# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

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

data_1-123K
_database_code_depnum_ccdc_archive 'CCDC 1430791'
_audit_update_record             
;
2016-07-05 deposited with the CCDC.
2016-07-19 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         ?
_chemical_formula_sum            'C34 H36 B2 F8 Fe N14 O3'
_chemical_formula_weight         918.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   9.2819(7)
_cell_length_b                   19.2352(14)
_cell_length_c                   21.4352(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3827.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4449
_cell_measurement_theta_min      2.437
_cell_measurement_theta_max      25.175

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_F_000             1880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.491
_shelx_estimated_absorpt_T_min   0.895
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25172
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.422
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8544
_reflns_number_gt                6582
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_max     0.949
_reflns_Friedel_fraction_full    0.999

_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.1000P)²] 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_abs_structure_details 
;
 Flack x determined using 2289 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8544
_refine_ls_number_parameters     559
_refine_ls_number_restraints     553
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0666
_refine_ls_wR_factor_ref         0.1852
_refine_ls_wR_factor_gt          0.1676
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.144
_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 0.78527(9) 0.49946(4) 0.72965(3) 0.0128(2) Uani 1 1 d . U . . .
C1 C 0.7121(7) 0.6140(3) 0.6306(3) 0.0187(12) Uani 1 1 d . U . . .
H1 H 0.6096 0.6124 0.6301 0.023 Uiso 1 1 d . U . . .
C2 C 0.9358(7) 0.6442(3) 0.6080(3) 0.0208(13) Uani 1 1 d . U . . .
H2 H 1.0171 0.6663 0.5900 0.024 Uiso 1 1 d . U . . .
C3 C 0.9360(7) 0.5932(3) 0.6522(3) 0.0171(12) Uani 1 1 d . U . . .
C4 C 1.0455(7) 0.5554(3) 0.6841(3) 0.0158(12) Uani 1 1 d . U . . .
H4 H 1.1464 0.5617 0.6765 0.019 Uiso 1 1 d . U . . .
C5 C 1.1712(7) 0.4207(3) 0.7195(3) 0.0183(12) Uani 1 1 d . U . . .
C6 C 1.2467(7) 0.3660(3) 0.7540(3) 0.0181(13) Uani 1 1 d . U . . .
C7 C 1.3175(8) 0.3137(3) 0.7221(3) 0.0262(14) Uani 1 1 d . U . . .
H7 H 1.3106 0.3115 0.6782 0.033 Uiso 1 1 d . U . . .
C8 C 1.3981(8) 0.2652(4) 0.7530(3) 0.0279(15) Uani 1 1 d . U . . .
H8 H 1.4434 0.2281 0.7310 0.033 Uiso 1 1 d . U . . .
C9 C 1.4133(7) 0.2710(4) 0.8181(3) 0.0263(15) Uani 1 1 d . U . . .
H9 H 1.4727 0.2389 0.8401 0.032 Uiso 1 1 d . U . . .
C10 C 1.3434(7) 0.3225(4) 0.8507(3) 0.0224(14) Uani 1 1 d . U . . .
H10 H 1.3531 0.3252 0.8947 0.027 Uiso 1 1 d . U . . .
C11 C 1.2569(7) 0.3708(3) 0.8200(3) 0.0195(13) Uani 1 1 d . U . . .
C12 C 1.0628(7) 0.4540(3) 0.8205(3) 0.0180(13) Uani 1 1 d . U . . .
H12 H 1.0427 0.4991 0.8421 0.022 Uiso 1 1 d . U . . .
C13 C 0.9315(7) 0.4104(3) 0.8261(3) 0.0185(13) Uani 1 1 d . U . . .
C14 C 0.9058(7) 0.3562(4) 0.8653(3) 0.0231(14) Uani 1 1 d . U . . .
H14 H 0.9719 0.3364 0.8943 0.028 Uiso 1 1 d . U . . .
C15 C 0.7114(7) 0.3767(3) 0.8100(3) 0.0201(12) Uani 1 1 d . U . . .
H15 H 0.6171 0.3725 0.7937 0.024 Uiso 1 1 d . U . . .
C16 C 0.8532(7) 0.6187(3) 0.8149(3) 0.0200(13) Uani 1 1 d . U . . .
H16 H 0.9463 0.6258 0.7978 0.025 Uiso 1 1 d . U . . .
C17 C 0.6562(8) 0.6331(3) 0.8724(3) 0.0220(14) Uani 1 1 d . U . . .
H17 H 0.5893 0.6504 0.9020 0.027 Uiso 1 1 d . U . . .
C18 C 0.6386(7) 0.5789(3) 0.8323(3) 0.0182(12) Uani 1 1 d . U . . .
C19 C 0.5068(7) 0.5333(3) 0.8241(3) 0.0173(13) Uani 1 1 d . U . . .
H19 H 0.5286 0.4860 0.8409 0.020 Uiso 1 1 d . U . . .
C20 C 0.3103(7) 0.6149(4) 0.8318(3) 0.0234(14) Uani 1 1 d . U . . .
C21 C 0.2243(8) 0.6595(4) 0.8687(3) 0.0326(16) Uani 1 1 d . U . . .
H21 H 0.2163 0.6517 0.9123 0.039 Uiso 1 1 d . U . . .
C22 C 0.1560(8) 0.7132(4) 0.8415(4) 0.0367(17) Uani 1 1 d . U . . .
H22 H 0.0979 0.7425 0.8667 0.049 Uiso 1 1 d . U . . .
C23 C 0.1661(7) 0.7278(4) 0.7769(4) 0.0347(17) Uani 1 1 d . U . . .
H23 H 0.1194 0.7668 0.7582 0.041 Uiso 1 1 d . U . . .
C24 C 0.2471(7) 0.6831(3) 0.7406(3) 0.0266(15) Uani 1 1 d . U . . .
H24 H 0.2529 0.6900 0.6971 0.031 Uiso 1 1 d . U . . .
C25 C 0.3197(7) 0.6274(3) 0.7678(3) 0.0218(13) Uani 1 1 d . U . . .
C26 C 0.3987(6) 0.5793(3) 0.7264(3) 0.0189(12) Uani 1 1 d . U . . .
C27 C 0.5268(7) 0.4508(3) 0.6779(3) 0.0178(13) Uani 1 1 d . U . . .
H27 H 0.4274 0.4459 0.6691 0.022 Uiso 1 1 d . U . . .
C28 C 0.6375(8) 0.3730(4) 0.5915(3) 0.0238(14) Uani 1 1 d . U . . .
H28 H 0.5567 0.3545 0.5700 0.029 Uiso 1 1 d . U . . .
C29 C 0.8611(7) 0.3972(3) 0.6198(3) 0.0189(13) Uani 1 1 d . U . . .
H29 H 0.9632 0.3974 0.6201 0.022 Uiso 1 1 d . U . . .
C30 C 0.6366(7) 0.4162(3) 0.6419(3) 0.0192(13) Uani 1 1 d . U . . .
O1 O 0.3951(5) 0.5823(2) 0.66908(19) 0.0210(10) Uani 1 1 d . U . . .
N1 N 0.8060(6) 0.4230(3) 0.7921(2) 0.0164(11) Uani 1 1 d . U . . .
F1 F 0.7006(6) 0.2091(3) 0.9235(2) 0.0471(12) Uani 1 1 d . U . . .
B1 B 0.6051(10) 0.2215(5) 0.9722(4) 0.036(2) Uani 1 1 d . U . . .
O2 O 1.1786(5) 0.4264(3) 0.66227(19) 0.0241(11) Uani 1 1 d . U . . .
N2 N 0.7670(7) 0.3352(3) 0.8548(3) 0.0258(13) Uani 1 1 d . U . . .
H2A H 0.7224 0.3012 0.8739 0.031 Uiso 1 1 d . U . . .
F2 F 0.5789(7) 0.2953(3) 0.9707(3) 0.0637(16) Uani 1 1 d . U . . .
B2 B 0.6594(10) 0.1998(5) 0.4695(4) 0.0315(18) Uani 1 1 d . U . . .
N3 N 1.1863(6) 0.4229(3) 0.8500(2) 0.0205(11) Uani 1 1 d . U . . .
H3 H 1.2164 0.4375 0.8869 0.024 Uiso 1 1 d . U . . .
F3 F 0.6572(6) 0.2071(3) 1.0285(2) 0.0561(15) Uani 1 1 d . U . . .
N4 N 1.0987(6) 0.4694(3) 0.7552(2) 0.0151(10) Uani 1 1 d . U . . .
F4 F 0.4761(5) 0.1879(3) 0.9610(2) 0.0516(14) Uani 1 1 d . U . . .
N5 N 0.9953(5) 0.5118(3) 0.7248(2) 0.0167(11) Uani 1 1 d . U . . .
F5 F 0.6979(7) 0.2610(3) 0.4954(3) 0.0651(16) Uani 1 1 d . U . . .
N6 N 0.7952(6) 0.5747(3) 0.6665(2) 0.0149(10) Uani 1 1 d . U . . .
F6 F 0.5498(7) 0.1674(4) 0.5005(2) 0.076(2) Uani 1 1 d . U . . .
N7 N 0.7938(6) 0.6566(3) 0.5954(2) 0.0224(12) Uani 1 1 d . U . . .
H7A H 0.7617 0.6874 0.5682 0.027 Uiso 1 1 d . U . . .
F7 F 0.6147(5) 0.2124(2) 0.40835(19) 0.0330(10) Uani 1 1 d . U . . .
N8 N 0.7784(7) 0.3618(3) 0.5787(2) 0.0223(12) Uani 1 1 d . U . . .
H8A H 0.8121 0.3358 0.5480 0.027 Uiso 1 1 d . U . . .
F8 F 0.7817(7) 0.1596(4) 0.4673(3) 0.0737(18) Uani 1 1 d . U . . .
N9 N 0.7769(6) 0.4321(3) 0.6598(2) 0.0163(10) Uani 1 1 d . U . . .
N10 N 0.5747(5) 0.4880(2) 0.7226(2) 0.0146(10) Uani 1 1 d . U . . .
N11 N 0.4700(6) 0.5262(3) 0.7572(2) 0.0161(11) Uani 1 1 d . U . . .
N12 N 0.3844(6) 0.5600(3) 0.8567(2) 0.0239(12) Uani 1 1 d . U . . .
H12A H 0.3568 0.5414 0.8922 0.029 Uiso 1 1 d . U . . .
N13 N 0.7932(7) 0.6579(3) 0.8605(2) 0.0222(12) Uani 1 1 d . U . . .
H13 H 0.8347 0.6928 0.8796 0.026 Uiso 1 1 d . U . . .
N14 N 0.7616(6) 0.5694(3) 0.7969(2) 0.0159(11) Uani 1 1 d . U . . .
O3 O 1.2489(16) 0.5110(7) 0.4754(5) 0.146(5) Uani 1 1 d . U . . .
C31 C 0.983(2) 0.5375(8) 0.4687(7) 0.150(7) Uani 1 1 d D U . . .
H31A H 0.9000 0.5519 0.4940 0.225 Uiso 1 1 calc R U . . .
H31B H 0.9993 0.5716 0.4355 0.225 Uiso 1 1 calc R U . . .
H31C H 0.9632 0.4919 0.4501 0.225 Uiso 1 1 calc R U . . .
C33 C 1.362(3) 0.5014(10) 0.5181(9) 0.145(6) Uani 1 1 d . U . . .
H33A H 1.3513 0.4616 0.5446 0.142 Uiso 1 1 d . U . . .
