# 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 2017

####################################################################### 
# 
# 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_CPX1
_database_code_depnum_ccdc_archive 'CCDC 1505681'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C39 H27 Fe N6 O6), 0.5(H2 O)'
_chemical_formula_sum            'C39 H28 Fe N6 O6.50'
_chemical_formula_weight         740.52

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

_cell_length_a                   14.2613(7)
_cell_length_b                   14.2613(7)
_cell_length_c                   30.489(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5370.2(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1483
_cell_measurement_theta_min      3.5590
_cell_measurement_theta_max      29.4910

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_F_000             2292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.479
_shelx_estimated_absorpt_T_min   0.910
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_process_details   sadabs

_exptl_special_details           ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4761
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.857
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2104
_reflns_number_gt                1503
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.1627P)²+10.5326P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2104
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0751
_refine_ls_wR_factor_ref         0.2725
_refine_ls_wR_factor_gt          0.2468
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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 0.3333 0.6667 0.06400(4) 0.0424(5) Uani 1 3 d S T P . .
O1 O 0.2556(3) 0.5382(3) 0.02463(11) 0.0515(10) Uani 1 1 d . . . . .
O1W O 0.0000 0.0000 -0.0480(4) 0.088(5) Uani 0.5 3 d S T P . .
H1W H -0.0003 -0.0538 -0.0375 0.106 Uiso 0.3333 1 d R U P . .
O2 O 0.2001(3) 0.6017(3) 0.10047(10) 0.0439(9) Uani 1 1 d . . . . .
C13 C -0.0873(4) 0.4426(4) 0.11144(18) 0.0645(15) Uani 0.3333 1 d . . P A 1
H13 H -0.1052 0.4049 0.0850 0.077 Uiso 0.3333 1 calc R U P A 1
N2 N -0.1646(5) 0.4266(5) 0.1403(2) 0.0793(19) Uani 0.3333 1 d . . P A 1
N2A N -0.0873(4) 0.4426(4) 0.11144(18) 0.0645(15) Uani 0.6667 1 d . . P A 2
C13A C -0.1646(5) 0.4266(5) 0.1403(2) 0.0793(19) Uani 0.6667 1 d . . P A 2
H13A H -0.2361 0.3763 0.1336 0.095 Uiso 0.6667 1 calc R U P A 2
N1 N 0.0112(5) 0.3357(5) -0.02610(17) 0.0667(17) Uani 0.3333 1 d . . P B 1
C1 C -0.0204(6) 0.2735(6) -0.0634(2) 0.094(2) Uani 0.3333 1 d . . P B 1
H1 H -0.0932 0.2246 -0.0685 0.113 Uiso 0.3333 1 calc R U P B 1
C1A C 0.0112(5) 0.3357(5) -0.02610(17) 0.0667(17) Uani 0.6667 1 d . . P B 2
H1A H -0.0401 0.3292 -0.0056 0.080 Uiso 0.6667 1 calc R U P B 2
N1A N -0.0204(6) 0.2735(6) -0.0634(2) 0.094(2) Uani 0.6667 1 d . . P B 2
C2 C 0.0557(6) 0.2842(6) -0.0928(2) 0.079(2) Uani 1 1 d . . . . .
H2 H 0.0338 0.2412 -0.1178 0.095 Uiso 1 1 calc R U . B 1
C3 C 0.1636(6) 0.3559(7) -0.0870(2) 0.084(2) Uani 1 1 d . . . . .
H3 H 0.2146 0.3616 -0.1074 0.101 Uiso 1 1 calc R U . . .
C4 C 0.1937(5) 0.4183(6) -0.0504(2) 0.074(2) Uani 1 1 d . . . . .
H4 H 0.2661 0.4697 -0.0461 0.089 Uiso 1 1 calc R U . . .
C5 C 0.1170(5) 0.4062(5) -0.01936(16) 0.0506(13) Uani 1 1 d . . . . .
C6 C 0.1530(4) 0.4776(4) 0.02049(15) 0.0438(12) Uani 1 1 d . . . . .
C7 C 0.0776(4) 0.4731(5) 0.05034(17) 0.0499(13) Uani 1 1 d . . . . .
H7 H 0.0048 0.4272 0.0441 0.060 Uiso 1 1 calc R U . . .
C8 C 0.1035(4) 0.5325(4) 0.08892(15) 0.0411(11) Uani 1 1 d . . . . .
C9 C 0.0166(4) 0.5139(4) 0.12111(16) 0.0431(12) Uani 1 1 d . . . . .
C10 C 0.0420(5) 0.5686(5) 0.16082(17) 0.0558(15) Uani 1 1 d . . . . .
H10 H 0.1139 0.6167 0.1679 0.067 Uiso 1 1 calc R U . . .
C11 C -0.0385(5) 0.5521(5) 0.18973(19) 0.0636(16) Uani 1 1 d . . . . .
H11 H -0.0220 0.5891 0.2163 0.076 Uiso 1 1 calc R U . . .
C12 C -0.1432(5) 0.4804(5) 0.1788(2) 0.0700(18) Uani 1 1 d . . . . .
H12 H -0.1993 0.4686 0.1977 0.084 Uiso 1 1 calc R U . A 1


_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 O2 1.986(3) . ?
Fe1 O2 1.986(3) 3_565 ?
Fe1 O2 1.986(3) 2_665 ?
Fe1 O1 1.999(3) 3_565 ?
Fe1 O1 1.999(3) 2_665 ?
Fe1 O1 1.999(3) . ?
O1 C6 1.280(6) . ?
O1W H1W 0.8300 . ?
O2 C8 1.280(6) . ?
C13 N2 1.338(8) . ?
C13 C9 1.345(7) . ?
C13 H13 0.9300 . ?
N2 C12 1.350(9) . ?
N2A C13A 1.338(8) . ?
N2A C9 1.345(7) . ?
C13A C12 1.350(9) . ?
C13A H13A 0.9300 . ?
N1 C5 1.346(8) . ?
N1 C1 1.373(8) . ?
C1 C2 1.355(9) . ?
C1 H1 0.9300 . ?
C1A C5 1.346(8) . ?
C1A N1A 1.373(8) . ?
C1A H1A 0.9300 . ?
N1A C2 1.355(9) . ?
C2 C3 1.367(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.355(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.501(7) . ?
C6 C7 1.386(7) . ?
C7 C8 1.387(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.497(7) . ?
C9 C10 1.387(7) . ?
C10 C11 1.371(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.364(9) . ?
C11 H11 0.9300 . ?
C12 H12 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
O2 Fe1 O2 91.71(13) . 3_565 ?
O2 Fe1 O2 91.71(13) . 2_665 ?
O2 Fe1 O2 91.70(13) 3_565 2_665 ?
O2 Fe1 O1 93.88(15) . 3_565 ?
O2 Fe1 O1 86.91(14) 3_565 3_565 ?
O2 Fe1 O1 174.29(14) 2_665 3_565 ?
O2 Fe1 O1 174.28(14) . 2_665 ?
O2 Fe1 O1 93.88(15) 3_565 2_665 ?
O2 Fe1 O1 86.91(14) 2_665 2_665 ?
O1 Fe1 O1 87.65(15) 3_565 2_665 ?
O2 Fe1 O1 86.91(14) . . ?
O2 Fe1 O1 174.29(14) 3_565 . ?
O2 Fe1 O1 93.88(15) 2_665 . ?
O1 Fe1 O1 87.65(15) 3_565 . ?
O1 Fe1 O1 87.65(15) 2_665 . ?
C6 O1 Fe1 127.0(3) . . ?
C8 O2 Fe1 128.0(3) . . ?
N2 C13 C9 119.1(5) . . ?
N2 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?
C13 N2 C12 122.8(6) . . ?
C13A N2A C9 119.1(5) . . ?
N2A C13A C12 122.8(6) . . ?
N2A C13A H13A 118.6 . . ?
C12 C13A H13A 118.6 . . ?
C5 N1 C1 119.5(6) . . ?
C2 C1 N1 119.2(6) . . ?
C2 C1 H1 120.4 . . ?
N1 C1 H1 120.4 . . ?
C5 C1A N1A 119.5(6) . . ?
C5 C1A H1A 120.3 . . ?
N1A C1A H1A 120.3 . . ?
C2 N1A C1A 119.2(6) . . ?
N1A C2 C3 122.5(6) . . ?
C1 C2 C3 122.5(6) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C4 C3 C2 117.8(6) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
C3 C4 C5 120.5(6) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C1A C5 C4 120.5(5) . . ?
N1 C5 C4 120.5(5) . . ?
C1A C5 C6 120.4(5) . . ?
N1 C5 C6 120.4(5) . . ?
C4 C5 C6 119.1(5) . . ?
O1 C6 C7 124.4(4) . . ?
O1 C6 C5 115.2(4) . . ?
C7 C6 C5 120.4(5) . . ?
C6 C7 C8 124.5(5) . . ?
C6 C7 H7 117.8 . . ?
C8 C7 H7 117.8 . . ?
O2 C8 C7 124.0(5) . . ?
O2 C8 C9 115.7(4) . . ?
C7 C8 C9 120.3(5) . . ?
N2A C9 C10 119.7(5) . . ?
C13 C9 C10 119.7(5) . . ?
N2A C9 C8 119.4(4) . . ?
C13 C9 C8 119.4(4) . . ?
C10 C9 C8 120.8(5) . . ?
C11 C10 C9 120.3(6) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 118.7(5) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C13A C12 C11 119.4(6) . . ?
N2 C12 C11 119.4(6) . . ?
N2 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?

_refine_diff_density_max         1.206
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.108

####################################################################### 
# 
# 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_t
_database_code_depnum_ccdc_archive 'CCDC 1545277'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H27 Fe N6 O6, 0.5(C6 H14), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C42.50 H35 Cl Fe N6 O6'
_chemical_formula_weight         817.06

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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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                   10.5081(12)
_cell_length_b                   12.0042(18)
_cell_length_c                   16.4968(18)
_cell_angle_alpha                77.517(3)
_cell_angle_beta                 73.321(3)
_cell_angle_gamma                75.069(3)
_cell_volume                     1903.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9778
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.433

