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

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

data_mo_annma45_0ma-auto_sq
_database_code_depnum_ccdc_archive 'CCDC 1829612'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H26 Cu N8 O, 3(F6 P)'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C20 H26 Cu F18 N8 O P3'
_chemical_formula_iupac          ?
_chemical_formula_weight         892.95
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_Int_Tables_number      12

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,z

_cell_length_a                   22.923(2)
_cell_length_b                   11.8528(11)
_cell_length_c                   15.482(3)
_cell_angle_alpha                90
_cell_angle_beta                 127.476(2)
_cell_angle_gamma                90
_cell_volume                     3338.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    5575
_cell_measurement_theta_min      2.2391
_cell_measurement_theta_max      26.2621
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear colourless'

_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.060
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    0.931
_exptl_crystal_density_meas_temp ?

# Permitted for _exptl_absorpt_correction_type :
# analytical     'analytical from crystal shape'
#                Example: de Meulenaer&Tompa: ABST
# cylinder       'cylindrical'
# gaussian       'Gaussian from crystal shape'
#                Example: PLATON/ABSG
# integration    'integration from crystal shape'
# multi-scan     'symmetry-related measurements'
#                Example: SADABS, MULABS
# none           'no absorption corr. applied'
# numerical      'numerical from crystal shape'
# psi-scan       'psi-scan corrections'
#                Example: PLATON/ABSP
# refdelf        'refined from delta-F'
#                Example: SHELXA,
# sphere         'spherical'
#                Example: PLATON/ABSS
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_T_max  0.7454


#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             F. Kaiser
scanspeed                           60 s per frame
dx                                  45 mm
385 frames measured in 4 data sets
omega-scans with delta_omega     = 1.0
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_monochromator  'Helios optic'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            19163
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             3111
# number of observed reflections (> n sig(I))
_reflns_number_gt                2420
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'


#===============================================================================

# 8. REFINEMENT DATA

_platon_squeeze_details          
;
The unit cell contains 4 disordered molecules of acetonitrile which were
treated as a diffuse contribution to the overall scattering without specific
atom positions by SQUEEZE/PLATON.
;

_refine_special_details          
;Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.,SQUEEZE,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0461P)²+57.8523P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom


# Permitted for _refine_ls_hydrogen_treatment :
# refall            - refined all H-atom parameters
# refxyz            - refined H-atom coordinates only
# refU              - refined H-atom U only
# noref             - no refinement of H-atom parameters
# constr            - H-atom parameters constrained
# hetero            - H-atom parameters constrained for H on C,
#                     all H-atom parameters refined for H on
#                     heteroatoms
# heteroxyz         - H-atom parameters constrained for H on C,
#                     refined H-atom coordinates only for H
#                     on heteroatoms
# heteroU           - H-atom parameters constrained for H on C,
#                     refined H-atom U's only for H on
#                     heteroatoms
# heteronoref       - H-atom parameters constrained for H on C,
#                     no refinement of H-atom parameters for
#                     H on heteroatoms
# hetero-mixed      - H-atom parameters constrained for H on C
#                     and some heteroatoms, all H-atom
#                     parameters refined for H on remaining
#                     heteroatoms.
# heteroxyz-mixed   - H-atom parameters constrained for H on C
#                     and some heteroatoms, refined H-atom
#                     coordinates only for H on remaining
#                     heteroatoms.
# heteroU-mixed     - H-atom parameters constrained for H on C
#                     and some heteroatoms, refined H-atom
#                     U's only for H on remaining heteroatoms
# heteronoref-mixed - H-atom parameters constrained for H on C
#                     and some heteroatoms, no refinement of
#                     H-atom parameters for H on remaining
#                     heteroatoms
# mixed   - some constrained, some independent
# undef   - H-atom parameters not defined
_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         3111
_refine_ls_number_parameters     342
_refine_ls_number_restraints     281
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0655
_refine_ls_wR_factor_ref         0.1561
_refine_ls_wR_factor_gt          0.1435
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.314
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.120

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu Uani 0.21419(5) 0.50000 0.22901(7) 1.000 0.0142(3) d STP . .
P2 P Uani 0.46514(11) 0.50000 0.79316(15) 1.000 0.0160(6) d STP . .
P1 P Uani 0.08353(11) 0.50000 0.32298(16) 1.000 0.0199(6) d STP . .
P3A P Uani 0.2176(6) 0.50000 -0.2028(11) 0.584(8) 0.0332(19) d SDT B 4
O1 O Uani 0.295(6) 0.50000 0.186(12) 0.496(12) 0.031(7) d SDT . 5
O1A O Uani 0.298(6) 0.50000 0.176(12) 0.506(12) 0.034(7) d SDT . 6
N1 N Uani 0.1169(2) 0.6000(4) 0.0161(3) 1.000 0.0225(14) d . . .
N2 N Uani 0.1454(2) 0.7183(4) 0.1409(3) 1.000 0.0181(12) d . . .
N3 N Uani 0.2442(2) 0.7185(4) 0.3326(3) 1.000 0.0180(12) d . . .
P3 P Uani 0.2126(8) 0.50000 -0.2218(15) 0.418(8) 0.029(3) d SDT B 3
N4 N Uani 0.3301(2) 0.6003(4) 0.4345(3) 1.000 0.0148(12) d . . .
F6 F Uani 0.3798(2) 0.50000 0.6903(4) 1.000 0.0361(16) d STP A .
F7 F Uani 0.4339(6) 0.50000 0.8600(8) 0.606(8) 0.061(4) d STU A 1
F7A F Uani 0.4588(6) 0.4074(13) 0.8584(10) 0.394(9) 0.071(3) d UP A 2
F8 F Uani 0.5494(3) 0.50000 0.8949(4) 1.000 0.0359(14) d STP A .
F9 F Uani 0.4922(5) 0.50000 0.7226(7) 0.606(8) 0.059(4) d STU A 1
F10 F Uani 0.4637(4) 0.3675(7) 0.7925(10) 0.606(9) 0.070(3) d UP A 1
F10A F Uani 0.4738(7) 0.4046(15) 0.7324(10) 0.394(9) 0.078(4) d UP A 2
C1 C Uani 0.1562(3) 0.6128(5) 0.1248(4) 1.000 0.0200(17) d . . .
C2 C Uani 0.0812(3) 0.7003(5) -0.0352(5) 1.000 0.0278(17) d . . .
C3 C Uani 0.0991(3) 0.7740(5) 0.0421(4) 1.000 0.0261(17) d . . .
C4 C Uani 0.1726(3) 0.7676(5) 0.2455(4) 1.000 0.0212(17) d . . .
C5 C Uani 0.2650(3) 0.6124(4) 0.3361(4) 1.000 0.0145(16) d . . .
C6 C Uani 0.2955(3) 0.7732(5) 0.4296(4) 1.000 0.0221(17) d . . .
C7 C Uani 0.3498(3) 0.6993(5) 0.4935(4) 1.000 0.0202(17) d . . .
C8 C Uani 0.3759(4) 0.50000 0.4675(6) 1.000 0.018(2) d STP . .
C9 C Uani 0.1198(5) 0.50000 -0.0350(6) 1.000 0.025(3) d STP . .
C10 C Uani 0.3327(18) 0.597(2) 0.1906(19) 0.495(12) 0.055(4) d DUP . 5
C10A C Uani 0.3232(17) 0.599(2) 0.1569(18) 0.505(12) 0.057(5) d DUP . 6
C11 C Uani 0.3035(10) 0.6718(16) 0.0950(14) 0.495(12) 0.064(4) d DUP . 5
C11A C Uani 0.3843(9) 0.6623(15) 0.2542(14) 0.505(12) 0.060(4) d DUP . 6
F2 F Uani 0.0622(3) 0.50000 0.2030(4) 1.000 0.0392(17) d STP . .
F3 F Uani 0.1434(2) 0.5946(4) 0.3597(3) 1.000 0.0515(16) d . . .
F4 F Uani 0.1045(2) 0.50000 0.4421(3) 1.000 0.0265(14) d STP . .
F5 F Uani 0.0233(2) 0.5949(4) 0.2858(3) 1.000 0.0511(16) d . . .
F11A F Uani 0.2311(5) 0.6289(7) -0.1826(8) 0.583(9) 0.060(3) d DUP B 4
F12A F Uani 0.3010(5) 0.50000 -0.1580(9) 0.584(8) 0.050(3) d SDT B 4
F13A F Uani 0.2399(8) 0.50000 -0.0872(10) 0.584(8) 0.086(4) d SDT B 4
F14A F Uani 0.1375(5) 0.50000 -0.2352(11) 0.584(8) 0.066(4) d SDT B 4
F15A F Uani 0.2012(8) 0.50000 -0.3152(9) 0.584(8) 0.076(4) d SDT B 4
F11 F Uani 0.1989(7) 0.6289(8) -0.2445(11) 0.417(9) 0.052(3) d DUP B 3
F12 F Uani 0.2898(9) 0.50000 -0.1150(13) 0.418(8) 0.091(5) d SDT B 3
F13 F Uani 0.1387(9) 0.50000 -0.3290(13) 0.418(8) 0.104(5) d SDT B 3
F14 F Uani 0.2418(8) 0.50000 -0.2960(11) 0.418(8) 0.031(3) d SDT B 3
F15 F Uani 0.1868(9) 0.50000 -0.1491(13) 0.418(8) 0.056(4) d SDT B 3
H4AB H Uiso 0.17770 0.85030 0.24310 1.000 0.0260 c RU . .
H2 H Uiso 0.04970 0.71380 -0.11140 1.000 0.0340 c RU . .
H8AB H Uiso 0.40070 0.50000 0.43300 1.000 0.0210 c RUP . .
H3 H Uiso 0.08330 0.85020 0.03170 1.000 0.0320 c RU . .
H9AB H Uiso 0.16590 0.50000 -0.02760 1.000 0.0290 c RUP . .
H4A H Uiso 0.13700 0.75320 0.26050 1.000 0.0260 c RU . .
H6 H Uiso 0.29290 0.84870 0.44750 1.000 0.0270 c RU . .
H7 H Uiso 0.39320 0.71240 0.56510 1.000 0.0230 c RU . .
H8A H Uiso 0.41410 0.50000 0.54740 1.000 0.0210 c RUP . .
H9A H Uiso 0.07790 0.50000 -0.11350 1.000 0.0290 c RUP . .
H10A H Uiso 0.38160 0.57070 0.21510 0.495(12) 0.0660 c RUP . 5
H10B H Uiso 0.34110 0.64490 0.24940 0.495(12) 0.0660 c RUP . 5
H10C H Uiso 0.28080 0.65090 0.11290 0.505(12) 0.0680 c RUP . 6
H10D H Uiso 0.33930 0.57880 0.11220 0.505(12) 0.0680 c RUP . 6
H11A H Uiso 0.30020 0.62960 0.03780 0.495(12) 0.0950 c RUP . 5
H11B H Uiso 0.33650 0.73640 0.11730 0.495(12) 0.0950 c RUP . 5
H11C H Uiso 0.25450 0.69880 0.06720 0.495(12) 0.0950 c RUP . 5
H11D H Uiso 0.42880 0.61580 0.29430 0.505(12) 0.0900 c RUP . 6
H11E H Uiso 0.37050 0.68030 0.30140 0.505(12) 0.0900 c RUP . 6
H11F H Uiso 0.39360 0.73230 0.23070 0.505(12) 0.0900 c RUP . 6


#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1A 2.51(18) . . yes
Cu1 O1 2.32(18) . . yes
Cu1 C1 1.884(6) . . yes
Cu1 C5 1.879(5) . . yes
Cu1 C1 1.884(6) . 4_565 yes
Cu1 C5 1.879(5) . 4_565 yes
P2 F10A 1.559(17) . . yes
P2 F10 1.571(8) . 4_565 yes
P2 F7A 1.557(15) . 4_565 yes
P2 F10A 1.559(17) . 4_565 yes
P2 F8 1.584(7) . . yes
P2 F9 1.550(12) . . yes
P2 F10 1.571(8) . . yes
P2 F7A 1.557(15) . . yes
P2 F6 1.604(6) . . yes
P2 F7 1.577(15) . . yes
P1 F3 1.586(5) . 4_565 yes
P1 F2 1.608(6) . . yes
P1 F3 1.586(5) . . yes
P1 F4 1.598(5) . . yes
P1 F5 1.592(5) . . yes
P1 F5 1.592(5) . 4_565 yes
P3A F11A 1.552(9) . 4_565 yes
P3A F12A 1.59(2) . . yes
P3A F11A 1.552(9) . . yes
P3A F15A 1.54(2) . . yes
P3A F13A 1.53(2) . . yes
P3A F14A 1.58(2) . . yes
O1 C10 1.41(10) . 4_565 yes
O1 C10 1.41(10) . . yes
O1A C10A 1.42(10) . 4_565 yes
O1A C10A 1.42(10) . . yes
N1 C9 1.449(7) . . yes
N1 C2 1.387(8) . . yes
N1 C1 1.350(6) . . yes
N2 C1 1.328(8) . . yes
N2 C3 1.388(7) . . yes
N2 C4 1.457(7) . . yes
N3 C4 1.469(8) . . yes
P3 F13 1.48(3) . . yes
P3 F14 1.64(3) . . yes
P3 F12 1.52(3) . . yes
P3 F11 1.556(10) . 4_565 yes
N3 C5 1.334(7) . . yes
P3 F15 1.56(3) . . yes
P3 F11 1.556(10) . . yes
N3 C6 1.382(7) . . yes
N4 C8 1.457(8) . . yes
N4 C5 1.342(7) . . yes
N4 C7 1.383(7) . . yes
C2 C3 1.329(8) . . no
C6 C7 1.341(9) . . no
C10 C11 1.49(3) . . no
C10A C11A 1.49(3) . . no
C2 H2 0.9500 . . no
C3 H3 0.9500 . . no
C4 H4A 0.9900 . . no
C4 H4AB 0.9900 . . no
C6 H6 0.9500 . . no
C7 H7 0.9500 . . no
C8 H8AB 0.9900 . . no
C8 H8A 0.9900 . . no
C9 H9A 0.9900 . . no
C9 H9AB 0.9900 . . no
C10 H10A 0.9900 . . no
C10 H10B 0.9900 . . no
C10A H10C 0.9900 . . no
C10A H10D 0.9900 . . no
C11 H11C 0.9800 . . no
C11 H11B 0.9800 . . no
C11 H11A 0.9800 . . no
C11A H11F 0.9800 . . no
C11A H11D 0.9800 . . no
C11A H11E 0.9800 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1A Cu1 C1 90(2) . . . yes
O1A Cu1 C5 96(2) . . . yes
O1A Cu1 C1 90(2) . . 4_565 yes
O1A Cu1 C5 96(2) . . 4_565 yes
O1 Cu1 C1 91(3) . . . yes
O1 Cu1 C5 95(3) . . . yes
O1 Cu1 C1 91(3) . . 4_565 yes
O1 Cu1 C5 95(3) . . 4_565 yes
C1 Cu1 C5 89.3(2) . . . yes
C1 Cu1 C1 90.4(2) . . 4_565 yes
C1 Cu1 C5 174.1(3) . . 4_565 yes
C1 Cu1 C5 174.1(3) 4_565 . . yes
C5 Cu1 C5 90.3(2) . . 4_565 yes
C1 Cu1 C5 89.3(2) 4_565 . 4_565 yes
F8 P2 F10A 94.3(6) . . . yes
F8 P2 F10 90.8(5) . . 4_565 yes
F7A P2 F8 83.9(6) 4_565 . . yes
F8 P2 F10A 94.3(6) . . 4_565 yes
F9 P2 F10 90.6(5) . . . yes
F9 P2 F10 90.6(5) . . 4_565 yes
F10 P2 F10 178.0(7) . . 4_565 yes
F7A P2 F10A 88.7(8) . . . yes
F7A P2 F7A 89.6(8) . . 4_565 yes
F7A P2 F10A 177.6(8) . . 4_565 yes
F7A P2 F10A 177.6(7) 4_565 . . yes
F10A P2 F10A 93.0(9) . . 4_565 yes
F7A P2 F10A 88.7(8) 4_565 . 4_565 yes
F8 P2 F9 86.1(5) . . . yes
F8 P2 F10 90.8(5) . . . yes
F6 P2 F7 83.4(5) . . . yes
F6 P2 F8 179.9(4) . . . yes
F6 P2 F9 94.0(4) . . . yes
F6 P2 F10 89.2(5) . . . yes
F6 P2 F7A 96.0(6) . . . yes
F6 P2 F10A 85.8(6) . . . yes
F6 P2 F10 89.2(5) . . 4_565 yes
F6 P2 F7A 96.0(6) . . 4_565 yes
F6 P2 F10A 85.8(6) . . 4_565 yes
F7 P2 F8 96.5(5) . . . yes
F7 P2 F9 177.4(6) . . . yes
F7 P2 F10 89.3(5) . . . yes
F7 P2 F10 89.3(5) . . 4_565 yes
F7A P2 F8 83.9(6) . . . yes
F2 P1 F3 90.2(3) . . . yes
F2 P1 F4 179.8(4) . . . yes
F2 P1 F5 89.7(3) . . . yes
F2 P1 F3 90.2(3) . . 4_565 yes
F2 P1 F5 89.7(3) . . 4_565 yes
F3 P1 F4 90.0(2) . . . yes
F3 P1 F5 90.1(3) . . . yes
F3 P1 F3 90.0(3) . . 4_565 yes
F3 P1 F5 179.9(3) . . 4_565 yes
F4 P1 F5 90.2(2) . . . yes
F3 P1 F4 90.0(2) 4_565 . . yes
F4 P1 F5 90.2(2) . . 4_565 yes
F3 P1 F5 179.9(2) 4_565 . . yes
F5 P1 F5 89.9(3) . . 4_565 yes
F3 P1 F5 90.1(3) 4_565 . 4_565 yes
F11A P3A F12A 82.7(8) . . . yes
F11A P3A F13A 83.2(6) . . . yes
F12A P3A F13A 91.9(11) . . . yes
F12A P3A F14A 174.3(12) . . . yes
F12A P3A F15A 84.0(12) . . . yes
F11A P3A F12A 82.7(8) 4_565 . . yes
F13A P3A F14A 82.4(12) . . . yes
F13A P3A F15A 175.8(16) . . . yes
F11A P3A F13A 83.2(6) 4_565 . . yes
F14A P3A F15A 101.7(12) . . . yes
F11A P3A F14A 96.6(8) 4_565 . . yes
F11A P3A F15A 96.3(7) 4_565 . . yes
F11A P3A F11A 159.6(12) . . 4_565 yes
F11A P3A F14A 96.6(8) . . . yes
F11A P3A F15A 96.3(7) . . . yes
Cu1 O1 C10 124(6) . . 4_565 yes
C10 O1 C10 109(13) . . 4_565 yes
Cu1 O1 C10 124(6) . . . yes
Cu1 O1A C10A 124(6) . . 4_565 yes
C10A O1A C10A 112(13) . . 4_565 yes
Cu1 O1A C10A 124(6) . . . yes
C1 N1 C2 109.4(5) . . . yes
C2 N1 C9 126.6(5) . . . yes
C1 N1 C9 123.7(5) . . . yes
C1 N2 C3 110.3(4) . . . yes
C3 N2 C4 123.9(5) . . . yes
C1 N2 C4 125.7(4) . . . yes
F11 P3 F11 158.0(16) . . 4_565 yes
F11 P3 F14 87.4(10) . . . yes
F11 P3 F15 92.9(11) . . . yes
F11 P3 F12 100.8(9) . . . yes
F11 P3 F13 79.1(9) . . . yes
F13 P3 F15 97.5(17) . . . yes
F11 P3 F13 79.1(9) 4_565 . . yes
C5 N3 C6 110.6(5) . . . yes
C4 N3 C6 123.3(5) . . . yes
C4 N3 C5 125.7(4) . . . yes
F11 P3 F12 100.8(9) 4_565 . . yes
F13 P3 F14 83.8(14) . . . yes
F12 P3 F14 93.5(16) . . . yes
F12 P3 F15 85.2(14) . . . yes
F14 P3 F15 178.7(17) . . . yes
F11 P3 F14 87.4(10) 4_565 . . yes
F11 P3 F15 92.9(11) 4_565 . . yes
F12 P3 F13 177(2) . . . yes
C7 N4 C8 125.8(5) . . . yes
C5 N4 C7 110.5(5) . . . yes
C5 N4 C8 123.5(5) . . . yes
Cu1 C1 N1 125.2(4) . . . yes
Cu1 C1 N2 128.5(4) . . . yes
N1 C1 N2 106.3(5) . . . yes
N1 C2 C3 107.3(5) . . . yes
N2 C3 C2 106.9(5) . . . yes
N2 C4 N3 110.2(5) . . . yes
Cu1 C5 N3 128.2(4) . . . yes
Cu1 C5 N4 126.2(4) . . . yes
N3 C5 N4 105.7(4) . . . yes
N3 C6 C7 106.8(5) . . . yes
N4 C7 C6 106.5(5) . . . yes
N4 C8 N4 109.3(7) . . 4_565 yes
N1 C9 N1 109.8(7) . . 4_565 yes
O1 C10 C11 123(6) . . . yes
O1A C10A C11A 117(6) . . . yes
C3 C2 H2 126.00 . . . no
N1 C2 H2 126.00 . . . no
N2 C3 H3 127.00 . . . no
C2 C3 H3 127.00 . . . no
N2 C4 H4AB 110.00 . . . no
N2 C4 H4A 110.00 . . . no
H4AB C4 H4A 108.00 . . . no
N3 C4 H4AB 110.00 . . . no
N3 C4 H4A 110.00 . . . no
C7 C6 H6 127.00 . . . no
N3 C6 H6 127.00 . . . no
C6 C7 H7 127.00 . . . no
N4 C7 H7 127.00 . . . no
N4 C8 H8AB 110.00 . . . no
N4 C8 H8AB 110.00 4_565 . . no
N4 C8 H8A 110.00 4_565 . . no
N4 C8 H8A 110.00 . . . no
H8AB C8 H8A 108.00 . . . no
H9AB C9 H9A 108.00 . . . no
N1 C9 H9AB 110.00 . . . no
N1 C9 H9A 110.00 . . . no
N1 C9 H9A 110.00 4_565 . . no
N1 C9 H9AB 110.00 4_565 . . no
O1 C10 H10B 107.00 . . . no
H10A C10 H10B 107.00 . . . no
C11 C10 H10B 107.00 . . . no
O1 C10 H10A 106.00 . . . no
C11 C10 H10A 107.00 . . . no
H10C C10A H10D 107.00 . . . no
C11A C10A H10D 108.00 . . . no
O1A C10A H10D 109.00 . . . no
C11A C10A H10C 108.00 . . . no
O1A C10A H10C 108.00 . . . no
C10 C11 H11C 109.00 . . . no
H11A C11 H11C 109.00 . . . no
H11B C11 H11C 109.00 . . . no
C10 C11 H11A 110.00 . . . no
C10 C11 H11B 109.00 . . . no
H11A C11 H11B 110.00 . . . no
C10A C11A H11D 109.00 . . . no
C10A C11A H11E 109.00 . . . no
C10A C11A H11F 109.00 . . . no
H11D C11A H11E 110.00 . . . no
H11D C11A H11F 110.00 . . . no
H11E C11A H11F 110.00 . . . no

