# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

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

data_DH43F_FeBa
_database_code_depnum_ccdc_archive 'CCDC 1834781'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;

_audit_creation_date             2017-12-07T14:54:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C42 H44 Ba Cl8 Fe2 O6 S8'
_chemical_formula_sum            'C42 H44 Ba Cl8 Fe2 O6 S8'
_chemical_formula_weight         1433.89
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.672(3)
_cell_length_b                   10.887(3)
_cell_length_c                   25.613(2)
_cell_angle_alpha                94.871(12)
_cell_angle_beta                 97.871(11)
_cell_angle_gamma                94.413(15)
_cell_volume                     2925.1(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    3420
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark blue'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.213
0 2 -1 0.159
0 -3 2 0.161
0 0 -1 0.16
-6 1 2 0.091
10 -2 -3 0.054


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    1.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.248
_exptl_absorpt_correction_T_max  0.31

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_number            38379
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.011
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.972
_reflns_Friedel_coverage         0
_reflns_number_total             10277
_reflns_number_gt                6663
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+35.9810P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10277
_refine_ls_number_parameters     580
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.134
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_ref         0.1668
_refine_ls_wR_factor_gt          0.1412
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.435
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.145

#----------------------------------------------------------------------------#
#                   start Validation Reply Form                               #
#----------------------------------------------------------------------------#

_vrf_PLAT910_DH43F_FeBa          
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).21 Note
RESPONSE: Most of them are below the value of theta minimum in the data 
collection.
;
# end Validation Reply Form


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2351(9) -0.0358(10) 0.1023(3) 0.037(2) Uani 1 1 d . . . . .
C2 C 0.2106(10) -0.1178(10) 0.0560(4) 0.043(3) Uani 1 1 d . . . . .
C3 C 0.1763(11) -0.0753(13) 0.0072(4) 0.061(3) Uani 1 1 d . . . . .
H3 H 0.160898 -0.131472 -0.023962 0.073 Uiso 1 1 calc R U . . .
C4 C 0.1645(12) 0.0481(13) 0.0040(4) 0.061(3) Uani 1 1 d . . . . .
H4 H 0.140649 0.077044 -0.029566 0.073 Uiso 1 1 calc R U . . .
C5 C 0.1868(11) 0.1320(11) 0.0488(4) 0.050(3) Uani 1 1 d . . . . .
C6 C 0.2234(9) 0.0917(10) 0.0991(4) 0.038(2) Uani 1 1 d . . . . .
C7 C 0.3632(8) 0.0585(9) 0.3424(3) 0.034(2) Uani 1 1 d . . . . .
C8 C 0.3772(10) 0.0108(10) 0.3915(4) 0.045(3) Uani 1 1 d . . . . .
C9 C 0.3822(10) 0.0890(12) 0.4382(4) 0.050(3) Uani 1 1 d . . . . .
H9 H 0.395676 0.056612 0.47158 0.06 Uiso 1 1 calc R U . . .
C10 C 0.3673(10) 0.2157(12) 0.4355(4) 0.050(3) Uani 1 1 d . . . . .
H10 H 0.366975 0.26906 0.466825 0.06 Uiso 1 1 calc R U . . .
C11 C 0.3530(9) 0.2606(9) 0.3867(4) 0.042(3) Uani 1 1 d . . . . .
C12 C 0.3512(9) 0.1862(9) 0.3396(4) 0.036(2) Uani 1 1 d . . . . .
C13 C 0.5638(9) 0.1834(9) 0.1447(3) 0.032(2) Uani 1 1 d . . . . .
C14 C 0.5610(10) 0.1102(9) 0.0955(4) 0.040(2) Uani 1 1 d . . . . .
C15 C 0.5521(10) 0.1639(10) 0.0488(4) 0.043(3) Uani 1 1 d . . . . .
H15 H 0.551917 0.114114 0.016467 0.052 Uiso 1 1 calc R U . . .
C16 C 0.5434(11) 0.2896(11) 0.0482(4) 0.048(3) Uani 1 1 d . . . . .
H16 H 0.5337 0.325455 0.015537 0.058 Uiso 1 1 calc R U . . .
C17 C 0.5487(10) 0.3637(9) 0.0956(4) 0.041(3) Uani 1 1 d . . . . .
C18 C 0.5590(9) 0.3132(9) 0.1439(3) 0.033(2) Uani 1 1 d . . . . .
C19 C 0.6793(9) 0.2469(9) 0.3860(3) 0.034(2) Uani 1 1 d . . . . .
C20 C 0.7028(9) 0.1988(10) 0.4345(4) 0.042(3) Uani 1 1 d . . . . .
C21 C 0.7065(11) 0.2708(13) 0.4816(4) 0.061(4) Uani 1 1 d . . . . .
H21 H 0.720937 0.235266 0.514239 0.074 Uiso 1 1 calc R U . . .
C22 C 0.6889(11) 0.3959(12) 0.4810(4) 0.055(3) Uani 1 1 d . . . . .
H22 H 0.688851 0.445594 0.513293 0.066 Uiso 1 1 calc R U . . .
C23 C 0.6717(11) 0.4474(11) 0.4342(4) 0.053(3) Uani 1 1 d . . . . .
C24 C 0.6619(9) 0.3764(9) 0.3852(4) 0.036(2) Uani 1 1 d . . . . .
C25 C 1.0062(12) 0.3048(12) 0.3874(5) 0.0645(19) Uani 1 1 d . . . . .
C26 C 1.0245(14) 0.1704(13) 0.3921(7) 0.097(5) Uani 1 1 d . . . . .
H26A H 0.95199 0.119014 0.371573 0.145 Uiso 1 1 calc R U . . .
H26B H 1.03091 0.154117 0.429391 0.145 Uiso 1 1 calc R U . . .
H26C H 1.102673 0.150367 0.378433 0.145 Uiso 1 1 calc R U . . .
C27 C 1.0206(13) 0.3877(14) 0.4368(5) 0.085(5) Uani 1 1 d . . . . .
H27A H 1.033349 0.473765 0.428741 0.128 Uiso 1 1 calc R U . . .
H27B H 1.094124 0.367742 0.460886 0.128 Uiso 1 1 calc R U . . .
H27C H 0.943844 0.376631 0.453592 0.128 Uiso 1 1 calc R U . . .
C28 C 0.9233(13) 0.1459(12) 0.1958(6) 0.073(2) Uani 1 1 d . . . . .
C29 C 0.9077(14) 0.1120(19) 0.1385(5) 0.128(8) Uani 1 1 d . . . . .
H29A H 0.838878 0.045809 0.128629 0.193 Uiso 1 1 calc R U . . .
H29B H 0.986933 0.083228 0.128797 0.193 Uiso 1 1 calc R U . . .
H29C H 0.886971 0.184438 0.119879 0.193 Uiso 1 1 calc R U . . .
C30 C 0.9495(17) 0.0496(15) 0.2311(7) 0.117(7) Uani 1 1 d . . . . .
H30A H 1.041533 0.049342 0.241007 0.176 Uiso 1 1 calc R U . . .
H30B H 0.914627 -0.031178 0.213017 0.176 Uiso 1 1 calc R U . . .
H30C H 0.910044 0.065962 0.263101 0.176 Uiso 1 1 calc R U . . .
C31 C 1.0104(15) 0.7462(13) 0.3655(6) 0.083(2) Uani 1 1 d . . . . .
C32 C 1.0044(17) 0.8013(15) 0.4200(6) 0.113(6) Uani 1 1 d . . . . .
H32A H 0.936227 0.856824 0.419095 0.17 Uiso 1 1 calc R U . . .
H32B H 1.08561 0.848197 0.434309 0.17 Uiso 1 1 calc R U . . .
H32C H 0.987252 0.735281 0.442444 0.17 Uiso 1 1 calc R U . . .
C33 C 1.0493(15) 0.8298(14) 0.3275(7) 0.105(6) Uani 1 1 d . . . . .
H33A H 1.119623 0.797424 0.311289 0.158 Uiso 1 1 calc R U . . .
H33B H 1.076789 0.91209 0.345833 0.158 Uiso 1 1 calc R U . . .
H33C H 0.977344 0.835693 0.299839 0.158 Uiso 1 1 calc R U . . .
C34 C 1.2218(13) 0.5553(15) 0.2338(8) 0.091(3) Uani 1 1 d . . . . .
C35 C 1.2375(12) 0.5359(12) 0.1772(5) 0.073(4) Uani 1 1 d . . . . .
H35A H 1.161496 0.488557 0.15725 0.11 Uiso 1 1 calc R U . . .
H35B H 1.31184 0.490028 0.173646 0.11 Uiso 1 1 calc R U . . .
H35C H 1.249386 0.616283 0.163105 0.11 Uiso 1 1 calc R U . . .
C36 C 1.3317(14) 0.6090(13) 0.2709(6) 0.082(4) Uani 1 1 d . . . . .
H36A H 1.30909 0.617327 0.30672 0.123 Uiso 1 1 calc R U . . .
H36B H 1.359223 0.690761 0.261004 0.123 Uiso 1 1 calc R U . . .
H36C H 1.400963 0.555094 0.269814 0.123 Uiso 1 1 calc R U . . .
C37 C 0.8853(14) 0.5691(17) 0.1203(5) 0.088(3) Uani 1 1 d . . . . .
C38 C 0.8955(18) 0.7059(14) 0.1196(7) 0.109(6) Uani 1 1 d . . . . .
H38A H 0.821198 0.73011 0.097182 0.163 Uiso 1 1 calc R U . . .
H38B H 0.972778 0.732457 0.105319 0.163 Uiso 1 1 calc R U . . .
H38C H 0.899285 0.745171 0.155674 0.163 Uiso 1 1 calc R U . . .
C39 C 0.8802(16) 0.4947(14) 0.0683(5) 0.095(5) Uani 1 1 d . . . . .
H39A H 0.86603 0.406566 0.072943 0.143 Uiso 1 1 calc R U . . .
H39B H 0.960796 0.510277 0.054647 0.143 Uiso 1 1 calc R U . . .
H39C H 0.810596 0.518518 0.043196 0.143 Uiso 1 1 calc R U . . .
C40 C 0.6925(12) 0.7504(11) 0.2617(6) 0.067(2) Uani 1 1 d . . . . .
C41 C 0.6634(12) 0.8004(12) 0.3134(5) 0.066(4) Uani 1 1 d . . . . .
H41A H 0.578645 0.766089 0.318386 0.1 Uiso 1 1 calc R U . . .
H41B H 0.665474 0.890756 0.314737 0.1 Uiso 1 1 calc R U . . .
H41C H 0.726566 0.7776 0.341612 0.1 Uiso 1 1 calc R U . . .
C42 C 0.6092(12) 0.7781(12) 0.2122(5) 0.066(4) Uani 1 1 d . . . . .
H42A H 0.607083 0.867884 0.211904 0.1 Uiso 1 1 calc R U . . .
H42B H 0.522939 0.739634 0.211761 0.1 Uiso 1 1 calc R U . . .
H42C H 0.643678 0.744819 0.180947 0.1 Uiso 1 1 calc R U . . .
Ba1 Ba 0.88687(6) 0.46965(6) 0.26313(2) 0.03795(18) Uani 1 1 d . . . . .
Cl1 Cl 0.2296(3) -0.2753(3) 0.05976(11) 0.0680(9) Uani 1 1 d . . . . .
Cl2 Cl 0.1700(4) 0.2879(3) 0.04305(13) 0.0796(11) Uani 1 1 d . . . . .
Cl3 Cl 0.3982(3) -0.1450(3) 0.39730(11) 0.0617(8) Uani 1 1 d . . . . .
Cl4 Cl 0.3311(3) 0.4188(3) 0.38377(11) 0.0569(8) Uani 1 1 d . . . . .
Cl5 Cl 0.5703(3) -0.0490(2) 0.09548(10) 0.0477(7) Uani 1 1 d . . . . .
Cl6 Cl 0.5359(3) 0.5227(3) 0.09298(11) 0.0606(8) Uani 1 1 d . . . . .
Cl7 Cl 0.7239(3) 0.0400(3) 0.43630(11) 0.0611(8) Uani 1 1 d . . . . .
Cl8 Cl 0.6519(4) 0.6057(3) 0.43356(12) 0.0732(10) Uani 1 1 d . . . . .
Fe1 Fe 0.34300(13) 0.08302(12) 0.21839(5) 0.0297(3) Uani 1 1 d . . . . .
Fe2 Fe 0.56807(13) 0.27220(12) 0.26616(5) 0.0281(3) Uani 1 1 d . . . . .
S1 S 0.2776(3) -0.0884(2) 0.16522(9) 0.0373(6) Uani 1 1 d . . . . .
S2 S 0.2539(2) 0.1939(2) 0.15646(10) 0.0380(6) Uani 1 1 d . . . . .
S3 S 0.3584(3) -0.0401(2) 0.28399(9) 0.0366(6) Uani 1 1 d . . . . .
S4 S 0.3402(2) 0.2468(2) 0.27736(9) 0.0320(6) Uani 1 1 d . . . . .
S5 S 0.5711(2) 0.1150(2) 0.20482(8) 0.0291(5) Uani 1 1 d . . . . .
S6 S 0.5693(2) 0.4046(2) 0.20401(9) 0.0341(6) Uani 1 1 d . . . . .
S7 S 0.6643(2) 0.1554(2) 0.32509(9) 0.0348(6) Uani 1 1 d . . . . .
S8 S 0.6290(3) 0.4383(2) 0.32439(9) 0.0366(6) Uani 1 1 d . . . . .
O1 O 0.9776(8) 0.3447(8) 0.3451(3) 0.0645(19) Uani 1 1 d . . . . .
O2 O 0.9077(8) 0.2497(7) 0.2131(4) 0.073(2) Uani 1 1 d . . . . .
O3 O 0.9806(9) 0.6368(8) 0.3514(4) 0.083(2) Uani 1 1 d . . . . .
O4 O 1.1193(8) 0.5281(9) 0.2478(4) 0.091(3) Uani 1 1 d . . . . .
O5 O 0.8760(9) 0.5185(10) 0.1599(3) 0.088(3) Uani 1 1 d . . . . .
O6 O 0.7803(8) 0.6848(7) 0.2577(4) 0.067(2) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.405(13) . ?
C1 C6 1.411(14) . ?
C1 S1 1.768(9) . ?
C2 C3 1.382(15) . ?
C2 Cl1 1.752(11) . ?
C3 C4 1.368(16) . ?
C3 H3 0.95 . ?
C4 C5 1.386(15) . ?
C4 H4 0.95 . ?
C5 C6 1.409(13) . ?
C5 Cl2 1.738(12) . ?
C6 S2 1.744(10) . ?
C7 C8 1.396(13) . ?
C7 C12 1.412(14) . ?
C7 S3 1.758(9) . ?
C8 C9 1.399(14) . ?
C8 Cl3 1.743(11) . ?
C9 C10 1.407(15) . ?
C9 H9 0.95 . ?
C10 C11 1.374(15) . ?
C10 H10 0.95 . ?
C11 C12 1.392(13) . ?
C11 Cl4 1.762(11) . ?
C12 S4 1.770(10) . ?
C13 C18 1.420(13) . ?
C13 C14 1.427(13) . ?
C13 S5 1.762(9) . ?
C14 C15 1.372(13) . ?
C14 Cl5 1.743(10) . ?
C15 C16 1.380(14) . ?
C15 H15 0.95 . ?
C16 C17 1.390(13) . ?
C16 H16 0.95 . ?
C17 C18 1.391(13) . ?
C17 Cl6 1.753(10) . ?
C18 S6 1.746(9) . ?
C19 C20 1.387(13) . ?
C19 C24 1.437(14) . ?
C19 S7 1.760(9) . ?
C20 C21 1.375(14) . ?
C20 Cl7 1.764(11) . ?
C21 C22 1.391(17) . ?
C21 H21 0.95 . ?
C22 C23 1.360(15) . ?
C22 H22 0.95 . ?
C23 C24 1.405(13) . ?
C23 Cl8 1.753(12) . ?
C24 S8 1.752(10) . ?
C25 O1 1.210(13) . ?
C25 C27 1.473(17) . ?
C25 C26 1.504(17) . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 O2 1.210(13) . ?
C28 C30 1.460(19) . ?
C28 C29 1.466(18) . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
C31 O3 1.220(15) . ?
C31 C33 1.47(2) . ?
C31 C32 1.48(2) . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C33 H33A 0.98 . ?
C33 H33B 0.98 . ?
C33 H33C 0.98 . ?
C34 O4 1.220(14) . ?
C34 C36 1.45(2) . ?
C34 C35 1.48(2) . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?
C36 H36A 0.98 . ?
C36 H36B 0.98 . ?
C36 H36C 0.98 . ?
C37 O5 1.206(14) . ?
C37 C38 1.49(2) . ?
C37 C39 1.491(19) . ?
C38 H38A 0.98 . ?
C38 H38B 0.98 . ?
C38 H38C 0.98 . ?
C39 H39A 0.98 . ?
C39 H39B 0.98 . ?
C39 H39C 0.98 . ?
C40 O6 1.231(13) . ?
C40 C41 1.471(17) . ?
C40 C42 1.511(17) . ?
C41 H41A 0.98 . ?
C41 H41B 0.98 . ?
C41 H41C 0.98 . ?
C42 H42A 0.98 . ?
C42 H42B 0.98 . ?
C42 H42C 0.98 . ?
Ba1 O4 2.603(8) . ?
Ba1 O2 2.658(8) . ?
Ba1 O6 2.687(7) . ?
Ba1 O1 2.707(8) . ?
Ba1 O5 2.730(8) . ?
Ba1 O3 2.797(9) . ?
Ba1 S8 3.359(3) . ?
Ba1 S6 3.511(3) . ?
Ba1 Fe2 3.8956(17) . ?
Fe1 S1 2.221(3) . ?
Fe1 S2 2.228(3) . ?
Fe1 S3 2.233(3) . ?
Fe1 S4 2.241(3) . ?
Fe1 S5 2.508(3) . ?
Fe2 S5 2.228(2) . ?
Fe2 S6 2.237(3) . ?
Fe2 S8 2.239(3) . ?
Fe2 S7 2.248(3) . ?
Fe2 S4 2.485(3) . ?

