# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_anx_em1b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H38 Cl3 N O7'
_chemical_formula_weight         691.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4484(2)
_cell_length_b                   12.9132(2)
_cell_length_c                   14.4521(3)
_cell_angle_alpha                105.509(2)
_cell_angle_beta                 110.788(2)
_cell_angle_gamma                101.371(2)
_cell_volume                     1661.71(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    15588
_cell_measurement_theta_min      3.4980
_cell_measurement_theta_max      76.5070

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             724
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3674
_exptl_absorpt_correction_T_max  0.6692
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector_area_resol_mean 5.1725
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18060
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         76.67
_reflns_number_total             6656
_reflns_number_gt                6453
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6656
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.2795
_refine_ls_wR_factor_gt          0.2765
_refine_ls_goodness_of_fit_ref   2.637
_refine_ls_restrained_S_all      2.637
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl50 Cl -0.95318(12) 0.11605(9) -0.38494(13) 0.0810(5) Uani 1 1 d . . .
Cl51 Cl -1.02869(8) 0.29162(6) -0.45946(6) 0.0450(3) Uani 1 1 d . . .
Cl52 Cl -0.75540(9) 0.34933(12) -0.28527(9) 0.0767(4) Uani 1 1 d . . .
O1 O -1.50159(16) 0.28627(13) -0.40003(12) 0.0191(4) Uani 1 1 d . . .
O2 O -0.91339(16) 0.60728(14) -0.33923(11) 0.0186(4) Uani 1 1 d . . .
O3 O -0.51820(16) 0.60358(13) -0.14573(13) 0.0195(4) Uani 1 1 d . . .
O4 O -0.27561(16) 0.36522(13) -0.00958(13) 0.0198(4) Uani 1 1 d . . .
O5 O 0.0823(2) 0.75299(17) 0.19834(15) 0.0356(5) Uani 1 1 d . . .
H5 H 0.1573 0.8100 0.2347 0.043 Uiso 1 1 calc R . .
O6 O -0.60396(17) 0.06744(13) -0.06902(12) 0.0199(4) Uani 1 1 d . . .
O7 O -1.28266(17) -0.14469(13) -0.25507(13) 0.0208(4) Uani 1 1 d . . .
N1 N -1.35220(19) 0.07727(15) -0.32835(14) 0.0160(4) Uani 1 1 d . . .
C1 C -1.6440(2) -0.0474(2) -0.42295(17) 0.0221(5) Uani 1 1 d . . .
H1 H -1.7440 -0.0899 -0.4543 0.027 Uiso 1 1 calc R . .
C2 C -1.6004(2) 0.06818(19) -0.40467(17) 0.0198(5) Uani 1 1 d . . .
H2 H -1.6697 0.1056 -0.4238 0.024 Uiso 1 1 calc R . .
C3 C -1.4530(2) 0.12738(18) -0.35773(16) 0.0160(4) Uani 1 1 d . . .
C4 C -1.3934(2) 0.25118(18) -0.33667(17) 0.0181(4) Uani 1 1 d . . .
H4A H -1.3603 0.2962 -0.2604 0.022 Uiso 1 1 calc R . .
H4B H -1.3091 0.2645 -0.3536 0.022 Uiso 1 1 calc R . .
C5 C -1.4649(2) 0.40821(19) -0.36322(18) 0.0197(5) Uani 1 1 d . . .
H5A H -1.4660 0.4361 -0.2928 0.024 Uiso 1 1 calc R . .
H5B H -1.5395 0.4285 -0.4132 0.024 Uiso 1 1 calc R . .
C6 C -1.3189(2) 0.46699(18) -0.35392(17) 0.0169(4) Uani 1 1 d . . .
C7 C -1.2989(2) 0.46723(18) -0.44431(16) 0.0175(4) Uani 1 1 d . . .
H7 H -1.3798 0.4332 -0.5121 0.021 Uiso 1 1 calc R . .
C8 C -1.1629(2) 0.51629(19) -0.43735(16) 0.0180(4) Uani 1 1 d . . .
H8 H -1.1516 0.5170 -0.4996 0.022 Uiso 1 1 calc R . .
C9 C -1.0429(2) 0.56455(18) -0.33777(16) 0.0167(4) Uani 1 1 d . . .
C10 C -1.0602(2) 0.56597(18) -0.24658(16) 0.0163(4) Uani 1 1 d . . .
H10 H -0.9794 0.5999 -0.1788 0.020 Uiso 1 1 calc R . .
C11 C -1.1980(2) 0.51685(18) -0.25591(16) 0.0173(4) Uani 1 1 d . . .
H11 H -1.2096 0.5175 -0.1935 0.021 Uiso 1 1 calc R . .
C12 C -0.7859(2) 0.6465(2) -0.24041(16) 0.0185(4) Uani 1 1 d . . .
H12A H -0.7826 0.5866 -0.2096 0.022 Uiso 1 1 calc R . .
H12B H -0.7854 0.7147 -0.1886 0.022 Uiso 1 1 calc R . .
C13 C -0.6578(2) 0.6746(2) -0.26593(17) 0.0208(5) Uani 1 1 d . . .
H13A H -0.6577 0.7397 -0.2897 0.025 Uiso 1 1 calc R . .
H13B H -0.6680 0.6087 -0.3253 0.025 Uiso 1 1 calc R . .
C14 C -0.5143(2) 0.70390(19) -0.17084(17) 0.0183(4) Uani 1 1 d . . .
H14A H -0.4325 0.7252 -0.1890 0.022 Uiso 1 1 calc R . .
H14B H -0.5031 0.7681 -0.1096 0.022 Uiso 1 1 calc R . .
C15 C -0.3905(2) 0.59594(18) -0.07986(15) 0.0159(4) Uani 1 1 d . . .
C16 C -0.4009(2) 0.48863(18) -0.07496(16) 0.0166(4) Uani 1 1 d . . .
H16 H -0.4913 0.4293 -0.1124 0.020 Uiso 1 1 calc R . .
C17 C -0.2780(2) 0.46918(18) -0.01491(16) 0.0164(4) Uani 1 1 d . . .
C18 C -0.1450(2) 0.5581(2) 0.04328(17) 0.0208(5) Uani 1 1 d . . .
H18 H -0.0605 0.5448 0.0842 0.025 Uiso 1 1 calc R . .
C19 C -0.1390(2) 0.66515(19) 0.04017(17) 0.0197(5) Uani 1 1 d . . .
C20 C -0.2615(2) 0.68538(18) -0.02186(16) 0.0173(4) Uani 1 1 d . . .
H20 H -0.2564 0.7588 -0.0242 0.021 Uiso 1 1 calc R . .
C21 C 0.0028(3) 0.7625(2) 0.1022(2) 0.0279(5) Uani 1 1 d . . .
H21A H 0.0593 0.7611 0.0598 0.033 Uiso 1 1 calc R . .
H21B H -0.0167 0.8357 0.1164 0.033 Uiso 1 1 calc R . .
C22 C -0.4110(2) 0.27365(18) -0.06899(17) 0.0173(4) Uani 1 1 d . . .
