# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_Dimim2Fe2Cl4O
_database_code_depnum_ccdc_archive 'CCDC 1840841'
_audit_update_record             
;
2018-05-01 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL

_chemical_name_systematic        
;
1,3-dimethylimidazolium (?-oxido)bis[trichloridoferrate(III)] 
;
_chemical_melting_point          '391 K'
_chemical_formula_moiety         'Cl6 Fe2 O, 2(C5 H9 N2)'
_chemical_formula_sum            'C10 H18 Cl6 Fe2 N4 O'
_chemical_formula_weight         534.68

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                   7.3221(11)
_cell_length_b                   7.5071(8)
_cell_length_c                   10.4916(12)
_cell_angle_alpha                102.996(10)
_cell_angle_beta                 100.472(11)
_cell_angle_gamma                92.433(11)
_cell_volume                     550.47(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1267
_cell_measurement_theta_min      4.3980
_cell_measurement_theta_max      73.8830

_exptl_crystal_description       prismatic
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      'note measured'
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    17.321
_exptl_absorpt_correction_T_min  0.01070
_exptl_absorpt_correction_T_max  0.08097
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_diffrn_ambient_temperature      293(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3365
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.411
_diffrn_reflns_theta_max         74.285
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2130
_reflns_number_gt                1664
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.1687P)²+0.3119P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2130
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0865
_refine_ls_wR_factor_ref         0.2806
_refine_ls_wR_factor_gt          0.2617
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.000
_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 0.83193(18) 0.43590(18) 0.85445(10) 0.0887(5) Uani 1 1 d . . . . .
Cl1 Cl 0.7413(3) 0.1394(3) 0.81232(19) 0.0943(6) Uani 1 1 d . . . . .
Cl2 Cl 0.9491(4) 0.4745(3) 0.6816(2) 0.1058(7) Uani 1 1 d . . . . .
Cl3 Cl 0.5896(6) 0.6001(5) 0.8626(6) 0.182(2) Uani 1 1 d . . . . .
O1 O 1.037(3) 0.465(3) 0.9911(18) 0.106(5) Uani 0.5 1 d . . P . .
N3 N 0.7649(8) -0.0027(8) 0.2461(6) 0.0773(14) Uani 1 1 d . . . . .
C4 C 0.7922(14) 0.1248(12) 0.3653(9) 0.094(2) Uani 1 1 d . . . . .
H4 H 0.8272 0.2495 0.3802 0.113 Uiso 1 1 calc R U . . .
C5 C 0.7585(14) 0.0343(13) 0.4562(8) 0.095(2) Uani 1 1 d . . . . .
H5 H 0.7657 0.0851 0.5466 0.114 Uiso 1 1 calc R U . . .
N1 N 0.7121(9) -0.1438(10) 0.3934(7) 0.0857(16) Uani 1 1 d . . . . .
C2 C 0.7173(11) -0.1628(11) 0.2661(8) 0.0837(18) Uani 1 1 d . . . . .
H2 H 0.6913 -0.2723 0.2010 0.100 Uiso 1 1 calc R U . . .
C6 C 0.6587(17) -0.2888(17) 0.4569(12) 0.117(3) Uani 1 1 d . . . . .
H6A H 0.6670 -0.2380 0.5505 0.175 Uiso 1 1 calc R U . . .
H6B H 0.5330 -0.3383 0.4169 0.175 Uiso 1 1 calc R U . . .
H6C H 0.7412 -0.3845 0.4448 0.175 Uiso 1 1 calc R U . . .
C7 C 0.7814(15) 0.0345(14) 0.1177(9) 0.102(2) Uani 1 1 d . . . . .
H7A H 0.8182 0.1624 0.1298 0.152 Uiso 1 1 calc R U . . .
H7B H 0.8735 -0.0376 0.0817 0.152 Uiso 1 1 calc R U . . .
H7C H 0.6634 0.0031 0.0572 0.152 Uiso 1 1 calc R U . . .


