# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_compound_1
_audit_block_doi                 10.5517/cc754bv
_database_code_depnum_ccdc_archive 'CCDC 213476'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/ja0370342 2004
_audit_update_record             
;
2003-06-23 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
alanyl-glycyl-glycine hydrochloride
;
_chemical_name_common            'ala-gly-gly HCl'
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H14 N3 O4, Cl'
_chemical_formula_sum            'C7 H14 Cl N3 O4'
_chemical_formula_weight         239.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)
_symmetry_space_group_name_Hall  ' P 2ac 2ab '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   5.2258(5)
_cell_length_b                   8.7007(9)
_cell_length_c                   22.970(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1044.42(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4816
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.32

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             504
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   
;
Sheldrick, G. M.; SADABS (1996).
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω-scans
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        <0.1
_diffrn_reflns_number            8593
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2214
_reflns_number_gt                2065
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART 5.625 (Bruker, 2001)'
_computing_cell_refinement       'SAINT 6.22 (Bruker, 2001)'
_computing_data_reduction        'SAINT 6.22 (Bruker, 2001)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F².
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0539P)²+0.9950P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_abs_structure_Flack   0.05(9)
_refine_ls_abs_structure_details ad

_vrf_strde_01_2                  
;

PROBLEM: Alert B A value for _refine_ls_abs_structure_flack has been given,

RESPONSE: Refinement of the non-centrosymmetric structure as the correct
absolute structure was completed based on anomalous dispersion
effects from the chlorine atom in diffraction
measurements on the crystal.
;

_refine_ls_number_reflns         2214
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.053
_refine_ls_R_factor_gt           0.048
_refine_ls_wR_factor_ref         0.109
_refine_ls_wR_factor_gt          0.106
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_restrained_S_all      1.05
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.6354(4) 0.2185(2) 0.04697(9) 0.0129(4) Uani 1 1 d . . .
O2 O 0.8267(4) 0.0131(3) 0.21160(9) 0.0125(5) Uani 1 1 d . . .
O3 O 0.6092(5) -0.2594(3) 0.32138(9) 0.0168(5) Uani 1 1 d . . .
O4 O 0.8237(4) -0.3303(3) 0.24111(10) 0.0147(5) Uani 1 1 d . . .
H4O H 0.923(10) -0.382(6) 0.268(2) 0.022(16) Uiso 1 1 d . . .
N1 N 0.8832(6) 0.4909(3) 0.02787(12) 0.0112(5) Uani 1 1 d . . .
H1NC H 0.983(8) 0.576(5) 0.0258(16) 0.015(10) Uiso 1 1 d . . .
H1NB H 0.917(9) 0.438(5) -0.0021(17) 0.021(11) Uiso 1 1 d . . .
H1NA H 0.718(9) 0.525(5) 0.0307(18) 0.025(11) Uiso 1 1 d . . .
N2 N 0.9685(5) 0.1235(3) 0.10041(11) 0.0102(6) Uani 1 1 d . . .
H2N H 1.113(8) 0.149(4) 0.1190(16) 0.020(10) Uiso 1 1 d . . .
N3 N 0.5483(5) -0.1490(3) 0.17117(12) 0.0117(6) Uani 1 1 d . . .
H3N H 0.500(7) -0.197(4) 0.1396(16) 0.012(9) Uiso 1 1 d . . .
C1 C 0.8402(6) 0.2354(3) 0.07299(13) 0.0091(6) Uani 1 1 d . . .
C2 C 0.9669(6) 0.3926(4) 0.07771(14) 0.0095(6) Uani 1 1 d . . .
H2 H 1.138(7) 0.385(3) 0.0728(13) 0.016(7) Uiso 1 1 d . . .
C3 C 0.8968(7) 0.4721(4) 0.13423(13) 0.0130(6) Uani 1 1 d . . .
H3C H 0.9732 0.5749 0.1350 0.020 Uiso 1 1 calc R . .
H3B H 0.9615 0.4118 0.1671 0.020 Uiso 1 1 calc R . .
H3A H 0.7102 0.4808 0.1371 0.020 Uiso 1 1 calc R . .
C4 C 0.8645(7) -0.0304(3) 0.10781(13) 0.0120(6) Uani 1 1 d . . .
H4B H 1.0033 -0.1067 0.1027 0.014 Uiso 1 1 calc R . .
H4A H 0.7342 -0.0496 0.0774 0.014 Uiso 1 1 calc R . .
C5 C 0.7433(6) -0.0517(3) 0.16751(13) 0.0102(6) Uani 1 1 d . . .
C6 C 0.4426(5) -0.1887(4) 0.22775(13) 0.0132(6) Uani 1 1 d . . .
H6B H 0.2982 -0.2608 0.2220 0.016 Uiso 1 1 calc R . .
H6A H 0.3736 -0.0945 0.2461 0.016 Uiso 1 1 calc R . .
C7 C 0.6342(7) -0.2616(3) 0.26888(13) 0.0117(6) Uani 1 1 d . . .
Cl1 Cl 0.37687(14) 0.68926(8) 0.05423(3) 0.01184(18) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.235(4) . no
O2 C5 1.238(4) . no
O3 C7 1.213(4) . no
O4 C7 1.321(4) . no
O4 H4O 0.92(5) . no
N1 C2 1.495(4) . no
N1 H1NC 0.90(4) . no
N1 H1NB 0.85(4) . no
N1 H1NA 0.91(5) . no
N2 C1 1.340(4) . no
N2 C4 1.455(4) . no
N2 H2N 0.89(4) . no
N3 C5 1.328(4) . no
N3 C6 1.454(4) . no
N3 H3N 0.88(4) . no
C1 C2 1.524(4) . no
C2 C3 1.516(4) . no
C2 H2 0.90(3) . no
C3 H3C 0.9800 . no
C3 H3B 0.9800 . no
C3 H3A 0.9800 . no
C4 C5 1.522(4) . no
C4 H4B 0.9900 . no
C4 H4A 0.9900 . no
C6 C7 1.515(4) . no
C6 H6B 0.9900 . no
C6 H6A 0.9900 . 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_3
_geom_angle_publ_flag
C7 O4 H4O 109(3) . . no
C2 N1 H1NC 110(2) . . no
C2 N1 H1NB 105(3) . . no
H1NC N1 H1NB 106(4) . . no
C2 N1 H1NA 114(3) . . no
H1NC N1 H1NA 107(4) . . no
H1NB N1 H1NA 115(4) . . no
C1 N2 C4 122.5(3) . . no
C1 N2 H2N 118(3) . . no
C4 N2 H2N 119(2) . . no
C5 N3 C6 120.0(3) . . no
C5 N3 H3N 118(2) . . no
C6 N3 H3N 121(2) . . no
O1 C1 N2 125.1(3) . . no
O1 C1 C2 121.2(3) . . no
N2 C1 C2 113.7(3) . . no
N1 C2 C3 108.9(3) . . no
N1 C2 C1 109.4(3) . . no
C3 C2 C1 111.4(2) . . no
N1 C2 H2 103.5(19) . . no
C3 C2 H2 112.2(19) . . no
C1 C2 H2 111(2) . . no
C2 C3 H3C 109.5 . . no
C2 C3 H3B 109.5 . . no
H3C C3 H3B 109.5 . . no
C2 C3 H3A 109.5 . . no
H3C C3 H3A 109.5 . . no
H3B C3 H3A 109.5 . . no
N2 C4 C5 111.9(3) . . no
N2 C4 H4B 109.2 . . no
C5 C4 H4B 109.2 . . no
N2 C4 H4A 109.2 . . no
C5 C4 H4A 109.2 . . no
H4B C4 H4A 107.9 . . no
O2 C5 N3 120.6(3) . . no
O2 C5 C4 122.3(3) . . no
N3 C5 C4 117.0(3) . . no
N3 C6 C7 114.0(2) . . no
N3 C6 H6B 108.8 . . no
C7 C6 H6B 108.8 . . no
N3 C6 H6A 108.8 . . no
C7 C6 H6A 108.8 . . no
H6B C6 H6A 107.7 . . no
O3 C7 O4 124.6(3) . . no
O3 C7 C6 122.8(3) . . no
O4 C7 C6 112.5(3) . . 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
C4 N2 C1 O1 -6.7(5) . . . . no
C4 N2 C1 C2 171.6(3) . . . . no
O1 C1 C2 N1 -25.5(4) . . . . no
N2 C1 C2 N1 156.0(3) . . . . no
O1 C1 C2 C3 95.1(3) . . . . no
N2 C1 C2 C3 -83.4(3) . . . . no
C1 N2 C4 C5 -97.7(3) . . . . no
C6 N3 C5 O2 -4.6(4) . . . . no
C6 N3 C5 C4 172.8(3) . . . . no
N2 C4 C5 O2 -33.3(4) . . . . no
N2 C4 C5 N3 149.3(3) . . . . no
C5 N3 C6 C7 -59.2(4) . . . . no
N3 C6 C7 O3 156.7(3) . . . . no
N3 C6 C7 O4 -25.1(4) . . . . no

_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.946
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_compound1
_audit_block_doi                 10.5517/cc7547r
_database_code_depnum_ccdc_archive 'CCDC 213473'
loop_
_citation_id
_citation_doi
_citation_year
1 10.2174/1570178043400631 2004
_audit_update_record             
;
2003-06-23 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;

_chemical_name_systematic        
;
3-[(RS)-(2,3,4,6-tetra-O-acetyl-alpha-D-glucopyranosyl)sulfinyl]propanenitrile
;
_chemical_formula_moiety         'C17 H23 N O10 S'
_chemical_formula_sum            'C17 H23 N O10 S'
_chemical_formula_weight         433.42
_chemical_absolute_configuration ad

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   8.0982(10)
_cell_length_b                   15.8199(14)
_cell_length_c                   16.3510(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2094.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    51
_cell_measurement_theta_min      5.24
_cell_measurement_theta_max      13.41

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

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.32
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             912
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_T_max  0.5007

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

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 197
_diffrn_standards_decay_%        1
_diffrn_reflns_av_R_equivalents  0.0105
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_number            3528
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             3325
_reflns_number_gt                2694
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0436P)²+0.4248P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0036(9)
_refine_ls_number_reflns         3325
_refine_ls_number_parameters     287
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0914
_refine_ls_wR_factor_gt          0.0835
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.09(10)
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.037

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.14971(10) -0.00290(5) 0.24356(4) 0.04496(18) Uani 1 1 d . . .
O1 O 0.2283(3) -0.08763(12) 0.25397(14) 0.0654(6) Uani 1 1 d . . .
O2 O 0.0246(2) -0.05700(12) 0.40542(11) 0.0410(5) Uani 1 1 d . . .
O3 O -0.1905(2) 0.06684(12) 0.47106(11) 0.0398(5) Uani 1 1 d . . .
O4 O -0.2236(2) 0.20929(12) 0.35473(11) 0.0413(4) Uani 1 1 d . . .
O5 O 0.2031(2) 0.14144(11) 0.33128(11) 0.0381(4) Uani 1 1 d . . .
O6 O 0.2014(3) 0.27626(11) 0.22620(12) 0.0490(5) Uani 1 1 d . . .
O7 O 0.2512(3) -0.08341(14) 0.48045(14) 0.0635(6) Uani 1 1 d . . .
O8 O -0.4278(3) 0.05539(18) 0.40230(13) 0.0618(6) Uani 1 1 d . . .
O9 O -0.2491(4) 0.2814(2) 0.47042(18) 0.1160(13) Uani 1 1 d U . .
O10 O 0.2564(3) 0.41168(12) 0.25174(14) 0.0639(6) Uani 1 1 d . . .
N1 N 0.6569(5) 0.1253(3) 0.1001(3) 0.1065(13) Uani 1 1 d . . .
C1' C 0.1906(3) 0.05331(16) 0.34177(16) 0.0345(6) Uani 1 1 d . . .
C2' C 0.0625(3) 0.03182(16) 0.40703(18) 0.0359(6) Uani 1 1 d . . .
C3' C -0.1001(3) 0.07777(17) 0.39559(16) 0.0351(6) Uani 1 1 d . . .
C4' C -0.0706(3) 0.17171(17) 0.38044(16) 0.0364(6) Uani 1 1 d . . .
C5' C 0.0521(4) 0.18335(16) 0.31096(17) 0.0370(6) Uani 1 1 d . . .
C6' C 0.0960(4) 0.27464(18) 0.2971(2) 0.0443(7) Uani 1 1 d . . .
C7 C 0.1345(4) -0.10886(19) 0.44333(18) 0.0456(7) Uani 1 1 d . . .
C8 C 0.0888(6) -0.1999(2) 0.4310(2) 0.0709(11) Uani 1 1 d . . .
H8A H -0.0273 -0.2041 0.4197 0.09 Uiso 0.5 1 calc PR . .
H8B H 0.1142 -0.2313 0.4796 0.09 Uiso 0.5 1 calc PR . .
H8C H 0.1502 -0.2225 0.3858 0.09 Uiso 0.5 1 calc PR . .
H8D H 0.1853 -0.2346 0.4371 0.09 Uiso 0.5 1 calc PR . .
H8E H 0.0439 -0.2073 0.3771 0.09 Uiso 0.5 1 calc PR . .
H8F H 0.0079 -0.2161 0.471 0.09 Uiso 0.5 1 calc PR . .
C9 C -0.3551(3) 0.05472(18) 0.46514(18) 0.0406(6) Uani 1 1 d . . .
C10 C -0.4313(4) 0.0403(2) 0.54755(19) 0.0614(9) Uani 1 1 d . . .
H10A H -0.3471 0.0425 0.5888 0.09 Uiso 1 1 calc R . .
H10B H -0.4836 -0.0142 0.5486 0.09 Uiso 1 1 calc R . .
H10C H -0.5121 0.0834 0.5581 0.09 Uiso 1 1 calc R . .
C11 C -0.3030(4) 0.2625(2) 0.4056(2) 0.0530(8) Uani 1 1 d U . .
C3 C 0.2881(4) 0.0585(2) 0.18034(17) 0.0501(7) Uani 1 1 d . . .
H3B H 0.2834 0.0369 0.1248 0.09 Uiso 1 1 calc R . .
H3A H 0.2499 0.1166 0.1792 0.09 Uiso 1 1 calc R . .
C13 C 0.2767(4) 0.35046(18) 0.21068(19) 0.0477(7) Uani 1 1 d . . .
C1 C 0.5747(5) 0.0950(2) 0.1482(2) 0.0667(10) Uani 1 1 d . . .
C14 C 0.3855(5) 0.3440(2) 0.1373(2) 0.0720(11) Uani 1 1 d . . .
H14A H 0.3501 0.2975 0.1039 0.09 Uiso 0.5 1 calc PR . .
H14B H 0.4975 0.3348 0.1545 0.09 Uiso 0.5 1 calc PR . .
H14C H 0.379 0.3954 0.1063 0.09 Uiso 0.5 1 calc PR . .
H14D H 0.4677 0.3877 0.1392 0.09 Uiso 0.5 1 calc PR . .
H14E H 0.3202 0.3503 0.0887 0.09 Uiso 0.5 1 calc PR . .
H14F H 0.4387 0.2897 0.1368 0.09 Uiso 0.5 1 calc PR . .
C2 C 0.4654(4) 0.0573(2) 0.2088(2) 0.0587(9) Uani 1 1 d . . .
H2A H 0.4745 0.0882 0.2598 0.09 Uiso 1 1 calc R . .
H2B H 0.499 -0.0007 0.2189 0.09 Uiso 1 1 calc R . .
C12 C -0.4615(4) 0.2907(2) 0.3704(2) 0.0601(9) Uani 1 1 d . . .
H12A H -0.4577 0.2853 0.312 0.09 Uiso 0.5 1 calc PR . .
H12B H -0.4804 0.3487 0.3848 0.09 Uiso 0.5 1 calc PR . .
H12C H -0.5494 0.2564 0.3917 0.09 Uiso 0.5 1 calc PR . .
H12D H -0.534 0.3083 0.4136 0.09 Uiso 0.5 1 calc PR . .
H12E H -0.5113 0.2449 0.3408 0.09 Uiso 0.5 1 calc PR . .
H12F H -0.4423 0.3372 0.334 0.09 Uiso 0.5 1 calc PR . .
H1' H 0.299(4) 0.0361(17) 0.3590(16) 0.04 Uiso 1 1 d . . .
H2' H 0.106(3) 0.0457(17) 0.4612(17) 0.04 Uiso 1 1 d . . .
H3' H -0.166(4) 0.0530(17) 0.3509(16) 0.04 Uiso 1 1 d . . .
H4' H -0.021(3) 0.1997(17) 0.4312(16) 0.04 Uiso 1 1 d . . .
H5' H 0.009(4) 0.1597(16) 0.2604(18) 0.04 Uiso 1 1 d . . .
H6'A H 0.155(4) 0.2972(17) 0.3418(17) 0.04 Uiso 1 1 d . . .
H6'B H -0.007(4) 0.3067(17) 0.2859(16) 0.04 Uiso 1 1 d . . .



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

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.494(2) . ?
S1 C3 1.808(3) . ?
S1 C1' 1.865(3) . ?
O2 C7 1.360(3) . ?
O2 C2' 1.439(3) . ?
O3 C9 1.350(3) . ?
O3 C3' 1.445(3) . ?
O4 C11 1.346(4) . ?
O4 C4' 1.437(3) . ?
O5 C1' 1.408(3) . ?
O5 C5' 1.430(3) . ?
O6 C13 1.347(3) . ?
O6 C6' 1.440(3) . ?
O7 C7 1.193(4) . ?
O8 C9 1.184(3) . ?
O9 C11 1.185(4) . ?
O10 C13 1.190(3) . ?
N1 C1 1.136(5) . ?
C1' C2' 1.526(4) . ?
C1' H1' 0.96(3) . ?
C2' C3' 1.516(4) . ?
C2' H2' 0.98(3) . ?
C3' C4' 1.525(4) . ?
C3' H3' 0.99(3) . ?
C4' C5' 1.520(4) . ?
C4' H4' 1.02(3) . ?
C5' C6' 1.505(4) . ?
C5' H5' 0.97(3) . ?
C6' H6'A 0.94(3) . ?
C6' H6'B 0.99(3) . ?
C7 C8 1.501(5) . ?
C8 H8A 0.96 . ?
C8 H8B 0.96 . ?
C8 H8C 0.96 . ?
C8 H8D 0.96 . ?
C8 H8E 0.96 . ?
C8 H8F 0.96 . ?
C9 C10 1.500(4) . ?
C10 H10A 0.96 . ?
C10 H10B 0.96 . ?
C10 H10C 0.96 . ?
C11 C12 1.475(4) . ?
C3 C2 1.509(5) . ?
C3 H3B 0.97 . ?
C3 H3A 0.97 . ?
C13 C14 1.492(5) . ?
C1 C2 1.457(5) . ?
C14 H14A 0.96 . ?
C14 H14B 0.96 . ?
C14 H14C 0.96 . ?
C14 H14D 0.96 . ?
C14 H14E 0.96 . ?
C14 H14F 0.96 . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C12 H12A 0.96 . ?
C12 H12B 0.96 . ?
C12 H12C 0.96 . ?
C12 H12D 0.96 . ?
C12 H12E 0.96 . ?
C12 H12F 0.96 . ?

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
O1 S1 C3 106.43(14) . . ?
O1 S1 C1' 104.72(13) . . ?
C3 S1 C1' 97.24(13) . . ?
C7 O2 C2' 116.2(2) . . ?
C9 O3 C3' 117.1(2) . . ?
C11 O4 C4' 119.3(2) . . ?
C1' O5 C5' 115.2(2) . . ?
C13 O6 C6' 115.8(2) . . ?
O5 C1' C2' 110.8(2) . . ?
O5 C1' S1 112.33(17) . . ?
C2' C1' S1 112.03(18) . . ?
O5 C1' H1' 104.6(16) . . ?
C2' C1' H1' 110.6(16) . . ?
S1 C1' H1' 106.2(16) . . ?
O2 C2' C3' 106.3(2) . . ?
O2 C2' C1' 110.5(2) . . ?
C3' C2' C1' 113.4(2) . . ?
O2 C2' H2' 108.2(16) . . ?
C3' C2' H2' 108.4(16) . . ?
C1' C2' H2' 109.9(16) . . ?
O3 C3' C2' 106.1(2) . . ?
O3 C3' C4' 109.5(2) . . ?
C2' C3' C4' 110.6(2) . . ?
O3 C3' H3' 108.2(16) . . ?
C2' C3' H3' 111.7(16) . . ?
C4' C3' H3' 110.6(16) . . ?
O4 C4' C5' 107.1(2) . . ?
O4 C4' C3' 108.4(2) . . ?
C5' C4' C3' 110.0(2) . . ?
O4 C4' H4' 113.2(16) . . ?
C5' C4' H4' 107.5(15) . . ?
C3' C4' H4' 110.6(15) . . ?
O5 C5' C6' 106.1(2) . . ?
O5 C5' C4' 109.2(2) . . ?
C6' C5' C4' 112.5(2) . . ?
O5 C5' H5' 109.0(16) . . ?
C6' C5' H5' 109.0(15) . . ?
C4' C5' H5' 110.7(17) . . ?
O6 C6' C5' 106.2(2) . . ?
O6 C6' H6'A 108.3(17) . . ?
C5' C6' H6'A 111.5(17) . . ?
O6 C6' H6'B 110.0(16) . . ?
C5' C6' H6'B 108.6(16) . . ?
H6'A C6' H6'B 112(2) . . ?
O7 C7 O2 123.1(3) . . ?
O7 C7 C8 126.0(3) . . ?
O2 C7 C8 110.9(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8 H8D 109.5 . . ?
H8A C8 H8D 141.1 . . ?
H8B C8 H8D 56.3 . . ?
H8C C8 H8D 56.3 . . ?
C7 C8 H8E 109.5 . . ?
H8A C8 H8E 56.3 . . ?
H8B C8 H8E 141.1 . . ?
H8C C8 H8E 56.3 . . ?
H8D C8 H8E 109.5 . . ?
C7 C8 H8F 109.5 . . ?
H8A C8 H8F 56.3 . . ?
H8B C8 H8F 56.3 . . ?
H8C C8 H8F 141.1 . . ?
H8D C8 H8F 109.5 . . ?
H8E C8 H8F 109.5 . . ?
O8 C9 O3 123.5(3) . . ?
O8 C9 C10 125.2(3) . . ?
O3 C9 C10 111.3(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O9 C11 O4 122.3(3) . . ?
O9 C11 C12 126.3(3) . . ?
O4 C11 C12 111.4(3) . . ?
C2 C3 S1 114.0(2) . . ?
C2 C3 H3B 108.8 . . ?
S1 C3 H3B 108.8 . . ?
C2 C3 H3A 108.8 . . ?
S1 C3 H3A 108.8 . . ?
H3B C3 H3A 107.7 . . ?
O10 C13 O6 122.7(3) . . ?
O10 C13 C14 126.3(3) . . ?
O6 C13 C14 111.0(3) . . ?
N1 C1 C2 178.5(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C14 H14D 109.5 . . ?
H14A C14 H14D 141.1 . . ?
H14B C14 H14D 56.3 . . ?
H14C C14 H14D 56.3 . . ?
C13 C14 H14E 109.5 . . ?
H14A C14 H14E 56.3 . . ?
H14B C14 H14E 141.1 . . ?
H14C C14 H14E 56.3 . . ?
H14D C14 H14E 109.5 . . ?
C13 C14 H14F 109.5 . . ?
H14A C14 H14F 56.3 . . ?
H14B C14 H14F 56.3 . . ?
H14C C14 H14F 141.1 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
C1 C2 C3 111.2(3) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12D 109.5 . . ?
H12A C12 H12D 141.1 . . ?
H12B C12 H12D 56.3 . . ?
H12C C12 H12D 56.3 . . ?
C11 C12 H12E 109.5 . . ?
H12A C12 H12E 56.3 . . ?
H12B C12 H12E 141.1 . . ?
H12C C12 H12E 56.3 . . ?
H12D C12 H12E 109.5 . . ?
C11 C12 H12F 109.5 . . ?
H12A C12 H12F 56.3 . . ?
H12B C12 H12F 56.3 . . ?
H12C C12 H12F 141.1 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 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
C5' O5 C1' C2' -56.6(3) . . . . ?
C5' O5 C1' S1 69.5(2) . . . . ?
O1 S1 C1' O5 150.03(19) . . . . ?
C3 S1 C1' O5 40.9(2) . . . . ?
O1 S1 C1' C2' -84.5(2) . . . . ?
C3 S1 C1' C2' 166.3(2) . . . . ?
C7 O2 C2' C3' -156.6(2) . . . . ?
C7 O2 C2' C1' 80.0(3) . . . . ?
O5 C1' C2' O2 167.8(2) . . . . ?
S1 C1' C2' O2 41.5(3) . . . . ?
O5 C1' C2' C3' 48.5(3) . . . . ?
S1 C1' C2' C3' -77.7(3) . . . . ?
C9 O3 C3' C2' -141.8(2) . . . . ?
C9 O3 C3' C4' 98.8(3) . . . . ?
O2 C2' C3' O3 71.8(3) . . . . ?
C1' C2' C3' O3 -166.6(2) . . . . ?
O2 C2' C3' C4' -169.4(2) . . . . ?
C1' C2' C3' C4' -47.9(3) . . . . ?
C11 O4 C4' C5' -131.6(3) . . . . ?
C11 O4 C4' C3' 109.7(3) . . . . ?
O3 C3' C4' O4 -74.2(3) . . . . ?
C2' C3' C4' O4 169.2(2) . . . . ?
O3 C3' C4' C5' 169.0(2) . . . . ?
C2' C3' C4' C5' 52.4(3) . . . . ?
C1' O5 C5' C6' -176.2(2) . . . . ?
C1' O5 C5' C4' 62.2(3) . . . . ?
O4 C4' C5' O5 -175.79(19) . . . . ?
C3' C4' C5' O5 -58.2(3) . . . . ?
O4 C4' C5' C6' 66.6(3) . . . . ?
C3' C4' C5' C6' -175.8(3) . . . . ?
C13 O6 C6' C5' -169.7(3) . . . . ?
O5 C5' C6' O6 65.0(3) . . . . ?
C4' C5' C6' O6 -175.6(2) . . . . ?
C2' O2 C7 O7 4.4(4) . . . . ?
C2' O2 C7 C8 -175.0(3) . . . . ?
C3' O3 C9 O8 -2.5(4) . . . . ?
C3' O3 C9 C10 177.3(2) . . . . ?
C4' O4 C11 O9 2.0(5) . . . . ?
C4' O4 C11 C12 -176.8(2) . . . . ?
O1 S1 C3 C2 -49.7(3) . . . . ?
C1' S1 C3 C2 58.1(3) . . . . ?
C6' O6 C13 O10 -1.2(4) . . . . ?
C6' O6 C13 C14 178.6(3) . . . . ?
N1 C1 C2 C3 18(18) . . . . ?
S1 C3 C2 C1 170.0(2) . . . . ?