H22A H -0.4555 0.2694 -0.1435 0.021 Uiso 1 1 calc R . .
H22B H -0.4787 0.2867 -0.0370 0.021 Uiso 1 1 calc R . .
C23 C -0.3817(2) 0.16401(19) -0.06650(17) 0.0200(5) Uani 1 1 d . . .
H23A H -0.3375 0.1690 0.0082 0.024 Uiso 1 1 calc R . .
H23B H -0.3120 0.1528 -0.0970 0.024 Uiso 1 1 calc R . .
C24 C -0.5197(2) 0.06347(19) -0.12904(17) 0.0211(5) Uani 1 1 d . . .
H24A H -0.5751 0.0668 -0.1991 0.025 Uiso 1 1 calc R . .
H24B H -0.4965 -0.0083 -0.1411 0.025 Uiso 1 1 calc R . .
C25 C -0.7430(2) -0.00503(18) -0.11821(17) 0.0182(4) Uani 1 1 d . . .
C26 C -0.8129(3) -0.01118(19) -0.05173(18) 0.0203(5) Uani 1 1 d . . .
H26 H -0.7628 0.0326 0.0224 0.024 Uiso 1 1 calc R . .
C27 C -0.9542(3) -0.08080(19) -0.09417(19) 0.0205(5) Uani 1 1 d . . .
H27 H -0.9997 -0.0853 -0.0483 0.025 Uiso 1 1 calc R . .
C28 C -1.0326(2) -0.14542(18) -0.20413(19) 0.0197(5) Uani 1 1 d . . .
C29 C -0.9605(2) -0.1400(2) -0.26819(19) 0.0217(5) Uani 1 1 d . . .
H29 H -1.0105 -0.1839 -0.3423 0.026 Uiso 1 1 calc R . .
C30 C -0.8162(2) -0.0714(2) -0.22625(18) 0.0207(5) Uani 1 1 d . . .
H30 H -0.7686 -0.0703 -0.2713 0.025 Uiso 1 1 calc R . .
C31 C -1.1889(3) -0.2139(2) -0.2490(2) 0.0239(5) Uani 1 1 d . . .
H31A H -1.2185 -0.2691 -0.3213 0.029 Uiso 1 1 calc R . .
H31B H -1.2010 -0.2574 -0.2040 0.029 Uiso 1 1 calc R . .
C32 C -1.2767(2) -0.08723(19) -0.32521(18) 0.0214(5) Uani 1 1 d . . .
H32A H -1.2874 -0.1415 -0.3926 0.026 Uiso 1 1 calc R . .
H32B H -1.1815 -0.0273 -0.2927 0.026 Uiso 1 1 calc R . .
C33 C -1.3949(2) -0.03464(18) -0.34806(17) 0.0177(4) Uani 1 1 d . . .
C34 C -1.5407(2) -0.10000(19) -0.39519(17) 0.0201(5) Uani 1 1 d . . .
H34 H -1.5684 -0.1790 -0.4080 0.024 Uiso 1 1 calc R . .
C50 C -0.9357(3) 0.2601(3) -0.3472(2) 0.0374(6) Uani 1 1 d . . .
H50 H -0.9799 0.2781 -0.2963 0.045 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl50 C50 1.745(3) . ?
Cl51 C50 1.770(3) . ?
Cl52 C50 1.753(3) . ?
O1 C4 1.418(2) . ?
O1 C5 1.442(3) . ?
O2 C9 1.367(2) . ?
O2 C12 1.438(2) . ?
O3 C15 1.377(2) . ?
O3 C14 1.433(3) . ?
O4 C17 1.370(3) . ?
O4 C22 1.439(2) . ?
O5 C21 1.396(3) . ?
O6 C25 1.367(3) . ?
O6 C24 1.438(2) . ?
O7 C32 1.418(3) . ?
O7 C31 1.447(2) . ?
N1 C33 1.343(3) . ?
N1 C3 1.344(3) . ?
C1 C34 1.383(3) . ?
C1 C2 1.394(3) . ?
C2 C3 1.390(3) . ?
C3 C4 1.500(3) . ?
C5 C6 1.505(3) . ?
C6 C11 1.392(3) . ?
C6 C7 1.395(3) . ?
C7 C8 1.393(3) . ?
C8 C9 1.401(3) . ?
C9 C10 1.388(3) . ?
C10 C11 1.396(3) . ?
C12 C13 1.513(3) . ?
C13 C14 1.522(3) . ?
C15 C20 1.386(3) . ?
C15 C16 1.391(3) . ?
C16 C17 1.385(3) . ?
C17 C18 1.407(3) . ?
C18 C19 1.385(3) . ?
C19 C20 1.397(3) . ?
C19 C21 1.517(3) . ?
C22 C23 1.513(3) . ?
C23 C24 1.514(3) . ?
C25 C30 1.391(3) . ?
C25 C26 1.406(3) . ?
C26 C27 1.379(3) . ?
C27 C28 1.411(3) . ?
C28 C29 1.392(3) . ?
C28 C31 1.497(3) . ?
C29 C30 1.401(3) . ?
C32 C33 1.502(3) . ?
C33 C34 1.395(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
C4 O1 C5 112.08(16) . . ?
C9 O2 C12 116.86(15) . . ?
C15 O3 C14 118.45(16) . . ?
C17 O4 C22 116.50(15) . . ?
C25 O6 C24 117.89(16) . . ?
C32 O7 C31 110.91(16) . . ?
C33 N1 C3 119.02(19) . . ?
C34 C1 C2 119.6(2) . . ?
C3 C2 C1 118.4(2) . . ?
N1 C3 C2 122.28(19) . . ?
N1 C3 C4 114.54(18) . . ?
C2 C3 C4 123.18(18) . . ?
O1 C4 C3 109.80(17) . . ?
O1 C5 C6 113.08(17) . . ?
C11 C6 C7 117.87(19) . . ?
C11 C6 C5 121.20(19) . . ?
C7 C6 C5 120.8(2) . . ?
C8 C7 C6 121.41(19) . . ?
C7 C8 C9 119.43(19) . . ?
O2 C9 C10 124.57(18) . . ?
O2 C9 C8 115.24(18) . . ?
C10 C9 C8 120.19(19) . . ?
C9 C10 C11 119.10(19) . . ?
C6 C11 C10 121.97(18) . . ?
O2 C12 C13 106.51(16) . . ?
C12 C13 C14 112.41(17) . . ?
O3 C14 C13 105.96(17) . . ?
O3 C15 C20 124.50(19) . . ?
O3 C15 C16 114.01(18) . . ?
C20 C15 C16 121.49(19) . . ?
C17 C16 C15 119.32(19) . . ?
O4 C17 C16 123.66(19) . . ?
O4 C17 C18 116.05(18) . . ?
C16 C17 C18 120.28(19) . . ?
C19 C18 C17 119.17(19) . . ?
C18 C19 C20 121.1(2) . . ?
C18 C19 C21 120.29(19) . . ?
C20 C19 C21 118.6(2) . . ?
