# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_shi_3469_divi
_database_code_depnum_ccdc_archive 'CCDC 1582395'
_audit_update_record             
;
2017-10-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;
_audit_creation_date             2017-10-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C40 H38 B2 Dy2 Fe2 N28 O14, 4(H2 O)'
_chemical_formula_sum            'C40 H46 B2 Dy2 Fe2 N28 O18'
_chemical_formula_weight         1665.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N8 O8 Fe1 Dy1'
_chemical_oxdiff_usercomment     FeDypyim
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   11.0216(9)
_cell_length_b                   13.5484(8)
_cell_length_c                   13.8450(11)
_cell_angle_alpha                61.208(8)
_cell_angle_beta                 77.217(7)
_cell_angle_gamma                66.516(8)
_cell_volume                     1660.7(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4009
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6600
_cell_measurement_theta_min      1.7740
_exptl_absorpt_coefficient_mu    2.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12061
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.68
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  18.00   1.00   60.00    --  -15.44 -99.00 -90.00   37
  2  ω    -22.00  24.00   1.00   60.00    --  -15.44 -99.00 150.00   46
  3  ω    -33.00  38.00   1.00   60.00    --   17.71 -77.00   0.00   71
  4  ω     43.00  85.00   1.00   60.00    --   17.71  38.00 -30.00   42
  5  ω     12.00  85.00   1.00   60.00    --   17.71  57.00-180.00   73
  6  ω     35.00  84.00   1.00   60.00    --   17.71 178.00   0.00   49
  7  ω      0.00  87.00   1.00   60.00    --   17.71  38.00 120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0680159000
_diffrn_orient_matrix_UB_12      -0.0266327000
_diffrn_orient_matrix_UB_13      0.0123589000
_diffrn_orient_matrix_UB_21      -0.0171448000
_diffrn_orient_matrix_UB_22      -0.0267042000
_diffrn_orient_matrix_UB_23      0.0570373000
_diffrn_orient_matrix_UB_31      0.0033084000
_diffrn_orient_matrix_UB_32      -0.0511414000
_diffrn_orient_matrix_UB_33      -0.0042144000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4933
_reflns_number_total             5818
_reflns_odcompleteness_completeness 99.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.422
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5818
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0406
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0279P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0846
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O5W(0.15) H5WA(0.15) H5WB(0.15) O6W(0.25) H6WA(0.25) H6WB(0.25)
 O4W(0.4) H4WA(0.4) H4WB(0.4) O7W(0.25) H7WA(0.25) H7WB(0.25) O2W(0.2)
 H2WA(0.2) H2WB(0.2) O3W(0.75) H3WA(0.75) H3WB(0.75)
3.a Riding coordinates:
 O1W(H1WA,H1WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O4W(H4WA,H4WB), O7W(H7WA,
 H7WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
3.b Ternary CH refined with riding coordinates:
 B1(H1A)
3.c Aromatic/amide H refined with riding coordinates:
 N11(H11), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Dy1 Dy 0.53245(3) 0.25306(2) 0.49529(2) 0.02910(10) Uani 1 d . . .
Fe1 Fe 0.42836(8) -0.13373(7) 0.83689(6) 0.02847(19) Uani 1 d . . .
O1 O 0.3019(4) 0.2659(4) 0.4947(4) 0.0517(11) Uani 1 d . . .
O1W O 0.4016(4) 0.3537(3) 0.6021(3) 0.0474(11) Uani 1 d . . .
H1WA H 0.4521 0.3533 0.6407 0.071 Uiso 1 d . . R
H1WB H 0.3489 0.3174 0.6443 0.071 Uiso 1 d . . R
O2 O 0.3564(5) 0.4153(4) 0.3701(3) 0.0526(12) Uani 1 d . . .
O3 O 0.1613(7) 0.4128(6) 0.3723(6) 0.129(3) Uani 1 d . . .
O4 O 0.5835(4) 0.4448(3) 0.3991(3) 0.0397(10) Uani 1 d . . .
O5 O 0.7036(4) 0.3054(3) 0.3513(3) 0.0448(10) Uani 1 d . . .
O6 O 0.7597(5) 0.4600(4) 0.2965(4) 0.0692(14) Uani 1 d . . .
N1 N 0.3895(5) -0.0822(4) 0.9543(3) 0.0335(11) Uani 1 d . . .
N2 N 0.4319(5) -0.1626(5) 1.0565(4) 0.0421(13) Uani 1 d . . .
N3 N 0.3832(5) -0.2772(4) 0.9401(4) 0.0419(13) Uani 1 d . . .
N4 N 0.4260(5) -0.3369(4) 1.0450(4) 0.0454(13) Uani 1 d . . .
N5 N 0.6121(5) -0.2260(4) 0.8858(4) 0.0341(11) Uani 1 d . . .
N6 N 0.6319(6) -0.2912(4) 0.9971(4) 0.0446(13) Uani 1 d . . .
N7 N 0.1440(6) 0.0062(6) 0.7601(5) 0.076(2) Uani 1 d . . .
N8 N 0.4942(5) 0.0883(4) 0.6637(4) 0.0341(11) Uani 1 d . . .
N9 N 0.4723(5) -0.1895(4) 0.6400(4) 0.0452(13) Uani 1 d . . .
N10 N 0.7428(5) 0.0593(4) 0.5407(3) 0.0340(11) Uani 1 d . . .
N11 N 0.8890(5) 0.1545(5) 0.6784(4) 0.0549(15) Uani 1 d . . .
H11 H 0.9652 0.1035 0.7038 0.066 Uiso 1 calc . . R
N12 N 0.6980(4) 0.2386(4) 0.5969(4) 0.0337(11) Uani 1 d . . .
N13 N 0.2688(7) 0.3660(6) 0.4108(5) 0.0653(17) Uani 1 d . . .
N14 N 0.6868(5) 0.4041(4) 0.3474(4) 0.0402(12) Uani 1 d . . .
C1 C 0.3242(6) 0.0231(6) 0.9574(5) 0.0475(16) Uani 1 d . . .
H1 H 0.2832 0.0945 0.8981 0.057 Uiso 1 calc . . R
C2 C 0.3269(7) 0.0096(7) 1.0620(6) 0.056(2) Uani 1 d . . .
H2 H 0.2893 0.0687 1.0866 0.067 Uiso 1 calc . . R
C3 C 0.3954(7) -0.1068(7) 1.1213(5) 0.056(2) Uani 1 d . . .
H3 H 0.4143 -0.1428 1.1954 0.068 Uiso 1 calc . . R
C4 C 0.3813(8) -0.4303(6) 1.1010(6) 0.065(2) Uani 1 d . . .
H4 H 0.3950 -0.4843 1.1749 0.078 Uiso 1 calc . . R
C5 C 0.3131(8) -0.4327(7) 1.0317(7) 0.076(3) Uani 1 d . . .
H5 H 0.2731 -0.4881 1.0481 0.091 Uiso 1 calc . . R
C6 C 0.3157(7) -0.3362(6) 0.9329(6) 0.0546(18) Uani 1 d . . .
H6 H 0.2762 -0.3147 0.8697 0.066 Uiso 1 calc . . R
C7 C 0.7614(7) -0.3440(6) 1.0119(6) 0.0606(19) Uani 1 d . . .
H7 H 0.8011 -0.3933 1.0798 0.073 Uiso 1 calc . . R
C8 C 0.8270(7) -0.3142(6) 0.9113(6) 0.0622(19) Uani 1 d . . .
H8 H 0.9181 -0.3383 0.8973 0.075 Uiso 1 calc . . R
C9 C 0.7306(6) -0.2420(5) 0.8362(5) 0.0441(15) Uani 1 d . . .
H9 H 0.7459 -0.2084 0.7602 0.053 Uiso 1 calc . . R
C10 C 0.2503(7) -0.0459(6) 0.7898(5) 0.0422(15) Uani 1 d . . .
C11 C 0.4709(5) 0.0066(5) 0.7310(4) 0.0307(13) Uani 1 d . . .
C12 C 0.4609(5) -0.1734(5) 0.7151(5) 0.0345(13) Uani 1 d . . .
C13 C 0.7634(6) -0.0310(5) 0.5144(5) 0.0409(15) Uani 1 d . . .
H13 H 0.7024 -0.0219 0.4711 0.049 Uiso 1 calc . . R
C14 C 0.8697(6) -0.1342(5) 0.5489(5) 0.0466(16) Uani 1 d . . .
H14 H 0.8796 -0.1943 0.5300 0.056 Uiso 1 calc . . R
C15 C 0.9616(7) -0.1495(6) 0.6109(5) 0.0541(17) Uani 1 d . . .
H15 H 1.0358 -0.2187 0.6332 0.065 Uiso 1 calc . . R
C16 C 0.9422(6) -0.0606(5) 0.6398(5) 0.0466(16) Uani 1 d . . .
H16 H 1.0019 -0.0697 0.6841 0.056 Uiso 1 calc . . R
C17 C 0.8337(6) 0.0423(5) 0.6027(4) 0.0348(13) Uani 1 d . . .
C18 C 0.8070(6) 0.1435(5) 0.6270(4) 0.0332(13) Uani 1 d . . .
C19 C 0.8252(7) 0.2651(6) 0.6820(6) 0.0585(19) Uani 1 d . . .
H19 H 0.8561 0.2975 0.7133 0.070 Uiso 1 calc . . R
C20 C 0.7096(6) 0.3152(5) 0.6309(5) 0.0430(15) Uani 1 d . . .
H20 H 0.6473 0.3900 0.6201 0.052 Uiso 1 calc . . R
B1 B 0.5101(8) -0.2916(7) 1.0770(6) 0.051(2) Uani 1 d . . .
H1A H 0.5360 -0.3423 1.1539 0.061 Uiso 1 calc . . R
O5W O -0.002(5) 0.248(5) 0.891(4) 0.144(18) Uiso 0.15 d A 1 .
H5WA H 0.0215 0.2374 0.9503 0.217 Uiso 0.15 d A 1 R
H5WB H -0.0133 0.3198 0.8425 0.217 Uiso 0.15 d A 1 R
O6W O 0.039(3) -0.141(3) 1.051(2) 0.123(10) Uiso 0.25 d B 2 .
H6WA H 0.1122 -0.1793 1.0827 0.185 Uiso 0.25 d B 2 R
H6WB H 0.0378 -0.1662 1.0057 0.185 Uiso 0.25 d B 2 R
O4W O -0.0158(16) 0.3816(16) 0.8170(14) 0.121(6) Uiso 0.40 d C 2 .
H4WA H -0.0559 0.4469 0.7538 0.181 Uiso 0.40 d C 2 R
H4WB H -0.0426 0.3204 0.8475 0.181 Uiso 0.40 d C 2 R
O7W O 1.023(2) -0.0562(17) 1.0210(17) 0.075(6) Uiso 0.25 d . 1 .
H7WA H 0.9564 -0.0577 1.0014 0.113 Uiso 0.25 d . 1 R
H7WB H 1.0913 -0.1140 1.0187 0.113 Uiso 0.25 d . 1 R
O2W O 0.129(4) 0.395(4) 0.632(3) 0.129(14) Uiso 0.20 d D 1 .
H2WA H 0.1633 0.3608 0.5895 0.194 Uiso 0.20 d D 1 R
H2WB H 0.0609 0.4568 0.6014 0.194 Uiso 0.20 d D 1 R
O3W O 0.1900(9) 0.2923(10) 0.7111(8) 0.127(4) Uani 0.75 d E 2 .
H3WA H 0.1244 0.3240 0.7445 0.190 Uiso 0.75 d E 2 R
H3WB H 0.1792 0.2705 0.6661 0.190 Uiso 0.75 d E 2 R


_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
Dy1 O1 2.478(4) . ?
Dy1 O1W 2.357(3) . ?
Dy1 O2 2.454(4) . ?
Dy1 O4 2.517(4) . ?
Dy1 O5 2.465(4) . ?
Dy1 N8 2.428(5) . ?
Dy1 N9 2.426(4) 2_656 ?
Dy1 N10 2.620(5) . ?
Dy1 N12 2.436(4) . ?
Dy1 N13 2.896(6) . ?
Dy1 N14 2.910(5) . ?
Fe1 N1 1.964(4) . ?
Fe1 N3 1.962(5) . ?
Fe1 N5 1.974(5) . ?
Fe1 C10 1.910(7) . ?
Fe1 C11 1.925(6) . ?
Fe1 C12 1.927(5) . ?
O1 N13 1.264(7) . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8497 . ?
O2 N13 1.267(7) . ?
O3 N13 1.202(7) . ?
O4 N14 1.277(6) . ?
O5 N14 1.249(5) . ?
O6 N14 1.199(6) . ?
N1 N2 1.346(6) . ?
N1 C1 1.336(7) . ?
N2 C3 1.337(7) . ?
N2 B1 1.520(9) . ?
N3 N4 1.362(6) . ?
N3 C6 1.335(6) . ?
N4 C4 1.352(7) . ?
N4 B1 1.525(8) . ?
N5 N6 1.373(6) . ?
N5 C9 1.321(7) . ?
N6 C7 1.329(8) . ?
N6 B1 1.539(9) . ?
N7 C10 1.147(7) . ?
N8 C11 1.135(6) . ?
N9 Dy1 2.426(4) 2_656 ?
N9 C12 1.133(6) . ?
N10 C13 1.362(6) . ?
N10 C17 1.342(7) . ?
N11 H11 0.8600 . ?
N11 C18 1.357(7) . ?
N11 C19 1.399(8) . ?
N12 C18 1.322(7) . ?
N12 C20 1.385(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.375(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.346(9) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.363(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.367(9) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.368(9) . ?
C8 H8 0.9300 . ?
C8 C9 1.360(8) . ?
C9 H9 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.362(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.361(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.370(8) . ?
C16 H16 0.9300 . ?
C16 C17 1.375(8) . ?
C17 C18 1.469(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.354(8) . ?
C20 H20 0.9300 . ?
B1 H1A 0.9800 . ?
O5W H5WA 0.8500 . ?
O5W H5WB 0.8501 . ?
O5W H4WB 0.8518 . ?
O6W H6WA 0.8499 . ?
O6W H6WB 0.8503 . ?
O4W H5WB 0.7270 . ?
O4W H4WA 0.9263 . ?
O4W H4WB 0.8695 . ?
O7W O7W 1.26(4) 2_757 ?
O7W H7WA 0.8501 . ?
O7W H7WB 0.8497 . ?
O2W H2WA 0.8515 . ?
O2W H2WB 0.8647 . ?
O2W H3WA 1.3819 . ?
O2W H3WB 1.4035 . ?
O3W H3WA 0.8467 . ?
O3W H3WB 0.8541 . ?

