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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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 
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data_15rfs09a_squeezed
_database_code_depnum_ccdc_archive 'CCDC 1870002'
_audit_update_record             
;
2018-09-26 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;


_vrf_PLAT234_15rfs09a_squeezed   
;
PROBLEM: Large Hirshfeld Difference F2     --  C17     ..       0.32 Ang.  
RESPONSE: This error is associated with a triflate molecule that is less
 well behaved than the main molecular residue.
;

_vrf_CHEMW03_15rfs09a_squeezed   
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: SQUEEZE from Platon has been applied to this structure.  The 
reported MF reflects the addition of a molecule of ether solvent.
;



_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H17 Ag N9 O), C F3 O3 S, C4 H10 O'
_chemical_formula_sum            'C37 H44 Ag2 B0 F3 N18 O6 S'
_chemical_formula_weight         1141.67

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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_H-M_alt        'C m'
_space_group_name_Hall           'C -2y'

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

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

_cell_length_a                   12.2382(4)
_cell_length_b                   27.6761(10)
_cell_length_c                   7.7791(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.565(2)
_cell_angle_gamma                90
_cell_volume                     2415.10(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3985
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      68.03

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.5697
_exptl_crystal_F_000             1070
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    7.493
_shelx_estimated_absorpt_T_min   0.472
_shelx_estimated_absorpt_T_max   0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   'SADABS-2014/7, Bruker AXS'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18285
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.193
_diffrn_reflns_theta_max         68.211
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_point_group_measured_fraction_full 0.904
_reflns_number_total             4075
_reflns_number_gt                3427
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_max     0.820
_reflns_Friedel_fraction_full    0.823

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       APEX2
_computing_data_reduction        
;
SADABS (Bruker, 2013) and XPREP (Bruker, 2013)
;
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'

_refine_special_details          
;
All nonhydrogen atoms were located in a single difference Fourier electron
 density map and refined using anisotropic diplacement parameters. All C-H
 hydrogen atoms were placed in calculated positions with Uiso = 1.2xUeqiv
 (1.5Ueq for methyl groups) of the connected C atoms. Those H atoms attached
 to nitrogen were located in Fourier diff maps and assigned Uiso = 1.2xUeqiv
 with O-H bond distances restrained to 0.85(2) angstroms.

Pyrazole (N10) was modeled with 66:33 two-part disorder as determined
 from refinement of the ocupancy factors.  The N10-N and N10-C distance
 of the two components were restrained to be the same using the 
 SADI command.  Also, the atomic displacement parameters of the minor
 component were constrained to be the same as the major component
 atoms (EADP).
;


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 0.615 0.000 0.180 217 86 ' '
2 0.115 0.500 0.131 217 86 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
Refinement with the un-SQUEEZED model resulted in a final R value of 6.03%.  
 Significant somewhat identifiable residual electron density was observed at
 the 3-4 e/A3 level suggesting the possible presence of disorded solvent
 (ether and/or acetone).  

 With space group Cm and Z=2, the 86 electrons correspond to 43 electrons 
 (86 electrons/2 = 43) in the asymmetric unit. Given electrons
 associated with acetonitrile (22) and ether (44), ether seems to
 be the match for the available electrons.  Since ether is the
 closest match in electron count, the formula should reflect the 
 inclusion of one molecule of ether per unit cell.
;



_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0374P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1213 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(11)
_chemical_absolute_configuration .
_refine_ls_number_reflns         4075
_refine_ls_number_parameters     290
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.0972
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.26504(9) 0.24580(2) 0.85001(13) 0.0514(2) Uani 1 1 d . . . . .
S1 S 0.6646(4) 0.500000 0.4479(7) 0.0774(12) Uani 1 2 d S T P . .
F1 F 0.4537(8) 0.5384(3) 0.3515(17) 0.135(4) Uani 1 1 d D . . . .
F2 F 0.4964(18) 0.500000 0.129(3) 0.165(7) Uani 1 2 d DS T P . .
O1 O -0.1255(5) 0.3008(2) 0.5608(9) 0.0451(15) Uani 1 1 d . . . . .
O2 O 0.6766(18) 0.500000 0.651(2) 0.144(7) Uani 1 2 d S T P . .
O3 O 0.7084(8) 0.5437(2) 0.4011(13) 0.080(2) Uani 1 1 d . . . . .
N1 N 0.1802(6) 0.2890(2) 1.0298(11) 0.0420(16) Uani 1 1 d . . . . .
N2 N 0.1896(6) 0.3378(2) 1.0405(10) 0.0356(15) Uani 1 1 d . . . . .
N3 N 0.3427(6) 0.3179(3) 0.8217(10) 0.0444(17) Uani 1 1 d . . . . .
N4 N 0.3082(6) 0.3606(3) 0.8697(10) 0.0384(18) Uani 1 1 d . . . . .
N5 N -0.0214(6) 0.3674(3) 0.7081(11) 0.0425(17) Uani 1 1 d . . . . .
H5N H -0.026(8) 0.402(4) 0.732(13) 0.051 Uiso 1 1 d . U . . .
N6 N -0.2080(5) 0.3677(2) 0.8538(11) 0.0406(18) Uani 1 1 d . . . . .
N7 N -0.1706(6) 0.3293(3) 0.9709(10) 0.0445(17) Uani 1 1 d . . . . .
N8 N -0.3373(6) 0.3390(3) 0.5466(11) 0.0336(17) Uani 1 1 d . . . . .
N9 N -0.3661(5) 0.2959(2) 0.5946(9) 0.0356(15) Uani 1 1 d . . . . .
C1 C 0.1856(8) 0.2747(4) 1.1986(14) 0.050(2) Uani 1 1 d . . . . .
H1 H 0.182105 0.242073 1.233591 0.060 Uiso 1 1 calc R U . . .
C2 C 0.1970(9) 0.3137(4) 1.3125(15) 0.064(3) Uani 1 1 d . . . . .
H2 H 0.201560 0.313142 1.437355 0.077 Uiso 1 1 calc R U . . .
C3 C 0.2005(9) 0.3541(4) 1.2107(14) 0.058(3) Uani 1 1 d . . . . .
H3 H 0.208795 0.386764 1.251771 0.070 Uiso 1 1 calc R U . . .
C4 C 0.4483(9) 0.3287(5) 0.8135(16) 0.075(4) Uani 1 1 d . . . . .
H4 H 0.495762 0.306305 0.780998 0.090 Uiso 1 1 calc R U . . .
C5 C 0.4785(10) 0.3770(6) 0.8590(18) 0.085(4) Uani 1 1 d . . . . .
H5 H 0.549650 0.392860 0.868990 0.102 Uiso 1 1 calc R U . . .
C6 C 0.3881(9) 0.3958(4) 0.8850(17) 0.072(3) Uani 1 1 d . . . . .
H6 H 0.379925 0.428917 0.910404 0.086 Uiso 1 1 calc R U . . .
C7 C 0.1944(8) 0.3656(3) 0.8848(13) 0.038(2) Uani 1 1 d . . . . .
H7 H 0.185662 0.400432 0.911272 0.046 Uiso 1 1 calc R U . . .
C8 C 0.0913(6) 0.3532(3) 0.6985(12) 0.0398(19) Uani 1 1 d . . . . .
H8A H 0.101410 0.370557 0.594483 0.048 Uiso 1 1 calc R U . . .
H8B H 0.090807 0.318093 0.674287 0.048 Uiso 1 1 calc R U . . .
C9 C -0.1180(6) 0.3402(3) 0.6386(10) 0.0285(16) Uani 1 1 d . . . . .
C10 C -0.2261(6) 0.3638(3) 0.6590(11) 0.0328(17) Uani 1 1 d . . . . .
H10 H -0.232665 0.397415 0.608819 0.039 Uiso 1 1 calc R U . . .
C11 C -0.2107(8) 0.4090(4) 0.9487(15) 0.055(3) Uani 1 1 d . . . . .
H11 H -0.232705 0.440481 0.898380 0.066 Uiso 1 1 calc R U . . .
C12 C -0.1748(10) 0.3951(5) 1.1314(17) 0.073(3) Uani 1 1 d . . . . .
H12 H -0.165405 0.415386 1.234886 0.088 Uiso 1 1 calc R U . . .
C13 C -0.1554(10) 0.3473(5) 1.1367(16) 0.058(3) Uani 1 1 d . . . . .
H13 H -0.133194 0.328345 1.247435 0.070 Uiso 1 1 calc R U . . .
C14 C -0.4162(7) 0.3529(3) 0.3714(13) 0.045(2) Uani 1 1 d . . . . .
H14 H -0.412346 0.381223 0.304880 0.054 Uiso 1 1 calc R U . . .
C15 C -0.5009(7) 0.3179(3) 0.3128(14) 0.046(2) Uani 1 1 d . . . . .
H15 H -0.569824 0.317469 0.198503 0.055 Uiso 1 1 calc R U . . .
C16 C -0.4673(7) 0.2828(3) 0.4521(12) 0.0381(18) Uani 1 1 d . . . . .
H16 H -0.509937 0.253783 0.447170 0.046 Uiso 1 1 calc R U . . .
C17 C 0.516(3) 0.500000 0.320(4) 0.142(11) Uani 1 2 d DS T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N3 2.258(8) . ?
Ag1 N7 2.287(7) 4 ?
Ag1 N9 2.303(7) 4 ?
Ag1 N1 2.372(7) . ?
S1 O3 1.428(8) 2_565 ?
S1 O3 1.428(8) . ?
S1 O2 1.525(16) . ?
S1 C17 1.69(3) . ?
F1 C17 1.381(16) . ?
F2 C17 1.41(2) . ?
O1 C9 1.232(9) . ?
N1 C1 1.347(11) . ?
N1 N2 1.353(9) . ?
N2 C3 1.355(11) . ?
N2 C7 1.456(12) . ?
N3 C4 1.353(11) . ?
N3 N4 1.356(11) . ?
N4 C6 1.353(12) . ?
N4 C7 1.451(11) . ?
N5 C9 1.323(10) . ?
N5 C8 1.464(10) . ?
N5 H5N 0.97(10) . ?
N6 N7 1.357(10) . ?
N6 C11 1.367(11) . ?
N6 C10 1.445(11) . ?
N7 C13 1.324(13) . ?
N8 N9 1.339(9) . ?
N8 C14 1.373(11) . ?
N8 C10 1.461(10) . ?
N9 C16 1.340(10) . ?
C1 C2 1.368(15) . ?
C1 H1 0.9500 . ?
C2 C3 1.380(15) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.394(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.311(18) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.532(12) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.540(10) . ?
C10 H10 1.0000 . ?
C11 C12 1.364(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.343(17) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.358(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(12) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ag1 N7 138.9(3) . 4 ?
N3 Ag1 N9 122.2(3) . 4 ?
N7 Ag1 N9 84.6(2) 4 4 ?
N3 Ag1 N1 85.0(2) . . ?
N7 Ag1 N1 112.1(2) 4 . ?
N9 Ag1 N1 116.3(2) 4 . ?
O3 S1 O3 115.7(7) 2_565 . ?
O3 S1 O2 111.9(5) 2_565 . ?
O3 S1 O2 111.9(5) . . ?
O3 S1 C17 106.1(6) 2_565 . ?
O3 S1 C17 106.1(6) . . ?
O2 S1 C17 104.1(12) . . ?
C1 N1 N2 105.3(8) . . ?
C1 N1 Ag1 124.3(6) . . ?
N2 N1 Ag1 119.5(5) . . ?
N1 N2 C3 111.4(8) . . ?
N1 N2 C7 120.4(7) . . ?
C3 N2 C7 128.0(8) . . ?
C4 N3 N4 103.2(9) . . ?
C4 N3 Ag1 130.4(8) . . ?
N4 N3 Ag1 123.6(5) . . ?
C6 N4 N3 111.1(8) . . ?
C6 N4 C7 127.3(10) . . ?
N3 N4 C7 121.4(7) . . ?
C9 N5 C8 122.2(7) . . ?
C9 N5 H5N 121(6) . . ?
C8 N5 H5N 114(6) . . ?
N7 N6 C11 111.5(8) . . ?
N7 N6 C10 120.9(7) . . ?
C11 N6 C10 127.1(8) . . ?
C13 N7 N6 103.7(9) . . ?
C13 N7 Ag1 129.3(7) . 4_455 ?
N6 N7 Ag1 117.9(5) . 4_455 ?
N9 N8 C14 111.6(7) . . ?
N9 N8 C10 122.5(7) . . ?
C14 N8 C10 125.4(7) . . ?
N8 N9 C16 105.6(7) . . ?
N8 N9 Ag1 121.1(5) . 4_455 ?
C16 N9 Ag1 132.3(5) . 4_455 ?
N1 C1 C2 110.6(9) . . ?
N1 C1 H1 124.7 . . ?
C2 C1 H1 124.7 . . ?
C1 C2 C3 106.6(9) . . ?
C1 C2 H2 126.7 . . ?
C3 C2 H2 126.7 . . ?
N2 C3 C2 106.1(9) . . ?
N2 C3 H3 127.0 . . ?
C2 C3 H3 127.0 . . ?
N3 C4 C5 111.2(11) . . ?
N3 C4 H4 124.4 . . ?
C5 C4 H4 124.4 . . ?
C6 C5 C4 105.5(9) . . ?
C6 C5 H5 127.3 . . ?
C4 C5 H5 127.3 . . ?
C5 C6 N4 108.9(12) . . ?
C5 C6 H6 125.6 . . ?
N4 C6 H6 125.6 . . ?
N4 C7 N2 112.1(7) . . ?
N4 C7 C8 110.9(7) . . ?
N2 C7 C8 112.1(7) . . ?
N4 C7 H7 107.2 . . ?
N2 C7 H7 107.2 . . ?
C8 C7 H7 107.2 . . ?
N5 C8 C7 109.2(7) . . ?
N5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
O1 C9 N5 125.8(7) . . ?
O1 C9 C10 121.8(7) . . ?
N5 C9 C10 112.4(6) . . ?
N6 C10 N8 112.2(7) . . ?
N6 C10 C9 111.3(6) . . ?
N8 C10 C9 111.9(6) . . ?
N6 C10 H10 107.1 . . ?
N8 C10 H10 107.1 . . ?
C9 C10 H10 107.1 . . ?
C12 C11 N6 105.1(10) . . ?
C12 C11 H11 127.4 . . ?
N6 C11 H11 127.4 . . ?
C13 C12 C11 106.8(9) . . ?
C13 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
N7 C13 C12 112.7(11) . . ?
N7 C13 H13 123.6 . . ?
C12 C13 H13 123.6 . . ?
C15 C14 N8 105.8(8) . . ?
C15 C14 H14 127.1 . . ?
N8 C14 H14 127.1 . . ?
C14 C15 C16 106.8(7) . . ?
C14 C15 H15 126.6 . . ?
C16 C15 H15 126.6 . . ?
N9 C16 C15 110.1(7) . . ?
N9 C16 H16 124.9 . . ?
C15 C16 H16 124.9 . . ?
F1 C17 F1 100.5(18) 2_565 . ?
F1 C17 F2 108.4(18) 2_565 . ?
F1 C17 F2 108.4(18) . . ?
F1 C17 S1 115.7(15) 2_565 . ?
F1 C17 S1 115.7(15) . . ?
F2 C17 S1 107.8(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 C3 -0.1(9) . . . . ?
Ag1 N1 N2 C3 -145.8(6) . . . . ?
C1 N1 N2 C7 176.2(7) . . . . ?
Ag1 N1 N2 C7 30.6(9) . . . . ?
C4 N3 N4 C6 1.5(10) . . . . ?
Ag1 N3 N4 C6 164.1(7) . . . . ?
C4 N3 N4 C7 176.9(8) . . . . ?
Ag1 N3 N4 C7 -20.5(10) . . . . ?
C11 N6 N7 C13 2.6(9) . . . . ?
C10 N6 N7 C13 175.3(7) . . . . ?
C11 N6 N7 Ag1 152.7(5) . . . 4_455 ?
C10 N6 N7 Ag1 -34.6(9) . . . 4_455 ?
C14 N8 N9 C16 -2.5(9) . . . . ?
C10 N8 N9 C16 -174.6(7) . . . . ?
C14 N8 N9 Ag1 167.6(6) . . . 4_455 ?
C10 N8 N9 Ag1 -4.5(10) . . . 4_455 ?
N2 N1 C1 C2 0.6(10) . . . . ?
Ag1 N1 C1 C2 144.1(7) . . . . ?
N1 C1 C2 C3 -0.9(12) . . . . ?
N1 N2 C3 C2 -0.4(10) . . . . ?
C7 N2 C3 C2 -176.4(8) . . . . ?
C1 C2 C3 N2 0.8(11) . . . . ?
N4 N3 C4 C5 1.0(12) . . . . ?
Ag1 N3 C4 C5 -159.9(8) . . . . ?
N3 C4 C5 C6 -3.2(14) . . . . ?
C4 C5 C6 N4 4.0(14) . . . . ?
N3 N4 C6 C5 -3.7(13) . . . . ?
C7 N4 C6 C5 -178.7(9) . . . . ?
C6 N4 C7 N2 -118.3(11) . . . . ?
N3 N4 C7 N2 67.2(10) . . . . ?
C6 N4 C7 C8 115.6(11) . . . . ?
N3 N4 C7 C8 -58.9(10) . . . . ?
N1 N2 C7 N4 -73.2(10) . . . . ?
C3 N2 C7 N4 102.5(10) . . . . ?
N1 N2 C7 C8 52.2(10) . . . . ?
C3 N2 C7 C8 -132.1(9) . . . . ?
C9 N5 C8 C7 -139.0(8) . . . . ?
N4 C7 C8 N5 -169.3(8) . . . . ?
N2 C7 C8 N5 64.6(9) . . . . ?
C8 N5 C9 O1 0.3(13) . . . . ?
C8 N5 C9 C10 -177.8(7) . . . . ?
N7 N6 C10 N8 77.1(8) . . . . ?
C11 N6 C10 N8 -111.4(8) . . . . ?
N7 N6 C10 C9 -49.1(9) . . . . ?
C11 N6 C10 C9 122.4(8) . . . . ?
N9 N8 C10 N6 -52.0(10) . . . . ?
C14 N8 C10 N6 137.0(8) . . . . ?
N9 N8 C10 C9 73.9(10) . . . . ?
C14 N8 C10 C9 -97.1(9) . . . . ?
O1 C9 C10 N6 115.5(8) . . . . ?
N5 C9 C10 N6 -66.3(8) . . . . ?
O1 C9 C10 N8 -10.9(11) . . . . ?
N5 C9 C10 N8 167.3(7) . . . . ?
N7 N6 C11 C12 -0.8(10) . . . . ?
C10 N6 C11 C12 -172.9(8) . . . . ?
N6 C11 C12 C13 -1.3(11) . . . . ?
N6 N7 C13 C12 -3.5(12) . . . . ?
Ag1 N7 C13 C12 -148.8(8) 4_455 . . . ?
C11 C12 C13 N7 3.1(13) . . . . ?
N9 N8 C14 C15 3.2(10) . . . . ?
C10 N8 C14 C15 175.0(8) . . . . ?
N8 C14 C15 C16 -2.5(11) . . . . ?
N8 N9 C16 C15 0.9(9) . . . . ?
Ag1 N9 C16 C15 -167.7(6) 4_455 . . . ?
C14 C15 C16 N9 1.0(11) . . . . ?
O3 S1 C17 F1 59.7(17) 2_565 . . 2_565 ?
O3 S1 C17 F1 -176.8(13) . . . 2_565 ?
O2 S1 C17 F1 -58.5(14) . . . 2_565 ?
O3 S1 C17 F1 176.8(13) 2_565 . . . ?
O3 S1 C17 F1 -59.7(17) . . . . ?
O2 S1 C17 F1 58.5(14) . . . . ?
O3 S1 C17 F2 -61.8(4) 2_565 . . . ?
O3 S1 C17 F2 61.8(4) . . . . ?
O2 S1 C17 F2 180.000(2) . . . . ?