C15 C20 C19 118.55(19) . . ?
O5 C21 C19 109.86(19) . . ?
O4 C22 C23 108.30(16) . . ?
C22 C23 C24 111.16(17) . . ?
O6 C24 C23 108.30(17) . . ?
O6 C25 C30 124.77(18) . . ?
O6 C25 C26 115.6(2) . . ?
C30 C25 C26 119.6(2) . . ?
C27 C26 C25 120.0(2) . . ?
C26 C27 C28 121.48(19) . . ?
C29 C28 C27 117.6(2) . . ?
C29 C28 C31 122.1(2) . . ?
C27 C28 C31 120.29(19) . . ?
C28 C29 C30 121.7(2) . . ?
C25 C30 C29 119.53(19) . . ?
O7 C31 C28 112.87(18) . . ?
O7 C32 C33 110.54(17) . . ?
N1 C33 C34 122.11(19) . . ?
N1 C33 C32 115.91(19) . . ?
C34 C33 C32 121.8(2) . . ?
C1 C34 C33 118.6(2) . . ?
Cl50 C50 Cl52 113.25(18) . . ?
Cl50 C50 Cl51 110.39(18) . . ?
Cl52 C50 Cl51 107.80(16) . . ?

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        76.67
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.090
_database_code_depnum_ccdc_archive 'CCDC 1002573'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_em1agtfr

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H82 Ag2 F6 N2 O22 S2'
_chemical_formula_weight         1721.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0298(7)
_cell_length_b                   12.4731(10)
_cell_length_c                   15.6946(12)
_cell_angle_alpha                87.500(4)
_cell_angle_beta                 72.011(4)
_cell_angle_gamma                67.114(4)
_cell_volume                     1884.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    89(2)
_cell_measurement_reflns_used    4931
_cell_measurement_theta_min      2.741
_cell_measurement_theta_max      25.4455

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8786
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      89(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34942
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         26.43
_reflns_number_total             7687
_reflns_number_gt                5673
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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)+(0.0508P)²+0.2713P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7687
_refine_ls_number_parameters     487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.28412(2) 0.12853(2) 0.333034(18) 0.02499(10) Uani 1 1 d . . .
O7 O 0.1767(2) 0.1685(2) 0.22510(16) 0.0227(6) Uani 1 1 d . . .
C35 C 0.0306(4) 0.3154(3) 0.5085(2) 0.0288(9) Uani 1 1 d . . .
H35A H 0.1154 0.2984 0.5241 0.043 Uiso 1 1 calc R . .
H35B H -0.0436 0.3146 0.5622 0.043 Uiso 1 1 calc R . .
H35C H 0.0026 0.3925 0.4854 0.043 Uiso 1 1 calc R . .
O2 O 0.3719(2) 0.28475(18) 0.38687(15) 0.0188(5) Uani 1 1 d . . .
C6 C 0.1876(3) 0.4528(3) 0.1725(2) 0.0178(7) Uani 1 1 d . . .
H6 H 0.1064 0.4585 0.1600 0.021 Uiso 1 1 calc R . .
O1 O 0.3046(2) 0.47107(19) 0.01649(15) 0.0207(5) Uani 1 1 d . . .
O6 O 0.6869(2) -0.2221(2) 0.12060(17) 0.0298(6) Uani 1 1 d . . .
O5 O 0.3195(2) -0.1610(2) -0.09030(17) 0.0281(6) Uani 1 1 d . . .
O4 O 0.0813(2) -0.13937(19) 0.11524(16) 0.0244(6) Uani 1 1 d . . .
O3 O 0.2972(2) -0.06219(19) 0.42860(15) 0.0216(5) Uani 1 1 d . . .
O8 O 0.0561(3) 0.2292(2) 0.44152(18) 0.0316(6) Uani 1 1 d . . .
N1 N 0.4857(3) 0.0398(2) 0.35846(18) 0.0182(6) Uani 1 1 d . . .
C2 C 0.4163(3) 0.4550(3) 0.1236(2) 0.0184(7) Uani 1 1 d . . .
H2 H 0.4919 0.4611 0.0771 0.022 Uiso 1 1 calc R . .
C13 C 0.5287(3) -0.0713(3) 0.3804(2) 0.0200(7) Uani 1 1 d . . .
C12 C 0.6527(4) -0.1260(3) 0.3986(3) 0.0297(9) Uani 1 1 d . . .
H12 H 0.6799 -0.2042 0.4148 0.036 Uiso 1 1 calc R . .
C11 C 0.7357(3) -0.0666(3) 0.3931(3) 0.0300(9) Uani 1 1 d . . .
H11 H 0.8229 -0.1041 0.4029 0.036 Uiso 1 1 calc R . .
C10 C 0.6913(3) 0.0489(3) 0.3732(2) 0.0237(8) Uani 1 1 d . . .
H10 H 0.7463 0.0924 0.3707 0.028 Uiso 1 1 calc R . .
C9 C 0.5652(3) 0.0997(3) 0.3572(2) 0.0189(7) Uani 1 1 d . . .
C8 C 0.5145(3) 0.2239(3) 0.3340(2) 0.0231(8) Uani 1 1 d . . .
H8A H 0.5715 0.2625 0.3461 0.028 Uiso 1 1 calc R . .
H8B H 0.5236 0.2258 0.2692 0.028 Uiso 1 1 calc R . .
C7 C 0.3227(3) 0.4071(3) 0.3726(2) 0.0211(8) Uani 1 1 d . . .
H7A H 0.3863 0.4395 0.3832 0.025 Uiso 1 1 calc R . .
H7B H 0.2301 0.4482 0.4173 0.025 Uiso 1 1 calc R . .
C4 C 0.3125(3) 0.4308(3) 0.2796(2) 0.0176(7) Uani 1 1 d . . .
C3 C 0.4217(3) 0.4413(3) 0.2108(2) 0.0195(7) Uani 1 1 d . . .
H3 H 0.5013 0.4391 0.2238 0.023 Uiso 1 1 calc R . .
C1 C 0.2988(3) 0.4599(3) 0.1052(2) 0.0174(7) Uani 1 1 d . . .
C5 C 0.1967(3) 0.4371(3) 0.2587(2) 0.0195(7) Uani 1 1 d . . .
H5 H 0.1211 0.4305 0.3049 0.023 Uiso 1 1 calc R . .
C27 C 0.7989(3) -0.4539(3) 0.0120(2) 0.0213(8) Uani 1 1 d . . .
H27A H 0.8211 -0.3894 -0.0180 0.026 Uiso 1 1 calc R . .
H27B H 0.8850 -0.5258 -0.0028 0.026 Uiso 1 1 calc R . .
C28 C 0.7375(3) -0.4243(3) 0.1125(2) 0.0238(8) Uani 1 1 d . . .
H28A H 0.8109 -0.4275 0.1375 0.029 Uiso 1 1 calc R . .
H28B H 0.7007 -0.4827 0.1404 0.029 Uiso 1 1 calc R . .