H33B H 1.3930 0.5431 0.5389 0.142 Uiso 1 1 d . U . . .
C34 C 1.481(3) 0.4813(11) 0.4653(9) 0.158(7) Uani 1 1 d . U . . .
H34A H 1.5726 0.4739 0.4873 0.208 Uiso 1 1 d . U . . .
H34B H 1.4908 0.5221 0.4378 0.208 Uiso 1 1 d . U . . .
H34C H 1.4499 0.4415 0.4436 0.208 Uiso 1 1 d . U . . .
C32 C 1.127(3) 0.5324(12) 0.5133(8) 0.172(8) Uani 1 1 d D U . . .
H32A H 1.1536 0.5788 0.5329 0.189 Uiso 1 1 d . U . . .
H32B H 1.1184 0.4989 0.5486 0.189 Uiso 1 1 d . 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 N5 1.967(5) . ?
Fe1 N10 1.972(5) . ?
Fe1 N9 1.981(5) . ?
Fe1 N6 1.983(5) . ?
Fe1 N14 1.983(5) . ?
Fe1 N1 1.998(5) . ?
C1 N6 1.327(8) . ?
C1 N7 1.348(8) . ?
C1 H1 0.952(7) . ?
C2 C3 1.364(9) . ?
C2 N7 1.366(9) . ?
C2 H2 0.948(7) . ?
C3 N6 1.389(9) . ?
C3 C4 1.425(9) . ?
C4 N5 1.296(8) . ?
C4 H4 0.958(6) . ?
C5 O2 1.234(7) . ?
C5 N4 1.384(8) . ?
C5 C6 1.464(8) . ?
C6 C7 1.382(9) . ?
C6 C11 1.421(8) . ?
C7 C8 1.368(10) . ?
C7 H7 0.944(7) . ?
C8 C9 1.407(10) . ?
C8 H8 0.953(7) . ?
C9 C10 1.374(10) . ?
C9 H9 0.953(7) . ?
C10 C11 1.392(9) . ?
C10 H10 0.950(7) . ?
C11 N3 1.359(9) . ?
C12 N3 1.439(8) . ?
C12 N4 1.470(8) . ?
C12 C13 1.485(9) . ?
C12 H12 1.001(6) . ?
C13 C14 1.359(9) . ?
C13 N1 1.395(8) . ?
C14 N2 1.369(9) . ?
C14 H14 0.953(6) . ?
C15 N1 1.308(8) . ?
C15 N2 1.349(8) . ?
C15 H15 0.946(7) . ?
C16 N14 1.331(8) . ?
C16 N13 1.353(8) . ?
C16 H16 0.949(7) . ?
C17 C18 1.362(9) . ?
C17 N13 1.382(9) . ?
C17 H17 0.948(7) . ?
C18 N14 1.384(8) . ?
C18 C19 1.515(9) . ?
C19 N12 1.429(8) . ?
C19 N11 1.479(7) . ?
C19 H19 1.000(7) . ?
C20 N12 1.368(9) . ?
C20 C25 1.397(10) . ?
C20 C21 1.414(10) . ?
C21 C22 1.345(12) . ?
C21 H21 0.949(8) . ?
C22 C23 1.416(13) . ?
C22 H22 0.949(7) . ?
C23 C24 1.381(10) . ?
C23 H23 0.955(8) . ?
C24 C25 1.393(10) . ?
C24 H24 0.944(7) . ?
C25 C26 1.476(9) . ?
C26 O1 1.231(8) . ?
C26 N11 1.384(8) . ?
C27 N10 1.276(8) . ?
C27 C30 1.441(9) . ?
C27 H27 0.946(6) . ?
C28 N8 1.354(9) . ?
C28 C30 1.363(9) . ?
C28 H28 0.949(7) . ?
C29 N9 1.341(8) . ?
C29 N8 1.351(8) . ?
C29 H29 0.948(7) . ?
C30 N9 1.392(9) . ?
F1 B1 1.391(10) . ?
B1 F3 1.330(10) . ?
B1 F4 1.381(10) . ?
B1 F2 1.441(12) . ?
N2 H2A 0.877(5) . ?
B2 F5 1.351(10) . ?
B2 F6 1.366(10) . ?
B2 F8 1.374(11) . ?
B2 F7 1.396(9) . ?
N3 H3 0.884(5) . ?
N4 N5 1.418(7) . ?
N7 H7A 0.883(5) . ?
N8 H8A 0.884(5) . ?
N10 N11 1.428(7) . ?
N12 H12A 0.879(5) . ?
N13 H13 0.876(5) . ?
O3 C33 1.40(2) . ?
O3 C32 1.45(2) . ?
C31 C32 1.65(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C33 C34 1.63(3) . ?
C33 H33A 0.959(19) . ?
C33 H33B 0.963(17) . ?
C34 H34A 0.98(2) . ?
C34 H34B 0.986(17) . ?
C34 H34C 0.94(2) . ?
C32 H32A 1.02(2) . ?
C32 H32B 1.00(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Fe1 N10 172.5(2) . . ?
N5 Fe1 N9 94.4(2) . . ?
N10 Fe1 N9 80.2(2) . . ?
N5 Fe1 N6 80.2(2) . . ?
N10 Fe1 N6 94.3(2) . . ?
N9 Fe1 N6 87.9(2) . . ?
N5 Fe1 N14 93.8(2) . . ?
N10 Fe1 N14 91.3(2) . . ?
N9 Fe1 N14 171.2(2) . . ?
N6 Fe1 N14 90.4(2) . . ?
N5 Fe1 N1 91.7(2) . . ?
N10 Fe1 N1 93.7(2) . . ?
N9 Fe1 N1 91.6(2) . . ?
N6 Fe1 N1 171.8(3) . . ?
N14 Fe1 N1 91.3(2) . . ?
N6 C1 N7 110.1(6) . . ?
N6 C1 H1 124.7(6) . . ?
N7 C1 H1 125.2(6) . . ?
C3 C2 N7 105.3(6) . . ?
C3 C2 H2 127.2(7) . . ?
N7 C2 H2 127.5(6) . . ?
C2 C3 N6 109.7(6) . . ?
C2 C3 C4 134.5(6) . . ?
N6 C3 C4 115.7(5) . . ?
N5 C4 C3 113.4(6) . . ?
N5 C4 H4 123.2(6) . . ?
C3 C4 H4 123.4(6) . . ?
O2 C5 N4 121.1(6) . . ?
O2 C5 C6 122.6(6) . . ?
N4 C5 C6 116.1(5) . . ?
C7 C6 C11 120.5(6) . . ?
C7 C6 C5 120.1(6) . . ?
C11 C6 C5 119.2(6) . . ?
C8 C7 C6 121.2(6) . . ?
C8 C7 H7 119.3(7) . . ?
C6 C7 H7 119.6(6) . . ?
C7 C8 C9 118.7(7) . . ?
C7 C8 H8 120.8(7) . . ?
C9 C8 H8 120.5(7) . . ?
C10 C9 C8 120.9(6) . . ?
C10 C9 H9 119.3(7) . . ?
C8 C9 H9 119.8(7) . . ?
C9 C10 C11 120.9(6) . . ?
C9 C10 H10 119.9(7) . . ?
C11 C10 H10 119.2(7) . . ?
N3 C11 C10 123.1(6) . . ?
N3 C11 C6 119.1(6) . . ?
C10 C11 C6 117.7(6) . . ?
N3 C12 N4 108.8(5) . . ?
N3 C12 C13 112.6(5) . . ?
N4 C12 C13 112.1(5) . . ?
N3 C12 H12 107.9(5) . . ?
N4 C12 H12 107.9(5) . . ?
C13 C12 H12 107.4(6) . . ?
C14 C13 N1 108.1(6) . . ?
C14 C13 C12 128.8(6) . . ?
N1 C13 C12 123.0(5) . . ?
C13 C14 N2 106.8(6) . . ?
C13 C14 H14 126.7(7) . . ?
N2 C14 H14 126.5(7) . . ?
N1 C15 N2 110.8(6) . . ?
N1 C15 H15 124.8(6) . . ?
N2 C15 H15 124.4(6) . . ?
N14 C16 N13 110.1(6) . . ?
N14 C16 H16 124.9(6) . . ?
N13 C16 H16 125.0(6) . . ?
C18 C17 N13 104.9(6) . . ?
C18 C17 H17 127.8(7) . . ?
N13 C17 H17 127.3(7) . . ?
C17 C18 N14 110.4(6) . . ?
C17 C18 C19 127.9(6) . . ?
N14 C18 C19 121.7(5) . . ?
N12 C19 N11 108.8(5) . . ?
N12 C19 C18 112.2(5) . . ?
N11 C19 C18 110.7(5) . . ?
N12 C19 H19 108.1(5) . . ?
N11 C19 H19 108.2(6) . . ?
C18 C19 H19 108.7(5) . . ?
N12 C20 C25 119.0(6) . . ?
N12 C20 C21 122.3(6) . . ?
C25 C20 C21 118.7(7) . . ?
C22 C21 C20 119.3(7) . . ?
C22 C21 H21 120.7(8) . . ?
C20 C21 H21 120.0(8) . . ?
C21 C22 C23 123.1(7) . . ?
C21 C22 H22 118.5(9) . . ?
C23 C22 H22 118.5(9) . . ?
C24 C23 C22 117.6(7) . . ?
C24 C23 H23 120.0(9) . . ?
C22 C23 H23 122.4(8) . . ?
C23 C24 C25 120.4(7) . . ?
C23 C24 H24 120.0(7) . . ?
C25 C24 H24 119.5(7) . . ?
C24 C25 C20 120.9(6) . . ?
C24 C25 C26 118.2(6) . . ?
C20 C25 C26 120.8(6) . . ?
O1 C26 N11 121.6(6) . . ?
O1 C26 C25 123.8(6) . . ?
N11 C26 C25 114.4(6) . . ?
N10 C27 C30 114.5(6) . . ?
N10 C27 H27 123.0(6) . . ?
C30 C27 H27 122.5(6) . . ?
N8 C28 C30 105.2(6) . . ?
N8 C28 H28 127.3(7) . . ?
C30 C28 H28 127.5(7) . . ?
N9 C29 N8 109.8(6) . . ?
N9 C29 H29 125.1(6) . . ?
N8 C29 H29 125.1(6) . . ?
C28 C30 N9 110.3(6) . . ?
C28 C30 C27 135.2(6) . . ?
N9 C30 C27 114.4(5) . . ?
C15 N1 C13 106.8(5) . . ?
C15 N1 Fe1 129.3(5) . . ?
C13 N1 Fe1 123.9(4) . . ?
F3 B1 F4 112.1(7) . . ?
F3 B1 F1 114.5(8) . . ?
F4 B1 F1 109.9(7) . . ?
F3 B1 F2 106.7(7) . . ?
F4 B1 F2 108.0(8) . . ?
F1 B1 F2 105.0(7) . . ?
C15 N2 C14 107.6(5) . . ?
C15 N2 H2A 126.4(7) . . ?
C14 N2 H2A 126.0(6) . . ?
F5 B2 F6 113.2(8) . . ?
F5 B2 F8 106.6(7) . . ?
F6 B2 F8 112.1(8) . . ?
F5 B2 F7 108.2(6) . . ?
F6 B2 F7 108.4(7) . . ?
F8 B2 F7 108.2(7) . . ?
C11 N3 C12 118.8(5) . . ?
C11 N3 H3 120.4(6) . . ?
C12 N3 H3 120.8(6) . . ?
C5 N4 N5 117.6(5) . . ?
C5 N4 C12 120.0(5) . . ?
N5 N4 C12 113.6(5) . . ?
C4 N5 N4 116.0(5) . . ?
C4 N5 Fe1 118.0(4) . . ?
N4 N5 Fe1 125.3(4) . . ?
C1 N6 C3 105.8(5) . . ?
C1 N6 Fe1 141.7(5) . . ?
C3 N6 Fe1 112.4(4) . . ?
C1 N7 C2 109.0(5) . . ?
C1 N7 H7A 126.0(7) . . ?
C2 N7 H7A 125.0(6) . . ?
C29 N8 C28 109.7(5) . . ?
C29 N8 H8A 124.7(6) . . ?
C28 N8 H8A 125.6(6) . . ?
C29 N9 C30 105.0(5) . . ?
C29 N9 Fe1 142.0(5) . . ?
C30 N9 Fe1 112.9(4) . . ?
C27 N10 N11 116.2(5) . . ?
C27 N10 Fe1 117.8(4) . . ?
N11 N10 Fe1 125.2(4) . . ?
C26 N11 N10 117.3(5) . . ?
C26 N11 C19 120.3(5) . . ?
N10 N11 C19 113.2(5) . . ?
C20 N12 C19 119.1(5) . . ?
C20 N12 H12A 120.3(6) . . ?
C19 N12 H12A 120.6(6) . . ?
C16 N13 C17 108.7(5) . . ?
C16 N13 H13 125.7(7) . . ?
C17 N13 H13 125.6(6) . . ?
C16 N14 C18 105.9(5) . . ?
C16 N14 Fe1 128.6(4) . . ?
C18 N14 Fe1 125.4(4) . . ?
C33 O3 C32 104.7(14) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O3 C33 C34 95.0(14) . . ?
O3 C33 H33A 114.7(19) . . ?
C34 C33 H33A 107(2) . . ?
O3 C33 H33B 115(2) . . ?
C34 C33 H33B 108(2) . . ?
H33A C33 H33B 114.8(18) . . ?
C33 C34 H34A 106.9(17) . . ?
C33 C34 H34B 107(2) . . ?
H34A C34 H34B 109(2) . . ?
C33 C34 H34C 109(2) . . ?
H34A C34 H34C 113(2) . . ?
H34B C34 H34C 112.3(19) . . ?
O3 C32 C31 109.0(13) . . ?
O3 C32 H32A 107(2) . . ?
C31 C32 H32A 112.7(19) . . ?
O3 C32 H32B 108(2) . . ?
C31 C32 H32B 114(2) . . ?
H32A C32 H32B 105.9(16) . . ?

