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

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

data_1a
_database_code_depnum_ccdc_archive 'CCDC 1833568'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT043_ALERT_1a            
;
 PROBLEM: Calculated and Reported Mol. Weight Differ by 12.08 
 RESPONSE: The hydrogens of water and THF molecules are missing: they 
 were not placed in calculated position or located in the difference 
 Fourier map
;
_vrf_PLAT430_ALERT_1a            
;
 PROBLEM: Short Inter D...A Contact
 RESPONSE: this alert is due to water molecules (O1w and O2w) that are 
 disordered over two positions related by symmetry 
;
_vrf_PLAT241_ALERT_1a            
;
 PROBLEM: The U(eq) value of an atom is compared with the average U(eq) 
 for to non-hydrogen atoms bonded to it.
 RESPONSE:O1 and O2 atoms are bonded to a disordered S-O3-CF3 models, that
 has been treated by using two models of different weights (one isotropic 
 and one anisotropic). The U(eq) values of the considered atoms 
 cannot be compared.
;
# end Validation Reply Form

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

_chemical_formula_sum            'C26 H28 Cu F6 N4 O9 S2'
_chemical_formula_moiety         'C22 H16 Cu F6 N4 O6 S2, C4 H8 O, 2(H2 O)'
_chemical_formula_weight         782.19

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

_space_group_name_Hall           '-I 4bd 2c'
_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 41/acd'
_symmetry_Int_Tables_number      142
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   28.576(2)
_cell_length_b                   28.576(2)
_cell_length_c                   17.9860(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14687.1(17)
_cell_formula_units_Z            16
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9632
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      23.2

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

_exptl_crystal_description       'polyhedral block'
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6384
_exptl_special_details           
;
 1440 frames were collected on a Bruker APEX CCD diffractometer with a 
 sample to detector distance of 60.00 mm. The counting time per frame 
 was 30 sec and the scan width per frame 0.5 deg. 
;
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'

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

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD_plate
_diffrn_measurement_device       'Bruker smart apex ccd diffractometer'
_diffrn_measurement_method       omega-scan
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_number            64915
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         24.83
_diffrn_reflns_theta_full        24.83
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             3174
_reflns_number_gt                2871
_reflns_threshold_expression     >2sigma(I)

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

_computing_structure_solution    
'SIR 2014: C. Giacovazzo et all., J. Appl. Cryst.(2015) 48, 306'
_computing_structure_refinement  
'SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122'
_computing_molecular_graphics    
'VESTA 3: K. Momma and F. Izumi, J. Appl. Crystallogr.(2011),44,127'
_computing_publication_material  
'WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1318P)²+96.3987P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3174
_refine_ls_number_parameters     235
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0716
_refine_ls_wR_factor_ref         0.2233
_refine_ls_wR_factor_gt          0.2183
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.165

#----------------------------------------------------------------------------#
#                   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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1N O 0.1938(10) 0.0562(10) 0.125 0.340(16) Uiso 1 2 d SD . .
C2N C 0.2353(14) 0.0771(17) 0.162(3) 0.212(18) Uiso 0.5 1 d PD . .
C3N C 0.236(3) 0.051(3) 0.229(4) 0.39(5) Uiso 0.5 1 d PD . .
C4N C 0.1999(19) 0.0170(19) 0.221(3) 0.24(2) Uiso 0.5 1 d PD . .
C5N C 0.1899(15) 0.0063(12) 0.146(3) 0.178(14) Uiso 0.5 1 d PD . .
O2W O 0.3164(9) 0.1064(9) 0.3316(14) 0.192(9) Uiso 0.5 1 d P . .
O1W O 0.9592(12) 0.7713(14) 0.126(2) 0.248(14) Uiso 0.5 1 d P . .
Cu Cu 0.75 0.25963(2) 0 0.0203(3) Uani 1 2 d S . .
N1 N 0.70869(13) 0.30864(12) 0.0460(2) 0.0223(8) Uani 1 1 d . . .
C11 C 0.69744(18) 0.30569(17) 0.1186(3) 0.0323(11) Uani 1 1 d . . .
H11 H 0.7123 0.2827 0.1485 0.039 Uiso 1 1 calc R . .
C12 C 0.66505(19) 0.33506(18) 0.1507(3) 0.0364(12) Uani 1 1 d . . .
H12 H 0.6575 0.3318 0.2019 0.044 Uiso 1 1 calc R . .
C13 C 0.64338(16) 0.36930(16) 0.1086(3) 0.0266(10) Uani 1 1 d . . .
C14 C 0.65544(17) 0.37245(16) 0.0342(3) 0.0299(10) Uani 1 1 d . . .
H14 H 0.6414 0.3955 0.0034 0.036 Uiso 1 1 calc R . .
C15 C 0.68805(16) 0.34188(16) 0.0053(2) 0.0264(10) Uani 1 1 d . . .
H15 H 0.6962 0.3446 -0.0457 0.032 Uiso 1 1 calc R . .
N2 N 0.79122(12) 0.20935(12) -0.0451(2) 0.0239(8) Uani 1 1 d . . .
C21 C 0.83571(18) 0.2056(2) -0.0246(3) 0.0438(14) Uani 1 1 d . . .
H21 H 0.8474 0.2264 0.0122 0.053 Uiso 1 1 calc R . .
C22 C 0.86550(18) 0.1730(2) -0.0544(3) 0.0476(15) Uani 1 1 d . . .
H22 H 0.8972 0.1716 -0.0384 0.057 Uiso 1 1 calc R . .
C23 C 0.60806(16) 0.40070(16) 0.1422(3) 0.0281(10) Uani 1 1 d . . .
C24 C 0.60291(18) 0.44646(17) 0.1192(3) 0.0367(12) Uani 1 1 d . . .
H24 H 0.6224 0.4588 0.0812 0.044 Uiso 1 1 calc R . .
C25 C 0.77583(17) 0.18080(17) -0.0980(3) 0.0352(11) Uani 1 1 d . . .
H25 H 0.7443 0.1837 -0.114 0.042 Uiso 1 1 calc R . .
O1 O 0.80014(12) 0.25927(12) 0.11066(18) 0.0325(8) Uani 1 1 d . . .
O2 O 0.8068(3) 0.2563(3) 0.2452(3) 0.120(3) Uani 1 1 d . . .
S1A S 0.81917(7) 0.27748(8) 0.17845(9) 0.0422(7) Uani 0.788(7) 1 d P A 1
O3A O 0.8160(2) 0.32763(19) 0.1817(3) 0.0591(17) Uani 0.788(7) 1 d P A 1
C1T C 0.8816(4) 0.2649(3) 0.1683(5) 0.098(6) Uani 0.788(7) 1 d PD A 1
F1A F 0.8870(3) 0.2181(3) 0.1727(5) 0.118(3) Uani 0.788(7) 1 d PDU A 1
F2A F 0.9072(3) 0.2845(3) 0.2218(4) 0.117(3) Uani 0.788(7) 1 d PDU A 1
F3A F 0.8989(2) 0.2791(3) 0.1038(4) 0.099(2) Uani 0.788(7) 1 d PDU A 1
S1B S 0.8272(5) 0.2508(6) 0.1759(7) 0.088(4) Uiso 0.212(7) 1 d PD A 2
O3B O 0.8421(9) 0.2024(9) 0.1727(13) 0.070(7) Uiso 0.212(7) 1 d P A 2
C2T C 0.8806(11) 0.2778(12) 0.177(2) 0.14(4) Uiso 0.212(7) 1 d PD A 2
F1B F 0.8762(15) 0.3252(15) 0.150(2) 0.159(10) Uiso 0.212(7) 1 d PD A 2
F2B F 0.8815(18) 0.2790(16) 0.259(2) 0.159(10) Uiso 0.212(7) 1 d PD A 2
F3B F 0.8992(18) 0.2413(18) 0.130(3) 0.159(10) Uiso 0.212(7) 1 d PD A 2



#----------------------------------------------------------------------------#
#                   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
O1N C5N 1.48(3) . ?
O1N C5N 1.48(3) 8 ?
O1N C2N 1.48(3) 8 ?
O1N C2N 1.48(3) . ?
C2N C5N 1.18(5) 8 ?
C2N C3N 1.42(4) . ?
C3N C4N 1.42(4) . ?
C4N C5N 1.41(4) . ?
C4N C4N 1.42(9) 6 ?
C5N C2N 1.18(5) 8 ?
Cu N1 2.010(3) . ?
Cu N1 2.010(3) 5_655 ?
Cu N2 2.027(3) 5_655 ?
Cu N2 2.027(3) . ?
N1 C15 1.337(6) . ?
N1 C11 1.347(6) . ?
C11 C12 1.376(7) . ?
C12 C13 1.384(7) . ?
C13 C14 1.384(7) . ?
C13 C23 1.480(6) . ?
C14 C15 1.379(6) . ?
N2 C21 1.328(6) . ?
N2 C25 1.328(6) . ?
C21 C22 1.371(7) . ?
C22 C23 1.387(7) 31_665 ?
C23 C24 1.379(7) . ?
C23 C22 1.387(7) 23_676 ?
C24 C25 1.379(7) 23_676 ?
C25 C24 1.379(7) 31_665 ?
O1 S1B 1.427(14) . ?
O1 S1A 1.433(4) . ?
O2 S1B 1.386(14) . ?
O2 S1A 1.391(6) . ?
S1A O3A 1.437(6) . ?
S1A C1T 1.827(13) . ?
C1T F3A 1.325(8) . ?
C1T F2A 1.333(7) . ?
C1T F1A 1.350(8) . ?
S1B O3B 1.45(3) . ?
S1B C2T 1.71(2) . ?
C2T F1B 1.44(3) . ?
C2T F3B 1.45(3) . ?
C2T F2B 1.46(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
C5N O1N C5N 102(4) . 8 ?
C5N O1N C2N 47(2) . 8 ?
C5N O1N C2N 109(4) 8 8 ?
C5N O1N C2N 109(4) . . ?
C5N O1N C2N 47(2) 8 . ?
C2N O1N C2N 147(5) 8 . ?
C5N C2N C3N 122(6) 8 . ?
C5N C2N O1N 66.6(14) 8 . ?
C3N C2N O1N 100(4) . . ?
C2N C3N C4N 105(6) . . ?
C5N C4N C4N 123(6) . 6 ?
C5N C4N C3N 113(5) . . ?
C4N C4N C3N 113(5) 6 . ?
C2N C5N C4N 152(4) 8 . ?
C2N C5N O1N 66.7(14) 8 . ?
C4N C5N O1N 91(3) . . ?
N1 Cu N1 91.7(2) . 5_655 ?
N1 Cu N2 89.29(14) . 5_655 ?
N1 Cu N2 178.97(14) 5_655 5_655 ?
N1 Cu N2 178.97(14) . . ?
N1 Cu N2 89.29(14) 5_655 . ?
N2 Cu N2 89.7(2) 5_655 . ?
C15 N1 C11 118.1(4) . . ?
C15 N1 Cu 121.9(3) . . ?
C11 N1 Cu 119.7(3) . . ?
N1 C11 C12 121.9(4) . . ?
C11 C12 C13 120.2(4) . . ?
C12 C13 C14 117.6(4) . . ?
C12 C13 C23 120.7(4) . . ?
C14 C13 C23 121.7(4) . . ?
C15 C14 C13 119.4(4) . . ?
N1 C15 C14 122.8(4) . . ?
C21 N2 C25 117.8(4) . . ?
C21 N2 Cu 120.2(3) . . ?
C25 N2 Cu 122.0(3) . . ?
N2 C21 C22 122.8(5) . . ?
C21 C22 C23 119.8(5) . 31_665 ?
C24 C23 C22 117.1(4) . 23_676 ?
C24 C23 C13 121.7(4) . . ?
C22 C23 C13 121.1(4) 23_676 . ?
C23 C24 C25 119.4(5) . 23_676 ?
N2 C25 C24 123.0(4) . 31_665 ?
S1B O1 S1A 32.4(7) . . ?
S1B O2 S1A 33.4(7) . . ?
O2 S1A O1 118.7(4) . . ?
O2 S1A O3A 112.5(4) . . ?
O1 S1A O3A 111.9(3) . . ?
O2 S1A C1T 104.4(5) . . ?
O1 S1A C1T 102.4(3) . . ?
O3A S1A C1T 105.1(4) . . ?
F3A C1T F2A 107.3(8) . . ?
F3A C1T F1A 108.1(9) . . ?
F2A C1T F1A 108.1(7) . . ?
F3A C1T S1A 113.1(6) . . ?
F2A C1T S1A 112.5(8) . . ?
F1A C1T S1A 107.6(7) . . ?
O2 S1B O1 119.4(11) . . ?
O2 S1B O3B 105.4(14) . . ?
O1 S1B O3B 106.7(14) . . ?
O2 S1B C2T 108.2(16) . . ?
O1 S1B C2T 114.9(16) . . ?
O3B S1B C2T 99.9(19) . . ?
F1B C2T F3B 120(3) . . ?
F1B C2T F2B 109(3) . . ?
F3B C2T F2B 127(4) . . ?
F1B C2T S1B 110(3) . . ?
F3B C2T S1B 90(3) . . ?
F2B C2T S1B 92(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_1c
_database_code_depnum_ccdc_archive 'CCDC 1833570'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_1c                  
;
 PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
 RESPONSE:It is due to poor x-ray refinement data: measurement 
 has been carried out at 293K on a in situ totally deydrated crystal 
 that has lost crystallinity but maintains his single crystal nature.
 The structure is essential to track the dehydration behavior of the system.
;
_vrf_GOODF01_1c                  
;
 PROBLEM: The least squares goodness of fit parameter lies
 RESPONSE: see answer for THETM01
;
_vrf_PLAT084_1c                  
;
 PROBLEM: High wR2 Value (i.e. > 0.25)       0.53 Report
 RESPONSE: RESPONSE: see answer for THETM01
;
_vrf_PLAT201_1c                  
;
 PROBLEM: Isotropic non-H Atoms in Main Residue(s)    12 Report
 RESPONSE: see answer for THETM01
;
_vrf_PLAT087_1c                  
;
 PROBLEM: Unsatisfactory S value (Too High)  2.19 Check 
 RESPONSE: see answer for THETM01
;
_vrf_PLAT220_1c                  
;
 PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range   3.6 Ratio 
 RESPONSE: see answer for THETM01
;
_vrf_PLAT222_1c                  
;
 PROBLEM: Non-Solvent Resd 1   H Uiso(max)/Uiso(min) Range   5.4 Ratio 
 RESPONSE: see answer for THETM01
;
_vrf_PLAT242_1c                  
;
 PROBLEM: Low     MainMol  Ueq as Compared to Neighbors of   S1 Check 
 RESPONSE: RESPONSE: see answer for THETM01
;
_vrf_PLAT341_1c                  
;
 PROBLEM: Low Bond Precision on  C-C Bonds .   0.012 Ang.  
 RESPONSE: see answer for THETM01
;
# end Validation Reply Form