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_F_000             846
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.525
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            79809
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.359
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8753
_reflns_number_gt                6925
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0465P)²+2.5562P] 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         8753
_refine_ls_number_parameters     623
_refine_ls_number_restraints     324
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1329
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.038
_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
C1 C 0.5841(7) -0.0298(6) 0.4723(6) 0.070(2) Uani 0.5 1 d . . P . .
H1A H 0.6645 -0.0001 0.4662 0.084 Uiso 0.5 1 calc R U P . .
H1B H 0.6147 -0.1063 0.4546 0.084 Uiso 0.5 1 calc R U P . .
Fe1 Fe 0.20417(4) 0.29751(3) 0.75114(2) 0.02772(11) Uani 1 1 d . . . . .
Cl1 Cl 0.50495(14) 0.04907(13) 0.41144(8) 0.0968(4) Uani 1 1 d . . . . .
O1 O 0.09699(18) 0.43661(15) 0.69100(10) 0.0331(4) Uani 1 1 d . . . . .
O2 O 0.33302(19) 0.28015(15) 0.63704(10) 0.0338(4) Uani 1 1 d . . . . .
O3 O 0.07817(18) 0.20588(15) 0.74056(11) 0.0325(4) Uani 1 1 d . . . . .
N3 N 0.7251(3) 0.2762(3) 0.3873(2) 0.0681(9) Uani 1 1 d . . . . .
O4 O 0.30935(19) 0.14508(15) 0.79760(11) 0.0343(4) Uani 1 1 d . . . . .
O5 O 0.33727(18) 0.37291(15) 0.77229(10) 0.0323(4) Uani 1 1 d . . . . .
O6 O 0.09151(17) 0.33540(15) 0.86428(10) 0.0311(4) Uani 1 1 d . . . . .
N1 N -0.1757(3) 0.3288(3) 1.16363(18) 0.0663(9) Uani 1 1 d . . . . .
N2 N 0.6419(3) 0.4480(2) 0.90616(17) 0.0491(6) Uani 1 1 d . . . . .
C2 C 0.0567(6) 0.9519(4) 0.0087(3) 0.0894(15) Uani 1 1 d . . . . .
H2A H 0.0177 0.8910 0.0496 0.107 Uiso 1 1 calc R U . . .
H2B H 0.1016 0.9201 -0.0441 0.107 Uiso 1 1 calc R U . . .
C3 C 0.1595(6) 0.9745(5) 0.0404(3) 0.1001(16) Uani 1 1 d . . . . .
H3A H 0.1155 1.0058 0.0934 0.120 Uiso 1 1 calc R U . . .
H3B H 0.1994 1.0350 -0.0004 0.120 Uiso 1 1 calc R U . . .
C4 C 0.2770(6) 0.8701(4) 0.0576(3) 0.1001(17) Uani 1 1 d . . . . .
H4A H 0.2407 0.8118 0.1016 0.150 Uiso 1 1 calc R U . . .
H4B H 0.3413 0.8971 0.0758 0.150 Uiso 1 1 calc R U . . .
H4C H 0.3216 0.8371 0.0061 0.150 Uiso 1 1 calc R U . . .
C5 C 0.4923(3) 0.3960(2) 0.84091(16) 0.0317(5) Uani 1 1 d . . . . .
C6 C 0.1341(2) 0.3407(2) 0.92839(14) 0.0273(5) Uani 1 1 d . . . . .
C7 C 0.0298(3) 0.3381(2) 1.01178(15) 0.0295(5) Uani 1 1 d . . . . .
C8 C 0.1003(3) 0.0974(2) 0.73748(16) 0.0321(5) Uani 1 1 d . . . . .
C9 C 0.2567(3) 0.4614(2) 0.55839(16) 0.0353(6) Uani 1 1 d . . . . .
H9 H 0.2791 0.5138 0.5087 0.042 Uiso 1 1 calc R U . . .
C10 C 0.1315(3) 0.4911(2) 0.61542(15) 0.0296(5) Uani 1 1 d . . . . .
C11 C 0.3501(3) 0.3581(2) 0.57133(15) 0.0292(5) Uani 1 1 d . . . . .
C12 C 0.3584(3) 0.3716(2) 0.84494(16) 0.0293(5) Uani 1 1 d . . . . .
C13 C 0.2647(3) 0.3515(2) 0.92304(16) 0.0331(5) Uani 1 1 d . . . . .
H13 H 0.2908 0.3450 0.9734 0.040 Uiso 1 1 calc R U . . .
C14 C 0.4935(3) 0.3783(3) 0.41872(18) 0.0465(7) Uani 1 1 d . . . . .
H14 H 0.4204 0.4287 0.4002 0.056 Uiso 1 1 calc R U . . .
C15 C 0.0245(3) 0.5888(2) 0.58803(16) 0.0311(5) Uani 1 1 d . . . . .
C16 C 0.4796(3) 0.3313(2) 0.50487(16) 0.0347(6) Uani 1 1 d . . . . .
C17 C -0.0930(3) 0.6285(3) 0.64666(19) 0.0430(7) Uani 1 1 d . . . . .
H17 H -0.1024 0.5985 0.7045 0.052 Uiso 1 1 calc R U . A 1
C18 C -0.1035(3) 0.3457(3) 1.01279(18) 0.0411(6) Uani 1 1 d . . . . .
H18 H -0.1279 0.3538 0.9616 0.049 Uiso 1 1 calc R U . . .
C19 C 0.7167(3) 0.4146(3) 0.7615(2) 0.0449(7) Uani 1 1 d . . . . .
H19 H 0.7853 0.4120 0.7112 0.054 Uiso 1 1 calc R U . . .
C20 C 0.7368(3) 0.4418(3) 0.8322(2) 0.0446(7) Uani 1 1 d . . . . .
H20 H 0.8208 0.4568 0.8290 0.054 Uiso 1 1 calc R U . . .
C21 C 0.3075(3) 0.0425(2) 0.78960(17) 0.0347(6) Uani 1 1 d . . . . .
C22 C 0.5221(3) 0.4253(3) 0.90941(18) 0.0408(6) Uani 1 1 d . . . . .
H22 H 0.4551 0.4294 0.9604 0.049 Uiso 1 1 calc R U . . .
C23 C 0.5935(3) 0.3911(2) 0.76525(18) 0.0392(6) Uani 1 1 d . . . . .
H23 H 0.5781 0.3721 0.7176 0.047 Uiso 1 1 calc R U . . .
C24 C -0.2002(3) 0.3415(3) 1.0883(2) 0.0510(8) Uani 1 1 d . . . . .
H24 H -0.2893 0.3481 1.0862 0.061 Uiso 1 1 calc R U . . .
C25 C 0.0321(3) 0.6375(3) 0.50271(19) 0.0488(7) Uani 1 1 d . . . . .
H25 H 0.1095 0.6135 0.4608 0.059 Uiso 1 1 calc R U . B 1
C26 C 0.5916(3) 0.2573(3) 0.5287(2) 0.0462(7) Uani 1 1 d . . . . .
H26 H 0.5857 0.2246 0.5858 0.055 Uiso 1 1 calc R U . . .
C27 C 0.0576(4) 0.3286(4) 1.09008(19) 0.0601(10) Uani 1 1 d . . . . .
H27 H 0.1453 0.3246 1.0939 0.072 Uiso 1 1 calc R U . . .
C28 C -0.0737(4) 0.7207(3) 0.4800(2) 0.0682(10) Uani 0.5 1 d . . P C 1
H28 H -0.0675 0.7526 0.4227 0.082 Uiso 0.5 1 calc R U P C 1
N29 N -0.1962(3) 0.7114(3) 0.6209(2) 0.0587(8) Uani 0.5 1 d . . P C 1
N30 N -0.0737(4) 0.7207(3) 0.4800(2) 0.0682(10) Uani 0.5 1 d . . P C 2
C31 C -0.1962(3) 0.7114(3) 0.6209(2) 0.0587(8) Uani 0.5 1 d . . P C 2
H31 H -0.2749 0.7363 0.6616 0.070 Uiso 0.5 1 calc R U P C 2
C32 C 0.2092(3) 0.0158(2) 0.7602(2) 0.0440(7) Uani 1 1 d . . . . .
H32 H 0.2170 -0.0616 0.7555 0.053 Uiso 1 1 calc R U . . .
C33 C -0.1867(3) 0.7568(3) 0.5398(2) 0.0498(8) Uani 1 1 d . . . . .
H33 H -0.2578 0.8135 0.5238 0.060 Uiso 1 1 calc R U . C 1
C34 C 0.6166(4) 0.3493(3) 0.3611(2) 0.0572(9) Uani 1 1 d . . . . .
H34 H 0.6257 0.3801 0.3034 0.069 Uiso 1 1 calc R U . . .
C35 C 0.7101(3) 0.2322(3) 0.4691(2) 0.0484(7) Uani 1 1 d . . . . .
H35 H 0.7840 0.1817 0.4867 0.058 Uiso 1 1 calc R U . . .
C36 C -0.0488(4) 0.3251(5) 1.1631(2) 0.0829(14) Uani 1 1 d . . . . .
H36 H -0.0292 0.3198 1.2154 0.100 Uiso 1 1 calc R U . . .
C37 C 0.431(3) -0.160(2) 0.805(2) 0.048(5) Uani 0.5 1 d . . P D 1
H37 H 0.3763 -0.1800 0.7773 0.057 Uiso 0.5 1 calc R U P D 1
C38 C 0.545(4) -0.246(3) 0.840(2) 0.052(5) Uani 0.5 1 d . . P D 1
H38 H 0.5621 -0.3223 0.8305 0.063 Uiso 0.5 1 calc R U P D 1
C39 C 0.4935(14) -0.0285(12) 0.8694(7) 0.061(3) Uani 0.5 1 d . . P D 1
H39 H 0.4747 0.0461 0.8833 0.073 Uiso 0.5 1 calc R U P D 1
C40 C 0.5908(13) -0.1154(11) 0.8967(8) 0.075(4) Uani 0.5 1 d . . P D 1
H40 H 0.6406 -0.0967 0.9284 0.090 Uiso 0.5 1 calc R U P D 1
N41 N 0.6201(18) -0.2226(15) 0.8822(8) 0.058(3) Uani 0.5 1 d . . P D 1
C42 C 0.423(3) -0.058(2) 0.819(2) 0.037(4) Uani 0.5 1 d . . P D 1
N43 N 0.638(2) -0.2286(16) 0.8504(9) 0.066(4) Uani 0.5 1 d . U P D 2
C44 C 0.5259(14) -0.0249(13) 0.8292(8) 0.068(4) Uani 0.5 1 d . U P D 2
H44 H 0.5304 0.0519 0.8278 0.081 Uiso 0.5 1 calc R U P D 2
C45 C 0.6309(13) -0.1125(12) 0.8495(9) 0.082(4) Uani 0.5 1 d . U P D 2
H45 H 0.7007 -0.0920 0.8633 0.098 Uiso 0.5 1 calc R U P D 2
C46 C 0.414(3) -0.045(2) 0.811(2) 0.042(4) Uani 0.5 1 d . U P D 2
C47 C 0.540(4) -0.250(3) 0.824(2) 0.052(4) Uani 0.5 1 d . U P D 2
H47 H 0.5431 -0.3258 0.8177 0.063 Uiso 0.5 1 calc R U P D 2
C48 C 0.445(3) -0.173(2) 0.807(2) 0.045(4) Uani 0.5 1 d . U P D 2
H48 H 0.3819 -0.1971 0.7882 0.054 Uiso 0.5 1 calc R U P D 2
C49 C -0.219(3) 0.092(2) 0.692(2) 0.063(5) Uani 0.5 1 d . U P E 2
H49 H -0.3068 0.1366 0.7034 0.075 Uiso 0.5 1 calc R U P E 2
C50 C -0.008(2) 0.063(2) 0.704(2) 0.034(3) Uani 0.5 1 d . U P F 1
N1A N -0.222(2) 0.1113(16) 0.6752(14) 0.049(3) Uani 0.5 1 d . U P F 1
C51 C -0.118(2) 0.122(2) 0.7136(18) 0.047(3) Uani 0.5 1 d . U P F 1
H51 H -0.1401 0.1799 0.7480 0.056 Uiso 0.5 1 calc R U P F 1
C52 C -0.1758(13) 0.0098(12) 0.6327(8) 0.060(3) Uani 0.5 1 d . U P F 1
H52 H -0.2392 -0.0164 0.6163 0.072 Uiso 0.5 1 calc R U P F 1
C53 C 0.0446(14) -0.0249(12) 0.6509(8) 0.066(3) Uani 0.5 1 d . U P F 1
H53 H 0.1353 -0.0635 0.6409 0.080 Uiso 0.5 1 calc R U P F 1
C54 C -0.0441(12) -0.0499(11) 0.6152(8) 0.077(3) Uani 0.5 1 d . U P F 1
H54 H -0.0158 -0.1067 0.5796 0.093 Uiso 0.5 1 calc R U P F 1
C55 C 0.0177(16) -0.0476(13) 0.6883(11) 0.099(5) Uani 0.5 1 d . U P E 2
H55 H 0.0937 -0.1062 0.6935 0.118 Uiso 0.5 1 calc R U P E 2
C56 C 0.010(2) 0.059(3) 0.710(2) 0.043(4) Uani 0.5 1 d . U P E 2
C57 C -0.135(2) 0.131(2) 0.7073(17) 0.048(3) Uani 0.5 1 d . U P E 2
H57 H -0.1588 0.2072 0.7184 0.057 Uiso 0.5 1 calc R U P E 2
C58 C -0.2063(17) 0.0106(18) 0.6660(11) 0.098(5) Uani 0.5 1 d . U P E 2
H58 H -0.2774 -0.0026 0.6488 0.117 Uiso 0.5 1 calc R U P E 2
N4A N -0.0829(15) -0.0725(14) 0.6591(11) 0.141(5) Uani 0.5 1 d . U P E 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
C1 Cl1 1.504(9) . ?
C1 Cl1 1.869(9) 2_656 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
Fe1 O6 1.9782(17) . ?
Fe1 O3 1.9898(18) . ?
Fe1 O5 1.9916(18) . ?
Fe1 O2 1.9952(17) . ?
Fe1 O4 1.9987(17) . ?
Fe1 O1 1.9992(17) . ?
Cl1 C1 1.869(9) 2_656 ?
O1 C10 1.274(3) . ?
O2 C11 1.273(3) . ?
O3 C8 1.272(3) . ?
N3 C35 1.319(4) . ?
N3 C34 1.363(5) . ?
O4 C21 1.273(3) . ?
O5 C12 1.276(3) . ?
O6 C6 1.280(3) . ?
N1 C24 1.309(4) . ?
N1 C36 1.321(5) . ?
N2 C20 1.338(4) . ?
N2 C22 1.340(4) . ?
C2 C3 1.431(7) . ?
C2 C2 1.477(9) 2_575 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.558(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C22 1.389(4) . ?
C5 C23 1.389(4) . ?
C5 C12 1.490(4) . ?
C6 C13 1.387(4) . ?
C6 C7 1.493(3) . ?
C7 C18 1.375(4) . ?
C7 C27 1.380(4) . ?
C8 C56 1.37(2) . ?
C8 C32 1.386(4) . ?
C8 C50 1.568(18) . ?
C9 C11 1.387(4) . ?
C9 C10 1.392(4) . ?
C9 H9 0.9300 . ?
C10 C15 1.492(3) . ?
C11 C16 1.493(3) . ?
C12 C13 1.395(3) . ?
C13 H13 0.9300 . ?
C14 C34 1.380(4) . ?
C14 C16 1.391(4) . ?
C14 H14 0.9300 . ?
C15 C17 1.378(4) . ?
C15 C25 1.390(4) . ?
C16 C26 1.379(4) . ?
C17 C31 1.368(4) . ?
C17 N29 1.368(4) . ?
C17 H17 0.9300 . ?
C18 C24 1.363(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.363(4) . ?
C19 C23 1.376(4) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C32 1.388(4) . ?
C21 C46 1.39(2) . ?
C21 C42 1.57(2) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 N30 1.371(4) . ?
C25 C28 1.371(4) . ?
C25 H25 0.9300 . ?
C26 C35 1.357(4) . ?
C26 H26 0.9300 . ?
C27 C36 1.390(5) . ?
C27 H27 0.9300 . ?
C28 C33 1.349(5) . ?
C28 H28 0.9300 . ?
N29 C33 1.315(5) . ?
N30 C33 1.349(5) . ?
C31 C33 1.315(5) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C42 1.28(4) . ?
C37 C38 1.52(4) . ?
C37 H37 0.9300 . ?
C38 N41 1.30(2) . ?
C38 H38 0.9300 . ?
C39 C40 1.360(15) . ?
C39 C42 1.41(3) . ?
C39 H39 0.9300 . ?
C40 N41 1.301(17) . ?
C40 H40 0.9300 . ?
N43 C47 1.33(3) . ?
N43 C45 1.37(2) . ?
C44 C45 1.377(17) . ?
C44 C46 1.38(3) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 C48 1.50(4) . ?
C47 C48 1.23(5) . ?
C47 H47 0.9300 . ?
C48 H48 0.9300 . ?
C49 C58 1.11(3) . ?
C49 C57 1.20(4) . ?
C49 H49 0.9300 . ?
C50 C51 1.18(4) . ?
C50 C53 1.42(3) . ?
N1A C52 1.44(2) . ?
N1A C51 1.46(3) . ?
C51 H51 0.9300 . ?
C52 C54 1.364(15) . ?
C52 H52 0.9300 . ?
C53 C54 1.357(15) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 C56 1.37(3) . ?
C55 N4A 1.398(17) . ?
C55 H55 0.9300 . ?
C56 C57 1.56(4) . ?
C57 H57 0.9300 . ?
C58 N4A 1.410(19) . ?
C58 H58 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
Cl1 C1 Cl1 117.3(4) . 2_656 ?
Cl1 C1 H1A 108.0 . . ?
Cl1 C1 H1A 108.0 2_656 . ?
Cl1 C1 H1B 108.0 . . ?
Cl1 C1 H1B 108.0 2_656 . ?
H1A C1 H1B 107.2 . . ?
O6 Fe1 O3 92.76(7) . . ?
O6 Fe1 O5 85.26(7) . . ?
O3 Fe1 O5 172.99(7) . . ?
O6 Fe1 O2 170.51(8) . . ?
O3 Fe1 O2 96.43(8) . . ?
O5 Fe1 O2 85.89(7) . . ?
O6 Fe1 O4 95.13(7) . . ?
O3 Fe1 O4 86.16(7) . . ?
O5 Fe1 O4 87.33(7) . . ?
O2 Fe1 O4 87.87(7) . . ?
O6 Fe1 O1 91.31(7) . . ?
O3 Fe1 O1 87.36(7) . . ?
O5 Fe1 O1 99.39(8) . . ?
O2 Fe1 O1 86.76(7) . . ?
O4 Fe1 O1 171.07(7) . . ?
C1 Cl1 C1 62.7(4) . 2_656 ?
C10 O1 Fe1 128.81(17) . . ?
C11 O2 Fe1 127.76(16) . . ?
C8 O3 Fe1 128.63(17) . . ?
C35 N3 C34 118.8(3) . . ?
C21 O4 Fe1 128.73(17) . . ?
C12 O5 Fe1 126.09(16) . . ?
C6 O6 Fe1 126.78(16) . . ?
C24 N1 C36 115.6(3) . . ?
C20 N2 C22 117.2(3) . . ?
C3 C2 C2 119.4(5) . 2_575 ?
C3 C2 H2A 107.5 . . ?
C2 C2 H2A 107.5 2_575 . ?
C3 C2 H2B 107.5 . . ?
C2 C2 H2B 107.5 2_575 . ?
H2A C2 H2B 107.0 . . ?
C2 C3 C4 117.5(4) . . ?
C2 C3 H3A 107.9 . . ?
C4 C3 H3A 107.9 . . ?
C2 C3 H3B 107.9 . . ?
C4 C3 H3B 107.9 . . ?
H3A C3 H3B 107.2 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C22 C5 C23 117.3(2) . . ?
C22 C5 C12 123.3(2) . . ?
C23 C5 C12 119.5(2) . . ?
O6 C6 C13 124.3(2) . . ?
O6 C6 C7 114.6(2) . . ?
C13 C6 C7 121.1(2) . . ?
C18 C7 C27 116.4(2) . . ?
C18 C7 C6 119.5(2) . . ?
C27 C7 C6 124.1(2) . . ?
O3 C8 C56 117.8(12) . . ?
O3 C8 C32 124.3(2) . . ?
C56 C8 C32 117.9(12) . . ?
O3 C8 C50 113.3(10) . . ?
C32 C8 C50 122.3(10) . . ?
C11 C9 C10 123.8(2) . . ?
C11 C9 H9 118.1 . . ?
C10 C9 H9 118.1 . . ?
O1 C10 C9 124.3(2) . . ?
O1 C10 C15 115.5(2) . . ?
C9 C10 C15 120.1(2) . . ?
O2 C11 C9 124.4(2) . . ?
O2 C11 C16 115.5(2) . . ?
C9 C11 C16 120.1(2) . . ?
O5 C12 C13 124.0(2) . . ?
O5 C12 C5 114.7(2) . . ?
C13 C12 C5 121.3(2) . . ?
C6 C13 C12 122.5(2) . . ?
C6 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
C34 C14 C16 119.4(3) . . ?
C34 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
C17 C15 C25 116.7(3) . . ?
C17 C15 C10 120.6(2) . . ?
C25 C15 C10 122.6(2) . . ?
C26 C16 C14 117.7(3) . . ?
C26 C16 C11 119.5(2) . . ?
C14 C16 C11 122.8(3) . . ?
C31 C17 C15 120.8(3) . . ?
N29 C17 C15 120.8(3) . . ?
N29 C17 H17 119.6 . . ?
C15 C17 H17 119.6 . . ?
C24 C18 C7 120.5(3) . . ?
C24 C18 H18 119.7 . . ?
C7 C18 H18 119.7 . . ?
C20 C19 C23 119.2(3) . . ?
C20 C19 H19 120.4 . . ?
C23 C19 H19 120.4 . . ?
N2 C20 C19 123.3(3) . . ?
N2 C20 H20 118.3 . . ?
C19 C20 H20 118.3 . . ?
O4 C21 C32 124.0(2) . . ?
O4 C21 C46 115.4(11) . . ?
C32 C21 C46 120.5(11) . . ?
O4 C21 C42 115.8(11) . . ?
C32 C21 C42 120.2(11) . . ?
N2 C22 C5 123.6(3) . . ?
N2 C22 H22 118.2 . . ?
C5 C22 H22 118.2 . . ?
C19 C23 C5 119.4(3) . . ?
C19 C23 H23 120.3 . . ?
C5 C23 H23 120.3 . . ?
N1 C24 C18 124.3(3) . . ?
N1 C24 H24 117.8 . . ?
C18 C24 H24 117.8 . . ?
N30 C25 C15 120.4(3) . . ?
C28 C25 C15 120.4(3) . . ?
C28 C25 H25 119.8 . . ?
C15 C25 H25 119.8 . . ?
C35 C26 C16 120.2(3) . . ?
C35 C26 H26 119.9 . . ?
C16 C26 H26 119.9 . . ?
C7 C27 C36 118.2(3) . . ?
C7 C27 H27 120.9 . . ?
C36 C27 H27 120.9 . . ?
C33 C28 C25 120.7(3) . . ?
C33 C28 H28 119.7 . . ?
C25 C28 H28 119.7 . . ?
C33 N29 C17 121.6(3) . . ?
C33 N30 C25 120.7(3) . . ?
C33 C31 C17 121.6(3) . . ?
C33 C31 H31 119.2 . . ?
C17 C31 H31 119.2 . . ?
C8 C32 C21 124.1(3) . . ?
C8 C32 H32 118.0 . . ?
C21 C32 H32 118.0 . . ?
N29 C33 C28 119.8(3) . . ?
C31 C33 N30 119.8(3) . . ?
N29 C33 H33 120.1 . . ?
C28 C33 H33 120.1 . . ?
N3 C34 C14 121.1(3) . . ?
N3 C34 H34 119.5 . . ?
C14 C34 H34 119.5 . . ?
N3 C35 C26 122.8(3) . . ?
N3 C35 H35 118.6 . . ?
C26 C35 H35 118.6 . . ?
N1 C36 C27 124.9(3) . . ?
N1 C36 H36 117.5 . . ?
C27 C36 H36 117.5 . . ?
C42 C37 C38 110(3) . . ?
C42 C37 H37 125.0 . . ?
C38 C37 H37 125.0 . . ?
N41 C38 C37 127(3) . . ?
N41 C38 H38 116.6 . . ?
C37 C38 H38 116.6 . . ?
C40 C39 C42 116.3(14) . . ?
C40 C39 H39 121.8 . . ?
C42 C39 H39 121.8 . . ?
N41 C40 C39 125.5(12) . . ?
N41 C40 H40 117.3 . . ?
C39 C40 H40 117.3 . . ?
C40 N41 C38 115.1(19) . . ?
C37 C42 C39 126(2) . . ?
C37 C42 C21 118(2) . . ?
C39 C42 C21 116.1(19) . . ?
C47 N43 C45 114(2) . . ?
C45 C44 C46 123.6(16) . . ?
C45 C44 H44 118.2 . . ?
C46 C44 H44 118.2 . . ?
N43 C45 C44 123.5(13) . . ?
N43 C45 H45 118.3 . . ?
C44 C45 H45 118.3 . . ?
C44 C46 C21 125(2) . . ?
C44 C46 C48 106(2) . . ?
C21 C46 C48 129(2) . . ?
C48 C47 N43 122(3) . . ?
C48 C47 H47 118.8 . . ?
N43 C47 H47 118.8 . . ?
C47 C48 C46 130(3) . . ?
C47 C48 H48 115.2 . . ?
C46 C48 H48 115.2 . . ?
C58 C49 C57 130(3) . . ?
C58 C49 H49 115.2 . . ?
C57 C49 H49 115.2 . . ?
C51 C50 C53 125(2) . . ?
C51 C50 C8 119(2) . . ?
C53 C50 C8 115.0(17) . . ?
C52 N1A C51 109.8(18) . . ?
C50 C51 N1A 125(3) . . ?
C50 C51 H51 117.6 . . ?
N1A C51 H51 117.6 . . ?
C54 C52 N1A 123.8(13) . . ?
C54 C52 H52 118.1 . . ?
N1A C52 H52 118.1 . . ?
C54 C53 C50 116.7(13) . . ?
C54 C53 H53 121.7 . . ?
C50 C53 H53 121.7 . . ?
C53 C54 C52 118.6(11) . . ?
C53 C54 H54 120.7 . . ?
C52 C54 H54 120.7 . . ?
C56 C55 N4A 123.6(16) . . ?
C56 C55 H55 118.2 . . ?
N4A C55 H55 118.2 . . ?
C55 C56 C8 131(2) . . ?
C55 C56 C57 106.0(19) . . ?
C8 C56 C57 123(2) . . ?
C49 C57 C56 123(3) . . ?
C49 C57 H57 118.6 . . ?
C56 C57 H57 118.6 . . ?
C49 C58 N4A 120(2) . . ?
C49 C58 H58 120.0 . . ?
N4A C58 H58 120.0 . . ?
C55 N4A C58 116.5(13) . . ?