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 Dy1 O4 118.03(14) . . ?
O1 Dy1 N10 126.13(14) . . ?
O1 Dy1 N13 25.74(15) . . ?
O1 Dy1 N14 133.18(14) . . ?
O1W Dy1 O1 73.09(13) . . ?
O1W Dy1 O2 77.42(14) . . ?
O1W Dy1 O4 78.73(13) . . ?
O1W Dy1 O5 128.70(12) . . ?
O1W Dy1 N8 78.67(14) . . ?
O1W Dy1 N9 144.65(15) . 2_656 ?
O1W Dy1 N10 131.89(13) . . ?
O1W Dy1 N12 77.75(14) . . ?
O1W Dy1 N13 74.42(16) . . ?
O1W Dy1 N14 103.65(13) . . ?
O2 Dy1 O1 51.45(14) . . ?
O2 Dy1 O4 69.25(14) . . ?
O2 Dy1 O5 91.05(15) . . ?
O2 Dy1 N10 150.57(13) . . ?
O2 Dy1 N13 25.74(15) . . ?
O2 Dy1 N14 81.90(15) . . ?
O4 Dy1 N10 113.92(13) . . ?
O4 Dy1 N13 93.93(16) . . ?
O4 Dy1 N14 25.95(12) . . ?
O5 Dy1 O1 134.66(13) . . ?
O5 Dy1 O4 50.85(12) . . ?
O5 Dy1 N10 72.75(13) . . ?
O5 Dy1 N13 113.18(17) . . ?
O5 Dy1 N14 25.17(11) . . ?
N8 Dy1 O1 72.72(15) . . ?
N8 Dy1 O2 123.42(16) . . ?
N8 Dy1 O4 150.34(13) . . ?
N8 Dy1 O5 142.12(14) . . ?
N8 Dy1 N10 69.39(14) . . ?
N8 Dy1 N12 85.78(15) . . ?
N8 Dy1 N13 98.23(18) . . ?
N8 Dy1 N14 153.90(15) . . ?
N9 Dy1 O1 72.92(15) 2_656 . ?
N9 Dy1 O2 74.04(15) 2_656 . ?
N9 Dy1 O4 109.39(14) 2_656 . ?
N9 Dy1 O5 72.59(15) 2_656 . ?
N9 Dy1 N8 100.16(15) 2_656 . ?
N9 Dy1 N10 77.65(15) 2_656 . ?
N9 Dy1 N12 137.60(15) 2_656 . ?
N9 Dy1 N13 70.77(17) 2_656 . ?
N9 Dy1 N14 92.60(15) 2_656 . ?
N10 Dy1 N13 143.47(15) . . ?
N10 Dy1 N14 91.57(14) . . ?
N12 Dy1 O1 146.48(14) . . ?
N12 Dy1 O2 136.15(14) . . ?
N12 Dy1 O4 70.83(14) . . ?
N12 Dy1 O5 77.30(14) . . ?
N12 Dy1 N10 65.21(14) . . ?
N12 Dy1 N13 150.45(16) . . ?
N12 Dy1 N14 69.68(14) . . ?
N13 Dy1 N14 107.49(17) . . ?
N1 Fe1 N5 89.26(18) . . ?
N3 Fe1 N1 89.75(18) . . ?
N3 Fe1 N5 87.9(2) . . ?
C10 Fe1 N1 91.1(2) . . ?
C10 Fe1 N3 91.6(2) . . ?
C10 Fe1 N5 179.4(2) . . ?
C10 Fe1 C11 87.4(2) . . ?
C10 Fe1 C12 86.4(2) . . ?
C11 Fe1 N1 92.25(19) . . ?
C11 Fe1 N3 177.78(19) . . ?
C11 Fe1 N5 93.1(2) . . ?
C11 Fe1 C12 84.9(2) . . ?
C12 Fe1 N1 176.2(2) . . ?
C12 Fe1 N3 93.1(2) . . ?
C12 Fe1 N5 93.3(2) . . ?
N13 O1 Dy1 95.9(4) . . ?
Dy1 O1W H1WA 108.8 . . ?
Dy1 O1W H1WB 109.1 . . ?
H1WA O1W H1WB 109.4 . . ?
N13 O2 Dy1 97.0(4) . . ?
N14 O4 Dy1 94.5(3) . . ?
N14 O5 Dy1 97.7(3) . . ?
N2 N1 Fe1 119.8(3) . . ?
C1 N1 Fe1 133.3(4) . . ?
C1 N1 N2 106.9(4) . . ?
N1 N2 B1 118.2(4) . . ?
C3 N2 N1 109.0(5) . . ?
C3 N2 B1 132.8(6) . . ?
N4 N3 Fe1 118.6(3) . . ?
C6 N3 Fe1 134.5(4) . . ?
C6 N3 N4 106.9(5) . . ?
N3 N4 B1 118.9(5) . . ?
C4 N4 N3 108.1(5) . . ?
C4 N4 B1 133.0(6) . . ?
N6 N5 Fe1 118.1(4) . . ?
C9 N5 Fe1 135.4(4) . . ?
C9 N5 N6 106.5(5) . . ?
N5 N6 B1 118.5(5) . . ?
C7 N6 N5 108.3(5) . . ?
C7 N6 B1 133.2(5) . . ?
C11 N8 Dy1 168.7(4) . . ?
C12 N9 Dy1 167.0(5) . 2_656 ?
C13 N10 Dy1 125.6(4) . . ?
C17 N10 Dy1 117.7(3) . . ?
C17 N10 C13 116.5(5) . . ?
C18 N11 H11 126.8 . . ?
C18 N11 C19 106.5(5) . . ?
C19 N11 H11 126.8 . . ?
C18 N12 Dy1 120.4(3) . . ?
C18 N12 C20 106.0(4) . . ?
C20 N12 Dy1 133.6(4) . . ?
O1 N13 Dy1 58.3(3) . . ?
O1 N13 O2 115.5(6) . . ?
O2 N13 Dy1 57.2(3) . . ?
O3 N13 Dy1 177.7(6) . . ?
O3 N13 O1 122.8(7) . . ?
O3 N13 O2 121.7(7) . . ?
O4 N14 Dy1 59.6(3) . . ?
O5 N14 Dy1 57.1(3) . . ?
O5 N14 O4 115.8(5) . . ?
O6 N14 Dy1 172.4(4) . . ?
O6 N14 O4 121.1(5) . . ?
O6 N14 O5 123.1(5) . . ?
N1 C1 H1 125.3 . . ?
N1 C1 C2 109.4(6) . . ?
C2 C1 H1 125.3 . . ?
C1 C2 H2 127.2 . . ?
C3 C2 C1 105.7(5) . . ?
C3 C2 H2 127.2 . . ?
N2 C3 C2 109.0(6) . . ?
N2 C3 H3 125.5 . . ?
C2 C3 H3 125.5 . . ?
N4 C4 H4 125.5 . . ?
N4 C4 C5 109.1(6) . . ?
C5 C4 H4 125.5 . . ?
C4 C5 H5 127.3 . . ?
C4 C5 C6 105.4(6) . . ?
C6 C5 H5 127.3 . . ?
N3 C6 C5 110.5(6) . . ?
N3 C6 H6 124.7 . . ?
C5 C6 H6 124.7 . . ?
N6 C7 H7 125.5 . . ?
N6 C7 C8 109.1(6) . . ?
C8 C7 H7 125.5 . . ?
C7 C8 H8 127.4 . . ?
C9 C8 C7 105.2(6) . . ?
C9 C8 H8 127.4 . . ?
N5 C9 C8 110.9(6) . . ?
N5 C9 H9 124.6 . . ?
C8 C9 H9 124.6 . . ?
N7 C10 Fe1 178.8(5) . . ?
N8 C11 Fe1 175.8(4) . . ?
N9 C12 Fe1 175.0(5) . . ?
N10 C13 H13 118.7 . . ?
N10 C13 C14 122.5(6) . . ?
C14 C13 H13 118.7 . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.1(6) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 120.8 . . ?
C14 C15 C16 118.4(7) . . ?
C16 C15 H15 120.8 . . ?
C15 C16 H16 120.3 . . ?
C15 C16 C17 119.4(6) . . ?
C17 C16 H16 120.3 . . ?
N10 C17 C16 122.9(5) . . ?
N10 C17 C18 114.0(5) . . ?
C16 C17 C18 123.1(5) . . ?
N11 C18 C17 125.9(5) . . ?
N12 C18 N11 111.5(5) . . ?
N12 C18 C17 122.5(5) . . ?
N11 C19 H19 126.9 . . ?
C20 C19 N11 106.2(5) . . ?
C20 C19 H19 126.9 . . ?
N12 C20 H20 125.1 . . ?
C19 C20 N12 109.8(5) . . ?
C19 C20 H20 125.1 . . ?
N2 B1 N4 108.3(6) . . ?
N2 B1 N6 107.6(5) . . ?
N2 B1 H1A 111.4 . . ?
N4 B1 N6 106.5(5) . . ?
N4 B1 H1A 111.4 . . ?
N6 B1 H1A 111.4 . . ?
H5WA O5W H5WB 109.5 . . ?
H5WA O5W H4WB 114.9 . . ?
H5WB O5W H4WB 21.1 . . ?
H6WA O6W H6WB 109.5 . . ?
H5WB O4W H4WA 130.9 . . ?
H5WB O4W H4WB 20.1 . . ?
H4WA O4W H4WB 118.5 . . ?
O7W O7W H7WA 90.4 2_757 . ?
O7W O7W H7WB 142.0 2_757 . ?
H7WA O7W H7WB 109.5 . . ?
H2WA O2W H2WB 108.7 . . ?
H2WA O2W H3WA 118.8 . . ?
H2WA O2W H3WB 54.7 . . ?
H2WB O2W H3WA 119.4 . . ?
H2WB O2W H3WB 140.4 . . ?
H3WA O2W H3WB 64.2 . . ?
H3WA O3W H3WB 120.9 . . ?