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
C2 C1 C6 119.6(9) . . ?
C2 C1 S1 121.6(8) . . ?
C6 C1 S1 118.8(7) . . ?
C3 C2 C1 120.9(11) . . ?
C3 C2 Cl1 119.5(8) . . ?
C1 C2 Cl1 119.6(8) . . ?
C4 C3 C2 119.5(11) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 121.4(11) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C6 120.5(11) . . ?
C4 C5 Cl2 119.8(9) . . ?
C6 C5 Cl2 119.7(8) . . ?
C5 C6 C1 118.1(9) . . ?
C5 C6 S2 122.1(8) . . ?
C1 C6 S2 119.7(7) . . ?
C8 C7 C12 119.8(9) . . ?
C8 C7 S3 120.2(8) . . ?
C12 C7 S3 120.0(7) . . ?
C7 C8 C9 120.4(10) . . ?
C7 C8 Cl3 121.6(8) . . ?
C9 C8 Cl3 117.9(8) . . ?
C8 C9 C10 119.9(10) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 118.6(9) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 123.0(10) . . ?
C10 C11 Cl4 118.3(8) . . ?
C12 C11 Cl4 118.7(8) . . ?
C11 C12 C7 118.2(9) . . ?
C11 C12 S4 122.4(8) . . ?
C7 C12 S4 119.4(7) . . ?
C18 C13 C14 118.3(8) . . ?
C18 C13 S5 120.6(7) . . ?
C14 C13 S5 121.1(7) . . ?
C15 C14 C13 120.7(9) . . ?
C15 C14 Cl5 120.1(8) . . ?
C13 C14 Cl5 119.2(8) . . ?
C14 C15 C16 120.6(9) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C17 119.9(9) . . ?
C15 C16 H16 120 . . ?
C17 C16 H16 120 . . ?
C16 C17 C18 121.3(10) . . ?
C16 C17 Cl6 118.4(8) . . ?
C18 C17 Cl6 120.3(8) . . ?
C17 C18 C13 119.1(8) . . ?
C17 C18 S6 122.2(8) . . ?
C13 C18 S6 118.7(7) . . ?
C20 C19 C24 118.9(9) . . ?
C20 C19 S7 122.9(8) . . ?
C24 C19 S7 118.2(7) . . ?
C21 C20 C19 121.8(11) . . ?
C21 C20 Cl7 118.6(9) . . ?
C19 C20 Cl7 119.5(8) . . ?
C20 C21 C22 119.5(11) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C23 C22 C21 120.2(10) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 122.1(11) . . ?
C22 C23 Cl8 120.2(9) . . ?
C24 C23 Cl8 117.6(9) . . ?
C23 C24 C19 117.4(9) . . ?
C23 C24 S8 123.1(8) . . ?
C19 C24 S8 119.6(7) . . ?
O1 C25 C27 120.2(13) . . ?
O1 C25 C26 122.3(13) . . ?
C27 C25 C26 117.5(13) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O2 C28 C30 121.1(15) . . ?
O2 C28 C29 120.4(15) . . ?
C30 C28 C29 118.4(14) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O3 C31 C33 120.0(15) . . ?
O3 C31 C32 122.6(16) . . ?
C33 C31 C32 117.4(14) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O4 C34 C36 122.4(17) . . ?
O4 C34 C35 120.2(15) . . ?
C36 C34 C35 117.4(12) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O5 C37 C38 123.1(15) . . ?
O5 C37 C39 120.4(16) . . ?
C38 C37 C39 116.4(12) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O6 C40 C41 122.1(12) . . ?
O6 C40 C42 119.4(12) . . ?
C41 C40 C42 118.5(11) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O4 Ba1 O2 86.6(3) . . ?
O4 Ba1 O6 103.2(3) . . ?
O2 Ba1 O6 145.7(3) . . ?
O4 Ba1 O1 89.2(3) . . ?
O2 Ba1 O1 79.1(3) . . ?
O6 Ba1 O1 133.0(3) . . ?
O4 Ba1 O5 73.3(3) . . ?
O2 Ba1 O5 76.9(3) . . ?
O6 Ba1 O5 74.7(3) . . ?
O1 Ba1 O5 150.9(3) . . ?
O4 Ba1 O3 77.5(3) . . ?
O2 Ba1 O3 145.3(3) . . ?
O6 Ba1 O3 68.7(3) . . ?
O1 Ba1 O3 70.2(3) . . ?
O5 Ba1 O3 125.6(3) . . ?
O4 Ba1 S8 160.4(3) . . ?
O2 Ba1 S8 106.63(19) . . ?
O6 Ba1 S8 74.24(19) . . ?
O1 Ba1 S8 79.49(18) . . ?
O5 Ba1 S8 123.2(2) . . ?
O3 Ba1 S8 83.6(2) . . ?
O4 Ba1 S6 145.9(2) . . ?
O2 Ba1 S6 81.77(19) . . ?
O6 Ba1 S6 71.79(18) . . ?
O1 Ba1 S6 119.47(18) . . ?
O5 Ba1 S6 72.9(2) . . ?
O3 Ba1 S6 127.3(2) . . ?
S8 Ba1 S6 52.60(6) . . ?
O4 Ba1 Fe2 160.2(2) . . ?
O2 Ba1 Fe2 73.83(19) . . ?
O6 Ba1 Fe2 94.64(18) . . ?
O1 Ba1 Fe2 84.80(17) . . ?
O5 Ba1 Fe2 103.9(2) . . ?
O3 Ba1 Fe2 117.6(2) . . ?
S8 Ba1 Fe2 34.96(4) . . ?
S6 Ba1 Fe2 34.67(4) . . ?
S1 Fe1 S2 89.33(10) . . ?
S1 Fe1 S3 85.92(10) . . ?
S2 Fe1 S3 159.16(12) . . ?
S1 Fe1 S4 160.32(11) . . ?
S2 Fe1 S4 87.78(10) . . ?
S3 Fe1 S4 89.90(10) . . ?
S1 Fe1 S5 101.41(10) . . ?
S2 Fe1 S5 100.06(10) . . ?
S3 Fe1 S5 100.76(10) . . ?
S4 Fe1 S5 98.27(9) . . ?
S5 Fe2 S6 89.96(9) . . ?
S5 Fe2 S8 162.01(11) . . ?
S6 Fe2 S8 85.79(10) . . ?
S5 Fe2 S7 87.25(10) . . ?
S6 Fe2 S7 152.75(11) . . ?
S8 Fe2 S7 88.56(10) . . ?
S5 Fe2 S4 99.30(9) . . ?
S6 Fe2 S4 102.68(10) . . ?
S8 Fe2 S4 98.68(10) . . ?
S7 Fe2 S4 104.52(10) . . ?
S5 Fe2 Ba1 103.29(8) . . ?
S6 Fe2 Ba1 63.21(7) . . ?
S8 Fe2 Ba1 59.30(7) . . ?
S7 Fe2 Ba1 91.10(8) . . ?
S4 Fe2 Ba1 153.07(7) . . ?
C1 S1 Fe1 104.4(3) . . ?
C6 S2 Fe1 104.7(4) . . ?
C7 S3 Fe1 105.4(4) . . ?
C12 S4 Fe1 105.2(3) . . ?
C12 S4 Fe2 100.6(3) . . ?
Fe1 S4 Fe2 81.30(9) . . ?
C13 S5 Fe2 104.7(3) . . ?
C13 S5 Fe1 103.7(3) . . ?
Fe2 S5 Fe1 81.04(8) . . ?
C18 S6 Fe2 105.8(3) . . ?
C18 S6 Ba1 110.9(3) . . ?
Fe2 S6 Ba1 82.12(8) . . ?
C19 S7 Fe2 104.3(4) . . ?
C24 S8 Fe2 104.1(3) . . ?
C24 S8 Ba1 112.2(3) . . ?
Fe2 S8 Ba1 85.74(8) . . ?
C25 O1 Ba1 167.3(9) . . ?
C28 O2 Ba1 172.6(10) . . ?
C31 O3 Ba1 143.3(10) . . ?
C34 O4 Ba1 171.6(12) . . ?
C37 O5 Ba1 163.2(12) . . ?
C40 O6 Ba1 152.7(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.5(15) . . . . ?
S1 C1 C2 C3 179.3(9) . . . . ?
C6 C1 C2 Cl1 178.2(8) . . . . ?
S1 C1 C2 Cl1 -3.0(12) . . . . ?
C1 C2 C3 C4 -0.7(17) . . . . ?
Cl1 C2 C3 C4 -178.4(9) . . . . ?
C2 C3 C4 C5 0.2(19) . . . . ?
C3 C4 C5 C6 0.6(18) . . . . ?
C3 C4 C5 Cl2 -179.7(10) . . . . ?
C4 C5 C6 C1 -0.8(16) . . . . ?
Cl2 C5 C6 C1 179.5(8) . . . . ?
C4 C5 C6 S2 179.4(9) . . . . ?
Cl2 C5 C6 S2 -0.4(13) . . . . ?
C2 C1 C6 C5 0.2(15) . . . . ?
S1 C1 C6 C5 -178.6(8) . . . . ?
C2 C1 C6 S2 -179.9(7) . . . . ?
S1 C1 C6 S2 1.3(12) . . . . ?
C12 C7 C8 C9 -1.3(15) . . . . ?
S3 C7 C8 C9 179.4(8) . . . . ?
C12 C7 C8 Cl3 -177.6(7) . . . . ?
S3 C7 C8 Cl3 3.2(12) . . . . ?
C7 C8 C9 C10 2.9(16) . . . . ?
Cl3 C8 C9 C10 179.3(8) . . . . ?
C8 C9 C10 C11 -2.6(16) . . . . ?
C9 C10 C11 C12 0.8(16) . . . . ?
C9 C10 C11 Cl4 178.7(8) . . . . ?
C10 C11 C12 C7 0.7(15) . . . . ?
Cl4 C11 C12 C7 -177.2(7) . . . . ?
C10 C11 C12 S4 -177.0(8) . . . . ?
Cl4 C11 C12 S4 5.1(12) . . . . ?
C8 C7 C12 C11 -0.4(14) . . . . ?
S3 C7 C12 C11 178.8(7) . . . . ?
C8 C7 C12 S4 177.4(7) . . . . ?
S3 C7 C12 S4 -3.4(11) . . . . ?
C18 C13 C14 C15 -0.9(14) . . . . ?
S5 C13 C14 C15 178.3(8) . . . . ?
C18 C13 C14 Cl5 178.6(7) . . . . ?
S5 C13 C14 Cl5 -2.1(12) . . . . ?
C13 C14 C15 C16 -1.2(16) . . . . ?
Cl5 C14 C15 C16 179.3(8) . . . . ?
C14 C15 C16 C17 2.6(17) . . . . ?
C15 C16 C17 C18 -1.9(17) . . . . ?
C15 C16 C17 Cl6 -179.5(8) . . . . ?
C16 C17 C18 C13 -0.1(15) . . . . ?
Cl6 C17 C18 C13 177.3(7) . . . . ?
C16 C17 C18 S6 178.6(8) . . . . ?
Cl6 C17 C18 S6 -3.9(12) . . . . ?
C14 C13 C18 C17 1.5(14) . . . . ?
S5 C13 C18 C17 -177.7(7) . . . . ?
C14 C13 C18 S6 -177.3(7) . . . . ?
S5 C13 C18 S6 3.5(11) . . . . ?
C24 C19 C20 C21 1.7(15) . . . . ?
S7 C19 C20 C21 -176.0(8) . . . . ?
C24 C19 C20 Cl7 179.8(7) . . . . ?
S7 C19 C20 Cl7 2.1(12) . . . . ?
C19 C20 C21 C22 -1.3(17) . . . . ?
Cl7 C20 C21 C22 -179.4(9) . . . . ?
C20 C21 C22 C23 -1.8(18) . . . . ?
C21 C22 C23 C24 4.7(18) . . . . ?
C21 C22 C23 Cl8 -179.1(9) . . . . ?
C22 C23 C24 C19 -4.2(16) . . . . ?
Cl8 C23 C24 C19 179.5(7) . . . . ?
C22 C23 C24 S8 175.5(9) . . . . ?
Cl8 C23 C24 S8 -0.8(13) . . . . ?
C20 C19 C24 C23 1.0(14) . . . . ?
S7 C19 C24 C23 178.8(8) . . . . ?
C20 C19 C24 S8 -178.7(7) . . . . ?
S7 C19 C24 S8 -0.9(11) . . . . ?
C2 C1 S1 Fe1 168.2(8) . . . . ?
C6 C1 S1 Fe1 -13.0(9) . . . . ?
C5 C6 S2 Fe1 -169.0(8) . . . . ?
C1 C6 S2 Fe1 11.1(9) . . . . ?
C8 C7 S3 Fe1 -177.8(7) . . . . ?
C12 C7 S3 Fe1 3.0(8) . . . . ?
C11 C12 S4 Fe1 179.6(7) . . . . ?
C7 C12 S4 Fe1 1.9(8) . . . . ?
C11 C12 S4 Fe2 95.9(8) . . . . ?
C7 C12 S4 Fe2 -81.8(7) . . . . ?
C18 C13 S5 Fe2 0.6(8) . . . . ?
C14 C13 S5 Fe2 -178.6(7) . . . . ?
C18 C13 S5 Fe1 84.7(8) . . . . ?
C14 C13 S5 Fe1 -94.5(8) . . . . ?
C17 C18 S6 Fe2 175.6(8) . . . . ?
C13 C18 S6 Fe2 -5.6(8) . . . . ?
C17 C18 S6 Ba1 -97.0(8) . . . . ?
C13 C18 S6 Ba1 81.8(8) . . . . ?
C20 C19 S7 Fe2 162.5(8) . . . . ?
C24 C19 S7 Fe2 -15.2(8) . . . . ?
C23 C24 S8 Fe2 -163.1(8) . . . . ?
C19 C24 S8 Fe2 16.6(8) . . . . ?
C23 C24 S8 Ba1 105.8(8) . . . . ?
C19 C24 S8 Ba1 -74.6(8) . . . . ?
C27 C25 O1 Ba1 -30(5) . . . . ?
C26 C25 O1 Ba1 148(3) . . . . ?
C33 C31 O3 Ba1 -25(3) . . . . ?
C32 C31 O3 Ba1 152.4(12) . . . . ?
C38 C37 O5 Ba1 -23(4) . . . . ?
C39 C37 O5 Ba1 161(3) . . . . ?
C41 C40 O6 Ba1 76(2) . . . . ?
C42 C40 O6 Ba1 -103(2) . . . . ?

####################################################################### 
# 
# 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_02139ElisaHernandez
_database_code_depnum_ccdc_archive 'CCDC 1834788'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            NG18_LT
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H14 Fe K O S4'
_chemical_formula_iupac          ?
_chemical_formula_weight         421.44

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.5364(7)
_cell_length_b                   9.1640(9)
_cell_length_c                   24.2084(18)
_cell_angle_alpha                90
_cell_angle_beta                 91.334(4)
_cell_angle_gamma                90
_cell_volume                     1671.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7434
_cell_measurement_theta_min      2.3765
_cell_measurement_theta_max      26.4038
_cell_measurement_temperature    200.(2)

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860

_exptl_absorpt_coefficient_mu    1.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  0.85

_exptl_special_details           
;
;

_diffrn_ambient_temperature      200.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            23488
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29

_refine_special_details          
;
;

_reflns_number_total             3052
_reflns_number_gt                2768
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0643
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_number_reflns         3052
_refine_ls_number_parameters     195
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0172P)²+1.6498P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.338
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.4481(3) 0.9214(3) 0.61353(9) 0.0243(5) Uani d . . . 1 . .
C C2 0.4522(3) 0.9864(3) 0.66539(10) 0.0311(6) Uani d . . . 1 . .
H H2 0.4007 1.0799 0.6705 0.037 Uiso calc U . R 1 . .
C C3 0.5313(4) 0.9143(4) 0.70942(10) 0.0395(7) Uani d . . . 1 . .
H H3 0.5358 0.9587 0.7449 0.047 Uiso calc U . R 1 . .
C C4 0.6037(4) 0.7781(4) 0.70207(11) 0.0422(8) Uani d . . . 1 . .
H H4 0.6575 0.7288 0.7327 0.051 Uiso calc U . R 1 . .
C C5 0.5992(4) 0.7124(3) 0.65087(11) 0.0369(7) Uani d . . . 1 . .
H H5 0.6496 0.6182 0.6463 0.044 Uiso calc U . R 1 . .
C C6 0.5209(3) 0.7840(3) 0.60574(10) 0.0263(6) Uani d . . . 1 . .
C C7 0.2219(3) 0.7768(3) 0.36682(10) 0.0255(6) Uani d . . . 1 . .
C C8 0.2093(4) 0.7158(3) 0.31420(11) 0.0355(7) Uani d . . . 1 . .
H H8 0.2713 0.6282 0.3063 0.043 Uiso calc U . R 1 . .
C C9 0.1072(4) 0.7821(3) 0.27355(11) 0.0414(7) Uani d . . . 1 . .
H H9 0.1003 0.7408 0.2376 0.05 Uiso calc U . R 1 . .
C C10 0.0147(4) 0.9086(3) 0.28477(10) 0.0389(7) Uani d . . . 1 . .
H H10 -0.057 0.953 0.2567 0.047 Uiso calc U . R 1 . .
C C11 0.0264(3) 0.9704(3) 0.33661(10) 0.0303(6) Uani d . . . 1 . .
H H11 -0.0387 1.0564 0.3444 0.036 Uiso calc U . R 1 . .
C C12 0.1333(3) 0.9069(3) 0.37762(9) 0.0223(5) Uani d . . . 1 . .
C C14 -0.1104(5) 0.4427(4) 0.38207(13) 0.0553(9) Uani d . . . 1 . .
H H14A -0.1513 0.3463 0.3684 0.066 Uiso calc U . R 1 . .
H H14B 0.017 0.4523 0.3737 0.066 Uiso calc U . R 1 . .
C C15 -0.2117(4) 0.5591(4) 0.35266(13) 0.0609(10) Uani d . . . 1 . .
H H15A -0.3379 0.5504 0.361 0.091 Uiso calc U . R 1 . .
H H15B -0.1963 0.5489 0.3128 0.091 Uiso calc U . R 1 . .
H H15C -0.1677 0.6548 0.3648 0.091 Uiso calc U . R 1 . .
Fe Fe1 0.38569(4) 0.86699(4) 0.48346(2) 0.02090(10) Uani d . . . 1 . .
K K1 -0.08045(9) 0.71541(7) 0.48915(3) 0.04161(17) Uani d . . . 1 . .
O O1 -0.1312(3) 0.4489(2) 0.44106(9) 0.0475(6) Uani d . . . 1 . .
S S1 0.35394(8) 1.01413(7) 0.55586(2) 0.02243(15) Uani d . . . 1 . .
S S2 0.51451(9) 0.70207(7) 0.53958(2) 0.02759(16) Uani d . . . 1 . .
S S3 0.34644(9) 0.69232(7) 0.42055(3) 0.03033(16) Uani d . . . 1 . .
S S4 0.15909(8) 0.98545(7) 0.44350(2) 0.02365(15) Uani d . . . 1 . .
H H1O -0.235(6) 0.416(5) 0.4472(17) 0.098(16) Uiso d . . . 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C6 . 1.388(4) ?
C1 C2 . 1.389(3) ?
C1 S1 . 1.769(2) ?
C2 C3 . 1.378(4) ?
C2 H2 . 0.95 ?
C3 C4 . 1.376(4) ?
C3 H3 . 0.95 ?
C4 C5 . 1.378(4) ?
C4 H4 . 0.95 ?
C5 C6 . 1.394(3) ?
C5 H5 . 0.95 ?
C6 S2 . 1.768(3) ?
C7 C8 . 1.393(3) ?
C7 C12 . 1.394(3) ?
C7 S3 . 1.765(2) ?
C8 C9 . 1.377(4) ?
C8 H8 . 0.95 ?
C9 C10 . 1.383(4) ?
C9 H9 . 0.95 ?
C10 C11 . 1.378(4) ?
C10 H10 . 0.95 ?
C11 C12 . 1.391(3) ?
C11 H11 . 0.95 ?
C12 S4 . 1.756(2) ?
C14 O1 . 1.441(4) ?
C14 C15 . 1.484(5) ?
C14 H14A . 0.99 ?
C14 H14B . 0.99 ?
C15 H15A . 0.98 ?
C15 H15B . 0.98 ?
C15 H15C . 0.98 ?
Fe1 S3 . 2.2245(7) ?
Fe1 S4 . 2.2256(7) ?
Fe1 S1 . 2.2287(7) ?
Fe1 S2 . 2.2385(7) ?
Fe1 S1 3_676 2.4557(7) ?
Fe1 K1 . 3.7832(8) ?
K1 O1 . 2.728(2) ?
K1 O1 3_566 2.746(2) ?
K1 S4 3_576 3.2512(9) ?
K1 S4 . 3.2706(9) ?
K1 S2 1_455 3.3162(10) ?
K1 S1 3_576 3.3873(9) ?
K1 S3 . 3.6608(10) ?
K1 K1 3_566 4.1598(13) ?
O1 K1 3_566 2.746(2) ?
O1 H1O . 0.85(4) ?
S1 Fe1 3_676 2.4557(7) ?
S1 K1 3_576 3.3873(9) ?
S2 K1 1_655 3.3162(10) ?
S4 K1 3_576 3.2512(9) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 C1 C2 . . 120.8(2) ?
C6 C1 S1 . . 118.77(18) ?
C2 C1 S1 . . 120.5(2) ?
C3 C2 C1 . . 119.6(3) ?
C3 C2 H2 . . 120.2 ?
C1 C2 H2 . . 120.2 ?
C4 C3 C2 . . 120.1(3) ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C3 C4 C5 . . 120.8(2) ?
C3 C4 H4 . . 119.6 ?
C5 C4 H4 . . 119.6 ?
C4 C5 C6 . . 120.0(3) ?
C4 C5 H5 . . 120.0 ?
C6 C5 H5 . . 120.0 ?
C1 C6 C5 . . 118.8(2) ?
C1 C6 S2 . . 120.37(18) ?
C5 C6 S2 . . 120.8(2) ?
C8 C7 C12 . . 119.5(2) ?
C8 C7 S3 . . 121.4(2) ?
C12 C7 S3 . . 119.07(18) ?
C9 C8 C7 . . 120.1(3) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
C8 C9 C10 . . 120.4(2) ?
C8 C9 H9 . . 119.8 ?
C10 C9 H9 . . 119.8 ?
C11 C10 C9 . . 120.1(2) ?
C11 C10 H10 . . 120.0 ?
C9 C10 H10 . . 120.0 ?
C10 C11 C12 . . 120.1(3) ?
C10 C11 H11 . . 119.9 ?
C12 C11 H11 . . 119.9 ?
C11 C12 C7 . . 119.7(2) ?
C11 C12 S4 . . 121.78(19) ?
C7 C12 S4 . . 118.50(17) ?
O1 C14 C15 . . 112.4(3) ?
O1 C14 H14A . . 109.1 ?
C15 C14 H14A . . 109.1 ?
O1 C14 H14B . . 109.1 ?
C15 C14 H14B . . 109.1 ?
H14A C14 H14B . . 107.9 ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
S3 Fe1 S4 . . 87.99(3) ?
S3 Fe1 S1 . . 163.50(3) ?
S4 Fe1 S1 . . 87.21(2) ?
S3 Fe1 S2 . . 88.77(3) ?
S4 Fe1 S2 . . 155.59(3) ?
S1 Fe1 S2 . . 89.09(3) ?
S3 Fe1 S1 . 3_676 98.54(3) ?
S4 Fe1 S1 . 3_676 103.13(3) ?
S1 Fe1 S1 . 3_676 97.92(2) ?
S2 Fe1 S1 . 3_676 101.28(3) ?
S3 Fe1 K1 . . 69.63(2) ?
S4 Fe1 K1 . . 59.41(2) ?
S1 Fe1 K1 . . 94.40(2) ?
S2 Fe1 K1 . . 96.89(2) ?
S1 Fe1 K1 3_676 . 158.14(2) ?
O1 K1 O1 . 3_566 81.10(7) ?
O1 K1 S4 . 3_576 160.61(6) ?
O1 K1 S4 3_566 3_576 105.30(5) ?
O1 K1 S4 . . 127.30(5) ?
O1 K1 S4 3_566 . 107.79(5) ?
S4 K1 S4 3_576 . 68.90(2) ?
O1 K1 S2 . 1_455 90.17(5) ?
O1 K1 S2 3_566 1_455 106.24(5) ?
S4 K1 S2 3_576 1_455 70.51(2) ?
S4 K1 S2 . 1_455 132.25(3) ?
O1 K1 S1 . 3_576 116.07(5) ?
O1 K1 S1 3_566 3_576 159.97(5) ?
S4 K1 S1 3_576 3_576 55.088(18) ?
S4 K1 S1 . 3_576 70.99(2) ?
S2 K1 S1 1_455 3_576 65.603(19) ?
O1 K1 S3 . . 82.57(5) ?
O1 K1 S3 3_566 . 75.13(5) ?
S4 K1 S3 3_576 . 116.66(2) ?
S4 K1 S3 . . 52.600(18) ?
S2 K1 S3 1_455 . 172.34(3) ?
S1 K1 S3 3_576 . 115.53(2) ?
O1 K1 Fe1 . . 115.73(5) ?
O1 K1 Fe1 3_566 . 72.38(5) ?
S4 K1 Fe1 3_576 . 83.622(19) ?
S4 K1 Fe1 . . 35.860(13) ?
S2 K1 Fe1 1_455 . 152.93(2) ?
S1 K1 Fe1 3_576 . 106.15(2) ?
S3 K1 Fe1 . . 34.725(13) ?
O1 K1 K1 . 3_566 40.71(5) ?
O1 K1 K1 3_566 3_566 40.39(5) ?
S4 K1 K1 3_576 3_566 142.46(3) ?
S4 K1 K1 . 3_566 126.81(3) ?
S2 K1 K1 1_455 3_566 100.76(3) ?
S1 K1 K1 3_576 3_566 155.30(3) ?
S3 K1 K1 . 3_566 75.27(2) ?
Fe1 K1 K1 . 3_566 94.87(2) ?
C14 O1 K1 . . 116.2(2) ?
C14 O1 K1 . 3_566 120.85(19) ?
K1 O1 K1 . 3_566 98.90(7) ?
C14 O1 H1O . . 106.(3) ?
K1 O1 H1O . . 111.(3) ?
K1 O1 H1O 3_566 . 103.(3) ?
C1 S1 Fe1 . . 106.35(9) ?
C1 S1 Fe1 . 3_676 102.10(8) ?
Fe1 S1 Fe1 . 3_676 82.08(2) ?
C1 S1 K1 . 3_576 146.66(9) ?
Fe1 S1 K1 . 3_576 105.39(2) ?
Fe1 S1 K1 3_676 3_576 92.09(2) ?
C6 S2 Fe1 . . 105.39(9) ?
C6 S2 K1 . 1_655 108.19(8) ?
Fe1 S2 K1 . 1_655 98.14(3) ?
C7 S3 Fe1 . . 104.40(9) ?
C7 S3 K1 . . 81.43(8) ?
Fe1 S3 K1 . . 75.65(2) ?
C12 S4 Fe1 . . 105.21(8) ?
C12 S4 K1 . 3_576 141.56(9) ?
Fe1 S4 K1 . 3_576 109.89(3) ?
C12 S4 K1 . . 86.93(8) ?
Fe1 S4 K1 . . 84.73(2) ?
K1 S4 K1 3_576 . 111.10(2) ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . 0.8(4) ?
S1 C1 C2 C3 . . . . -177.9(2) ?
C1 C2 C3 C4 . . . . -0.8(4) ?
C2 C3 C4 C5 . . . . 0.4(4) ?
C3 C4 C5 C6 . . . . 0.1(4) ?
C2 C1 C6 C5 . . . . -0.4(4) ?
S1 C1 C6 C5 . . . . 178.34(19) ?
C2 C1 C6 S2 . . . . 179.85(19) ?
S1 C1 C6 S2 . . . . -1.4(3) ?
C4 C5 C6 C1 . . . . -0.1(4) ?
C4 C5 C6 S2 . . . . 179.7(2) ?
C12 C7 C8 C9 . . . . -1.3(4) ?
S3 C7 C8 C9 . . . . 178.2(2) ?
C7 C8 C9 C10 . . . . -0.8(5) ?
C8 C9 C10 C11 . . . . 1.0(5) ?
C9 C10 C11 C12 . . . . 0.9(4) ?
C10 C11 C12 C7 . . . . -3.0(4) ?
C10 C11 C12 S4 . . . . 177.5(2) ?
C8 C7 C12 C11 . . . . 3.2(4) ?
S3 C7 C12 C11 . . . . -176.31(19) ?
C8 C7 C12 S4 . . . . -177.3(2) ?
S3 C7 C12 S4 . . . . 3.1(3) ?
C15 C14 O1 K1 . . . . -49.3(3) ?
C15 C14 O1 K1 . . . 3_566 -169.0(2) ?
C6 C1 S1 Fe1 . . . . 0.1(2) ?
C2 C1 S1 Fe1 . . . . 178.77(18) ?
C6 C1 S1 Fe1 . . . 3_676 -85.12(19) ?
C2 C1 S1 Fe1 . . . 3_676 93.6(2) ?
C6 C1 S1 K1 . . . 3_576 161.70(13) ?
C2 C1 S1 K1 . . . 3_576 -19.6(3) ?
C1 C6 S2 Fe1 . . . . 2.0(2) ?
C5 C6 S2 Fe1 . . . . -177.75(19) ?
C1 C6 S2 K1 . . . 1_655 106.20(19) ?
C5 C6 S2 K1 . . . 1_655 -73.6(2) ?
C8 C7 S3 Fe1 . . . . 163.1(2) ?
C12 C7 S3 Fe1 . . . . -17.4(2) ?
C8 C7 S3 K1 . . . . -124.2(2) ?
C12 C7 S3 K1 . . . . 55.31(19) ?
C11 C12 S4 Fe1 . . . . -167.74(19) ?
C7 C12 S4 Fe1 . . . . 12.8(2) ?
C11 C12 S4 K1 . . . 3_576 -12.2(3) ?
C7 C12 S4 K1 . . . 3_576 168.31(14) ?
C11 C12 S4 K1 . . . . 108.6(2) ?
C7 C12 S4 K1 . . . . -70.87(19) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1O S2 3_566 0.85(4) 2.40(4) 3.247(2) 173.(4) ?

