# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 2225058'
loop_
_audit_author_name
_audit_author_address
'Catherine Raptopoulou'
;NCSR Demokritos
Greece
;
_audit_update_record             
;
2022-12-07 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31.80 H33.70 Cl6 Fe4 N4.70 O6.40'
_chemical_formula_weight         1020.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'y, x, -z+1/2'
'-x+y, -x, z'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'-y, -x, z-1/2'
'x-y, x, -z'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x-y+2/3, x+1/3, -z+1/3'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x-y+1/3, x+2/3, -z+2/3'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'

_cell_length_a                   34.0344(2)
_cell_length_b                   34.0344(2)
_cell_length_c                   21.8653(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     21934.2(4)
_cell_formula_units_Z            18
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    23647
_cell_measurement_theta_min      6.61
_cell_measurement_theta_max      71.87

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_F_000             9263
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    12.726
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32103
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_av_R_equivalents  0.1231
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         6.607
_diffrn_reflns_theta_max         64.994
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.932
_reflns_number_total             4124
_reflns_number_gt                3032
_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       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0751P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4124
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1583
_refine_ls_wR_factor_gt          0.1346
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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
Fe1 Fe 0.23430(2) 0.85980(2) 0.03687(4) 0.0282(2) Uani 1 1 d . . . . .
Fe2 Fe 0.17571(2) 0.75192(2) 0.01262(4) 0.0321(3) Uani 1 1 d . . . . .
Cl1 Cl 0.31023(4) 0.90778(4) 0.03261(6) 0.0407(4) Uani 1 1 d . . . . .
Cl2 Cl 0.17230(4) 0.70254(4) 0.08119(6) 0.0504(4) Uani 1 1 d . . . . .
Cl3 Cl 0.18419(5) 0.73271(5) -0.08065(7) 0.0549(4) Uani 1 1 d . . . . .
N1 N 0.22785(13) 0.87362(12) -0.05712(18) 0.0327(10) Uani 1 1 d . . . . .
N2 N 0.10404(13) 0.72659(12) 0.00727(18) 0.0347(10) Uani 1 1 d . . . . .
O1 O 0.20096(10) 0.89496(9) 0.04085(14) 0.0282(8) Uani 1 1 d . . . . .
O2 O 0.16912(9) 0.80574(9) 0.02085(13) 0.0301(8) Uani 1 1 d . . . . .
O3 O 0.23681(10) 0.80315(10) 0.02854(15) 0.0350(8) Uani 1 1 d . . . . .
C1 C 0.24972(18) 0.86740(18) -0.1050(3) 0.0421(14) Uani 1 1 d . . . . .
C2 C 0.24168(18) 0.87474(18) -0.1644(3) 0.0435(15) Uani 1 1 d . . . . .
C3 C 0.21048(19) 0.88882(18) -0.1751(3) 0.0475(15) Uani 1 1 d . . . . .
C4 C 0.18831(18) 0.89526(16) -0.1262(3) 0.0390(14) Uani 1 1 d . . . . .
C5 C 0.19759(15) 0.88706(14) -0.0673(2) 0.0288(11) Uani 1 1 d . . . . .
C6 C 0.17186(16) 0.88857(15) -0.0109(2) 0.0297(11) Uani 1 1 d . . . . .
C7 C 0.12917(15) 0.84267(15) -0.0074(2) 0.0289(12) Uani 1 1 d . . . . .
H7 H 0.1038(15) 0.8390(15) -0.013(2) 0.038 Uiso 1 1 d . U . . .
C8 C 0.12989(15) 0.80521(15) 0.0063(2) 0.0288(11) Uani 1 1 d . . . . .
C9 C 0.09109(15) 0.75830(15) 0.0043(2) 0.0284(11) Uani 1 1 d . . . . .
C10 C 0.04624(17) 0.74629(17) -0.0008(2) 0.0365(13) Uani 1 1 d . . . . .
C11 C 0.01337(17) 0.70139(17) -0.0039(2) 0.0437(14) Uani 1 1 d . . . . .