C29 C 0.6215(4) -0.3033(3) 0.1355(2) 0.0256(8) Uani 1 1 d . . .
H29A H 0.5623 -0.2904 0.0966 0.031 Uiso 1 1 calc R . .
H29B H 0.5629 -0.2941 0.1991 0.031 Uiso 1 1 calc R . .
C30 C 0.6086(3) -0.1053(3) 0.1199(2) 0.0223(8) Uani 1 1 d . . .
C26 C 0.3175(3) 0.0350(3) -0.1094(2) 0.0226(8) Uani 1 1 d . . .
H26 H 0.2225 0.0680 -0.1062 0.027 Uiso 1 1 calc R . .
C25 C 0.3831(3) -0.0840(3) -0.1037(2) 0.0219(8) Uani 1 1 d . . .
C24 C 0.1731(3) -0.1155(3) -0.0738(3) 0.0260(8) Uani 1 1 d . . .
H24A H 0.1515 -0.0949 -0.1305 0.031 Uiso 1 1 calc R . .
H24B H 0.1263 -0.0445 -0.0312 0.031 Uiso 1 1 calc R . .
C23 C 0.1245(3) -0.2102(3) -0.0341(2) 0.0245(8) Uani 1 1 d . . .
H23A H 0.0236 -0.1828 -0.0240 0.029 Uiso 1 1 calc R . .
H23B H 0.1722 -0.2803 -0.0776 0.029 Uiso 1 1 calc R . .
C22 C 0.1527(4) -0.2431(3) 0.0534(2) 0.0254(8) Uani 1 1 d . . .
H22A H 0.1186 -0.3044 0.0778 0.031 Uiso 1 1 calc R . .
H22B H 0.2537 -0.2738 0.0440 0.031 Uiso 1 1 calc R . .
C20 C 0.1142(3) -0.1433(3) 0.1929(2) 0.0217(8) Uani 1 1 d . . .
C18 C 0.0559(3) -0.0380(3) 0.2459(2) 0.0213(8) Uani 1 1 d . . .
H18 H -0.0042 0.0304 0.2278 0.026 Uiso 1 1 calc R . .
C17 C 0.0850(3) -0.0325(3) 0.3247(2) 0.0216(8) Uani 1 1 d . . .
H17 H 0.0441 0.0400 0.3602 0.026 Uiso 1 1 calc R . .
C16 C 0.1724(3) -0.1303(3) 0.3534(2) 0.0200(7) Uani 1 1 d . . .
C15 C 0.2041(3) -0.1203(3) 0.4386(2) 0.0243(8) Uani 1 1 d . . .
H15A H 0.1163 -0.0765 0.4868 0.029 Uiso 1 1 calc R . .
H15B H 0.2460 -0.1995 0.4574 0.029 Uiso 1 1 calc R . .
C14 C 0.4368(3) -0.1350(3) 0.3818(3) 0.0260(8) Uani 1 1 d . . .
H14A H 0.4456 -0.1562 0.3194 0.031 Uiso 1 1 calc R . .
H14B H 0.4657 -0.2079 0.4118 0.031 Uiso 1 1 calc R . .
C19 C 0.2285(3) -0.2353(3) 0.3004(2) 0.0249(8) Uani 1 1 d . . .
H19 H 0.2881 -0.3035 0.3190 0.030 Uiso 1 1 calc R . .
C21 C 0.2004(3) -0.2438(3) 0.2216(2) 0.0257(8) Uani 1 1 d . . .
H21 H 0.2391 -0.3168 0.1872 0.031 Uiso 1 1 calc R . .
C33 C 0.4764(3) 0.1331(3) 0.1113(2) 0.0205(8) Uani 1 1 d . . .
H33 H 0.4314 0.2147 0.1078 0.025 Uiso 1 1 calc R . .
C32 C 0.4031(3) 0.0622(3) 0.1239(2) 0.0199(7) Uani 1 1 d . . .
C34 C 0.2508(3) 0.1179(3) 0.1341(2) 0.0215(8) Uani 1 1 d . . .
H34A H 0.2338 0.1791 0.0917 0.026 Uiso 1 1 calc R . .
H34B H 0.2190 0.0585 0.1205 0.026 Uiso 1 1 calc R . .
C31 C 0.4685(3) -0.0583(3) 0.1285(2) 0.0215(8) Uani 1 1 d . . .
H31 H 0.4179 -0.1067 0.1374 0.026 Uiso 1 1 calc R . .
S1 S 0.81399(8) 0.36255(8) 0.30366(6) 0.0209(2) Uani 1 1 d . . .
O12 O 0.9392(2) 0.3662(2) 0.24157(16) 0.0246(6) Uani 1 1 d . . .
O10 O 0.8362(2) 0.2811(2) 0.37163(17) 0.0319(6) Uani 1 1 d . . .
O11 O 0.7143(2) 0.3622(2) 0.26306(18) 0.0368(7) Uani 1 1 d . . .
C36 C 0.7328(4) 0.5038(4) 0.3685(3) 0.0390(10) Uani 1 1 d . . .
F3 F 0.8171(3) 0.5204(2) 0.40720(16) 0.0545(7) Uani 1 1 d . . .
F1 F 0.7004(3) 0.5918(2) 0.31637(16) 0.0581(8) Uani 1 1 d . . .
F2 F 0.6169(3) 0.5143(3) 0.43281(17) 0.0747(9) Uani 1 1 d . . .
H100 H -0.009(4) 0.252(4) 0.422(3) 0.039(12) Uiso 1 1 d . . .
H101 H 0.107(4) 0.225(4) 0.228(3) 0.053(14) Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Ag1 N1 2.219(3) . ?
Ag1 O7 2.287(2) . ?
Ag1 O8 2.426(2) . ?
O7 C34 1.437(4) . ?
O7 H101 0.81(4) . ?
C35 O8 1.422(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
O2 C8 1.435(4) . ?
O2 C7 1.440(4) . ?
C6 C1 1.381(4) . ?
C6 C5 1.387(4) . ?
C6 H6 0.9500 . ?
O1 C1 1.377(4) . ?
O1 C27 1.436(4) 2_655 ?
O6 C30 1.376(4) . ?
O6 C29 1.430(4) . ?
O5 C25 1.369(4) . ?
O5 C24 1.428(4) . ?
O4 C20 1.369(4) . ?
O4 C22 1.443(4) . ?
O3 C14 1.417(4) . ?
O3 C15 1.440(4) . ?
O8 H100 0.81(4) . ?
N1 C13 1.346(4) . ?
N1 C9 1.351(4) . ?
C2 C3 1.389(4) . ?
C2 C1 1.391(4) . ?
C2 H2 0.9500 . ?
C13 C12 1.385(5) . ?
C13 C14 1.507(4) . ?
C12 C11 1.367(5) . ?
C12 H12 0.9500 . ?
C11 C10 1.386(5) . ?
C11 H11 0.9500 . ?
C10 C9 1.385(4) . ?
C10 H10 0.9500 . ?
C9 C8 1.499(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 C4 1.507(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C4 C5 1.387(4) . ?
