0.8163(19) 0.2871(7) 0.038(3) Uani 1 1 d . . . . .
O5 O 0.6290(8) 0.7042(19) 0.2854(8) 0.040(3) Uani 1 1 d . . . . .
O18 O 0.2847(9) 0.631(3) 0.7469(9) 0.060(4) Uani 1 1 d . . . . .
H18A H 0.312569 0.584592 0.791739 0.090 Uiso 1 1 d G . . . .
H18B H 0.315184 0.685171 0.717778 0.090 Uiso 1 1 d G . . . .
O9 O 0.6773(8) 0.4852(18) 0.6015(7) 0.039(3) Uani 1 1 d . . . . .
O6 O 0.7453(7) 0.7394(19) 0.4248(8) 0.038(3) Uani 1 1 d . . . . .
O3 O 0.5798(7) 0.3328(17) 0.3326(8) 0.035(3) Uani 1 1 d . . . . .
O13 O 0.5245(9) 0.640(2) 0.6099(8) 0.044(3) Uani 1 1 d . . . . .
C7 C 0.3102(10) 0.866(3) 0.3671(10) 0.028(4) Uani 1 1 d . . . . .
H7 H 0.327421 0.920656 0.419951 0.033 Uiso 1 1 calc R . . . .
C3 C 0.7580(11) 0.861(2) 0.4814(12) 0.032(4) Uani 1 1 d . . . . .
H3 H 0.798010 0.952482 0.479332 0.038 Uiso 1 1 calc R . . . .
C2 C 0.5660(12) 0.797(3) 0.2562(10) 0.033(4) Uani 1 1 d . . . . .
H2 H 0.564899 0.858227 0.204755 0.040 Uiso 1 1 calc R . . . .
C1 C 0.5050(10) 0.326(2) 0.3171(11) 0.031(4) Uani 1 1 d . . . . .
H1 H 0.482423 0.218364 0.285988 0.037 Uiso 1 1 calc R . . . .
C6 C 0.4552(10) 0.598(3) 0.5700(11) 0.033(5) Uani 1 1 d . . . . .
H6 H 0.419806 0.547574 0.601826 0.040 Uiso 1 1 calc R . . . .
C5 C 0.5171(12) 1.078(3) 0.4969(12) 0.038(5) Uani 1 1 d . . . . .
H5 H 0.506269 1.210075 0.502093 0.046 Uiso 1 1 calc R . . . .
C4 C 0.6975(11) 0.348(3) 0.5596(12) 0.032(4) Uani 1 1 d . . . . .
H4 H 0.714722 0.234958 0.589397 0.038 Uiso 1 1 calc R . . . .
C8 C 0.8658(14) 0.580(5) 0.6465(15) 0.062(7) Uani 1 1 d . . . . .
H8 H 0.843538 0.662354 0.681663 0.074 Uiso 1 1 calc R . . . .
O17 O 0.8923(15) 0.639(5) 0.5963(16) 0.143(11) Uani 1 1 d . . . . .
O16 O 0.8657(15) 0.377(5) 0.6574(18) 0.144(11) Uani 1 1 d . . . . .
H16 H 0.832454 0.327597 0.620122 0.216 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe1 O15 2.082(12) 3_545 ?
Fe1 O1 1.927(11) . ?
Fe1 O8 2.031(12) . ?
Fe1 O5 2.016(12) . ?
Fe1 O6 2.045(13) . ?
Fe1 O3 2.017(11) . ?
Fe2 O14 2.089(11) . ?
Fe2 O12 2.046(12) . ?
Fe2 O2 2.048(11) . ?
Fe2 O10 2.026(12) . ?
Fe2 O1 1.918(11) . ?
Fe2 O4 2.031(12) . ?
Fe3 O7 2.017(13) . ?
Fe3 O1 1.925(11) . ?
Fe3 O00B 2.101(11) . ?
Fe3 O11 2.022(12) . ?
Fe3 O9 2.031(13) . ?
Fe3 O13 2.036(15) . ?