_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 O1 1.712(18) 2_767 ?
Fe1 O1 1.848(17) . ?
Fe1 Cl3 2.206(4) . ?
Fe1 Cl2 2.211(2) . ?
Fe1 Cl1 2.217(2) . ?
O1 O1 0.80(2) 2_767 ?
O1 Fe1 1.712(18) 2_767 ?
N3 C2 1.309(10) . ?
N3 C4 1.369(10) . ?
N3 C7 1.461(10) . ?
C4 C5 1.340(13) . ?
C4 H4 0.9300 . ?
C5 N1 1.349(12) . ?
C5 H5 0.9300 . ?
N1 C2 1.319(10) . ?
N1 C6 1.472(11) . ?
C2 H2 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

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 O1 25.5(8) 2_767 . ?
O1 Fe1 Cl3 99.0(4) 2_767 . ?
O1 Fe1 Cl3 124.5(5) . . ?
O1 Fe1 Cl2 116.3(8) 2_767 . ?
O1 Fe1 Cl2 104.3(7) . . ?
Cl3 Fe1 Cl2 107.21(17) . . ?
O1 Fe1 Cl1 117.4(7) 2_767 . ?
O1 Fe1 Cl1 103.1(6) . . ?
Cl3 Fe1 Cl1 110.38(13) . . ?
Cl2 Fe1 Cl1 106.01(10) . . ?
O1 O1 Fe1 87(3) 2_767 2_767 ?
O1 O1 Fe1 68(2) 2_767 . ?
Fe1 O1 Fe1 154.5(8) 2_767 . ?
C2 N3 C4 108.5(6) . . ?
C2 N3 C7 125.7(7) . . ?
C4 N3 C7 125.7(7) . . ?
C5 C4 N3 106.3(7) . . ?
C5 C4 H4 126.8 . . ?
N3 C4 H4 126.8 . . ?
C4 C5 N1 107.9(7) . . ?
C4 C5 H5 126.0 . . ?
N1 C5 H5 126.0 . . ?
C2 N1 C5 108.3(7) . . ?
C2 N1 C6 126.5(9) . . ?
C5 N1 C6 125.2(8) . . ?
N3 C2 N1 109.0(7) . . ?
N3 C2 H2 125.5 . . ?
N1 C2 H2 125.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         0.560
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.113


####################################################################### 
# 
# 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_BHET
_database_code_depnum_ccdc_archive 'CCDC 1840842'
_audit_update_record             
;
2018-05-01 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL

_chemical_name_systematic        
;
bis(2-hydroxyethyl)terephthalate
;
_chemical_formula_moiety         'C12 H14 O6'
_chemical_formula_sum            'C12 H14 O6'
_chemical_formula_weight         254.23

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'

_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                   8.2252(3)
_cell_length_b                   9.3639(9)
_cell_length_c                   16.5008(12)
_cell_angle_alpha                87.306(7)
_cell_angle_beta                 84.160(5)
_cell_angle_gamma                80.338(6)
_cell_volume                     1245.78(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    2744
_cell_measurement_theta_min      5.8540
_cell_measurement_theta_max      73.6450

_exptl_crystal_description       needle-like
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.73398
_exptl_absorpt_correction_T_max  1.00000
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8599
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.793
_diffrn_reflns_theta_max         74.092
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8599
_reflns_number_gt                5726
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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.
;