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

_chemical_formula_sum            'C22 H16 Cu F6 N4 O6 S2'
_chemical_formula_moiety         'C22 H16 Cu F6 N4 O6 S2'
_chemical_formula_weight         674.05

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

_space_group_name_Hall           '-I 4bd 2c'
_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 41/acd'
_symmetry_Int_Tables_number      142
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'y+3/4, x+1/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'y+5/4, x+3/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z-1/2'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-y-3/4, -x-1/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
'-y-1/4, -x+1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'

_cell_length_a                   28.280(7)
_cell_length_b                   28.280
_cell_length_c                   19.059(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15243(5)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6313
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      26.3

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

_exptl_crystal_description       'polyhedral block'
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5424
_exptl_special_details           
;
 1440 frames were collected on a Brucker APEX CCD diffractometer with a 
 sample to detector distance of 50.00 mm. The counting time per frame 
 was 30 sec and the scan width per frame 0.5 deg. 
;

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

_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD_plate
_diffrn_measurement_device       'Bruker smart apex ccd diffractometer'
_diffrn_measurement_method       omega-scan
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_number            43955
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         19.99
_diffrn_reflns_theta_full        19.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             1784
_reflns_number_gt                1276
_reflns_threshold_expression     >2sigma(I)

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

_computing_structure_solution    
'SIR 2014: C. Giacovazzo et all., J. Appl. Cryst.(2015) 48, 306'
_computing_structure_refinement  
'SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122'
_computing_molecular_graphics    
'VESTA 3: K. Momma and F. Izumi, J. Appl. Crystallogr.(2011),44,127'
_computing_publication_material  
'WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1784
_refine_ls_number_parameters     93
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.1937
_refine_ls_R_factor_gt           0.1712
_refine_ls_wR_factor_ref         0.5337
_refine_ls_wR_factor_gt          0.5198
_refine_ls_goodness_of_fit_ref   2.194
_refine_ls_restrained_S_all      2.185
_refine_ls_shift/su_max          0.111
_refine_ls_shift/su_mean         0.022
_refine_diff_density_max         0.739
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.149
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.250 0.366 413 233 ' '
2 0.000 0.750 0.104 413 233 ' '
3 0.073 0.000 0.750 11 3 ' '
4 0.073 0.500 0.250 11 3 ' '
5 0.250 0.000 0.256 692 315 ' '
6 0.250 0.500 0.744 692 315 ' '
7 0.250 0.177 0.500 11 4 ' '
8 0.250 0.323 0.000 11 3 ' '
9 0.250 0.677 0.500 11 4 ' '
10 0.250 0.823 0.000 11 3 ' '
11 0.427 0.000 0.250 11 3 ' '
12 0.427 0.500 0.750 11 4 ' '
13 0.500 0.250 0.147 413 233 ' '
14 0.500 0.750 0.381 413 233 ' '
15 0.573 0.000 0.750 11 3 ' '
16 0.573 0.500 0.250 11 3 ' '
17 0.750 0.000 0.244 692 315 ' '
18 0.750 0.500 0.756 692 315 ' '
19 0.750 0.177 0.000 11 4 ' '
20 0.750 0.323 0.500 11 3 ' '
21 0.750 0.677 0.000 11 4 ' '
22 0.750 0.823 0.500 11 3 ' '
23 0.927 0.000 0.250 11 4 ' '
24 0.927 0.500 0.750 11 3 ' '
_platon_squeeze_details          
;
 Attempts to refine peaks of residual electron density as guest
 atoms were unsuccessful. The data were corrected for disordered
 electron density through use of the SQUEEZE procedure (Sluis, P. van der;
 Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON
 (Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13)
 A total solvent-accessible surface of 1983,21 A³ (13,0%) and a 
 contact surface of 5292,87 A³ (34.7%)
;

#----------------------------------------------------------------------------#
#                   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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.75 0.25 0.75 0.0635(18) Uani 1 2 d S . .
N1 N 0.7102(3) 0.3011(3) 0.7016(4) 0.040(3) Uiso 1 1 d GD . .
C11 C 0.7287(2) 0.3365(4) 0.6589(8) 0.057(7) Uiso 0.5 1 d PG A 1
H11 H 0.7612 0.3386 0.6521 0.069 Uiso 0.5 1 calc PR A 1
C12 C 0.6986(4) 0.3686(4) 0.6264(7) 0.086(9) Uiso 0.5 1 d PG A 1
H12 H 0.711 0.3922 0.5978 0.104 Uiso 0.5 1 calc PR A 1
C13 C 0.6500(3) 0.3653(3) 0.6365(6) 0.061(4) Uiso 1 1 d GD A .
C14 C 0.6316(2) 0.3300(5) 0.6792(9) 0.20(2) Uiso 0.5 1 d PG A 1
H14 H 0.5991 0.3279 0.686 0.244 Uiso 0.5 1 calc PR A 1
C15 C 0.6616(3) 0.2979(5) 0.7117(8) 0.095(11) Uiso 0.5 1 d PG A 1
H15 H 0.6493 0.2743 0.7403 0.115 Uiso 0.5 1 calc PR A 1
C31 C 0.6948(6) 0.3373(6) 0.7425(11) 0.047(7) Uiso 0.5 1 d PD A 2
H31 H 0.7037 0.3402 0.7893 0.057 Uiso 0.5 1 calc PR A 2
C32 C 0.6637(7) 0.3707(9) 0.7092(11) 0.088(10) Uiso 0.5 1 d PD A 2
H32 H 0.6523 0.3963 0.7348 0.105 Uiso 0.5 1 calc PR A 2
C34 C 0.6677(6) 0.3261(5) 0.5978(11) 0.038(6) Uiso 0.5 1 d PD A 2
H34 H 0.6591 0.3213 0.5512 0.045 Uiso 0.5 1 calc PR A 2
C35 C 0.6991(7) 0.2944(8) 0.6331(10) 0.080(9) Uiso 0.5 1 d PD A 2
H35 H 0.7119 0.2689 0.6089 0.096 Uiso 0.5 1 calc PR A 2
N2 N 0.7934(3) 0.2991(3) 0.7913(4) 0.048(3) Uiso 1 1 d GD . .
C21 C 0.8166(5) 0.3331(4) 0.7516(3) 0.089(10) Uiso 0.5 1 d PG A 1
H21 H 0.8127 0.3339 0.7031 0.107 Uiso 0.5 1 calc PR A 1
C22 C 0.8457(5) 0.3660(4) 0.7842(4) 0.066(8) Uiso 0.5 1 d PG A 1
H22 H 0.8613 0.3888 0.7576 0.08 Uiso 0.5 1 calc PR A 1
C23 C 0.8517(3) 0.3649(3) 0.8566(5) 0.031(3) Uiso 1 1 d GD A .
C24 C 0.8284(5) 0.3308(4) 0.8963(3) 0.089(10) Uiso 0.5 1 d PG A 1
H24 H 0.8324 0.3301 0.9447 0.106 Uiso 0.5 1 calc PR A 1
C25 C 0.7993(4) 0.2979(4) 0.8637(4) 0.063(8) Uiso 0.5 1 d PG A 1
H25 H 0.7838 0.2751 0.8902 0.076 Uiso 0.5 1 calc PR A 1
C42 C 0.8679(8) 0.3300(6) 0.8095(8) 0.061(7) Uiso 0.5 1 d PD A 2
H42 H 0.9001 0.3293 0.8001 0.073 Uiso 0.5 1 calc PR A 2
C41 C 0.8392(6) 0.2958(8) 0.7752(11) 0.075(9) Uiso 0.5 1 d PD A 2
H41 H 0.8512 0.2733 0.7445 0.09 Uiso 0.5 1 calc PR A 2
C45 C 0.7725(9) 0.3305(7) 0.8354(9) 0.085(9) Uiso 0.5 1 d PD A 2
H45 H 0.7401 0.3299 0.8433 0.101 Uiso 0.5 1 calc PR A 2
C44 C 0.8020(6) 0.3647(7) 0.8694(10) 0.065(8) Uiso 0.5 1 d PD A 2
H44 H 0.7888 0.3867 0.8998 0.078 Uiso 0.5 1 calc PR A 2
S1 S 0.8390(3) 0.2600(3) 0.6003(5) 0.175(4) Uiso 1 1 d D A .
O1 O 0.7997(3) 0.2496(3) 0.6488(5) 0.066(3) Uiso 1 1 d D . .
O3 O 0.8878(6) 0.2448(5) 0.6221(11) 0.179(8) Uiso 1 1 d D . .
O2 O 0.8360(6) 0.3057(7) 0.5608(12) 0.237(10) Uiso 1 1 d D . .
C1T C 0.8417(7) 0.2177(7) 0.5376(11) 0.38(3) Uiso 1 1 d D . .
F3 F 0.8446(9) 0.1715(8) 0.5590(14) 0.316(8) Uiso 1 1 d D A .
F2 F 0.8788(9) 0.2201(9) 0.4914(12) 0.316(8) Uiso 1 1 d D A .
F1 F 0.8029(9) 0.2162(9) 0.4936(11) 0.316(8) Uiso 1 1 d D A .