_refine_diff_density_max         1.012
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.294

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

data_1-298K
_database_code_depnum_ccdc_archive 'CCDC 1430792'
_audit_update_record             
;
2016-07-05 deposited with the CCDC.
2016-07-19 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         ?
_chemical_formula_sum            'C34 H36 B2 F8 Fe N14 O3'
_chemical_formula_weight         918.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

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

_cell_length_a                   19.426(6)
_cell_length_b                   9.389(3)
_cell_length_c                   10.942(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1995.7(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3518
_cell_measurement_theta_min      2.410
_cell_measurement_theta_max      24.497

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_F_000             940
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.471
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12427
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.861
_diffrn_reflns_theta_max         27.597
_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 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4567
_reflns_number_gt                3553
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_max     0.977
_reflns_Friedel_fraction_full    0.997

_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.1750P)²] 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_abs_structure_details 
;
 Flack x determined using 1230 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4567
_refine_ls_number_parameters     294
_refine_ls_number_restraints     322
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_ref         0.2389
_refine_ls_wR_factor_gt          0.2182
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.077
_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 0.5000 0.52893(10) 0.0366(4) Uani 1 2 d S TU P . .
C1 C 0.6111(4) 0.4423(8) 0.7400(6) 0.0501(15) Uani 1 1 d . U . . .
H1 H 0.6117 0.3433 0.7430 0.060 Uiso 1 1 calc R U . . .
C2 C 0.6347(4) 0.6645(10) 0.7869(7) 0.0603(18) Uani 1 1 d . U . . .
H2 H 0.6527 0.7450 0.8247 0.072 Uiso 1 1 calc R U . . .
C3 C 0.5873(3) 0.6601(7) 0.6927(6) 0.0432(13) Uani 1 1 d . U . . .
C4 C 0.5496(3) 0.7659(7) 0.6288(6) 0.0444(13) Uani 1 1 d . U . . .
H4 H 0.5526 0.8622 0.6480 0.053 Uiso 1 1 calc R U . . .
C5 C 0.4168(3) 0.8834(6) 0.5517(5) 0.0422(12) Uani 1 1 d . U . . .
C6 C 0.3646(3) 0.9620(6) 0.4801(7) 0.0454(13) Uani 1 1 d . U . . .
C7 C 0.3120(4) 1.0302(7) 0.5420(8) 0.0576(17) Uani 1 1 d . U . . .
H7 H 0.3068 1.0182 0.6258 0.069 Uiso 1 1 calc R U . . .
C8 C 0.2671(4) 1.1172(9) 0.4767(10) 0.071(2) Uani 1 1 d . U . . .
H8 H 0.2310 1.1618 0.5172 0.085 Uiso 1 1 calc R U . . .
C9 C 0.2752(4) 1.1377(9) 0.3560(9) 0.068(2) Uani 1 1 d . U . . .
H9 H 0.2454 1.1989 0.3153 0.081 Uiso 1 1 calc R U . . .
C10 C 0.3270(4) 1.0696(9) 0.2904(8) 0.0634(19) Uani 1 1 d . U . . .
H10 H 0.3315 1.0828 0.2066 0.076 Uiso 1 1 calc R U . . .
C11 C 0.3723(3) 0.9806(8) 0.3549(6) 0.0501(15) Uani 1 1 d . U . . .
C12 C 0.4566(4) 0.7891(8) 0.3521(6) 0.0490(15) Uani 1 1 d . U . . .
H12 H 0.5015 0.7720 0.3140 0.059 Uiso 1 1 calc R U . . .
C13 C 0.4133(4) 0.6559(8) 0.3350(6) 0.0484(14) Uani 1 1 d . U . . .
C14 C 0.3606(4) 0.6359(11) 0.2545(8) 0.067(2) Uani 1 1 d . U . . .
H14 H 0.3422 0.7022 0.2004 0.081 Uiso 1 1 calc R U . . .
C15 C 0.3810(4) 0.4385(10) 0.3577(8) 0.066(2) Uani 1 1 d . U . . .
H15 H 0.3770 0.3452 0.3852 0.079 Uiso 1 1 calc R U . . .
N1 N 0.5736(2) 0.5184(6) 0.6659(4) 0.0396(11) Uani 1 1 d . U . . .
N2 N 0.6492(3) 0.5289(8) 0.8119(5) 0.0583(16) Uani 1 1 d . U . . .
H2A H 0.6784 0.5007 0.8657 0.070 Uiso 1 1 calc R U . . .
N3 N 0.5106(3) 0.7182(5) 0.5413(4) 0.0417(11) Uani 1 1 d . U . . .
N4 N 0.4683(3) 0.8193(6) 0.4823(5) 0.0423(11) Uani 1 1 d . U . . .
N5 N 0.4271(3) 0.9132(7) 0.2959(6) 0.0587(15) Uani 1 1 d . U . . .
H5 H 0.4176 0.8973 0.2203 0.070 Uiso 1 1 d R U . . .
N6 N 0.3406(3) 0.4985(11) 0.2700(6) 0.0739(17) Uani 1 1 d . U . . .
N7 N 0.4260(3) 0.5306(6) 0.3976(5) 0.0489(14) Uani 1 1 d . U . . .
O1 O 0.4182(3) 0.8816(6) 0.6628(4) 0.0566(12) Uani 1 1 d . U . . .
F3 F 0.7819(8) 0.6133(13) 0.9372(7) 0.136(3) Uani 0.75 1 d D U P A 1
F0AA F 0.789(3) 0.636(6) 1.168(2) 0.145(5) Uani 0.25 1 d D U P A 2
B1 B 0.7829(7) 0.6520(13) 1.0480(7) 0.105(3) Uani 1 1 d D U . . .
F1 F 0.8156(10) 0.7763(14) 1.0688(11) 0.152(4) Uani 0.75 1 d D U P A 1
F1AA F 0.7097(7) 0.666(2) 1.0517(13) 0.167(5) Uani 0.75 1 d D U P A 1
O2 O 0.5000 1.0000 1.0512(17) 0.298(18) Uani 1 2 d DS TU P . .
C17 C 0.5125(18) 0.8781(16) 0.9699(15) 0.318(18) Uani 1 1 d D U . . .
H17A H 0.5506 0.8977 0.9152 0.382 Uiso 1 1 calc R U . . .
H17B H 0.4719 0.8575 0.9214 0.382 Uiso 1 1 calc R U . . .
C16 C 0.5299(15) 0.750(4) 1.056(2) 0.32(2) Uani 1 1 d D U . . .
H16A H 0.5675 0.7754 1.1090 0.486 Uiso 1 1 calc R U . . .
H16B H 0.5426 0.6685 1.0082 0.486 Uiso 1 1 calc R U . . .
H16C H 0.4903 0.7269 1.1052 0.486 Uiso 1 1 calc R U . . .
F2 F 0.7873(9) 0.5647(16) 1.1422(9) 0.145(5) Uani 0.75 1 d D U P A 1
F4 F 0.8453(13) 0.615(4) 0.997(2) 0.136(3) Uani 0.25 1 d D U P A 2
F6 F 0.789(3) 0.795(3) 1.026(4) 0.152(4) Uani 0.25 1 d D U P A 2
F7 F 0.734(2) 0.568(6) 1.002(4) 0.167(5) Uani 0.25 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 2.052(6) . ?
Fe1 N7 2.052(6) 2_665 ?
Fe1 N3 2.064(5) . ?
Fe1 N3 2.064(5) 2_665 ?
Fe1 N1 2.078(5) . ?
Fe1 N1 2.078(5) 2_665 ?
C1 N1 1.304(8) . ?
C1 N2 1.351(10) . ?
C1 H1 0.9300 . ?
C2 N2 1.332(12) . ?
C2 C3 1.382(10) . ?
C2 H2 0.9300 . ?
C3 N1 1.389(9) . ?
C3 C4 1.419(10) . ?
C4 N3 1.301(8) . ?
C4 H4 0.9300 . ?
C5 O1 1.216(8) . ?
C5 N4 1.393(8) . ?
C5 C6 1.479(9) . ?
C6 C7 1.383(11) . ?
C6 C11 1.389(10) . ?
C7 C8 1.393(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.343(13) . ?
C8 H8 0.9300 . ?
C9 C10 1.392(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.403(10) . ?
C10 H10 0.9300 . ?
C11 N5 1.396(10) . ?
C12 N5 1.438(10) . ?
C12 N4 1.470(8) . ?
C12 C13 1.518(10) . ?
C12 H12 0.9800 . ?
C13 C14 1.364(10) . ?
C13 N7 1.385(10) . ?
C14 N6 1.358(14) . ?
C14 H14 0.9300 . ?
C15 N7 1.306(9) . ?
C15 N6 1.361(12) . ?
C15 H15 0.9300 . ?
N2 H2A 0.8600 . ?
N3 N4 1.411(7) . ?
N5 H5 0.8600 . ?
F3 B1 1.266(11) . ?
F0AA B1 1.332(19) . ?
B1 F2 1.321(13) . ?
B1 F7 1.33(2) . ?
B1 F1 1.348(13) . ?
B1 F6 1.37(2) . ?
B1 F4 1.38(2) . ?
B1 F1AA 1.427(16) . ?
O2 C17 1.469(15) . ?
O2 C17 1.469(15) 2_675 ?
C17 C16 1.57(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Fe1 N7 91.1(3) . 2_665 ?
N7 Fe1 N3 88.7(2) . . ?
N7 Fe1 N3 96.6(2) 2_665 . ?
N7 Fe1 N3 96.6(2) . 2_665 ?
N7 Fe1 N3 88.7(2) 2_665 2_665 ?
N3 Fe1 N3 172.5(3) . 2_665 ?
N7 Fe1 N1 167.1(2) . . ?
N7 Fe1 N1 92.0(2) 2_665 . ?
N3 Fe1 N1 78.6(2) . . ?
N3 Fe1 N1 95.9(2) 2_665 . ?
N7 Fe1 N1 92.0(2) . 2_665 ?
N7 Fe1 N1 167.1(2) 2_665 2_665 ?
N3 Fe1 N1 95.9(2) . 2_665 ?
N3 Fe1 N1 78.6(2) 2_665 2_665 ?
N1 Fe1 N1 87.7(3) . 2_665 ?
N1 C1 N2 109.8(7) . . ?
N1 C1 H1 125.1 . . ?
N2 C1 H1 125.1 . . ?
N2 C2 C3 105.3(7) . . ?
N2 C2 H2 127.3 . . ?
C3 C2 H2 127.3 . . ?
C2 C3 N1 108.3(6) . . ?
C2 C3 C4 133.7(7) . . ?
N1 C3 C4 117.9(5) . . ?
N3 C4 C3 115.0(6) . . ?
N3 C4 H4 122.5 . . ?
C3 C4 H4 122.5 . . ?
O1 C5 N4 121.6(6) . . ?
O1 C5 C6 123.5(6) . . ?
N4 C5 C6 114.8(5) . . ?
C7 C6 C11 120.2(7) . . ?
C7 C6 C5 118.5(7) . . ?
C11 C6 C5 120.8(6) . . ?
C6 C7 C8 118.9(8) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 121.0(9) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 121.7(8) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C9 C10 C11 117.9(7) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C6 C11 N5 118.7(6) . . ?
C6 C11 C10 120.3(7) . . ?
N5 C11 C10 121.0(6) . . ?
N5 C12 N4 108.7(6) . . ?
N5 C12 C13 113.2(6) . . ?
N4 C12 C13 111.4(5) . . ?
N5 C12 H12 107.8 . . ?
N4 C12 H12 107.8 . . ?
C13 C12 H12 107.8 . . ?
C14 C13 N7 109.7(7) . . ?
C14 C13 C12 127.6(8) . . ?
N7 C13 C12 122.6(6) . . ?
N6 C14 C13 105.4(8) . . ?
N6 C14 H14 127.3 . . ?
C13 C14 H14 127.3 . . ?
N7 C15 N6 110.4(9) . . ?
N7 C15 H15 124.8 . . ?
N6 C15 H15 124.8 . . ?
C1 N1 C3 106.6(5) . . ?
C1 N1 Fe1 142.0(5) . . ?
C3 N1 Fe1 111.4(4) . . ?
C2 N2 C1 109.9(6) . . ?
C2 N2 H2A 125.0 . . ?
C1 N2 H2A 125.0 . . ?
C4 N3 N4 116.4(5) . . ?
C4 N3 Fe1 116.6(4) . . ?
N4 N3 Fe1 125.4(4) . . ?
C5 N4 N3 117.3(5) . . ?
C5 N4 C12 120.0(5) . . ?
N3 N4 C12 113.8(5) . . ?
C11 N5 C12 118.3(6) . . ?
C11 N5 H5 111.1 . . ?
C12 N5 H5 110.8 . . ?
C14 N6 C15 108.5(6) . . ?
C15 N7 C13 106.1(6) . . ?
C15 N7 Fe1 127.7(6) . . ?
C13 N7 Fe1 126.2(4) . . ?
F3 B1 F2 124.8(13) . . ?
F7 B1 F0AA 112(3) . . ?
F3 B1 F1 114.7(11) . . ?
F2 B1 F1 112.1(10) . . ?
F7 B1 F6 126(4) . . ?
F0AA B1 F6 106(3) . . ?
F7 B1 F4 109(3) . . ?
F0AA B1 F4 107(3) . . ?
F6 B1 F4 96(3) . . ?
F3 B1 F1AA 92.1(11) . . ?
F2 B1 F1AA 95.6(13) . . ?
F1 B1 F1AA 112.7(16) . . ?
C17 O2 C17 105.5(16) . 2_675 ?
O2 C17 C16 105.6(18) . . ?
O2 C17 H17A 110.6 . . ?
C16 C17 H17A 110.6 . . ?
O2 C17 H17B 110.6 . . ?
C16 C17 H17B 110.6 . . ?
H17A C17 H17B 108.8 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_refine_diff_density_max         1.466
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.128