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
C3 H3A O6 0.97 2.67 3.595(4) 159.8 .
C3 H3B O7 0.97 2.49 3.307(4) 142 2_554
C2 H2A O8 0.97 2.51 3.280(4) 135.8 1_655
C1' H1' O8 0.96(3) 2.34(3) 3.245(3) 156(2) 1_655
C12 H12F O1 0.96 2.55 3.377(4) 145 3
C14 H14C O8 0.96 2.57 3.424(5) 149 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_rev.sk13
_audit_block_doi                 10.5517/cc7543m
_database_code_depnum_ccdc_archive 'CCDC 213469'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.poly.2004.01.015 2004
_audit_update_record             
;
2003-06-23 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H33 Cl6 N P2 Pt'
_chemical_formula_weight         985.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.72070(10)
_cell_length_b                   13.8244(2)
_cell_length_c                   14.5320(2)
_cell_angle_alpha                114.84
_cell_angle_beta                 91.4020(10)
_cell_angle_gamma                96.5590(10)
_cell_volume                     1935.45(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    4.152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2875
_exptl_absorpt_correction_T_max  0.5941
_exptl_absorpt_process_details   'Blessing, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'Area detector ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18848
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.08
_diffrn_reflns_theta_max         27.47
_reflns_number_total             8348
_reflns_number_gt                7780
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_cell_refinement       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT  (Siemens, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0304P)²+2.9518P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8348
_refine_ls_number_parameters     490
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0654
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt Pt -0.106109(11) -0.166976(9) 0.189537(9) 0.02554(5) Uani 1 1 d D . .
P1 P 0.06989(8) -0.04184(7) 0.25824(7) 0.03157(18) Uani 1 1 d D A .
P2 P -0.26982(8) -0.30214(7) 0.11227(7) 0.03003(18) Uani 1 1 d D A .
Cl1 Cl -0.20667(9) -0.09911(9) 0.33589(7) 0.0467(2) Uani 1 1 d . A .
Cl1A Cl -0.14788(9) -0.65289(8) 0.23445(7) 0.0431(2) Uani 1 1 d . . .
Cl Cl -0.61386(17) -0.12165(12) 0.71431(17) 0.1000(6) Uani 1 1 d . . .
N' N -0.0128(3) -0.2002(3) 0.0615(3) 0.0253(8) Uani 0.668(4) 1 d PD A 1
C1' C -0.0176(4) -0.2911(4) -0.0187(3) 0.0269(8) Uani 0.668(4) 1 d PD A 1
H1'A H 0.0336 -0.2909 -0.0702 0.032 Uiso 0.668(4) 1 calc PR A 1
C31A C 0.1221(7) -0.0294(6) 0.1459(6) 0.0303(7) Uani 0.668(4) 1 d PD A 1
C32A C 0.2030(9) 0.0599(6) 0.1483(6) 0.0301(11) Uani 0.668(4) 1 d PD A 1
H32A H 0.2332 0.1170 0.2134 0.036 Uiso 0.668(4) 1 d PR A 1
C33A C 0.2309(7) 0.0662(5) 0.0593(5) 0.0336(13) Uani 0.668(4) 1 d PD A 1
H33A H 0.2856 0.1281 0.0633 0.040 Uiso 0.668(4) 1 d PR A 1
C34A C 0.1778(5) -0.0165(5) -0.0310(5) 0.0343(14) Uani 0.668(4) 1 d PD A 1
H34A H 0.1995 -0.0097 -0.0919 0.041 Uiso 0.668(4) 1 d PR A 1
C35A C 0.0983(4) -0.1040(4) -0.0327(4) 0.0331(13) Uani 0.668(4) 1 d PD A 1
H35A H 0.0663 -0.1597 -0.0980 0.040 Uiso 0.668(4) 1 d PR A 1
C36A C 0.0701(4) -0.1105(4) 0.0568(5) 0.0294(11) Uani 0.668(4) 1 d PD A 1
C41A C -0.2026(7) -0.4129(6) 0.0152(6) 0.0299(8) Uani 0.668(4) 1 d PD A 1
C42A C -0.0946(5) -0.3955(5) -0.0383(4) 0.0314(12) Uani 0.668(4) 1 d PD A 1
C43A C -0.0526(5) -0.4819(5) -0.1174(4) 0.0338(12) Uani 0.668(4) 1 d PD A 1
H43A H 0.0175 -0.4679 -0.1520 0.041 Uiso 0.668(4) 1 d PR A 1
C44A C -0.1124(5) -0.5843(5) -0.1458(5) 0.0386(14) Uani 0.668(4) 1 d PD A 1
H44A H -0.0780 -0.6421 -0.1980 0.046 Uiso 0.668(4) 1 d PR A 1
C45A C -0.2158(7) -0.6031(6) -0.0958(6) 0.0376(14) Uani 0.668(4) 1 d PD A 1
H45A H -0.2549 -0.6762 -0.1193 0.045 Uiso 0.668(4) 1 d PR A 1
C46A C -0.2606(9) -0.5180(6) -0.0160(6) 0.0292(17) Uani 0.668(4) 1 d PD A 1
H46A H -0.3346 -0.5350 0.0131 0.035 Uiso 0.668(4) 1 d PR A 1
N'' N -0.0410(6) -0.2578(4) 0.0470(6) 0.0253(8) Uani 0.332(4) 1 d PD A 2
C1'' C 0.0306(8) -0.2142(5) 0.0054(6) 0.0269(8) Uani 0.332(4) 1 d PD A 2
H1'B H 0.0423 -0.2590 -0.0625 0.032 Uiso 0.332(4) 1 calc PR A 2
C31B C 0.1291(15) -0.0232(10) 0.1484(7) 0.0303(7) Uani 0.332(4) 1 d PD A 2
C32B C 0.1977(18) 0.0750(10) 0.1641(8) 0.0301(11) Uani 0.332(4) 1 d PD A 2
H32B H 0.2279 0.1321 0.2292 0.036 Uiso 0.332(4) 1 d PR A 2
C33B C 0.2375(15) 0.0935(9) 0.0810(8) 0.0336(13) Uani 0.332(4) 1 d PD A 2
H33B H 0.2922 0.1555 0.0850 0.040 Uiso 0.332(4) 1 d PR A 2
C34B C 0.2098(11) 0.0151(9) -0.0189(7) 0.0343(14) Uani 0.332(4) 1 d PD A 2
H34B H 0.2315 0.0219 -0.0798 0.041 Uiso 0.332(4) 1 d PR A 2
C35B C 0.1428(9) -0.0823(8) -0.0379(6) 0.0331(13) Uani 0.332(4) 1 d PD A 2
H35B H 0.1108 -0.1380 -0.1032 0.040 Uiso 0.332(4) 1 d PR A 2
C36B C 0.1016(7) -0.1034(7) 0.0439(6) 0.0294(11) Uani 0.332(4) 1 d PD A 2
C41B C -0.2031(11) -0.4071(8) 0.0127(12) 0.0299(8) Uani 0.332(4) 1 d PD A 2
C42B C -0.0873(8) -0.3730(6) -0.0094(5) 0.0314(12) Uani 0.332(4) 1 d PD A 2
C43B C -0.0253(8) -0.4471(7) -0.0805(7) 0.0338(12) Uani 0.332(4) 1 d PD A 2
H43B H 0.0448 -0.4331 -0.1150 0.041 Uiso 0.332(4) 1 d PR A 2
C44B C -0.0784(10) -0.5546(7) -0.1293(8) 0.0386(14) Uani 0.332(4) 1 d PD A 2
H44B H -0.0440 -0.6125 -0.1814 0.046 Uiso 0.332(4) 1 d PR A 2
C45B C -0.1948(13) -0.5899(8) -0.1076(11) 0.0376(14) Uani 0.332(4) 1 d PD A 2
H45B H -0.2340 -0.6631 -0.1311 0.045 Uiso 0.332(4) 1 d PR A 2
C46B C -0.2576(16) -0.5154(8) -0.0361(14) 0.0292(17) Uani 0.332(4) 1 d PD A 2
H46B H -0.3317 -0.5324 -0.0070 0.035 Uiso 0.332(4) 1 d PR A 2
C11 C 0.0564(3) 0.0919(3) 0.3535(3) 0.0340(7) Uani 1 1 d . . .
C12 C -0.0353(4) 0.1484(3) 0.3375(3) 0.0423(8) Uani 1 1 d . A .
H12A H -0.0905 0.1156 0.2762 0.051 Uiso 1 1 d R . .
C13 C -0.0474(5) 0.2508(4) 0.4100(3) 0.0505(10) Uani 1 1 d . . .
H13A H -0.1115 0.2889 0.3992 0.061 Uiso 1 1 d R A .
C14 C 0.0317(5) 0.2965(3) 0.4987(4) 0.0538(11) Uani 1 1 d . A .
H14A H 0.0263 0.3685 0.5478 0.065 Uiso 1 1 d R . .
C15 C 0.1196(5) 0.2406(4) 0.5156(4) 0.0596(12) Uani 1 1 d . . .
H15A H 0.1724 0.2716 0.5782 0.072 Uiso 1 1 d R A .
C16 C 0.1330(4) 0.1382(3) 0.4429(3) 0.0485(10) Uani 1 1 d . A .
H16A H 0.1951 0.0990 0.4548 0.058 Uiso 1 1 d R . .
C21 C 0.1945(3) -0.0861(3) 0.3122(3) 0.0358(8) Uani 1 1 d . . .
C22 C 0.1611(4) -0.1342(4) 0.3769(4) 0.0475(10) Uani 1 1 d . A .
H22A H 0.0739 -0.1500 0.3858 0.057 Uiso 1 1 d R . .
C23 C 0.2553(5) -0.1576(4) 0.4293(4) 0.0574(12) Uani 1 1 d . . .
H23A H 0.2333 -0.1905 0.4743 0.069 Uiso 1 1 d R A .
C24 C 0.3804(4) -0.1349(4) 0.4157(4) 0.0515(10) Uani 1 1 d . A .
H24A H 0.4450 -0.1505 0.4524 0.062 Uiso 1 1 d R . .
C25 C 0.4125(4) -0.0896(4) 0.3506(4) 0.0535(11) Uani 1 1 d . . .
H25A H 0.4997 -0.0732 0.3421 0.064 Uiso 1 1 d R A .
C26 C 0.3201(4) -0.0658(4) 0.2980(3) 0.0465(9) Uani 1 1 d . A .
H26A H 0.3432 -0.0364 0.2506 0.056 Uiso 1 1 d R . .
C51 C -0.3926(3) -0.2642(3) 0.0508(3) 0.0314(7) Uani 1 1 d . . .
C52 C -0.4585(4) -0.3358(3) -0.0409(3) 0.0381(8) Uani 1 1 d . A .
H52A H -0.4370 -0.4072 -0.0755 0.046 Uiso 1 1 d R . .
C53 C -0.5553(4) -0.3035(3) -0.0818(3) 0.0452(9) Uani 1 1 d . . .
H53A H -0.6013 -0.3532 -0.1446 0.054 Uiso 1 1 d R A .
C54 C -0.5852(4) -0.2008(4) -0.0335(3) 0.0455(9) Uani 1 1 d . A .
H54A H -0.6539 -0.1797 -0.0611 0.055 Uiso 1 1 d R . .
C55 C -0.5185(4) -0.1280(3) 0.0567(3) 0.0478(10) Uani 1 1 d . . .
H55A H -0.5356 -0.0549 0.0886 0.057 Uiso 1 1 d R A .
C56 C -0.4231(4) -0.1599(3) 0.0993(3) 0.0390(8) Uani 1 1 d . A .
H56A H -0.3779 -0.1103 0.1625 0.047 Uiso 1 1 d R . .
C61 C -0.3481(3) -0.3592(3) 0.1910(3) 0.0321(7) Uani 1 1 d . . .
C62 C -0.4717(4) -0.3463(3) 0.2134(3) 0.0436(9) Uani 1 1 d . A .
H62A H -0.5195 -0.3117 0.1822 0.052 Uiso 1 1 d R . .
C63 C -0.5277(4) -0.3860(3) 0.2781(4) 0.0502(10) Uani 1 1 d . . .
H63A H -0.6131 -0.3767 0.2941 0.060 Uiso 1 1 d R A .
C64 C -0.4591(4) -0.4370(3) 0.3220(3) 0.0468(9) Uani 1 1 d . A .
H64A H -0.4969 -0.4623 0.3685 0.056 Uiso 1 1 d R . .
C65 C -0.3353(4) -0.4501(3) 0.3007(3) 0.0436(9) Uani 1 1 d . . .
H65A H -0.2892 -0.4875 0.3297 0.052 Uiso 1 1 d R A .
C66 C -0.2800(4) -0.4116(3) 0.2347(3) 0.0384(8) Uani 1 1 d . A .
H66A H -0.1940 -0.4199 0.2201 0.046 Uiso 1 1 d R . .
Cl1B Cl -0.4701(2) -0.2874(2) 0.59454(16) 0.1179(7) Uani 1 1 d . . .
C10A C 0.1715(5) 0.3910(5) 0.3331(5) 0.0798(17) Uani 1 1 d . . .
H1B H 0.1717 0.3352 0.3561 0.096 Uiso 1 1 d R . .
H1C H 0.0860 0.3925 0.3133 0.096 Uiso 1 1 d R . .
C20A C -0.5663(6) -0.2460(5) 0.6924(5) 0.0828(18) Uani 1 1 d . . .
H2A H -0.5224 -0.2402 0.7533 0.099 Uiso 1 1 d R . .
H2B H -0.6393 -0.2991 0.6763 0.099 Uiso 1 1 d R . .
Cl2A Cl 0.25921(14) 0.35977(11) 0.22870(11) 0.0707(3) Uani 1 1 d . . .
Cl2B Cl 0.2254(2) 0.51580(18) 0.43277(18) 0.1267(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt N' 2.038(4) . ?
Pt N'' 2.107(7) . ?
Pt P2 2.2857(8) . ?
Pt Cl1 2.2875(9) . ?
Pt P1 2.2936(8) . ?
P1 C31A 1.807(7) . ?
P1 C11 1.810(4) . ?
P1 C21 1.820(4) . ?
P1 C31B 1.837(8) . ?
P2 C41B 1.798(8) . ?
P2 C61 1.814(4) . ?
P2 C51 1.816(3) . ?
P2 C41A 1.827(7) . ?
Cl C20A 1.751(6) . ?
N' C1' 1.301(6) . ?
N' C36A 1.467(6) . ?
C1' C42A 1.488(7) . ?
C31A C36A 1.359(10) . ?
C31A C32A 1.413(9) . ?
C32A C33A 1.371(10) . ?
C33A C34A 1.381(8) . ?
C34A C35A 1.389(7) . ?
C35A C36A 1.379(8) . ?
C41A C46A 1.389(9) . ?
C41A C42A 1.464(10) . ?
C42A C43A 1.395(8) . ?
C43A C44A 1.369(7) . ?
C44A C45A 1.399(9) . ?
C45A C46A 1.403(10) . ?
N'' C1'' 1.241(8) . ?
N'' C42B 1.469(8) . ?
C1'' C36B 1.494(8) . ?
C31B C32B 1.393(11) . ?
C31B C36B 1.453(11) . ?
C32B C33B 1.403(11) . ?
C33B C34B 1.398(10) . ?
C34B C35B 1.365(8) . ?
C35B C36B 1.407(9) . ?
C41B C42B 1.371(11) . ?
C41B C46B 1.406(10) . ?
C42B C43B 1.363(9) . ?
C43B C44B 1.392(8) . ?
C44B C45B 1.380(9) . ?
C45B C46B 1.374(11) . ?
C11 C16 1.379(5) . ?
C11 C12 1.396(5) . ?
C12 C13 1.388(6) . ?
C13 C14 1.386(6) . ?
C14 C15 1.364(7) . ?
C15 C16 1.392(6) . ?
C21 C26 1.383(5) . ?
C21 C22 1.393(5) . ?
C22 C23 1.396(6) . ?
C23 C24 1.381(7) . ?
C24 C25 1.369(6) . ?
C25 C26 1.387(6) . ?
C51 C52 1.393(5) . ?
C51 C56 1.395(5) . ?
C52 C53 1.388(5) . ?
C53 C54 1.374(6) . ?
C54 C55 1.388(6) . ?
C55 C56 1.388(5) . ?
C61 C62 1.387(5) . ?
C61 C66 1.394(5) . ?
C62 C63 1.390(6) . ?
C63 C64 1.385(6) . ?
C64 C65 1.385(6) . ?
C65 C66 1.393(5) . ?
Cl1B C20A 1.714(6) . ?
C10A Cl2A 1.728(6) . ?
C10A Cl2B 1.744(7) . ?

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
N' Pt N'' 20.93(18) . . ?
N' Pt P2 95.14(10) . . ?
N'' Pt P2 77.33(16) . . ?
N' Pt Cl1 169.83(10) . . ?
N'' Pt Cl1 168.19(14) . . ?
P2 Pt Cl1 91.29(3) . . ?
N' Pt P1 80.85(10) . . ?
N'' Pt P1 98.09(16) . . ?
P2 Pt P1 174.84(3) . . ?
Cl1 Pt P1 93.14(3) . . ?
C31A P1 C11 107.7(3) . . ?
C31A P1 C21 108.8(3) . . ?
C11 P1 C21 104.53(17) . . ?
C31A P1 C31B 3.0(6) . . ?
C11 P1 C31B 105.6(4) . . ?
C21 P1 C31B 107.6(6) . . ?
C31A P1 Pt 100.5(3) . . ?
C11 P1 Pt 120.32(12) . . ?
C21 P1 Pt 114.48(12) . . ?
C31B P1 Pt 103.4(4) . . ?
C41B P2 C61 108.2(5) . . ?
C41B P2 C51 106.5(7) . . ?
C61 P2 C51 106.42(16) . . ?
C41B P2 C41A 3.1(9) . . ?
C61 P2 C41A 105.2(3) . . ?
C51 P2 C41A 108.6(3) . . ?
C41B P2 Pt 105.2(3) . . ?
C61 P2 Pt 116.91(11) . . ?
C51 P2 Pt 113.09(11) . . ?
C41A P2 Pt 106.1(2) . . ?
C1' N' C36A 114.6(4) . . ?
C1' N' Pt 128.6(3) . . ?
C36A N' Pt 116.8(3) . . ?
N' C1' C42A 127.6(4) . . ?
C36A C31A C32A 121.6(6) . . ?
C36A C31A P1 114.3(5) . . ?
C32A C31A P1 123.9(6) . . ?
C33A C32A C31A 120.0(6) . . ?
C32A C33A C34A 118.0(6) . . ?
C33A C34A C35A 121.6(6) . . ?
C36A C35A C34A 120.5(5) . . ?
C31A C36A C35A 118.3(5) . . ?
C31A C36A N' 118.0(5) . . ?
C35A C36A N' 123.8(5) . . ?
C46A C41A C42A 117.4(6) . . ?
C46A C41A P2 119.8(6) . . ?
C42A C41A P2 122.6(5) . . ?
C43A C42A C41A 120.6(5) . . ?
C43A C42A C1' 112.1(5) . . ?
C41A C42A C1' 127.2(5) . . ?
C44A C43A C42A 120.1(6) . . ?
C43A C44A C45A 120.3(6) . . ?
C44A C45A C46A 121.0(6) . . ?
C41A C46A C45A 120.5(6) . . ?
C1'' N'' C42B 118.1(6) . . ?
C1'' N'' Pt 121.0(5) . . ?
C42B N'' Pt 120.7(4) . . ?
N'' C1'' C36B 131.6(7) . . ?
C32B C31B C36B 117.3(7) . . ?
C32B C31B P1 119.0(7) . . ?
C36B C31B P1 123.5(6) . . ?
C31B C32B C33B 120.2(7) . . ?
C34B C33B C32B 121.4(7) . . ?
C35B C34B C33B 120.4(7) . . ?
C34B C35B C36B 119.6(7) . . ?
C35B C36B C31B 121.1(6) . . ?
C35B C36B C1'' 110.3(6) . . ?
C31B C36B C1'' 128.6(6) . . ?
C42B C41B C46B 121.5(7) . . ?
C42B C41B P2 113.3(6) . . ?
C46B C41B P2 125.1(7) . . ?
C43B C42B C41B 118.3(6) . . ?
C43B C42B N'' 125.7(6) . . ?
C41B C42B N'' 116.0(6) . . ?
C42B C43B C44B 120.8(6) . . ?
C45B C44B C43B 121.5(7) . . ?
C46B C45B C44B 117.9(7) . . ?
C45B C46B C41B 120.1(7) . . ?
C16 C11 C12 119.2(4) . . ?
C16 C11 P1 121.3(3) . . ?
C12 C11 P1 119.5(3) . . ?
C13 C12 C11 120.2(4) . . ?
C14 C13 C12 119.6(4) . . ?
C15 C14 C13 120.3(4) . . ?
C14 C15 C16 120.4(4) . . ?
C11 C16 C15 120.2(4) . . ?
C26 C21 C22 119.6(3) . . ?
C26 C21 P1 122.5(3) . . ?
C22 C21 P1 117.7(3) . . ?
C21 C22 C23 119.5(4) . . ?
C24 C23 C22 120.2(4) . . ?
C25 C24 C23 120.0(4) . . ?
C24 C25 C26 120.5(4) . . ?
C21 C26 C25 120.2(4) . . ?
C52 C51 C56 119.4(3) . . ?
C52 C51 P2 122.5(3) . . ?
C56 C51 P2 118.1(3) . . ?
C53 C52 C51 119.8(4) . . ?
C54 C53 C52 120.6(4) . . ?
C53 C54 C55 120.2(4) . . ?
C54 C55 C56 119.8(4) . . ?
C55 C56 C51 120.3(4) . . ?
C62 C61 C66 119.4(3) . . ?
C62 C61 P2 121.3(3) . . ?
C66 C61 P2 119.2(3) . . ?
C61 C62 C63 120.2(4) . . ?
C64 C63 C62 120.0(4) . . ?
C65 C64 C63 120.4(4) . . ?
C64 C65 C66 119.5(4) . . ?
C65 C66 C61 120.4(4) . . ?
Cl2A C10A Cl2B 113.6(3) . . ?
Cl1B C20A Cl 111.9(3) . . ?