_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6227 6182 2487 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.3773 6090 2487 nmt 1.0003 0.0000 -0.0008 0.3851 -1.0007 0.0009 0.4010
-0.0035 -1.0003
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -179.8910° 
 around [0.96 0.19 0.19] (reciprocal) or [1.00 0.00 -0.00] (direct)
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
 Refined as a 2-component twin.
 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)+(0.1502P)²] 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         8599
_refine_ls_number_parameters     330
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.2097
_refine_ls_wR_factor_gt          0.1975
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_restrained_S_all      0.948
_refine_ls_shift/su_max          0.000
_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
O16 O 0.2375(2) 0.1817(2) 0.58884(12) 0.0305(4) Uani 1 1 d . . . . .
025 O 0.2176(3) 0.7365(2) 0.64386(14) 0.0397(5) Uani 1 1 d . . . . .
O46 O 0.6455(3) 0.3178(2) 0.90607(13) 0.0352(5) Uani 1 1 d . . . . .
O15 O 0.3109(3) 0.1749(2) 0.45394(13) 0.0367(5) Uani 1 1 d . . . . .
O49 O 0.8490(3) 0.3620(3) 0.76068(14) 0.0380(5) Uani 1 1 d . . . . .
H49 H 0.9404 0.3553 0.7777 0.057 Uiso 1 1 calc R U . . .
O45 O 0.6556(3) 0.3347(3) 1.04063(14) 0.0437(6) Uani 1 1 d . . . . .
026 O 0.3263(3) 0.5328(2) 0.70993(13) 0.0337(5) Uani 1 1 d . . . . .
O29 O 0.1586(3) 0.3361(2) 0.80952(15) 0.0386(5) Uani 1 1 d . . . . .
H29 H 0.2305 0.2861 0.7802 0.058 Uiso 1 1 calc R U . . .
O19 O 0.3995(3) 0.1350(2) 0.73436(14) 0.0378(5) Uani 1 1 d . . . . .
H19 H 0.4911 0.1514 0.7157 0.057 Uiso 1 1 calc R U . . .
C44 C 0.6246(3) 0.2709(3) 0.98370(18) 0.0332(6) Uani 1 1 d . . . . .
C14 C 0.2293(3) 0.2330(3) 0.51201(17) 0.0279(6) Uani 1 1 d . . . . .
C24 C 0.3082(3) 0.6201(3) 0.64344(19) 0.0300(6) Uani 1 1 d . . . . .
C17 C 0.3596(3) 0.0535(3) 0.60070(18) 0.0314(6) Uani 1 1 d . . . . .
H17A H 0.4688 0.0706 0.5787 0.038 Uiso 1 1 calc R U . . .
H17B H 0.3328 -0.0277 0.5732 0.038 Uiso 1 1 calc R U . . .
C27 C 0.2197(4) 0.5784(3) 0.78292(19) 0.0360(7) Uani 1 1 d . . . . .
H27A H 0.1070 0.6113 0.7697 0.043 Uiso 1 1 calc R U . . .
H27B H 0.2583 0.6573 0.8073 0.043 Uiso 1 1 calc R U . . .
C28 C 0.2263(4) 0.4497(3) 0.84072(19) 0.0351(7) Uani 1 1 d . . . . .
H28A H 0.3405 0.4146 0.8507 0.042 Uiso 1 1 calc R U . . .
H28B H 0.1651 0.4788 0.8923 0.042 Uiso 1 1 calc R U . . .
C47 C 0.7163(4) 0.4493(4) 0.8918(2) 0.0370(7) Uani 1 1 d . . . . .
H47A H 0.8225 0.4382 0.9141 0.044 Uiso 1 1 calc R U . . .
H47B H 0.6432 0.5302 0.9175 0.044 Uiso 1 1 calc R U . . .
C11 C 0.1091(3) 0.3713(3) 0.50676(17) 0.0254(5) Uani 1 1 d . . . . .
C21 C 0.4101(3) 0.5571(3) 0.57006(17) 0.0268(6) Uani 1 1 d . . . . .
C42 C 0.5213(4) 0.0653(4) 0.92292(19) 0.0353(7) Uani 1 1 d . . . . .
H42 H 0.5351 0.1090 0.8715 0.042 Uiso 1 1 calc R U . . .
C22 C 0.3903(3) 0.6302(3) 0.49518(19) 0.0301(6) Uani 1 1 d . . . . .
H22 H 0.3164 0.7166 0.4922 0.036 Uiso 1 1 calc R U . . .
C23 C 0.5191(3) 0.4263(3) 0.57458(18) 0.0308(6) Uani 1 1 d . . . . .
H23 H 0.5309 0.3771 0.6245 0.037 Uiso 1 1 calc R U . . .
C41 C 0.5589(3) 0.1314(4) 0.99100(18) 0.0320(6) Uani 1 1 d . . . . .
C13 C 0.0887(3) 0.4374(3) 0.43064(18) 0.0302(6) Uani 1 1 d . . . . .
H13 H 0.1477 0.3949 0.3844 0.036 Uiso 1 1 calc R U . . .
C18 C 0.3562(4) 0.0215(3) 0.69095(19) 0.0329(6) Uani 1 1 d . . . . .
H18A H 0.2459 0.0054 0.7118 0.039 Uiso 1 1 calc R U . . .
H18B H 0.4326 -0.0671 0.7006 0.039 Uiso 1 1 calc R U . . .
C48 C 0.7374(4) 0.4750(3) 0.8011(2) 0.0360(7) Uani 1 1 d . . . . .
H48B H 0.6303 0.4837 0.7799 0.043 Uiso 1 1 calc R U . . .
H48A H 0.7781 0.5659 0.7894 0.043 Uiso 1 1 calc R U . . .
C43 C 0.4634(4) -0.0657(4) 0.93209(19) 0.0365(7) Uani 1 1 d . . . . .
H43 H 0.4392 -0.1101 0.8865 0.044 Uiso 1 1 calc R U . . .
C12 C 0.0195(3) 0.4331(3) 0.57644(18) 0.0298(6) Uani 1 1 d . . . . .
H12 H 0.0323 0.3877 0.6273 0.036 Uiso 1 1 calc R U . . .
O35 O 0.1380(3) 0.2374(2) 0.14151(15) 0.0429(6) Uani 1 1 d . . . . .
O36 O 0.0894(3) 0.0317(2) 0.20765(14) 0.0355(5) Uani 1 1 d . . . . .
O39 O 0.2813(3) -0.1641(2) 0.31316(16) 0.0409(6) Uani 1 1 d . . . . .
H39A H 0.2404 -0.2177 0.2861 0.061 Uiso 1 1 calc R U . . .
C34 C 0.0952(3) 0.1200(3) 0.14191(19) 0.0316(6) Uani 1 1 d . . . . .
C37 C 0.1467(4) 0.0789(3) 0.2805(2) 0.0356(7) Uani 1 1 d . . . . .
H37A H 0.0697 0.1607 0.3028 0.043 Uiso 1 1 calc R U . . .
H37B H 0.2545 0.1080 0.2680 0.043 Uiso 1 1 calc R U . . .
C38 C 0.1577(4) -0.0473(4) 0.3406(2) 0.0380(7) Uani 1 1 d . . . . .
H38A H 0.1829 -0.0162 0.3924 0.046 Uiso 1 1 calc R U . . .
H38B H 0.0513 -0.0801 0.3490 0.046 Uiso 1 1 calc R U . . .
C32 C 0.0568(4) 0.1319(3) -0.0054(2) 0.0340(6) Uani 1 1 d . . . . .
H32 H 0.0950 0.2202 -0.0088 0.041 Uiso 1 1 calc R U . . .
C31 C 0.0435(3) 0.0569(3) 0.06933(19) 0.0305(6) Uani 1 1 d . . . . .
C33 C 0.0134(4) 0.0757(3) -0.0746(2) 0.0342(6) Uani 1 1 d . . . . .
H33 H 0.0222 0.1260 -0.1244 0.041 Uiso 1 1 calc R U . . .