H11 H -0.0177 0.6928 -0.0078 0.057 Uiso 1 1 calc R U . . .
C12 C 0.02627(19) 0.66873(19) -0.0012(3) 0.0511(16) Uani 1 1 d . . . . .
C13 C 0.07172(18) 0.68242(18) 0.0045(3) 0.0462(15) Uani 1 1 d . . . . .
C14 C 0.16207(17) 0.92749(16) -0.0130(3) 0.0426(14) Uani 1 1 d . . . . .
H14A H 0.1907 0.9564 -0.0137 0.064 Uiso 1 1 calc R U . . .
H14B H 0.1445 0.9263 0.0232 0.064 Uiso 1 1 calc R U . . .
H14C H 0.1446 0.9249 -0.0500 0.064 Uiso 1 1 calc R U . . .
C15 C 0.27592(18) 0.79696(19) 0.0226(3) 0.0643(19) Uani 1 1 d . . . . .
H15A H 0.2693 0.7683 0.0419 0.096 Uiso 1 1 calc R U . . .
H15B H 0.3022 0.8222 0.0426 0.096 Uiso 1 1 calc R U . . .
H15C H 0.2826 0.7962 -0.0209 0.096 Uiso 1 1 calc R U . . .
H1 H 0.2729(14) 0.8584(14) -0.0909(18) 0.027(12) Uiso 1 1 d . . . . .
H2 H 0.2547(17) 0.8715(16) -0.202(2) 0.054(17) Uiso 1 1 d . . . . .
H3 H 0.2042(16) 0.8974(16) -0.218(2) 0.051(16) Uiso 1 1 d . . . . .
H4 H 0.1665(16) 0.9041(16) -0.129(2) 0.046(16) Uiso 1 1 d . . . . .
H10 H 0.0398(14) 0.7685(13) -0.0010(18) 0.024(12) Uiso 1 1 d . . . . .
H12 H 0.0030(18) 0.6377(18) -0.004(2) 0.062(17) Uiso 1 1 d . . . . .
H13 H 0.0823(16) 0.6602(17) 0.002(2) 0.051(16) Uiso 1 1 d . . . . .
N1S N 0.3953(7) 0.8510(7) 0.0508(9) 0.113(7) Uiso 0.35 1 d . . P A 1
C1S C 0.3997(7) 0.8238(8) 0.0312(11) 0.094(7) Uiso 0.35 1 d . . P A 1
C2S C 0.4062(8) 0.7868(9) 0.0114(12) 0.112(8) Uiso 0.35 1 d . . P A 1
O1M O 0.4189(17) 0.7655(18) -0.026(2) 0.095(16) Uiso 0.1 1 d . . P B 2
C1M C 0.376(2) 0.761(2) -0.031(3) 0.08(2) Uiso 0.1 1 d . . P B 2
O2M O 0.080(2) 0.994(3) 0.023(3) 0.16(3) Uiso 0.1 1 d . . P . .
C2M C 0.044(3) 0.955(3) 0.015(4) 0.09(2) Uiso 0.1 1 d . . P . .


_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 O3 1.981(3) . ?
Fe1 O1 1.987(3) 15_454 ?
Fe1 O1 2.021(3) . ?
Fe1 O2 2.085(3) . ?
Fe1 N1 2.144(4) . ?
Fe1 Cl1 2.2656(13) . ?
Fe2 O2 1.962(3) . ?
Fe2 O3 1.965(3) . ?
Fe2 N2 2.146(4) . ?
Fe2 Cl3 2.2043(16) . ?
Fe2 Cl2 2.2116(15) . ?
N1 C5 1.338(5) . ?
N1 C1 1.361(6) . ?
N2 C13 1.349(6) . ?
N2 C9 1.356(5) . ?
O1 C6 1.446(5) . ?
O1 Fe1 1.987(3) 15_454 ?
O2 C8 1.364(5) . ?