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
Dy1 O1 N13 O2 -3.2(6) . . . . ?
Dy1 O1 N13 O3 177.7(7) . . . . ?
Dy1 O2 N13 O1 3.2(6) . . . . ?
Dy1 O2 N13 O3 -177.6(7) . . . . ?
Dy1 O4 N14 O5 10.7(5) . . . . ?
Dy1 O4 N14 O6 -171.2(5) . . . . ?
Dy1 O5 N14 O4 -11.0(5) . . . . ?
Dy1 O5 N14 O6 171.0(5) . . . . ?
Dy1 N8 C11 Fe1 0(10) . . . . ?
Dy1 N9 C12 Fe1 -95(6) 2_656 . . . ?
Dy1 N10 C13 C14 -174.1(4) . . . . ?
Dy1 N10 C17 C16 174.2(4) . . . . ?
Dy1 N10 C17 C18 -6.0(6) . . . . ?
Dy1 N12 C18 N11 177.4(3) . . . . ?
Dy1 N12 C18 C17 -0.7(7) . . . . ?
Dy1 N12 C20 C19 -177.7(4) . . . . ?
Fe1 N1 N2 C3 179.2(4) . . . . ?
Fe1 N1 N2 B1 0.4(7) . . . . ?
Fe1 N1 C1 C2 -179.7(4) . . . . ?
Fe1 N3 N4 C4 178.9(4) . . . . ?
Fe1 N3 N4 B1 -1.5(7) . . . . ?
Fe1 N3 C6 C5 -179.7(5) . . . . ?
Fe1 N5 N6 C7 -178.8(4) . . . . ?
Fe1 N5 N6 B1 1.8(6) . . . . ?
Fe1 N5 C9 C8 178.4(4) . . . . ?
O1 Dy1 O2 N13 -1.9(3) . . . . ?
O1 Dy1 O4 N14 -132.7(3) . . . . ?
O1 Dy1 O5 N14 99.1(3) . . . . ?
O1 Dy1 N8 C11 56(2) . . . . ?
O1 Dy1 N10 C13 35.5(5) . . . . ?
O1 Dy1 N10 C17 -138.9(4) . . . . ?
O1 Dy1 N12 C18 116.9(4) . . . . ?
O1 Dy1 N12 C20 -66.2(6) . . . . ?
O1 Dy1 N13 O2 176.6(6) . . . . ?
O1 Dy1 N13 O3 -120(14) . . . . ?
O1 Dy1 N14 O4 62.9(3) . . . . ?
O1 Dy1 N14 O5 -105.6(3) . . . . ?
O1 Dy1 N14 O6 160(3) . . . . ?
O1W Dy1 O1 N13 89.1(4) . . . . ?
O1W Dy1 O2 N13 -80.2(4) . . . . ?
O1W Dy1 O4 N14 163.6(3) . . . . ?
O1W Dy1 O5 N14 -6.4(4) . . . . ?
O1W Dy1 N8 C11 131(2) . . . . ?
O1W Dy1 N10 C13 135.3(4) . . . . ?
O1W Dy1 N10 C17 -39.0(4) . . . . ?
O1W Dy1 N12 C18 146.8(4) . . . . ?
O1W Dy1 N12 C20 -36.3(5) . . . . ?
O1W Dy1 N13 O1 -83.3(4) . . . . ?
O1W Dy1 N13 O2 93.3(4) . . . . ?
O1W Dy1 N13 O3 156(14) . . . . ?
O1W Dy1 N14 O4 -16.6(3) . . . . ?
O1W Dy1 N14 O5 174.9(3) . . . . ?
O1W Dy1 N14 O6 81(3) . . . . ?
O2 Dy1 O1 N13 1.9(3) . . . . ?
O2 Dy1 O4 N14 -115.7(3) . . . . ?
O2 Dy1 O5 N14 68.3(3) . . . . ?
O2 Dy1 N8 C11 65(2) . . . . ?
O2 Dy1 N10 C13 -38.5(6) . . . . ?
O2 Dy1 N10 C17 147.2(4) . . . . ?
O2 Dy1 N12 C18 -156.4(4) . . . . ?
O2 Dy1 N12 C20 20.5(6) . . . . ?
O2 Dy1 N13 O1 -176.6(6) . . . . ?
O2 Dy1 N13 O3 63(14) . . . . ?
O2 Dy1 N14 O4 58.3(3) . . . . ?
O2 Dy1 N14 O5 -110.3(3) . . . . ?
O2 Dy1 N14 O6 156(3) . . . . ?
O4 Dy1 O1 N13 22.3(4) . . . . ?
O4 Dy1 O2 N13 -162.7(4) . . . . ?
O4 Dy1 O5 N14 6.4(3) . . . . ?
O4 Dy1 N8 C11 172(2) . . . . ?
O4 Dy1 N10 C13 -128.3(4) . . . . ?
O4 Dy1 N10 C17 57.3(4) . . . . ?
O4 Dy1 N12 C18 -131.0(4) . . . . ?
O4 Dy1 N12 C20 45.9(5) . . . . ?
O4 Dy1 N13 O1 -160.4(3) . . . . ?
O4 Dy1 N13 O2 16.2(4) . . . . ?
O4 Dy1 N13 O3 79(14) . . . . ?
O4 Dy1 N14 O5 -168.6(5) . . . . ?
O4 Dy1 N14 O6 97(3) . . . . ?
O5 Dy1 O1 N13 -39.1(4) . . . . ?
O5 Dy1 O2 N13 150.3(4) . . . . ?
O5 Dy1 O4 N14 -6.2(3) . . . . ?
O5 Dy1 N8 C11 -87(2) . . . . ?
O5 Dy1 N10 C13 -97.7(4) . . . . ?
O5 Dy1 N10 C17 87.9(4) . . . . ?
O5 Dy1 N12 C18 -78.4(4) . . . . ?
O5 Dy1 N12 C20 98.5(5) . . . . ?
O5 Dy1 N13 O1 150.8(3) . . . . ?
O5 Dy1 N13 O2 -32.6(4) . . . . ?
O5 Dy1 N13 O3 30(14) . . . . ?
O5 Dy1 N14 O4 168.6(5) . . . . ?
O5 Dy1 N14 O6 -94(3) . . . . ?
N1 Fe1 N3 N4 -42.0(4) . . . . ?
N1 Fe1 N3 C6 138.2(6) . . . . ?
N1 Fe1 N5 N6 42.7(4) . . . . ?
N1 Fe1 N5 C9 -136.3(5) . . . . ?
N1 Fe1 C10 N7 178(100) . . . . ?
N1 Fe1 C11 N8 -156(7) . . . . ?
N1 Fe1 C12 N9 -24(8) . . . . ?
N1 N2 C3 C2 1.1(7) . . . . ?
N1 N2 B1 N4 -57.1(7) . . . . ?
N1 N2 B1 N6 57.7(7) . . . . ?
N1 C1 C2 C3 -0.2(7) . . . . ?
N2 N1 C1 C2 0.8(6) . . . . ?
N3 Fe1 N1 N2 43.1(4) . . . . ?
N3 Fe1 N1 C1 -136.3(5) . . . . ?
N3 Fe1 N5 N6 -47.1(4) . . . . ?
N3 Fe1 N5 C9 134.0(5) . . . . ?
N3 Fe1 C10 N7 -92(35) . . . . ?
N3 Fe1 C11 N8 -2(12) . . . . ?
N3 Fe1 C12 N9 115(6) . . . . ?
N3 N4 C4 C5 1.6(8) . . . . ?
N3 N4 B1 N2 58.0(7) . . . . ?
N3 N4 B1 N6 -57.5(7) . . . . ?
N4 N3 C6 C5 0.5(8) . . . . ?
N4 C4 C5 C6 -1.2(9) . . . . ?
N5 Fe1 N1 N2 -44.8(4) . . . . ?
N5 Fe1 N1 C1 135.8(5) . . . . ?
N5 Fe1 N3 N4 47.3(4) . . . . ?
N5 Fe1 N3 C6 -132.5(6) . . . . ?
N5 Fe1 C10 N7 -61(47) . . . . ?
N5 Fe1 C11 N8 114(7) . . . . ?
N5 Fe1 C12 N9 -157(6) . . . . ?
N5 N6 C7 C8 -0.1(7) . . . . ?
N5 N6 B1 N2 -58.9(6) . . . . ?
N5 N6 B1 N4 57.1(7) . . . . ?
N6 N5 C9 C8 -0.7(7) . . . . ?
N6 C7 C8 C9 -0.4(8) . . . . ?
N8 Dy1 O1 N13 172.2(4) . . . . ?
N8 Dy1 O2 N13 -13.0(4) . . . . ?
N8 Dy1 O4 N14 122.6(3) . . . . ?
N8 Dy1 O5 N14 -134.7(3) . . . . ?
N8 Dy1 N10 C13 83.6(4) . . . . ?
N8 Dy1 N10 C17 -90.7(4) . . . . ?
N8 Dy1 N12 C18 67.5(4) . . . . ?
N8 Dy1 N12 C20 -115.6(5) . . . . ?
N8 Dy1 N13 O1 -7.5(4) . . . . ?
N8 Dy1 N13 O2 169.0(4) . . . . ?
N8 Dy1 N13 O3 -128(14) . . . . ?
N8 Dy1 N14 O4 -108.6(4) . . . . ?
N8 Dy1 N14 O5 82.8(4) . . . . ?
N8 Dy1 N14 O6 -11(3) . . . . ?
N9 Dy1 O1 N13 -81.0(4) 2_656 . . . ?
N9 Dy1 O2 N13 78.7(4) 2_656 . . . ?
N9 Dy1 O4 N14 -52.2(3) 2_656 . . . ?
N9 Dy1 O5 N14 141.2(4) 2_656 . . . ?
N9 Dy1 N8 C11 -13(2) 2_656 . . . ?
N9 Dy1 N10 C13 -22.4(4) 2_656 . . . ?
N9 Dy1 N10 C17 163.3(4) 2_656 . . . ?
N9 Dy1 N12 C18 -32.9(5) 2_656 . . . ?
N9 Dy1 N12 C20 143.9(5) 2_656 . . . ?
N9 Dy1 N13 O1 90.4(4) 2_656 . . . ?
N9 Dy1 N13 O2 -93.0(4) 2_656 . . . ?
N9 Dy1 N13 O3 -30(14) 2_656 . . . ?
N9 Dy1 N14 O4 131.8(3) 2_656 . . . ?
N9 Dy1 N14 O5 -36.8(3) 2_656 . . . ?
N9 Dy1 N14 O6 -131(3) 2_656 . . . ?
N10 Dy1 O1 N13 -140.9(3) . . . . ?
N10 Dy1 O2 N13 95.1(5) . . . . ?
N10 Dy1 O4 N14 32.6(3) . . . . ?
N10 Dy1 O5 N14 -136.7(3) . . . . ?
N10 Dy1 N8 C11 -85(2) . . . . ?
N10 Dy1 N12 C18 -1.7(4) . . . . ?
N10 Dy1 N12 C20 175.2(5) . . . . ?
N10 Dy1 N13 O1 58.7(5) . . . . ?
N10 Dy1 N13 O2 -124.7(3) . . . . ?
N10 Dy1 N13 O3 -62(14) . . . . ?
N10 Dy1 N14 O4 -150.5(3) . . . . ?
N10 Dy1 N14 O5 40.9(3) . . . . ?
N10 Dy1 N14 O6 -53(3) . . . . ?
N10 C13 C14 C15 -0.9(9) . . . . ?
N10 C17 C18 N11 -173.2(5) . . . . ?
N10 C17 C18 N12 4.7(8) . . . . ?
N11 C19 C20 N12 1.0(7) . . . . ?
N12 Dy1 O1 N13 119.7(4) . . . . ?
N12 Dy1 O2 N13 -137.1(4) . . . . ?
N12 Dy1 O4 N14 82.8(3) . . . . ?
N12 Dy1 O5 N14 -69.1(3) . . . . ?
N12 Dy1 N8 C11 -150(2) . . . . ?
N12 Dy1 N10 C13 178.6(4) . . . . ?
N12 Dy1 N10 C17 4.2(4) . . . . ?
N12 Dy1 N13 O1 -103.5(4) . . . . ?
N12 Dy1 N13 O2 73.1(5) . . . . ?
N12 Dy1 N13 O3 136(14) . . . . ?
N12 Dy1 N14 O4 -87.7(3) . . . . ?
N12 Dy1 N14 O5 103.7(3) . . . . ?
N12 Dy1 N14 O6 10(3) . . . . ?
N13 Dy1 O4 N14 -123.2(3) . . . . ?
N13 Dy1 O5 N14 81.8(3) . . . . ?
N13 Dy1 N8 C11 59(2) . . . . ?
N13 Dy1 N10 C13 8.1(5) . . . . ?
N13 Dy1 N10 C17 -166.2(4) . . . . ?
N13 Dy1 N12 C18 166.8(4) . . . . ?
N13 Dy1 N12 C20 -16.4(7) . . . . ?
N13 Dy1 N14 O4 61.1(3) . . . . ?
N13 Dy1 N14 O5 -107.4(3) . . . . ?
N13 Dy1 N14 O6 158(3) . . . . ?
N14 Dy1 O1 N13 -3.9(4) . . . . ?
N14 Dy1 O2 N13 173.8(4) . . . . ?
N14 Dy1 N8 C11 -131(2) . . . . ?
N14 Dy1 N10 C13 -114.7(4) . . . . ?
N14 Dy1 N10 C17 71.0(4) . . . . ?
N14 Dy1 N12 C18 -103.4(4) . . . . ?
N14 Dy1 N12 C20 73.4(5) . . . . ?
N14 Dy1 N13 O1 177.0(3) . . . . ?
N14 Dy1 N13 O2 -6.4(4) . . . . ?
N14 Dy1 N13 O3 57(14) . . . . ?
C1 N1 N2 C3 -1.2(6) . . . . ?
C1 N1 N2 B1 180.0(5) . . . . ?
C1 C2 C3 N2 -0.6(7) . . . . ?
C3 N2 B1 N4 124.4(6) . . . . ?
C3 N2 B1 N6 -120.8(6) . . . . ?
C4 N4 B1 N2 -122.5(7) . . . . ?
C4 N4 B1 N6 122.0(7) . . . . ?
C4 C5 C6 N3 0.4(9) . . . . ?
C6 N3 N4 C4 -1.3(7) . . . . ?
C6 N3 N4 B1 178.3(6) . . . . ?
C7 N6 B1 N2 121.8(7) . . . . ?
C7 N6 B1 N4 -122.2(7) . . . . ?
C7 C8 C9 N5 0.7(7) . . . . ?
C9 N5 N6 C7 0.5(6) . . . . ?
C9 N5 N6 B1 -179.0(5) . . . . ?
C10 Fe1 N1 N2 134.7(4) . . . . ?
C10 Fe1 N1 C1 -44.7(6) . . . . ?
C10 Fe1 N3 N4 -133.0(4) . . . . ?
C10 Fe1 N3 C6 47.1(6) . . . . ?
C10 Fe1 N5 N6 -79(21) . . . . ?
C10 Fe1 N5 C9 102(21) . . . . ?
C10 Fe1 C11 N8 -65(7) . . . . ?
C10 Fe1 C12 N9 23(6) . . . . ?
C11 Fe1 N1 N2 -137.8(4) . . . . ?
C11 Fe1 N1 C1 42.7(6) . . . . ?
C11 Fe1 N3 N4 164(6) . . . . ?
C11 Fe1 N3 C6 -16(6) . . . . ?
C11 Fe1 N5 N6 134.9(4) . . . . ?
C11 Fe1 N5 C9 -44.0(5) . . . . ?
C11 Fe1 C10 N7 86(35) . . . . ?
C11 Fe1 C12 N9 -64(6) . . . . ?
C12 Fe1 N1 N2 -178(3) . . . . ?
C12 Fe1 N1 C1 3(3) . . . . ?
C12 Fe1 N3 N4 140.5(4) . . . . ?
C12 Fe1 N3 C6 -39.3(6) . . . . ?
C12 Fe1 N5 N6 -140.1(4) . . . . ?
C12 Fe1 N5 C9 41.0(5) . . . . ?
C12 Fe1 C10 N7 1(35) . . . . ?
C12 Fe1 C11 N8 21(7) . . . . ?
C13 N10 C17 C16 -0.6(8) . . . . ?
C13 N10 C17 C18 179.2(4) . . . . ?
C13 C14 C15 C16 1.8(10) . . . . ?
C14 C15 C16 C17 -2.0(9) . . . . ?
C15 C16 C17 N10 1.5(9) . . . . ?
C15 C16 C17 C18 -178.3(5) . . . . ?
C16 C17 C18 N11 6.6(9) . . . . ?
C16 C17 C18 N12 -175.5(5) . . . . ?
C17 N10 C13 C14 0.3(8) . . . . ?
C18 N11 C19 C20 -1.1(7) . . . . ?
C18 N12 C20 C19 -0.5(7) . . . . ?
C19 N11 C18 N12 0.8(7) . . . . ?
C19 N11 C18 C17 178.9(5) . . . . ?
C20 N12 C18 N11 -0.2(6) . . . . ?
C20 N12 C18 C17 -178.3(5) . . . . ?
B1 N2 C3 C2 179.7(6) . . . . ?
B1 N4 C4 C5 -177.9(7) . . . . ?
B1 N6 C7 C8 179.3(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.676
_oxdiff_exptl_absorpt_empirical_full_min 0.764
####################################################################### 
# 
# 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_shi_3471_divi
_database_code_depnum_ccdc_archive 'CCDC 1582396'
_audit_update_record             
;
2017-10-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;
_audit_creation_date             2017-10-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C40 H38 B2 Fe2 N28 O14 Tb2, 1.38(H4 O2)'
_chemical_formula_sum            'C40 H43.50 B2 Fe2 N28 O16.75 Tb2'
_chemical_formula_weight         1635.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N8 O6 Tb1 Fe1'
_chemical_oxdiff_usercomment     FeTbpyim
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'
B B 0.0013 0.0007 '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'
Tb Tb -0.1723 4.1537 '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'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   10.9953(14)
_cell_length_b                   13.5584(12)
_cell_length_c                   13.8383(16)
_cell_angle_alpha                61.283(10)
_cell_angle_beta                 77.182(10)
_cell_angle_gamma                66.269(10)
_cell_volume                     1655.2(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    607
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2040
_cell_measurement_theta_min      2.5710
_exptl_absorpt_coefficient_mu    2.620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12365
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.68
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  15.00   1.00   50.00    --   17.71 -57.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0575057000
_diffrn_orient_matrix_UB_12      0.0173811000
_diffrn_orient_matrix_UB_13      -0.0274441000
_diffrn_orient_matrix_UB_21      -0.0386828000
_diffrn_orient_matrix_UB_22      0.0278791000
_diffrn_orient_matrix_UB_23      0.0340901000
_diffrn_orient_matrix_UB_31      0.0099906000
_diffrn_orient_matrix_UB_32      0.0544484000
_diffrn_orient_matrix_UB_33      -0.0387434000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4639
_reflns_number_total             5753
_reflns_odcompleteness_completeness 24.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.399
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5753
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0551P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1194
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, {H5WA,H5WB} of O5W, All C(H) groups, All N(H) groups
 At 1.5 times of:
  {H4WA,H4WB} of O4W, {H2WA,H2WB} of O2W, {H3WA,H3WB} of O3W, {H6WA,H6WB} of
  O6W, {H1WA,H1WB} of O1W
2. Others
 Fixed Sof: O5W(0.125) H5WA(0.125) H5WB(0.125) O4W(0.25) H4WA(0.25) H4WB(0.25)
 O2W(0.5) H2WA(0.5) H2WB(0.5) O3W(0.25) H3WA(0.25) H3WB(0.25) O6W(0.25)
 H6WA(0.25) H6WB(0.25)
3.a Riding coordinates:
 O1W(H1WA,H1WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB), O2W(H2WA,H2WB), O3W(H3WA,
 H3WB), O6W(H6WA,H6WB)
3.b Ternary CH refined with riding coordinates:
 B1(H1A)
3.c Aromatic/amide H refined with riding coordinates:
 N11(H11), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Tb1 Tb -0.46854(3) -0.24673(3) -0.50465(2) 0.02957(13) Uani 1 d . . 1 . . .
Fe1 Fe -0.57171(10) -0.63382(8) -0.16290(7) 0.0285(2) Uani 1 d . . 1 . . .
O1 O -0.7007(6) -0.2342(5) -0.5051(5) 0.0545(15) Uani 1 d . . 1 . . .
O1W O -0.5993(5) -0.1466(4) -0.3962(4) 0.0492(14) Uani 1 d . . 1 . . .
H1WA H -0.5982 -0.1977 -0.3291 0.074 Uiso 1 d . . 1 R . .
H1WB H -0.5676 -0.0959 -0.4027 0.074 Uiso 1 d . . 1 R . .
O2 O -0.6445(6) -0.0842(5) -0.6311(4) 0.0557(15) Uani 1 d . . 1 . . .
O3 O -0.8413(8) -0.0881(8) -0.6282(8) 0.131(4) Uani 1 d . . 1 . . .
O4 O -0.4180(5) -0.0554(4) -0.6012(4) 0.0409(12) Uani 1 d . . 1 . . .
O5 O -0.2975(5) -0.1957(4) -0.6495(4) 0.0495(14) Uani 1 d . . 1 . . .
O6 O -0.2384(6) -0.0404(5) -0.7047(5) 0.0672(18) Uani 1 d . . 1 . . .
N1 N -0.6124(6) -0.5817(5) -0.0451(4) 0.0354(14) Uani 1 d . . 1 . . .
N2 N -0.5681(6) -0.6624(6) 0.0570(4) 0.0433(16) Uani 1 d . . 1 . . .
N3 N -0.6166(7) -0.7774(5) -0.0591(5) 0.0434(16) Uani 1 d . . 1 . . .
N4 N -0.5748(7) -0.8364(5) 0.0453(5) 0.0465(17) Uani 1 d . . 1 . . .
N5 N -0.3886(6) -0.7261(5) -0.1130(4) 0.0323(13) Uani 1 d . . 1 . . .
N6 N -0.3688(6) -0.7909(5) -0.0028(5) 0.0408(15) Uani 1 d . . 1 . . .
N7 N -0.8562(8) -0.4936(8) -0.2406(7) 0.073(2) Uani 1 d . . 1 . . .
N8 N -0.5061(6) -0.4121(5) -0.3361(5) 0.0394(15) Uani 1 d . . 1 . . .
N9 N -0.5261(7) -0.6891(6) -0.3602(5) 0.0478(16) Uani 1 d . . 1 . . .
N10 N -0.2554(6) -0.4413(5) -0.4594(4) 0.0353(14) Uani 1 d . . 1 . . .
N11 N -0.1120(6) -0.3453(6) -0.3221(6) 0.0521(17) Uani 1 d . . 1 . . .
H11 H -0.0361 -0.3972 -0.2958 0.062 Uiso 1 calc . . 1 R . .
N12 N -0.3009(6) -0.2621(5) -0.4030(5) 0.0353(14) Uani 1 d . . 1 . . .
N13 N -0.7317(8) -0.1325(7) -0.5883(7) 0.065(2) Uani 1 d . . 1 . . .
N14 N -0.3146(6) -0.0945(5) -0.6549(5) 0.0408(15) Uani 1 d . . 1 . . .
C1 C -0.6761(8) -0.4774(7) -0.0414(6) 0.0439(19) Uani 1 d . . 1 . . .
H1 H -0.7163 -0.4058 -0.1010 0.053 Uiso 1 calc . . 1 R . .
C2 C -0.6744(9) -0.4900(9) 0.0623(7) 0.058(2) Uani 1 d . . 1 . . .
H2 H -0.7124 -0.4302 0.0863 0.070 Uiso 1 calc . . 1 R . .
C3 C -0.6066(9) -0.6062(9) 0.1227(7) 0.059(3) Uani 1 d . . 1 . . .
H3 H -0.5892 -0.6419 0.1971 0.071 Uiso 1 calc . . 1 R . .
C4 C -0.6153(10) -0.9320(7) 0.1019(8) 0.067(3) Uani 1 d . . 1 . . .
H4 H -0.5974 -0.9885 0.1747 0.080 Uiso 1 calc . . 1 R . .
C5 C -0.6869(11) -0.9300(8) 0.0325(9) 0.076(3) Uani 1 d . . 1 . . .
H5 H -0.7293 -0.9838 0.0497 0.091 Uiso 1 calc . . 1 R . .
C6 C -0.6857(9) -0.8342(7) -0.0678(7) 0.059(2) Uani 1 d . . 1 . . .
H6 H -0.7260 -0.8127 -0.1308 0.071 Uiso 1 calc . . 1 R . .
C7 C -0.2391(9) -0.8437(7) 0.0105(8) 0.058(2) Uani 1 d . . 1 . . .
H7 H -0.1989 -0.8939 0.0782 0.070 Uiso 1 calc . . 1 R . .
C8 C -0.1728(9) -0.8140(8) -0.0891(8) 0.064(3) Uani 1 d . . 1 . . .
H8 H -0.0814 -0.8373 -0.1030 0.077 Uiso 1 calc . . 1 R . .
C9 C -0.2697(8) -0.7432(7) -0.1633(7) 0.047(2) Uani 1 d . . 1 . . .
H9 H -0.2549 -0.7109 -0.2394 0.056 Uiso 1 calc . . 1 R . .
C10 C -0.7504(8) -0.5459(7) -0.2109(6) 0.0437(19) Uani 1 d . . 1 . . .
C11 C -0.5291(7) -0.4945(6) -0.2692(5) 0.0313(16) Uani 1 d . . 1 . . .
C12 C -0.5391(7) -0.6732(6) -0.2841(6) 0.0344(16) Uani 1 d . . 1 . . .
C13 C -0.2366(8) -0.5313(6) -0.4846(6) 0.0403(18) Uani 1 d . . 1 . . .
H13 H -0.2988 -0.5225 -0.5267 0.048 Uiso 1 calc . . 1 R . .
C14 C -0.1279(8) -0.6359(7) -0.4497(7) 0.047(2) Uani 1 d . . 1 . . .
H14 H -0.1173 -0.6962 -0.4685 0.056 Uiso 1 calc . . 1 R . .
C15 C -0.0376(8) -0.6501(7) -0.3886(7) 0.054(2) Uani 1 d . . 1 . . .
H15 H 0.0368 -0.7197 -0.3662 0.064 Uiso 1 calc . . 1 R . .
C16 C -0.0553(8) -0.5619(7) -0.3593(7) 0.047(2) Uani 1 d . . 1 . . .
H16 H 0.0051 -0.5715 -0.3153 0.057 Uiso 1 calc . . 1 R . .
C17 C -0.1660(7) -0.4576(6) -0.3970(5) 0.0355(17) Uani 1 d . . 1 . . .
C18 C -0.1938(7) -0.3560(6) -0.3736(6) 0.0337(16) Uani 1 d . . 1 . . .
C19 C -0.1725(9) -0.2361(7) -0.3194(7) 0.055(2) Uani 1 d . . 1 . . .
H19 H -0.1399 -0.2037 -0.2893 0.066 Uiso 1 calc . . 1 R . .
C20 C -0.2889(8) -0.1856(7) -0.3691(6) 0.0437(19) Uani 1 d . . 1 . . .
H20 H -0.3515 -0.1109 -0.3792 0.052 Uiso 1 calc . . 1 R . .
B1 B -0.4904(10) -0.7921(8) 0.0771(6) 0.046(2) Uani 1 d . . 1 . . .
H1A H -0.4640 -0.8431 0.1539 0.055 Uiso 1 calc . . 1 R . .
O5W O -1.0000 -0.5000 0.0000 0.130(18) Uiso 0.25 d A 2 2 S T P
H5WA H -1.0192 -0.4510 -0.0649 0.156 Uiso 0.13 d A 2 1 R . .
H5WB H -0.9169 -0.5082 -0.0070 0.156 Uiso 0.13 d A 2 1 R . .
O4W O -0.985(2) -0.883(2) 0.185(2) 0.067(7) Uiso 0.25 d . . 1 . . .
H4WA H -0.9374 -0.9159 0.2404 0.101 Uiso 0.25 d . . 1 R . .
H4WB H -1.0062 -0.8073 0.1571 0.101 Uiso 0.25 d . . 1 R . .
O2W O -0.8016(13) -0.2185(12) -0.2827(11) 0.073(4) Uiso 0.50 d B 2 1 . . .
H2WA H -0.7930 -0.2081 -0.3501 0.109 Uiso 0.50 d B 2 1 R . .
H2WB H -0.8759 -0.1877 -0.2556 0.109 Uiso 0.50 d B 2 1 R . .
O3W O -0.868(3) -0.140(3) -0.335(2) 0.085(8) Uiso 0.25 d C 1 1 . . .
H3WA H -0.8838 -0.2019 -0.3222 0.128 Uiso 0.25 d C 1 1 R . .
H3WB H -0.8194 -0.1222 -0.3938 0.128 Uiso 0.25 d C 1 1 R . .
O6W O -0.957(3) -0.611(3) 0.036(3) 0.105(10) Uiso 0.25 d D 1 1 . . .
H6WA H -0.9198 -0.6820 0.0402 0.158 Uiso 0.25 d D 1 1 R . .
H6WB H -0.9396 -0.6104 0.0918 0.158 Uiso 0.25 d D 1 1 R . .