_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
O16 C14 1.339(4) . ?
O16 C17 1.450(3) . ?
025 C24 1.213(4) . ?
O46 C44 1.338(4) . ?
O46 C47 1.448(4) . ?
O15 C14 1.208(4) . ?
O49 C48 1.423(4) . ?
O45 C44 1.207(4) . ?
026 C24 1.342(4) . ?
026 C27 1.452(4) . ?
O29 C28 1.420(4) . ?
O19 C18 1.422(4) . ?
C44 C41 1.491(5) . ?
C14 C11 1.496(4) . ?
C24 C21 1.487(4) . ?
C17 C18 1.503(4) . ?
C27 C28 1.499(4) . ?
C47 C48 1.501(5) . ?
C11 C13 1.387(4) . ?
C11 C12 1.396(4) . ?
C21 C22 1.395(4) . ?
C21 C23 1.396(4) . ?
C42 C43 1.385(5) . ?
C42 C41 1.393(4) . ?
C22 C23 1.382(4) 2_666 ?
C23 C22 1.382(4) 2_666 ?
C41 C43 1.393(5) 2_657 ?
C13 C12 1.386(4) 2_566 ?
C43 C41 1.393(5) 2_657 ?
C12 C13 1.386(4) 2_566 ?
O35 C34 1.208(4) . ?
O36 C34 1.335(4) . ?
O36 C37 1.448(4) . ?
O39 C38 1.419(4) . ?
C34 C31 1.490(4) . ?
C37 C38 1.503(5) . ?
C32 C33 1.381(5) . ?
C32 C31 1.394(5) . ?
C31 C33 1.394(4) 2 ?
C33 C31 1.394(4) 2 ?