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
Cl1 C1 Cl1 C1 -0.002(1) 2_656 . . 2_656 ?
C2 C2 C3 C4 -180.0(5) 2_575 . . . ?
Fe1 O6 C6 C13 18.1(3) . . . . ?
Fe1 O6 C6 C7 -163.68(16) . . . . ?
O6 C6 C7 C18 -8.3(3) . . . . ?
C13 C6 C7 C18 169.9(3) . . . . ?
O6 C6 C7 C27 171.8(3) . . . . ?
C13 C6 C7 C27 -10.0(4) . . . . ?
Fe1 O3 C8 C56 -164.5(16) . . . . ?
Fe1 O3 C8 C32 15.3(4) . . . . ?
Fe1 O3 C8 C50 -164.2(13) . . . . ?
Fe1 O1 C10 C9 0.1(4) . . . . ?
Fe1 O1 C10 C15 177.08(15) . . . . ?
C11 C9 C10 O1 11.3(4) . . . . ?
C11 C9 C10 C15 -165.6(2) . . . . ?
Fe1 O2 C11 C9 -19.2(4) . . . . ?
Fe1 O2 C11 C16 162.05(17) . . . . ?
C10 C9 C11 O2 -1.2(4) . . . . ?
C10 C9 C11 C16 177.4(2) . . . . ?
Fe1 O5 C12 C13 -22.0(3) . . . . ?
Fe1 O5 C12 C5 159.16(16) . . . . ?
C22 C5 C12 O5 164.5(2) . . . . ?
C23 C5 C12 O5 -14.7(3) . . . . ?
C22 C5 C12 C13 -14.4(4) . . . . ?
C23 C5 C12 C13 166.4(2) . . . . ?
O6 C6 C13 C12 7.9(4) . . . . ?
C7 C6 C13 C12 -170.2(2) . . . . ?
O5 C12 C13 C6 -5.7(4) . . . . ?
C5 C12 C13 C6 173.1(2) . . . . ?
O1 C10 C15 C17 11.1(4) . . . . ?
C9 C10 C15 C17 -171.8(3) . . . . ?
O1 C10 C15 C25 -163.5(3) . . . . ?
C9 C10 C15 C25 13.6(4) . . . . ?
C34 C14 C16 C26 0.2(4) . . . . ?
C34 C14 C16 C11 180.0(3) . . . . ?
O2 C11 C16 C26 -26.5(4) . . . . ?
C9 C11 C16 C26 154.7(3) . . . . ?
O2 C11 C16 C14 153.7(3) . . . . ?
C9 C11 C16 C14 -25.1(4) . . . . ?
C25 C15 C17 C31 0.2(4) . . . . ?
C10 C15 C17 C31 -174.6(3) . . . . ?
C25 C15 C17 N29 0.2(4) . . . . ?
C10 C15 C17 N29 -174.6(3) . . . . ?
C27 C7 C18 C24 -1.2(5) . . . . ?
C6 C7 C18 C24 178.9(3) . . . . ?
C22 N2 C20 C19 0.4(5) . . . . ?
C23 C19 C20 N2 -0.6(5) . . . . ?
Fe1 O4 C21 C32 -13.6(4) . . . . ?
Fe1 O4 C21 C46 165.0(16) . . . . ?
Fe1 O4 C21 C42 168.8(14) . . . . ?
C20 N2 C22 C5 0.1(5) . . . . ?
C23 C5 C22 N2 -0.4(4) . . . . ?
C12 C5 C22 N2 -179.6(3) . . . . ?
C20 C19 C23 C5 0.3(4) . . . . ?
C22 C5 C23 C19 0.2(4) . . . . ?
C12 C5 C23 C19 179.4(2) . . . . ?
C36 N1 C24 C18 2.9(6) . . . . ?
C7 C18 C24 N1 -0.9(5) . . . . ?
C17 C15 C25 N30 0.0(5) . . . . ?
C10 C15 C25 N30 174.7(3) . . . . ?
C17 C15 C25 C28 0.0(5) . . . . ?
C10 C15 C25 C28 174.7(3) . . . . ?
C14 C16 C26 C35 -0.1(4) . . . . ?
C11 C16 C26 C35 -179.9(3) . . . . ?
C18 C7 C27 C36 1.2(5) . . . . ?
C6 C7 C27 C36 -178.9(3) . . . . ?
C15 C25 C28 C33 0.1(5) . . . . ?
C15 C17 N29 C33 -0.5(5) . . . . ?
C15 C25 N30 C33 0.1(5) . . . . ?
C15 C17 C31 C33 -0.5(5) . . . . ?
O3 C8 C32 C21 0.3(5) . . . . ?
C56 C8 C32 C21 -179.9(16) . . . . ?
C50 C8 C32 C21 179.7(14) . . . . ?
O4 C21 C32 C8 -1.1(5) . . . . ?
C46 C21 C32 C8 -179.7(17) . . . . ?
C42 C21 C32 C8 176.4(15) . . . . ?
C17 C31 C33 N30 0.6(5) . . . . ?
C17 N29 C33 C28 0.6(5) . . . . ?
C25 C28 C33 N29 -0.3(5) . . . . ?
C25 N30 C33 C31 -0.3(5) . . . . ?
C35 N3 C34 C14 0.7(5) . . . . ?
C16 C14 C34 N3 -0.5(5) . . . . ?
C34 N3 C35 C26 -0.7(5) . . . . ?
C16 C26 C35 N3 0.3(5) . . . . ?
C24 N1 C36 C27 -2.9(7) . . . . ?
C7 C27 C36 N1 0.9(7) . . . . ?
C42 C37 C38 N41 3(6) . . . . ?
C42 C39 C40 N41 -2(2) . . . . ?
C39 C40 N41 C38 -2(3) . . . . ?
C37 C38 N41 C40 2(5) . . . . ?
C38 C37 C42 C39 -8(5) . . . . ?
C38 C37 C42 C21 -178(3) . . . . ?
C40 C39 C42 C37 8(4) . . . . ?
C40 C39 C42 C21 178.5(16) . . . . ?
O4 C21 C42 C37 -174(3) . . . . ?
C32 C21 C42 C37 8(4) . . . . ?
O4 C21 C42 C39 15(3) . . . . ?
C32 C21 C42 C39 -162.8(15) . . . . ?
C47 N43 C45 C44 5(3) . . . . ?
C46 C44 C45 N43 2(3) . . . . ?
C45 C44 C46 C21 -180(2) . . . . ?
C45 C44 C46 C48 -7(3) . . . . ?
O4 C21 C46 C44 -8(4) . . . . ?
C32 C21 C46 C44 171(2) . . . . ?
O4 C21 C46 C48 -178(3) . . . . ?
C32 C21 C46 C48 0(4) . . . . ?
C45 N43 C47 C48 -6(5) . . . . ?
N43 C47 C48 C46 0(7) . . . . ?
C44 C46 C48 C47 7(6) . . . . ?
C21 C46 C48 C47 179(4) . . . . ?
O3 C8 C50 C51 -26(4) . . . . ?
C32 C8 C50 C51 154(3) . . . . ?
O3 C8 C50 C53 142.4(16) . . . . ?
C32 C8 C50 C53 -37(3) . . . . ?
C53 C50 C51 N1A 3(6) . . . . ?
C8 C50 C51 N1A 171(2) . . . . ?
C52 N1A C51 C50 7(4) . . . . ?
C51 N1A C52 C54 -13(3) . . . . ?
C51 C50 C53 C54 -7(4) . . . . ?
C8 C50 C53 C54 -174.8(15) . . . . ?
C50 C53 C54 C52 0(2) . . . . ?
N1A C52 C54 C53 11(2) . . . . ?
N4A C55 C56 C8 -179(2) . . . . ?
N4A C55 C56 C57 8(4) . . . . ?
O3 C8 C56 C55 170(3) . . . . ?
C32 C8 C56 C55 -10(4) . . . . ?
O3 C8 C56 C57 -18(4) . . . . ?
C32 C8 C56 C57 162(3) . . . . ?
C58 C49 C57 C56 -12(6) . . . . ?
C55 C56 C57 C49 2(5) . . . . ?
C8 C56 C57 C49 -172(3) . . . . ?
C57 C49 C58 N4A 10(5) . . . . ?
C56 C55 N4A C58 -11(3) . . . . ?
C49 C58 N4A C55 2(3) . . . . ?