#----------------------------------------------------------------------------#
#                   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
Cu1 N2 2.013(7) 25_656 ?
Cu1 N2 2.013(7) . ?
Cu1 N1 2.052(7) 25_656 ?
Cu1 N1 2.052(7) . ?
Cu1 O1 2.386(9) . ?
Cu1 O1 2.386(9) 25_656 ?
N1 C35 1.355(17) . ?
N1 C31 1.358(16) . ?
N1 C11 1.39 . ?
N1 C15 1.39 . ?
C11 C12 1.39 . ?
C12 C13 1.39 . ?
C13 C14 1.39 . ?
C13 C34 1.423(16) . ?
C13 C32 1.446(17) . ?
C13 C23 1.48(3) 7_564 ?
C14 C15 1.39 . ?
C31 C32 1.438(18) . ?
C34 C35 1.430(18) . ?
N2 C41 1.334(16) . ?
N2 C45 1.359(16) . ?
N2 C21 1.39 . ?
N2 C25 1.39 . ?
C21 C22 1.39 . ?
C22 C23 1.39 . ?
C23 C42 1.411(15) . ?
C23 C24 1.39 . ?
C23 C44 1.424(15) . ?
C23 C13 1.48(3) 8_645 ?
C24 C25 1.39 . ?
C42 C41 1.420(17) . ?
C45 C44 1.431(18) . ?
S1 O1 1.476(11) . ?
S1 O2 1.498(15) . ?
S1 O3 1.505(15) . ?
S1 C1T 1.69(2) . ?
C1T F3 1.37(2) . ?
C1T F2 1.37(2) . ?
C1T F1 1.38(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
N2 Cu1 N2 180.0(4) 25_656 . ?
N2 Cu1 N1 91.4(4) 25_656 25_656 ?
N2 Cu1 N1 88.6(4) . 25_656 ?
N2 Cu1 N1 88.6(4) 25_656 . ?
N2 Cu1 N1 91.4(4) . . ?
N1 Cu1 N1 180.0(4) 25_656 . ?
N2 Cu1 O1 92.3(3) 25_656 . ?
N2 Cu1 O1 87.7(3) . . ?
N1 Cu1 O1 92.1(3) 25_656 . ?
N1 Cu1 O1 87.9(3) . . ?
N2 Cu1 O1 87.7(3) 25_656 25_656 ?
N2 Cu1 O1 92.3(3) . 25_656 ?
N1 Cu1 O1 87.9(3) 25_656 25_656 ?
N1 Cu1 O1 92.1(3) . 25_656 ?
O1 Cu1 O1 180.0(4) . 25_656 ?
C35 N1 C31 125.7(16) . . ?
C35 N1 C11 68.0(10) . . ?
C31 N1 C11 85.2(9) . . ?
C35 N1 C15 84.0(10) . . ?
C31 N1 C15 69.6(9) . . ?
C11 N1 C15 120 . . ?
C35 N1 Cu1 117.5(11) . . ?
C31 N1 Cu1 116.7(10) . . ?
C11 N1 Cu1 124.3(5) . . ?
C15 N1 Cu1 115.7(5) . . ?
C12 C11 N1 120 . . ?
C13 C12 C11 120 . . ?
C12 C13 C14 120 . . ?
C12 C13 C34 68.4(9) . . ?
C14 C13 C34 82.8(9) . . ?
C12 C13 C32 82.0(10) . . ?
C14 C13 C32 67.4(9) . . ?
C34 C13 C32 119.0(15) . . ?
C12 C13 C23 124.7(11) . 7_564 ?
C14 C13 C23 115.3(11) . 7_564 ?
C34 C13 C23 122(3) . 7_564 ?
C32 C13 C23 119(3) . 7_564 ?
C15 C14 C13 120 . . ?
C14 C15 N1 120 . . ?
N1 C31 C32 115.9(19) . . ?
C31 C32 C13 121(2) . . ?
C13 C34 C35 117.5(18) . . ?
N1 C35 C34 121(2) . . ?
C41 N2 C45 127.5(18) . . ?
C41 N2 C21 57.6(8) . . ?
C45 N2 C21 95.1(9) . . ?
C41 N2 C25 96.3(9) . . ?
C45 N2 C25 56.8(8) . . ?
C21 N2 C25 120 . . ?
C41 N2 Cu1 117.1(12) . . ?
C45 N2 Cu1 115.4(12) . . ?
C21 N2 Cu1 123.6(5) . . ?
C25 N2 Cu1 116.4(5) . . ?
C22 C21 N2 120 . . ?
C21 C22 C23 120 . . ?
C42 C23 C24 90.9(8) . . ?
C42 C23 C22 54.8(7) . . ?
C24 C23 C22 120 . . ?
C42 C23 C44 115.2(12) . . ?
C24 C23 C44 55.8(7) . . ?
C22 C23 C44 93.0(8) . . ?
C42 C23 C13 120.7(15) . 8_645 ?
C24 C23 C13 124(3) . 8_645 ?
C22 C23 C13 116(3) . 8_645 ?
C44 C23 C13 124.0(14) . 8_645 ?
C23 C24 C25 120 . . ?
C24 C25 N2 120 . . ?
C23 C42 C41 125.7(16) . . ?
N2 C41 C42 113.7(16) . . ?
N2 C45 C44 117.9(17) . . ?
C23 C44 C45 120.0(16) . . ?
O1 S1 O2 116.5(8) . . ?
O1 S1 O3 117.3(9) . . ?
O2 S1 O3 116.0(9) . . ?
O1 S1 C1T 109.5(9) . . ?
O2 S1 C1T 105.0(13) . . ?
O3 S1 C1T 87.1(11) . . ?
S1 O1 Cu1 161.6(7) . . ?
F3 C1T F2 101.2(17) . . ?
F3 C1T F1 101.5(17) . . ?
F2 C1T F1 102.7(18) . . ?
F3 C1T S1 117.8(16) . . ?
F2 C1T S1 116.9(16) . . ?
F1 C1T S1 114.4(15) . . ?
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1833572'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT201_3                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) 
RESPONSE:  the triflate groups are disordered about the sulfur or
coordinated oxygen atom and have been modelled with a refined
occupancy as described in the refinment explanation
;
_vrf_PLAT601_3                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of  535 Ang3
RESPONSE: The  highest  peak  in  the  final  difference  map  
is  2.4  e/A3 but  no model for any solvent could be found
;
_vrf_PLAT084_3                   
;
PROBLEM: High wR2 Value (i.e. > 0.25)  0.27 Report
RESPONSE: The  alert  come  from  weak diffraction  
of  the  crystals  and  subsequent 
poor quality of the data
;
_vrf_PLAT202_3                   
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent 
RESPONSE: Atoms of free disordered solvent molecules 
refined with partial ocuupancy of the atom sites
;
_vrf_PLAT241_3                   
;
PROBLEM: High MainMol Ueq as Compared to Neighbors of C24 Check
RESPONSE: These alert is generated because there is a large amount 
of disorder in the structure involving both the main residue and the
solvent molecules.
;
_vrf_PLAT242_3                   
;
PROBLEM: Low  MainMol  Ueq as Compared to Neighbors of S2 Check
RESPONSE: This is unremarkable for the S atom of a very disordered 
triflate group 
;
_vrf_PLAT243_3                   
;
PROBLEM: High Solvent Ueq as Compared to Neighbors of C2R Check
RESPONSE: These alert is generated because there is a large amount 
of disorder in the structure involving both the main residue and the
solvent molecules. Dynamically disordered groups can exhibit 
such unusual ratios. 
;
_vrf_PLAT250_3                   
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.3 Note
RESPONSE: Tthere is a large amount  of disordered solvent molecules 
and coordinated triflate ions in the structure, which also results in
a higher flexibility of some of the atoms modelled on 
discrete atomic positions.This results in a high ratio 
of the average Ui,j Tensor.  
;
_vrf_PLAT342_3                   
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00867 Ang.
RESPONSE: These alert is generated because there is a large amount 
of disorder in the structure involving both the main residue and the
solvent molecules.
;
_vrf_PLAT410_3                   
;
PROBLEM: Short Intra H...H Contact H2R1 .. H3R1 . 1.96 Ang.
RESPONSE: These alert is generated because there is a large amount 
of disorder in the structure involving both the main residue and the
solvent molecules.
;
_vrf_PLAT411_3                   
;
PROBLEM: Short Inter H...H Contact H12 .. H1D1 . 2.07 Ang.
RESPONSE:These alert is generated because there is a large amount 
of disorder in the structure involving both the main residue and the
solvent molecules.
;
# end Validation Reply Form

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

_chemical_formula_sum            'C24.375 H20.75 Cd Cl0.75 F6 N4 O6.50 S2'
_chemical_formula_moiety         
'(C22 H16 Cd F6 N4 O6 S2), 0.5(C4 H8 O), 0.375(C H2 Cl2)'
_chemical_formula_weight         790.81

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_Int_Tables_number      70
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   17.338(1)
_cell_length_b                   42.746(2)
_cell_length_c                   43.404(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     32168(3)
_cell_formula_units_Z            32
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9927
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      29.44

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

_exptl_crystal_description       'polyhedral block'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             12600
_exptl_special_details           
;
 1800 frames were collected on a Brucker SMART CCD diffractometer with a 
 sample to detector distance of 60.00 mm. The counting time per frame 
 was 30 sec and the scan width per frame 0.3 deg. 
;

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

_exptl_absorpt_coefficient_mu    0.76
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6677
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'

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

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD_plate
_diffrn_measurement_device       'Bruker smart apex ccd diffractometer'
_diffrn_measurement_method       omega-scan
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_number            73251
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         29.63
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_reflns_number_total             10885
_reflns_number_gt                9114
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_structure_solution    
'SIR 2014: C. Giacovazzo et all., J. Appl. Cryst.(2015) 48, 306'
_computing_structure_refinement  
'SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122'
_computing_molecular_graphics    
'VESTA 3: K. Momma and F. Izumi, J. Appl. Crystallogr.(2011),44,127'
_computing_publication_material  
'WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1563P)²+721.4664P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10885
_refine_ls_number_parameters     387
_refine_ls_number_restraints     103
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0846
_refine_ls_wR_factor_ref         0.2721
_refine_ls_wR_factor_gt          0.2594
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.465
_refine_diff_density_min         -2.351
_refine_diff_density_rms         0.324