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 Cu1 O1A C10A 43(10) . . . . no
C1 Cu1 O1A C10A -134(10) . . . 4_565 no
C5 Cu1 O1A C10A -46(10) . . . . no
C5 Cu1 O1A C10A 137(9) . . . 4_565 no
C1 Cu1 O1A C10A 134(10) 4_565 . . . no
C5 Cu1 O1A C10A -137(9) 4_565 . . . no
O1A Cu1 C1 N1 65(3) . . . . no
O1A Cu1 C1 N2 -115(3) . . . . no
C5 Cu1 C1 N1 160.8(7) . . . . no
C5 Cu1 C1 N2 -19.0(7) . . . . no
C1 Cu1 C1 N1 -25.1(7) 4_565 . . . no
C1 Cu1 C1 N2 155.1(7) 4_565 . . . no
O1A Cu1 C5 N3 109(3) . . . . no
O1A Cu1 C5 N4 -73(3) . . . . no
C1 Cu1 C5 N3 18.6(7) . . . . no
C1 Cu1 C5 N4 -163.2(7) . . . . no
C5 Cu1 C5 N3 -155.5(7) 4_565 . . . no
C5 Cu1 C5 N4 22.8(7) 4_565 . . . no
Cu1 O1A C10A C11A 78(10) . . . . no
C10A O1A C10A C11A -104(8) 4_565 . . . no
C9 N1 C1 Cu1 -6.4(11) . . . . no
C2 N1 C1 Cu1 -179.9(6) . . . . no
C2 N1 C1 N2 -0.1(8) . . . . no
C9 N1 C2 C3 -172.9(8) . . . . no
C1 N1 C9 N1 44.4(11) . . . 4_565 no
C2 N1 C9 N1 -143.2(7) . . . 4_565 no
C9 N1 C1 N2 173.4(7) . . . . no
C1 N1 C2 C3 0.4(9) . . . . no
C3 N2 C1 Cu1 179.6(6) . . . . no
C4 N2 C1 N1 175.0(6) . . . . no
C3 N2 C1 N1 -0.2(8) . . . . no
C4 N2 C1 Cu1 -5.2(11) . . . . no
C1 N2 C4 N3 33.7(9) . . . . no
C3 N2 C4 N3 -151.7(6) . . . . no
C1 N2 C3 C2 0.5(9) . . . . no
C4 N2 C3 C2 -174.9(7) . . . . no
C4 N3 C5 Cu1 5.5(10) . . . . no
C5 N3 C4 N2 -33.9(9) . . . . no
C6 N3 C4 N2 155.2(6) . . . . no
C6 N3 C5 N4 -1.1(8) . . . . no
C4 N3 C6 C7 173.2(6) . . . . no
C5 N3 C6 C7 1.1(8) . . . . no
C4 N3 C5 N4 -173.0(6) . . . . no
C6 N3 C5 Cu1 177.4(5) . . . . no
C8 N4 C5 Cu1 8.2(10) . . . . no
C7 N4 C5 Cu1 -177.9(5) . . . . no
C7 N4 C5 N3 0.7(8) . . . . no
C8 N4 C7 C6 173.7(7) . . . . no
C5 N4 C8 N4 -44.7(9) . . . 4_565 no
C7 N4 C8 N4 142.4(6) . . . 4_565 no
C5 N4 C7 C6 0.0(8) . . . . no
C8 N4 C5 N3 -173.2(6) . . . . no
N1 C2 C3 N2 -0.5(8) . . . . no
N3 C6 C7 N4 -0.7(8) . . . . no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
C4 H4AB F12A 0.9900 2.4300 3.284(10) 144.00 6_555 yes
C4 H4AB F14 0.9900 2.3200 3.191(12) 146.00 6_555 yes
C2 H2 F10 0.9500 2.4200 3.091(13) 128.00 5_454 yes
C3 H3 F8 0.9500 2.5000 3.242(6) 135.00 5_454 yes
C3 H3 F7A 0.9500 2.5500 3.131(15) 120.00 5_454 yes
C3 H3 F7A 0.9500 2.5100 3.020(17) 114.00 6_556 yes
C9 H9AB F13A 0.9900 2.3700 3.31(2) 157.00 . yes
C9 H9AB F15 0.9900 2.2100 2.96(3) 132.00 . yes
C4 H4A F3 0.9900 2.3700 3.036(8) 124.00 . yes
C4 H4A F10 0.9900 2.3500 3.045(15) 126.00 6_556 yes
C6 H6 F3 0.9500 2.4900 3.082(7) 121.00 7_566 yes
C7 H7 F10A 0.9500 2.4900 3.238(14) 135.00 4_565 yes
C8 H8A F9 0.9900 2.1600 3.145(11) 177.00 . yes
C9 H9A F5 0.9900 2.5000 3.406(9) 153.00 2_555 yes
C9 H9A F5 0.9900 2.5000 3.406(9) 153.00 3_565 yes
C11A H11D F9 0.9800 2.4100 3.26(2) 144.00 2_656 yes

# Loop Mechanism for Extra Tables(s)

# start Validation Reply Form
_vrf_PLAT076_mo_annma45_0ma-auto_sq 
;
PROBLEM: Occupancy      0.496 Less Than 1.0 for Sp.pos  .           O1     
RESPONSE: O1 is disordered and thus refined in two split layers, 
leading to occupancies other than 1.0. 
;
_vrf_PLAT088_mo_annma45_0ma-auto_sq 
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.10 Note  
RESPONSE: ...
;
_vrf_PLAT244_mo_annma45_0ma-auto_sq 
;
PROBLEM: Low    'Solvent' Ueq as Compared to Neighbors of         P2 Check 
RESPONSE: The hexafluoro phosphate counterions as well as the weakly coordinated
diethyl ether are heavily disordered and 
partly located at special positions, leading to bigger ellipsoids 
in these cases and furthermore increased R-values.
;
_vrf_PLAT250_mo_annma45_0ma-auto_sq 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.7 Note  
RESPONSE: The hexafluoro phosphate counterions as well as the weakly coordinated
diethyl etherare heavily disordered and 
partly located at special positions, leading to big ellipsoids 
in these cases and furthermore increased R-values.
;
_vrf_PLAT341_mo_annma45_0ma-auto_sq 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0085 Ang.  
RESPONSE: ...
;
_vrf_PLAT906_mo_annma45_0ma-auto_sq 
;
PROBLEM: Large K Value in the Analysis of Variance ......      3.911 Check 
RESPONSE: ...
;
_vrf_PLAT978_mo_annma45_0ma-auto_sq 
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: ...
;
# end Validation Reply Form

#loop_
#_publ_manuscript_incl_extra_item
#'_geom_extra_tableA_col_1'
#'_geom_extra_tableA_col_2'
#'_geom_extra_tableA_col_3'
#'_geom_extra_table_head_A'
#'_geom_table_footnote_A'
#'_geom_extra_tableB_col_1'
#'_geom_extra_tableB_col_2'
#'_geom_extra_tableB_col_3'
#'_geom_extra_table_head_B'
#'_geom_table_footnote_B'


#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
# ? ? ?


#
#loop_
#_geom_extra_tableB_col_1
#_geom_extra_tableB_col_2
#_geom_extra_tableB_col_3
# ? ? ?


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;


#===END
####################################################################### 
# 
# 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_annma37_2_0m-auto
_database_code_depnum_ccdc_archive 'CCDC 1829614'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C36 H44 Cu4 N16 O2 S2, 4(F6 P), 2(C2 H6 O S), C2 H3 N'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C42 H59 Cu4 F24 N17 O4 P4 S4'
_chemical_formula_iupac          ?
_chemical_formula_weight         1828.38
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C c'
_symmetry_Int_Tables_number      9

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-y,1/2+z
3 1/2+x,1/2+y,z
4 1/2+x,1/2-y,1/2+z

_cell_length_a                   26.950(2)
_cell_length_b                   11.6280(8)
_cell_length_c                   21.3978(16)
_cell_angle_alpha                90
_cell_angle_beta                 90.293(4)
_cell_angle_gamma                90
_cell_volume                     6705.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    106
_cell_measurement_reflns_used    9992
_cell_measurement_theta_min      2.4368
_cell_measurement_theta_max      26.9848
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear colourless'

_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.077
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             3672
_exptl_absorpt_coefficient_mu    1.593
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.6038
_exptl_absorpt_correction_T_max  0.7455

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           5 s per frame
dx                                  34 mm
1481 frames measured in 6 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
shutterless mode
;
_diffrn_ambient_temperature      106
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_monochromator  'Helios optic'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            80700
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             14207
# number of observed reflections (> n sig(I))
_reflns_number_gt                12904
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0870P)²+39.4392P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom


_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   ?

_chemical_absolute_configuration unk

_refine_ls_number_reflns         14207
_refine_ls_number_parameters     1077
_refine_ls_number_restraints     599
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1539
_refine_ls_wR_factor_gt          0.1459
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.127


# start Validation Reply Form
_vrf_PLAT341_annma37_2_0m-auto   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.019 Ang.  
RESPONSE: This is caused by the significant disorder in the counterions
and cocrystallized solvent molecules.
;
# end Validation Reply Form

