# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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_LP30Et3
_database_code_depnum_ccdc_archive 'CCDC 1996673'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2020-07-08 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C36 H30 Fe N10 O2, 1.5 (C2 H6 O), 0.5 (H2 O), 2(Cl O4) 
;
_chemical_formula_sum            'C39 H40 Cl2 Fe N10 O12'
_chemical_formula_weight         967.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N 0.0076 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1697 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.3555 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_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                   12.790(4)
_cell_length_b                   13.158(4)
_cell_length_c                   15.054(5)
_cell_angle_alpha                71.548(4)
_cell_angle_beta                 69.217(4)
_cell_angle_gamma                63.267(4)
_cell_volume                     2077.7(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    4411
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      25.5

_exptl_crystal_description       block
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_F_000             1000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.713
_shelx_estimated_absorpt_T_min   0.871
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_process_details   'TWINABS-2008/4 (Sheldrick, 2008) '
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            5983
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.092
_diffrn_reflns_theta_max         25.637
_diffrn_reflns_theta_full        25.637
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             5983
_reflns_number_gt                4675
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Apex2 v2010.3 (Bruker, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_refine_special_details          
;Refined as a 2-component twin.

This stucture contains one half occupancy waters,one half occupancy 
ethanol disordered over an inversion center, one full occupancy ethanol
and two perchlorate anions, one disordered, one not.
The disordered perchlorate was modeled as split sites, using the 
following restraints:

SADI 0.01 Cl1 O11 Cl1 O12 Cl1 O13 Cl1 O14 Cl1' O11' Cl1' O12' =
 CL1' O13' CL1' O14'
SADI 0.02 O11 O12 O11 O13 O11 O14 O12 O13 O12 O14 O13 O14 O11' O12' =
 O11' O13' O11' O14' O12' O13' O12' O14' O13' O14'
SIMU 0.01 Cl1 > O14'

EXYZ O2S C4S'
EXYZ O2S' C4S
EADP O2S C4S'
EADP O2S' C4S

SIMU 0.01 O2S > C4S'
DFIX 1.54 0.01 C3S C4S C3S' C4S'
DFIX 1.40 0.02 O2S C3S O2S' C3S'

As this crystal has undergone solvent removal and re-uptake, 
the mosaicity has increased. The data beyond 0.9 angstroms had I/σ
values of less then 2, therefore this data was omitted.,Twin
;
_vrf_THETM01_LP30Et3             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: As this crystal has undergone solvent removal and re-uptake, 
the mosaicity has increased. The data beyond 0.9 angstroms had I/\s
values of less then 2, therefore this data was omitted. 
;
_vrf_PLAT430_LP30Et3             
;
PROBLEM: Short Inter D...A Contact  O2W      ..O23      .       2.77 Ang.  
RESPONSE: This is probably a hydrogen bond. The hydrogen atoms for O2W, 
 could not be found or places with confidence and therefore were
 omitted from the refinement but not the formula.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0857P)²+5.6898P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5983
_refine_ls_number_parameters     602
_refine_ls_number_restraints     197
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.1865
_refine_ls_wR_factor_gt          0.1600
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.49382(10) 0.23501(10) 0.23466(8) 0.0324(3) Uani 1 1 d . . . . .
O1 O 0.1887(5) 0.3712(5) 0.5578(4) 0.0500(15) Uani 1 1 d . . . . .
O2 O 0.9400(5) 0.0725(6) -0.1657(4) 0.0561(16) Uani 1 1 d . . . . .
N1 N 0.2629(6) 0.2941(5) 0.3979(4) 0.0359(14) Uani 1 1 d . . . . .
H1A H 0.286471 0.317963 0.432281 0.043 Uiso 1 1 calc R U . . .
N2 N 0.3329(6) 0.2577(5) 0.3137(4) 0.0373(16) Uani 1 1 d . . . . .
N3 N 0.4352(5) 0.1847(5) 0.1621(4) 0.0326(14) Uani 1 1 d . . . . .
N4 N 0.6381(5) 0.1932(5) 0.1258(4) 0.0313(13) Uani 1 1 d . . . . .
N5 N 0.7512(5) 0.1904(5) 0.0929(4) 0.0343(14) Uani 1 1 d . . . . .
H5A H 0.783211 0.210581 0.123367 0.041 Uiso 1 1 calc R U . . .
N6 N 0.3933(5) 0.4704(5) 0.1042(4) 0.0382(15) Uani 1 1 d . . . . .
H6A H 0.370839 0.449053 0.067187 0.046 Uiso 1 1 calc R U . . .
N7 N 0.4447(5) 0.3995(5) 0.1763(4) 0.0296(13) Uani 1 1 d . . . . .
N8 N 0.5413(5) 0.2898(5) 0.3122(4) 0.0311(14) Uani 1 1 d . . . . .
N9 N 0.5649(5) 0.0901(5) 0.3198(4) 0.0284(13) Uani 1 1 d . . . . .
N10 N 0.5841(6) -0.0217(5) 0.3333(4) 0.0391(16) Uani 1 1 d . . . . .
H10A H 0.563067 -0.049333 0.299895 0.047 Uiso 1 1 calc R U . . .
C1 C 0.0762(8) 0.3666(7) 0.5772(6) 0.051(2) Uani 1 1 d . . . . .
C2 C -0.0148(9) 0.4008(7) 0.6599(6) 0.057(2) Uani 1 1 d . . . . .
H2A H -0.001244 0.426729 0.704724 0.068 Uiso 1 1 calc R U . . .
C3 C -0.1274(9) 0.3953(9) 0.6738(7) 0.068(3) Uani 1 1 d . . . . .
H3A H -0.191397 0.421425 0.726873 0.082 Uiso 1 1 calc R U . . .
C4 C -0.1435(9) 0.3525(9) 0.6109(7) 0.064(3) Uani 1 1 d . . . . .
H4A H -0.217212 0.344815 0.623257 0.076 Uiso 1 1 calc R U . . .
C5 C -0.0535(8) 0.3198(8) 0.5289(6) 0.053(2) Uani 1 1 d . . . . .
H5B H -0.068084 0.293994 0.484538 0.064 Uiso 1 1 calc R U . . .
C6 C 0.0562(8) 0.3249(7) 0.5121(6) 0.043(2) Uani 1 1 d . . . . .
C7 C 0.1508(8) 0.2895(6) 0.4232(6) 0.042(2) Uani 1 1 d . . . . .
C8 C 0.1508(7) 0.2478(6) 0.3510(5) 0.0397(19) Uani 1 1 d . . . . .
H8A H 0.086480 0.234947 0.346325 0.048 Uiso 1 1 calc R U . . .
C9 C 0.2631(7) 0.2280(6) 0.2860(5) 0.0325(17) Uani 1 1 d . . . . .
C10 C 0.3233(7) 0.1877(6) 0.1934(5) 0.0371(18) Uani 1 1 d . . . . .
C11 C 0.2753(7) 0.1571(7) 0.1393(5) 0.0405(19) Uani 1 1 d . . . . .
H11A H 0.196837 0.156810 0.162376 0.049 Uiso 1 1 calc R U . . .
C12 C 0.3488(7) 0.1273(7) 0.0501(6) 0.042(2) Uani 1 1 d . . . . .
H12A H 0.319247 0.107025 0.012104 0.051 Uiso 1 1 calc R U . . .
C13 C 0.4640(7) 0.1270(7) 0.0170(6) 0.0382(19) Uani 1 1 d . . . . .
H13A H 0.512495 0.109447 -0.044087 0.046 Uiso 1 1 calc R U . . .
C14 C 0.5062(7) 0.1534(6) 0.0762(5) 0.0347(17) Uani 1 1 d . . . . .
C15 C 0.6260(7) 0.1551(6) 0.0578(5) 0.0354(18) Uani 1 1 d . . . . .
C16 C 0.7318(7) 0.1281(6) -0.0159(5) 0.0361(18) Uani 1 1 d . . . . .
H16A H 0.746363 0.098953 -0.070447 0.043 Uiso 1 1 calc R U . . .
C17 C 0.8104(7) 0.1536(6) 0.0085(5) 0.0360(18) Uani 1 1 d . . . . .
C18 C 0.9337(7) 0.1520(6) -0.0429(5) 0.0339(17) Uani 1 1 d . . . . .
C19 C 0.9869(8) 0.1941(8) -0.0059(6) 0.047(2) Uani 1 1 d . . . . .
H19A H 0.945701 0.220109 0.053184 0.057 Uiso 1 1 calc R U . . .
C20 C 1.1001(8) 0.1992(8) -0.0534(7) 0.053(2) Uani 1 1 d . . . . .
H20A H 1.134720 0.230027 -0.028112 0.064 Uiso 1 1 calc R U . . .
C21 C 1.1608(8) 0.1574(8) -0.1396(6) 0.051(2) Uani 1 1 d . . . . .
H21A H 1.237972 0.158950 -0.172104 0.061 Uiso 1 1 calc R U . . .
C22 C 1.1103(8) 0.1137(7) -0.1783(6) 0.049(2) Uani 1 1 d . . . . .
H22A H 1.152693 0.084619 -0.235962 0.058 Uiso 1 1 calc R U . . .
C23 C 0.9962(7) 0.1138(7) -0.1305(5) 0.0409(19) Uani 1 1 d . . . . .
C24 C 0.2103(10) 0.4153(9) 0.6229(7) 0.069(3) Uani 1 1 d . . . . .
H24A H 0.285334 0.428119 0.593649 0.103 Uiso 1 1 calc R U . . .
H24B H 0.216228 0.359619 0.683028 0.103 Uiso 1 1 calc R U . . .
H24C H 0.144102 0.487892 0.635879 0.103 Uiso 1 1 calc R U . . .
C25 C 0.9987(9) 0.0376(9) -0.2575(6) 0.062(3) Uani 1 1 d . . . . .
H25A H 0.946009 0.017406 -0.275907 0.093 Uiso 1 1 calc R U . . .
H25B H 1.073364 -0.029185 -0.253243 0.093 Uiso 1 1 calc R U . . .
H25C H 1.016551 0.100738 -0.305693 0.093 Uiso 1 1 calc R U . . .
C26 C 0.3813(7) 0.5793(7) 0.0971(6) 0.0403(19) Uani 1 1 d . . . . .
H26A H 0.348349 0.643482 0.051316 0.048 Uiso 1 1 calc R U . . .
C27 C 0.4243(8) 0.5821(7) 0.1666(6) 0.043(2) Uani 1 1 d . . . . .
H27A H 0.426878 0.646434 0.179083 0.052 Uiso 1 1 calc R U . . .
C28 C 0.4640(7) 0.4666(7) 0.2152(5) 0.0369(18) Uani 1 1 d . . . . .
C29 C 0.5160(7) 0.4037(6) 0.2982(5) 0.0353(18) Uani 1 1 d . . . . .
C30 C 0.5404(7) 0.4478(7) 0.3587(6) 0.0397(19) Uani 1 1 d . . . . .
H30A H 0.523743 0.527282 0.348576 0.048 Uiso 1 1 calc R U . . .
C31 C 0.5909(8) 0.3690(7) 0.4356(6) 0.046(2) Uani 1 1 d . . . . .
H31A H 0.606051 0.396224 0.478562 0.056 Uiso 1 1 calc R U . . .
C32 C 0.6177(7) 0.2530(7) 0.4475(5) 0.0383(18) Uani 1 1 d . . . . .
H32A H 0.653818 0.199992 0.497186 0.046 Uiso 1 1 calc R U . . .
C33 C 0.5908(7) 0.2149(7) 0.3853(5) 0.0339(17) Uani 1 1 d . . . . .
C34 C 0.6078(7) 0.0959(7) 0.3868(5) 0.0351(18) Uani 1 1 d . . . . .
C35 C 0.6571(8) -0.0133(7) 0.4411(6) 0.042(2) Uani 1 1 d . . . . .
H35A H 0.693891 -0.032822 0.491426 0.050 Uiso 1 1 calc R U . . .
C36 C 0.6398(7) -0.0861(6) 0.4045(5) 0.0388(18) Uani 1 1 d . . . . .
H36A H 0.662915 -0.166636 0.425583 0.047 Uiso 1 1 calc R U . . .
O1S O 0.2852(7) 0.4311(7) -0.0019(5) 0.080(2) Uani 1 1 d . . . . .
H1S H 0.312896 0.410310 -0.055025 0.120 Uiso 1 1 calc R U . . .
C1S C 0.1515(8) 0.4676(8) 0.0265(7) 0.055(2) Uani 1 1 d . . . . .
H1SA H 0.116409 0.531750 -0.022614 0.066 Uiso 1 1 calc R U . . .
H1SB H 0.130345 0.402878 0.030873 0.066 Uiso 1 1 calc R U . . .
C2S C 0.1016(10) 0.5047(10) 0.1215(8) 0.077(3) Uani 1 1 d . . . . .
H2SA H 0.014371 0.528453 0.139889 0.116 Uiso 1 1 calc R U . . .
H2SB H 0.135878 0.440686 0.170045 0.116 Uiso 1 1 calc R U . . .
H2SC H 0.121975 0.569250 0.116686 0.116 Uiso 1 1 calc R U . . .
Cl2 Cl 0.1220(2) 0.6891(2) -0.24191(15) 0.0554(6) Uani 1 1 d . . . . .
O21 O 0.2026(5) 0.7178(6) -0.2193(4) 0.0607(17) Uani 1 1 d . . . . .
O22 O 0.0134(6) 0.7060(6) -0.1689(5) 0.0679(19) Uani 1 1 d . . . . .
O23 O 0.1777(10) 0.5708(9) -0.2509(9) 0.156(5) Uani 1 1 d . . . . .
O24 O 0.1047(9) 0.7538(12) -0.3348(6) 0.147(5) Uani 1 1 d . . . . .
O2S O 0.8787(19) 0.0250(18) -0.5390(14) 0.088(5) Uiso 0.25 1 d D U P A -1
H2S H 0.889971 0.077634 -0.584391 0.132 Uiso 0.25 1 calc R U P A -1
C3S C 0.923(3) 0.019(9) -0.463(4) 0.091(8) Uiso 0.25 1 d D U P A -1
H3S1 H 0.905893 -0.038985 -0.407115 0.109 Uiso 0.25 1 calc R U P A -1
H3S2 H 0.887622 0.094304 -0.443747 0.109 Uiso 0.25 1 calc R U P A -1
C4S C 1.061(2) -0.016(3) -0.5077(19) 0.093(6) Uiso 0.25 1 d D U P A -1
H4S1 H 1.099405 -0.022512 -0.459987 0.139 Uiso 0.25 1 calc R U P A -1
H4S2 H 1.094195 -0.090557 -0.527306 0.139 Uiso 0.25 1 calc R U P A -1
H4S3 H 1.076053 0.041785 -0.563677 0.139 Uiso 0.25 1 calc R U P A -1
O2S' O 1.061(2) -0.016(3) -0.5077(19) 0.093(6) Uiso 0.25 1 d D U P B -2
H2S' H 1.097984 -0.012372 -0.474180 0.139 Uiso 0.25 1 calc R U P B -2
C3S' C 0.933(3) 0.035(8) -0.467(4) 0.095(8) Uiso 0.25 1 d D U P B -2
H3S3 H 0.908690 0.116411 -0.464511 0.114 Uiso 0.25 1 calc R U P B -2
H3S4 H 0.909065 -0.007079 -0.402401 0.114 Uiso 0.25 1 calc R U P B -2
C4S' C 0.8787(19) 0.0250(18) -0.5390(14) 0.088(5) Uiso 0.25 1 d D U P B -2
H4S4 H 0.791124 0.057993 -0.517722 0.132 Uiso 0.25 1 calc R U P B -2
H4S5 H 0.905042 0.066491 -0.602877 0.132 Uiso 0.25 1 calc R U P B -2
H4S6 H 0.905414 -0.056029 -0.541255 0.132 Uiso 0.25 1 calc R U P B -2
Cl1 Cl 0.4169(2) -0.14593(18) 0.27554(14) 0.0398(5) Uani 0.868 1 d D U P C 1
O11 O 0.3500(6) -0.1320(6) 0.2107(4) 0.0492(16) Uani 0.868 1 d D U P C 1
O12 O 0.3437(5) -0.0700(5) 0.3426(4) 0.0456(16) Uani 0.868 1 d D U P C 1
O13 O 0.5203(7) -0.1172(7) 0.2199(5) 0.0552(19) Uani 0.868 1 d D U P C 1
O14 O 0.4562(8) -0.2630(5) 0.3252(5) 0.069(2) Uani 0.868 1 d D U P C 1
Cl1' Cl 0.5190(14) -0.2098(14) 0.2432(11) 0.055(3) Uiso 0.132 1 d D U P D 2
O11' O 0.606(3) -0.289(3) 0.181(2) 0.067(11) Uiso 0.132 1 d D U P D 2
O12' O 0.543(3) -0.251(3) 0.3365(16) 0.066(7) Uiso 0.132 1 d D U P D 2
O13' O 0.4006(19) -0.201(4) 0.251(3) 0.064(6) Uiso 0.132 1 d D U P D 2
O14' O 0.526(4) -0.098(2) 0.204(3) 0.053(7) Uiso 0.132 1 d D U P D 2
O2W O 0.6851(10) -0.3604(10) 0.1567(8) 0.052(3) Uiso 0.5 1 d . . P E 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.917(7) . ?
Fe1 N3 1.919(6) . ?
Fe1 N8 1.919(6) . ?
Fe1 N7 1.953(6) . ?
Fe1 N9 1.956(6) . ?
Fe1 N4 1.976(6) . ?
O1 C1 1.389(11) . ?
O1 C24 1.439(11) . ?
O2 C23 1.377(10) . ?
O2 C25 1.429(9) . ?
N1 N2 1.352(8) . ?
N1 C7 1.371(10) . ?
N1 H1A 0.8700 . ?
N2 C9 1.345(10) . ?
N3 C10 1.325(10) . ?
N3 C14 1.354(9) . ?
N4 N5 1.339(9) . ?
N4 C15 1.353(9) . ?
N5 C17 1.341(9) . ?
N5 H5A 0.8700 . ?
N6 N7 1.341(8) . ?
N6 C26 1.343(10) . ?
N6 H6A 0.8700 . ?
N7 C28 1.346(10) . ?
N8 C29 1.344(9) . ?
N8 C33 1.353(9) . ?
N9 N10 1.336(8) . ?
N9 C34 1.344(9) . ?
N10 C36 1.342(10) . ?
N10 H10A 0.8700 . ?
C1 C2 1.400(12) . ?
C1 C6 1.405(12) . ?
C2 C3 1.412(15) . ?
C2 H2A 0.9400 . ?
C3 C4 1.355(14) . ?
C3 H3A 0.9400 . ?
C4 C5 1.385(13) . ?
C4 H4A 0.9400 . ?
C5 C6 1.363(12) . ?
C5 H5B 0.9400 . ?
C6 C7 1.487(11) . ?
C7 C8 1.364(11) . ?
C8 C9 1.384(11) . ?
C8 H8A 0.9400 . ?
C9 C10 1.468(10) . ?
C10 C11 1.409(11) . ?
C11 C12 1.395(11) . ?
C11 H11A 0.9400 . ?
C12 C13 1.376(11) . ?
C12 H12A 0.9400 . ?
C13 C14 1.383(10) . ?
C13 H13A 0.9400 . ?
C14 C15 1.467(11) . ?
C15 C16 1.392(10) . ?
C16 C17 1.379(11) . ?
C16 H16A 0.9400 . ?
C17 C18 1.483(10) . ?
C18 C19 1.372(11) . ?
C18 C23 1.393(11) . ?
C19 C20 1.392(12) . ?
C19 H19A 0.9400 . ?
C20 C21 1.394(12) . ?
C20 H20A 0.9400 . ?
C21 C22 1.377(13) . ?
C21 H21A 0.9400 . ?
C22 C23 1.380(12) . ?
C22 H22A 0.9400 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.359(12) . ?
C26 H26A 0.9400 . ?
C27 C28 1.403(11) . ?
C27 H27A 0.9400 . ?
C28 C29 1.459(11) . ?
C29 C30 1.401(10) . ?
C30 C31 1.413(12) . ?
C30 H30A 0.9400 . ?
C31 C32 1.370(11) . ?
C31 H31A 0.9400 . ?
C32 C33 1.389(10) . ?
C32 H32A 0.9400 . ?
C33 C34 1.474(10) . ?
C34 C35 1.392(11) . ?
C35 C36 1.370(11) . ?
C35 H35A 0.9400 . ?
C36 H36A 0.9400 . ?
O1S C1S 1.487(11) . ?
O1S H1S 0.8300 . ?
C1S C2S 1.486(14) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
C2S H2SC 0.9700 . ?
Cl2 O22 1.408(7) . ?
Cl2 O21 1.415(6) . ?
Cl2 O23 1.420(10) . ?
Cl2 O24 1.424(9) . ?
O2S C3S 1.41(2) . ?
O2S H2S 0.8300 . ?
C3S C4S 1.546(10) . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C4S H4S1 0.9700 . ?
C4S H4S2 0.9700 . ?
C4S H4S3 0.9700 . ?
O2S' C3S' 1.43(2) . ?
O2S' H2S' 0.8300 . ?
C3S' C4S' 1.541(10) . ?
C3S' H3S3 0.9800 . ?
C3S' H3S4 0.9800 . ?
C4S' H4S4 0.9700 . ?
C4S' H4S5 0.9700 . ?
C4S' H4S6 0.9700 . ?
Cl1 O12 1.421(5) . ?
Cl1 O14 1.423(5) . ?
Cl1 O11 1.434(5) . ?
Cl1 O13 1.435(6) . ?
Cl1' O12' 1.427(8) . ?
Cl1' O14' 1.428(8) . ?
Cl1' O11' 1.429(8) . ?
Cl1' O13' 1.430(8) . ?