C4 C3 1.394(4) . ?
C3 H3 0.9500 . ?
C5 H5 0.9500 . ?
C27 O1 1.436(4) 2_655 ?
C27 C28 1.510(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.518(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.387(4) . ?
C30 C26 1.387(5) 2_655 ?
C26 C25 1.388(5) . ?
C26 C30 1.387(5) 2_655 ?
C26 H26 0.9500 . ?
C25 C33 1.394(4) 2_655 ?
C24 C23 1.514(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C23 C22 1.506(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C20 C18 1.392(5) . ?
C20 C21 1.402(5) . ?
C18 C17 1.381(5) . ?
C18 H18 0.9500 . ?
C17 C16 1.387(5) . ?
C17 H17 0.9500 . ?
C16 C19 1.393(5) . ?
C16 C15 1.505(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C19 C21 1.382(5) . ?
C19 H19 0.9500 . ?
C21 H21 0.9500 . ?
C33 C32 1.385(4) . ?
C33 C25 1.394(4) 2_655 ?
C33 H33 0.9500 . ?
C32 C31 1.401(5) . ?
C32 C34 1.505(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C31 H31 0.9500 . ?
S1 O11 1.433(2) . ?
S1 O12 1.440(2) . ?
S1 O10 1.450(2) . ?
S1 C36 1.819(4) . ?
C36 F2 1.325(4) . ?
C36 F3 1.337(5) . ?
C36 F1 1.341(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ag1 O7 144.69(9) . . ?
N1 Ag1 O8 128.29(9) . . ?
O7 Ag1 O8 86.97(9) . . ?
C34 O7 Ag1 121.07(19) . . ?
C34 O7 H101 111(3) . . ?
Ag1 O7 H101 125(3) . . ?
O8 C35 H35A 109.5 . . ?
O8 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O8 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C8 O2 C7 111.3(2) . . ?
C1 C6 C5 118.7(3) . . ?
C1 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
C1 O1 C27 118.6(2) . 2_655 ?
C30 O6 C29 119.5(3) . . ?
C25 O5 C24 118.2(3) . . ?
C20 O4 C22 117.5(3) . . ?
C14 O3 C15 112.6(2) . . ?
C35 O8 Ag1 122.0(2) . . ?
C35 O8 H100 108(3) . . ?
Ag1 O8 H100 116(3) . . ?
C13 N1 C9 118.2(3) . . ?
C13 N1 Ag1 121.9(2) . . ?
C9 N1 Ag1 119.8(2) . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
N1 C13 C12 122.1(3) . . ?
N1 C13 C14 116.6(3) . . ?
C12 C13 C14 121.3(3) . . ?
C11 C12 C13 119.4(3) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C12 C11 C10 119.4(3) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C10 C9 118.6(3) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
N1 C9 C10 122.3(3) . . ?
N1 C9 C8 117.4(3) . . ?
C10 C9 C8 120.2(3) . . ?
O2 C8 C9 109.5(3) . . ?
O2 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
O2 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
O2 C7 C4 113.4(3) . . ?
O2 C7 H7A 108.9 . . ?
C4 C7 H7A 108.9 . . ?
O2 C7 H7B 108.9 . . ?
C4 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C5 C4 C3 117.9(3) . . ?
C5 C4 C7 121.0(3) . . ?
C3 C4 C7 121.1(3) . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
O1 C1 C6 124.2(3) . . ?
O1 C1 C2 114.9(3) . . ?
C6 C1 C2 120.9(3) . . ?
C4 C5 C6 122.2(3) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
O1 C27 C28 106.2(3) 2_655 . ?
O1 C27 H27A 110.5 2_655 . ?
C28 C27 H27A 110.5 . . ?
O1 C27 H27B 110.5 2_655 . ?
C28 C27 H27B 110.5 . . ?
H27A C27 H27B 108.7 . . ?
C27 C28 C29 111.1(3) . . ?
C27 C28 H28A 109.4 . . ?
C29 C28 H28A 109.4 . . ?
C27 C28 H28B 109.4 . . ?
C29 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
O6 C29 C28 106.4(3) . . ?
O6 C29 H29A 110.4 . . ?
C28 C29 H29A 110.4 . . ?
O6 C29 H29B 110.4 . . ?
C28 C29 H29B 110.4 . . ?
H29A C29 H29B 108.6 . . ?
O6 C30 C31 125.0(3) . . ?
O6 C30 C26 113.9(3) . 2_655 ?
C31 C30 C26 121.1(3) . 2_655 ?
C25 C26 C30 119.6(3) . 2_655 ?
C25 C26 H26 120.2 . . ?
C30 C26 H26 120.2 2_655 . ?
O5 C25 C26 124.7(3) . . ?
O5 C25 C33 115.1(3) . 2_655 ?
C26 C25 C33 120.3(3) . 2_655 ?
O5 C24 C23 106.9(3) . . ?
O5 C24 H24A 110.3 . . ?
C23 C24 H24A 110.3 . . ?
O5 C24 H24B 110.3 . . ?
C23 C24 H24B 110.3 . . ?
H24A C24 H24B 108.6 . . ?
C22 C23 C24 112.3(3) . . ?
C22 C23 H23A 109.1 . . ?
C24 C23 H23A 109.1 . . ?
C22 C23 H23B 109.1 . . ?
C24 C23 H23B 109.1 . . ?
H23A C23 H23B 107.9 . . ?
O4 C22 C23 107.6(3) . . ?
O4 C22 H22A 110.2 . . ?
C23 C22 H22A 110.2 . . ?
O4 C22 H22B 110.2 . . ?
C23 C22 H22B 110.2 . . ?
H22A C22 H22B 108.5 . . ?
O4 C20 C18 115.9(3) . . ?
O4 C20 C21 125.0(3) . . ?
C18 C20 C21 119.1(3) . . ?
C17 C18 C20 120.3(3) . . ?
C17 C18 H18 119.9 . . ?
C20 C18 H18 119.9 . . ?
C18 C17 C16 121.6(3) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C16 C19 117.5(3) . . ?
C17 C16 C15 120.1(3) . . ?
C19 C16 C15 122.4(3) . . ?
O3 C15 C16 112.7(3) . . ?
O3 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
O3 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
O3 C14 C13 109.3(3) . . ?
O3 C14 H14A 109.8 . . ?
C13 C14 H14A 109.8 . . ?
O3 C14 H14B 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
C21 C19 C16 122.2(3) . . ?
C21 C19 H19 118.9 . . ?
C16 C19 H19 118.9 . . ?
C19 C21 C20 119.3(3) . . ?
C19 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C32 C33 C25 119.5(3) . 2_655 ?
C32 C33 H33 120.3 . . ?
C25 C33 H33 120.3 2_655 . ?
C33 C32 C31 120.8(3) . . ?
C33 C32 C34 118.4(3) . . ?
C31 C32 C34 120.8(3) . . ?
O7 C34 C32 108.1(3) . . ?
O7 C34 H34A 110.1 . . ?
C32 C34 H34A 110.1 . . ?