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
Cu1 Cu 0.57977(12) 0.83138(11) 0.46856(14) 0.0126(3) Uani 1 1 d . . . . .
Cu2 Cu 0.49553(12) 0.68576(12) 0.41264(14) 0.0155(3) Uani 1 1 d . . . . .
Cu3 Cu 0.57139(12) 0.52650(11) 0.35340(14) 0.0138(3) Uani 1 1 d . . . . .
Cu4 Cu 0.65571(12) 0.67140(12) 0.40870(15) 0.0142(3) Uani 1 1 d . U . . .
N1 N 0.6218(4) 0.9995(9) 0.3813(5) 0.0126(11) Uani 1 1 d . U . . .
N2 N 0.5415(4) 1.0070(9) 0.3812(5) 0.0129(11) Uani 1 1 d . U . . .
N3 N 0.4762(4) 0.8937(9) 0.3377(5) 0.0151(12) Uani 1 1 d . U . . .
N4 N 0.4712(4) 0.7411(9) 0.2824(5) 0.0148(12) Uani 1 1 d . U . . .
N5 N 0.5298(5) 0.6154(9) 0.2367(5) 0.0168(12) Uani 1 1 d . U . . .
N6 N 0.6086(5) 0.6106(9) 0.2330(5) 0.0169(12) Uani 1 1 d . U . . .
N7 N 0.6744(4) 0.7241(9) 0.2771(5) 0.0140(9) Uani 1 1 d . U . . .
N8 N 0.6788(5) 0.8742(9) 0.3346(5) 0.0145(9) Uani 1 1 d . U . . .
N9 N 0.6218(4) 0.7371(9) 0.5853(5) 0.0153(12) Uani 1 1 d . U . . .
N10 N 0.5419(4) 0.7414(9) 0.5891(5) 0.0154(12) Uani 1 1 d . U . . .
N11 N 0.4757(4) 0.6318(9) 0.5450(5) 0.014(2) Uani 1 1 d . . . . .
N12 N 0.4717(4) 0.4818(9) 0.4871(5) 0.013(2) Uani 1 1 d . . . . .
N13 N 0.5296(4) 0.3582(8) 0.4407(5) 0.012(2) Uani 1 1 d . . . . .
N14 N 0.6082(4) 0.3489(9) 0.4404(5) 0.010(2) Uani 1 1 d . . . . .
N15 N 0.6753(4) 0.4617(9) 0.4823(5) 0.0138(9) Uani 1 1 d . U . . .
N16 N 0.6803(5) 0.6135(9) 0.5372(5) 0.0137(9) Uani 1 1 d . U . . .
C1 C 0.5806(5) 0.9456(9) 0.4043(5) 0.0127(11) Uani 1 1 d . U . . .
C2 C 0.6075(5) 1.0929(10) 0.3439(6) 0.0130(11) Uani 1 1 d . U . . .
H2 H 0.6290 1.1439 0.3223 0.016 Uiso 1 1 calc R U . . .
C3 C 0.5581(5) 1.0968(10) 0.3443(6) 0.0130(11) Uani 1 1 d . U . . .
H3 H 0.5379 1.1513 0.3230 0.016 Uiso 1 1 calc R U . . .
C16 C 0.6714(5) 0.9537(11) 0.3849(6) 0.0146(12) Uani 1 1 d . U . . .
H16A H 0.6959 1.0170 0.3821 0.018 Uiso 1 1 calc R U . . .
H16B H 0.6763 0.9140 0.4254 0.018 Uiso 1 1 calc R U . . .
C4 C 0.4904(6) 0.9729(11) 0.3868(6) 0.018(3) Uani 1 1 d . . . . .
H4A H 0.4690 1.0420 0.3847 0.022 Uiso 1 1 calc R U . . .
H4B H 0.4853 0.9359 0.4280 0.022 Uiso 1 1 calc R U . . .
C5 C 0.4855(5) 0.7796(10) 0.3403(6) 0.0148(12) Uani 1 1 d . U . . .
C6 C 0.4568(5) 0.9261(11) 0.2797(6) 0.0152(12) Uani 1 1 d . U . . .
H6 H 0.4482 1.0017 0.2667 0.018 Uiso 1 1 calc R U . . .
C7 C 0.4528(5) 0.8285(10) 0.2457(6) 0.0152(12) Uani 1 1 d . U . . .
H7 H 0.4398 0.8217 0.2045 0.018 Uiso 1 1 calc R U . . .
C8 C 0.4801(6) 0.6236(10) 0.2603(7) 0.017(3) Uani 1 1 d . . . . .
H8A H 0.4756 0.5685 0.2950 0.020 Uiso 1 1 calc R U . . .
H8B H 0.4560 0.6041 0.2268 0.020 Uiso 1 1 calc R U . . .
C9 C 0.5699(6) 0.5939(9) 0.2722(5) 0.0167(12) Uani 1 1 d . U . . .
C10 C 0.5428(6) 0.6456(10) 0.1757(6) 0.0174(12) Uani 1 1 d . U . . .
H10 H 0.5208 0.6644 0.1425 0.021 Uiso 1 1 calc R U . . .
C11 C 0.5922(6) 0.6427(11) 0.1734(6) 0.0175(12) Uani 1 1 d . U . . .
H11 H 0.6123 0.6591 0.1382 0.021 Uiso 1 1 calc R U . . .
C12 C 0.6605(5) 0.6107(10) 0.2539(7) 0.017(3) Uani 1 1 d . . . . .
H12A H 0.6651 0.5530 0.2875 0.021 Uiso 1 1 calc R U . . .
H12B H 0.6823 0.5893 0.2186 0.021 Uiso 1 1 calc R U . . .
C14 C 0.6917(5) 0.8117(10) 0.2383(6) 0.0146(10) Uani 1 1 d . U . . .
H14 H 0.7002 0.8055 0.1954 0.017 Uiso 1 1 calc R U . . .
C15 C 0.6937(5) 0.9079(10) 0.2747(6) 0.0146(10) Uani 1 1 d . U . . .
H15 H 0.7033 0.9829 0.2619 0.017 Uiso 1 1 calc R U . . .
C13 C 0.6650(5) 0.7606(10) 0.3349(6) 0.0141(7) Uani 1 1 d . U . . .
C17 C 0.5813(6) 0.7618(10) 0.5498(6) 0.0153(12) Uani 1 1 d . U . . .
C18 C 0.5601(5) 0.7008(10) 0.6455(6) 0.0155(12) Uani 1 1 d . U . . .
H18 H 0.5403 0.6785 0.6801 0.019 Uiso 1 1 calc R U . . .
C19 C 0.6096(5) 0.6977(11) 0.6441(6) 0.0155(12) Uani 1 1 d . U . . .
H19 H 0.6315 0.6738 0.6765 0.019 Uiso 1 1 calc R U . . .
C20 C 0.4918(6) 0.7436(11) 0.5684(6) 0.018(3) Uani 1 1 d . . . . .
H20A H 0.4881 0.8016 0.5349 0.021 Uiso 1 1 calc R U . . .
H20B H 0.4703 0.7668 0.6036 0.021 Uiso 1 1 calc R U . . .
C21 C 0.4853(5) 0.5952(11) 0.4856(6) 0.014(2) Uani 1 1 d . . . . .
C22 C 0.4579(6) 0.5443(12) 0.5822(7) 0.022(3) Uani 1 1 d . . . . .
H22 H 0.4492 0.5490 0.6251 0.027 Uiso 1 1 calc R U . . .
C23 C 0.4553(6) 0.4508(13) 0.5452(7) 0.023(3) Uani 1 1 d . . . . .
H23 H 0.4440 0.3767 0.5572 0.027 Uiso 1 1 calc R U . . .
C24 C 0.4786(5) 0.4048(11) 0.4352(6) 0.015(2) Uani 1 1 d . . . . .
H24A H 0.4745 0.4465 0.3951 0.018 Uiso 1 1 calc R U . . .
H24B H 0.4540 0.3416 0.4366 0.018 Uiso 1 1 calc R U . . .
C25 C 0.5697(5) 0.4096(9) 0.4166(5) 0.012(2) Uani 1 1 d . . . . .
C26 C 0.5437(6) 0.2656(11) 0.4786(7) 0.018(3) Uani 1 1 d . . . . .
H26 H 0.5218 0.2146 0.4995 0.022 Uiso 1 1 calc R U . . .
C27 C 0.5922(6) 0.2616(11) 0.4801(7) 0.020(3) Uani 1 1 d . . . . .
H27 H 0.6123 0.2099 0.5035 0.025 Uiso 1 1 calc R U . . .
C28 C 0.6596(5) 0.3825(10) 0.4319(6) 0.012(2) Uani 1 1 d . . . . .
H28A H 0.6633 0.4208 0.3909 0.014 Uiso 1 1 calc R U . . .
H28B H 0.6810 0.3132 0.4323 0.014 Uiso 1 1 calc R U . . .
C29 C 0.6668(5) 0.5764(10) 0.4797(6) 0.0138(7) Uani 1 1 d . U . . .
C30 C 0.6951(5) 0.4285(11) 0.5397(6) 0.0141(10) Uani 1 1 d . U . . .
H30 H 0.7042 0.3528 0.5517 0.017 Uiso 1 1 calc R U . . .
C31 C 0.6987(5) 0.5237(10) 0.5748(6) 0.0140(10) Uani 1 1 d . U . . .
H31 H 0.7111 0.5292 0.6163 0.017 Uiso 1 1 calc R U . . .
C32 C 0.6708(5) 0.7299(11) 0.5605(6) 0.015(3) Uani 1 1 d . . . . .
H32A H 0.6953 0.7494 0.5934 0.018 Uiso 1 1 calc R U . . .
H32B H 0.6745 0.7859 0.5260 0.018 Uiso 1 1 calc R U . . .
P1 P 0.20101(17) 0.5648(3) 0.5587(2) 0.0170(7) Uani 1 1 d . . . . .
F1 F 0.1947(4) 0.4838(7) 0.6184(4) 0.030(2) Uani 1 1 d . . . . .
F2 F 0.2072(4) 0.6463(8) 0.4986(4) 0.033(2) Uani 1 1 d . . . . .
F3 F 0.1524(4) 0.5114(8) 0.5276(4) 0.0277(19) Uani 1 1 d . . . . .
F4 F 0.1673(4) 0.6619(6) 0.5905(4) 0.026(2) Uani 1 1 d . . . . .
F5 F 0.2486(4) 0.6189(8) 0.5896(5) 0.042(2) Uani 1 1 d . . . . .
F6 F 0.2332(4) 0.4682(7) 0.5258(4) 0.032(2) Uani 1 1 d . . . . .
S1 S 0.30133(18) 0.8451(3) 0.6813(2) 0.0260(8) Uani 1 1 d . . . . .
O1 O 0.2492(4) 0.8712(9) 0.6625(5) 0.027(2) Uani 1 1 d . . . . .
C35 C 0.3291(7) 0.9834(14) 0.6971(10) 0.037(4) Uani 1 1 d . . . . .
H35A H 0.3649 0.9739 0.7039 0.056 Uiso 1 1 calc R U . . .
H35B H 0.3141 1.0169 0.7345 0.056 Uiso 1 1 calc R U . . .
H35C H 0.3235 1.0346 0.6613 0.056 Uiso 1 1 calc R U . . .
C36 C 0.3348(7) 0.8164(17) 0.6127(10) 0.046(5) Uani 1 1 d . . . . .
H36A H 0.3702 0.8298 0.6203 0.069 Uiso 1 1 calc R U . . .
H36B H 0.3231 0.8672 0.5791 0.069 Uiso 1 1 calc R U . . .
H36C H 0.3296 0.7361 0.6003 0.069 Uiso 1 1 calc R U . . .
P2 P 0.43565(19) 0.0602(3) 0.5492(2) 0.0220(8) Uani 1 1 d . . . . .
F7 F 0.4391(4) -0.0145(7) 0.6111(4) 0.030(2) Uani 1 1 d . . . . .
F8 F 0.4327(4) 0.1365(8) 0.4859(4) 0.029(2) Uani 1 1 d . . . . .
F9 F 0.3807(4) 0.0977(8) 0.5654(5) 0.044(3) Uani 1 1 d . . . . .
F10 F 0.4574(5) 0.1698(7) 0.5860(5) 0.038(3) Uani 1 1 d . . . . .
F11 F 0.4913(4) 0.0211(8) 0.5319(5) 0.028(2) Uani 1 1 d . . . . .
F12 F 0.4150(4) -0.0490(7) 0.5112(5) 0.028(2) Uani 1 1 d . . . . .
S2 S 0.34877(18) 0.4303(3) 0.6383(2) 0.0215(8) Uani 0.870(8) 1 d D U P A 3
O2 O 0.3962(5) 0.3749(12) 0.6635(6) 0.0222(13) Uani 0.870(8) 1 d D U P A 3
C37 C 0.3176(6) 0.4865(15) 0.7040(8) 0.0224(13) Uani 0.870(8) 1 d D U P A 3
H37A H 0.2867 0.5234 0.6904 0.034 Uiso 0.870(8) 1 calc R U P A 3
H37B H 0.3101 0.4240 0.7331 0.034 Uiso 0.870(8) 1 calc R U P A 3
H37C H 0.3389 0.5434 0.7248 0.034 Uiso 0.870(8) 1 calc R U P A 3
C38 C 0.3077(6) 0.3178(14) 0.6183(8) 0.0221(13) Uani 0.870(8) 1 d D U P A 3
H38A H 0.2767 0.3503 0.6019 0.033 Uiso 0.870(8) 1 calc R U P A 3
H38B H 0.3229 0.2689 0.5864 0.033 Uiso 0.870(8) 1 calc R U P A 3
H38C H 0.3006 0.2717 0.6556 0.033 Uiso 0.870(8) 1 calc R U P A 3
S2A S 0.3521(10) 0.341(2) 0.6840(13) 0.0218(10) Uani 0.130(8) 1 d D U P A 4
O2A O 0.3965(19) 0.385(7) 0.648(3) 0.0219(13) Uani 0.130(8) 1 d D U P A 4
C37A C 0.327(3) 0.460(6) 0.723(4) 0.0218(14) Uani 0.130(8) 1 d D U P A 4
H37D H 0.2977 0.4354 0.7473 0.033 Uiso 0.130(8) 1 calc R U P A 4
H37E H 0.3515 0.4933 0.7514 0.033 Uiso 0.130(8) 1 calc R U P A 4
H37F H 0.3162 0.5182 0.6925 0.033 Uiso 0.130(8) 1 calc R U P A 4
C38A C 0.304(3) 0.304(9) 0.633(4) 0.0217(14) Uani 0.130(8) 1 d D U P A 4
H38D H 0.2754 0.2755 0.6579 0.033 Uiso 0.130(8) 1 calc R U P A 4
H38E H 0.2933 0.3713 0.6093 0.033 Uiso 0.130(8) 1 calc R U P A 4
H38F H 0.3147 0.2431 0.6049 0.033 Uiso 0.130(8) 1 calc R U P A 4
P3 P 0.22182(18) 0.7965(3) 0.2778(2) 0.0164(7) Uani 1 1 d . . . . .
F13 F 0.2230(4) 0.7238(8) 0.3415(4) 0.032(2) Uani 1 1 d . . . . .
F14 F 0.2203(4) 0.8717(7) 0.2150(4) 0.030(2) Uani 1 1 d . . . . .
F15 F 0.2066(4) 0.6832(7) 0.2393(5) 0.036(2) Uani 1 1 d . . . . .
F16 F 0.1644(4) 0.8252(7) 0.2880(4) 0.0255(19) Uani 1 1 d . . . . .
F17 F 0.2364(4) 0.9097(8) 0.3168(4) 0.0278(19) Uani 1 1 d . . . . .
F18 F 0.2791(4) 0.7713(8) 0.2685(5) 0.032(2) Uani 1 1 d . . . . .
S3 S 0.3537(9) 0.6389(19) 0.3839(10) 0.0463(16) Uani 0.38(3) 1 d D U P B 5
O3 O 0.4044(12) 0.599(3) 0.384(2) 0.0460(18) Uani 0.38(3) 1 d D U P B 5
C39 C 0.3375(17) 0.661(4) 0.4609(14) 0.0465(18) Uani 0.38(3) 1 d D U P B 5
H39A H 0.3043 0.6958 0.4627 0.070 Uiso 0.38(3) 1 calc R U P B 5
H39B H 0.3616 0.7134 0.4806 0.070 Uiso 0.38(3) 1 calc R U P B 5
H39C H 0.3374 0.5878 0.4832 0.070 Uiso 0.38(3) 1 calc R U P B 5
C40 C 0.3560(18) 0.792(2) 0.365(2) 0.046(2) Uani 0.38(3) 1 d D U P B 5
H40A H 0.3222 0.8234 0.3636 0.069 Uiso 0.38(3) 1 calc R U P B 5
H40B H 0.3721 0.8033 0.3248 0.069 Uiso 0.38(3) 1 calc R U P B 5
H40C H 0.3750 0.8328 0.3978 0.069 Uiso 0.38(3) 1 calc R U P B 5
S3A S 0.3536(6) 0.6180(12) 0.3855(7) 0.0462(16) Uani 0.62(3) 1 d D U P B 6
O3A O 0.4060(9) 0.593(2) 0.3795(14) 0.0460(18) Uani 0.62(3) 1 d D U P B 6
C39A C 0.3377(11) 0.591(3) 0.4622(12) 0.0467(19) Uani 0.62(3) 1 d D U P B 6
H39D H 0.3045 0.6217 0.4704 0.070 Uiso 0.62(3) 1 calc R U P B 6
H39E H 0.3618 0.6275 0.4902 0.070 Uiso 0.62(3) 1 calc R U P B 6
H39F H 0.3377 0.5075 0.4695 0.070 Uiso 0.62(3) 1 calc R U P B 6
C40A C 0.3484(12) 0.774(2) 0.3940(17) 0.0463(18) Uani 0.62(3) 1 d D U P B 6
H40D H 0.3292 0.7920 0.4315 0.069 Uiso 0.62(3) 1 calc R U P B 6
H40E H 0.3317 0.8062 0.3572 0.069 Uiso 0.62(3) 1 calc R U P B 6