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
N2 Fe1 N3 79.2(3) . . ?
N2 Fe1 N8 97.0(3) . . ?
N3 Fe1 N8 176.1(3) . . ?
N2 Fe1 N7 91.3(2) . . ?
N3 Fe1 N7 99.7(2) . . ?
N8 Fe1 N7 79.4(2) . . ?
N2 Fe1 N9 92.7(2) . . ?
N3 Fe1 N9 101.5(2) . . ?
N8 Fe1 N9 79.5(2) . . ?
N7 Fe1 N9 158.8(2) . . ?
N2 Fe1 N4 159.2(3) . . ?
N3 Fe1 N4 80.0(3) . . ?
N8 Fe1 N4 103.8(2) . . ?
N7 Fe1 N4 92.1(2) . . ?
N9 Fe1 N4 91.5(2) . . ?
C1 O1 C24 119.0(7) . . ?
C23 O2 C25 118.4(7) . . ?
N2 N1 C7 112.9(6) . . ?
N2 N1 H1A 123.6 . . ?
C7 N1 H1A 123.6 . . ?
C9 N2 N1 104.0(6) . . ?
C9 N2 Fe1 117.9(5) . . ?
N1 N2 Fe1 138.0(5) . . ?
C10 N3 C14 120.6(6) . . ?
C10 N3 Fe1 119.8(5) . . ?
C14 N3 Fe1 119.4(5) . . ?
N5 N4 C15 103.7(6) . . ?
N5 N4 Fe1 140.9(5) . . ?
C15 N4 Fe1 115.4(5) . . ?
N4 N5 C17 113.7(6) . . ?
N4 N5 H5A 123.2 . . ?
C17 N5 H5A 123.2 . . ?
N7 N6 C26 110.3(6) . . ?
N7 N6 H6A 124.8 . . ?
C26 N6 H6A 124.8 . . ?
N6 N7 C28 105.9(6) . . ?
N6 N7 Fe1 137.4(5) . . ?
C28 N7 Fe1 116.7(5) . . ?
C29 N8 C33 120.7(6) . . ?
C29 N8 Fe1 119.5(5) . . ?
C33 N8 Fe1 119.5(5) . . ?
N10 N9 C34 105.0(6) . . ?
N10 N9 Fe1 137.8(5) . . ?
C34 N9 Fe1 117.2(5) . . ?
N9 N10 C36 111.8(6) . . ?
N9 N10 H10A 124.1 . . ?
C36 N10 H10A 124.1 . . ?
O1 C1 C2 121.3(9) . . ?
O1 C1 C6 118.1(7) . . ?
C2 C1 C6 120.5(9) . . ?
C1 C2 C3 118.0(10) . . ?
C1 C2 H2A 121.0 . . ?
C3 C2 H2A 121.0 . . ?
C4 C3 C2 120.2(9) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C3 C4 C5 121.3(10) . . ?
C3 C4 H4A 119.3 . . ?
C5 C4 H4A 119.3 . . ?
C6 C5 C4 120.2(9) . . ?
C6 C5 H5B 119.9 . . ?
C4 C5 H5B 119.9 . . ?
C5 C6 C1 119.6(8) . . ?
C5 C6 C7 119.0(8) . . ?
C1 C6 C7 121.5(8) . . ?
C8 C7 N1 104.9(7) . . ?
C8 C7 C6 131.2(8) . . ?
N1 C7 C6 123.9(7) . . ?
C7 C8 C9 107.2(7) . . ?
C7 C8 H8A 126.4 . . ?
C9 C8 H8A 126.4 . . ?
N2 C9 C8 111.0(7) . . ?
N2 C9 C10 112.3(6) . . ?
C8 C9 C10 136.6(7) . . ?
N3 C10 C11 121.2(7) . . ?
N3 C10 C9 110.6(6) . . ?
C11 C10 C9 128.2(7) . . ?
C12 C11 C10 117.4(7) . . ?
C12 C11 H11A 121.3 . . ?
C10 C11 H11A 121.3 . . ?
C13 C12 C11 121.1(7) . . ?
C13 C12 H12A 119.5 . . ?
C11 C12 H12A 119.5 . . ?
C12 C13 C14 118.0(7) . . ?
C12 C13 H13A 121.0 . . ?
C14 C13 H13A 121.0 . . ?
N3 C14 C13 121.6(7) . . ?
N3 C14 C15 110.7(6) . . ?
C13 C14 C15 127.7(7) . . ?
N4 C15 C16 111.3(7) . . ?
N4 C15 C14 114.3(6) . . ?
C16 C15 C14 134.3(7) . . ?
C17 C16 C15 105.1(6) . . ?
C17 C16 H16A 127.5 . . ?
C15 C16 H16A 127.5 . . ?
N5 C17 C16 106.2(7) . . ?
N5 C17 C18 121.7(7) . . ?
C16 C17 C18 131.9(7) . . ?
C19 C18 C23 118.2(7) . . ?
C19 C18 C17 119.5(7) . . ?
C23 C18 C17 122.2(7) . . ?
C18 C19 C20 121.8(8) . . ?
C18 C19 H19A 119.1 . . ?
C20 C19 H19A 119.1 . . ?
C19 C20 C21 118.1(9) . . ?
C19 C20 H20A 121.0 . . ?
C21 C20 H20A 121.0 . . ?
C22 C21 C20 121.6(8) . . ?
C22 C21 H21A 119.2 . . ?
C20 C21 H21A 119.2 . . ?
C21 C22 C23 118.4(8) . . ?
C21 C22 H22A 120.8 . . ?
C23 C22 H22A 120.8 . . ?
O2 C23 C22 121.4(7) . . ?
O2 C23 C18 116.7(7) . . ?
C22 C23 C18 121.9(8) . . ?
O1 C24 H24A 109.5 . . ?
O1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 109.3(7) . . ?
N6 C26 H26A 125.3 . . ?
C27 C26 H26A 125.3 . . ?
C26 C27 C28 103.9(7) . . ?
C26 C27 H27A 128.0 . . ?
C28 C27 H27A 128.0 . . ?
N7 C28 C27 110.6(7) . . ?
N7 C28 C29 113.4(6) . . ?
C27 C28 C29 136.0(7) . . ?
N8 C29 C30 120.9(7) . . ?
N8 C29 C28 110.7(6) . . ?
C30 C29 C28 128.3(7) . . ?
C29 C30 C31 117.9(7) . . ?
C29 C30 H30A 121.1 . . ?
C31 C30 H30A 121.1 . . ?
C32 C31 C30 120.2(7) . . ?
C32 C31 H31A 119.9 . . ?
C30 C31 H31A 119.9 . . ?
C31 C32 C33 119.1(7) . . ?
C31 C32 H32A 120.5 . . ?
C33 C32 H32A 120.5 . . ?
N8 C33 C32 121.1(7) . . ?
N8 C33 C34 110.6(6) . . ?
C32 C33 C34 128.3(7) . . ?
N9 C34 C35 111.0(7) . . ?
N9 C34 C33 113.0(6) . . ?
C35 C34 C33 135.9(7) . . ?
C36 C35 C34 104.4(7) . . ?
C36 C35 H35A 127.8 . . ?
C34 C35 H35A 127.8 . . ?
N10 C36 C35 107.7(7) . . ?
N10 C36 H36A 126.1 . . ?
C35 C36 H36A 126.1 . . ?
C1S O1S H1S 109.5 . . ?
C2S C1S O1S 109.6(8) . . ?
C2S C1S H1SA 109.7 . . ?
O1S C1S H1SA 109.7 . . ?
C2S C1S H1SB 109.7 . . ?
O1S C1S H1SB 109.7 . . ?
H1SA C1S H1SB 108.2 . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
O22 Cl2 O21 111.2(4) . . ?
O22 Cl2 O23 108.8(5) . . ?
O21 Cl2 O23 108.8(6) . . ?
O22 Cl2 O24 113.3(6) . . ?
O21 Cl2 O24 108.5(5) . . ?
O23 Cl2 O24 106.0(8) . . ?
C3S O2S H2S 109.5 . . ?
O2S C3S C4S 104(2) . . ?
O2S C3S H3S1 111.0 . . ?
C4S C3S H3S1 111.0 . . ?
O2S C3S H3S2 111.0 . . ?
C4S C3S H3S2 111.0 . . ?
H3S1 C3S H3S2 109.0 . . ?
C3S C4S H4S1 109.5 . . ?
C3S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
C3S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
C3S' O2S' H2S' 109.5 . . ?
O2S' C3S' C4S' 103(2) . . ?
O2S' C3S' H3S3 111.1 . . ?
C4S' C3S' H3S3 111.1 . . ?
O2S' C3S' H3S4 111.1 . . ?
C4S' C3S' H3S4 111.1 . . ?
H3S3 C3S' H3S4 109.1 . . ?
C3S' C4S' H4S4 109.5 . . ?
C3S' C4S' H4S5 109.5 . . ?
H4S4 C4S' H4S5 109.5 . . ?
C3S' C4S' H4S6 109.5 . . ?
H4S4 C4S' H4S6 109.5 . . ?
H4S5 C4S' H4S6 109.5 . . ?
O12 Cl1 O14 110.4(4) . . ?
O12 Cl1 O11 110.0(4) . . ?
O14 Cl1 O11 109.8(4) . . ?
O12 Cl1 O13 109.0(4) . . ?
O14 Cl1 O13 109.3(5) . . ?
O11 Cl1 O13 108.4(4) . . ?
O12' Cl1' O14' 109.5(10) . . ?
O12' Cl1' O11' 109.4(10) . . ?
O14' Cl1' O11' 109.6(10) . . ?
O12' Cl1' O13' 109.6(10) . . ?
O14' Cl1' O13' 109.3(10) . . ?
O11' Cl1' O13' 109.5(10) . . ?

_refine_diff_density_max         0.765
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.104



####################################################################### 
# 
# 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_LBB15P14B
_database_code_depnum_ccdc_archive 'CCDC 1996676'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2020-07-08 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Fe N10 O2, 2(Cl O4), 0.35(C3 H8 O)'
_chemical_formula_sum            'C37.05 H32.80 Cl2 Fe N10 O10.35'
_chemical_formula_weight         910.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1697 0.1896
'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8268(6)
_cell_length_b                   11.9498(6)
_cell_length_c                   17.0106(7)
_cell_angle_alpha                100.463(3)
_cell_angle_beta                 106.141(3)
_cell_angle_gamma                107.590(3)
_cell_volume                     1928.55(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6738
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      24.63

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.758
_shelx_estimated_absorpt_T_min   0.722
_shelx_estimated_absorpt_T_max   0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            16403
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.118
_diffrn_reflns_theta_max         24.704
_diffrn_reflns_theta_full        24.620
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5015
_reflns_number_gt                3589
_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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically, except the two
 components of the partial lattice propanol molecule. The latter
 was refined with distance parameters restraints and the same 
 isotropic displacement parameter. After refining their respective
 occupancies, and taking into account it is bumped into the minor
 component of the disordered methoxyphenyl group (see below), 
 these were fixed at 0.25:0.10 for the final
 refinement. Hydrogens were placed geometrically on their carrier 
 atom and refined with a riding model, except those on the 
 partial disordered propanol that are omitted in the structural
 model, although included in the formula.
 One of the perchlorate ion is disordered over two positions 
 (Cl1 and Cl1A, with relative occupancies 0.46:0.54) and the two
 components were refined with distance and displacement parameters
 restraints. Associated with disorder of the propanol lattice
 molecule, the adjacent methoxyphenyl group is disordered over
 two positions with relative occupancies 0.65:0.35 
 (C19-C20-C21-C22-C23-C24-O10-C25 and same labelling+A). These are 
 slightly shifted and rotated with respect to one another and 
 were refined with displacement parameters restraints and a 
 rigid body restraint (AFIX 66 for the main component and SAME 
 for the minor component). The outer carbons (C30-C31-C32) of 
 the pyridine ring of the bpp ligand also show some lateral 
 disorder, likely also associated with the propanol disorder. 
 These were refined with displacement parameters restraints. 
;

_vrf_THETM01_LBB15P14B           
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.5393
RESPONSE: The crystal has suffered a transformation upon losing part
of its lattice propanol through a thermal treatment at 375 K. This 
results in an increased mosaicity and diffraction decreasing quickly.
Indeed there was significant diffraction only to ca. 0.95 ansgtrom resolution,
and the present data were cut at 0.93 angstrom. All this leads to a
rather low values of thetamax and thetafull and a poor though acceptable data
to parameters ratio of 7.50.
;

_vrf_PLAT088_LBB15P14B           
;
PROBLEM:  Poor Data / Parameter Ratio ....................       7.50 Note
RESPONSE: The crystal has suffered a transformation upon losing part
of its lattice propanol through a thermal treatment at 375 K. This 
results in an increased mosaicity and diffraction decreasing quickly.
Indeed there was significant diffraction only to ca. 0.95 ansgtrom resolution,
and the present data were cut at 0.93 angstrom. All this leads to a
rather low values of thetamax and thetafull and a poor though acceptable data
to parameters ratio of 7.50.
;


_vrf_PLAT027_LBB15P14B           
;
PROBLEM:  _diffrn_reflns_theta_full value (too) Low ......      24.62 Degree
RESPONSE: The crystal has suffered a transformation upon losing part
of its lattice propanol through a thermal treatment at 375 K. This 
results in an increased mosaicity and diffraction decreasing quickly.
Indeed there was significant diffraction only to ca. 0.95 ansgtrom resolution,
and the present data were cut at 0.93 angstrom. All this leads to a
rather low values of thetamax and thetafull and a poor though acceptable data
to parameters ratio of 7.50.
;