O3 C15 1.454(6) . ?
C1 C2 1.376(8) . ?
C1 H1 1.02(4) . ?
C2 C3 1.386(8) . ?
C2 H2 0.97(5) . ?
C3 C4 1.388(8) . ?
C3 H3 1.03(5) . ?
C4 C5 1.387(7) . ?
C4 H4 0.93(5) . ?
C5 C6 1.529(6) . ?
C6 C7 1.512(6) . ?
C6 C14 1.520(6) . ?
C7 C8 1.322(6) . ?
C7 H7 0.82(4) . ?
C8 C9 1.478(6) . ?
C9 C10 1.373(6) . ?
C10 C11 1.372(6) . ?
C10 H10 0.89(4) . ?
C11 C12 1.385(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.380(7) . ?
C12 H12 0.95(5) . ?
C13 H13 0.99(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N1S C1S 1.10(3) . ?
C1S C2S 1.45(3) . ?
O1M C1M 1.41(8) . ?
O2M C2M 1.28(9) . ?
O2M C2M 1.78(9) 22_665 ?
C2M O2M 1.78(9) 20_455 ?

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
O3 Fe1 O1 106.13(13) . 15_454 ?
O3 Fe1 O1 152.95(12) . . ?
O1 Fe1 O1 75.68(14) 15_454 . ?
O3 Fe1 O2 70.75(12) . . ?
O1 Fe1 O2 98.47(12) 15_454 . ?
O1 Fe1 O2 82.25(11) . . ?
O3 Fe1 N1 100.62(14) . . ?
O1 Fe1 N1 151.65(14) 15_454 . ?
O1 Fe1 N1 76.24(14) . . ?
O2 Fe1 N1 81.49(13) . . ?
O3 Fe1 Cl1 96.25(9) . . ?
O1 Fe1 Cl1 95.76(9) 15_454 . ?
O1 Fe1 Cl1 110.54(9) . . ?
O2 Fe1 Cl1 162.93(9) . . ?
N1 Fe1 Cl1 90.43(11) . . ?
O2 Fe2 O3 73.73(12) . . ?
O2 Fe2 N2 75.07(13) . . ?
O3 Fe2 N2 148.49(13) . . ?
O2 Fe2 Cl3 117.05(10) . . ?
O3 Fe2 Cl3 100.93(11) . . ?
N2 Fe2 Cl3 96.98(12) . . ?
O2 Fe2 Cl2 131.33(10) . . ?
O3 Fe2 Cl2 100.62(10) . . ?
N2 Fe2 Cl2 96.58(11) . . ?
Cl3 Fe2 Cl2 111.51(6) . . ?
C5 N1 C1 120.0(5) . . ?
C5 N1 Fe1 114.5(3) . . ?
C1 N1 Fe1 125.4(4) . . ?
C13 N2 C9 118.4(4) . . ?
C13 N2 Fe2 125.4(3) . . ?
C9 N2 Fe2 116.1(3) . . ?
C6 O1 Fe1 131.6(3) . 15_454 ?
C6 O1 Fe1 115.0(2) . . ?
Fe1 O1 Fe1 104.29(14) 15_454 . ?
C8 O2 Fe2 122.3(2) . . ?
C8 O2 Fe1 130.8(2) . . ?
Fe2 O2 Fe1 105.75(13) . . ?
C15 O3 Fe2 119.7(3) . . ?
C15 O3 Fe1 129.6(3) . . ?
Fe2 O3 Fe1 109.77(14) . . ?
N1 C1 C2 121.6(5) . . ?
N1 C1 H1 112(2) . . ?
C2 C1 H1 126(2) . . ?
C1 C2 C3 118.6(6) . . ?
C1 C2 H2 130(3) . . ?
C3 C2 H2 111(3) . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3 124(3) . . ?
C4 C3 H3 117(3) . . ?
C5 C4 C3 119.2(6) . . ?
C5 C4 H4 115(3) . . ?
C3 C4 H4 126(3) . . ?