_refine_diff_density_max         0.422
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_15rfs06
_database_code_depnum_ccdc_archive 'CCDC 1870004'
_audit_update_record             
;
2018-09-26 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H17 Fe0.50 N9 O, B F4'
_chemical_formula_sum            'C16 H17 B F4 Fe0.50 N9 O'
_chemical_formula_weight         466.12

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'
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.7191(2)
_cell_length_b                   11.2092(3)
_cell_length_c                   11.6297(3)
_cell_angle_alpha                75.435(2)
_cell_angle_beta                 89.899(2)
_cell_angle_gamma                86.181(2)
_cell_volume                     971.64(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7653
_cell_measurement_theta_min      3.927
_cell_measurement_theta_max      68.191

_exptl_crystal_description       'transparent blade'
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_F_000             476
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.104
_exptl_absorpt_coefficient_mu    3.982
_shelx_estimated_absorpt_T_min   0.426
_shelx_estimated_absorpt_T_max   0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   'SADABS-2014/5, Bruker AXS'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19858
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.928
_diffrn_reflns_theta_max         68.222
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             3476
_reflns_number_gt                3024
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       APEX2
_computing_data_reduction        
;
SADABS (Bruker, 2013 v8.34a) and XPREP (Bruker, 2013)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'

_refine_special_details          
;
All nonhydrogen atoms were located in a single difference Fourier electron
 density maps and refined using anisotropic diplacement parameters. All C-H
 hydrogen atoms were placed in calculated positions with Uiso = 1.2xUeqiv
 (1.5Ueq for methyl groups) of the connected C atoms. The N-H hydrogen
 was located in a difference map and was refined with Uiso = 1.2xUeqiv
 of the attached N atom. The N-H distance was restrained to 0.85(2)
 angstroms.

Pyrazole (N10) was madeled with 66:33 two-part disorder as determined
 from refinement of the ocupancy factors.  The N10-N and N10-C distance
 of the two components were restrained to be the same using the 
 SADI command.  Also, the atomic displacement parameters of the minor
 component were constrained to be the same as the minor component
 atoms (EADP). 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0606P)²+0.2067P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3476
_refine_ls_number_parameters     302
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0965
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.0000 0.0000 0.02206(14) Uani 1 2 d S . P . .
F1 F 0.3889(2) 0.66672(13) 0.04955(14) 0.0466(4) Uani 1 1 d . . . . .
F2 F 0.17047(19) 0.57823(15) 0.16658(14) 0.0455(4) Uani 1 1 d . . . . .
F3 F 0.4518(2) 0.50172(16) 0.20381(14) 0.0483(4) Uani 1 1 d . . . . .
F4 F 0.30367(19) 0.47847(13) 0.04202(13) 0.0392(4) Uani 1 1 d . . . . .
O1 O -0.06482(19) 0.15021(14) 0.07904(14) 0.0273(3) Uani 1 1 d . . . . .
N1 N 0.1799(2) 0.22795(16) -0.12102(16) 0.0239(4) Uani 1 1 d . . . . .
N2 N 0.0790(2) 0.14300(17) -0.14794(16) 0.0251(4) Uani 1 1 d . . . . .
N3 N 0.3133(2) 0.11742(16) 0.06574(16) 0.0229(4) Uani 1 1 d . . . . .
N4 N 0.2490(2) 0.00441(16) 0.07950(16) 0.0246(4) Uani 1 1 d . . . . .
N5 N 0.0112(2) 0.32967(17) 0.11497(17) 0.0255(4) Uani 1 1 d D . . . .
H5N H 0.085(3) 0.384(2) 0.103(2) 0.031 Uiso 1 1 d D U . . .
N6 N -0.1787(3) 0.35265(19) 0.40379(17) 0.0325(5) Uani 1 1 d D . . . .
N7 N -0.1717(7) 0.4122(6) 0.4886(4) 0.0372(11) Uani 0.661(12) 1 d D . P A 1
N8 N 0.0838(3) 0.2460(2) 0.35969(17) 0.0329(5) Uani 1 1 d . . . . .
N9 N 0.0401(3) 0.1282(3) 0.3850(3) 0.0621(8) Uani 1 1 d . . . . .
C1 C 0.2112(3) 0.22809(19) 0.00221(19) 0.0238(5) Uani 1 1 d . . . . .
H1 H 0.2754 0.3022 0.0044 0.029 Uiso 1 1 calc R U . . .
C2 C 0.0368(3) 0.2337(2) 0.06853(19) 0.0240(5) Uani 1 1 d . . . . .
C3 C -0.1284(3) 0.3381(2) 0.1988(2) 0.0290(5) Uani 1 1 d . . . . .
H3A H -0.1959 0.2639 0.2128 0.035 Uiso 1 1 calc R U . . .
H3B H -0.2080 0.4118 0.1659 0.035 Uiso 1 1 calc R U . . .
C4 C -0.0461(3) 0.3479(2) 0.3158(2) 0.0292(5) Uani 1 1 d . . . . .
H4 H 0.0138 0.4267 0.2998 0.035 Uiso 1 1 calc R U . . .
C5 C 0.2351(3) 0.3070(2) -0.2207(2) 0.0285(5) Uani 1 1 d . . . . .
H5 H 0.3068 0.3734 -0.2243 0.034 Uiso 1 1 calc R U . . .
C6 C 0.1669(3) 0.2723(2) -0.3156(2) 0.0323(5) Uani 1 1 d . . . . .
H6 H 0.1814 0.3097 -0.3976 0.039 Uiso 1 1 calc R U . . .
C7 C 0.0716(3) 0.1703(2) -0.2660(2) 0.0314(5) Uani 1 1 d . . . . .
H7 H 0.0098 0.1264 -0.3108 0.038 Uiso 1 1 calc R U . . .
C8 C 0.4680(3) 0.1085(2) 0.1235(2) 0.0275(5) Uani 1 1 d . . . . .
H8 H 0.5370 0.1747 0.1267 0.033 Uiso 1 1 calc R U . . .
C9 C 0.5056(3) -0.0139(2) 0.1762(2) 0.0309(5) Uani 1 1 d . . . . .
H9 H 0.6053 -0.0498 0.2232 0.037 Uiso 1 1 calc R U . . .
C10 C 0.3670(3) -0.0755(2) 0.1468(2) 0.0278(5) Uani 1 1 d . . . . .
H10 H 0.3580 -0.1623 0.1713 0.033 Uiso 1 1 calc R U . . .
C11 C -0.3117(8) 0.3821(8) 0.5624(5) 0.0385(13) Uani 0.661(12) 1 d D . P A 1
H11 H -0.3494 0.4184 0.6245 0.046 Uiso 0.661(12) 1 calc R U P A 1
C12 C -0.3846(8) 0.2883(6) 0.5265(4) 0.0381(11) Uani 0.661(12) 1 d D . P A 1
H12 H -0.4811 0.2468 0.5637 0.046 Uiso 0.661(12) 1 calc R U P A 1
C13 C -0.3037(7) 0.2625(7) 0.4335(5) 0.0348(11) Uani 0.661(12) 1 d D . P A 1
H13 H -0.3247 0.1988 0.3957 0.042 Uiso 0.661(12) 1 calc R U P A 1
C14 C 0.2532(3) 0.2537(3) 0.3734(3) 0.0481(7) Uani 1 1 d . . . . .
H14 H 0.3135 0.3270 0.3600 0.058 Uiso 1 1 calc R U . . .
C15 C 0.3229(4) 0.1353(3) 0.4104(3) 0.0542(8) Uani 1 1 d . . . . .
H15 H 0.4419 0.1101 0.4285 0.065 Uiso 1 1 calc R U . . .
C16 C 0.1902(4) 0.0597(3) 0.4167(3) 0.0525(7) Uani 1 1 d . . . . .
H16 H 0.2020 -0.0280 0.4400 0.063 Uiso 1 1 calc R U . . .
B1 B 0.3309(4) 0.5569(3) 0.1156(2) 0.0306(6) Uani 1 1 d . . . . .
N7A N -0.3279(13) 0.3061(11) 0.4141(8) 0.0372(11) Uani 0.339(12) 1 d D . P A 2
C11A C -0.3982(17) 0.3351(13) 0.5170(9) 0.0385(13) Uani 0.339(12) 1 d D . P A 2
H11A H -0.5087 0.3185 0.5511 0.046 Uiso 0.339(12) 1 calc R U P A 2
C12A C -0.2672(16) 0.3931(18) 0.5551(13) 0.0381(11) Uani 0.339(12) 1 d D . P A
2
H12A H -0.2687 0.4063 0.6327 0.046 Uiso 0.339(12) 1 calc R U P A 2
C13A C -0.1357(19) 0.4314(15) 0.4809(12) 0.0348(11) Uani 0.339(12) 1 d D . P A
2
H13A H -0.0488 0.4879 0.4795 0.042 Uiso 0.339(12) 1 calc R U P A 2