H40F H 0.3817 0.8077 0.3979 0.069 Uiso 0.62(3) 1 calc R U P B 6
P4 P 0.4415(3) 0.2842(6) 0.2703(3) 0.028(2) Uani 0.54(2) 1 d D U P C 1
F19 F 0.4484(7) 0.2129(13) 0.3336(6) 0.030(3) Uani 0.54(2) 1 d D U P C 1
F20 F 0.4309(7) 0.3473(13) 0.2060(6) 0.031(3) Uani 0.54(2) 1 d D U P C 1
F21 F 0.3921(5) 0.2111(15) 0.2601(7) 0.032(3) Uani 0.54(2) 1 d D U P C 1
F22 F 0.4715(5) 0.1863(10) 0.2343(6) 0.030(3) Uani 0.54(2) 1 d D U P C 1
F23 F 0.4920(5) 0.3493(13) 0.2819(8) 0.030(3) Uani 0.54(2) 1 d D U P C 1
F24 F 0.4133(5) 0.3828(10) 0.3051(6) 0.031(3) Uani 0.54(2) 1 d D U P C 1
P4A P 0.4395(3) 0.2794(6) 0.2644(3) 0.021(3) Uani 0.46(2) 1 d D U P C 2
F19A F 0.4645(6) 0.2516(16) 0.3306(6) 0.024(3) Uani 0.46(2) 1 d D U P C 2
F20A F 0.4120(6) 0.2967(15) 0.1994(6) 0.025(3) Uani 0.46(2) 1 d D U P C 2
F21A F 0.4026(6) 0.1755(12) 0.2790(8) 0.023(3) Uani 0.46(2) 1 d D U P C 2
F22A F 0.4764(5) 0.1895(10) 0.2328(7) 0.023(3) Uani 0.46(2) 1 d D U P C 2
F23A F 0.4785(6) 0.3772(11) 0.2517(8) 0.025(3) Uani 0.46(2) 1 d D U P C 2
F24A F 0.4038(5) 0.3702(11) 0.2943(7) 0.024(3) Uani 0.46(2) 1 d D U P C 2
S4 S 0.2970(6) 0.2294(12) 0.4345(7) 0.0571(9) Uani 0.55(3) 1 d D U P D 7
O4 O 0.2450(8) 0.256(3) 0.4490(15) 0.0571(9) Uani 0.55(3) 1 d D U P D 7
C41 C 0.3019(14) 0.226(3) 0.3518(12) 0.0571(9) Uani 0.55(3) 1 d D U P D 7
H41A H 0.3362 0.2089 0.3402 0.086 Uiso 0.55(3) 1 calc R U P D 7
H41B H 0.2798 0.1667 0.3350 0.086 Uiso 0.55(3) 1 calc R U P D 7
H41C H 0.2924 0.3012 0.3347 0.086 Uiso 0.55(3) 1 calc R U P D 7
C42 C 0.3043(15) 0.078(2) 0.4409(18) 0.0571(9) Uani 0.55(3) 1 d D U P D 7
H42A H 0.3387 0.0570 0.4315 0.086 Uiso 0.55(3) 1 calc R U P D 7
H42B H 0.2962 0.0534 0.4835 0.086 Uiso 0.55(3) 1 calc R U P D 7
H42C H 0.2819 0.0395 0.4112 0.086 Uiso 0.55(3) 1 calc R U P D 7
S4A S 0.3003(7) 0.2514(14) 0.4317(8) 0.0571(9) Uani 0.45(3) 1 d D U P D 8
O4A O 0.2479(9) 0.246(3) 0.4500(17) 0.0571(9) Uani 0.45(3) 1 d D U P D 8
C41A C 0.3020(17) 0.308(3) 0.3547(14) 0.0571(9) Uani 0.45(3) 1 d D U P D 8
H41D H 0.3365 0.3125 0.3407 0.086 Uiso 0.45(3) 1 calc R U P D 8
H41E H 0.2833 0.2573 0.3265 0.086 Uiso 0.45(3) 1 calc R U P D 8
H41F H 0.2872 0.3848 0.3543 0.086 Uiso 0.45(3) 1 calc R U P D 8
C42A C 0.3173(16) 0.111(2) 0.406(2) 0.0571(9) Uani 0.45(3) 1 d D U P D 8
H42D H 0.3522 0.1112 0.3936 0.086 Uiso 0.45(3) 1 calc R U P D 8
H42E H 0.3126 0.0564 0.4405 0.086 Uiso 0.45(3) 1 calc R U P D 8
H42F H 0.2964 0.0889 0.3707 0.086 Uiso 0.45(3) 1 calc R U P D 8
N17 N 0.5754(6) 0.1325(9) 0.7612(5) 0.026(2) Uani 1 1 d . . . . .
C33 C 0.5727(7) 0.0812(11) 0.7159(6) 0.027(3) Uani 1 1 d . . . . .
C34 C 0.5670(8) 0.0133(16) 0.6588(9) 0.047(5) Uani 1 1 d . . . . .
H34A H 0.5962 -0.0359 0.6534 0.071 Uiso 1 1 calc R U . . .
H34B H 0.5638 0.0650 0.6229 0.071 Uiso 1 1 calc R U . . .
H34C H 0.5373 -0.0347 0.6619 0.071 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 C1 1.911(11) . ?
Cu1 C17 1.918(12) . ?
Cu1 Cu4 3.052(2) . ?
Cu2 C21 1.904(13) . ?
Cu2 C5 1.912(13) . ?
Cu2 Cu3 3.040(2) . ?
Cu3 C9 1.906(11) . ?
Cu3 C25 1.918(11) . ?
Cu4 C29 1.900(12) . ?
Cu4 C13 1.907(12) . ?
N1 C1 1.370(17) . ?
N1 C2 1.403(15) . ?
N1 C16 1.441(17) . ?
N2 C1 1.363(17) . ?
N2 C3 1.384(16) . ?
N2 C4 1.439(19) . ?
N3 C5 1.351(16) . ?
N3 C6 1.397(16) . ?
N3 C4 1.448(16) . ?
N4 C5 1.371(16) . ?
N4 C7 1.376(16) . ?
N4 C8 1.466(16) . ?
N5 C9 1.341(19) . ?
N5 C10 1.397(17) . ?
N5 C8 1.437(19) . ?
N6 C9 1.355(19) . ?
N6 C11 1.399(17) . ?
N6 C12 1.468(19) . ?
N7 C13 1.331(16) . ?
N7 C14 1.395(16) . ?
N7 C12 1.458(16) . ?
N8 C13 1.373(16) . ?
N8 C15 1.401(16) . ?
N8 C16 1.434(16) . ?
N9 C17 1.357(18) . ?
N9 C19 1.381(17) . ?
N9 C32 1.427(18) . ?
N10 C17 1.379(17) . ?
N10 C18 1.384(16) . ?
N10 C20 1.418(19) . ?
N11 C21 1.366(17) . ?
N11 C22 1.380(16) . ?
N11 C20 1.459(17) . ?
N12 C21 1.369(15) . ?
N12 C23 1.371(17) . ?
N12 C24 1.439(16) . ?
N13 C25 1.340(17) . ?
N13 C26 1.399(16) . ?
N13 C24 1.481(17) . ?
N14 C25 1.354(17) . ?
N14 C27 1.394(16) . ?
N14 C28 1.450(16) . ?
N15 C29 1.354(16) . ?
N15 C30 1.390(16) . ?
N15 C28 1.479(15) . ?
N16 C29 1.353(16) . ?
N16 C31 1.407(16) . ?
N16 C32 1.465(16) . ?
C2 C3 1.333(18) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 C7 1.351(17) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 C11 1.33(2) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.364(17) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C18 C19 1.33(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C22 C23 1.35(2) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C27 1.31(2) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C30 C31 1.341(17) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
P1 F5 1.572(10) . ?
P1 F6 1.585(9) . ?
P1 F3 1.592(9) . ?
P1 F1 1.596(9) . ?
P1 F4 1.604(8) . ?
P1 F2 1.607(9) . ?
S1 O1 1.490(12) . ?
S1 C36 1.760(18) . ?
S1 C35 1.806(17) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
P2 F9 1.585(11) . ?
P2 F7 1.587(9) . ?
P2 F12 1.606(9) . ?
P2 F10 1.609(10) . ?
P2 F11 1.613(10) . ?
P2 F8 1.621(9) . ?
S2 O2 1.528(12) . ?
S2 C38 1.766(16) . ?
S2 C37 1.766(17) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
S2A O2A 1.52(3) . ?
S2A C38A 1.75(3) . ?
S2A C37A 1.76(3) . ?
C37A H37D 0.9800 . ?
C37A H37E 0.9800 . ?
C37A H37F 0.9800 . ?
C38A H38D 0.9800 . ?
C38A H38E 0.9800 . ?
C38A H38F 0.9800 . ?
P3 F18 1.585(10) . ?
P3 F16 1.598(10) . ?
P3 F14 1.603(8) . ?
P3 F13 1.604(8) . ?
P3 F17 1.605(9) . ?
P3 F15 1.606(9) . ?
S3 O3 1.445(14) . ?
S3 C39 1.73(2) . ?
S3 C40 1.83(2) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
S3A O3A 1.446(14) . ?
S3A C39A 1.73(2) . ?
S3A C40A 1.83(2) . ?
C39A H39D 0.9800 . ?
C39A H39E 0.9800 . ?
C39A H39F 0.9800 . ?
C40A H40D 0.9800 . ?
C40A H40E 0.9800 . ?
C40A H40F 0.9800 . ?
P4 F24 1.568(10) . ?
P4 F23 1.574(13) . ?
P4 F20 1.585(12) . ?
P4 F21 1.595(12) . ?
P4 F22 1.596(10) . ?
P4 F19 1.598(11) . ?
P4A F24A 1.567(10) . ?
P4A F23A 1.574(13) . ?
P4A F20A 1.585(12) . ?
P4A F21A 1.595(12) . ?
P4A F22A 1.596(10) . ?
P4A F19A 1.598(11) . ?
S4 O4 1.469(16) . ?
S4 C41 1.78(2) . ?
S4 C42 1.78(2) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
S4A O4A 1.469(16) . ?
S4A C41A 1.78(2) . ?
S4A C42A 1.78(2) . ?
C41A H41D 0.9800 . ?
C41A H41E 0.9800 . ?
C41A H41F 0.9800 . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 0.9800 . ?
N17 C33 1.141(17) . ?
C33 C34 1.46(2) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 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
C1 Cu1 C17 160.9(5) . . ?
C1 Cu1 Cu4 96.4(4) . . ?
C17 Cu1 Cu4 96.4(4) . . ?
C21 Cu2 C5 163.4(6) . . ?
C21 Cu2 Cu3 96.1(4) . . ?
C5 Cu2 Cu3 95.9(4) . . ?
C9 Cu3 C25 159.0(5) . . ?
C9 Cu3 Cu2 96.8(4) . . ?
C25 Cu3 Cu2 96.9(4) . . ?
C29 Cu4 C13 163.2(6) . . ?
C29 Cu4 Cu1 97.0(4) . . ?
C13 Cu4 Cu1 96.2(4) . . ?
C1 N1 C2 109.8(11) . . ?
C1 N1 C16 124.5(10) . . ?
C2 N1 C16 124.7(11) . . ?
C1 N2 C3 110.7(11) . . ?
C1 N2 C4 124.2(11) . . ?
C3 N2 C4 124.5(11) . . ?
C5 N3 C6 111.7(10) . . ?
C5 N3 C4 123.2(11) . . ?
C6 N3 C4 124.7(10) . . ?
C5 N4 C7 111.9(10) . . ?
C5 N4 C8 123.4(10) . . ?
C7 N4 C8 124.3(11) . . ?
C9 N5 C10 111.8(12) . . ?
C9 N5 C8 124.3(11) . . ?
C10 N5 C8 123.3(12) . . ?
C9 N6 C11 111.2(12) . . ?
C9 N6 C12 123.2(11) . . ?
C11 N6 C12 125.1(12) . . ?
C13 N7 C14 112.7(10) . . ?
C13 N7 C12 123.7(11) . . ?
C14 N7 C12 122.9(11) . . ?
C13 N8 C15 110.6(10) . . ?
C13 N8 C16 125.3(10) . . ?
C15 N8 C16 123.3(10) . . ?
C17 N9 C19 112.6(11) . . ?
C17 N9 C32 123.1(11) . . ?
C19 N9 C32 123.1(11) . . ?
C17 N10 C18 108.6(11) . . ?
C17 N10 C20 122.9(11) . . ?
C18 N10 C20 127.6(11) . . ?
C21 N11 C22 112.0(11) . . ?
C21 N11 C20 122.7(11) . . ?
C22 N11 C20 124.3(12) . . ?
C21 N12 C23 111.2(11) . . ?
C21 N12 C24 123.1(11) . . ?
C23 N12 C24 125.5(11) . . ?
C25 N13 C26 110.4(11) . . ?
C25 N13 C24 123.8(10) . . ?
C26 N13 C24 125.2(11) . . ?
C25 N14 C27 111.7(11) . . ?
C25 N14 C28 122.9(10) . . ?
C27 N14 C28 125.0(11) . . ?
C29 N15 C30 112.0(10) . . ?
C29 N15 C28 122.4(11) . . ?
C30 N15 C28 125.3(10) . . ?
C29 N16 C31 112.0(10) . . ?
C29 N16 C32 123.9(11) . . ?
C31 N16 C32 123.6(10) . . ?
N2 C1 N1 104.8(9) . . ?
N2 C1 Cu1 127.9(10) . . ?
N1 C1 Cu1 126.1(10) . . ?
C3 C2 N1 107.1(11) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 107.6(12) . . ?
C2 C3 H3 126.2 . . ?
N2 C3 H3 126.2 . . ?
N8 C16 N1 109.3(11) . . ?
N8 C16 H16A 109.8 . . ?
N1 C16 H16A 109.8 . . ?
N8 C16 H16B 109.8 . . ?
N1 C16 H16B 109.8 . . ?
H16A C16 H16B 108.3 . . ?
N2 C4 N3 111.4(11) . . ?
N2 C4 H4A 109.4 . . ?
N3 C4 H4A 109.4 . . ?
N2 C4 H4B 109.4 . . ?
N3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N3 C5 N4 103.5(10) . . ?
N3 C5 Cu2 128.3(10) . . ?
N4 C5 Cu2 125.7(9) . . ?
C7 C6 N3 106.2(11) . . ?
C7 C6 H6 126.9 . . ?
N3 C6 H6 126.9 . . ?
C6 C7 N4 106.7(11) . . ?
C6 C7 H7 126.7 . . ?
N4 C7 H7 126.7 . . ?
N5 C8 N4 109.3(11) . . ?
N5 C8 H8A 109.8 . . ?
N4 C8 H8A 109.8 . . ?
N5 C8 H8B 109.8 . . ?
N4 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
N5 C9 N6 104.0(10) . . ?
N5 C9 Cu3 127.3(11) . . ?
N6 C9 Cu3 127.6(11) . . ?
C11 C10 N5 106.5(12) . . ?
C11 C10 H10 126.8 . . ?
N5 C10 H10 126.8 . . ?
C10 C11 N6 106.5(13) . . ?
C10 C11 H11 126.8 . . ?
N6 C11 H11 126.8 . . ?
N7 C12 N6 110.3(11) . . ?
N7 C12 H12A 109.6 . . ?
N6 C12 H12A 109.6 . . ?
N7 C12 H12B 109.6 . . ?
N6 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C15 C14 N7 105.7(11) . . ?
C15 C14 H14 127.1 . . ?
N7 C14 H14 127.1 . . ?
C14 C15 N8 106.4(11) . . ?
C14 C15 H15 126.8 . . ?
N8 C15 H15 126.8 . . ?
N7 C13 N8 104.4(10) . . ?
N7 C13 Cu4 128.4(9) . . ?
N8 C13 Cu4 124.3(9) . . ?
N9 C17 N10 104.1(10) . . ?
N9 C17 Cu1 127.6(10) . . ?
N10 C17 Cu1 127.7(10) . . ?
C19 C18 N10 109.9(12) . . ?
C19 C18 H18 125.1 . . ?
N10 C18 H18 125.1 . . ?
C18 C19 N9 104.8(12) . . ?
C18 C19 H19 127.6 . . ?
N9 C19 H19 127.6 . . ?
N10 C20 N11 111.8(11) . . ?
N10 C20 H20A 109.3 . . ?
N11 C20 H20A 109.3 . . ?
N10 C20 H20B 109.3 . . ?
N11 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
N11 C21 N12 103.1(11) . . ?
N11 C21 Cu2 128.3(9) . . ?
N12 C21 Cu2 126.2(10) . . ?
C23 C22 N11 105.8(12) . . ?
C23 C22 H22 127.1 . . ?
N11 C22 H22 127.1 . . ?
C22 C23 N12 107.8(12) . . ?
C22 C23 H23 126.1 . . ?
N12 C23 H23 126.1 . . ?
N12 C24 N13 106.8(10) . . ?
N12 C24 H24A 110.4 . . ?