_refine_diff_density_max         0.928
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_CPX3
_database_code_depnum_ccdc_archive 'CCDC 1545275'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C39 H27 Fe N6 O6), 0.5(H2 O)'
_chemical_formula_sum            'C39 H28 Fe N6 O6.50'
_chemical_formula_weight         740.52

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

_cell_length_a                   13.7398(16)
_cell_length_b                   13.7398(16)
_cell_length_c                   33.050(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5403.3(17)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6375
_cell_measurement_theta_min      2.9991
_cell_measurement_theta_max      27.4894

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             2292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.476
_shelx_estimated_absorpt_T_min   0.911
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_process_details   sadabs

_exptl_special_details           ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'AFC10: Fixed Chi 2 circle'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14450
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         3.001
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_full        24.995
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2118
_reflns_number_gt                1876
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0935P)²+3.4312P] 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         2118
_refine_ls_number_parameters     246
_refine_ls_number_restraints     516
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.1900
_refine_ls_wR_factor_gt          0.1807
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_restrained_S_all      1.117
_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 0.3333 0.6667 0.01899(3) 0.0760(4) Uani 1 3 d S T P . .
O1 O 0.20229(19) 0.6270(2) 0.05524(8) 0.0794(7) Uani 1 1 d . . . . .
O2 O 0.22959(19) 0.5350(2) -0.01438(7) 0.0787(7) Uani 1 1 d . . . . .
C2 C -0.0812(17) 0.4226(18) 0.0929(5) 0.095(6) Uani 0.3333 1 d G U P A 1
H2 H -0.1044 0.3730 0.0712 0.114 Uiso 0.3333 1 calc R U P A 1
C1 C -0.1544(13) 0.4041(15) 0.1248(6) 0.144(8) Uani 0.3333 1 d G U P A 1
H1 H -0.2266 0.3421 0.1244 0.173 Uiso 0.3333 1 calc R U P A 1
N1 N -0.1198(10) 0.4783(14) 0.1573(5) 0.106(5) Uani 0.3333 1 d G U P A 1
C3 C -0.0118(10) 0.5710(12) 0.1579(4) 0.075(4) Uani 0.3333 1 d G U P A 1
H3 H 0.0114 0.6206 0.1796 0.090 Uiso 0.3333 1 calc R U P A 1
C4 C 0.0614(12) 0.5895(13) 0.1260(5) 0.073(4) Uani 0.3333 1 d G U P A 1
H4 H 0.1336 0.6515 0.1264 0.088 Uiso 0.3333 1 calc R U P A 1
C5 C 0.0267(16) 0.5153(17) 0.0935(5) 0.049(3) Uani 0.3333 1 d G U P A 1
N1A N -0.0570(8) 0.4347(9) 0.0981(2) 0.092(2) Uani 0.6667 1 d G U P A 2
C1A C -0.1209(6) 0.4264(7) 0.1319(2) 0.102(2) Uani 0.6667 1 d G U P A 2
H1A H -0.1923 0.3643 0.1351 0.123 Uiso 0.6667 1 calc R U P A 2
C2A C -0.0780(6) 0.5110(6) 0.1609(2) 0.091(3) Uani 0.6667 1 d G U P A 2
H2A H -0.1208 0.5054 0.1835 0.109 Uiso 0.6667 1 calc R U P A 2
C3A C 0.0287(7) 0.6038(7) 0.1561(3) 0.120(4) Uani 0.6667 1 d G U P A 2
H3A H 0.0574 0.6603 0.1755 0.144 Uiso 0.6667 1 calc R U P A 2
C4A C 0.0926(7) 0.6121(8) 0.1223(3) 0.100(3) Uani 0.6667 1 d G U P A 2
H4A H 0.1640 0.6742 0.1191 0.120 Uiso 0.6667 1 calc R U P A 2
C5A C 0.0497(9) 0.5275(10) 0.0933(3) 0.078(3) Uani 0.6667 1 d G U P A 2
C6 C 0.1102(3) 0.5334(3) 0.05783(10) 0.0663(8) Uani 1 1 d . . . . .
C7 C 0.0750(3) 0.4464(3) 0.03005(10) 0.0728(9) Uani 1 1 d . . . . .
H7 H 0.0071 0.3810 0.0349 0.087 Uiso 1 1 calc R U . . .
C8 C 0.1348(3) 0.4511(3) -0.00447(10) 0.0655(8) Uani 1 1 d . . . . .
N2 N 0.0051(8) 0.1706(9) -0.0848(3) 0.106(3) Uani 0.6667 1 d . U P B 1
C9 C 0.0826(13) 0.3578(14) -0.0345(5) 0.058(2) Uani 0.6667 1 d . U P B 1
C10 C -0.0185(14) 0.2671(15) -0.0299(6) 0.095(4) Uani 0.6667 1 d . U P B 1
H10 H -0.0708 0.2620 -0.0109 0.115 Uiso 0.6667 1 calc R U P B 1
C11 C -0.0395(12) 0.1741(13) -0.0586(5) 0.131(5) Uani 0.6667 1 d . U P B 1
H11 H -0.1036 0.1062 -0.0526 0.157 Uiso 0.6667 1 calc R U P B 1
C12 C 0.1004(11) 0.2587(11) -0.0922(5) 0.107(4) Uani 0.6667 1 d . U P B 1
H12 H 0.1433 0.2571 -0.1137 0.128 Uiso 0.6667 1 calc R U P B 1
C13 C 0.1430(10) 0.3598(14) -0.0684(4) 0.083(3) Uani 0.6667 1 d . U P B 1
H13 H 0.2092 0.4245 -0.0755 0.100 Uiso 0.6667 1 calc R U P B 1
C10A C 0.039(2) 0.192(3) -0.0928(9) 0.105(7) Uani 0.3333 1 d . U P B 2
H10A H 0.0208 0.1396 -0.1133 0.126 Uiso 0.3333 1 calc R U P B 2
C9A C 0.102(3) 0.348(3) -0.0312(11) 0.057(4) Uani 0.3333 1 d . U P B 2
N2A N 0.000(2) 0.250(2) -0.0236(9) 0.098(7) Uani 0.3333 1 d . U P B 2
C11A C -0.061(2) 0.176(3) -0.0495(8) 0.115(7) Uani 0.3333 1 d . U P B 2
H11A H -0.1381 0.1249 -0.0477 0.139 Uiso 0.3333 1 calc R U P B 2
C12A C 0.134(2) 0.285(3) -0.0906(11) 0.108(7) Uani 0.3333 1 d . U P B 2
H12A H 0.1832 0.3015 -0.1123 0.129 Uiso 0.3333 1 calc R U P B 2
C13A C 0.169(2) 0.356(3) -0.0607(8) 0.073(4) Uani 0.3333 1 d . U P B 2
H13A H 0.2432 0.4141 -0.0604 0.087 Uiso 0.3333 1 calc R U P B 2
O1W O -0.3333 0.3333 0.1931(4) 0.143(5) Uani 0.5 3 d S T 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 O2 1.985(2) 3_565 ?
Fe1 O2 1.985(2) 2_665 ?
Fe1 O2 1.985(2) . ?
Fe1 O1 1.998(2) 3_565 ?
Fe1 O1 1.998(2) 2_665 ?
Fe1 O1 1.998(2) . ?
O1 C6 1.279(4) . ?
O2 C8 1.278(4) . ?
C2 C1 1.3900 . ?
C2 C5 1.3900 . ?
C2 H2 0.9300 . ?
C1 N1 1.3900 . ?
C1 H1 0.9300 . ?
N1 C3 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.575(13) . ?
N1A C1A 1.3900 . ?
N1A C5A 1.3900 . ?
C1A C2A 1.3900 . ?
C1A H1A 0.9300 . ?
C2A C3A 1.3900 . ?
C2A H2A 0.9300 . ?
C3A C4A 1.3900 . ?
C3A H3A 0.9300 . ?
C4A C5A 1.3900 . ?
C4A H4A 0.9300 . ?
C5A C6 1.415(7) . ?
C6 C7 1.388(4) . ?
C7 C8 1.388(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.490(17) . ?
C8 C9A 1.53(3) . ?
N2 C11 1.076(16) . ?
N2 C12 1.286(13) . ?
C9 C10 1.332(17) . ?
C9 C13 1.387(16) . ?
C10 C11 1.50(2) . ?
C10 H10 0.9300 . ?
C11 C12 2.01(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.442(18) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C10A C12A 1.29(3) . ?
C10A C11A 1.92(4) . ?
C10A H10A 0.9300 . ?
C9A C13A 1.31(3) . ?
C9A N2A 1.39(3) . ?
N2A C11A 1.28(4) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.30(3) . ?
C12A H12A 0.9300 . ?
C13A H13A 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
O2 Fe1 O2 92.13(10) 3_565 2_665 ?
O2 Fe1 O2 92.13(10) 3_565 . ?
O2 Fe1 O2 92.13(10) 2_665 . ?
O2 Fe1 O1 86.90(9) 3_565 3_565 ?
O2 Fe1 O1 93.31(10) 2_665 3_565 ?
O2 Fe1 O1 174.50(9) . 3_565 ?
O2 Fe1 O1 174.50(10) 3_565 2_665 ?
O2 Fe1 O1 86.90(9) 2_665 2_665 ?
O2 Fe1 O1 93.32(10) . 2_665 ?
O1 Fe1 O1 87.76(11) 3_565 2_665 ?
O2 Fe1 O1 93.32(10) 3_565 . ?
O2 Fe1 O1 174.50(9) 2_665 . ?
O2 Fe1 O1 86.90(9) . . ?
O1 Fe1 O1 87.76(11) 3_565 . ?
O1 Fe1 O1 87.75(11) 2_665 . ?
C6 O1 Fe1 128.2(2) . . ?
C8 O2 Fe1 128.6(2) . . ?
C1 C2 C5 120.0 . . ?
C1 C2 H2 120.0 . . ?
C5 C2 H2 120.0 . . ?
N1 C1 C2 120.0 . . ?
N1 C1 H1 120.0 . . ?
C2 C1 H1 120.0 . . ?
C3 N1 C1 120.0 . . ?
C4 C3 N1 120.0 . . ?
C4 C3 H3 120.0 . . ?
N1 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C2 120.0 . . ?
C4 C5 C6 120.4(10) . . ?
C2 C5 C6 119.6(10) . . ?
C1A N1A C5A 120.0 . . ?
N1A C1A C2A 120.0 . . ?
N1A C1A H1A 120.0 . . ?
C2A C1A H1A 120.0 . . ?
C3A C2A C1A 120.0 . . ?
C3A C2A H2A 120.0 . . ?
C1A C2A H2A 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C4A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C3A C4A C5A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C4A C5A N1A 120.0 . . ?
C4A C5A C6 122.2(7) . . ?
N1A C5A C6 117.8(7) . . ?
O1 C6 C7 124.4(3) . . ?
O1 C6 C5A 111.7(5) . . ?
C7 C6 C5A 123.9(5) . . ?
O1 C6 C5 119.0(7) . . ?
C7 C6 C5 116.5(7) . . ?
C6 C7 C8 124.1(3) . . ?
C6 C7 H7 118.0 . . ?
C8 C7 H7 118.0 . . ?
O2 C8 C7 124.4(3) . . ?
O2 C8 C9 116.2(7) . . ?
C7 C8 C9 119.2(7) . . ?
O2 C8 C9A 112.7(13) . . ?
C7 C8 C9A 122.3(14) . . ?
C11 N2 C12 116.4(14) . . ?
C10 C9 C13 116.3(14) . . ?
C10 C9 C8 123.9(13) . . ?
C13 C9 C8 119.7(12) . . ?
C9 C10 C11 113.1(15) . . ?
C9 C10 H10 123.4 . . ?
C11 C10 H10 123.4 . . ?
N2 C11 C10 132.6(16) . . ?
N2 C11 C12 35.0(8) . . ?
C10 C11 C12 97.8(11) . . ?
N2 C11 H11 113.7 . . ?
C10 C11 H11 113.7 . . ?
C12 C11 H11 148.3 . . ?
N2 C12 C13 122.4(12) . . ?
N2 C12 C11 28.7(7) . . ?
C13 C12 C11 93.8(10) . . ?
N2 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C11 C12 H12 147.4 . . ?
C9 C13 C12 118.1(13) . . ?
C9 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C12A C10A C11A 113(3) . . ?
C12A C10A H10A 123.5 . . ?
C11A C10A H10A 123.5 . . ?
C13A C9A N2A 123(3) . . ?
C13A C9A C8 119(3) . . ?
N2A C9A C8 119(2) . . ?
C11A N2A C9A 127(3) . . ?
N2A C11A C10A 105(2) . . ?
N2A C11A H11A 127.7 . . ?
C10A C11A H11A 127.7 . . ?
C10A C12A C13A 126(3) . . ?
C10A C12A H12A 116.9 . . ?
C13A C12A H12A 116.9 . . ?
C12A C13A C9A 122(3) . . ?
C12A C13A H13A 119.2 . . ?
C9A C13A H13A 119.2 . . ?