O14 C7 1.24(2) . ?
O12 C6 1.22(2) . ?
O7 C3 1.29(2) . ?
O2 C1 1.242(19) . ?
O15 C7 1.250(19) . ?
O10 C5 1.24(2) . ?
O00B H00A 0.8533 . ?
O00B H00B 0.8531 . ?
O8 C4 1.24(2) . ?
O11 C5 1.24(2) . ?
O4 C2 1.23(2) . ?
O5 C2 1.26(2) . ?
O18 H18A 0.8499 . ?
O18 H18B 0.8498 . ?
O9 C4 1.24(2) . ?
O6 C3 1.22(2) . ?
O3 C1 1.25(2) . ?
O13 C6 1.27(2) . ?
C7 H7 0.9300 . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C8 H8 0.9300 . ?
C8 O17 1.08(3) . ?
C8 O16 1.39(4) . ?
O16 H16 0.8200 . ?

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
O1 Fe1 O15 176.2(5) . 3_545 ?
O1 Fe1 O8 93.8(5) . . ?
O1 Fe1 O5 96.2(5) . . ?
O1 Fe1 O6 94.2(5) . . ?
O1 Fe1 O3 96.5(5) . . ?
O8 Fe1 O15 82.7(5) . 3_545 ?
O8 Fe1 O6 95.7(5) . . ?
O5 Fe1 O15 87.3(5) . 3_545 ?
O5 Fe1 O8 170.0(5) . . ?
O5 Fe1 O6 84.1(5) . . ?
O5 Fe1 O3 88.7(5) . . ?
O6 Fe1 O15 84.7(5) . 3_545 ?
O3 Fe1 O15 85.0(5) . 3_545 ?
O3 Fe1 O8 89.7(5) . . ?
O3 Fe1 O6 167.7(5) . . ?
O12 Fe2 O14 86.0(5) . . ?
O12 Fe2 O2 90.5(5) . . ?
O2 Fe2 O14 83.7(5) . . ?
O10 Fe2 O14 85.6(5) . . ?
O10 Fe2 O12 91.9(5) . . ?
O10 Fe2 O2 168.8(5) . . ?
O10 Fe2 O4 87.9(5) . . ?
O1 Fe2 O14 178.7(5) . . ?
O1 Fe2 O12 92.7(5) . . ?
O1 Fe2 O2 96.0(5) . . ?
O1 Fe2 O10 94.8(5) . . ?
O1 Fe2 O4 95.9(5) . . ?
O4 Fe2 O14 85.4(5) . . ?
O4 Fe2 O12 171.4(5) . . ?
O4 Fe2 O2 88.1(5) . . ?
O7 Fe3 O00B 82.0(5) . . ?
O7 Fe3 O11 86.6(5) . . ?
O7 Fe3 O9 93.5(6) . . ?
O7 Fe3 O13 168.7(5) . . ?
O1 Fe3 O7 95.1(5) . . ?
O1 Fe3 O00B 176.6(6) . . ?
O1 Fe3 O11 95.8(4) . . ?
O1 Fe3 O9 94.7(5) . . ?
O1 Fe3 O13 95.9(5) . . ?
O11 Fe3 O00B 85.8(5) . . ?
O11 Fe3 O9 169.4(5) . . ?
O11 Fe3 O13 89.4(6) . . ?
O9 Fe3 O00B 83.8(5) . . ?
O9 Fe3 O13 88.5(6) . . ?
O13 Fe3 O00B 87.1(5) . . ?
C7 O14 Fe2 124.5(10) . . ?
C6 O12 Fe2 134.6(11) . . ?
C3 O7 Fe3 131.9(11) . . ?
C1 O2 Fe2 130.8(11) . . ?
C7 O15 Fe1 122.7(11) . 3_455 ?
C5 O10 Fe2 130.8(11) . . ?
Fe2 O1 Fe1 119.3(5) . . ?
Fe2 O1 Fe3 120.8(6) . . ?