_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 N4 2.1431(18) 2 ?
Fe1 N4 2.1431(18) . ?
Fe1 O1 2.1435(14) 2 ?
Fe1 O1 2.1435(14) . ?
Fe1 N2 2.1543(18) . ?
Fe1 N2 2.1543(18) 2 ?
F1 B1 1.379(3) . ?
F2 B1 1.404(3) . ?
F3 B1 1.383(3) . ?
F4 B1 1.398(3) . ?
O1 C2 1.244(3) . ?
N1 C5 1.358(3) . ?
N1 N2 1.364(2) . ?
N1 C1 1.454(3) . ?
N2 C7 1.330(3) . ?
N3 C8 1.356(3) . ?
N3 N4 1.363(2) . ?
N3 C1 1.455(3) . ?
N4 C10 1.336(3) . ?
N5 C2 1.323(3) . ?
N5 C3 1.466(3) . ?
N5 H5N 0.848(16) . ?
N6 N7A 1.288(9) . ?
N6 N7 1.326(5) . ?
N6 C13 1.423(7) . ?
N6 C4 1.454(3) . ?
N6 C13A 1.461(13) . ?
N7 C11 1.385(5) . ?
N8 C14 1.328(3) . ?
N8 N9 1.344(3) . ?
N8 C4 1.458(3) . ?
N9 C16 1.345(4) . ?
C1 C2 1.556(3) . ?
C1 H1 1.0000 . ?
C3 C4 1.535(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4 1.0000 . ?
C5 C6 1.375(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.400(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.367(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.399(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.378(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.332(7) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.362(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.363(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N7A C11A 1.415(11) . ?
C11A C12A 1.370(13) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.352(13) . ?
C12A H12A 0.9500 . ?
C13A H13A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Fe1 N4 180.0 2 . ?
N4 Fe1 O1 82.61(6) 2 2 ?
N4 Fe1 O1 97.39(6) . 2 ?
N4 Fe1 O1 97.39(6) 2 . ?
N4 Fe1 O1 82.61(6) . . ?
O1 Fe1 O1 180.00(8) 2 . ?
N4 Fe1 N2 92.66(7) 2 . ?
N4 Fe1 N2 87.34(7) . . ?
O1 Fe1 N2 95.86(6) 2 . ?
O1 Fe1 N2 84.14(6) . . ?
N4 Fe1 N2 87.34(7) 2 2 ?
N4 Fe1 N2 92.66(7) . 2 ?
O1 Fe1 N2 84.14(6) 2 2 ?
O1 Fe1 N2 95.86(6) . 2 ?
N2 Fe1 N2 180.0 . 2 ?
C2 O1 Fe1 119.04(13) . . ?
C5 N1 N2 111.43(18) . . ?
C5 N1 C1 128.28(19) . . ?
N2 N1 C1 120.26(17) . . ?
C7 N2 N1 105.25(18) . . ?
C7 N2 Fe1 138.25(16) . . ?
N1 N2 Fe1 116.18(13) . . ?
C8 N3 N4 111.38(18) . . ?
C8 N3 C1 128.61(18) . . ?
N4 N3 C1 119.87(17) . . ?
C10 N4 N3 105.11(18) . . ?
C10 N4 Fe1 137.87(15) . . ?
N3 N4 Fe1 116.98(13) . . ?
C2 N5 C3 122.38(19) . . ?
C2 N5 H5N 119.0(18) . . ?
C3 N5 H5N 118.2(18) . . ?
N7 N6 C13 109.4(3) . . ?
N7A N6 C4 128.7(4) . . ?
N7 N6 C4 125.8(3) . . ?
C13 N6 C4 122.0(3) . . ?
N7A N6 C13A 118.8(6) . . ?
C4 N6 C13A 112.3(5) . . ?
N6 N7 C11 108.2(4) . . ?
C14 N8 N9 112.1(2) . . ?
C14 N8 C4 127.0(2) . . ?
N9 N8 C4 120.8(2) . . ?
N8 N9 C16 105.0(2) . . ?
N1 C1 N3 111.73(17) . . ?
N1 C1 C2 110.71(17) . . ?
N3 C1 C2 107.60(17) . . ?
N1 C1 H1 108.9 . . ?
N3 C1 H1 108.9 . . ?
C2 C1 H1 108.9 . . ?
O1 C2 N5 124.16(19) . . ?
O1 C2 C1 120.80(18) . . ?
N5 C2 C1 114.99(18) . . ?
N5 C3 C4 108.32(18) . . ?
N5 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
N5 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
N6 C4 N8 111.32(19) . . ?
N6 C4 C3 110.67(18) . . ?
N8 C4 C3 110.70(18) . . ?
N6 C4 H4 108.0 . . ?
N8 C4 H4 108.0 . . ?
C3 C4 H4 108.0 . . ?
N1 C5 C6 106.7(2) . . ?
N1 C5 H5 126.7 . . ?
C6 C5 H5 126.7 . . ?
C5 C6 C7 105.6(2) . . ?
C5 C6 H6 127.2 . . ?
C7 C6 H6 127.2 . . ?
N2 C7 C6 111.1(2) . . ?
N2 C7 H7 124.4 . . ?
C6 C7 H7 124.4 . . ?
N3 C8 C9 106.9(2) . . ?
N3 C8 H8 126.5 . . ?
C9 C8 H8 126.5 . . ?
C8 C9 C10 105.8(2) . . ?
C8 C9 H9 127.1 . . ?
C10 C9 H9 127.1 . . ?
N4 C10 C9 110.8(2) . . ?
N4 C10 H10 124.6 . . ?
C9 C10 H10 124.6 . . ?
C12 C11 N7 105.2(6) . . ?
C12 C11 H11 127.4 . . ?
N7 C11 H11 127.4 . . ?
C13 C12 C11 112.1(5) . . ?
C13 C12 H12 124.0 . . ?
C11 C12 H12 124.0 . . ?
C12 C13 N6 103.9(4) . . ?
C12 C13 H13 128.1 . . ?
N6 C13 H13 128.1 . . ?
N8 C14 C15 106.1(3) . . ?
N8 C14 H14 126.9 . . ?
C15 C14 H14 126.9 . . ?
C14 C15 C16 107.1(3) . . ?
C14 C15 H15 126.4 . . ?
C16 C15 H15 126.4 . . ?
N9 C16 C15 109.7(3) . . ?
N9 C16 H16 125.2 . . ?
C15 C16 H16 125.2 . . ?
F1 B1 F3 109.5(2) . . ?
F1 B1 F4 110.0(2) . . ?
F3 B1 F4 110.3(2) . . ?
F1 B1 F2 110.2(2) . . ?
F3 B1 F2 109.9(2) . . ?
F4 B1 F2 106.8(2) . . ?
N6 N7A C11A 104.1(8) . . ?
C12A C11A N7A 102.7(12) . . ?
C12A C11A H11A 128.7 . . ?
N7A C11A H11A 128.7 . . ?
C13A C12A C11A 119.1(13) . . ?
C13A C12A H12A 120.4 . . ?
C11A C12A H12A 120.4 . . ?
C12A C13A N6 92.4(11) . . ?
C12A C13A H13A 133.8 . . ?
N6 C13A H13A 133.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 C7 -0.1(2) . . . . ?
C1 N1 N2 C7 177.96(18) . . . . ?
C5 N1 N2 Fe1 174.53(14) . . . . ?
C1 N1 N2 Fe1 -7.4(2) . . . . ?
C8 N3 N4 C10 -0.2(2) . . . . ?
C1 N3 N4 C10 -176.27(18) . . . . ?
C8 N3 N4 Fe1 177.74(13) . . . . ?
C1 N3 N4 Fe1 1.7(2) . . . . ?
C13 N6 N7 C11 -11.7(7) . . . . ?
C4 N6 N7 C11 -172.8(4) . . . . ?
C14 N8 N9 C16 0.4(3) . . . . ?
C4 N8 N9 C16 177.0(2) . . . . ?
C5 N1 C1 N3 -116.0(2) . . . . ?
N2 N1 C1 N3 66.3(2) . . . . ?
C5 N1 C1 C2 124.1(2) . . . . ?
N2 N1 C1 C2 -53.6(2) . . . . ?
C8 N3 C1 N1 122.2(2) . . . . ?
N4 N3 C1 N1 -62.5(2) . . . . ?
C8 N3 C1 C2 -116.1(2) . . . . ?
N4 N3 C1 C2 59.2(2) . . . . ?
Fe1 O1 C2 N5 -179.01(17) . . . . ?
Fe1 O1 C2 C1 -1.7(3) . . . . ?
C3 N5 C2 O1 9.2(4) . . . . ?
C3 N5 C2 C1 -168.22(19) . . . . ?
N1 C1 C2 O1 61.3(3) . . . . ?
N3 C1 C2 O1 -61.1(3) . . . . ?
N1 C1 C2 N5 -121.2(2) . . . . ?
N3 C1 C2 N5 116.4(2) . . . . ?
C2 N5 C3 C4 119.9(2) . . . . ?
N7A N6 C4 N8 -95.1(8) . . . . ?
N7 N6 C4 N8 88.0(5) . . . . ?
C13 N6 C4 N8 -70.8(4) . . . . ?
C13A N6 C4 N8 91.1(8) . . . . ?
N7A N6 C4 C3 28.5(8) . . . . ?
N7 N6 C4 C3 -148.4(4) . . . . ?
C13 N6 C4 C3 52.7(4) . . . . ?
C13A N6 C4 C3 -145.4(7) . . . . ?
C14 N8 C4 N6 -120.2(3) . . . . ?
N9 N8 C4 N6 63.7(3) . . . . ?
C14 N8 C4 C3 116.2(3) . . . . ?
N9 N8 C4 C3 -59.8(3) . . . . ?
N5 C3 C4 N6 -178.22(18) . . . . ?
N5 C3 C4 N8 -54.3(2) . . . . ?
N2 N1 C5 C6 0.2(2) . . . . ?
C1 N1 C5 C6 -177.7(2) . . . . ?
N1 C5 C6 C7 -0.2(2) . . . . ?
N1 N2 C7 C6 0.0(3) . . . . ?
Fe1 N2 C7 C6 -172.83(17) . . . . ?
C5 C6 C7 N2 0.2(3) . . . . ?
N4 N3 C8 C9 0.1(2) . . . . ?
C1 N3 C8 C9 175.74(19) . . . . ?
N3 C8 C9 C10 0.0(2) . . . . ?
N3 N4 C10 C9 0.2(2) . . . . ?
Fe1 N4 C10 C9 -177.05(16) . . . . ?
C8 C9 C10 N4 -0.2(3) . . . . ?
N6 N7 C11 C12 8.8(8) . . . . ?
N7 C11 C12 C13 -2.5(8) . . . . ?
C11 C12 C13 N6 -4.2(6) . . . . ?
N7 N6 C13 C12 9.9(5) . . . . ?
C4 N6 C13 C12 171.8(3) . . . . ?
N9 N8 C14 C15 -0.6(4) . . . . ?
C4 N8 C14 C15 -176.9(2) . . . . ?
N8 C14 C15 C16 0.5(4) . . . . ?
N8 N9 C16 C15 -0.1(4) . . . . ?
C14 C15 C16 N9 -0.3(4) . . . . ?
C4 N6 N7A C11A 177.9(6) . . . . ?
C13A N6 N7A C11A -8.6(12) . . . . ?
N6 N7A C11A C12A -2.5(12) . . . . ?
N7A C11A C12A C13A 14(2) . . . . ?
C11A C12A C13A N6 -17(2) . . . . ?
N7A N6 C13A C12A 15.2(15) . . . . ?
C4 N6 C13A C12A -170.2(9) . . . . ?

_refine_diff_density_max         0.337
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.050

####################################################################### 
# 
# 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_15rfs16
_database_code_depnum_ccdc_archive 'CCDC 1870003'
_audit_update_record             
;
2018-09-26 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H17 Cl4 N9 O1 Pd2, C2 H6 O1 S1'
_chemical_formula_sum            'C18 H23 Cl4 N9 O2 Pd2 S'
_chemical_formula_weight         784.11

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'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.1580(2)
_cell_length_b                   11.6246(3)
_cell_length_c                   15.2480(4)
_cell_angle_alpha                99.275(1)
_cell_angle_beta                 104.487(2)
_cell_angle_gamma                100.988(2)
_cell_volume                     1340.78(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9983
_cell_measurement_theta_min      3.974
_cell_measurement_theta_max      68.283

_exptl_crystal_description       'tranparent plate'
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_F_000             772
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    15.532
_shelx_estimated_absorpt_T_min   0.210
_shelx_estimated_absorpt_T_max   0.456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.468
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   'SADABS-2014/5, Bruker AXS'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28788
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.068
_diffrn_reflns_theta_max         68.198
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             4780
_reflns_number_gt                4343
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       APEX2
_computing_data_reduction        
;
SADABS (Bruker, 2013) and XPREP (Bruker, 2013)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'