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
N' Pt P1 C31A 22.3(3) . . . . ?
N'' Pt P1 C31A 34.3(3) . . . . ?
P2 Pt P1 C31A 61.4(4) . . . . ?
Cl1 Pt P1 C31A -149.4(3) . . . . ?
N' Pt P1 C11 140.17(17) . . . . ?
N'' Pt P1 C11 152.1(2) . . . . ?
P2 Pt P1 C11 179(14) . . . . ?
Cl1 Pt P1 C11 -31.57(14) . . . . ?
N' Pt P1 C21 -93.98(17) . . . . ?
N'' Pt P1 C21 -82.1(2) . . . . ?
P2 Pt P1 C21 -54.9(4) . . . . ?
Cl1 Pt P1 C21 94.27(14) . . . . ?
N' Pt P1 C31B 22.8(6) . . . . ?
N'' Pt P1 C31B 34.7(6) . . . . ?
P2 Pt P1 C31B 61.9(7) . . . . ?
Cl1 Pt P1 C31B -149.0(6) . . . . ?
N' Pt P2 C41B 31.0(7) . . . . ?
N'' Pt P2 C41B 19.9(7) . . . . ?
Cl1 Pt P2 C41B -156.9(7) . . . . ?
P1 Pt P2 C41B -7.7(8) . . . . ?
N' Pt P2 C61 151.06(16) . . . . ?
N'' Pt P2 C61 140.0(2) . . . . ?
Cl1 Pt P2 C61 -36.84(13) . . . . ?
P1 Pt P2 C61 112.4(4) . . . . ?
N' Pt P2 C51 -84.82(16) . . . . ?
N'' Pt P2 C51 -95.9(2) . . . . ?
Cl1 Pt P2 C51 87.28(13) . . . . ?
P1 Pt P2 C51 -123.5(3) . . . . ?
N' Pt P2 C41A 34.1(3) . . . . ?
N'' Pt P2 C41A 23.0(4) . . . . ?
Cl1 Pt P2 C41A -153.8(3) . . . . ?
P1 Pt P2 C41A -4.6(5) . . . . ?
N'' Pt N' C1' 6.2(7) . . . . ?
P2 Pt N' C1' -25.4(4) . . . . ?
Cl1 Pt N' C1' -154.3(4) . . . . ?
P1 Pt N' C1' 151.4(4) . . . . ?
N'' Pt N' C36A -174.6(8) . . . . ?
P2 Pt N' C36A 153.8(2) . . . . ?
Cl1 Pt N' C36A 24.8(8) . . . . ?
P1 Pt N' C36A -29.5(2) . . . . ?
C36A N' C1' C42A -178.4(3) . . . . ?
Pt N' C1' C42A 0.7(6) . . . . ?
C11 P1 C31A C36A -143.1(4) . . . . ?
C21 P1 C31A C36A 104.2(4) . . . . ?
C31B P1 C31A C36A 172(16) . . . . ?
Pt P1 C31A C36A -16.3(5) . . . . ?
C11 P1 C31A C32A 32.7(3) . . . . ?
C21 P1 C31A C32A -80.1(2) . . . . ?
C31B P1 C31A C32A -12(16) . . . . ?
Pt P1 C31A C32A 159.43(14) . . . . ?
C36A C31A C32A C33A -0.01(9) . . . . ?
P1 C31A C32A C33A -175.5(5) . . . . ?
C31A C32A C33A C34A 0.01(8) . . . . ?
C32A C33A C34A C35A 0.02(19) . . . . ?
C33A C34A C35A C36A 0.0(3) . . . . ?
C32A C31A C36A C35A -0.02(19) . . . . ?
P1 C31A C36A C35A 175.8(5) . . . . ?
C32A C31A C36A N' 179.95(11) . . . . ?
P1 C31A C36A N' -4.2(5) . . . . ?
C34A C35A C36A C31A 0.1(2) . . . . ?
C34A C35A C36A N' -179.93(17) . . . . ?
C1' N' C36A C31A -153.0(4) . . . . ?
Pt N' C36A C31A 27.7(4) . . . . ?
C1' N' C36A C35A 26.9(5) . . . . ?
Pt N' C36A C35A -152.3(3) . . . . ?
C41B P2 C41A C46A -132(12) . . . . ?
C61 P2 C41A C46A 29.3(3) . . . . ?
C51 P2 C41A C46A -84.3(3) . . . . ?
Pt P2 C41A C46A 153.83(16) . . . . ?
C41B P2 C41A C42A 43(12) . . . . ?
C61 P2 C41A C42A -155.9(4) . . . . ?
C51 P2 C41A C42A 90.5(5) . . . . ?
Pt P2 C41A C42A -31.4(6) . . . . ?
C46A C41A C42A C43A 0.02(8) . . . . ?
P2 C41A C42A C43A -174.9(6) . . . . ?
C46A C41A C42A C1' -179.87(12) . . . . ?
P2 C41A C42A C1' 5.2(6) . . . . ?
N' C1' C42A C43A -163.7(4) . . . . ?
N' C1' C42A C41A 16.2(4) . . . . ?
C41A C42A C43A C44A 0.01(8) . . . . ?
C1' C42A C43A C44A 179.92(11) . . . . ?
C42A C43A C44A C45A -0.11(18) . . . . ?
C43A C44A C45A C46A 0.2(2) . . . . ?
C42A C41A C46A C45A 0.05(18) . . . . ?
P2 C41A C46A C45A 175.1(6) . . . . ?
C44A C45A C46A C41A -0.2(2) . . . . ?
N' Pt N'' C1'' 1.0(6) . . . . ?
P2 Pt N'' C1'' 148.7(7) . . . . ?
Cl1 Pt N'' C1'' 164.3(7) . . . . ?
P1 Pt N'' C1'' -33.8(7) . . . . ?
N' Pt N'' C42B -174.1(10) . . . . ?
P2 Pt N'' C42B -26.4(4) . . . . ?
Cl1 Pt N'' C42B -10.8(13) . . . . ?
P1 Pt N'' C42B 151.1(4) . . . . ?
C42B N'' C1'' C36B -174.2(7) . . . . ?
Pt N'' C1'' C36B 10.6(12) . . . . ?
C31A P1 C31B C32B 161(16) . . . . ?
C11 P1 C31B C32B 25.0(4) . . . . ?
C21 P1 C31B C32B -86.3(4) . . . . ?
Pt P1 C31B C32B 152.2(3) . . . . ?
C31A P1 C31B C36B -15(15) . . . . ?
C11 P1 C31B C36B -151.0(9) . . . . ?
C21 P1 C31B C36B 97.8(10) . . . . ?
Pt P1 C31B C36B -23.7(12) . . . . ?
C36B C31B C32B C33B 0.00(8) . . . . ?
P1 C31B C32B C33B -176.2(11) . . . . ?
C31B C32B C33B C34B 0.01(9) . . . . ?
C32B C33B C34B C35B 0.0(2) . . . . ?
C33B C34B C35B C36B 0.0(3) . . . . ?
C34B C35B C36B C31B 0.0(3) . . . . ?
C34B C35B C36B C1'' -179.98(17) . . . . ?
C32B C31B C36B C35B -0.02(19) . . . . ?
P1 C31B C36B C35B 176.0(12) . . . . ?
C32B C31B C36B C1'' 179.98(14) . . . . ?
P1 C31B C36B C1'' -4.0(12) . . . . ?
N'' C1'' C36B C35B -164.2(9) . . . . ?
N'' C1'' C36B C31B 15.8(10) . . . . ?
C61 P2 C41B C42B -141.2(8) . . . . ?
C51 P2 C41B C42B 104.8(10) . . . . ?
C41A P2 C41B C42B -122(13) . . . . ?
Pt P2 C41B C42B -15.5(12) . . . . ?
C61 P2 C41B C46B 35.6(5) . . . . ?
C51 P2 C41B C46B -78.4(4) . . . . ?
C41A P2 C41B C46B 54(12) . . . . ?
Pt P2 C41B C46B 161.3(3) . . . . ?
C46B C41B C42B C43B 0.01(9) . . . . ?
P2 C41B C42B C43B 177.0(12) . . . . ?
C46B C41B C42B N'' -179.94(12) . . . . ?
P2 C41B C42B N'' -3.0(12) . . . . ?
C1'' N'' C42B C43B 29.2(10) . . . . ?
Pt N'' C42B C43B -155.6(7) . . . . ?
C1'' N'' C42B C41B -150.9(10) . . . . ?
Pt N'' C42B C41B 24.4(7) . . . . ?
C41B C42B C43B C44B 0.01(9) . . . . ?
N'' C42B C43B C44B 179.96(13) . . . . ?
C42B C43B C44B C45B -0.1(2) . . . . ?
C43B C44B C45B C46B 0.1(3) . . . . ?
C44B C45B C46B C41B -0.1(3) . . . . ?
C42B C41B C46B C45B 0.0(2) . . . . ?
P2 C41B C46B C45B -176.6(13) . . . . ?
C31A P1 C11 C16 -114.9(4) . . . . ?
C21 P1 C11 C16 0.7(4) . . . . ?
C31B P1 C11 C16 -112.7(6) . . . . ?
Pt P1 C11 C16 131.1(3) . . . . ?
C31A P1 C11 C12 66.6(4) . . . . ?
C21 P1 C11 C12 -177.8(3) . . . . ?
C31B P1 C11 C12 68.8(6) . . . . ?
Pt P1 C11 C12 -47.4(3) . . . . ?
C16 C11 C12 C13 1.2(6) . . . . ?
P1 C11 C12 C13 179.7(3) . . . . ?
C11 C12 C13 C14 -0.3(6) . . . . ?
C12 C13 C14 C15 -1.1(7) . . . . ?
C13 C14 C15 C16 1.6(8) . . . . ?
C12 C11 C16 C15 -0.7(6) . . . . ?
P1 C11 C16 C15 -179.1(4) . . . . ?
C14 C15 C16 C11 -0.7(7) . . . . ?
C31A P1 C21 C26 26.2(5) . . . . ?
C11 P1 C21 C26 -88.7(4) . . . . ?
C31B P1 C21 C26 23.3(5) . . . . ?
Pt P1 C21 C26 137.6(3) . . . . ?
C31A P1 C21 C22 -159.3(4) . . . . ?
C11 P1 C21 C22 85.9(3) . . . . ?
C31B P1 C21 C22 -162.2(5) . . . . ?
Pt P1 C21 C22 -47.8(4) . . . . ?
C26 C21 C22 C23 2.3(7) . . . . ?
P1 C21 C22 C23 -172.4(4) . . . . ?
C21 C22 C23 C24 -1.1(8) . . . . ?
C22 C23 C24 C25 -0.1(8) . . . . ?
C23 C24 C25 C26 0.2(8) . . . . ?
C22 C21 C26 C25 -2.3(7) . . . . ?
P1 C21 C26 C25 172.2(4) . . . . ?
C24 C25 C26 C21 1.0(7) . . . . ?
C41B P2 C51 C52 28.1(5) . . . . ?
C61 P2 C51 C52 -87.2(3) . . . . ?
C41A P2 C51 C52 25.7(4) . . . . ?
Pt P2 C51 C52 143.1(3) . . . . ?
C41B P2 C51 C56 -153.5(5) . . . . ?
C61 P2 C51 C56 91.2(3) . . . . ?
C41A P2 C51 C56 -155.9(4) . . . . ?
Pt P2 C51 C56 -38.5(3) . . . . ?
C56 C51 C52 C53 -1.3(6) . . . . ?
P2 C51 C52 C53 177.0(3) . . . . ?
C51 C52 C53 C54 1.2(6) . . . . ?
C52 C53 C54 C55 0.2(7) . . . . ?
C53 C54 C55 C56 -1.3(7) . . . . ?
C54 C55 C56 C51 1.1(6) . . . . ?
C52 C51 C56 C55 0.2(6) . . . . ?
P2 C51 C56 C55 -178.3(3) . . . . ?
C41B P2 C61 C62 -128.3(6) . . . . ?
C51 P2 C61 C62 -14.2(3) . . . . ?
C41A P2 C61 C62 -129.3(4) . . . . ?
Pt P2 C61 C62 113.2(3) . . . . ?
C41B P2 C61 C66 55.5(6) . . . . ?
C51 P2 C61 C66 169.6(3) . . . . ?
C41A P2 C61 C66 54.5(4) . . . . ?
Pt P2 C61 C66 -62.9(3) . . . . ?
C66 C61 C62 C63 -0.6(6) . . . . ?
P2 C61 C62 C63 -176.7(3) . . . . ?
C61 C62 C63 C64 1.2(6) . . . . ?
C62 C63 C64 C65 -1.0(7) . . . . ?
C63 C64 C65 C66 0.0(6) . . . . ?
C64 C65 C66 C61 0.7(6) . . . . ?
C62 C61 C66 C65 -0.4(5) . . . . ?
P2 C61 C66 C65 175.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         1.377
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.091
####################################################################### 
# 
# 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_pp52
_audit_block_doi                 10.5517/cc7548s
_database_code_depnum_ccdc_archive 'CCDC 213474'
_audit_update_record             
;
2003-06-23 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H18 O4 S'
_chemical_formula_weight         318.37

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   5.7898(3)
_cell_length_b                   8.4887(5)
_cell_length_c                   15.9793(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8490(10)
_cell_angle_gamma                90.00
_cell_volume                     784.38(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    3781
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             336
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
The temperature of the crystal was controlled using the Oxford Cryosystem
Cryostream Cooler (Cosier & Glazer, 1986).
The data collection nominally covered over a hemisphere of reciprocal
space, by a combination of three sets of exposures with
different φ angles for the crystal; each 10 s exposure covered 0.3° in ω.
The crystal-to-detector distance was 5.0 cm.  Coverage of the unique set
is over 97% complete to at least 26° in θ.
Crystal decay was found to be negligible by by repeating the initial frames at t
data collection and analyzing the duplicate reflections.

Hydrogen atoms were added at calculated positions and refined using a
riding model.  Anisotropic displacement parameters were used for all non-H atoms
H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met
atoms) times the equivalent isotropic displacement parameter of the atom
to which they are attached.
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens SMART diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        nil
_diffrn_reflns_number            5097
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         29.16
_reflns_number_total             3471
_reflns_number_gt                2738
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Siemens, 1994)'
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0590P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(8)
_refine_ls_number_reflns         3471
_refine_ls_number_parameters     202
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.1003
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_restrained_S_all      0.926
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.46689(11) 0.69443(9) 0.17809(4) 0.0402(2) Uani 1 1 d . . .
O1 O 0.3305(3) 0.82962(19) 0.21955(9) 0.0257(4) Uani 1 1 d . . .
C2 C 0.3776(4) 0.8536(3) 0.31083(13) 0.0208(5) Uani 1 1 d . . .
H2A H 0.5083 0.7837 0.3305 0.025 Uiso 1 1 calc R . .
C3 C 0.1614(4) 0.8071(3) 0.35508(13) 0.0227(5) Uani 1 1 d . . .
H3A H 0.1396 0.6905 0.3509 0.027 Uiso 1 1 calc R . .
O4 O -0.0380(3) 0.8844(2) 0.31791(10) 0.0333(4) Uani 1 1 d . . .
H4A H -0.0794 0.8387 0.2730 0.050 Uiso 1 1 calc R . .
C5 C 0.1851(3) 0.8544(3) 0.44691(13) 0.0193(5) Uani 1 1 d . . .
C6 C 0.0289(4) 0.7928(3) 0.50235(15) 0.0285(5) Uani 1 1 d . . .
H6A H -0.0911 0.7246 0.4818 0.034 Uiso 1 1 calc R . .
C7 C 0.0464(4) 0.8295(3) 0.58641(15) 0.0341(6) Uani 1 1 d . . .
H7A H -0.0637 0.7893 0.6230 0.041 Uiso 1 1 calc R . .
C8 C 0.2232(4) 0.9244(3) 0.61738(14) 0.0314(6) Uani 1 1 d . . .
H8A H 0.2386 0.9475 0.6756 0.038 Uiso 1 1 calc R . .
C9 C 0.3782(4) 0.9858(3) 0.56292(14) 0.0267(5) Uani 1 1 d . . .
H9A H 0.5019 1.0497 0.5846 0.032 Uiso 1 1 calc R . .
C10 C 0.3577(4) 0.9562(3) 0.47681(13) 0.0205(5) Uani 1 1 d . . .
C11 C 0.5207(4) 1.0365(3) 0.41920(14) 0.0255(5) Uani 1 1 d . . .
H11A H 0.6767 0.9896 0.4280 0.031 Uiso 1 1 calc R . .
H11B H 0.5322 1.1494 0.4343 0.031 Uiso 1 1 calc R . .
C12 C 0.4444(4) 1.0223(3) 0.32692(14) 0.0250(5) Uani 1 1 d . . .
H12A H 0.3110 1.0925 0.3137 0.030 Uiso 1 1 calc R . .
H12B H 0.5723 1.0529 0.2914 0.030 Uiso 1 1 calc R . .
O13 O 0.4093(5) 0.5475(3) 0.21729(13) 0.0753(9) Uani 1 1 d . . .
O14 O 0.7035(3) 0.7337(4) 0.17800(13) 0.0850(11) Uani 1 1 d . . .
C15 C 0.3427(4) 0.7030(4) 0.07623(13) 0.0291(5) Uani 1 1 d . . .
C16 C 0.1371(4) 0.6235(3) 0.05905(16) 0.0360(6) Uani 1 1 d . . .
H16A H 0.0639 0.5680 0.1020 0.043 Uiso 1 1 calc R . .
C17 C 0.0399(5) 0.6264(3) -0.02180(17) 0.0370(7) Uani 1 1 d . . .
H17A H -0.1008 0.5715 -0.0341 0.044 Uiso 1 1 calc R . .
C18 C 0.1432(4) 0.7075(3) -0.08510(13) 0.0337(6) Uani 1 1 d . . .
C19 C 0.0319(6) 0.7117(5) -0.17282(16) 0.0590(9) Uani 1 1 d . . .
H19A H 0.1333 0.7678 -0.2101 0.088 Uiso 1 1 calc R . .
H19B H -0.1172 0.7662 -0.1720 0.088 Uiso 1 1 calc R . .
H19C H 0.0075 0.6038 -0.1932 0.088 Uiso 1 1 calc R . .
C20 C 0.3489(5) 0.7860(3) -0.06628(16) 0.0410(7) Uani 1 1 d . . .
H20A H 0.4217 0.8422 -0.1091 0.049 Uiso 1 1 calc R . .
C21 C 0.4505(5) 0.7838(4) 0.01432(16) 0.0384(7) Uani 1 1 d . . .
H21A H 0.5923 0.8373 0.0266 0.046 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O14 1.410(2) . ?
S1 O13 1.442(3) . ?
S1 O1 1.5591(16) . ?
S1 C15 1.748(2) . ?
O1 C2 1.484(2) . ?
C2 C12 1.502(3) . ?
C2 C3 1.520(3) . ?
C3 O4 1.431(3) . ?
C3 C5 1.521(3) . ?
C5 C10 1.388(3) . ?
C5 C6 1.399(3) . ?
C6 C7 1.378(3) . ?
C7 C8 1.375(4) . ?
C8 C9 1.383(4) . ?
C9 C10 1.398(3) . ?
C10 C11 1.513(3) . ?
C11 C12 1.523(3) . ?
C15 C21 1.379(4) . ?
C15 C16 1.384(4) . ?
C16 C17 1.384(3) . ?
C17 C18 1.384(4) . ?
C18 C20 1.385(4) . ?
C18 C19 1.514(3) . ?
C20 C21 1.389(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O14 S1 O13 116.79(18) . . ?
O14 S1 O1 109.80(14) . . ?
O13 S1 O1 108.61(12) . . ?
O14 S1 C15 110.11(12) . . ?
O13 S1 C15 110.30(14) . . ?
O1 S1 C15 99.89(11) . . ?
C2 O1 S1 116.50(13) . . ?
O1 C2 C12 109.39(17) . . ?
O1 C2 C3 107.83(16) . . ?
C12 C2 C3 112.26(19) . . ?
O4 C3 C2 110.74(18) . . ?
O4 C3 C5 108.18(17) . . ?
C2 C3 C5 110.07(17) . . ?
C10 C5 C6 119.5(2) . . ?
C10 C5 C3 121.70(19) . . ?
C6 C5 C3 118.81(19) . . ?
C7 C6 C5 120.9(2) . . ?
C8 C7 C6 120.1(2) . . ?
C7 C8 C9 119.3(2) . . ?
C8 C9 C10 121.7(2) . . ?
C5 C10 C9 118.4(2) . . ?
C5 C10 C11 122.09(19) . . ?
C9 C10 C11 119.54(19) . . ?
C10 C11 C12 113.20(18) . . ?
C2 C12 C11 107.50(19) . . ?
C21 C15 C16 121.1(2) . . ?
C21 C15 S1 120.6(2) . . ?
C16 C15 S1 118.32(19) . . ?
C17 C16 C15 118.9(2) . . ?
C16 C17 C18 121.4(2) . . ?
C17 C18 C20 118.6(2) . . ?
C17 C18 C19 120.6(3) . . ?
C20 C18 C19 120.8(3) . . ?
C18 C20 C21 121.0(2) . . ?
C15 C21 C20 119.1(2) . . ?

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        29.16
_diffrn_measured_fraction_theta_full 0.914
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_sk15arev
_audit_block_doi                 10.5517/cc7546q
_database_code_depnum_ccdc_archive 'CCDC 213472'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.poly.2004.01.015 2004
_audit_update_record             
;
2003-06-23 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H40 B2 F8 N4 P2 Pt'
_chemical_formula_weight         1151.53

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

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

_cell_length_a                   11.289(2)
_cell_length_b                   16.021(3)
_cell_length_c                   13.684(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.97(3)
_cell_angle_gamma                90.00
_cell_volume                     2354.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    3.122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3995
_exptl_absorpt_correction_T_max  0.7252
_exptl_absorpt_process_details   'Blessing, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'Area detector ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19782
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         25.56
_reflns_number_total             4368
_reflns_number_gt                3544
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0607P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4368
_refine_ls_number_parameters     388
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1119
_refine_ls_wR_factor_gt          0.1047
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt Pt 0.81183(3) 0.7500 0.71515(3) 0.02844(14) Uani 1 2 d S . .
P1 P 0.80468(16) 0.60620(10) 0.71736(12) 0.0323(4) Uani 1 1 d D . .
C11 C 0.9573(6) 0.5571(3) 0.7545(5) 0.0377(15) Uani 1 1 d D . .
C12 C 1.0186(7) 0.5453(4) 0.6816(6) 0.055(2) Uani 1 1 d D . .
H12A H 0.9795 0.5606 0.6120 0.065 Uiso 1 1 calc R . .
C13 C 1.1363(8) 0.5114(5) 0.7109(8) 0.074(3) Uani 1 1 d D . .
H13A H 1.1793 0.5050 0.6617 0.088 Uiso 1 1 calc R . .
C14 C 1.1925(8) 0.4867(5) 0.8108(8) 0.071(3) Uani 1 1 d D . .
H14A H 1.2731 0.4624 0.8300 0.086 Uiso 1 1 calc R . .
C15 C 1.1329(8) 0.4972(5) 0.8816(7) 0.062(2) Uani 1 1 d D . .
H15A H 1.1726 0.4803 0.9505 0.075 Uiso 1 1 calc R . .
C16 C 1.0141(6) 0.5323(4) 0.8556(5) 0.0464(18) Uani 1 1 d D . .
H16A H 0.9728 0.5391 0.9060 0.056 Uiso 1 1 calc R . .
C21 C 0.7133(5) 0.5562(4) 0.7909(3) 0.0355(15) Uani 1 1 d D . .
C22 C 0.7244(7) 0.4705(4) 0.8117(5) 0.0413(16) Uani 1 1 d D . .
H22A H 0.7847 0.4385 0.7927 0.050 Uiso 1 1 calc R . .
C23 C 0.6474(7) 0.4324(5) 0.8600(5) 0.0457(17) Uani 1 1 d D . .
H23A H 0.6530 0.3739 0.8720 0.055 Uiso 1 1 calc R . .
C24 C 0.5626(7) 0.4793(5) 0.8908(5) 0.0475(18) Uani 1 1 d D . .
H24A H 0.5085 0.4528 0.9223 0.057 Uiso 1 1 calc R . .
C25 C 0.5564(7) 0.5638(5) 0.8760(5) 0.0492(18) Uani 1 1 d D . .
H25A H 0.4997 0.5957 0.8995 0.059 Uiso 1 1 calc R . .
C26 C 0.6318(7) 0.6040(4) 0.8269(5) 0.0445(17) Uani 1 1 d D . .
H26A H 0.6279 0.6628 0.8180 0.053 Uiso 1 1 calc R . .
C31 C 0.7247(10) 0.5757(11) 0.5930(11) 0.0329(19) Uani 0.50 1 d PD . -1
C32 C 0.7087(15) 0.4943(12) 0.5540(12) 0.048(2) Uani 0.50 1 d PD . -1
H32A H 0.7465 0.4489 0.5971 0.058 Uiso 0.50 1 calc PR . -1
C33 C 0.6377(16) 0.4791(10) 0.4522(11) 0.039(3) Uani 0.50 1 d PD . -1
H33A H 0.6236 0.4236 0.4268 0.047 Uiso 0.50 1 calc PR . -1
C34 C 0.5880(16) 0.5462(9) 0.3887(10) 0.054(4) Uani 0.50 1 d PD . -1
H34A H 0.5400 0.5365 0.3193 0.065 Uiso 0.50 1 calc PR . -1
C35 C 0.6076(14) 0.6277(8) 0.4256(10) 0.051(3) Uani 0.50 1 d PD . -1
H35A H 0.5769 0.6731 0.3802 0.061 Uiso 0.50 1 calc PR . -1
C36 C 0.6720(15) 0.6431(9) 0.5287(11) 0.035(2) Uani 0.50 1 d PD . -1
N N 0.6929(9) 0.7289(5) 0.5710(7) 0.023(3) Uani 0.50 1 d PD . -1
C1 C 0.6288(14) 0.7873(8) 0.5123(11) 0.041(3) Uani 0.50 1 d PD . -1
H1A H 0.5584 0.7660 0.4605 0.049 Uiso 0.50 1 calc PR . -1
C41 C 0.7160(12) 0.9276(11) 0.5810(12) 0.0329(19) Uani 0.50 1 d PD . -1
C42 C 0.7220(15) 1.0121(12) 0.5648(11) 0.048(2) Uani 0.50 1 d PD . -1
H42A H 0.7703 1.0470 0.6185 0.058 Uiso 0.50 1 calc PR . -1
C43 C 0.6577(16) 1.0462(9) 0.4702(11) 0.039(3) Uani 0.50 1 d PD . -1
H43A H 0.6686 1.1032 0.4557 0.047 Uiso 0.50 1 calc PR . -1
C44 C 0.5785(14) 0.9963(8) 0.3982(10) 0.054(4) Uani 0.50 1 d PD . -1
H44A H 0.5307 1.0194 0.3342 0.065 Uiso 0.50 1 calc PR . -1
C45 C 0.5673(14) 0.9135(8) 0.4171(10) 0.051(3) Uani 0.50 1 d PD . -1
H45A H 0.5088 0.8804 0.3674 0.061 Uiso 0.50 1 calc PR . -1
C46 C 0.6393(14) 0.8768(9) 0.5072(11) 0.035(2) Uani 0.50 1 d PD . -1
N1 N 0.9282(7) 0.7500 0.8645(5) 0.0280(16) Uani 1 2 d S . .
C101 C 0.8759(10) 0.7500 0.9407(7) 0.044(2) Uani 1 2 d S . .
H10A H 0.7876 0.7500 0.9233 0.052 Uiso 1 2 calc SR . .
C102 C 0.9467(13) 0.7500 1.0440(8) 0.064(3) Uani 1 2 d S . .
H10B H 0.9074 0.7500 1.0962 0.077 Uiso 1 2 calc SR . .
C103 C 1.0723(12) 0.7500 1.0687(9) 0.070(4) Uani 1 2 d S . .
H10C H 1.1217 0.7500 1.1389 0.084 Uiso 1 2 calc SR . .
C104 C 1.1293(11) 0.7500 0.9926(8) 0.054(3) Uani 1 2 d S . .
H10D H 1.2176 0.7500 1.0103 0.064 Uiso 1 2 calc SR . .
C105 C 1.0562(9) 0.7500 0.8893(7) 0.037(2) Uani 1 2 d S . .
N2 N 1.0416(6) 0.7500 0.7081(5) 0.0292(16) Uani 1 2 d S . .
C106 C 1.1147(9) 0.7500 0.8059(7) 0.037(2) Uani 1 2 d S . .
C107 C 1.2450(10) 0.7500 0.8301(9) 0.059(3) Uani 1 2 d S . .
H10E H 1.2966 0.7500 0.8996 0.071 Uiso 1 2 calc SR . .
C108 C 1.2971(11) 0.7500 0.7503(10) 0.072(4) Uani 1 2 d S . .
H10F H 1.3849 0.7500 0.7643 0.086 Uiso 1 2 calc SR . .
C109 C 1.2187(10) 0.7500 0.6502(9) 0.054(3) Uani 1 2 d S . .
H10G H 1.2521 0.7500 0.5944 0.065 Uiso 1 2 calc SR . .
C110 C 1.0916(8) 0.7500 0.6322(6) 0.032(2) Uani 1 2 d S . .
N3 N 0.9152(12) 0.8012(8) 0.4993(9) 0.052(3) Uani 0.50 1 d P . -1
C111 C 1.0066(9) 0.7500 0.5213(7) 0.039(2) Uani 1 2 d S . .
C112 C 1.0299(16) 0.6930(9) 0.4502(12) 0.052(4) Uani 0.50 1 d P . -1
H11A H 1.0973 0.6547 0.4712 0.062 Uiso 0.50 1 calc PR . -1
C113 C 0.9531(17) 0.6940(12) 0.3506(12) 0.065(5) Uani 0.50 1 d P . -1
H11B H 0.9668 0.6563 0.3015 0.078 Uiso 0.50 1 calc PR . -1
C114 C 0.8564(13) 0.7500 0.3222(10) 0.078(4) Uani 1 2 d S . .
H11C H 0.8010 0.7518 0.2541 0.093 Uiso 1 2 calc SR . .
C115 C 0.8428(17) 0.8053(14) 0.3997(15) 0.086(7) Uani 0.50 1 d P . -1
H11D H 0.7801 0.8470 0.3807 0.103 Uiso 0.50 1 calc PR . -1
B1 B 0.5753(13) 0.7500 0.0571(11) 0.053(3) Uani 1 2 d S . .
F11 F 0.4577(7) 0.7500 0.0585(6) 0.092(2) Uani 1 2 d S . .
F12 F 0.6364(6) 0.6802(3) 0.1008(5) 0.109(2) Uani 1 1 d . . .
F13 F 0.5632(9) 0.7500 -0.0500(6) 0.091(2) Uani 1 2 d S . .
B2 B 0.7192(12) 0.2500 0.6511(9) 0.044(3) Uani 1 2 d S . .
F21 F 0.6309(6) 0.2500 0.7022(5) 0.073(2) Uani 1 2 d S . .
F22 F 0.7937(5) 0.3193(3) 0.6807(4) 0.0736(15) Uani 1 1 d . . .
F23 F 0.6604(7) 0.2500 0.5464(5) 0.087(3) Uani 1 2 d S . .