Fe3 O1 Fe1 119.8(5) . . ?
Fe3 O00B H00A 109.5 . . ?
Fe3 O00B H00B 109.8 . . ?
H00A O00B H00B 109.3 . . ?
C4 O8 Fe1 131.6(12) . . ?
C5 O11 Fe3 130.5(12) . . ?
C2 O4 Fe2 132.0(11) . . ?
C2 O5 Fe1 130.3(12) . . ?
H18A O18 H18B 109.5 . . ?
C4 O9 Fe3 131.2(12) . . ?
C3 O6 Fe1 133.1(12) . . ?
C1 O3 Fe1 132.0(11) . . ?
C6 O13 Fe3 129.4(11) . . ?
O14 C7 O15 123.8(15) . . ?
O14 C7 H7 118.1 . . ?
O15 C7 H7 118.1 . . ?
O7 C3 H3 117.2 . . ?
O6 C3 O7 125.6(16) . . ?
O6 C3 H3 117.2 . . ?
O4 C2 O5 128.4(16) . . ?
O4 C2 H2 115.8 . . ?
O5 C2 H2 115.8 . . ?
O2 C1 O3 127.7(16) . . ?
O2 C1 H1 116.1 . . ?
O3 C1 H1 116.1 . . ?
O12 C6 O13 127.6(16) . . ?
O12 C6 H6 116.2 . . ?
O13 C6 H6 116.2 . . ?
O10 C5 H5 115.0 . . ?
O11 C5 O10 130.0(17) . . ?
O11 C5 H5 115.0 . . ?
O8 C4 O9 128.3(17) . . ?
O8 C4 H4 115.9 . . ?
O9 C4 H4 115.9 . . ?
O17 C8 H8 120.8 . . ?
O17 C8 O16 118(3) . . ?
O16 C8 H8 120.8 . . ?
C8 O16 H16 109.5 . . ?

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
Fe1 O15 C7 O14 172.8(13) 3_455 . . . ?
Fe1 O8 C4 O9 -7(3) . . . . ?
Fe1 O5 C2 O4 4(3) . . . . ?
Fe1 O6 C3 O7 10(3) . . . . ?
Fe1 O3 C1 O2 -4(3) . . . . ?
Fe2 O14 C7 O15 179.7(13) . . . . ?
Fe2 O12 C6 O13 0(3) . . . . ?
Fe2 O2 C1 O3 7(3) . . . . ?
Fe2 O10 C5 O11 0(3) . . . . ?
Fe2 O4 C2 O5 -1(3) . . . . ?
Fe3 O7 C3 O6 -11(3) . . . . ?
Fe3 O11 C5 O10 5(3) . . . . ?
Fe3 O9 C4 O8 10(3) . . . . ?
Fe3 O13 C6 O12 -2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.761
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.82(10)
2 0.18(10)
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1861920'
loop_
_audit_author_name
_audit_author_address
'Jiong-Peng Zhao'
;Tianjin University Of Technology
China
;
_audit_update_record             
;
2018-08-14 deposited with the CCDC.	2019-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-05-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.33(C18 H24 Fe9 O42)'
_chemical_formula_sum            'C6 H8 Fe3 O14'
_chemical_formula_weight         471.67
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Fe Fe 0.3463 0.8444 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_H-M_alt        'P 32 2 1'
_space_group_name_Hall           'P 32 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'

_cell_length_a                   10.4091(12)
_cell_length_b                   10.4091(12)
_cell_length_c                   11.015(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1033.6(3)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    791
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.3830
_cell_measurement_theta_min      2.2050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             702
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2942
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.918
_diffrn_reflns_theta_min         2.259
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -31.00  82.00   1.00    8.00    --   30.00  54.00   0.00  113
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0496754000
_diffrn_orient_matrix_UB_12      -0.0112223000
_diffrn_orient_matrix_UB_13      0.0364519000
_diffrn_orient_matrix_UB_21      -0.0558330000
_diffrn_orient_matrix_UB_22      -0.0345698000
_diffrn_orient_matrix_UB_23      0.0451118000
_diffrn_orient_matrix_UB_31      -0.0243793000
_diffrn_orient_matrix_UB_32      -0.0695147000
_diffrn_orient_matrix_UB_33      -0.0283234000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.583
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.724
_reflns_number_gt                1629
_reflns_number_total             2204
_reflns_odcompleteness_completeness 94.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.84
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.662
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details 
;
 Flack x determined using 468 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0701
_refine_ls_restrained_S_all      1.053
_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/[σ²(Fo²)+(0.0818P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1757
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.81116(13) 0.74085(13) 0.35897(11) 0.0350(3) Uani 1 1 d . . . . .