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
C14 O16 C17 116.1(2) . . ?
C44 O46 C47 116.4(2) . . ?
C24 026 C27 116.5(2) . . ?
O45 C44 O46 123.6(3) . . ?
O45 C44 C41 124.5(3) . . ?
O46 C44 C41 111.9(3) . . ?
O15 C14 O16 123.8(3) . . ?
O15 C14 C11 124.1(3) . . ?
O16 C14 C11 112.1(2) . . ?
025 C24 026 123.2(3) . . ?
025 C24 C21 124.4(3) . . ?
026 C24 C21 112.4(2) . . ?
O16 C17 C18 107.2(2) . . ?
026 C27 C28 107.1(2) . . ?
O29 C28 C27 111.8(3) . . ?
O46 C47 C48 106.8(2) . . ?
C13 C11 C12 120.4(3) . . ?
C13 C11 C14 118.4(3) . . ?
C12 C11 C14 121.2(3) . . ?
C22 C21 C23 120.2(3) . . ?
C22 C21 C24 118.2(3) . . ?
C23 C21 C24 121.6(3) . . ?
C43 C42 C41 119.8(3) . . ?
C23 C22 C21 119.8(3) 2_666 . ?
C22 C23 C21 119.9(3) 2_666 . ?
C43 C41 C42 119.7(3) 2_657 . ?
C43 C41 C44 118.7(3) 2_657 . ?
C42 C41 C44 121.6(3) . . ?
C12 C13 C11 120.0(3) 2_566 . ?
O19 C18 C17 112.9(3) . . ?
O49 C48 C47 112.7(3) . . ?
C42 C43 C41 120.5(3) . 2_657 ?
C13 C12 C11 119.6(3) 2_566 . ?
C34 O36 C37 116.7(2) . . ?
O35 C34 O36 123.7(3) . . ?
O35 C34 C31 124.1(3) . . ?
O36 C34 C31 112.2(2) . . ?
O36 C37 C38 107.0(2) . . ?
O39 C38 C37 111.7(3) . . ?
C33 C32 C31 120.3(3) . . ?
C33 C31 C32 120.1(3) 2 . ?
C33 C31 C34 121.5(3) 2 . ?
C32 C31 C34 118.4(3) . . ?
C32 C33 C31 119.7(3) . 2 ?

_refine_diff_density_max         0.725
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.108



#==END