_vrf_PLAT315_LBB15P14B           
;
PROBLEM:  Singly Bonded Carbon Detected (H-atoms Missing).
RESPONSE: Due to the disorder, hydrogens on both components of 
the partial disordered propanol are omitted in the structural
model (but included in the formula), leading to this alert.
;

_vrf_PLAT309_LBB15P14B           
;
PROBLEM:  Single Bonded Oxygen (C-O > 1.3 Ang)
RESPONSE: Due to the disorder, hydrogens on both components of 
the partial disordered propanol are omitted in the structural
model (but included in the formula), leading to this alert.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²+11.8896P] 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         5015
_refine_ls_number_parameters     669
_refine_ls_number_restraints     586
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0787
_refine_ls_wR_factor_ref         0.1949
_refine_ls_wR_factor_gt          0.1773
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.56229(11) 0.51642(9) 0.26850(6) 0.0351(3) Uani 1 1 d . . . . .
O9 O 0.3519(5) 0.7944(5) 0.1046(3) 0.0478(14) Uani 1 1 d . . . . .
N1 N 0.5356(7) 0.7397(5) 0.2103(3) 0.0412(16) Uani 1 1 d . . . . .
H1A H 0.444928 0.711818 0.185346 0.049 Uiso 1 1 calc R U . . .
N2 N 0.6042(6) 0.6801(5) 0.2512(3) 0.0376(15) Uani 1 1 d . . . . .
N3 N 0.7614(6) 0.5850(5) 0.3219(3) 0.0370(15) Uani 1 1 d . . . . .
N4 N 0.5980(6) 0.3796(5) 0.3062(3) 0.0347(15) Uani 1 1 d . . . . .
N5 N 0.5248(7) 0.2660(5) 0.3071(4) 0.0419(16) Uani 1 1 d . . . . .
H5A H 0.434069 0.229811 0.283016 0.050 Uiso 1 1 calc R U . . .
N6 N 0.5778(7) 0.6268(5) 0.4514(4) 0.0428(17) Uani 1 1 d . . . . .
H6A H 0.668318 0.662014 0.476852 0.051 Uiso 1 1 calc R U . . .
N7 N 0.5139(7) 0.5658(5) 0.3684(4) 0.0398(16) Uani 1 1 d . . . . .
N8 N 0.3642(7) 0.4504(6) 0.2182(4) 0.0423(16) Uani 1 1 d . . . . .
N9 N 0.5361(7) 0.4428(5) 0.1488(3) 0.0342(15) Uani 1 1 d . . . . .
N10 N 0.6139(7) 0.4318(5) 0.1022(4) 0.0428(16) Uani 1 1 d . . . . .
H10A H 0.705016 0.458846 0.122703 0.051 Uiso 1 1 calc R U . . .
C1 C 0.2174(9) 0.7567(9) 0.0410(6) 0.067(3) Uani 1 1 d . . . . .
H1B H 0.169067 0.808268 0.058828 0.101 Uiso 1 1 calc R U . . .
H1C H 0.164094 0.670804 0.034125 0.101 Uiso 1 1 calc R U . . .
H1D H 0.226727 0.765093 -0.013505 0.101 Uiso 1 1 calc R U . . .
C2 C 0.4441(8) 0.9106(6) 0.1202(4) 0.0395(19) Uani 1 1 d . . . . .
C3 C 0.4087(9) 0.9971(8) 0.0837(5) 0.052(2) Uani 1 1 d . . . . .
H3A H 0.316412 0.976891 0.046584 0.063 Uiso 1 1 calc R U . . .
C4 C 0.5070(10) 1.1113(7) 0.1011(5) 0.051(2) Uani 1 1 d . . . . .
H4A H 0.481973 1.170099 0.076379 0.062 Uiso 1 1 calc R U . . .
C5 C 0.6428(10) 1.1420(8) 0.1547(5) 0.057(2) Uani 1 1 d . . . . .
H5B H 0.710973 1.221098 0.167018 0.068 Uiso 1 1 calc R U . . .
C6 C 0.6756(9) 1.0558(6) 0.1890(5) 0.044(2) Uani 1 1 d . . . . .
H6B H 0.768348 1.076617 0.225574 0.052 Uiso 1 1 calc R U . . .
C7 C 0.5793(8) 0.9380(6) 0.1731(4) 0.0400(19) Uani 1 1 d . . . . .
C8 C 0.6256(8) 0.8521(6) 0.2119(4) 0.0398(19) Uani 1 1 d . . . . .
C9 C 0.7537(9) 0.8594(7) 0.2551(5) 0.050(2) Uani 1 1 d . . . . .
H9A H 0.837889 0.925906 0.267373 0.060 Uiso 1 1 calc R U . . .
C10 C 0.7406(8) 0.7502(6) 0.2790(4) 0.043(2) Uani 1 1 d . . . . .
C11 C 0.8309(8) 0.6995(7) 0.3227(4) 0.043(2) Uani 1 1 d . . . . .
C12 C 0.9765(8) 0.7514(7) 0.3614(5) 0.052(2) Uani 1 1 d . . . . .
H12A H 1.026669 0.832266 0.362275 0.063 Uiso 1 1 calc R U . . .
C13 C 1.0445(9) 0.6831(8) 0.3977(5) 0.057(2) Uani 1 1 d . . . . .
H13A H 1.142582 0.717106 0.424197 0.069 Uiso 1 1 calc R U . . .
C14 C 0.9717(8) 0.5657(8) 0.3960(5) 0.048(2) Uani 1 1 d . . . . .
H14A H 1.018482 0.517856 0.420493 0.058 Uiso 1 1 calc R U . . .
C15 C 0.8281(8) 0.5188(7) 0.3574(4) 0.0406(19) Uani 1 1 d . . . . .
C16 C 0.7316(8) 0.3995(6) 0.3497(4) 0.0380(18) Uani 1 1 d . . . . .
C17 C 0.7423(10) 0.2999(7) 0.3779(5) 0.048(2) Uani 1 1 d . . . . .
H17A H 0.824611 0.291877 0.409958 0.058 Uiso 1 1 calc R U . . .
C18 C 0.6084(9) 0.2146(7) 0.3497(4) 0.044(2) Uani 1 1 d D . . . .
C19 C 0.5442(10) 0.0882(7) 0.3573(7) 0.052(3) Uani 0.6521 1 d DG U P A 1
C20 C 0.6348(9) 0.0470(8) 0.4083(6) 0.057(2) Uani 0.6521 1 d G U P A 1
H20A H 0.730363 0.097439 0.435133 0.069 Uiso 0.6521 1 calc R U P A 1
C21 C 0.5856(11) -0.0681(8) 0.4202(7) 0.066(3) Uani 0.6521 1 d G U P A 1
H21A H 0.647493 -0.096220 0.455092 0.079 Uiso 0.6521 1 calc R U P A 1
C22 C 0.4458(12) -0.1419(7) 0.3810(7) 0.073(3) Uani 0.6521 1 d G U P A 1
H22A H 0.412153 -0.220535 0.389067 0.088 Uiso 0.6521 1 calc R U P A 1
C23 C 0.3552(9) -0.1007(8) 0.3299(6) 0.065(3) Uani 0.6521 1 d G U P A 1
H23A H 0.259682 -0.151191 0.303082 0.078 Uiso 0.6521 1 calc R U P A 1
C24 C 0.4045(9) 0.0143(8) 0.3180(7) 0.060(2) Uani 0.6521 1 d G U P A 1
O10 O 0.3261(10) 0.0569(8) 0.2677(6) 0.065(2) Uani 0.6521 1 d . U P A 1
C25 C 0.1794(16) -0.0200(14) 0.2254(11) 0.085(4) Uani 0.6521 1 d . U P A 1
H25A H 0.136321 0.013770 0.181786 0.127 Uiso 0.6521 1 calc R U P A 1
H25B H 0.133657 -0.022085 0.267652 0.127 Uiso 0.6521 1 calc R U P A 1
H25C H 0.169663 -0.103429 0.198187 0.127 Uiso 0.6521 1 calc R U P A 1
C19A C 0.589(3) 0.101(2) 0.371(2) 0.056(3) Uani 0.348 1 d D U P A 2
C20A C 0.725(3) 0.072(2) 0.4165(16) 0.051(3) Uani 0.348 1 d . U P A 2
H20B H 0.816956 0.130752 0.434026 0.062 Uiso 0.348 1 calc R U P A 2
C21A C 0.697(3) -0.040(2) 0.4272(16) 0.065(4) Uani 0.348 1 d . U P A 2
H21B H 0.766733 -0.071880 0.446553 0.077 Uiso 0.348 1 calc R U P A 2
C22A C 0.536(4) -0.114(3) 0.404(2) 0.067(3) Uani 0.348 1 d . U P A 2
H22B H 0.515580 -0.192507 0.414155 0.080 Uiso 0.348 1 calc R U P A 2
C23A C 0.438(4) -0.090(2) 0.377(2) 0.069(3) Uani 0.348 1 d . U P A 2
H23B H 0.345690 -0.142727 0.366778 0.083 Uiso 0.348 1 calc R U P A 2
C24A C 0.472(3) 0.033(2) 0.3604(18) 0.063(3) Uani 0.348 1 d . U P A 2
O10A O 0.371(2) 0.0718(16) 0.3359(13) 0.067(3) Uani 0.348 1 d . U P A 2
C25A C 0.241(3) -0.002(3) 0.334(2) 0.084(5) Uani 0.348 1 d . U P A 2
H25D H 0.168168 0.016195 0.295833 0.126 Uiso 0.348 1 calc R U P A 2
H25E H 0.237711 0.013960 0.391469 0.126 Uiso 0.348 1 calc R U P A 2
H25F H 0.226684 -0.088772 0.312177 0.126 Uiso 0.348 1 calc R U P A 2
C26 C 0.4871(10) 0.6279(7) 0.4909(5) 0.051(2) Uani 1 1 d . . . . .
H26A H 0.509492 0.664205 0.550132 0.061 Uiso 1 1 calc R U . . .
C27 C 0.3576(10) 0.5682(8) 0.4317(5) 0.054(2) Uani 1 1 d . . . . .
H27A H 0.271918 0.555640 0.440211 0.064 Uiso 1 1 calc R U . . .
C28 C 0.3776(9) 0.5294(7) 0.3561(5) 0.046(2) Uani 1 1 d . . . . .
C29 C 0.2882(10) 0.4625(9) 0.2673(5) 0.064(3) Uani 1 1 d . . . . .
C30 C 0.1461(12) 0.4193(14) 0.2338(7) 0.116(4) Uani 1 1 d . U . . .
H30A H 0.093709 0.430103 0.269041 0.139 Uiso 1 1 calc R U . . .
C31 C 0.0817(13) 0.3597(14) 0.1472(7) 0.121(4) Uani 1 1 d . U . . .
H31A H -0.016609 0.326860 0.122341 0.145 Uiso 1 1 calc R U . . .
C32 C 0.1602(11) 0.3478(13) 0.0966(7) 0.110(4) Uani 1 1 d . U . . .
H32A H 0.116186 0.308677 0.036857 0.132 Uiso 1 1 calc R U . . .
C33 C 0.3022(9) 0.3928(8) 0.1335(5) 0.054(2) Uani 1 1 d . . . . .
C34 C 0.4041(8) 0.3895(6) 0.0937(4) 0.0394(19) Uani 1 1 d . . . . .
C35 C 0.4007(10) 0.3453(6) 0.0115(5) 0.047(2) Uani 1 1 d . . . . .
H35A H 0.321149 0.304220 -0.039100 0.056 Uiso 1 1 calc R U . . .
C36 C 0.5347(10) 0.3733(6) 0.0189(5) 0.046(2) Uani 1 1 d . . . . .
H36A H 0.567640 0.355226 -0.026320 0.056 Uiso 1 1 calc R U . . .
Cl1 Cl 0.9215(9) 0.7520(11) 0.6192(5) 0.085(3) Uani 0.463(12) 1 d D U P B 1
O1 O 0.7950(19) 0.735(2) 0.6354(16) 0.088(5) Uani 0.463(12) 1 d D U P B 1
O2 O 0.8874(17) 0.6752(16) 0.5398(8) 0.087(5) Uani 0.463(12) 1 d D U P B 1
O3 O 0.9979(18) 0.8741(14) 0.6303(12) 0.100(5) Uani 0.463(12) 1 d D U P B 1
O4 O 1.0018(17) 0.7083(18) 0.6772(10) 0.111(5) Uani 0.463(12) 1 d D U P B 1
Cl1A Cl 0.8934(8) 0.8035(6) 0.6060(4) 0.0646(18) Uani 0.537(12) 1 d D U P B 2
O2A O 0.8557(16) 0.7446(16) 0.5214(7) 0.100(5) Uani 0.537(12) 1 d D U P B 2
O3A O 0.929(2) 0.9288(11) 0.6103(11) 0.128(5) Uani 0.537(12) 1 d D U P B 2
O1A O 0.7762(16) 0.7714(17) 0.6335(13) 0.080(4) Uani 0.537(12) 1 d D U P B 2
O4A O 1.0046(14) 0.8035(19) 0.6707(10) 0.116(5) Uani 0.537(12) 1 d D U P B 2
Cl2 Cl 0.9687(3) 0.6126(3) 0.14623(15) 0.0920(10) Uani 1 1 d . U . . .
O5 O 0.8991(6) 0.5278(6) 0.1845(4) 0.0732(18) Uani 1 1 d . U . . .
O6 O 0.9369(9) 0.5528(9) 0.0598(4) 0.133(3) Uani 1 1 d . U . . .
O7 O 1.1148(8) 0.6596(9) 0.1931(5) 0.138(3) Uani 1 1 d . U . . .
O8 O 0.9223(10) 0.7123(9) 0.1500(5) 0.129(3) Uani 1 1 d . U . . .
O1S O 0.258(2) 0.1999(18) 0.2152(13) 0.037(3) Uiso 0.248 1 d D U P C 3
C1S C 0.162(3) 0.095(2) 0.1506(16) 0.037(3) Uiso 0.248 1 d D U P C 3