####################################################################### 
# 
# 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_01692ElisaHernandez
_database_code_depnum_ccdc_archive 'CCDC 1834786'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H76 Cl8 Fe Ni2 O10 S8'
_chemical_formula_iupac          ?
_chemical_formula_weight         1622.51

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9301(5)
_cell_length_b                   13.2950(8)
_cell_length_c                   14.7803(8)
_cell_angle_alpha                63.606(2)
_cell_angle_beta                 76.591(2)
_cell_angle_gamma                69.262(2)
_cell_volume                     1792.14(17)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9850
_cell_measurement_theta_min      2.4160
_cell_measurement_theta_max      25.6812
_cell_measurement_temperature    200.(2)

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             838

_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.86

_exptl_special_details           
;
;

_diffrn_ambient_temperature      200.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            56197
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             6526
_reflns_number_gt                5339
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1262
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_number_reflns         6526
_refine_ls_number_parameters     396
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0776P)²+0.9761P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.341
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_cell_refinement       'APEX2 v2010.9-1 (Bruker AXS)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.8128(3) 0.9071(3) 0.6879(2) 0.0377(6) Uani d . . . 1 . .
C C2 0.7255(3) 0.8918(3) 0.7755(3) 0.0461(7) Uani d . . . 1 . .
C C3 0.6804(4) 0.7953(3) 0.8243(3) 0.0537(9) Uani d . . . 1 . .
H H3 0.6199 0.7884 0.8829 0.064 Uiso calc U . R 1 . .
C C4 0.7233(3) 0.7077(3) 0.7878(3) 0.0518(8) Uani d . . . 1 . .
H H4 0.6933 0.6399 0.8217 0.062 Uiso calc U . R 1 . .
C C5 0.8094(3) 0.7196(3) 0.7025(2) 0.0430(7) Uani d . . . 1 . .
C C6 0.8558(3) 0.8191(3) 0.6503(2) 0.0369(6) Uani d . . . 1 . .
C C7 0.7689(3) 0.3198(3) 0.0615(2) 0.0448(7) Uani d . . . 1 . .
C C8 0.8915(3) 0.2595(4) 0.1004(3) 0.0553(9) Uani d . . . 1 . .
C C9 0.9544(4) 0.1453(4) 0.1113(3) 0.0660(11) Uani d . . . 1 . .
H H9 1.0368 0.1053 0.1393 0.079 Uiso calc U . R 1 . .
C C10 0.8961(4) 0.0897(4) 0.0812(3) 0.0668(11) Uani d . . . 1 . .
H H10 0.9383 0.0109 0.0885 0.08 Uiso calc U . R 1 . .
C C11 0.7773(4) 0.1483(3) 0.0406(3) 0.0577(9) Uani d . . . 1 . .
C C12 0.7104(3) 0.2629(3) 0.0308(2) 0.0448(7) Uani d . . . 1 . .
C C13 0.3136(4) 0.6954(4) 0.5778(4) 0.0688(12) Uani d . . . 1 . .
H H13A 0.2334 0.6704 0.5923 0.083 Uiso calc U . R 1 . .
H H13B 0.3186 0.7508 0.5059 0.083 Uiso calc U . R 1 . .
C C14 0.3090(4) 0.7521(4) 0.6444(4) 0.0711(12) Uani d . . . 1 . .
H H14A 0.2429 0.733 0.7029 0.085 Uiso calc U . R 1 . .
H H14B 0.2862 0.8383 0.607 0.085 Uiso calc U . R 1 . .
C C15 0.4439(4) 0.7047(3) 0.6793(3) 0.0553(9) Uani d . . . 1 . .
H H15A 0.4405 0.6992 0.7488 0.066 Uiso calc U . R 1 . .
H H15B 0.5006 0.7545 0.6331 0.066 Uiso calc U . R 1 . .
C C16 0.4925(4) 0.5856(3) 0.6765(3) 0.0610(10) Uani d . . . 1 . .
H H16A 0.5891 0.5629 0.6616 0.073 Uiso calc U . R 1 . .
H H16B 0.4691 0.5261 0.7423 0.073 Uiso calc U . R 1 . .
C C17 0.1967(3) 0.5737(4) 0.4479(3) 0.0582(9) Uani d . . . 1 . .
H H17A 0.1618 0.5802 0.5137 0.07 Uiso calc U . R 1 . .
H H17B 0.2048 0.4938 0.4555 0.07 Uiso calc U . R 1 . .
C C18 0.1077(4) 0.6644(4) 0.3667(4) 0.0735(13) Uani d . . . 1 . .
H H18A 0.045 0.6315 0.3581 0.088 Uiso calc U . R 1 . .
H H18B 0.0579 0.7334 0.3831 0.088 Uiso calc U . R 1 . .
C C19 0.2005(5) 0.6966(4) 0.2731(4) 0.0770(12) Uani d . . . 1 . .
H H19A 0.1625 0.7766 0.2231 0.092 Uiso calc U . R 1 . .
H H19B 0.2235 0.6402 0.2409 0.092 Uiso calc U . R 1 . .
C C20 0.3187(4) 0.6901(3) 0.3144(3) 0.0598(9) Uani d . . . 1 . .
H H20A 0.4 0.6714 0.2712 0.072 Uiso calc U . R 1 . .
H H20B 0.3086 0.7654 0.3177 0.072 Uiso calc U . R 1 . .
C C21 0.3281(5) 0.2537(4) 0.8656(3) 0.0787(12) Uani d . . . 1 . .
H H21A 0.3968 0.2507 0.9009 0.094 Uiso calc U . R 1 . .
H H21B 0.356 0.1823 0.8515 0.094 Uiso calc U . R 1 . .
C C22 0.2022(6) 0.2623(6) 0.9274(5) 0.131(3) Uani d . . . 1 . .
H H22A 0.183 0.1858 0.9577 0.158 Uiso calc U . R 1 . .
H H22B 0.2061 0.2829 0.9831 0.158 Uiso calc U . R 1 . .
C C23 0.1028(6) 0.3489(7) 0.8660(5) 0.136(3) Uani d . . . 1 . .
H H23A 0.0394 0.3962 0.9021 0.163 Uiso calc U . R 1 . .
H H23B 0.0549 0.3133 0.8446 0.163 Uiso calc U . R 1 . .
C C24 0.1744(7) 0.4209(6) 0.7782(5) 0.133(3) Uani d . . . 1 . .
H H24A 0.1372 0.4426 0.7148 0.159 Uiso calc U . R 1 . .
H H24B 0.1668 0.4938 0.7849 0.159 Uiso calc U . R 1 . .
C C25 0.4730(6) 0.0775(5) 0.6179(6) 0.119(2) Uani d . . . 1 . .
H H25A 0.5408 0.0762 0.653 0.142 Uiso calc U . R 1 . .
H H25B 0.5174 0.0474 0.5646 0.142 Uiso calc U . R 1 . .
C C26 0.3891(8) 0.0057(5) 0.6903(6) 0.144(3) Uani d . . . 1 . .
H H26A 0.4124 -0.0698 0.6834 0.172 Uiso calc U . R 1 . .
H H26B 0.4001 -0.0108 0.7606 0.172 Uiso calc U . R 1 . .
C C27 0.2591(8) 0.0706(7) 0.6673(6) 0.169(4) Uani d . . . 1 . .
H H27A 0.2025 0.073 0.7297 0.202 Uiso calc U . R 1 . .
H H27B 0.2242 0.0344 0.637 0.202 Uiso calc U . R 1 . .
C C28 0.2609(6) 0.1864(5) 0.5970(6) 0.145(3) Uani d . . . 1 . .
H H28A 0.2241 0.2061 0.534 0.174 Uiso calc U . R 1 . .
H H28B 0.2064 0.2437 0.6265 0.174 Uiso calc U . R 1 . .
Cl Cl1 0.67205(11) 0.99865(9) 0.82513(8) 0.0692(3) Uani d . . . 1 . .
Cl Cl2 0.86525(11) 0.60747(8) 0.65924(8) 0.0633(3) Uani d . . . 1 . .
Cl Cl3 0.96704(10) 0.32970(11) 0.13559(9) 0.0768(3) Uani d . . . 1 . .
Cl Cl4 0.70694(14) 0.07533(11) 0.00416(11) 0.0897(4) Uani d . . . 1 . .
Fe Fe1 0.5 0.5 0.5 0.03626(16) Uani d . P S 1 . .
Ni Ni1 1.0 1.0 0.5 0.03349(15) Uani d . P S 1 . .
Ni Ni2 0.5 0.5 0 0.03915(16) Uani d . P S 1 . .
O O1 0.4283(2) 0.59498(19) 0.59637(17) 0.0448(5) Uani d . . . 1 . .
O O2 0.3230(2) 0.59723(19) 0.41490(18) 0.0470(5) Uani d . . . 1 . .
O O3 0.4140(3) 0.3731(2) 0.5949(2) 0.0542(6) Uani d . . . 1 . .
O O4 0.3072(4) 0.3544(3) 0.7755(2) 0.0943(11) Uani d . . . 1 . .
O O5 0.3894(3) 0.1922(2) 0.5750(2) 0.0699(8) Uani d . . . 1 . .
S S1 0.87252(8) 1.02787(7) 0.62647(6) 0.0423(2) Uani d . . . 1 . .
S S2 0.96600(8) 0.83481(7) 0.54310(6) 0.04087(19) Uani d . . . 1 . .
S S3 0.68550(8) 0.46189(8) 0.05180(6) 0.0477(2) Uani d . . . 1 . .
S S4 0.55868(9) 0.33802(8) -0.01862(7) 0.0494(2) Uani d . . . 1 . .
H H3WA 0.407(4) 0.324(4) 0.585(3) 0.058(13) Uiso d . . . 1 . .
H H3WB 0.386(5) 0.358(4) 0.656(4) 0.088(17) Uiso d . . . 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.399(4) ?
C1 C6 . 1.403(4) ?
C1 S1 . 1.732(3) ?
C2 C3 . 1.367(5) ?
C2 Cl1 . 1.743(3) ?
C3 C4 . 1.386(5) ?
C3 H3 . 0.95 ?
C4 C5 . 1.371(5) ?
C4 H4 . 0.95 ?
C5 C6 . 1.410(4) ?
C5 Cl2 . 1.739(3) ?
C6 S2 . 1.733(3) ?
C7 C8 . 1.398(5) ?
C7 C12 . 1.404(5) ?
C7 S3 . 1.738(3) ?
C8 C9 . 1.378(6) ?
C8 Cl3 . 1.733(4) ?
C9 C10 . 1.381(6) ?
C9 H9 . 0.95 ?
C10 C11 . 1.372(6) ?
C10 H10 . 0.95 ?
C11 C12 . 1.393(5) ?
C11 Cl4 . 1.735(4) ?
C12 S4 . 1.738(3) ?
C13 O1 . 1.441(4) ?
C13 C14 . 1.467(5) ?
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
C14 C15 . 1.498(5) ?
C14 H14A . 0.99 ?
C14 H14B . 0.99 ?
C15 C16 . 1.499(5) ?
C15 H15A . 0.99 ?
C15 H15B . 0.99 ?
C16 O1 . 1.449(4) ?
C16 H16A . 0.99 ?
C16 H16B . 0.99 ?
C17 O2 . 1.449(4) ?
C17 C18 . 1.505(6) ?
C17 H17A . 0.99 ?
C17 H17B . 0.99 ?
C18 C19 . 1.502(7) ?
C18 H18A . 0.99 ?
C18 H18B . 0.99 ?
C19 C20 . 1.513(6) ?
C19 H19A . 0.99 ?
C19 H19B . 0.99 ?
C20 O2 . 1.447(4) ?
C20 H20A . 0.99 ?
C20 H20B . 0.99 ?
C21 O4 . 1.398(5) ?
C21 C22 . 1.463(7) ?
C21 H21A . 0.99 ?
C21 H21B . 0.99 ?
C22 C23 . 1.405(8) ?
C22 H22A . 0.99 ?
C22 H22B . 0.99 ?
C23 C24 . 1.473(8) ?
C23 H23A . 0.99 ?
C23 H23B . 0.99 ?
C24 O4 . 1.409(7) ?
C24 H24A . 0.99 ?
C24 H24B . 0.99 ?
C25 O5 . 1.409(6) ?
C25 C26 . 1.468(9) ?
C25 H25A . 0.99 ?
C25 H25B . 0.99 ?
C26 C27 . 1.406(9) ?
C26 H26A . 0.99 ?
C26 H26B . 0.99 ?
C27 C28 . 1.428(8) ?
C27 H27A . 0.99 ?
C27 H27B . 0.99 ?
C28 O5 . 1.388(6) ?
C28 H28A . 0.99 ?
C28 H28B . 0.99 ?
Fe1 O3 2_666 2.026(3) ?
Fe1 O3 . 2.026(3) ?
Fe1 O1 . 2.149(2) ?
Fe1 O1 2_666 2.149(2) ?
Fe1 O2 . 2.215(2) ?
Fe1 O2 2_666 2.215(2) ?
Ni1 S2 2_776 2.1427(7) ?
Ni1 S2 . 2.1427(7) ?
Ni1 S1 . 2.1483(8) ?
Ni1 S1 2_776 2.1483(8) ?
Ni2 S4 2_665 2.1428(9) ?
Ni2 S4 . 2.1428(9) ?
Ni2 S3 2_665 2.1451(8) ?
Ni2 S3 . 2.1451(8) ?
O3 H3WA . 0.75(4) ?
O3 H3WB . 0.84(5) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 118.2(3) ?
C2 C1 S1 . . 122.8(2) ?
C6 C1 S1 . . 119.0(2) ?
C3 C2 C1 . . 122.3(3) ?
C3 C2 Cl1 . . 118.4(3) ?
C1 C2 Cl1 . . 119.3(3) ?
C2 C3 C4 . . 119.7(3) ?
C2 C3 H3 . . 120.2 ?
C4 C3 H3 . . 120.2 ?
C5 C4 C3 . . 119.5(3) ?
C5 C4 H4 . . 120.3 ?
C3 C4 H4 . . 120.3 ?
C4 C5 C6 . . 121.7(3) ?
C4 C5 Cl2 . . 119.0(2) ?
C6 C5 Cl2 . . 119.3(3) ?
C1 C6 C5 . . 118.5(3) ?
C1 C6 S2 . . 119.1(2) ?
C5 C6 S2 . . 122.3(2) ?
C8 C7 C12 . . 118.8(3) ?
C8 C7 S3 . . 122.3(3) ?
C12 C7 S3 . . 118.9(3) ?
C9 C8 C7 . . 121.7(4) ?
C9 C8 Cl3 . . 118.9(3) ?
C7 C8 Cl3 . . 119.4(3) ?
C8 C9 C10 . . 119.2(4) ?
C8 C9 H9 . . 120.4 ?
C10 C9 H9 . . 120.4 ?
C11 C10 C9 . . 120.0(4) ?
C11 C10 H10 . . 120.0 ?
C9 C10 H10 . . 120.0 ?
C10 C11 C12 . . 122.0(4) ?
C10 C11 Cl4 . . 118.7(3) ?
C12 C11 Cl4 . . 119.4(3) ?
C11 C12 C7 . . 118.3(3) ?
C11 C12 S4 . . 122.7(3) ?
C7 C12 S4 . . 119.0(3) ?
O1 C13 C14 . . 107.9(3) ?
O1 C13 H13A . . 110.1 ?
C14 C13 H13A . . 110.1 ?
O1 C13 H13B . . 110.1 ?
C14 C13 H13B . . 110.1 ?
H13A C13 H13B . . 108.4 ?
C13 C14 C15 . . 105.6(3) ?
C13 C14 H14A . . 110.6 ?
C15 C14 H14A . . 110.6 ?
C13 C14 H14B . . 110.6 ?
C15 C14 H14B . . 110.6 ?
H14A C14 H14B . . 108.7 ?
C14 C15 C16 . . 103.2(3) ?
C14 C15 H15A . . 111.1 ?
C16 C15 H15A . . 111.1 ?
C14 C15 H15B . . 111.1 ?
C16 C15 H15B . . 111.1 ?
H15A C15 H15B . . 109.1 ?
O1 C16 C15 . . 105.7(3) ?
O1 C16 H16A . . 110.6 ?
C15 C16 H16A . . 110.6 ?
O1 C16 H16B . . 110.6 ?
C15 C16 H16B . . 110.6 ?
H16A C16 H16B . . 108.7 ?
O2 C17 C18 . . 106.0(3) ?
O2 C17 H17A . . 110.5 ?
C18 C17 H17A . . 110.5 ?
O2 C17 H17B . . 110.5 ?
C18 C17 H17B . . 110.5 ?
H17A C17 H17B . . 108.7 ?
C19 C18 C17 . . 103.7(3) ?
C19 C18 H18A . . 111.0 ?
C17 C18 H18A . . 111.0 ?
C19 C18 H18B . . 111.0 ?
C17 C18 H18B . . 111.0 ?
H18A C18 H18B . . 109.0 ?
C18 C19 C20 . . 102.5(3) ?
C18 C19 H19A . . 111.3 ?
C20 C19 H19A . . 111.3 ?
C18 C19 H19B . . 111.3 ?
C20 C19 H19B . . 111.3 ?
H19A C19 H19B . . 109.2 ?
O2 C20 C19 . . 105.1(3) ?
O2 C20 H20A . . 110.7 ?
C19 C20 H20A . . 110.7 ?
O2 C20 H20B . . 110.7 ?
C19 C20 H20B . . 110.7 ?
H20A C20 H20B . . 108.8 ?
O4 C21 C22 . . 105.9(4) ?
O4 C21 H21A . . 110.6 ?
C22 C21 H21A . . 110.6 ?
O4 C21 H21B . . 110.6 ?
C22 C21 H21B . . 110.6 ?
H21A C21 H21B . . 108.7 ?
C23 C22 C21 . . 109.1(5) ?
C23 C22 H22A . . 109.9 ?
C21 C22 H22A . . 109.9 ?
C23 C22 H22B . . 109.9 ?
C21 C22 H22B . . 109.9 ?
H22A C22 H22B . . 108.3 ?
C22 C23 C24 . . 103.8(5) ?
C22 C23 H23A . . 111.0 ?
C24 C23 H23A . . 111.0 ?
C22 C23 H23B . . 111.0 ?
C24 C23 H23B . . 111.0 ?
H23A C23 H23B . . 109.0 ?
O4 C24 C23 . . 107.9(5) ?
O4 C24 H24A . . 110.1 ?
C23 C24 H24A . . 110.1 ?
O4 C24 H24B . . 110.1 ?
C23 C24 H24B . . 110.1 ?
H24A C24 H24B . . 108.4 ?
O5 C25 C26 . . 106.3(5) ?
O5 C25 H25A . . 110.5 ?
C26 C25 H25A . . 110.5 ?
O5 C25 H25B . . 110.5 ?
C26 C25 H25B . . 110.5 ?
H25A C25 H25B . . 108.7 ?
C27 C26 C25 . . 106.6(5) ?
C27 C26 H26A . . 110.4 ?
C25 C26 H26A . . 110.4 ?
C27 C26 H26B . . 110.4 ?
C25 C26 H26B . . 110.4 ?
H26A C26 H26B . . 108.6 ?
C26 C27 C28 . . 107.2(5) ?
C26 C27 H27A . . 110.3 ?
C28 C27 H27A . . 110.3 ?
C26 C27 H27B . . 110.3 ?
C28 C27 H27B . . 110.3 ?
H27A C27 H27B . . 108.5 ?
O5 C28 C27 . . 109.2(5) ?
O5 C28 H28A . . 109.8 ?
C27 C28 H28A . . 109.8 ?
O5 C28 H28B . . 109.8 ?
C27 C28 H28B . . 109.8 ?
H28A C28 H28B . . 108.3 ?
O3 Fe1 O3 2_666 . 180.0 ?
O3 Fe1 O1 2_666 . 87.44(11) ?
O3 Fe1 O1 . . 92.56(11) ?
O3 Fe1 O1 2_666 2_666 92.56(11) ?
O3 Fe1 O1 . 2_666 87.44(11) ?
O1 Fe1 O1 . 2_666 180.00(9) ?
O3 Fe1 O2 2_666 . 89.91(10) ?
O3 Fe1 O2 . . 90.09(10) ?
O1 Fe1 O2 . . 91.97(8) ?
O1 Fe1 O2 2_666 . 88.03(8) ?
O3 Fe1 O2 2_666 2_666 90.09(10) ?
O3 Fe1 O2 . 2_666 89.91(10) ?
O1 Fe1 O2 . 2_666 88.03(8) ?
O1 Fe1 O2 2_666 2_666 91.97(8) ?
O2 Fe1 O2 . 2_666 180.00(12) ?
S2 Ni1 S2 2_776 . 180.0 ?
S2 Ni1 S1 2_776 . 88.04(3) ?
S2 Ni1 S1 . . 91.96(3) ?
S2 Ni1 S1 2_776 2_776 91.96(3) ?
S2 Ni1 S1 . 2_776 88.04(3) ?
S1 Ni1 S1 . 2_776 180.0 ?
S4 Ni2 S4 2_665 . 180.00(5) ?
S4 Ni2 S3 2_665 2_665 92.08(3) ?
S4 Ni2 S3 . 2_665 87.92(3) ?
S4 Ni2 S3 2_665 . 87.92(3) ?
S4 Ni2 S3 . . 92.08(3) ?
S3 Ni2 S3 2_665 . 180.0 ?
C13 O1 C16 . . 108.3(2) ?
C13 O1 Fe1 . . 122.7(2) ?
C16 O1 Fe1 . . 128.25(19) ?
C20 O2 C17 . . 109.5(3) ?
C20 O2 Fe1 . . 124.7(2) ?
C17 O2 Fe1 . . 125.7(2) ?
Fe1 O3 H3WA . . 128.(3) ?
Fe1 O3 H3WB . . 128.(3) ?
H3WA O3 H3WB . . 104.(4) ?
C21 O4 C24 . . 109.2(4) ?
C28 O5 C25 . . 108.0(4) ?
C1 S1 Ni1 . . 104.91(11) ?
C6 S2 Ni1 . . 104.97(10) ?
C7 S3 Ni2 . . 104.76(12) ?
C12 S4 Ni2 . . 104.75(12) ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . -0.6(5) ?
S1 C1 C2 C3 . . . . -179.0(3) ?
C6 C1 C2 Cl1 . . . . 179.1(2) ?
S1 C1 C2 Cl1 . . . . 0.7(4) ?
C1 C2 C3 C4 . . . . 1.1(6) ?
Cl1 C2 C3 C4 . . . . -178.6(3) ?
C2 C3 C4 C5 . . . . -0.8(5) ?
C3 C4 C5 C6 . . . . 0.0(5) ?
C3 C4 C5 Cl2 . . . . 178.6(3) ?
C2 C1 C6 C5 . . . . -0.2(4) ?
S1 C1 C6 C5 . . . . 178.3(2) ?
C2 C1 C6 S2 . . . . -179.0(2) ?
S1 C1 C6 S2 . . . . -0.5(3) ?
C4 C5 C6 C1 . . . . 0.5(5) ?
Cl2 C5 C6 C1 . . . . -178.1(2) ?
C4 C5 C6 S2 . . . . 179.3(2) ?
Cl2 C5 C6 S2 . . . . 0.7(4) ?
C12 C7 C8 C9 . . . . -1.5(5) ?
S3 C7 C8 C9 . . . . 177.5(3) ?
C12 C7 C8 Cl3 . . . . 178.4(2) ?
S3 C7 C8 Cl3 . . . . -2.7(4) ?
C7 C8 C9 C10 . . . . 1.4(6) ?
Cl3 C8 C9 C10 . . . . -178.5(3) ?
C8 C9 C10 C11 . . . . 0.2(6) ?
C9 C10 C11 C12 . . . . -1.7(6) ?
C9 C10 C11 Cl4 . . . . -179.7(3) ?
C10 C11 C12 C7 . . . . 1.5(5) ?
Cl4 C11 C12 C7 . . . . 179.6(2) ?
C10 C11 C12 S4 . . . . -179.1(3) ?
Cl4 C11 C12 S4 . . . . -1.0(4) ?
C8 C7 C12 C11 . . . . 0.0(5) ?
S3 C7 C12 C11 . . . . -179.0(2) ?
C8 C7 C12 S4 . . . . -179.4(2) ?
S3 C7 C12 S4 . . . . 1.6(4) ?
O1 C13 C14 C15 . . . . 16.8(5) ?
C13 C14 C15 C16 . . . . -28.4(5) ?
C14 C15 C16 O1 . . . . 29.9(4) ?
O2 C17 C18 C19 . . . . 25.8(4) ?
C17 C18 C19 C20 . . . . -35.7(4) ?
C18 C19 C20 O2 . . . . 33.0(4) ?
O4 C21 C22 C23 . . . . 14.7(9) ?
C21 C22 C23 C24 . . . . -20.4(10) ?
C22 C23 C24 O4 . . . . 19.0(9) ?
O5 C25 C26 C27 . . . . 16.0(9) ?
C25 C26 C27 C28 . . . . -10.7(11) ?
C26 C27 C28 O5 . . . . 1.4(11) ?
C14 C13 O1 C16 . . . . 2.2(5) ?
C14 C13 O1 Fe1 . . . . -168.5(3) ?
C15 C16 O1 C13 . . . . -20.3(4) ?
C15 C16 O1 Fe1 . . . . 149.7(2) ?
C19 C20 O2 C17 . . . . -17.6(4) ?
C19 C20 O2 Fe1 . . . . 159.0(2) ?
C18 C17 O2 C20 . . . . -5.1(4) ?
C18 C17 O2 Fe1 . . . . 178.3(2) ?
C22 C21 O4 C24 . . . . -2.1(7) ?
C23 C24 O4 C21 . . . . -10.5(8) ?
C27 C28 O5 C25 . . . . 8.9(9) ?
C26 C25 O5 C28 . . . . -15.2(8) ?
C2 C1 S1 Ni1 . . . . 179.9(2) ?
C6 C1 S1 Ni1 . . . . 1.4(3) ?
C1 C6 S2 Ni1 . . . . -0.7(3) ?
C5 C6 S2 Ni1 . . . . -179.5(2) ?
C8 C7 S3 Ni2 . . . . -175.3(3) ?
C12 C7 S3 Ni2 . . . . 3.7(3) ?
C11 C12 S4 Ni2 . . . . 174.6(3) ?
C7 C12 S4 Ni2 . . . . -6.0(3) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C3 H3 S4 2_666 0.95 2.86 3.673(4) 144.5 ?
C13 H13A S2 1_455 0.99 2.98 3.633(4) 124.3 ?
C14 H14A Cl3 2_666 0.99 2.95 3.936(5) 174.0 ?
C16 H16A O2 2_666 0.99 2.63 3.159(4) 113.5 ?
C17 H17B Cl2 2_666 0.99 2.94 3.716(4) 136.0 ?
C20 H20B Cl1 2_676 0.99 2.95 3.742(4) 137.4 ?
C24 H24B Cl3 2_666 0.99 2.87 3.770(7) 151.3 ?
C25 H25A Cl1 1_545 0.99 2.81 3.720(8) 152.7 ?
C28 H28A Cl2 2_666 0.99 2.92 3.778(7) 145.2 ?
C28 H28A S2 2_666 0.99 2.89 3.731(6) 143.1 ?
O3 H3WA O5 . 0.75(4) 1.91(4) 2.658(4) 174.(4) ?
O3 H3WB O4 . 0.84(5) 1.76(6) 2.593(4) 169.(5) ?