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

data_2-123K
_database_code_depnum_ccdc_archive 'CCDC 1430793'
_audit_update_record             
;
2016-07-05 deposited with the CCDC.
2016-07-19 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         ?
_chemical_formula_sum            'C30 H32 B2 F8 Fe N14 O5'
_chemical_formula_weight         898.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   9.3220(19)
_cell_length_b                   19.465(4)
_cell_length_c                   21.148(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3837.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3147
_cell_measurement_theta_min      2.431
_cell_measurement_theta_max      24.871

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.492
_shelx_estimated_absorpt_T_min   0.895
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22685
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.073
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             8663
_reflns_number_gt                6625
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_max     0.980
_reflns_Friedel_fraction_full    0.991

_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
There are partial occupancy water molecules in the structure and
 some restraints have been used to treat these problems.
We made several attempts to obtain better quality data for 
this structure but failed, due to disorder, poor crystal quality etc.
 We are confidant the structural characterization is valid.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1900 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8663
_refine_ls_number_parameters     578
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0707
_refine_ls_wR_factor_ref         0.1853
_refine_ls_wR_factor_gt          0.1677
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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 0.71211(8) 0.49770(4) 0.22788(4) 0.0232(2) Uani 1 1 d . . . . .
C1 C 0.6469(6) 0.6161(3) 0.3140(3) 0.0274(13) Uani 1 1 d . . . . .
H1 H 0.5566 0.6243 0.2967 0.032 Uiso 1 1 d . U . . .
C2 C 0.8408(7) 0.6300(3) 0.3722(3) 0.0312(14) Uani 1 1 d . . . . .
H2 H 0.9065 0.6467 0.4013 0.037 Uiso 1 1 d . U . . .
C3 C 0.8576(6) 0.5746(3) 0.3325(3) 0.0270(12) Uani 1 1 d . . . . .
C4 C 0.9856(7) 0.5291(3) 0.3243(3) 0.0285(13) Uani 1 1 d . . . . .
H4 H 0.9614 0.4830 0.3397 0.034 Uiso 1 1 d . U . . .
C5 C 1.1838(7) 0.6079(4) 0.3361(3) 0.0367(16) Uani 1 1 d . . . . .
C6 C 1.2695(7) 0.6501(4) 0.3747(4) 0.049(2) Uani 1 1 d . . . . .
H6 H 1.2797 0.6401 0.4177 0.060 Uiso 1 1 d . U . . .
C7 C 1.3398(8) 0.7067(4) 0.3485(5) 0.056(2) Uani 1 1 d . . . . .
H7 H 1.3952 0.7346 0.3744 0.071 Uiso 1 1 d . U . . .
C8 C 1.3301(7) 0.7226(4) 0.2844(5) 0.050(2) Uani 1 1 d . . . . .
H8 H 1.3744 0.7611 0.2679 0.061 Uiso 1 1 d . U . . .
C9 C 1.2501(7) 0.6790(4) 0.2458(4) 0.0421(17) Uani 1 1 d . . . . .
H9 H 1.2459 0.6880 0.2023 0.049 Uiso 1 1 d . U . . .
C10 C 1.1762(6) 0.6227(3) 0.2705(3) 0.0317(14) Uani 1 1 d . . . . .
C11 C 1.0984(6) 0.5760(3) 0.2274(3) 0.0285(13) Uani 1 1 d . . . . .
C12 C 0.9712(6) 0.4505(3) 0.1745(3) 0.0297(13) Uani 1 1 d . . . . .
H12 H 1.0690 0.4483 0.1652 0.036 Uiso 1 1 d . U . . .
C13 C 0.8611(6) 0.4172(3) 0.1380(3) 0.0278(13) Uani 1 1 d . . . . .
C14 C 0.8590(7) 0.3733(3) 0.0873(3) 0.0309(14) Uani 1 1 d . . . . .
H14 H 0.9382 0.3562 0.0653 0.034 Uiso 1 1 d . U . . .
C15 C 0.6371(6) 0.3972(3) 0.1171(3) 0.0270(13) Uani 1 1 d . . . . .
H15 H 0.5367 0.3983 0.1173 0.031 Uiso 1 1 d . U . . .
C16 C 0.7854(7) 0.3737(3) 0.3065(3) 0.0304(13) Uani 1 1 d . . . . .
H16 H 0.8780 0.3704 0.2905 0.035 Uiso 1 1 d . U . . .
C17 C 0.5906(7) 0.3516(4) 0.3618(3) 0.0365(15) Uani 1 1 d . . . . .
H17 H 0.5263 0.3317 0.3897 0.043 Uiso 1 1 d . U . . .
C18 C 0.5677(7) 0.4073(3) 0.3241(3) 0.0292(13) Uani 1 1 d . . . . .
C19 C 0.4363(6) 0.4521(3) 0.3203(3) 0.0285(13) Uani 1 1 d . . . . .
H19 H 0.4574 0.4954 0.3418 0.033 Uiso 1 1 d . U . . .
C20 C 0.2416(6) 0.3687(3) 0.3188(3) 0.0303(14) Uani 1 1 d . . . . .
C21 C 0.1572(7) 0.3200(4) 0.3501(3) 0.0371(16) Uani 1 1 d . . . . .
H21 H 0.1448 0.3228 0.3936 0.043 Uiso 1 1 d . U . . .
C22 C 0.0865(7) 0.2697(4) 0.3165(4) 0.0391(16) Uani 1 1 d . . . . .
H22 H 0.0346 0.2361 0.3381 0.046 Uiso 1 1 d . U . . .
C23 C 0.0956(8) 0.2667(4) 0.2505(3) 0.0401(16) Uani 1 1 d . . . . .
H23 H 0.0445 0.2325 0.2287 0.048 Uiso 1 1 d . U . . .
C24 C 0.1766(7) 0.3146(3) 0.2191(3) 0.0345(14) Uani 1 1 d . . . . .
H24 H 0.1840 0.3130 0.1747 0.041 Uiso 1 1 d . U . . .
C25 C 0.2494(7) 0.3664(3) 0.2522(3) 0.0300(14) Uani 1 1 d . . . . .
C26 C 0.3249(6) 0.4204(3) 0.2172(3) 0.0289(13) Uani 1 1 d . . . . .
C27 C 0.4516(6) 0.5531(3) 0.1817(3) 0.0292(13) Uani 1 1 d . . . . .
H27 H 0.3549 0.5592 0.1740 0.035 Uiso 1 1 d . U . . .
C28 C 0.5613(6) 0.5907(3) 0.1493(3) 0.0270(12) Uani 1 1 d . . . . .
C29 C 0.5627(6) 0.6420(3) 0.1047(3) 0.0299(13) Uani 1 1 d . . . . .
H29 H 0.4841 0.6631 0.0857 0.037 Uiso 1 1 d . U . . .
C30 C 0.7845(7) 0.6119(3) 0.1298(3) 0.0277(12) Uani 1 1 d . . . . .
H30 H 0.8839 0.6113 0.1300 0.033 Uiso 1 1 d . U . . .
N1 N 0.7345(5) 0.5665(3) 0.2966(2) 0.0266(11) Uani 1 1 d . . . . .