_refine_special_details          
;
All nonhydrogen atoms were located in a single difference Fourier electron
 density maps and refined using anisotropic diplacement parameters. All C-H
 hydrogen atoms were placed in calculated positions with Uiso = 1.2xUeqiv
 (1.5Ueq for methyl groups) of the connected C atoms. Those H atoms attached
 to the nitrogen atom was located in Fourier diff map and assigned Uiso
 = 1.2xUeqiv  with a N-H bond distance restrained to 0.85(2) angstroms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0317P)²+1.9350P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4780
_refine_ls_number_parameters     331
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0646
_refine_ls_wR_factor_gt          0.0614
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.02315(3) 0.08208(2) 0.87355(2) 0.01302(7) Uani 1 1 d . . . . .
Pd2 Pd -0.56809(3) 0.29064(2) 0.55275(2) 0.01595(7) Uani 1 1 d . . . . .
Cl1 Cl 0.00303(11) -0.09261(7) 0.77230(5) 0.01980(17) Uani 1 1 d . . . . .
Cl2 Cl -0.22260(10) 0.00236(7) 0.90962(6) 0.02047(17) Uani 1 1 d . . . . .
Cl3 Cl -0.66462(11) 0.41401(8) 0.64988(6) 0.02271(18) Uani 1 1 d . . . . .
Cl4 Cl -0.81961(11) 0.14488(8) 0.52244(6) 0.02644(19) Uani 1 1 d . . . . .
S1 S 0.50122(12) 0.29445(7) 1.08301(6) 0.02170(18) Uani 1 1 d . . . . .
O1 O -0.1445(3) 0.3380(2) 0.79196(17) 0.0217(5) Uani 1 1 d . . . . .
O2 O 0.6299(5) 0.4086(2) 1.0892(2) 0.0445(8) Uani 1 1 d . . . . .
N1 N 0.2815(4) 0.2771(2) 0.84460(19) 0.0166(6) Uani 1 1 d . . . . .
N2 N 0.2427(4) 0.1581(2) 0.84615(19) 0.0153(6) Uani 1 1 d . . . . .
N3 N 0.1244(4) 0.3452(2) 0.9444(2) 0.0164(6) Uani 1 1 d . . . . .
N4 N 0.0521(4) 0.2393(2) 0.9625(2) 0.0161(6) Uani 1 1 d . . . . .
N5 N -0.1906(4) 0.3899(3) 0.57176(19) 0.0181(6) Uani 1 1 d . . . . .
N6 N -0.3405(4) 0.4166(3) 0.58318(19) 0.0184(6) Uani 1 1 d . . . . .
N7 N -0.3179(4) 0.2029(3) 0.4602(2) 0.0198(6) Uani 1 1 d . . . . .
N8 N -0.4876(4) 0.1891(3) 0.4593(2) 0.0192(6) Uani 1 1 d . . . . .
N9 N -0.0153(4) 0.2431(3) 0.6967(2) 0.0175(6) Uani 1 1 d D . . . .
C1 C 0.4481(5) 0.3135(3) 0.8429(2) 0.0199(7) Uani 1 1 d . . . . .
H1 H 0.5056 0.3925 0.8425 0.024 Uiso 1 1 calc R U . . .
C2 C 0.5185(5) 0.2156(3) 0.8420(3) 0.0239(8) Uani 1 1 d . . . . .
H2 H 0.6332 0.2123 0.8403 0.029 Uiso 1 1 calc R U . . .
C3 C 0.3848(5) 0.1214(3) 0.8442(2) 0.0221(7) Uani 1 1 d . . . . .
H3 H 0.3956 0.0415 0.8443 0.026 Uiso 1 1 calc R U . . .
C4 C 0.1570(4) 0.4352(3) 1.0188(2) 0.0190(7) Uani 1 1 d . . . . .
H4 H 0.2080 0.5175 1.0236 0.023 Uiso 1 1 calc R U . . .
C5 C 0.1036(5) 0.3872(3) 1.0864(2) 0.0212(7) Uani 1 1 d . . . . .
H5 H 0.1081 0.4287 1.1463 0.025 Uiso 1 1 calc R U . . .
C6 C 0.0410(5) 0.2637(3) 1.0482(2) 0.0200(7) Uani 1 1 d . . . . .
H6 H -0.0029 0.2059 1.0794 0.024 Uiso 1 1 calc R U . . .
C7 C 0.1576(4) 0.3479(3) 0.8557(2) 0.0160(7) Uani 1 1 d . . . . .
H7 H 0.2120 0.4329 0.8565 0.019 Uiso 1 1 calc R U . . .
C8 C -0.0185(4) 0.3075(3) 0.7774(2) 0.0164(7) Uani 1 1 d . . . . .
C9 C -0.1734(5) 0.1950(3) 0.6199(2) 0.0198(7) Uani 1 1 d . . . . .
H9A H -0.2763 0.1978 0.6427 0.024 Uiso 1 1 calc R U . . .
H9B H -0.1804 0.1100 0.5935 0.024 Uiso 1 1 calc R U . . .
C10 C -0.1764(5) 0.2671(3) 0.5437(2) 0.0183(7) Uani 1 1 d . . . . .
H10 H -0.0640 0.2714 0.5278 0.022 Uiso 1 1 calc R U . . .
C11 C -0.0601(5) 0.4901(3) 0.5994(2) 0.0216(7) Uani 1 1 d . . . . .
H11 H 0.0574 0.4948 0.5993 0.026 Uiso 1 1 calc R U . . .
C12 C -0.1277(5) 0.5845(3) 0.6278(3) 0.0246(8) Uani 1 1 d . . . . .
H12 H -0.0675 0.6666 0.6506 0.029 Uiso 1 1 calc R U . . .
C13 C -0.3029(5) 0.5344(3) 0.6159(2) 0.0211(7) Uani 1 1 d . . . . .
H13 H -0.3840 0.5782 0.6293 0.025 Uiso 1 1 calc R U . . .
C14 C -0.3046(5) 0.1313(3) 0.3849(3) 0.0257(8) Uani 1 1 d . . . . .
H14 H -0.1999 0.1229 0.3708 0.031 Uiso 1 1 calc R U . . .
C15 C -0.4721(5) 0.0727(4) 0.3323(3) 0.0284(8) Uani 1 1 d . . . . .
H15 H -0.5059 0.0164 0.2746 0.034 Uiso 1 1 calc R U . . .
C16 C -0.5808(5) 0.1119(3) 0.3800(2) 0.0241(8) Uani 1 1 d . . . . .
H16 H -0.7046 0.0875 0.3594 0.029 Uiso 1 1 calc R U . . .
C17 C 0.4747(6) 0.3010(3) 1.1964(3) 0.0305(9) Uani 1 1 d . . . . .
H17A H 0.5876 0.3078 1.2411 0.046 Uiso 1 1 calc R U . . .
H17B H 0.3921 0.2277 1.1963 0.046 Uiso 1 1 calc R U . . .
H17C H 0.4297 0.3710 1.2139 0.046 Uiso 1 1 calc R U . . .
C18 C 0.6174(5) 0.1797(4) 1.0823(3) 0.0297(9) Uani 1 1 d . . . . .
H18A H 0.6603 0.1723 1.0276 0.045 Uiso 1 1 calc R U . . .
H18B H 0.5395 0.1033 1.0802 0.045 Uiso 1 1 calc R U . . .
H18C H 0.7163 0.2004 1.1386 0.045 Uiso 1 1 calc R U . . .
H9 H 0.081(3) 0.233(3) 0.690(3) 0.017(10) Uiso 1 1 d 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
Pd1 N2 2.013(3) . ?
Pd1 N4 2.027(3) . ?
Pd1 Cl2 2.2778(8) . ?
Pd1 Cl1 2.2956(8) . ?
Pd2 N8 2.018(3) . ?
Pd2 N6 2.030(3) . ?
Pd2 Cl3 2.2803(8) . ?
Pd2 Cl4 2.2897(9) . ?
S1 O2 1.500(3) . ?
S1 C18 1.777(4) . ?
S1 C17 1.787(4) . ?
O1 C8 1.208(4) . ?
N1 C1 1.352(4) . ?
N1 N2 1.365(4) . ?
N1 C7 1.444(4) . ?
N2 C3 1.315(5) . ?
N3 C4 1.347(4) . ?
N3 N4 1.362(4) . ?
N3 C7 1.448(4) . ?
N4 C6 1.321(5) . ?
N5 C11 1.346(5) . ?
N5 N6 1.362(4) . ?
N5 C10 1.458(4) . ?
N6 C13 1.327(4) . ?
N7 C14 1.346(5) . ?
N7 N8 1.359(4) . ?
N7 C10 1.463(4) . ?
N8 C16 1.332(5) . ?
N9 C8 1.341(4) . ?
N9 C9 1.452(4) . ?
N9 H9 0.844(19) . ?
C1 C2 1.368(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.402(5) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.372(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.554(5) . ?
C7 H7 1.0000 . ?
C9 C10 1.535(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10 1.0000 . ?
C11 C12 1.376(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.390(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.377(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 N4 87.83(11) . . ?
N2 Pd1 Cl2 177.68(8) . . ?
N4 Pd1 Cl2 89.91(8) . . ?
N2 Pd1 Cl1 89.56(8) . . ?
N4 Pd1 Cl1 177.35(8) . . ?
Cl2 Pd1 Cl1 92.69(3) . . ?
N8 Pd2 N6 88.96(12) . . ?
N8 Pd2 Cl3 175.52(8) . . ?
N6 Pd2 Cl3 90.19(8) . . ?
N8 Pd2 Cl4 90.89(9) . . ?
N6 Pd2 Cl4 177.82(8) . . ?
Cl3 Pd2 Cl4 90.13(3) . . ?
O2 S1 C18 106.2(2) . . ?
O2 S1 C17 106.12(18) . . ?
C18 S1 C17 97.8(2) . . ?
C1 N1 N2 110.6(3) . . ?
C1 N1 C7 129.2(3) . . ?
N2 N1 C7 119.8(3) . . ?
C3 N2 N1 105.8(3) . . ?
C3 N2 Pd1 132.1(2) . . ?
N1 N2 Pd1 121.0(2) . . ?
C4 N3 N4 109.9(3) . . ?
C4 N3 C7 129.8(3) . . ?
N4 N3 C7 120.2(3) . . ?
C6 N4 N3 106.8(3) . . ?
C6 N4 Pd1 132.1(2) . . ?
N3 N4 Pd1 120.1(2) . . ?
C11 N5 N6 110.1(3) . . ?
C11 N5 C10 126.8(3) . . ?
N6 N5 C10 122.7(3) . . ?
C13 N6 N5 106.5(3) . . ?
C13 N6 Pd2 130.5(2) . . ?
N5 N6 Pd2 123.0(2) . . ?
C14 N7 N8 110.7(3) . . ?
C14 N7 C10 127.0(3) . . ?
N8 N7 C10 121.0(3) . . ?
C16 N8 N7 105.9(3) . . ?
C16 N8 Pd2 129.6(3) . . ?
N7 N8 Pd2 123.7(2) . . ?
C8 N9 C9 121.0(3) . . ?
C8 N9 H9 120(3) . . ?
C9 N9 H9 119(3) . . ?
N1 C1 C2 107.4(3) . . ?
N1 C1 H1 126.3 . . ?
C2 C1 H1 126.3 . . ?
C1 C2 C3 105.0(3) . . ?
C1 C2 H2 127.5 . . ?
C3 C2 H2 127.5 . . ?
N2 C3 C2 111.2(3) . . ?
N2 C3 H3 124.4 . . ?
C2 C3 H3 124.4 . . ?
N3 C4 C5 107.9(3) . . ?
N3 C4 H4 126.1 . . ?
C5 C4 H4 126.1 . . ?
C4 C5 C6 105.2(3) . . ?
C4 C5 H5 127.4 . . ?
C6 C5 H5 127.4 . . ?
N4 C6 C5 110.1(3) . . ?
N4 C6 H6 124.9 . . ?
C5 C6 H6 124.9 . . ?
N1 C7 N3 109.2(3) . . ?
N1 C7 C8 114.4(3) . . ?
N3 C7 C8 109.3(3) . . ?
N1 C7 H7 107.9 . . ?
N3 C7 H7 107.9 . . ?
C8 C7 H7 107.9 . . ?
O1 C8 N9 125.2(3) . . ?
O1 C8 C7 118.9(3) . . ?
N9 C8 C7 115.9(3) . . ?
N9 C9 C10 111.0(3) . . ?
N9 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
N9 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N5 C10 N7 110.5(3) . . ?
N5 C10 C9 113.9(3) . . ?
N7 C10 C9 109.5(3) . . ?
N5 C10 H10 107.6 . . ?
N7 C10 H10 107.6 . . ?
C9 C10 H10 107.6 . . ?
N5 C11 C12 107.6(3) . . ?
N5 C11 H11 126.2 . . ?
C12 C11 H11 126.2 . . ?
C11 C12 C13 105.5(3) . . ?
C11 C12 H12 127.3 . . ?
C13 C12 H12 127.3 . . ?
N6 C13 C12 110.3(3) . . ?
N6 C13 H13 124.8 . . ?
C12 C13 H13 124.8 . . ?
N7 C14 C15 106.7(3) . . ?
N7 C14 H14 126.7 . . ?
C15 C14 H14 126.7 . . ?
C16 C15 C14 106.3(3) . . ?
C16 C15 H15 126.9 . . ?
C14 C15 H15 126.9 . . ?
N8 C16 C15 110.3(3) . . ?
N8 C16 H16 124.8 . . ?
C15 C16 H16 124.8 . . ?
S1 C17 H17A 109.5 . . ?
S1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
S1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
S1 C18 H18A 109.5 . . ?
S1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
S1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 C3 -0.8(4) . . . . ?
C7 N1 N2 C3 -173.7(3) . . . . ?
C1 N1 N2 Pd1 168.1(2) . . . . ?
C7 N1 N2 Pd1 -4.8(4) . . . . ?
C4 N3 N4 C6 -0.4(4) . . . . ?
C7 N3 N4 C6 178.6(3) . . . . ?
C4 N3 N4 Pd1 -170.0(2) . . . . ?
C7 N3 N4 Pd1 8.9(4) . . . . ?
C11 N5 N6 C13 1.5(4) . . . . ?
C10 N5 N6 C13 175.0(3) . . . . ?
C11 N5 N6 Pd2 -178.6(2) . . . . ?
C10 N5 N6 Pd2 -5.1(4) . . . . ?
C14 N7 N8 C16 -2.8(4) . . . . ?
C10 N7 N8 C16 -170.3(3) . . . . ?
C14 N7 N8 Pd2 -174.0(2) . . . . ?
C10 N7 N8 Pd2 18.5(4) . . . . ?
N2 N1 C1 C2 0.9(4) . . . . ?
C7 N1 C1 C2 172.9(3) . . . . ?
N1 C1 C2 C3 -0.6(4) . . . . ?
N1 N2 C3 C2 0.4(4) . . . . ?
Pd1 N2 C3 C2 -166.7(2) . . . . ?
C1 C2 C3 N2 0.1(4) . . . . ?
N4 N3 C4 C5 -0.5(4) . . . . ?
C7 N3 C4 C5 -179.3(3) . . . . ?
N3 C4 C5 C6 1.1(4) . . . . ?
N3 N4 C6 C5 1.1(4) . . . . ?
Pd1 N4 C6 C5 169.0(2) . . . . ?
C4 C5 C6 N4 -1.4(4) . . . . ?
C1 N1 C7 N3 -111.8(4) . . . . ?
N2 N1 C7 N3 59.5(4) . . . . ?
C1 N1 C7 C8 125.3(3) . . . . ?
N2 N1 C7 C8 -63.3(4) . . . . ?
C4 N3 C7 N1 116.6(4) . . . . ?
N4 N3 C7 N1 -62.1(4) . . . . ?
C4 N3 C7 C8 -117.6(4) . . . . ?
N4 N3 C7 C8 63.7(4) . . . . ?
C9 N9 C8 O1 -5.2(5) . . . . ?
C9 N9 C8 C7 176.8(3) . . . . ?
N1 C7 C8 O1 160.4(3) . . . . ?
N3 C7 C8 O1 37.6(4) . . . . ?
N1 C7 C8 N9 -21.5(4) . . . . ?
N3 C7 C8 N9 -144.3(3) . . . . ?
C8 N9 C9 C10 105.4(3) . . . . ?
C11 N5 C10 N7 -136.1(3) . . . . ?
N6 N5 C10 N7 51.6(4) . . . . ?
C11 N5 C10 C9 100.2(4) . . . . ?
N6 N5 C10 C9 -72.1(4) . . . . ?
C14 N7 C10 N5 135.6(4) . . . . ?
N8 N7 C10 N5 -59.0(4) . . . . ?
C14 N7 C10 C9 -98.1(4) . . . . ?
N8 N7 C10 C9 67.2(4) . . . . ?
N9 C9 C10 N5 -67.0(4) . . . . ?
N9 C9 C10 N7 168.7(3) . . . . ?
N6 N5 C11 C12 -1.2(4) . . . . ?
C10 N5 C11 C12 -174.3(3) . . . . ?
N5 C11 C12 C13 0.4(4) . . . . ?
N5 N6 C13 C12 -1.3(4) . . . . ?
Pd2 N6 C13 C12 178.8(2) . . . . ?
C11 C12 C13 N6 0.6(4) . . . . ?
N8 N7 C14 C15 2.1(4) . . . . ?
C10 N7 C14 C15 168.7(3) . . . . ?
N7 C14 C15 C16 -0.5(4) . . . . ?
N7 N8 C16 C15 2.5(4) . . . . ?
Pd2 N8 C16 C15 172.9(3) . . . . ?
C14 C15 C16 N8 -1.2(5) . . . . ?