#----------------------------------------------------------------------------#
#                   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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cd Cd -0.8075 1.2024 '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
Cd Cd 0.25586(2) 0.00331(2) 0.01480(2) 0.02635(15) Uani 1 1 d . . . . .
N1 N 0.3052(3) 0.00215(12) 0.06396(10) 0.0323(10) Uani 1 1 d . . . . .
N2 N 0.4555(3) -0.00261(11) 0.21516(11) 0.0347(11) Uani 1 1 d . . . . .
N3 N 0.2015(3) -0.04577(11) 0.02021(11) 0.0332(10) Uani 1 1 d . . . . .
N4 N 0.0590(3) -0.19800(10) -0.00561(11) 0.0320(10) Uani 1 1 d . . . . .
C11 C 0.2600(3) -0.00432(17) 0.08797(14) 0.0378(13) Uani 1 1 d . U . . .
H11 H 0.2071 -0.0086 0.0842 0.045 Uiso 1 1 calc R U . . .
C12 C 0.2857(3) -0.00508(16) 0.11801(13) 0.0369(13) Uani 1 1 d . U . . .
H12 H 0.251 -0.0093 0.1344 0.044 Uiso 1 1 calc R U . . .
C13 C 0.3641(3) 0.00054(13) 0.12390(12) 0.0323(11) Uani 1 1 d . U . . .
C14 C 0.4098(4) 0.0075(2) 0.09880(16) 0.061(2) Uani 1 1 d . U . . .
H14 H 0.4628 0.0124 0.1018 0.073 Uiso 1 1 calc R U . . .
C15 C 0.3798(4) 0.0076(2) 0.06952(15) 0.060(2) Uani 1 1 d . U . . .
H15 H 0.4132 0.0116 0.0526 0.073 Uiso 1 1 calc R U . . .
C21 C 0.3970(4) -0.02098(16) 0.20678(13) 0.0399(13) Uani 1 1 d . U . . .
H21 H 0.3755 -0.0348 0.2216 0.048 Uiso 1 1 calc R U . . .
C22 C 0.3660(4) -0.02064(17) 0.17710(13) 0.0413(14) Uani 1 1 d . U . . .
H22 H 0.3248 -0.0343 0.1719 0.05 Uiso 1 1 calc R U . . .
C23 C 0.3950(4) -0.00068(14) 0.15566(12) 0.0342(12) Uani 1 1 d . U . . .
C24 C 0.4527(6) 0.0199(2) 0.16472(17) 0.068(3) Uani 1 1 d . U . . .
H24 H 0.4716 0.0354 0.151 0.081 Uiso 1 1 calc R U . . .
C25 C 0.4822(6) 0.0172(2) 0.19452(17) 0.067(3) Uani 1 1 d . U . . .
H25 H 0.5238 0.0304 0.2002 0.081 Uiso 1 1 calc R U . . .
C31 C 0.1298(4) -0.05037(14) 0.00976(16) 0.0403(14) Uani 1 1 d . . . . .
H31 H 0.0985 -0.0327 0.0052 0.048 Uiso 1 1 calc R U . . .
C32 C 0.0997(4) -0.08018(13) 0.00536(16) 0.0399(13) Uani 1 1 d . . . . .
H32 H 0.0485 -0.0828 -0.0021 0.048 Uiso 1 1 calc R U . . .
C33 C 0.1449(3) -0.10592(12) 0.01187(13) 0.0328(11) Uani 1 1 d . . . . .
C34 C 0.2182(4) -0.10109(13) 0.02354(16) 0.0396(14) Uani 1 1 d . . . . .
H34 H 0.2502 -0.1183 0.0288 0.048 Uiso 1 1 calc R U . . .
C35 C 0.2441(4) -0.07063(14) 0.02743(16) 0.0393(14) Uani 1 1 d . . . . .
H35 H 0.2943 -0.0674 0.0356 0.047 Uiso 1 1 calc R U . . .
C41 C 0.0445(4) -0.17443(14) -0.02491(15) 0.0438(15) Uani 1 1 d . . . . .
H41 H 0.0153 -0.1785 -0.043 0.053 Uiso 1 1 calc R U . . .
C42 C 0.0704(4) -0.14420(14) -0.01970(16) 0.0446(16) Uani 1 1 d . . . . .
H42 H 0.0579 -0.1279 -0.0337 0.054 Uiso 1 1 calc R U . . .
C43 C 0.1150(4) -0.13796(12) 0.00631(13) 0.0333(11) Uani 1 1 d . . . . .
C44 C 0.1312(4) -0.16249(14) 0.02566(15) 0.0418(14) Uani 1 1 d . . . . .
H43 H 0.1621 -0.1594 0.0435 0.05 Uiso 1 1 calc R U . . .
C45 C 0.1018(4) -0.19193(14) 0.01889(14) 0.0402(14) Uani 1 1 d . . . . .
H44 H 0.1131 -0.2086 0.0326 0.048 Uiso 1 1 calc R U . . .
O11 O 0.3685(3) -0.02073(12) -0.00318(12) 0.0498(11) Uani 1 1 d D . . . .
S1A S 0.4360(5) -0.0393(2) -0.0015(2) 0.0873(12) Uiso 0.374(5) 1 d D . P A 1
C1T1 C 0.4309(16) -0.0660(7) -0.0349(6) 0.138(7) Uiso 0.374(5) 1 d D . P A 1
O12A O 0.4323(14) -0.0591(7) 0.0256(6) 0.141(11) Uiso 0.374(5) 1 d D . P A 1
O13A O 0.5016(17) -0.0187(8) 0.0039(12) 0.170(8) Uiso 0.374(5) 1 d D . P A 1
F11A F 0.3728(16) -0.0862(8) -0.0278(8) 0.167(4) Uiso 0.374(5) 1 d D . P A 1
F12A F 0.4925(15) -0.0860(8) -0.0375(8) 0.167(4) Uiso 0.374(5) 1 d D . P A 1
F13A F 0.4170(16) -0.0580(8) -0.0648(7) 0.167(4) Uiso 0.374(5) 1 d D . P A 1
S1B S 0.4346(3) -0.02694(14) -0.01833(13) 0.0873(12) Uiso 0.626(5) 1 d D . P A
2
C1T2 C 0.4362(11) -0.0693(6) -0.0260(4) 0.138(7) Uiso 0.626(5) 1 d D . P A 2
O12B O 0.4362(10) -0.0121(5) -0.0480(4) 0.152(7) Uiso 0.626(5) 1 d D . P A 2
O13B O 0.5042(10) -0.0219(7) -0.0031(5) 0.170(8) Uiso 0.626(5) 1 d D . P A 2
F11B F 0.3763(10) -0.0766(5) -0.0447(4) 0.167(4) Uiso 0.626(5) 1 d D . P A 2
F12B F 0.4310(10) -0.0838(5) 0.0011(4) 0.167(4) Uiso 0.626(5) 1 d D . P A 2
F13B F 0.5057(10) -0.0725(5) -0.0405(5) 0.167(4) Uiso 0.626(5) 1 d D . P A 2
S2 S 0.07571(10) 0.02825(4) 0.04740(4) 0.0452(4) Uani 1 1 d . . . . .
O21 O 0.1482(3) 0.03128(12) 0.03146(11) 0.0468(11) Uani 1 1 d . . . . .
O22 O 0.0738(3) 0.00205(13) 0.06866(14) 0.0563(14) Uani 1 1 d . . . . .
O23 O 0.0094(4) 0.0319(2) 0.0292(2) 0.098(3) Uani 1 1 d . U . . .
C2T1 C 0.0884(10) 0.0622(5) 0.0746(4) 0.064(5) Uiso 0.51(2) 1 d D . P B 1
F21 F 0.1588(10) 0.0611(3) 0.0883(3) 0.085(4) Uiso 0.51(2) 1 d D . P B 1
F22 F 0.0860(10) 0.0891(4) 0.0592(4) 0.095(5) Uiso 0.51(2) 1 d D . P B 1
F23 F 0.0349(10) 0.0631(4) 0.0969(4) 0.103(6) Uiso 0.51(2) 1 d D . P B 1
C2T2 C 0.0624(10) 0.0626(5) 0.0689(4) 0.061(5) Uiso 0.49(2) 1 d D . P B 2
F21B F 0.1210(11) 0.0656(3) 0.0885(3) 0.084(5) Uiso 0.49(2) 1 d D . P B 2
F22B F -0.0040(10) 0.0620(4) 0.0844(4) 0.101(6) Uiso 0.49(2) 1 d D . P B 2
F23B F 0.0602(10) 0.0878(3) 0.0508(4) 0.087(5) Uiso 0.49(2) 1 d D . P B 2
C1D C 0.125 -0.0554(10) 0.125 0.058(10) Uiso 0.25 2 d DS . P . .
H1D1 H 0.1696 -0.0418 0.1203 0.07 Uiso 0.125 1 calc R U P . .
H1D2 H 0.0804 -0.0418 0.1297 0.07 Uiso 0.125 1 calc R U P . .
Cl2D Cl 0.1079(11) -0.0737(5) 0.0991(4) 0.135(6) Uiso 0.25 1 d D . P . .
C1E C 0.375 -0.125 0.0934(11) 0.057(10) Uiso 0.25 2 d DS . P . .
H1E1 H 0.4159 -0.1329 0.1073 0.068 Uiso 0.125 1 calc R U P . .
H1E2 H 0.3341 -0.1171 0.1073 0.068 Uiso 0.125 1 calc R U P . .
Cl2E Cl 0.4069(18) -0.0980(7) 0.0816(8) 0.216(13) Uiso 0.25 1 d D . P . .
C1F C 0.375 0.0402(13) -0.125 0.068(13) Uiso 0.25 2 d DS . P . .
H1F1 H 0.4059 0.0261 -0.1117 0.082 Uiso 0.125 1 calc R U P . .
H1F2 H 0.3441 0.0261 -0.1383 0.082 Uiso 0.125 1 calc R U P . .
Cl2F Cl 0.3198(18) 0.0524(9) -0.1045(8) 0.236(14) Uiso 0.25 1 d D . P . .
O1R O -0.1687(15) -0.1036(6) 0.0527(6) 0.140(8) Uiso 0.5 1 d . . P . .
C2R C -0.0840(14) -0.1038(6) 0.0355(6) 0.173(9) Uiso 1 1 d . . . . .
H2R1 H -0.0953 -0.0824 0.043 0.207 Uiso 1 1 calc R U . . .
H2R2 H -0.0447 -0.1013 0.0192 0.207 Uiso 1 1 calc R U . . .
C3R C -0.201(2) -0.1329(10) 0.0578(10) 0.147(13) Uiso 0.5 1 d . . P . .
H3R1 H -0.1874 -0.1418 0.0781 0.177 Uiso 0.5 1 calc R U P . .
H3R2 H -0.258 -0.1329 0.0551 0.177 Uiso 0.5 1 calc R U P . .
C4R C -0.143(2) -0.1122(9) 0.0219(10) 0.142(13) Uiso 0.5 1 d . . P . .
H4R1 H -0.1339 -0.1135 -0.0006 0.17 Uiso 0.5 1 calc R U P . .
H4R2 H -0.1856 -0.0971 0.0256 0.17 Uiso 0.5 1 calc R U P . .



#----------------------------------------------------------------------------#
#                   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
Cd N1 2.299(4) . ?
Cd N4 2.310(4) 30 ?
Cd N3 2.312(4) . ?
Cd N2 2.325(4) 20 ?
Cd O21 2.331(5) . ?
Cd O11 2.340(5) . ?
N1 C11 1.333(7) . ?
N1 C15 1.336(8) . ?
N2 C25 1.317(9) . ?
N2 C21 1.334(8) . ?
N2 Cd 2.325(4) 28 ?
N3 C35 1.331(8) . ?
N3 C31 1.338(7) . ?
N4 C45 1.323(8) . ?
N4 C41 1.334(8) . ?
N4 Cd 2.310(4) 18 ?
C11 C12 1.378(8) . ?
C12 C13 1.404(8) . ?
C13 C14 1.380(9) . ?
C13 C23 1.481(7) . ?
C14 C15 1.373(9) . ?
C21 C22 1.396(7) . ?
C22 C23 1.359(8) . ?
C23 C24 1.390(9) . ?
C24 C25 1.395(9) . ?
C31 C32 1.390(7) . ?
C32 C33 1.381(8) . ?
C33 C34 1.383(8) . ?
C33 C43 1.485(7) . ?
C34 C35 1.387(7) . ?
C41 C42 1.387(8) . ?
C42 C43 1.394(8) . ?
C43 C44 1.373(8) . ?
C44 C45 1.389(8) . ?
O11 S1B 1.349(7) . ?
O11 S1A 1.416(10) . ?
S1A O12A 1.453(18) . ?
S1A O13A 1.456(19) . ?
S1A C1T1 1.85(3) . ?
C1T1 F11A 1.363(17) . ?
C1T1 F13A 1.366(17) . ?
C1T1 F12A 1.374(17) . ?
O13A O13A 1.63(6) 17_655 ?
S1B O13B 1.392(15) . ?
S1B O12B 1.436(14) . ?
S1B C1T2 1.84(2) . ?
C1T2 F12B 1.332(16) . ?
C1T2 F11B 1.355(15) . ?
C1T2 F13B 1.368(15) . ?
S2 O23 1.404(6) . ?
S2 O21 1.441(5) . ?
S2 O22 1.452(6) . ?
S2 C2T2 1.76(2) . ?
S2 C2T1 1.88(2) . ?
C2T1 F22 1.333(15) . ?
C2T1 F23 1.342(16) . ?
C2T1 F21 1.357(16) . ?
C2T2 F21B 1.332(16) . ?
C2T2 F22B 1.334(15) . ?
C2T2 F23B 1.334(16) . ?
C1D Cl2D 1.40(2) 4 ?
C1D Cl2D 1.40(2) . ?
Cl2D Cl2D 2.33(4) 4 ?
C1E Cl2E 1.38(2) 14_545 ?
C1E Cl2E 1.38(2) . ?
C1F Cl2F 1.41(2) 12_554 ?
C1F Cl2F 1.41(2) . ?
O1R C3R 1.39(4) . ?
C2R C4R 1.24(4) . ?
C2R C3R 1.28(4) 14_445 ?
C3R C2R 1.28(4) 14_445 ?
C4R C2R 1.62(4) 14_445 ?