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1834784'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   start Validation Reply Form                               #
#----------------------------------------------------------------------------#

_vrf_PLAT241_shelx               
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O7 Check
RESPONSE: O7 belongs to a slightly disordered acetone molecule, no improvement was achieved after using SIMU or EADP commands.
;
_vrf_PLAT242_shelx               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C31 Check
RESPONSE: C31 belongs to a slightly disordered acetone molecule, no improvement was achieved after using SIMU or EADP commands.
;
_vrf_PLAT242_shelx_2             
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C34 Check
RESPONSE: C34 belongs to a slightly disordered acetone molecule, no improvement was achieved after using SIMU or EADP commands.
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         18 Note
RESPONSE: Data collection was performed betwee theta 3 and 25 degrees, it seems logic to miss 18 reflections with theta lower than 3 degrees.
;
_vrf_PLAT242_shelx_3             
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O4 Check
RESPONSE: C31 belongs to a slightly disordered acetone molecule, no improvement was achieved after using SIMU or EADP commands.
;
# Added during the CSD deposition process: Wednesday 04 April 2018 02:02 PM
# end Validation Reply Form


_audit_creation_date             2017-12-07T12:54:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C45 H56 Ca Cl8 Fe2 O10 S8'
_chemical_formula_sum            'C45 H56 Ca Cl8 Fe2 O10 S8'
_chemical_formula_weight         1448.75
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.7382(14)
_cell_length_b                   13.0035(11)
_cell_length_c                   21.730(4)
_cell_angle_alpha                86.715(12)
_cell_angle_beta                 89.542(12)
_cell_angle_gamma                63.187(12)
_cell_volume                     3206.5(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    156
_cell_measurement_theta_min      3
_cell_measurement_theta_max      19
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark blue'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-11 9 1 0.28
2 8 -1 0.192
5 6 -1 0.205
-2 -10 1 0.205
-12 -11 -7 0.404
-8 -7 3 0.394
-5 -4 9 0.461
-1 0 20 0.544
13 12 1 0.263
6 5 -8 0.214
2 1 -19 0.324


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_T_max  0.72

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_number            46297
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.025
_diffrn_reflns_theta_max         25.241
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_Friedel_coverage         0
_reflns_number_total             11552
_reflns_number_gt                7670
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (CCDC, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0583P)²+12.6036P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         11552
_refine_ls_number_parameters     705
_refine_ls_number_restraints     14
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1779
_refine_ls_wR_factor_gt          0.1477
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.511
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.107
# end Validation Reply Form