N2 N 0.7060(6) 0.6553(3) 0.3598(2) 0.0309(11) Uani 1 1 d . . . . .
H2A H 0.6658 0.6897 0.3779 0.037 Uiso 1 1 d . U . . .
N3 N 1.1083(6) 0.5532(3) 0.3585(2) 0.0364(13) Uani 1 1 d . . . . .
H3 H 1.1350 0.5330 0.3931 0.044 Uiso 1 1 d . U . . .
N4 N 1.0262(5) 0.5233(3) 0.2566(2) 0.0262(11) Uani 1 1 d . . . . .
N5 N 0.9207(5) 0.4873(2) 0.2209(2) 0.0254(11) Uani 1 1 d . . . . .
N6 N 0.7200(6) 0.4318(3) 0.1571(2) 0.0246(10) Uani 1 1 d . . . . .
N7 N 0.7174(6) 0.3617(3) 0.0754(2) 0.0300(11) Uani 1 1 d . . . . .
H7A H 0.6835 0.3353 0.0461 0.037 Uiso 1 1 d . U . . .
N8 N 0.6922(6) 0.4209(3) 0.2900(2) 0.0275(11) Uani 1 1 d . . . . .
N9 N 0.7289(7) 0.3310(3) 0.3499(3) 0.0399(14) Uani 1 1 d . . . . .
H9A H 0.7712 0.2958 0.3665 0.047 Uiso 1 1 d . U . . .
N10 N 0.3154(6) 0.4203(3) 0.3503(3) 0.0342(12) Uani 1 1 d . . . . .
H10 H 0.2869 0.4339 0.3868 0.041 Uiso 1 1 d . U . . .
N11 N 0.3983(5) 0.4672(3) 0.2538(2) 0.0262(11) Uani 1 1 d . . . . .
N12 N 0.5020(5) 0.5090(2) 0.2232(2) 0.0242(10) Uani 1 1 d . . . . .
N13 N 0.7024(6) 0.5726(2) 0.1646(2) 0.0237(10) Uani 1 1 d . . . . .
N14 N 0.7038(6) 0.6542(3) 0.0935(2) 0.0330(12) Uani 1 1 d . . . . .
H14A H 0.7372 0.6840 0.0671 0.041 Uiso 1 1 d . U . . .
B1 B 0.3401(8) 0.2990(4) 0.0344(3) 0.0336(16) Uani 1 1 d . . . . .
B2 B 0.8976(10) 0.2244(6) 0.4702(4) 0.047(2) Uani 1 1 d . . . . .
F1 F 0.2248(6) 0.3432(3) 0.0369(2) 0.0728(16) Uani 1 1 d . . . . .
F2 F 0.4514(6) 0.3274(3) 0.0019(2) 0.0721(16) Uani 1 1 d . . . . .
F3 F 0.2954(7) 0.2392(3) 0.0092(2) 0.0738(16) Uani 1 1 d . . . . .
F4 F 0.3861(4) 0.28579(19) 0.09673(16) 0.0365(9) Uani 1 1 d . . . . .
F5 F 0.8421(5) 0.2139(3) 0.5287(2) 0.0663(15) Uani 1 1 d . . . . .
F6 F 1.0205(5) 0.1879(3) 0.4613(2) 0.0622(14) Uani 1 1 d . . . . .
F7 F 0.9264(6) 0.2968(3) 0.4662(2) 0.0660(14) Uani 1 1 d . . . . .
F8 F 0.7995(5) 0.2099(2) 0.4222(2) 0.0580(12) Uani 1 1 d . . . . .
O0AA O 1.1037(4) 0.5814(2) 0.1692(2) 0.0326(10) Uani 1 1 d . . . . .
O1AA O 0.3158(4) 0.4272(2) 0.1587(2) 0.0321(10) Uani 1 1 d . . . . .
O4AA O 1.1406(15) 0.5138(6) 0.4962(6) 0.062(3) Uani 0.5 1 d . . P . .
O2 O 0.8928(17) 0.4430(7) 0.4544(6) 0.057(4) Uani 0.4 1 d . . P . .
O5AA O 0.6366(19) 0.5061(9) 0.4604(8) 0.081(5) Uani 0.4 1 d . . P . .
O4 O 0.3946(19) 0.4433(7) 0.4889(7) 0.070(5) Uani 0.4 1 d . . P . .
O2AA O 1.249(2) 0.4864(11) 0.4754(10) 0.046(5) Uiso 0.25 1 d . . P . .
O3AA O 0.378(4) 0.4926(18) 0.5135(16) 0.045(8) Uiso 0.15 1 d . . P . .
O1 O 0.501(3) 0.5056(16) 0.4673(13) 0.078(7) Uiso 0.25 1 d . . P . .
O3 O 0.991(3) 0.4623(16) 0.4745(15) 0.083(9) Uiso 0.25 1 d . . P . .
O5 O 1.132(4) 0.443(2) 0.4601(19) 0.060(10) Uiso 0.15 1 d . . P . .
O6AA O 1.142(4) 0.466(2) 0.5135(18) 0.049(9) Uiso 0.15 1 d . . P . .
O7AA O 0.309(4) 0.496(2) 0.5589(19) 0.061(10) Uiso 0.15 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 1.960(5) . ?
Fe1 N6 1.973(5) . ?
Fe1 N12 1.973(5) . ?
Fe1 N13 1.982(5) . ?
Fe1 N1 1.987(5) . ?
Fe1 N8 1.998(5) . ?
C1 N1 1.317(7) . ?
C1 N2 1.350(8) . ?
C1 H1 0.932(6) . ?
C2 N2 1.374(8) . ?
C2 C3 1.376(8) . ?
C2 H2 0.927(6) . ?
C3 N1 1.385(7) . ?
C3 C4 1.496(9) . ?
C4 N3 1.433(8) . ?
C4 N4 1.485(7) . ?
C4 H4 0.981(7) . ?
C5 N3 1.361(9) . ?
C5 C6 1.407(9) . ?
C5 C10 1.419(10) . ?
C6 C7 1.395(13) . ?
C6 H6 0.936(8) . ?
C7 C8 1.394(13) . ?
C7 H7 0.928(8) . ?
C8 C9 1.394(10) . ?
C8 H8 0.924(8) . ?
C9 C10 1.395(10) . ?
C9 H9 0.937(8) . ?
C10 C11 1.478(8) . ?
C11 O0AA 1.236(8) . ?
C11 N4 1.375(8) . ?
C12 N5 1.303(8) . ?
C12 C13 1.438(8) . ?
C12 H12 0.934(6) . ?
C13 C14 1.372(8) . ?
C13 N6 1.405(8) . ?
C14 N7 1.362(8) . ?
C14 H14 0.934(6) . ?
C15 N6 1.329(7) . ?
C15 N7 1.347(7) . ?
C15 H15 0.936(6) . ?
C16 N8 1.312(8) . ?
C16 N9 1.345(8) . ?
C16 H16 0.930(6) . ?
C17 C18 1.363(9) . ?
C17 N9 1.374(9) . ?
C17 H17 0.926(7) . ?
C18 N8 1.392(8) . ?
C18 C19 1.506(9) . ?
C19 N10 1.434(8) . ?
C19 N11 1.480(8) . ?
C19 H19 0.977(6) . ?
C20 N10 1.388(8) . ?
C20 C21 1.399(9) . ?
C20 C25 1.410(9) . ?
C21 C22 1.378(10) . ?
C21 H21 0.928(7) . ?
C22 C23 1.399(10) . ?
C22 H22 0.933(6) . ?
C23 C24 1.371(10) . ?
C23 H23 0.940(7) . ?
C24 C25 1.402(9) . ?
C24 H24 0.943(7) . ?
C25 C26 1.466(9) . ?
C26 O1AA 1.247(7) . ?
C26 N11 1.377(8) . ?
C27 N12 1.313(8) . ?
C27 C28 1.432(9) . ?
C27 H27 0.924(6) . ?
C28 C29 1.372(9) . ?
C28 N13 1.399(8) . ?
C29 N14 1.358(8) . ?
C29 H29 0.932(6) . ?
C30 N13 1.308(8) . ?
C30 N14 1.355(8) . ?
C30 H30 0.926(6) . ?
N2 H2A 0.858(5) . ?
N3 H3 0.867(5) . ?
N4 N5 1.424(7) . ?
N7 H7A 0.865(5) . ?
N9 H9A 0.865(6) . ?
N10 H10 0.858(5) . ?
N11 N12 1.420(7) . ?
N14 H14A 0.863(5) . ?
B1 F3 1.347(9) . ?
B1 F2 1.361(9) . ?
B1 F1 1.378(9) . ?
B1 F4 1.409(8) . ?
B2 F5 1.357(9) . ?
B2 F6 1.361(10) . ?
B2 F8 1.395(10) . ?
B2 F7 1.437(11) . ?
O4AA O6AA 0.99(4) . ?
O4AA O2AA 1.22(2) . ?
O4AA O5 1.57(4) . ?
O4AA O3 1.78(3) . ?
O2 O3 1.07(3) . ?
O5AA O1 1.27(3) . ?
O4 O3AA 1.10(4) . ?
O4 O2AA 1.63(3) 1_455 ?
O4 O1 1.63(3) . ?
O2AA O6AA 1.34(4) . ?
O2AA O5 1.42(4) . ?
O2AA O3AA 1.46(4) 1_655 ?
O2AA O4 1.63(3) 1_655 ?
O3AA O7AA 1.16(5) . ?
O3AA O2AA 1.46(4) 1_455 ?
O3AA O1 1.53(4) . ?
O3 O5 1.40(5) . ?
O3 O6AA 1.64(5) . ?
O5 O6AA 1.22(5) . ?