O7 C34 H34B 110.1 . . ?
C32 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
C30 C31 C32 118.6(3) . . ?
C30 C31 H31 120.7 . . ?
C32 C31 H31 120.7 . . ?
O11 S1 O12 114.71(15) . . ?
O11 S1 O10 115.44(15) . . ?
O12 S1 O10 114.38(14) . . ?
O11 S1 C36 104.27(18) . . ?
O12 S1 C36 102.96(17) . . ?
O10 S1 C36 102.78(17) . . ?
F2 C36 F3 107.8(3) . . ?
F2 C36 F1 107.5(3) . . ?
F3 C36 F1 106.6(4) . . ?
F2 C36 S1 111.5(3) . . ?
F3 C36 S1 111.6(3) . . ?
F1 C36 S1 111.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.43
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 1002574'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_tpclfe

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H32 B2 Cl2 F8 Fe N6'
_chemical_formula_weight         945.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.892(5)
_cell_length_b                   14.886(5)
_cell_length_c                   15.952(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 110.371(5)
_cell_angle_gamma                90.000
_cell_volume                     3983(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    16294
_cell_measurement_theta_min      4.1850
_cell_measurement_theta_max      76.5110

_exptl_crystal_description       ?
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7928
_exptl_absorpt_correction_T_max  0.8755
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24933
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         26.64
_reflns_number_total             8281
_reflns_number_gt                7667
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0427P)²+9.8100P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8281
_refine_ls_number_parameters     568
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1320
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.73475(2) 0.13530(3) 0.24152(3) 0.01474(11) Uani 1 1 d . . .
Cl1 Cl 1.39790(4) 0.18891(7) 0.38771(6) 0.0349(2) Uani 1 1 d . . .
Cl31 Cl 0.07173(4) 0.05264(7) -0.13099(6) 0.0381(2) Uani 1 1 d . . .
F1 F 0.48718(11) -0.15951(13) 0.35954(14) 0.0338(5) Uani 1 1 d . . .
F2 F 0.43634(12) -0.03893(16) 0.27094(19) 0.0485(7) Uani 1 1 d . . .
F3 F 0.51392(14) -0.13839(19) 0.23087(15) 0.0499(6) Uani 1 1 d . . .
F4 F 0.56986(11) -0.04652(13) 0.35058(13) 0.0284(4) Uani 1 1 d . . .
F21 F 0.92217(13) 0.24694(17) 0.61317(14) 0.0397(5) Uani 1 1 d . . .
F22 F 0.96742(12) 0.15426(14) 0.52923(14) 0.0330(5) Uani 1 1 d . . .
F23 F 1.04302(11) 0.27369(13) 0.60009(13) 0.0303(4) Uani 1 1 d . . .
F24 F 0.92870(12) 0.29595(14) 0.48096(12) 0.0320(5) Uani 1 1 d . . .
N1 N 0.75860(13) 0.26499(15) 0.23962(14) 0.0104(4) Uani 1 1 d . . .
N2 N 0.84721(13) 0.13042(15) 0.28739(14) 0.0112(4) Uani 1 1 d . . .
N3 N 0.74899(13) 0.00468(15) 0.26608(15) 0.0124(4) Uani 1 1 d . . .
N31 N 0.72105(14) 0.12164(15) 0.11301(15) 0.0123(4) Uani 1 1 d . . .
N32 N 0.62244(13) 0.13577(14) 0.19192(14) 0.0108(4) Uani 1 1 d . . .
N33 N 0.71063(13) 0.15064(14) 0.35233(14) 0.0101(4) Uani 1 1 d . . .
C1 C 0.70611(15) 0.33353(18) 0.21979(17) 0.0124(5) Uani 1 1 d . . .
H1 H 0.6511 0.3206 0.2055 0.015 Uiso 1 1 calc R . .
C2 C 0.72970(16) 0.42233(18) 0.21952(18) 0.0151(5) Uani 1 1 d . . .
H2 H 0.6914 0.4693 0.2053 0.018 Uiso 1 1 calc R . .
C3 C 0.81005(17) 0.44163(19) 0.24030(18) 0.0166(5) Uani 1 1 d . . .
H3 H 0.8273 0.5018 0.2388 0.020 Uiso 1 1 calc R . .
C4 C 0.86472(16) 0.37202(18) 0.26314(18) 0.0144(5) Uani 1 1 d . . .
H4 H 0.9201 0.3840 0.2789 0.017 Uiso 1 1 calc R . .
C5 C 0.83764(15) 0.28440(18) 0.26274(17) 0.0114(5) Uani 1 1 d . . .
C6 C 0.88950(15) 0.20563(17) 0.28889(16) 0.0109(5) Uani 1 1 d . . .
C7 C 0.97147(16) 0.20274(18) 0.31387(17) 0.0134(5) Uani 1 1 d . . .
H7 H 1.0004 0.2559 0.3126 0.016 Uiso 1 1 calc R . .
C8 C 1.01180(15) 0.12154(18) 0.34104(17) 0.0135(5) Uani 1 1 d . . .
C9 C 0.96687(16) 0.04429(19) 0.34149(17) 0.0145(5) Uani 1 1 d . . .
H9 H 0.9925 -0.0117 0.3609 0.017 Uiso 1 1 calc R . .
C10 C 0.88434(15) 0.05095(18) 0.31309(17) 0.0122(5) Uani 1 1 d . . .
C11 C 0.82685(16) -0.02159(18) 0.30447(18) 0.0137(5) Uani 1 1 d . . .
C12 C 0.84768(17) -0.10859(19) 0.3340(2) 0.0186(6) Uani 1 1 d . . .
H12 H 0.9021 -0.1255 0.3595 0.022 Uiso 1 1 calc R . .
C13 C 0.78757(18) -0.1708(2) 0.3255(2) 0.0220(6) Uani 1 1 d . . .
H13 H 0.8004 -0.2306 0.3462 0.026 Uiso 1 1 calc R . .
C14 C 0.70877(18) -0.1446(2) 0.2867(2) 0.0217(6) Uani 1 1 d . . .
H14 H 0.6669 -0.1862 0.2803 0.026 Uiso 1 1 calc R . .
C15 C 0.69173(16) -0.05663(19) 0.25714(18) 0.0160(5) Uani 1 1 d . . .
H15 H 0.6376 -0.0392 0.2296 0.019 Uiso 1 1 calc R . .
C16 C 1.09957(16) 0.11905(18) 0.36803(18) 0.0147(5) Uani 1 1 d . . .
C17 C 1.13751(16) 0.17038(19) 0.32144(19) 0.0167(5) Uani 1 1 d . . .
H17 H 1.1065 0.2043 0.2708 0.020 Uiso 1 1 calc R . .
C18 C 1.22013(17) 0.1723(2) 0.3484(2) 0.0205(6) Uani 1 1 d . . .
H18 H 1.2451 0.2070 0.3156 0.025 Uiso 1 1 calc R . .
C19 C 1.26670(17) 0.1241(2) 0.4229(2) 0.0207(6) Uani 1 1 d . . .