#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6299(6) 0.1768(6) 0.1150(3) 0.0426(16) Uani 1 1 d . . . . .
C2 C 0.6651(6) 0.0599(6) 0.1301(3) 0.0511(18) Uani 1 1 d . . . . .
C3 C 0.7820(7) -0.0183(6) 0.1436(3) 0.057(2) Uani 1 1 d . . . . .
H3 H 0.802882 -0.097217 0.153843 0.069 Uiso 1 1 calc R U . . .
C4 C 0.8673(6) 0.0197(6) 0.1418(3) 0.0529(18) Uani 1 1 d . . . . .
H4 H 0.947377 -0.032542 0.150888 0.063 Uiso 1 1 calc R U . . .
C5 C 0.8340(5) 0.1354(6) 0.1266(3) 0.0447(16) Uani 1 1 d . . . . .
C6 C 0.7173(5) 0.2169(6) 0.1136(3) 0.0408(16) Uani 1 1 d . . . . .
C7 C 0.2498(5) 0.6761(6) 0.0544(3) 0.0387(15) Uani 1 1 d . . . . .
C8 C 0.1316(5) 0.7604(6) 0.0510(3) 0.0404(15) Uani 1 1 d . . . . .
C9 C 0.1001(6) 0.8763(6) 0.0448(3) 0.0463(17) Uani 1 1 d . . . . .
H9 H 0.01918 0.930371 0.042124 0.056 Uiso 1 1 calc R U . . .
C10 C 0.1851(6) 0.9151(6) 0.0424(3) 0.0443(16) Uani 1 1 d . . . . .
H10 H 0.163707 0.995317 0.038514 0.053 Uiso 1 1 calc R U . . .
C11 C 0.3029(5) 0.8333(6) 0.0457(3) 0.0380(14) Uani 1 1 d . . . . .
C12 C 0.3366(5) 0.7147(5) 0.0503(3) 0.0344(14) Uani 1 1 d . . . . .
C13 C 0.5262(5) 0.2885(5) 0.4493(3) 0.0334(13) Uani 1 1 d . . . . .
C14 C 0.4915(5) 0.2010(5) 0.4565(3) 0.0374(14) Uani 1 1 d . . . . .
C15 C 0.5711(6) 0.0844(5) 0.4545(3) 0.0412(15) Uani 1 1 d . . . . .
H15 H 0.54447 0.026825 0.4579 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6890(6) 0.0540(6) 0.4474(3) 0.0448(16) Uani 1 1 d . . . . .
H16 H 0.745013 -0.025039 0.447822 0.054 Uiso 1 1 calc R U . . .
C17 C 0.7247(5) 0.1388(5) 0.4399(3) 0.0377(14) Uani 1 1 d . . . . .
C18 C 0.6462(5) 0.2565(5) 0.4390(2) 0.0335(13) Uani 1 1 d . . . . .
C19 C 0.3940(5) 0.7977(5) 0.3875(2) 0.0327(13) Uani 1 1 d . . . . .
C20 C 0.3088(5) 0.9150(6) 0.3804(3) 0.0390(15) Uani 1 1 d . . . . .
C21 C 0.3359(6) 1.0025(6) 0.3598(3) 0.0474(16) Uani 1 1 d . . . . .
H21 H 0.276551 1.080281 0.356161 0.057 Uiso 1 1 calc R U . . .
C22 C 0.4505(6) 0.9754(6) 0.3444(3) 0.0498(17) Uani 1 1 d . . . . .
H22 H 0.471084 1.034044 0.329721 0.06 Uiso 1 1 calc R U . . .
C23 C 0.5357(5) 0.8603(6) 0.3508(3) 0.0460(16) Uani 1 1 d . . . . .
C24 C 0.5123(5) 0.7702(5) 0.3732(3) 0.0362(14) Uani 1 1 d . . . . .
C25 C 0.7853(11) 0.6364(11) 0.1387(6) 0.142(6) Uani 1 1 d D . . . .
C26 C 0.7445(12) 0.6794(16) 0.0795(5) 0.175(8) Uani 1 1 d D . . . .
H26A H 0.747424 0.753008 0.071501 0.262 Uiso 1 1 calc R U . . .
H26B H 0.663086 0.691666 0.075044 0.262 Uiso 1 1 calc R U . . .
H26C H 0.793855 0.624282 0.05004 0.262 Uiso 1 1 calc R U . . .
C27 C 0.6635(12) 0.6718(16) 0.1754(7) 0.178(7) Uani 1 1 d D . . . .
H27A H 0.6792 0.666972 0.219835 0.266 Uiso 1 1 calc R U . . .
H27B H 0.630897 0.618806 0.16641 0.266 Uiso 1 1 calc R U . . .
H27C H 0.607025 0.750865 0.162197 0.266 Uiso 1 1 calc R U . . .
C28 C 0.9860(6) 0.7787(6) 0.2977(3) 0.0467(17) Uani 1 1 d . . . . .
C29 C 0.9203(7) 0.9078(7) 0.3012(4) 0.064(2) Uani 1 1 d . . . . .
H29A H 0.84916 0.93808 0.275085 0.096 Uiso 1 1 calc R U . . .
H29B H 0.970682 0.942839 0.286944 0.096 Uiso 1 1 calc R U . . .
H29C H 0.898335 0.926408 0.343998 0.096 Uiso 1 1 calc R U . . .
C30 C 1.0928(7) 0.7135(7) 0.3392(3) 0.064(2) Uani 1 1 d . . . . .
H30A H 1.108911 0.632349 0.344328 0.095 Uiso 1 1 calc R U . . .
H30B H 1.078152 0.747075 0.37948 0.095 Uiso 1 1 calc R U . . .
H30C H 1.160731 0.71876 0.32062 0.095 Uiso 1 1 calc R U . . .
C31 C 1.1693(11) 0.3061(12) 0.1436(5) 0.100(4) Uani 1 1 d . . . . .
C32 C 1.1991(13) 0.2595(17) 0.0879(8) 0.210(10) Uani 1 1 d . . . . .
H32A H 1.146719 0.314107 0.055741 0.315 Uiso 1 1 calc R U . . .
H32B H 1.191543 0.187686 0.08851 0.315 Uiso 1 1 calc R U . . .
H32C H 1.28065 0.242931 0.079137 0.315 Uiso 1 1 calc R U . . .
C33 C 1.2504(14) 0.1911(13) 0.1889(10) 0.198(9) Uani 1 1 d . . . . .
H33A H 1.333325 0.162371 0.178174 0.298 Uiso 1 1 calc R U . . .
H33B H 1.225654 0.130855 0.183359 0.298 Uiso 1 1 calc R U . . .
H33C H 1.240181 0.211763 0.231929 0.298 Uiso 1 1 calc R U . . .
C34 C 0.9025(7) 0.3277(7) 0.2652(3) 0.057(2) Uani 1 1 d . . . . .
C35 C 0.7782(11) 0.372(2) 0.2563(5) 0.240(12) Uani 1 1 d . . . . .
H35A H 0.73792 0.446341 0.275501 0.36 Uiso 1 1 calc R U . . .
H35B H 0.75233 0.317573 0.275276 0.36 Uiso 1 1 calc R U . . .
H35C H 0.759046 0.383663 0.212078 0.36 Uiso 1 1 calc R U . . .
C36 C 0.9635(17) 0.2088(11) 0.2901(6) 0.204(10) Uani 1 1 d . . . . .
H36A H 1.048431 0.183908 0.290894 0.306 Uiso 1 1 calc R U . . .
H36B H 0.945963 0.159069 0.264101 0.306 Uiso 1 1 calc R U . . .
H36C H 0.93709 0.203167 0.332102 0.306 Uiso 1 1 calc R U . . .
C37 C 0.9904(6) 0.3496(6) 0.4686(3) 0.0462(16) Uani 1 1 d . . . . .
C38 C 1.0585(7) 0.2332(7) 0.5002(4) 0.070(2) Uani 1 1 d . . . . .
H38A H 1.118244 0.182911 0.472368 0.105 Uiso 1 1 calc R U . . .
H38B H 1.005079 0.199954 0.51142 0.105 Uiso 1 1 calc R U . . .
H38C H 1.097028 0.240096 0.537479 0.105 Uiso 1 1 calc R U . . .
C39 C 0.8935(6) 0.4391(6) 0.5035(3) 0.0548(19) Uani 1 1 d . . . . .
H39A H 0.856164 0.511228 0.477807 0.082 Uiso 1 1 calc R U . . .
H39B H 0.926086 0.452478 0.541223 0.082 Uiso 1 1 calc R U . . .
H39C H 0.834915 0.412083 0.514384 0.082 Uiso 1 1 calc R U . . .
C40 C 1.2551(8) 0.7993(7) 0.2103(3) 0.060(2) Uani 1 1 d . . . . .
C41 C 1.3737(8) 0.6989(8) 0.2195(4) 0.087(3) Uani 1 1 d . . . . .
H41A H 1.394915 0.685651 0.26347 0.13 Uiso 1 1 calc R U . . .
H41B H 1.431801 0.715121 0.196693 0.13 Uiso 1 1 calc R U . . .
H41C H 1.37227 0.630019 0.204291 0.13 Uiso 1 1 calc R U . . .
C42 C 1.2533(9) 0.9158(8) 0.2087(4) 0.081(3) Uani 1 1 d . . . . .
H42A H 1.172346 0.976145 0.201675 0.122 Uiso 1 1 calc R U . . .
H42B H 1.30275 0.921613 0.175233 0.122 Uiso 1 1 calc R U . . .
H42C H 1.28349 0.92567 0.248089 0.122 Uiso 1 1 calc R U . . .
C43 C 0.4765(7) 0.2763(6) 0.2876(3) 0.0556(19) Uani 1 1 d . . . . .
C44 C 0.4582(8) 0.3986(7) 0.2771(4) 0.074(2) Uani 1 1 d . . . . .
H44A H 0.375324 0.451864 0.283366 0.111 Uiso 1 1 calc R U . . .
H44B H 0.479552 0.410826 0.234868 0.111 Uiso 1 1 calc R U . . .
H44C H 0.507659 0.412955 0.306299 0.111 Uiso 1 1 calc R U . . .
C45 C 0.5994(7) 0.1804(7) 0.2814(4) 0.066(2) Uani 1 1 d . . . . .
H45A H 0.595594 0.108043 0.275266 0.1 Uiso 1 1 calc R U . . .
H45B H 0.64539 0.171573 0.319017 0.1 Uiso 1 1 calc R U . . .
H45C H 0.63696 0.19926 0.246 0.1 Uiso 1 1 calc R U . . .
Ca1 Ca 1.01998(11) 0.52494(12) 0.24383(6) 0.0423(3) Uani 1 1 d . . . . .
Cl1 Cl 0.55935(19) 0.00914(18) 0.13291(12) 0.0769(6) Uani 1 1 d . . . . .
Cl2 Cl 0.94417(14) 0.18171(18) 0.12299(8) 0.0580(5) Uani 1 1 d . . . . .
Cl3 Cl 0.02068(14) 0.71644(18) 0.05549(9) 0.0620(5) Uani 1 1 d . . . . .
Cl4 Cl 0.40838(15) 0.88432(16) 0.04409(9) 0.0543(4) Uani 1 1 d . . . . .
Cl5 Cl 0.34236(14) 0.23739(15) 0.46719(8) 0.0512(4) Uani 1 1 d . . . . .
Cl6 Cl 0.87589(14) 0.09545(15) 0.43289(9) 0.0542(5) Uani 1 1 d . . . . .
Cl7 Cl 0.16274(14) 0.95185(15) 0.39786(8) 0.0528(4) Uani 1 1 d . . . . .
Cl8 Cl 0.68014(16) 0.82930(17) 0.33041(11) 0.0711(6) Uani 1 1 d . . . . .
Fe1 Fe 0.48767(7) 0.43700(8) 0.06094(4) 0.0348(2) Uani 1 1 d . . . . .
Fe2 Fe 0.53171(7) 0.53352(7) 0.43561(4) 0.0322(2) Uani 1 1 d . . . . .
O1 O 1.1630(4) 0.4075(4) 0.3210(2) 0.0524(12) Uani 1 1 d D . . . .
O2 O 1.1663(5) 0.5713(5) 0.2012(2) 0.0562(13) Uani 1 1 d D . . . .
O3 O 0.9092(4) 0.5663(5) 0.3387(2) 0.0598(14) Uani 1 1 d D . . . .
O4 O 0.8675(4) 0.6137(5) 0.1691(3) 0.0673(15) Uani 1 1 d . . . . .
O5 O 0.9537(4) 0.7296(4) 0.2609(2) 0.0486(11) Uani 1 1 d . . . . .
O6 O 1.1258(5) 0.3846(5) 0.1699(3) 0.0812(18) Uani 1 1 d . . . . .
O7 O 0.9481(8) 0.3847(7) 0.2521(3) 0.126(3) Uani 1 1 d . . . . .
O8 O 1.0147(4) 0.3703(5) 0.4170(2) 0.0648(14) Uani 1 1 d . . . . .
O9 O 1.1665(6) 0.7892(5) 0.2040(3) 0.0744(16) Uani 1 1 d . . . . .
O10 O 0.3955(5) 0.2555(5) 0.3018(3) 0.0716(16) Uani 1 1 d . . . . .
S1 S 0.48208(14) 0.27837(15) 0.10100(8) 0.0450(4) Uani 1 1 d . . . . .
S2 S 0.67361(13) 0.36471(14) 0.09518(7) 0.0393(4) Uani 1 1 d . . . . .
S3 S 0.29138(13) 0.52605(14) 0.06288(7) 0.0391(4) Uani 1 1 d . . . . .
S4 S 0.48684(13) 0.61065(14) 0.04984(7) 0.0360(4) Uani 1 1 d . . . . .
S5 S 0.42728(12) 0.43582(13) 0.45597(7) 0.0328(3) Uani 1 1 d . . . . .
S6 S 0.69156(13) 0.36547(13) 0.42457(7) 0.0366(4) Uani 1 1 d . . . . .
S7 S 0.35932(12) 0.68695(13) 0.41287(7) 0.0360(4) Uani 1 1 d . . . . .
S8 S 0.61950(13) 0.62489(14) 0.38285(7) 0.0402(4) Uani 1 1 d . . . . .
H1A H 1.155(6) 0.359(6) 0.356(3) 0.09(3) Uiso 1 1 d D . . . .
H1B H 1.241(2) 0.364(6) 0.316(4) 0.10(3) Uiso 1 1 d D . . . .
H2A H 1.201(9) 0.553(8) 0.159(2) 0.15(4) Uiso 1 1 d D . . . .
H2B H 1.167(8) 0.641(4) 0.201(4) 0.11(4) Uiso 1 1 d D . . . .
H3A H 0.929(6) 0.501(5) 0.371(3) 0.11(3) Uiso 1 1 d D . . . .
H3B H 0.8312(19) 0.591(6) 0.339(3) 0.08(3) Uiso 1 1 d D . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.396(9) . ?
C1 C6 1.426(9) . ?
C1 S1 1.761(6) . ?
C2 C3 1.394(9) . ?
C2 Cl1 1.747(7) . ?
C3 C4 1.381(10) . ?
C3 H3 0.95 . ?
C4 C5 1.387(10) . ?
C4 H4 0.95 . ?
C5 C6 1.402(8) . ?
C5 Cl2 1.759(7) . ?
C6 S2 1.765(7) . ?
C7 C12 1.406(8) . ?
C7 C8 1.406(8) . ?
C7 S3 1.775(7) . ?
C8 C9 1.371(9) . ?
C8 Cl3 1.748(6) . ?
C9 C10 1.387(9) . ?
C9 H9 0.95 . ?
C10 C11 1.393(9) . ?
C10 H10 0.95 . ?
C11 C12 1.400(9) . ?
C11 Cl4 1.746(6) . ?
C12 S4 1.777(6) . ?
C13 C14 1.394(8) . ?
C13 C18 1.412(8) . ?
C13 S5 1.769(6) . ?
C14 C15 1.397(9) . ?
C14 Cl5 1.756(6) . ?
C15 C16 1.380(9) . ?
C15 H15 0.95 . ?
C16 C17 1.371(9) . ?
C16 H16 0.95 . ?
C17 C18 1.400(8) . ?
C17 Cl6 1.753(6) . ?
C18 S6 1.767(6) . ?
C19 C20 1.418(8) . ?
C19 C24 1.420(8) . ?
C19 S7 1.747(6) . ?
C20 C21 1.382(9) . ?
C20 Cl7 1.744(6) . ?
C21 C22 1.382(9) . ?
C21 H21 0.95 . ?
C22 C23 1.397(9) . ?
C22 H22 0.95 . ?
C23 C24 1.394(9) . ?
C23 Cl8 1.756(6) . ?
C24 S8 1.763(6) . ?
C25 O4 1.155(10) . ?
C25 C26 1.378(12) . ?
C25 C27 1.622(14) . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 O5 1.233(8) . ?
C28 C29 1.506(10) . ?
C28 C30 1.507(10) . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
C31 O6 1.108(11) . ?
C31 C32 1.359(15) . ?
C31 C33 1.65(2) . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C33 H33A 0.98 . ?
C33 H33B 0.98 . ?
C33 H33C 0.98 . ?
C34 O7 1.154(9) . ?
C34 C35 1.430(13) . ?
C34 C36 1.454(14) . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?
C36 H36A 0.98 . ?
C36 H36B 0.98 . ?
C36 H36C 0.98 . ?
C37 O8 1.209(7) . ?
C37 C38 1.490(10) . ?
C37 C39 1.498(9) . ?
C38 H38A 0.98 . ?
C38 H38B 0.98 . ?
C38 H38C 0.98 . ?
C39 H39A 0.98 . ?
C39 H39B 0.98 . ?
C39 H39C 0.98 . ?
C40 O9 1.204(9) . ?
C40 C41 1.490(12) . ?
C40 C42 1.504(11) . ?
C41 H41A 0.98 . ?
C41 H41B 0.98 . ?
C41 H41C 0.98 . ?
C42 H42A 0.98 . ?
C42 H42B 0.98 . ?
C42 H42C 0.98 . ?
C43 O10 1.212(9) . ?
C43 C44 1.504(11) . ?
C43 C45 1.510(10) . ?
C44 H44A 0.98 . ?
C44 H44B 0.98 . ?
C44 H44C 0.98 . ?
C45 H45A 0.98 . ?
C45 H45B 0.98 . ?
C45 H45C 0.98 . ?
Ca1 O4 2.356(5) . ?
Ca1 O2 2.369(5) . ?
Ca1 O7 2.380(6) . ?
Ca1 O1 2.389(5) . ?
Ca1 O6 2.411(6) . ?
Ca1 O3 2.434(5) . ?
Ca1 O5 2.452(5) . ?
Fe1 S1 2.2233(19) . ?
Fe1 S3 2.2330(17) . ?
Fe1 S2 2.2330(17) . ?
Fe1 S4 2.2524(18) . ?
Fe1 S4 2.5022(18) 2_665 ?
Fe2 S7 2.2357(17) . ?
Fe2 S8 2.2357(17) . ?
Fe2 S6 2.2399(17) . ?
Fe2 S5 2.2428(16) . ?
Fe2 S5 2.5096(17) 2_666 ?
O1 H1A 0.995(18) . ?
O1 H1B 0.90(2) . ?
O2 H2A 1.003(18) . ?
O2 H2B 0.90(2) . ?
O3 H3A 1.005(18) . ?
O3 H3B 0.90(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
C2 C1 C6 118.4(6) . . ?
C2 C1 S1 123.2(5) . . ?
C6 C1 S1 118.3(5) . . ?
C3 C2 C1 122.4(7) . . ?
C3 C2 Cl1 118.4(6) . . ?
C1 C2 Cl1 119.1(5) . . ?
C4 C3 C2 119.6(7) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 118.8(6) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C6 123.3(7) . . ?
C4 C5 Cl2 118.2(5) . . ?
C6 C5 Cl2 118.5(6) . . ?
C5 C6 C1 117.5(6) . . ?
C5 C6 S2 123.7(5) . . ?
C1 C6 S2 118.8(5) . . ?
C12 C7 C8 117.4(6) . . ?
C12 C7 S3 120.0(5) . . ?
C8 C7 S3 122.6(5) . . ?
C9 C8 C7 122.4(6) . . ?
C9 C8 Cl3 118.6(5) . . ?
C7 C8 Cl3 119.0(5) . . ?
C8 C9 C10 120.6(6) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C11 118.1(6) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C10 C11 C12 122.0(6) . . ?
C10 C11 Cl4 117.3(5) . . ?
C12 C11 Cl4 120.7(5) . . ?
C11 C12 C7 119.5(5) . . ?
C11 C12 S4 121.8(5) . . ?
C7 C12 S4 118.8(5) . . ?
C14 C13 C18 118.0(6) . . ?
C14 C13 S5 122.6(4) . . ?
C18 C13 S5 119.3(4) . . ?
C13 C14 C15 122.4(6) . . ?
C13 C14 Cl5 119.5(5) . . ?
C15 C14 Cl5 118.1(5) . . ?
C16 C15 C14 118.9(6) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C17 C16 C15 119.5(6) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 122.8(6) . . ?
C16 C17 Cl6 117.6(5) . . ?
C18 C17 Cl6 119.6(5) . . ?
C17 C18 C13 118.2(5) . . ?
C17 C18 S6 122.5(4) . . ?
C13 C18 S6 119.2(5) . . ?
C20 C19 C24 117.9(5) . . ?
C20 C19 S7 122.9(4) . . ?
C24 C19 S7 119.1(4) . . ?
C21 C20 C19 123.0(6) . . ?
C21 C20 Cl7 117.9(5) . . ?
C19 C20 Cl7 119.1(5) . . ?
C22 C21 C20 119.1(6) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C21 C22 C23 118.9(6) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 H22 120.6 . . ?
C24 C23 C22 123.6(6) . . ?
C24 C23 Cl8 118.9(5) . . ?
C22 C23 Cl8 117.4(5) . . ?
C23 C24 C19 117.4(6) . . ?
C23 C24 S8 124.1(5) . . ?
C19 C24 S8 118.4(4) . . ?
O4 C25 C26 138.8(12) . . ?
O4 C25 C27 115.5(12) . . ?
C26 C25 C27 101.8(11) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O5 C28 C29 120.2(6) . . ?
O5 C28 C30 121.8(7) . . ?
C29 C28 C30 118.0(7) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O6 C31 C32 148.1(17) . . ?
O6 C31 C33 111.8(11) . . ?
C32 C31 C33 99.4(14) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O7 C34 C35 120.1(13) . . ?
O7 C34 C36 124.3(12) . . ?
C35 C34 C36 115.6(14) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O8 C37 C38 120.4(7) . . ?
O8 C37 C39 121.9(6) . . ?
C38 C37 C39 117.7(6) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O9 C40 C41 123.1(8) . . ?
O9 C40 C42 121.6(8) . . ?
C41 C40 C42 115.2(8) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O10 C43 C44 121.0(7) . . ?
O10 C43 C45 121.1(7) . . ?
C44 C43 C45 117.9(7) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O4 Ca1 O2 101.41(19) . . ?
O4 Ca1 O7 82.9(3) . . ?
O2 Ca1 O7 145.4(3) . . ?
O4 Ca1 O1 169.36(19) . . ?
O2 Ca1 O1 87.13(18) . . ?
O7 Ca1 O1 86.5(2) . . ?
O4 Ca1 O6 87.4(2) . . ?
O2 Ca1 O6 72.3(2) . . ?
O7 Ca1 O6 73.7(2) . . ?
O1 Ca1 O6 89.2(2) . . ?
O4 Ca1 O3 101.23(19) . . ?
O2 Ca1 O3 134.8(2) . . ?
O7 Ca1 O3 76.1(2) . . ?
O1 Ca1 O3 76.49(17) . . ?
O6 Ca1 O3 147.2(2) . . ?
O4 Ca1 O5 78.81(18) . . ?
O2 Ca1 O5 74.22(18) . . ?
O7 Ca1 O5 139.4(3) . . ?
O1 Ca1 O5 109.92(18) . . ?
O6 Ca1 O5 140.2(2) . . ?
O3 Ca1 O5 72.51(17) . . ?
S1 Fe1 S3 88.26(7) . . ?
S1 Fe1 S2 88.55(7) . . ?
S3 Fe1 S2 158.81(7) . . ?
S1 Fe1 S4 162.98(7) . . ?
S3 Fe1 S4 89.17(7) . . ?
S2 Fe1 S4 87.79(7) . . ?
S1 Fe1 S4 98.94(7) . 2_665 ?
S3 Fe1 S4 99.01(6) . 2_665 ?
S2 Fe1 S4 102.19(6) . 2_665 ?
S4 Fe1 S4 98.07(6) . 2_665 ?
S7 Fe2 S8 88.15(6) . . ?
S7 Fe2 S6 159.32(7) . . ?
S8 Fe2 S6 89.41(6) . . ?
S7 Fe2 S5 86.42(6) . . ?
S8 Fe2 S5 160.55(7) . . ?
S6 Fe2 S5 89.11(6) . . ?
S7 Fe2 S5 102.62(6) . 2_666 ?
S8 Fe2 S5 100.39(6) . 2_666 ?
S6 Fe2 S5 98.02(6) . 2_666 ?
S5 Fe2 S5 99.02(6) . 2_666 ?
Ca1 O1 H1A 129(4) . . ?
Ca1 O1 H1B 128(5) . . ?
H1A O1 H1B 96(4) . . ?
Ca1 O2 H2A 126(6) . . ?
Ca1 O2 H2B 126(6) . . ?
H2A O2 H2B 95(4) . . ?
Ca1 O3 H3A 118(5) . . ?
Ca1 O3 H3B 122(5) . . ?
H3A O3 H3B 96(4) . . ?
C25 O4 Ca1 162.8(6) . . ?
C28 O5 Ca1 132.2(4) . . ?
C31 O6 Ca1 166.1(7) . . ?
C34 O7 Ca1 167.5(7) . . ?
C1 S1 Fe1 105.6(2) . . ?
C6 S2 Fe1 105.3(2) . . ?
C7 S3 Fe1 106.0(2) . . ?
C12 S4 Fe1 106.0(2) . . ?
C12 S4 Fe1 101.72(19) . 2_665 ?
Fe1 S4 Fe1 81.93(6) . 2_665 ?
C13 S5 Fe2 105.93(19) . . ?
C13 S5 Fe2 101.82(19) . 2_666 ?
Fe2 S5 Fe2 80.98(6) . 2_666 ?
C18 S6 Fe2 106.1(2) . . ?
C19 S7 Fe2 105.6(2) . . ?
C24 S8 Fe2 105.5(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.3(10) . . . . ?
S1 C1 C2 C3 -177.3(5) . . . . ?
C6 C1 C2 Cl1 179.3(5) . . . . ?
S1 C1 C2 Cl1 2.4(8) . . . . ?
C1 C2 C3 C4 -0.2(11) . . . . ?
Cl1 C2 C3 C4 -179.9(5) . . . . ?
C2 C3 C4 C5 -0.1(10) . . . . ?
C3 C4 C5 C6 0.9(10) . . . . ?
C3 C4 C5 Cl2 -178.7(5) . . . . ?
C4 C5 C6 C1 -1.5(9) . . . . ?
Cl2 C5 C6 C1 178.1(4) . . . . ?
C4 C5 C6 S2 179.2(5) . . . . ?
Cl2 C5 C6 S2 -1.2(7) . . . . ?
C2 C1 C6 C5 1.1(9) . . . . ?
S1 C1 C6 C5 178.2(4) . . . . ?
C2 C1 C6 S2 -179.5(5) . . . . ?
S1 C1 C6 S2 -2.4(7) . . . . ?
C12 C7 C8 C9 -1.0(9) . . . . ?
S3 C7 C8 C9 179.6(5) . . . . ?
C12 C7 C8 Cl3 179.7(4) . . . . ?
S3 C7 C8 Cl3 0.3(7) . . . . ?
C7 C8 C9 C10 -0.7(10) . . . . ?
Cl3 C8 C9 C10 178.6(5) . . . . ?
C8 C9 C10 C11 0.7(9) . . . . ?
C9 C10 C11 C12 1.1(9) . . . . ?
C9 C10 C11 Cl4 -178.8(5) . . . . ?
C10 C11 C12 C7 -2.8(9) . . . . ?
Cl4 C11 C12 C7 177.1(4) . . . . ?
C10 C11 C12 S4 176.1(5) . . . . ?
Cl4 C11 C12 S4 -4.1(7) . . . . ?
C8 C7 C12 C11 2.6(8) . . . . ?
S3 C7 C12 C11 -177.9(4) . . . . ?
C8 C7 C12 S4 -176.2(4) . . . . ?
S3 C7 C12 S4 3.2(7) . . . . ?
C18 C13 C14 C15 0.8(9) . . . . ?
S5 C13 C14 C15 -176.5(5) . . . . ?
C18 C13 C14 Cl5 -178.2(4) . . . . ?
S5 C13 C14 Cl5 4.6(7) . . . . ?
C13 C14 C15 C16 2.4(9) . . . . ?
Cl5 C14 C15 C16 -178.6(5) . . . . ?
C14 C15 C16 C17 -2.8(9) . . . . ?
C15 C16 C17 C18 0.0(10) . . . . ?
C15 C16 C17 Cl6 178.6(5) . . . . ?
C16 C17 C18 C13 3.2(9) . . . . ?
Cl6 C17 C18 C13 -175.3(4) . . . . ?
C16 C17 C18 S6 -176.1(5) . . . . ?
Cl6 C17 C18 S6 5.4(7) . . . . ?
C14 C13 C18 C17 -3.5(8) . . . . ?
S5 C13 C18 C17 173.8(4) . . . . ?
C14 C13 C18 S6 175.8(4) . . . . ?
S5 C13 C18 S6 -6.8(6) . . . . ?
C24 C19 C20 C21 0.7(9) . . . . ?
S7 C19 C20 C21 -179.3(5) . . . . ?
C24 C19 C20 Cl7 -179.8(4) . . . . ?
S7 C19 C20 Cl7 0.2(7) . . . . ?
C19 C20 C21 C22 0.9(10) . . . . ?
Cl7 C20 C21 C22 -178.6(5) . . . . ?
C20 C21 C22 C23 -0.6(10) . . . . ?
C21 C22 C23 C24 -1.3(11) . . . . ?
C21 C22 C23 Cl8 179.7(5) . . . . ?
C22 C23 C24 C19 2.8(10) . . . . ?
Cl8 C23 C24 C19 -178.2(5) . . . . ?
C22 C23 C24 S8 -178.8(5) . . . . ?
Cl8 C23 C24 S8 0.3(8) . . . . ?
C20 C19 C24 C23 -2.4(8) . . . . ?
S7 C19 C24 C23 177.6(5) . . . . ?
C20 C19 C24 S8 179.1(4) . . . . ?
S7 C19 C24 S8 -0.9(7) . . . . ?
C26 C25 O4 Ca1 -148(2) . . . . ?
C27 C25 O4 Ca1 60(4) . . . . ?
C29 C28 O5 Ca1 -174.4(4) . . . . ?
C30 C28 O5 Ca1 7.2(9) . . . . ?
C32 C31 O6 Ca1 146(2) . . . . ?
C33 C31 O6 Ca1 -46(4) . . . . ?
C35 C34 O7 Ca1 70(4) . . . . ?
C36 C34 O7 Ca1 -111(4) . . . . ?
C2 C1 S1 Fe1 -168.6(5) . . . . ?
C6 C1 S1 Fe1 14.5(5) . . . . ?
C5 C6 S2 Fe1 168.4(5) . . . . ?
C1 C6 S2 Fe1 -10.9(5) . . . . ?
C12 C7 S3 Fe1 -2.1(5) . . . . ?
C8 C7 S3 Fe1 177.3(5) . . . . ?
C11 C12 S4 Fe1 178.6(4) . . . . ?
C7 C12 S4 Fe1 -2.6(5) . . . . ?
C11 C12 S4 Fe1 -96.6(5) . . . 2_665 ?
C7 C12 S4 Fe1 82.3(5) . . . 2_665 ?
C14 C13 S5 Fe2 -177.4(4) . . . . ?
C18 C13 S5 Fe2 5.3(5) . . . . ?
C14 C13 S5 Fe2 98.7(5) . . . 2_666 ?
C18 C13 S5 Fe2 -78.5(4) . . . 2_666 ?
C17 C18 S6 Fe2 -176.1(4) . . . . ?
C13 C18 S6 Fe2 4.6(5) . . . . ?
C20 C19 S7 Fe2 -166.9(4) . . . . ?
C24 C19 S7 Fe2 13.1(5) . . . . ?
C23 C24 S8 Fe2 169.9(5) . . . . ?
C19 C24 S8 Fe2 -11.7(5) . . . . ?

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

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1834785'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;

_audit_creation_date             2018-01-16T12:23:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C48 H56 Cl8 Fe3 O10 S8'
_chemical_formula_sum            'C48 H56 Cl8 Fe3 O10 S8'
_chemical_formula_weight         1500.55

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6545(3)
_cell_length_b                   11.3055(3)
_cell_length_c                   14.3597(4)
_cell_angle_alpha                93.025(2)
_cell_angle_beta                 111.050(2)
_cell_angle_gamma                98.246(2)
_cell_volume                     1587.36(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6367
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      24.8
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.042
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             766

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_T_max  0.938

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       'Bruker Kappa Apex II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_number            24353
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.994
_diffrn_reflns_theta_max         24.106
_diffrn_reflns_theta_full        24.106
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             5033
_reflns_number_gt                3792
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1355P)²+1.4768P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5033
_refine_ls_number_parameters     349
_refine_ls_number_restraints     45
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.2165
_refine_ls_wR_factor_gt          0.2013
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.146
_refine_diff_density_min         -2.355
_refine_diff_density_rms         0.135

