# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_J_11_100
_audit_block_doi                 10.5517/ccdc.csd.cc242ty0
_database_code_depnum_ccdc_archive 'CCDC 1968932'
loop_
_audit_author_name
_audit_author_address
'Jan Janczak '
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2020-06-06 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Fe (C2 O4)2 (K H2 O)3'
_chemical_formula_sum            'C6 H6 Fe K3 O15'
_chemical_formula_weight         491.26

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'
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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.7175(4)
_cell_length_b                   19.8009(7)
_cell_length_c                   10.2623(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.634(5)
_cell_angle_gamma                90
_cell_volume                     1494.53(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4578
_cell_measurement_theta_min      2.7740
_cell_measurement_theta_max      28.7650

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.927
_shelx_estimated_absorpt_T_min   0.655
_shelx_estimated_absorpt_T_max   0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9152
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'KUMA KM-4 with CCD detector'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            19107
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.769
_diffrn_reflns_theta_max         29.451
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3745
_reflns_number_gt                2806
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrysAlis CCD 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0259P)²+3.0723P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3745
_refine_ls_number_parameters     237
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0864
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Fe Fe 0.76313(5) 0.63127(2) 0.25144(4) 0.00917(10) Uani 1 1 d . . . . .
K1 K 0.25832(9) 0.58639(3) 0.25415(7) 0.01628(15) Uani 1 1 d . . . . .
K2 K 0.46161(8) 0.57830(3) 0.66322(6) 0.01476(15) Uani 1 1 d . . . . .
K3 K 1.02455(8) 0.57276(3) 0.83780(6) 0.01316(14) Uani 1 1 d . . . . .
C1 C 0.7777(4) 0.55766(13) 0.4894(3) 0.0103(6) Uani 1 1 d . . . . .
O1 O 0.6610(3) 0.57359(9) 0.3746(2) 0.0114(4) Uani 1 1 d . . . . .
O2 O 0.7428(3) 0.52913(10) 0.5846(2) 0.0123(4) Uani 1 1 d . . . . .
C2 C 0.9763(4) 0.57734(13) 0.4998(3) 0.0102(6) Uani 1 1 d . . . . .
O3 O 0.9942(3) 0.61015(10) 0.3967(2) 0.0115(4) Uani 1 1 d . . . . .
O4 O 1.1016(3) 0.55999(10) 0.6004(2) 0.0123(4) Uani 1 1 d . . . . .
C3 C 0.5272(4) 0.58656(14) 0.0018(3) 0.0106(6) Uani 1 1 d . . . . .
O5 O 0.5263(3) 0.62267(10) 0.1062(2) 0.0131(4) Uani 1 1 d . . . . .
O6 O 0.3954(3) 0.57530(10) -0.0979(2) 0.0159(4) Uani 1 1 d . . . . .
C4 C 0.7146(4) 0.55477(14) 0.0107(3) 0.0110(6) Uani 1 1 d . . . . .
O7 O 0.8379(3) 0.56573(9) 0.1257(2) 0.0119(4) Uani 1 1 d . . . . .
O8 O 0.7352(3) 0.52228(10) -0.0847(2) 0.0135(4) Uani 1 1 d . . . . .
C5 C 0.7396(4) 0.77215(15) 0.2960(3) 0.0164(6) Uani 1 1 d . . . . .
O9 O 0.6846(3) 0.71511(10) 0.3302(2) 0.0163(4) Uani 1 1 d . . . . .
O10 O 0.6972(3) 0.82823(11) 0.3251(2) 0.0256(5) Uani 1 1 d . . . . .
C6 C 0.8683(4) 0.76451(15) 0.2076(3) 0.0184(7) Uani 1 1 d . . . . .
O11 O 0.8883(3) 0.70295(10) 0.1742(2) 0.0185(5) Uani 1 1 d . . . . .
O12 O 0.9412(3) 0.81401(11) 0.1750(2) 0.0272(6) Uani 1 1 d . . . . .
O13 O 0.1145(3) 0.66711(12) 0.0263(2) 0.0275(6) Uani 1 1 d . . . . .
H13A H 0.020334 0.689778 0.031581 0.041 Uiso 1 1 calc R U . . .