C2S C 0.003(3) 0.072(3) 0.1361(19) 0.037(3) Uiso 0.248 1 d . U P C 3
C3S C -0.101(3) -0.045(3) 0.0776(18) 0.037(3) Uiso 0.248 1 d . U P C 3
O1SA O 0.212(5) 0.172(4) 0.209(3) 0.037(3) Uiso 0.1 1 d D U P D 4
C1SA C 0.093(6) 0.066(5) 0.157(4) 0.037(3) Uiso 0.1 1 d D U P D 4
C2SA C -0.036(6) 0.003(7) 0.083(3) 0.037(3) Uiso 0.1 1 d D U P D 4
C3SA C -0.043(7) -0.039(6) -0.005(3) 0.037(3) Uiso 0.1 1 d D U P D 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N8 1.914(6) . ?
Fe1 N3 1.928(6) . ?
Fe1 N7 1.957(6) . ?
Fe1 N4 1.965(5) . ?
Fe1 N2 1.966(5) . ?
Fe1 N9 1.969(6) . ?
O9 C2 1.369(8) . ?
O9 C1 1.431(9) . ?
N1 N2 1.325(8) . ?
N1 C8 1.392(9) . ?
N1 H1A 0.8800 . ?
N2 C10 1.351(9) . ?
N3 C15 1.337(9) . ?
N3 C11 1.343(9) . ?
N4 C16 1.352(9) . ?
N4 N5 1.354(7) . ?
N5 C18 1.362(9) . ?
N5 H5A 0.8800 . ?
N6 C26 1.338(10) . ?
N6 N7 1.334(8) . ?
N6 H6A 0.8800 . ?
N7 C28 1.348(10) . ?
N8 C29 1.345(10) . ?
N8 C33 1.350(10) . ?
N9 N10 1.326(8) . ?
N9 C34 1.347(9) . ?
N10 C36 1.355(9) . ?
N10 H10A 0.8800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 C7 1.389(10) . ?
C2 C3 1.394(11) . ?
C3 C4 1.373(11) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(12) . ?
C4 H4A 0.9500 . ?
C5 C6 1.360(11) . ?
C5 H5B 0.9500 . ?
C6 C7 1.400(10) . ?
C6 H6B 0.9500 . ?
C7 C8 1.454(10) . ?
C8 C9 1.345(11) . ?
C9 C10 1.415(10) . ?
C9 H9A 0.9500 . ?
C10 C11 1.411(11) . ?
C11 C12 1.409(11) . ?
C12 C13 1.372(11) . ?
C12 H12A 0.9500 . ?
C13 C14 1.376(11) . ?
C13 H13A 0.9500 . ?
C14 C15 1.391(10) . ?
C14 H14A 0.9500 . ?
C15 C16 1.448(10) . ?
C16 C17 1.386(10) . ?
C17 C18 1.383(11) . ?
C17 H17A 0.9500 . ?
C18 C19A 1.445(18) . ?
C18 C19 1.506(9) . ?
C19 C20 1.3900 . ?
C19 C24 1.3900 . ?
C20 C21 1.3900 . ?
C20 H20A 0.9500 . ?
C21 C22 1.3900 . ?
C21 H21A 0.9500 . ?
C22 C23 1.3900 . ?
C22 H22A 0.9500 . ?
C23 C24 1.3900 . ?
C23 H23A 0.9500 . ?
C24 O10 1.314(12) . ?
O10 C25 1.459(17) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C19A C24A 1.22(4) . ?
C19A C20A 1.62(4) . ?
C20A C21A 1.34(3) . ?
C20A H20B 0.9500 . ?
C21A C22A 1.60(4) . ?
C21A H21B 0.9500 . ?
C22A C23A 1.19(4) . ?
C22A H22B 0.9500 . ?
C23A C24A 1.51(4) . ?
C23A H23B 0.9500 . ?
C24A O10A 1.31(3) . ?
O10A C25A 1.40(3) . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C26 C27 1.356(12) . ?
C26 H26A 0.9500 . ?
C27 C28 1.383(11) . ?
C27 H27A 0.9500 . ?
C28 C29 1.463(11) . ?
C29 C30 1.372(14) . ?
C30 C31 1.383(15) . ?
C30 H30A 0.9500 . ?
C31 C32 1.385(15) . ?
C31 H31A 0.9500 . ?
C32 C33 1.374(13) . ?
C32 H32A 0.9500 . ?
C33 C34 1.453(11) . ?
C34 C35 1.388(10) . ?
C35 C36 1.350(11) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
Cl1 O2 1.367(11) . ?
Cl1 O3 1.389(12) . ?
Cl1 O4 1.409(12) . ?
Cl1 O1 1.434(12) . ?
Cl1A O2A 1.366(10) . ?
Cl1A O4A 1.388(11) . ?
Cl1A O3A 1.410(11) . ?
Cl1A O1A 1.441(11) . ?
Cl2 O6 1.406(8) . ?
Cl2 O8 1.424(11) . ?
Cl2 O7 1.433(8) . ?
Cl2 O5 1.438(6) . ?
O1S C1S 1.393(19) . ?
C1S C2S 1.60(4) . ?
C2S C3S 1.46(4) . ?
O1SA C1SA 1.42(2) . ?
C1SA C2SA 1.47(2) . ?
C2SA C3SA 1.45(2) . ?
C2SA C3SA 1.82(10) 2 ?
C3SA C3SA 1.05(12) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 178.5(3) . . ?
N8 Fe1 N7 79.5(3) . . ?
N3 Fe1 N7 99.1(3) . . ?
N8 Fe1 N4 101.4(2) . . ?
N3 Fe1 N4 78.7(2) . . ?
N7 Fe1 N4 90.9(2) . . ?
N8 Fe1 N2 100.6(3) . . ?
N3 Fe1 N2 79.2(2) . . ?
N7 Fe1 N2 92.7(2) . . ?
N4 Fe1 N2 158.0(3) . . ?
N8 Fe1 N9 79.3(3) . . ?
N3 Fe1 N9 102.1(3) . . ?
N7 Fe1 N9 158.8(3) . . ?
N4 Fe1 N9 93.7(2) . . ?
N2 Fe1 N9 90.8(2) . . ?
C2 O9 C1 117.9(6) . . ?
N2 N1 C8 111.2(6) . . ?
N2 N1 H1A 124.4 . . ?
C8 N1 H1A 124.4 . . ?
N1 N2 C10 107.3(5) . . ?
N1 N2 Fe1 137.3(5) . . ?
C10 N2 Fe1 114.9(5) . . ?
C15 N3 C11 121.1(6) . . ?
C15 N3 Fe1 120.0(5) . . ?
C11 N3 Fe1 118.9(5) . . ?
C16 N4 N5 104.9(5) . . ?
C16 N4 Fe1 116.5(4) . . ?
N5 N4 Fe1 138.4(5) . . ?
N4 N5 C18 111.9(6) . . ?
N4 N5 H5A 124.1 . . ?
C18 N5 H5A 124.1 . . ?
C26 N6 N7 111.6(7) . . ?
C26 N6 H6A 124.2 . . ?
N7 N6 H6A 124.2 . . ?
N6 N7 C28 104.8(6) . . ?
N6 N7 Fe1 138.7(6) . . ?
C28 N7 Fe1 116.5(5) . . ?
C29 N8 C33 120.6(7) . . ?
C29 N8 Fe1 119.8(5) . . ?
C33 N8 Fe1 119.6(6) . . ?
N10 N9 C34 105.6(6) . . ?
N10 N9 Fe1 138.1(5) . . ?
C34 N9 Fe1 116.2(5) . . ?
N9 N10 C36 111.1(7) . . ?
N9 N10 H10A 124.4 . . ?
C36 N10 H10A 124.4 . . ?
O9 C1 H1B 109.5 . . ?
O9 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O9 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
O9 C2 C7 116.3(6) . . ?
O9 C2 C3 123.2(7) . . ?
C7 C2 C3 120.5(7) . . ?
C4 C3 C2 120.1(8) . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C3 C4 C5 120.7(7) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C6 C5 C4 118.3(8) . . ?
C6 C5 H5B 120.8 . . ?
C4 C5 H5B 120.8 . . ?
C5 C6 C7 123.2(8) . . ?
C5 C6 H6B 118.4 . . ?
C7 C6 H6B 118.4 . . ?
C2 C7 C6 117.2(7) . . ?
C2 C7 C8 124.0(7) . . ?
C6 C7 C8 118.8(7) . . ?
C9 C8 N1 105.8(6) . . ?
C9 C8 C7 130.9(7) . . ?
N1 C8 C7 123.3(7) . . ?
C8 C9 C10 107.8(7) . . ?
C8 C9 H9A 126.1 . . ?
C10 C9 H9A 126.1 . . ?
N2 C10 C11 115.4(6) . . ?
N2 C10 C9 107.9(7) . . ?
C11 C10 C9 136.7(7) . . ?
N3 C11 C12 119.8(7) . . ?
N3 C11 C10 111.4(7) . . ?
C12 C11 C10 128.7(7) . . ?
C13 C12 C11 118.9(7) . . ?
C13 C12 H12A 120.5 . . ?
C11 C12 H12A 120.5 . . ?
C12 C13 C14 120.5(8) . . ?
C12 C13 H13A 119.8 . . ?
C14 C13 H13A 119.8 . . ?
C13 C14 C15 118.5(7) . . ?
C13 C14 H14A 120.8 . . ?
C15 C14 H14A 120.8 . . ?
N3 C15 C14 121.2(7) . . ?
N3 C15 C16 111.0(7) . . ?
C14 C15 C16 127.8(7) . . ?
N4 C16 C17 111.0(7) . . ?
N4 C16 C15 113.6(6) . . ?
C17 C16 C15 135.3(8) . . ?
C18 C17 C16 105.9(7) . . ?
C18 C17 H17A 127.1 . . ?
C16 C17 H17A 127.1 . . ?
N5 C18 C17 106.3(6) . . ?
N5 C18 C19A 136.3(15) . . ?
C17 C18 C19A 117.4(15) . . ?
N5 C18 C19 119.1(8) . . ?
C17 C18 C19 134.5(7) . . ?
C20 C19 C24 120.0 . . ?
C20 C19 C18 115.5(6) . . ?
C24 C19 C18 124.5(6) . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20A 120.0 . . ?
C21 C20 H20A 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21A 120.0 . . ?
C20 C21 H21A 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C21 C22 H22A 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
O10 C24 C23 123.3(7) . . ?
O10 C24 C19 116.7(7) . . ?
C23 C24 C19 120.0 . . ?
C24 O10 C25 117.4(10) . . ?
O10 C25 H25A 109.5 . . ?
O10 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O10 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24A C19A C18 118(3) . . ?
C24A C19A C20A 123(2) . . ?
C18 C19A C20A 119(2) . . ?
C21A C20A C19A 114(2) . . ?
C21A C20A H20B 122.8 . . ?
C19A C20A H20B 122.8 . . ?
C20A C21A C22A 113(3) . . ?
C20A C21A H21B 123.3 . . ?
C22A C21A H21B 123.3 . . ?
C23A C22A C21A 132(3) . . ?
C23A C22A H22B 114.2 . . ?
C21A C22A H22B 114.2 . . ?
C22A C23A C24A 113(3) . . ?
C22A C23A H23B 123.3 . . ?
C24A C23A H23B 123.3 . . ?
C19A C24A O10A 119(2) . . ?
C19A C24A C23A 124(3) . . ?
O10A C24A C23A 118(3) . . ?
C24A O10A C25A 116(2) . . ?
O10A C25A H25D 109.5 . . ?
O10A C25A H25E 109.5 . . ?
H25D C25A H25E 109.5 . . ?
O10A C25A H25F 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
N6 C26 C27 107.9(7) . . ?
N6 C26 H26A 126.0 . . ?
C27 C26 H26A 126.0 . . ?
C26 C27 C28 104.9(8) . . ?
C26 C27 H27A 127.6 . . ?
C28 C27 H27A 127.6 . . ?
N7 C28 C27 110.8(7) . . ?
N7 C28 C29 113.4(7) . . ?
C27 C28 C29 135.8(9) . . ?
N8 C29 C30 121.9(8) . . ?
N8 C29 C28 110.7(8) . . ?
C30 C29 C28 127.3(9) . . ?
C29 C30 C31 117.9(11) . . ?
C29 C30 H30A 121.1 . . ?
C31 C30 H30A 121.1 . . ?
C30 C31 C32 120.1(11) . . ?
C30 C31 H31A 119.9 . . ?
C32 C31 H31A 119.9 . . ?
C33 C32 C31 119.5(10) . . ?
C33 C32 H32A 120.2 . . ?
C31 C32 H32A 120.2 . . ?
N8 C33 C32 120.0(9) . . ?
N8 C33 C34 111.0(7) . . ?
C32 C33 C34 129.0(8) . . ?
N9 C34 C35 110.3(7) . . ?
N9 C34 C33 113.7(6) . . ?
C35 C34 C33 136.0(8) . . ?
C36 C35 C34 105.2(7) . . ?
C36 C35 H35A 127.4 . . ?
C34 C35 H35A 127.4 . . ?
C35 C36 N10 107.8(7) . . ?
C35 C36 H36A 126.1 . . ?
N10 C36 H36A 126.1 . . ?
O2 Cl1 O3 114.6(11) . . ?
O2 Cl1 O4 105.9(11) . . ?
O3 Cl1 O4 108.6(11) . . ?
O2 Cl1 O1 107.0(11) . . ?
O3 Cl1 O1 112.9(13) . . ?
O4 Cl1 O1 107.4(12) . . ?
O2A Cl1A O4A 124.4(12) . . ?
O2A Cl1A O3A 104.6(10) . . ?
O4A Cl1A O3A 102.9(10) . . ?
O2A Cl1A O1A 110.7(9) . . ?
O4A Cl1A O1A 106.4(11) . . ?
O3A Cl1A O1A 106.1(11) . . ?
O6 Cl2 O8 108.4(6) . . ?
O6 Cl2 O7 111.6(6) . . ?
O8 Cl2 O7 108.7(6) . . ?
O6 Cl2 O5 109.4(4) . . ?
O8 Cl2 O5 109.8(5) . . ?
O7 Cl2 O5 108.9(4) . . ?
O1S C1S C2S 116(2) . . ?
C3S C2S C1S 118(2) . . ?
O1SA C1SA C2SA 152(7) . . ?
C3SA C2SA C1SA 124(6) . . ?
C3SA C2SA C3SA 35(5) . 2 ?
C1SA C2SA C3SA 95(5) . 2 ?
C3SA C3SA C2SA 92(7) 2 . ?