_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
Pt N 2.044(10) 4_575 ?
Pt N 2.044(10) . ?
Pt N1 2.061(7) . ?
Pt P1 2.3058(16) . ?
Pt P1 2.3058(16) 4_575 ?
Pt N2 2.626(7) . ?
P1 C31 1.733(15) . ?
P1 C11 1.818(7) . ?
P1 C21 1.832(6) . ?
P1 C41 1.904(15) 4_575 ?
C11 C16 1.391(9) . ?
C11 C12 1.392(9) . ?
C12 C13 1.375(11) . ?
C13 C14 1.376(13) . ?
C14 C15 1.350(12) . ?
C15 C16 1.395(11) . ?
C21 C26 1.398(9) . ?
C21 C22 1.401(9) . ?
C22 C23 1.385(9) . ?
C23 C24 1.381(10) . ?
C24 C25 1.368(10) . ?
C25 C26 1.394(10) . ?
C31 C32 1.400(14) . ?
C31 C36 1.403(14) . ?
C32 C33 1.398(14) . ?
C33 C34 1.387(13) . ?
C34 C35 1.392(13) . ?
C35 C36 1.396(13) . ?
C36 N 1.482(15) . ?
N C1 1.297(15) . ?
C1 C46 1.44(2) . ?
C41 C46 1.375(14) . ?
C41 C42 1.376(14) . ?
C41 P1 1.904(15) 4_575 ?
C42 C43 1.387(14) . ?
C43 C44 1.367(13) . ?
C44 C45 1.365(14) . ?
C45 C46 1.381(13) . ?
N1 C101 1.348(11) . ?
N1 C105 1.379(12) . ?
C101 C102 1.393(14) . ?
C102 C103 1.352(17) . ?
C103 C104 1.384(16) . ?
C104 C105 1.399(13) . ?
C105 C106 1.485(13) . ?
N2 C110 1.326(11) . ?
N2 C106 1.338(11) . ?
C106 C107 1.405(14) . ?
C107 C108 1.390(17) . ?
C108 C109 1.382(15) . ?
C109 C110 1.379(14) . ?
C110 C111 1.526(12) . ?
N3 C111 1.279(14) . ?
N3 C115 1.36(2) . ?
C111 N3 1.279(14) 4_575 ?
C111 C112 1.417(16) 4_575 ?
C111 C112 1.417(16) . ?
C112 C113 1.37(2) . ?
C113 C114 1.37(2) . ?
C114 C113 1.37(2) 4_575 ?
C114 C115 1.42(2) . ?
C114 C115 1.42(2) 4_575 ?
B1 F11 1.335(15) . ?
B1 F12 1.353(9) 4_575 ?
B1 F12 1.353(9) . ?
B1 F13 1.429(16) . ?
B2 F22 1.376(9) . ?
B2 F22 1.376(9) 4_565 ?
B2 F23 1.380(13) . ?
B2 F21 1.383(13) . ?

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
N Pt N 19.0(4) 4_575 . ?
N Pt N1 170.3(2) 4_575 . ?
N Pt N1 170.3(2) . . ?
N Pt P1 99.4(2) 4_575 . ?
N Pt P1 80.3(2) . . ?
N1 Pt P1 90.07(4) . . ?
N Pt P1 80.3(2) 4_575 4_575 ?
N Pt P1 99.4(2) . 4_575 ?
N1 Pt P1 90.07(4) . 4_575 ?
P1 Pt P1 175.30(8) . 4_575 ?
N Pt N2 109.1(3) 4_575 . ?
N Pt N2 109.1(3) . . ?
N1 Pt N2 72.6(3) . . ?
P1 Pt N2 92.26(4) . . ?
P1 Pt N2 92.26(4) 4_575 . ?
C31 P1 C11 108.3(5) . . ?
C31 P1 C21 101.8(4) . . ?
C11 P1 C21 107.6(3) . . ?
C31 P1 C41 0.4(7) . 4_575 ?
C11 P1 C41 108.5(5) . 4_575 ?
C21 P1 C41 101.5(4) . 4_575 ?
C31 P1 Pt 106.2(6) . . ?
C11 P1 Pt 113.71(14) . . ?
C21 P1 Pt 118.1(2) . . ?
C41 P1 Pt 106.3(6) 4_575 . ?
C16 C11 C12 119.7(7) . . ?
C16 C11 P1 120.5(5) . . ?
C12 C11 P1 119.8(6) . . ?
C13 C12 C11 119.6(8) . . ?
C12 C13 C14 120.8(9) . . ?
C15 C14 C13 119.9(8) . . ?
C14 C15 C16 121.3(8) . . ?
C11 C16 C15 118.8(7) . . ?
C26 C21 C22 119.5(6) . . ?
C26 C21 P1 119.9(5) . . ?
C22 C21 P1 120.7(5) . . ?
C23 C22 C21 119.9(6) . . ?
C24 C23 C22 120.1(7) . . ?
C25 C24 C23 120.2(7) . . ?
C24 C25 C26 121.1(7) . . ?
C25 C26 C21 119.0(7) . . ?
C32 C31 C36 119.9(9) . . ?
C32 C31 P1 127.2(11) . . ?
C36 C31 P1 113.0(11) . . ?
C33 C32 C31 120.6(9) . . ?
C34 C33 C32 119.1(9) . . ?
C33 C34 C35 120.8(9) . . ?
C34 C35 C36 120.4(9) . . ?
C35 C36 C31 119.1(9) . . ?
C35 C36 N 121.9(12) . . ?
C31 C36 N 118.9(12) . . ?
C1 N C36 115.9(11) . . ?
C1 N Pt 123.6(8) . . ?
C36 N Pt 120.5(8) . . ?
N C1 C46 135.1(12) . . ?
C46 C41 C42 121.0(9) . . ?
C46 C41 P1 125.0(11) . 4_575 ?
C42 C41 P1 113.6(11) . 4_575 ?
C41 C42 C43 120.1(9) . . ?
C44 C43 C42 118.7(9) . . ?
C45 C44 C43 120.7(9) . . ?
C44 C45 C46 121.3(9) . . ?
C41 C46 C45 117.9(9) . . ?
C41 C46 C1 126.5(12) . . ?
C45 C46 C1 115.5(12) . . ?
C101 N1 C105 119.0(7) . . ?
C101 N1 Pt 118.0(6) . . ?
C105 N1 Pt 123.0(5) . . ?
N1 C101 C102 122.2(10) . . ?
C103 C102 C101 118.9(10) . . ?
C102 C103 C104 120.4(10) . . ?
C103 C104 C105 119.6(11) . . ?
N1 C105 C104 119.7(9) . . ?
N1 C105 C106 119.4(7) . . ?
C104 C105 C106 120.8(9) . . ?
C110 N2 C106 120.2(8) . . ?
C110 N2 Pt 133.8(6) . . ?
C106 N2 Pt 106.0(6) . . ?
N2 C106 C107 120.9(9) . . ?
N2 C106 C105 119.0(8) . . ?
C107 C106 C105 120.1(9) . . ?
C108 C107 C106 118.7(10) . . ?
C109 C108 C107 118.8(10) . . ?
C110 C109 C108 119.3(10) . . ?
N2 C110 C109 122.1(8) . . ?
N2 C110 C111 119.4(8) . . ?
C109 C110 C111 118.5(8) . . ?
C111 N3 C115 117.4(13) . . ?
N3 C111 N3 79.8(14) 4_575 . ?
N3 C111 C112 124.0(11) 4_575 4_575 ?
N3 C111 C112 74.4(9) . 4_575 ?
N3 C111 C112 74.4(9) 4_575 . ?
N3 C111 C112 124.0(11) . . ?
C112 C111 C112 80.3(13) 4_575 . ?
N3 C111 C110 116.6(8) 4_575 . ?
N3 C111 C110 116.6(8) . . ?
C112 C111 C110 119.4(9) 4_575 . ?
C112 C111 C110 119.4(9) . . ?
C113 C112 C111 118.7(15) . . ?
C112 C113 C114 119.4(15) . . ?
C113 C114 C113 81.6(16) 4_575 . ?
C113 C114 C115 69.1(11) 4_575 . ?
C113 C114 C115 117.1(14) . . ?
C113 C114 C115 117.1(14) 4_575 4_575 ?
C113 C114 C115 69.1(11) . 4_575 ?
C115 C114 C115 76.9(17) . 4_575 ?
N3 C115 C114 123.1(15) . . ?
F11 B1 F12 111.5(8) . 4_575 ?
F11 B1 F12 111.5(8) . . ?
F12 B1 F12 111.6(11) 4_575 . ?
F11 B1 F13 103.5(11) . . ?
F12 B1 F13 109.1(8) 4_575 . ?
F12 B1 F13 109.1(8) . . ?
F22 B2 F22 107.5(10) . 4_565 ?
F22 B2 F23 111.1(6) . . ?
F22 B2 F23 111.1(6) 4_565 . ?
F22 B2 F21 108.8(6) . . ?
F22 B2 F21 108.8(6) 4_565 . ?
F23 B2 F21 109.6(10) . . ?

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
N Pt P1 C31 9.3(4) 4_575 . . . ?
N Pt P1 C31 8.5(4) . . . . ?
N1 Pt P1 C31 -173.1(3) . . . . ?
P1 Pt P1 C31 95.3(11) 4_575 . . . ?
N2 Pt P1 C31 -100.5(3) . . . . ?
N Pt P1 C11 128.3(4) 4_575 . . . ?
N Pt P1 C11 127.5(4) . . . . ?
N1 Pt P1 C11 -54.1(3) . . . . ?
P1 Pt P1 C11 -145.7(10) 4_575 . . . ?
N2 Pt P1 C11 18.5(3) . . . . ?
N Pt P1 C21 -104.1(3) 4_575 . . . ?
N Pt P1 C21 -104.9(3) . . . . ?
N1 Pt P1 C21 73.5(3) . . . . ?
P1 Pt P1 C21 -18.1(11) 4_575 . . . ?
N2 Pt P1 C21 146.1(2) . . . . ?
N Pt P1 C41 9.0(4) 4_575 . . 4_575 ?
N Pt P1 C41 8.2(4) . . . 4_575 ?
N1 Pt P1 C41 -173.4(4) . . . 4_575 ?
P1 Pt P1 C41 95.0(11) 4_575 . . 4_575 ?
N2 Pt P1 C41 -100.8(4) . . . 4_575 ?
C31 P1 C11 C16 -145.9(7) . . . . ?
C21 P1 C11 C16 -36.5(4) . . . . ?
C41 P1 C11 C16 -145.6(6) 4_575 . . . ?
Pt P1 C11 C16 96.3(4) . . . . ?
C31 P1 C11 C12 35.0(7) . . . . ?
C21 P1 C11 C12 144.4(4) . . . . ?
C41 P1 C11 C12 35.4(6) 4_575 . . . ?
Pt P1 C11 C12 -82.7(4) . . . . ?
C16 C11 C12 C13 -1.9(8) . . . . ?
P1 C11 C12 C13 177.2(6) . . . . ?
C11 C12 C13 C14 2.0(11) . . . . ?
C12 C13 C14 C15 -1.3(13) . . . . ?
C13 C14 C15 C16 0.4(13) . . . . ?
C12 C11 C16 C15 1.1(8) . . . . ?
P1 C11 C16 C15 -178.0(5) . . . . ?
C14 C15 C16 C11 -0.3(11) . . . . ?
C31 P1 C21 C26 -103.5(7) . . . . ?
C11 P1 C21 C26 142.7(4) . . . . ?
C41 P1 C21 C26 -103.5(7) 4_575 . . . ?
Pt P1 C21 C26 12.3(4) . . . . ?
C31 P1 C21 C22 76.6(7) . . . . ?
C11 P1 C21 C22 -37.2(4) . . . . ?
C41 P1 C21 C22 76.7(7) 4_575 . . . ?
Pt P1 C21 C22 -167.6(3) . . . . ?
C26 C21 C22 C23 5.4(7) . . . . ?
P1 C21 C22 C23 -174.7(5) . . . . ?
C21 C22 C23 C24 -2.2(9) . . . . ?
C22 C23 C24 C25 -1.6(10) . . . . ?
C23 C24 C25 C26 2.1(10) . . . . ?
C24 C25 C26 C21 1.1(10) . . . . ?
C22 C21 C26 C25 -4.9(8) . . . . ?
P1 C21 C26 C25 175.3(5) . . . . ?
C11 P1 C31 C32 50.0(5) . . . . ?
C21 P1 C31 C32 -63.3(6) . . . . ?
C41 P1 C31 C32 -72(100) 4_575 . . . ?
Pt P1 C31 C32 172.4(5) . . . . ?
C11 P1 C31 C36 -130.5(8) . . . . ?
C21 P1 C31 C36 116.2(8) . . . . ?
C41 P1 C31 C36 107(100) 4_575 . . . ?
Pt P1 C31 C36 -8.0(8) . . . . ?
C36 C31 C32 C33 -1.8(12) . . . . ?
P1 C31 C32 C33 177.7(10) . . . . ?
C31 C32 C33 C34 3.0(18) . . . . ?
C32 C33 C34 C35 0(2) . . . . ?
C33 C34 C35 C36 -4(2) . . . . ?
C34 C35 C36 C31 5(2) . . . . ?
C34 C35 C36 N -179.0(13) . . . . ?
C32 C31 C36 C35 -2.1(16) . . . . ?
P1 C31 C36 C35 178.3(11) . . . . ?
C32 C31 C36 N -178.4(9) . . . . ?
P1 C31 C36 N 2.0(14) . . . . ?
C35 C36 N C1 12.4(19) . . . . ?
C31 C36 N C1 -171.3(12) . . . . ?
C35 C36 N Pt -169.6(11) . . . . ?
C31 C36 N Pt 6.6(15) . . . . ?
N Pt N C1 -8.8(11) 4_575 . . . ?
N1 Pt N C1 159.4(16) . . . . ?
P1 Pt N C1 168.8(11) . . . . ?
P1 Pt N C1 -6.4(11) 4_575 . . . ?
N2 Pt N C1 -102.1(10) . . . . ?
N Pt N C36 173.4(8) 4_575 . . . ?
N1 Pt N C36 -18(2) . . . . ?
P1 Pt N C36 -9.0(8) . . . . ?
P1 Pt N C36 175.8(8) 4_575 . . . ?
N2 Pt N C36 80.1(9) . . . . ?
C36 N C1 C46 -160.9(13) . . . . ?
Pt N C1 C46 21(2) . . . . ?
C46 C41 C42 C43 -5.0(11) . . . . ?
P1 C41 C42 C43 -177.5(11) 4_575 . . . ?
C41 C42 C43 C44 7.0(17) . . . . ?
C42 C43 C44 C45 -3(2) . . . . ?
C43 C44 C45 C46 -3(2) . . . . ?
C42 C41 C46 C45 -1.0(16) . . . . ?
P1 C41 C46 C45 170.6(11) 4_575 . . . ?
C42 C41 C46 C1 176.7(9) . . . . ?
P1 C41 C46 C1 -11.7(19) 4_575 . . . ?
C44 C45 C46 C41 5(2) . . . . ?
C44 C45 C46 C1 -173.0(13) . . . . ?
N C1 C46 C41 -13(3) . . . . ?
N C1 C46 C45 165.0(15) . . . . ?
N Pt N1 C101 78.3(19) 4_575 . . . ?
N Pt N1 C101 -78.3(19) . . . . ?
P1 Pt N1 C101 -87.65(4) . . . . ?
P1 Pt N1 C101 87.65(4) 4_575 . . . ?
N2 Pt N1 C101 180.000(4) . . . . ?
N Pt N1 C105 -101.7(19) 4_575 . . . ?
N Pt N1 C105 101.7(19) . . . . ?
P1 Pt N1 C105 92.35(4) . . . . ?
P1 Pt N1 C105 -92.35(4) 4_575 . . . ?
N2 Pt N1 C105 0.000(3) . . . . ?
C105 N1 C101 C102 0.000(6) . . . . ?
Pt N1 C101 C102 180.000(5) . . . . ?
N1 C101 C102 C103 0.000(7) . . . . ?
C101 C102 C103 C104 0.000(8) . . . . ?
C102 C103 C104 C105 0.000(7) . . . . ?
C101 N1 C105 C104 0.000(5) . . . . ?
Pt N1 C105 C104 180.000(4) . . . . ?
C101 N1 C105 C106 180.000(4) . . . . ?
Pt N1 C105 C106 0.000(4) . . . . ?
C103 C104 C105 N1 0.000(5) . . . . ?
C103 C104 C105 C106 180.000(5) . . . . ?
N Pt N2 C110 -10.1(2) 4_575 . . . ?
N Pt N2 C110 10.1(2) . . . . ?
N1 Pt N2 C110 180.000(4) . . . . ?
P1 Pt N2 C110 90.64(4) . . . . ?
P1 Pt N2 C110 -90.64(4) 4_575 . . . ?
N Pt N2 C106 169.9(2) 4_575 . . . ?
N Pt N2 C106 -169.9(2) . . . . ?
N1 Pt N2 C106 0.000(3) . . . . ?
P1 Pt N2 C106 -89.36(4) . . . . ?
P1 Pt N2 C106 89.36(4) 4_575 . . . ?
C110 N2 C106 C107 0.000(4) . . . . ?
Pt N2 C106 C107 180.000(3) . . . . ?
C110 N2 C106 C105 180.000(4) . . . . ?
Pt N2 C106 C105 0.000(3) . . . . ?
N1 C105 C106 N2 0.000(4) . . . . ?
C104 C105 C106 N2 180.000(4) . . . . ?
N1 C105 C106 C107 180.000(4) . . . . ?
C104 C105 C106 C107 0.000(6) . . . . ?
N2 C106 C107 C108 0.000(6) . . . . ?
C105 C106 C107 C108 180.000(5) . . . . ?
C106 C107 C108 C109 0.000(6) . . . . ?
C107 C108 C109 C110 0.000(5) . . . . ?
C106 N2 C110 C109 0.000(4) . . . . ?
Pt N2 C110 C109 180.000(3) . . . . ?
C106 N2 C110 C111 180.000(3) . . . . ?
Pt N2 C110 C111 0.000(4) . . . . ?
C108 C109 C110 N2 0.000(4) . . . . ?
C108 C109 C110 C111 180.000(4) . . . . ?
C115 N3 C111 N3 -68.8(15) . . . 4_575 ?
C115 N3 C111 C112 61.0(15) . . . 4_575 ?
C115 N3 C111 C112 -6(2) . . . . ?
C115 N3 C111 C110 176.4(12) . . . . ?
N2 C110 C111 N3 -45.8(8) . . . 4_575 ?
C109 C110 C111 N3 134.2(8) . . . 4_575 ?
N2 C110 C111 N3 45.8(8) . . . . ?
C109 C110 C111 N3 -134.2(8) . . . . ?
N2 C110 C111 C112 132.2(9) . . . 4_575 ?
C109 C110 C111 C112 -47.8(9) . . . 4_575 ?
N2 C110 C111 C112 -132.2(9) . . . . ?
C109 C110 C111 C112 47.8(9) . . . . ?
N3 C111 C112 C113 68.2(15) 4_575 . . . ?
N3 C111 C112 C113 2(2) . . . . ?
C112 C111 C112 C113 -61.2(17) 4_575 . . . ?
C110 C111 C112 C113 -179.6(11) . . . . ?
C111 C112 C113 C114 0(2) . . . . ?
C112 C113 C114 C113 62.1(18) . . . 4_575 ?
C112 C113 C114 C115 1(2) . . . . ?
C112 C113 C114 C115 -61.2(16) . . . 4_575 ?
C111 N3 C115 C114 7(2) . . . . ?
C113 C114 C115 N3 -72.4(18) 4_575 . . . ?
C113 C114 C115 N3 -4(2) . . . . ?
C115 C114 C115 N3 54(2) 4_575 . . . ?

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
C1 H1A F23 0.95 2.46 3.169(17) 131.8 3_666
C107 H10E F11 0.95 2.37 3.303(14) 168.7 1_656
C109 H10G F23 0.95 2.42 3.371(13) 179.3 3_766
C22 H22A F22 0.95 2.47 3.250(8) 139.2 .
C32 H32A F22 0.95 2.35 3.280(18) 165.6 .
C42 H42A F22 0.95 2.29 3.111(18) 144.2 4_575

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        25.56
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         2.307
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.161


####################################################################### 
# 
# 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_pyran
_audit_block_doi                 10.5517/cc754m4
_database_code_depnum_ccdc_archive 'CCDC 213485'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/jo034492k 2003
_audit_update_record             
;
2003-06-23 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(4aR,6S,7S,8R,8aS)-7,8-diacetyloxy-6-methylhexahydro-4aH-[1,4]dithiino
[2,3b]pyran.
;
_chemical_name_common            ?
_chemical_melting_point          110-112
_chemical_formula_moiety         'C12 H18 O5 S2'
_chemical_formula_sum            'C12 H18 O5 S2'
_chemical_formula_weight         306.38

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   9.1347(3)
_cell_length_b                   9.4741(3)
_cell_length_c                   18.1026(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1566.65(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    100
_cell_measurement_theta_min      7
_cell_measurement_theta_max      15

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            10469
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3086
_reflns_number_gt                2659
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XPMA (Zsolnai, 1997)'
_computing_publication_material  'CIFTAB (Sheldrick, 1992-7)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0694P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.076(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(8)
_refine_ls_number_reflns         2659
_refine_ls_number_parameters     193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1004
_refine_ls_wR_factor_gt          0.0964
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S2 S 0.36400(7) 0.32799(7) 0.20112(3) 0.0656(2) Uani 1 1 d . . .
S1 S 0.14744(8) 0.62437(7) 0.17122(4) 0.0687(2) Uani 1 1 d . . .
O3 O 0.2271(2) 0.09767(18) 0.10196(8) 0.0633(4) Uani 1 1 d . . .
O1 O -0.03793(19) 0.44004(19) 0.12798(9) 0.0630(4) Uani 1 1 d . . .
C4 C -0.0153(3) 0.1924(3) 0.10263(12) 0.0589(6) Uani 1 1 d . . .
C1 C 0.0876(3) 0.4417(3) 0.17420(13) 0.0560(5) Uani 1 1 d . . .
C2 C 0.1992(2) 0.3363(2) 0.14442(12) 0.0526(5) Uani 1 1 d . . .
O4 O -0.0857(2) 0.0586(2) 0.11591(8) 0.0682(5) Uani 1 1 d . . .
C8 C 0.4241(3) 0.5091(3) 0.19239(14) 0.0662(6) Uani 1 1 d . . .
H8A H 0.5169 0.5206 0.2177 0.079 Uiso 1 1 calc R . .
H8B H 0.4391 0.5310 0.1406 0.079 Uiso 1 1 calc R . .
O9 O 0.2671(3) -0.0406(2) 0.20023(12) 0.0917(7) Uani 1 1 d . . .
C5 C -0.1143(3) 0.3093(3) 0.13279(13) 0.0610(6) Uani 1 1 d . . .
C3 C 0.1309(3) 0.1910(2) 0.14247(11) 0.0542(5) Uani 1 1 d . . .
C7 C 0.3127(3) 0.6116(3) 0.22475(14) 0.0670(6) Uani 1 1 d . . .
H7A H 0.3571 0.7044 0.2282 0.080 Uiso 1 1 calc R . .
H7B H 0.2880 0.5814 0.2744 0.080 Uiso 1 1 calc R . .
C9 C 0.2908(3) -0.0098(3) 0.13748(16) 0.0680(7) Uani 1 1 d . . .
C11 C -0.1016(4) -0.0325(4) 0.05942(16) 0.0825(9) Uani 1 1 d . . .
C6 C -0.2560(3) 0.3243(4) 0.08985(17) 0.0858(8) Uani 1 1 d . . .
H6A H -0.3143 0.3978 0.1114 0.129 Uiso 1 1 calc R . .
H6B H -0.3090 0.2368 0.0915 0.129 Uiso 1 1 calc R . .
H6C H -0.2344 0.3477 0.0394 0.129 Uiso 1 1 calc R . .
O11 O -0.0625(5) -0.0065(4) -0.00103(13) 0.1503(14) Uani 1 1 d . . .
C12 C -0.1745(4) -0.1661(4) 0.0851(2) 0.0979(10) Uani 1 1 d . . .
H12A H -0.1938 -0.1599 0.1371 0.147 Uiso 1 1 calc R . .
H12B H -0.1113 -0.2450 0.0756 0.147 Uiso 1 1 calc R . .
H12C H -0.2650 -0.1786 0.0589 0.147 Uiso 1 1 calc R . .
C10 C 0.3970(5) -0.0827(4) 0.0884(2) 0.1080(12) Uani 1 1 d . . .
H10A H 0.3967 -0.0385 0.0407 0.162 Uiso 1 1 calc R . .
H10B H 0.3696 -0.1801 0.0834 0.162 Uiso 1 1 calc R . .
H10C H 0.4933 -0.0766 0.1095 0.162 Uiso 1 1 calc R . .
H5A H -0.129(2) 0.294(2) 0.1884(13) 0.049(5) Uiso 1 1 d . . .
H1A H 0.061(2) 0.417(2) 0.2267(11) 0.038(5) Uiso 1 1 d . . .
H2A H 0.226(3) 0.364(3) 0.0918(14) 0.066(7) Uiso 1 1 d . . .
H4A H -0.001(3) 0.212(3) 0.0471(14) 0.055(6) Uiso 1 1 d . . .
H3A H 0.114(3) 0.155(3) 0.1891(16) 0.069(7) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S2 C8 1.808(3) . ?
S2 C2 1.824(2) . ?
S1 C7 1.798(3) . ?
S1 C1 1.816(3) . ?
O3 C9 1.338(3) . ?
O3 C3 1.446(3) . ?
O1 C1 1.420(3) . ?
O1 C5 1.424(3) . ?
C4 O4 1.442(3) . ?
C4 C3 1.518(3) . ?
C4 C5 1.530(4) . ?
C1 C2 1.525(3) . ?
C2 C3 1.512(3) . ?
O4 C11 1.345(3) . ?
C8 C7 1.523(4) . ?
O9 C9 1.192(3) . ?
C5 C6 1.517(4) . ?
C9 C10 1.485(4) . ?
C11 O11 1.177(4) . ?
C11 C12 1.504(5) . ?