_refine_diff_density_max         0.248
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.041

####################################################################### 
# 
# 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_CPX4
_database_code_depnum_ccdc_archive 'CCDC 1505684'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H27 Fe N6 O6, 0.5(C6 H14)'
_chemical_formula_sum            'C42 H34 Fe N6 O6'
_chemical_formula_weight         774.60

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'
N N 0.0061 0.0033 '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'

_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                   10.600(3)
_cell_length_b                   12.147(4)
_cell_length_c                   16.590(5)
_cell_angle_alpha                77.320(9)
_cell_angle_beta                 73.287(9)
_cell_angle_gamma                74.385(9)
_cell_volume                     1946.8(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9791
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      30.55

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             804
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.442
_shelx_estimated_absorpt_T_min   0.917
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_process_details   sadabs

_exptl_special_details           ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6846
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.328
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6846
_reflns_number_gt                5458
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0861P)²+3.9524P] 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         6846
_refine_ls_number_parameters     586
_refine_ls_number_restraints     972
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0744
_refine_ls_wR_factor_ref         0.2016
_refine_ls_wR_factor_gt          0.1914
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.027
_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 0.21043(6) 0.29611(5) 0.24941(3) 0.0409(2) Uani 1 1 d . U . . .
O1 O 0.0972(3) 0.3311(3) 0.36272(16) 0.0453(7) Uani 1 1 d . U . . .
O2 O 0.3410(3) 0.3696(3) 0.27277(17) 0.0471(7) Uani 1 1 d . U . . .
O3 O 0.1029(3) 0.4357(3) 0.19089(17) 0.0488(7) Uani 1 1 d . U . . .
O4 O 0.3391(3) 0.2818(2) 0.13570(17) 0.0488(7) Uani 1 1 d . U . . .
O5 O 0.0868(3) 0.2069(2) 0.23681(18) 0.0467(7) Uani 1 1 d . U . . .
O6 O 0.3163(3) 0.1436(3) 0.29416(18) 0.0478(7) Uani 1 1 d . U . . .
N2 N 0.6392(5) 0.4450(5) 0.4069(3) 0.0790(14) Uani 1 1 d . U . . .
N3 N -0.1876(6) 0.7573(5) 0.0461(4) 0.1002(17) Uani 1 1 d . U . . .
N4 N 0.7124(5) 0.2360(5) -0.0344(4) 0.0977(17) Uani 1 1 d . U . . .
C1 C 0.0327(10) 0.3369(9) 0.5101(5) 0.0410(18) Uani 0.5 1 d G U P A 1
C2 C 0.0721(7) 0.3111(8) 0.5863(6) 0.056(2) Uani 0.5 1 d G U P A 1
H2 H 0.1628 0.2993 0.5858 0.067 Uiso 0.5 1 calc R U P A 1
C3 C -0.0239(9) 0.3029(9) 0.6635(5) 0.071(2) Uani 0.5 1 d G U P A 1
H3 H 0.0025 0.2857 0.7145 0.086 Uiso 0.5 1 calc R U P A 1
N1 N -0.1594(8) 0.3206(9) 0.6644(5) 0.072(2) Uani 0.5 1 d G U P A 1
C4 C -0.1988(8) 0.3463(9) 0.5881(6) 0.056(2) Uani 0.5 1 d G U P A 1
H4 H -0.2895 0.3581 0.5887 0.067 Uiso 0.5 1 calc R U P A 1
C5 C -0.1028(11) 0.3545(9) 0.5110(5) 0.0456(19) Uani 0.5 1 d G U P A 1
H5 H -0.1292 0.3717 0.4600 0.055 Uiso 0.5 1 calc R U P A 1
C1A C 0.0302(10) 0.3367(9) 0.5098(5) 0.0411(18) Uani 0.5 1 d G U P A 2
C2A C 0.0459(7) 0.3501(8) 0.5872(6) 0.0464(19) Uani 0.5 1 d G U P A 2
H2A H 0.1286 0.3581 0.5912 0.056 Uiso 0.5 1 calc R U P A 2
C3A C -0.0621(8) 0.3517(8) 0.6586(5) 0.055(2) Uani 0.5 1 d G U P A 2
H3A H -0.0516 0.3607 0.7104 0.066 Uiso 0.5 1 calc R U P A 2
N1A N -0.1858(7) 0.3399(9) 0.6526(6) 0.067(2) Uani 0.5 1 d G U P A 2
C5A C -0.2015(9) 0.3265(10) 0.5752(7) 0.069(2) Uani 0.5 1 d G U P A 2
H5A H -0.2842 0.3186 0.5712 0.083 Uiso 0.5 1 calc R U P A 2
C4A C -0.0935(11) 0.3249(10) 0.5038(6) 0.052(2) Uani 0.5 1 d G U P A 2
H4A H -0.1039 0.3159 0.4520 0.063 Uiso 0.5 1 calc R U P A 2
C6 C 0.4914(4) 0.3938(4) 0.3415(3) 0.0449(9) Uani 1 1 d . U . . .
C7 C 0.5910(5) 0.3919(4) 0.2663(3) 0.0600(12) Uani 1 1 d . U . . .
H7 H 0.5758 0.3754 0.2182 0.072 Uiso 1 1 calc R U . . .
C8 C 0.7123(5) 0.4144(5) 0.2634(4) 0.0693(14) Uani 1 1 d . U . . .
H8 H 0.7803 0.4125 0.2133 0.083 Uiso 1 1 calc R U . . .
C9 C 0.7328(5) 0.4395(5) 0.3334(4) 0.0716(14) Uani 1 1 d . U . . .
H9 H 0.8162 0.4537 0.3301 0.086 Uiso 1 1 calc R U . . .
C10 C 0.5208(5) 0.4211(5) 0.4105(3) 0.0645(13) Uani 1 1 d . U . . .
H10 H 0.4552 0.4228 0.4617 0.077 Uiso 1 1 calc R U . . .
C11 C 0.1371(4) 0.3393(3) 0.4265(2) 0.0371(8) Uani 1 1 d . U . . .
C12 C 0.2659(4) 0.3511(4) 0.4222(3) 0.0457(10) Uani 1 1 d . U . . .
H12 H 0.2901 0.3465 0.4727 0.055 Uiso 1 1 calc R U . . .
C13 C 0.3606(4) 0.3698(3) 0.3445(3) 0.0405(9) Uani 1 1 d . U . . .
C14 C 0.0258(4) 0.5866(4) 0.0897(3) 0.0450(10) Uani 1 1 d . U . . .
C15 C -0.0900(5) 0.6265(5) 0.1487(3) 0.0617(12) Uani 1 1 d . U . . .
H15 H -0.0978 0.5958 0.2060 0.074 Uiso 1 1 calc R U . . .
C16 C -0.1913(6) 0.7082(5) 0.1254(4) 0.0770(16) Uani 1 1 d . U . . .
H16 H -0.2682 0.7314 0.1674 0.092 Uiso 1 1 calc R U . . .
C17 C -0.0743(7) 0.7192(6) -0.0150(4) 0.0893(19) Uani 1 1 d . U . . .
H17 H -0.0694 0.7509 -0.0719 0.107 Uiso 1 1 calc R U . . .
C18 C 0.0302(6) 0.6365(5) 0.0062(4) 0.0783(17) Uani 1 1 d . U . . .
H18 H 0.1063 0.6130 -0.0362 0.094 Uiso 1 1 calc R U . . .
C19 C 0.4806(5) 0.3325(4) 0.0029(3) 0.0487(10) Uani 1 1 d . U . . .
C20 C 0.4936(6) 0.3786(5) -0.0823(3) 0.0648(13) Uani 1 1 d . U . . .
H20 H 0.4207 0.4289 -0.1008 0.078 Uiso 1 1 calc R U . . .
C21 C 0.6162(7) 0.3490(6) -0.1396(4) 0.0804(16) Uani 1 1 d . U . . .
H21 H 0.6243 0.3790 -0.1970 0.096 Uiso 1 1 calc R U . . .
C22 C 0.7222(6) 0.2792(5) -0.1151(4) 0.0772(16) Uani 1 1 d . U . . .
H22 H 0.8036 0.2608 -0.1549 0.093 Uiso 1 1 calc R U . . .
C23 C 0.5942(5) 0.2608(5) 0.0260(4) 0.0687(14) Uani 1 1 d . U . . .
H23 H 0.5902 0.2292 0.0828 0.082 Uiso 1 1 calc R U . . .
C24 C 0.1351(4) 0.4885(3) 0.1150(2) 0.0412(9) Uani 1 1 d . U . . .
C25 C 0.2568(5) 0.4589(4) 0.0573(3) 0.0505(11) Uani 1 1 d . U . . .
H25 H 0.2755 0.5100 0.0070 0.061 Uiso 1 1 calc R U . . .
C26 C 0.3526(4) 0.3584(4) 0.0693(2) 0.0420(9) Uani 1 1 d . U . . .
C32 C 0.4245(10) -0.0561(11) 0.3091(9) 0.056(4) Uani 0.5 1 d G U P B 1
C33 C 0.4195(12) -0.1711(12) 0.3158(11) 0.058(4) Uani 0.5 1 d G U P B 1
H33 H 0.3462 -0.1891 0.3056 0.070 Uiso 0.5 1 calc R U P B 1
C34 C 0.5241(16) -0.2592(9) 0.3379(12) 0.086(5) Uani 0.5 1 d G U P B 1
H34 H 0.5208 -0.3361 0.3425 0.104 Uiso 0.5 1 calc R U P B 1
N6 N 0.6338(14) -0.2323(10) 0.3533(11) 0.103(5) Uani 0.5 1 d G U P B 1
C35 C 0.6387(10) -0.1174(11) 0.3465(9) 0.107(6) Uani 0.5 1 d G U P B 1
H35 H 0.7121 -0.0994 0.3568 0.128 Uiso 0.5 1 calc R U P B 1
C36 C 0.5341(11) -0.0293(9) 0.3244(8) 0.084(5) Uani 0.5 1 d G U P B 1
H36 H 0.5375 0.0476 0.3199 0.101 Uiso 0.5 1 calc R U P B 1
C32A C 0.4219(10) -0.0518(10) 0.3186(8) 0.053(4) Uani 0.5 1 d G U P B 2
C33A C 0.4537(12) -0.1619(10) 0.2966(9) 0.048(3) Uani 0.5 1 d G U P B 2
H33A H 0.4087 -0.1780 0.2616 0.057 Uiso 0.5 1 calc R U P B 2
C34A C 0.5529(14) -0.2477(8) 0.3271(10) 0.066(4) Uani 0.5 1 d G U P B 2
H34A H 0.5742 -0.3213 0.3124 0.079 Uiso 0.5 1 calc R U P B 2
N6A N 0.6202(13) -0.2235(10) 0.3795(10) 0.094(5) Uani 0.5 1 d G U P B 2
C35A C 0.5884(12) -0.1135(11) 0.4014(7) 0.103(5) Uani 0.5 1 d G U P B 2
H35A H 0.6334 -0.0973 0.4364 0.123 Uiso 0.5 1 calc R U P B 2
C36A C 0.4892(11) -0.0277(9) 0.3709(7) 0.082(5) Uani 0.5 1 d G U P B 2
H36A H 0.4679 0.0460 0.3856 0.098 Uiso 0.5 1 calc R U P B 2
C27 C 0.0076(11) 0.0619(9) 0.2060(7) 0.057(4) Uani 0.5 1 d G U P C 1
C28 C -0.1246(12) 0.1260(8) 0.2186(7) 0.054(3) Uani 0.5 1 d G U P C 1
H28 H -0.1531 0.1845 0.2520 0.065 Uiso 0.5 1 calc R U P C 1
C29 C -0.2144(10) 0.1029(9) 0.1811(8) 0.078(4) Uani 0.5 1 d G U P C 1
H29 H -0.3029 0.1458 0.1895 0.093 Uiso 0.5 1 calc R U P C 1
C30 C -0.1719(11) 0.0155(10) 0.1311(8) 0.088(4) Uani 0.5 1 d G U P C 1
H30 H -0.2320 0.0000 0.1060 0.105 Uiso 0.5 1 calc R U P C 1
N5 N -0.0396(11) -0.0487(9) 0.1185(7) 0.112(4) Uani 0.5 1 d G U P C 1
C31 C 0.0501(9) -0.0255(9) 0.1560(8) 0.082(4) Uani 0.5 1 d G U P C 1
H31 H 0.1386 -0.0685 0.1475 0.098 Uiso 0.5 1 calc R U P C 1
C27A C 0.0067(11) 0.0661(10) 0.2065(8) 0.057(4) Uani 0.5 1 d G U P C 2
C28A C -0.1068(13) 0.1511(8) 0.1945(8) 0.059(4) Uani 0.5 1 d G U P C 2
H28A H -0.1117 0.2274 0.1984 0.071 Uiso 0.5 1 calc R U P C 2
C29A C -0.2131(11) 0.1220(10) 0.1767(9) 0.083(5) Uani 0.5 1 d G U P C 2
H29A H -0.2890 0.1789 0.1686 0.100 Uiso 0.5 1 calc R U P C 2
C30A C -0.2059(11) 0.0080(12) 0.1709(9) 0.110(5) Uani 0.5 1 d G U P C 2
H30A H -0.2770 -0.0115 0.1590 0.132 Uiso 0.5 1 calc R U P C 2
N5A N -0.0924(14) -0.0770(9) 0.1829(10) 0.152(6) Uani 0.5 1 d G U P C 2
C31A C 0.0139(11) -0.0480(9) 0.2007(9) 0.112(6) Uani 0.5 1 d G U P C 2
H31A H 0.0898 -0.1049 0.2088 0.135 Uiso 0.5 1 calc R U P C 2
C37 C 0.1073(4) 0.0987(4) 0.2352(3) 0.0436(9) Uani 1 1 d . U . . .
C38 C 0.2143(5) 0.0170(4) 0.2590(3) 0.0576(12) Uani 1 1 d . U . . .
H38 H 0.2210 -0.0598 0.2555 0.069 Uiso 1 1 calc R U . . .
C39 C 0.3123(4) 0.0421(4) 0.2877(3) 0.0446(9) Uani 1 1 d . U . . .
C40 C 0.2729(13) 0.8755(10) 0.5596(6) 0.165(4) Uani 1 1 d . U . . .
H40A H 0.3333 0.8990 0.5825 0.247 Uiso 1 1 calc R U . . .
H40B H 0.2352 0.8156 0.5996 0.247 Uiso 1 1 calc R U . . .
H40C H 0.3216 0.8468 0.5072 0.247 Uiso 1 1 calc R U . . .
C41 C 0.1545(16) 0.9834(13) 0.5421(8) 0.185(5) Uani 1 1 d . U . . .
H41A H 0.1076 1.0128 0.5952 0.222 Uiso 1 1 calc R U . . .
H41B H 0.1938 1.0441 0.5028 0.222 Uiso 1 1 calc R U . . .
C42 C 0.0613(13) 0.9584(10) 0.5087(8) 0.172(5) Uani 1 1 d . U . . .
H42A H 0.0309 0.8926 0.5469 0.206 Uiso 1 1 calc R U . . .
H42B H 0.1116 0.9311 0.4554 0.206 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 1.983(3) . ?
Fe1 O5 1.989(3) . ?
Fe1 O4 1.996(3) . ?
Fe1 O2 1.997(3) . ?
Fe1 O3 1.997(3) . ?
Fe1 O6 2.000(3) . ?
O1 C11 1.278(5) . ?
O2 C13 1.267(5) . ?
O3 C24 1.277(5) . ?
O4 C26 1.277(5) . ?
O5 C37 1.277(5) . ?
O6 C39 1.274(5) . ?
N2 C9 1.335(7) . ?
N2 C10 1.345(7) . ?
N3 C16 1.314(8) . ?
N3 C17 1.374(9) . ?
N4 C22 1.311(8) . ?
N4 C23 1.369(7) . ?
C1 C2 1.3900 . ?
C1 C5 1.3900 . ?
C1 C11 1.506(8) . ?
C2 C3 1.3900 . ?
C2 H2 0.9300 . ?
C3 N1 1.3900 . ?
C3 H3 0.9300 . ?
N1 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C1A C2A 1.3900 . ?
C1A C4A 1.3900 . ?
C1A C11 1.514(8) . ?
C2A C3A 1.3900 . ?
C2A H2A 0.9300 . ?
C3A N1A 1.3900 . ?
C3A H3A 0.9300 . ?
N1A C5A 1.3900 . ?
C5A C4A 1.3900 . ?
C5A H5A 0.9300 . ?
C4A H4A 0.9300 . ?
C6 C7 1.384(6) . ?
C6 C10 1.394(7) . ?
C6 C13 1.477(6) . ?
C7 C8 1.371(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.350(8) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.391(6) . ?
C12 C13 1.404(6) . ?
C12 H12 0.9300 . ?
C14 C18 1.378(7) . ?
C14 C15 1.376(7) . ?
C14 C24 1.501(6) . ?
C15 C16 1.336(7) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.353(8) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C23 1.381(7) . ?
C19 C20 1.383(6) . ?
C19 C26 1.489(6) . ?
C20 C21 1.382(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.321(9) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.379(6) . ?
C25 C26 1.380(6) . ?
C25 H25 0.9300 . ?
C32 C33 1.3900 . ?
C32 C36 1.3900 . ?
C32 C39 1.503(11) . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 N6 1.3900 . ?
C34 H34 0.9300 . ?
N6 C35 1.3900 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C32A C33A 1.3900 . ?
C32A C36A 1.3900 . ?
C32A C39 1.512(10) . ?
C33A C34A 1.3900 . ?
C33A H33A 0.9300 . ?
C34A N6A 1.3900 . ?
C34A H34A 0.9300 . ?
N6A C35A 1.3900 . ?
C35A C36A 1.3900 . ?
C35A H35A 0.9300 . ?
C36A H36A 0.9300 . ?
C27 C28 1.3900 . ?
C27 C31 1.3900 . ?
C27 C37 1.482(9) . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 N5 1.3900 . ?
C30 H30 0.9300 . ?
N5 C31 1.3900 . ?
C31 H31 0.9300 . ?
C27A C28A 1.3900 . ?
C27A C31A 1.3900 . ?
C27A C37 1.458(10) . ?
C28A C29A 1.3900 . ?
C28A H28A 0.9300 . ?
C29A C30A 1.3900 . ?
C29A H29A 0.9300 . ?
C30A N5A 1.3900 . ?
C30A H30A 0.9300 . ?
N5A C31A 1.3900 . ?
C31A H31A 0.9300 . ?
C37 C38 1.380(6) . ?
C38 C39 1.384(6) . ?
C38 H38 0.9300 . ?
C40 C41 1.591(16) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.387(16) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C42 1.48(2) 2_576 ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?