Fe2 Fe 0.50851(16) 0.50851(16) 0.500000 0.0368(4) Uani 1 2 d S T P . .
O6 O 0.4543(8) 0.5057(7) 0.3207(6) 0.0467(16) Uani 1 1 d . . . . .
O7 O 0.6875(8) 0.6875(8) 0.500000 0.0362(18) Uani 1 2 d S T P . .
O1 O 0.8226(8) 0.9509(7) 0.3550(6) 0.0387(14) Uani 1 1 d . . . . .
O2 O 0.8484(7) 1.0203(7) 0.5500(5) 0.0369(12) Uani 1 1 d . . . . .
O5 O 0.6595(8) 0.6701(9) 0.2228(6) 0.0500(16) Uani 1 1 d . . . . .
O1W O 0.3141(9) 0.3141(9) 0.500000 0.048(2) Uani 1 2 d S T P . .
O4 O 0.6077(8) 0.3876(7) 0.4579(7) 0.0506(16) Uani 1 1 d . . . . .
O3 O 0.8154(8) 0.5468(8) 0.3551(7) 0.0501(17) Uani 1 1 d . . . . .
C3 C 0.5238(10) 0.5756(11) 0.2283(8) 0.044(2) Uani 1 1 d . . . . .
H3 H 0.469841 0.555724 0.156689 0.053 Uiso 1 1 calc R . . . .
C2 C 0.7258(12) 0.4246(11) 0.4012(9) 0.050(2) Uani 1 1 d . . . . .
H2 H 0.749918 0.350351 0.392097 0.060 Uiso 1 1 calc R . . . .
C1 C 0.8459(11) 1.0411(9) 0.4369(8) 0.0380(18) Uani 1 1 d . . . . .
H1 H 0.863471 1.134234 0.413019 0.046 Uiso 1 1 calc R . . . .
H1W H 0.282(9) 0.268(9) 0.434(6) 0.017(19) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe1 O7 1.914(4) . ?
Fe1 O1 2.130(6) . ?
Fe1 O2 2.136(6) 4_556 ?
Fe1 O2 2.183(6) 2_764 ?
Fe1 O5 2.030(7) . ?
Fe1 O3 2.043(7) . ?
Fe2 O6 2.051(7) 4_556 ?
Fe2 O6 2.051(7) . ?
Fe2 O7 1.863(8) . ?
Fe2 O1W 2.024(10) . ?
Fe2 O4 2.040(7) . ?
Fe2 O4 2.040(7) 4_556 ?
O6 C3 1.250(11) . ?
O1 C1 1.236(10) . ?
O2 C1 1.267(10) . ?
O5 C3 1.256(12) . ?
O1W H1W 0.84(7) 4_556 ?
O1W H1W 0.84(7) . ?
O4 C2 1.256(13) . ?
O3 C2 1.248(12) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?

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
O7 Fe1 O1 89.9(2) . . ?
O7 Fe1 O2 97.6(2) . 4_556 ?
O7 Fe1 O2 170.9(3) . 2_764 ?
O7 Fe1 O5 101.9(2) . . ?
O7 Fe1 O3 94.2(2) . . ?
O1 Fe1 O2 87.3(3) . 4_556 ?
O1 Fe1 O2 86.4(3) . 2_764 ?