N1 C5 C4 121.0(5) . . ?
N1 C5 C6 115.4(4) . . ?
C4 C5 C6 123.4(5) . . ?
O1 C6 C7 110.4(4) . . ?
O1 C6 C14 109.0(4) . . ?
C7 C6 C14 112.7(4) . . ?
O1 C6 C5 106.0(4) . . ?
C7 C6 C5 106.1(4) . . ?
C14 C6 C5 112.5(4) . . ?
C8 C7 C6 122.4(4) . . ?
C8 C7 H7 114(3) . . ?
C6 C7 H7 123(3) . . ?
C7 C8 O2 122.0(4) . . ?
C7 C8 C9 126.7(4) . . ?
O2 C8 C9 111.2(4) . . ?
N2 C9 C10 121.5(4) . . ?
N2 C9 C8 112.8(4) . . ?
C10 C9 C8 125.7(4) . . ?
C11 C10 C9 120.1(5) . . ?
C11 C10 H10 123(3) . . ?
C9 C10 H10 117(3) . . ?
C10 C11 C12 118.9(5) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 119.0(5) . . ?
C13 C12 H12 123(3) . . ?
C11 C12 H12 118(3) . . ?
N2 C13 C12 122.1(5) . . ?
N2 C13 H13 117(3) . . ?
C12 C13 H13 121(3) . . ?
C6 C14 H14A 109.5 . . ?
C6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1S C1S C2S 174(3) . . ?
C2M O2M C2M 123(7) . 22_665 ?
O2M C2M O2M 156(7) . 20_455 ?

_refine_diff_density_max         0.586
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.098

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_shelxl_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2225059'
loop_
_audit_author_name
_audit_author_address
'Catherine Raptopoulou'
;NCSR Demokritos
Greece
;
_audit_update_record             
;
2022-12-07 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H32.40 Cl4 Fe3 N3 O8.20'
_chemical_formula_weight         803.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   11.0768(2)
_cell_length_b                   12.9640(2)
_cell_length_c                   13.9148(3)
_cell_angle_alpha                112.9060(10)
_cell_angle_beta                 101.9300(10)
_cell_angle_gamma                105.5150(10)
_cell_volume                     1661.21(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    17569
_cell_measurement_theta_min      6.52
_cell_measurement_theta_max      71.88

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_F_000             818
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    13.743
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21930
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         6.525
_diffrn_reflns_theta_max         62.491
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.834
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.834
_reflns_number_total             5011
_reflns_number_gt                3356
_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       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0329P)²+10.0246P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5011
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1591
_refine_ls_wR_factor_gt          0.1115
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.002
_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
Fe1 Fe 0.17488(11) 0.12083(9) 0.86417(8) 0.0181(3) Uani 1 1 d . . . . .
Fe2 Fe 0.25264(10) 0.22834(9) 0.70839(8) 0.0157(3) Uani 1 1 d . . . . .
Fe3 Fe 0.12172(12) 0.36731(10) 0.60715(9) 0.0245(3) Uani 1 1 d . . . . .
Cl1 Cl -0.0215(2) -0.01629(17) 0.82687(15) 0.0379(5) Uani 1 1 d . . . . .
Cl2 Cl 0.3427(2) 0.08702(18) 0.94791(15) 0.0354(5) Uani 1 1 d . . . . .
Cl3 Cl -0.0977(2) 0.32145(18) 0.55319(17) 0.0437(6) Uani 1 1 d . . . . .
Cl4 Cl 0.2011(3) 0.4032(2) 0.48488(17) 0.0543(7) Uani 1 1 d . . . . .
N1 N 0.1792(6) 0.2574(5) 1.0133(4) 0.0243(15) Uani 1 1 d . . . . .
N2 N 0.1642(6) 0.5460(5) 0.7240(5) 0.0275(15) Uani 1 1 d . . . . .
N3 N 0.3150(6) 0.1145(5) 0.5782(4) 0.0208(14) Uani 1 1 d . . . . .