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
N1 H1A O9 0.88 2.05 2.615(8) 121.2 . yes
N5 H5A O1S^c 0.88 1.82 2.66(2) 159.0 . yes
N6 H6A O2^a 0.88 2.26 2.70(2) 157.5 . yes
N10 H10A O5 0.88 1.90 2.772(9) 170.5 . yes

_refine_diff_density_max         0.895
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.087



####################################################################### 
# 
# 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_LBB15P13
_database_code_depnum_ccdc_archive 'CCDC 1996675'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2020-04-13 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Fe N10 O2, 2(Cl O4), 0.875(C3 H8 O)'
_chemical_formula_sum            'C38.62 H37 Cl2 Fe N10 O10.88'
_chemical_formula_weight         942.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1697 0.1896
'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2961(4)
_cell_length_b                   12.0540(4)
_cell_length_c                   17.1342(5)
_cell_angle_alpha                100.716(2)
_cell_angle_beta                 107.7683(19)
_cell_angle_gamma                108.3975(19)
_cell_volume                     2002.72(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      33.61

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_F_000             972
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.735
_shelx_estimated_absorpt_T_min   0.729
_shelx_estimated_absorpt_T_max   0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            34216
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.097
_diffrn_reflns_theta_max         33.744
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12234
_reflns_number_gt                8584
_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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were
 placed geometrically on their carrier atom and refined with a
 riding model, except those on the pyrazole and propanol 
  O and N donors that were refined with their thermal parameter 
 1.5 times that of their carrier atom and a distance restraint.
 One of the perchlorate ion is disordered
 over two positions (Cl1 and Cl1A, with relative occupancies
 0.81:0.19) and the two components were refined with distance 
 and displacement parameters restraints.  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0809P)²+2.4872P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12234
_refine_ls_number_parameters     632
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1730
_refine_ls_wR_factor_gt          0.1562
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.57615(4) 0.51693(3) 0.27128(2) 0.01660(10) Uani 1 1 d . . . . .
Cl1 Cl 0.92172(10) 0.74237(16) 0.62648(7) 0.0247(4) Uani 0.810(6) 1 d D U P A 1
O1 O 0.7980(4) 0.7258(4) 0.6402(3) 0.0262(8) Uani 0.810(6) 1 d D U P A 1
O2 O 0.8832(3) 0.6665(3) 0.54028(18) 0.0379(8) Uani 0.810(6) 1 d D U P A 1
O3 O 0.9934(3) 0.8674(3) 0.6369(2) 0.0411(8) Uani 0.810(6) 1 d D U P A 1
O4 O 1.0052(3) 0.7020(3) 0.6865(2) 0.0395(8) Uani 0.810(6) 1 d D U P A 1
Cl1A Cl 0.9050(7) 0.7914(9) 0.6153(4) 0.0464(18) Uani 0.190(6) 1 d D U P A 2
O1A O 0.7909(19) 0.758(2) 0.6396(17) 0.050(5) Uani 0.190(6) 1 d D U P A 2
O2A O 0.8661(17) 0.736(2) 0.5257(8) 0.071(5) Uani 0.190(6) 1 d D U P A 2
O3A O 0.959(2) 0.9195(14) 0.6335(13) 0.093(6) Uani 0.190(6) 1 d D U P A 2
O4A O 1.0071(17) 0.761(2) 0.6703(12) 0.082(5) Uani 0.190(6) 1 d D U P A 2
Cl2 Cl 0.96655(7) 0.61572(7) 0.15408(5) 0.03014(17) Uani 1 1 d . . . . .
O5 O 0.9068(2) 0.5187(2) 0.18690(14) 0.0327(5) Uani 1 1 d . . . . .
O6 O 0.9590(3) 0.5601(2) 0.07031(15) 0.0417(6) Uani 1 1 d . . . . .
O7 O 1.1045(2) 0.6872(2) 0.21181(17) 0.0459(6) Uani 1 1 d . . . . .
O8 O 0.8908(3) 0.6914(3) 0.14801(17) 0.0470(6) Uani 1 1 d . . . . .
O9 O 0.3596(2) 0.78861(18) 0.11052(13) 0.0263(4) Uani 1 1 d . . . . .
O10 O 0.3727(2) 0.0744(2) 0.34125(18) 0.0444(6) Uani 1 1 d . . . . .
N1 N 0.5473(2) 0.7373(2) 0.21191(14) 0.0204(4) Uani 1 1 d D . . . .
H1A H 0.4581(19) 0.709(3) 0.194(2) 0.031 Uiso 1 1 d D U . . .
N2 N 0.6162(2) 0.6790(2) 0.25345(14) 0.0197(4) Uani 1 1 d . . . . .
N3 N 0.7711(2) 0.5879(2) 0.32403(13) 0.0188(4) Uani 1 1 d . . . . .
N4 N 0.6118(2) 0.3797(2) 0.30999(13) 0.0183(4) Uani 1 1 d . . . . .
N5 N 0.5427(2) 0.2679(2) 0.31352(14) 0.0207(4) Uani 1 1 d D . . . .
H5B H 0.4530(19) 0.234(3) 0.288(2) 0.031 Uiso 1 1 d D U . . .
N6 N 0.5957(2) 0.6243(2) 0.45590(14) 0.0220(5) Uani 1 1 d D . . . .
H6B H 0.685(2) 0.643(3) 0.479(2) 0.033 Uiso 1 1 d D U . . .
N7 N 0.5306(2) 0.5671(2) 0.37042(14) 0.0192(4) Uani 1 1 d . . . . .
N8 N 0.3828(2) 0.4572(2) 0.21600(14) 0.0197(4) Uani 1 1 d . . . . .
N9 N 0.5484(2) 0.4413(2) 0.15180(14) 0.0193(4) Uani 1 1 d . . . . .
N10 N 0.6243(3) 0.4265(2) 0.10748(15) 0.0227(5) Uani 1 1 d D . . . .
H10A H 0.7153(19) 0.459(3) 0.136(2) 0.034 Uiso 1 1 d D U . . .
C1 C 0.2217(3) 0.7522(3) 0.0537(2) 0.0377(8) Uani 1 1 d . . . . .
H1B H 0.183665 0.806499 0.077240 0.057 Uiso 1 1 calc R U . . .
H1C H 0.168992 0.667108 0.048223 0.057 Uiso 1 1 calc R U . . .
H1D H 0.218156 0.758169 -0.003154 0.057 Uiso 1 1 calc R U . . .
C2 C 0.4505(3) 0.9038(3) 0.12315(18) 0.0236(5) Uani 1 1 d . . . . .
C3 C 0.4144(3) 0.9901(3) 0.0891(2) 0.0299(6) Uani 1 1 d . . . . .
H3A H 0.322454 0.970019 0.054311 0.036 Uiso 1 1 calc R U . . .
C4 C 0.5120(4) 1.1049(3) 0.1060(2) 0.0335(7) Uani 1 1 d . . . . .
H4A H 0.486529 1.163425 0.082785 0.040 Uiso 1 1 calc R U . . .
C5 C 0.6463(4) 1.1356(3) 0.1562(2) 0.0325(7) Uani 1 1 d . . . . .
H5A H 0.712770 1.214807 0.167525 0.039 Uiso 1 1 calc R U . . .
C6 C 0.6833(3) 1.0500(3) 0.18972(19) 0.0281(6) Uani 1 1 d . . . . .
H6A H 0.775651 1.071061 0.224107 0.034 Uiso 1 1 calc R U . . .
C7 C 0.5869(3) 0.9332(2) 0.17385(17) 0.0231(5) Uani 1 1 d . . . . .
C8 C 0.6325(3) 0.8467(2) 0.21178(17) 0.0216(5) Uani 1 1 d . . . . .
C9 C 0.7623(3) 0.8570(3) 0.25456(18) 0.0239(6) Uani 1 1 d . . . . .
H9A H 0.844522 0.922502 0.264943 0.029 Uiso 1 1 calc R U . . .
C10 C 0.7478(3) 0.7513(2) 0.27951(17) 0.0217(5) Uani 1 1 d . . . . .
C11 C 0.8402(3) 0.7021(3) 0.32424(17) 0.0218(5) Uani 1 1 d . . . . .
C12 C 0.9806(3) 0.7562(3) 0.36208(19) 0.0280(6) Uani 1 1 d . . . . .
H12A H 1.028595 0.837373 0.363213 0.034 Uiso 1 1 calc R U . . .
C13 C 1.0493(3) 0.6897(3) 0.39812(19) 0.0293(6) Uani 1 1 d . . . . .
H13A H 1.145503 0.725024 0.423963 0.035 Uiso 1 1 calc R U . . .
C14 C 0.9786(3) 0.5717(3) 0.39677(18) 0.0262(6) Uani 1 1 d . . . . .
H14A H 1.025106 0.524987 0.420776 0.031 Uiso 1 1 calc R U . . .
C15 C 0.8379(3) 0.5235(3) 0.35934(16) 0.0209(5) Uani 1 1 d . . . . .
C16 C 0.7430(3) 0.4050(3) 0.35270(16) 0.0209(5) Uani 1 1 d . . . . .
C17 C 0.7591(3) 0.3100(3) 0.38405(17) 0.0244(6) Uani 1 1 d . . . . .
H17A H 0.841504 0.305827 0.416525 0.029 Uiso 1 1 calc R U . . .
C18 C 0.6296(3) 0.2232(3) 0.35775(17) 0.0243(6) Uani 1 1 d . . . . .
C19 C 0.5940(4) 0.1036(3) 0.3734(2) 0.0334(7) Uani 1 1 d . . . . .
C20 C 0.7041(4) 0.0642(3) 0.4038(2) 0.0355(7) Uani 1 1 d . . . . .
H20A H 0.793811 0.115380 0.413157 0.043 Uiso 1 1 calc R U . . .
C21 C 0.6783(4) -0.0471(4) 0.4191(2) 0.0454(9) Uani 1 1 d . . . . .
H21A H 0.748855 -0.074734 0.438111 0.054 Uiso 1 1 calc R U . . .
C22 C 0.5483(4) -0.1171(3) 0.4062(3) 0.0451(9) Uani 1 1 d . . . . .
H22A H 0.531202 -0.194077 0.416841 0.054 Uiso 1 1 calc R U . . .
C23 C 0.4438(4) -0.0850(4) 0.3798(3) 0.0485(9) Uani 1 1 d . . . . .
H23A H 0.355199 -0.137851 0.371318 0.058 Uiso 1 1 calc R U . . .
C24 C 0.4688(4) 0.0312(3) 0.3647(2) 0.0389(8) Uani 1 1 d . . . . .
C25 C 0.2432(4) 0.0063(4) 0.3424(3) 0.0483(9) Uani 1 1 d . . . . .
H25A H 0.206320 -0.078490 0.304350 0.072 Uiso 1 1 calc R U . . .
H25B H 0.180604 0.045257 0.322208 0.072 Uiso 1 1 calc R U . . .
H25C H 0.254552 0.005819 0.401337 0.072 Uiso 1 1 calc R U . . .
C26 C 0.5084(3) 0.6334(3) 0.49304(19) 0.0267(6) Uani 1 1 d . . . . .
H26A H 0.531382 0.669662 0.552663 0.032 Uiso 1 1 calc R U . . .
C27 C 0.3806(3) 0.5811(3) 0.42967(19) 0.0256(6) Uani 1 1 d . . . . .
H27A H 0.298041 0.574011 0.435861 0.031 Uiso 1 1 calc R U . . .
C28 C 0.3986(3) 0.5403(2) 0.35336(17) 0.0210(5) Uani 1 1 d . . . . .
C29 C 0.3108(3) 0.4790(3) 0.26266(18) 0.0229(5) Uani 1 1 d . . . . .
C30 C 0.1730(3) 0.4464(3) 0.2230(2) 0.0313(7) Uani 1 1 d . . . . .
H30A H 0.122193 0.461537 0.255736 0.038 Uiso 1 1 calc R U . . .
C31 C 0.1108(3) 0.3914(3) 0.1346(2) 0.0366(7) Uani 1 1 d . . . . .
H31A H 0.016112 0.368673 0.106224 0.044 Uiso 1 1 calc R U . . .
C32 C 0.1848(3) 0.3690(3) 0.0868(2) 0.0309(6) Uani 1 1 d . . . . .
H32A H 0.141954 0.331249 0.025997 0.037 Uiso 1 1 calc R U . . .
C33 C 0.3219(3) 0.4028(3) 0.12938(17) 0.0236(5) Uani 1 1 d . . . . .
C34 C 0.4200(3) 0.3931(2) 0.09314(17) 0.0218(5) Uani 1 1 d . . . . .
C35 C 0.4153(3) 0.3466(3) 0.00998(17) 0.0253(6) Uani 1 1 d . . . . .
H35A H 0.337876 0.307543 -0.042749 0.030 Uiso 1 1 calc R U . . .
C36 C 0.5475(3) 0.3706(3) 0.02240(18) 0.0260(6) Uani 1 1 d . . . . .
H36A H 0.579831 0.351286 -0.021264 0.031 Uiso 1 1 calc R U . . .
O1S O 0.2631(3) 0.1960(2) 0.21649(16) 0.0295(5) Uani 0.875 1 d D . P . .
H1S H 0.227(4) 0.209(4) 0.255(2) 0.044 Uiso 0.875 1 d D U P . .
C1S C 0.1645(4) 0.0815(4) 0.1568(2) 0.0377(9) Uani 0.875 1 d . . P . .
H1SA H 0.176807 0.014797 0.180031 0.045 Uiso 0.875 1 calc R U P . .
H1SB H 0.179190 0.069973 0.102300 0.045 Uiso 0.875 1 calc R U P . .
C2S C 0.0193(4) 0.0702(4) 0.1373(3) 0.0401(9) Uani 0.875 1 d . . P . .
H2SA H 0.007947 0.091117 0.192481 0.048 Uiso 0.875 1 calc R U P . .
H2SB H 0.004292 0.131212 0.108252 0.048 Uiso 0.875 1 calc R U P . .
C3S C -0.0867(5) -0.0550(4) 0.0816(3) 0.0553(13) Uani 0.875 1 d . . P . .
H3SA H -0.176831 -0.055143 0.071963 0.083 Uiso 0.875 1 calc R U P . .
H3SB H -0.078075 -0.075826 0.026123 0.083 Uiso 0.875 1 calc R U P . .
H3SC H -0.074415 -0.115979 0.110473 0.083 Uiso 0.875 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N8 1.917(2) . ?
Fe1 N3 1.925(2) . ?
Fe1 N9 1.963(2) . ?
Fe1 N2 1.966(2) . ?
Fe1 N7 1.966(2) . ?
Fe1 N4 2.001(2) . ?
Cl1 O3 1.415(3) . ?
Cl1 O2 1.436(3) . ?
Cl1 O4 1.438(3) . ?
Cl1 O1 1.445(3) . ?
Cl1A O3A 1.401(12) . ?
Cl1A O2A 1.420(11) . ?
Cl1A O1A 1.436(12) . ?
Cl1A O4A 1.441(11) . ?
Cl2 O7 1.430(2) . ?
Cl2 O8 1.431(3) . ?
Cl2 O6 1.431(2) . ?
Cl2 O5 1.455(2) . ?
O9 C2 1.372(3) . ?
O9 C1 1.432(4) . ?
O10 C24 1.334(4) . ?
O10 C25 1.442(4) . ?
N1 N2 1.341(3) . ?
N1 C8 1.365(3) . ?
N1 H1A 0.884(18) . ?
N2 C10 1.342(4) . ?
N3 C15 1.343(3) . ?
N3 C11 1.349(3) . ?
N4 C16 1.340(3) . ?
N4 N5 1.350(3) . ?
N5 C18 1.364(4) . ?
N5 H5B 0.887(18) . ?
N6 N7 1.345(3) . ?
N6 C26 1.348(4) . ?
N6 H6B 0.893(18) . ?
N7 C28 1.344(4) . ?
N8 C29 1.350(4) . ?
N8 C33 1.355(3) . ?
N9 N10 1.337(3) . ?
N9 C34 1.347(3) . ?
N10 C36 1.351(4) . ?
N10 H10A 0.904(18) . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 C3 1.391(4) . ?
C2 C7 1.406(4) . ?
C3 C4 1.381(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.381(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.384(4) . ?
C5 H5A 0.9500 . ?
C6 C7 1.397(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.470(4) . ?
C8 C9 1.377(4) . ?
C9 C10 1.396(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.449(4) . ?
C11 C12 1.387(4) . ?
C12 C13 1.383(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.386(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.390(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.450(4) . ?
C16 C17 1.391(4) . ?
C17 C18 1.376(4) . ?
C17 H17A 0.9500 . ?
C18 C19 1.468(4) . ?
C19 C24 1.352(5) . ?
C19 C20 1.454(5) . ?
C20 C21 1.372(5) . ?
C20 H20A 0.9500 . ?
C21 C22 1.367(6) . ?
C21 H21A 0.9500 . ?
C22 C23 1.332(6) . ?
C22 H22A 0.9500 . ?
C23 C24 1.427(5) . ?
C23 H23A 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.369(4) . ?
C26 H26A 0.9500 . ?
C27 C28 1.406(4) . ?
C27 H27A 0.9500 . ?
C28 C29 1.454(4) . ?
C29 C30 1.382(4) . ?
C30 C31 1.383(5) . ?
C30 H30A 0.9500 . ?
C31 C32 1.386(5) . ?
C31 H31A 0.9500 . ?
C32 C33 1.378(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.450(4) . ?
C34 C35 1.409(4) . ?
C35 C36 1.368(4) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
O1S C1S 1.415(5) . ?
O1S H1S 0.883(19) . ?
C1S C2S 1.526(6) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S C3S 1.500(6) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 175.59(9) . . ?
N8 Fe1 N9 79.43(9) . . ?
N3 Fe1 N9 100.07(9) . . ?
N8 Fe1 N2 96.47(9) . . ?
N3 Fe1 N2 79.14(9) . . ?
N9 Fe1 N2 90.44(9) . . ?
N8 Fe1 N7 79.34(9) . . ?
N3 Fe1 N7 101.18(9) . . ?
N9 Fe1 N7 158.75(10) . . ?
N2 Fe1 N7 93.04(9) . . ?
N8 Fe1 N4 105.26(9) . . ?
N3 Fe1 N4 79.13(9) . . ?
N9 Fe1 N4 93.29(9) . . ?
N2 Fe1 N4 158.27(10) . . ?
N7 Fe1 N4 91.21(9) . . ?
O3 Cl1 O2 110.8(2) . . ?
O3 Cl1 O4 109.8(2) . . ?
O2 Cl1 O4 109.1(2) . . ?
O3 Cl1 O1 110.5(2) . . ?
O2 Cl1 O1 106.8(2) . . ?
O4 Cl1 O1 109.8(2) . . ?
O3A Cl1A O2A 108.6(12) . . ?
O3A Cl1A O1A 108.0(13) . . ?
O2A Cl1A O1A 111.4(12) . . ?
O3A Cl1A O4A 107.1(11) . . ?
O2A Cl1A O4A 114.1(12) . . ?
O1A Cl1A O4A 107.6(12) . . ?
O7 Cl2 O8 110.32(17) . . ?
O7 Cl2 O6 110.47(16) . . ?
O8 Cl2 O6 109.78(16) . . ?
O7 Cl2 O5 109.16(14) . . ?
O8 Cl2 O5 108.52(15) . . ?
O6 Cl2 O5 108.55(15) . . ?
C2 O9 C1 117.9(2) . . ?
C24 O10 C25 117.1(3) . . ?
N2 N1 C8 111.6(2) . . ?
N2 N1 H1A 121(2) . . ?
C8 N1 H1A 127(2) . . ?
N1 N2 C10 105.9(2) . . ?
N1 N2 Fe1 137.45(18) . . ?
C10 N2 Fe1 116.10(18) . . ?
C15 N3 C11 120.2(2) . . ?
C15 N3 Fe1 120.16(18) . . ?
C11 N3 Fe1 119.62(18) . . ?
C16 N4 N5 105.7(2) . . ?
C16 N4 Fe1 114.48(17) . . ?
N5 N4 Fe1 139.47(18) . . ?
N4 N5 C18 110.6(2) . . ?
N4 N5 H5B 120(2) . . ?
C18 N5 H5B 130(2) . . ?
N7 N6 C26 111.3(2) . . ?
N7 N6 H6B 117(2) . . ?
C26 N6 H6B 131(2) . . ?
C28 N7 N6 105.8(2) . . ?
C28 N7 Fe1 116.27(18) . . ?
N6 N7 Fe1 137.96(19) . . ?
C29 N8 C33 120.9(2) . . ?
C29 N8 Fe1 119.56(18) . . ?
C33 N8 Fe1 119.27(19) . . ?
N10 N9 C34 105.8(2) . . ?
N10 N9 Fe1 137.80(18) . . ?
C34 N9 Fe1 116.34(19) . . ?
N9 N10 C36 111.2(2) . . ?
N9 N10 H10A 119(2) . . ?
C36 N10 H10A 130(2) . . ?
O9 C1 H1B 109.5 . . ?
O9 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O9 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
O9 C2 C3 123.7(3) . . ?
O9 C2 C7 116.4(2) . . ?
C3 C2 C7 119.9(3) . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C5 C4 C3 120.9(3) . . ?
C5 C4 H4A 119.6 . . ?
C3 C4 H4A 119.6 . . ?
C4 C5 C6 119.5(3) . . ?
C4 C5 H5A 120.3 . . ?
C6 C5 H5A 120.3 . . ?
C5 C6 C7 121.1(3) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C6 C7 C2 118.7(3) . . ?
C6 C7 C8 118.4(3) . . ?
C2 C7 C8 122.9(2) . . ?
N1 C8 C9 106.4(2) . . ?
N1 C8 C7 124.2(3) . . ?
C9 C8 C7 129.4(3) . . ?
C8 C9 C10 105.7(2) . . ?
C8 C9 H9A 127.1 . . ?
C10 C9 H9A 127.1 . . ?
N2 C10 C9 110.4(2) . . ?
N2 C10 C11 114.4(2) . . ?
C9 C10 C11 135.1(3) . . ?
N3 C11 C12 121.1(3) . . ?
N3 C11 C10 110.5(2) . . ?
C12 C11 C10 128.4(3) . . ?
C13 C12 C11 118.6(3) . . ?
C13 C12 H12A 120.7 . . ?
C11 C12 H12A 120.7 . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 H13A 119.8 . . ?
C14 C13 H13A 119.8 . . ?
C13 C14 C15 118.2(3) . . ?
C13 C14 H14A 120.9 . . ?
C15 C14 H14A 120.9 . . ?
N3 C15 C14 121.4(3) . . ?
N3 C15 C16 110.4(2) . . ?
C14 C15 C16 128.2(3) . . ?
N4 C16 C17 111.2(2) . . ?
N4 C16 C15 115.8(2) . . ?
C17 C16 C15 133.0(3) . . ?
C18 C17 C16 105.0(2) . . ?
C18 C17 H17A 127.5 . . ?
C16 C17 H17A 127.5 . . ?
N5 C18 C17 107.5(2) . . ?
N5 C18 C19 127.1(3) . . ?
C17 C18 C19 125.5(3) . . ?
C24 C19 C20 118.5(3) . . ?
C24 C19 C18 124.8(3) . . ?
C20 C19 C18 116.6(3) . . ?
C21 C20 C19 119.9(4) . . ?
C21 C20 H20A 120.1 . . ?
C19 C20 H20A 120.1 . . ?
C22 C21 C20 118.2(4) . . ?
C22 C21 H21A 120.9 . . ?
C20 C21 H21A 120.9 . . ?
C23 C22 C21 124.6(4) . . ?
C23 C22 H22A 117.7 . . ?
C21 C22 H22A 117.7 . . ?
C22 C23 C24 118.1(4) . . ?
C22 C23 H23A 121.0 . . ?
C24 C23 H23A 121.0 . . ?
O10 C24 C19 116.3(3) . . ?
O10 C24 C23 123.0(3) . . ?
C19 C24 C23 120.6(3) . . ?
O10 C25 H25A 109.5 . . ?
O10 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O10 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 107.9(3) . . ?
N6 C26 H26A 126.0 . . ?
C27 C26 H26A 126.0 . . ?
C26 C27 C28 104.8(3) . . ?
C26 C27 H27A 127.6 . . ?
C28 C27 H27A 127.6 . . ?
N7 C28 C27 110.2(2) . . ?
N7 C28 C29 113.9(2) . . ?
C27 C28 C29 135.8(3) . . ?
N8 C29 C30 120.6(3) . . ?
N8 C29 C28 110.8(2) . . ?
C30 C29 C28 128.6(3) . . ?
C29 C30 C31 118.5(3) . . ?
C29 C30 H30A 120.7 . . ?
C31 C30 H30A 120.7 . . ?
C30 C31 C32 120.8(3) . . ?
C30 C31 H31A 119.6 . . ?
C32 C31 H31A 119.6 . . ?
C33 C32 C31 118.5(3) . . ?
C33 C32 H32A 120.8 . . ?
C31 C32 H32A 120.8 . . ?
N8 C33 C32 120.6(3) . . ?
N8 C33 C34 111.0(2) . . ?
C32 C33 C34 128.3(3) . . ?
N9 C34 C35 110.4(3) . . ?
N9 C34 C33 113.9(2) . . ?
C35 C34 C33 135.7(3) . . ?
C36 C35 C34 104.3(2) . . ?
C36 C35 H35A 127.8 . . ?
C34 C35 H35A 127.8 . . ?
N10 C36 C35 108.2(3) . . ?
N10 C36 H36A 125.9 . . ?
C35 C36 H36A 125.9 . . ?
C1S O1S H1S 102(3) . . ?
O1S C1S C2S 113.4(3) . . ?
O1S C1S H1SA 108.9 . . ?
C2S C1S H1SA 108.9 . . ?
O1S C1S H1SB 108.9 . . ?
C2S C1S H1SB 108.9 . . ?
H1SA C1S H1SB 107.7 . . ?
C3S C2S C1S 114.2(4) . . ?
C3S C2S H2SA 108.7 . . ?
C1S C2S H2SA 108.7 . . ?
C3S C2S H2SB 108.7 . . ?
C1S C2S H2SB 108.7 . . ?
H2SA C2S H2SB 107.6 . . ?
C2S C3S H3SA 109.5 . . ?
C2S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?