_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
Tb1 O1 2.491(5) . ?
Tb1 O1W 2.365(5) . ?
Tb1 O2 2.455(5) . ?
Tb1 O4 2.515(4) . ?
Tb1 O5 2.464(5) . ?
Tb1 N8 2.436(5) . ?
Tb1 N9 2.432(6) 2_444 ?
Tb1 N10 2.633(6) . ?
Tb1 N12 2.445(5) . ?
Fe1 N1 1.971(5) . ?
Fe1 N3 1.967(6) . ?
Fe1 N5 1.963(6) . ?
Fe1 C10 1.912(8) . ?
Fe1 C11 1.920(7) . ?
Fe1 C12 1.914(7) . ?
O1 N13 1.270(9) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2 N13 1.257(9) . ?
O3 N13 1.230(9) . ?
O4 N14 1.283(7) . ?
O5 N14 1.274(7) . ?
O6 N14 1.212(7) . ?
N1 N2 1.350(8) . ?
N1 C1 1.323(9) . ?
N2 C3 1.350(9) . ?
N2 B1 1.525(11) . ?
N3 N4 1.351(8) . ?
N3 C6 1.336(9) . ?
N4 C4 1.352(9) . ?
N4 B1 1.516(11) . ?
N5 N6 1.360(7) . ?
N5 C9 1.325(9) . ?
N6 C7 1.322(10) . ?
N6 B1 1.534(11) . ?
N7 C10 1.137(10) . ?
N8 C11 1.139(8) . ?
N9 Tb1 2.432(6) 2_444 ?
N9 C12 1.141(8) . ?
N10 C13 1.351(8) . ?
N10 C17 1.335(9) . ?
N11 H11 0.8600 . ?
N11 C18 1.353(9) . ?
N11 C19 1.373(10) . ?
N12 C18 1.297(8) . ?
N12 C20 1.386(8) . ?
C1 H1 0.9300 . ?
C1 C2 1.366(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.342(12) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.354(13) . ?
C5 H5 0.9300 . ?
C5 C6 1.373(12) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.360(12) . ?
C8 H8 0.9300 . ?
C8 C9 1.351(11) . ?
C9 H9 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.381(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.341(11) . ?
C15 H15 0.9300 . ?
C15 C16 1.369(11) . ?
C16 H16 0.9300 . ?
C16 C17 1.393(10) . ?
C17 C18 1.462(9) . ?
C19 H19 0.9300 . ?
C19 C20 1.346(10) . ?
C20 H20 0.9300 . ?
B1 H1A 0.9800 . ?
O5W H5WA 0.8310 . ?
O5W H5WB 0.8636 . ?
O4W H4WA 0.8503 . ?
O4W H4WB 0.8498 . ?
O2W H2WA 0.8624 . ?
O2W H2WB 0.8500 . ?
O3W H2WB 0.9776 . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8500 . ?
O6W H6WA 0.8502 . ?
O6W H6WB 0.8499 . ?

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 Tb1 O4 118.19(17) . . ?
O1 Tb1 N10 126.07(18) . . ?
O1W Tb1 O1 73.55(18) . . ?
O1W Tb1 O2 78.30(19) . . ?
O1W Tb1 O4 79.04(16) . . ?
O1W Tb1 O5 129.28(16) . . ?
O1W Tb1 N8 78.53(18) . . ?
O1W Tb1 N9 144.8(2) . 2_444 ?
O1W Tb1 N10 131.43(18) . . ?
O1W Tb1 N12 77.65(19) . . ?
O2 Tb1 O1 51.90(19) . . ?
O2 Tb1 O4 68.99(18) . . ?
O2 Tb1 O5 90.48(19) . . ?
O2 Tb1 N10 150.18(19) . . ?
O4 Tb1 N10 113.74(16) . . ?
O5 Tb1 O1 134.26(18) . . ?
O5 Tb1 O4 51.15(15) . . ?
O5 Tb1 N10 72.50(16) . . ?
N8 Tb1 O1 72.6(2) . . ?
N8 Tb1 O2 123.9(2) . . ?
N8 Tb1 O4 150.65(18) . . ?
N8 Tb1 O5 141.90(19) . . ?
N8 Tb1 N10 69.40(18) . . ?
N8 Tb1 N12 85.8(2) . . ?
N9 Tb1 O1 72.5(2) 2_444 . ?
N9 Tb1 O2 73.7(2) 2_444 . ?
N9 Tb1 O4 109.43(19) 2_444 . ?
N9 Tb1 O5 72.29(19) 2_444 . ?
N9 Tb1 N8 99.8(2) 2_444 . ?
N9 Tb1 N10 77.8(2) 2_444 . ?
N9 Tb1 N12 137.5(2) 2_444 . ?
N12 Tb1 O1 146.78(19) . . ?
N12 Tb1 O2 136.37(19) . . ?
N12 Tb1 O4 71.04(18) . . ?
N12 Tb1 O5 77.61(18) . . ?
N12 Tb1 N10 64.84(18) . . ?
N3 Fe1 N1 89.4(2) . . ?
N5 Fe1 N1 89.2(2) . . ?
N5 Fe1 N3 87.6(2) . . ?
C10 Fe1 N1 91.1(3) . . ?
C10 Fe1 N3 91.7(3) . . ?
C10 Fe1 N5 179.3(3) . . ?
C10 Fe1 C11 87.4(3) . . ?
C10 Fe1 C12 86.0(3) . . ?
C11 Fe1 N1 92.8(2) . . ?
C11 Fe1 N3 177.6(3) . . ?
C11 Fe1 N5 93.3(3) . . ?
C12 Fe1 N1 176.0(3) . . ?
C12 Fe1 N3 93.4(3) . . ?
C12 Fe1 N5 93.8(3) . . ?
C12 Fe1 C11 84.3(3) . . ?
N13 O1 Tb1 94.1(5) . . ?
Tb1 O1W H1WA 109.1 . . ?
Tb1 O1W H1WB 109.5 . . ?
H1WA O1W H1WB 109.5 . . ?
N13 O2 Tb1 96.1(5) . . ?
N14 O4 Tb1 95.4(4) . . ?
N14 O5 Tb1 98.0(4) . . ?
N2 N1 Fe1 119.4(5) . . ?
C1 N1 Fe1 133.9(5) . . ?
C1 N1 N2 106.7(6) . . ?
N1 N2 B1 118.1(6) . . ?
C3 N2 N1 108.7(7) . . ?
C3 N2 B1 133.2(7) . . ?
N4 N3 Fe1 119.0(4) . . ?
C6 N3 Fe1 133.3(6) . . ?
C6 N3 N4 107.7(6) . . ?
N3 N4 C4 109.3(7) . . ?
N3 N4 B1 118.7(6) . . ?
C4 N4 B1 131.9(7) . . ?
N6 N5 Fe1 118.5(5) . . ?
C9 N5 Fe1 134.6(5) . . ?
C9 N5 N6 106.9(6) . . ?
N5 N6 B1 118.7(6) . . ?
C7 N6 N5 107.5(6) . . ?
C7 N6 B1 133.7(7) . . ?
C11 N8 Tb1 168.3(5) . . ?
C12 N9 Tb1 165.9(6) . 2_444 ?
C13 N10 Tb1 124.9(5) . . ?
C17 N10 Tb1 117.1(4) . . ?
C17 N10 C13 117.6(6) . . ?
C18 N11 H11 126.3 . . ?
C18 N11 C19 107.3(6) . . ?
C19 N11 H11 126.3 . . ?
C18 N12 Tb1 120.3(4) . . ?
C18 N12 C20 106.1(6) . . ?
C20 N12 Tb1 133.5(5) . . ?
O2 N13 O1 117.9(7) . . ?
O3 N13 O1 119.8(9) . . ?
O3 N13 O2 122.2(9) . . ?
O5 N14 O4 114.4(6) . . ?
O6 N14 O4 122.4(6) . . ?
O6 N14 O5 123.1(7) . . ?
N1 C1 H1 124.9 . . ?
N1 C1 C2 110.3(7) . . ?
C2 C1 H1 124.9 . . ?
C1 C2 H2 127.0 . . ?
C3 C2 C1 106.0(7) . . ?
C3 C2 H2 127.0 . . ?
N2 C3 H3 125.8 . . ?
C2 C3 N2 108.4(7) . . ?
C2 C3 H3 125.8 . . ?
N4 C4 H4 126.5 . . ?
N4 C4 C5 107.0(8) . . ?
C5 C4 H4 126.5 . . ?
C4 C5 H5 126.1 . . ?
C4 C5 C6 107.8(8) . . ?
C6 C5 H5 126.1 . . ?
N3 C6 C5 108.2(9) . . ?
N3 C6 H6 125.9 . . ?
C5 C6 H6 125.9 . . ?
N6 C7 H7 124.9 . . ?
N6 C7 C8 110.3(8) . . ?
C8 C7 H7 124.9 . . ?
C7 C8 H8 127.8 . . ?
C9 C8 C7 104.5(8) . . ?
C9 C8 H8 127.8 . . ?
N5 C9 C8 110.8(7) . . ?
N5 C9 H9 124.6 . . ?
C8 C9 H9 124.6 . . ?
N7 C10 Fe1 179.2(7) . . ?
N8 C11 Fe1 176.7(6) . . ?
N9 C12 Fe1 175.3(7) . . ?
N10 C13 H13 119.0 . . ?
N10 C13 C14 122.0(7) . . ?
C14 C13 H13 119.0 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.7(7) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.8(8) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 120.7 . . ?
C15 C16 C17 118.5(8) . . ?
C17 C16 H16 120.7 . . ?
N10 C17 C16 122.4(7) . . ?
N10 C17 C18 114.1(6) . . ?
C16 C17 C18 123.6(7) . . ?
N11 C18 C17 125.5(7) . . ?
N12 C18 N11 111.1(6) . . ?
N12 C18 C17 123.4(6) . . ?
N11 C19 H19 127.0 . . ?
C20 C19 N11 106.0(6) . . ?
C20 C19 H19 127.0 . . ?
N12 C20 H20 125.3 . . ?
C19 C20 N12 109.5(7) . . ?
C19 C20 H20 125.3 . . ?
N2 B1 N6 106.7(6) . . ?
N2 B1 H1A 111.4 . . ?
N4 B1 N2 108.7(7) . . ?
N4 B1 N6 107.0(6) . . ?
N4 B1 H1A 111.4 . . ?
N6 B1 H1A 111.4 . . ?
H5WA O5W H5WB 96.9 . . ?
H5WA O5W H6WB 159.3 . . ?
H5WB O5W H6WB 75.2 . . ?
H4WA O4W H4WB 109.5 . . ?
H2WA O2W H2WB 121.6 . . ?
H2WA O2W H3WA 60.1 . . ?
H2WA O2W H3WB 40.1 . . ?
H2WB O2W H3WA 66.5 . . ?
H2WB O2W H3WB 96.7 . . ?
H3WA O2W H3WB 65.1 . . ?
H2WA O3W H2WB 96.3 . . ?
H2WA O3W H3WA 61.5 . . ?
H2WA O3W H3WB 61.1 . . ?
H2WB O3W H3WA 70.2 . . ?
H2WB O3W H3WB 150.1 . . ?
H3WA O3W H3WB 109.5 . . ?
H5WB O6W H6WA 135.0 . . ?
H5WB O6W H6WB 74.5 . . ?
H6WA O6W H6WB 109.5 . . ?