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
C8 S2 C2 99.21(11) . . ?
C7 S1 C1 99.93(11) . . ?
C9 O3 C3 119.09(18) . . ?
C1 O1 C5 111.67(17) . . ?
O4 C4 C3 107.79(18) . . ?
O4 C4 C5 108.26(19) . . ?
C3 C4 C5 110.89(19) . . ?
O1 C1 C2 108.92(18) . . ?
O1 C1 S1 103.66(15) . . ?
C2 C1 S1 114.34(17) . . ?
C3 C2 C1 109.17(19) . . ?
C3 C2 S2 108.32(15) . . ?
C1 C2 S2 112.41(16) . . ?
C11 O4 C4 119.0(2) . . ?
C7 C8 S2 111.64(19) . . ?
O1 C5 C6 107.8(2) . . ?
O1 C5 C4 108.55(19) . . ?
C6 C5 C4 112.9(2) . . ?
O3 C3 C2 108.52(18) . . ?
O3 C3 C4 107.40(17) . . ?
C2 C3 C4 111.49(18) . . ?
C8 C7 S1 113.34(17) . . ?
O9 C9 O3 124.4(3) . . ?
O9 C9 C10 125.1(3) . . ?
O3 C9 C10 110.5(3) . . ?
O11 C11 O4 122.7(3) . . ?
O11 C11 C12 126.7(3) . . ?
O4 C11 C12 110.6(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.080
####################################################################### 
# 
# 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__s64j
_audit_block_doi                 10.5517/cc7549t
_database_code_depnum_ccdc_archive 'CCDC 213475'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.poly.2003.11.034 2004
_audit_update_record             
;
2003-06-23 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;

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

_computing_data_collection       'Bruker SMART-1000 Diffractometer Control'
_computing_cell_refinement       'Bruker SAINT-1000 Diffractometer Control'
_computing_data_reduction        'Bruker SAINT-1000 Diffractometer Control'
_computing_structure_solution    ?
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
#------------------------------------------------------------------------------
_cell_length_a                   10.784(2)
_cell_length_b                   11.371(2)
_cell_length_c                   29.455(4)
_cell_angle_alpha                97.326(3)
_cell_angle_beta                 97.564(2)
_cell_angle_gamma                96.209(3)
_cell_volume                     3522.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    153.2
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0.0
_cell_measurement_theta_max      0.0
#------------------------------------------------------------------------------
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1       '
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_meas      'not measured'
_chemical_formula_weight         1498.56
_chemical_formula_analytical     ?
_chemical_formula_sum            'C74.50 H69 Br2 Cl N8 O2 S2 Zn2 '
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_compound_source        ?
_exptl_crystal_F_000             1534.00
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.9317
_exptl_absorpt_correction_T_max  0.7465
_exptl_special_details           ?



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

# EXPERIMENTAL DATA

_diffrn_special_details          
;
?
;
_diffrn_ambient_temperature      153.2
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       'scintillation counter'
_diffrn_measurement_device       'Bruker SMART-1000 CCD'
_diffrn_measurement_method       ω-2θ


_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0.00
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?

_diffrn_reflns_number            32478
_reflns_number_total             16280
_reflns_number_gt                8660
_reflns_threshold_expression     I>3.00σ(I)
_diffrn_reflns_av_R_equivalents  0.04372
_diffrn_reflns_av_sigmaI/netI    0.096
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
#------------------------------------------------------------------------------
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 149 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
H 0 138 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N 0 16 0.004 0.003
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 4 0.008 0.006
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
S 0 4 0.110 0.124
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Zn 0 4 0.222 1.431
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Br 0 4 -0.374 2.456
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl 0 2 0.132 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;

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

# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_refinement_flags
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Br(1) 0.48921(5) 0.42801(5) 0.18947(2) 0.0336(2) 1.000 . Uani d ?
Br(2) 0.02275(5) 0.71704(5) 0.29518(2) 0.0346(2) 1.000 . Uani d ?
Zn(1) 0.41564(5) 0.49180(5) 0.25979(2) 0.0218(2) 1.000 . Uani d ?
Zn(2) 0.15727(5) 0.59548(5) 0.25994(2) 0.0235(2) 1.000 . Uani d ?
Cl(1) 1.0941(11) 0.2381(11) -0.0260(4) 0.018(3) 0.125 S Uiso d ?
Cl(2) 1.0744(11) 0.2120(10) -0.0323(4) 0.103(5) 0.250 S Uiso d ?
Cl(3) 0.8834(8) 0.0431(7) -0.0447(3) 0.086(2) 0.250 S Uiso d ?
Cl(4) 0.973(3) 0.062(2) -0.0616(9) 0.134(8) 0.125 S Uiso d ?
Cl(5) 0.986(2) 0.133(2) -0.0662(6) 0.079(5) 0.125 S Uiso d ?
Cl(6) 0.971(2) -0.037(2) -0.0118(6) 0.085(5) 0.125 S Uiso d ?
S(1) 0.37128(10) 0.68967(10) 0.26886(4) 0.0209(3) 1.000 . Uani d ?
S(2) 0.21874(10) 0.41034(10) 0.27822(4) 0.0225(3) 1.000 . Uani d ?
O(1) 0.6313(3) 0.8064(3) 0.31903(9) 0.0241(9) 1.000 . Uani d ?
O(2) -0.0406(3) 0.4125(3) 0.24069(11) 0.0353(10) 1.000 . Uani d ?
N(1) 0.6566(3) 0.9023(3) 0.41181(12) 0.0237(11) 1.000 . Uani d ?
N(2) 0.5864(3) 0.7261(3) 0.42973(12) 0.0231(11) 1.000 . Uani d ?
N(3) 0.7260(3) 0.5898(3) 0.36330(12) 0.0218(10) 1.000 . Uani d ?
N(4) 0.5563(3) 0.5037(3) 0.31542(11) 0.0196(10) 1.000 . Uani d ?
N(5) -0.1744(3) 0.2691(3) 0.14326(12) 0.0235(11) 1.000 . Uani d ?
N(6) -0.0936(3) 0.1301(3) 0.17971(12) 0.0258(11) 1.000 . Uani d ?
N(7) 0.1067(4) 0.3885(3) 0.13373(12) 0.0275(11) 1.000 . Uani d ?
N(8) 0.1112(3) 0.5354(3) 0.19047(12) 0.0219(11) 1.000 . Uani d ?
C(1) 0.4181(4) 0.7283(4) 0.3327(1) 0.0209(12) 1.000 . Uani d ?
C(2) 0.3457(4) 0.6450(4) 0.3593(1) 0.0221(12) 1.000 . Uani d ?
C(3) 0.3829(4) 0.8548(4) 0.3444(1) 0.028(1) 1.000 . Uani d ?
C(4) 0.5661(4) 0.7296(4) 0.3449(1) 0.0196(12) 1.000 . Uani d ?
C(5) 0.6780(4) 0.7581(4) 0.2786(2) 0.029(1) 1.000 . Uani d ?
C(6) 0.6022(4) 0.7869(4) 0.3962(2) 0.0206(12) 1.000 . Uani d ?
C(7) 0.6954(5) 0.9995(4) 0.3868(2) 0.041(2) 1.000 . Uani d ?
C(8) 0.6762(4) 0.9117(4) 0.4601(2) 0.0253(13) 1.000 . Uani d ?
C(9) 0.6330(4) 0.8021(4) 0.4704(2) 0.0229(13) 1.000 . Uani d ?
C(10) 0.7362(4) 1.0232(4) 0.4906(2) 0.0270(13) 1.000 . Uani d ?
C(11) 0.6761(5) 1.1260(4) 0.4929(2) 0.035(2) 1.000 . Uani d ?
C(12) 0.7314(5) 1.2270(4) 0.5243(2) 0.040(2) 1.000 . Uani d ?
C(13) 0.8411(5) 1.2243(5) 0.5529(2) 0.046(2) 1.000 . Uani d ?
C(14) 0.8998(5) 1.1246(6) 0.5504(2) 0.050(2) 1.000 . Uani d ?
C(15) 0.8488(5) 1.0231(5) 0.5194(2) 0.037(2) 1.000 . Uani d ?
C(16) 0.6268(4) 0.7591(4) 0.5150(2) 0.0244(13) 1.000 . Uani d ?
C(17) 0.6309(4) 0.8363(4) 0.5564(2) 0.033(2) 1.000 . Uani d ?
C(18) 0.6197(5) 0.7905(5) 0.5974(2) 0.038(2) 1.000 . Uani d ?
C(19) 0.6040(5) 0.6707(5) 0.5983(2) 0.038(2) 1.000 . Uani d ?
C(20) 0.5999(5) 0.5929(4) 0.5579(2) 0.034(2) 1.000 . Uani d ?
C(21) 0.6126(4) 0.6372(4) 0.5171(2) 0.030(1) 1.000 . Uani d ?
C(22) 0.8241(4) 0.6787(4) 0.3912(2) 0.030(1) 1.000 . Uani d ?
C(23) 0.7411(4) 0.4703(4) 0.3535(2) 0.0234(13) 1.000 . Uani d ?
C(24) 0.6356(4) 0.4181(4) 0.3234(1) 0.0210(12) 1.000 . Uani d ?
C(25) 0.9694(4) 0.4373(5) 0.3652(2) 0.033(2) 1.000 . Uani d ?
C(26) 1.0671(5) 0.3901(5) 0.3880(2) 0.039(2) 1.000 . Uani d ?
C(27) 1.0467(5) 0.3221(5) 0.4221(2) 0.049(2) 1.000 . Uani d ?
C(28) 0.9271(5) 0.3003(5) 0.4339(2) 0.051(2) 1.000 . Uani d ?
C(29) 0.8276(4) 0.3506(5) 0.4117(2) 0.039(2) 1.000 . Uani d ?
C(30) 0.8484(4) 0.4191(4) 0.3772(2) 0.027(1) 1.000 . Uani d ?
C(31) 0.6096(4) 0.2911(4) 0.3015(2) 0.0246(13) 1.000 . Uani d ?
C(32) 0.7076(5) 0.2305(5) 0.2879(2) 0.039(2) 1.000 . Uani d ?
C(33) 0.6861(5) 0.1118(5) 0.2681(2) 0.045(2) 1.000 . Uani d ?
C(34) 0.5680(5) 0.0512(4) 0.2612(2) 0.041(2) 1.000 . Uani d ?
C(35) 0.4691(4) 0.1090(4) 0.2739(2) 0.033(2) 1.000 . Uani d ?
C(36) 0.4896(4) 0.2287(4) 0.2934(2) 0.028(1) 1.000 . Uani d ?
C(37) 0.6135(4) 0.6070(4) 0.3410(1) 0.0197(12) 1.000 . Uani d ?
C(38) 0.1199(4) 0.2857(4) 0.2378(1) 0.0209(12) 1.000 . Uani d ?
C(39) 0.0660(4) 0.2042(4) 0.2699(2) 0.031(1) 1.000 . Uani d ?
C(40) 0.2030(4) 0.2220(4) 0.2076(2) 0.029(1) 1.000 . Uani d ?
C(41) 0.0147(4) 0.3402(4) 0.2072(2) 0.0222(13) 1.000 . Uani d ?
C(42) -0.1568(5) 0.4511(5) 0.2330(2) 0.046(2) 1.000 . Uani d ?
C(43) -0.0846(4) 0.2441(4) 0.1772(2) 0.0233(13) 1.000 . Uani d ?
C(44) -0.2020(5) 0.3804(4) 0.1271(2) 0.034(2) 1.000 . Uani d ?
C(45) -0.2449(4) 0.1590(4) 0.1243(2) 0.0251(13) 1.000 . Uani d ?
C(46) -0.3594(4) 0.1547(4) 0.0890(2) 0.030(1) 1.000 . Uani d ?
C(47) -0.3493(5) 0.1601(5) 0.0431(2) 0.046(2) 1.000 . Uani d ?
C(48) -0.4586(7) 0.1554(5) 0.0119(2) 0.059(2) 1.000 . Uani d ?
C(49) -0.5737(6) 0.1456(6) 0.0254(2) 0.065(2) 1.000 . Uani d ?
C(50) -0.5855(5) 0.1404(5) 0.0708(2) 0.063(2) 1.000 . Uani d ?
C(51) -0.4777(5) 0.1454(5) 0.1030(2) 0.044(2) 1.000 . Uani d ?
C(52) -0.1929(4) 0.0754(4) 0.1471(2) 0.0243(13) 1.000 . Uani d ?
C(53) -0.2300(4) -0.0537(4) 0.1424(2) 0.0247(13) 1.000 . Uani d ?
C(54) -0.3145(5) -0.1171(4) 0.1049(2) 0.036(2) 1.000 . Uani d ?
C(55) -0.3525(5) -0.2386(5) 0.1022(2) 0.042(2) 1.000 . Uani d ?
C(56) -0.3043(5) -0.3001(4) 0.1361(2) 0.041(2) 1.000 . Uani d ?
C(57) -0.2168(5) -0.2419(4) 0.1723(2) 0.033(2) 1.000 . Uani d ?
C(58) -0.1824(4) -0.1192(4) 0.1757(2) 0.032(2) 1.000 . Uani d ?
C(59) 0.0761(4) 0.4199(4) 0.1766(2) 0.0235(13) 1.000 . Uani d ?
C(60) 0.0829(5) 0.2721(4) 0.1035(2) 0.037(2) 1.000 . Uani d ?
C(61) 0.1621(4) 0.4902(4) 0.1197(2) 0.028(1) 1.000 . Uani d ?
C(62) 0.2068(5) 0.4931(4) 0.0741(2) 0.032(2) 1.000 . Uani d ?
C(63) 0.1457(6) 0.5526(6) 0.0424(2) 0.058(2) 1.000 . Uani d ?
C(64) 0.1881(7) 0.5594(7) 0.0001(2) 0.079(3) 1.000 . Uani d ?
C(65) 0.2897(6) 0.5056(6) -0.0099(2) 0.064(2) 1.000 . Uani d ?
C(66) 0.3518(5) 0.4460(5) 0.0216(2) 0.049(2) 1.000 . Uani d ?
C(67) 0.3103(5) 0.4399(5) 0.0641(2) 0.042(2) 1.000 . Uani d ?
C(68) 0.1654(4) 0.5809(4) 0.1552(2) 0.026(1) 1.000 . Uani d ?
C(69) 0.2117(4) 0.7084(4) 0.1587(2) 0.0257(13) 1.000 . Uani d ?
C(70) 0.3253(5) 0.7475(4) 0.1429(2) 0.037(2) 1.000 . Uani d ?
C(71) 0.3656(5) 0.8669(5) 0.1470(2) 0.047(2) 1.000 . Uani d ?
C(72) 0.2979(5) 0.9501(5) 0.1666(2) 0.049(2) 1.000 . Uani d ?
C(73) 0.1899(5) 0.9128(5) 0.1831(2) 0.050(2) 1.000 . Uani d ?
C(74) 0.1473(5) 0.7927(5) 0.1792(2) 0.039(2) 1.000 . Uani d ?
C(76) 1.006(2) 0.059(2) -0.0265(7) 0.109(6) 0.500 S Uiso d ?
H(1) 0.3674 0.6720 0.3916 0.027 1.000 . Uiso c ?
H(2) 0.2578 0.6447 0.3505 0.027 1.000 . Uiso c ?
H(3) 0.3671 0.5664 0.3526 0.027 1.000 . Uiso c ?
H(4) 0.3801 0.8711 0.3766 0.034 1.000 . Uiso c ?
H(5) 0.4446 0.9112 0.3360 0.034 1.000 . Uiso c ?
H(6) 0.3028 0.8602 0.3276 0.034 1.000 . Uiso c ?
H(7) 0.7316 0.7001 0.2861 0.035 1.000 . Uiso c ?
H(8) 0.6092 0.7213 0.2559 0.035 1.000 . Uiso c ?
H(9) 0.7241 0.8203 0.2668 0.035 1.000 . Uiso c ?
H(10) 0.7247 1.0699 0.4083 0.049 1.000 . Uiso c ?
H(11) 0.7609 0.9784 0.3701 0.049 1.000 . Uiso c ?
H(12) 0.6253 1.0137 0.3660 0.049 1.000 . Uiso c ?
H(13) 0.6920 1.2980 0.5254 0.048 1.000 . Uiso c ?
H(14) 0.8765 1.2929 0.5745 0.056 1.000 . Uiso c ?
H(15) 0.9767 1.1238 0.5701 0.059 1.000 . Uiso c ?
H(16) 0.8910 0.9538 0.5176 0.045 1.000 . Uiso c ?
H(17) 0.6413 0.9204 0.5563 0.039 1.000 . Uiso c ?
H(18) 0.6228 0.8439 0.6251 0.046 1.000 . Uiso c ?
H(19) 0.5961 0.6402 0.6266 0.046 1.000 . Uiso c ?
H(20) 0.5887 0.5088 0.5582 0.042 1.000 . Uiso c ?
H(21) 0.6114 0.5828 0.4897 0.036 1.000 . Uiso c ?
H(22) 0.8217 0.6747 0.4231 0.037 1.000 . Uiso c ?
H(23) 0.9044 0.6626 0.3839 0.037 1.000 . Uiso c ?
H(24) 0.8098 0.7562 0.3848 0.037 1.000 . Uiso c ?
H(25) 0.9841 0.4831 0.3413 0.039 1.000 . Uiso c ?
H(26) 1.1493 0.4044 0.3802 0.047 1.000 . Uiso c ?
H(27) 1.1149 0.2896 0.4378 0.058 1.000 . Uiso c ?
H(28) 0.9124 0.2508 0.4569 0.062 1.000 . Uiso c ?
H(29) 0.7459 0.3380 0.4203 0.047 1.000 . Uiso c ?
H(30) 0.7904 0.2716 0.2924 0.047 1.000 . Uiso c ?
H(31) 0.7539 0.0722 0.2593 0.054 1.000 . Uiso c ?
H(32) 0.5533 -0.0305 0.2477 0.049 1.000 . Uiso c ?
H(33) 0.3865 0.0666 0.2692 0.040 1.000 . Uiso c ?
H(34) 0.4204 0.2679 0.3010 0.034 1.000 . Uiso c ?
H(35) 0.0890 0.2414 0.3011 0.037 1.000 . Uiso c ?
H(36) -0.0233 0.1909 0.2625 0.037 1.000 . Uiso c ?
H(37) 0.0989 0.1300 0.2660 0.037 1.000 . Uiso c ?
H(38) 0.2568 0.1794 0.2258 0.035 1.000 . Uiso c ?
H(39) 0.1521 0.1678 0.1834 0.035 1.000 . Uiso c ?
H(40) 0.2533 0.2793 0.1945 0.035 1.000 . Uiso c ?
H(41) -0.1896 0.4635 0.2614 0.055 1.000 . Uiso c ?
H(42) -0.1490 0.5240 0.2205 0.055 1.000 . Uiso c ?
H(43) -0.2126 0.3925 0.2118 0.055 1.000 . Uiso c ?
H(44) -0.2142 0.4359 0.1526 0.042 1.000 . Uiso c ?
H(45) -0.1334 0.4121 0.1133 0.042 1.000 . Uiso c ?
H(46) -0.2763 0.3655 0.1050 0.042 1.000 . Uiso c ?
H(47) -0.2687 0.1665 0.0331 0.055 1.000 . Uiso c ?
H(48) -0.4517 0.1597 -0.0199 0.072 1.000 . Uiso c ?
H(49) -0.6470 0.1413 0.0033 0.079 1.000 . Uiso c ?
H(50) -0.6665 0.1339 0.0803 0.076 1.000 . Uiso c ?
H(51) -0.4850 0.1423 0.1346 0.054 1.000 . Uiso c ?
H(52) -0.3470 -0.0760 0.0807 0.043 1.000 . Uiso c ?
H(53) -0.4122 -0.2791 0.0770 0.050 1.000 . Uiso c ?
H(54) -0.3316 -0.3830 0.1346 0.049 1.000 . Uiso c ?
H(55) -0.1806 -0.2852 0.1951 0.039 1.000 . Uiso c ?
H(56) -0.1243 -0.0796 0.2017 0.039 1.000 . Uiso c ?
H(57) 0.0690 0.2099 0.1217 0.044 1.000 . Uiso c ?
H(58) 0.0108 0.2707 0.0811 0.044 1.000 . Uiso c ?
H(59) 0.1541 0.2604 0.0884 0.044 1.000 . Uiso c ?
H(60) 0.0742 0.5898 0.0494 0.069 1.000 . Uiso c ?
H(61) 0.1449 0.6016 -0.0217 0.096 1.000 . Uiso c ?
H(62) 0.3173 0.5101 -0.0390 0.076 1.000 . Uiso c ?
H(63) 0.4230 0.4095 0.0146 0.059 1.000 . Uiso c ?
H(64) 0.3533 0.3989 0.0863 0.050 1.000 . Uiso c ?
H(65) 0.3731 0.6905 0.1293 0.044 1.000 . Uiso c ?
H(66) 0.4421 0.8925 0.1365 0.057 1.000 . Uiso c ?
H(67) 0.3260 1.0330 0.1686 0.059 1.000 . Uiso c ?
H(68) 0.1440 0.9701 0.1975 0.060 1.000 . Uiso c ?
H(69) 0.0721 0.7681 0.1909 0.047 1.000 . Uiso c ?