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4067(7) 0.1504(6) 0.2373(5) 0.0356(16) Uani 1 1 d . . . . .
C2 C 0.2999(8) 0.1509(7) 0.1450(6) 0.0481(19) Uani 1 1 d . . . . .
C3 C 0.3206(11) 0.1400(9) 0.0557(6) 0.069(3) Uani 1 1 d . . . . .
H3 H 0.246015 0.134944 -0.006433 0.083 Uiso 1 1 calc R U . . .
C4 C 0.4478(11) 0.1365(10) 0.0569(6) 0.079(3) Uani 1 1 d . . . . .
H4 H 0.462988 0.134571 -0.004432 0.094 Uiso 1 1 calc R U . . .
C5 C 0.5554(9) 0.1359(8) 0.1459(6) 0.061(2) Uani 1 1 d . . . . .
C6 C 0.5381(8) 0.1442(6) 0.2373(5) 0.0421(18) Uani 1 1 d . . . . .
C7 C 0.6177(6) 0.1452(5) 0.6919(4) 0.0264(14) Uani 1 1 d . . . . .
C8 C 0.7499(7) 0.1443(5) 0.6930(5) 0.0303(14) Uani 1 1 d . . . . .
C9 C 0.8577(7) 0.1547(6) 0.7859(5) 0.0388(16) Uani 1 1 d . . . . .
C10 C 0.8367(9) 0.1679(7) 0.8750(5) 0.051(2) Uani 1 1 d . . . . .
H10 H 0.911033 0.173116 0.937258 0.061 Uiso 1 1 calc R U . . .
C11 C 0.7070(8) 0.1736(7) 0.8735(5) 0.0468(19) Uani 1 1 d . . . . .
H11 H 0.69237 0.185329 0.934571 0.056 Uiso 1 1 calc R U . . .
C12 C 0.6005(7) 0.1620(6) 0.7834(5) 0.0372(16) Uani 1 1 d . . . . .
C13 C 0.0470(9) 0.2656(6) 0.3780(6) 0.052(2) Uani 1 1 d . . . . .
H13A H 0.115184 0.290297 0.347549 0.062 Uiso 1 1 calc R U . . .
H13B H -0.044495 0.273585 0.330336 0.062 Uiso 1 1 calc R U . . .
C14 C 0.0494(9) 0.1368(6) 0.4041(7) 0.054(2) Uani 1 1 d . . . . .
H14A H -0.043788 0.088576 0.376436 0.064 Uiso 1 1 calc R U . . .
H14B H 0.108524 0.098357 0.376596 0.064 Uiso 1 1 calc R U . . .
C15 C 0.1064(8) 0.1471(6) 0.5182(6) 0.049(2) Uani 1 1 d . . . . .
H15A H 0.033163 0.121797 0.543811 0.058 Uiso 1 1 calc R U . . .
H15B H 0.177827 0.096797 0.542867 0.058 Uiso 1 1 calc R U . . .
C16 C 0.1644(9) 0.2756(7) 0.5497(7) 0.057(2) Uani 1 1 d . . . . .
H16A H 0.160544 0.300741 0.615596 0.069 Uiso 1 1 calc R U . . .
H16B H 0.260654 0.292242 0.554944 0.069 Uiso 1 1 calc R U . . .
C17 C 0.7573(11) 0.4896(10) 0.7778(8) 0.079(3) Uani 1 1 d . . . . .
H17A H 0.826762 0.552497 0.827551 0.095 Uiso 1 1 calc R U . . .
H17B H 0.772714 0.410001 0.800724 0.095 Uiso 1 1 calc R U . . .
C18 C 0.6156(12) 0.5087(10) 0.7666(10) 0.088(3) Uani 1 1 d . . . . .
H18A H 0.579839 0.457806 0.808642 0.106 Uiso 1 1 calc R U . . .
H18B H 0.615163 0.594047 0.78576 0.106 Uiso 1 1 calc R U . . .
C19 C 0.5379(11) 0.4746(11) 0.6636(10) 0.091(3) Uani 1 1 d . . . . .
H19A H 0.46564 0.524195 0.639349 0.109 Uiso 1 1 calc R U . . .
H19B H 0.494027 0.389039 0.652285 0.109 Uiso 1 1 calc R U . . .
C20 C 0.6347(10) 0.4938(10) 0.6082(10) 0.088(3) Uani 1 1 d . . . . .
H20A H 0.613744 0.427325 0.554291 0.106 Uiso 1 1 calc R U . . .
H20B H 0.630363 0.570914 0.578456 0.106 Uiso 1 1 calc R U . . .
C21 C 0.7779(12) 0.4788(13) 0.1946(9) 0.106(4) Uani 1 1 d D U . . .
H21A H 0.751078 0.397195 0.210645 0.127 Uiso 1 1 calc R U . . .
H21B H 0.816103 0.533211 0.258153 0.127 Uiso 1 1 calc R U . . .
C22 C 0.6714(16) 0.5137(17) 0.1360(10) 0.147(6) Uani 1 1 d D U . . .
H22A H 0.66299 0.593928 0.161941 0.177 Uiso 1 1 calc R U . . .
H22B H 0.587768 0.455796 0.127064 0.177 Uiso 1 1 calc R U . . .
C23 C 0.6956(19) 0.518(2) 0.0405(13) 0.201(7) Uani 1 1 d D U . . .
H23A H 0.642082 0.446478 -0.006844 0.241 Uiso 1 1 calc R U . . .
H23B H 0.666166 0.590734 0.009101 0.241 Uiso 1 1 calc R U . . .
C24 C 0.8345(18) 0.523(2) 0.0612(12) 0.184(7) Uani 1 1 d D U . . .
H24A H 0.880823 0.606412 0.066272 0.221 Uiso 1 1 calc R U . . .
H24B H 0.848379 0.473726 0.007563 0.221 Uiso 1 1 calc R U . . .
Cl1 Cl 0.1388(2) 0.1604(2) 0.14367(17) 0.0672(7) Uani 1 1 d . . . . .
Cl2 Cl 0.7170(3) 0.1232(3) 0.14489(17) 0.0967(11) Uani 1 1 d . . . . .
Cl3 Cl 1.0205(2) 0.1458(2) 0.78945(15) 0.0643(6) Uani 1 1 d . . . . .
Cl4 Cl 0.4393(2) 0.17150(18) 0.78381(14) 0.0516(5) Uani 1 1 d . . . . .
Fe1 Fe 0.56923(8) 0.10262(7) 0.45930(6) 0.0230(3) Uani 1 1 d . . . . .
Fe2 Fe 0 0.5 0.5 0.0684(6) Uani 1 2 d S . P . .
O1 O 0.0802(5) 0.3378(4) 0.4721(4) 0.0472(13) Uani 1 1 d . . . . .
O2 O 0.7662(7) 0.4957(6) 0.6856(5) 0.0735(18) Uani 1 1 d . . . . .
O3 O 0.8859(14) 0.4757(17) 0.1526(10) 0.224(6) Uani 1 1 d D U . . .
O4W O -0.1943(5) 0.4305(4) 0.3744(4) 0.0535(14) Uani 1 1 d . . . . .
O5W O -0.0752(6) 0.4044(4) 0.6036(4) 0.0547(14) Uani 1 1 d . . . . .
S1 S 0.38264(17) 0.15464(14) 0.35161(12) 0.0326(4) Uani 1 1 d . . . . .
S2 S 0.67175(17) 0.14166(15) 0.35168(12) 0.0350(4) Uani 1 1 d . . . . .
S3 S 0.47879(15) 0.12095(13) 0.57603(11) 0.0250(4) Uani 1 1 d . . . . .
S4 S 0.77522(16) 0.12649(14) 0.57937(12) 0.0286(4) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.404(10) . ?
C1 C6 1.411(10) . ?
C1 S1 1.749(7) . ?
C2 C3 1.380(12) . ?
C2 Cl1 1.729(8) . ?
C3 C4 1.356(14) . ?
C3 H3 0.95 . ?
C4 C5 1.378(12) . ?
C4 H4 0.95 . ?
C5 C6 1.390(10) . ?
C5 Cl2 1.753(9) . ?
C6 S2 1.751(7) . ?
C7 C12 1.397(9) . ?
C7 C8 1.405(9) . ?
C7 S3 1.761(6) . ?
C8 C9 1.399(9) . ?
C8 S4 1.753(6) . ?
C9 C10 1.381(10) . ?
C9 Cl3 1.734(7) . ?
C10 C11 1.384(11) . ?
C10 H10 0.95 . ?
C11 C12 1.366(10) . ?
C11 H11 0.95 . ?
C12 Cl4 1.738(7) . ?
C13 O1 1.439(9) . ?
C13 C14 1.524(10) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 C15 1.520(12) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.473(10) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 O1 1.445(9) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 O2 1.366(11) . ?
C17 C18 1.508(14) . ?
C17 H17A 0.99 . ?
C17 H17B 0.99 . ?
C18 C19 1.411(16) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 C20 1.512(15) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 O2 1.438(13) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 C22 1.277(13) . ?
C21 O3 1.482(13) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 C23 1.486(15) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C23 C24 1.394(15) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 O3 1.394(14) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
Fe1 S1 2.2164(18) . ?
Fe1 S4 2.2192(17) . ?
Fe1 S2 2.2188(17) . ?
Fe1 S3 2.2275(16) . ?
Fe1 S3 2.4931(16) 2_656 ?
Fe2 O5W 2.192(5) . ?
Fe2 O5W 2.192(5) 2_566 ?
Fe2 O4W 2.204(6) . ?
Fe2 O4W 2.204(6) 2_566 ?
Fe2 O1 2.208(4) 2_566 ?
Fe2 O1 2.208(4) . ?

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
C2 C1 C6 118.4(6) . . ?
C2 C1 S1 122.6(6) . . ?
C6 C1 S1 118.9(5) . . ?
C3 C2 C1 121.1(8) . . ?
C3 C2 Cl1 119.8(6) . . ?
C1 C2 Cl1 119.1(6) . . ?
C4 C3 C2 119.7(8) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.8(8) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 121.0(9) . . ?
C4 C5 Cl2 120.0(7) . . ?
C6 C5 Cl2 119.0(6) . . ?
C5 C6 C1 118.7(7) . . ?
C5 C6 S2 122.3(6) . . ?
C1 C6 S2 118.9(5) . . ?
C12 C7 C8 118.7(6) . . ?
C12 C7 S3 122.1(5) . . ?
C8 C7 S3 119.2(5) . . ?
C9 C8 C7 118.4(6) . . ?
C9 C8 S4 121.8(5) . . ?
C7 C8 S4 119.7(5) . . ?
C10 C9 C8 121.4(7) . . ?
C10 C9 Cl3 119.1(5) . . ?
C8 C9 Cl3 119.4(5) . . ?
C9 C10 C11 119.9(7) . . ?
C9 C10 H10 120 . . ?
C11 C10 H10 120 . . ?
C12 C11 C10 119.3(6) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C7 122.2(7) . . ?
C11 C12 Cl4 118.3(5) . . ?
C7 C12 Cl4 119.5(5) . . ?
O1 C13 C14 105.2(6) . . ?
O1 C13 H13A 110.7 . . ?
C14 C13 H13A 110.7 . . ?
O1 C13 H13B 110.7 . . ?
C14 C13 H13B 110.7 . . ?
H13A C13 H13B 108.8 . . ?
C15 C14 C13 105.3(6) . . ?
C15 C14 H14A 110.7 . . ?
C13 C14 H14A 110.7 . . ?
C15 C14 H14B 110.7 . . ?
C13 C14 H14B 110.7 . . ?
H14A C14 H14B 108.8 . . ?
C16 C15 C14 104.5(6) . . ?
C16 C15 H15A 110.9 . . ?
C14 C15 H15A 110.9 . . ?
C16 C15 H15B 110.9 . . ?
C14 C15 H15B 110.9 . . ?
H15A C15 H15B 108.9 . . ?
O1 C16 C15 104.9(6) . . ?
O1 C16 H16A 110.8 . . ?
C15 C16 H16A 110.8 . . ?
O1 C16 H16B 110.8 . . ?
C15 C16 H16B 110.8 . . ?
H16A C16 H16B 108.8 . . ?
O2 C17 C18 107.0(9) . . ?
O2 C17 H17A 110.3 . . ?
C18 C17 H17A 110.3 . . ?
O2 C17 H17B 110.3 . . ?
C18 C17 H17B 110.3 . . ?
H17A C17 H17B 108.6 . . ?
C19 C18 C17 103.8(9) . . ?
C19 C18 H18A 111 . . ?
C17 C18 H18A 111 . . ?
C19 C18 H18B 111 . . ?
C17 C18 H18B 111 . . ?
H18A C18 H18B 109 . . ?
C18 C19 C20 107.3(9) . . ?
C18 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
C18 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.5 . . ?
O2 C20 C19 103.2(9) . . ?
O2 C20 H20A 111.1 . . ?
C19 C20 H20A 111.1 . . ?
O2 C20 H20B 111.1 . . ?
C19 C20 H20B 111.1 . . ?
H20A C20 H20B 109.1 . . ?
C22 C21 O3 114.1(11) . . ?
C22 C21 H21A 108.7 . . ?
O3 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
O3 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 C23 102.9(13) . . ?
C21 C22 H22A 111.2 . . ?
C23 C22 H22A 111.2 . . ?
C21 C22 H22B 111.2 . . ?
C23 C22 H22B 111.2 . . ?
H22A C22 H22B 109.1 . . ?
C24 C23 C22 108.8(14) . . ?
C24 C23 H23A 109.9 . . ?
C22 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
C22 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
C23 C24 O3 105.9(13) . . ?
C23 C24 H24A 110.6 . . ?
O3 C24 H24A 110.6 . . ?
C23 C24 H24B 110.6 . . ?
O3 C24 H24B 110.6 . . ?
H24A C24 H24B 108.7 . . ?
S1 Fe1 S4 157.99(7) . . ?
S1 Fe1 S2 88.85(7) . . ?
S4 Fe1 S2 87.74(6) . . ?
S1 Fe1 S3 87.54(6) . . ?
S4 Fe1 S3 89.59(6) . . ?
S2 Fe1 S3 163.45(7) . . ?
S1 Fe1 S3 102.54(6) . 2_656 ?
S4 Fe1 S3 99.47(6) . 2_656 ?
S2 Fe1 S3 97.70(6) . 2_656 ?
S3 Fe1 S3 98.85(5) . 2_656 ?
O5W Fe2 O5W 180.00(17) . 2_566 ?
O5W Fe2 O4W 90.5(2) . . ?
O5W Fe2 O4W 89.5(2) 2_566 . ?
O5W Fe2 O4W 89.5(2) . 2_566 ?
O5W Fe2 O4W 90.5(2) 2_566 2_566 ?
O4W Fe2 O4W 180 . 2_566 ?
O5W Fe2 O1 92.04(19) . 2_566 ?
O5W Fe2 O1 87.97(19) 2_566 2_566 ?
O4W Fe2 O1 90.15(19) . 2_566 ?
O4W Fe2 O1 89.85(19) 2_566 2_566 ?
O5W Fe2 O1 87.97(19) . . ?
O5W Fe2 O1 92.03(19) 2_566 . ?
O4W Fe2 O1 89.85(19) . . ?
O4W Fe2 O1 90.15(19) 2_566 . ?
O1 Fe2 O1 180 2_566 . ?
C13 O1 C16 106.9(6) . . ?
C13 O1 Fe2 128.1(4) . . ?
C16 O1 Fe2 124.6(5) . . ?
C17 O2 C20 111.7(8) . . ?
C24 O3 C21 103.7(11) . . ?
C1 S1 Fe1 104.7(2) . . ?
C6 S2 Fe1 104.6(2) . . ?
C7 S3 Fe1 105.6(2) . . ?
C7 S3 Fe1 102.28(19) . 2_656 ?
Fe1 S3 Fe1 81.15(5) . 2_656 ?
C8 S4 Fe1 105.8(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 2.9(11) . . . . ?
S1 C1 C2 C3 -176.0(6) . . . . ?
C6 C1 C2 Cl1 -179.2(5) . . . . ?
S1 C1 C2 Cl1 2.0(8) . . . . ?
C1 C2 C3 C4 -4.3(14) . . . . ?
Cl1 C2 C3 C4 177.8(8) . . . . ?
C2 C3 C4 C5 4.3(16) . . . . ?
C3 C4 C5 C6 -3.0(16) . . . . ?
C3 C4 C5 Cl2 176.6(8) . . . . ?
C4 C5 C6 C1 1.6(13) . . . . ?
Cl2 C5 C6 C1 -177.9(6) . . . . ?
C4 C5 C6 S2 179.1(7) . . . . ?
Cl2 C5 C6 S2 -0.4(10) . . . . ?
C2 C1 C6 C5 -1.5(10) . . . . ?
S1 C1 C6 C5 177.4(6) . . . . ?
C2 C1 C6 S2 -179.2(5) . . . . ?
S1 C1 C6 S2 -0.3(8) . . . . ?
C12 C7 C8 C9 2.9(9) . . . . ?
S3 C7 C8 C9 -175.3(5) . . . . ?
C12 C7 C8 S4 -178.7(4) . . . . ?
S3 C7 C8 S4 3.1(7) . . . . ?
C7 C8 C9 C10 -1.2(10) . . . . ?
S4 C8 C9 C10 -179.6(6) . . . . ?
C7 C8 C9 Cl3 176.6(5) . . . . ?
S4 C8 C9 Cl3 -1.8(8) . . . . ?
C8 C9 C10 C11 -1.3(11) . . . . ?
Cl3 C9 C10 C11 -179.1(6) . . . . ?
C9 C10 C11 C12 2.1(12) . . . . ?
C10 C11 C12 C7 -0.3(11) . . . . ?
C10 C11 C12 Cl4 -179.2(6) . . . . ?
C8 C7 C12 C11 -2.2(9) . . . . ?
S3 C7 C12 C11 175.9(5) . . . . ?
C8 C7 C12 Cl4 176.6(5) . . . . ?
S3 C7 C12 Cl4 -5.3(7) . . . . ?
O1 C13 C14 C15 -8.3(8) . . . . ?
C13 C14 C15 C16 -13.8(8) . . . . ?
C14 C15 C16 O1 31.1(8) . . . . ?
O2 C17 C18 C19 23.9(12) . . . . ?
C17 C18 C19 C20 -26.6(12) . . . . ?
C18 C19 C20 O2 20.3(12) . . . . ?
O3 C21 C22 C23 9(2) . . . . ?
C21 C22 C23 C24 -19(3) . . . . ?
C22 C23 C24 O3 22(3) . . . . ?
C14 C13 O1 C16 28.3(8) . . . . ?
C14 C13 O1 Fe2 -144.4(5) . . . . ?
C15 C16 O1 C13 -37.8(8) . . . . ?
C15 C16 O1 Fe2 135.2(5) . . . . ?
C18 C17 O2 C20 -11.4(11) . . . . ?
C19 C20 O2 C17 -4.8(11) . . . . ?
C23 C24 O3 C21 -16(3) . . . . ?
C22 C21 O3 C24 4(2) . . . . ?
C2 C1 S1 Fe1 165.1(5) . . . . ?
C6 C1 S1 Fe1 -13.7(6) . . . . ?
C5 C6 S2 Fe1 -163.5(6) . . . . ?
C1 C6 S2 Fe1 14.1(6) . . . . ?
C12 C7 S3 Fe1 179.5(4) . . . . ?
C8 C7 S3 Fe1 -2.4(5) . . . . ?
C12 C7 S3 Fe1 -96.4(5) . . . 2_656 ?
C8 C7 S3 Fe1 81.7(5) . . . 2_656 ?
C9 C8 S4 Fe1 176.2(5) . . . . ?
C7 C8 S4 Fe1 -2.1(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
C14 H14B S4 0.99 2.98 3.710(8) 131 2_656 yes
C15 H15A S4 0.99 2.98 3.910(8) 157.6 1_455 yes
C21 H21B O4W 0.99 2.11 2.589(12) 107.7 1_655 yes

####################################################################### 
# 
# 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_02190ElisaHernandez_transp
_database_code_depnum_ccdc_archive 'CCDC 1834789'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_02190ElisaHernandez_transp 
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        6.3 Ratio
RESPONSE: Tetrahydrofurane coordinated molecules presented some disorder, we could get only a few crystals of compound 8 and restraints did not improve our chemical model.
;
_vrf_PLAT234_02190ElisaHernandez_transp 
;
PROBLEM: Large Hirshfeld Difference C25      --C26              0.26 Ang.
RESPONSE: Tetrahydrofurane coordinated molecules presented some disorder, we could get only a few crystals of compound 8 and restraints did not improve our chemical model.
;
_vrf_PLAT241_02190ElisaHernandez_transp 
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C25 Check
RESPONSE: Tetrahydrofurane coordinated molecules presented some disorder, we could get only a few crystals of compound 8 and restraints did not improve our chemical model.
;
_vrf_PLAT341_02190ElisaHernandez_transp 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01597 Ang.
RESPONSE: Tetrahydrofurane coordinated molecules presented some disorder, we could get only a few crystals of compound 8 and restraints did not improve our chemical model.
;
# Added during the CSD deposition process: Wednesday 04 April 2018 02:02 PM
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            DH194_transp_200K
_chemical_formula_moiety         'C34 H37 Cl7 K O6 S6 Zn3'
_chemical_formula_sum            'C34 H37 Cl7 K O6 S6 Zn3'
_chemical_formula_iupac          ?
_chemical_formula_weight         1217.35

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.7557(4)
_cell_length_b                   13.7884(4)
_cell_length_c                   14.2273(4)
_cell_angle_alpha                94.417(2)
_cell_angle_beta                 112.4710(10)
_cell_angle_gamma                105.8270(10)
_cell_volume                     2348.67(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7363
_cell_measurement_theta_min      2.4444
_cell_measurement_theta_max      20.3040
_cell_measurement_temperature    200.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.042
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1226

_exptl_absorpt_coefficient_mu    2.314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  0.91

_exptl_special_details           
;
;