O2 Fe1 O2 73.9(3) 4_556 2_764 ?
O5 Fe1 O1 89.5(3) . . ?
O5 Fe1 O2 86.4(2) . 2_764 ?
O5 Fe1 O2 160.2(2) . 4_556 ?
O5 Fe1 O3 91.3(3) . . ?
O3 Fe1 O1 175.5(3) . . ?
O3 Fe1 O2 90.4(3) . 4_556 ?
O3 Fe1 O2 89.2(3) . 2_764 ?
O6 Fe2 O6 163.3(4) 4_556 . ?
O7 Fe2 O6 98.33(19) . . ?
O7 Fe2 O6 98.33(19) . 4_556 ?
O7 Fe2 O1W 180.00(17) . . ?
O7 Fe2 O4 93.2(2) . 4_556 ?
O7 Fe2 O4 93.2(2) . . ?
O1W Fe2 O6 81.67(19) . 4_556 ?
O1W Fe2 O6 81.67(19) . . ?
O1W Fe2 O4 86.8(2) . . ?
O1W Fe2 O4 86.8(2) . 4_556 ?
O4 Fe2 O6 89.5(3) 4_556 . ?
O4 Fe2 O6 89.6(3) 4_556 4_556 ?
O4 Fe2 O6 89.5(3) . 4_556 ?
O4 Fe2 O6 89.6(3) . . ?
O4 Fe2 O4 173.6(4) 4_556 . ?
C3 O6 Fe2 134.5(6) . . ?
Fe1 O7 Fe1 122.5(4) 4_556 . ?
Fe2 O7 Fe1 118.8(2) . 4_556 ?
Fe2 O7 Fe1 118.8(2) . . ?
C1 O1 Fe1 130.8(6) . . ?
Fe1 O2 Fe1 106.1(3) 4_556 3_675 ?
C1 O2 Fe1 127.0(5) . 3_675 ?
C1 O2 Fe1 126.2(5) . 4_556 ?
C3 O5 Fe1 127.9(6) . . ?
Fe2 O1W H1W 119(6) . . ?
Fe2 O1W H1W 119(6) . 4_556 ?
H1W O1W H1W 122(10) . 4_556 ?
C2 O4 Fe2 130.1(6) . . ?
C2 O3 Fe1 128.7(6) . . ?
O6 C3 O5 126.4(9) . . ?
O6 C3 H3 116.8 . . ?
O5 C3 H3 116.8 . . ?
O4 C2 H2 115.4 . . ?
O3 C2 O4 129.2(9) . . ?
O3 C2 H2 115.4 . . ?
O1 C1 O2 127.0(8) . . ?
O1 C1 H1 116.5 . . ?
O2 C1 H1 116.5 . . ?

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
Fe1 O1 C1 O2 -11.0(15) . . . . ?
Fe1 O2 C1 O1 167.5(7) 3_675 . . . ?
Fe1 O2 C1 O1 -23.7(14) 4_556 . . . ?
Fe1 O5 C3 O6 0.3(15) . . . . ?
Fe1 O3 C2 O4 2.7(17) . . . . ?
Fe2 O6 C3 O5 3.3(16) . . . . ?
Fe2 O4 C2 O3 0.3(18) . . . . ?
O6 Fe2 O7 Fe1 144.6(2) 4_556 . . . ?
O6 Fe2 O7 Fe1 -35.4(2) 4_556 . . 4_556 ?
O6 Fe2 O7 Fe1 144.6(2) . . . 4_556 ?
O6 Fe2 O7 Fe1 -35.4(2) . . . . ?
O4 Fe2 O7 Fe1 -125.3(2) . . . 4_556 ?
O4 Fe2 O7 Fe1 54.7(2) . . . . ?
O4 Fe2 O7 Fe1 54.7(2) 4_556 . . 4_556 ?
O4 Fe2 O7 Fe1 -125.3(2) 4_556 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.555
_oxdiff_exptl_absorpt_empirical_full_min 0.275


#############end