N13 C24 H24A 110.4 . . ?
N12 C24 H24B 110.4 . . ?
N13 C24 H24B 110.4 . . ?
H24A C24 H24B 108.6 . . ?
N13 C25 N14 104.0(9) . . ?
N13 C25 Cu3 127.6(10) . . ?
N14 C25 Cu3 127.9(10) . . ?
C27 C26 N13 108.1(13) . . ?
C27 C26 H26 126.0 . . ?
N13 C26 H26 126.0 . . ?
C26 C27 N14 105.8(13) . . ?
C26 C27 H27 127.1 . . ?
N14 C27 H27 127.1 . . ?
N14 C28 N15 110.2(10) . . ?
N14 C28 H28A 109.6 . . ?
N15 C28 H28A 109.6 . . ?
N14 C28 H28B 109.6 . . ?
N15 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
N16 C29 N15 103.4(11) . . ?
N16 C29 Cu4 125.6(9) . . ?
N15 C29 Cu4 129.2(9) . . ?
C31 C30 N15 107.0(11) . . ?
C31 C30 H30 126.5 . . ?
N15 C30 H30 126.5 . . ?
C30 C31 N16 105.5(11) . . ?
C30 C31 H31 127.2 . . ?
N16 C31 H31 127.2 . . ?
N9 C32 N16 110.0(11) . . ?
N9 C32 H32A 109.7 . . ?
N16 C32 H32A 109.7 . . ?
N9 C32 H32B 109.7 . . ?
N16 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
F5 P1 F6 91.3(6) . . ?
F5 P1 F3 179.3(6) . . ?
F6 P1 F3 89.4(5) . . ?
F5 P1 F1 89.4(5) . . ?
F6 P1 F1 89.9(5) . . ?
F3 P1 F1 90.8(5) . . ?
F5 P1 F4 90.1(5) . . ?
F6 P1 F4 178.5(6) . . ?
F3 P1 F4 89.2(5) . . ?
F1 P1 F4 90.7(5) . . ?
F5 P1 F2 90.7(6) . . ?
F6 P1 F2 90.2(5) . . ?
F3 P1 F2 89.1(5) . . ?
F1 P1 F2 179.8(6) . . ?
F4 P1 F2 89.2(5) . . ?
O1 S1 C36 107.4(9) . . ?
O1 S1 C35 105.0(7) . . ?
C36 S1 C35 96.4(9) . . ?
S1 C35 H35A 109.5 . . ?
S1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
S1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
S1 C36 H36A 109.5 . . ?
S1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
S1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
F9 P2 F7 91.0(5) . . ?
F9 P2 F12 90.4(6) . . ?
F7 P2 F12 90.5(5) . . ?
F9 P2 F10 90.8(6) . . ?
F7 P2 F10 90.3(5) . . ?
F12 P2 F10 178.6(6) . . ?
F9 P2 F11 179.3(7) . . ?
F7 P2 F11 89.2(5) . . ?
F12 P2 F11 89.0(5) . . ?
F10 P2 F11 89.9(6) . . ?
F9 P2 F8 89.5(5) . . ?
F7 P2 F8 179.5(6) . . ?
F12 P2 F8 89.7(5) . . ?
F10 P2 F8 89.5(5) . . ?
F11 P2 F8 90.3(5) . . ?
O2 S2 C38 107.2(8) . . ?
O2 S2 C37 106.0(7) . . ?
C38 S2 C37 99.6(8) . . ?
S2 C37 H37A 109.5 . . ?
S2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
S2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
S2 C38 H38A 109.5 . . ?
S2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
S2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O2A S2A C38A 111(3) . . ?
O2A S2A C37A 107(3) . . ?
C38A S2A C37A 101(3) . . ?
S2A C37A H37D 109.5 . . ?
S2A C37A H37E 109.5 . . ?
H37D C37A H37E 109.5 . . ?
S2A C37A H37F 109.5 . . ?
H37D C37A H37F 109.5 . . ?
H37E C37A H37F 109.5 . . ?
S2A C38A H38D 109.5 . . ?
S2A C38A H38E 109.5 . . ?
H38D C38A H38E 109.5 . . ?
S2A C38A H38F 109.5 . . ?
H38D C38A H38F 109.5 . . ?
H38E C38A H38F 109.5 . . ?
F18 P3 F16 178.4(5) . . ?
F18 P3 F14 91.0(5) . . ?
F16 P3 F14 88.9(5) . . ?
F18 P3 F13 89.7(5) . . ?
F16 P3 F13 90.4(5) . . ?
F14 P3 F13 178.7(5) . . ?
F18 P3 F17 88.9(5) . . ?
F16 P3 F17 89.5(5) . . ?
F14 P3 F17 89.6(5) . . ?
F13 P3 F17 89.3(5) . . ?
F18 P3 F15 91.8(5) . . ?
F16 P3 F15 89.8(5) . . ?
F14 P3 F15 90.7(5) . . ?
F13 P3 F15 90.4(5) . . ?
F17 P3 F15 179.2(6) . . ?
O3 S3 C39 107.2(11) . . ?
O3 S3 C40 106.3(11) . . ?
C39 S3 C40 93.9(16) . . ?
S3 C39 H39A 109.5 . . ?
S3 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
S3 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
S3 C40 H40A 109.5 . . ?
S3 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
S3 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O3A S3A C39A 107.2(11) . . ?
O3A S3A C40A 106.3(11) . . ?
C39A S3A C40A 93.9(16) . . ?
S3A C39A H39D 109.5 . . ?
S3A C39A H39E 109.5 . . ?
H39D C39A H39E 109.5 . . ?
S3A C39A H39F 109.5 . . ?
H39D C39A H39F 109.5 . . ?
H39E C39A H39F 109.5 . . ?
S3A C40A H40D 109.5 . . ?
S3A C40A H40E 109.5 . . ?
H40D C40A H40E 109.5 . . ?
S3A C40A H40F 109.5 . . ?
H40D C40A H40F 109.5 . . ?
H40E C40A H40F 109.5 . . ?
F24 P4 F23 89.7(6) . . ?
F24 P4 F20 89.3(6) . . ?
F23 P4 F20 93.8(9) . . ?
F24 P4 F21 92.7(6) . . ?
F23 P4 F21 176.5(9) . . ?
F20 P4 F21 88.9(9) . . ?
F24 P4 F22 178.4(6) . . ?
F23 P4 F22 88.9(6) . . ?
F20 P4 F22 90.0(6) . . ?
F21 P4 F22 88.8(6) . . ?
F24 P4 F19 91.7(6) . . ?
F23 P4 F19 91.2(9) . . ?
F20 P4 F19 174.9(10) . . ?
F21 P4 F19 86.2(9) . . ?
F22 P4 F19 89.0(6) . . ?
F24A P4A F23A 89.8(6) . . ?
F24A P4A F20A 89.3(6) . . ?
F23A P4A F20A 93.7(9) . . ?
F24A P4A F21A 92.7(6) . . ?
F23A P4A F21A 176.5(9) . . ?
F20A P4A F21A 88.8(9) . . ?
F24A P4A F22A 178.4(6) . . ?
F23A P4A F22A 88.9(6) . . ?
F20A P4A F22A 90.0(6) . . ?
F21A P4A F22A 88.7(6) . . ?
F24A P4A F19A 91.8(6) . . ?
F23A P4A F19A 91.2(9) . . ?
F20A P4A F19A 174.9(10) . . ?
F21A P4A F19A 86.2(9) . . ?
F22A P4A F19A 89.0(6) . . ?
O4 S4 C41 106.9(12) . . ?
O4 S4 C42 107.1(13) . . ?
C41 S4 C42 92.7(16) . . ?
S4 C41 H41A 109.5 . . ?
S4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
S4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
S4 C42 H42A 109.5 . . ?
S4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
S4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O4A S4A C41A 106.9(12) . . ?
O4A S4A C42A 107.1(13) . . ?
C41A S4A C42A 92.7(16) . . ?
S4A C41A H41D 109.5 . . ?
S4A C41A H41E 109.5 . . ?
H41D C41A H41E 109.5 . . ?
S4A C41A H41F 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
S4A C42A H42D 109.5 . . ?
S4A C42A H42E 109.5 . . ?
H42D C42A H42E 109.5 . . ?
S4A C42A H42F 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
N17 C33 C34 177.4(19) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 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
C3 N2 C1 N1 0.4(12) . . . . ?
C4 N2 C1 N1 171.8(11) . . . . ?
C3 N2 C1 Cu1 168.1(8) . . . . ?
C4 N2 C1 Cu1 -20.4(16) . . . . ?
C2 N1 C1 N2 -0.5(12) . . . . ?
C16 N1 C1 N2 -169.2(11) . . . . ?
C2 N1 C1 Cu1 -168.5(8) . . . . ?
C16 N1 C1 Cu1 22.8(16) . . . . ?
C1 N1 C2 C3 0.4(14) . . . . ?
C16 N1 C2 C3 169.1(11) . . . . ?
N1 C2 C3 N2 -0.2(15) . . . . ?
C1 N2 C3 C2 -0.1(14) . . . . ?
C4 N2 C3 C2 -171.6(11) . . . . ?
C13 N8 C16 N1 -83.5(15) . . . . ?
C15 N8 C16 N1 85.4(15) . . . . ?
C1 N1 C16 N8 82.9(14) . . . . ?
C2 N1 C16 N8 -84.2(14) . . . . ?
C1 N2 C4 N3 -84.5(14) . . . . ?
C3 N2 C4 N3 85.8(14) . . . . ?
C5 N3 C4 N2 82.5(15) . . . . ?
C6 N3 C4 N2 -89.8(16) . . . . ?
C6 N3 C5 N4 -0.2(15) . . . . ?
C4 N3 C5 N4 -173.4(12) . . . . ?
C6 N3 C5 Cu2 -162.5(11) . . . . ?
C4 N3 C5 Cu2 24(2) . . . . ?
C7 N4 C5 N3 -1.2(15) . . . . ?
C8 N4 C5 N3 172.1(12) . . . . ?
C7 N4 C5 Cu2 161.7(10) . . . . ?
C8 N4 C5 Cu2 -25.0(19) . . . . ?
C5 N3 C6 C7 1.5(16) . . . . ?
C4 N3 C6 C7 174.6(13) . . . . ?
N3 C6 C7 N4 -2.1(15) . . . . ?
C5 N4 C7 C6 2.1(16) . . . . ?
C8 N4 C7 C6 -171.1(13) . . . . ?
C9 N5 C8 N4 85.4(14) . . . . ?
C10 N5 C8 N4 -84.9(14) . . . . ?
C5 N4 C8 N5 -82.6(15) . . . . ?
C7 N4 C8 N5 89.8(15) . . . . ?
C10 N5 C9 N6 0.0(12) . . . . ?
C8 N5 C9 N6 -171.3(11) . . . . ?
C10 N5 C9 Cu3 -169.1(9) . . . . ?
C8 N5 C9 Cu3 19.7(17) . . . . ?
C11 N6 C9 N5 0.1(13) . . . . ?
C12 N6 C9 N5 172.1(11) . . . . ?
C11 N6 C9 Cu3 169.1(8) . . . . ?
C12 N6 C9 Cu3 -18.9(16) . . . . ?
C9 N5 C10 C11 0.0(15) . . . . ?
C8 N5 C10 C11 171.4(11) . . . . ?
N5 C10 C11 N6 0.1(15) . . . . ?
C9 N6 C11 C10 -0.1(15) . . . . ?
C12 N6 C11 C10 -171.9(11) . . . . ?
C13 N7 C12 N6 82.9(16) . . . . ?
C14 N7 C12 N6 -86.4(15) . . . . ?
C9 N6 C12 N7 -84.6(14) . . . . ?
C11 N6 C12 N7 86.3(15) . . . . ?
C13 N7 C14 C15 0.9(16) . . . . ?
C12 N7 C14 C15 171.3(12) . . . . ?
N7 C14 C15 N8 1.5(15) . . . . ?
C13 N8 C15 C14 -3.4(16) . . . . ?
C16 N8 C15 C14 -173.8(12) . . . . ?
C14 N7 C13 N8 -3.0(15) . . . . ?
C12 N7 C13 N8 -173.3(12) . . . . ?
C14 N7 C13 Cu4 -164.3(11) . . . . ?
C12 N7 C13 Cu4 25(2) . . . . ?
C15 N8 C13 N7 3.9(15) . . . . ?
C16 N8 C13 N7 174.0(13) . . . . ?
C15 N8 C13 Cu4 166.2(10) . . . . ?
C16 N8 C13 Cu4 -23.7(19) . . . . ?
C19 N9 C17 N10 2.4(13) . . . . ?
C32 N9 C17 N10 170.4(11) . . . . ?
C19 N9 C17 Cu1 173.8(9) . . . . ?
C32 N9 C17 Cu1 -18.1(17) . . . . ?
C18 N10 C17 N9 -2.4(12) . . . . ?
C20 N10 C17 N9 -172.4(12) . . . . ?
C18 N10 C17 Cu1 -173.8(9) . . . . ?
C20 N10 C17 Cu1 16.2(17) . . . . ?
C17 N10 C18 C19 1.7(14) . . . . ?
C20 N10 C18 C19 171.0(12) . . . . ?
N10 C18 C19 N9 -0.2(15) . . . . ?
C17 N9 C19 C18 -1.4(15) . . . . ?
C32 N9 C19 C18 -169.4(12) . . . . ?
C17 N10 C20 N11 87.9(14) . . . . ?
C18 N10 C20 N11 -80.1(15) . . . . ?
C21 N11 C20 N10 -82.7(15) . . . . ?
C22 N11 C20 N10 84.9(16) . . . . ?
C22 N11 C21 N12 1.1(15) . . . . ?
C20 N11 C21 N12 170.0(12) . . . . ?
C22 N11 C21 Cu2 164.4(10) . . . . ?
C20 N11 C21 Cu2 -26.7(19) . . . . ?
C23 N12 C21 N11 -0.7(15) . . . . ?
C24 N12 C21 N11 -175.5(11) . . . . ?
C23 N12 C21 Cu2 -164.4(10) . . . . ?
C24 N12 C21 Cu2 20.8(18) . . . . ?
C21 N11 C22 C23 -1.1(17) . . . . ?
C20 N11 C22 C23 -169.8(13) . . . . ?
N11 C22 C23 N12 0.6(17) . . . . ?
C21 N12 C23 C22 0.1(17) . . . . ?
C24 N12 C23 C22 174.7(13) . . . . ?
C21 N12 C24 N13 86.3(14) . . . . ?
C23 N12 C24 N13 -87.7(15) . . . . ?
C25 N13 C24 N12 -87.6(13) . . . . ?
C26 N13 C24 N12 82.7(14) . . . . ?
C26 N13 C25 N14 -0.7(12) . . . . ?
C24 N13 C25 N14 170.8(11) . . . . ?
C26 N13 C25 Cu3 171.0(9) . . . . ?
C24 N13 C25 Cu3 -17.5(16) . . . . ?
C27 N14 C25 N13 -1.1(12) . . . . ?
C28 N14 C25 N13 -173.2(11) . . . . ?
C27 N14 C25 Cu3 -172.8(9) . . . . ?
C28 N14 C25 Cu3 15.1(16) . . . . ?
C25 N13 C26 C27 2.3(16) . . . . ?
C24 N13 C26 C27 -169.0(12) . . . . ?
N13 C26 C27 N14 -2.9(17) . . . . ?
C25 N14 C27 C26 2.6(16) . . . . ?
C28 N14 C27 C26 174.5(12) . . . . ?
C25 N14 C28 N15 88.5(13) . . . . ?
C27 N14 C28 N15 -82.5(14) . . . . ?
C29 N15 C28 N14 -84.5(14) . . . . ?
C30 N15 C28 N14 88.1(15) . . . . ?
C31 N16 C29 N15 2.1(15) . . . . ?
C32 N16 C29 N15 -170.4(12) . . . . ?
C31 N16 C29 Cu4 -163.7(10) . . . . ?
C32 N16 C29 Cu4 23.8(19) . . . . ?
C30 N15 C29 N16 -1.8(15) . . . . ?
C28 N15 C29 N16 171.8(11) . . . . ?
C30 N15 C29 Cu4 163.3(10) . . . . ?
C28 N15 C29 Cu4 -23.2(19) . . . . ?
C29 N15 C30 C31 0.8(16) . . . . ?
C28 N15 C30 C31 -172.5(12) . . . . ?
N15 C30 C31 N16 0.5(15) . . . . ?
C29 N16 C31 C30 -1.7(16) . . . . ?
C32 N16 C31 C30 170.8(12) . . . . ?
C17 N9 C32 N16 -87.1(14) . . . . ?
C19 N9 C32 N16 79.7(14) . . . . ?
C29 N16 C32 N9 84.3(15) . . . . ?
C31 N16 C32 N9 -87.4(15) . . . . ?