O1 O 0.1791(4) 0.2568(4) 0.8322(3) 0.0161(10) Uani 1 1 d . . . . .
O2 O 0.2620(4) 0.3950(4) 0.7359(3) 0.0178(11) Uani 1 1 d . . . . .
O3 O 0.0689(5) 0.3891(4) 0.8577(4) 0.0307(13) Uani 1 1 d . . . . .
O4 O 0.1201(4) 0.2023(4) 0.5722(3) 0.0198(11) Uani 1 1 d . . . . .
O5 O 0.1982(5) 0.0740(4) 0.7196(3) 0.0192(11) Uani 1 1 d . . . . .
O6 O 0.4419(5) 0.2857(4) 0.7934(4) 0.0222(11) Uani 1 1 d . . . . .
O7 O 0.6349(5) 0.2654(5) 0.8000(4) 0.0402(15) Uani 1 1 d . . . . .
O8 O 0.4965(7) 0.8887(7) 0.6137(6) 0.072(2) Uani 1 1 d . . . . .
C1 C 0.1797(8) 0.2451(7) 1.1045(6) 0.0302(19) Uani 1 1 d . . . . .
H1 H 0.1829 0.1728 1.1050 0.042 Uiso 1 1 calc R U . . .
C2 C 0.1757(9) 0.3339(8) 1.1977(6) 0.044(2) Uani 1 1 d . . . . .
H2 H 0.1776 0.3239 1.2620 0.062 Uiso 1 1 calc R U . . .
C3 C 0.1689(10) 0.4375(8) 1.1953(7) 0.054(3) Uani 1 1 d . . . . .
H3 H 0.1666 0.5005 1.2585 0.075 Uiso 1 1 calc R U . . .
C4 C 0.1655(9) 0.4489(7) 1.1006(7) 0.040(2) Uani 1 1 d . . . . .
H4 H 0.1583 0.5187 1.0968 0.056 Uiso 1 1 calc R U . . .
C5 C 0.1728(7) 0.3569(6) 1.0110(6) 0.0235(17) Uani 1 1 d . . . . .
C6 C 0.1784(7) 0.3664(6) 0.9067(5) 0.0178(16) Uani 1 1 d . . . . .
C7 C 0.3039(7) 0.4721(6) 0.9338(5) 0.0196(16) Uani 1 1 d . . . . .
H7A H 0.3823 0.4541 0.9593 0.023 Uiso 1 1 calc R U . . .
H7B H 0.3088 0.5451 0.9973 0.023 Uiso 1 1 calc R U . . .
C8 C 0.3175(7) 0.5044(6) 0.8399(5) 0.0187(16) Uani 1 1 d . . . . .
C9 C 0.2434(7) 0.5857(7) 0.8281(6) 0.0270(19) Uani 1 1 d . . . . .
C10 C 0.2664(8) 0.6959(7) 0.9148(6) 0.033(2) Uani 1 1 d . . . . .
H10 H 0.3206 0.7204 0.9885 0.046 Uiso 1 1 calc R U . . .
C11 C 0.2087(9) 0.7698(7) 0.8920(7) 0.048(3) Uani 1 1 d . . . . .
H11 H 0.2237 0.8467 0.9500 0.067 Uiso 1 1 calc R U . . .
C12 C 0.1289(9) 0.7308(7) 0.7838(7) 0.041(2) Uani 1 1 d . . . . .
H12 H 0.0897 0.7810 0.7664 0.058 Uiso 1 1 calc R U . . .
C13 C 0.1075(9) 0.6193(8) 0.7032(7) 0.039(2) Uani 1 1 d . . . . .
H13 H 0.0508 0.5918 0.6295 0.055 Uiso 1 1 calc R U . . .
C14 C -0.0595(8) 0.2944(8) 0.8219(8) 0.047(2) Uani 1 1 d . . . . .
H14A H -0.1292 0.3111 0.7817 0.066 Uiso 1 1 calc R U . . .