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
Tb1 O1 N13 O2 -0.6(8) . . . . ?
Tb1 O1 N13 O3 175.0(8) . . . . ?
Tb1 O2 N13 O1 0.6(8) . . . . ?
Tb1 O2 N13 O3 -174.8(9) . . . . ?
Tb1 O4 N14 O5 9.7(6) . . . . ?
Tb1 O4 N14 O6 -169.0(6) . . . . ?
Tb1 O5 N14 O4 -10.0(6) . . . . ?
Tb1 O5 N14 O6 168.7(6) . . . . ?
Tb1 N8 C11 Fe1 -9(15) . . . . ?
Tb1 N9 C12 Fe1 -103(7) 2_444 . . . ?
Tb1 N10 C13 C14 -174.0(5) . . . . ?
Tb1 N10 C17 C16 174.1(5) . . . . ?
Tb1 N10 C17 C18 -6.8(7) . . . . ?
Tb1 N12 C18 N11 177.8(4) . . . . ?
Tb1 N12 C18 C17 -0.7(8) . . . . ?
Tb1 N12 C20 C19 -177.2(5) . . . . ?
Fe1 N1 N2 C3 179.4(5) . . . . ?
Fe1 N1 N2 B1 -1.4(8) . . . . ?
Fe1 N1 C1 C2 -179.0(5) . . . . ?
Fe1 N3 N4 C4 -179.5(5) . . . . ?
Fe1 N3 N4 B1 -2.3(9) . . . . ?
Fe1 N3 C6 C5 -179.1(6) . . . . ?
Fe1 N5 N6 C7 -179.4(5) . . . . ?
Fe1 N5 N6 B1 1.9(8) . . . . ?
Fe1 N5 C9 C8 178.4(6) . . . . ?
O1 Tb1 O2 N13 -0.4(4) . . . . ?
O1 Tb1 O4 N14 -131.7(4) . . . . ?
O1 Tb1 O5 N14 99.5(4) . . . . ?
O1 Tb1 N8 C11 56(3) . . . . ?
O1 Tb1 N10 C13 34.2(6) . . . . ?
O1 Tb1 N10 C17 -138.4(4) . . . . ?
O1 Tb1 N12 C18 116.0(5) . . . . ?
O1 Tb1 N12 C20 -67.0(8) . . . . ?
O1W Tb1 O1 N13 88.2(5) . . . . ?
O1W Tb1 O2 N13 -78.5(5) . . . . ?
O1W Tb1 O4 N14 163.9(4) . . . . ?
O1W Tb1 O5 N14 -7.1(5) . . . . ?
O1W Tb1 N8 C11 132(3) . . . . ?
O1W Tb1 N10 C13 134.3(5) . . . . ?
O1W Tb1 N10 C17 -38.3(5) . . . . ?
O1W Tb1 N12 C18 146.3(5) . . . . ?
O1W Tb1 N12 C20 -36.7(6) . . . . ?
O2 Tb1 O1 N13 0.4(4) . . . . ?
O2 Tb1 O4 N14 -114.6(4) . . . . ?
O2 Tb1 O5 N14 68.1(4) . . . . ?
O2 Tb1 N8 C11 65(3) . . . . ?
O2 Tb1 N10 C13 -40.4(7) . . . . ?
O2 Tb1 N10 C17 146.9(5) . . . . ?
O2 Tb1 N12 C18 -155.7(4) . . . . ?
O2 Tb1 N12 C20 21.2(8) . . . . ?
O4 Tb1 O1 N13 20.8(5) . . . . ?
O4 Tb1 O2 N13 -161.1(5) . . . . ?
O4 Tb1 O5 N14 5.9(4) . . . . ?
O4 Tb1 N8 C11 173(3) . . . . ?
O4 Tb1 N10 C13 -129.3(5) . . . . ?
O4 Tb1 N10 C17 58.1(5) . . . . ?
O4 Tb1 N12 C18 -131.2(5) . . . . ?
O4 Tb1 N12 C20 45.8(6) . . . . ?
O5 Tb1 O1 N13 -41.1(5) . . . . ?
O5 Tb1 O2 N13 151.3(5) . . . . ?
O5 Tb1 O4 N14 -5.9(4) . . . . ?
O5 Tb1 N8 C11 -86(3) . . . . ?
O5 Tb1 N10 C13 -98.3(5) . . . . ?
O5 Tb1 N10 C17 89.1(5) . . . . ?
O5 Tb1 N12 C18 -78.3(5) . . . . ?
O5 Tb1 N12 C20 98.6(6) . . . . ?
N1 Fe1 N3 N4 -42.0(6) . . . . ?
N1 Fe1 N3 C6 137.1(8) . . . . ?
N1 Fe1 N5 N6 42.9(5) . . . . ?
N1 Fe1 N5 C9 -137.6(7) . . . . ?
N1 Fe1 C10 N7 162(60) . . . . ?
N1 Fe1 C11 N8 -147(12) . . . . ?
N1 Fe1 C12 N9 -11(10) . . . . ?
N1 N2 C3 C2 -0.4(9) . . . . ?
N1 N2 B1 N4 -56.2(8) . . . . ?
N1 N2 B1 N6 58.9(8) . . . . ?
N1 C1 C2 C3 0.3(9) . . . . ?
N2 N1 C1 C2 -0.5(8) . . . . ?
N3 Fe1 N1 N2 44.0(5) . . . . ?
N3 Fe1 N1 C1 -137.7(7) . . . . ?
N3 Fe1 N5 N6 -46.6(5) . . . . ?
N3 Fe1 N5 C9 132.9(7) . . . . ?
N3 Fe1 C10 N7 -108(60) . . . . ?
N3 Fe1 C11 N8 11(17) . . . . ?
N3 Fe1 C12 N9 124(8) . . . . ?
N3 N4 C4 C5 -2.0(10) . . . . ?
N3 N4 B1 N2 58.6(9) . . . . ?
N3 N4 B1 N6 -56.4(9) . . . . ?
N4 N3 C6 C5 0.0(10) . . . . ?
N4 C4 C5 C6 1.9(12) . . . . ?
N5 Fe1 N1 N2 -43.7(5) . . . . ?
N5 Fe1 N1 C1 134.7(7) . . . . ?
N5 Fe1 N3 N4 47.3(5) . . . . ?
N5 Fe1 N3 C6 -133.7(8) . . . . ?
N5 Fe1 C10 N7 -87(68) . . . . ?
N5 Fe1 C11 N8 123(12) . . . . ?
N5 Fe1 C12 N9 -148(8) . . . . ?
N5 N6 C7 C8 0.5(9) . . . . ?
N5 N6 B1 N2 -59.6(8) . . . . ?
N5 N6 B1 N4 56.7(8) . . . . ?
N6 N5 C9 C8 -2.1(9) . . . . ?
N6 C7 C8 C9 -1.7(10) . . . . ?
N8 Tb1 O1 N13 171.1(5) . . . . ?
N8 Tb1 O2 N13 -11.1(5) . . . . ?
N8 Tb1 O4 N14 123.1(5) . . . . ?
N8 Tb1 O5 N14 -135.9(4) . . . . ?
N8 Tb1 N10 C13 82.3(5) . . . . ?
N8 Tb1 N10 C17 -90.3(5) . . . . ?
N8 Tb1 N12 C18 67.1(5) . . . . ?
N8 Tb1 N12 C20 -115.9(6) . . . . ?
N9 Tb1 O1 N13 -82.4(5) 2_444 . . . ?
N9 Tb1 O2 N13 80.0(5) 2_444 . . . ?
N9 Tb1 O4 N14 -51.6(4) 2_444 . . . ?
N9 Tb1 O5 N14 140.8(4) 2_444 . . . ?
N9 Tb1 N8 C11 -12(3) 2_444 . . . ?
N9 Tb1 N10 C13 -23.2(5) 2_444 . . . ?
N9 Tb1 N10 C17 164.1(5) 2_444 . . . ?
N9 Tb1 N12 C18 -32.8(6) 2_444 . . . ?
N9 Tb1 N12 C20 144.1(6) 2_444 . . . ?
N10 Tb1 O1 N13 -142.1(4) . . . . ?
N10 Tb1 O2 N13 97.5(6) . . . . ?
N10 Tb1 O4 N14 33.3(4) . . . . ?
N10 Tb1 O5 N14 -136.8(4) . . . . ?
N10 Tb1 N8 C11 -85(3) . . . . ?
N10 Tb1 N12 C18 -2.0(5) . . . . ?
N10 Tb1 N12 C20 174.9(7) . . . . ?
N10 C13 C14 C15 0.3(11) . . . . ?
N10 C17 C18 N11 -172.9(6) . . . . ?
N10 C17 C18 N12 5.3(9) . . . . ?
N11 C19 C20 N12 -0.2(9) . . . . ?
N12 Tb1 O1 N13 119.1(5) . . . . ?
N12 Tb1 O2 N13 -136.3(5) . . . . ?
N12 Tb1 O4 N14 83.3(4) . . . . ?
N12 Tb1 O5 N14 -69.6(4) . . . . ?
N12 Tb1 N8 C11 -149(3) . . . . ?
N12 Tb1 N10 C13 177.5(6) . . . . ?
N12 Tb1 N10 C17 4.9(4) . . . . ?
C1 N1 N2 C3 0.6(8) . . . . ?
C1 N1 N2 B1 179.8(6) . . . . ?
C1 C2 C3 N2 0.1(9) . . . . ?
C3 N2 B1 N4 122.9(8) . . . . ?
C3 N2 B1 N6 -122.0(8) . . . . ?
C4 N4 B1 N2 -124.9(9) . . . . ?
C4 N4 B1 N6 120.2(9) . . . . ?
C4 C5 C6 N3 -1.2(12) . . . . ?
C6 N3 N4 C4 1.2(9) . . . . ?
C6 N3 N4 B1 178.5(7) . . . . ?
C7 N6 B1 N2 122.2(9) . . . . ?
C7 N6 B1 N4 -121.5(9) . . . . ?
C7 C8 C9 N5 2.3(10) . . . . ?
C9 N5 N6 C7 0.9(8) . . . . ?
C9 N5 N6 B1 -177.7(6) . . . . ?
C10 Fe1 N1 N2 135.7(5) . . . . ?
C10 Fe1 N1 C1 -46.0(7) . . . . ?
C10 Fe1 N3 N4 -133.0(6) . . . . ?
C10 Fe1 N3 C6 46.0(8) . . . . ?
C10 Fe1 N5 N6 -68(22) . . . . ?
C10 Fe1 N5 C9 111(21) . . . . ?
C10 Fe1 C11 N8 -57(12) . . . . ?
C10 Fe1 C12 N9 32(8) . . . . ?
C11 Fe1 N1 N2 -136.9(5) . . . . ?
C11 Fe1 N1 C1 41.5(7) . . . . ?
C11 Fe1 N3 N4 159(7) . . . . ?
C11 Fe1 N3 C6 -22(8) . . . . ?
C11 Fe1 N5 N6 135.6(5) . . . . ?
C11 Fe1 N5 C9 -44.9(7) . . . . ?
C11 Fe1 C10 N7 70(60) . . . . ?
C11 Fe1 C12 N9 -55(8) . . . . ?
C12 Fe1 N1 N2 179(100) . . . . ?
C12 Fe1 N1 C1 -3(4) . . . . ?
C12 Fe1 N3 N4 140.9(6) . . . . ?
C12 Fe1 N3 C6 -40.1(8) . . . . ?
C12 Fe1 N5 N6 -139.9(5) . . . . ?
C12 Fe1 N5 C9 39.7(7) . . . . ?
C12 Fe1 C10 N7 -15(60) . . . . ?
C12 Fe1 C11 N8 30(12) . . . . ?
C13 N10 C17 C16 0.9(9) . . . . ?
C13 N10 C17 C18 -180.0(6) . . . . ?
C13 C14 C15 C16 1.4(11) . . . . ?
C14 C15 C16 C17 -1.8(11) . . . . ?
C15 C16 C17 N10 0.7(10) . . . . ?
C15 C16 C17 C18 -178.4(7) . . . . ?
C16 C17 C18 N11 6.2(11) . . . . ?
C16 C17 C18 N12 -175.6(6) . . . . ?
C17 N10 C13 C14 -1.4(10) . . . . ?
C18 N11 C19 C20 0.2(9) . . . . ?
C18 N12 C20 C19 0.1(9) . . . . ?
C19 N11 C18 N12 -0.2(8) . . . . ?
C19 N11 C18 C17 178.2(7) . . . . ?
C20 N12 C18 N11 0.1(8) . . . . ?
C20 N12 C18 C17 -178.4(6) . . . . ?
B1 N2 C3 C2 -179.5(8) . . . . ?
B1 N4 C4 C5 -178.7(9) . . . . ?
B1 N6 C7 C8 178.9(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.968
_oxdiff_exptl_absorpt_empirical_full_min 0.659
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1582397'
_audit_update_record             
;
2017-10-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;
_audit_creation_date             2017-10-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C40 H38 B2 Fe2 Gd2 N28 O14, 6(H2 O)'
_chemical_formula_sum            'C40 H50 B2 Fe2 Gd2 N28 O20'
_chemical_formula_weight         1690.90
_chemical_melting_point          ?
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'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1650 3.9040 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   10.9350(10)
_cell_length_b                   13.5290(12)
_cell_length_c                   13.8570(12)
_cell_angle_alpha                61.132(5)
_cell_angle_beta                 77.180(5)
_cell_angle_gamma                67.107(4)
_cell_volume                     1652.4(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3875
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      2.75
_cell_measurement_theta_min      25.10
_exptl_absorpt_coefficient_mu    2.498
_exptl_absorpt_correction_T_max  0.8251
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_av_unetI/netI     0.1410
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10584
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         1.85
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4105
_reflns_number_total             5400
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.861
_refine_diff_density_min         -2.116
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         5400
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0892
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0999P)²+30.3923P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2086
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O5W(0.6) H5WA(0.6) H5WB(0.6) O4W(0.5) H4WA(0.5) H4WB(0.5) O3W(0.5)
 H3WA(0.5) H3WB(0.5) O6W(0.4) H6WA(0.4) H6WB(0.4)
4.a Riding coordinates:
 O1W(H1WB,H1WA), O5W(H5WA,H5WB), O4W(H4WA,H4WB), O2W(H2WA,H2WB), O3W(H3WA,
 H3WB), O6W(H6WA,H6WB)
4.b Ternary CH refined with riding coordinates:
 B1(H1A)
4.c Aromatic/amide H refined with riding coordinates:
 N11(H11), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Gd1 Gd 0.53326(8) 0.25345(6) -0.00530(6) 0.0202(2) Uani 1 d . . . .
Fe1 Fe 0.4316(2) -0.13739(17) 0.34078(16) 0.0260(5) Uani 1 d . . . .
O1 O 0.3007(11) 0.2593(9) 0.0044(8) 0.036(3) Uani 1 d . . . .
O1W O 0.4088(11) 0.3491(9) 0.1056(8) 0.034(3) Uani 1 d . . . .
H1WB H 0.3417 0.3319 0.1459 0.051 Uiso 1 d . . R .
H1WA H 0.3949 0.4253 0.0693 0.051 Uiso 1 d . . R .
O2 O 0.3502(12) 0.4122(9) -0.1267(9) 0.041(3) Uani 1 d . . . .
O3 O 0.1510(15) 0.4008(12) -0.1130(14) 0.082(5) Uani 1 d . . . .
O4 O 0.5817(11) 0.4470(8) -0.1049(8) 0.032(2) Uani 1 d . . . .
O5 O 0.7021(11) 0.3093(8) -0.1543(8) 0.037(3) Uani 1 d . . . .
O6 O 0.7625(12) 0.4632(10) -0.2050(10) 0.050(3) Uani 1 d . . . .
N1 N 0.3916(13) -0.0877(10) 0.4586(10) 0.031(3) Uani 1 d . . . .
N2 N 0.4320(13) -0.1682(11) 0.5621(10) 0.034(3) Uani 1 d . . . .
N3 N 0.3853(13) -0.2823(10) 0.4431(9) 0.031(3) Uani 1 d . . . .
N4 N 0.4289(13) -0.3431(11) 0.5472(10) 0.033(3) Uani 1 d . . . .
N5 N 0.6150(13) -0.2308(10) 0.3913(9) 0.026(3) Uani 1 d . . . .
N6 N 0.6363(13) -0.2946(11) 0.5026(9) 0.030(3) Uani 1 d . . . .
N7 N 0.1468(15) 0.0030(14) 0.2606(12) 0.048(4) Uani 1 d . . . .
N8 N 0.4971(12) 0.0873(11) 0.1674(10) 0.031(3) Uani 1 d . . . .
N9 N 0.4745(14) -0.1900(11) 0.1413(10) 0.037(3) Uani 1 d . . . .
N10 N 0.7449(12) 0.0607(10) 0.0376(9) 0.028(3) Uani 1 d . . . .
N11 N 0.8927(13) 0.1555(12) 0.1768(11) 0.039(3) Uani 1 d . . . .
H11 H 0.9666 0.1023 0.2049 0.046 Uiso 1 calc . . R .
N12 N 0.7049(12) 0.2430(10) 0.0923(9) 0.025(3) Uani 1 d . . . .
N13 N 0.2623(16) 0.3608(12) -0.0809(12) 0.044(4) Uani 1 d . . . .
N14 N 0.6860(13) 0.4079(10) -0.1563(10) 0.029(3) Uani 1 d . . . .
C1 C 0.3267(15) 0.0212(13) 0.4598(13) 0.032(4) Uani 1 d . . . .
H1 H 0.2876 0.0927 0.4002 0.039 Uiso 1 calc . . R .
C2 C 0.3297(17) 0.0055(16) 0.5662(15) 0.043(4) Uani 1 d . . . .
H2 H 0.2938 0.0646 0.5906 0.052 Uiso 1 calc . . R .
C3 C 0.3959(18) -0.1141(15) 0.6288(13) 0.041(4) Uani 1 d . . . U
H3 H 0.4125 -0.1506 0.7034 0.049 Uiso 1 calc . . R .
C4 C 0.384(2) -0.4394(15) 0.6029(15) 0.051(5) Uani 1 d . . . .
H4 H 0.3973 -0.4943 0.6766 0.061 Uiso 1 calc . . R .
C5 C 0.3172(19) -0.4405(15) 0.5316(14) 0.047(5) Uani 1 d . . . .
H5 H 0.2778 -0.4964 0.5460 0.057 Uiso 1 calc . . R .
C6 C 0.3201(15) -0.3395(12) 0.4317(13) 0.030(4) Uani 1 d . . . .
H6 H 0.2818 -0.3166 0.3674 0.036 Uiso 1 calc . . R .
C7 C 0.7669(18) -0.3448(15) 0.5168(13) 0.042(4) Uani 1 d . . . .
H7 H 0.8066 -0.3933 0.5846 0.050 Uiso 1 calc . . R .
C8 C 0.8321(18) -0.3146(15) 0.4182(13) 0.044(4) Uani 1 d . . . .
H8 H 0.9236 -0.3377 0.4039 0.052 Uiso 1 calc . . R .
C9 C 0.7343(18) -0.2422(14) 0.3427(13) 0.038(4) Uani 1 d . . . .
H9 H 0.7504 -0.2058 0.2668 0.046 Uiso 1 calc . . R .
C10 C 0.2520(17) -0.0486(13) 0.2899(12) 0.029(3) Uani 1 d . . . .
C11 C 0.4774(16) 0.0020(13) 0.2370(11) 0.029(3) Uani 1 d . . . .
C12 C 0.4649(15) -0.1758(12) 0.2197(12) 0.027(3) Uani 1 d . . . .
C13 C 0.7660(16) -0.0301(13) 0.0146(13) 0.034(4) Uani 1 d . . . .
H13 H 0.7036 -0.0219 -0.0271 0.041 Uiso 1 calc . . R .
C14 C 0.8708(16) -0.1330(14) 0.0471(12) 0.034(4) Uani 1 d . . . .
H14 H 0.8804 -0.1910 0.0254 0.040 Uiso 1 calc . . R .
C15 C 0.9649(16) -0.1513(14) 0.1138(13) 0.039(4) Uani 1 d . . . .
H15 H 1.0375 -0.2211 0.1382 0.047 Uiso 1 calc . . R .
C16 C 0.9437(15) -0.0591(13) 0.1416(14) 0.038(4) Uani 1 d . . . .
H16 H 1.0018 -0.0668 0.1866 0.046 Uiso 1 calc . . R .
C17 C 0.8356(15) 0.0436(12) 0.1013(10) 0.026(3) Uani 1 d . . . .
C18 C 0.8113(15) 0.1459(12) 0.1228(11) 0.026(3) Uani 1 d . . . .
C19 C 0.8364(16) 0.2656(14) 0.1788(14) 0.040(4) Uani 1 d . . . .
H19 H 0.8697 0.2972 0.2097 0.048 Uiso 1 calc . . R .
C20 C 0.7195(16) 0.3180(14) 0.1242(11) 0.031(4) Uani 1 d . . . .
H20 H 0.6595 0.3938 0.1113 0.037 Uiso 1 calc . . R .
B1 B 0.5094(18) -0.2961(15) 0.5826(15) 0.033(4) Uani 1 d . . . .
H1A H 0.5333 -0.3470 0.6599 0.040 Uiso 1 calc . . R .
O5W O 0.025(2) -0.0633(19) 0.5230(18) 0.063(6) Uiso 0.60 d A 2 . .
H5WA H 0.0279 -0.1116 0.5912 0.094 Uiso 0.60 d A 2 R .
H5WB H 0.0506 -0.1023 0.4850 0.094 Uiso 0.60 d A 2 R .
O4W O -0.043(4) 0.381(4) 0.298(3) 0.092(13) Uiso 0.50 d B 2 . .
H4WA H -0.0618 0.4563 0.2614 0.138 Uiso 0.50 d B 2 R .
H4WB H -0.0393 0.3680 0.3644 0.138 Uiso 0.50 d B 2 R .
O2W O 0.2056(15) 0.2743(12) 0.2265(11) 0.070(4) Uani 1 d . . . .
H2WA H 0.1309 0.3297 0.2173 0.105 Uiso 1 d . . R .
H2WB H 0.1977 0.2110 0.2336 0.105 Uiso 1 d . . R .
O3W O -0.005(4) 0.398(3) 0.310(3) 0.075(10) Uiso 0.50 d C 1 . .
H3WA H -0.0652 0.4548 0.2669 0.113 Uiso 0.50 d C 1 R .
H3WB H 0.0114 0.4274 0.3458 0.113 Uiso 0.50 d C 1 R .
O6W O 0.052(4) -0.162(4) 0.555(3) 0.081(11) Uiso 0.40 d D 1 . .
H6WA H 0.0554 -0.2106 0.6233 0.121 Uiso 0.40 d D 1 R .
H6WB H 0.0781 -0.2012 0.5171 0.121 Uiso 0.40 d D 1 R .