H13B H 0.195096 0.694756 0.012906 0.041 Uiso 1 1 calc R U . . .
O15 O 0.2931(3) 0.70934(12) 0.6604(3) 0.0332(6) Uani 1 1 d . . . . .
H15A H 0.341633 0.730503 0.738021 0.050 Uiso 1 1 d R U . . .
H15B H 0.178879 0.704497 0.657526 0.050 Uiso 1 1 d R U . . .
O14A O 0.4147(15) 0.6795(5) 0.4513(9) 0.031(2) Uani 0.5 1 d . . P A 1
H14A H 0.341511 0.712072 0.456924 0.047 Uiso 0.5 1 calc R U P A 1
H14B H 0.516786 0.695614 0.445036 0.047 Uiso 0.5 1 calc R U P A 1
O14B O 0.3841(14) 0.6988(5) 0.4062(10) 0.0273(19) Uani 0.5 1 d . . P A 2
H14C H 0.377975 0.693892 0.492475 0.041 Uiso 0.5 1 d R U P A 2
H14D H 0.309923 0.734406 0.373895 0.041 Uiso 0.5 1 d R U P A 2


_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
Fe O5 1.985(2) . ?
Fe O3 1.991(2) . ?
Fe O11 2.010(2) . ?
Fe O9 2.018(2) . ?
Fe O1 2.0314(19) . ?
Fe O7 2.0327(19) . ?
K1 O14B 2.723(11) . ?
K1 O14A 2.734(11) . ?
K1 O13 2.772(3) . ?
K1 O8 2.777(2) 3_665 ?
K1 O2 2.824(2) 3_666 ?
K1 O3 2.885(2) 1_455 ?
K1 O1 2.987(2) . ?
K1 O5 3.000(2) . ?
K1 O7 3.137(2) 1_455 ?
K2 O6 2.652(2) 1_556 ?
K2 O4 2.680(2) 1_455 ?
K2 O2 2.715(2) . ?
K2 O10 2.768(2) 4_576 ?
K2 O14A 2.899(8) . ?
K2 O15 2.899(3) . ?
K2 O8 3.012(2) 1_556 ?
K2 O1 3.141(2) 3_666 ?
K2 O2 3.324(2) 3_666 ?
K3 O13 2.627(2) 1_656 ?
K3 O4 2.689(2) . ?
K3 O6 2.736(2) 1_656 ?
K3 O12 2.753(2) 4_576 ?
K3 O8 2.774(2) 1_556 ?
K3 O7 2.923(2) 3_766 ?
K3 O2 2.967(2) . ?
K3 O10 3.169(2) 4_576 ?
K3 O8 3.248(2) 3_766 ?
C1 O2 1.228(3) . ?
C1 O1 1.287(3) . ?
C1 C2 1.553(4) . ?
C2 O4 1.230(3) . ?
C2 O3 1.285(3) . ?
C3 O6 1.225(3) . ?
C3 O5 1.290(3) . ?
C3 C4 1.554(4) . ?
C4 O8 1.221(3) . ?
C4 O7 1.291(3) . ?
C5 O10 1.220(4) . ?
C5 O9 1.292(4) . ?
C5 C6 1.542(4) . ?
C6 O12 1.225(4) . ?
C6 O11 1.288(4) . ?
O13 H13A 0.8700 . ?
O13 H13B 0.8700 . ?
O15 H15A 0.8775 . ?
O15 H15B 0.8781 . ?
O14A H14A 0.8700 . ?
O14A H14B 0.8700 . ?
O14B H14C 0.9059 . ?
O14B H14D 0.9047 . ?

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
O5 Fe O3 162.93(8) . . ?
O5 Fe O11 102.00(9) . . ?
O3 Fe O11 90.86(9) . . ?
O5 Fe O9 92.95(8) . . ?
O3 Fe O9 100.51(8) . . ?
O11 Fe O9 79.35(8) . . ?
O5 Fe O1 88.64(8) . . ?
O3 Fe O1 81.05(8) . . ?
O11 Fe O1 164.96(8) . . ?
O9 Fe O1 89.62(8) . . ?
O5 Fe O7 80.94(8) . . ?