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
N5 Fe1 N6 80.7(2) . . ?
N5 Fe1 N12 172.8(2) . . ?
N6 Fe1 N12 94.1(2) . . ?
N5 Fe1 N13 94.1(2) . . ?
N6 Fe1 N13 88.12(19) . . ?
N12 Fe1 N13 80.7(2) . . ?
N5 Fe1 N1 91.2(2) . . ?
N6 Fe1 N1 171.6(2) . . ?
N12 Fe1 N1 93.8(2) . . ?
N13 Fe1 N1 90.2(2) . . ?
N5 Fe1 N8 93.7(2) . . ?
N6 Fe1 N8 90.9(2) . . ?
N12 Fe1 N8 91.4(2) . . ?
N13 Fe1 N8 171.9(2) . . ?
N1 Fe1 N8 91.9(2) . . ?
N1 C1 N2 111.2(5) . . ?
N1 C1 H1 125.2(6) . . ?
N2 C1 H1 123.6(6) . . ?
N2 C2 C3 105.6(5) . . ?
N2 C2 H2 127.3(6) . . ?
C3 C2 H2 127.2(7) . . ?
C2 C3 N1 109.2(5) . . ?
C2 C3 C4 128.8(6) . . ?
N1 C3 C4 121.9(5) . . ?
N3 C4 N4 108.0(5) . . ?
N3 C4 C3 112.6(5) . . ?
N4 C4 C3 111.2(5) . . ?
N3 C4 H4 108.4(5) . . ?
N4 C4 H4 108.0(5) . . ?
C3 C4 H4 108.6(5) . . ?
N3 C5 C6 123.3(7) . . ?
N3 C5 C10 118.3(5) . . ?
C6 C5 C10 118.4(7) . . ?
C7 C6 C5 119.9(7) . . ?
C7 C6 H6 120.2(8) . . ?
C5 C6 H6 119.9(8) . . ?
C8 C7 C6 122.0(7) . . ?
C8 C7 H7 118.7(9) . . ?
C6 C7 H7 119.3(10) . . ?
C9 C8 C7 118.0(8) . . ?
C9 C8 H8 120.8(10) . . ?
C7 C8 H8 121.2(8) . . ?
C8 C9 C10 121.5(8) . . ?
C8 C9 H9 118.9(8) . . ?
C10 C9 H9 119.6(7) . . ?
C9 C10 C5 120.1(6) . . ?
C9 C10 C11 119.6(6) . . ?
C5 C10 C11 120.2(6) . . ?
O0AA C11 N4 122.0(6) . . ?
O0AA C11 C10 122.9(6) . . ?
N4 C11 C10 115.0(6) . . ?
N5 C12 C13 113.2(5) . . ?
N5 C12 H12 122.5(6) . . ?
C13 C12 H12 124.3(6) . . ?
C14 C13 N6 109.7(5) . . ?
C14 C13 C12 135.3(6) . . ?
N6 C13 C12 115.0(5) . . ?
N7 C14 C13 105.1(5) . . ?
N7 C14 H14 128.0(6) . . ?
C13 C14 H14 126.8(6) . . ?
N6 C15 N7 110.7(5) . . ?
N6 C15 H15 124.5(6) . . ?
N7 C15 H15 124.7(6) . . ?
N8 C16 N9 110.8(5) . . ?
N8 C16 H16 124.5(6) . . ?
N9 C16 H16 124.6(6) . . ?
C18 C17 N9 105.8(6) . . ?
C18 C17 H17 127.2(7) . . ?
N9 C17 H17 127.0(7) . . ?
C17 C18 N8 108.9(5) . . ?
C17 C18 C19 128.3(6) . . ?
N8 C18 C19 122.7(5) . . ?
N10 C19 N11 108.6(5) . . ?
N10 C19 C18 111.4(5) . . ?
N11 C19 C18 111.1(5) . . ?
N10 C19 H19 109.0(5) . . ?
N11 C19 H19 108.6(5) . . ?
C18 C19 H19 108.1(5) . . ?
N10 C20 C21 122.8(6) . . ?
N10 C20 C25 118.5(5) . . ?
C21 C20 C25 118.7(6) . . ?
C22 C21 C20 120.4(7) . . ?
C22 C21 H21 119.6(7) . . ?
C20 C21 H21 119.9(7) . . ?
C21 C22 C23 121.0(6) . . ?
C21 C22 H22 119.5(8) . . ?
C23 C22 H22 119.4(8) . . ?
C24 C23 C22 119.2(7) . . ?
C24 C23 H23 121.6(7) . . ?
C22 C23 H23 119.2(7) . . ?
C23 C24 C25 120.9(6) . . ?
C23 C24 H24 120.0(7) . . ?
C25 C24 H24 119.1(6) . . ?
C24 C25 C20 119.7(6) . . ?
C24 C25 C26 119.7(6) . . ?
C20 C25 C26 120.5(6) . . ?
O1AA C26 N11 121.4(6) . . ?
O1AA C26 C25 123.1(6) . . ?
N11 C26 C25 115.4(5) . . ?
N12 C27 C28 113.5(5) . . ?
N12 C27 H27 123.4(6) . . ?
C28 C27 H27 123.1(6) . . ?
C29 C28 N13 109.4(5) . . ?
C29 C28 C27 135.0(6) . . ?
N13 C28 C27 115.6(5) . . ?
N14 C29 C28 104.9(5) . . ?
N14 C29 H29 127.5(6) . . ?
C28 C29 H29 127.6(6) . . ?
N13 C30 N14 110.4(5) . . ?
N13 C30 H30 125.2(6) . . ?
N14 C30 H30 124.4(6) . . ?
C1 N1 C3 106.1(5) . . ?
C1 N1 Fe1 129.3(4) . . ?
C3 N1 Fe1 124.4(4) . . ?
C1 N2 C2 107.9(5) . . ?
C1 N2 H2A 125.6(6) . . ?
C2 N2 H2A 126.4(6) . . ?
C5 N3 C4 119.5(5) . . ?
C5 N3 H3 120.0(6) . . ?
C4 N3 H3 120.5(6) . . ?
C11 N4 N5 117.8(5) . . ?
C11 N4 C4 120.1(5) . . ?
N5 N4 C4 111.8(4) . . ?
C12 N5 N4 114.8(5) . . ?
C12 N5 Fe1 118.2(4) . . ?
N4 N5 Fe1 126.5(4) . . ?
C15 N6 C13 105.0(5) . . ?
C15 N6 Fe1 142.3(4) . . ?
C13 N6 Fe1 112.6(4) . . ?
C15 N7 C14 109.4(5) . . ?
C15 N7 H7A 124.8(6) . . ?
C14 N7 H7A 125.8(6) . . ?
C16 N8 C18 106.3(5) . . ?
C16 N8 Fe1 129.6(4) . . ?
C18 N8 Fe1 124.1(4) . . ?
C16 N9 C17 108.2(5) . . ?
C16 N9 H9A 126.1(6) . . ?
C17 N9 H9A 125.7(7) . . ?
C20 N10 C19 119.3(5) . . ?
C20 N10 H10 120.2(5) . . ?
C19 N10 H10 120.5(6) . . ?
C26 N11 N12 117.5(5) . . ?
C26 N11 C19 121.5(5) . . ?
N12 N11 C19 112.6(4) . . ?
C27 N12 N11 115.8(5) . . ?
C27 N12 Fe1 117.5(4) . . ?
N11 N12 Fe1 126.0(4) . . ?
C30 N13 C28 105.9(5) . . ?
C30 N13 Fe1 141.5(4) . . ?
C28 N13 Fe1 112.6(4) . . ?
C30 N14 C29 109.4(5) . . ?
C30 N14 H14A 125.1(6) . . ?
C29 N14 H14A 125.5(6) . . ?
F3 B1 F2 112.7(7) . . ?
F3 B1 F1 108.2(6) . . ?
F2 B1 F1 111.1(7) . . ?
F3 B1 F4 107.9(6) . . ?
F2 B1 F4 108.4(6) . . ?
F1 B1 F4 108.5(6) . . ?
F5 B2 F6 111.6(7) . . ?
F5 B2 F8 112.5(7) . . ?
F6 B2 F8 110.2(7) . . ?
F5 B2 F7 105.8(7) . . ?
F6 B2 F7 110.2(7) . . ?
F8 B2 F7 106.2(6) . . ?
O6AA O4AA O2AA 74(2) . . ?
O6AA O4AA O5 51(3) . . ?
O2AA O4AA O5 59.2(17) . . ?
O6AA O4AA O3 65(2) . . ?
O2AA O4AA O3 108.0(15) . . ?
O5 O4AA O3 48.8(17) . . ?
O3AA O4 O2AA 61(2) . 1_455 ?
O3AA O4 O1 65(2) . . ?
O2AA O4 O1 94.5(14) 1_455 . ?
O4AA O2AA O6AA 45.3(18) . . ?
O4AA O2AA O5 73(2) . . ?
O6AA O2AA O5 52(2) . . ?
O4AA O2AA O3AA 117(2) . 1_655 ?
O6AA O2AA O3AA 108(2) . 1_655 ?
O5 O2AA O3AA 144(3) . 1_655 ?
O4AA O2AA O4 148.4(18) . 1_655 ?
O6AA O2AA O4 111(2) . 1_655 ?
O5 O2AA O4 112(2) . 1_655 ?
O3AA O2AA O4 41.5(15) 1_655 1_655 ?
O4 O3AA O7AA 122(4) . . ?
O4 O3AA O2AA 78(2) . 1_455 ?
O7AA O3AA O2AA 91(3) . 1_455 ?
O4 O3AA O1 75(2) . . ?
O7AA O3AA O1 159(4) . . ?
O2AA O3AA O1 106(2) 1_455 . ?
O5AA O1 O3AA 145(3) . . ?
O5AA O1 O4 130(2) . . ?
O3AA O1 O4 40.6(15) . . ?
O2 O3 O5 128(3) . . ?
O2 O3 O6AA 161(3) . . ?
O5 O3 O6AA 47(2) . . ?
O2 O3 O4AA 165(3) . . ?
O5 O3 O4AA 58(2) . . ?
O6AA O3 O4AA 33.5(15) . . ?
O6AA O5 O3 77(3) . . ?
O6AA O5 O2AA 61(3) . . ?
O3 O5 O2AA 121(3) . . ?
O6AA O5 O4AA 39(2) . . ?
O3 O5 O4AA 73(2) . . ?
O2AA O5 O4AA 47.8(16) . . ?
O4AA O6AA O5 90(4) . . ?
O4AA O6AA O2AA 61(2) . . ?
O5 O6AA O2AA 67(3) . . ?
O4AA O6AA O3 81(3) . . ?
O5 O6AA O3 56(3) . . ?
O2AA O6AA O3 110(3) . . ?

_refine_diff_density_max         0.818
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.092


# start Validation Reply Form

_vrf_PLAT430_2-123K              
;
PROBLEM: Short Inter D...A Contact  O1     ..  O2AA    ..       2.39 Ang.
Short Inter D...A Contact  O2     ..  O5AA    ..       2.69 Ang. 
Short Inter D...A Contact  O4     ..  O5AA    ..       2.64 Ang. 
Short Inter D...A Contact  O5     ..  O3AA    ..       2.73 Ang. 
RESPONSE: There is evidence of large thermal motion of the water molcules
 in the crystal structure,which lead to some heavy disorder.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-298K
_database_code_depnum_ccdc_archive 'CCDC 1430794'
_audit_update_record             
;
2016-07-05 deposited with the CCDC.
2016-07-19 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         ?
_chemical_formula_sum            'C30 H32 B2 F8 Fe N14 O5'
_chemical_formula_weight         898.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   9.4524(19)
_cell_length_b                   19.536(4)
_cell_length_c                   21.598(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3988.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1417
_cell_measurement_theta_min      2.487
_cell_measurement_theta_max      24.316

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.473
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30236
_diffrn_reflns_av_unetI/netI     0.4269
_diffrn_reflns_av_R_equivalents  0.2422
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.999
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9057
_reflns_number_gt                1902
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    0.998