_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
Gd1 O1 2.489(10) . ?
Gd1 O1W 2.347(9) . ?
Gd1 O2 2.472(11) . ?
Gd1 O4 2.512(9) . ?
Gd1 O5 2.476(11) . ?
Gd1 N8 2.452(13) . ?
Gd1 N9 2.446(13) 2_655 ?
Gd1 N10 2.632(12) . ?
Gd1 N12 2.471(12) . ?
Gd1 N13 2.923(15) . ?
Gd1 N14 2.911(12) . ?
Fe1 N1 1.955(12) . ?
Fe1 N3 1.970(11) . ?
Fe1 N5 1.976(13) . ?
Fe1 C10 1.939(17) . ?
Fe1 C11 1.916(14) . ?
Fe1 C12 1.908(15) . ?
O1 N13 1.289(16) . ?
O1W H1WB 0.8544 . ?
O1W H1WA 0.8668 . ?
O2 N13 1.278(18) . ?
O3 N13 1.211(18) . ?
O4 N14 1.274(15) . ?
O5 N14 1.263(14) . ?
O6 N14 1.210(15) . ?
N1 N2 1.356(17) . ?
N1 C1 1.371(18) . ?
N2 C3 1.346(19) . ?
N2 B1 1.51(2) . ?
N3 N4 1.356(16) . ?
N3 C6 1.315(18) . ?
N4 C4 1.375(19) . ?
N4 B1 1.53(2) . ?
N5 N6 1.376(16) . ?
N5 C9 1.32(2) . ?
N6 C7 1.33(2) . ?
N6 B1 1.57(2) . ?
N7 C10 1.133(19) . ?
N8 C11 1.155(17) . ?
N9 Gd1 2.446(13) 2_655 ?
N9 C12 1.168(18) . ?
N10 C13 1.338(18) . ?
N10 C17 1.352(18) . ?
N11 H11 0.8600 . ?
N11 C18 1.361(18) . ?
N11 C19 1.384(19) . ?
N12 C18 1.323(18) . ?
N12 C20 1.358(17) . ?
C1 H1 0.9300 . ?
C1 C2 1.39(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.38(2) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.36(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.40(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.34(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.37(2) . ?
C9 H9 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.36(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.41(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.40(2) . ?
C16 H16 0.9300 . ?
C16 C17 1.38(2) . ?
C17 C18 1.466(18) . ?
C19 H19 0.9300 . ?
C19 C20 1.38(2) . ?
C20 H20 0.9300 . ?
B1 H1A 0.9800 . ?
O5W H5WA 0.8499 . ?
O5W H5WB 0.8500 . ?
O4W H4WA 0.8498 . ?
O4W H4WB 0.8499 . ?
O4W H3WA 0.8259 . ?
O2W H2WA 0.8499 . ?
O2W H2WB 0.8516 . ?
O3W H4WA 0.8717 . ?
O3W H4WB 0.7494 . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8502 . ?
O6W H5WA 0.9573 . ?
O6W H5WB 0.9156 . ?
O6W H6WA 0.8498 . ?
O6W H6WB 0.8501 . ?

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 Gd1 O4 118.6(3) . . ?
O1 Gd1 N10 125.2(3) . . ?
O1 Gd1 N13 26.0(4) . . ?
O1 Gd1 N14 134.7(3) . . ?
O1W Gd1 O1 73.3(3) . . ?
O1W Gd1 O2 78.7(4) . . ?
O1W Gd1 O4 79.2(3) . . ?
O1W Gd1 O5 129.0(3) . . ?
O1W Gd1 N8 77.3(4) . . ?
O1W Gd1 N9 145.9(4) . 2_655 ?
O1W Gd1 N10 130.6(3) . . ?
O1W Gd1 N12 76.7(4) . . ?
O1W Gd1 N13 75.0(4) . . ?
O1W Gd1 N14 103.6(3) . . ?
O2 Gd1 O1 51.7(3) . . ?
O2 Gd1 O4 69.8(3) . . ?
O2 Gd1 O5 91.6(4) . . ?
O2 Gd1 N10 150.5(4) . . ?
O2 Gd1 N13 25.7(4) . . ?
O2 Gd1 N14 83.0(4) . . ?
O4 Gd1 N10 114.6(3) . . ?
O4 Gd1 N13 94.3(4) . . ?
O4 Gd1 N14 25.8(3) . . ?
O5 Gd1 O1 135.7(3) . . ?
O5 Gd1 O4 50.9(3) . . ?
O5 Gd1 N10 73.2(3) . . ?
O5 Gd1 N13 114.0(4) . . ?
O5 Gd1 N14 25.5(3) . . ?
N8 Gd1 O1 71.4(4) . . ?
N8 Gd1 O2 122.4(4) . . ?
N8 Gd1 O4 150.1(4) . . ?
N8 Gd1 O5 142.6(4) . . ?
N8 Gd1 N10 69.5(4) . . ?
N8 Gd1 N12 85.8(4) . . ?
N8 Gd1 N13 97.2(4) . . ?
N8 Gd1 N14 153.5(4) . . ?
N9 Gd1 O1 74.0(4) 2_655 . ?
N9 Gd1 O2 73.6(4) 2_655 . ?
N9 Gd1 O4 108.6(4) 2_655 . ?
N9 Gd1 O5 71.9(4) 2_655 . ?
N9 Gd1 N8 101.2(4) 2_655 . ?
N9 Gd1 N10 77.6(4) 2_655 . ?
N9 Gd1 N12 137.4(4) 2_655 . ?
N9 Gd1 N13 71.3(4) 2_655 . ?
N9 Gd1 N14 92.5(4) 2_655 . ?
N10 Gd1 N13 143.0(4) . . ?
N10 Gd1 N14 91.9(3) . . ?
N12 Gd1 O1 145.5(4) . . ?
N12 Gd1 O2 136.7(4) . . ?
N12 Gd1 O4 70.9(3) . . ?
N12 Gd1 O5 77.3(3) . . ?
N12 Gd1 N10 65.6(4) . . ?
N12 Gd1 N13 150.2(4) . . ?
N12 Gd1 N14 69.0(3) . . ?
N14 Gd1 N13 108.7(4) . . ?
N1 Fe1 N3 89.8(5) . . ?
N1 Fe1 N5 89.3(5) . . ?
N3 Fe1 N5 87.1(5) . . ?
C10 Fe1 N1 91.9(5) . . ?
C10 Fe1 N3 92.2(6) . . ?
C10 Fe1 N5 178.6(5) . . ?
C11 Fe1 N1 92.3(5) . . ?
C11 Fe1 N3 177.9(5) . . ?
C11 Fe1 N5 93.1(6) . . ?
C11 Fe1 C10 87.5(6) . . ?
C12 Fe1 N1 176.4(6) . . ?
C12 Fe1 N3 92.8(5) . . ?
C12 Fe1 N5 93.3(6) . . ?
C12 Fe1 C10 85.5(6) . . ?
C12 Fe1 C11 85.1(6) . . ?
N13 O1 Gd1 96.2(9) . . ?
Gd1 O1W H1WB 122.2 . . ?
Gd1 O1W H1WA 110.1 . . ?
H1WB O1W H1WA 113.2 . . ?
N13 O2 Gd1 97.3(8) . . ?
N14 O4 Gd1 94.9(7) . . ?
N14 O5 Gd1 96.9(8) . . ?
N2 N1 Fe1 120.5(9) . . ?
N2 N1 C1 107.3(11) . . ?
C1 N1 Fe1 132.2(10) . . ?
N1 N2 B1 117.9(12) . . ?
C3 N2 N1 110.3(13) . . ?
C3 N2 B1 131.7(13) . . ?
N4 N3 Fe1 118.5(9) . . ?
C6 N3 Fe1 132.9(10) . . ?
C6 N3 N4 108.5(12) . . ?
N3 N4 C4 108.1(13) . . ?
N3 N4 B1 119.5(11) . . ?
C4 N4 B1 132.4(14) . . ?
N6 N5 Fe1 119.5(10) . . ?
C9 N5 Fe1 135.0(10) . . ?
C9 N5 N6 105.3(12) . . ?
N5 N6 B1 116.8(12) . . ?
C7 N6 N5 108.8(12) . . ?
C7 N6 B1 134.4(13) . . ?
C11 N8 Gd1 168.2(11) . . ?
C12 N9 Gd1 166.4(11) . 2_655 ?
C13 N10 Gd1 127.1(10) . . ?
C13 N10 C17 115.4(13) . . ?
C17 N10 Gd1 117.0(9) . . ?
C18 N11 H11 125.8 . . ?
C18 N11 C19 108.4(12) . . ?
C19 N11 H11 125.8 . . ?
C18 N12 Gd1 118.4(8) . . ?
C18 N12 C20 107.0(12) . . ?
C20 N12 Gd1 134.5(10) . . ?
O1 N13 Gd1 57.8(7) . . ?
O2 N13 Gd1 57.0(7) . . ?
O2 N13 O1 114.8(13) . . ?
O3 N13 Gd1 177.0(11) . . ?
O3 N13 O1 120.7(16) . . ?
O3 N13 O2 124.5(14) . . ?
O4 N14 Gd1 59.3(6) . . ?
O5 N14 Gd1 57.6(7) . . ?
O5 N14 O4 115.4(11) . . ?
O6 N14 Gd1 169.5(10) . . ?
O6 N14 O4 121.8(12) . . ?
O6 N14 O5 122.8(13) . . ?
N1 C1 H1 126.1 . . ?
N1 C1 C2 107.8(14) . . ?
C2 C1 H1 126.1 . . ?
C1 C2 H2 126.4 . . ?
C3 C2 C1 107.2(15) . . ?
C3 C2 H2 126.4 . . ?
N2 C3 C2 107.4(14) . . ?
N2 C3 H3 126.3 . . ?
C2 C3 H3 126.3 . . ?
N4 C4 H4 125.9 . . ?
C5 C4 N4 108.3(15) . . ?
C5 C4 H4 125.9 . . ?
C4 C5 H5 127.3 . . ?
C4 C5 C6 105.5(14) . . ?
C6 C5 H5 127.3 . . ?
N3 C6 C5 109.6(14) . . ?
N3 C6 H6 125.2 . . ?
C5 C6 H6 125.2 . . ?
N6 C7 H7 125.3 . . ?
N6 C7 C8 109.4(15) . . ?
C8 C7 H7 125.3 . . ?
C7 C8 H8 127.5 . . ?
C7 C8 C9 104.9(16) . . ?
C9 C8 H8 127.5 . . ?
N5 C9 C8 111.6(14) . . ?
N5 C9 H9 124.2 . . ?
C8 C9 H9 124.2 . . ?
N7 C10 Fe1 179.7(19) . . ?
N8 C11 Fe1 173.3(13) . . ?
N9 C12 Fe1 173.5(13) . . ?
N10 C13 H13 117.3 . . ?
N10 C13 C14 125.3(15) . . ?
C14 C13 H13 117.3 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.3(14) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 121.7 . . ?
C16 C15 C14 116.6(15) . . ?
C16 C15 H15 121.7 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.2(16) . . ?
C17 C16 H16 120.4 . . ?
N10 C17 C16 124.1(14) . . ?
N10 C17 C18 114.0(12) . . ?
C16 C17 C18 121.9(14) . . ?
N11 C18 C17 125.8(13) . . ?
N12 C18 N11 109.9(12) . . ?
N12 C18 C17 124.3(13) . . ?
N11 C19 H19 127.9 . . ?
C20 C19 N11 104.3(12) . . ?
C20 C19 H19 127.9 . . ?
N12 C20 C19 110.3(13) . . ?
N12 C20 H20 124.8 . . ?
C19 C20 H20 124.8 . . ?
N2 B1 N4 109.5(13) . . ?
N2 B1 N6 107.3(12) . . ?
N2 B1 H1A 111.5 . . ?
N4 B1 N6 105.4(12) . . ?
N4 B1 H1A 111.5 . . ?
N6 B1 H1A 111.5 . . ?
H5WA O5W H5WB 109.5 . . ?
H4WA O4W H4WB 104.5 . . ?
H4WA O4W H3WA 4.8 . . ?
H4WA O4W H3WB 69.0 . . ?
H4WB O4W H3WA 100.6 . . ?
H4WB O4W H3WB 47.0 . . ?
H3WA O4W H3WB 67.2 . . ?
H2WA O2W H2WB 111.3 . . ?
H4WA O3W H4WB 111.8 . . ?
H4WA O3W H3WA 4.7 . . ?
H4WA O3W H3WB 106.1 . . ?
H4WB O3W H3WA 107.3 . . ?
H4WB O3W H3WB 81.9 . . ?
H3WA O3W H3WB 104.5 . . ?
H5WA O6W H5WB 95.6 . . ?
H5WA O6W H6WA 76.2 . . ?
H5WA O6W H6WB 173.2 . . ?
H5WB O6W H6WA 171.2 . . ?
H5WB O6W H6WB 78.5 . . ?
H6WA O6W H6WB 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1585318'
_audit_update_record             
;
2017-11-13 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H48 B2 Fe2 La2 N34 O11, 10(O)'
_chemical_formula_sum            'C56 H48 B2 Fe2 La2 N34 O22'
_chemical_formula_weight         1960.42