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
N1 H1A O9 0.884(18) 2.10(3) 2.622(3) 117(3) . yes
N5 H5B O1S 0.887(18) 1.97(2) 2.832(4) 164(3) . yes
N6 H6B O2^a 0.893(18) 1.82(4) 2.67(2) 159(3) . yes
N10 H10A O5 0.904(18) 1.894(19) 2.796(3) 175(3) . yes
O1S H1S O1^a 0.883(19) 1.86(4) 2.72(3) 163(4) 2_666 yes
O1S H1S O1A^b 0.883(19) 1.87(3) 2.72(2) 161(4) 2_666 yes

_refine_diff_density_max         1.238
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.096



####################################################################### 
# 
# 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_LBB15P
_database_code_depnum_ccdc_archive 'CCDC 1996674'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2020-04-13 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Fe N10 O2, 2(Cl O4), C3 H8 O'
_chemical_formula_sum            'C39 H38 Cl2 Fe N10 O11'
_chemical_formula_weight         949.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1697 0.1896
'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1233(5)
_cell_length_b                   11.9616(5)
_cell_length_c                   16.9794(7)
_cell_angle_alpha                100.602(2)
_cell_angle_beta                 105.946(2)
_cell_angle_gamma                107.618(2)
_cell_volume                     1980.42(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9863
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      37.96

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.744
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            41373
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.116
_diffrn_reflns_theta_max         38.035
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16425
_reflns_number_gt                11337
_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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were
 placed geometrically on their carrier atom and refined with a
 riding model, except those on the pyrazole and propanol 
  O and N donors that were found in a difference Fourier map and
 refined with their thermal parameter 1.5 times that of their carrier
 atom and a distance restraint.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0707P)²+1.4524P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16425
_refine_ls_number_parameters     585
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1558
_refine_ls_wR_factor_gt          0.1380
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.55842(3) 0.50924(2) 0.26703(2) 0.01214(6) Uani 1 1 d . . . . .
Cl1 Cl 0.90114(5) 0.78470(5) 0.60987(3) 0.02738(11) Uani 1 1 d . . . . .
O1 O 0.78329(17) 0.74067(17) 0.63262(11) 0.0322(4) Uani 1 1 d . . . . .
O2 O 0.8578(2) 0.7530(2) 0.51784(12) 0.0485(6) Uani 1 1 d . . . . .
O3 O 0.9625(2) 0.9140(2) 0.64428(15) 0.0605(7) Uani 1 1 d . . . . .
O4 O 0.9929(3) 0.7310(3) 0.64362(19) 0.0708(8) Uani 1 1 d . . . . .
Cl2 Cl 0.95618(5) 0.60349(5) 0.14821(3) 0.02641(11) Uani 1 1 d . . . . .
O5 O 0.88909(17) 0.50872(17) 0.18157(11) 0.0303(4) Uani 1 1 d . . . . .
O6 O 0.9461(2) 0.54744(18) 0.06359(11) 0.0405(5) Uani 1 1 d . . . . .
O7 O 0.8919(2) 0.6909(2) 0.14648(13) 0.0460(5) Uani 1 1 d . . . . .
O8 O 1.0940(2) 0.66214(19) 0.20292(14) 0.0470(5) Uani 1 1 d . . . . .
N1 N 0.53569(17) 0.73665(14) 0.21170(10) 0.0157(3) Uani 1 1 d D . . . .
H1D H 0.448(2) 0.708(2) 0.1917(17) 0.024 Uiso 1 1 d D U . . .
N2 N 0.60190(16) 0.67280(14) 0.24997(10) 0.0153(3) Uani 1 1 d . . . . .
N3 N 0.75152(16) 0.57468(14) 0.31968(10) 0.0142(3) Uani 1 1 d . . . . .
N4 N 0.58880(16) 0.37000(14) 0.30389(10) 0.0151(3) Uani 1 1 d . . . . .
N5 N 0.51280(18) 0.25835(14) 0.30464(11) 0.0170(3) Uani 1 1 d D . . . .
H5B H 0.425(2) 0.225(2) 0.2724(17) 0.025 Uiso 1 1 d D U . . .
N6 N 0.57356(18) 0.62268(15) 0.45006(10) 0.0178(3) Uani 1 1 d D . . . .
H6B H 0.6577(17) 0.658(2) 0.4696(17) 0.027 Uiso 1 1 d D U . . .
N7 N 0.50963(16) 0.56082(14) 0.36658(10) 0.0147(3) Uani 1 1 d . . . . .
N8 N 0.36586(16) 0.44894(14) 0.21538(10) 0.0159(3) Uani 1 1 d . . . . .
N9 N 0.53385(17) 0.43642(14) 0.14731(10) 0.0160(3) Uani 1 1 d . . . . .
N10 N 0.61167(18) 0.42375(15) 0.10142(11) 0.0184(3) Uani 1 1 d D . . . .
H10A H 0.6982(17) 0.455(2) 0.1256(17) 0.028 Uiso 1 1 d D U . . .
C1 C 0.2218(3) 0.7599(2) 0.05236(19) 0.0378(6) Uani 1 1 d . . . . .
H1A H 0.178039 0.809940 0.076610 0.057 Uiso 1 1 calc R U . . .
H1B H 0.170910 0.673097 0.043368 0.057 Uiso 1 1 calc R U . . .
H1C H 0.224252 0.773237 -0.002517 0.057 Uiso 1 1 calc R U . . .
C2 C 0.4476(2) 0.90921(19) 0.12445(13) 0.0222(4) Uani 1 1 d . . . . .
C3 C 0.4146(3) 0.9973(2) 0.08996(15) 0.0292(5) Uani 1 1 d . . . . .
H3A H 0.324638 0.978871 0.054181 0.035 Uiso 1 1 calc R U . . .
C4 C 0.5126(3) 1.1119(2) 0.10762(16) 0.0319(5) Uani 1 1 d . . . . .
H4A H 0.489374 1.171391 0.083385 0.038 Uiso 1 1 calc R U . . .
C5 C 0.6439(3) 1.1406(2) 0.16015(16) 0.0295(5) Uani 1 1 d . . . . .
H5A H 0.710278 1.219535 0.172195 0.035 Uiso 1 1 calc R U . . .
C6 C 0.6781(2) 1.05345(18) 0.19522(14) 0.0230(4) Uani 1 1 d . . . . .
H6A H 0.768143 1.073346 0.231515 0.028 Uiso 1 1 calc R U . . .
C7 C 0.5812(2) 0.93648(17) 0.17761(12) 0.0187(4) Uani 1 1 d . . . . .
C8 C 0.6232(2) 0.84701(16) 0.21380(12) 0.0168(3) Uani 1 1 d . . . . .
O9 O 0.35625(15) 0.79411(14) 0.11014(10) 0.0248(3) Uani 1 1 d . . . . .
C9 C 0.7515(2) 0.85285(17) 0.25514(13) 0.0190(4) Uani 1 1 d . . . . .
H9A H 0.834352 0.917715 0.266581 0.023 Uiso 1 1 calc R U . . .
O10 O 0.73543(19) 0.07831(16) 0.42822(12) 0.0337(4) Uani 1 1 d . . . . .
C10 C 0.73355(19) 0.74269(17) 0.27665(12) 0.0162(3) Uani 1 1 d . . . . .
C11 C 0.82294(19) 0.68752(17) 0.31892(12) 0.0162(3) Uani 1 1 d . . . . .
C12 C 0.9623(2) 0.73740(19) 0.35530(13) 0.0218(4) Uani 1 1 d . . . . .
H12A H 1.012003 0.817090 0.354644 0.026 Uiso 1 1 calc R U . . .
C13 C 1.0275(2) 0.6679(2) 0.39274(13) 0.0240(4) Uani 1 1 d . . . . .
H13A H 1.123068 0.700248 0.418117 0.029 Uiso 1 1 calc R U . . .
C14 C 0.9541(2) 0.5513(2) 0.39336(13) 0.0221(4) Uani 1 1 d . . . . .
H14A H 0.998224 0.503211 0.418669 0.026 Uiso 1 1 calc R U . . .
C15 C 0.81452(19) 0.50700(17) 0.35598(12) 0.0165(3) Uani 1 1 d . . . . .
C16 C 0.7171(2) 0.38870(17) 0.34877(12) 0.0168(3) Uani 1 1 d . . . . .
C17 C 0.7221(2) 0.28780(19) 0.37857(13) 0.0205(4) Uani 1 1 d . . . . .
H17A H 0.800063 0.277960 0.411858 0.025 Uiso 1 1 calc R U . . .
C18 C 0.5903(2) 0.20558(18) 0.34957(12) 0.0192(4) Uani 1 1 d . . . . .
C19 C 0.5259(2) 0.08383(19) 0.35944(14) 0.0238(4) Uani 1 1 d . . . . .
C20 C 0.3848(3) 0.0283(2) 0.32911(17) 0.0336(5) Uani 1 1 d . . . . .
H20A H 0.332304 0.071021 0.304474 0.040 Uiso 1 1 calc R U . . .
C21 C 0.3199(3) -0.0883(2) 0.3343(2) 0.0426(7) Uani 1 1 d . . . . .
H21A H 0.224315 -0.126034 0.311430 0.051 Uiso 1 1 calc R U . . .
C22 C 0.3962(3) -0.1478(2) 0.3730(2) 0.0424(7) Uani 1 1 d . . . . .
H22A H 0.352500 -0.227047 0.377066 0.051 Uiso 1 1 calc R U . . .
C23 C 0.5346(3) -0.0946(2) 0.40595(17) 0.0359(6) Uani 1 1 d . . . . .
H23A H 0.585678 -0.136503 0.433326 0.043 Uiso 1 1 calc R U . . .
C24 C 0.6008(3) 0.0221(2) 0.39912(15) 0.0279(5) Uani 1 1 d . . . . .
C25 C 0.8144(3) 0.0156(2) 0.46945(18) 0.0360(6) Uani 1 1 d . . . . .
H25A H 0.796228 0.006399 0.521697 0.054 Uiso 1 1 calc R U . . .
H25B H 0.910376 0.063273 0.484197 0.054 Uiso 1 1 calc R U . . .
H25C H 0.790152 -0.065601 0.430489 0.054 Uiso 1 1 calc R U . . .
C26 C 0.4853(2) 0.62906(19) 0.48932(13) 0.0215(4) Uani 1 1 d . . . . .
H26A H 0.507136 0.668467 0.548129 0.026 Uiso 1 1 calc R U . . .
C27 C 0.3575(2) 0.56844(19) 0.42933(13) 0.0213(4) Uani 1 1 d . . . . .
H27A H 0.274184 0.556959 0.437862 0.026 Uiso 1 1 calc R U . . .
C28 C 0.3772(2) 0.52749(17) 0.35310(12) 0.0166(3) Uani 1 1 d . . . . .
C29 C 0.2912(2) 0.46404(18) 0.26409(13) 0.0188(4) Uani 1 1 d . . . . .
C30 C 0.1525(2) 0.4273(2) 0.22841(15) 0.0274(4) Uani 1 1 d . . . . .
H30A H 0.100295 0.437031 0.263170 0.033 Uiso 1 1 calc R U . . .
C31 C 0.0921(2) 0.3760(2) 0.14037(16) 0.0326(5) Uani 1 1 d . . . . .
H31A H -0.002676 0.351390 0.114365 0.039 Uiso 1 1 calc R U . . .
C32 C 0.1680(2) 0.3598(2) 0.08959(15) 0.0284(5) Uani 1 1 d . . . . .
H32A H 0.126595 0.324761 0.029278 0.034 Uiso 1 1 calc R U . . .
C33 C 0.3065(2) 0.39679(18) 0.12995(12) 0.0199(4) Uani 1 1 d . . . . .
C34 C 0.4064(2) 0.38931(17) 0.09080(12) 0.0180(3) Uani 1 1 d . . . . .
C35 C 0.4047(2) 0.34625(19) 0.00787(12) 0.0224(4) Uani 1 1 d . . . . .
H35A H 0.328546 0.308906 -0.043670 0.027 Uiso 1 1 calc R U . . .
C36 C 0.5374(2) 0.36999(19) 0.01761(13) 0.0230(4) Uani 1 1 d . . . . .
H36A H 0.571077 0.351746 -0.026877 0.028 Uiso 1 1 calc R U . . .
O1S O 0.23053(19) 0.17152(16) 0.20782(12) 0.0333(4) Uani 1 1 d D . . . .
H1S H 0.205(3) 0.206(3) 0.252(2) 0.050 Uiso 1 1 d D U . . .
C1S C 0.1236(3) 0.0560(2) 0.15842(19) 0.0389(6) Uani 1 1 d . . . . .
H1SA H 0.120352 -0.001079 0.193958 0.047 Uiso 1 1 calc R U . . .
H1SB H 0.144397 0.021025 0.108579 0.047 Uiso 1 1 calc R U . . .
C2S C -0.0136(3) 0.0639(2) 0.12651(19) 0.0380(6) Uani 1 1 d . . . . .
H2SA H -0.033593 0.101466 0.175925 0.046 Uiso 1 1 calc R U . . .
H2SB H -0.012191 0.117733 0.088668 0.046 Uiso 1 1 calc R U . . .
C3S C -0.1233(3) -0.0595(3) 0.07821(18) 0.0411(6) Uani 1 1 d . . . . .
H3SA H -0.210099 -0.049941 0.058817 0.062 Uiso 1 1 calc R U . . .
H3SB H -0.104938 -0.096406 0.028509 0.062 Uiso 1 1 calc R U . . .
H3SC H -0.126339 -0.112672 0.115759 0.062 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N8 1.9176(16) . ?
Fe1 N3 1.9223(16) . ?
Fe1 N7 1.9635(16) . ?
Fe1 N2 1.9642(15) . ?
Fe1 N9 1.9658(16) . ?
Fe1 N4 1.9719(15) . ?
Cl1 O4 1.412(2) . ?
Cl1 O3 1.417(2) . ?
Cl1 O2 1.4407(19) . ?
Cl1 O1 1.4423(18) . ?
Cl2 O8 1.426(2) . ?
Cl2 O6 1.4277(18) . ?
Cl2 O7 1.435(2) . ?
Cl2 O5 1.4559(18) . ?
N1 N2 1.345(2) . ?
N1 C8 1.370(2) . ?
N1 H1D 0.87(2) . ?
N2 C10 1.343(2) . ?
N3 C15 1.348(2) . ?
N3 C11 1.348(2) . ?
N4 C16 1.346(2) . ?
N4 N5 1.352(2) . ?
N5 C18 1.367(2) . ?
N5 H5B 0.89(2) . ?
N6 C26 1.342(3) . ?
N6 N7 1.343(2) . ?
N6 H6B 0.839(17) . ?
N7 C28 1.344(3) . ?
N8 C29 1.349(3) . ?
N8 C33 1.349(2) . ?
N9 N10 1.336(2) . ?
N9 C34 1.348(2) . ?
N10 C36 1.348(3) . ?
N10 H10A 0.862(17) . ?
C1 O9 1.429(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O9 1.372(3) . ?
C2 C3 1.389(3) . ?
C2 C7 1.410(3) . ?
C3 C4 1.387(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.390(3) . ?
C5 H5A 0.9500 . ?
C6 C7 1.402(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.459(3) . ?
C8 C9 1.381(3) . ?
C9 C10 1.403(3) . ?
C9 H9A 0.9500 . ?
O10 C24 1.342(3) . ?
O10 C25 1.442(3) . ?
C10 C11 1.455(3) . ?
C11 C12 1.386(3) . ?
C12 C13 1.388(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.390(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.390(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.459(3) . ?
C16 C17 1.402(3) . ?
C17 C18 1.383(3) . ?
C17 H17A 0.9500 . ?
C18 C19 1.479(3) . ?
C19 C24 1.394(3) . ?
C19 C20 1.403(3) . ?
C20 C21 1.394(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.375(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.376(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.410(3) . ?
C23 H23A 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.376(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.397(3) . ?
C27 H27A 0.9500 . ?
C28 C29 1.456(3) . ?
C29 C30 1.385(3) . ?
C30 C31 1.387(3) . ?
C30 H30A 0.9500 . ?
C31 C32 1.389(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.391(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.459(3) . ?
C34 C35 1.400(3) . ?
C35 C36 1.372(3) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
O1S C1S 1.435(3) . ?
O1S H1S 0.95(3) . ?
C1S C2S 1.511(4) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S C3S 1.501(4) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 178.26(7) . . ?
N8 Fe1 N7 79.22(7) . . ?
N3 Fe1 N7 99.96(7) . . ?
N8 Fe1 N2 99.10(7) . . ?
N3 Fe1 N2 79.36(6) . . ?
N7 Fe1 N2 92.34(7) . . ?
N8 Fe1 N9 79.31(7) . . ?
N3 Fe1 N9 101.48(7) . . ?
N7 Fe1 N9 158.51(7) . . ?
N2 Fe1 N9 90.37(6) . . ?
N8 Fe1 N4 102.42(7) . . ?
N3 Fe1 N4 79.11(7) . . ?
N7 Fe1 N4 91.57(6) . . ?
N2 Fe1 N4 158.48(7) . . ?
N9 Fe1 N4 93.69(6) . . ?
O4 Cl1 O3 109.64(18) . . ?
O4 Cl1 O2 111.65(16) . . ?
O3 Cl1 O2 109.12(14) . . ?
O4 Cl1 O1 109.25(14) . . ?
O3 Cl1 O1 109.32(14) . . ?
O2 Cl1 O1 107.82(11) . . ?
O8 Cl2 O6 110.35(14) . . ?
O8 Cl2 O7 110.12(14) . . ?
O6 Cl2 O7 109.96(12) . . ?
O8 Cl2 O5 108.43(12) . . ?
O6 Cl2 O5 108.73(11) . . ?
O7 Cl2 O5 109.21(12) . . ?
N2 N1 C8 111.38(16) . . ?
N2 N1 H1D 120.1(18) . . ?
C8 N1 H1D 128.5(17) . . ?
C10 N2 N1 105.98(15) . . ?
C10 N2 Fe1 116.10(12) . . ?
N1 N2 Fe1 137.68(13) . . ?
C15 N3 C11 120.54(16) . . ?
C15 N3 Fe1 119.90(13) . . ?
C11 N3 Fe1 119.56(12) . . ?
C16 N4 N5 106.03(15) . . ?
C16 N4 Fe1 116.26(12) . . ?
N5 N4 Fe1 137.30(13) . . ?
N4 N5 C18 111.40(17) . . ?
N4 N5 H5B 119.9(17) . . ?
C18 N5 H5B 128.2(18) . . ?
C26 N6 N7 111.07(17) . . ?
C26 N6 H6B 128.3(19) . . ?
N7 N6 H6B 120.1(19) . . ?
N6 N7 C28 106.01(16) . . ?
N6 N7 Fe1 137.53(13) . . ?
C28 N7 Fe1 116.46(13) . . ?
C29 N8 C33 120.44(17) . . ?
C29 N8 Fe1 119.79(13) . . ?
C33 N8 Fe1 119.71(14) . . ?
N10 N9 C34 105.92(16) . . ?
N10 N9 Fe1 137.55(13) . . ?
C34 N9 Fe1 116.44(14) . . ?
N9 N10 C36 111.22(18) . . ?
N9 N10 H10A 120.0(19) . . ?
C36 N10 H10A 128.5(19) . . ?
O9 C1 H1A 109.5 . . ?
O9 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O9 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O9 C2 C3 123.5(2) . . ?
O9 C2 C7 116.54(17) . . ?
C3 C2 C7 119.9(2) . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C5 C4 C3 120.7(2) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C4 C5 C6 119.7(2) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
C5 C6 C7 120.7(2) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C6 C7 C2 118.79(18) . . ?
C6 C7 C8 118.59(19) . . ?
C2 C7 C8 122.61(18) . . ?
N1 C8 C9 106.68(16) . . ?
N1 C8 C7 124.04(18) . . ?
C9 C8 C7 129.28(18) . . ?
C2 O9 C1 118.39(17) . . ?
C8 C9 C10 105.38(17) . . ?
C8 C9 H9A 127.3 . . ?
C10 C9 H9A 127.3 . . ?
C24 O10 C25 117.44(19) . . ?
N2 C10 C9 110.58(17) . . ?
N2 C10 C11 114.24(16) . . ?
C9 C10 C11 135.17(18) . . ?
N3 C11 C12 121.33(17) . . ?
N3 C11 C10 110.61(16) . . ?
C12 C11 C10 128.06(17) . . ?
C11 C12 C13 118.28(19) . . ?
C11 C12 H12A 120.9 . . ?
C13 C12 H12A 120.9 . . ?
C12 C13 C14 120.50(19) . . ?
C12 C13 H13A 119.8 . . ?
C14 C13 H13A 119.8 . . ?
C15 C14 C13 118.26(19) . . ?
C15 C14 H14A 120.9 . . ?
C13 C14 H14A 120.9 . . ?
N3 C15 C14 121.10(18) . . ?
N3 C15 C16 110.68(16) . . ?
C14 C15 C16 128.22(17) . . ?
N4 C16 C17 110.18(17) . . ?
N4 C16 C15 113.84(16) . . ?
C17 C16 C15 135.97(18) . . ?
C18 C17 C16 105.88(17) . . ?
C18 C17 H17A 127.1 . . ?
C16 C17 H17A 127.1 . . ?
N5 C18 C17 106.51(16) . . ?
N5 C18 C19 119.88(19) . . ?
C17 C18 C19 133.60(19) . . ?
C24 C19 C20 118.3(2) . . ?
C24 C19 C18 122.1(2) . . ?
C20 C19 C18 119.56(19) . . ?
C21 C20 C19 121.5(2) . . ?
C21 C20 H20A 119.3 . . ?
C19 C20 H20A 119.3 . . ?
C22 C21 C20 119.0(3) . . ?
C22 C21 H21A 120.5 . . ?
C20 C21 H21A 120.5 . . ?
C21 C22 C23 121.1(2) . . ?
C21 C22 H22A 119.4 . . ?
C23 C22 H22A 119.4 . . ?
C22 C23 C24 120.0(2) . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
O10 C24 C19 116.8(2) . . ?
O10 C24 C23 123.2(2) . . ?
C19 C24 C23 120.0(2) . . ?
O10 C25 H25A 109.5 . . ?
O10 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O10 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 C27 107.91(18) . . ?
N6 C26 H26A 126.0 . . ?
C27 C26 H26A 126.0 . . ?
C26 C27 C28 104.79(18) . . ?
C26 C27 H27A 127.6 . . ?
C28 C27 H27A 127.6 . . ?
N7 C28 C27 110.23(18) . . ?
N7 C28 C29 113.82(17) . . ?
C27 C28 C29 135.88(19) . . ?
N8 C29 C30 121.44(19) . . ?
N8 C29 C28 110.62(17) . . ?
C30 C29 C28 127.9(2) . . ?
C29 C30 C31 117.9(2) . . ?
C29 C30 H30A 121.0 . . ?
C31 C30 H30A 121.0 . . ?
C30 C31 C32 121.1(2) . . ?
C30 C31 H31A 119.4 . . ?
C32 C31 H31A 119.4 . . ?
C31 C32 C33 117.8(2) . . ?
C31 C32 H32A 121.1 . . ?
C33 C32 H32A 121.1 . . ?
N8 C33 C32 121.2(2) . . ?
N8 C33 C34 110.83(17) . . ?
C32 C33 C34 127.93(19) . . ?
N9 C34 C35 110.26(19) . . ?
N9 C34 C33 113.57(17) . . ?
C35 C34 C33 136.16(19) . . ?
C36 C35 C34 104.64(18) . . ?
C36 C35 H35A 127.7 . . ?
C34 C35 H35A 127.7 . . ?
N10 C36 C35 107.96(19) . . ?
N10 C36 H36A 126.0 . . ?
C35 C36 H36A 126.0 . . ?
C1S O1S H1S 107(2) . . ?
O1S C1S C2S 114.0(2) . . ?
O1S C1S H1SA 108.7 . . ?
C2S C1S H1SA 108.7 . . ?
O1S C1S H1SB 108.7 . . ?
C2S C1S H1SB 108.7 . . ?
H1SA C1S H1SB 107.6 . . ?
C3S C2S C1S 112.3(2) . . ?
C3S C2S H2SA 109.1 . . ?
C1S C2S H2SA 109.1 . . ?
C3S C2S H2SB 109.1 . . ?
C1S C2S H2SB 109.1 . . ?
H2SA C2S H2SB 107.9 . . ?
C2S C3S H3SA 109.5 . . ?
C2S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?