_diffrn_ambient_temperature      200.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            77400
_diffrn_reflns_av_R_equivalents  0.0987
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             8578
_reflns_number_gt                5503
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1798
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_number_reflns         8578
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1029P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.896
_refine_diff_density_min         -1.040
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.1495(5) 0.5629(5) 0.9705(5) 0.0337(16) Uani d . . . 1 . .
C C2 0.0587(6) 0.6006(6) 0.9476(6) 0.0436(18) Uani d . . . 1 . .
C C3 0.0696(7) 0.6897(7) 1.0075(7) 0.054(2) Uani d . . . 1 . .
H H3 0.0073 0.7131 0.9914 0.065 Uiso calc U . R 1 . .
C C4 0.1656(7) 0.7440(6) 1.0875(7) 0.050(2) Uani d . . . 1 . .
H H4 0.1719 0.8057 1.1274 0.06 Uiso calc U . R 1 . .
C C5 0.2564(6) 0.7089(5) 1.1117(5) 0.0407(17) Uani d . . . 1 . .
C C6 0.2498(5) 0.6177(5) 1.0547(5) 0.0339(16) Uani d . . . 1 . .
C C8 0.6669(5) 0.8050(5) 0.9965(5) 0.0377(16) Uani d . . . 1 . .
C C9 0.6264(6) 0.8839(5) 1.0148(6) 0.0425(17) Uani d . . . 1 . .
C C10 0.6355(7) 0.9672(6) 0.9692(7) 0.058(2) Uani d . . . 1 . .
H H10 0.6067 1.0193 0.9825 0.07 Uiso calc U . R 1 . .
C C11 0.6878(7) 0.9739(6) 0.9031(8) 0.070(3) Uani d . . . 1 . .
H H11 0.6946 1.0311 0.8701 0.084 Uiso calc U . R 1 . .
C C12 0.7302(7) 0.8989(6) 0.8843(7) 0.057(2) Uani d . . . 1 . .
C C13 0.7203(6) 0.8107(6) 0.9290(6) 0.0448(18) Uani d . . . 1 . .
C C14 0.3992(5) 0.6981(5) 0.7772(5) 0.0336(15) Uani d . . . 1 . .
C C15 0.4170(6) 0.7878(6) 0.7368(6) 0.0448(18) Uani d . . . 1 . .
C C16 0.4743(7) 0.8000(6) 0.6751(6) 0.057(2) Uani d . . . 1 . .
C C17 0.5159(7) 0.7246(7) 0.6523(7) 0.061(2) Uani d . . . 1 . .
H H17 0.5607 0.7364 0.6148 0.073 Uiso calc U . R 1 . .
C C18 0.4917(6) 0.6316(6) 0.6846(6) 0.0490(19) Uani d . . . 1 . .
H H18 0.5152 0.5777 0.665 0.059 Uiso calc U . R 1 . .
C C19 0.4321(5) 0.6185(5) 0.7464(5) 0.0362(16) Uani d . . . 1 . .
C C20 0.3113(10) 0.4545(8) 0.3929(8) 0.086(3) Uani d . . . 1 . .
H H20A 0.2535 0.4082 0.327 0.103 Uiso calc U . R 1 . .
H H20B 0.3658 0.4198 0.4272 0.103 Uiso calc U . R 1 . .
C C21 0.3668(11) 0.5526(9) 0.3736(10) 0.100(4) Uani d . . . 1 . .
H H21A 0.3621 0.544 0.3021 0.12 Uiso calc U . R 1 . .
H H21B 0.4461 0.5802 0.4234 0.12 Uiso calc U . R 1 . .
C C22 0.3051(8) 0.6233(8) 0.3879(8) 0.075(3) Uani d . . . 1 . .
H H22A 0.2532 0.6301 0.3198 0.09 Uiso calc U . R 1 . .
H H22B 0.3579 0.6925 0.4272 0.09 Uiso calc U . R 1 . .
C C23 0.2412(8) 0.5734(8) 0.4486(9) 0.081(3) Uani d . . . 1 . .
H H23A 0.2681 0.6178 0.5176 0.097 Uiso calc U . R 1 . .
H H23B 0.1604 0.5613 0.4101 0.097 Uiso calc U . R 1 . .
C C24 -0.1138(13) 0.2247(16) 0.5768(13) 0.161(7) Uani d . . . 1 . .
H H24A -0.1252 0.2906 0.5613 0.193 Uiso calc U . R 1 . .
H H24B -0.164 0.1698 0.5144 0.193 Uiso calc U . R 1 . .
C C25 -0.1385(16) 0.2023(19) 0.6594(17) 0.208(11) Uani d . . . 1 . .
H H25A -0.2123 0.1487 0.6347 0.25 Uiso calc U . R 1 . .
H H25B -0.1395 0.2647 0.698 0.25 Uiso calc U . R 1 . .
C C26 -0.0510(15) 0.1653(12) 0.7264(14) 0.148(6) Uani d . . . 1 . .
H H26A -0.0792 0.0896 0.7184 0.178 Uiso calc U . R 1 . .
H H26B -0.0243 0.1976 0.8002 0.178 Uiso calc U . R 1 . .
C C27 0.0404(12) 0.1957(11) 0.6915(11) 0.117(4) Uani d . . . 1 . .
H H27A 0.1063 0.2497 0.7457 0.141 Uiso calc U . R 1 . .
H H27B 0.0627 0.1355 0.6775 0.141 Uiso calc U . R 1 . .
C C28 -0.0051(12) 0.2258(9) 0.2434(8) 0.107(4) Uani d . . . 1 . .
H H28A 0.0626 0.2395 0.2302 0.128 Uiso calc U . R 1 . .
H H28B -0.0301 0.2868 0.2358 0.128 Uiso calc U . R 1 . .
C C29 -0.0916(12) 0.1361(9) 0.1704(9) 0.130(6) Uani d . . . 1 . .
H H29A -0.1629 0.1503 0.1395 0.156 Uiso calc U . R 1 . .
H H29B -0.0715 0.1158 0.1139 0.156 Uiso calc U . R 1 . .
C C30 -0.1014(13) 0.0561(9) 0.2285(10) 0.129(5) Uani d . . . 1 . .
H H30A -0.0586 0.0111 0.2208 0.154 Uiso calc U . R 1 . .
H H30B -0.1803 0.0134 0.2053 0.154 Uiso calc U . R 1 . .
C C31 -0.0548(15) 0.1118(11) 0.3359(10) 0.167(8) Uani d . . . 1 . .
H H31A -0.1152 0.1206 0.3537 0.2 Uiso calc U . R 1 . .
H H31B -0.0161 0.0724 0.3838 0.2 Uiso calc U . R 1 . .
C C32 0.2936(17) 0.2058(15) 0.4978(14) 0.179(8) Uani d . . . 1 . .
H H32 0.2987 0.2346 0.4406 0.214 Uiso calc U . R 1 . .
C C33 0.3201(19) 0.1160(14) 0.5222(12) 0.183(9) Uani d . . . 1 . .
H H33A 0.2656 0.0546 0.4684 0.22 Uiso calc U . R 1 . .
H H33B 0.3956 0.1222 0.5277 0.22 Uiso calc U . R 1 . .
C C34 0.3150(15) 0.1094(10) 0.6166(10) 0.146(6) Uani d . . . 1 . .
H H34A 0.3813 0.0958 0.6657 0.175 Uiso calc U . R 1 . .
H H34B 0.2473 0.0538 0.6079 0.175 Uiso calc U . R 1 . .
C C35 0.3119(14) 0.2119(11) 0.6542(9) 0.138(6) Uani d . . . 1 . .
H H35A 0.2701 0.2053 0.698 0.165 Uiso calc U . R 1 . .
H H35B 0.3884 0.26 0.6959 0.165 Uiso calc U . R 1 . .
Cl Cl1 -0.06732(17) 0.53562(19) 0.84546(18) 0.0637(6) Uani d . . . 1 . .
Cl Cl2 0.37944(17) 0.78306(16) 1.21552(16) 0.0561(5) Uani d . . . 1 . .
Cl Cl3 0.56054(18) 0.87573(15) 1.09812(16) 0.0573(5) Uani d . . . 1 . .
Cl Cl4 0.7933(2) 0.9121(2) 0.7985(3) 0.0939(9) Uani d . . . 1 . .
Cl Cl5 0.39852(13) 0.49005(13) 0.77042(12) 0.0363(4) Uani d . . . 1 . .
Cl Cl6 0.4936(3) 0.9091(2) 0.6226(2) 0.0971(9) Uani d . . . 1 . .
Cl Cl7 0.06674(17) 0.54828(18) 0.63370(14) 0.0581(6) Uani d . . . 1 . .
K K1 0.11477(14) 0.35854(13) 0.51886(12) 0.0468(4) Uani d . . . 1 . .
O O1 0.2621(7) 0.4799(6) 0.4591(7) 0.099(2) Uani d . . . 1 . .
O O2 -0.0007(7) 0.2323(7) 0.6020(8) 0.122(3) Uani d . . . 1 . .
O O3 0.0187(6) 0.2062(5) 0.3462(5) 0.087(2) Uani d . . . 1 . .
O O4 0.2595(7) 0.2470(6) 0.5671(6) 0.107(3) Uani d . . . 1 . .
O O5 0.4443(4) 0.5038(3) 0.8881(3) 0.0336(10) Uani d . . . 1 . .
O O6 0.2726(3) 0.4554(3) 0.7269(3) 0.0360(11) Uani d . . . 1 . .
S S1 0.13087(14) 0.44805(14) 0.89066(13) 0.0373(4) Uani d . . . 1 . .
S S2 0.36683(13) 0.57338(13) 1.09688(12) 0.0332(4) Uani d . . . 1 . .
S S3 0.65012(13) 0.70057(13) 1.06094(13) 0.0323(4) Uani d . . . 1 . .
S S4 0.77576(17) 0.71784(16) 0.89848(17) 0.0509(5) Uani d . . . 1 . .
S S5 0.33690(14) 0.68979(13) 0.86651(13) 0.0346(4) Uani d . . . 1 . .
S S6 0.3693(2) 0.88338(16) 0.76517(17) 0.0573(6) Uani d . . . 1 . .
Zn Zn1 0.19286(6) 0.53193(6) 0.77831(6) 0.0352(2) Uani d . . . 1 . .
Zn Zn2 0.45734(6) 0.62236(6) 0.99052(6) 0.0314(2) Uani d . . . 1 . .
Zn Zn3 0.72528(6) 0.60096(6) 0.98839(6) 0.0346(2) Uani d . . . 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C6 . 1.392(9) ?
C1 C2 . 1.417(9) ?
C1 S1 . 1.773(7) ?
C2 C3 . 1.378(11) ?
C2 Cl1 . 1.716(8) ?
C3 C4 . 1.334(12) ?
C3 H3 . 0.95 ?
C4 C5 . 1.393(10) ?
C4 H4 . 0.95 ?
C5 C6 . 1.404(10) ?
C5 Cl2 . 1.733(8) ?
C6 S2 . 1.784(6) ?
C8 C9 . 1.401(10) ?
C8 C13 . 1.410(10) ?
C8 S3 . 1.774(7) ?
C9 C10 . 1.361(10) ?
C9 Cl3 . 1.739(8) ?
C10 C11 . 1.381(12) ?
C10 H10 . 0.95 ?
C11 C12 . 1.373(12) ?
C11 H11 . 0.95 ?
C12 C13 . 1.412(10) ?
C12 Cl4 . 1.742(8) ?
C13 S4 . 1.764(8) ?
C14 C19 . 1.396(9) ?
C14 C15 . 1.404(9) ?
C14 S5 . 1.778(7) ?
C15 C16 . 1.379(10) ?
C15 S6 . 1.710(7) ?
C16 C17 . 1.387(11) ?
C16 Cl6 . 1.732(8) ?
C17 C18 . 1.393(11) ?
C17 H17 . 0.95 ?
C18 C19 . 1.406(9) ?
C18 H18 . 0.95 ?
C19 Cl5 . 1.798(7) ?
C20 O1 . 1.425(11) ?
C20 C21 . 1.465(14) ?
C20 H20A . 0.99 ?
C20 H20B . 0.99 ?
C21 C22 . 1.504(14) ?
C21 H21A . 0.99 ?
C21 H21B . 0.99 ?
C22 C23 . 1.527(13) ?
C22 H22A . 0.99 ?
C22 H22B . 0.99 ?
C23 O1 . 1.403(11) ?
C23 K1 . 3.432(11) ?
C23 H23A . 0.99 ?
C23 H23B . 0.99 ?
C24 C25 . 1.376(19) ?
C24 O2 . 1.428(16) ?
C24 H24A . 0.99 ?
C24 H24B . 0.99 ?
C25 C26 . 1.47(2) ?
C25 H25A . 0.99 ?
C25 H25B . 0.99 ?
C26 C27 . 1.492(16) ?
C26 H26A . 0.99 ?
C26 H26B . 0.99 ?
C27 O2 . 1.380(14) ?
C27 H27A . 0.99 ?
C27 H27B . 0.99 ?
C28 O3 . 1.437(12) ?
C28 C29 . 1.441(15) ?
C28 H28A . 0.99 ?
C28 H28B . 0.99 ?
C29 C30 . 1.436(15) ?
C29 H29A . 0.99 ?
C29 H29B . 0.99 ?
C30 C31 . 1.463(16) ?
C30 H30A . 0.99 ?
C30 H30B . 0.99 ?
C31 O3 . 1.370(14) ?
C31 H31A . 0.99 ?
C31 H31B . 0.99 ?
C32 O4 . 1.388(15) ?
C32 C33 . 1.414(19) ?
C32 H32 . 0.95 ?
C33 C34 . 1.380(16) ?
C33 H33A . 0.99 ?
C33 H33B . 0.99 ?
C34 C35 . 1.490(16) ?
C34 H34A . 0.99 ?
C34 H34B . 0.99 ?
C35 O4 . 1.376(13) ?
C35 H35A . 0.99 ?
C35 H35B . 0.99 ?
Cl5 O6 . 1.514(4) ?
Cl5 O5 . 1.521(4) ?
Cl7 Zn1 . 2.2021(19) ?
Cl7 K1 2_566 3.261(2) ?
Cl7 K1 . 3.326(3) ?
K1 O2 . 2.682(7) ?
K1 O1 . 2.706(7) ?
K1 O3 . 2.721(6) ?
K1 O4 . 2.755(7) ?
K1 O6 . 2.856(5) ?
K1 Cl7 2_566 3.261(2) ?
K1 Zn1 . 3.8345(18) ?
O5 Zn2 . 2.025(4) ?
O6 Zn1 . 1.994(4) ?
S1 Zn1 . 2.3257(18) ?
S1 Zn3 2_667 2.3746(18) ?
S2 Zn2 . 2.3314(17) ?
S2 Zn3 2_667 2.3603(19) ?
S3 Zn3 . 2.3221(17) ?
S3 Zn2 . 2.3327(18) ?
S4 Zn3 . 2.259(2) ?
S5 Zn1 . 2.3589(19) ?
S5 Zn2 . 2.3623(18) ?
Zn3 S2 2_667 2.3603(19) ?
Zn3 S1 2_667 2.3746(18) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 C1 C2 . . 118.6(6) ?
C6 C1 S1 . . 122.7(5) ?
C2 C1 S1 . . 118.6(5) ?
C3 C2 C1 . . 120.6(7) ?
C3 C2 Cl1 . . 118.7(6) ?
C1 C2 Cl1 . . 120.7(6) ?
C4 C3 C2 . . 121.5(7) ?
C4 C3 H3 . . 119.2 ?
C2 C3 H3 . . 119.2 ?
C3 C4 C5 . . 119.1(7) ?
C3 C4 H4 . . 120.4 ?
C5 C4 H4 . . 120.4 ?
C4 C5 C6 . . 121.9(7) ?
C4 C5 Cl2 . . 117.2(6) ?
C6 C5 Cl2 . . 120.9(5) ?
C1 C6 C5 . . 118.2(6) ?
C1 C6 S2 . . 122.8(5) ?
C5 C6 S2 . . 118.9(5) ?
C9 C8 C13 . . 119.7(6) ?
C9 C8 S3 . . 118.4(6) ?
C13 C8 S3 . . 122.0(5) ?
C10 C9 C8 . . 122.7(7) ?
C10 C9 Cl3 . . 118.2(6) ?
C8 C9 Cl3 . . 119.2(5) ?
C9 C10 C11 . . 118.2(8) ?
C9 C10 H10 . . 120.9 ?
C11 C10 H10 . . 120.9 ?
C12 C11 C10 . . 120.9(8) ?
C12 C11 H11 . . 119.5 ?
C10 C11 H11 . . 119.5 ?
C11 C12 C13 . . 122.2(8) ?
C11 C12 Cl4 . . 118.1(6) ?
C13 C12 Cl4 . . 119.7(7) ?
C8 C13 C12 . . 116.3(7) ?
C8 C13 S4 . . 125.0(5) ?
C12 C13 S4 . . 118.7(6) ?
C19 C14 C15 . . 118.7(6) ?
C19 C14 S5 . . 122.1(5) ?
C15 C14 S5 . . 119.2(5) ?
C16 C15 C14 . . 120.2(7) ?
C16 C15 S6 . . 119.5(6) ?
C14 C15 S6 . . 120.2(5) ?
C15 C16 C17 . . 120.8(7) ?
C15 C16 Cl6 . . 120.3(6) ?
C17 C16 Cl6 . . 118.8(6) ?
C16 C17 C18 . . 119.9(7) ?
C16 C17 H17 . . 120.0 ?
C18 C17 H17 . . 120.0 ?
C17 C18 C19 . . 119.2(7) ?
C17 C18 H18 . . 120.4 ?
C19 C18 H18 . . 120.4 ?
C14 C19 C18 . . 120.7(6) ?
C14 C19 Cl5 . . 126.7(5) ?
C18 C19 Cl5 . . 112.5(5) ?
O1 C20 C21 . . 105.6(9) ?
O1 C20 H20A . . 110.6 ?
C21 C20 H20A . . 110.6 ?
O1 C20 H20B . . 110.6 ?
C21 C20 H20B . . 110.6 ?
H20A C20 H20B . . 108.8 ?
C20 C21 C22 . . 105.1(8) ?
C20 C21 H21A . . 110.7 ?
C22 C21 H21A . . 110.7 ?
C20 C21 H21B . . 110.7 ?
C22 C21 H21B . . 110.7 ?
H21A C21 H21B . . 108.8 ?
C21 C22 C23 . . 105.7(8) ?
C21 C22 H22A . . 110.6 ?
C23 C22 H22A . . 110.6 ?
C21 C22 H22B . . 110.6 ?
C23 C22 H22B . . 110.6 ?
H22A C22 H22B . . 108.7 ?
O1 C23 C22 . . 105.0(8) ?
O1 C23 K1 . . 48.1(4) ?
C22 C23 K1 . . 150.2(7) ?
O1 C23 H23A . . 110.8 ?
C22 C23 H23A . . 110.8 ?
K1 C23 H23A . . 93.4 ?
O1 C23 H23B . . 110.8 ?
C22 C23 H23B . . 110.8 ?
K1 C23 H23B . . 75.5 ?
H23A C23 H23B . . 108.8 ?
C25 C24 O2 . . 109.4(14) ?
C25 C24 H24A . . 109.8 ?
O2 C24 H24A . . 109.8 ?
C25 C24 H24B . . 109.8 ?
O2 C24 H24B . . 109.8 ?
H24A C24 H24B . . 108.2 ?
C24 C25 C26 . . 106.6(13) ?
C24 C25 H25A . . 110.4 ?
C26 C25 H25A . . 110.4 ?
C24 C25 H25B . . 110.4 ?
C26 C25 H25B . . 110.4 ?
H25A C25 H25B . . 108.6 ?
C25 C26 C27 . . 105.5(12) ?
C25 C26 H26A . . 110.6 ?
C27 C26 H26A . . 110.6 ?
C25 C26 H26B . . 110.6 ?
C27 C26 H26B . . 110.6 ?
H26A C26 H26B . . 108.8 ?
O2 C27 C26 . . 106.6(12) ?
O2 C27 H27A . . 110.4 ?
C26 C27 H27A . . 110.4 ?
O2 C27 H27B . . 110.4 ?
C26 C27 H27B . . 110.4 ?
H27A C27 H27B . . 108.6 ?
O3 C28 C29 . . 107.9(9) ?
O3 C28 H28A . . 110.1 ?
C29 C28 H28A . . 110.1 ?
O3 C28 H28B . . 110.1 ?
C29 C28 H28B . . 110.1 ?
H28A C28 H28B . . 108.4 ?
C30 C29 C28 . . 106.2(10) ?
C30 C29 H29A . . 110.5 ?
C28 C29 H29A . . 110.5 ?
C30 C29 H29B . . 110.5 ?
C28 C29 H29B . . 110.5 ?
H29A C29 H29B . . 108.7 ?
C29 C30 C31 . . 104.0(10) ?
C29 C30 H30A . . 111.0 ?
C31 C30 H30A . . 111.0 ?
C29 C30 H30B . . 111.0 ?
C31 C30 H30B . . 111.0 ?
H30A C30 H30B . . 109.0 ?
O3 C31 C30 . . 108.7(11) ?
O3 C31 H31A . . 109.9 ?
C30 C31 H31A . . 109.9 ?
O3 C31 H31B . . 109.9 ?
C30 C31 H31B . . 109.9 ?
H31A C31 H31B . . 108.3 ?
O4 C32 C33 . . 112.3(12) ?
O4 C32 H32 . . 123.9 ?
C33 C32 H32 . . 123.9 ?
C34 C33 C32 . . 104.6(12) ?
C34 C33 H33A . . 110.8 ?
C32 C33 H33A . . 110.8 ?
C34 C33 H33B . . 110.8 ?
C32 C33 H33B . . 110.8 ?
H33A C33 H33B . . 108.9 ?
C33 C34 C35 . . 104.5(11) ?
C33 C34 H34A . . 110.9 ?
C35 C34 H34A . . 110.9 ?
C33 C34 H34B . . 110.9 ?
C35 C34 H34B . . 110.9 ?
H34A C34 H34B . . 108.9 ?
O4 C35 C34 . . 106.3(10) ?
O4 C35 H35A . . 110.5 ?
C34 C35 H35A . . 110.5 ?
O4 C35 H35B . . 110.5 ?
C34 C35 H35B . . 110.5 ?
H35A C35 H35B . . 108.7 ?
O6 Cl5 O5 . . 108.2(3) ?
O6 Cl5 C19 . . 102.3(3) ?
O5 Cl5 C19 . . 105.0(3) ?
Zn1 Cl7 K1 . 2_566 158.62(10) ?
Zn1 Cl7 K1 . . 85.28(7) ?
K1 Cl7 K1 2_566 . 116.06(6) ?
O2 K1 O1 . . 170.1(3) ?
O2 K1 O3 . . 87.8(3) ?
O1 K1 O3 . . 95.4(2) ?
O2 K1 O4 . . 87.3(3) ?
O1 K1 O4 . . 84.3(3) ?
O3 K1 O4 . . 78.2(2) ?
O2 K1 O6 . . 86.8(2) ?
O1 K1 O6 . . 86.2(2) ?
O3 K1 O6 . . 153.52(19) ?
O4 K1 O6 . . 75.70(19) ?
O2 K1 Cl7 . 2_566 103.6(2) ?
O1 K1 Cl7 . 2_566 86.11(18) ?
O3 K1 Cl7 . 2_566 80.83(16) ?
O4 K1 Cl7 . 2_566 155.90(17) ?
O6 K1 Cl7 . 2_566 125.63(11) ?
O2 K1 Cl7 . . 86.7(2) ?
O1 K1 Cl7 . . 96.47(17) ?
O3 K1 Cl7 . . 141.78(17) ?
O4 K1 Cl7 . . 139.16(18) ?
O6 K1 Cl7 . . 63.66(10) ?
Cl7 K1 Cl7 2_566 . 63.94(6) ?
O2 K1 C23 . . 162.7(3) ?
O1 K1 C23 . . 22.7(2) ?
O3 K1 C23 . . 105.4(2) ?
O4 K1 C23 . . 106.2(3) ?
O6 K1 C23 . . 86.0(2) ?
Cl7 K1 C23 2_566 . 68.36(17) ?
Cl7 K1 C23 . . 76.03(18) ?
O2 K1 Zn1 . . 78.4(2) ?
O1 K1 Zn1 . . 98.88(18) ?
O3 K1 Zn1 . . 165.70(17) ?
O4 K1 Zn1 . . 104.44(17) ?
O6 K1 Zn1 . . 30.45(9) ?
Cl7 K1 Zn1 2_566 . 98.84(6) ?
Cl7 K1 Zn1 . . 34.91(4) ?
C23 K1 Zn1 . . 87.56(18) ?
C23 O1 C20 . . 112.0(8) ?
C23 O1 K1 . . 109.1(5) ?
C20 O1 K1 . . 130.7(6) ?
C27 O2 C24 . . 109.3(10) ?
C27 O2 K1 . . 127.9(8) ?
C24 O2 K1 . . 119.7(9) ?
C31 O3 C28 . . 107.0(8) ?
C31 O3 K1 . . 124.1(7) ?
C28 O3 K1 . . 123.1(6) ?
C35 O4 C32 . . 101.1(10) ?
C35 O4 K1 . . 134.1(7) ?
C32 O4 K1 . . 124.7(8) ?
Cl5 O5 Zn2 . . 127.5(2) ?
Cl5 O6 Zn1 . . 122.0(3) ?
Cl5 O6 K1 . . 128.1(2) ?
Zn1 O6 K1 . . 103.03(16) ?
C1 S1 Zn1 . . 94.7(2) ?
C1 S1 Zn3 . 2_667 98.1(2) ?
Zn1 S1 Zn3 . 2_667 110.13(7) ?
C6 S2 Zn2 . . 105.9(2) ?
C6 S2 Zn3 . 2_667 98.7(2) ?
Zn2 S2 Zn3 . 2_667 97.18(6) ?
C8 S3 Zn3 . . 99.0(2) ?
C8 S3 Zn2 . . 103.2(2) ?
Zn3 S3 Zn2 . . 108.93(7) ?
C13 S4 Zn3 . . 99.5(2) ?
C14 S5 Zn1 . . 97.3(2) ?
C14 S5 Zn2 . . 98.8(2) ?
Zn1 S5 Zn2 . . 96.75(7) ?
O6 Zn1 Cl7 . . 102.89(14) ?
O6 Zn1 S1 . . 110.54(14) ?
Cl7 Zn1 S1 . . 117.77(8) ?
O6 Zn1 S5 . . 100.64(13) ?
Cl7 Zn1 S5 . . 111.54(8) ?
S1 Zn1 S5 . . 111.69(7) ?
O6 Zn1 K1 . . 46.52(12) ?
Cl7 Zn1 K1 . . 59.81(6) ?
S1 Zn1 K1 . . 114.48(6) ?
S5 Zn1 K1 . . 130.50(5) ?
O5 Zn2 S2 . . 114.28(13) ?
O5 Zn2 S3 . . 98.16(13) ?
S2 Zn2 S3 . . 120.86(6) ?
O5 Zn2 S5 . . 96.07(12) ?
S2 Zn2 S5 . . 103.72(6) ?
S3 Zn2 S5 . . 121.09(7) ?
S4 Zn3 S3 . . 94.40(7) ?
S4 Zn3 S2 . 2_667 118.86(8) ?
S3 Zn3 S2 . 2_667 124.54(6) ?
S4 Zn3 S1 . 2_667 116.90(7) ?
S3 Zn3 S1 . 2_667 115.32(7) ?
S2 Zn3 S1 2_667 2_667 88.98(6) ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . 0.0(9) ?
S1 C1 C2 C3 . . . . -179.8(5) ?
C6 C1 C2 Cl1 . . . . -179.5(5) ?
S1 C1 C2 Cl1 . . . . 0.7(8) ?
C1 C2 C3 C4 . . . . 0.9(11) ?
Cl1 C2 C3 C4 . . . . -179.5(6) ?
C2 C3 C4 C5 . . . . -0.8(11) ?
C3 C4 C5 C6 . . . . -0.3(11) ?
C3 C4 C5 Cl2 . . . . 179.3(6) ?
C2 C1 C6 C5 . . . . -1.1(9) ?
S1 C1 C6 C5 . . . . 178.8(5) ?
C2 C1 C6 S2 . . . . 175.4(5) ?
S1 C1 C6 S2 . . . . -4.8(8) ?
C4 C5 C6 C1 . . . . 1.2(10) ?
Cl2 C5 C6 C1 . . . . -178.4(5) ?
C4 C5 C6 S2 . . . . -175.4(5) ?
Cl2 C5 C6 S2 . . . . 5.0(8) ?
C13 C8 C9 C10 . . . . 0.4(11) ?
S3 C8 C9 C10 . . . . 179.9(6) ?
C13 C8 C9 Cl3 . . . . 179.9(5) ?
S3 C8 C9 Cl3 . . . . -0.6(8) ?
C8 C9 C10 C11 . . . . -0.5(12) ?
Cl3 C9 C10 C11 . . . . 179.9(6) ?
C9 C10 C11 C12 . . . . -0.5(13) ?
C10 C11 C12 C13 . . . . 1.6(14) ?
C10 C11 C12 Cl4 . . . . 179.1(7) ?
C9 C8 C13 C12 . . . . 0.7(10) ?
S3 C8 C13 C12 . . . . -178.7(6) ?
C9 C8 C13 S4 . . . . 179.9(5) ?
S3 C8 C13 S4 . . . . 0.4(9) ?
C11 C12 C13 C8 . . . . -1.7(12) ?
Cl4 C12 C13 C8 . . . . -179.2(6) ?
C11 C12 C13 S4 . . . . 179.1(7) ?
Cl4 C12 C13 S4 . . . . 1.6(10) ?
C19 C14 C15 C16 . . . . -5.5(11) ?
S5 C14 C15 C16 . . . . 174.0(6) ?
C19 C14 C15 S6 . . . . 175.4(5) ?
S5 C14 C15 S6 . . . . -5.1(9) ?
C14 C15 C16 C17 . . . . -0.4(13) ?
S6 C15 C16 C17 . . . . 178.8(7) ?
C14 C15 C16 Cl6 . . . . 178.5(6) ?
S6 C15 C16 Cl6 . . . . -2.3(10) ?
C15 C16 C17 C18 . . . . 5.5(13) ?
Cl6 C16 C17 C18 . . . . -173.4(7) ?
C16 C17 C18 C19 . . . . -4.6(12) ?
C15 C14 C19 C18 . . . . 6.3(10) ?
S5 C14 C19 C18 . . . . -173.2(5) ?
C15 C14 C19 Cl5 . . . . -169.3(5) ?
S5 C14 C19 Cl5 . . . . 11.3(9) ?
C17 C18 C19 C14 . . . . -1.3(11) ?
C17 C18 C19 Cl5 . . . . 174.9(6) ?
O1 C20 C21 C22 . . . . -25.4(13) ?
C20 C21 C22 C23 . . . . 17.8(12) ?
C21 C22 C23 O1 . . . . -3.6(11) ?
C21 C22 C23 K1 . . . . -26.1(17) ?
O2 C24 C25 C26 . . . . -17.(3) ?
C24 C25 C26 C27 . . . . 15.(2) ?
C25 C26 C27 O2 . . . . -8.4(19) ?
O3 C28 C29 C30 . . . . -12.3(18) ?
C28 C29 C30 C31 . . . . 22.3(19) ?
C29 C30 C31 O3 . . . . -25.(2) ?
O4 C32 C33 C34 . . . . -7.(3) ?
C32 C33 C34 C35 . . . . -13.(2) ?
C33 C34 C35 O4 . . . . 30.(2) ?
C14 C19 Cl5 O6 . . . . 54.2(6) ?
C18 C19 Cl5 O6 . . . . -121.6(5) ?
C14 C19 Cl5 O5 . . . . -58.6(6) ?
C18 C19 Cl5 O5 . . . . 125.5(5) ?
C22 C23 O1 C20 . . . . -13.0(12) ?
K1 C23 O1 C20 . . . . 152.2(10) ?
C22 C23 O1 K1 . . . . -165.2(6) ?
C21 C20 O1 C23 . . . . 24.8(13) ?
C21 C20 O1 K1 . . . . 169.3(7) ?
C26 C27 O2 C24 . . . . -1.4(17) ?
C26 C27 O2 K1 . . . . 158.0(9) ?
C25 C24 O2 C27 . . . . 11.(2) ?
C25 C24 O2 K1 . . . . -149.8(15) ?
C30 C31 O3 C28 . . . . 18.0(18) ?
C30 C31 O3 K1 . . . . 171.7(10) ?
C29 C28 O3 C31 . . . . -3.6(17) ?
C29 C28 O3 K1 . . . . -157.6(9) ?
C34 C35 O4 C32 . . . . -33.0(17) ?
C34 C35 O4 K1 . . . . 143.7(10) ?
C33 C32 O4 C35 . . . . 26.(2) ?
C33 C32 O4 K1 . . . . -151.2(14) ?
O6 Cl5 O5 Zn2 . . . . -76.9(4) ?
C19 Cl5 O5 Zn2 . . . . 31.8(4) ?
O5 Cl5 O6 Zn1 . . . . 52.5(4) ?
C19 Cl5 O6 Zn1 . . . . -58.1(4) ?
O5 Cl5 O6 K1 . . . . -161.5(3) ?
C19 Cl5 O6 K1 . . . . 87.9(3) ?
C6 C1 S1 Zn1 . . . . -87.7(5) ?
C2 C1 S1 Zn1 . . . . 92.1(5) ?
C6 C1 S1 Zn3 . . . 2_667 23.4(5) ?
C2 C1 S1 Zn3 . . . 2_667 -156.8(5) ?
C1 C6 S2 Zn2 . . . . 83.0(5) ?
C5 C6 S2 Zn2 . . . . -100.6(5) ?
C1 C6 S2 Zn3 . . . 2_667 -17.1(5) ?
C5 C6 S2 Zn3 . . . 2_667 159.3(5) ?
C9 C8 S3 Zn3 . . . . 177.1(5) ?
C13 C8 S3 Zn3 . . . . -3.4(6) ?
C9 C8 S3 Zn2 . . . . 65.1(6) ?
C13 C8 S3 Zn2 . . . . -115.4(5) ?
C8 C13 S4 Zn3 . . . . 2.9(7) ?
C12 C13 S4 Zn3 . . . . -177.9(6) ?
C19 C14 S5 Zn1 . . . . -53.5(6) ?
C15 C14 S5 Zn1 . . . . 127.1(5) ?
C19 C14 S5 Zn2 . . . . 44.6(6) ?
C15 C14 S5 Zn2 . . . . -134.9(5) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C3 H3 S4 1_455 0.95 2.97 3.879(8) 161.3 ?
C10 H10 Cl3 2_677 0.95 2.96 3.796(8) 147.8 ?
C21 H21A S2 1_554 0.99 3.00 3.969(11) 166.2 ?
C22 H22A Cl1 2_566 0.99 2.95 3.632(11) 127.3 ?
C23 H23B Cl7 2_566 0.99 2.87 3.762(10) 150.6 ?
C34 H34A Cl2 2_667 0.99 2.97 3.735(18) 135.3 ?