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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                   12.0687(9)
_cell_length_b                   13.3292(10)
_cell_length_c                   13.3974(8)
_cell_angle_alpha                89.017(6)
_cell_angle_beta                 77.566(6)
_cell_angle_gamma                89.386(6)
_cell_volume                     2104.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3168
_cell_measurement_theta_min      2.1940
_cell_measurement_theta_max      23.0260

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_F_000             974
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.418
_shelx_estimated_absorpt_T_min   0.794
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.44620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'KappaCCD 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       CCD

# Orientation matrix from 'scale_all.out'


_diffrn_orient_matrix_UB_11      -0.0217718

_diffrn_orient_matrix_UB_21      -0.0774066

_diffrn_orient_matrix_UB_31      -0.0280047

_diffrn_orient_matrix_UB_12      0.0726326

_diffrn_orient_matrix_UB_22      -0.0196007

_diffrn_orient_matrix_UB_32      -0.0013858

_diffrn_orient_matrix_UB_13      -0.0021773

_diffrn_orient_matrix_UB_23      -0.0085678

_diffrn_orient_matrix_UB_33      0.0764462



_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            36885
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_av_R_equivalents  0.1299
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.198
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8561
_reflns_number_gt                6125
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.0649P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8561
_refine_ls_number_parameters     533
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0632
_refine_ls_wR_factor_ref         0.1586
_refine_ls_wR_factor_gt          0.1368
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.004
_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
C11 C 0.1240(5) 0.1174(4) -0.1336(5) 0.0324(14) Uani 1 1 d . . . . .
C12 C 0.2579(5) -0.0110(5) -0.2602(5) 0.0379(15) Uani 1 1 d . . . . .
C10 C 0.0315(5) -0.0260(4) -0.2226(4) 0.0282(13) Uani 1 1 d . . . . .
C1 C 0.1471(5) -0.0431(5) -0.4655(5) 0.0382(15) Uani 1 1 d . . . . .
H1 H 0.147685 -0.107342 -0.433889 0.046 Uiso 1 1 calc R U . . .
C2 C 0.1485(6) -0.0269(6) -0.5677(5) 0.0492(18) Uani 1 1 d . . . . .
H2 H 0.150838 -0.076122 -0.618622 0.059 Uiso 1 1 calc R U . . .
C3 C 0.1459(6) 0.0756(6) -0.5802(5) 0.0487(18) Uani 1 1 d . . . . .
H3 H 0.145877 0.110652 -0.642476 0.058 Uiso 1 1 calc R U . . .
C6 C -0.0854(5) 0.2020(5) -0.2256(5) 0.0422(16) Uani 1 1 d . . . . .
H6 H -0.116794 0.171371 -0.161317 0.051 Uiso 1 1 calc R U . . .
C5 C -0.1361(6) 0.2788(6) -0.2721(7) 0.058(2) Uani 1 1 d . . . . .
H5 H -0.207115 0.310541 -0.246311 0.070 Uiso 1 1 calc R U . . .
C4 C -0.0620(7) 0.2989(5) -0.3630(7) 0.057(2) Uani 1 1 d . . . . .
H4 H -0.073382 0.347961 -0.412172 0.068 Uiso 1 1 calc R U . . .
C9 C 0.3438(5) 0.2165(6) -0.2945(6) 0.0505(19) Uani 1 1 d . . . . .
H9 H 0.372057 0.188444 -0.239153 0.061 Uiso 1 1 calc R U . . .
C8 C 0.3930(7) 0.2947(6) -0.3574(6) 0.061(2) Uani 1 1 d . . . . .
H8 H 0.460423 0.329386 -0.354117 0.073 Uiso 1 1 calc R U . . .
C7 C 0.3241(6) 0.3121(6) -0.4259(6) 0.055(2) Uani 1 1 d . . . . .
H7 H 0.335352 0.361682 -0.478826 0.066 Uiso 1 1 calc R U . . .
C13 C -0.1572(6) 0.2753(5) 0.1592(6) 0.0512(19) Uani 1 1 d . . . . .
H13 H -0.150043 0.233437 0.215587 0.061 Uiso 1 1 calc R U . . .
C14 C -0.2641(6) 0.3064(5) 0.1500(7) 0.060(2) Uani 1 1 d . . . . .
H14 H -0.328588 0.287542 0.200750 0.072 Uiso 1 1 calc R U . . .
C15 C -0.2774(7) 0.3647(6) 0.0676(7) 0.063(2) Uani 1 1 d . . . . .
H15 H -0.350833 0.385900 0.060607 0.076 Uiso 1 1 calc R U . . .
C16 C -0.1822(6) 0.3919(5) -0.0047(6) 0.053(2) Uani 1 1 d . . . . .
H16 H -0.188658 0.431919 -0.062607 0.064 Uiso 1 1 calc R U . . .
C17 C -0.0763(5) 0.3592(4) 0.0093(5) 0.0363(15) Uani 1 1 d . . . . .
C18 C 0.0275(5) 0.3859(4) -0.0631(5) 0.0358(15) Uani 1 1 d . . . . .
C19 C 0.1477(7) 0.4401(5) -0.2018(5) 0.0491(18) Uani 1 1 d . . . . .
H19 H 0.179112 0.468923 -0.266961 0.059 Uiso 1 1 calc R U . . .
C20 C 0.2037(6) 0.3963(5) -0.1353(5) 0.0432(16) Uani 1 1 d . . . . .
H20 H 0.283907 0.389980 -0.146894 0.052 Uiso 1 1 calc R U . . .
C21 C 0.2677(6) -0.0171(5) 0.0430(6) 0.0481(18) Uani 1 1 d . . . . .
H21 H 0.207692 -0.016473 0.007343 0.058 Uiso 1 1 calc R U . . .
C22 C 0.3364(6) -0.1012(5) 0.0366(6) 0.055(2) Uani 1 1 d . . . . .
H22 H 0.325628 -0.155389 -0.005358 0.066 Uiso 1 1 calc R U . . .
C23 C 0.4200(7) -0.1058(6) 0.0908(7) 0.063(2) Uani 1 1 d . . . . .
H23 H 0.466025 -0.164265 0.089306 0.075 Uiso 1 1 calc R U . . .
C24 C 0.4365(6) -0.0247(5) 0.1477(6) 0.0525(19) Uani 1 1 d . . . . .
H24 H 0.495541 -0.025154 0.184506 0.063 Uiso 1 1 calc R U . . .
C25 C 0.3647(5) 0.0585(5) 0.1504(5) 0.0355(15) Uani 1 1 d . . . . .
C26 C 0.3724(5) 0.1483(5) 0.2115(5) 0.0374(15) Uani 1 1 d . . . . .
C27 C 0.4326(6) 0.2546(6) 0.3101(6) 0.0475(18) Uani 1 1 d . . . . .
H27 H 0.476142 0.286390 0.351483 0.057 Uiso 1 1 calc R U . . .
C28 C 0.3350(6) 0.2898(5) 0.2863(5) 0.0464(17) Uani 1 1 d . . . . .
H28 H 0.298705 0.351415 0.308867 0.056 Uiso 1 1 calc R U . . .
N9 N 0.3336(5) -0.0619(5) -0.2557(5) 0.0511(15) Uani 1 1 d . . . . .
N8 N 0.1188(5) 0.1403(4) -0.0514(4) 0.0405(13) Uani 1 1 d . . . . .
N7 N -0.0276(4) -0.0902(4) -0.1895(4) 0.0346(12) Uani 1 1 d . . . . .
N5 N 0.2502(4) 0.1864(4) -0.3236(4) 0.0380(13) Uani 1 1 d . . . . .
N6 N 0.2379(5) 0.2463(4) -0.4043(4) 0.0435(14) Uani 1 1 d . . . . .
N3 N 0.0151(4) 0.1781(4) -0.2860(4) 0.0327(12) Uani 1 1 d . . . . .
N4 N 0.0293(5) 0.2382(4) -0.3717(5) 0.0456(14) Uani 1 1 d . . . . .
N1 N 0.1448(4) 0.0436(4) -0.4172(4) 0.0334(12) Uani 1 1 d . . . . .
N2 N 0.1434(4) 0.1181(4) -0.4886(4) 0.0404(13) Uani 1 1 d . . . . .
N13 N 0.2814(4) 0.0640(4) 0.0974(4) 0.0374(13) Uani 1 1 d . . . . .
N15 N 0.2969(4) 0.2224(4) 0.2245(4) 0.0362(12) Uani 1 1 d . . . . .
N14 N 0.4552(5) 0.1653(4) 0.2631(4) 0.0484(15) Uani 1 1 d . . . . .
H14A H 0.513222 0.125535 0.265648 0.058 Uiso 1 1 calc R U . . .
N10 N -0.0630(4) 0.3021(4) 0.0909(4) 0.0379(13) Uani 1 1 d . . . . .
N12 N 0.1303(4) 0.3623(4) -0.0492(4) 0.0388(13) Uani 1 1 d . . . . .
N11 N 0.0353(5) 0.4337(4) -0.1543(5) 0.0488(15) Uani 1 1 d . . . . .
H11 H -0.022099 0.456854 -0.178965 0.059 Uiso 1 1 calc R U . . .
N16 N 0.3850(5) 0.3315(5) 0.0080(5) 0.0492(15) Uani 1 1 d . . . . .
N17 N 0.0436(5) 0.3708(5) 0.2905(5) 0.0461(14) Uani 1 1 d . . . . .
O2 O 0.3504(3) 0.2505(3) -0.0204(4) 0.0461(12) Uani 1 1 d . . . . .
O3 O 0.4829(5) 0.3595(5) -0.0227(6) 0.090(2) Uani 1 1 d . . . . .
O1 O 0.3149(4) 0.3847(4) 0.0695(4) 0.0530(13) Uani 1 1 d . . . . .
O5 O 0.1100(4) 0.4080(3) 0.2098(4) 0.0475(12) Uani 1 1 d . . . . .
O6 O -0.0084(5) 0.4255(4) 0.3570(5) 0.0805(18) Uani 1 1 d . . . . .
O4 O 0.0336(4) 0.2777(3) 0.2931(3) 0.0454(11) Uani 1 1 d . . . . .
O7A O 0.410(3) -0.141(3) -0.493(2) 0.132(16) Uiso 0.31(3) 1 d . . P A 1
O7B O 0.470(2) -0.044(2) -0.517(2) 0.253(14) Uiso 0.69(3) 1 d . . P A 2
O8 O 0.4116(16) 0.5002(13) -0.6064(13) 0.112(9) Uiso 0.48(3) 1 d . . P B 1
O8B O 0.308(4) 0.543(3) -0.586(3) 0.28(2) Uiso 0.52(3) 1 d . . P B 2
O9 O 0.331(4) 0.618(3) -0.431(4) 0.05(2) Uiso 0.11(3) 1 d . . P C 1
O9B O 0.3817(19) 0.5776(16) -0.4025(16) 0.248(9) Uiso 0.89(3) 1 d . . P C 2
O10 O 0.273(3) 0.651(3) -0.454(3) 0.39(2) Uiso 0.73(2) 1 d . . P C 1
O10B O 0.361(3) 0.785(3) -0.460(3) 0.126(17) Uiso 0.27(2) 1 d . . P C 2
O11 O -0.3660(14) 0.4508(10) -0.1984(10) 0.078(7) Uiso 0.53(4) 1 d . . P D 1
O11B O -0.428(4) 0.475(3) -0.208(2) 0.209(15) Uiso 0.47(4) 1 d . . P D 2
Fe1 Fe 0.13633(7) 0.08067(6) -0.27400(6) 0.0276(2) Uani 1 1 d . . . . .
La1 La 0.15252(3) 0.24153(2) 0.10425(3) 0.02918(14) Uani 1 1 d . . . . .
B1 B 0.1367(7) 0.2277(6) -0.4547(6) 0.048(2) Uani 1 1 d . . . . .
H1A H 0.136580 0.275160 -0.513250 0.057 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
C11 N8 1.136(8) . ?
C11 Fe1 1.926(6) . ?
C12 N9 1.144(8) . ?
C12 Fe1 1.936(7) . ?
C10 N7 1.141(7) . ?
C10 Fe1 1.930(6) . ?
C1 N1 1.331(8) . ?
C1 C2 1.379(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.374(10) . ?
C2 H2 0.9500 . ?
C3 N2 1.355(8) . ?
C3 H3 0.9500 . ?
C6 N3 1.344(8) . ?
C6 C5 1.393(9) . ?
C6 H6 0.9500 . ?
C5 C4 1.371(11) . ?
C5 H5 0.9500 . ?
C4 N4 1.346(9) . ?
C4 H4 0.9500 . ?
C9 N5 1.339(8) . ?
C9 C8 1.385(10) . ?
C9 H9 0.9500 . ?
C8 C7 1.379(11) . ?
C8 H8 0.9500 . ?
C7 N6 1.348(8) . ?
C7 H7 0.9500 . ?
C13 N10 1.344(8) . ?
C13 C14 1.380(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.395(9) . ?
C16 H16 0.9500 . ?
C17 N10 1.358(8) . ?
C17 C18 1.454(9) . ?
C18 N12 1.327(8) . ?
C18 N11 1.354(8) . ?
C19 C20 1.350(9) . ?
C19 N11 1.371(9) . ?
C19 H19 0.9500 . ?
C20 N12 1.368(8) . ?
C20 H20 0.9500 . ?
C21 N13 1.345(8) . ?
C21 C22 1.379(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.365(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.375(10) . ?
C23 H23 0.9500 . ?
C24 C25 1.395(9) . ?
C24 H24 0.9500 . ?
C25 N13 1.350(8) . ?
C25 C26 1.477(9) . ?
C26 N15 1.325(8) . ?
C26 N14 1.355(8) . ?
C27 N14 1.353(8) . ?
C27 C28 1.361(9) . ?
C27 H27 0.9500 . ?
C28 N15 1.379(8) . ?
C28 H28 0.9500 . ?
N8 La1 2.609(5) . ?
N7 La1 2.625(5) 2 ?
N5 N6 1.365(7) . ?
N5 Fe1 1.983(5) . ?
N6 B1 1.541(10) . ?
N3 N4 1.369(7) . ?
N3 Fe1 1.977(5) . ?
N4 B1 1.522(10) . ?
N1 N2 1.370(7) . ?
N1 Fe1 1.970(5) . ?
N2 B1 1.533(10) . ?
N13 La1 2.810(5) . ?
N15 La1 2.623(5) . ?
N14 H14A 0.8800 . ?
N10 La1 2.757(5) . ?
N12 La1 2.647(5) . ?
N11 H11 0.8800 . ?
N16 O3 1.225(7) . ?
N16 O2 1.254(7) . ?
N16 O1 1.266(8) . ?
N17 O6 1.221(7) . ?
N17 O4 1.248(7) . ?
N17 O5 1.294(7) . ?
O2 La1 2.606(4) . ?
O1 La1 2.712(5) . ?
O5 La1 2.638(5) . ?
O4 La1 2.675(5) . ?
O7B O7B 1.51(5) 2_654 ?
O9 O10 0.92(6) . ?
B1 H1A 1.0000 . ?