_refine_diff_density_max         0.735
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.120

####################################################################### 
# 
# 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_16rfs02
_database_code_depnum_ccdc_archive 'CCDC 1870005'
_audit_update_record             
;
2018-09-26 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H34 Ag B3 F12 Fe N18 O2'
_chemical_formula_weight         1126.92

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'
B B 0.0090 0.0039 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9228(5)
_cell_length_b                   13.0749(5)
_cell_length_c                   14.3672(6)
_cell_angle_alpha                78.345(2)
_cell_angle_beta                 84.386(2)
_cell_angle_gamma                81.075(2)
_cell_volume                     2161.84(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9916
_cell_measurement_theta_min      3.15
_cell_measurement_theta_max      68.42

_exptl_crystal_description       'transparent prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.048
_exptl_absorpt_coefficient_mu    7.301
_shelx_estimated_absorpt_T_min   0.372
_shelx_estimated_absorpt_T_max   0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   'SADABS-2014/7, Bruker AXS'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            46993
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.148
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             7737
_reflns_number_gt                6937
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_cell_refinement       APEX2
_computing_data_reduction        
;
SADABS (Bruker, 2013) and XPREP (Bruker, 2013)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'

_refine_special_details          
;         
All nonhydrogen atoms were located in a single difference Fourier electron
 density maps and refined using anisotropic diplacement parameters. All C-H
 hydrogen atoms were placed in calculated positions with Uiso = 1.2xUeqiv
 of the connected C atoms. Those H atoms attached to nitrogen were
 located in Fourier diff maps and assigned Uiso = 1.2xUeqiv
 with N-H bond distances restrained to 0.85(2) angstroms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0304P)²+1.5827P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7737
_refine_ls_number_parameters     628
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0657
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag -0.26349(2) -0.01499(2) 0.36968(2) 0.02389(6) Uani 1 1 d . . . . .
Fe1 Fe -0.27407(3) 0.35329(3) 0.21370(2) 0.01420(8) Uani 1 1 d . . . . .
F1 F -0.15154(13) 0.07357(14) 0.76661(10) 0.0384(4) Uani 1 1 d . . . . .
F2 F -0.31615(15) 0.18607(14) 0.75687(12) 0.0487(5) Uani 1 1 d . . . . .
F3 F -0.26631(13) 0.09466(12) 0.90130(10) 0.0337(3) Uani 1 1 d . . . . .
F4 F -0.1672(2) 0.2234(2) 0.82599(15) 0.0823(8) Uani 1 1 d . . . . .
F5 F -0.31465(15) 0.41919(11) 0.62747(10) 0.0361(4) Uani 1 1 d . . . . .
F6 F -0.24099(12) 0.56643(11) 0.55170(10) 0.0258(3) Uani 1 1 d . . . . .
F7 F -0.42563(13) 0.57891(14) 0.60509(13) 0.0463(4) Uani 1 1 d . . . . .
F8 F -0.28873(13) 0.54323(11) 0.71157(10) 0.0313(3) Uani 1 1 d . . . . .
F9 F 0.09018(13) 0.10472(12) 0.05199(11) 0.0354(4) Uani 1 1 d . . . . .
F10 F 0.21636(12) 0.22190(13) 0.00580(12) 0.0375(4) Uani 1 1 d . . . . .
F11 F 0.02919(13) 0.28083(13) 0.02434(11) 0.0389(4) Uani 1 1 d . . . . .
F12 F 0.12652(17) 0.20741(15) 0.15440(11) 0.0537(5) Uani 1 1 d . . . . .
O1 O -0.34904(12) 0.28010(12) 0.35017(10) 0.0166(3) Uani 1 1 d . . . . .
O2 O -0.18781(13) 0.20714(12) 0.18141(11) 0.0186(3) Uani 1 1 d . . . . .
N1 N -0.15730(15) 0.08762(14) 0.42332(13) 0.0165(4) Uani 1 1 d . . . . .
N2 N -0.16807(15) 0.10026(14) 0.51569(13) 0.0150(4) Uani 1 1 d . . . . .
N3 N -0.33134(16) -0.06942(15) 0.53068(13) 0.0205(4) Uani 1 1 d . . . . .
N4 N -0.29042(15) -0.02493(14) 0.59628(13) 0.0164(4) Uani 1 1 d . . . . .
N5 N -0.35484(16) 0.49751(15) 0.25348(13) 0.0196(4) Uani 1 1 d . . . . .
N6 N -0.34828(15) 0.50709(14) 0.34487(13) 0.0159(4) Uani 1 1 d . . . . .
N7 N -0.13815(15) 0.36882(14) 0.29617(13) 0.0161(4) Uani 1 1 d . . . . .
N8 N -0.16897(15) 0.40218(14) 0.38019(13) 0.0153(4) Uani 1 1 d . . . . .
N9 N -0.35474(15) 0.26666(14) 0.51042(13) 0.0150(4) Uani 1 1 d D . . . .
H50 H -0.349(2) 0.2959(19) 0.5564(15) 0.018 Uiso 1 1 d D U . . .
N10 N -0.35560(16) 0.00552(16) 0.23562(14) 0.0210(4) Uani 1 1 d . . . . .
N11 N -0.31262(16) -0.05066(14) 0.16661(13) 0.0176(4) Uani 1 1 d . . . . .
N12 N -0.16625(17) -0.17142(15) 0.31929(14) 0.0227(4) Uani 1 1 d . . . . .
N13 N -0.15322(16) -0.17647(14) 0.22529(13) 0.0188(4) Uani 1 1 d . . . . .
N14 N -0.20438(16) 0.42100(15) 0.07683(13) 0.0186(4) Uani 1 1 d . . . . .
N15 N -0.21315(16) 0.36942(15) 0.00473(13) 0.0177(4) Uani 1 1 d . . . . .
N16 N -0.41034(15) 0.32603(15) 0.13755(13) 0.0179(4) Uani 1 1 d . . . . .
N17 N -0.37881(15) 0.28574(15) 0.05706(13) 0.0172(4) Uani 1 1 d . . . . .
N18 N -0.16356(15) 0.09386(14) 0.07835(13) 0.0159(4) Uani 1 1 d D . . . .
H51 H -0.171(2) 0.086(2) 0.0230(13) 0.019 Uiso 1 1 d D U . . .
C1 C -0.05362(19) 0.11085(17) 0.39160(17) 0.0187(5) Uani 1 1 d . . . . .
H1 H -0.0215 0.1088 0.3287 0.022 Uiso 1 1 calc R U . . .
C2 C 0.00206(19) 0.13870(17) 0.46223(16) 0.0189(5) Uani 1 1 d . . . . .
H2 H 0.0762 0.1583 0.4569 0.023 Uiso 1 1 calc R U . . .
C3 C -0.07358(18) 0.13146(17) 0.54064(16) 0.0177(5) Uani 1 1 d . . . . .
H3 H -0.0621 0.1456 0.6011 0.021 Uiso 1 1 calc R U . . .
C4 C -0.3283(2) -0.17085(18) 0.57226(18) 0.0229(5) Uani 1 1 d . . . . .
H4 H -0.3524 -0.2226 0.5438 0.028 Uiso 1 1 calc R U . . .
C5 C -0.28568(19) -0.19203(18) 0.66231(17) 0.0222(5) Uani 1 1 d . . . . .
H5 H -0.2755 -0.2579 0.7051 0.027 Uiso 1 1 calc R U . . .
C6 C -0.26174(18) -0.09680(17) 0.67548(16) 0.0182(5) Uani 1 1 d . . . . .
H6 H -0.2309 -0.0837 0.7298 0.022 Uiso 1 1 calc R U . . .
C7 C -0.4077(2) 0.59032(19) 0.21164(18) 0.0258(5) Uani 1 1 d . . . . .
H7 H -0.4249 0.6072 0.1467 0.031 Uiso 1 1 calc R U . . .
C8 C -0.4345(2) 0.6598(2) 0.27547(18) 0.0286(6) Uani 1 1 d . . . . .
H8 H -0.4720 0.7303 0.2628 0.034 Uiso 1 1 calc R U . . .
C9 C -0.39497(19) 0.60403(18) 0.36043(17) 0.0218(5) Uani 1 1 d . . . . .
H9 H -0.3995 0.6287 0.4187 0.026 Uiso 1 1 calc R U . . .
C10 C -0.02509(19) 0.36008(17) 0.28753(17) 0.0198(5) Uani 1 1 d . . . . .
H10 H 0.0209 0.3380 0.2354 0.024 Uiso 1 1 calc R U . . .
C11 C 0.01756(19) 0.38771(17) 0.36535(17) 0.0213(5) Uani 1 1 d . . . . .
H11 H 0.0950 0.3881 0.3757 0.026 Uiso 1 1 calc R U . . .
C12 C -0.07688(19) 0.41416(17) 0.42344(17) 0.0181(5) Uani 1 1 d . . . . .
H12 H -0.0775 0.4365 0.4825 0.022 Uiso 1 1 calc R U . . .
C13 C -0.27247(18) 0.08542(17) 0.57526(15) 0.0153(4) Uani 1 1 d . . . . .
H13 H -0.2629 0.1056 0.6373 0.018 Uiso 1 1 calc R U . . .
C14 C -0.37719(18) 0.15719(16) 0.53284(15) 0.0154(4) Uani 1 1 d . . . . .
H14A H -0.3942 0.1353 0.4743 0.019 Uiso 1 1 calc R U . . .
H14B H -0.4441 0.1507 0.5791 0.019 Uiso 1 1 calc R U . . .
C15 C -0.33656(17) 0.31661(17) 0.42089(15) 0.0149(4) Uani 1 1 d . . . . .
C16 C -0.28898(17) 0.42189(16) 0.41110(15) 0.0146(4) Uani 1 1 d . . . . .
H16 H -0.2957 0.4421 0.4751 0.017 Uiso 1 1 calc R U . . .
C17 C -0.4658(2) 0.0300(2) 0.22256(18) 0.0279(6) Uani 1 1 d . . . . .
H17 H -0.5185 0.0693 0.2606 0.033 Uiso 1 1 calc R U . . .
C18 C -0.4948(2) -0.0092(2) 0.14566(19) 0.0322(6) Uani 1 1 d . . . . .
H18 H -0.5680 -0.0023 0.1224 0.039 Uiso 1 1 calc R U . . .
C19 C -0.3951(2) -0.05944(19) 0.11146(17) 0.0251(5) Uani 1 1 d . . . . .
H19 H -0.3853 -0.0942 0.0586 0.030 Uiso 1 1 calc R U . . .
C20 C -0.1198(2) -0.26635(19) 0.36288(18) 0.0269(5) Uani 1 1 d . . . . .
H20 H -0.1166 -0.2874 0.4300 0.032 Uiso 1 1 calc R U . . .
C21 C -0.0763(2) -0.3308(2) 0.2976(2) 0.0339(6) Uani 1 1 d . . . . .
H21 H -0.0390 -0.4013 0.3111 0.041 Uiso 1 1 calc R U . . .
C22 C -0.0988(2) -0.27103(18) 0.21016(18) 0.0264(5) Uani 1 1 d . . . . .
H22 H -0.0799 -0.2918 0.1503 0.032 Uiso 1 1 calc R U . . .
C23 C -0.1658(2) 0.51030(19) 0.03441(18) 0.0247(5) Uani 1 1 d . . . . .
H23 H -0.1505 0.5626 0.0668 0.030 Uiso 1 1 calc R U . . .
C24 C -0.1510(2) 0.5169(2) -0.06382(19) 0.0316(6) Uani 1 1 d . . . . .
H24 H -0.1247 0.5728 -0.1096 0.038 Uiso 1 1 calc R U . . .
C25 C -0.1821(2) 0.42619(19) -0.08088(17) 0.0256(5) Uani 1 1 d . . . . .
H25 H -0.1818 0.4069 -0.1412 0.031 Uiso 1 1 calc R U . . .
C26 C -0.5236(2) 0.33293(19) 0.14691(18) 0.0237(5) Uani 1 1 d . . . . .
H26 H -0.5702 0.3593 0.1967 0.028 Uiso 1 1 calc R U . . .
C27 C -0.5645(2) 0.2961(2) 0.07372(19) 0.0279(6) Uani 1 1 d . . . . .
H27 H -0.6415 0.2923 0.0648 0.034 Uiso 1 1 calc R U . . .
C28 C -0.4699(2) 0.26662(19) 0.01729(17) 0.0229(5) Uani 1 1 d . . . . .
H28 H -0.4686 0.2383 -0.0388 0.027 Uiso 1 1 calc R U . . .
C29 C -0.19144(19) -0.08610(17) 0.15261(16) 0.0173(5) Uani 1 1 d . . . . .
H29 H -0.1786 -0.1096 0.0899 0.021 Uiso 1 1 calc R U . . .
C30 C -0.11918(18) 0.00239(17) 0.14741(16) 0.0170(4) Uani 1 1 d . . . . .
H30A H -0.1215 0.0216 0.2108 0.020 Uiso 1 1 calc R U . . .
H30B H -0.0391 -0.0219 0.1281 0.020 Uiso 1 1 calc R U . . .
C31 C -0.19736(18) 0.18765(17) 0.10171(15) 0.0155(4) Uani 1 1 d . . . . .
C32 C -0.25892(18) 0.27065(17) 0.02428(16) 0.0169(4) Uani 1 1 d . . . . .
H32 H -0.2516 0.2419 -0.0358 0.020 Uiso 1 1 calc R U . . .
B1 B -0.2239(3) 0.1452(2) 0.8119(2) 0.0291(6) Uani 1 1 d . . . . .
B2 B -0.3184(2) 0.5266(2) 0.6259(2) 0.0218(6) Uani 1 1 d . . . . .
B3 B 0.1153(2) 0.2029(2) 0.0608(2) 0.0253(6) 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
Ag1 N10 2.2587(19) . ?
Ag1 N1 2.2653(18) . ?
Ag1 N3 2.3788(19) . ?
Ag1 N12 2.398(2) . ?
Fe1 N14 2.1321(19) . ?
Fe1 N5 2.1387(19) . ?
Fe1 O2 2.1400(15) . ?
Fe1 N7 2.1556(18) . ?
Fe1 N16 2.1561(18) . ?
Fe1 O1 2.1734(15) . ?
F1 B1 1.389(3) . ?
F2 B1 1.391(4) . ?
F3 B1 1.406(3) . ?
F4 B1 1.367(3) . ?
F5 B2 1.394(3) . ?
F6 B2 1.412(3) . ?
F7 B2 1.383(3) . ?
F8 B2 1.380(3) . ?
F9 B3 1.394(3) . ?
F10 B3 1.402(3) . ?
F11 B3 1.390(3) . ?
F12 B3 1.379(3) . ?
O1 C15 1.237(3) . ?
O2 C31 1.242(3) . ?
N1 C1 1.334(3) . ?
N1 N2 1.362(3) . ?
N2 C3 1.358(3) . ?
N2 C13 1.456(3) . ?
N3 C4 1.336(3) . ?
N3 N4 1.365(3) . ?
N4 C6 1.356(3) . ?
N4 C13 1.458(3) . ?
N5 C7 1.332(3) . ?
N5 N6 1.355(3) . ?
N6 C9 1.356(3) . ?
N6 C16 1.451(3) . ?
N7 C10 1.331(3) . ?
N7 N8 1.363(3) . ?
N8 C12 1.357(3) . ?
N8 C16 1.456(3) . ?
N9 C15 1.333(3) . ?
N9 C14 1.463(3) . ?
N9 H50 0.840(16) . ?
N10 C17 1.326(3) . ?
N10 N11 1.365(3) . ?
N11 C19 1.353(3) . ?
N11 C29 1.455(3) . ?
N12 C20 1.334(3) . ?
N12 N13 1.358(3) . ?
N13 C22 1.352(3) . ?
N13 C29 1.457(3) . ?
N14 C23 1.331(3) . ?
N14 N15 1.365(3) . ?
N15 C25 1.352(3) . ?
N15 C32 1.445(3) . ?
N16 C26 1.334(3) . ?
N16 N17 1.362(3) . ?
N17 C28 1.353(3) . ?
N17 C32 1.457(3) . ?
N18 C31 1.329(3) . ?
N18 C30 1.457(3) . ?
N18 H51 0.838(16) . ?