C20 C 1.22900(17) 0.0716(2) 0.46866(19) 0.0203(6) Uani 1 1 d . . .
H20 H 1.2602 0.0376 0.5191 0.024 Uiso 1 1 calc R . .
C21 C 1.14625(17) 0.0683(2) 0.44125(19) 0.0189(6) Uani 1 1 d . . .
H21 H 1.1213 0.0314 0.4725 0.023 Uiso 1 1 calc R . .
C22 C 1.35630(18) 0.1272(3) 0.4585(3) 0.0334(8) Uani 1 1 d . . .
H22A H 1.3771 0.0650 0.4653 0.040 Uiso 1 1 calc R . .
H22B H 1.3743 0.1553 0.5185 0.040 Uiso 1 1 calc R . .
C31 C 0.77839(17) 0.11922(18) 0.07684(19) 0.0166(5) Uani 1 1 d . . .
H31 H 0.8325 0.1231 0.1152 0.020 Uiso 1 1 calc R . .
C32 C 0.76153(18) 0.11129(19) -0.01466(19) 0.0184(6) Uani 1 1 d . . .
H32 H 0.8035 0.1104 -0.0382 0.022 Uiso 1 1 calc R . .
C33 C 0.68308(19) 0.10476(19) -0.07113(19) 0.0198(6) Uani 1 1 d . . .
H33 H 0.6706 0.0981 -0.1338 0.024 Uiso 1 1 calc R . .
C34 C 0.62303(18) 0.10806(19) -0.03520(18) 0.0177(6) Uani 1 1 d . . .
H34 H 0.5687 0.1044 -0.0729 0.021 Uiso 1 1 calc R . .
C35 C 0.64320(16) 0.11684(17) 0.05683(18) 0.0134(5) Uani 1 1 d . . .
C36 C 0.58561(16) 0.12333(17) 0.10299(17) 0.0129(5) Uani 1 1 d . . .
C37 C 0.50320(16) 0.11832(18) 0.06613(17) 0.0148(5) Uani 1 1 d . . .
H37 H 0.4781 0.1092 0.0036 0.018 Uiso 1 1 calc R . .
C38 C 0.45656(16) 0.12657(17) 0.12044(18) 0.0137(5) Uani 1 1 d . . .
C39 C 0.49701(15) 0.13863(18) 0.21239(18) 0.0124(5) Uani 1 1 d . . .
H39 H 0.4677 0.1445 0.2516 0.015 Uiso 1 1 calc R . .
C40 C 0.57949(15) 0.14200(17) 0.24621(17) 0.0112(5) Uani 1 1 d . . .
C41 C 0.63137(15) 0.15090(17) 0.34044(17) 0.0111(5) Uani 1 1 d . . .
C42 C 0.60416(16) 0.15654(19) 0.41103(18) 0.0149(5) Uani 1 1 d . . .
H42 H 0.5486 0.1560 0.4009 0.018 Uiso 1 1 calc R . .
C43 C 0.65926(17) 0.1630(2) 0.49739(18) 0.0172(6) Uani 1 1 d . . .
H43 H 0.6419 0.1665 0.5472 0.021 Uiso 1 1 calc R . .
C44 C 0.73974(16) 0.16424(19) 0.50990(17) 0.0157(5) Uani 1 1 d . . .
H44 H 0.7782 0.1693 0.5683 0.019 Uiso 1 1 calc R . .
C45 C 0.76355(15) 0.15799(18) 0.43630(18) 0.0134(5) Uani 1 1 d . . .
H45 H 0.8189 0.1589 0.4452 0.016 Uiso 1 1 calc R . .
C46 C 0.36847(16) 0.12293(18) 0.08258(18) 0.0145(5) Uani 1 1 d . . .
C47 C 0.32260(16) 0.11135(19) 0.13731(18) 0.0161(5) Uani 1 1 d . . .
H47 H 0.3484 0.1064 0.2002 0.019 Uiso 1 1 calc R . .
C48 C 0.24023(16) 0.10703(19) 0.10123(19) 0.0176(6) Uani 1 1 d . . .
H48 H 0.2105 0.0992 0.1398 0.021 Uiso 1 1 calc R . .
C49 C 0.20014(17) 0.1140(2) 0.0092(2) 0.0197(6) Uani 1 1 d . . .
C50 C 0.24542(18) 0.1247(2) -0.0455(2) 0.0230(6) Uani 1 1 d . . .
H50 H 0.2193 0.1290 -0.1084 0.028 Uiso 1 1 calc R . .
C51 C 0.32762(17) 0.1292(2) -0.0101(2) 0.0203(6) Uani 1 1 d . . .
H51 H 0.3570 0.1366 -0.0490 0.024 Uiso 1 1 calc R . .
C52 C 0.11044(18) 0.1132(3) -0.0271(2) 0.0308(8) Uani 1 1 d . . .
H52A H 0.0906 0.1758 -0.0366 0.037 Uiso 1 1 calc R . .
H52B H 0.0905 0.0852 0.0173 0.037 Uiso 1 1 calc R . .
B1 B 0.5021(2) -0.0954(3) 0.3035(3) 0.0288(8) Uani 1 1 d . . .
B21 B 0.9654(2) 0.2435(3) 0.5560(2) 0.0214(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N32 1.886(2) . ?
Fe1 N2 1.888(2) . ?
Fe1 N33 1.973(2) . ?
Fe1 N1 1.980(2) . ?
Fe1 N3 1.982(2) . ?
Fe1 N31 1.988(2) . ?
Cl1 C22 1.805(4) . ?
Cl31 C52 1.800(3) . ?
F1 B1 1.395(4) . ?
F2 B1 1.391(4) . ?
F3 B1 1.403(5) . ?
F4 B1 1.389(4) . ?
F21 B21 1.387(4) . ?
F22 B21 1.400(4) . ?
F23 B21 1.394(4) . ?
F24 B21 1.388(4) . ?
N1 C1 1.348(3) . ?
N1 C5 1.363(3) . ?
N2 C6 1.347(3) . ?
N2 C10 1.349(3) . ?
N3 C15 1.342(4) . ?
N3 C11 1.369(3) . ?
N31 C31 1.341(4) . ?
N31 C35 1.371(3) . ?
N32 C40 1.346(3) . ?
N32 C36 1.353(3) . ?
N33 C45 1.349(3) . ?
N33 C41 1.364(3) . ?
C1 C2 1.388(4) . ?
C2 C3 1.388(4) . ?
C3 C4 1.384(4) . ?
C4 C5 1.391(4) . ?
C5 C6 1.463(4) . ?
C6 C7 1.380(4) . ?
C7 C8 1.397(4) . ?
C8 C9 1.405(4) . ?
C8 C16 1.477(4) . ?
C9 C10 1.389(4) . ?
C10 C11 1.464(4) . ?
C11 C12 1.384(4) . ?
C12 C13 1.390(4) . ?
C13 C14 1.384(4) . ?
C14 C15 1.389(4) . ?
C16 C17 1.396(4) . ?
C16 C21 1.397(4) . ?