_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
There are partial occupancy water molecules in the structure and
 some restraints have been used to treat these problems.
We made several attempts to obtain better quality data for 
this structure but failed, due to disorder, poor crystal quality etc.
 We are confidant the structural characterization is valid.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1230P)²] 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_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.03(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9057
_refine_ls_number_parameters     558
_refine_ls_number_restraints     543
_refine_ls_R_factor_all          0.2754
_refine_ls_R_factor_gt           0.0850
_refine_ls_wR_factor_ref         0.2313
_refine_ls_wR_factor_gt          0.1979
_refine_ls_goodness_of_fit_ref   0.603
_refine_ls_restrained_S_all      0.617
_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 0.77880(16) 0.49760(8) 0.77152(6) 0.0954(6) Uani 1 1 d . U . . .
C1 C 0.7049(14) 0.3774(6) 0.6916(5) 0.109(3) Uani 1 1 d . U . . .
C2 C 0.8998(15) 0.3570(6) 0.6366(5) 0.121(4) Uani 1 1 d . U . . .
H2 H 0.9638 0.3378 0.6089 0.145 Uiso 1 1 calc R U . . .
C3 C 0.9214(14) 0.4111(6) 0.6759(5) 0.102(3) Uani 1 1 d . U . . .
C4 C 1.0477(13) 0.4549(5) 0.6803(5) 0.102(3) Uani 1 1 d . U . . .
H4 H 1.0288 0.4987 0.6598 0.123 Uiso 1 1 calc R U . . .
C5 C 1.2461(14) 0.3719(6) 0.6800(6) 0.108(4) Uani 1 1 d . U . . .
C6 C 1.3301(15) 0.3251(7) 0.6482(6) 0.124(4) Uani 1 1 d . U . . .
H6 H 1.3384 0.3283 0.6053 0.149 Uiso 1 1 calc R U . . .
C7 C 1.3993(14) 0.2755(7) 0.6788(7) 0.134(4) Uani 1 1 d . U . . .
H7 H 1.4551 0.2449 0.6566 0.161 Uiso 1 1 calc R U . . .
C8 C 1.3893(15) 0.2680(7) 0.7474(6) 0.137(4) Uani 1 1 d . U . . .
H8 H 1.4363 0.2337 0.7689 0.165 Uiso 1 1 calc R U . . .
C9 C 1.3084(14) 0.3139(6) 0.7754(6) 0.118(4) Uani 1 1 d . U . . .
H9 H 1.2966 0.3104 0.8180 0.142 Uiso 1 1 calc R U . . .
C10 C 1.2389(13) 0.3680(6) 0.7441(6) 0.109(3) Uani 1 1 d . U . . .
C11 C 1.1622(13) 0.4220(6) 0.7784(6) 0.103(3) Uani 1 1 d . U . . .
C12 C 1.0401(14) 0.5500(5) 0.8206(5) 0.104(3) Uani 1 1 d . U . . .
H12 H 1.1355 0.5538 0.8307 0.124 Uiso 1 1 calc R U . . .
C13 C 0.9301(14) 0.5875(6) 0.8509(5) 0.099(3) Uani 1 1 d . U . . .
C14 C 0.9332(15) 0.6391(6) 0.8966(5) 0.113(4) Uani 1 1 d . U . . .
H14 H 1.0105 0.6611 0.9144 0.135 Uiso 1 1 calc R U . . .
C15 C 0.7099(15) 0.6074(6) 0.8709(5) 0.101(3) Uani 1 1 d . U . . .
H15 H 0.6116 0.6064 0.8708 0.121 Uiso 1 1 calc R U . . .
C16 C 0.8472(14) 0.6182(6) 0.6882(6) 0.117(4) Uani 1 1 d . U . . .
C17 C 0.6495(15) 0.6324(7) 0.6301(5) 0.112(4) Uani 1 1 d . U . . .
C18 C 0.6323(14) 0.5767(6) 0.6686(5) 0.104(3) Uani 1 1 d . U . . .
C19 C 0.5079(14) 0.5307(6) 0.6786(5) 0.110(3) Uani 1 1 d . U . . .
H19 H 0.5320 0.4850 0.6631 0.133 Uiso 1 1 calc R U . . .
C20 C 0.3143(15) 0.6129(8) 0.6688(7) 0.126(4) Uani 1 1 d . U . . .
C21 C 0.2201(15) 0.6571(8) 0.6319(7) 0.145(5) Uani 1 1 d . U . . .
H21 H 0.2052 0.6491 0.5900 0.174 Uiso 1 1 calc R U . . .
C22 C 0.1516(17) 0.7135(9) 0.6637(8) 0.158(6) Uani 1 1 d . U . . .
H22 H 0.0970 0.7443 0.6411 0.189 Uiso 1 1 calc R U . . .
C23 C 0.1649(16) 0.7215(8) 0.7214(8) 0.149(5) Uani 1 1 d . U . . .
H23 H 0.1174 0.7580 0.7397 0.179 Uiso 1 1 calc R U . . .
C24 C 0.2436(15) 0.6807(6) 0.7586(7) 0.130(4) Uani 1 1 d . U . . .
H24 H 0.2478 0.6895 0.8008 0.156 Uiso 1 1 calc R U . . .
C25 C 0.3198(13) 0.6244(6) 0.7335(6) 0.113(4) Uani 1 1 d . U . . .
C26 C 0.3927(12) 0.5765(6) 0.7754(6) 0.101(3) Uani 1 1 d . U . . .
C27 C 0.5234(13) 0.4512(6) 0.8211(5) 0.106(4) Uani 1 1 d . U . . .
H27 H 0.4274 0.4495 0.8303 0.127 Uiso 1 1 calc R U . . .
C28 C 0.6226(14) 0.4143(6) 0.8562(5) 0.100(3) Uani 1 1 d . U . . .
C29 C 0.6270(17) 0.3698(7) 0.9067(6) 0.126(4) Uani 1 1 d . U . . .
H29 H 0.5501 0.3524 0.9284 0.151 Uiso 1 1 calc R U . . .
C30 C 0.8496(15) 0.3942(6) 0.8787(5) 0.107(3) Uani 1 1 d . U . . .
H30 H 0.9479 0.3950 0.8791 0.128 Uiso 1 1 calc R U . . .
N1 N 0.7966(12) 0.4233(4) 0.7085(4) 0.097(3) Uani 1 1 d . U . . .
N2 N 0.7616(13) 0.3374(5) 0.6476(4) 0.122(3) Uani 1 1 d . U . . .
H2A H 0.7185 0.3045 0.6291 0.146 Uiso 1 1 calc R U . . .
N3 N 1.1763(11) 0.4219(5) 0.6511(4) 0.114(3) Uani 1 1 d . U . . .
H3 H 1.2048 0.4356 0.6154 0.137 Uiso 1 1 calc R U . . .
N4 N 1.0885(10) 0.4674(4) 0.7451(4) 0.097(3) Uani 1 1 d . U . . .
N5 N 0.9911(9) 0.5092(4) 0.7766(4) 0.095(2) Uani 1 1 d . U . . .
N6 N 0.7905(14) 0.6482(5) 0.9078(4) 0.123(3) Uani 1 1 d . U . . .
H6A H 0.7568 0.6762 0.9347 0.148 Uiso 1 1 calc R U . . .
N7 N 0.7885(11) 0.5709(4) 0.8369(3) 0.084(2) Uani 1 1 d . U . . .
N8 N 0.7858(13) 0.6566(5) 0.6401(4) 0.119(3) Uani 1 1 d . U . . .
H8A H 0.8258 0.6895 0.6203 0.142 Uiso 1 1 calc R U . . .
N9 N 0.7572(11) 0.5686(4) 0.7046(4) 0.100(3) Uani 1 1 d . U . . .
N10 N 0.3847(12) 0.5553(5) 0.6447(4) 0.126(3) Uani 1 1 d . U . . .
H10 H 0.4035 0.5605 0.6061 0.151 Uiso 1 1 d R U . . .
N11 N 0.4697(10) 0.5249(5) 0.7430(4) 0.099(3) Uani 1 1 d . U . . .
N12 N 0.5694(10) 0.4868(5) 0.7766(4) 0.102(2) Uani 1 1 d . U . . .
N13 N 0.7691(12) 0.4297(4) 0.8391(4) 0.095(3) Uani 1 1 d . U . . .
N14 N 0.7688(13) 0.3568(5) 0.9181(4) 0.118(3) Uani 1 1 d . U . . .
H14A H 0.8006 0.3292 0.9459 0.141 Uiso 1 1 calc R U . . .
O0AA O 1.1682(9) 0.4254(4) 0.8369(4) 0.114(3) Uani 1 1 d . U . . .
O1AA O 0.3906(9) 0.5773(4) 0.8313(4) 0.123(3) Uani 1 1 d . U . . .
B1 B 0.603(2) 0.2172(11) 0.5297(8) 0.197(7) Uani 1 1 d D U . . .
F0AA F 0.4829(14) 0.1847(6) 0.5357(4) 0.229(5) Uani 1 1 d D U . . .
F2AA F 0.6479(13) 0.2121(7) 0.4733(4) 0.250(5) Uani 1 1 d D U . . .
F3AA F 0.5887(17) 0.2879(7) 0.5339(5) 0.272(6) Uani 1 1 d D U . . .
F1AA F 0.6798(14) 0.2086(6) 0.5794(5) 0.239(5) Uani 1 1 d D U . . .
F1 F 1.1135(9) 0.2812(4) 0.9078(4) 0.161(3) Uani 1 1 d D U . . .
F2 F 1.1945(15) 0.2404(6) 0.9943(5) 0.249(5) Uani 1 1 d D U . . .
F3 F 1.0390(15) 0.3237(7) 0.9957(5) 0.262(6) Uani 1 1 d D U . . .
F4 F 1.2583(15) 0.3379(8) 0.9648(6) 0.273(6) Uani 1 1 d D U . . .
B11 B 1.145(2) 0.2902(9) 0.9668(8) 0.178(7) Uani 1 1 d D U . . .
O1 O 1.000(5) 0.531(2) 0.538(2) 0.163(17) Uiso 0.25 1 d . . P . .
O5AA O 0.463(6) 0.516(3) 0.517(2) 0.184(16) Uiso 0.25 1 d . . P . .
O5 O 0.669(7) 0.453(2) 0.5448(19) 0.161(14) Uiso 0.25 1 d . . P . .
O6 O 0.543(8) 0.455(2) 0.540(2) 0.169(15) Uiso 0.25 1 d . . P . .
O7 O 0.757(6) 0.492(3) 0.514(2) 0.22(2) Uiso 0.25 1 d . . P . .
O2AA O 0.952(7) 0.495(3) 0.537(2) 0.22(2) Uiso 0.25 1 d . . P . .
O3AA O 1.200(4) 0.4955(18) 0.4497(17) 0.170(13) Uiso 0.25 1 d . . P . .
O4AA O 1.407(7) 0.453(3) 0.529(2) 0.186(18) Uiso 0.25 1 d . . P . .
O3 O 1.105(9) 0.463(4) 0.508(3) 0.18(3) Uiso 0.15 1 d . . P . .
O6AA O 1.263(8) 0.503(4) 0.528(3) 0.18(2) Uiso 0.15 1 d . . P . .
O7AA O 0.362(9) 0.494(4) 0.494(3) 0.17(2) Uiso 0.15 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N13 1.974(9) . ?
Fe1 N12 1.994(10) . ?
Fe1 N1 1.998(9) . ?
Fe1 N9 2.013(9) . ?
Fe1 N7 2.014(8) . ?
Fe1 N5 2.023(9) . ?
C1 N1 1.299(13) . ?
C1 N2 1.341(13) . ?
C2 C3 1.370(14) . ?
C2 N2 1.382(15) . ?
C2 H2 0.9300 . ?
C3 N1 1.394(14) . ?
C3 C4 1.473(15) . ?
C4 N4 1.472(12) . ?
C4 N3 1.513(13) . ?
C4 H4 0.9800 . ?
C5 N3 1.334(13) . ?
C5 C10 1.387(14) . ?
C5 C6 1.392(16) . ?
C6 C7 1.345(16) . ?
C6 H6 0.9300 . ?
C7 C8 1.491(16) . ?
C7 H7 0.9300 . ?
C8 C9 1.323(15) . ?
C8 H8 0.9300 . ?
C9 C10 1.416(15) . ?
C9 H9 0.9300 . ?
C10 C11 1.480(16) . ?
C11 O0AA 1.266(12) . ?
C11 N4 1.339(13) . ?