O3 Fe O7 88.80(8) . . ?
O11 Fe O7 86.45(8) . . ?
O9 Fe O7 163.06(8) . . ?
O1 Fe O7 105.90(8) . . ?
O14B K1 O13 89.66(16) . . ?
O14A K1 O13 102.09(16) . . ?
O14A K1 O8 154.0(2) . 3_665 ?
O13 K1 O8 89.83(7) . 3_665 ?
O14A K1 O2 101.06(17) . 3_666 ?
O13 K1 O2 152.83(7) . 3_666 ?
O8 K1 O2 75.12(6) 3_665 3_666 ?
O14A K1 O3 74.7(2) . 1_455 ?
O13 K1 O3 99.78(6) . 1_455 ?
O8 K1 O3 126.40(6) 3_665 1_455 ?
O2 K1 O3 72.97(6) 3_666 1_455 ?
O14B K1 O1 71.75(19) . . ?
O14A K1 O1 65.2(2) . . ?
O13 K1 O1 119.90(6) . . ?
O8 K1 O1 88.83(6) 3_665 . ?
O2 K1 O1 82.90(6) 3_666 . ?
O3 K1 O1 127.62(6) 1_455 . ?
O14B K1 O5 85.0(2) . . ?
O14A K1 O5 89.7(2) . . ?
O13 K1 O5 66.18(6) . . ?
O8 K1 O5 73.90(6) 3_665 . ?
O2 K1 O5 127.98(6) 3_666 . ?
O3 K1 O5 156.75(6) 1_455 . ?
O1 K1 O5 55.91(5) . . ?
O14A K1 O7 124.6(2) . 1_455 ?
O13 K1 O7 67.79(6) . 1_455 ?
O8 K1 O7 81.28(6) 3_665 1_455 ?
O2 K1 O7 87.37(6) 3_666 1_455 ?
O3 K1 O7 55.56(5) 1_455 1_455 ?
O1 K1 O7 167.63(6) . 1_455 ?
O5 K1 O7 127.04(6) . 1_455 ?
O6 K2 O4 75.13(6) 1_556 1_455 ?
O6 K2 O2 131.44(7) 1_556 . ?
O4 K2 O2 138.08(6) 1_455 . ?
O6 K2 O10 74.67(7) 1_556 4_576 ?
O4 K2 O10 132.80(7) 1_455 4_576 ?
O2 K2 O10 88.81(7) . 4_576 ?
O6 K2 O14A 133.9(2) 1_556 . ?
O4 K2 O14A 91.6(2) 1_455 . ?
O2 K2 O14A 87.4(2) . . ?
O10 K2 O14A 84.1(2) 4_576 . ?
O6 K2 O15 79.50(7) 1_556 . ?
O4 K2 O15 71.89(7) 1_455 . ?
O2 K2 O15 135.62(7) . . ?
O10 K2 O15 67.58(7) 4_576 . ?
O14A K2 O15 54.5(2) . . ?
O6 K2 O8 58.60(6) 1_556 1_556 ?
O4 K2 O8 124.25(6) 1_455 1_556 ?
O2 K2 O8 73.00(6) . 1_556 ?
O10 K2 O8 64.44(6) 4_576 1_556 ?
O14A K2 O8 142.6(2) . 1_556 ?
O15 K2 O8 122.27(7) . 1_556 ?
O6 K2 O1 87.57(6) 1_556 3_666 ?
O4 K2 O1 65.75(6) 1_455 3_666 ?
O2 K2 O1 81.84(6) . 3_666 ?
O10 K2 O1 146.39(6) 4_576 3_666 ?
O14A K2 O1 127.2(2) . 3_666 ?
O15 K2 O1 137.58(7) . 3_666 ?
O8 K2 O1 81.96(5) 1_556 3_666 ?
O6 K2 O2 120.88(6) 1_556 3_666 ?
O4 K2 O2 60.81(5) 1_455 3_666 ?
O2 K2 O2 77.30(6) . 3_666 ?
O10 K2 O2 163.79(6) 4_576 3_666 ?
O14A K2 O2 86.9(2) . 3_666 ?
O15 K2 O2 117.23(7) . 3_666 ?