####################################################################### 
# 
# 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_DH84_2_ZnFE
_database_code_depnum_ccdc_archive 'CCDC 1834783'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;

_audit_creation_date             2017-12-07T15:39:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C42 H50 Cl8 Fe2 N6 O6 S8 Zn'
_chemical_formula_sum            'C42 H50 Cl8 Fe2 N6 O6 S8 Zn'
_chemical_formula_weight         1452.03

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9680(12)
_cell_length_b                   13.4770(10)
_cell_length_c                   14.2440(9)
_cell_angle_alpha                108.073(6)
_cell_angle_beta                 109.857(7)
_cell_angle_gamma                93.674(8)
_cell_volume                     1679.9(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    57
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark blue'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             738
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 17 1 0.114
-1 -18 -1 0.08
-3 1 6 0.197
2 1 -4 0.238
7 -1 -4 0.286
1 -5 12 0.072
-7 1 4 0.276
-1 3 -7 0.111


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    1.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_T_max  1.076

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.09
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_number            34585
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.067
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_reflns_Friedel_coverage         0
_reflns_number_total             7636
_reflns_number_gt                5061
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (Macrae, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+3.8798P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7636
_refine_ls_number_parameters     337
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0548
_refine_ls_wR_factor_ref         0.1153
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.093

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C8 C 0.2487(5) 0.3627(3) 0.6879(3) 0.0330(10) Uani 1 1 d . . . . .
C7 C 0.3646(4) 0.3687(3) 0.7804(3) 0.0265(9) Uani 1 1 d . . . . .
C9 C 0.2696(5) 0.3459(3) 0.5932(3) 0.0395(11) Uani 1 1 d . . . . .
H9 H 0.190961 0.341616 0.530486 0.047 Uiso 1 1 calc R U . . .
C12 C 0.4997(4) 0.3524(3) 0.7763(3) 0.0277(9) Uani 1 1 d . . . . .
C1 C 0.5778(4) 0.3749(3) 1.2377(3) 0.0261(9) Uani 1 1 d . . . . .
C10 C 0.4043(6) 0.3356(3) 0.5906(3) 0.0417(12) Uani 1 1 d . . . . .
H10 H 0.41955 0.327245 0.526485 0.05 Uiso 1 1 calc R U . . .
C6 C 0.7162(4) 0.3642(3) 1.2369(3) 0.0276(9) Uani 1 1 d . . . . .
C2 C 0.5546(5) 0.3853(3) 1.3315(3) 0.0330(10) Uani 1 1 d . . . . .
C11 C 0.5173(5) 0.3370(3) 0.6794(3) 0.0326(10) Uani 1 1 d . . . . .
C5 C 0.8262(5) 0.3651(3) 1.3298(3) 0.0343(10) Uani 1 1 d . . . . .
C4 C 0.8014(5) 0.3777(4) 1.4222(3) 0.0445(12) Uani 1 1 d . . . . .
H4 H 0.877976 0.379216 1.484761 0.053 Uiso 1 1 calc R U . . .
C3 C 0.6657(6) 0.3881(4) 1.4232(3) 0.0462(12) Uani 1 1 d . . . . .
H3 H 0.648146 0.397201 1.486597 0.055 Uiso 1 1 calc R U . . .
C13 C 0.2366(6) -0.0081(4) 1.1909(4) 0.0472(12) Uani 1 1 d . . . . .
H13 H 0.207092 -0.081627 1.148717 0.057 Uiso 1 1 calc R U . . .
C14 C 0.4000(7) -0.0622(4) 1.3287(5) 0.077(2) Uani 1 1 d . . . . .
H14A H 0.369623 -0.131811 1.271295 0.116 Uiso 1 1 calc R U . . .
H14B H 0.364973 -0.065403 1.384426 0.116 Uiso 1 1 calc R U . . .
H14C H 0.506252 -0.042847 1.359212 0.116 Uiso 1 1 calc R U . . .
C15 C 0.3923(9) 0.1274(5) 1.3567(5) 0.103(3) Uani 1 1 d . . . . .
H15A H 0.34185 0.173957 1.321682 0.155 Uiso 1 1 calc R U . . .
H15B H 0.496876 0.145728 1.374425 0.155 Uiso 1 1 calc R U . . .
H15C H 0.374618 0.136702 1.422271 0.155 Uiso 1 1 calc R U . . .
C16 C 0.0478(5) 0.2364(3) 1.0588(4) 0.0381(10) Uani 1 1 d . . . . .
H16 H 0.068557 0.242333 1.130804 0.046 Uiso 1 1 calc R U . . .
C17 C 0.0820(6) 0.4291(4) 1.1171(5) 0.0580(15) Uani 1 1 d . . . . .
H17A H -0.004672 0.461478 1.105063 0.087 Uiso 1 1 calc R U . . .
H17B H 0.160091 0.473714 1.113272 0.087 Uiso 1 1 calc R U . . .
H17C H 0.113349 0.422902 1.187847 0.087 Uiso 1 1 calc R U . . .
C19 C -0.2485(6) -0.0314(4) 1.0661(4) 0.0466(12) Uani 1 1 d . . . . .
H19 H -0.252786 -0.103192 1.025512 0.056 Uiso 1 1 calc R U . . .
C20 C -0.4523(6) -0.0984(4) 1.0993(5) 0.0709(17) Uani 1 1 d . . . . .
H20A H -0.445728 -0.1653 1.049686 0.106 Uiso 1 1 calc R U . . .
H20B H -0.550088 -0.08325 1.072122 0.106 Uiso 1 1 calc R U . . .
H20C H -0.432539 -0.104563 1.169353 0.106 Uiso 1 1 calc R U . . .
C21 C -0.3473(7) 0.0949(4) 1.1725(5) 0.0669(16) Uani 1 1 d . . . . .
H21A H -0.278145 0.145485 1.166696 0.1 Uiso 1 1 calc R U . . .
H21B H -0.319625 0.10134 1.247376 0.1 Uiso 1 1 calc R U . . .
H21C H -0.445085 0.110275 1.146096 0.1 Uiso 1 1 calc R U . . .
O1 O 0.1749(4) 0.0540(2) 1.1511(3) 0.0510(9) Uani 1 1 d . . . . .
O2 O 0.0216(4) 0.1470(2) 0.9908(2) 0.0427(8) Uani 1 1 d . . . . .
O3 O -0.1520(4) 0.0364(2) 1.0741(3) 0.0518(9) Uani 1 1 d . . . . .
S1 S 0.44046(10) 0.37668(8) 1.12242(7) 0.0258(2) Uani 1 1 d . . . . .
S2 S 0.74566(11) 0.34955(8) 1.11937(7) 0.0282(2) Uani 1 1 d . . . . .
S3 S 0.34502(10) 0.40358(8) 0.90408(7) 0.0247(2) Uani 1 1 d . . . . .
S4 S 0.64171(11) 0.35318(8) 0.89064(7) 0.0276(2) Uani 1 1 d . . . . .
Cl1 Cl 0.38418(14) 0.39893(10) 1.33580(9) 0.0455(3) Uani 1 1 d . . . . .
Cl2 Cl 0.99860(13) 0.35059(11) 1.33028(9) 0.0532(3) Uani 1 1 d . . . . .
Cl3 Cl 0.07796(12) 0.37527(10) 0.69006(9) 0.0453(3) Uani 1 1 d . . . . .
Cl4 Cl 0.68569(14) 0.32147(9) 0.67135(9) 0.0465(3) Uani 1 1 d . . . . .
Fe1 Fe 0.55902(6) 0.40091(4) 1.02136(4) 0.02157(14) Uani 1 1 d . . . . .
Zn1 Zn 0 0 1 0.0428(2) Uani 1 2 d S . P . .
N1 N 0.3387(5) 0.0180(3) 1.2857(3) 0.0528(11) Uani 1 1 d . . . . .
N2 N 0.0482(4) 0.3241(3) 1.0360(3) 0.0373(9) Uani 1 1 d . . . . .
N3 N -0.3457(5) -0.0122(3) 1.1095(3) 0.0516(11) Uani 1 1 d . . . . .
C18 C 0.0142(6) 0.3178(4) 0.9271(4) 0.0554(14) Uani 1 1 d . . . . .
H18A H 0.012353 0.245167 0.883067 0.083 Uiso 1 1 calc R U . . .
H18B H 0.088223 0.367233 0.924592 0.083 Uiso 1 1 calc R U . . .
H18C H -0.081168 0.336627 0.899791 0.083 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C8 C9 1.385(6) . ?
C8 C7 1.402(5) . ?
C8 Cl3 1.731(5) . ?
C7 C12 1.396(6) . ?
C7 S3 1.758(4) . ?
C9 C10 1.370(7) . ?
C9 H9 0.95 . ?
C12 C11 1.404(5) . ?
C12 S4 1.754(4) . ?
C1 C2 1.399(5) . ?
C1 C6 1.400(6) . ?
C1 S1 1.753(4) . ?
C10 C11 1.373(6) . ?
C10 H10 0.95 . ?
C6 C5 1.398(5) . ?
C6 S2 1.750(4) . ?
C2 C3 1.384(6) . ?
C2 Cl1 1.739(4) . ?
C11 Cl4 1.742(5) . ?
C5 C4 1.382(6) . ?
C5 Cl2 1.740(4) . ?
C4 C3 1.374(7) . ?
C4 H4 0.95 . ?
C3 H3 0.95 . ?
C13 O1 1.234(5) . ?
C13 N1 1.308(6) . ?
C13 H13 0.95 . ?
C14 N1 1.469(6) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 N1 1.446(7) . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
C16 O2 1.233(5) . ?
C16 N2 1.320(5) . ?
C16 H16 0.95 . ?
C17 N2 1.454(6) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C19 O3 1.234(5) . ?
C19 N3 1.315(6) . ?
C19 H19 0.95 . ?
C20 N3 1.460(6) . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C21 N3 1.448(6) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
O1 Zn1 2.126(3) . ?
O2 Zn1 2.028(3) . ?
O3 Zn1 2.124(3) . ?
S1 Fe1 2.2301(11) . ?
S2 Fe1 2.2111(11) . ?
S3 Fe1 2.2291(11) . ?
S3 Fe1 2.4973(12) 2_667 ?
S4 Fe1 2.2198(11) . ?
N2 C18 1.443(6) . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?

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
C9 C8 C7 120.2(4) . . ?
C9 C8 Cl3 119.2(3) . . ?
C7 C8 Cl3 120.6(3) . . ?
C12 C7 C8 120.1(4) . . ?
C12 C7 S3 119.1(3) . . ?
C8 C7 S3 120.8(3) . . ?
C10 C9 C8 119.7(4) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C7 C12 C11 118.0(4) . . ?
C7 C12 S4 120.0(3) . . ?
C11 C12 S4 122.0(3) . . ?
C2 C1 C6 118.6(4) . . ?
C2 C1 S1 122.2(3) . . ?
C6 C1 S1 119.2(3) . . ?
C9 C10 C11 120.8(4) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C5 C6 C1 118.9(4) . . ?
C5 C6 S2 122.2(3) . . ?
C1 C6 S2 118.9(3) . . ?
C3 C2 C1 121.5(4) . . ?
C3 C2 Cl1 118.5(3) . . ?
C1 C2 Cl1 120.0(3) . . ?
C10 C11 C12 121.1(4) . . ?
C10 C11 Cl4 119.0(3) . . ?
C12 C11 Cl4 119.9(3) . . ?
C4 C5 C6 121.4(4) . . ?
C4 C5 Cl2 118.8(3) . . ?
C6 C5 Cl2 119.8(3) . . ?
C3 C4 C5 119.8(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
O1 C13 N1 126.0(5) . . ?
O1 C13 H13 117 . . ?
N1 C13 H13 117 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 C16 N2 122.8(4) . . ?
O2 C16 H16 118.6 . . ?
N2 C16 H16 118.6 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 C19 N3 125.1(4) . . ?
O3 C19 H19 117.5 . . ?
N3 C19 H19 117.5 . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C13 O1 Zn1 122.1(3) . . ?
C16 O2 Zn1 131.6(3) . . ?
C19 O3 Zn1 123.1(3) . . ?
C1 S1 Fe1 104.03(14) . . ?
C6 S2 Fe1 104.57(14) . . ?
C7 S3 Fe1 105.62(14) . . ?
C7 S3 Fe1 100.88(13) . 2_667 ?
Fe1 S3 Fe1 82.82(4) . 2_667 ?
C12 S4 Fe1 105.53(14) . . ?
S2 Fe1 S4 88.17(4) . . ?
S2 Fe1 S3 163.74(5) . . ?
S4 Fe1 S3 89.47(4) . . ?
S2 Fe1 S1 88.55(4) . . ?
S4 Fe1 S1 156.15(5) . . ?
S3 Fe1 S1 87.12(4) . . ?
S2 Fe1 S3 99.08(4) . 2_667 ?
S4 Fe1 S3 99.78(4) . 2_667 ?
S3 Fe1 S3 97.18(4) . 2_667 ?
S1 Fe1 S3 104.06(4) . 2_667 ?
O2 Zn1 O2 180 2_557 . ?
O2 Zn1 O3 88.95(13) 2_557 . ?
O2 Zn1 O3 91.05(13) . . ?
O2 Zn1 O3 91.05(13) 2_557 2_557 ?
O2 Zn1 O3 88.95(13) . 2_557 ?
O3 Zn1 O3 180.00(18) . 2_557 ?
O2 Zn1 O1 90.92(12) 2_557 2_557 ?
O2 Zn1 O1 89.08(12) . 2_557 ?
O3 Zn1 O1 88.98(14) . 2_557 ?
O3 Zn1 O1 91.02(14) 2_557 2_557 ?
O2 Zn1 O1 89.08(12) 2_557 . ?
O2 Zn1 O1 90.92(12) . . ?
O3 Zn1 O1 91.02(14) . . ?
O3 Zn1 O1 88.98(14) 2_557 . ?
O1 Zn1 O1 180.00(18) 2_557 . ?
C13 N1 C15 121.8(5) . . ?
C13 N1 C14 122.1(4) . . ?
C15 N1 C14 116.0(5) . . ?
C16 N2 C18 120.0(4) . . ?
C16 N2 C17 122.3(4) . . ?
C18 N2 C17 117.6(4) . . ?
C19 N3 C21 121.1(4) . . ?
C19 N3 C20 121.2(4) . . ?
C21 N3 C20 117.7(4) . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C8 C7 C12 -3.3(6) . . . . ?
Cl3 C8 C7 C12 176.3(3) . . . . ?
C9 C8 C7 S3 173.4(3) . . . . ?
Cl3 C8 C7 S3 -7.0(5) . . . . ?
C7 C8 C9 C10 -0.2(6) . . . . ?
Cl3 C8 C9 C10 -179.8(3) . . . . ?
C8 C7 C12 C11 4.1(6) . . . . ?
S3 C7 C12 C11 -172.6(3) . . . . ?
C8 C7 C12 S4 -176.7(3) . . . . ?
S3 C7 C12 S4 6.6(4) . . . . ?
C8 C9 C10 C11 2.8(6) . . . . ?
C2 C1 C6 C5 -0.5(6) . . . . ?
S1 C1 C6 C5 178.7(3) . . . . ?
C2 C1 C6 S2 179.2(3) . . . . ?
S1 C1 C6 S2 -1.6(4) . . . . ?
C6 C1 C2 C3 1.8(6) . . . . ?
S1 C1 C2 C3 -177.3(3) . . . . ?
C6 C1 C2 Cl1 179.9(3) . . . . ?
S1 C1 C2 Cl1 0.8(5) . . . . ?
C9 C10 C11 C12 -1.9(6) . . . . ?
C9 C10 C11 Cl4 179.0(3) . . . . ?
C7 C12 C11 C10 -1.5(6) . . . . ?
S4 C12 C11 C10 179.3(3) . . . . ?
C7 C12 C11 Cl4 177.5(3) . . . . ?
S4 C12 C11 Cl4 -1.7(5) . . . . ?
C1 C6 C5 C4 -0.9(6) . . . . ?
S2 C6 C5 C4 179.4(3) . . . . ?
C1 C6 C5 Cl2 179.4(3) . . . . ?
S2 C6 C5 Cl2 -0.4(5) . . . . ?
C6 C5 C4 C3 1.0(7) . . . . ?
Cl2 C5 C4 C3 -179.3(4) . . . . ?
C5 C4 C3 C2 0.3(7) . . . . ?
C1 C2 C3 C4 -1.8(7) . . . . ?
Cl1 C2 C3 C4 -179.9(4) . . . . ?
N1 C13 O1 Zn1 -175.7(4) . . . . ?
N2 C16 O2 Zn1 -175.3(3) . . . . ?
N3 C19 O3 Zn1 -179.1(4) . . . . ?
C2 C1 S1 Fe1 165.3(3) . . . . ?
C6 C1 S1 Fe1 -13.8(3) . . . . ?
C5 C6 S2 Fe1 -163.9(3) . . . . ?
C1 C6 S2 Fe1 16.3(3) . . . . ?
C12 C7 S3 Fe1 -3.3(3) . . . . ?
C8 C7 S3 Fe1 180.0(3) . . . . ?
C12 C7 S3 Fe1 82.2(3) . . . 2_667 ?
C8 C7 S3 Fe1 -94.5(3) . . . 2_667 ?
C7 C12 S4 Fe1 -6.2(3) . . . . ?
C11 C12 S4 Fe1 172.9(3) . . . . ?
O1 C13 N1 C15 -0.1(9) . . . . ?
O1 C13 N1 C14 176.4(5) . . . . ?
O2 C16 N2 C18 1.3(7) . . . . ?
O2 C16 N2 C17 -178.8(4) . . . . ?
O3 C19 N3 C21 0.1(8) . . . . ?
O3 C19 N3 C20 -177.4(5) . . . . ?






# END of CIF
_refine_special_details          SQUEEZE