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

# REFINEMENT DATA

_refine_special_details          
;
?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00002|Fo|²]'
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         8660
_refine_ls_number_parameters     839
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.041
_refine_ls_R_factor_gt           0.066
_refine_ls_wR_factor_all         0.097
_refine_ls_wR_factor_ref         0.088
_refine_ls_goodness_of_fit_all   1.258
_refine_ls_goodness_of_fit_ref   1.600
_refine_ls_shift/su_max          0.0800
_refine_ls_shift/su_mean         0.0014
_refine_diff_density_min         -0.57
_refine_diff_density_max         0.91

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

# MOLECULAR GEOMETRY

_geom_special_details            
;
?
;
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
BR1 ZN1 2.3705(9) . . ?
BR2 ZN2 2.3571(9) . . ?
ZN1 S1 2.340(2) . . ?
ZN1 S2 2.381(2) . . ?
ZN1 N4 2.061(4) . . ?
ZN2 S1 2.403(2) . . ?
ZN2 S2 2.379(2) . . ?
ZN2 N8 2.050(4) . . ?
CL1 CL2 0.36(2) . . ?
CL1 CL4 2.31(4) . . ?
CL1 CL5 1.78(3) . . ?
CL2 CL4 1.95(4) . . ?
CL2 CL5 1.43(2) . . ?
CL2 C76 1.85(3) . . ?
CL3 CL4 1.16(3) . . ?
CL3 CL5 1.67(3) . . ?
CL3 CL6 1.68(2) . . ?
CL3 CL6 2.15(2) . . ?
CL3 C76 1.35(3) . . ?
CL4 CL5 0.84(3) . . ?
CL4 CL6 1.96(5) . . ?
CL4 CL6 2.23(4) . . ?
CL4 C76 1.06(3) . . ?
CL5 C76 1.53(3) . . ?
CL6 CL6 1.10(3) . . ?
CL6 C76 1.27(3) . . ?
CL6 C76 1.19(3) . . ?
S1 C1 1.863(5) . . ?
S2 C38 1.864(5) . . ?
O1 C4 1.421(6) . . ?
O1 C5 1.422(6) . . ?
O2 C41 1.434(6) . . ?
O2 C42 1.373(7) . . ?
N1 C6 1.373(7) . . ?
N1 C7 1.458(7) . . ?
N1 C8 1.398(6) . . ?
N2 C6 1.294(7) . . ?
N2 C9 1.385(6) . . ?
N3 C22 1.465(6) . . ?
N3 C23 1.384(7) . . ?
N3 C37 1.347(6) . . ?
N4 C24 1.385(6) . . ?
N4 C37 1.350(6) . . ?
N5 C43 1.378(6) . . ?
N5 C44 1.454(7) . . ?
N5 C45 1.401(7) . . ?
N6 C43 1.302(7) . . ?
N6 C52 1.375(6) . . ?
N7 C59 1.362(7) . . ?
N7 C60 1.476(7) . . ?
N7 C61 1.379(7) . . ?
N8 C59 1.323(7) . . ?
N8 C68 1.387(7) . . ?
C1 C2 1.521(7) . . ?
C1 C3 1.536(8) . . ?
C1 C4 1.587(7) . . ?
C2 H1 0.95 . . no
C2 H2 0.95 . . no
C2 H3 0.95 . . no
C3 H4 0.95 . . no
C3 H5 0.95 . . no
C3 H6 0.95 . . no
C4 C6 1.550(7) . . ?
C4 C37 1.532(7) . . ?
C5 H7 0.95 . . no
C5 H8 0.95 . . no
C5 H9 0.95 . . no
C7 H10 0.95 . . no
C7 H11 0.95 . . no
C7 H12 0.95 . . no
C8 C9 1.368(8) . . ?
C8 C10 1.487(7) . . ?
C9 C16 1.467(8) . . ?
C10 C11 1.395(8) . . ?
C10 C15 1.386(8) . . ?
C11 C12 1.401(8) . . ?
C12 C13 1.364(8) . . ?
C12 H13 0.95 . . no
C13 C14 1.356(9) . . ?
C13 H14 0.95 . . no
C14 C15 1.390(8) . . ?
C14 H15 0.95 . . no
C15 H16 0.95 . . no
C16 C17 1.400(7) . . ?
C16 C21 1.388(8) . . ?
C17 C18 1.390(8) . . ?
C17 H17 0.95 . . no
C18 C19 1.359(9) . . ?
C18 H18 0.95 . . no
C19 C20 1.382(8) . . ?
C19 H19 0.95 . . no
C20 C21 1.378(8) . . ?
C20 H20 0.95 . . no
C21 H21 0.95 . . no
C22 H22 0.95 . . no
C22 H23 0.95 . . no
C22 H24 0.95 . . no
C23 C24 1.373(7) . . ?
C23 C30 1.483(7) . . ?
C24 C31 1.486(7) . . ?
C25 C26 1.369(8) . . ?
C25 C30 1.397(8) . . ?
C25 H25 0.95 . . no
C26 C27 1.369(9) . . ?
C26 H26 0.95 . . no
C27 C28 1.384(9) . . ?
C27 H27 0.95 . . no
C28 C29 1.397(8) . . ?
C28 H28 0.95 . . no
C29 C30 1.384(8) . . ?
C29 H29 0.95 . . no
C31 C32 1.397(8) . . ?
C31 C36 1.383(7) . . ?
C32 C33 1.383(8) . . ?
C32 H30 0.95 . . no
C33 C34 1.358(8) . . ?
C33 H31 0.95 . . no
C34 C35 1.379(8) . . ?
C34 H32 0.95 . . no
C35 C36 1.390(8) . . ?
C35 H33 0.95 . . no
C36 H34 0.95 . . no
C38 C39 1.532(8) . . ?
C38 C40 1.517(8) . . ?
C38 C41 1.584(7) . . ?
C39 H35 0.95 . . no
C39 H36 0.95 . . no
C39 H37 0.95 . . no
C40 H38 0.95 . . no
C40 H39 0.95 . . no
C40 H40 0.95 . . no
C41 C43 1.540(7) . . ?
C41 C59 1.519(8) . . ?
C42 H41 0.95 . . no
C42 H42 0.95 . . no
C42 H43 0.95 . . no
C44 H44 0.95 . . no
C44 H45 0.95 . . no
C44 H46 0.95 . . no
C45 C46 1.499(7) . . ?
C45 C52 1.359(7) . . ?
C46 C47 1.378(8) . . ?
C46 C51 1.388(8) . . ?
C47 C48 1.389(9) . . ?
C47 H47 0.95 . . no
C48 C49 1.350(11) . . ?
C48 H48 0.95 . . no
C49 C50 1.367(11) . . ?
C49 H49 0.95 . . no
C50 C51 1.390(9) . . ?
C50 H50 0.95 . . no
C51 H51 0.95 . . no
C52 C53 1.463(8) . . ?
C53 C54 1.399(7) . . ?
C53 C58 1.387(8) . . ?
C54 C55 1.387(9) . . ?
C54 H52 0.95 . . no
C55 C56 1.369(9) . . ?
C55 H53 0.95 . . no
C56 C57 1.373(8) . . ?
C56 H54 0.95 . . no
C57 C58 1.392(8) . . ?
C57 H55 0.95 . . no
C58 H56 0.95 . . no
C60 H57 0.95 . . no
C60 H58 0.95 . . no
C60 H59 0.95 . . no
C61 C62 1.488(8) . . ?
C61 C68 1.364(7) . . ?
C62 C63 1.365(8) . . ?
C62 C67 1.373(9) . . ?
C63 C64 1.392(9) . . ?
C63 H60 0.95 . . no
C64 C65 1.358(10) . . ?
C64 H61 0.95 . . no
C65 C66 1.365(9) . . ?
C65 H62 0.95 . . no
C66 C67 1.390(9) . . ?
C66 H63 0.95 . . no
C67 H64 0.95 . . no
C68 C69 1.467(8) . . ?
C69 C70 1.414(8) . . ?
C69 C74 1.368(8) . . ?
C70 C71 1.365(8) . . ?
C70 H65 0.95 . . no
C71 C72 1.372(9) . . ?
C71 H66 0.95 . . no
C72 C73 1.366(9) . . ?
C72 H67 0.95 . . no
C73 C74 1.378(9) . . ?
C73 H68 0.95 . . no
C74 H69 0.95 . . 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
BR1 ZN1 S1 114.89(5) . . . ?
BR1 ZN1 S2 122.76(5) . . . ?
BR1 ZN1 N4 111.01(12) . . . ?
S1 ZN1 S2 94.84(5) . . . ?
S1 ZN1 N4 99.19(13) . . . ?
S2 ZN1 N4 110.77(13) . . . ?
BR2 ZN2 S1 113.13(5) . . . ?
BR2 ZN2 S2 129.23(5) . . . ?
BR2 ZN2 N8 117.77(13) . . . ?
S1 ZN2 S2 93.25(5) . . . ?
S1 ZN2 N8 104.65(13) . . . ?
S2 ZN2 N8 94.08(13) . . . ?
CL2 CL1 CL4 5.0(43) . . . ?
CL2 CL1 CL5 13.4(41) . . . ?
CL4 CL1 CL5 18.3(11) . . . ?
CL1 CL2 CL4 174.1(51) . . . ?
CL1 CL2 CL5 163.2(52) . . . ?
CL1 CL2 C76 142.2(50) . . . ?
CL4 CL2 CL5 22.6(13) . . . ?
CL4 CL2 C76 32.1(10) . . . ?
CL5 CL2 C76 53.9(13) . . . ?
CL4 CL3 CL5 27.8(18) . . . ?
CL4 CL3 CL6 85.3(22) . . . ?
CL4 CL3 CL6 78.6(19) . . . ?
CL4 CL3 C76 49.2(17) . . . ?
CL5 CL3 CL6 105.9(12) . . . ?
CL5 CL3 CL6 88.1(10) . . . ?
CL5 CL3 C76 60.0(14) . . . ?
CL6 CL3 CL6 30.3(11) . . . ?
CL6 CL3 C76 47.9(11) . . . ?
CL6 CL3 C76 29.7(13) 2_755 2_755 2_755 ?
CL1 CL4 CL2 0.9(8) . . . ?
CL1 CL4 CL3 111.5(22) . . . ?
CL1 CL4 CL5 41.6(26) . . . ?
CL1 CL4 CL6 103.4(16) . . . ?
CL1 CL4 CL6 73.9(11) . . . ?
CL1 CL4 C76 67.6(24) . . . ?
CL2 CL4 CL3 111.8(23) . . . ?
CL2 CL4 CL5 40.7(25) . . . ?
CL2 CL4 CL6 104.3(18) . . . ?
CL2 CL4 CL6 74.8(13) . . . ?
CL2 CL4 C76 68.5(23) . . . ?
CL3 CL4 CL5 112.4(42) . . . ?
CL3 CL4 CL6 58.7(18) . . . ?
CL3 CL4 CL6 70.9(19) . . . ?
CL3 CL4 C76 74.8(28) . . . ?
CL5 CL4 CL6 141.8(39) . . . ?
CL5 CL4 CL6 113.4(35) . . . ?
CL5 CL4 C76 107.4(42) . . . ?
CL6 CL4 CL6 29.5(11) . . . ?
CL6 CL4 C76 35.8(21) . . . ?
CL6 CL4 C76 6.3(22) 2_755 2_755 2_755 ?
CL1 CL5 CL2 3.4(10) . . . ?
CL1 CL5 CL3 117.3(13) . . . ?
CL1 CL5 CL4 120.1(35) . . . ?
CL1 CL5 C76 80.5(16) . . . ?
CL2 CL5 CL3 115.0(15) . . . ?
CL2 CL5 CL4 116.7(35) . . . ?
CL2 CL5 C76 77.3(15) . . . ?
CL3 CL5 CL4 39.9(29) . . . ?
CL3 CL5 C76 49.5(12) . . . ?
CL4 CL5 C76 41.0(27) . . . ?
CL3 CL6 CL3 149.7(11) . . . ?
CL3 CL6 CL4 36.0(11) . . . ?
CL3 CL6 CL4 142.2(15) . . . ?
CL3 CL6 CL6 99.2(27) . . . ?
CL3 CL6 C76 52.1(16) . . . ?
CL3 CL6 C76 143.5(20) . . . ?
CL3 CL6 CL4 128.5(14) 2_755 2_755 2_755 ?
CL3 CL6 CL4 30.5(9) 2_755 2_755 2_755 ?
CL3 CL6 CL6 50.5(21) 2_755 2_755 2_755 ?
CL3 CL6 C76 102.8(17) 2_755 2_755 2_755 ?
CL3 CL6 C76 34.2(13) 2_755 2_755 2_755 ?
CL4 CL6 CL4 150.5(11) . . . ?
CL4 CL6 CL6 89.0(28) . . . ?
CL4 CL6 C76 29.2(17) . . . ?
CL4 CL6 C76 156.0(24) . . . ?
CL4 CL6 CL6 61.5(25) 2_755 2_755 2_755 ?
CL4 CL6 C76 121.2(20) 2_755 2_755 2_755 ?
CL4 CL6 C76 5.6(19) 2_755 2_755 2_755 ?
CL6 CL6 C76 59.8(20) 2_755 2_755 2_755 ?
CL6 CL6 C76 67.1(21) 2_755 2_755 2_755 ?
C76 CL6 C76 126.8(21) . . . ?
ZN1 S1 ZN2 82.92(5) . . . ?
ZN1 S1 C1 99.2(2) . . . ?
ZN2 S1 C1 104.2(2) . . . ?
ZN1 S2 ZN2 82.59(5) . . . ?
ZN1 S2 C38 119.7(2) . . . ?
ZN2 S2 C38 109.1(2) . . . ?
C4 O1 C5 120.2(4) . . . ?
C41 O2 C42 125.3(4) . . . ?
C6 N1 C7 131.2(5) . . . ?
C6 N1 C8 105.5(5) . . . ?
C7 N1 C8 123.3(5) . . . ?
C6 N2 C9 106.6(5) . . . ?
C22 N3 C23 122.8(5) . . . ?
C22 N3 C37 128.5(5) . . . ?
C23 N3 C37 108.6(4) . . . ?
ZN1 N4 C24 125.7(4) . . . ?
ZN1 N4 C37 124.8(4) . . . ?
C24 N4 C37 106.4(4) . . . ?
C43 N5 C44 132.1(5) . . . ?
C43 N5 C45 105.7(5) . . . ?
C44 N5 C45 122.2(5) . . . ?
C43 N6 C52 107.2(5) . . . ?
C59 N7 C60 130.1(5) . . . ?
C59 N7 C61 107.7(5) . . . ?
C60 N7 C61 122.1(5) . . . ?
ZN2 N8 C59 119.0(4) . . . ?
ZN2 N8 C68 126.5(4) . . . ?
C59 N8 C68 107.1(5) . . . ?
S1 C1 C2 112.4(4) . . . ?
S1 C1 C3 104.9(4) . . . ?
S1 C1 C4 109.2(4) . . . ?
C2 C1 C3 108.5(4) . . . ?
C2 C1 C4 111.8(4) . . . ?
C3 C1 C4 109.9(4) . . . ?
C1 C2 H1 109.4 . . . no
C1 C2 H2 109.5 . . . no
C1 C2 H3 109.4 . . . no
H1 C2 H2 109.6 . . . no
H1 C2 H3 109.5 . . . no
H2 C2 H3 109.5 . . . no
C1 C3 H4 109.4 . . . no
C1 C3 H5 109.2 . . . no
C1 C3 H6 109.4 . . . no
H4 C3 H5 109.6 . . . no
H4 C3 H6 109.8 . . . no
H5 C3 H6 109.4 . . . no
O1 C4 C1 110.7(4) . . . ?
O1 C4 C6 105.8(4) . . . ?
O1 C4 C37 110.8(4) . . . ?
C1 C4 C6 106.4(4) . . . ?
C1 C4 C37 115.8(4) . . . ?
C6 C4 C37 106.6(4) . . . ?
O1 C5 H7 109.5 . . . no
O1 C5 H8 109.5 . . . no
O1 C5 H9 109.6 . . . no
H7 C5 H8 109.3 . . . no
H7 C5 H9 109.5 . . . no
H8 C5 H9 109.4 . . . no
N1 C6 N2 112.4(5) . . . ?
N1 C6 C4 126.0(5) . . . ?
N2 C6 C4 121.6(5) . . . ?
N1 C7 H10 109.4 . . . no
N1 C7 H11 109.5 . . . no
N1 C7 H12 109.3 . . . no
H10 C7 H11 109.6 . . . no
H10 C7 H12 109.3 . . . no
H11 C7 H12 109.7 . . . no
N1 C8 C9 106.3(5) . . . ?
N1 C8 C10 122.8(5) . . . ?
C9 C8 C10 130.9(5) . . . ?
N2 C9 C8 109.2(5) . . . ?
N2 C9 C16 119.6(5) . . . ?
C8 C9 C16 131.1(5) . . . ?
C8 C10 C11 120.6(5) . . . ?
C8 C10 C15 119.9(6) . . . ?
C11 C10 C15 119.3(5) . . . ?
C10 C11 C12 119.1(6) . . . ?
C11 C12 C13 120.6(6) . . . ?
C11 C12 H13 119.4 . . . no
C13 C12 H13 120.0 . . . no
C12 C13 C14 120.2(6) . . . ?
C12 C13 H14 119.7 . . . no
C14 C13 H14 120.1 . . . no
C13 C14 C15 120.8(6) . . . ?
C13 C14 H15 119.8 . . . no
C15 C14 H15 119.4 . . . no
C10 C15 C14 119.9(6) . . . ?
C10 C15 H16 119.8 . . . no
C14 C15 H16 120.3 . . . no
C9 C16 C17 122.7(6) . . . ?
C9 C16 C21 119.9(5) . . . ?
C17 C16 C21 117.4(6) . . . ?
C16 C17 C18 120.2(6) . . . ?
C16 C17 H17 119.6 . . . no
C18 C17 H17 120.1 . . . no
C17 C18 C19 121.2(6) . . . ?
C17 C18 H18 119.2 . . . no
C19 C18 H18 119.6 . . . no
C18 C19 C20 119.5(6) . . . ?
C18 C19 H19 120.5 . . . no
C20 C19 H19 120.0 . . . no
C19 C20 C21 119.9(6) . . . ?
C19 C20 H20 120.2 . . . no
C21 C20 H20 119.9 . . . no
C16 C21 C20 121.7(5) . . . ?
C16 C21 H21 119.2 . . . no
C20 C21 H21 119.1 . . . no
N3 C22 H22 109.5 . . . no
N3 C22 H23 109.4 . . . no
N3 C22 H24 109.4 . . . no
H22 C22 H23 109.5 . . . no
H22 C22 H24 109.6 . . . no
H23 C22 H24 109.5 . . . no
N3 C23 C24 105.9(5) . . . ?
N3 C23 C30 121.9(5) . . . ?
C24 C23 C30 131.9(5) . . . ?
N4 C24 C23 109.2(5) . . . ?
N4 C24 C31 124.4(5) . . . ?
C23 C24 C31 126.3(5) . . . ?
C26 C25 C30 120.5(6) . . . ?
C26 C25 H25 119.8 . . . no
C30 C25 H25 119.7 . . . no
C25 C26 C27 120.4(6) . . . ?
C25 C26 H26 120.0 . . . no
C27 C26 H26 119.7 . . . no
C26 C27 C28 120.4(6) . . . ?
C26 C27 H27 120.0 . . . no
C28 C27 H27 119.6 . . . no
C27 C28 C29 119.7(6) . . . ?
C27 C28 H28 120.3 . . . no
C29 C28 H28 120.0 . . . no
C28 C29 C30 119.8(6) . . . ?
C28 C29 H29 120.1 . . . no
C30 C29 H29 120.1 . . . no
C23 C30 C25 121.8(5) . . . ?
C23 C30 C29 119.0(5) . . . ?
C25 C30 C29 119.2(6) . . . ?
C24 C31 C32 120.3(5) . . . ?
C24 C31 C36 122.3(5) . . . ?
C32 C31 C36 117.4(5) . . . ?
C31 C32 C33 121.3(6) . . . ?
C31 C32 H30 119.2 . . . no
C33 C32 H30 119.5 . . . no
C32 C33 C34 120.4(6) . . . ?
C32 C33 H31 120.0 . . . no
C34 C33 H31 119.6 . . . no
C33 C34 C35 119.5(6) . . . ?
C33 C34 H32 120.4 . . . no
C35 C34 H32 120.1 . . . no
C34 C35 C36 120.4(6) . . . ?
C34 C35 H33 119.7 . . . no
C36 C35 H33 119.9 . . . no
C31 C36 C35 120.8(6) . . . ?
C31 C36 H34 119.7 . . . no
C35 C36 H34 119.5 . . . no
N3 C37 N4 109.9(5) . . . ?
N3 C37 C4 122.2(5) . . . ?
N4 C37 C4 127.9(5) . . . ?
S2 C38 C39 103.8(4) . . . ?
S2 C38 C40 109.2(4) . . . ?
S2 C38 C41 108.3(4) . . . ?
C39 C38 C40 111.3(5) . . . ?
C39 C38 C41 113.1(4) . . . ?
C40 C38 C41 110.8(4) . . . ?
C38 C39 H35 109.4 . . . no
C38 C39 H36 109.3 . . . no
C38 C39 H37 109.4 . . . no
H35 C39 H36 109.7 . . . no
H35 C39 H37 109.7 . . . no
H36 C39 H37 109.4 . . . no
C38 C40 H38 109.7 . . . no
C38 C40 H39 109.8 . . . no
C38 C40 H40 109.6 . . . no
H38 C40 H39 109.5 . . . no
H38 C40 H40 109.1 . . . no
H39 C40 H40 109.1 . . . no
O2 C41 C38 103.5(4) . . . ?
O2 C41 C43 111.4(4) . . . ?
O2 C41 C59 109.2(4) . . . ?
C38 C41 C43 113.0(4) . . . ?
C38 C41 C59 109.6(4) . . . ?
C43 C41 C59 109.9(4) . . . ?
O2 C42 H41 109.5 . . . no
O2 C42 H42 109.6 . . . no
O2 C42 H43 109.5 . . . no
H41 C42 H42 109.4 . . . no
H41 C42 H43 109.3 . . . no
H42 C42 H43 109.5 . . . no
N5 C43 N6 111.3(5) . . . ?
N5 C43 C41 123.4(5) . . . ?
N6 C43 C41 125.3(5) . . . ?
N5 C44 H44 109.4 . . . no
N5 C44 H45 109.4 . . . no
N5 C44 H46 109.4 . . . no
H44 C44 H45 109.5 . . . no
H44 C44 H46 109.6 . . . no
H45 C44 H46 109.6 . . . no
N5 C45 C46 119.8(5) . . . ?
N5 C45 C52 106.3(5) . . . ?
C46 C45 C52 133.6(5) . . . ?
C45 C46 C47 121.2(6) . . . ?
C45 C46 C51 119.1(6) . . . ?
C47 C46 C51 119.7(6) . . . ?
C46 C47 C48 118.7(7) . . . ?
C46 C47 H47 120.5 . . . no
C48 C47 H47 120.7 . . . no
C47 C48 C49 121.5(7) . . . ?
C47 C48 H48 118.8 . . . no
C49 C48 H48 119.6 . . . no
C48 C49 C50 120.5(7) . . . ?
C48 C49 H49 119.8 . . . no
C50 C49 H49 119.7 . . . no
C49 C50 C51 119.3(8) . . . ?
C49 C50 H50 120.4 . . . no
C51 C50 H50 120.3 . . . no
C46 C51 C50 120.2(7) . . . ?
C46 C51 H51 119.9 . . . no
C50 C51 H51 119.9 . . . no
N6 C52 C45 109.5(5) . . . ?
N6 C52 C53 120.4(5) . . . ?
C45 C52 C53 130.1(5) . . . ?
C52 C53 C54 122.7(5) . . . ?
C52 C53 C58 120.6(5) . . . ?
C54 C53 C58 116.7(6) . . . ?
C53 C54 C55 121.6(6) . . . ?
C53 C54 H52 119.3 . . . no
C55 C54 H52 119.1 . . . no
C54 C55 C56 120.0(6) . . . ?
C54 C55 H53 120.1 . . . no
C56 C55 H53 119.9 . . . no
C55 C56 C57 120.1(6) . . . ?
C55 C56 H54 120.0 . . . no
C57 C56 H54 120.0 . . . no
C56 C57 C58 119.7(6) . . . ?
C56 C57 H55 120.1 . . . no
C58 C57 H55 120.2 . . . no
C53 C58 C57 121.8(5) . . . ?
C53 C58 H56 119.3 . . . no
C57 C58 H56 118.9 . . . no
N7 C59 N8 110.0(5) . . . ?
N7 C59 C41 128.2(5) . . . ?
N8 C59 C41 121.7(5) . . . ?
N7 C60 H57 109.3 . . . no
N7 C60 H58 109.6 . . . no
N7 C60 H59 109.4 . . . no
H57 C60 H58 109.6 . . . no
H57 C60 H59 109.3 . . . no
H58 C60 H59 109.7 . . . no
N7 C61 C62 124.0(5) . . . ?
N7 C61 C68 106.5(5) . . . ?
C62 C61 C68 129.5(6) . . . ?
C61 C62 C63 119.2(6) . . . ?
C61 C62 C67 121.2(6) . . . ?
C63 C62 C67 119.6(6) . . . ?
C62 C63 C64 120.2(7) . . . ?
C62 C63 H60 119.7 . . . no
C64 C63 H60 120.1 . . . no
C63 C64 C65 119.9(7) . . . ?
C63 C64 H61 119.3 . . . no
C65 C64 H61 120.7 . . . no
C64 C65 C66 120.5(7) . . . ?
C64 C65 H62 119.3 . . . no
C66 C65 H62 120.2 . . . no
C65 C66 C67 119.7(7) . . . ?
C65 C66 H63 120.1 . . . no
C67 C66 H63 120.2 . . . no
C62 C67 C66 120.1(6) . . . ?
C62 C67 H64 119.6 . . . no
C66 C67 H64 120.3 . . . no
N8 C68 C61 108.7(5) . . . ?
N8 C68 C69 121.3(5) . . . ?
C61 C68 C69 130.0(6) . . . ?
C68 C69 C70 121.5(6) . . . ?
C68 C69 C74 120.2(6) . . . ?
C70 C69 C74 118.3(5) . . . ?
C69 C70 C71 119.8(6) . . . ?
C69 C70 H65 119.9 . . . no
C71 C70 H65 120.3 . . . no
C70 C71 C72 121.0(6) . . . ?
C70 C71 H66 119.4 . . . no
C72 C71 H66 119.6 . . . no
C71 C72 C73 119.4(6) . . . ?
C71 C72 H67 120.2 . . . no
C73 C72 H67 120.4 . . . no
C72 C73 C74 120.5(6) . . . ?
C72 C73 H68 119.7 . . . no
C74 C73 H68 119.7 . . . no
C69 C74 C73 120.9(6) . . . ?
C69 C74 H69 119.5 . . . no
C73 C74 H69 119.6 . . . no
CL2 C76 CL3 108.7(16) . . . ?
CL2 C76 CL4 79.4(26) . . . ?
CL2 C76 CL5 48.8(11) . . . ?
CL2 C76 CL6 165.5(26) . . . ?
CL2 C76 CL6 112.4(23) . . . ?
CL3 C76 CL4 56.0(22) . . . ?
CL3 C76 CL5 70.5(16) . . . ?
CL3 C76 CL6 80.0(18) . . . ?
CL3 C76 CL6 116.1(23) . . . ?
CL4 C76 CL5 31.5(21) . . . ?
CL4 C76 CL6 114.9(35) . . . ?
CL4 C76 CL6 168.0(40) . . . ?
CL5 C76 CL6 145.0(28) . . . ?
CL5 C76 CL6 159.4(28) . . . ?
CL6 C76 CL6 53.2(21) . . . ?
#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O1 C34 3.525(7) . 1_565 no
O2 H25 2.9377 . 1_455 no
O2 H30 2.9885 . 1_455 no
N4 H19 3.0286 . 2_666 no
C5 H32 3.0582 . 1_565 no
C5 C57 3.467(8) . 1_665 no
C11 C17 3.529(8) . 2_676 no
C12 H1 2.9725 . 2_676 no
C12 H28 2.9766 . 1_565 no
C18 C36 3.592(9) . 2_666 no
C19 H26 2.8972 . 2_766 no
C19 H34 3.0111 . 2_666 no
C19 C36 3.558(9) . 2_666 no
C20 H21 2.9354 . 2_666 no
C20 H26 3.0508 . 2_766 no
C20 C21 3.590(8) . 2_666 no
C21 H27 3.0417 . 2_766 no
C22 H15 2.9350 . 2_776 no
C23 H41 2.9011 . 1_655 no
C24 H41 2.8445 . 1_655 no
C26 H35 2.9361 . 1_655 no
C32 H41 2.9962 . 1_655 no
C32 C42 3.452(10) . 1_655 no
C35 C72 3.598(9) . 1_545 no
C36 H19 2.9342 . 2_666 no
C36 H18 2.9937 . 2_666 no
C40 H68 2.8355 . 1_545 no
C40 H67 2.8435 . 1_545 no
C40 C72 3.481(9) . 1_545 no
C40 C73 3.482(9) . 1_545 no
C42 H30 2.9117 . 1_455 no
C48 C48 3.51(2) . 2_455 no
C48 C49 3.528(10) . 2_455 no
C54 H66 2.9059 . 1_445 no
C55 H66 3.0104 . 1_445 no
C57 H9 2.9507 . 1_445 no
C72 H38 3.0538 . 1_565 no
C73 H39 2.9710 . 1_565 no
H1 H13 2.5998 . 2_676 no
H3 H19 2.5614 . 2_666 no
H9 H55 2.6733 . 1_665 no
H9 H32 2.6902 . 1_565 no
H14 H23 2.4830 . 2_776 no
H15 H24 2.6422 . 2_776 no
H19 H34 2.2911 . 2_666 no
H20 H21 2.4643 . 2_666 no
H30 H41 2.4693 . 1_655 no
H30 H36 2.5130 . 1_655 no
H31 H36 2.6095 . 1_655 no
H37 H68 2.6701 . 1_545 no
H38 H67 2.4592 . 1_545 no
H38 H68 2.5382 . 1_545 no
H39 H68 2.3328 . 1_545 no
H39 H67 2.5927 . 1_545 no
H42 H55 2.4266 . 1_565 no
H44 H54 2.6057 . 1_565 no
H45 H61 2.6685 . 2_565 no
H46 H62 2.5662 . 2_565 no
H48 H52 2.6313 . 2_455 no
H48 H53 2.6827 . 2_455 no
H49 H52 2.4817 . 2_455 no
H50 H59 2.5498 . 1_455 no
H51 H67 2.6469 . 1_445 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
BR1 ZN1 S1 ZN2 . . . . 110.59(4) no
BR1 ZN1 S1 C1 . . . . -146.1(2) no
BR1 ZN1 S2 ZN2 . . . . -104.57(5) no
BR1 ZN1 S2 C38 . . . . 3.3(2) no
BR1 ZN1 N4 C24 . . . . -46.7(4) no
BR1 ZN1 N4 C37 . . . . 110.3(4) no
BR2 ZN2 S1 ZN1 . . . . 154.51(4) no
BR2 ZN2 S1 C1 . . . . 56.8(2) no
BR2 ZN2 S2 ZN1 . . . . -142.36(5) no
BR2 ZN2 S2 C38 . . . . 98.7(2) no
BR2 ZN2 N8 C59 . . . . -112.3(4) no
BR2 ZN2 N8 C68 . . . . 101.9(4) no
ZN1 S1 ZN2 S2 . . . . 19.03(5) no
ZN1 S1 ZN2 N8 . . . . -76.05(13) no
ZN1 S1 C1 C2 . . . . -57.6(4) no
ZN1 S1 C1 C3 . . . . -175.3(3) no
ZN1 S1 C1 C4 . . . . 67.0(4) no
ZN1 S2 ZN2 S1 . . . . -18.71(5) no
ZN1 S2 ZN2 N8 . . . . 86.25(13) no
ZN1 S2 C38 C39 . . . . 140.9(3) no
ZN1 S2 C38 C40 . . . . 22.1(5) no
ZN1 S2 C38 C41 . . . . -98.7(4) no
ZN1 N4 C24 C23 . . . . 159.9(4) no
ZN1 N4 C24 C31 . . . . -18.8(7) no
ZN1 N4 C37 N3 . . . . -158.9(3) no
ZN1 N4 C37 C4 . . . . 19.5(8) no
ZN2 S1 ZN1 S2 . . . . -19.05(5) no
ZN2 S1 ZN1 N4 . . . . -131.02(13) no
ZN2 S1 C1 C2 . . . . 27.3(4) no
ZN2 S1 C1 C3 . . . . -90.3(4) no
ZN2 S1 C1 C4 . . . . 151.9(3) no
ZN2 S2 ZN1 S1 . . . . 19.27(5) no
ZN2 S2 ZN1 N4 . . . . 121.01(13) no
ZN2 S2 C38 C39 . . . . -126.8(3) no
ZN2 S2 C38 C40 . . . . 114.4(4) no
ZN2 S2 C38 C41 . . . . -6.3(4) no
ZN2 N8 C59 N7 . . . . -151.3(4) no
ZN2 N8 C59 C41 . . . . 27.2(7) no
ZN2 N8 C68 C61 . . . . 149.1(4) no
ZN2 N8 C68 C69 . . . . -32.7(7) no
CL1 CL2 CL4 CL3 . . . . 74(48) no
CL1 CL2 CL4 CL5 . . . . 174(47) no
CL1 CL2 CL4 CL6 . . . . 13(48) no
CL1 CL2 CL4 CL6 . . . . 12(47) no
CL1 CL2 CL4 C76 . . . . 12(48) no
CL1 CL2 CL5 CL3 . . . . -133(17) no
CL1 CL2 CL5 CL4 . . . . -178(17) no
CL1 CL2 CL5 C76 . . . . -166(18) no
CL1 CL2 C76 CL3 . . . . 133.5(76) no
CL1 CL2 C76 CL4 . . . . -178.1(79) no
CL1 CL2 C76 CL5 . . . . 173.5(82) no
CL1 CL2 C76 CL6 . . . . 8(13) no
CL1 CL2 C76 CL6 . . . . 3.6(84) no
CL1 CL4 CL2 CL5 . . . . -174(47) no