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 O5 92.67(12) . . ?
O1 Fe1 O4 170.43(13) . . ?
O5 Fe1 O4 96.57(13) . . ?
O1 Fe1 O2 85.13(12) . . ?
O5 Fe1 O2 173.03(12) . . ?
O4 Fe1 O2 85.98(12) . . ?
O1 Fe1 O3 91.26(12) . . ?
O5 Fe1 O3 87.39(13) . . ?
O4 Fe1 O3 86.69(12) . . ?
O2 Fe1 O3 99.25(13) . . ?
O1 Fe1 O6 95.15(12) . . ?
O5 Fe1 O6 86.11(12) . . ?
O4 Fe1 O6 87.98(12) . . ?
O2 Fe1 O6 87.50(12) . . ?
O3 Fe1 O6 171.08(12) . . ?
C11 O1 Fe1 127.5(3) . . ?
C13 O2 Fe1 127.3(3) . . ?
C24 O3 Fe1 128.6(3) . . ?
C26 O4 Fe1 128.7(3) . . ?
C37 O5 Fe1 129.3(3) . . ?
C39 O6 Fe1 129.0(3) . . ?
C9 N2 C10 117.1(5) . . ?
C16 N3 C17 117.2(6) . . ?
C22 N4 C23 121.7(6) . . ?
C2 C1 C5 120.0 . . ?
C2 C1 C11 120.2(6) . . ?
C5 C1 C11 119.8(7) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 N1 120.0 . . ?
C2 C3 H3 120.0 . . ?
N1 C3 H3 120.0 . . ?
C4 N1 C3 120.0 . . ?
N1 C4 C5 120.0 . . ?
N1 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C1 120.0 . . ?
C4 C5 H5 120.0 . . ?
C1 C5 H5 120.0 . . ?
C2A C1A C4A 120.0 . . ?
C2A C1A C11 125.4(7) . . ?
C4A C1A C11 114.6(7) . . ?
C3A C2A C1A 120.0 . . ?
C3A C2A H2A 120.0 . . ?
C1A C2A H2A 120.0 . . ?
C2A C3A N1A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
N1A C3A H3A 120.0 . . ?
C5A N1A C3A 120.0 . . ?
N1A C5A C4A 120.0 . . ?
N1A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C4A C1A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C1A C4A H4A 120.0 . . ?
C7 C6 C10 117.0(4) . . ?
C7 C6 C13 119.3(4) . . ?
C10 C6 C13 123.7(4) . . ?
C8 C7 C6 119.4(5) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C9 C8 C7 119.8(5) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
N2 C9 C8 123.3(5) . . ?
N2 C9 H9 118.4 . . ?
C8 C9 H9 118.4 . . ?
N2 C10 C6 123.4(5) . . ?
N2 C10 H10 118.3 . . ?
C6 C10 H10 118.3 . . ?
O1 C11 C12 124.5(4) . . ?
O1 C11 C1 115.2(5) . . ?
C12 C11 C1 120.3(5) . . ?
O1 C11 C1A 114.2(5) . . ?
C12 C11 C1A 121.3(5) . . ?
C11 C12 C13 122.4(4) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
O2 C13 C12 123.7(4) . . ?
O2 C13 C6 115.1(4) . . ?
C12 C13 C6 121.1(4) . . ?
C18 C14 C15 115.9(5) . . ?
C18 C14 C24 122.5(4) . . ?
C15 C14 C24 121.4(4) . . ?
C16 C15 C14 121.5(5) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
N3 C16 C15 123.2(6) . . ?
N3 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
C18 C17 N3 121.2(6) . . ?
C18 C17 H17 119.4 . . ?
N3 C17 H17 119.4 . . ?
C17 C18 C14 121.0(6) . . ?
C17 C18 H18 119.5 . . ?
C14 C18 H18 119.5 . . ?
C23 C19 C20 117.1(5) . . ?
C23 C19 C26 119.7(4) . . ?
C20 C19 C26 123.2(4) . . ?
C21 C20 C19 119.2(6) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C22 C21 C20 121.8(6) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
N4 C22 C21 119.9(5) . . ?
N4 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
N4 C23 C19 120.3(5) . . ?
N4 C23 H23 119.9 . . ?
C19 C23 H23 119.9 . . ?
O3 C24 C25 124.9(4) . . ?
O3 C24 C14 114.5(4) . . ?
C25 C24 C14 120.5(4) . . ?
C24 C25 C26 124.3(4) . . ?
C24 C25 H25 117.9 . . ?
C26 C25 H25 117.9 . . ?
O4 C26 C25 123.8(4) . . ?
O4 C26 C19 115.5(4) . . ?
C25 C26 C19 120.7(4) . . ?
C33 C32 C36 120.0 . . ?
C33 C32 C39 122.0(7) . . ?
C36 C32 C39 117.9(7) . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 N6 120.0 . . ?
C33 C34 H34 120.0 . . ?
N6 C34 H34 120.0 . . ?
C35 N6 C34 120.0 . . ?
N6 C35 C36 120.0 . . ?
N6 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C32 120.0 . . ?
C35 C36 H36 120.0 . . ?
C32 C36 H36 120.0 . . ?
C33A C32A C36A 120.0 . . ?
C33A C32A C39 120.9(7) . . ?
C36A C32A C39 119.1(7) . . ?
C32A C33A C34A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
C33A C34A N6A 120.0 . . ?
C33A C34A H34A 120.0 . . ?
N6A C34A H34A 120.0 . . ?
C35A N6A C34A 120.0 . . ?
C36A C35A N6A 120.0 . . ?
C36A C35A H35A 120.0 . . ?
N6A C35A H35A 120.0 . . ?
C35A C36A C32A 120.0 . . ?
C35A C36A H36A 120.0 . . ?
C32A C36A H36A 120.0 . . ?
C28 C27 C31 120.0 . . ?
C28 C27 C37 119.3(7) . . ?
C31 C27 C37 120.1(7) . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
N5 C30 C29 120.0 . . ?
N5 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 N5 C31 120.0 . . ?
N5 C31 C27 120.0 . . ?
N5 C31 H31 120.0 . . ?
C27 C31 H31 120.0 . . ?
C28A C27A C31A 120.0 . . ?
C28A C27A C37 117.5(8) . . ?
C31A C27A C37 122.0(8) . . ?
C27A C28A C29A 120.0 . . ?
C27A C28A H28A 120.0 . . ?
C29A C28A H28A 120.0 . . ?
C30A C29A C28A 120.0 . . ?
C30A C29A H29A 120.0 . . ?
C28A C29A H29A 120.0 . . ?
C29A C30A N5A 120.0 . . ?
C29A C30A H30A 120.0 . . ?
N5A C30A H30A 120.0 . . ?
C30A N5A C31A 120.0 . . ?
N5A C31A C27A 120.0 . . ?
N5A C31A H31A 120.0 . . ?
C27A C31A H31A 120.0 . . ?
O5 C37 C38 124.1(4) . . ?
O5 C37 C27A 114.5(6) . . ?
C38 C37 C27A 121.4(6) . . ?
O5 C37 C27 116.3(5) . . ?
C38 C37 C27 119.6(6) . . ?
C37 C38 C39 124.2(4) . . ?
C37 C38 H38 117.9 . . ?
C39 C38 H38 117.9 . . ?
O6 C39 C38 124.3(4) . . ?
O6 C39 C32 117.8(6) . . ?
C38 C39 C32 117.9(6) . . ?
O6 C39 C32A 113.8(6) . . ?
C38 C39 C32A 121.9(6) . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C40 114.0(11) . . ?
C42 C41 H41A 108.8 . . ?
C40 C41 H41A 108.8 . . ?
C42 C41 H41B 108.8 . . ?
C40 C41 H41B 108.8 . . ?
H41A C41 H41B 107.6 . . ?
C41 C42 C42 124.6(15) . 2_576 ?
C41 C42 H42A 106.2 . . ?
C42 C42 H42A 106.2 2_576 . ?
C41 C42 H42B 106.2 . . ?
C42 C42 H42B 106.2 2_576 . ?
H42A C42 H42B 106.4 . . ?

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
C5 C1 C2 C3 0.0 . . . . ?
C11 C1 C2 C3 -176.6(8) . . . . ?
C1 C2 C3 N1 0.0 . . . . ?
C2 C3 N1 C4 0.0 . . . . ?
C3 N1 C4 C5 0.0 . . . . ?
N1 C4 C5 C1 0.0 . . . . ?
C2 C1 C5 C4 0.0 . . . . ?
C11 C1 C5 C4 176.6(8) . . . . ?
C4A C1A C2A C3A 0.0 . . . . ?
C11 C1A C2A C3A 176.9(8) . . . . ?
C1A C2A C3A N1A 0.0 . . . . ?
C2A C3A N1A C5A 0.0 . . . . ?
C3A N1A C5A C4A 0.0 . . . . ?
N1A C5A C4A C1A 0.0 . . . . ?
C2A C1A C4A C5A 0.0 . . . . ?
C11 C1A C4A C5A -177.2(8) . . . . ?
C10 C6 C7 C8 1.1(7) . . . . ?
C13 C6 C7 C8 179.8(4) . . . . ?
C6 C7 C8 C9 -0.8(8) . . . . ?
C10 N2 C9 C8 1.7(9) . . . . ?
C7 C8 C9 N2 -0.7(9) . . . . ?
C9 N2 C10 C6 -1.4(9) . . . . ?
C7 C6 C10 N2 0.0(8) . . . . ?
C13 C6 C10 N2 -178.7(5) . . . . ?
Fe1 O1 C11 C12 15.5(6) . . . . ?
Fe1 O1 C11 C1 -165.2(5) . . . . ?
Fe1 O1 C11 C1A -165.3(5) . . . . ?
C2 C1 C11 O1 161.1(5) . . . . ?
C5 C1 C11 O1 -15.5(7) . . . . ?
C2 C1 C11 C12 -19.7(8) . . . . ?
C5 C1 C11 C12 163.7(5) . . . . ?
C2A C1A C11 O1 -176.5(5) . . . . ?
C4A C1A C11 O1 0.5(7) . . . . ?
C2A C1A C11 C12 2.7(9) . . . . ?
C4A C1A C11 C12 179.8(5) . . . . ?
O1 C11 C12 C13 8.2(7) . . . . ?
C1 C11 C12 C13 -171.0(6) . . . . ?
C1A C11 C12 C13 -170.9(6) . . . . ?
Fe1 O2 C13 C12 -21.5(6) . . . . ?
Fe1 O2 C13 C6 159.7(3) . . . . ?
C11 C12 C13 O2 -5.0(7) . . . . ?
C11 C12 C13 C6 173.8(4) . . . . ?
C7 C6 C13 O2 -12.3(6) . . . . ?
C10 C6 C13 O2 166.4(4) . . . . ?
C7 C6 C13 C12 168.9(4) . . . . ?
C10 C6 C13 C12 -12.5(7) . . . . ?
C18 C14 C15 C16 0.3(8) . . . . ?
C24 C14 C15 C16 -175.3(5) . . . . ?
C17 N3 C16 C15 1.7(10) . . . . ?
C14 C15 C16 N3 -1.1(10) . . . . ?
C16 N3 C17 C18 -1.5(11) . . . . ?
N3 C17 C18 C14 0.8(11) . . . . ?
C15 C14 C18 C17 -0.2(9) . . . . ?
C24 C14 C18 C17 175.3(5) . . . . ?
C23 C19 C20 C21 1.7(8) . . . . ?
C26 C19 C20 C21 -179.5(5) . . . . ?
C19 C20 C21 C22 -1.1(9) . . . . ?
C23 N4 C22 C21 0.3(10) . . . . ?
C20 C21 C22 N4 0.1(10) . . . . ?
C22 N4 C23 C19 0.3(10) . . . . ?
C20 C19 C23 N4 -1.3(8) . . . . ?
C26 C19 C23 N4 179.8(5) . . . . ?
Fe1 O3 C24 C25 -1.3(6) . . . . ?
Fe1 O3 C24 C14 176.2(3) . . . . ?
C18 C14 C24 O3 -165.2(5) . . . . ?
C15 C14 C24 O3 10.0(6) . . . . ?
C18 C14 C24 C25 12.4(7) . . . . ?
C15 C14 C24 C25 -172.3(4) . . . . ?
O3 C24 C25 C26 9.9(7) . . . . ?
C14 C24 C25 C26 -167.6(4) . . . . ?
Fe1 O4 C26 C25 -17.0(6) . . . . ?
Fe1 O4 C26 C19 163.6(3) . . . . ?
C24 C25 C26 O4 -0.3(7) . . . . ?
C24 C25 C26 C19 179.1(4) . . . . ?
C23 C19 C26 O4 -25.9(6) . . . . ?
C20 C19 C26 O4 155.3(4) . . . . ?
C23 C19 C26 C25 154.6(5) . . . . ?
C20 C19 C26 C25 -24.2(7) . . . . ?
C36 C32 C33 C34 0.0 . . . . ?
C39 C32 C33 C34 -178.3(12) . . . . ?
C32 C33 C34 N6 0.0 . . . . ?
C33 C34 N6 C35 0.0 . . . . ?
C34 N6 C35 C36 0.0 . . . . ?
N6 C35 C36 C32 0.0 . . . . ?
C33 C32 C36 C35 0.0 . . . . ?
C39 C32 C36 C35 178.4(11) . . . . ?
C36A C32A C33A C34A 0.0 . . . . ?
C39 C32A C33A C34A -178.7(10) . . . . ?
C32A C33A C34A N6A 0.0 . . . . ?
C33A C34A N6A C35A 0.0 . . . . ?
C34A N6A C35A C36A 0.0 . . . . ?
N6A C35A C36A C32A 0.0 . . . . ?
C33A C32A C36A C35A 0.0 . . . . ?
C39 C32A C36A C35A 178.7(10) . . . . ?
C31 C27 C28 C29 0.0 . . . . ?
C37 C27 C28 C29 170.8(9) . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 N5 0.0 . . . . ?
C29 C30 N5 C31 0.0 . . . . ?
C30 N5 C31 C27 0.0 . . . . ?
C28 C27 C31 N5 0.0 . . . . ?
C37 C27 C31 N5 -170.8(9) . . . . ?
C31A C27A C28A C29A 0.0 . . . . ?
C37 C27A C28A C29A -172.6(10) . . . . ?
C27A C28A C29A C30A 0.0 . . . . ?
C28A C29A C30A N5A 0.0 . . . . ?
C29A C30A N5A C31A 0.0 . . . . ?
C30A N5A C31A C27A 0.0 . . . . ?
C28A C27A C31A N5A 0.0 . . . . ?
C37 C27A C31A N5A 172.3(10) . . . . ?
Fe1 O5 C37 C38 13.4(6) . . . . ?
Fe1 O5 C37 C27A -167.1(6) . . . . ?
Fe1 O5 C37 C27 -166.8(5) . . . . ?
C28A C27A C37 O5 -7.7(9) . . . . ?
C31A C27A C37 O5 179.8(6) . . . . ?
C28A C27A C37 C38 171.8(6) . . . . ?
C31A C27A C37 C38 -0.7(10) . . . . ?
C28 C27 C37 O5 -28.6(9) . . . . ?
C31 C27 C37 O5 142.2(6) . . . . ?
C28 C27 C37 C38 151.1(6) . . . . ?
C31 C27 C37 C38 -38.0(9) . . . . ?
O5 C37 C38 C39 0.2(8) . . . . ?
C27A C37 C38 C39 -179.2(7) . . . . ?
C27 C37 C38 C39 -179.6(7) . . . . ?
Fe1 O6 C39 C38 -11.3(6) . . . . ?
Fe1 O6 C39 C32 166.0(6) . . . . ?
Fe1 O6 C39 C32A 171.5(6) . . . . ?
C37 C38 C39 O6 -1.2(8) . . . . ?
C37 C38 C39 C32 -178.5(7) . . . . ?
C37 C38 C39 C32A 175.7(7) . . . . ?
C33 C32 C39 O6 170.6(7) . . . . ?
C36 C32 C39 O6 -7.8(11) . . . . ?
C33 C32 C39 C38 -11.9(11) . . . . ?
C36 C32 C39 C38 169.7(6) . . . . ?
C33A C32A C39 O6 -163.5(6) . . . . ?
C36A C32A C39 O6 17.8(9) . . . . ?
C33A C32A C39 C38 19.3(10) . . . . ?
C36A C32A C39 C38 -159.4(6) . . . . ?
C40 C41 C42 C42 176.6(15) . . . 2_576 ?