H14B H -0.0776 0.2915 0.8870 0.066 Uiso 1 1 calc R U . . .
H14C H -0.0591 0.2162 0.7726 0.066 Uiso 1 1 calc R U . . .
C15 C 0.4647(6) 0.5681(7) 0.8592(6) 0.0265(18) Uani 1 1 d . . . . .
H15A H 0.5116 0.5139 0.8597 0.037 Uiso 1 1 calc R U . . .
H15B H 0.5057 0.6424 0.9310 0.037 Uiso 1 1 calc R U . . .
H15C H 0.4712 0.5889 0.7994 0.037 Uiso 1 1 calc R U . . .
C16 C 0.1177(7) 0.1186(7) 0.4667(5) 0.0249(16) Uani 1 1 d . . . . .
H16A H 0.0845 0.1408 0.4089 0.030 Uiso 1 1 calc R U . . .
H16B H 0.0565 0.0355 0.4447 0.030 Uiso 1 1 calc R U . . .
C17 C 0.2590(7) 0.1222(7) 0.4763(6) 0.0245(17) Uani 1 1 d . . . . .
H17A H 0.2561 0.0532 0.4101 0.029 Uiso 1 1 calc R U . . .
H17B H 0.3155 0.1987 0.4809 0.029 Uiso 1 1 calc R U . . .
C18 C 0.2552(7) -0.0126(6) 0.5599(6) 0.0215(16) Uani 1 1 d . . . . .
H18A H 0.3068 -0.0598 0.5277 0.026 Uiso 1 1 calc R U . . .
H18B H 0.1618 -0.0529 0.5073 0.026 Uiso 1 1 calc R U . . .
C19 C 0.2587(8) -0.0077(6) 0.6708(5) 0.0233(17) Uani 1 1 d . . . . .
H19A H 0.2088 -0.0895 0.6600 0.028 Uiso 1 1 calc R U . . .
H19B H 0.3522 0.0214 0.7199 0.028 Uiso 1 1 calc R U . . .
C20 C 0.4628(7) 0.1628(7) 0.6219(6) 0.0308(19) Uani 1 1 d . . . . .
H20A H 0.4982 0.2110 0.5863 0.037 Uiso 1 1 calc R U . . .
H20B H 0.4928 0.0942 0.6024 0.037 Uiso 1 1 calc R U . . .
C21 C 0.5190(8) 0.2420(7) 0.7474(6) 0.033(2) Uani 1 1 d . . . . .
C22 C 0.6154(11) 0.9863(10) 0.8040(8) 0.072(3) Uani 1 1 d . . . . .
H22A H 0.6496 1.0555 0.7906 0.101 Uiso 1 1 calc R U . . .
H22B H 0.6899 0.9670 0.8332 0.101 Uiso 1 1 calc R U . . .
H22C H 0.5703 1.0069 0.8582 0.101 Uiso 1 1 calc R U . . .
C23 C 0.5198(10) 0.8805(11) 0.6988(9) 0.058(3) Uani 1 1 d . . . . .
C24 C 0.4622(18) 0.7725(16) 0.7002(17) 0.199(11) Uani 1 1 d . . . . .
H24A H 0.4575 0.7047 0.6333 0.278 Uiso 1 1 calc R U . . .
H24B H 0.3718 0.7620 0.7019 0.278 Uiso 1 1 calc R U . . .
H24C H 0.5166 0.7743 0.7666 0.278 Uiso 1 1 calc R U . . .
O1W O 0.455(4) 0.573(4) 0.448(4) 0.103(14) Uiso 0.2 1 d . . P . .


_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 O5 1.958(4) . ?
Fe1 O1 1.970(4) . ?
Fe1 N1 2.121(6) . ?
Fe1 Cl1 2.215(2) . ?
Fe1 Cl2 2.223(2) . ?
Fe2 O6 1.950(5) . ?
Fe2 O4 1.987(4) . ?
Fe2 O1 2.004(4) . ?
Fe2 O5 2.007(5) . ?