CL1 CL4 CL2 C76 . . . . -12(48) no
CL1 CL4 CL3 CL5 . . . . 45.0(32) no
CL1 CL4 CL3 CL6 . . . . -93.0(19) no
CL1 CL4 CL3 CL6 . . . . -63.1(17) no
CL1 CL4 CL3 C76 . . . . -57.9(21) no
CL1 CL4 CL5 CL2 . . . . 0.2(11) no
CL1 CL4 CL5 CL3 . . . . -97.7(38) no
CL1 CL4 CL5 C76 . . . . -17.3(57) no
CL1 CL4 CL6 CL3 . . . . 107.2(21) no
CL1 CL4 CL6 CL3 . . . . -34.2(23) no
CL1 CL4 CL6 CL4 . . . . -0.1(27) no
CL1 CL4 CL6 CL6 . . . . -0.1(27) no
CL1 CL4 CL6 C76 . . . . -1.4(26) no
CL1 CL4 CL6 C76 . . . . 1.6(64) no
CL1 CL4 CL6 CL3 . . . . 120.2(21) no
CL1 CL4 CL6 CL3 . . . . -113.8(22) no
CL1 CL4 CL6 CL4 . . . . 179.9(27) no
CL1 CL4 CL6 CL6 . . . . 179.9(27) no
CL1 CL4 CL6 C76 . . . . -7(16) no
CL1 CL4 CL6 C76 . . . . 179.2(21) no
CL1 CL4 C76 CL2 . . . . 0.2(8) no
CL1 CL4 C76 CL3 . . . . 121.5(16) no
CL1 CL4 C76 CL5 . . . . 12.4(41) no
CL1 CL4 C76 CL6 . . . . 178.5(27) no
CL1 CL4 C76 CL6 . . . . 173(17) no
CL1 CL5 CL2 CL4 . . . . 178(17) no
CL1 CL5 CL2 C76 . . . . 166(18) no
CL1 CL5 CL3 CL4 . . . . -105.2(47) no
CL1 CL5 CL3 CL6 . . . . -61.3(17) no
CL1 CL5 CL3 CL6 . . . . -36.4(14) no
CL1 CL5 CL3 C76 . . . . -46.8(17) no
CL1 CL5 CL4 CL2 . . . . -0.2(11) no
CL1 CL5 CL4 CL3 . . . . 97.7(38) no
CL1 CL5 CL4 CL6 . . . . 30.4(80) no
CL1 CL5 CL4 CL6 . . . . 19.7(47) no
CL1 CL5 CL4 C76 . . . . 17.3(57) no
CL1 CL5 C76 CL2 . . . . -0.8(10) no
CL1 CL5 C76 CL3 . . . . 138.9(14) no
CL1 CL5 C76 CL4 . . . . -164.8(50) no
CL1 CL5 C76 CL6 . . . . 172.9(37) no
CL1 CL5 C76 CL6 . . . . 26.6(67) no
CL2 CL1 CL4 CL3 . . . . -106(47) no
CL2 CL1 CL4 CL5 . . . . -6(47) no
CL2 CL1 CL4 CL6 . . . . -167(48) no
CL2 CL1 CL4 CL6 . . . . -168(48) no
CL2 CL1 CL4 C76 . . . . -168(48) no
CL2 CL1 CL5 CL3 . . . . 48(17) no
CL2 CL1 CL5 CL4 . . . . 2(17) no
CL2 CL1 CL5 C76 . . . . 14(17) no
CL2 CL4 CL1 CL5 . . . . 6(47) no
CL2 CL4 CL3 CL5 . . . . 44.1(30) no
CL2 CL4 CL3 CL6 . . . . -94.0(22) no
CL2 CL4 CL3 CL6 . . . . -64.1(20) no
CL2 CL4 CL3 C76 . . . . -58.9(21) no
CL2 CL4 CL5 CL3 . . . . -97.8(39) no
CL2 CL4 CL5 C76 . . . . -17.5(56) no
CL2 CL4 CL6 CL3 . . . . 107.0(22) no
CL2 CL4 CL6 CL3 . . . . -34.4(24) no
CL2 CL4 CL6 CL4 . . . . -0.3(28) no
CL2 CL4 CL6 CL6 . . . . -0.3(28) no
CL2 CL4 CL6 C76 . . . . -1.6(26) no
CL2 CL4 CL6 C76 . . . . 1.4(65) no
CL2 CL4 CL6 CL3 . . . . 120.0(22) no
CL2 CL4 CL6 CL3 . . . . -114.0(22) no
CL2 CL4 CL6 CL4 . . . . 179.7(28) no
CL2 CL4 CL6 CL6 . . . . 179.7(28) no
CL2 CL4 CL6 C76 . . . . -7(16) no
CL2 CL4 CL6 C76 . . . . 179.0(21) no
CL2 CL4 C76 CL3 . . . . 121.3(17) no
CL2 CL4 C76 CL5 . . . . 12.2(40) no
CL2 CL4 C76 CL6 . . . . 178.3(27) no
CL2 CL4 C76 CL6 . . . . 172(17) no
CL2 CL5 CL1 CL4 . . . . -2(17) no
CL2 CL5 CL3 CL4 . . . . -102.4(47) no
CL2 CL5 CL3 CL6 . . . . -58.6(19) no
CL2 CL5 CL3 CL6 . . . . -33.7(17) no
CL2 CL5 CL3 C76 . . . . -44.0(19) no
CL2 CL5 CL4 CL3 . . . . 97.8(39) no
CL2 CL5 CL4 CL6 . . . . 30.6(79) no
CL2 CL5 CL4 CL6 . . . . 19.8(47) no
CL2 CL5 CL4 C76 . . . . 17.5(56) no
CL2 CL5 C76 CL3 . . . . 139.8(16) no
CL2 CL5 C76 CL4 . . . . -164.0(52) no
CL2 CL5 C76 CL6 . . . . 173.7(38) no
CL2 CL5 C76 CL6 . . . . 27.4(67) no
CL2 C76 CL3 CL4 . . . . 62.5(26) no
CL2 C76 CL3 CL5 . . . . 30.9(13) no
CL2 C76 CL3 CL6 . . . . -168.1(26) no
CL2 C76 CL3 CL6 . . . . -127.9(32) no
CL2 C76 CL4 CL3 . . . . -121.3(17) no
CL2 C76 CL4 CL5 . . . . -12.2(40) no
CL2 C76 CL4 CL6 . . . . -178.3(27) no
CL2 C76 CL4 CL6 . . . . -172(17) no
CL2 C76 CL5 CL3 . . . . -139.8(16) no
CL2 C76 CL5 CL4 . . . . 164.0(52) no
CL2 C76 CL6 CL3 . . . . 128.5(86) no
CL2 C76 CL6 CL3 . . . . -32.4(87) no
CL2 C76 CL6 CL4 . . . . 173(11) no
CL2 C76 CL6 CL4 . . . . -5.9(96) no
CL2 C76 CL6 CL6 . . . . -5.1(89) no
CL2 C76 CL6 C76 . . . . -5.1(89) no
CL2 C76 CL6 CL3 . . . . 126.0(29) no
CL2 C76 CL6 CL3 . . . . -107.6(34) no
CL2 C76 CL6 CL4 . . . . 172(18) no
CL2 C76 CL6 CL4 . . . . -179.5(47) no
CL2 C76 CL6 CL6 . . . . 178.6(24) no
CL2 C76 CL6 C76 . . . . 178.6(24) no
CL3 CL4 CL1 CL5 . . . . -99.9(49) no
CL3 CL4 CL2 CL5 . . . . -99.5(49) no
CL3 CL4 CL2 C76 . . . . 62.6(27) no
CL3 CL4 CL5 C76 . . . . 80.3(42) no
CL3 CL4 CL6 CL4 . . . . -107.3(28) no
CL3 CL4 CL6 CL6 . . . . -107.3(28) no
CL3 CL4 CL6 C76 . . . . -108.6(37) no
CL3 CL4 CL6 C76 . . . . -105.6(58) no
CL3 CL4 CL6 CL4 . . . . 59.7(27) no
CL3 CL4 CL6 CL6 . . . . 59.7(27) no
CL3 CL4 CL6 C76 . . . . -127(17) no
CL3 CL4 CL6 C76 . . . . 58.9(28) no
CL3 CL4 C76 CL5 . . . . -109.1(46) no
CL3 CL4 C76 CL6 . . . . 57.0(29) no
CL3 CL4 C76 CL6 . . . . 51(17) no
CL3 CL5 CL1 CL4 . . . . 45.6(35) no
CL3 CL5 CL2 CL4 . . . . 44.5(34) no
CL3 CL5 CL2 C76 . . . . 32.8(14) no
CL3 CL5 CL4 CL6 . . . . -67.3(54) no
CL3 CL5 CL4 CL6 . . . . -78.0(35) no
CL3 CL5 CL4 C76 . . . . -80.3(42) no
CL3 CL5 C76 CL4 . . . . 56.2(43) no
CL3 CL5 C76 CL6 . . . . 34.0(33) no
CL3 CL5 C76 CL6 . . . . -112.3(68) no
CL3 CL6 CL3 CL4 . . . . 100.4(33) no
CL3 CL6 CL3 CL5 . . . . 126.7(28) no
CL3 CL6 CL3 CL6 . . . . 0.0000 no
CL3 CL6 CL3 C76 . . . . 108.4(34) no
CL3 CL6 CL4 CL5 . . . . 87.0(66) no
CL3 CL6 CL4 CL6 . . . . 107.3(28) no
CL3 CL6 CL4 C76 . . . . 108.6(37) no
CL3 CL6 CL4 CL5 . . . . 127.3(39) no
CL3 CL6 CL4 CL6 . . . . -66.2(26) no
CL3 CL6 CL4 C76 . . . . 107(17) no
CL3 CL6 CL6 CL3 . . . . 180.0000 no
CL3 CL6 CL6 CL4 . . . . -34.7(13) no
CL3 CL6 CL6 CL4 . . . . 145.3(13) no
CL3 CL6 CL6 C76 . . . . -35.4(18) no
CL3 CL6 CL6 C76 . . . . 144.6(18) no
CL3 CL6 C76 CL4 . . . . -44.9(27) no
CL3 CL6 C76 CL5 . . . . -32.3(31) no
CL3 CL6 C76 CL6 . . . . 133.6(26) no
CL3 CL6 C76 CL4 . . . . -81(17) no
CL3 CL6 C76 CL5 . . . . 129.6(54) no
CL3 CL6 C76 CL6 . . . . -73.8(35) no
CL3 CL6 CL3 CL4 . . . . -75.3(31) no
CL3 CL6 CL3 CL5 . . . . -56.4(29) no
CL3 CL6 CL3 CL6 . . . . 0.00000(10) no
CL3 CL6 CL3 C76 . . . . -39.4(23) no
CL3 CL6 CL4 CL5 . . . . 106.8(45) no
CL3 CL6 CL4 CL6 . . . . -59.7(27) no
CL3 CL6 CL4 C76 . . . . 127(17) no
CL3 CL6 CL4 CL5 . . . . 54.4(71) no
CL3 CL6 CL4 CL6 . . . . 34.1(16) no
CL3 CL6 CL4 C76 . . . . 32.8(36) no
CL3 CL6 CL6 CL3 . . . . -180.0000 no
CL3 CL6 CL6 CL4 . . . . 34.7(13) no
CL3 CL6 CL6 CL4 . . . . -145.3(13) no
CL3 CL6 CL6 C76 . . . . 35.4(18) no
CL3 CL6 CL6 C76 . . . . -144.6(18) no
CL3 CL6 C76 CL4 . . . . -46(16) no
CL3 CL6 C76 CL5 . . . . 104.0(69) no
CL3 CL6 C76 CL6 . . . . -52.6(29) no
CL3 CL6 C76 CL4 . . . . -154.3(29) no
CL3 CL6 C76 CL5 . . . . -166.9(31) no
CL3 CL6 C76 CL6 . . . . 27.3(16) no
CL3 C76 CL2 CL4 . . . . -48.4(21) no
CL3 C76 CL2 CL5 . . . . -40.0(18) no
CL3 C76 CL4 CL5 . . . . 109.1(46) no
CL3 C76 CL4 CL6 . . . . -57.0(29) no
CL3 C76 CL4 CL6 . . . . -51(17) no
CL3 C76 CL5 CL4 . . . . -56.2(43) no
CL3 C76 CL6 CL4 . . . . 44.9(27) no
CL3 C76 CL6 CL4 . . . . -134.3(18) no
CL3 C76 CL6 CL6 . . . . -133.6(26) no
CL3 C76 CL6 C76 . . . . -133.6(26) no
CL3 C76 CL6 CL4 . . . . 46(16) no
CL3 C76 CL6 CL4 . . . . 54.4(65) no
CL3 C76 CL6 CL6 . . . . 52.6(29) no
CL3 C76 CL6 C76 . . . . 52.6(29) no
CL4 CL1 CL2 CL5 . . . . 171(63) no
CL4 CL1 CL2 C76 . . . . 10(41) no
CL4 CL1 CL5 C76 . . . . 11.4(38) no
CL4 CL2 CL1 CL5 . . . . -171(63) no
CL4 CL2 CL5 C76 . . . . 11.7(38) no
CL4 CL2 C76 CL5 . . . . -8.4(27) no
CL4 CL2 C76 CL6 . . . . -173.9(98) no
CL4 CL2 C76 CL6 . . . . -178.3(37) no
CL4 CL3 CL5 C76 . . . . -58.4(41) no
CL4 CL3 CL6 CL6 . . . . 75.3(31) no
CL4 CL3 CL6 C76 . . . . 35.9(23) no
CL4 CL3 CL6 C76 . . . . 138.9(42) no
CL4 CL3 CL6 CL6 . . . . -100.4(33) no
CL4 CL3 CL6 C76 . . . . 8.0(33) no
CL4 CL3 CL6 C76 . . . . -131.3(26) no
CL4 CL3 C76 CL5 . . . . 31.6(25) no
CL4 CL3 C76 CL6 . . . . -129.4(34) no
CL4 CL3 C76 CL6 . . . . -169.7(43) no
CL4 CL5 CL2 C76 . . . . -11.7(38) no
CL4 CL5 CL3 CL6 . . . . 43.8(45) no
CL4 CL5 CL3 CL6 . . . . 68.7(44) no
CL4 CL5 CL3 C76 . . . . 58.4(41) no
CL4 CL5 C76 CL6 . . . . -22.3(55) no
CL4 CL5 C76 CL6 . . . . -168.5(86) no
CL4 CL6 CL3 CL5 . . . . -18.9(19) no
CL4 CL6 CL3 CL6 . . . . -75.3(31) no
CL4 CL6 CL3 C76 . . . . -35.9(23) no
CL4 CL6 CL3 CL5 . . . . 173.3(20) no
CL4 CL6 CL3 CL6 . . . . 46.6(24) no
CL4 CL6 CL3 C76 . . . . 155.0(35) no
CL4 CL6 CL4 CL5 . . . . -166.5(48) no
CL4 CL6 CL4 CL6 . . . . 0.0000 no
CL4 CL6 CL4 C76 . . . . 173(18) no
CL4 CL6 CL6 CL4 . . . . 180.0000 no
CL4 CL6 CL6 C76 . . . . -0.7(19) no
CL4 CL6 CL6 C76 . . . . 179.3(19) no
CL4 CL6 C76 CL5 . . . . 12.6(31) no
CL4 CL6 C76 CL6 . . . . 178.5(39) no
CL4 CL6 C76 CL5 . . . . -158.4(54) no
CL4 CL6 C76 CL6 . . . . -1.8(47) no
CL4 CL6 CL3 CL5 . . . . -26.3(18) no
CL4 CL6 CL3 CL6 . . . . 100.4(33) no
CL4 CL6 CL3 C76 . . . . -8.0(33) no
CL4 CL6 CL3 CL5 . . . . -111.0(22) no
CL4 CL6 CL3 CL6 . . . . -54.6(23) no
CL4 CL6 CL3 C76 . . . . -93.9(25) no
CL4 CL6 CL4 CL5 . . . . 20.3(72) no
CL4 CL6 CL4 CL6 . . . . 0.0000 no
CL4 CL6 CL4 C76 . . . . -1.3(34) no
CL4 CL6 CL6 CL4 . . . . -180.0000 no
CL4 CL6 CL6 C76 . . . . 0.7(19) no
CL4 CL6 CL6 C76 . . . . -179.3(19) no
CL4 CL6 C76 CL5 . . . . 150(21) no
CL4 CL6 C76 CL6 . . . . -7(17) no
CL4 CL6 C76 CL5 . . . . 166.6(29) no
CL4 CL6 C76 CL6 . . . . 0.8(19) no
CL4 C76 CL2 CL5 . . . . 8.4(27) no
CL4 C76 CL3 CL5 . . . . -31.6(25) no
CL4 C76 CL3 CL6 . . . . 129.4(34) no
CL4 C76 CL3 CL6 . . . . 169.7(43) no
CL4 C76 CL6 CL6 . . . . -178.5(39) no
CL4 C76 CL6 C76 . . . . -178.5(39) no
CL4 C76 CL6 CL6 . . . . 7(17) no
CL4 C76 CL6 C76 . . . . 7(17) no
CL5 CL1 CL2 C76 . . . . -161(23) no
CL5 CL1 CL4 CL6 . . . . -161.2(51) no
CL5 CL1 CL4 CL6 . . . . -161.2(46) no
CL5 CL1 CL4 C76 . . . . -162.1(59) no
CL5 CL2 CL4 CL6 . . . . -161.0(51) no
CL5 CL2 CL4 CL6 . . . . -161.2(46) no
CL5 CL2 CL4 C76 . . . . -162.1(58) no
CL5 CL2 C76 CL6 . . . . -165.5(86) no
CL5 CL2 C76 CL6 . . . . -169.9(24) no
CL5 CL3 CL4 CL6 . . . . 138.0(42) no
CL5 CL3 CL4 CL6 . . . . 108.2(41) no
CL5 CL3 CL4 C76 . . . . 103.0(46) no
CL5 CL3 CL6 CL6 . . . . 56.4(29) no
CL5 CL3 CL6 C76 . . . . 17.0(20) no
CL5 CL3 CL6 C76 . . . . 120.0(38) no
CL5 CL3 CL6 CL6 . . . . -126.7(28) no
CL5 CL3 CL6 C76 . . . . -18.3(26) no
CL5 CL3 CL6 C76 . . . . -157.6(19) no
CL5 CL3 C76 CL6 . . . . -161.0(22) no
CL5 CL3 C76 CL6 . . . . 158.7(30) no
CL5 CL4 CL2 C76 . . . . 162.1(58) no
CL5 CL4 CL3 CL6 . . . . -138.0(42) no
CL5 CL4 CL3 CL6 . . . . -108.2(41) no
CL5 CL4 CL3 C76 . . . . -103.0(46) no
CL5 CL4 CL6 CL6 . . . . -20.3(72) no
CL5 CL4 CL6 C76 . . . . -21.6(53) no
CL5 CL4 CL6 C76 . . . . -19(11) no
CL5 CL4 CL6 CL6 . . . . 166.5(48) no
CL5 CL4 CL6 C76 . . . . -21(15) no
CL5 CL4 CL6 C76 . . . . 165.7(37) no
CL5 CL4 C76 CL6 . . . . 166.2(34) no
CL5 CL4 C76 CL6 . . . . 160(14) no
CL5 C76 CL3 CL6 . . . . 161.0(22) no
CL5 C76 CL3 CL6 . . . . -158.7(30) no
CL5 C76 CL4 CL6 . . . . -166.2(34) no
CL5 C76 CL4 CL6 . . . . -160(14) no
CL5 C76 CL6 CL6 . . . . -165.9(39) no
CL5 C76 CL6 C76 . . . . -165.9(39) no
CL5 C76 CL6 CL6 . . . . 156.6(64) no
CL5 C76 CL6 C76 . . . . 156.6(64) no
CL6 CL3 CL4 C76 . . . . -35.1(22) no
CL6 CL3 CL5 C76 . . . . -14.5(17) no
CL6 CL3 CL6 CL3 . . . . 0.0000 no
CL6 CL3 CL6 C76 . . . . 108.4(34) no
CL6 CL3 CL6 C76 . . . . -30.9(19) no
CL6 CL3 CL4 C76 . . . . 5.2(22) no
CL6 CL3 CL5 C76 . . . . -10.4(14) no
CL6 CL3 CL6 CL3 . . . . 0.00000(10) no
CL6 CL3 CL6 C76 . . . . -63.6(32) no
CL6 CL3 CL6 C76 . . . . 39.4(23) no
CL6 CL4 CL2 C76 . . . . 1.0(16) no
CL6 CL4 CL3 C76 . . . . 35.1(22) no
CL6 CL4 CL5 C76 . . . . 13.1(32) no
CL6 CL4 CL6 CL4 . . . . 0.00000(10) no
CL6 CL4 CL6 C76 . . . . 173(18) no
CL6 CL4 CL6 C76 . . . . -0.8(19) no
CL6 CL4 CL2 C76 . . . . -0.9(19) no
CL6 CL4 CL3 C76 . . . . -5.2(22) no
CL6 CL4 CL5 C76 . . . . -2.3(17) no
CL6 CL4 CL6 CL4 . . . . 0.0000 no
CL6 CL4 CL6 C76 . . . . -1.7(43) no
CL6 CL4 CL6 C76 . . . . 1.3(34) no
CL6 CL6 CL3 C76 . . . . -108.4(34) no
CL6 CL6 CL3 C76 . . . . -39.4(23) no
CL6 CL6 CL4 C76 . . . . -173(18) no
CL6 CL6 CL4 C76 . . . . -1.3(34) no
CL6 C76 CL6 C76 . . . . 0.0000 no
CL6 C76 CL6 C76 . . . . 0.0000 no
S1 ZN1 S2 C38 . . . . 127.1(2) no
S1 ZN1 N4 C24 . . . . -168.0(4) no
S1 ZN1 N4 C37 . . . . -11.0(4) no
S1 ZN2 S2 C38 . . . . -137.6(2) no
S1 ZN2 N8 C59 . . . . 121.1(4) no
S1 ZN2 N8 C68 . . . . -24.8(5) no
S1 C1 C4 O1 . . . . 54.1(5) no
S1 C1 C4 C6 . . . . 168.6(4) no
S1 C1 C4 C37 . . . . -73.1(5) no
S2 ZN1 S1 C1 . . . . 84.3(2) no
S2 ZN1 N4 C24 . . . . 93.2(4) no
S2 ZN1 N4 C37 . . . . -109.7(4) no
S2 ZN2 S1 C1 . . . . -78.7(2) no
S2 ZN2 N8 C59 . . . . 26.6(4) no
S2 ZN2 N8 C68 . . . . -119.2(4) no
S2 C38 C41 O2 . . . . -51.1(5) no
S2 C38 C41 C43 . . . . -171.8(4) no
S2 C38 C41 C59 . . . . 65.3(5) no
O1 C4 C1 C2 . . . . 179.1(4) no
O1 C4 C1 C3 . . . . -60.5(5) no
O1 C4 C6 N1 . . . . 15.9(7) no
O1 C4 C6 N2 . . . . -161.8(5) no
O1 C4 C37 N3 . . . . 74.2(6) no
O1 C4 C37 N4 . . . . -104.0(6) no
O2 C41 C38 C39 . . . . 63.3(5) no
O2 C41 C38 C40 . . . . -170.8(4) no
O2 C41 C43 N5 . . . . 73.4(7) no
O2 C41 C43 N6 . . . . -108.2(6) no
O2 C41 C59 N7 . . . . -159.5(5) no
O2 C41 C59 N8 . . . . 22.4(7) no
N1 C6 N2 C9 . . . . -0.5(6) no
N1 C6 C4 C1 . . . . -101.8(6) no
N1 C6 C4 C37 . . . . 134.0(5) no
N1 C8 C9 N2 . . . . -0.5(6) no
N1 C8 C9 C16 . . . . -178.8(5) no
N1 C8 C10 C11 . . . . 66.4(8) no
N1 C8 C10 C15 . . . . -117.9(6) no
N2 C6 N1 C7 . . . . 177.4(6) no
N2 C6 N1 C8 . . . . 0.2(6) no
N2 C6 C4 C1 . . . . 80.5(6) no
N2 C6 C4 C37 . . . . -43.7(7) no
N2 C9 C8 C10 . . . . -179.0(6) no
N2 C9 C16 C17 . . . . -157.9(5) no
N2 C9 C16 C21 . . . . 20.1(8) no
N3 C23 C24 N4 . . . . -0.9(6) no
N3 C23 C24 C31 . . . . 177.8(5) no
N3 C23 C30 C25 . . . . -77.0(8) no
N3 C23 C30 C29 . . . . 103.7(7) no
N3 C37 N4 C24 . . . . 1.8(6) no
N3 C37 C4 C1 . . . . -158.7(5) no
N3 C37 C4 C6 . . . . -40.6(7) no
N4 ZN1 S1 C1 . . . . -27.7(2) no
N4 ZN1 S2 C38 . . . . -131.2(2) no
N4 C24 C23 C30 . . . . 173.0(6) no
N4 C24 C31 C32 . . . . 142.0(6) no
N4 C24 C31 C36 . . . . -37.4(8) no
N4 C37 N3 C22 . . . . 173.9(5) no
N4 C37 N3 C23 . . . . -2.4(6) no
N4 C37 C4 C1 . . . . 23.1(8) no
N4 C37 C4 C6 . . . . 141.3(5) no
N5 C43 N6 C52 . . . . -0.8(7) no
N5 C43 C41 C38 . . . . -170.5(5) no
N5 C43 C41 C59 . . . . -47.8(7) no
N5 C45 C46 C47 . . . . 81.1(7) no
N5 C45 C46 C51 . . . . -98.8(7) no
N5 C45 C52 N6 . . . . 0.5(7) no
N5 C45 C52 C53 . . . . 178.3(6) no
N6 C43 N5 C44 . . . . -179.4(6) no
N6 C43 N5 C45 . . . . 1.1(6) no
N6 C43 C41 C38 . . . . 7.9(8) no
N6 C43 C41 C59 . . . . 130.6(6) no
N6 C52 C45 C46 . . . . -173.7(6) no
N6 C52 C53 C54 . . . . -168.3(5) no
N6 C52 C53 C58 . . . . 12.1(9) no
N7 C59 N8 C68 . . . . 0.5(6) no
N7 C59 C41 C38 . . . . 87.8(6) no
N7 C59 C41 C43 . . . . -37.0(7) no
N7 C61 C62 C63 . . . . 112.1(8) no
N7 C61 C62 C67 . . . . -69.8(8) no
N7 C61 C68 N8 . . . . -0.6(6) no
N7 C61 C68 C69 . . . . -178.7(6) no
N8 ZN2 S1 C1 . . . . -173.8(2) no
N8 ZN2 S2 C38 . . . . -32.7(2) no
N8 C59 N7 C60 . . . . -177.5(5) no
N8 C59 N7 C61 . . . . -0.9(6) no
N8 C59 C41 C38 . . . . -90.4(6) no
N8 C59 C41 C43 . . . . 144.8(5) no
N8 C68 C61 C62 . . . . 179.3(6) no
N8 C68 C69 C70 . . . . 140.0(6) no
N8 C68 C69 C74 . . . . -37.6(8) no
C1 C4 O1 C5 . . . . -99.9(5) no
C2 C1 C4 C6 . . . . -66.4(5) no
C2 C1 C4 C37 . . . . 51.9(6) no
C3 C1 C4 C6 . . . . 54.1(6) no
C3 C1 C4 C37 . . . . 172.3(4) no
C4 C6 N1 C7 . . . . -0.5(9) no
C4 C6 N1 C8 . . . . -177.6(5) no
C4 C6 N2 C9 . . . . 177.5(5) no
C4 C37 N3 C22 . . . . -4.6(9) no
C4 C37 N3 C23 . . . . 179.1(5) no
C4 C37 N4 C24 . . . . -179.8(5) no
C5 O1 C4 C6 . . . . 145.2(4) no
C5 O1 C4 C37 . . . . 30.0(6) no
C6 N1 C8 C9 . . . . 0.2(6) no
C6 N1 C8 C10 . . . . 178.8(5) no
C6 N2 C9 C8 . . . . 0.6(6) no
C6 N2 C9 C16 . . . . 179.2(5) no
C7 N1 C8 C9 . . . . -177.3(5) no
C7 N1 C8 C10 . . . . 1.4(8) no
C8 C9 C16 C17 . . . . 20.2(9) no
C8 C9 C16 C21 . . . . -161.8(6) no
C8 C10 C11 C12 . . . . 175.9(6) no
C8 C10 C15 C14 . . . . -175.1(6) no
C9 C8 C10 C11 . . . . -115.3(7) no
C9 C8 C10 C15 . . . . 60.4(9) no
C9 C16 C17 C18 . . . . 177.5(5) no
C9 C16 C21 C20 . . . . -176.6(5) no
C10 C8 C9 C16 . . . . 2.7(11) no
C10 C11 C12 C13 . . . . -1.4(10) no
C10 C15 C14 C13 . . . . -0.3(11) no
C11 C10 C15 C14 . . . . 0.7(9) no
C11 C12 C13 C14 . . . . 1.8(11) no
C12 C11 C10 C15 . . . . 0.2(9) no
C12 C13 C14 C15 . . . . -0.9(11) no
C16 C17 C18 C19 . . . . -0.4(10) no
C16 C21 C20 C19 . . . . -1.4(10) no
C17 C16 C21 C20 . . . . 1.5(9) no
C17 C18 C19 C20 . . . . 0.5(10) no
C18 C17 C16 C21 . . . . -0.6(9) no
C18 C19 C20 C21 . . . . 0.4(10) no
C22 N3 C23 C24 . . . . -174.6(5) no
C22 N3 C23 C30 . . . . 10.8(8) no
C23 C24 N4 C37 . . . . -0.5(6) no
C23 C24 C31 C32 . . . . -36.4(9) no
C23 C24 C31 C36 . . . . 144.2(6) no
C23 C30 C25 C26 . . . . 179.2(6) no
C23 C30 C29 C28 . . . . 179.1(6) no
C24 C23 N3 C37 . . . . 2.0(6) no
C24 C23 C30 C25 . . . . 110.0(8) no
C24 C23 C30 C29 . . . . -69.4(9) no
C24 C31 C32 C33 . . . . 179.0(6) no
C24 C31 C36 C35 . . . . -178.4(5) no
C25 C26 C27 C28 . . . . -0.1(11) no
C25 C30 C29 C28 . . . . -0.3(10) no
C26 C25 C30 C29 . . . . -1.4(9) no
C26 C27 C28 C29 . . . . -1.6(11) no
C27 C26 C25 C30 . . . . 1.6(10) no
C27 C28 C29 C30 . . . . 1.8(11) no
C30 C23 N3 C37 . . . . -172.6(5) no
C30 C23 C24 C31 . . . . -8.4(10) no
C31 C24 N4 C37 . . . . -179.2(5) no
C31 C32 C33 C34 . . . . 0.4(11) no
C31 C36 C35 C34 . . . . -1.6(9) no
C32 C31 C36 C35 . . . . 2.2(9) no
C32 C33 C34 C35 . . . . 0.2(11) no
C33 C32 C31 C36 . . . . -1.6(10) no
C33 C34 C35 C36 . . . . 0.4(10) no
C38 C41 O2 C42 . . . . -160.7(5) no
C39 C38 C41 C43 . . . . -57.3(6) no
C39 C38 C41 C59 . . . . 179.7(4) no
C40 C38 C41 C43 . . . . 68.5(6) no
C40 C38 C41 C59 . . . . -54.4(6) no
C41 C43 N5 C44 . . . . -0.8(9) no
C41 C43 N5 C45 . . . . 179.7(5) no
C41 C43 N6 C52 . . . . -179.4(5) no
C41 C59 N7 C60 . . . . 4.2(10) no
C41 C59 N7 C61 . . . . -179.2(5) no
C41 C59 N8 C68 . . . . 179.0(5) no
C42 O2 C41 C43 . . . . -38.9(8) no
C42 O2 C41 C59 . . . . 82.6(7) no
C43 N5 C45 C46 . . . . 174.2(5) no
C43 N5 C45 C52 . . . . -0.9(6) no
C43 N6 C52 C45 . . . . 0.2(7) no
C43 N6 C52 C53 . . . . -177.9(5) no
C44 N5 C45 C46 . . . . -5.3(8) no
C44 N5 C45 C52 . . . . 179.5(5) no
C45 C46 C47 C48 . . . . 179.8(6) no
C45 C46 C51 C50 . . . . -179.5(6) no
C45 C52 C53 C54 . . . . 14.0(10) no
C45 C52 C53 C58 . . . . -165.5(6) no
C46 C45 C52 C53 . . . . 4.1(12) no
C46 C47 C48 C49 . . . . -0.1(12) no
C46 C51 C50 C49 . . . . -0.4(11) no
C47 C46 C45 C52 . . . . -105.3(9) no
C47 C46 C51 C50 . . . . 0.6(10) no
C47 C48 C49 C50 . . . . 0.3(13) no
C48 C47 C46 C51 . . . . -0.3(10) no
C48 C49 C50 C51 . . . . -0.0(13) no
C51 C46 C45 C52 . . . . 74.8(9) no
C52 C53 C54 C55 . . . . -177.1(6) no
C52 C53 C58 C57 . . . . 179.4(6) no
C53 C54 C55 C56 . . . . -2.0(11) no
C53 C58 C57 C56 . . . . -2.7(10) no
C54 C53 C58 C57 . . . . -0.1(9) no
C54 C55 C56 C57 . . . . -1.0(11) no
C55 C54 C53 C58 . . . . 2.5(9) no
C55 C56 C57 C58 . . . . 3.3(10) no
C59 N7 C61 C62 . . . . -178.9(5) no
C59 N7 C61 C68 . . . . 0.9(6) no
C59 N8 C68 C61 . . . . 0.1(6) no
C59 N8 C68 C69 . . . . 178.3(5) no
C60 N7 C61 C62 . . . . -2.0(9) no
C60 N7 C61 C68 . . . . 177.9(5) no
C61 C62 C63 C64 . . . . 178.2(7) no
C61 C62 C67 C66 . . . . -178.6(6) no
C61 C68 C69 C70 . . . . -42.2(9) no
C61 C68 C69 C74 . . . . 140.2(7) no
C62 C61 C68 C69 . . . . 1.2(11) no
C62 C63 C64 C65 . . . . 0.7(14) no
C62 C67 C66 C65 . . . . 0.3(11) no
C63 C62 C61 C68 . . . . -67.8(9) no
C63 C62 C67 C66 . . . . -0.5(11) no
C63 C64 C65 C66 . . . . -0.9(15) no
C64 C63 C62 C67 . . . . -0.0(12) no
C64 C65 C66 C67 . . . . 0.3(13) no
C67 C62 C61 C68 . . . . 110.4(8) no
C68 C69 C70 C71 . . . . -179.7(6) no
C68 C69 C74 C73 . . . . 179.6(6) no
C69 C70 C71 C72 . . . . 0.3(11) no
C69 C74 C73 C72 . . . . -0.1(12) no
C70 C69 C74 C73 . . . . 1.9(10) no
C70 C71 C72 C73 . . . . 1.5(12) no
C71 C70 C69 C74 . . . . -2.0(9) no
C71 C72 C73 C74 . . . . -1.6(12) no
C76 CL6 CL6 C76 . . . . 180.0000 no
C76 CL6 C76 CL6 . . . . 0.0000 no
C76 CL6 CL6 C76 . . . . 180.0000 no
C76 CL6 C76 CL6 . . . . 0.0000 no
#------------------------------------------------------------------------------