C12 N5 1.324(12) . ?
C12 C13 1.432(14) . ?
C12 H12 0.9300 . ?
C13 N7 1.410(14) . ?
C13 C14 1.411(14) . ?
C14 N6 1.381(15) . ?
C14 H14 0.9300 . ?
C15 N7 1.264(12) . ?
C15 N6 1.360(14) . ?
C15 H15 0.9300 . ?
C16 N9 1.338(13) . ?
C16 N8 1.406(14) . ?
C17 C18 1.381(14) . ?
C17 N8 1.389(15) . ?
C18 N9 1.423(14) . ?
C18 C19 1.495(15) . ?
C19 N11 1.442(12) . ?
C19 N10 1.455(14) . ?
C19 H19 0.9800 . ?
C20 N10 1.408(16) . ?
C20 C25 1.416(16) . ?
C20 C21 1.473(18) . ?
C21 C22 1.45(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.263(17) . ?
C22 H22 0.9300 . ?
C23 C24 1.355(17) . ?
C23 H23 0.9300 . ?
C24 C25 1.421(16) . ?
C24 H24 0.9300 . ?
C25 C26 1.472(15) . ?
C26 O1AA 1.206(12) . ?
C26 N11 1.427(14) . ?
C27 N12 1.263(12) . ?
C27 C28 1.405(15) . ?
C27 H27 0.9300 . ?
C28 C29 1.395(15) . ?
C28 N13 1.464(15) . ?
C29 N14 1.386(15) . ?
C29 H29 0.9300 . ?
C30 N13 1.338(13) . ?
C30 N14 1.358(14) . ?
C30 H30 0.9300 . ?
N2 H2A 0.8600 . ?
N3 H3 0.8600 . ?
N4 N5 1.406(10) . ?
N6 H6A 0.8600 . ?
N8 H8A 0.8600 . ?
N10 H10 0.8598 . ?
N11 N12 1.404(11) . ?
N14 H14A 0.8600 . ?
B1 F2AA 1.294(15) . ?
B1 F0AA 1.305(15) . ?
B1 F1AA 1.308(15) . ?
B1 F3AA 1.391(17) . ?
F1 B11 1.321(15) . ?
F2 B11 1.230(15) . ?
F3 B11 1.352(15) . ?
F4 B11 1.418(16) . ?
O1 O2AA 0.84(7) . ?
O1 O3 1.78(8) . ?
O5AA O7AA 1.15(8) . ?
O5AA O4AA 1.37(6) 1_455 ?
O5AA O6 1.49(6) . ?
O5 O6 1.20(6) . ?
O5 O7 1.30(6) . ?
O6 O4AA 1.30(6) 1_455 ?
O2AA O3 1.69(8) . ?
O3AA O3 1.67(7) . ?
O3AA O6AA 1.80(8) . ?
O3AA O7AA 1.81(9) 1_655 ?
O4AA O7AA 1.19(8) 1_655 ?
O4AA O6 1.30(6) 1_655 ?
O4AA O5AA 1.37(6) 1_655 ?
O4AA O6AA 1.67(9) . ?
O3 O6AA 1.74(9) . ?
O6AA O7AA 1.20(8) 1_655 ?
O7AA O4AA 1.19(8) 1_455 ?
O7AA O6AA 1.20(8) 1_455 ?
O7AA O3AA 1.81(9) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N13 Fe1 N12 80.9(4) . . ?
N13 Fe1 N1 91.1(3) . . ?
N12 Fe1 N1 92.5(4) . . ?
N13 Fe1 N9 171.4(5) . . ?
N12 Fe1 N9 90.7(4) . . ?
N1 Fe1 N9 91.2(3) . . ?
N13 Fe1 N7 87.8(3) . . ?
N12 Fe1 N7 94.7(4) . . ?
N1 Fe1 N7 172.4(5) . . ?
N9 Fe1 N7 91.0(3) . . ?
N13 Fe1 N5 94.7(4) . . ?
N12 Fe1 N5 173.7(3) . . ?
N1 Fe1 N5 92.0(4) . . ?
N9 Fe1 N5 93.6(4) . . ?
N7 Fe1 N5 80.6(4) . . ?
N1 C1 N2 109.6(12) . . ?
C3 C2 N2 104.4(12) . . ?
C3 C2 H2 127.8 . . ?
N2 C2 H2 127.8 . . ?
C2 C3 N1 108.6(11) . . ?
C2 C3 C4 127.5(12) . . ?
N1 C3 C4 123.7(11) . . ?
N4 C4 C3 111.7(9) . . ?
N4 C4 N3 104.8(9) . . ?
C3 C4 N3 112.1(9) . . ?
N4 C4 H4 109.4 . . ?
C3 C4 H4 109.4 . . ?
N3 C4 H4 109.4 . . ?
N3 C5 C10 118.8(13) . . ?
N3 C5 C6 122.1(12) . . ?
C10 C5 C6 119.0(14) . . ?
C7 C6 C5 120.5(14) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 122.0(14) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 115.1(14) . . ?
C9 C8 H8 122.5 . . ?
C7 C8 H8 122.5 . . ?
C8 C9 C10 123.7(13) . . ?
C8 C9 H9 118.1 . . ?
C10 C9 H9 118.1 . . ?
C5 C10 C9 119.6(13) . . ?
C5 C10 C11 119.0(12) . . ?
C9 C10 C11 121.3(11) . . ?
O0AA C11 N4 121.7(12) . . ?
O0AA C11 C10 121.1(12) . . ?
N4 C11 C10 117.2(11) . . ?
N5 C12 C13 112.5(12) . . ?
N5 C12 H12 123.8 . . ?
C13 C12 H12 123.8 . . ?
N7 C13 C14 109.5(11) . . ?
N7 C13 C12 118.3(11) . . ?
C14 C13 C12 132.1(12) . . ?
N6 C14 C13 101.1(12) . . ?
N6 C14 H14 129.4 . . ?
C13 C14 H14 129.4 . . ?
N7 C15 N6 110.0(13) . . ?
N7 C15 H15 125.0 . . ?
N6 C15 H15 125.0 . . ?
N9 C16 N8 108.7(12) . . ?
C18 C17 N8 106.5(11) . . ?
C17 C18 N9 108.6(11) . . ?
C17 C18 C19 130.8(12) . . ?
N9 C18 C19 120.5(11) . . ?
N11 C19 N10 108.1(10) . . ?
N11 C19 C18 112.5(9) . . ?
N10 C19 C18 111.0(10) . . ?
N11 C19 H19 108.4 . . ?
N10 C19 H19 108.4 . . ?
C18 C19 H19 108.4 . . ?
N10 C20 C25 118.2(14) . . ?
N10 C20 C21 123.7(14) . . ?
C25 C20 C21 117.6(15) . . ?
C22 C21 C20 117.3(15) . . ?
C22 C21 H21 121.3 . . ?
C20 C21 H21 121.3 . . ?
C23 C22 C21 121.1(18) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 124.5(18) . . ?
C22 C23 H23 117.7 . . ?
C24 C23 H23 117.7 . . ?
C23 C24 C25 120.6(14) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C20 C25 C24 118.6(13) . . ?
C20 C25 C26 121.6(14) . . ?
C24 C25 C26 119.6(12) . . ?
O1AA C26 N11 120.5(12) . . ?
O1AA C26 C25 126.8(13) . . ?
N11 C26 C25 112.7(11) . . ?
N12 C27 C28 117.6(13) . . ?
N12 C27 H27 121.2 . . ?
C28 C27 H27 121.2 . . ?
C29 C28 C27 139.6(13) . . ?
C29 C28 N13 107.3(11) . . ?
C27 C28 N13 112.9(11) . . ?
N14 C29 C28 106.4(12) . . ?
N14 C29 H29 126.8 . . ?
C28 C29 H29 126.8 . . ?
N13 C30 N14 111.1(13) . . ?
N13 C30 H30 124.5 . . ?
N14 C30 H30 124.5 . . ?
C1 N1 C3 107.7(10) . . ?
C1 N1 Fe1 129.6(9) . . ?
C3 N1 Fe1 122.6(8) . . ?
C1 N2 C2 109.7(11) . . ?
C1 N2 H2A 125.1 . . ?
C2 N2 H2A 125.1 . . ?
C5 N3 C4 121.0(10) . . ?
C5 N3 H3 119.5 . . ?
C4 N3 H3 119.5 . . ?
C11 N4 N5 117.7(9) . . ?
C11 N4 C4 122.5(10) . . ?
N5 N4 C4 112.7(9) . . ?
C12 N5 N4 117.9(10) . . ?
C12 N5 Fe1 117.0(8) . . ?
N4 N5 Fe1 124.0(7) . . ?
C15 N6 C14 111.7(11) . . ?
C15 N6 H6A 124.2 . . ?
C14 N6 H6A 124.2 . . ?
C15 N7 C13 107.7(11) . . ?
C15 N7 Fe1 141.4(10) . . ?
C13 N7 Fe1 111.0(8) . . ?
C17 N8 C16 108.5(11) . . ?
C17 N8 H8A 125.7 . . ?
C16 N8 H8A 125.7 . . ?
C16 N9 C18 107.6(10) . . ?
C16 N9 Fe1 128.7(9) . . ?
C18 N9 Fe1 123.6(8) . . ?
C20 N10 C19 117.2(11) . . ?
C20 N10 H10 111.2 . . ?
C19 N10 H10 111.2 . . ?
N12 N11 C26 117.6(9) . . ?
N12 N11 C19 111.9(10) . . ?
C26 N11 C19 123.1(10) . . ?
C27 N12 N11 117.0(10) . . ?
C27 N12 Fe1 116.2(8) . . ?
N11 N12 Fe1 125.6(7) . . ?
C30 N13 C28 105.7(11) . . ?
C30 N13 Fe1 142.5(10) . . ?
C28 N13 Fe1 111.6(8) . . ?
C30 N14 C29 109.5(12) . . ?
C30 N14 H14A 125.3 . . ?
C29 N14 H14A 125.3 . . ?
F2AA B1 F0AA 110.1(15) . . ?
F2AA B1 F1AA 125.3(19) . . ?
F0AA B1 F1AA 109.8(15) . . ?
F2AA B1 F3AA 99.7(15) . . ?
F0AA B1 F3AA 113.3(18) . . ?
F1AA B1 F3AA 97.3(14) . . ?
F2 B11 F1 116.5(16) . . ?
F2 B11 F3 116.2(17) . . ?
F1 B11 F3 110.0(15) . . ?
F2 B11 F4 104.4(16) . . ?
F1 B11 F4 103.3(15) . . ?
F3 B11 F4 104.8(15) . . ?
O2AA O1 O3 70(6) . . ?
O7AA O5AA O4AA 56(5) . 1_455 ?
O7AA O5AA O6 105(6) . . ?
O4AA O5AA O6 54(3) 1_455 . ?
O6 O5 O7 125(5) . . ?
O5 O6 O4AA 174(5) . 1_455 ?
O5 O6 O5AA 124(6) . . ?
O4AA O6 O5AA 58(4) 1_455 . ?
O1 O2AA O3 82(7) . . ?
O3 O3AA O6AA 60(3) . . ?
O3 O3AA O7AA 93(4) . 1_655 ?
O6AA O3AA O7AA 39(3) . 1_655 ?
O7AA O4AA O6 116(7) 1_655 1_655 ?
O7AA O4AA O5AA 53(4) 1_655 1_655 ?
O6 O4AA O5AA 68(4) 1_655 1_655 ?
O7AA O4AA O6AA 46(4) 1_655 . ?
O6 O4AA O6AA 142(5) 1_655 . ?
O5AA O4AA O6AA 78(5) 1_655 . ?
O3AA O3 O2AA 127(5) . . ?
O3AA O3 O6AA 64(4) . . ?
O2AA O3 O6AA 119(5) . . ?
O3AA O3 O1 107(4) . . ?
O2AA O3 O1 28(3) . . ?
O6AA O3 O1 94(5) . . ?
O7AA O6AA O4AA 45(5) 1_655 . ?
O7AA O6AA O3 118(8) 1_655 . ?
O4AA O6AA O3 117(6) . . ?
O7AA O6AA O3AA 71(6) 1_655 . ?
O4AA O6AA O3AA 104(4) . . ?
O3 O6AA O3AA 56(3) . . ?
O5AA O7AA O4AA 71(6) . 1_455 ?
O5AA O7AA O6AA 110(8) . 1_455 ?
O4AA O7AA O6AA 89(7) 1_455 1_455 ?
O5AA O7AA O3AA 157(8) . 1_455 ?
O4AA O7AA O3AA 130(8) 1_455 1_455 ?
O6AA O7AA O3AA 70(6) 1_455 1_455 ?

_refine_diff_density_max         0.456
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.073


_vrf_PLAT430_2-298K              
;
PROBLEM: Short Inter D...A Contact  O1     ..  O7      ..       2.48 Ang. 
Short Inter D...A Contact  O2AA   ..  O7      ..       1.91 Ang.  
RESPONSE: There is evidence of large thermal motion of the water molcules
 in the crystal structure,which lead to some heavy disorder.
;
_vrf_PLAT026_2-298K              
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         21 % 
RESPONSE: The cystal is very unstable at room temperature. 
;
# end Validation Reply Form