Fe2 O2 2.011(4) . ?
Fe2 N3 2.217(6) . ?
Fe3 O2 1.950(4) . ?
Fe3 O4 1.995(5) . ?
Fe3 N2 2.098(6) . ?
Fe3 Cl4 2.214(2) . ?
Fe3 Cl3 2.224(2) . ?
N1 C5 1.324(9) . ?
N1 C1 1.338(8) . ?
N2 C9 1.336(9) . ?
N2 C13 1.356(10) . ?
N3 C20 1.479(9) . ?
N3 C17 1.479(8) . ?
N3 C18 1.497(9) . ?
O1 C6 1.398(8) . ?
O2 C8 1.433(7) . ?
O3 C6 1.424(8) . ?
O3 C14 1.441(9) . ?
O4 C16 1.435(8) . ?
O5 C19 1.428(8) . ?
O6 C21 1.289(9) . ?
O7 C21 1.226(9) . ?
O8 C23 1.211(11) . ?
C1 C2 1.377(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.378(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.515(9) . ?
C6 C7 1.521(9) . ?
C7 C8 1.542(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C15 1.530(9) . ?
C8 C9 1.535(10) . ?
C9 C10 1.377(10) . ?
C10 C11 1.381(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.360(11) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.530(9) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.511(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.518(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C22 C23 1.471(14) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.385(16) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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 Fe1 O1 74.35(18) . . ?
O5 Fe1 N1 149.2(2) . . ?
O1 Fe1 N1 75.8(2) . . ?
O5 Fe1 Cl1 104.15(14) . . ?
O1 Fe1 Cl1 118.80(15) . . ?
N1 Fe1 Cl1 96.66(17) . . ?
O5 Fe1 Cl2 98.23(15) . . ?
O1 Fe1 Cl2 129.58(15) . . ?
N1 Fe1 Cl2 94.87(18) . . ?
Cl1 Fe1 Cl2 111.43(9) . . ?
O6 Fe2 O4 145.80(19) . . ?
O6 Fe2 O1 99.67(19) . . ?
O4 Fe2 O1 110.92(19) . . ?
O6 Fe2 O5 95.42(19) . . ?
O4 Fe2 O5 107.79(19) . . ?
O1 Fe2 O5 72.57(18) . . ?
O6 Fe2 O2 93.71(19) . . ?
O4 Fe2 O2 74.76(18) . . ?
O1 Fe2 O2 84.91(18) . . ?
O5 Fe2 O2 156.81(19) . . ?
O6 Fe2 N3 80.4(2) . . ?
O4 Fe2 N3 79.60(19) . . ?
O1 Fe2 N3 151.9(2) . . ?
O5 Fe2 N3 79.4(2) . . ?
O2 Fe2 N3 123.2(2) . . ?
O2 Fe3 O4 75.92(18) . . ?
O2 Fe3 N2 76.9(2) . . ?
O4 Fe3 N2 150.2(2) . . ?
O2 Fe3 Cl4 112.62(15) . . ?
O4 Fe3 Cl4 102.09(15) . . ?
N2 Fe3 Cl4 99.50(18) . . ?
O2 Fe3 Cl3 137.40(15) . . ?
O4 Fe3 Cl3 99.06(15) . . ?
N2 Fe3 Cl3 92.67(19) . . ?
Cl4 Fe3 Cl3 109.81(10) . . ?
C5 N1 C1 119.6(6) . . ?
C5 N1 Fe1 116.2(4) . . ?
C1 N1 Fe1 124.1(5) . . ?
C9 N2 C13 118.1(7) . . ?
C9 N2 Fe3 117.3(5) . . ?
C13 N2 Fe3 124.3(5) . . ?
C20 N3 C17 113.6(5) . . ?
C20 N3 C18 111.6(6) . . ?
C17 N3 C18 110.5(5) . . ?
C20 N3 Fe2 106.9(4) . . ?
C17 N3 Fe2 107.0(4) . . ?