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
N1 Cd N4 91.81(17) . 30 ?
N1 Cd N3 92.16(16) . . ?
N4 Cd N3 175.87(16) 30 . ?
N1 Cd N2 178.02(17) . 20 ?
N4 Cd N2 90.06(17) 30 20 ?
N3 Cd N2 85.96(16) . 20 ?
N1 Cd O21 91.20(18) . . ?
N4 Cd O21 84.88(18) 30 . ?
N3 Cd O21 96.16(18) . . ?
N2 Cd O21 89.63(19) 20 . ?
N1 Cd O11 89.42(19) . . ?
N4 Cd O11 90.31(19) 30 . ?
N3 Cd O11 88.60(19) . . ?
N2 Cd O11 89.90(19) 20 . ?
O21 Cd O11 175.17(18) . . ?
C11 N1 C15 117.6(5) . . ?
C11 N1 Cd 120.8(4) . . ?
C15 N1 Cd 121.6(4) . . ?
C25 N2 C21 117.4(5) . . ?
C25 N2 Cd 120.5(4) . 28 ?
C21 N2 Cd 122.0(4) . 28 ?
C35 N3 C31 118.5(5) . . ?
C35 N3 Cd 121.5(4) . . ?
C31 N3 Cd 118.5(4) . . ?
C45 N4 C41 117.5(5) . . ?
C45 N4 Cd 122.6(4) . 18 ?
C41 N4 Cd 119.8(4) . 18 ?
N1 C11 C12 123.7(5) . . ?
C11 C12 C13 118.8(5) . . ?
C14 C13 C12 116.7(5) . . ?
C14 C13 C23 122.3(5) . . ?
C12 C13 C23 121.0(5) . . ?
C15 C14 C13 120.9(6) . . ?
N1 C15 C14 122.3(6) . . ?
N2 C21 C22 122.6(6) . . ?
C23 C22 C21 119.7(6) . . ?
C22 C23 C24 118.1(5) . . ?
C22 C23 C13 121.7(5) . . ?
C24 C23 C13 120.1(6) . . ?
C23 C24 C25 118.2(6) . . ?
N2 C25 C24 123.8(6) . . ?
N3 C31 C32 122.0(6) . . ?
C33 C32 C31 119.3(5) . . ?
C32 C33 C34 118.5(5) . . ?
C32 C33 C43 120.2(5) . . ?
C34 C33 C43 121.3(5) . . ?
C33 C34 C35 118.8(5) . . ?
N3 C35 C34 122.8(5) . . ?
N4 C41 C42 122.7(6) . . ?
C41 C42 C43 119.3(6) . . ?
C44 C43 C42 117.6(5) . . ?
C44 C43 C33 122.2(5) . . ?
C42 C43 C33 120.1(5) . . ?
C43 C44 C45 119.2(5) . . ?
N4 C45 C44 123.6(6) . . ?
S1B O11 Cd 163.5(4) . . ?
S1A O11 Cd 156.8(5) . . ?
O11 S1A O12A 109.3(12) . . ?
O11 S1A O13A 108.4(15) . . ?
O12A S1A O13A 104.9(14) . . ?
O11 S1A C1T1 105.4(11) . . ?
O12A S1A C1T1 105.8(18) . . ?
O13A S1A C1T1 123(3) . . ?
F11A C1T1 F13A 104(2) . . ?
F11A C1T1 F12A 101(2) . . ?
F13A C1T1 F12A 102.4(19) . . ?
F11A C1T1 S1A 105(2) . . ?
F13A C1T1 S1A 127(3) . . ?
F12A C1T1 S1A 114(3) . . ?
S1A O13A O13A 122(2) . 17_655 ?
O11 S1B O13B 118.3(11) . . ?
O11 S1B O12B 111.5(8) . . ?
O13B S1B O12B 110.0(10) . . ?
O11 S1B C1T2 107.1(7) . . ?
O13B S1B C1T2 103.0(15) . . ?
O12B S1B C1T2 105.8(11) . . ?
F12B C1T2 F11B 111.6(15) . . ?
F12B C1T2 F13B 114.7(15) . . ?
F11B C1T2 F13B 112.1(15) . . ?
F12B C1T2 S1B 107.4(17) . . ?
F11B C1T2 S1B 109.0(17) . . ?
F13B C1T2 S1B 101.3(17) . . ?
O23 S2 O21 115.7(4) . . ?
O23 S2 O22 115.1(4) . . ?
O21 S2 O22 113.2(3) . . ?
O23 S2 C2T2 95.7(7) . . ?
O21 S2 C2T2 107.1(6) . . ?
O22 S2 C2T2 107.7(5) . . ?
O23 S2 C2T1 111.4(7) . . ?
O21 S2 C2T1 97.5(5) . . ?
O22 S2 C2T1 101.4(5) . . ?
S2 O21 Cd 143.3(3) . . ?
F22 C2T1 F23 108.5(13) . . ?
F22 C2T1 F21 106.1(14) . . ?
F23 C2T1 F21 107.9(14) . . ?
F22 C2T1 S2 110.3(14) . . ?
F23 C2T1 S2 113.1(13) . . ?
F21 C2T1 S2 110.6(12) . . ?
F21B C2T2 F22B 109.7(13) . . ?
F21B C2T2 F23B 108.9(13) . . ?
F22B C2T2 F23B 106.8(13) . . ?
F21B C2T2 S2 108.6(12) . . ?
F22B C2T2 S2 111.4(13) . . ?
F23B C2T2 S2 111.4(13) . . ?
Cl2D C1D Cl2D 112(3) 4 . ?
C1D Cl2D Cl2D 33.9(16) . 4 ?
Cl2E C1E Cl2E 136(5) 14_545 . ?
Cl2F C1F Cl2F 136(5) 12_554 . ?
C4R C2R C3R 129(4) . 14_445 ?
C2R C3R O1R 95(3) 14_445 . ?
C2R C4R C2R 107(3) . 14_445 ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1833571'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT082_2                   
;
PROBLEM: High R1 Value .................................. 0.11 Report
RESPONSE: It is due to poor quality of x-ray data 
;
_vrf_PLAT084_2                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.33 Report
RESPONSE: It is due to poor quality of x-ray data
;
_vrf_PLAT220_2                   
;
PROBLEM: Non-Solvent Resd 1 O Ueq(max)/Ueq(min) Range 3.9 Ratio
RESPONSE: Non-Solvent Resd 1 O Ueq(max)/Ueq(min) Range
;
_vrf_PLAT241_2                   
;
PROBLEM: High MainMol Ueq as Compared to Neighbors of O23 Check
RESPONSE: These alert is generated because there is a large amount 
of disorder in the structure involving the triflate counteranion 
in the main residue
;
_vrf_PLAT341_2                   
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00772 Ang.
RESPONSE: It is due to poor quality of x-ray data
;
# end Validation Reply Form

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

_chemical_formula_sum            'C22 H16.75 F6 Fe N4 O6.375 S2'
_chemical_formula_moiety         
'(C21.625 H16.75 F4.875 Fe N4 O5.25 S1.625), 0.375(C F3 O3 S)'
_chemical_formula_weight         673.11

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_Int_Tables_number      70
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   16.993(9)
_cell_length_b                   42.006(2)
_cell_length_c                   42.426(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     30283(3)
_cell_formula_units_Z            32
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      23.96

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

_exptl_crystal_description       'polyhedral block'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10872
_exptl_special_details           
;
 2400 frames were collected on a Brucker SMART CCD diffractometer with a 
 sample to detector distance of 60.00 mm. The counting time per frame 
 was 30 sec and the scan width per frame 0.3 deg. 
;

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

_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'

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

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD_plate
_diffrn_measurement_device       'bruker smart apex ccd diffractometer'
_diffrn_measurement_method       omega-scan
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.027
_diffrn_reflns_number            62609
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_full        23.97
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             5899
_reflns_number_gt                4978
_reflns_threshold_expression     >2sigma(I)

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

_computing_structure_solution    
'SIR 2014: C. Giacovazzo et all., J. Appl. Cryst.(2015) 48, 306'
_computing_structure_refinement  
'SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122'
_computing_molecular_graphics    
'VESTA 3: K. Momma and F. Izumi, J. Appl. Crystallogr.(2011),44,127'
_computing_publication_material  
'WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5899
_refine_ls_number_parameters     401
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.1085
_refine_ls_wR_factor_ref         0.3311
_refine_ls_wR_factor_gt          0.3232
_refine_ls_goodness_of_fit_ref   1.472
_refine_ls_restrained_S_all      1.471
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.154
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.091 -0.125 0.125 911 401 ' '
2 0.355 0.125 0.375 911 400 ' '
3 0.591 -0.125 0.625 911 401 ' '
4 0.856 0.125 0.875 911 400 ' '
5 0.625 0.125 0.125 312 219 ' '
6 0.125 0.125 0.625 312 219 ' '
7 0.100 0.375 0.125 911 401 ' '
8 0.600 0.375 0.625 911 401 ' '
9 0.375 0.375 0.375 312 220 ' '
10 0.875 0.375 0.875 312 220 ' '
11 0.899 0.625 0.375 911 400 ' '
12 0.399 0.625 0.875 911 400 ' '
13 0.125 0.625 0.125 312 219 ' '
14 0.625 0.625 0.625 312 219 ' '
15 0.875 0.875 0.375 312 220 ' '
16 0.375 0.875 0.875 312 220 ' '
_platon_squeeze_details          
;
 Attempts to refine peaks of residual electron density as guest
 atoms were unsuccessful. The data were corrected for disordered
 electron density through use of the SQUEEZE procedure (Sluis, P. van der;
 Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON
 (Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13)
 A total solvent-accessible surface of 3237.24 A³ (10,7%) and a 
 contact surface of 8373,03 A³ (27.6%)
;
#----------------------------------------------------------------------------#
#                   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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Fe Fe 0.3463 0.8444 '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
Fe Fe 0.49546(4) 0.00165(2) 0.23613(2) 0.0253(4) Uani 1 1 d . . . . .
N4 N 0.4466(3) 0.04918(10) 0.24433(10) 0.0294(10) Uani 1 1 d . . . . .
C45 C 0.4622(4) 0.07332(13) 0.22478(12) 0.0360(13) Uani 1 1 d . . . . .
H45 H 0.4932 0.0692 0.2066 0.043 Uiso 1 1 calc R U . . .
C44 C 0.4356(4) 0.10360(13) 0.22963(13) 0.0388(14) Uani 1 1 d . . . . .
H44 H 0.451 0.1201 0.2157 0.047 Uiso 1 1 calc R U . . .
C43 C 0.3862(3) 0.11039(12) 0.25497(13) 0.0297(12) Uani 1 1 d . . . . .
C42 C 0.3666(4) 0.08534(14) 0.27451(13) 0.0410(14) Uani 1 1 d . . . . .
H42 H 0.3318 0.0885 0.2918 0.049 Uiso 1 1 calc R U . . .
C41 C 0.3988(4) 0.05517(13) 0.26855(13) 0.0386(14) Uani 1 1 d . . . . .
H41 H 0.386 0.0382 0.2824 0.046 Uiso 1 1 calc R U . . .
N3 N 0.5462(3) -0.04567(10) 0.23185(10) 0.0313(10) Uani 1 1 d . . . . .
C31 C 0.5021(3) -0.07190(14) 0.22488(14) 0.0376(14) Uani 1 1 d . . . . .
H31 H 0.4502 -0.0688 0.2172 0.045 Uiso 1 1 calc R U . . .
C32 C 0.5287(3) -0.10230(13) 0.22841(13) 0.0352(13) Uani 1 1 d . . . . .
H32 H 0.4956 -0.1198 0.2235 0.042 Uiso 1 1 calc R U . . .
C33 C 0.6056(3) -0.10740(13) 0.23946(13) 0.0313(12) Uani 1 1 d . . . . .
C34 C 0.6513(3) -0.08063(12) 0.24549(13) 0.0345(13) Uani 1 1 d . . . . .
H34 H 0.7038 -0.0829 0.2529 0.041 Uiso 1 1 calc R U . . .
C35 C 0.6200(4) -0.05079(14) 0.24059(14) 0.0392(14) Uani 1 1 d . . . . .
H35 H 0.6532 -0.0329 0.2437 0.047 Uiso 1 1 calc R U . . .
N1 N 0.4466(3) -0.00078(10) 0.18886(10) 0.0312(11) Uani 1 1 d . . . . .
C15 C 0.4891(3) -0.01220(14) 0.16511(12) 0.0328(13) Uani 1 1 d . . . . .
H15 H 0.5404 -0.0199 0.1696 0.039 Uiso 1 1 calc R U . . .
C14 C 0.4633(3) -0.01355(14) 0.13407(12) 0.0378(13) Uani 1 1 d . . . . .
H14 H 0.4953 -0.0226 0.1181 0.045 Uiso 1 1 calc R U . . .
C13 C 0.3878(3) -0.00100(12) 0.12682(14) 0.0344(13) Uani 1 1 d . . . . .
C12 C 0.3442(3) 0.01091(14) 0.15239(13) 0.0363(13) Uani 1 1 d . . . . .
H12 H 0.2924 0.0186 0.149 0.044 Uiso 1 1 calc R U . . .
C11 C 0.3750(3) 0.01154(16) 0.18169(13) 0.0410(14) Uani 1 1 d . . . . .
H11 H 0.345 0.021 0.1981 0.049 Uiso 1 1 calc R U . . .
N2 N 0.5460(3) 0.00264(10) 0.28381(11) 0.0325(11) Uani 1 1 d . . . . .
C25 C 0.5928(4) 0.02539(14) 0.29395(12) 0.0397(14) Uani 1 1 d . . . . .
H25 H 0.6061 0.0421 0.2798 0.048 Uiso 1 1 calc R U . . .
C24 C 0.6235(3) 0.02627(14) 0.32401(12) 0.0368(13) Uani 1 1 d . . . . .
H24 H 0.6554 0.0437 0.3304 0.044 Uiso 1 1 calc R U . . .
C23 C 0.6079(3) 0.00171(12) 0.34503(13) 0.0317(13) Uani 1 1 d . . . . .
C22 C 0.5577(4) -0.02275(14) 0.33471(15) 0.0455(15) Uani 1 1 d . . . . .
H22 H 0.5431 -0.0397 0.3483 0.055 Uiso 1 1 calc R U . . .
C21 C 0.5306(4) -0.02114(13) 0.30435(13) 0.0390(14) Uani 1 1 d . . . . .
H21 H 0.4984 -0.0381 0.2971 0.047 Uiso 1 1 calc R U . . .
S1A S 0.3165(2) -0.03353(9) 0.25322(9) 0.0764(13) Uani 0.624(6) 1 d D . P A 1
O11A O 0.3919(9) -0.0168(3) 0.2547(4) 0.034(4) Uani 0.624(6) 1 d D . P A 1
O12A O 0.3038(7) -0.0518(3) 0.2243(3) 0.106(4) Uani 0.624(6) 1 d D . P A 1
O13A O 0.2521(5) -0.0124(3) 0.2602(3) 0.084(3) Uani 0.624(6) 1 d D . P A 1
C1A C 0.3125(6) -0.0601(3) 0.2824(3) 0.073(4) Uani 0.624(6) 1 d D . P A 1
F11A F 0.3721(5) -0.0799(3) 0.2857(2) 0.096(3) Uani 0.624(6) 1 d D . P A 1
F12A F 0.3253(8) -0.0470(4) 0.3107(3) 0.116(4) Uani 0.624(6) 1 d D . P A 1
F13A F 0.2432(6) -0.0742(3) 0.2879(2) 0.095(3) Uani 0.624(6) 1 d D . P A 1
O1W O 0.3867(16) -0.0229(6) 0.2534(7) 0.027(6) Uiso 0.376(6) 1 d . . P A 2
S1B S 0.3495(5) -0.06365(19) 0.3294(2) 0.096(3) Uiso 0.376(6) 1 d D . P A 2
O11B O 0.3181(10) -0.0635(4) 0.3597(4) 0.097(5) Uiso 0.376(6) 1 d D . P A 2
O12B O 0.4207(12) -0.0801(6) 0.3260(5) 0.132(8) Uiso 0.376(6) 1 d D . P A 2
O13B O 0.3490(18) -0.0337(6) 0.3142(8) 0.144(16) Uiso 0.376(6) 1 d D . P A 2
C1B C 0.2956(14) -0.0878(5) 0.3048(6) 0.079(7) Uiso 0.376(6) 1 d D . P A 2
F11B F 0.324(3) -0.0914(9) 0.2753(9) 0.254(11) Uiso 0.376(6) 1 d D . P A 2
F12B F 0.268(2) -0.1167(8) 0.3130(9) 0.254(11) Uiso 0.376(6) 1 d D . P A 2
F13B F 0.228(2) -0.0706(10) 0.3004(11) 0.254(11) Uiso 0.376(6) 1 d D . P A 2
O21 O 0.5975(2) 0.02261(9) 0.21753(9) 0.0386(9) Uani 1 1 d . . . . .
O23 O 0.7401(3) 0.02618(16) 0.21871(16) 0.0829(18) Uani 1 1 d . . . . .
C2T C 0.6662(5) 0.0541(2) 0.1743(2) 0.075(2) Uani 1 1 d . . . . .
S2A S 0.67337(17) 0.02255(8) 0.20177(7) 0.0442(11) Uiso 0.530(6) 1 d . . P B 3
O22 O 0.6799(6) -0.0040(2) 0.1808(2) 0.059(2) Uiso 0.530(6) 1 d . . P B 3
F21A F 0.6617(6) 0.0834(2) 0.1925(2) 0.087(3) Uiso 0.530(6) 1 d . . P B 3
F22A F 0.7313(7) 0.0577(3) 0.1561(3) 0.089(3) Uiso 0.530(6) 1 d . . P B 3
F23A F 0.5966(6) 0.0570(3) 0.1597(3) 0.077(3) Uiso 0.530(6) 1 d . . P B 3
S2B S 0.66936(19) 0.04020(8) 0.21361(8) 0.0409(11) Uiso 0.470(6) 1 d . . P B 4
O22B O 0.6631(6) 0.0697(2) 0.2303(2) 0.054(3) Uiso 0.470(6) 1 d . . P B 4
F21B F 0.6117(7) 0.0693(3) 0.1656(3) 0.068(3) Uiso 0.470(6) 1 d . . P B 4
F22B F 0.7351(8) 0.0700(4) 0.1665(4) 0.096(4) Uiso 0.470(6) 1 d . . P B 4
F23B F 0.6729(7) 0.0266(3) 0.1543(3) 0.092(4) Uiso 0.470(6) 1 d . . P B 4