_refine_diff_density_max         0.424
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.072

####################################################################### 
# 
# 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_JM32FE
_database_code_depnum_ccdc_archive 'CCDC 1545276'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H27 Fe N6 O6, 4(H2 O)'
_chemical_formula_sum            'C39 H35 Fe N6 O10'
_chemical_formula_weight         803.58

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

_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'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   16.0478(7)
_cell_length_b                   16.0478(7)
_cell_length_c                   8.2848(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1847.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3002
_cell_measurement_theta_min      2.812
_cell_measurement_theta_max      27.146

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_F_000             834
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_absorpt_coefficient_mu    0.477
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.863333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1999)'

_exptl_special_details           
; 
The crystal was coated in Exxon Paratone N hydrocarbon
oil and mounted on a thin mohair fibre attached to a copper pin.
Upon mounting on the diffractometer,
the crystal was quenched to 150(K) under a cold nitrogen gas stream
supplied by an Oxford Cryosystems Cryostream and data were
collected at this temperature. 
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       ω+φ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13108
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.931
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3056
_reflns_number_gt                2149
_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       'APEX (Bruker-Nonius, 2003)'
_computing_cell_refinement       'SAINT (Bruker-Nonius, 2003)'
_computing_data_reduction        
'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999) 
;
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'
_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)+(0.0669P)²+1.5303P] 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         3056
_refine_ls_number_parameters     169
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1506
_refine_ls_wR_factor_gt          0.1327
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.6667 0.3333 0.22961(7) 0.03008(19) Uani 1 3 d S T P . .
O1 O 0.54982(12) 0.27563(13) 0.0904(2) 0.0352(4) Uani 1 1 d . . . . .
N1 N 0.2633(3) 0.1064(2) -0.2598(5) 0.0791(10) Uani 1 1 d . . . . .
C1 C 0.3579(3) 0.1451(3) -0.2793(4) 0.0629(10) Uani 1 1 d . . . . .
H1 H 0.3811 0.1385 -0.3812 0.075 Uiso 1 1 calc R U . . .
O2 O 0.59425(12) 0.37434(12) 0.3754(2) 0.0339(4) Uani 1 1 d . . . . .
N2 N 0.37377(18) 0.33827(19) 0.5437(3) 0.0506(6) Uani 1 1 d . . . . .
C2 C 0.4238(2) 0.1943(2) -0.1588(3) 0.0448(7) Uani 1 1 d . . . . .
H2 H 0.4907 0.2210 -0.1784 0.054 Uiso 1 1 calc R U . . .
O3 O 0.1944(2) 0.0998(3) 0.3888(4) 0.1079(11) Uani 1 1 d . . . . .
C3 C 0.39149(19) 0.20437(17) -0.0087(3) 0.0350(5) Uani 1 1 d . . . . .
O4 O 0.0000 0.0000 0.2822(6) 0.0734(12) Uani 1 3 d S T P . .
C4 C 0.2947(2) 0.1650(2) 0.0176(4) 0.0515(7) Uani 1 1 d . . . . .
H4 H 0.2703 0.1703 0.1192 0.062 Uiso 1 1 calc R U . . .
C5 C 0.2336(3) 0.1169(3) -0.1119(6) 0.0747(12) Uani 1 1 d . . . . .
H5 H 0.1664 0.0895 -0.0950 0.090 Uiso 1 1 calc R U . . .
C6 C 0.46438(17) 0.25867(16) 0.1212(3) 0.0303(5) Uani 1 1 d . . . . .
C7 C 0.43753(18) 0.28791(18) 0.2607(3) 0.0342(5) Uani 1 1 d . . . . .
H7 H 0.3718 0.2693 0.2750 0.041 Uiso 1 1 calc R U . . .
C8 C 0.50378(18) 0.34368(17) 0.3809(3) 0.0305(5) Uani 1 1 d . . . . .
C9 C 0.46923(18) 0.37156(18) 0.5288(3) 0.0336(5) Uani 1 1 d . . . . .
C10 C 0.5350(2) 0.4286(2) 0.6448(3) 0.0436(6) Uani 1 1 d . . . . .
H10 H 0.6017 0.4510 0.6311 0.052 Uiso 1 1 calc R U . . .
C11 C 0.5014(2) 0.4526(2) 0.7823(4) 0.0543(8) Uani 1 1 d . . . . .
H11 H 0.5454 0.4921 0.8632 0.065 Uiso 1 1 calc R U . . .
C12 C 0.4061(3) 0.4196(3) 0.8005(4) 0.0566(8) Uani 1 1 d . . . . .
H12 H 0.3823 0.4351 0.8939 0.068 Uiso 1 1 calc R U . . .
C13 C 0.3445(3) 0.3629(3) 0.6804(4) 0.0613(9) Uani 1 1 d . . . . .
H13 H 0.2776 0.3397 0.6938 0.074 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 1.9916(17) 2_655 ?
Fe1 O1 1.9916(17) . ?
Fe1 O1 1.9916(17) 3_665 ?
Fe1 O2 2.0019(17) 3_665 ?
Fe1 O2 2.0019(17) 2_655 ?
Fe1 O2 2.0019(17) . ?
O1 C6 1.283(3) . ?
N1 C1 1.331(5) . ?
N1 C5 1.356(5) . ?
C1 C2 1.380(4) . ?
C1 H1 0.9500 . ?
O2 C8 1.280(3) . ?
N2 C9 1.352(3) . ?
N2 C13 1.358(4) . ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.370(4) . ?
C3 C6 1.505(3) . ?
C4 C5 1.397(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.394(3) . ?
C7 C8 1.404(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.502(3) . ?
C9 C10 1.382(4) . ?
C10 C11 1.395(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.354(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.377(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?

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 89.84(7) 2_655 . ?
O1 Fe1 O1 89.84(7) 2_655 3_665 ?
O1 Fe1 O1 89.84(7) . 3_665 ?
O1 Fe1 O2 96.98(7) 2_655 3_665 ?
O1 Fe1 O2 172.15(7) . 3_665 ?
O1 Fe1 O2 86.33(7) 3_665 3_665 ?
O1 Fe1 O2 86.33(7) 2_655 2_655 ?
O1 Fe1 O2 96.99(7) . 2_655 ?
O1 Fe1 O2 172.15(7) 3_665 2_655 ?
O2 Fe1 O2 87.34(7) 3_665 2_655 ?
O1 Fe1 O2 172.15(7) 2_655 . ?
O1 Fe1 O2 86.33(7) . . ?
O1 Fe1 O2 96.98(7) 3_665 . ?
O2 Fe1 O2 87.34(7) 3_665 . ?
O2 Fe1 O2 87.34(7) 2_655 . ?
C6 O1 Fe1 129.92(15) . . ?
C1 N1 C5 116.2(3) . . ?
N1 C1 C2 123.2(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C8 O2 Fe1 128.94(15) . . ?
C9 N2 C13 116.7(3) . . ?
C1 C2 C3 119.4(3) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 C6 121.8(3) . . ?
C2 C3 C6 118.7(2) . . ?
C3 C4 C5 116.9(3) . . ?
C3 C4 H4 121.5 . . ?
C5 C4 H4 121.5 . . ?
N1 C5 C4 124.7(3) . . ?
N1 C5 H5 117.6 . . ?
C4 C5 H5 117.6 . . ?
O1 C6 C7 124.8(2) . . ?
O1 C6 C3 114.8(2) . . ?
C7 C6 C3 120.4(2) . . ?
C6 C7 C8 122.7(2) . . ?
C6 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
O2 C8 C7 124.9(2) . . ?
O2 C8 C9 115.5(2) . . ?
C7 C8 C9 119.6(2) . . ?
N2 C9 C10 122.5(2) . . ?
N2 C9 C8 118.1(2) . . ?
C10 C9 C8 119.4(2) . . ?
C9 C10 C11 118.6(3) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 118.4(3) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
N2 C13 C12 123.7(3) . . ?
N2 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?

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
C5 N1 C1 C2 -0.6(6) . . . . ?
N1 C1 C2 C3 0.3(5) . . . . ?
C1 C2 C3 C4 0.3(4) . . . . ?
C1 C2 C3 C6 -179.7(3) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C6 C3 C4 C5 179.5(3) . . . . ?
C1 N1 C5 C4 0.4(6) . . . . ?
C3 C4 C5 N1 0.2(5) . . . . ?
Fe1 O1 C6 C7 7.2(4) . . . . ?
Fe1 O1 C6 C3 -173.80(15) . . . . ?
C4 C3 C6 O1 167.5(2) . . . . ?
C2 C3 C6 O1 -12.6(3) . . . . ?
C4 C3 C6 C7 -13.5(4) . . . . ?
C2 C3 C6 C7 166.5(2) . . . . ?
O1 C6 C7 C8 2.9(4) . . . . ?
C3 C6 C7 C8 -176.1(2) . . . . ?
Fe1 O2 C8 C7 -14.5(3) . . . . ?
Fe1 O2 C8 C9 165.83(15) . . . . ?
C6 C7 C8 O2 0.9(4) . . . . ?
C6 C7 C8 C9 -179.4(2) . . . . ?
C13 N2 C9 C10 -0.5(4) . . . . ?
C13 N2 C9 C8 178.6(3) . . . . ?
O2 C8 C9 N2 -177.7(2) . . . . ?
C7 C8 C9 N2 2.6(3) . . . . ?
O2 C8 C9 C10 1.5(3) . . . . ?
C7 C8 C9 C10 -178.3(2) . . . . ?
N2 C9 C10 C11 0.0(4) . . . . ?
C8 C9 C10 C11 -179.1(3) . . . . ?
C9 C10 C11 C12 0.4(5) . . . . ?
C10 C11 C12 C13 -0.4(5) . . . . ?
C9 N2 C13 C12 0.6(5) . . . . ?
C11 C12 C13 N2 -0.2(5) . . . . ?