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

data_annma34_0m-auto
_database_code_depnum_ccdc_archive 'CCDC 1829613'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H19 N8 O, 3(F6 P), 3(C2 H3 N)'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C22 H28 F18 N11 O P3'
_chemical_formula_iupac          ?
_chemical_formula_weight         897.46
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   10.1257(13)
_cell_length_b                   12.8486(17)
_cell_length_c                   14.7435(18)
_cell_angle_alpha                110.335(6)
_cell_angle_beta                 96.001(7)
_cell_angle_gamma                97.292(7)
_cell_volume                     1761.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    7868
_cell_measurement_theta_min      2.3382
_cell_measurement_theta_max      25.4354
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear colourless'

_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.070
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.304
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_T_max  0.7453

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           10 s per frame
dx                                  34 mm
1222 frames measured in 7 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
shutterless mode
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_monochromator  'Helios optic'

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            30556
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             6450
# number of observed reflections (> n sig(I))
_reflns_number_gt                4834
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0378P)²+2.3714P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom


_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         6450
_refine_ls_number_parameters     648
_refine_ls_number_restraints     221
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1063
_refine_ls_wR_factor_gt          0.0955
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.063

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
P1 P 0.25274(7) 0.43173(6) 0.30246(5) 0.02108(17) Uani 1 1 d . . . . .
F1 F 0.38617(17) 0.47983(14) 0.27006(13) 0.0326(4) Uani 1 1 d . . . . .
F2 F 0.11791(16) 0.38639(14) 0.33510(12) 0.0293(4) Uani 1 1 d . . . . .
F3 F 0.30225(18) 0.31523(14) 0.28599(14) 0.0386(5) Uani 1 1 d . . . . .
F4 F 0.17740(18) 0.38511(14) 0.19183(12) 0.0321(4) Uani 1 1 d . . . . .
F5 F 0.20262(17) 0.54995(14) 0.32005(12) 0.0298(4) Uani 1 1 d . . . . .
F6 F 0.32703(18) 0.47938(15) 0.41385(12) 0.0353(4) Uani 1 1 d . . . . .
O1 O 0.4955(2) 0.62073(16) 0.11748(14) 0.0272(5) Uani 1 1 d . . . . .
N1 N 0.6730(2) 0.71261(19) 0.06827(16) 0.0224(5) Uani 1 1 d . . . . .
N2 N 0.5623(2) 0.81640(19) 0.17326(16) 0.0227(5) Uani 1 1 d . . . . .
N3 N 0.5201(2) 0.83061(18) 0.33389(16) 0.0198(5) Uani 1 1 d . . . . .
N4 N 0.5805(2) 0.74963(19) 0.43307(15) 0.0189(5) Uani 1 1 d . . . . .
N5 N 0.7111(2) 0.60566(18) 0.42831(15) 0.0183(5) Uani 1 1 d . . . . .
N6 N 0.8151(2) 0.49932(18) 0.32294(15) 0.0171(5) Uani 1 1 d . . . . .
N7 N 0.8529(2) 0.48220(18) 0.16148(16) 0.0194(5) Uani 1 1 d . . . . .
N8 N 0.7983(2) 0.56568(18) 0.06293(15) 0.0216(5) Uani 1 1 d . . . . .
C1 C 0.5675(3) 0.7061(2) 0.11885(19) 0.0223(6) Uani 1 1 d . . . . .
C2 C 0.7326(3) 0.8246(2) 0.0937(2) 0.0279(7) Uani 1 1 d . . . . .
H2 H 0.8078 0.8510 0.0692 0.033 Uiso 1 1 calc R U . . .
C3 C 0.6655(3) 0.8883(2) 0.1584(2) 0.0275(7) Uani 1 1 d . . . . .
H3 H 0.6847 0.9681 0.1889 0.033 Uiso 1 1 calc R U . . .
C4 C 0.4694(3) 0.8438(2) 0.2414(2) 0.0247(6) Uani 1 1 d . . . . .
H4A H 0.3811 0.7938 0.2121 0.030 Uiso 1 1 calc R U . . .
H4B H 0.4562 0.9226 0.2554 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5099(3) 0.7329(2) 0.3464(2) 0.0213(6) Uani 1 1 d . . . . .
H5 H 0.4607 0.6628 0.3012 0.026 Uiso 1 1 calc R U . . .
C6 C 0.6008(3) 0.9129(2) 0.41467(19) 0.0231(6) Uani 1 1 d . . . . .
H6 H 0.6255 0.9903 0.4244 0.028 Uiso 1 1 calc R U . . .
C7 C 0.6378(3) 0.8623(2) 0.4771(2) 0.0232(6) Uani 1 1 d . . . . .
H7 H 0.6928 0.8974 0.5396 0.028 Uiso 1 1 calc R U . . .
C8 C 0.6030(3) 0.6615(2) 0.4716(2) 0.0225(6) Uani 1 1 d . . . . .
H8A H 0.5190 0.6056 0.4556 0.027 Uiso 1 1 calc R U . . .
H8B H 0.6282 0.6952 0.5437 0.027 Uiso 1 1 calc R U . . .
C9 C 0.6946(3) 0.5230(2) 0.34131(19) 0.0197(6) Uani 1 1 d . . . . .
H9 H 0.6110 0.4870 0.2995 0.024 Uiso 1 1 calc R U . . .
C10 C 0.8470(3) 0.6355(2) 0.46649(19) 0.0209(6) Uani 1 1 d . . . . .
H10 H 0.8869 0.6924 0.5277 0.025 Uiso 1 1 calc R U . . .
C11 C 0.9117(3) 0.5691(2) 0.40102(19) 0.0198(6) Uani 1 1 d . . . . .
H11 H 1.0062 0.5699 0.4070 0.024 Uiso 1 1 calc R U . . .
C12 C 0.8392(3) 0.4221(2) 0.22887(19) 0.0207(6) Uani 1 1 d . . . . .
H12A H 0.9226 0.3919 0.2387 0.025 Uiso 1 1 calc R U . . .
H12B H 0.7631 0.3579 0.2008 0.025 Uiso 1 1 calc R U . . .
C13 C 0.7498(3) 0.4985(2) 0.10704(19) 0.0210(6) Uani 1 1 d . . . . .
H13 H 0.6575 0.4674 0.1009 0.025 Uiso 1 1 calc R U . . .
C14 C 0.9704(3) 0.5419(2) 0.1525(2) 0.0259(7) Uani 1 1 d . . . . .
H14 H 1.0589 0.5456 0.1836 0.031 Uiso 1 1 calc R U . . .
C15 C 0.9354(3) 0.5944(2) 0.0909(2) 0.0271(7) Uani 1 1 d . . . . .
H15 H 0.9949 0.6423 0.0706 0.033 Uiso 1 1 calc R U . . .
C16 C 0.7139(3) 0.6131(2) 0.0049(2) 0.0260(7) Uani 1 1 d . . . . .
H16A H 0.7654 0.6321 -0.0424 0.031 Uiso 1 1 calc R U . . .
H16B H 0.6331 0.5563 -0.0326 0.031 Uiso 1 1 calc R U . . .
P2 P 0.70889(8) 0.21923(6) 0.38953(5) 0.02344(18) Uani 1 1 d . . . . .
F7 F 0.57342(19) 0.12547(16) 0.34729(14) 0.0424(5) Uani 1 1 d . . . . .
F8 F 0.8420(2) 0.31019(17) 0.43039(16) 0.0525(6) Uani 1 1 d . . . . .
F9 F 0.6192(2) 0.31403(16) 0.40065(16) 0.0497(5) Uani 1 1 d . . . . .
F10 F 0.6935(2) 0.22179(19) 0.49667(13) 0.0526(6) Uani 1 1 d . . . . .
F11 F 0.7945(2) 0.12055(17) 0.37572(15) 0.0469(5) Uani 1 1 d . . . . .
F12 F 0.7213(2) 0.21333(17) 0.28108(13) 0.0424(5) Uani 1 1 d . . . . .
P3 P 0.8262(8) 0.1675(7) -0.0391(6) 0.0295(9) Uani 0.390(3) 1 d D U P A 3
F13 F 0.6931(6) 0.0938(4) -0.1070(5) 0.0338(12) Uani 0.390(3) 1 d D U P A 3
F14 F 0.9626(6) 0.2487(4) 0.0319(4) 0.0323(12) Uani 0.390(3) 1 d D U P A 3
F15 F 0.8799(7) 0.0614(6) -0.0274(7) 0.0301(14) Uani 0.390(3) 1 d D U P A 3
F16 F 0.9045(7) 0.1524(4) -0.1316(4) 0.0346(11) Uani 0.390(3) 1 d D U P A 3
F17 F 0.7806(10) 0.2838(7) -0.0379(6) 0.0309(14) Uani 0.390(3) 1 d D U P A 3
F18 F 0.7574(7) 0.1848(5) 0.0561(5) 0.0379(13) Uani 0.390(3) 1 d D U P A 3
P3A P 0.8222(6) 0.1648(6) -0.0390(5) 0.0141(7) Uani 0.394(3) 1 d D U P B 4
F13A F 0.6622(5) 0.1167(5) -0.0712(4) 0.0188(10) Uani 0.394(3) 1 d D U P B 4
F14A F 0.9782(4) 0.2148(5) -0.0018(5) 0.0203(10) Uani 0.394(3) 1 d D U P B 4
F15A F 0.8449(9) 0.0458(6) -0.0317(6) 0.0187(12) Uani 0.394(3) 1 d D U P B 4
F16A F 0.8413(7) 0.1220(5) -0.1498(3) 0.0242(10) Uani 0.394(3) 1 d D U P B 4
F17A F 0.7974(9) 0.2804(7) -0.0532(6) 0.0168(12) Uani 0.394(3) 1 d D U P B 4
F18A F 0.7988(6) 0.2104(5) 0.0744(3) 0.0195(10) Uani 0.394(3) 1 d D U P B 4
P3B P 0.8193(11) 0.1618(10) -0.0456(8) 0.0347(14) Uani 0.216(3) 1 d D U P C 5
F13B F 0.6630(9) 0.1497(8) -0.0331(8) 0.0375(18) Uani 0.216(3) 1 d D U P C 5
F14B F 0.9728(8) 0.1722(8) -0.0607(9) 0.0373(17) Uani 0.216(3) 1 d D U P C 5
F15B F 0.8292(16) 0.0557(11) -0.0141(10) 0.0350(19) Uani 0.216(3) 1 d D U P C 5
F16B F 0.7691(11) 0.0764(7) -0.1587(6) 0.0324(16) Uani 0.216(3) 1 d D U P C 5
F17B F 0.8022(12) 0.2626(8) -0.0867(8) 0.0345(18) Uani 0.216(3) 1 d D U P C 5
F18B F 0.8608(12) 0.2421(8) 0.0645(7) 0.0432(18) Uani 0.216(3) 1 d D U P C 5
N9 N 0.2049(3) 0.2663(2) 0.71361(18) 0.0307(6) Uani 1 1 d . U . . .
C17 C 0.0962(7) 0.2185(8) 0.6837(7) 0.0367(10) Uani 0.591(10) 1 d D U P D 1
C18 C -0.0465(8) 0.1658(7) 0.6481(6) 0.0559(15) Uani 0.591(10) 1 d D U P D 1
H18A H -0.0607 0.1289 0.5766 0.084 Uiso 0.591(10) 1 calc R U P D 1
H18B H -0.1034 0.2237 0.6665 0.084 Uiso 0.591(10) 1 calc R U P D 1
H18C H -0.0704 0.1096 0.6774 0.084 Uiso 0.591(10) 1 calc R U P D 1
C17A C 0.1163(10) 0.2057(11) 0.6737(11) 0.0376(10) Uani 0.409(10) 1 d D U P D 2
C18A C -0.0034(11) 0.1215(10) 0.6165(8) 0.0576(16) Uani 0.409(10) 1 d D U P D 2
H18D H -0.0671 0.1577 0.5883 0.086 Uiso 0.409(10) 1 calc R U P D 2
H18E H -0.0468 0.0892 0.6595 0.086 Uiso 0.409(10) 1 calc R U P D 2
H18F H 0.0240 0.0614 0.5637 0.086 Uiso 0.409(10) 1 calc R U P D 2
N10 N 0.5225(3) 0.3266(2) 0.12684(18) 0.0292(6) Uani 1 1 d . . . . .
C19 C 0.4854(3) 0.2388(3) 0.1257(2) 0.0274(7) Uani 1 1 d . . . . .
C20 C 0.4378(4) 0.1273(3) 0.1245(3) 0.0461(9) Uani 1 1 d . . . . .
H20A H 0.3481 0.0980 0.0846 0.069 Uiso 1 1 calc R U . . .
H20B H 0.4327 0.1312 0.1916 0.069 Uiso 1 1 calc R U . . .
H20C H 0.5003 0.0771 0.0965 0.069 Uiso 1 1 calc R U . . .
N11 N 0.1349(4) 0.1082(3) 0.3458(2) 0.0571(9) Uani 1 1 d . . . . .
C21 C 0.0770(3) 0.1123(3) 0.2774(2) 0.0335(8) Uani 1 1 d . . . . .
C22 C 0.0018(3) 0.1180(3) 0.1910(2) 0.0299(7) Uani 1 1 d . . . . .
H22A H 0.0524 0.1748 0.1714 0.045 Uiso 1 1 calc R U . . .
H22B H -0.0857 0.1389 0.2053 0.045 Uiso 1 1 calc R U . . .
H22C H -0.0125 0.0443 0.1376 0.045 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 F3 1.5857(18) . ?
P1 F4 1.5956(18) . ?
P1 F6 1.6011(18) . ?
P1 F1 1.6012(18) . ?
P1 F2 1.6017(17) . ?
P1 F5 1.6066(17) . ?
O1 C1 1.230(3) . ?
N1 C1 1.375(4) . ?
N1 C2 1.390(4) . ?
N1 C16 1.437(3) . ?
N2 C1 1.376(3) . ?
N2 C3 1.391(4) . ?
N2 C4 1.433(4) . ?
N3 C5 1.324(3) . ?
N3 C6 1.381(3) . ?
N3 C4 1.479(3) . ?
N4 C5 1.330(3) . ?
N4 C7 1.381(4) . ?
N4 C8 1.463(3) . ?
N5 C9 1.329(3) . ?
N5 C10 1.383(4) . ?
N5 C8 1.465(3) . ?
N6 C9 1.327(3) . ?
N6 C11 1.383(3) . ?
N6 C12 1.464(3) . ?
N7 C13 1.332(4) . ?
N7 C14 1.377(4) . ?
N7 C12 1.462(3) . ?
N8 C13 1.326(3) . ?
N8 C15 1.370(4) . ?
N8 C16 1.475(4) . ?
C2 C3 1.333(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5 0.9500 . ?
C6 C7 1.348(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9 0.9500 . ?
C10 C11 1.338(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13 0.9500 . ?
C14 C15 1.350(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
P2 F8 1.577(2) . ?
P2 F9 1.5841(19) . ?
P2 F10 1.5927(19) . ?
P2 F11 1.5928(19) . ?
P2 F12 1.5932(18) . ?
P2 F7 1.6128(19) . ?
P3 F13 1.566(9) . ?
P3 F15 1.586(9) . ?
P3 F18 1.590(9) . ?
P3 F17 1.614(9) . ?
P3 F16 1.615(9) . ?
P3 F14 1.632(8) . ?
P3A F16A 1.573(7) . ?
P3A F14A 1.589(7) . ?
P3A F15A 1.613(8) . ?
P3A F17A 1.615(8) . ?
P3A F13A 1.616(7) . ?
P3A F18A 1.623(7) . ?
P3B F18B 1.568(11) . ?
P3B F14B 1.590(12) . ?
P3B F15B 1.597(12) . ?
P3B F13B 1.606(12) . ?
P3B F16B 1.628(11) . ?
P3B F17B 1.630(12) . ?
N9 C17A 1.074(9) . ?
N9 C17 1.150(7) . ?
C17 C18 1.473(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17A C18A 1.473(7) . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
N10 C19 1.136(4) . ?
C19 C20 1.446(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N11 C21 1.133(4) . ?
C21 C22 1.444(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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
F3 P1 F4 90.66(10) . . ?
F3 P1 F6 89.89(10) . . ?
F4 P1 F6 179.35(11) . . ?
F3 P1 F1 91.16(10) . . ?
F4 P1 F1 90.36(10) . . ?
F6 P1 F1 89.98(10) . . ?
F3 P1 F2 90.23(10) . . ?
F4 P1 F2 89.53(9) . . ?
F6 P1 F2 90.11(9) . . ?
F1 P1 F2 178.61(10) . . ?
F3 P1 F5 179.55(10) . . ?
F4 P1 F5 89.74(9) . . ?
F6 P1 F5 89.71(10) . . ?
F1 P1 F5 89.05(9) . . ?
F2 P1 F5 89.57(9) . . ?
C1 N1 C2 110.0(2) . . ?
C1 N1 C16 121.5(2) . . ?
C2 N1 C16 128.4(3) . . ?
C1 N2 C3 110.1(2) . . ?
C1 N2 C4 121.1(2) . . ?
C3 N2 C4 128.5(2) . . ?
C5 N3 C6 109.1(2) . . ?
C5 N3 C4 124.2(2) . . ?
C6 N3 C4 126.1(2) . . ?
C5 N4 C7 108.8(2) . . ?
C5 N4 C8 125.4(2) . . ?
C7 N4 C8 125.6(2) . . ?
C9 N5 C10 108.8(2) . . ?
C9 N5 C8 124.8(2) . . ?
C10 N5 C8 126.2(2) . . ?
C9 N6 C11 108.9(2) . . ?
C9 N6 C12 123.9(2) . . ?
C11 N6 C12 126.7(2) . . ?
C13 N7 C14 109.0(2) . . ?
C13 N7 C12 124.5(2) . . ?
C14 N7 C12 126.1(2) . . ?
C13 N8 C15 109.0(2) . . ?
C13 N8 C16 124.1(2) . . ?
C15 N8 C16 126.4(2) . . ?
O1 C1 N1 127.8(3) . . ?
O1 C1 N2 127.6(3) . . ?
N1 C1 N2 104.6(2) . . ?
C3 C2 N1 107.9(3) . . ?
C3 C2 H2 126.1 . . ?
N1 C2 H2 126.1 . . ?
C2 C3 N2 107.4(3) . . ?
C2 C3 H3 126.3 . . ?
N2 C3 H3 126.3 . . ?
N2 C4 N3 110.9(2) . . ?
N2 C4 H4A 109.5 . . ?
N3 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N3 C5 N4 108.3(2) . . ?
N3 C5 H5 125.9 . . ?
N4 C5 H5 125.9 . . ?
C7 C6 N3 106.8(2) . . ?
C7 C6 H6 126.6 . . ?
N3 C6 H6 126.6 . . ?
C6 C7 N4 107.0(2) . . ?
C6 C7 H7 126.5 . . ?
N4 C7 H7 126.5 . . ?
N4 C8 N5 109.6(2) . . ?
N4 C8 H8A 109.8 . . ?
N5 C8 H8A 109.8 . . ?
N4 C8 H8B 109.8 . . ?
N5 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
N6 C9 N5 108.1(2) . . ?
N6 C9 H9 125.9 . . ?
N5 C9 H9 125.9 . . ?
C11 C10 N5 107.1(2) . . ?
C11 C10 H10 126.4 . . ?
N5 C10 H10 126.4 . . ?
C10 C11 N6 107.0(2) . . ?
C10 C11 H11 126.5 . . ?
N6 C11 H11 126.5 . . ?
N7 C12 N6 109.5(2) . . ?
N7 C12 H12A 109.8 . . ?
N6 C12 H12A 109.8 . . ?
N7 C12 H12B 109.8 . . ?
N6 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
N8 C13 N7 108.1(3) . . ?
N8 C13 H13 126.0 . . ?
N7 C13 H13 126.0 . . ?
C15 C14 N7 106.6(3) . . ?
C15 C14 H14 126.7 . . ?
N7 C14 H14 126.7 . . ?
C14 C15 N8 107.4(3) . . ?
C14 C15 H15 126.3 . . ?
N8 C15 H15 126.3 . . ?
N1 C16 N8 110.2(2) . . ?
N1 C16 H16A 109.6 . . ?
N8 C16 H16A 109.6 . . ?
N1 C16 H16B 109.6 . . ?
N8 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
F8 P2 F9 91.46(12) . . ?
F8 P2 F10 91.44(12) . . ?
F9 P2 F10 91.13(12) . . ?
F8 P2 F11 90.58(12) . . ?
F9 P2 F11 177.87(13) . . ?
F10 P2 F11 89.43(12) . . ?
F8 P2 F12 90.13(12) . . ?
F9 P2 F12 89.31(11) . . ?
F10 P2 F12 178.36(12) . . ?
F11 P2 F12 90.07(11) . . ?
F8 P2 F7 179.55(13) . . ?
F9 P2 F7 88.95(11) . . ?
F10 P2 F7 88.74(11) . . ?
F11 P2 F7 89.01(11) . . ?
F12 P2 F7 89.69(11) . . ?
F13 P3 F15 92.8(5) . . ?
F13 P3 F18 91.4(5) . . ?
F15 P3 F18 89.9(6) . . ?
F13 P3 F17 92.9(6) . . ?
F15 P3 F17 173.2(7) . . ?
F18 P3 F17 86.3(6) . . ?
F13 P3 F16 91.8(5) . . ?
F15 P3 F16 89.1(6) . . ?
F18 P3 F16 176.6(7) . . ?
F17 P3 F16 94.4(6) . . ?
F13 P3 F14 177.8(7) . . ?
F15 P3 F14 89.5(5) . . ?
F18 P3 F14 88.3(5) . . ?
F17 P3 F14 84.8(6) . . ?
F16 P3 F14 88.5(5) . . ?
F16A P3A F14A 92.8(4) . . ?
F16A P3A F15A 91.1(5) . . ?
F14A P3A F15A 90.8(5) . . ?
F16A P3A F17A 85.8(4) . . ?
F14A P3A F17A 90.5(5) . . ?
F15A P3A F17A 176.7(6) . . ?
F16A P3A F13A 90.1(4) . . ?
F14A P3A F13A 177.1(6) . . ?
F15A P3A F13A 89.4(5) . . ?
F17A P3A F13A 89.4(5) . . ?
F16A P3A F18A 178.4(5) . . ?
F14A P3A F18A 88.4(4) . . ?
F15A P3A F18A 90.1(5) . . ?
F17A P3A F18A 93.0(5) . . ?
F13A P3A F18A 88.7(4) . . ?
F18B P3B F14B 90.7(8) . . ?
F18B P3B F15B 89.6(8) . . ?
F14B P3B F15B 91.4(8) . . ?
F18B P3B F13B 90.7(8) . . ?
F14B P3B F13B 178.6(10) . . ?
F15B P3B F13B 88.8(8) . . ?
F18B P3B F16B 177.2(10) . . ?
F14B P3B F16B 92.0(8) . . ?
F15B P3B F16B 89.4(8) . . ?
F13B P3B F16B 86.7(7) . . ?
F18B P3B F17B 95.0(8) . . ?
F14B P3B F17B 89.8(8) . . ?
F15B P3B F17B 175.2(10) . . ?
F13B P3B F17B 89.9(8) . . ?
F16B P3B F17B 85.9(7) . . ?
N9 C17 C18 175.6(9) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N9 C17A C18A 178.4(14) . . ?
C17A C18A H18D 109.5 . . ?
C17A C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
C17A C18A H18F 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
N10 C19 C20 179.8(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N11 C21 C22 179.2(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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
C2 N1 C1 O1 -177.1(3) . . . . ?
C16 N1 C1 O1 -0.8(4) . . . . ?
C2 N1 C1 N2 1.6(3) . . . . ?
C16 N1 C1 N2 177.8(2) . . . . ?
C3 N2 C1 O1 176.7(3) . . . . ?
C4 N2 C1 O1 2.9(4) . . . . ?
C3 N2 C1 N1 -1.9(3) . . . . ?
C4 N2 C1 N1 -175.8(2) . . . . ?
C1 N1 C2 C3 -0.6(3) . . . . ?
C16 N1 C2 C3 -176.6(3) . . . . ?
N1 C2 C3 N2 -0.6(3) . . . . ?
C1 N2 C3 C2 1.6(3) . . . . ?
C4 N2 C3 C2 174.9(3) . . . . ?
C1 N2 C4 N3 79.3(3) . . . . ?
C3 N2 C4 N3 -93.3(3) . . . . ?
C5 N3 C4 N2 -80.5(3) . . . . ?
C6 N3 C4 N2 89.6(3) . . . . ?
C6 N3 C5 N4 0.6(3) . . . . ?
C4 N3 C5 N4 172.1(2) . . . . ?
C7 N4 C5 N3 -0.1(3) . . . . ?
C8 N4 C5 N3 -175.4(2) . . . . ?
C5 N3 C6 C7 -0.8(3) . . . . ?
C4 N3 C6 C7 -172.2(2) . . . . ?
N3 C6 C7 N4 0.7(3) . . . . ?
C5 N4 C7 C6 -0.4(3) . . . . ?
C8 N4 C7 C6 174.8(2) . . . . ?
C5 N4 C8 N5 79.9(3) . . . . ?
C7 N4 C8 N5 -94.6(3) . . . . ?
C9 N5 C8 N4 -83.0(3) . . . . ?
C10 N5 C8 N4 91.3(3) . . . . ?
C11 N6 C9 N5 0.2(3) . . . . ?
C12 N6 C9 N5 -172.3(2) . . . . ?
C10 N5 C9 N6 0.0(3) . . . . ?
C8 N5 C9 N6 175.2(2) . . . . ?
C9 N5 C10 C11 -0.1(3) . . . . ?
C8 N5 C10 C11 -175.2(2) . . . . ?
N5 C10 C11 N6 0.2(3) . . . . ?
C9 N6 C11 C10 -0.2(3) . . . . ?
C12 N6 C11 C10 172.0(2) . . . . ?
C13 N7 C12 N6 -83.8(3) . . . . ?
C14 N7 C12 N6 87.9(3) . . . . ?
C9 N6 C12 N7 83.4(3) . . . . ?
C11 N6 C12 N7 -87.7(3) . . . . ?
C15 N8 C13 N7 -0.9(3) . . . . ?
C16 N8 C13 N7 -173.0(2) . . . . ?
C14 N7 C13 N8 0.7(3) . . . . ?
C12 N7 C13 N8 173.6(2) . . . . ?
C13 N7 C14 C15 -0.2(3) . . . . ?
C12 N7 C14 C15 -173.0(2) . . . . ?
N7 C14 C15 N8 -0.3(3) . . . . ?
C13 N8 C15 C14 0.7(3) . . . . ?
C16 N8 C15 C14 172.7(2) . . . . ?
C1 N1 C16 N8 -80.0(3) . . . . ?
C2 N1 C16 N8 95.5(3) . . . . ?
C13 N8 C16 N1 83.1(3) . . . . ?
C15 N8 C16 N1 -87.7(3) . . . . ?


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

data_mo_annma42_0m-auto
_database_code_depnum_ccdc_archive 'CCDC 1829615'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 Cu3 N16 O2, 3(C F3 O3 S), 2(C H2 Cl2)'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C37 H36 Cl4 Cu3 F9 N16 O11 S3'
_chemical_formula_iupac          ?
_chemical_formula_weight         1480.45
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 1/2-x,1/2+y,1/2-z
3 -x,-y,-z
4 1/2+x,1/2-y,1/2+z

_cell_length_a                   13.8276(18)
_cell_length_b                   17.576(2)
_cell_length_c                   22.488(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.359(4)
_cell_angle_gamma                90
_cell_volume                     5420.3(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9348
_cell_measurement_theta_min      2.4879
_cell_measurement_theta_max      28.0983
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear yellow'


_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.164
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             2968
_exptl_absorpt_coefficient_mu    1.582
_exptl_crystal_density_meas_temp ?