C18 N3 Fe2 106.8(4) . . ?
C6 O1 Fe1 124.3(4) . . ?
C6 O1 Fe2 127.4(4) . . ?
Fe1 O1 Fe2 104.4(2) . . ?
C8 O2 Fe3 123.1(4) . . ?
C8 O2 Fe2 128.1(4) . . ?
Fe3 O2 Fe2 104.9(2) . . ?
C6 O3 C14 113.6(6) . . ?
C16 O4 Fe2 117.4(4) . . ?
C16 O4 Fe3 123.5(4) . . ?
Fe2 O4 Fe3 104.12(19) . . ?
C19 O5 Fe1 127.2(4) . . ?
C19 O5 Fe2 115.3(4) . . ?
Fe1 O5 Fe2 104.8(2) . . ?
C21 O6 Fe2 120.5(5) . . ?
N1 C1 C2 122.1(7) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 118.4(7) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.4(8) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 118.9(8) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.6(7) . . ?
N1 C5 C6 116.4(6) . . ?
C4 C5 C6 122.0(7) . . ?
O1 C6 O3 110.6(5) . . ?
O1 C6 C5 106.9(5) . . ?
O3 C6 C5 112.6(6) . . ?
O1 C6 C7 110.5(6) . . ?
O3 C6 C7 105.9(5) . . ?
C5 C6 C7 110.5(5) . . ?
C6 C7 C8 117.3(5) . . ?
C6 C7 H7A 108.0 . . ?
C8 C7 H7A 108.0 . . ?
C6 C7 H7B 108.0 . . ?
C8 C7 H7B 108.0 . . ?
H7A C7 H7B 107.2 . . ?
O2 C8 C15 107.9(6) . . ?
O2 C8 C9 107.3(5) . . ?
C15 C8 C9 108.5(6) . . ?
O2 C8 C7 109.2(5) . . ?
C15 C8 C7 110.7(5) . . ?
C9 C8 C7 113.1(6) . . ?
N2 C9 C10 122.7(8) . . ?
N2 C9 C8 114.1(6) . . ?
C10 C9 C8 122.9(7) . . ?
C9 C10 C11 118.4(7) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
C10 C11 C12 119.4(8) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 118.8(8) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
N2 C13 C12 122.5(8) . . ?
N2 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C15 H15A 109.5 . . ?
C8 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C8 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 C17 109.3(5) . . ?
O4 C16 H16A 109.8 . . ?
C17 C16 H16A 109.8 . . ?
O4 C16 H16B 109.8 . . ?
C17 C16 H16B 109.8 . . ?
H16A C16 H16B 108.3 . . ?
N3 C17 C16 107.8(6) . . ?
N3 C17 H17A 110.2 . . ?
C16 C17 H17A 110.2 . . ?
N3 C17 H17B 110.2 . . ?
C16 C17 H17B 110.2 . . ?
H17A C17 H17B 108.5 . . ?
N3 C18 C19 108.4(5) . . ?
N3 C18 H18A 110.0 . . ?
C19 C18 H18A 110.0 . . ?
N3 C18 H18B 110.0 . . ?
C19 C18 H18B 110.0 . . ?
H18A C18 H18B 108.4 . . ?
O5 C19 C18 107.4(6) . . ?
O5 C19 H19A 110.2 . . ?
C18 C19 H19A 110.2 . . ?
O5 C19 H19B 110.2 . . ?
C18 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
N3 C20 C21 111.7(6) . . ?
N3 C20 H20A 109.3 . . ?
C21 C20 H20A 109.3 . . ?
N3 C20 H20B 109.3 . . ?
C21 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
O7 C21 O6 122.9(7) . . ?
O7 C21 C20 119.9(8) . . ?
O6 C21 C20 117.1(7) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O8 C23 C24 122.0(13) . . ?
O8 C23 C22 119.9(11) . . ?
C24 C23 C22 118.1(12) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_refine_diff_density_max         0.836
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.147

_shelxl_version_number           2014/6