O8 K2 O2 117.93(5) 1_556 3_666 ?
O1 K2 O2 40.32(5) 3_666 3_666 ?
O13 K3 O4 130.72(7) 1_656 . ?
O13 K3 O6 77.61(7) 1_656 1_656 ?
O4 K3 O6 73.62(6) . 1_656 ?
O13 K3 O12 80.13(7) 1_656 4_576 ?
O4 K3 O12 66.55(6) . 4_576 ?
O6 K3 O12 99.58(7) 1_656 4_576 ?
O13 K3 O8 95.81(7) 1_656 1_556 ?
O4 K3 O8 130.10(6) . 1_556 ?
O6 K3 O8 144.26(7) 1_656 1_556 ?
O12 K3 O8 114.01(7) 4_576 1_556 ?
O13 K3 O7 124.62(7) 1_656 3_766 ?
O4 K3 O7 81.75(6) . 3_766 ?
O6 K3 O7 70.95(6) 1_656 3_766 ?
O12 K3 O7 148.28(6) 4_576 3_766 ?
O8 K3 O7 85.30(6) 1_556 3_766 ?
O13 K3 O2 144.30(7) 1_656 . ?
O4 K3 O2 58.91(6) . . ?
O6 K3 O2 130.71(6) 1_656 . ?
O12 K3 O2 74.41(7) 4_576 . ?
O8 K3 O2 72.91(6) 1_556 . ?
O7 K3 O2 88.88(6) 3_766 . ?
O13 K3 O10 67.66(7) 1_656 4_576 ?
O4 K3 O10 114.40(6) . 4_576 ?
O6 K3 O10 139.57(6) 1_656 4_576 ?
O12 K3 O10 55.55(6) 4_576 4_576 ?
O8 K3 O10 62.21(6) 1_556 4_576 ?
O7 K3 O10 147.10(6) 3_766 4_576 ?
O2 K3 O10 77.32(6) . 4_576 ?
O13 K3 O8 82.91(7) 1_656 3_766 ?
O4 K3 O8 114.94(6) . 3_766 ?
O6 K3 O8 60.94(6) 1_656 3_766 ?
O12 K3 O8 156.67(7) 4_576 3_766 ?
O8 K3 O8 83.48(6) 1_556 3_766 ?
O7 K3 O8 42.04(5) 3_766 3_766 ?
O2 K3 O8 127.45(6) . 3_766 ?
O10 K3 O8 130.54(6) 4_576 3_766 ?
Fe O1 K1 104.24(7) . . ?
C1 O1 K2 88.83(15) . 3_666 ?
Fe O1 K2 128.36(8) . 3_666 ?
K1 O1 K2 78.08(5) . 3_666 ?
C1 O2 K2 117.35(17) . . ?
C1 O2 K1 151.59(18) . 3_666 ?
K2 O2 K1 88.38(6) . 3_666 ?
C1 O2 K3 106.50(17) . . ?
K2 O2 K3 94.31(6) . . ?
K1 O2 K3 81.63(5) 3_666 . ?
C1 O2 K2 81.54(16) . 3_666 ?
K2 O2 K2 102.70(6) . 3_666 ?
K1 O2 K2 81.09(5) 3_666 3_666 ?
K3 O2 K2 155.29(7) . 3_666 ?
O4 C2 O3 125.4(3) . . ?
O4 C2 C1 119.7(2) . . ?
O3 C2 C1 114.8(2) . . ?
O4 C2 K3 46.87(14) . . ?
O3 C2 K3 148.68(18) . . ?
C1 C2 K3 82.17(15) . . ?
C2 O3 Fe 115.31(17) . . ?
C2 O3 K1 127.17(17) . 1_655 ?
Fe O3 K1 105.36(8) . 1_655 ?
C2 O4 K2 131.16(18) . 1_655 ?
C2 O4 K3 113.62(17) . . ?
K2 O4 K3 105.49(7) 1_655 . ?
O6 C3 O5 125.6(3) . . ?
O6 C3 C4 119.9(2) . . ?
O5 C3 C4 114.5(2) . . ?
O6 C3 K2 45.63(14) . 1_554 ?
O5 C3 K2 148.10(19) . 1_554 ?