#----------------------------------------------------------------------------#
#                   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
Fe O11A 2.078(14) . ?
Fe O21 2.098(4) . ?
Fe N1 2.173(4) . ?
Fe N3 2.174(4) . ?
Fe N4 2.190(4) . ?
Fe N2 2.198(5) . ?
Fe O1W 2.24(3) . ?
N4 C41 1.334(7) . ?
N4 C45 1.336(7) . ?
C45 C44 1.365(8) . ?
C44 C43 1.393(8) . ?
C43 C42 1.380(8) . ?
C43 C33 1.469(7) 22 ?
C42 C41 1.404(8) . ?
N3 C35 1.325(7) . ?
N3 C31 1.365(7) . ?
C31 C32 1.363(8) . ?
C32 C33 1.406(7) . ?
C33 C34 1.390(8) . ?
C33 C43 1.469(7) 26 ?
C34 C35 1.378(8) . ?
N1 C15 1.330(7) . ?
N1 C11 1.357(7) . ?
C15 C14 1.389(8) . ?
C14 C13 1.420(8) . ?
C13 C12 1.406(8) . ?
C13 C23 1.442(9) 20 ?
C12 C11 1.348(8) . ?
N2 C25 1.316(7) . ?
N2 C21 1.351(7) . ?
C25 C24 1.379(8) . ?
C24 C23 1.389(8) . ?
C23 C22 1.405(8) . ?
C23 C13 1.442(9) 28 ?
C22 C21 1.369(8) . ?
S1A O13A 1.440(9) . ?
S1A O11A 1.461(13) . ?
S1A O12A 1.462(10) . ?
S1A C1A 1.670(15) . ?
O13A O13A 1.36(2) 25 ?
C1A F11A 1.317(13) . ?
C1A F13A 1.338(12) . ?
C1A F12A 1.338(14) . ?
S1B O11B 1.392(17) . ?
S1B O12B 1.400(18) . ?
S1B O13B 1.41(2) . ?
S1B C1B 1.72(3) . ?
C1B F12B 1.35(3) . ?
C1B F11B 1.35(3) . ?
C1B F13B 1.37(3) . ?
O21 S2B 1.437(5) . ?
O21 S2A 1.453(5) . ?
O23 S2A 1.352(6) . ?
O23 S2B 1.356(6) . ?
C2T F21B 1.187(13) . ?
C2T F23A 1.340(14) . ?
C2T F22A 1.357(14) . ?
C2T F22B 1.387(16) . ?
C2T F23B 1.435(15) . ?
C2T F21A 1.458(14) . ?
C2T S2A 1.768(9) . ?
C2T S2B 1.768(9) . ?
S2A O22 1.430(10) . ?
S2B O22B 1.431(11) . ?

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
O11A Fe O21 177.1(5) . . ?
O11A Fe N1 90.5(5) . . ?
O21 Fe N1 89.32(17) . . ?
O11A Fe N3 91.5(5) . . ?
O21 Fe N3 91.41(17) . . ?
N1 Fe N3 91.81(15) . . ?
O11A Fe N4 87.7(4) . . ?
O21 Fe N4 89.45(16) . . ?
N1 Fe N4 92.56(16) . . ?
N3 Fe N4 175.56(15) . . ?
O11A Fe N2 89.4(5) . . ?
O21 Fe N2 90.88(16) . . ?
N1 Fe N2 178.31(16) . . ?
N3 Fe N2 86.51(16) . . ?
N4 Fe N2 89.12(16) . . ?
O21 Fe O1W 176.3(7) . . ?
N1 Fe O1W 88.0(7) . . ?
N3 Fe O1W 86.2(7) . . ?
N4 Fe O1W 93.2(7) . . ?
N2 Fe O1W 91.7(7) . . ?
C41 N4 C45 117.1(4) . . ?
C41 N4 Fe 121.7(4) . . ?
C45 N4 Fe 121.2(3) . . ?
N4 C45 C44 123.2(5) . . ?
C45 C44 C43 120.4(5) . . ?
C42 C43 C44 116.9(5) . . ?
C42 C43 C33 121.3(5) . 22 ?
C44 C43 C33 121.7(5) . 22 ?
C43 C42 C41 119.1(5) . . ?
N4 C41 C42 123.1(5) . . ?
C35 N3 C31 116.7(4) . . ?
C35 N3 Fe 120.0(3) . . ?
C31 N3 Fe 122.6(3) . . ?
C32 C31 N3 123.4(5) . . ?
C31 C32 C33 119.2(5) . . ?
C34 C33 C32 117.2(5) . . ?
C34 C33 C43 121.2(5) . 26 ?
C32 C33 C43 121.6(5) . 26 ?
C35 C34 C33 119.5(5) . . ?
N3 C35 C34 123.8(5) . . ?
C15 N1 C11 117.1(5) . . ?
C15 N1 Fe 120.6(3) . . ?
C11 N1 Fe 122.1(4) . . ?
N1 C15 C14 124.2(5) . . ?
C15 C14 C13 118.4(5) . . ?
C12 C13 C14 116.1(5) . . ?
C12 C13 C23 122.9(5) . 20 ?
C14 C13 C23 120.9(5) . 20 ?
C11 C12 C13 121.0(5) . . ?
C12 C11 N1 123.1(5) . . ?
C25 N2 C21 116.3(5) . . ?
C25 N2 Fe 123.4(4) . . ?
C21 N2 Fe 120.3(3) . . ?
N2 C25 C24 123.4(5) . . ?
C25 C24 C23 120.1(5) . . ?
C24 C23 C22 117.3(5) . . ?
C24 C23 C13 123.2(5) . 28 ?
C22 C23 C13 119.4(5) . 28 ?
C21 C22 C23 117.4(6) . . ?
N2 C21 C22 125.3(5) . . ?
O13A S1A O11A 111.2(8) . . ?
O13A S1A O12A 112.6(7) . . ?
O11A S1A O12A 114.7(9) . . ?
O13A S1A C1A 103.2(7) . . ?
O11A S1A C1A 109.0(8) . . ?
O12A S1A C1A 105.3(7) . . ?
S1A O11A Fe 154.9(11) . . ?
O13A O13A S1A 112.4(11) 25 . ?
F11A C1A F13A 112.2(11) . . ?
F11A C1A F12A 92.4(11) . . ?
F13A C1A F12A 99.9(13) . . ?
F11A C1A S1A 118.0(9) . . ?
F13A C1A S1A 117.4(10) . . ?
F12A C1A S1A 112.4(9) . . ?
O11B S1B O12B 115.4(10) . . ?
O11B S1B O13B 114.6(12) . . ?
O12B S1B O13B 113.3(11) . . ?
O11B S1B C1B 111.0(12) . . ?
O12B S1B C1B 96.1(14) . . ?
O13B S1B C1B 104.1(18) . . ?
F12B C1B F11B 106(2) . . ?
F12B C1B F13B 103(2) . . ?
F11B C1B F13B 104(2) . . ?
F12B C1B S1B 124(3) . . ?
F11B C1B S1B 116(3) . . ?
F13B C1B S1B 102(3) . . ?
S2B O21 Fe 164.0(3) . . ?
S2A O21 Fe 154.9(3) . . ?
F23A C2T F22A 116.5(9) . . ?
F21B C2T F22B 108.9(10) . . ?
F21B C2T F23B 108.3(11) . . ?
F22B C2T F23B 100.4(10) . . ?
F23A C2T F21A 96.9(9) . . ?
F22A C2T F21A 104.4(9) . . ?
F23A C2T S2A 115.7(7) . . ?
F22A C2T S2A 113.9(8) . . ?
F21A C2T S2A 106.7(7) . . ?
F21B C2T S2B 119.6(8) . . ?
F22B C2T S2B 111.0(9) . . ?
F23B C2T S2B 106.8(7) . . ?
O23 S2A O22 110.7(5) . . ?
O23 S2A O21 120.0(4) . . ?
O22 S2A O21 110.8(4) . . ?
O23 S2A C2T 108.9(5) . . ?
O22 S2A C2T 100.4(5) . . ?
O21 S2A C2T 104.0(4) . . ?
O23 S2B O22B 111.2(5) . . ?
O23 S2B O21 120.8(4) . . ?
O22B S2B O21 108.9(5) . . ?
O23 S2B C2T 108.6(5) . . ?
O22B S2B C2T 100.4(6) . . ?
O21 S2B C2T 104.7(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_1b
_database_code_depnum_ccdc_archive 'CCDC 1833569'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT082_1b                  
;
 PROBLEM: High R1 Value: 0.12 Report
 RESPONSE: It is due to poor x-ray refinement data: measurement 
 has been carried out at 293K on a in situ partially deydrated 
 crystal  that has lost some crystallinity but maintains his single 
 crystal nature. The structure is essential to track the dehydration 
 behavior of the system. 
;
_vrf_PLAT220_1b                  
;
 PROBLEM: Non-Solvent Resd 1 O Ueq(max)/Ueq(min) Range 3.3 Ratio
 RESPONSE: see answer for PLAT082
;
_vrf_PLAT241_1b                  
;
 PROBLEM: High  MainMol  Ueq as Compared to Neighbors of C21 Check
 RESPONSE: see answer for PLAT082
;
_vrf_PLAT242_1b                  
;
 PROBLEM: Low  MainMol  Ueq as Compared to Neighbors of O1 Check
 RESPONSE: see answer for PLAT082
;
_vrf_PLAT250_1b                  
;
 PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.1 Note
R ESPONSE: see answer for PLAT082
;
_vrf_PLAT341_1b                  
;
 PROBLEM: Low Bond Precision on C-C Bonds ......... 0.01011 Ang.
 RESPONSE: see answer for PLAT082
;
# end Validation Reply Form

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

_chemical_formula_sum            'C22 H16 Cu F6 N4 O6 S2'
_chemical_formula_moiety         'C22 H16 Cu F6 N4 O6 S2'
_chemical_formula_weight         674.06

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

_space_group_name_Hall           '-I 4bd 2c'
_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 41/acd'
_symmetry_Int_Tables_number      142
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   28.481(4)
_cell_length_b                   28.481
_cell_length_c                   18.723(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15187(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8401
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      21.3