# Permitted for _exptl_absorpt_correction_type :
# analytical     'analytical from crystal shape'
#                Example: de Meulenaer&Tompa: ABST
# cylinder       'cylindrical'
# gaussian       'Gaussian from crystal shape'
#                Example: PLATON/ABSG
# integration    'integration from crystal shape'
# multi-scan     'symmetry-related measurements'
#                Example: SADABS, MULABS
# none           'no absorption corr. applied'
# numerical      'numerical from crystal shape'
# psi-scan       'psi-scan corrections'
#                Example: PLATON/ABSP
# refdelf        'refined from delta-F'
#                Example: SHELXA,
# sphere         'spherical'
#                Example: PLATON/ABSS
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_absorpt_correction_T_min  0.6098
_exptl_absorpt_correction_T_max  0.6920


#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             F. Kaiser
scanspeed                           20 s per frame
dx                                  45 mm
2737 frames measured in 9 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_monochromator  'Helios optic'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            220273
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             11053
# number of observed reflections (> n sig(I))
_reflns_number_gt                9637
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0571P)²+47.3126P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom


# Permitted for _refine_ls_hydrogen_treatment :
# refall            - refined all H-atom parameters
# refxyz            - refined H-atom coordinates only
# refU              - refined H-atom U only
# noref             - no refinement of H-atom parameters
# constr            - H-atom parameters constrained
# hetero            - H-atom parameters constrained for H on C,
#                     all H-atom parameters refined for H on
#                     heteroatoms
# heteroxyz         - H-atom parameters constrained for H on C,
#                     refined H-atom coordinates only for H
#                     on heteroatoms
# heteroU           - H-atom parameters constrained for H on C,
#                     refined H-atom U's only for H on
#                     heteroatoms
# heteronoref       - H-atom parameters constrained for H on C,
#                     no refinement of H-atom parameters for
#                     H on heteroatoms
# hetero-mixed      - H-atom parameters constrained for H on C
#                     and some heteroatoms, all H-atom
#                     parameters refined for H on remaining
#                     heteroatoms.
# heteroxyz-mixed   - H-atom parameters constrained for H on C
#                     and some heteroatoms, refined H-atom
#                     coordinates only for H on remaining
#                     heteroatoms.
# heteroU-mixed     - H-atom parameters constrained for H on C
#                     and some heteroatoms, refined H-atom
#                     U's only for H on remaining heteroatoms
# heteronoref-mixed - H-atom parameters constrained for H on C
#                     and some heteroatoms, no refinement of
#                     H-atom parameters for H on remaining
#                     heteroatoms
# mixed   - some constrained, some independent
# undef   - H-atom parameters not defined
_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         11053
_refine_ls_number_parameters     922
_refine_ls_number_restraints     192
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0839
_refine_ls_wR_factor_ref         0.2023
_refine_ls_wR_factor_gt          0.1972
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.354
_refine_diff_density_min         -1.789
_refine_diff_density_rms         0.128


# start Validation Reply Form
_vrf_DIFMX02_mo_annma42_0m-auto  
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: The largest residual electron density 
amounts 2.34 and is located 0.855 A from Cu3.
For further information see below.
;
_vrf_PLAT097_mo_annma42_0m-auto  
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.34 eA-3  
RESPONSE: The copper atoms within the sandwich complex
and the whole sandwhich complex itself are rotationally
disordered. Due to the high electron count of copper
compared to the organic ligand frame the ligand related
disorder cannot be resolved. Only two split layers with 
occupancy ratios of approximately 82:18 and 94:6 for
copper atoms Cu1 and Cu3 have been included into the refinement.
All remaining electron densities in the central complex plane
were smaller and have thus been left "as is".
This, combined with the counter ion and
cocrystallized solvent related disorder also leads
to the comparatively high R-values.
;
_vrf_PLAT202_mo_annma42_0m-auto  
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          3 Check 
RESPONSE: One disordered, cocrystallized molecule of dichloromethane
is located centrally in the bowl shaped cavity, generated by the ligand
at the ends of the complex.
Due to disorder the atoms were refined isotropically.
;
_vrf_PLAT971_mo_annma42_0m-auto  
;
PROBLEM: Check Calcd Resid. Dens.  1.00A   From Cu3             2.41 eA-3  
RESPONSE: See above.
;
_vrf_PLAT972_mo_annma42_0m-auto  
;
PROBLEM: Check Calcd Resid. Dens.  0.73A   From Cu2            -1.75 eA-3  
RESPONSE: See above.
;
_vrf_PLAT234_mo_annma42_0m-auto  
;
PROBLEM: Large Hirshfeld Difference S3A      --O11A             0.17 Ang.  
RESPONSE: This arises from disorder in the counterion.
;
_vrf_PLAT244_mo_annma42_0m-auto  
;
PROBLEM: Low    'Solvent' Ueq as Compared to Neighbors of         S1 Check 
RESPONSE: This arises from disorder in the counterion.
;
# end Validation Reply Form

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
Cu1 Cu 0.38708(6) 0.31047(5) 0.55711(4) 0.0255(3) Uani 0.825(2) 1 d . U P A 1
Cu1A Cu 0.3303(3) 0.3315(2) 0.57626(17) 0.0245(9) Uani 0.175(2) 1 d . U P A 2
Cu2 Cu 0.19207(6) 0.23273(5) 0.60479(4) 0.0366(2) Uani 1 1 d . . . . .
Cu3 Cu 0.35665(7) 0.15282(4) 0.52784(3) 0.0322(2) Uani 0.9369(19) 1 d . U P B
11
Cu3A Cu 0.2972(10) 0.1307(7) 0.5471(5) 0.0316(12) Uani 0.0631(19) 1 d . U P B
12
O1 O 0.3042(3) 0.3570(3) 0.6313(2) 0.0404(11) Uani 1 1 d . . . . .
O2 O 0.1959(3) 0.1094(2) 0.53945(18) 0.0320(9) Uani 1 1 d . . . . .
N1 N 0.4249(4) 0.4157(3) 0.6950(3) 0.0435(14) Uani 1 1 d . . . . .
N2 N 0.3025(4) 0.3633(3) 0.7331(3) 0.0417(12) Uani 1 1 d . U . . .
N3 N 0.2422(4) 0.2362(3) 0.7341(2) 0.0338(12) Uani 1 1 d . . . . .
N4 N 0.2823(4) 0.1280(3) 0.7016(2) 0.0306(11) Uani 1 1 d . . . . .
N5 N 0.4110(4) 0.0848(3) 0.6502(2) 0.0298(11) Uani 1 1 d . . . . .
N6 N 0.5306(4) 0.1352(3) 0.6141(2) 0.0390(13) Uani 1 1 d . . . . .
N7 N 0.5918(5) 0.2634(4) 0.6084(3) 0.0446(13) Uani 1 1 d . U . . .
N8 N 0.5515(4) 0.3698(3) 0.6406(2) 0.0390(13) Uani 1 1 d . . . . .
N9 N 0.1470(4) 0.0474(3) 0.4492(2) 0.0314(11) Uani 1 1 d . . . . .
N10 N 0.0356(4) 0.1033(3) 0.4945(2) 0.0299(11) Uani 1 1 d . . . . .
N11 N 0.0090(4) 0.2326(3) 0.5229(2) 0.0304(11) Uani 1 1 d . . . . .
N12 N 0.0810(4) 0.3391(3) 0.5172(2) 0.0276(10) Uani 1 1 d . . . . .
N13 N 0.2215(4) 0.3832(3) 0.4769(2) 0.0282(10) Uani 1 1 d . . . . .
N14 N 0.3279(4) 0.3305(3) 0.4305(2) 0.0346(12) Uani 1 1 d . . . . .
N15 N 0.3551(4) 0.2020(3) 0.3999(2) 0.0373(12) Uani 1 1 d . . . . .
N16 N 0.2872(4) 0.0945(3) 0.4081(2) 0.0347(12) Uani 1 1 d . . . . .
C1 C 0.3392(5) 0.3759(4) 0.6814(3) 0.0404(13) Uani 1 1 d . U . . .
C2 C 0.4403(6) 0.4254(5) 0.7566(4) 0.056(2) Uani 1 1 d . . . . .
H2 H 0.4945 0.4504 0.7784 0.067 Uiso 1 1 calc R U . . .
C3 C 0.3652(6) 0.3931(5) 0.7804(4) 0.055(2) Uani 1 1 d . . . . .
H3 H 0.3570 0.3912 0.8217 0.067 Uiso 1 1 calc R U . . .
C4 C 0.2163(5) 0.3168(4) 0.7359(4) 0.0423(16) Uani 1 1 d . . . . .
H4A H 0.1665 0.3290 0.7016 0.051 Uiso 1 1 calc R U . . .
H4B H 0.1884 0.3279 0.7734 0.051 Uiso 1 1 calc R U . . .
C5 C 0.2469(4) 0.1977(4) 0.6830(3) 0.0344(14) Uani 1 1 d . . . . .
C6 C 0.2730(5) 0.1925(4) 0.7847(3) 0.0417(16) Uani 1 1 d . . . . .
H6 H 0.2754 0.2074 0.8255 0.050 Uiso 1 1 calc R U . . .
C7 C 0.2984(5) 0.1253(4) 0.7638(3) 0.0370(14) Uani 1 1 d . . . . .
H7 H 0.3231 0.0830 0.7873 0.044 Uiso 1 1 calc R U . . .
C8 C 0.3126(4) 0.0697(3) 0.6621(3) 0.0306(13) Uani 1 1 d . . . . .
H8A H 0.3096 0.0191 0.6812 0.037 Uiso 1 1 calc R U . . .
H8B H 0.2680 0.0693 0.6240 0.037 Uiso 1 1 calc R U . . .
C9 C 0.4326(5) 0.1284(4) 0.6027(3) 0.0317(13) Uani 1 1 d . . . . .
C10 C 0.4937(5) 0.0666(4) 0.6891(3) 0.0365(14) Uani 1 1 d . . . . .
H10 H 0.4966 0.0372 0.7247 0.044 Uiso 1 1 calc R U . . .
C11 C 0.5690(5) 0.0990(4) 0.6662(3) 0.0423(16) Uani 1 1 d . . . . .
H11 H 0.6357 0.0973 0.6828 0.051 Uiso 1 1 calc R U . . .
C12 C 0.5862(6) 0.1875(5) 0.5805(3) 0.0497(18) Uani 1 1 d . . . . .
H12A H 0.5543 0.1915 0.5387 0.060 Uiso 1 1 calc R U . . .
H12B H 0.6528 0.1673 0.5797 0.060 Uiso 1 1 calc R U . . .
C13 C 0.5152(5) 0.3115(4) 0.6025(3) 0.0414(14) Uani 1 1 d . U . . .
C14 C 0.6713(6) 0.2900(6) 0.6477(4) 0.058(2) Uani 1 1 d . . . . .
H14 H 0.7321 0.2650 0.6580 0.069 Uiso 1 1 calc R U . . .
C15 C 0.6454(5) 0.3571(5) 0.6679(4) 0.0503(19) Uani 1 1 d . . . . .
H15 H 0.6835 0.3896 0.6954 0.060 Uiso 1 1 calc R U . . .
C16 C 0.4907(6) 0.4343(4) 0.6526(3) 0.0474(18) Uani 1 1 d . . . . .
H16A H 0.5329 0.4771 0.6684 0.057 Uiso 1 1 calc R U . . .
H16B H 0.4526 0.4511 0.6146 0.057 Uiso 1 1 calc R U . . .
C17 C 0.1325(5) 0.0893(3) 0.4986(3) 0.0318(13) Uani 1 1 d . . . . .
C18 C 0.0571(5) 0.0367(4) 0.4145(3) 0.0386(15) Uani 1 1 d . . . . .
H18 H 0.0466 0.0101 0.3775 0.046 Uiso 1 1 calc R U . . .
C19 C -0.0121(5) 0.0704(4) 0.4421(3) 0.0368(15) Uani 1 1 d . . . . .
H19 H -0.0801 0.0716 0.4287 0.044 Uiso 1 1 calc R U . . .
C20 C -0.0074(5) 0.1529(3) 0.5356(3) 0.0341(14) Uani 1 1 d . . . . .
H20A H 0.0213 0.1412 0.5772 0.041 Uiso 1 1 calc R U . . .
H20B H -0.0784 0.1430 0.5322 0.041 Uiso 1 1 calc R U . . .
C21 C 0.0929(5) 0.2702(3) 0.5436(2) 0.0289(12) Uani 1 1 d . . . . .
C22 C -0.0526(5) 0.2773(4) 0.4843(3) 0.0418(16) Uani 1 1 d . . . . .
H22 H -0.1144 0.2631 0.4639 0.050 Uiso 1 1 calc R U . . .
C23 C -0.0081(5) 0.3443(4) 0.4814(3) 0.0381(15) Uani 1 1 d . . . . .
H23 H -0.0328 0.3874 0.4590 0.046 Uiso 1 1 calc R U . . .
C24 C 0.1561(5) 0.3978(3) 0.5214(3) 0.0300(13) Uani 1 1 d . . . . .
H24A H 0.1255 0.4484 0.5143 0.036 Uiso 1 1 calc R U . . .
H24B H 0.1934 0.3975 0.5620 0.036 Uiso 1 1 calc R U . . .
C25 C 0.3007(4) 0.3371(3) 0.4859(3) 0.0290(12) Uani 1 1 d . . . . .
C26 C 0.2004(5) 0.4050(3) 0.4167(3) 0.0325(13) Uani 1 1 d . . . . .
H26 H 0.1489 0.4372 0.3998 0.039 Uiso 1 1 calc R U . . .
C27 C 0.2672(5) 0.3712(4) 0.3880(3) 0.0359(14) Uani 1 1 d . . . . .
H27 H 0.2723 0.3743 0.3464 0.043 Uiso 1 1 calc R U . . .
C28 C 0.3998(5) 0.2758(4) 0.4159(3) 0.0406(15) Uani 1 1 d . . . . .
H28A H 0.4507 0.2696 0.4507 0.049 Uiso 1 1 calc R U . . .
H28B H 0.4315 0.2952 0.3819 0.049 Uiso 1 1 calc R U . . .
C29 C 0.3318(5) 0.1521(4) 0.4418(3) 0.0337(13) Uani 1 1 d . . . . .
C30 C 0.3250(6) 0.1766(5) 0.3417(3) 0.0488(18) Uani 1 1 d . . . . .
H30 H 0.3328 0.2023 0.3055 0.059 Uiso 1 1 calc R U . . .
C31 C 0.2832(6) 0.1092(4) 0.3469(3) 0.0436(16) Uani 1 1 d . . . . .
H31 H 0.2559 0.0772 0.3151 0.052 Uiso 1 1 calc R U . . .
C32 C 0.2431(5) 0.0288(3) 0.4341(3) 0.0374(15) Uani 1 1 d . . . . .
H32A H 0.2378 -0.0138 0.4050 0.045 Uiso 1 1 calc R U . . .
H32B H 0.2854 0.0121 0.4706 0.045 Uiso 1 1 calc R U . . .
S1 S 0.86008(12) 0.11177(9) 0.71547(7) 0.0355(4) Uani 1 1 d . . . . .
F1 F 0.9997(4) 0.2133(3) 0.7267(3) 0.0777(17) Uani 1 1 d . . . . .
F2 F 1.0187(4) 0.1227(3) 0.7901(2) 0.0734(15) Uani 1 1 d . . . . .
F3 F 1.0436(3) 0.1032(3) 0.6994(2) 0.0592(12) Uani 1 1 d . . . . .
O3 O 0.8090(4) 0.1612(3) 0.7517(2) 0.0505(13) Uani 1 1 d . . . . .
O4 O 0.8390(4) 0.1261(4) 0.6520(2) 0.0596(15) Uani 1 1 d . . . . .
O5 O 0.8616(4) 0.0325(3) 0.7301(3) 0.0554(14) Uani 1 1 d . . . . .
C33 C 0.9869(5) 0.1403(4) 0.7334(3) 0.0427(16) Uani 1 1 d . . . . .
S2 S 1.0086(15) 0.4743(13) 0.6546(11) 0.038(5) Uani 0.231(17) 1 d D . P C 9
F4 F 0.852(2) 0.399(2) 0.6237(14) 0.071(7) Uani 0.231(17) 1 d D U P C 9
F5 F 0.913(2) 0.3780(18) 0.7141(12) 0.062(6) Uani 0.231(17) 1 d D U P C 9
F6 F 0.983(3) 0.3276(18) 0.643(2) 0.045(7) Uani 0.231(17) 1 d D U P C 9
O6 O 0.951(2) 0.5298(15) 0.6815(13) 0.040(5) Uani 0.231(17) 1 d D U P C 9
O7 O 1.012(3) 0.483(2) 0.5905(12) 0.033(5) Uani 0.231(17) 1 d D U P C 9
O8 O 1.1004(18) 0.4570(15) 0.6893(15) 0.049(5) Uani 0.231(17) 1 d D U P C 9
C34 C 0.935(2) 0.3898(15) 0.6579(12) 0.042(5) Uani 0.231(17) 1 d D U P C 9
S2A S 1.0205(4) 0.4756(3) 0.6410(3) 0.0261(10) Uani 0.769(17) 1 d D . P C 10
F4A F 0.8525(6) 0.4164(7) 0.6513(6) 0.084(3) Uani 0.769(17) 1 d D U P C 10
F5A F 0.9643(9) 0.3875(5) 0.7236(3) 0.064(3) Uani 0.769(17) 1 d D U P C 10
F6A F 0.9628(13) 0.3340(6) 0.6373(8) 0.069(4) Uani 0.769(17) 1 d D U P C 10
O6A O 0.9908(8) 0.5408(4) 0.6731(4) 0.039(2) Uani 0.769(17) 1 d D U P C 10
O7A O 0.9911(8) 0.4794(7) 0.5768(3) 0.037(2) Uani 0.769(17) 1 d D U P C 10
O8A O 1.1191(5) 0.4513(5) 0.6597(5) 0.048(2) Uani 0.769(17) 1 d D U P C 10
C34A C 0.9452(8) 0.4003(6) 0.6639(5) 0.044(2) Uani 0.769(17) 1 d D U P C 10
S3 S 0.7040(3) 0.1743(3) 0.4418(2) 0.0321(10) Uani 0.457(6) 1 d D . P D 7
F7 F 0.5737(9) 0.1084(10) 0.3614(7) 0.0810(18) Uani 0.457(6) 1 d D U P D 7
F8 F 0.5609(8) 0.0832(8) 0.4554(7) 0.080(2) Uani 0.457(6) 1 d D U P D 7
F9 F 0.6763(15) 0.0361(8) 0.4189(9) 0.139(8) Uani 0.457(6) 1 d D . P D 7
O9 O 0.7618(13) 0.1913(11) 0.3959(8) 0.041(4) Uani 0.457(6) 1 d D U P D 7
O10 O 0.7529(9) 0.1461(9) 0.4967(5) 0.060(3) Uani 0.457(6) 1 d D U P D 7
O11 O 0.6398(11) 0.2368(7) 0.4532(7) 0.071(3) Uani 0.457(6) 1 d D U P D 7
C35 C 0.6193(12) 0.1002(10) 0.4180(9) 0.079(8) Uani 0.457(6) 1 d D . P D 7
S3A S 0.7259(4) 0.1442(3) 0.4301(2) 0.0419(11) Uani 0.543(6) 1 d D . P D 8
F7A F 0.5674(7) 0.2091(6) 0.3689(5) 0.0819(19) Uani 0.543(6) 1 d D U P D 8
F8A F 0.5369(7) 0.1122(7) 0.4217(6) 0.0805(18) Uani 0.543(6) 1 d D U P D 8
F9A F 0.6058(8) 0.1006(8) 0.3423(6) 0.080(2) Uani 0.543(6) 1 d D U P D 8
O9A O 0.7798(11) 0.1769(9) 0.3876(7) 0.045(3) Uani 0.543(6) 1 d D U P D 8
O10A O 0.7464(9) 0.0704(7) 0.4464(6) 0.084(4) Uani 0.543(6) 1 d D U P D 8
O11A O 0.7168(11) 0.1963(8) 0.4796(6) 0.077(3) Uani 0.543(6) 1 d D U P D 8
C35A C 0.6014(8) 0.1428(8) 0.3925(7) 0.061(5) Uani 0.543(6) 1 d D . P D 8
Cl2 Cl 0.7429(2) 0.42721(16) 0.41856(12) 0.0765(7) Uani 1 1 d . . . . .
Cl1 Cl 0.6061(6) 0.4559(5) 0.5057(3) 0.100(2) Uani 0.645(15) 1 d D U P E 3
C36 C 0.7066(9) 0.4001(7) 0.4886(6) 0.102(4) Uani 1 1 d D . . . .
H36A H 0.7622 0.4067 0.5206 0.122 Uiso 0.645(15) 1 calc R U P E 3
H36B H 0.6880 0.3457 0.4872 0.122 Uiso 0.645(15) 1 calc R U P E 3
H36C H 0.7222 0.3459 0.4969 0.122 Uiso 0.355(15) 1 calc R U P E 4
H36D H 0.7412 0.4312 0.5213 0.122 Uiso 0.355(15) 1 calc R U P E 4
Cl1A Cl 0.5858(9) 0.4143(11) 0.4839(7) 0.111(4) Uani 0.355(15) 1 d . U P E 4
Cl3 Cl 0.4932(3) 0.2443(2) 0.7421(2) 0.0648(14) Uiso 0.560(8) 1 d D . P F 5
Cl4 Cl 0.5831(4) 0.2747(3) 0.8628(3) 0.0821(17) Uiso 0.560(8) 1 d D . P F 5
C37 C 0.5778(9) 0.2129(7) 0.8017(5) 0.040(3) Uiso 0.560(8) 1 d D . P F 5
H37A H 0.5591 0.1615 0.8142 0.048 Uiso 0.560(8) 1 calc R U P F 5
H37B H 0.6430 0.2093 0.7883 0.048 Uiso 0.560(8) 1 calc R U P F 5
Cl3A Cl 0.5452(8) 0.2460(6) 0.7709(5) 0.115(3) Uiso 0.440(8) 1 d . . P F 6
Cl4A Cl 0.6079(4) 0.2765(3) 0.8951(3) 0.0555(15) Uiso 0.440(8) 1 d . . P F 6
C37A C 0.5133(15) 0.2338(12) 0.8393(9) 0.059(5) Uiso 0.440(8) 1 d . . P F 6
H37C H 0.5068 0.1789 0.8476 0.070 Uiso 0.440(8) 1 calc R U P F 6
H37D H 0.4496 0.2585 0.8418 0.070 Uiso 0.440(8) 1 calc R U P F 6