C1 C2 1.400(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.370(3) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.396(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.399(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.375(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.404(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.538(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.544(3) . ?
C16 H16 1.0000 . ?
C17 C18 1.401(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.364(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.395(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.365(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.392(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.369(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.397(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.375(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.532(3) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.542(3) . ?
C32 H32 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 Ag1 N1 133.04(7) . . ?
N10 Ag1 N3 128.76(7) . . ?
N1 Ag1 N3 87.48(6) . . ?
N10 Ag1 N12 83.79(7) . . ?
N1 Ag1 N12 117.54(7) . . ?
N3 Ag1 N12 105.87(7) . . ?
N14 Fe1 N5 97.04(7) . . ?
N14 Fe1 O2 84.84(7) . . ?
N5 Fe1 O2 176.58(7) . . ?
N14 Fe1 N7 97.99(7) . . ?
N5 Fe1 N7 85.06(7) . . ?
O2 Fe1 N7 91.86(6) . . ?
N14 Fe1 N16 85.18(7) . . ?
N5 Fe1 N16 97.48(7) . . ?
O2 Fe1 N16 85.50(6) . . ?
N7 Fe1 N16 175.69(7) . . ?
N14 Fe1 O1 177.47(7) . . ?
N5 Fe1 O1 84.32(7) . . ?
O2 Fe1 O1 93.91(6) . . ?
N7 Fe1 O1 84.24(6) . . ?
N16 Fe1 O1 92.53(6) . . ?
C15 O1 Fe1 117.63(14) . . ?
C31 O2 Fe1 118.06(14) . . ?
C1 N1 N2 104.52(18) . . ?
C1 N1 Ag1 128.94(15) . . ?
N2 N1 Ag1 121.85(13) . . ?
C3 N2 N1 111.65(18) . . ?
C3 N2 C13 126.65(18) . . ?
N1 N2 C13 121.64(17) . . ?
C4 N3 N4 103.90(19) . . ?
C4 N3 Ag1 122.63(15) . . ?
N4 N3 Ag1 115.86(13) . . ?
C6 N4 N3 111.98(18) . . ?
C6 N4 C13 126.57(19) . . ?
N3 N4 C13 121.23(18) . . ?
C7 N5 N6 104.87(19) . . ?
C7 N5 Fe1 138.06(17) . . ?
N6 N5 Fe1 116.90(13) . . ?
N5 N6 C9 111.92(18) . . ?
N5 N6 C16 120.31(17) . . ?
C9 N6 C16 127.62(19) . . ?
C10 N7 N8 105.10(18) . . ?
C10 N7 Fe1 138.01(16) . . ?
N8 N7 Fe1 116.78(13) . . ?
C12 N8 N7 111.58(18) . . ?
C12 N8 C16 128.82(19) . . ?
N7 N8 C16 119.59(17) . . ?
C15 N9 C14 121.79(18) . . ?
C15 N9 H50 120.8(18) . . ?
C14 N9 H50 117.3(18) . . ?
C17 N10 N11 104.92(19) . . ?
C17 N10 Ag1 129.73(16) . . ?
N11 N10 Ag1 119.94(14) . . ?
C19 N11 N10 111.11(19) . . ?
C19 N11 C29 126.7(2) . . ?
N10 N11 C29 121.96(17) . . ?
C20 N12 N13 104.28(19) . . ?
C20 N12 Ag1 135.53(17) . . ?
N13 N12 Ag1 120.14(14) . . ?
C22 N13 N12 112.09(19) . . ?
C22 N13 C29 126.5(2) . . ?
N12 N13 C29 121.40(18) . . ?
C23 N14 N15 105.09(19) . . ?
C23 N14 Fe1 138.26(17) . . ?
N15 N14 Fe1 115.87(13) . . ?
C25 N15 N14 111.32(19) . . ?
C25 N15 C32 128.1(2) . . ?
N14 N15 C32 120.45(18) . . ?
C26 N16 N17 105.07(18) . . ?
C26 N16 Fe1 138.65(16) . . ?
N17 N16 Fe1 116.22(13) . . ?
C28 N17 N16 111.64(19) . . ?
C28 N17 C32 128.9(2) . . ?
N16 N17 C32 119.42(17) . . ?
C31 N18 C30 122.11(19) . . ?
C31 N18 H51 119.3(18) . . ?
C30 N18 H51 118.5(18) . . ?
N1 C1 C2 111.8(2) . . ?
N1 C1 H1 124.1 . . ?
C2 C1 H1 124.1 . . ?
C3 C2 C1 105.0(2) . . ?
C3 C2 H2 127.5 . . ?
C1 C2 H2 127.5 . . ?
N2 C3 C2 107.1(2) . . ?
N2 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
N3 C4 C5 112.3(2) . . ?
N3 C4 H4 123.9 . . ?
C5 C4 H4 123.9 . . ?
C6 C5 C4 104.9(2) . . ?
C6 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
N4 C6 C5 107.0(2) . . ?
N4 C6 H6 126.5 . . ?
C5 C6 H6 126.5 . . ?
N5 C7 C8 111.4(2) . . ?
N5 C7 H7 124.3 . . ?
C8 C7 H7 124.3 . . ?
C9 C8 C7 105.1(2) . . ?
C9 C8 H8 127.4 . . ?
C7 C8 H8 127.4 . . ?
N6 C9 C8 106.7(2) . . ?
N6 C9 H9 126.7 . . ?
C8 C9 H9 126.7 . . ?
N7 C10 C11 111.3(2) . . ?
N7 C10 H10 124.4 . . ?
C11 C10 H10 124.4 . . ?
C12 C11 C10 105.2(2) . . ?
C12 C11 H11 127.4 . . ?
C10 C11 H11 127.4 . . ?
N8 C12 C11 106.8(2) . . ?
N8 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
N2 C13 N4 111.38(17) . . ?
N2 C13 C14 112.66(17) . . ?
N4 C13 C14 111.22(17) . . ?
N2 C13 H13 107.1 . . ?
N4 C13 H13 107.1 . . ?
C14 C13 H13 107.1 . . ?
N9 C14 C13 109.56(17) . . ?
N9 C14 H14A 109.8 . . ?
C13 C14 H14A 109.8 . . ?
N9 C14 H14B 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
O1 C15 N9 123.9(2) . . ?
O1 C15 C16 121.42(19) . . ?
N9 C15 C16 114.57(18) . . ?
N6 C16 N8 110.90(17) . . ?
N6 C16 C15 112.96(17) . . ?
N8 C16 C15 106.59(16) . . ?
N6 C16 H16 108.8 . . ?
N8 C16 H16 108.8 . . ?
C15 C16 H16 108.8 . . ?
N10 C17 C18 111.5(2) . . ?
N10 C17 H17 124.3 . . ?
C18 C17 H17 124.3 . . ?
C19 C18 C17 105.1(2) . . ?
C19 C18 H18 127.5 . . ?
C17 C18 H18 127.5 . . ?
N11 C19 C18 107.4(2) . . ?
N11 C19 H19 126.3 . . ?
C18 C19 H19 126.3 . . ?
N12 C20 C21 111.5(2) . . ?
N12 C20 H20 124.2 . . ?
C21 C20 H20 124.2 . . ?
C22 C21 C20 105.4(2) . . ?
C22 C21 H21 127.3 . . ?
C20 C21 H21 127.3 . . ?
N13 C22 C21 106.7(2) . . ?
N13 C22 H22 126.6 . . ?
C21 C22 H22 126.6 . . ?
N14 C23 C24 111.0(2) . . ?
N14 C23 H23 124.5 . . ?
C24 C23 H23 124.5 . . ?
C25 C24 C23 105.9(2) . . ?
C25 C24 H24 127.1 . . ?
C23 C24 H24 127.1 . . ?
N15 C25 C24 106.7(2) . . ?
N15 C25 H25 126.6 . . ?
C24 C25 H25 126.6 . . ?
N16 C26 C27 111.0(2) . . ?
N16 C26 H26 124.5 . . ?
C27 C26 H26 124.5 . . ?
C28 C27 C26 105.6(2) . . ?
C28 C27 H27 127.2 . . ?
C26 C27 H27 127.2 . . ?
N17 C28 C27 106.7(2) . . ?
N17 C28 H28 126.6 . . ?
C27 C28 H28 126.6 . . ?
N11 C29 N13 111.80(18) . . ?
N11 C29 C30 112.52(17) . . ?
N13 C29 C30 110.51(18) . . ?
N11 C29 H29 107.2 . . ?
N13 C29 H29 107.2 . . ?
C30 C29 H29 107.2 . . ?
N18 C30 C29 109.28(17) . . ?
N18 C30 H30A 109.8 . . ?
C29 C30 H30A 109.8 . . ?
N18 C30 H30B 109.8 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 108.3 . . ?
O2 C31 N18 123.7(2) . . ?
O2 C31 C32 121.19(19) . . ?
N18 C31 C32 114.92(19) . . ?
N15 C32 N17 110.91(17) . . ?
N15 C32 C31 112.91(18) . . ?
N17 C32 C31 107.00(17) . . ?
N15 C32 H32 108.6 . . ?
N17 C32 H32 108.6 . . ?
C31 C32 H32 108.6 . . ?
F4 B1 F1 110.5(2) . . ?
F4 B1 F2 111.3(3) . . ?
F1 B1 F2 108.8(2) . . ?
F4 B1 F3 107.9(2) . . ?
F1 B1 F3 110.5(2) . . ?
F2 B1 F3 107.8(2) . . ?
F8 B2 F7 111.0(2) . . ?
F8 B2 F5 110.7(2) . . ?
F7 B2 F5 109.9(2) . . ?
F8 B2 F6 109.7(2) . . ?
F7 B2 F6 107.4(2) . . ?
F5 B2 F6 108.0(2) . . ?
F12 B3 F11 109.5(2) . . ?
F12 B3 F9 111.6(2) . . ?
F11 B3 F9 109.3(2) . . ?
F12 B3 F10 110.1(2) . . ?
F11 B3 F10 107.6(2) . . ?
F9 B3 F10 108.7(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 C3 0.5(2) . . . . ?
Ag1 N1 N2 C3 158.18(14) . . . . ?
C1 N1 N2 C13 177.96(18) . . . . ?
Ag1 N1 N2 C13 -24.3(2) . . . . ?
C4 N3 N4 C6 0.7(2) . . . . ?
Ag1 N3 N4 C6 -136.80(15) . . . . ?
C4 N3 N4 C13 175.68(19) . . . . ?
Ag1 N3 N4 C13 38.2(2) . . . . ?
C7 N5 N6 C9 -0.5(2) . . . . ?
Fe1 N5 N6 C9 175.56(15) . . . . ?
C7 N5 N6 C16 -176.32(19) . . . . ?
Fe1 N5 N6 C16 -0.2(2) . . . . ?
C10 N7 N8 C12 0.0(2) . . . . ?
Fe1 N7 N8 C12 -176.87(14) . . . . ?
C10 N7 N8 C16 178.87(18) . . . . ?
Fe1 N7 N8 C16 2.0(2) . . . . ?
C17 N10 N11 C19 0.7(3) . . . . ?
Ag1 N10 N11 C19 157.09(15) . . . . ?
C17 N10 N11 C29 175.6(2) . . . . ?
Ag1 N10 N11 C29 -28.0(3) . . . . ?
C20 N12 N13 C22 -0.9(3) . . . . ?
Ag1 N12 N13 C22 -178.63(15) . . . . ?
C20 N12 N13 C29 -178.6(2) . . . . ?
Ag1 N12 N13 C29 3.6(3) . . . . ?
C23 N14 N15 C25 -0.8(2) . . . . ?
Fe1 N14 N15 C25 171.00(15) . . . . ?
C23 N14 N15 C32 -176.60(19) . . . . ?
Fe1 N14 N15 C32 -4.8(2) . . . . ?
C26 N16 N17 C28 -0.7(2) . . . . ?
Fe1 N16 N17 C28 176.91(15) . . . . ?
C26 N16 N17 C32 178.29(19) . . . . ?
Fe1 N16 N17 C32 -4.1(2) . . . . ?
N2 N1 C1 C2 -0.3(2) . . . . ?
Ag1 N1 C1 C2 -155.81(15) . . . . ?
N1 C1 C2 C3 0.0(3) . . . . ?
N1 N2 C3 C2 -0.5(2) . . . . ?
C13 N2 C3 C2 -177.82(19) . . . . ?
C1 C2 C3 N2 0.3(2) . . . . ?
N4 N3 C4 C5 -0.5(3) . . . . ?
Ag1 N3 C4 C5 133.33(17) . . . . ?
N3 C4 C5 C6 0.1(3) . . . . ?
N3 N4 C6 C5 -0.7(2) . . . . ?
C13 N4 C6 C5 -175.34(19) . . . . ?
C4 C5 C6 N4 0.4(2) . . . . ?
N6 N5 C7 C8 0.4(3) . . . . ?
Fe1 N5 C7 C8 -174.41(18) . . . . ?
N5 C7 C8 C9 -0.1(3) . . . . ?
N5 N6 C9 C8 0.5(3) . . . . ?
C16 N6 C9 C8 175.9(2) . . . . ?
C7 C8 C9 N6 -0.2(3) . . . . ?
N8 N7 C10 C11 -0.1(2) . . . . ?
Fe1 N7 C10 C11 175.75(16) . . . . ?
N7 C10 C11 C12 0.1(3) . . . . ?
N7 N8 C12 C11 0.1(2) . . . . ?
C16 N8 C12 C11 -178.7(2) . . . . ?
C10 C11 C12 N8 -0.1(2) . . . . ?
C3 N2 C13 N4 -114.3(2) . . . . ?
N1 N2 C13 N4 68.6(2) . . . . ?
C3 N2 C13 C14 119.9(2) . . . . ?
N1 N2 C13 C14 -57.2(2) . . . . ?
C6 N4 C13 N2 96.1(2) . . . . ?
N3 N4 C13 N2 -78.2(2) . . . . ?
C6 N4 C13 C14 -137.4(2) . . . . ?
N3 N4 C13 C14 48.4(3) . . . . ?
C15 N9 C14 C13 107.3(2) . . . . ?
N2 C13 C14 N9 -52.6(2) . . . . ?
N4 C13 C14 N9 -178.50(17) . . . . ?
Fe1 O1 C15 N9 -164.38(16) . . . . ?
Fe1 O1 C15 C16 10.8(2) . . . . ?
C14 N9 C15 O1 8.1(3) . . . . ?
C14 N9 C15 C16 -167.35(18) . . . . ?
N5 N6 C16 N8 62.6(2) . . . . ?
C9 N6 C16 N8 -112.5(2) . . . . ?
N5 N6 C16 C15 -57.0(2) . . . . ?
C9 N6 C16 C15 127.9(2) . . . . ?
C12 N8 C16 N6 115.4(2) . . . . ?
N7 N8 C16 N6 -63.2(2) . . . . ?
C12 N8 C16 C15 -121.2(2) . . . . ?
N7 N8 C16 C15 60.1(2) . . . . ?
O1 C15 C16 N6 51.4(3) . . . . ?
N9 C15 C16 N6 -132.96(19) . . . . ?
O1 C15 C16 N8 -70.6(2) . . . . ?
N9 C15 C16 N8 105.0(2) . . . . ?
N11 N10 C17 C18 -0.2(3) . . . . ?
Ag1 N10 C17 C18 -153.48(18) . . . . ?
N10 C17 C18 C19 -0.2(3) . . . . ?
N10 N11 C19 C18 -0.8(3) . . . . ?
C29 N11 C19 C18 -175.5(2) . . . . ?
C17 C18 C19 N11 0.6(3) . . . . ?
N13 N12 C20 C21 0.8(3) . . . . ?
Ag1 N12 C20 C21 177.97(18) . . . . ?
N12 C20 C21 C22 -0.4(3) . . . . ?
N12 N13 C22 C21 0.7(3) . . . . ?
C29 N13 C22 C21 178.3(2) . . . . ?
C20 C21 C22 N13 -0.2(3) . . . . ?
N15 N14 C23 C24 0.6(3) . . . . ?
Fe1 N14 C23 C24 -168.25(19) . . . . ?
N14 C23 C24 C25 -0.2(3) . . . . ?
N14 N15 C25 C24 0.7(3) . . . . ?
C32 N15 C25 C24 176.1(2) . . . . ?
C23 C24 C25 N15 -0.3(3) . . . . ?
N17 N16 C26 C27 0.7(3) . . . . ?
Fe1 N16 C26 C27 -175.98(18) . . . . ?
N16 C26 C27 C28 -0.5(3) . . . . ?
N16 N17 C28 C27 0.3(3) . . . . ?
C32 N17 C28 C27 -178.5(2) . . . . ?
C26 C27 C28 N17 0.1(3) . . . . ?
C19 N11 C29 N13 -110.0(2) . . . . ?
N10 N11 C29 N13 75.9(2) . . . . ?
C19 N11 C29 C30 125.0(2) . . . . ?
N10 N11 C29 C30 -49.1(3) . . . . ?
C22 N13 C29 N11 124.1(2) . . . . ?
N12 N13 C29 N11 -58.5(3) . . . . ?
C22 N13 C29 C30 -109.7(2) . . . . ?
N12 N13 C29 C30 67.7(3) . . . . ?
C31 N18 C30 C29 122.4(2) . . . . ?
N11 C29 C30 N18 -50.8(2) . . . . ?
N13 C29 C30 N18 -176.60(17) . . . . ?
Fe1 O2 C31 N18 -168.96(16) . . . . ?
Fe1 O2 C31 C32 6.3(3) . . . . ?
C30 N18 C31 O2 4.6(3) . . . . ?
C30 N18 C31 C32 -170.91(18) . . . . ?
C25 N15 C32 N17 -109.0(2) . . . . ?
N14 N15 C32 N17 66.0(2) . . . . ?
C25 N15 C32 C31 130.9(2) . . . . ?
N14 N15 C32 C31 -54.0(3) . . . . ?
C28 N17 C32 N15 119.1(2) . . . . ?
N16 N17 C32 N15 -59.7(2) . . . . ?
C28 N17 C32 C31 -117.4(2) . . . . ?
N16 N17 C32 C31 63.9(2) . . . . ?
O2 C31 C32 N15 54.6(3) . . . . ?
N18 C31 C32 N15 -129.7(2) . . . . ?
O2 C31 C32 N17 -67.7(2) . . . . ?
N18 C31 C32 N17 108.0(2) . . . . ?