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

_exptl_crystal_description       'polyhedral block'
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5424
_exptl_special_details           
;
 1500 frames were collected on a Bruker Smart APEX CCD diffractometer with a 
 sample to detector distance of 50.00 mm. The counting time per frame 
 was 30 sec and the scan width per frame 0.5 deg. 
;

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

_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD_plate
_diffrn_measurement_device       'Bruker smart apex ccd diffractometer'
_diffrn_measurement_method       omega-scan
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_number            89066
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         26.62
_diffrn_reflns_theta_full        26.62
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             3965
_reflns_number_gt                3050
_reflns_threshold_expression     >2sigma(I)

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

_computing_structure_solution    
'SIR 2014: C. Giacovazzo et all., J. Appl. Cryst.(2015) 48, 306'
_computing_structure_refinement  
'SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122'
_computing_molecular_graphics    
'VESTA 3: K. Momma and F. Izumi, J. Appl. Crystallogr.(2011),44,127'
_computing_publication_material  
'WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3965
_refine_ls_number_parameters     181
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1482
_refine_ls_R_factor_gt           0.1237
_refine_ls_wR_factor_ref         0.3948
_refine_ls_wR_factor_gt          0.3788
_refine_ls_goodness_of_fit_ref   1.54
_refine_ls_restrained_S_all      1.537
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.109

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.250 0.375 175 54 ' '
2 0.000 0.250 0.875 173 54 ' '
3 0.000 0.750 0.125 174 54 ' '
4 0.000 0.750 0.625 173 54 ' '
5 0.250 0.000 0.520 915 371 ' '
6 0.250 0.500 0.031 915 371 ' '
7 0.500 0.250 0.125 174 54 ' '
8 0.500 0.250 0.625 173 54 ' '
9 0.500 0.750 0.875 175 54 ' '
10 0.500 0.750 0.375 173 54 ' '
11 0.750 0.000 0.979 915 371 ' '
12 0.750 0.500 0.469 915 371 ' '
_platon_squeeze_details          
;
 Attempts to refine peaks of residual electron density as guest
 atoms were unsuccessful. The data were corrected for disordered
 electron density through use of the SQUEEZE procedure (Sluis, P. van der;
 Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON
 (Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13)
 A total solvent-accessible surface of 1950,18 A³ (12.8%) and a 
 contact surface of 5087.59 A³ (33.5%)
;

#----------------------------------------------------------------------------#
#                   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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu 0.75 0.25489(3) 0 0.0697(6) Uani 1 2 d S . .
N1 N 0.70755(18) 0.30400(14) 0.0451(3) 0.0622(13) Uani 1 1 d . . .
C11 C 0.7004(3) 0.3027(3) 0.1172(4) 0.084(2) Uani 1 1 d . . .
H11 H 0.7173 0.282 0.1457 0.101 Uiso 1 1 calc R . .
C12 C 0.6677(3) 0.3326(3) 0.1470(4) 0.083(2) Uani 1 1 d . . .
H12 H 0.6606 0.3294 0.1952 0.1 Uiso 1 1 calc R . .
C13 C 0.6451(2) 0.36698(19) 0.1080(3) 0.0644(15) Uani 1 1 d . . .
C14 C 0.6564(3) 0.3711(2) 0.0352(4) 0.087(2) Uani 1 1 d . . .
H14 H 0.6428 0.394 0.0063 0.104 Uiso 1 1 calc R . .
C15 C 0.6897(3) 0.3385(2) 0.0083(4) 0.084(2) Uani 1 1 d . . .
H15 H 0.6995 0.342 -0.0388 0.101 Uiso 1 1 calc R . .
N2 N 0.79119(17) 0.20411(15) -0.0445(3) 0.0649(14) Uani 1 1 d . . .
C21 C 0.8350(3) 0.2029(3) -0.0267(5) 0.101(3) Uani 1 1 d . . .
H21 H 0.8461 0.2243 0.0069 0.122 Uiso 1 1 calc R . .
C22 C 0.8671(3) 0.1695(3) -0.0572(4) 0.094(2) Uani 1 1 d . . .
H22 H 0.8983 0.1684 -0.0427 0.113 Uiso 1 1 calc R . .
C23 C 0.85044(19) 0.1392(2) -0.1083(3) 0.0657(16) Uani 1 1 d . . .
C24 C 0.8037(2) 0.1412(3) -0.1268(4) 0.088(2) Uani 1 1 d . . .
H24 H 0.791 0.1211 -0.1609 0.105 Uiso 1 1 calc R . .
C25 C 0.7756(3) 0.1754(3) -0.0912(6) 0.108(3) Uani 1 1 d . . .
H25 H 0.7438 0.1769 -0.1028 0.13 Uiso 1 1 calc R . .
O1 O 0.80221(19) 0.25717(17) 0.1077(3) 0.0834(14) Uani 1 1 d . . .
O2 O 0.7987(8) 0.2550(6) 0.2417(6) 0.258(8) Uani 1 1 d U . .
S1A S 0.8245(2) 0.2448(3) 0.1708(3) 0.148(3) Uiso 0.623(10) 1 d PD A 1
O3A O 0.8442(12) 0.1962(12) 0.1684(15) 0.280(12) Uiso 0.623(10) 1 d P A 1
C1T1 C 0.8817(19) 0.2696(9) 0.1703(13) 0.55(9) Uiso 0.623(10) 1 d PD A 1
F1A F 0.9066(7) 0.2450(6) 0.1200(9) 0.200(6) Uiso 0.623(10) 1 d PD A 1
F2A F 0.8904(13) 0.2557(9) 0.2392(17) 0.336(14) Uiso 0.623(10) 1 d PD A 1
F3A F 0.8838(14) 0.3176(12) 0.1618(14) 0.378(17) Uiso 0.623(10) 1 d PD A 1
S1B S 0.82057(18) 0.2741(2) 0.1749(3) 0.081(2) Uiso 0.377(10) 1 d PD A 2
O3B O 0.8138(8) 0.3241(9) 0.1847(12) 0.151(8) Uiso 0.377(10) 1 d P A 2
C1T2 C 0.8817(11) 0.2666(8) 0.1675(11) 0.133(11) Uiso 0.377(10) 1 d PD A 2
F1B F 0.8898(10) 0.2146(9) 0.1712(12) 0.196(9) Uiso 0.377(10) 1 d PD A 2
F2B F 0.9195(13) 0.2861(10) 0.2152(15) 0.261(14) Uiso 0.377(10) 1 d PD A 2
F3B F 0.9000(8) 0.2789(8) 0.0940(10) 0.160(7) Uiso 0.377(10) 1 d PD A 2



#----------------------------------------------------------------------------#
#                   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
Cu N1 2.033(4) 5_655 ?
Cu N1 2.033(4) . ?
Cu N2 2.040(4) . ?
Cu N2 2.040(4) 5_655 ?
N1 C15 1.304(8) . ?
N1 C11 1.364(8) . ?
C11 C12 1.378(10) . ?
C12 C13 1.382(10) . ?
C13 C14 1.405(9) . ?
C13 C23 1.489(8) 23_676 ?
C14 C15 1.420(9) . ?
N2 C25 1.277(10) . ?
N2 C21 1.292(11) . ?
C21 C22 1.439(10) . ?
C22 C23 1.372(9) . ?
C23 C24 1.378(9) . ?
C23 C13 1.489(8) 31_665 ?
C24 C25 1.426(9) . ?
O1 S1A 1.386(8) . ?
O1 S1B 1.446(7) . ?
O2 S1B 1.499(15) . ?
O2 S1A 1.545(16) . ?
S1A O3A 1.49(3) . ?
S1A C1T1 1.78(5) . ?
C1T1 F2A 1.37(3) . ?
C1T1 F1A 1.37(3) . ?
C1T1 F3A 1.38(3) . ?
S1B O3B 1.45(2) . ?
S1B C1T2 1.76(3) . ?
C1T2 F1B 1.50(2) . ?
C1T2 F2B 1.51(2) . ?
C1T2 F3B 1.51(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
N1 Cu N1 93.1(2) 5_655 . ?
N1 Cu N2 88.62(17) 5_655 . ?
N1 Cu N2 178.30(17) . . ?
N1 Cu N2 178.30(17) 5_655 5_655 ?
N1 Cu N2 88.62(17) . 5_655 ?
N2 Cu N2 89.7(2) . 5_655 ?
C15 N1 C11 119.1(5) . . ?
C15 N1 Cu 122.0(4) . . ?
C11 N1 Cu 118.7(4) . . ?
N1 C11 C12 119.0(7) . . ?
C11 C12 C13 122.5(6) . . ?
C12 C13 C14 117.8(5) . . ?
C12 C13 C23 121.6(6) . 23_676 ?
C14 C13 C23 120.6(6) . 23_676 ?
C13 C14 C15 116.2(7) . . ?
N1 C15 C14 124.4(6) . . ?
C25 N2 C21 119.8(5) . . ?
C25 N2 Cu 122.2(5) . . ?
C21 N2 Cu 117.9(4) . . ?
N2 C21 C22 121.9(7) . . ?
C23 C22 C21 118.3(8) . . ?
C22 C23 C24 118.9(6) . . ?
C22 C23 C13 119.5(6) . 31_665 ?
C24 C23 C13 121.6(5) . 31_665 ?
C23 C24 C25 117.0(7) . . ?
N2 C25 C24 124.2(7) . . ?
S1A O1 S1B 34.7(3) . . ?
S1B O2 S1A 32.3(4) . . ?
O1 S1A O3A 112.5(12) . . ?
O1 S1A O2 117.8(9) . . ?
O3A S1A O2 112.2(14) . . ?
O1 S1A C1T1 108.3(10) . . ?
O3A S1A C1T1 91.5(16) . . ?
O2 S1A C1T1 111.4(12) . . ?
F2A C1T1 F1A 114(2) . . ?
F2A C1T1 F3A 113(2) . . ?
F1A C1T1 F3A 114(2) . . ?
F2A C1T1 S1A 93(3) . . ?
F1A C1T1 S1A 106(3) . . ?
F3A C1T1 S1A 116(4) . . ?
O1 S1B O3B 113.0(10) . . ?
O1 S1B O2 117.0(9) . . ?
O3B S1B O2 101.4(12) . . ?
O1 S1B C1T2 104.4(8) . . ?
O3B S1B C1T2 105.2(12) . . ?
O2 S1B C1T2 115.6(11) . . ?
F1B C1T2 F2B 103.2(18) . . ?
F1B C1T2 F3B 102.6(17) . . ?
F2B C1T2 F3B 102.0(17) . . ?
F1B C1T2 S1B 105.5(18) . . ?
F2B C1T2 S1B 128(2) . . ?
F3B C1T2 S1B 112.6(17) . . ?
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1833573'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_REFNR01_4                   
;
PROBLEM: Ratio of reflections to parameters is < 10 for a
centrosymmetric structure
sine(theta)/lambda 0.5557
Proportion of unique data used 1.0000
Ratio reflections to parameters 8.8288
RESPONSE: The reflections to parameters ratio is low due to the 
number of refined parameters necessary to describe the disorder and the
weakly diffracting nature of the crystal at high angle.
;
_vrf_PLAT088_4                   
;
PROBLEM: Poor Data / Parameter Ratio .................... 8.87 Note
RESPONSE: see answer for REFNR01
;
_vrf_PLAT244_4                   
;
PROBLEM: Low  Solvent  Ueq as Compared to Neighbors of C33 Check
RESPONSE: This alert is a consequence of the relatively low quality of the 
diffraction data resulting in limitations of the structural model definition
;
_vrf_PLAT250_4                   
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.1 Note
RESPONSE: his alert is a consequence of the relatively low quality of the 
diffraction data resulting in limitations of the structural model definition
;
_vrf_PLAT341_4                   
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0112 Ang.
RESPONSE: This alert is a consequence of the relatively low quality of the 
diffraction data resulting in limitations of the structural model definition
;
_vrf_PLAT350_4                   
;
PROBLEM: Short C-H (X0.96,N1.08A) C22 - H22 .. 0.83 Ang.
RESPONSE:Despite the poor quality of the data,hydrogens 
have been located and their positions refined but with
low bond precision on C-H bonds
;
# end Validation Reply Form

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


_chemical_formula_sum            'C22 H20 F6 Fe N4 O8 S2'
_chemical_formula_moiety         '(C12  H12  N2  O8  F6  S2  Fe1),(C10 H8 N2)'
_chemical_formula_weight         702.39

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_Int_Tables_number      56
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.852(3)
_cell_length_b                   15.069(6)
_cell_length_c                   23.107(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2734.2(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2824
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      21.4
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_special_details           
;
 1500 frames were collected on a Brucker SMART CCD diffractometer with a 
 sample to detector distance of 60.00 mm. The counting time per frame 
 was 30 sec and the scan width per frame 0.5 deg. 
;