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
N1 H1D O9 0.87(2) 2.10(3) 2.609(2) 116(2) . yes
N5 H5B O1S 0.89(2) 1.98(2) 2.864(3) 172(3) . yes
N6 H6B O2 0.839(17) 2.010(17) 2.848(3) 177(3) . yes
N10 H10A O5 0.862(17) 1.914(17) 2.774(2) 174(3) . yes
O1S H1S O1 0.95(3) 1.89(3) 2.783(3) 155(3) 2_666 yes

_refine_diff_density_max         1.195
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.100



####################################################################### 
# 
# 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_LBB15P15
_database_code_depnum_ccdc_archive 'CCDC 1996677'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2020-04-13 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Cl2 Fe N10 O10'
_chemical_formula_sum            'C36 H30 Cl2 Fe N10 O10'
_chemical_formula_weight         889.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074 'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1697 0.1896
'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5958(4)
_cell_length_b                   11.8395(4)
_cell_length_c                   17.0521(5)
_cell_angle_alpha                101.136(2)
_cell_angle_beta                 105.917(2)
_cell_angle_gamma                106.551(2)
_cell_volume                     1884.61(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7727
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      24.06

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_F_000             912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.773
_shelx_estimated_absorpt_T_min   0.718
_shelx_estimated_absorpt_T_max   0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            17136
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.119
_diffrn_reflns_theta_max         24.120
_diffrn_reflns_theta_full        24.120
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4597
_reflns_number_gt                3435
_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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were
 placed geometrically on their carrier atom and refined with a
 riding model, including those on the pyrazole and propanol 
  O and N donors. One of the perchlorate ion is disordered
 over two positions (Cl1 and Cl1A, with relative occupancies
 0.59:0.41). Both perchlorates were refined with distance and 
 displacement parameters restraints.
;

_vrf_THETM01_LBB15P15            
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.5274
RESPONSE: The crystal has suffered a transformation upon losing propanol
through a thermal treatment at 400 K. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.95 angstrom. All this leads to a
rather low value of thetamax and a poor though acceptable data
to parameters ratio of 7.93.
;