_refine_diff_density_max         0.588
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.068

####################################################################### 
# 
# 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_16rfs03_sq_sqd
_database_code_depnum_ccdc_archive 'CCDC 1870006'
_audit_update_record             
;
2018-09-26 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H17 Br2 N9 O7 Re2'
_chemical_formula_weight         1051.66

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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.4206(4)
_cell_length_b                   13.4302(5)
_cell_length_c                   13.6824(6)
_cell_angle_alpha                63.050(2)
_cell_angle_beta                 78.311(2)
_cell_angle_gamma                71.078(2)
_cell_volume                     1611.16(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9889
_cell_measurement_theta_min      3.63
_cell_measurement_theta_max      68.18

_exptl_crystal_description       'transparent prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    17.835
_shelx_estimated_absorpt_T_min   0.135
_shelx_estimated_absorpt_T_max   0.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   'SADABS-2014/7, Bruker AXS'
_exptl_absorpt_special_details   ?


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36153
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.632
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             5772
_reflns_number_gt                5643
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       APEX2
_computing_data_reduction        
;
SADABS (Bruker, 2013) and XPREP (Bruker, 2013)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'

_refine_special_details          
;
All nonhydrogen atoms were located in a single difference Fourier electron
 density maps and refined using anisotropic diplacement parameters. All C-H
 hydrogen atoms were placed in calculated positions with Uiso = 1.2xUeqiv
 of the connected C atoms. Those H atoms attached
 to nitrogen were located in Fourier diff maps and assigned Uiso = 1.2xUeqiv
 with N-H bond distances restrained to 0.85(2) angstroms.

;

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 0.000 0.500 211 49 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
Refinement with the un-SQUEEZED model resulted in a final R value of 3.06%.  
 Significant somewhat identifiable residual electron density was observed at
 the 3-4 e/A3 level suggesting the possible presence of disorded solvent
 (ether and/or acetone).  