C17 C18 1.389(4) . ?
C18 C19 1.390(4) . ?
C19 C20 1.394(4) . ?
C19 C22 1.504(4) . ?
C20 C21 1.391(4) . ?
C31 C32 1.389(4) . ?
C32 C33 1.382(4) . ?
C33 C34 1.383(4) . ?
C34 C35 1.391(4) . ?
C35 C36 1.463(4) . ?
C36 C37 1.386(4) . ?
C37 C38 1.402(4) . ?
C38 C39 1.403(4) . ?
C38 C46 1.480(4) . ?
C39 C40 1.385(3) . ?
C40 C41 1.472(3) . ?
C41 C42 1.376(4) . ?
C42 C43 1.390(4) . ?
C43 C44 1.383(4) . ?
C44 C45 1.384(4) . ?
C46 C47 1.402(4) . ?
C46 C51 1.405(4) . ?
C47 C48 1.385(4) . ?
C48 C49 1.396(4) . ?
C49 C50 1.391(5) . ?
C49 C52 1.505(4) . ?
C50 C51 1.381(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N32 Fe1 N2 177.30(10) . . ?
N32 Fe1 N33 80.91(9) . . ?
N2 Fe1 N33 101.13(9) . . ?
N32 Fe1 N1 101.17(9) . . ?
N2 Fe1 N1 80.63(9) . . ?
N33 Fe1 N1 90.93(9) . . ?
N32 Fe1 N3 97.55(9) . . ?
N2 Fe1 N3 80.76(9) . . ?
N33 Fe1 N3 89.40(9) . . ?
N1 Fe1 N3 161.09(9) . . ?
N32 Fe1 N31 80.61(9) . . ?
N2 Fe1 N31 97.35(9) . . ?
N33 Fe1 N31 161.51(9) . . ?
N1 Fe1 N31 91.94(9) . . ?
N3 Fe1 N31 93.71(9) . . ?
C1 N1 C5 118.4(2) . . ?
C1 N1 Fe1 127.28(18) . . ?
C5 N1 Fe1 114.30(17) . . ?
C6 N2 C10 120.6(2) . . ?
C6 N2 Fe1 119.42(18) . . ?
C10 N2 Fe1 119.82(18) . . ?
C15 N3 C11 118.3(2) . . ?
C15 N3 Fe1 127.24(19) . . ?
C11 N3 Fe1 114.17(18) . . ?
C31 N31 C35 118.2(2) . . ?
C31 N31 Fe1 127.45(19) . . ?
C35 N31 Fe1 114.32(18) . . ?
C40 N32 C36 120.3(2) . . ?
C40 N32 Fe1 119.58(17) . . ?
C36 N32 Fe1 119.89(18) . . ?
C45 N33 C41 118.3(2) . . ?
C45 N33 Fe1 127.02(18) . . ?
C41 N33 Fe1 114.63(17) . . ?
N1 C1 C2 122.3(2) . . ?
C1 C2 C3 119.1(2) . . ?
C4 C3 C2 119.1(3) . . ?
C3 C4 C5 119.2(2) . . ?
N1 C5 C4 121.8(2) . . ?
N1 C5 C6 113.7(2) . . ?
C4 C5 C6 124.4(2) . . ?
N2 C6 C7 120.9(2) . . ?
N2 C6 C5 111.4(2) . . ?
C7 C6 C5 127.7(2) . . ?
C6 C7 C8 119.9(2) . . ?
C7 C8 C9 118.4(2) . . ?
C7 C8 C16 119.6(2) . . ?
C9 C8 C16 122.0(2) . . ?
C10 C9 C8 119.0(2) . . ?
N2 C10 C9 121.1(2) . . ?
N2 C10 C11 111.3(2) . . ?
C9 C10 C11 127.6(2) . . ?
N3 C11 C12 122.1(3) . . ?
N3 C11 C10 113.8(2) . . ?
C12 C11 C10 124.1(2) . . ?
C11 C12 C13 118.9(3) . . ?
C14 C13 C12 119.3(3) . . ?
C13 C14 C15 119.1(3) . . ?
N3 C15 C14 122.4(3) . . ?
C17 C16 C21 118.8(3) . . ?
C17 C16 C8 119.7(2) . . ?
C21 C16 C8 121.5(3) . . ?
C18 C17 C16 120.6(3) . . ?
C17 C18 C19 120.7(3) . . ?
C18 C19 C20 118.8(3) . . ?
C18 C19 C22 123.3(3) . . ?
C20 C19 C22 117.8(3) . . ?
C21 C20 C19 120.7(3) . . ?
C20 C21 C16 120.3(3) . . ?
C19 C22 Cl1 113.4(2) . . ?
N31 C31 C32 122.4(3) . . ?
C33 C32 C31 119.4(3) . . ?
C32 C33 C34 119.1(3) . . ?
C33 C34 C35 119.2(3) . . ?
N31 C35 C34 121.7(3) . . ?
N31 C35 C36 113.6(2) . . ?
C34 C35 C36 124.6(3) . . ?
N32 C36 C37 120.7(2) . . ?
N32 C36 C35 111.4(2) . . ?
C37 C36 C35 127.9(2) . . ?
C36 C37 C38 120.5(2) . . ?
C37 C38 C39 117.1(2) . . ?
C37 C38 C46 121.5(2) . . ?
C39 C38 C46 121.3(2) . . ?
C40 C39 C38 120.3(2) . . ?
N32 C40 C39 121.1(2) . . ?
N32 C40 C41 111.4(2) . . ?
C39 C40 C41 127.5(2) . . ?
N33 C41 C42 122.2(2) . . ?
N33 C41 C40 113.4(2) . . ?
C42 C41 C40 124.3(2) . . ?
C41 C42 C43 118.9(3) . . ?
C44 C43 C42 119.2(3) . . ?
C43 C44 C45 119.3(2) . . ?
N33 C45 C44 122.1(2) . . ?
C47 C46 C51 117.4(2) . . ?
C47 C46 C38 121.5(2) . . ?
C51 C46 C38 121.1(3) . . ?
C48 C47 C46 121.1(3) . . ?
C47 C48 C49 121.1(3) . . ?
C50 C49 C48 118.0(3) . . ?
C50 C49 C52 122.4(3) . . ?
C48 C49 C52 119.5(3) . . ?
C51 C50 C49 121.2(3) . . ?
C50 C51 C46 121.1(3) . . ?
C49 C52 Cl31 112.0(2) . . ?
F4 B1 F2 110.6(3) . . ?
F4 B1 F1 109.7(3) . . ?
F2 B1 F1 109.1(3) . . ?
F4 B1 F3 109.3(3) . . ?
F2 B1 F3 108.6(3) . . ?
F1 B1 F3 109.5(3) . . ?
F21 B21 F24 110.0(3) . . ?
F21 B21 F23 110.0(3) . . ?
F24 B21 F23 110.1(3) . . ?
F21 B21 F22 108.3(3) . . ?
F24 B21 F22 109.0(3) . . ?
F23 B21 F22 109.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        26.64
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 1002575'