_vrf_PLAT088_LBB15P15            
;
PROBLEM:  Poor Data / Parameter Ratio ....................       7.93 Note
RESPONSE: The crystal has suffered a transformation upon losing propanol
through a thermal treatment at 400 K. This results in an
increased mosaicity and diffraction decreasing quickly. Indeed there
was significant diffraction only to 0.95 ansgtrom resolution, and
the present data were cut at 0.95 angstrom. All this leads to a
rather low value of thetamax and a poor though acceptable data
to parameters ratio of 7.93.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1163P)²+7.3914P] 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         4597
_refine_ls_number_parameters     580
_refine_ls_number_restraints     350
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0740
_refine_ls_wR_factor_ref         0.2161
_refine_ls_wR_factor_gt          0.1938
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.55561(10) 0.51700(8) 0.26642(6) 0.0315(4) Uani 1 1 d . . . . .
Cl1 Cl 0.8877(13) 0.7817(12) 0.6034(8) 0.070(3) Uani 0.412(10) 1 d D U P A 1
O1 O 0.777(2) 0.756(2) 0.6356(17) 0.067(4) Uani 0.412(10) 1 d D U P A 1
O2 O 0.8379(17) 0.7724(16) 0.5143(8) 0.078(4) Uani 0.412(10) 1 d D U P A 1
O3 O 1.0024(17) 0.8909(16) 0.6459(12) 0.112(5) Uani 0.412(10) 1 d D U P A 1
O4 O 0.9487(17) 0.6898(16) 0.6102(13) 0.100(4) Uani 0.412(10) 1 d D U P A 1
Cl1A Cl 0.9094(10) 0.8033(9) 0.6054(6) 0.079(2) Uani 0.588(10) 1 d D U P A 2
O1A O 0.7794(17) 0.7752(18) 0.6266(13) 0.092(4) Uani 0.588(10) 1 d D U P A 2
O2A O 0.8763(12) 0.7039(12) 0.5342(8) 0.091(4) Uani 0.588(10) 1 d D U P A 2
O3A O 0.9269(18) 0.9213(11) 0.5978(10) 0.131(4) Uani 0.588(10) 1 d D U P A 2
O4A O 1.0098(12) 0.8031(15) 0.6744(7) 0.106(4) Uani 0.588(10) 1 d D U P A 2
Cl2 Cl 0.9695(2) 0.6102(2) 0.14151(14) 0.0731(7) Uani 1 1 d . U . . .
O5 O 0.8985(6) 0.5287(6) 0.1821(4) 0.0740(17) Uani 1 1 d . U . . .
O6 O 0.9189(8) 0.5506(7) 0.0537(4) 0.099(2) Uani 1 1 d . U . . .
O7 O 1.1149(7) 0.6440(8) 0.1800(5) 0.116(3) Uani 1 1 d . U . . .
O8 O 0.9317(9) 0.7185(7) 0.1526(5) 0.105(2) Uani 1 1 d . U . . .
O9 O 0.3475(6) 0.7990(5) 0.1038(3) 0.0559(14) Uani 1 1 d . . . . .
O10 O 0.3238(6) 0.0590(5) 0.2689(4) 0.0638(16) Uani 1 1 d . . . . .
N1 N 0.5296(7) 0.7425(5) 0.2097(4) 0.0458(16) Uani 1 1 d . . . . .
H1A H 0.437802 0.717228 0.184817 0.055 Uiso 1 1 calc R U . . .
N2 N 0.5982(7) 0.6816(5) 0.2500(3) 0.0410(15) Uani 1 1 d . . . . .
N3 N 0.7588(6) 0.5844(5) 0.3197(3) 0.0373(14) Uani 1 1 d . . . . .
N4 N 0.5941(6) 0.3805(5) 0.3034(3) 0.0317(13) Uani 1 1 d . . . . .
N5 N 0.5200(6) 0.2673(5) 0.3038(3) 0.0340(13) Uani 1 1 d . . . . .
H5B H 0.428115 0.231803 0.279560 0.041 Uiso 1 1 calc R U . . .
N6 N 0.5709(6) 0.6298(5) 0.4482(4) 0.0371(14) Uani 1 1 d . . . . .
H6B H 0.662477 0.667972 0.472218 0.045 Uiso 1 1 calc R U . . .
N7 N 0.5045(6) 0.5663(5) 0.3663(3) 0.0335(14) Uani 1 1 d . . . . .
N8 N 0.3546(6) 0.4454(5) 0.2173(4) 0.0388(14) Uani 1 1 d . . . . .
N9 N 0.5301(6) 0.4421(4) 0.1470(3) 0.0330(13) Uani 1 1 d . . . . .
N10 N 0.6100(7) 0.4337(5) 0.1001(4) 0.0393(14) Uani 1 1 d . . . . .
H10A H 0.702442 0.462951 0.120201 0.047 Uiso 1 1 calc R U . . .
C1 C 0.2145(9) 0.7592(9) 0.0369(6) 0.072(3) Uani 1 1 d . . . . .
H1B H 0.164180 0.814110 0.049714 0.107 Uiso 1 1 calc R U . . .
H1C H 0.159013 0.674829 0.032412 0.107 Uiso 1 1 calc R U . . .
H1D H 0.228995 0.761399 -0.017178 0.107 Uiso 1 1 calc R U . . .
C2 C 0.4413(7) 0.9124(6) 0.1196(4) 0.0382(17) Uani 1 1 d . . . . .
C3 C 0.4076(10) 1.0023(8) 0.0811(5) 0.060(2) Uani 1 1 d . . . . .
H3A H 0.314977 0.982845 0.042999 0.072 Uiso 1 1 calc R U . . .
C4 C 0.5038(11) 1.1125(8) 0.0980(5) 0.058(2) Uani 1 1 d . . . . .
H4A H 0.477234 1.171493 0.073453 0.069 Uiso 1 1 calc R U . . .
C5 C 0.6482(11) 1.1455(8) 0.1527(5) 0.062(2) Uani 1 1 d . . . . .
H5A H 0.718564 1.223262 0.163836 0.074 Uiso 1 1 calc R U . . .
C6 C 0.6745(8) 1.0587(6) 0.1859(4) 0.0367(17) Uani 1 1 d . . . . .
H6A H 0.768088 1.077985 0.222599 0.044 Uiso 1 1 calc R U . . .
C7 C 0.5790(8) 0.9420(7) 0.1727(4) 0.0452(19) Uani 1 1 d . . . . .
C8 C 0.6266(8) 0.8544(5) 0.2130(4) 0.0359(18) Uani 1 1 d . . . . .
C9 C 0.7566(8) 0.8613(6) 0.2567(4) 0.0440(18) Uani 1 1 d . . . . .
H9A H 0.842721 0.926508 0.269165 0.053 Uiso 1 1 calc R U . . .
C10 C 0.7384(8) 0.7514(6) 0.2799(4) 0.0421(19) Uani 1 1 d . . . . .
C11 C 0.8318(8) 0.6992(7) 0.3227(5) 0.0460(19) Uani 1 1 d . . . . .
C12 C 0.9807(8) 0.7493(7) 0.3640(5) 0.046(2) Uani 1 1 d . . . . .
H12A H 1.033025 0.831070 0.367470 0.056 Uiso 1 1 calc R U . . .
C13 C 1.0454(9) 0.6788(8) 0.3978(5) 0.054(2) Uani 1 1 d . . . . .
H13A H 1.144881 0.710673 0.423884 0.065 Uiso 1 1 calc R U . . .
C14 C 0.9727(8) 0.5634(8) 0.3958(5) 0.051(2) Uani 1 1 d . . . . .
H14A H 1.020104 0.514950 0.420572 0.061 Uiso 1 1 calc R U . . .
C15 C 0.8269(7) 0.5169(7) 0.3568(4) 0.0387(17) Uani 1 1 d . . . . .
C16 C 0.7294(8) 0.3994(6) 0.3469(4) 0.0392(17) Uani 1 1 d . . . . .
C17 C 0.7383(9) 0.2980(7) 0.3744(4) 0.0418(18) Uani 1 1 d . . . . .
H17A H 0.821355 0.288460 0.406471 0.050 Uiso 1 1 calc R U . . .
C18 C 0.6040(9) 0.2146(7) 0.3462(4) 0.0423(19) Uani 1 1 d . . . . .
C19 C 0.5468(11) 0.0906(7) 0.3576(5) 0.052(2) Uani 1 1 d . U . . .
C20 C 0.6460(12) 0.0528(8) 0.4101(5) 0.069(2) Uani 1 1 d . U . . .
H20A H 0.742640 0.103365 0.435783 0.083 Uiso 1 1 calc R U . . .
C21 C 0.5929(14) -0.0657(9) 0.4224(6) 0.080(2) Uani 1 1 d . U . . .
H21A H 0.654176 -0.094965 0.457971 0.095 Uiso 1 1 calc R U . . .
C22 C 0.4572(14) -0.1344(9) 0.3836(6) 0.083(2) Uani 1 1 d . U . . .
H22A H 0.424994 -0.213166 0.391893 0.099 Uiso 1 1 calc R U . . .
C23 C 0.3606(12) -0.0986(8) 0.3324(6) 0.073(2) Uani 1 1 d . U . . .
H23A H 0.264533 -0.150761 0.306630 0.088 Uiso 1 1 calc R U . . .
C24 C 0.4081(10) 0.0176(7) 0.3193(5) 0.054(2) Uani 1 1 d . . . . .
C25 C 0.1777(10) -0.0157(9) 0.2304(7) 0.089(3) Uani 1 1 d . . . . .
H25A H 0.136613 -0.023240 0.274949 0.133 Uiso 1 1 calc R U . . .
H25B H 0.167051 -0.097804 0.197784 0.133 Uiso 1 1 calc R U . . .
H25C H 0.129351 0.022680 0.192045 0.133 Uiso 1 1 calc R U . . .
C26 C 0.4783(9) 0.6277(7) 0.4896(5) 0.0445(19) Uani 1 1 d . . . . .
H26A H 0.500839 0.665734 0.548589 0.053 Uiso 1 1 calc R U . . .
C27 C 0.3495(9) 0.5623(8) 0.4326(5) 0.052(2) Uani 1 1 d . . . . .
H27A H 0.263012 0.545885 0.442482 0.063 Uiso 1 1 calc R U . . .
C28 C 0.3687(8) 0.5229(7) 0.3547(5) 0.0435(19) Uani 1 1 d . . . . .
C29 C 0.2771(8) 0.4527(8) 0.2676(5) 0.050(2) Uani 1 1 d . . . . .
C30 C 0.1352(10) 0.3991(12) 0.2356(6) 0.093(3) Uani 1 1 d . U . . .
H30A H 0.081702 0.404148 0.271747 0.111 Uiso 1 1 calc R U . . .
C31 C 0.0700(11) 0.3373(12) 0.1501(7) 0.101(3) Uani 1 1 d . U . . .
H31A H -0.029636 0.300877 0.126555 0.121 Uiso 1 1 calc R U . . .
C32 C 0.1493(10) 0.3279(12) 0.0979(6) 0.093(3) Uani 1 1 d . U . . .
H32A H 0.104905 0.283196 0.039081 0.112 Uiso 1 1 calc R U . . .
C33 C 0.2935(8) 0.3845(7) 0.1332(5) 0.049(2) Uani 1 1 d . . . . .
C34 C 0.3969(8) 0.3866(6) 0.0929(4) 0.0388(18) Uani 1 1 d . . . . .
C35 C 0.3943(10) 0.3426(6) 0.0093(5) 0.050(2) Uani 1 1 d . . . . .
H35A H 0.313923 0.300069 -0.040978 0.060 Uiso 1 1 calc R U . . .
C36 C 0.5297(10) 0.3736(6) 0.0162(5) 0.047(2) Uani 1 1 d . . . . .
H36A H 0.563767 0.356853 -0.029195 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
Fe1 N8 1.917(6) . ?
Fe1 N3 1.940(6) . ?
Fe1 N4 1.951(5) . ?
Fe1 N7 1.959(5) . ?
Fe1 N2 1.964(5) . ?
Fe1 N9 1.967(5) . ?
Cl1 O3 1.390(13) . ?
Cl1 O1 1.408(12) . ?
Cl1 O4 1.422(13) . ?
Cl1 O2 1.436(12) . ?
Cl1A O4A 1.354(11) . ?
Cl1A O3A 1.392(11) . ?
Cl1A O2A 1.401(11) . ?
Cl1A O1A 1.483(11) . ?
Cl2 O7 1.398(7) . ?
Cl2 O6 1.401(6) . ?
Cl2 O8 1.443(9) . ?
Cl2 O5 1.452(6) . ?
O9 C2 1.347(8) . ?
O9 C1 1.429(10) . ?
O10 C24 1.330(10) . ?
O10 C25 1.431(11) . ?
N1 N2 1.318(8) . ?
N1 C8 1.407(9) . ?
N1 H1A 0.8800 . ?
N2 C10 1.369(9) . ?
N3 C11 1.343(9) . ?
N3 C15 1.353(9) . ?
N4 N5 1.349(7) . ?
N4 C16 1.351(9) . ?
N5 C18 1.357(9) . ?
N5 H5B 0.8800 . ?
N6 N7 1.328(7) . ?
N6 C26 1.355(9) . ?
N6 H6B 0.8800 . ?
N7 C28 1.326(9) . ?
N8 C29 1.347(9) . ?
N8 C33 1.349(9) . ?
N9 N10 1.325(7) . ?
N9 C34 1.341(9) . ?
N10 C36 1.368(9) . ?
N10 H10A 0.8800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 C7 1.391(10) . ?
C2 C3 1.431(11) . ?
C3 C4 1.327(12) . ?
C3 H3A 0.9500 . ?
C4 C5 1.449(13) . ?
C4 H4A 0.9500 . ?
C5 C6 1.326(10) . ?
C5 H5A 0.9500 . ?
C6 C7 1.392(10) . ?
C6 H6A 0.9500 . ?
C7 C8 1.479(10) . ?
C8 C9 1.345(10) . ?
C9 C10 1.409(10) . ?
C9 H9A 0.9500 . ?
C10 C11 1.421(11) . ?
C11 C12 1.426(11) . ?
C12 C13 1.339(11) . ?
C12 H12A 0.9500 . ?
C13 C14 1.352(11) . ?
C13 H13A 0.9500 . ?
C14 C15 1.393(10) . ?
C14 H14A 0.9500 . ?
C15 C16 1.425(10) . ?
C16 C17 1.388(10) . ?
C17 C18 1.369(11) . ?
C17 H17A 0.9500 . ?
C18 C19 1.493(11) . ?
C19 C24 1.365(12) . ?
C19 C20 1.419(12) . ?
C20 C21 1.434(12) . ?
C20 H20A 0.9500 . ?
C21 C22 1.331(15) . ?
C21 H21A 0.9500 . ?
C22 C23 1.374(14) . ?
C22 H22A 0.9500 . ?
C23 C24 1.407(11) . ?
C23 H23A 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.337(11) . ?
C26 H26A 0.9500 . ?
C27 C28 1.409(10) . ?
C27 H27A 0.9500 . ?
C28 C29 1.454(11) . ?
C29 C30 1.354(12) . ?
C30 C31 1.373(14) . ?
C30 H30A 0.9500 . ?
C31 C32 1.391(14) . ?
C31 H31A 0.9500 . ?
C32 C33 1.379(12) . ?
C32 H32A 0.9500 . ?
C33 C34 1.442(11) . ?
C34 C35 1.409(10) . ?
C35 C36 1.341(11) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Fe1 N3 177.2(2) . . ?
N8 Fe1 N4 99.3(2) . . ?
N3 Fe1 N4 78.2(2) . . ?
N8 Fe1 N7 79.3(2) . . ?
N3 Fe1 N7 99.4(2) . . ?
N4 Fe1 N7 90.6(2) . . ?
N8 Fe1 N2 103.5(2) . . ?
N3 Fe1 N2 79.0(3) . . ?
N4 Fe1 N2 157.2(3) . . ?
N7 Fe1 N2 93.3(2) . . ?
N8 Fe1 N9 79.3(2) . . ?
N3 Fe1 N9 102.0(2) . . ?
N4 Fe1 N9 93.5(2) . . ?
N7 Fe1 N9 158.5(3) . . ?
N2 Fe1 N9 91.0(2) . . ?
O3 Cl1 O1 118.2(15) . . ?
O3 Cl1 O4 102.9(14) . . ?
O1 Cl1 O4 107.8(13) . . ?
O3 Cl1 O2 109.0(12) . . ?
O1 Cl1 O2 111.8(13) . . ?
O4 Cl1 O2 106.3(13) . . ?
O4A Cl1A O3A 112.5(11) . . ?
O4A Cl1A O2A 111.9(11) . . ?
O3A Cl1A O2A 120.9(11) . . ?
O4A Cl1A O1A 105.1(11) . . ?
O3A Cl1A O1A 100.5(11) . . ?
O2A Cl1A O1A 103.3(9) . . ?
O7 Cl2 O6 113.7(5) . . ?
O7 Cl2 O8 109.7(5) . . ?
O6 Cl2 O8 107.2(5) . . ?
O7 Cl2 O5 109.3(4) . . ?
O6 Cl2 O5 108.5(4) . . ?
O8 Cl2 O5 108.4(5) . . ?
C2 O9 C1 119.0(6) . . ?
C24 O10 C25 118.0(7) . . ?
N2 N1 C8 109.1(6) . . ?
N2 N1 H1A 125.5 . . ?
C8 N1 H1A 125.5 . . ?
N1 N2 C10 107.7(6) . . ?
N1 N2 Fe1 137.5(5) . . ?
C10 N2 Fe1 114.4(5) . . ?
C11 N3 C15 119.7(6) . . ?
C11 N3 Fe1 120.4(5) . . ?
C15 N3 Fe1 119.9(4) . . ?
N5 N4 C16 105.1(5) . . ?
N5 N4 Fe1 137.7(4) . . ?
C16 N4 Fe1 117.0(4) . . ?
N4 N5 C18 112.0(6) . . ?
N4 N5 H5B 124.0 . . ?
C18 N5 H5B 124.0 . . ?
N7 N6 C26 110.7(6) . . ?
N7 N6 H6B 124.6 . . ?
C26 N6 H6B 124.6 . . ?
C28 N7 N6 106.8(5) . . ?
C28 N7 Fe1 115.9(5) . . ?
N6 N7 Fe1 137.2(5) . . ?
C29 N8 C33 121.1(7) . . ?
C29 N8 Fe1 119.7(5) . . ?
C33 N8 Fe1 119.2(5) . . ?
N10 N9 C34 105.9(5) . . ?
N10 N9 Fe1 137.8(5) . . ?
C34 N9 Fe1 116.2(5) . . ?
N9 N10 C36 111.1(6) . . ?
N9 N10 H10A 124.5 . . ?
C36 N10 H10A 124.5 . . ?
O9 C1 H1B 109.5 . . ?
O9 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O9 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
O9 C2 C7 118.7(6) . . ?
O9 C2 C3 123.1(7) . . ?
C7 C2 C3 118.1(7) . . ?
C4 C3 C2 121.0(9) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C3 C4 C5 122.0(7) . . ?
C3 C4 H4A 119.0 . . ?
C5 C4 H4A 119.0 . . ?
C6 C5 C4 114.7(8) . . ?
C6 C5 H5A 122.7 . . ?
C4 C5 H5A 122.7 . . ?
C5 C6 C7 126.8(8) . . ?
C5 C6 H6A 116.6 . . ?
C7 C6 H6A 116.6 . . ?
C2 C7 C6 117.4(6) . . ?
C2 C7 C8 122.7(7) . . ?
C6 C7 C8 119.9(7) . . ?
C9 C8 N1 108.5(6) . . ?
C9 C8 C7 130.6(6) . . ?
N1 C8 C7 121.0(7) . . ?
C8 C9 C10 105.6(6) . . ?
C8 C9 H9A 127.2 . . ?
C10 C9 H9A 127.2 . . ?
N2 C10 C9 109.2(7) . . ?
N2 C10 C11 116.5(6) . . ?
C9 C10 C11 134.2(7) . . ?
N3 C11 C10 109.5(6) . . ?
N3 C11 C12 120.0(7) . . ?
C10 C11 C12 130.4(7) . . ?
C13 C12 C11 118.7(7) . . ?
C13 C12 H12A 120.6 . . ?
C11 C12 H12A 120.6 . . ?
C12 C13 C14 121.6(8) . . ?
C12 C13 H13A 119.2 . . ?
C14 C13 H13A 119.2 . . ?
C13 C14 C15 118.9(8) . . ?
C13 C14 H14A 120.6 . . ?
C15 C14 H14A 120.6 . . ?
N3 C15 C14 121.0(7) . . ?
N3 C15 C16 110.2(6) . . ?
C14 C15 C16 128.8(7) . . ?
N4 C16 C17 110.2(6) . . ?
N4 C16 C15 114.6(6) . . ?
C17 C16 C15 135.2(7) . . ?
C18 C17 C16 106.5(6) . . ?
C18 C17 H17A 126.8 . . ?
C16 C17 H17A 126.8 . . ?
N5 C18 C17 106.3(6) . . ?
N5 C18 C19 122.3(7) . . ?
C17 C18 C19 131.4(7) . . ?
C24 C19 C20 122.1(8) . . ?
C24 C19 C18 122.2(7) . . ?
C20 C19 C18 115.7(9) . . ?
C19 C20 C21 116.6(10) . . ?
C19 C20 H20A 121.7 . . ?
C21 C20 H20A 121.7 . . ?
C22 C21 C20 119.5(10) . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C21 C22 C23 124.2(10) . . ?
C21 C22 H22A 117.9 . . ?
C23 C22 H22A 117.9 . . ?
C22 C23 C24 118.1(10) . . ?
C22 C23 H23A 121.0 . . ?
C24 C23 H23A 121.0 . . ?
O10 C24 C19 117.8(6) . . ?
O10 C24 C23 122.6(9) . . ?
C19 C24 C23 119.5(9) . . ?
O10 C25 H25A 109.5 . . ?
O10 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O10 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N6 107.6(7) . . ?
C27 C26 H26A 126.2 . . ?
N6 C26 H26A 126.2 . . ?
C26 C27 C28 105.7(7) . . ?
C26 C27 H27A 127.1 . . ?
C28 C27 H27A 127.1 . . ?
N7 C28 C27 109.2(7) . . ?
N7 C28 C29 115.1(6) . . ?
C27 C28 C29 135.7(8) . . ?
N8 C29 C30 121.2(8) . . ?
N8 C29 C28 109.8(6) . . ?
C30 C29 C28 129.0(8) . . ?
C29 C30 C31 119.0(9) . . ?
C29 C30 H30A 120.5 . . ?
C31 C30 H30A 120.5 . . ?
C30 C31 C32 120.2(10) . . ?
C30 C31 H31A 119.9 . . ?
C32 C31 H31A 119.9 . . ?
C33 C32 C31 118.8(9) . . ?
C33 C32 H32A 120.6 . . ?
C31 C32 H32A 120.6 . . ?
N8 C33 C32 119.6(8) . . ?
N8 C33 C34 111.3(6) . . ?
C32 C33 C34 129.0(8) . . ?
N9 C34 C35 110.2(7) . . ?
N9 C34 C33 113.9(6) . . ?
C35 C34 C33 135.9(7) . . ?
C36 C35 C34 105.1(7) . . ?
C36 C35 H35A 127.4 . . ?
C34 C35 H35A 127.4 . . ?
C35 C36 N10 107.8(7) . . ?
C35 C36 H36A 126.1 . . ?
N10 C36 H36A 126.1 . . ?

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
N1 H1A O9 0.88 2.02 2.593(8) 121.7 . yes
N5 H5B O10 0.88 1.97 2.567(7) 123.5 . yes
N6 H6B O2^a 0.88 1.77 2.945(15) 167.4 . yes
N10 H10A O5 0.88 1.90 2.767(9) 170.2 . yes

_refine_diff_density_max         0.929
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.097