 With P-1 and Z=2, the 49 electrons correspond to 24.5 electrons 
 (49 electrons/2 = 24.5) in the asymmetric unit. Given electrons
 associated with acetone (32) and ether (42), neither solvent is
 an ideal match for the available electrons.  Since ether is 
 closest in electron count, the formula should reflect the 
 incllusion of one molecule of ether per unit cell.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0245P)²+3.8040P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5772
_refine_ls_number_parameters     382
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0527
_refine_ls_wR_factor_gt          0.0523
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re -0.30779(2) 0.15238(2) 0.13777(2) 0.01100(5) Uani 1 1 d . . . . .
Re2 Re -0.09773(2) 0.49389(2) -0.19515(2) 0.01236(5) Uani 1 1 d . . . . .
Br1 Br -0.25117(4) -0.07221(3) 0.19596(3) 0.02074(9) Uani 1 1 d . . . . .
Br2 Br -0.56682(6) 0.36173(4) -0.37908(4) 0.03593(12) Uani 1 1 d . . . . .
O1 O -0.2907(2) 0.4514(2) -0.1654(2) 0.0155(5) Uani 1 1 d . . . . .
O2 O -0.3668(3) 0.4101(2) 0.0841(2) 0.0268(6) Uani 1 1 d . . . . .
O3 O -0.0266(3) 0.1177(3) 0.2044(2) 0.0288(7) Uani 1 1 d . . . . .
O4 O -0.3941(3) 0.1177(3) 0.3760(3) 0.0343(7) Uani 1 1 d . . . . .
O5 O 0.1692(3) 0.5637(3) -0.2548(3) 0.0320(7) Uani 1 1 d . . . . .
O6 O -0.1695(3) 0.5897(3) -0.0194(2) 0.0254(6) Uani 1 1 d . . . . .
O7 O 0.0538(3) 0.2577(2) -0.0267(2) 0.0267(6) Uani 1 1 d . . . . .
N1 N -0.4709(3) 0.4402(3) -0.2255(3) 0.0144(6) Uani 1 1 d D . . . .
H30 H -0.511(4) 0.452(4) -0.280(3) 0.017 Uiso 1 1 d D U . . .
N2 N -0.2478(3) 0.1651(2) -0.0302(2) 0.0123(6) Uani 1 1 d . . . . .
N3 N -0.3336(3) 0.1945(2) -0.1088(3) 0.0139(6) Uani 1 1 d . . . . .
N4 N -0.5044(3) 0.1527(2) 0.1048(3) 0.0146(6) Uani 1 1 d . . . . .
N5 N -0.5389(3) 0.1706(3) 0.0055(3) 0.0155(6) Uani 1 1 d . . . . .
N6 N -0.2118(3) 0.6511(3) -0.3194(3) 0.0158(6) Uani 1 1 d . . . . .
N7 N -0.2924(3) 0.6457(3) -0.3825(3) 0.0153(6) Uani 1 1 d . . . . .
N8 N -0.0715(3) 0.4304(3) -0.3210(2) 0.0150(6) Uani 1 1 d . . . . .
N9 N -0.1780(3) 0.4598(3) -0.3819(2) 0.0149(6) Uani 1 1 d . . . . .
C1 C -0.1229(4) 0.1350(3) -0.0747(3) 0.0145(7) Uani 1 1 d . . . . .
H1 H -0.0416 0.1092 -0.0388 0.017 Uiso 1 1 calc R U . . .
C2 C -0.1272(4) 0.1461(3) -0.1804(3) 0.0177(8) Uani 1 1 d . . . . .
H2 H -0.0524 0.1308 -0.2290 0.021 Uiso 1 1 calc R U . . .
C3 C -0.2625(4) 0.1840(3) -0.1990(3) 0.0171(7) Uani 1 1 d . . . . .
H3 H -0.2997 0.2000 -0.2642 0.020 Uiso 1 1 calc R U . . .
C4 C -0.5944(4) 0.1012(3) 0.1783(4) 0.0226(8) Uani 1 1 d . . . . .
H4 H -0.5950 0.0767 0.2553 0.027 Uiso 1 1 calc R U . . .
C5 C -0.6873(4) 0.0880(3) 0.1279(4) 0.0270(9) Uani 1 1 d . . . . .
H5 H -0.7613 0.0548 0.1628 0.032 Uiso 1 1 calc R U . . .
C6 C -0.6503(4) 0.1328(3) 0.0178(4) 0.0220(8) Uani 1 1 d . . . . .
H6 H -0.6938 0.1368 -0.0391 0.026 Uiso 1 1 calc R U . . .
C7 C -0.4798(4) 0.2416(3) -0.0984(3) 0.0152(7) Uani 1 1 d . . . . .
H7 H -0.5191 0.2389 -0.1577 0.018 Uiso 1 1 calc R U . . .
C8 C -0.5213(4) 0.3693(3) -0.1160(3) 0.0145(7) Uani 1 1 d . . . . .
H8A H -0.6216 0.3971 -0.1085 0.017 Uiso 1 1 calc R U . . .
H8B H -0.4831 0.3764 -0.0595 0.017 Uiso 1 1 calc R U . . .
C9 C -0.3586(3) 0.4723(3) -0.2422(3) 0.0121(7) Uani 1 1 d . . . . .
C10 C -0.3084(4) 0.5340(3) -0.3622(3) 0.0148(7) Uani 1 1 d . . . . .
H10 H -0.3753 0.5459 -0.4122 0.018 Uiso 1 1 calc R U . . .
C11 C -0.2120(4) 0.7628(3) -0.3621(3) 0.0201(8) Uani 1 1 d . . . . .
H11 H -0.1653 0.7934 -0.3340 0.024 Uiso 1 1 calc R U . . .
C12 C -0.2900(4) 0.8282(3) -0.4533(4) 0.0251(9) Uani 1 1 d . . . . .
H12 H -0.3053 0.9090 -0.4983 0.030 Uiso 1 1 calc R U . . .
C13 C -0.3397(4) 0.7513(3) -0.4643(3) 0.0208(8) Uani 1 1 d . . . . .
H13 H -0.3968 0.7688 -0.5191 0.025 Uiso 1 1 calc R U . . .
C14 C 0.0314(4) 0.3619(3) -0.3569(3) 0.0178(8) Uani 1 1 d . . . . .
H14 H 0.1196 0.3280 -0.3300 0.021 Uiso 1 1 calc R U . . .
C15 C -0.0099(4) 0.3476(3) -0.4399(3) 0.0205(8) Uani 1 1 d . . . . .
H15 H 0.0435 0.3027 -0.4784 0.025 Uiso 1 1 calc R U . . .
C16 C -0.1430(4) 0.4113(3) -0.4544(3) 0.0180(8) Uani 1 1 d . . . . .
H16 H -0.1997 0.4197 -0.5055 0.022 Uiso 1 1 calc R U . . .
C17 C -0.3462(4) 0.3142(3) 0.1007(3) 0.0176(8) Uani 1 1 d . . . . .
C18 C -0.1295(4) 0.1328(3) 0.1750(3) 0.0176(8) Uani 1 1 d . . . . .
C19 C -0.3634(4) 0.1303(3) 0.2858(3) 0.0201(8) Uani 1 1 d . . . . .
C20 C 0.0695(4) 0.5371(3) -0.2326(3) 0.0186(8) Uani 1 1 d . . . . .
C21 C -0.1423(4) 0.5544(3) -0.0852(3) 0.0173(8) Uani 1 1 d . . . . .
C22 C -0.0035(4) 0.3461(3) -0.0889(3) 0.0188(8) 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
Re1 C19 1.902(4) . ?
Re1 C17 1.913(4) . ?
Re1 C18 1.930(4) . ?
Re1 N4 2.183(3) . ?
Re1 N2 2.198(3) . ?
Re1 Br1 2.6343(4) . ?
Re2 C20 1.914(4) . ?
Re2 C22 1.927(4) . ?
Re2 C21 1.928(4) . ?
Re2 N6 2.168(3) . ?
Re2 O1 2.177(2) . ?
Re2 N8 2.180(3) . ?
O1 C9 1.259(4) . ?
O2 C17 1.154(5) . ?
O3 C18 1.147(5) . ?
O4 C19 1.157(5) . ?
O5 C20 1.146(5) . ?
O6 C21 1.146(5) . ?
O7 C22 1.150(5) . ?
N1 C9 1.318(5) . ?
N1 C8 1.462(5) . ?
N1 H30 0.855(19) . ?
N2 C1 1.337(5) . ?
N2 N3 1.374(4) . ?
N3 C3 1.346(5) . ?
N3 C7 1.453(5) . ?
N4 C4 1.333(5) . ?
N4 N5 1.371(4) . ?
N5 C6 1.363(5) . ?
N5 C7 1.451(5) . ?
N6 C11 1.339(5) . ?
N6 N7 1.360(4) . ?
N7 C13 1.356(5) . ?
N7 C10 1.456(4) . ?
N8 C14 1.339(5) . ?
N8 N9 1.369(4) . ?
N9 C16 1.353(5) . ?
N9 C10 1.459(5) . ?
C1 C2 1.393(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.370(5) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.392(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.369(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.541(5) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.536(5) . ?
C10 H10 1.0000 . ?
C11 C12 1.394(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.370(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.401(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.372(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 Re1 C17 87.63(16) . . ?
C19 Re1 C18 85.36(17) . . ?
C17 Re1 C18 88.45(15) . . ?
C19 Re1 N4 93.53(15) . . ?
C17 Re1 N4 98.05(13) . . ?
C18 Re1 N4 173.36(13) . . ?
C19 Re1 N2 175.44(14) . . ?
C17 Re1 N2 96.51(13) . . ?
C18 Re1 N2 96.65(14) . . ?
N4 Re1 N2 84.01(11) . . ?
C19 Re1 Br1 90.60(12) . . ?
C17 Re1 Br1 177.76(11) . . ?
C18 Re1 Br1 90.03(11) . . ?
N4 Re1 Br1 83.43(8) . . ?
N2 Re1 Br1 85.30(7) . . ?
C20 Re2 C22 87.94(15) . . ?
C20 Re2 C21 89.26(16) . . ?
C22 Re2 C21 89.68(16) . . ?
C20 Re2 N6 95.80(14) . . ?
C22 Re2 N6 174.62(13) . . ?
C21 Re2 N6 94.22(14) . . ?
C20 Re2 O1 175.74(13) . . ?
C22 Re2 O1 95.35(12) . . ?
C21 Re2 O1 93.45(12) . . ?
N6 Re2 O1 80.74(11) . . ?
C20 Re2 N8 96.27(14) . . ?
C22 Re2 N8 93.62(14) . . ?
C21 Re2 N8 173.65(13) . . ?
N6 Re2 N8 82.15(11) . . ?
O1 Re2 N8 80.85(10) . . ?
C9 O1 Re2 122.6(2) . . ?
C9 N1 C8 122.4(3) . . ?
C9 N1 H30 120(3) . . ?
C8 N1 H30 117(3) . . ?
C1 N2 N3 104.8(3) . . ?
C1 N2 Re1 128.4(2) . . ?
N3 N2 Re1 126.5(2) . . ?
C3 N3 N2 110.8(3) . . ?
C3 N3 C7 125.4(3) . . ?
N2 N3 C7 123.5(3) . . ?
C4 N4 N5 104.8(3) . . ?
C4 N4 Re1 126.6(3) . . ?
N5 N4 Re1 125.5(2) . . ?
C6 N5 N4 111.2(3) . . ?
C6 N5 C7 125.3(3) . . ?
N4 N5 C7 122.4(3) . . ?
C11 N6 N7 105.2(3) . . ?
C11 N6 Re2 133.9(3) . . ?
N7 N6 Re2 120.4(2) . . ?
C13 N7 N6 111.0(3) . . ?
C13 N7 C10 129.1(3) . . ?
N6 N7 C10 119.7(3) . . ?
C14 N8 N9 105.4(3) . . ?
C14 N8 Re2 134.7(3) . . ?
N9 N8 Re2 120.0(2) . . ?
C16 N9 N8 111.5(3) . . ?
C16 N9 C10 129.0(3) . . ?
N8 N9 C10 119.6(3) . . ?
N2 C1 C2 111.4(3) . . ?
N2 C1 H1 124.3 . . ?
C2 C1 H1 124.3 . . ?
C3 C2 C1 105.1(3) . . ?
C3 C2 H2 127.4 . . ?
C1 C2 H2 127.4 . . ?
N3 C3 C2 107.9(3) . . ?
N3 C3 H3 126.0 . . ?
C2 C3 H3 126.0 . . ?
N4 C4 C5 111.4(4) . . ?
N4 C4 H4 124.3 . . ?
C5 C4 H4 124.3 . . ?
C6 C5 C4 105.9(3) . . ?
C6 C5 H5 127.0 . . ?
C4 C5 H5 127.0 . . ?
N5 C6 C5 106.7(4) . . ?
N5 C6 H6 126.7 . . ?
C5 C6 H6 126.7 . . ?
N5 C7 N3 111.5(3) . . ?
N5 C7 C8 111.1(3) . . ?
N3 C7 C8 113.1(3) . . ?
N5 C7 H7 106.9 . . ?
N3 C7 H7 106.9 . . ?
C8 C7 H7 106.9 . . ?
N1 C8 C7 109.8(3) . . ?
N1 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
O1 C9 N1 123.2(3) . . ?
O1 C9 C10 120.0(3) . . ?
N1 C9 C10 116.8(3) . . ?
N7 C10 N9 110.1(3) . . ?
N7 C10 C9 110.4(3) . . ?
N9 C10 C9 107.7(3) . . ?
N7 C10 H10 109.5 . . ?
N9 C10 H10 109.5 . . ?
C9 C10 H10 109.5 . . ?
N6 C11 C12 111.0(3) . . ?
N6 C11 H11 124.5 . . ?
C12 C11 H11 124.5 . . ?
C13 C12 C11 105.3(3) . . ?
C13 C12 H12 127.3 . . ?
C11 C12 H12 127.3 . . ?
N7 C13 C12 107.4(3) . . ?
N7 C13 H13 126.3 . . ?
C12 C13 H13 126.3 . . ?
N8 C14 C15 110.2(3) . . ?
N8 C14 H14 124.9 . . ?
C15 C14 H14 124.9 . . ?
C16 C15 C14 106.3(3) . . ?
C16 C15 H15 126.9 . . ?
C14 C15 H15 126.9 . . ?
N9 C16 C15 106.7(3) . . ?
N9 C16 H16 126.7 . . ?
C15 C16 H16 126.7 . . ?
O2 C17 Re1 176.1(3) . . ?
O3 C18 Re1 175.4(3) . . ?
O4 C19 Re1 178.1(4) . . ?
O5 C20 Re2 179.4(4) . . ?
O6 C21 Re2 179.4(3) . . ?
O7 C22 Re2 179.1(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N2 N3 C3 -0.9(4) . . . . ?
Re1 N2 N3 C3 -174.6(2) . . . . ?
C1 N2 N3 C7 -175.0(3) . . . . ?
Re1 N2 N3 C7 11.2(4) . . . . ?
C4 N4 N5 C6 1.2(4) . . . . ?
Re1 N4 N5 C6 162.2(2) . . . . ?
C4 N4 N5 C7 169.8(3) . . . . ?
Re1 N4 N5 C7 -29.3(4) . . . . ?
C11 N6 N7 C13 1.2(4) . . . . ?
Re2 N6 N7 C13 -171.7(3) . . . . ?
C11 N6 N7 C10 176.5(3) . . . . ?
Re2 N6 N7 C10 3.6(4) . . . . ?
C14 N8 N9 C16 -0.1(4) . . . . ?
Re2 N8 N9 C16 -179.2(2) . . . . ?
C14 N8 N9 C10 179.3(3) . . . . ?
Re2 N8 N9 C10 0.3(4) . . . . ?
N3 N2 C1 C2 0.9(4) . . . . ?
Re1 N2 C1 C2 174.5(2) . . . . ?
N2 C1 C2 C3 -0.6(4) . . . . ?
N2 N3 C3 C2 0.5(4) . . . . ?
C7 N3 C3 C2 174.5(3) . . . . ?
C1 C2 C3 N3 0.1(4) . . . . ?
N5 N4 C4 C5 -1.2(4) . . . . ?
Re1 N4 C4 C5 -161.9(3) . . . . ?
N4 C4 C5 C6 0.7(5) . . . . ?
N4 N5 C6 C5 -0.8(4) . . . . ?
C7 N5 C6 C5 -168.9(3) . . . . ?
C4 C5 C6 N5 0.1(4) . . . . ?
C6 N5 C7 N3 -131.4(4) . . . . ?
N4 N5 C7 N3 61.7(4) . . . . ?
C6 N5 C7 C8 101.5(4) . . . . ?
N4 N5 C7 C8 -65.4(4) . . . . ?
C3 N3 C7 N5 135.3(3) . . . . ?
N2 N3 C7 N5 -51.4(4) . . . . ?
C3 N3 C7 C8 -98.7(4) . . . . ?
N2 N3 C7 C8 74.6(4) . . . . ?
C9 N1 C8 C7 -98.9(4) . . . . ?
N5 C7 C8 N1 -174.7(3) . . . . ?
N3 C7 C8 N1 59.0(4) . . . . ?
Re2 O1 C9 N1 175.3(2) . . . . ?
Re2 O1 C9 C10 -2.2(4) . . . . ?
C8 N1 C9 O1 -4.7(5) . . . . ?
C8 N1 C9 C10 172.9(3) . . . . ?
C13 N7 C10 N9 111.1(4) . . . . ?
N6 N7 C10 N9 -63.3(4) . . . . ?
C13 N7 C10 C9 -130.1(4) . . . . ?
N6 N7 C10 C9 55.6(4) . . . . ?
C16 N9 C10 N7 -120.1(4) . . . . ?
N8 N9 C10 N7 60.6(4) . . . . ?
C16 N9 C10 C9 119.5(4) . . . . ?
N8 N9 C10 C9 -59.8(4) . . . . ?
O1 C9 C10 N7 -57.7(4) . . . . ?
N1 C9 C10 N7 124.7(3) . . . . ?
O1 C9 C10 N9 62.6(4) . . . . ?
N1 C9 C10 N9 -115.1(3) . . . . ?
N7 N6 C11 C12 -1.1(4) . . . . ?
Re2 N6 C11 C12 170.3(3) . . . . ?
N6 C11 C12 C13 0.7(5) . . . . ?
N6 N7 C13 C12 -0.8(5) . . . . ?
C10 N7 C13 C12 -175.5(4) . . . . ?
C11 C12 C13 N7 0.1(5) . . . . ?
N9 N8 C14 C15 -0.2(4) . . . . ?
Re2 N8 C14 C15 178.6(3) . . . . ?
N8 C14 C15 C16 0.5(4) . . . . ?
N8 N9 C16 C15 0.4(4) . . . . ?
C10 N9 C16 C15 -178.9(3) . . . . ?
C14 C15 C16 N9 -0.5(4) . . . . ?

_refine_diff_density_max         1.499
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.112