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

_exptl_absorpt_coefficient_mu    0.8
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sadabs 2.03 (Bruker AXS, 2002)'

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 CCD_plate
_diffrn_measurement_device       'Bruker smart apex ccd diffractometer'
_diffrn_measurement_method       omega-scan
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.041
_diffrn_reflns_number            21251
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_reflns_number_total             1960
_reflns_number_gt                1489
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_structure_solution    
'SIR 2014: C. Giacovazzo et all., J. Appl. Cryst.(2015) 48, 306'
_computing_structure_refinement  
'SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122'
_computing_molecular_graphics    
'VESTA 3: K. Momma and F. Izumi, J. Appl. Crystallogr.(2011),44,127'
_computing_publication_material  
'WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838'

#----------------------------------------------------------------------------#
#                   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)+(0.1354P)²+16.8495P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1960
_refine_ls_number_parameters     222
_refine_ls_number_restraints     40
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0804
_refine_ls_wR_factor_ref         0.2479
_refine_ls_wR_factor_gt          0.2179
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.02
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.122

#----------------------------------------------------------------------------#
#                   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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Fe Fe 0.3463 0.8444 '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
Fe Fe 0.75 0.25 0.38470(5) 0.0327(5) Uani 1 2 d S T P . .
O1W O 0.9336(7) 0.3488(3) 0.3873(2) 0.0455(13) Uani 1 1 d D . . . .
N1 N 0.75 0.25 0.4807(3) 0.0369(19) Uani 1 2 d S T P A .
C11 C 0.7852(12) 0.1779(5) 0.5113(3) 0.050(2) Uani 1 1 d . . . . .
C12 C 0.7854(12) 0.1747(5) 0.5704(3) 0.051(2) Uani 1 1 d . . . . .
C13 C 0.75 0.25 0.6026(4) 0.036(2) Uani 1 2 d S T P . .
N2 N 0.75 0.25 0.2879(3) 0.0367(19) Uani 1 2 d S T P A .
C21 C 0.8344(11) 0.3111(5) 0.2575(3) 0.0496(19) Uani 1 1 d . . . . .
C22 C 0.8365(11) 0.3131(5) 0.1982(3) 0.051(2) Uani 1 1 d . . . . .
C23 C 0.75 0.25 0.1665(4) 0.037(2) Uani 1 2 d S T P . .
N3 N 0.6258(9) 0.9771(4) 0.4143(3) 0.0560(18) Uani 1 1 d . . . . .
C31 C 0.6705(14) 0.9336(6) 0.4617(4) 0.067(3) Uani 1 1 d . . . . .
C32 C 0.7195(13) 0.8461(6) 0.4629(4) 0.066(3) Uani 1 1 d . . . . .
C33 C 0.7240(10) 0.7970(5) 0.4136(3) 0.0466(18) Uani 1 1 d . . . . .
C34 C 0.6765(15) 0.8407(6) 0.3639(4) 0.067(3) Uani 1 1 d . . . . .
C35 C 0.6286(15) 0.9286(6) 0.3665(4) 0.073(3) Uani 1 1 d . . . . .
S S 1.0834(3) 0.09829(15) 0.37879(9) 0.0587(7) Uani 1 1 d D . . . .
C1T C 1.1298(10) 0.0905(5) 0.3032(4) 0.067(2) Uani 1 1 d D U . . .
F1A F 1.1072(17) 0.1592(7) 0.2732(5) 0.089(4) Uiso 0.568(11) 1 d D . P A 1
F2A F 1.2837(14) 0.0589(9) 0.2922(6) 0.086(4) Uiso 0.568(11) 1 d D . P A 1
F3A F 1.0193(13) 0.0269(7) 0.2856(5) 0.087(4) Uiso 0.568(11) 1 d D . P A 1
F1B F 1.191(2) 0.1717(8) 0.2880(7) 0.089(5) Uiso 0.432(11) 1 d D . P A 2
F3B F 1.0047(16) 0.0846(10) 0.2650(6) 0.087(5) Uiso 0.432(11) 1 d D . P A 2
F2B F 1.245(2) 0.0277(11) 0.2931(8) 0.098(6) Uiso 0.432(11) 1 d D . P A 2
O1A O 0.9169(10) 0.1368(7) 0.3811(4) 0.038(3) Uiso 0.568(11) 1 d D . P A 1
O3A O 1.2052(14) 0.1687(7) 0.3936(5) 0.080(4) Uiso 0.568(11) 1 d D . P A 1
O2A O 1.1217(17) 0.0233(7) 0.4123(5) 0.089(4) Uiso 0.568(11) 1 d D . P A 1
O2B O 1.0161(18) 0.0073(6) 0.3795(7) 0.086(5) Uiso 0.432(11) 1 d D . P A 2
O3B O 1.2397(12) 0.1027(9) 0.4076(6) 0.068(5) Uiso 0.432(11) 1 d D . P A 2
O1B O 0.9566(15) 0.1623(8) 0.3874(6) 0.055(4) Uiso 0.432(11) 1 d D . P A 2
H11 H 0.811(11) 0.137(6) 0.498(4) 0.067 Uiso 1 1 d . U . . .
H12 H 0.799(12) 0.135(6) 0.585(4) 0.067 Uiso 1 1 d . U . . .
H21 H 0.906(10) 0.355(6) 0.281(4) 0.067 Uiso 1 1 d . U . . .
H22 H 0.894(11) 0.355(6) 0.185(4) 0.067 Uiso 1 1 d . U . . .
H31 H 0.656(11) 0.970(6) 0.487(4) 0.067 Uiso 1 1 d . U . . .
H32 H 0.752(10) 0.817(5) 0.496(4) 0.067 Uiso 1 1 d . U . . .
H34 H 0.593(11) 0.964(5) 0.334(4) 0.067 Uiso 1 1 d . U . . .
H35 H 0.662(10) 0.801(5) 0.327(4) 0.067 Uiso 1 1 d . U . . .
H1W H 1.030(9) 0.333(6) 0.396(4) 0.083 Uiso 1 1 d D U . . .
H2W H 0.914(13) 0.402(4) 0.391(4) 0.083 Uiso 1 1 d D 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
Fe O1W 2.073(5) 2_655 ?
Fe O1W 2.073(5) . ?
Fe O1B 2.094(8) 2_655 ?
Fe O1B 2.094(8) . ?
Fe O1A 2.153(7) . ?
Fe O1A 2.153(7) 2_655 ?
Fe N1 2.219(8) . ?
Fe N2 2.236(8) . ?
O1W H1W 0.82(6) . ?
O1W H2W 0.82(6) . ?
N1 C11 1.325(9) 2_655 ?
N1 C11 1.325(9) . ?
C11 C12 1.367(11) . ?
C11 H11 0.71(9) . ?
C12 C13 1.385(9) . ?
C12 H12 0.70(9) . ?
C13 C12 1.385(9) 2_655 ?
C13 C23 1.475(14) 7_756 ?
N2 C21 1.334(9) . ?
N2 C21 1.335(9) 2_655 ?
C21 C22 1.372(11) . ?
C21 H21 1.02(9) . ?
C22 C23 1.379(9) . ?
C22 H22 0.83(9) . ?
C23 C22 1.380(9) 2_655 ?
C23 C13 1.476(14) 7_755 ?
N3 C31 1.324(11) . ?
N3 C35 1.326(12) . ?
C31 C32 1.374(12) . ?
C31 H31 0.82(8) . ?
C32 C33 1.358(11) . ?
C32 H32 0.93(9) . ?
C33 C34 1.377(11) . ?
C33 C33 1.475(15) 2_665 ?
C34 C35 1.378(13) . ?
C34 H35 1.05(9) . ?
C35 H34 0.96(9) . ?
S O3B 1.397(8) . ?
S O1B 1.400(8) . ?
S O2A 1.402(8) . ?
S O1A 1.431(6) . ?
S O3A 1.470(8) . ?
S O2B 1.470(8) . ?
S C1T 1.787(10) . ?
C1T F1A 1.260(11) . ?
C1T F2A 1.323(11) . ?
C1T F3B 1.324(12) . ?
C1T F2B 1.328(12) . ?
C1T F3A 1.355(10) . ?
C1T F1B 1.361(12) . ?

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
O1W Fe O1W 176.6(3) 2_655 . ?
O1W Fe O1B 85.0(4) 2_655 2_655 ?
O1W Fe O1B 94.9(4) . 2_655 ?
O1W Fe O1B 94.9(4) 2_655 . ?
O1W Fe O1B 85.0(4) . . ?
O1B Fe O1B 176.6(8) 2_655 . ?
O1W Fe O1A 81.7(3) 2_655 . ?
O1W Fe O1A 98.4(3) . . ?
O1W Fe O1A 98.4(3) 2_655 2_655 ?
O1W Fe O1A 81.7(3) . 2_655 ?
O1A Fe O1A 175.6(5) . 2_655 ?
O1W Fe N1 88.32(15) 2_655 . ?
O1W Fe N1 88.32(15) . . ?
O1B Fe N1 88.3(4) 2_655 . ?
O1B Fe N1 88.3(4) . . ?
O1A Fe N1 92.2(2) . . ?
O1A Fe N1 92.2(2) 2_655 . ?
O1W Fe N2 91.68(15) 2_655 . ?
O1W Fe N2 91.68(15) . . ?
O1B Fe N2 91.7(4) 2_655 . ?
O1B Fe N2 91.7(4) . . ?
O1A Fe N2 87.8(2) . . ?
O1A Fe N2 87.8(2) 2_655 . ?
N1 Fe N2 180 . . ?
Fe O1W H1W 116(7) . . ?
Fe O1W H2W 125(7) . . ?
H1W O1W H2W 116(10) . . ?
C11 N1 C11 115.6(8) 2_655 . ?
C11 N1 Fe 122.2(4) 2_655 . ?
C11 N1 Fe 122.2(4) . . ?
N1 C11 C12 124.2(7) . . ?
N1 C11 H11 122(8) . . ?
C12 C11 H11 113(8) . . ?
C11 C12 C13 120.5(7) . . ?
C11 C12 H12 121(8) . . ?
C13 C12 H12 119(8) . . ?
C12 C13 C12 115.0(9) . 2_655 ?
C12 C13 C23 122.5(5) . 7_756 ?
C12 C13 C23 122.5(5) 2_655 7_756 ?
C21 N2 C21 116.5(9) . 2_655 ?
C21 N2 Fe 121.8(4) . . ?
C21 N2 Fe 121.8(4) 2_655 . ?
N2 C21 C22 123.2(7) . . ?
N2 C21 H21 116(5) . . ?
C22 C21 H21 120(5) . . ?
C21 C22 C23 120.6(7) . . ?
C21 C22 H22 112(6) . . ?
C23 C22 H22 127(6) . . ?
C22 C23 C22 115.9(9) . 2_655 ?
C22 C23 C13 122.1(5) . 7_755 ?
C22 C23 C13 122.1(5) 2_655 7_755 ?
C31 N3 C35 114.4(7) . . ?
N3 C31 C32 124.5(8) . . ?
N3 C31 H31 103(6) . . ?
C32 C31 H31 132(6) . . ?
C33 C32 C31 120.9(8) . . ?
C33 C32 H32 116(5) . . ?
C31 C32 H32 123(5) . . ?
C32 C33 C34 115.6(8) . . ?
C32 C33 C33 122.0(5) . 2_665 ?
C34 C33 C33 122.3(5) . 2_665 ?
C33 C34 C35 119.8(8) . . ?
C33 C34 H35 116(4) . . ?
C35 C34 H35 123(4) . . ?
N3 C35 C34 124.8(8) . . ?
N3 C35 H34 110(5) . . ?
C34 C35 H34 125(5) . . ?
O3B S O1B 121.6(7) . . ?
O2A S O1A 120.1(7) . . ?
O2A S O3A 108.3(7) . . ?
O1A S O3A 107.1(7) . . ?
O3B S O2B 110.8(7) . . ?
O1B S O2B 112.7(7) . . ?
O3B S C1T 106.8(7) . . ?
O1B S C1T 109.2(7) . . ?
O2A S C1T 116.2(6) . . ?
O1A S C1T 104.4(5) . . ?
O3A S C1T 98.2(6) . . ?
O2B S C1T 91.3(7) . . ?
F1A C1T F2A 108.6(10) . . ?
F3B C1T F2B 109.8(12) . . ?
F1A C1T F3A 109.0(10) . . ?
F2A C1T F3A 105.8(9) . . ?
F3B C1T F1B 98.6(11) . . ?
F2B C1T F1B 110.7(12) . . ?
F1A C1T S 117.1(8) . . ?
F2A C1T S 113.4(8) . . ?
F3B C1T S 120.3(8) . . ?
F2B C1T S 111.0(10) . . ?
F3A C1T S 102.1(7) . . ?
F1B C1T S 105.4(8) . . ?
S O1A Fe 151.5(7) . . ?
S O1B Fe 169.0(10) . . ?


# END of CIF