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
N8 C11 Fe1 178.5(6) . . ?
N9 C12 Fe1 176.3(6) . . ?
N7 C10 Fe1 177.2(5) . . ?
N1 C1 C2 110.9(6) . . ?
N1 C1 H1 124.6 . . ?
C2 C1 H1 124.6 . . ?
C3 C2 C1 105.2(6) . . ?
C3 C2 H2 127.4 . . ?
C1 C2 H2 127.4 . . ?
N2 C3 C2 108.5(6) . . ?
N2 C3 H3 125.7 . . ?
C2 C3 H3 125.7 . . ?
N3 C6 C5 109.2(7) . . ?
N3 C6 H6 125.4 . . ?
C5 C6 H6 125.4 . . ?
C4 C5 C6 105.5(6) . . ?
C4 C5 H5 127.3 . . ?
C6 C5 H5 127.3 . . ?
N4 C4 C5 109.3(7) . . ?
N4 C4 H4 125.3 . . ?
C5 C4 H4 125.3 . . ?
N5 C9 C8 109.6(7) . . ?
N5 C9 H9 125.2 . . ?
C8 C9 H9 125.2 . . ?
C7 C8 C9 106.0(6) . . ?
C7 C8 H8 127.0 . . ?
C9 C8 H8 127.0 . . ?
N6 C7 C8 107.8(7) . . ?
N6 C7 H7 126.1 . . ?
C8 C7 H7 126.1 . . ?
N10 C13 C14 122.2(7) . . ?
N10 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C15 C14 C13 120.2(8) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 118.8(7) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C15 C16 C17 118.4(7) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N10 C17 C16 122.9(7) . . ?
N10 C17 C18 115.8(5) . . ?
C16 C17 C18 121.4(6) . . ?
N12 C18 N11 110.1(6) . . ?
N12 C18 C17 123.4(6) . . ?
N11 C18 C17 126.5(6) . . ?
C20 C19 N11 104.6(6) . . ?
C20 C19 H19 127.7 . . ?
N11 C19 H19 127.7 . . ?
C19 C20 N12 111.4(6) . . ?
C19 C20 H20 124.3 . . ?
N12 C20 H20 124.3 . . ?
N13 C21 C22 123.3(7) . . ?
N13 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C23 C22 C21 119.5(7) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 119.0(7) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
C23 C24 C25 118.7(7) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
N13 C25 C24 122.9(6) . . ?
N13 C25 C26 113.8(5) . . ?
C24 C25 C26 123.2(6) . . ?
N15 C26 N14 111.0(6) . . ?
N15 C26 C25 123.8(5) . . ?
N14 C26 C25 125.1(6) . . ?
N14 C27 C28 106.4(6) . . ?
N14 C27 H27 126.8 . . ?
C28 C27 H27 126.8 . . ?
C27 C28 N15 109.7(6) . . ?
C27 C28 H28 125.1 . . ?
N15 C28 H28 125.1 . . ?
C11 N8 La1 160.1(5) . . ?
C10 N7 La1 175.5(5) . 2 ?
C9 N5 N6 107.1(6) . . ?
C9 N5 Fe1 133.8(5) . . ?
N6 N5 Fe1 119.1(4) . . ?
C7 N6 N5 109.5(6) . . ?
C7 N6 B1 132.0(6) . . ?
N5 N6 B1 118.5(5) . . ?
C6 N3 N4 107.6(5) . . ?
C6 N3 Fe1 133.8(4) . . ?
N4 N3 Fe1 118.5(4) . . ?
C4 N4 N3 108.4(6) . . ?
C4 N4 B1 132.3(6) . . ?
N3 N4 B1 119.4(5) . . ?
C1 N1 N2 106.7(5) . . ?
C1 N1 Fe1 134.4(4) . . ?
N2 N1 Fe1 118.9(4) . . ?
C3 N2 N1 108.7(5) . . ?
C3 N2 B1 132.3(6) . . ?
N1 N2 B1 118.9(5) . . ?
C21 N13 C25 116.5(5) . . ?
C21 N13 La1 124.6(4) . . ?
C25 N13 La1 118.9(4) . . ?
C26 N15 C28 105.2(5) . . ?
C26 N15 La1 120.5(4) . . ?
C28 N15 La1 131.9(4) . . ?
C27 N14 C26 107.6(5) . . ?
C27 N14 H14A 126.2 . . ?
C26 N14 H14A 126.2 . . ?
C13 N10 C17 117.5(6) . . ?
C13 N10 La1 123.6(4) . . ?
C17 N10 La1 118.8(4) . . ?
C18 N12 C20 105.3(5) . . ?
C18 N12 La1 119.7(4) . . ?
C20 N12 La1 133.8(4) . . ?
C18 N11 C19 108.5(5) . . ?
C18 N11 H11 125.7 . . ?
C19 N11 H11 125.7 . . ?
O3 N16 O2 121.8(7) . . ?
O3 N16 O1 120.3(7) . . ?
O2 N16 O1 117.9(5) . . ?
O6 N17 O4 123.4(7) . . ?
O6 N17 O5 120.8(6) . . ?
O4 N17 O5 115.8(6) . . ?
N16 O2 La1 99.4(4) . . ?
N16 O1 La1 93.9(4) . . ?
N17 O5 La1 98.2(4) . . ?
N17 O4 La1 97.7(4) . . ?
C11 Fe1 C10 86.8(2) . . ?
C11 Fe1 C12 88.6(3) . . ?
C10 Fe1 C12 87.7(2) . . ?
C11 Fe1 N1 178.6(2) . . ?
C10 Fe1 N1 92.5(2) . . ?
C12 Fe1 N1 92.6(2) . . ?
C11 Fe1 N3 90.1(2) . . ?
C10 Fe1 N3 93.9(2) . . ?
C12 Fe1 N3 177.9(2) . . ?
N1 Fe1 N3 88.8(2) . . ?
C11 Fe1 N5 92.1(2) . . ?
C10 Fe1 N5 176.9(2) . . ?
C12 Fe1 N5 89.4(2) . . ?
N1 Fe1 N5 88.7(2) . . ?
N3 Fe1 N5 89.0(2) . . ?
O2 La1 N8 77.94(16) . . ?
O2 La1 N15 76.03(16) . . ?
N8 La1 N15 133.38(16) . . ?
O2 La1 N7 132.42(15) . 2 ?
N8 La1 N7 76.45(16) . 2 ?
N15 La1 N7 93.83(16) . 2 ?
O2 La1 O5 110.55(15) . . ?
N8 La1 O5 146.53(15) . . ?
N15 La1 O5 79.42(15) . . ?
N7 La1 O5 112.98(16) 2 . ?
O2 La1 N12 73.01(15) . . ?
N8 La1 N12 68.67(16) . . ?
N15 La1 N12 135.70(16) . . ?
N7 La1 N12 130.47(15) 2 . ?
O5 La1 N12 82.65(15) . . ?
O2 La1 O4 145.95(14) . . ?
N8 La1 O4 135.47(16) . . ?
N15 La1 O4 74.13(15) . . ?
N7 La1 O4 66.03(15) 2 . ?
O5 La1 O4 47.82(14) . . ?
N12 La1 O4 119.86(15) . . ?
O2 La1 O1 47.87(15) . . ?
N8 La1 O1 118.11(17) . . ?
N15 La1 O1 67.08(15) . . ?
N7 La1 O1 160.74(15) 2 . ?
O5 La1 O1 62.69(16) . . ?
N12 La1 O1 68.67(15) . . ?
O4 La1 O1 104.37(15) . . ?
O2 La1 N10 133.90(15) . . ?
N8 La1 N10 77.68(16) . . ?
N15 La1 N10 145.36(16) . . ?
N7 La1 N10 77.48(15) 2 . ?
O5 La1 N10 73.64(15) . . ?
N12 La1 N10 61.82(16) . . ?
O4 La1 N10 71.70(15) . . ?
O1 La1 N10 116.51(15) . . ?
O2 La1 N13 65.91(14) . . ?
N8 La1 N13 73.07(16) . . ?
N15 La1 N13 61.15(15) . . ?
N7 La1 N13 68.55(15) 2 . ?
O5 La1 N13 140.34(14) . . ?
N12 La1 N13 128.27(16) . . ?
O4 La1 N13 111.78(14) . . ?
O1 La1 N13 102.26(15) . . ?
N10 La1 N13 139.21(15) . . ?
N4 B1 N2 106.9(6) . . ?
N4 B1 N6 107.1(6) . . ?
N2 B1 N6 107.6(6) . . ?
N4 B1 H1A 111.7 . . ?
N2 B1 H1A 111.7 . . ?
N6 B1 H1A 111.7 . . ?

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
N1 C1 C2 C3 -0.5(8) . . . . ?
C1 C2 C3 N2 0.2(8) . . . . ?
N3 C6 C5 C4 0.5(8) . . . . ?
C6 C5 C4 N4 -0.2(9) . . . . ?
N5 C9 C8 C7 0.8(9) . . . . ?
C9 C8 C7 N6 -0.3(9) . . . . ?
N10 C13 C14 C15 1.8(12) . . . . ?
C13 C14 C15 C16 -0.5(12) . . . . ?
C14 C15 C16 C17 -0.2(11) . . . . ?
C15 C16 C17 N10 -0.2(10) . . . . ?
C15 C16 C17 C18 -179.3(6) . . . . ?
N10 C17 C18 N12 -3.9(9) . . . . ?
C16 C17 C18 N12 175.2(6) . . . . ?
N10 C17 C18 N11 173.4(6) . . . . ?
C16 C17 C18 N11 -7.5(10) . . . . ?
N11 C19 C20 N12 0.6(8) . . . . ?
N13 C21 C22 C23 3.0(12) . . . . ?
C21 C22 C23 C24 -2.5(13) . . . . ?
C22 C23 C24 C25 1.9(12) . . . . ?
C23 C24 C25 N13 -1.8(11) . . . . ?
C23 C24 C25 C26 178.0(7) . . . . ?
N13 C25 C26 N15 8.1(9) . . . . ?
C24 C25 C26 N15 -171.7(7) . . . . ?
N13 C25 C26 N14 -173.2(6) . . . . ?
C24 C25 C26 N14 7.0(11) . . . . ?
N14 C27 C28 N15 0.0(8) . . . . ?
C8 C9 N5 N6 -1.0(8) . . . . ?
C8 C9 N5 Fe1 179.6(5) . . . . ?
C8 C7 N6 N5 -0.3(8) . . . . ?
C8 C7 N6 B1 -178.6(7) . . . . ?
C9 N5 N6 C7 0.8(7) . . . . ?
Fe1 N5 N6 C7 -179.6(5) . . . . ?
C9 N5 N6 B1 179.4(6) . . . . ?
Fe1 N5 N6 B1 -1.1(7) . . . . ?
C5 C6 N3 N4 -0.6(7) . . . . ?
C5 C6 N3 Fe1 179.0(5) . . . . ?
C5 C4 N4 N3 -0.1(8) . . . . ?
C5 C4 N4 B1 -179.7(7) . . . . ?
C6 N3 N4 C4 0.4(7) . . . . ?
Fe1 N3 N4 C4 -179.3(4) . . . . ?
C6 N3 N4 B1 -179.9(6) . . . . ?
Fe1 N3 N4 B1 0.4(7) . . . . ?
C2 C1 N1 N2 0.7(7) . . . . ?
C2 C1 N1 Fe1 177.4(5) . . . . ?
C2 C3 N2 N1 0.2(7) . . . . ?
C2 C3 N2 B1 -178.1(7) . . . . ?
C1 N1 N2 C3 -0.6(7) . . . . ?
Fe1 N1 N2 C3 -177.8(4) . . . . ?
C1 N1 N2 B1 178.0(6) . . . . ?
Fe1 N1 N2 B1 0.7(7) . . . . ?
C22 C21 N13 C25 -2.6(10) . . . . ?
C22 C21 N13 La1 176.3(6) . . . . ?
C24 C25 N13 C21 2.1(10) . . . . ?
C26 C25 N13 C21 -177.7(6) . . . . ?
C24 C25 N13 La1 -176.9(5) . . . . ?
C26 C25 N13 La1 3.3(7) . . . . ?
N14 C26 N15 C28 0.7(7) . . . . ?
C25 C26 N15 C28 179.6(6) . . . . ?
N14 C26 N15 La1 165.0(4) . . . . ?
C25 C26 N15 La1 -16.2(8) . . . . ?
C27 C28 N15 C26 -0.4(8) . . . . ?
C27 C28 N15 La1 -162.1(5) . . . . ?
C28 C27 N14 C26 0.4(8) . . . . ?
N15 C26 N14 C27 -0.7(8) . . . . ?
C25 C26 N14 C27 -179.6(6) . . . . ?
C14 C13 N10 C17 -2.2(10) . . . . ?
C14 C13 N10 La1 -179.6(5) . . . . ?
C16 C17 N10 C13 1.4(9) . . . . ?
C18 C17 N10 C13 -179.5(6) . . . . ?
C16 C17 N10 La1 178.9(5) . . . . ?
C18 C17 N10 La1 -1.9(7) . . . . ?
N11 C18 N12 C20 -0.4(7) . . . . ?
C17 C18 N12 C20 177.3(6) . . . . ?
N11 C18 N12 La1 -169.7(4) . . . . ?
C17 C18 N12 La1 8.0(8) . . . . ?
C19 C20 N12 C18 -0.2(7) . . . . ?
C19 C20 N12 La1 166.9(4) . . . . ?
N12 C18 N11 C19 0.8(7) . . . . ?
C17 C18 N11 C19 -176.8(6) . . . . ?
C20 C19 N11 C18 -0.8(7) . . . . ?
O3 N16 O2 La1 170.8(6) . . . . ?
O1 N16 O2 La1 -9.6(6) . . . . ?
O3 N16 O1 La1 -171.3(6) . . . . ?
O2 N16 O1 La1 9.1(6) . . . . ?
O6 N17 O5 La1 -171.2(5) . . . . ?
O4 N17 O5 La1 6.2(5) . . . . ?
O6 N17 O4 La1 171.2(6) . . . . ?
O5 N17 O4 La1 -6.1(5) . . . . ?
C4 N4 B1 N2 -123.3(8) . . . . ?
N3 N4 B1 N2 57.2(7) . . . . ?
C4 N4 B1 N6 121.6(8) . . . . ?
N3 N4 B1 N6 -57.9(8) . . . . ?
C3 N2 B1 N4 120.3(7) . . . . ?
N1 N2 B1 N4 -57.9(7) . . . . ?
C3 N2 B1 N6 -125.0(7) . . . . ?
N1 N2 B1 N6 56.9(7) . . . . ?
C7 N6 B1 N4 -123.7(8) . . . . ?
N5 N6 B1 N4 58.2(8) . . . . ?
C7 N6 B1 N2 121.7(8) . . . . ?
N5 N6 B1 N2 -56.4(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N14 H14A N9 0.88 2.00 2.868(8) 166.8 2_655 yes
N11 H11 O5 0.88 2.16 2.917(7) 143.8 2_565 yes

_refine_diff_density_max         1.443
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.142


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