C4 C3 K2 83.52(15) . 1_554 ?
C3 O5 Fe 115.82(18) . . ?
C3 O5 K1 117.78(16) . . ?
Fe O5 K1 105.05(8) . . ?
C3 O6 K2 115.09(17) . 1_554 ?
C3 O6 K3 138.44(18) . 1_454 ?
K2 O6 K3 104.94(7) 1_554 1_454 ?
O8 C4 O7 125.6(3) . . ?
O8 C4 C3 120.7(3) . . ?
O7 C4 C3 113.6(2) . . ?
O8 C4 K3 76.48(16) . 3_766 ?
O7 C4 K3 61.54(14) . 3_766 ?
C3 C4 K3 139.42(17) . 3_766 ?
O8 C4 K3 49.76(14) . 1_554 ?
O7 C4 K3 91.12(16) . 1_554 ?
C3 C4 K3 135.70(17) . 1_554 ?
K3 C4 K3 84.32(7) 3_766 1_554 ?
O8 C4 K2 55.11(15) . 1_554 ?
O7 C4 K2 158.18(18) . 1_554 ?
C3 C4 K2 70.61(14) . 1_554 ?
K3 C4 K2 130.19(9) 3_766 1_554 ?
K3 C4 K2 73.81(6) 1_554 1_554 ?
C4 O7 Fe 114.56(17) . . ?
C4 O7 K3 95.62(16) . 3_766 ?
Fe O7 K3 132.81(9) . 3_766 ?
C4 O7 K1 142.02(17) . 1_655 ?
Fe O7 K1 96.11(7) . 1_655 ?
K3 O7 K1 77.24(5) 3_766 1_655 ?
C4 O8 K3 110.60(17) . 1_554 ?
C4 O8 K1 160.32(18) . 3_665 ?
K3 O8 K1 86.03(6) 1_554 3_665 ?
C4 O8 K2 105.47(17) . 1_554 ?
K3 O8 K2 92.11(6) 1_554 1_554 ?
K1 O8 K2 83.58(6) 3_665 1_554 ?
C4 O8 K3 82.09(16) . 3_766 ?
K3 O8 K3 96.52(6) 1_554 3_766 ?
K1 O8 K3 85.72(5) 3_665 3_766 ?
K2 O8 K3 165.75(7) 1_554 3_766 ?
O10 C5 O9 126.5(3) . . ?
O10 C5 C6 120.1(3) . . ?
O9 C5 C6 113.4(2) . . ?
C5 O9 Fe 116.58(19) . . ?
C5 O10 K2 129.6(2) . 4_575 ?
C5 O10 K3 107.7(2) . 4_575 ?
K2 O10 K3 88.94(6) 4_575 4_575 ?
O12 C6 O11 125.7(3) . . ?
O12 C6 C5 120.8(3) . . ?
O11 C6 C5 113.5(3) . . ?
C6 O11 Fe 116.95(19) . . ?
C6 O12 K3 121.9(2) . 4_575 ?
K3 O13 K1 99.21(8) 1_454 . ?
K3 O13 H13A 111.9 1_454 . ?
K1 O13 H13A 111.9 . . ?
K3 O13 H13B 111.9 1_454 . ?
K1 O13 H13B 111.9 . . ?
H13A O13 H13B 109.6 . . ?
K2 O15 H15A 110.6 . . ?
K2 O15 H15B 110.2 . . ?
H15A O15 H15B 103.3 . . ?
K1 O14A K2 90.9(3) . . ?
K1 O14A H14A 113.5 . . ?
K2 O14A H14A 113.5 . . ?
K1 O14A H14B 113.5 . . ?
K2 O14A H14B 113.5 . . ?
H14A O14A H14B 110.8 . . ?
K1 O14B H14C 110.9 . . ?
K1 O14B H14D 110.5 . . ?
H14C O14B H14D 103.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O13 H13A O11 0.87 2.04 2.732(3) 136.0 1_455 yes
O13 H13B O15 0.87 2.40 2.937(3) 120.1 4_575 yes
O15 H15B O12 0.88 1.93 2.803(4) 171.6 4_476 yes

_refine_diff_density_max         0.812
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.108