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 C25 1.929(6) . ?
Cu1 C13 1.929(7) . ?
Cu1 O1 2.292(5) . ?
Cu1A O1 1.406(6) . ?
Cu1A C25 2.023(7) . ?
Cu1A C1 2.477(8) . ?
Cu2 C5 1.926(6) . ?
Cu2 C21 1.929(6) . ?
Cu3 C9 1.916(6) . ?
Cu3 C29 1.922(6) . ?
Cu3 O2 2.396(5) . ?
Cu3A O2 1.439(14) . ?
Cu3A C9 2.115(14) . ?
Cu3A C17 2.504(15) . ?
Cu3A C29 2.504(12) . ?
O1 C1 1.214(8) . ?
O2 C17 1.237(7) . ?
N1 C1 1.376(9) . ?
N1 C2 1.384(10) . ?
N1 C16 1.437(10) . ?
N2 C1 1.345(10) . ?
N2 C3 1.387(10) . ?
N2 C4 1.453(9) . ?
N3 C5 1.343(9) . ?
N3 C6 1.393(8) . ?
N3 C4 1.463(9) . ?
N4 C5 1.363(8) . ?
N4 C7 1.389(8) . ?
N4 C8 1.452(8) . ?
N5 C9 1.377(8) . ?
N5 C10 1.384(8) . ?
N5 C8 1.446(8) . ?
N6 C9 1.352(9) . ?
N6 C11 1.379(9) . ?
N6 C12 1.468(9) . ?
N7 C13 1.348(10) . ?
N7 C14 1.400(10) . ?
N7 C12 1.471(10) . ?
N8 C15 1.381(9) . ?
N8 C13 1.388(9) . ?
N8 C16 1.456(10) . ?
N9 C17 1.369(8) . ?
N9 C18 1.393(8) . ?
N9 C32 1.450(9) . ?
N10 C17 1.354(8) . ?
N10 C19 1.401(8) . ?
N10 C20 1.450(8) . ?
N11 C21 1.365(8) . ?
N11 C22 1.380(9) . ?
N11 C20 1.454(7) . ?
N12 C21 1.349(7) . ?
N12 C23 1.386(8) . ?
N12 C24 1.459(8) . ?
N13 C25 1.357(8) . ?
N13 C26 1.400(7) . ?
N13 C24 1.455(8) . ?
N14 C25 1.352(8) . ?
N14 C27 1.387(8) . ?
N14 C28 1.450(9) . ?
N15 C29 1.354(8) . ?
N15 C30 1.396(9) . ?
N15 C28 1.462(9) . ?
N16 C29 1.364(9) . ?
N16 C31 1.395(8) . ?
N16 C32 1.462(8) . ?
C2 C3 1.353(12) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 C7 1.336(10) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 C11 1.345(10) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.329(12) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 C19 1.343(10) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C22 C23 1.334(9) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C27 1.333(9) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C30 C31 1.329(11) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
S1 O5 1.430(5) . ?
S1 O3 1.436(5) . ?
S1 O4 1.441(5) . ?
S1 C33 1.818(7) . ?
F1 C33 1.307(8) . ?
F2 C33 1.330(9) . ?
F3 C33 1.333(9) . ?
S2 O8 1.435(16) . ?
S2 O6 1.440(16) . ?
S2 O7 1.455(16) . ?
S2 C34 1.803(17) . ?
F4 C34 1.309(19) . ?
F5 C34 1.354(18) . ?
F6 C34 1.342(18) . ?
S2A O8A 1.440(7) . ?
S2A O6A 1.442(7) . ?
S2A O7A 1.449(8) . ?
S2A C34A 1.801(10) . ?
F4A C34A 1.307(11) . ?
F5A C34A 1.353(10) . ?
F6A C34A 1.347(12) . ?
S3 O9 1.415(11) . ?
S3 O10 1.418(11) . ?
S3 O11 1.455(13) . ?
S3 C35 1.788(15) . ?
F7 C35 1.35(2) . ?
F8 C35 1.274(19) . ?
F9 C35 1.372(19) . ?
S3A O10A 1.366(12) . ?
S3A O9A 1.409(11) . ?
S3A O11A 1.460(13) . ?
S3A C35A 1.819(13) . ?
F7A C35A 1.340(17) . ?
F8A C35A 1.290(16) . ?
F9A C35A 1.360(18) . ?
Cl2 C36 1.777(11) . ?
Cl1 C36 1.782(11) . ?
C36 Cl1A 1.679(18) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 H36C 0.9900 . ?
C36 H36D 0.9900 . ?
Cl3 C37 1.751(11) . ?
Cl4 C37 1.745(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
Cl3A C37A 1.67(2) . ?
Cl4A C37A 1.85(2) . ?
C37A H37C 0.9900 . ?
C37A H37D 0.9900 . ?

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
C25 Cu1 C13 150.1(3) . . ?
C25 Cu1 O1 101.7(2) . . ?
C13 Cu1 O1 97.0(2) . . ?
O1 Cu1A C25 145.7(4) . . ?
O1 Cu1A C1 17.6(3) . . ?
C25 Cu1A C1 157.2(3) . . ?
C5 Cu2 C21 157.1(3) . . ?
C9 Cu3 C29 153.0(3) . . ?
C9 Cu3 O2 104.2(2) . . ?
C29 Cu3 O2 93.4(2) . . ?
O2 Cu3A C9 147.2(7) . . ?
O2 Cu3A C17 19.1(3) . . ?
C9 Cu3A C17 159.9(6) . . ?
O2 Cu3A C29 103.1(6) . . ?
C9 Cu3A C29 107.5(6) . . ?
C17 Cu3A C29 84.5(4) . . ?
C1 O1 Cu1A 141.9(6) . . ?
C1 O1 Cu1 126.6(5) . . ?
C17 O2 Cu3A 138.5(6) . . ?
C17 O2 Cu3 126.0(4) . . ?
C1 N1 C2 107.7(6) . . ?
C1 N1 C16 124.6(6) . . ?
C2 N1 C16 127.3(6) . . ?
C1 N2 C3 109.5(6) . . ?
C1 N2 C4 122.2(6) . . ?
C3 N2 C4 127.9(7) . . ?
C5 N3 C6 112.2(6) . . ?
C5 N3 C4 123.4(6) . . ?
C6 N3 C4 124.2(6) . . ?
C5 N4 C7 110.1(6) . . ?
C5 N4 C8 124.5(5) . . ?
C7 N4 C8 124.7(5) . . ?
C9 N5 C10 112.0(5) . . ?
C9 N5 C8 123.2(5) . . ?
C10 N5 C8 124.2(5) . . ?
C9 N6 C11 112.8(5) . . ?
C9 N6 C12 122.4(6) . . ?
C11 N6 C12 123.8(6) . . ?
C13 N7 C14 113.3(7) . . ?
C13 N7 C12 121.9(6) . . ?
C14 N7 C12 124.5(7) . . ?
C15 N8 C13 113.5(7) . . ?
C15 N8 C16 125.1(6) . . ?
C13 N8 C16 121.2(6) . . ?
C17 N9 C18 108.3(6) . . ?
C17 N9 C32 123.1(5) . . ?
C18 N9 C32 128.1(5) . . ?
C17 N10 C19 109.7(5) . . ?
C17 N10 C20 123.3(5) . . ?
C19 N10 C20 126.6(6) . . ?
C21 N11 C22 111.6(5) . . ?
C21 N11 C20 123.1(5) . . ?
C22 N11 C20 125.0(5) . . ?
C21 N12 C23 111.4(5) . . ?
C21 N12 C24 124.1(5) . . ?
C23 N12 C24 124.3(5) . . ?
C25 N13 C26 111.9(5) . . ?
C25 N13 C24 124.2(5) . . ?
C26 N13 C24 123.1(5) . . ?
C25 N14 C27 112.0(5) . . ?
C25 N14 C28 123.1(5) . . ?
C27 N14 C28 123.9(6) . . ?
C29 N15 C30 112.1(6) . . ?
C29 N15 C28 122.3(6) . . ?
C30 N15 C28 125.4(6) . . ?
C29 N16 C31 111.6(5) . . ?
C29 N16 C32 123.2(5) . . ?
C31 N16 C32 125.1(6) . . ?
O1 C1 N2 127.3(7) . . ?
O1 C1 N1 125.1(7) . . ?
N2 C1 N1 107.5(6) . . ?
O1 C1 Cu1A 20.5(3) . . ?
N2 C1 Cu1A 142.6(5) . . ?
N1 C1 Cu1A 108.0(5) . . ?
C3 C2 N1 108.5(7) . . ?
C3 C2 H2 125.8 . . ?
N1 C2 H2 125.8 . . ?
C2 C3 N2 106.9(7) . . ?
C2 C3 H3 126.5 . . ?
N2 C3 H3 126.5 . . ?
N2 C4 N3 109.8(5) . . ?
N2 C4 H4A 109.7 . . ?
N3 C4 H4A 109.7 . . ?
N2 C4 H4B 109.7 . . ?
N3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N3 C5 N4 104.2(5) . . ?
N3 C5 Cu2 124.3(5) . . ?
N4 C5 Cu2 130.6(5) . . ?
C7 C6 N3 105.4(6) . . ?
C7 C6 H6 127.3 . . ?
N3 C6 H6 127.3 . . ?
C6 C7 N4 108.0(6) . . ?
C6 C7 H7 126.0 . . ?
N4 C7 H7 126.0 . . ?
N5 C8 N4 109.6(5) . . ?
N5 C8 H8A 109.8 . . ?
N4 C8 H8A 109.8 . . ?
N5 C8 H8B 109.8 . . ?
N4 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
N6 C9 N5 102.3(5) . . ?
N6 C9 Cu3 124.7(4) . . ?
N5 C9 Cu3 131.1(5) . . ?
N6 C9 Cu3A 154.2(6) . . ?
N5 C9 Cu3A 101.9(5) . . ?
C11 C10 N5 106.2(6) . . ?
C11 C10 H10 126.9 . . ?
N5 C10 H10 126.9 . . ?
C10 C11 N6 106.7(6) . . ?
C10 C11 H11 126.6 . . ?
N6 C11 H11 126.6 . . ?
N6 C12 N7 110.6(5) . . ?
N6 C12 H12A 109.5 . . ?
N7 C12 H12A 109.5 . . ?
N6 C12 H12B 109.5 . . ?
N7 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N7 C13 N8 100.7(6) . . ?
N7 C13 Cu1 134.7(6) . . ?
N8 C13 Cu1 124.6(5) . . ?
C15 C14 N7 106.7(7) . . ?
C15 C14 H14 126.6 . . ?
N7 C14 H14 126.6 . . ?
C14 C15 N8 105.7(7) . . ?
C14 C15 H15 127.1 . . ?
N8 C15 H15 127.1 . . ?
N1 C16 N8 112.0(6) . . ?
N1 C16 H16A 109.2 . . ?
N8 C16 H16A 109.2 . . ?
N1 C16 H16B 109.2 . . ?
N8 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
O2 C17 N10 126.8(6) . . ?
O2 C17 N9 126.3(6) . . ?
N10 C17 N9 106.9(5) . . ?
O2 C17 Cu3A 22.4(4) . . ?
N10 C17 Cu3A 144.4(5) . . ?
N9 C17 Cu3A 106.9(5) . . ?
C19 C18 N9 108.7(6) . . ?
C19 C18 H18 125.7 . . ?
N9 C18 H18 125.7 . . ?
C18 C19 N10 106.5(6) . . ?
C18 C19 H19 126.8 . . ?
N10 C19 H19 126.8 . . ?
N10 C20 N11 111.5(5) . . ?
N10 C20 H20A 109.3 . . ?
N11 C20 H20A 109.3 . . ?
N10 C20 H20B 109.3 . . ?
N11 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
N12 C21 N11 103.4(5) . . ?
N12 C21 Cu2 131.0(5) . . ?
N11 C21 Cu2 125.1(4) . . ?
C23 C22 N11 106.4(6) . . ?
C23 C22 H22 126.8 . . ?
N11 C22 H22 126.8 . . ?
C22 C23 N12 107.1(6) . . ?
C22 C23 H23 126.5 . . ?
N12 C23 H23 126.5 . . ?
N13 C24 N12 109.4(4) . . ?
N13 C24 H24A 109.8 . . ?
N12 C24 H24A 109.8 . . ?
N13 C24 H24B 109.8 . . ?
N12 C24 H24B 109.8 . . ?
H24A C24 H24B 108.2 . . ?
N14 C25 N13 103.2(5) . . ?
N14 C25 Cu1 121.9(5) . . ?
N13 C25 Cu1 132.2(5) . . ?
N14 C25 Cu1A 151.3(5) . . ?
N13 C25 Cu1A 103.6(4) . . ?
C27 C26 N13 105.9(5) . . ?
C27 C26 H26 127.0 . . ?
N13 C26 H26 127.0 . . ?
C26 C27 N14 107.0(6) . . ?
C26 C27 H27 126.5 . . ?
N14 C27 H27 126.5 . . ?
N14 C28 N15 111.3(5) . . ?
N14 C28 H28A 109.4 . . ?
N15 C28 H28A 109.4 . . ?
N14 C28 H28B 109.4 . . ?
N15 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
N15 C29 N16 103.0(5) . . ?
N15 C29 Cu3 131.9(5) . . ?
N16 C29 Cu3 125.0(5) . . ?
N15 C29 Cu3A 147.8(5) . . ?
N16 C29 Cu3A 106.6(5) . . ?
C31 C30 N15 106.4(6) . . ?
C31 C30 H30 126.8 . . ?
N15 C30 H30 126.8 . . ?
C30 C31 N16 106.8(6) . . ?
C30 C31 H31 126.6 . . ?
N16 C31 H31 126.6 . . ?
N9 C32 N16 110.9(5) . . ?
N9 C32 H32A 109.5 . . ?
N16 C32 H32A 109.5 . . ?
N9 C32 H32B 109.5 . . ?
N16 C32 H32B 109.5 . . ?
H32A C32 H32B 108.0 . . ?
O5 S1 O3 116.9(3) . . ?
O5 S1 O4 113.1(4) . . ?
O3 S1 O4 113.8(3) . . ?
O5 S1 C33 103.4(3) . . ?
O3 S1 C33 103.7(3) . . ?
O4 S1 C33 103.8(4) . . ?
F1 C33 F2 107.8(6) . . ?
F1 C33 F3 108.3(6) . . ?
F2 C33 F3 106.8(6) . . ?
F1 C33 S1 112.7(6) . . ?
F2 C33 S1 109.9(5) . . ?
F3 C33 S1 111.1(5) . . ?
O8 S2 O6 114.3(18) . . ?
O8 S2 O7 115.0(19) . . ?
O6 S2 O7 115.6(19) . . ?
O8 S2 C34 105.4(15) . . ?
O6 S2 C34 101.4(15) . . ?
O7 S2 C34 102.6(16) . . ?
F4 C34 F6 112(2) . . ?
F4 C34 F5 106(2) . . ?
F6 C34 F5 107(2) . . ?
F4 C34 S2 109.3(18) . . ?
F6 C34 S2 111(2) . . ?
F5 C34 S2 111.2(18) . . ?
O8A S2A O6A 114.1(6) . . ?
O8A S2A O7A 116.0(6) . . ?
O6A S2A O7A 113.7(6) . . ?
O8A S2A C34A 105.0(5) . . ?
O6A S2A C34A 103.2(6) . . ?
O7A S2A C34A 102.8(6) . . ?
F4A C34A F6A 108.6(11) . . ?
F4A C34A F5A 108.2(9) . . ?
F6A C34A F5A 105.9(9) . . ?
F4A C34A S2A 111.4(7) . . ?
F6A C34A S2A 111.4(9) . . ?
F5A C34A S2A 111.1(8) . . ?
O9 S3 O10 117.2(10) . . ?
O9 S3 O11 112.6(10) . . ?
O10 S3 O11 110.1(10) . . ?
O9 S3 C35 110.1(10) . . ?
O10 S3 C35 103.1(9) . . ?
O11 S3 C35 102.3(8) . . ?
F8 C35 F7 112.7(14) . . ?
F8 C35 F9 102.1(18) . . ?
F7 C35 F9 107.5(15) . . ?
F8 C35 S3 114.7(12) . . ?
F7 C35 S3 114.3(14) . . ?
F9 C35 S3 103.9(13) . . ?
O10A S3A O9A 117.4(10) . . ?
O10A S3A O11A 115.2(9) . . ?
O9A S3A O11A 111.5(9) . . ?
O10A S3A C35A 105.3(8) . . ?
O9A S3A C35A 103.9(9) . . ?
O11A S3A C35A 101.2(8) . . ?
F8A C35A F7A 109.5(11) . . ?
F8A C35A F9A 107.5(12) . . ?
F7A C35A F9A 101.3(13) . . ?
F8A C35A S3A 116.3(12) . . ?
F7A C35A S3A 115.9(10) . . ?
F9A C35A S3A 104.7(9) . . ?
Cl1A C36 Cl2 107.2(8) . . ?
Cl2 C36 Cl1 111.1(6) . . ?
Cl2 C36 H36A 109.4 . . ?
Cl1 C36 H36A 109.4 . . ?
Cl2 C36 H36B 109.4 . . ?
Cl1 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
Cl1A C36 H36C 110.3 . . ?
Cl2 C36 H36C 110.3 . . ?
Cl1A C36 H36D 110.3 . . ?
Cl2 C36 H36D 110.3 . . ?
H36C C36 H36D 108.5 . . ?
Cl4 C37 Cl3 111.3(7) . . ?
Cl4 C37 H37A 109.4 . . ?
Cl3 C37 H37A 109.4 . . ?
Cl4 C37 H37B 109.4 . . ?
Cl3 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
Cl3A C37A Cl4A 109.0(12) . . ?
Cl3A C37A H37C 109.9 . . ?
Cl4A C37A H37C 109.9 . . ?
Cl3A C37A H37D 109.9 . . ?
Cl4A C37A H37D 109.9 . . ?
H37C C37A H37D 108.3 . . ?