_refine_diff_density_max         0.420
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.066

####################################################################### 
# 
# 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_CPX2
_database_code_depnum_ccdc_archive 'CCDC 1505682'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H27 Fe N6 O6'
_chemical_formula_sum            'C39 H27 Fe N6 O6'
_chemical_formula_weight         731.51

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-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                   9.0163(6)
_cell_length_b                   22.1308(13)
_cell_length_c                   17.6843(11)
_cell_angle_alpha                90
_cell_angle_beta                 91.643(6)
_cell_angle_gamma                90
_cell_volume                     3527.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2132
_cell_measurement_theta_min      3.4010
_cell_measurement_theta_max      22.6250

_exptl_crystal_description       Block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_F_000             1508
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.484
_shelx_estimated_absorpt_T_min   0.897
_shelx_estimated_absorpt_T_max   0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8275
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.950
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3105
_reflns_number_gt                2177
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0712P)²+3.4741P] 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         3105
_refine_ls_number_parameters     326
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1610
_refine_ls_wR_factor_gt          0.1408
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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 0.5000 0.24041(3) 0.2500 0.0561(3) Uani 1 2 d S T P . .
O1 O 0.3698(2) 0.30574(10) 0.28712(13) 0.0570(6) Uani 1 1 d . . . . .
O2 O 0.3739(3) 0.18148(12) 0.30289(17) 0.0764(8) Uani 1 1 d . . . . .
O3 O 0.6420(3) 0.23227(11) 0.33777(14) 0.0648(7) Uani 1 1 d . . . . .
C1 C 0.3804(3) 0.36316(15) 0.28043(18) 0.0480(8) Uani 1 1 d . . . . .
C2 C 0.2457(11) 0.3960(4) 0.2985(6) 0.051(3) Uani 0.5 1 d G U P A 1
C3 C 0.1222(13) 0.3678(3) 0.3279(7) 0.076(4) Uani 0.5 1 d G U P A 1
H3 H 0.1049 0.3270 0.3185 0.091 Uiso 0.5 1 calc R U P A 1
C4 C 0.0246(11) 0.4006(4) 0.3714(6) 0.123(5) Uani 0.5 1 d G U P A 1
H4 H -0.0580 0.3818 0.3911 0.148 Uiso 0.5 1 calc R U P A 1
C5 C 0.0504(9) 0.4616(4) 0.3855(4) 0.102(3) Uani 0.5 1 d G U P A 1
H5 H -0.0149 0.4835 0.4146 0.122 Uiso 0.5 1 calc R U P A 1
C6 C 0.1739(9) 0.4897(3) 0.3560(5) 0.099(3) Uani 0.5 1 d G U P A 1
H6 H 0.1912 0.5305 0.3654 0.119 Uiso 0.5 1 calc R U P A 1
N1 N 0.2715(9) 0.4569(4) 0.3125(5) 0.106(5) Uani 0.5 1 d G U P A 1
C2A C 0.2636(10) 0.3987(5) 0.3206(7) 0.050(3) Uani 0.5 1 d G U P A 2
C3A C 0.1380(13) 0.3694(3) 0.3459(8) 0.075(4) Uani 0.5 1 d G U P A 2
H3A H 0.1422 0.3286 0.3582 0.090 Uiso 0.5 1 calc R U P A 2
C4A C 0.0061(11) 0.4012(4) 0.3529(7) 0.161(9) Uani 0.5 1 d G U P A 2
H4A H -0.0779 0.3816 0.3699 0.193 Uiso 0.5 1 calc R U P A 2
C5A C -0.0002(9) 0.4622(4) 0.3346(6) 0.111(4) Uani 0.5 1 d G U P A 2
H5A H -0.0884 0.4835 0.3393 0.133 Uiso 0.5 1 calc R U P A 2
C6A C 0.1255(11) 0.4915(4) 0.3093(6) 0.119(4) Uani 0.5 1 d G U P A 2
H6A H 0.1213 0.5323 0.2970 0.143 Uiso 0.5 1 calc R U P A 2
N1A N 0.2573(9) 0.4597(5) 0.3023(6) 0.138(8) Uani 0.5 1 d G U P A 2
C7 C 0.5000 0.3929(2) 0.2500 0.0539(12) Uani 1 2 d S T P A .
H7 H 0.5000 0.4349 0.2500 0.065 Uiso 1 2 calc R U P . .
N2 N 0.2937(8) 0.0637(4) 0.4303(5) 0.076(3) Uani 0.5 1 d G U P B 1
C8 C 0.1852(8) 0.0206(4) 0.4435(4) 0.071(3) Uani 0.5 1 d G U P B 1
H8 H 0.2021 -0.0092 0.4798 0.085 Uiso 0.5 1 calc R U P B 1
C9 C 0.0515(8) 0.0221(3) 0.4024(5) 0.074(3) Uani 0.5 1 d G U P B 1
H9 H -0.0210 -0.0067 0.4112 0.089 Uiso 0.5 1 calc R U P B 1
C10 C 0.0263(8) 0.0666(4) 0.3481(4) 0.081(3) Uani 0.5 1 d G U P B 1
H10 H -0.0631 0.0676 0.3206 0.097 Uiso 0.5 1 calc R U P B 1
C11 C 0.1348(9) 0.1097(3) 0.3349(5) 0.064(3) Uani 0.5 1 d G U P B 1
H11 H 0.1179 0.1395 0.2986 0.077 Uiso 0.5 1 calc R U P B 1
C12 C 0.2685(9) 0.1082(3) 0.3761(5) 0.053(2) Uani 0.5 1 d G U P B 1
N2A N 0.3372(10) 0.0711(5) 0.4479(6) 0.097(3) Uani 0.5 1 d G U P B 2
C8A C 0.2378(12) 0.0269(5) 0.4700(5) 0.119(5) Uani 0.5 1 d G U P B 2
H8A H 0.2551 0.0058 0.5149 0.143 Uiso 0.5 1 calc R U P B 2
C9A C 0.1126(11) 0.0143(5) 0.4251(6) 0.118(5) Uani 0.5 1 d G U P B 2
H9A H 0.0461 -0.0152 0.4399 0.141 Uiso 0.5 1 calc R U P B 2
C10A C 0.0867(9) 0.0459(5) 0.3581(6) 0.101(4) Uani 0.5 1 d G U P B 2
H10A H 0.0028 0.0375 0.3281 0.121 Uiso 0.5 1 calc R U P B 2
C11A C 0.1860(10) 0.0901(4) 0.3360(6) 0.083(3) Uani 0.5 1 d G U P B 2
H11A H 0.1687 0.1113 0.2912 0.099 Uiso 0.5 1 calc R U P B 2
C12A C 0.3113(10) 0.1027(4) 0.3809(7) 0.079(4) Uani 0.5 1 d G U P B 2
C13 C 0.4053(5) 0.14798(17) 0.3597(2) 0.0655(10) Uani 1 1 d . . . . .
C14 C 0.5354(5) 0.15010(17) 0.4025(2) 0.0700(11) Uani 1 1 d . . . . .
H14 H 0.5483 0.1229 0.4422 0.084 Uiso 1 1 calc R U . . .
C15 C 0.6486(4) 0.19137(17) 0.3886(2) 0.0601(9) Uani 1 1 d . . . . .
C16 C 0.7834(7) 0.1886(4) 0.4280(4) 0.063(2) Uani 0.7 1 d G U P C 1
C17 C 0.9113(8) 0.2198(3) 0.4096(3) 0.073(2) Uani 0.7 1 d G U P C 1
H17 H 0.9124 0.2434 0.3662 0.087 Uiso 0.7 1 calc R U P C 1
C18 C 1.0376(7) 0.2156(3) 0.4563(4) 0.090(2) Uani 0.7 1 d G U P C 1
H18 H 1.1232 0.2364 0.4440 0.108 Uiso 0.7 1 calc R U P C 1
C19 C 1.0360(6) 0.1803(3) 0.5213(4) 0.082(2) Uani 0.7 1 d G U P C 1
H19 H 1.1205 0.1775 0.5525 0.099 Uiso 0.7 1 calc R U P C 1
C20 C 0.9081(6) 0.1492(3) 0.5396(4) 0.086(2) Uani 0.7 1 d G U P C 1
H20 H 0.9070 0.1255 0.5831 0.103 Uiso 0.7 1 calc R U P C 1
N3 N 0.7818(5) 0.1533(4) 0.4930(4) 0.078(2) Uani 0.7 1 d G U P C 1
C16A C 0.7953(14) 0.1946(8) 0.4445(9) 0.043(3) Uani 0.3 1 d G U P C 2
C17A C 0.8955(19) 0.2388(6) 0.4234(8) 0.058(4) Uani 0.3 1 d G U P C 2
H17A H 0.8693 0.2663 0.3856 0.069 Uiso 0.3 1 calc R U P C 2
C18A C 1.0350(17) 0.2418(6) 0.4588(11) 0.091(7) Uani 0.3 1 d G U P C 2
H18A H 1.1021 0.2714 0.4447 0.109 Uiso 0.3 1 calc R U P C 2
C19A C 1.0742(14) 0.2006(7) 0.5153(12) 0.100(8) Uani 0.3 1 d G U P C 2
H19A H 1.1676 0.2027 0.5389 0.119 Uiso 0.3 1 calc R U P C 2
C20A C 0.9740(15) 0.1564(7) 0.5363(10) 0.086(7) Uani 0.3 1 d G U P C 2
H20A H 1.0003 0.1289 0.5741 0.103 Uiso 0.3 1 calc R U P C 2
N3A N 0.8345(14) 0.1534(7) 0.5010(10) 0.069(4) Uani 0.3 1 d G U P C 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
Fe1 O2 1.982(3) 2_655 ?
Fe1 O2 1.982(3) . ?
Fe1 O1 1.986(2) . ?
Fe1 O1 1.986(2) 2_655 ?
Fe1 O3 1.992(2) 2_655 ?
Fe1 O3 1.992(2) . ?
O1 C1 1.280(4) . ?
O2 C13 1.273(5) . ?
O3 C15 1.276(4) . ?
C1 C7 1.385(4) . ?
C1 C2 1.458(8) . ?
C1 C2A 1.508(8) . ?
C2 C3 1.3900 . ?
C2 N1 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 N1 1.3900 . ?
C6 H6 0.9300 . ?
C2A C3A 1.3900 . ?
C2A N1A 1.3900 . ?
C3A C4A 1.3900 . ?
C3A H3A 0.9300 . ?
C4A C5A 1.3900 . ?
C4A H4A 0.9300 . ?
C5A C6A 1.3900 . ?
C5A H5A 0.9300 . ?
C6A N1A 1.3900 . ?
C6A H6A 0.9300 . ?
C7 C1 1.385(4) 2_655 ?
C7 H7 0.9300 . ?
N2 C8 1.3900 . ?
N2 C12 1.3900 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 C11 1.3900 . ?
C10 H10 0.9300 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.550(8) . ?
N2A C8A 1.3900 . ?
N2A C12A 1.3900 . ?
C8A C9A 1.3900 . ?
C8A H8A 0.9300 . ?
C9A C10A 1.3900 . ?
C9A H9A 0.9300 . ?
C10A C11A 1.3900 . ?
C10A H10A 0.9300 . ?
C11A C12A 1.3900 . ?
C11A H11A 0.9300 . ?
C12A C13 1.372(8) . ?
C13 C14 1.378(5) . ?
C14 C15 1.397(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.384(6) . ?
C15 C16A 1.629(12) . ?
C16 C17 1.3900 . ?
C16 N3 1.3900 . ?
C17 C18 1.3900 . ?
C17 H17 0.9300 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 N3 1.3900 . ?
C20 H20 0.9300 . ?
C16A C17A 1.3900 . ?
C16A N3A 1.3900 . ?
C17A C18A 1.3900 . ?
C17A H17A 0.9300 . ?
C18A C19A 1.3900 . ?
C18A H18A 0.9300 . ?
C19A C20A 1.3900 . ?
C19A H19A 0.9300 . ?
C20A N3A 1.3900 . ?
C20A H20A 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
O2 Fe1 O2 97.71(17) 2_655 . ?
O2 Fe1 O1 170.92(11) 2_655 . ?
O2 Fe1 O1 88.31(11) . . ?
O2 Fe1 O1 88.31(11) 2_655 2_655 ?
O2 Fe1 O1 170.92(11) . 2_655 ?
O1 Fe1 O1 86.57(13) . 2_655 ?
O2 Fe1 O3 86.40(11) 2_655 2_655 ?
O2 Fe1 O3 86.78(11) . 2_655 ?
O1 Fe1 O3 87.16(10) . 2_655 ?
O1 Fe1 O3 100.44(10) 2_655 2_655 ?
O2 Fe1 O3 86.78(11) 2_655 . ?
O2 Fe1 O3 86.40(11) . . ?
O1 Fe1 O3 100.44(10) . . ?
O1 Fe1 O3 87.16(10) 2_655 . ?
O3 Fe1 O3 169.62(15) 2_655 . ?
C1 O1 Fe1 130.2(2) . . ?
C13 O2 Fe1 129.6(3) . . ?
C15 O3 Fe1 129.0(2) . . ?
O1 C1 C7 124.7(3) . . ?
O1 C1 C2 114.1(5) . . ?
C7 C1 C2 120.7(6) . . ?
O1 C1 C2A 114.7(5) . . ?
C7 C1 C2A 119.8(5) . . ?
C3 C2 N1 120.0 . . ?
C3 C2 C1 122.7(7) . . ?
N1 C2 C1 112.7(7) . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 N1 120.0 . . ?
C5 C6 H6 120.0 . . ?
N1 C6 H6 120.0 . . ?
C6 N1 C2 120.0 . . ?
C3A C2A N1A 120.0 . . ?
C3A C2A C1 119.7(7) . . ?
N1A C2A C1 114.9(7) . . ?
C2A C3A C4A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C4A C3A H3A 120.0 . . ?
C5A C4A C3A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C5A C6A N1A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
N1A C6A H6A 120.0 . . ?
C6A N1A C2A 120.0 . . ?
C1 C7 C1 123.2(4) 2_655 . ?
C1 C7 H7 118.4 2_655 . ?
C1 C7 H7 118.4 . . ?
C8 N2 C12 120.0 . . ?
C9 C8 N2 120.0 . . ?
C9 C8 H8 120.0 . . ?
N2 C8 H8 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 N2 120.0 . . ?
C11 C12 C13 124.9(5) . . ?
N2 C12 C13 114.6(5) . . ?
C8A N2A C12A 120.0 . . ?
N2A C8A C9A 120.0 . . ?
N2A C8A H8A 120.0 . . ?
C9A C8A H8A 120.0 . . ?
C10A C9A C8A 120.0 . . ?
C10A C9A H9A 120.0 . . ?
C8A C9A H9A 120.0 . . ?
C9A C10A C11A 120.0 . . ?
C9A C10A H10A 120.0 . . ?
C11A C10A H10A 120.0 . . ?
C12A C11A C10A 120.0 . . ?
C12A C11A H11A 120.0 . . ?
C10A C11A H11A 120.0 . . ?
C13 C12A C11A 119.2(7) . . ?
C13 C12A N2A 120.7(7) . . ?
C11A C12A N2A 120.0 . . ?
O2 C13 C12A 121.1(6) . . ?
O2 C13 C14 125.4(4) . . ?
C12A C13 C14 113.4(6) . . ?
O2 C13 C12 108.5(5) . . ?
C14 C13 C12 125.9(5) . . ?
C13 C14 C15 122.8(4) . . ?
C13 C14 H14 118.6 . . ?
C15 C14 H14 118.6 . . ?
O3 C15 C16 114.1(4) . . ?
O3 C15 C14 124.6(3) . . ?
C16 C15 C14 121.3(5) . . ?
O3 C15 C16A 114.7(7) . . ?
C14 C15 C16A 120.5(6) . . ?
C15 C16 C17 125.7(5) . . ?
C15 C16 N3 114.2(5) . . ?
C17 C16 N3 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
N3 C20 C19 120.0 . . ?
N3 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 N3 C16 120.0 . . ?
C17A C16A N3A 120.0 . . ?
C17A C16A C15 113.0(9) . . ?
N3A C16A C15 126.3(9) . . ?
C18A C17A C16A 120.0 . . ?
C18A C17A H17A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C19A C18A C17A 120.0 . . ?
C19A C18A H18A 120.0 . . ?
C17A C18A H18A 120.0 . . ?
C20A C19A C18A 120.0 . . ?
C20A C19A H19A 120.0 . . ?
C18A C19A H19A 120.0 . . ?
C19A C20A N3A 120.0 . . ?
C19A C20A H20A 120.0 . . ?
N3A C20A H20A 120.0 . . ?
C20A N3A C16A 120.0 . . ?

_refine_diff_density_max         0.274
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.048