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one
# structure analysis in the CIF.
#==============================================================================
#     End of CIF
#==============================================================================

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

data_2-SO42-
_database_code_depnum_ccdc_archive 'CCDC 2131471'
loop_
_audit_author_name
_audit_author_address
'Shaochuan Li'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2022-05-25 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_audit_creation_date             2022-05-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C88 H144 Ag2 N24 Pd4, 4(O)'
_chemical_formula_sum            'C88 H144 Ag2 N24 O4 Pd4'
_chemical_formula_weight         2243.60
_chemical_melting_point          ?
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'
Ag Ag -0.8971 1.1015 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.785(3)
_cell_length_b                   15.8669(17)
_cell_length_c                   20.292(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.536(4)
_cell_angle_gamma                90
_cell_volume                     6955.4(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.40
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.960
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5759
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1182 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.7724.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40648
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.107
_diffrn_ambient_temperature      149.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6243
_reflns_number_total             7261
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.716
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         7261
_refine_ls_number_restraints     295
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.1138
_refine_ls_restrained_S_all      1.580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1390P)²+235.0692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2942
_refine_ls_wR_factor_ref         0.3068
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N21-C24 = N21-C22 = N21-C23 = N8-C7 = N13-C14 = N25-C28 = N25-C27 = N25-C26
 1.47 with sigma of 0.005
 C24-N21
 2.45 with sigma of 0.01
 N25-C27 = N25-C26 = N25-C28 = N13-C14 = N8-C7 = N21-C24 = N21-C23 = N21-C22
 1.47 with sigma of 0.005
 C24-C24_$2 = C28_$1-C28_$3 = C24_$1-C24_$3 = C28-C28_$2
 1.53 with sigma of 0.005
 N25_$2-C27_$2 = N25_$2-C28_$2 = N25_$2-C26_$2 = N25-C26 = N25-C27 = N25-C28 =
 N21_$2-C24_$2 = N21-C24 = N21-C22 = N21-C23 = N21_$2-C23_$2 = N21_$2-C22_$2 =
 N21_$1-C23_$1 = N21_$1-C22_$1 = N21_$1-C24_$1 = N21_$3-C24_$3 = N21_$3-C22_$3 =
  N21_$3-C23_$3 = N25_$1-C28_$1 = N25_$1-C26_$1 = N25_$1-C27_$1 = N25_$3-C28_$3
 = N25_$3-C27_$3 = N25_$3-C26_$3 = N8_$1-C7_$1 = N13-C14 = N8-C7 = N13_$1-
 C14_$1 = N8_$3-C7_$3 = N13_$2-C14_$2 = N8_$2-C7_$2 = N13_$3-C14_$3
 1.46 with sigma of 0.005
 N21-C24 = N21-C23 = N21-C22 = N8-C7 = N8-C8 = N13-C14 = N13-C0AA = N25-C28 =
 N25-C27 = N25-C26
 1.465 with sigma of 0.005
 N21-C23 = N21-C22 = N21-C24 = N21_$2-C24_$2 = N21_$2-C23_$2 = N21_$2-C22_$2 =
 N21_$3-C23_$3 = N21_$3-C24_$3 = N21_$3-C22_$3 = N21_$1-C22_$1 = N21_$1-C24_$1 =
  N21_$1-C23_$1
 1.465 with sigma of 0.005
 C24_$3-C24_$1 = C24_$2-C24
 1.53 with sigma of 0.005
 N13-C0AA
 1.465 with sigma of 0.005
 N8-C7 = N8-C8 = N13-C0AA = N13-C14
 1.465 with sigma of 0.005
 N25-C26 = N25-C27 = N25-C28 = N21-C24 = N21-C23 = N21-C22
 1.465 with sigma of 0.005
 C8-C0AA
 1.53 with sigma of 0.005
 N8_$2-C10_$2 = N13_$3-C2AA_$2 = N8_$3-C10_$3 = N13_$2-C2AA_$3 = N13_$1-C2AA =
 N8-C10 = N13-C2AA_$1 = N8_$1-C10_$1
 1.465 with sigma of 0.005
 C2AA_$1-C10_$1 = C2AA-C10 = C2AA_$3-C10_$3 = C2AA_$2-C10_$2
 1.53 with sigma of 0.005
 C10_$1-C8_$1
 2.35 with sigma of 0.01
 C8-C10
 2.35 with sigma of 0.01
 C0AA-C2AA_$1
 2.35 with sigma of 0.01
 C0AA_$1-C2AA
 2.35 with sigma of 0.01
 C10_$3-C8_$3
 2.35 with sigma of 0.01
 C8_$2-C10_$2
 2.35 with sigma of 0.01
 C2AA_$2-C0AA_$3
 2.35 with sigma of 0.01
 C0AA_$2-C2AA_$3
 2.35 with sigma of 0.01
 C22-C23
 2.4 with sigma of 0.005
 C27-C28
 2.4 with sigma of 0.005
3. Rigid bond restraints
 C27, C28, C26, C22, C24, C23
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N21
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C22 \\sim C23 \\sim C27 \\sim C28 \\sim C26: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(N13)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N25) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C8) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N21) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2AA)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq,
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C0AA) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C2AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C0AA)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C0AA)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C24(H24A,H24B), C28(H28A,H28B), C0AA(H0AA,H0AB),
 C8(H8A,H8B), C2AA(H2AA,H2AB), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C19(H19), C6(H6), C20(H20), C3(H3), C5(H5), C2(H2)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C23(H23B,H23A,H23C), C26(H26A,H26B,H26C), C22(H22A,H22B,
 H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Ag3 Ag 0.500000 0.75671(5) 0.500000 0.0349(3) Uani 1 2 d S TU P . .
Pd1 Pd 0.14532(5) 0.500000 0.19999(6) 0.0443(3) Uani 1 2 d S TU P . .
Pd2 Pd 0.32828(6) 0.500000 0.81429(6) 0.0449(3) Uani 1 2 d S TU P . .
N1 N 0.2100(4) 0.5878(5) 0.2524(4) 0.0447(18) Uani 1 1 d . U . . .
N18 N 0.3590(4) 0.5873(5) 0.7594(4) 0.0434(17) Uani 1 1 d . U . . .
N13 N 0.4577(4) 0.6784(4) 0.5824(4) 0.0484(19) Uani 1 1 d D U . . .
N8 N 0.4092(3) 0.6776(4) 0.4235(4) 0.050(2) Uani 1 1 d D U . . .
C7 C 0.3615(4) 0.7337(5) 0.3801(5) 0.045(2) Uani 1 1 d D U . . .
H7A H 0.379800 0.768377 0.351052 0.054 Uiso 1 1 calc R . . . .
H7B H 0.347665 0.772381 0.410502 0.054 Uiso 1 1 calc R . . . .
C14 C 0.4338(5) 0.7336(5) 0.6257(5) 0.044(2) Uani 1 1 d D U . . .
H14A H 0.400539 0.769318 0.595259 0.052 Uiso 1 1 calc R . . . .
H14B H 0.467494 0.771368 0.652787 0.052 Uiso 1 1 calc R . . . .
C15 C 0.4086(5) 0.6856(6) 0.6754(5) 0.043(2) Uani 1 1 d . U . . .
C4 C 0.3058(4) 0.6874(6) 0.3332(5) 0.043(2) Uani 1 1 d . U . . .
C17 C 0.3236(5) 0.6145(7) 0.6986(6) 0.052(2) Uani 1 1 d . U . . .
H17 H 0.280830 0.600704 0.684805 0.063 Uiso 1 1 calc R . . . .
C16 C 0.3445(5) 0.6618(7) 0.6537(6) 0.050(2) Uani 1 1 d . U . . .
H16 H 0.317284 0.678234 0.609594 0.060 Uiso 1 1 calc R . . . .
N21 N 0.0839(4) 0.4103(5) 0.1467(5) 0.060(2) Uani 1 1 d D U . . .
C19 C 0.4209(5) 0.6127(7) 0.7828(6) 0.049(2) Uani 1 1 d . U . . .
H19 H 0.446684 0.596298 0.827728 0.058 Uiso 1 1 calc R . . . .
C6 C 0.2102(5) 0.6136(8) 0.3161(6) 0.056(2) Uani 1 1 d . U . . .
H6 H 0.177565 0.596804 0.332899 0.067 Uiso 1 1 calc R . . . .
C20 C 0.4446(5) 0.6610(7) 0.7414(6) 0.051(2) Uani 1 1 d . U . . .
H20 H 0.486750 0.678073 0.758277 0.061 Uiso 1 1 calc R . . . .
C3 C 0.3022(5) 0.6614(7) 0.2672(6) 0.055(3) Uani 1 1 d . U . . .
H3 H 0.333505 0.678424 0.248286 0.066 Uiso 1 1 calc R . . . .
C5 C 0.2562(5) 0.6629(8) 0.3563(6) 0.057(3) Uani 1 1 d . U . . .
H5 H 0.255011 0.681080 0.400413 0.068 Uiso 1 1 calc R . . . .
N25 N 0.2977(4) 0.5890(6) 0.8714(5) 0.067(2) Uani 1 1 d D U . . .
C2 C 0.2550(5) 0.6120(8) 0.2285(6) 0.054(2) Uani 1 1 d . U . . .
H2 H 0.254345 0.594501 0.183501 0.065 Uiso 1 1 calc R . . . .
C24 C 0.0268(5) 0.45181(8) 0.1018(7) 0.076(3) Uani 1 1 d D U . . .
H24A H -0.008351 0.432316 0.116580 0.091 Uiso 1 1 calc R . . . .
H24B H 0.019191 0.432316 0.053468 0.091 Uiso 1 1 calc R . . . .
C27 C 0.3491(6) 0.6365(11) 0.9187(8) 0.099(5) Uani 1 1 d D U . . .
H27A H 0.341710 0.644148 0.963318 0.148 Uiso 1 1 calc GR . . . .
H27B H 0.352169 0.691662 0.898383 0.148 Uiso 1 1 calc GR . . . .
H27C H 0.387782 0.605297 0.925993 0.148 Uiso 1 1 calc GR . . . .
C28 C 0.2619(6) 0.54815(11) 0.9109(8) 0.098(5) Uani 1 1 d D U . . .
H28A H 0.218487 0.567657 0.892057 0.117 Uiso 1 1 calc R . . . .
H28B H 0.278160 0.567657 0.959674 0.117 Uiso 1 1 calc R . . . .
C23 C 0.1064(10) 0.3730(12) 0.0932(9) 0.127(6) Uani 1 1 d D U . . .
H23B H 0.108180 0.416436 0.059507 0.190 Uiso 1 1 calc GR . . . .
H23A H 0.078225 0.327961 0.069230 0.190 Uiso 1 1 calc GR . . . .
H23C H 0.147889 0.349590 0.114920 0.190 Uiso 1 1 calc GR . . . .
C26 C 0.2553(9) 0.6497(12) 0.8261(9) 0.110(5) Uani 1 1 d D U . . .
H26A H 0.278980 0.690149 0.808098 0.164 Uiso 1 1 calc GR . . . .
H26B H 0.232700 0.679880 0.852634 0.164 Uiso 1 1 calc GR . . . .
H26C H 0.225866 0.619883 0.787220 0.164 Uiso 1 1 calc GR . . . .
C22 C 0.0699(11) 0.3436(10) 0.1892(9) 0.133(7) Uani 1 1 d D U . . .
H22A H 0.035239 0.309620 0.160531 0.200 Uiso 1 1 calc GR . . . .
H22B H 0.058746 0.368872 0.227632 0.200 Uiso 1 1 calc GR . . . .
H22C H 0.106367 0.307530 0.207903 0.200 Uiso 1 1 calc GR . . . .
C0AA C 0.4160(7) 0.6117(8) 0.5450(6) 0.094(4) Uani 1 1 d D U . . .
H0AA H 0.385663 0.599473 0.569451 0.112 Uiso 1 1 calc R . . . .
H0AB H 0.440354 0.559799 0.545899 0.112 Uiso 1 1 calc R . . . .
C8 C 0.3810(6) 0.6339(9) 0.4696(6) 0.098(4) Uani 1 1 d D U . . .
H8A H 0.364037 0.580327 0.446164 0.118 Uiso 1 1 calc R . . . .
H8B H 0.344975 0.668345 0.470382 0.118 Uiso 1 1 calc R . . . .
C2AA C 0.4890(5) 0.6363(10) 0.3684(7) 0.122(6) Uani 1 1 d D U . . .
H2AA H 0.504865 0.583792 0.353790 0.146 Uiso 1 1 calc R . . . .
H2AB H 0.475165 0.672802 0.326733 0.146 Uiso 1 1 calc R . . . .
C10 C 0.4309(7) 0.6120(8) 0.3861(8) 0.095(4) Uani 1 1 d D U . . .
H10A H 0.397362 0.598817 0.342474 0.114 Uiso 1 1 calc R . . . .
H10B H 0.439521 0.560154 0.414772 0.114 Uiso 1 1 calc R . . . .
O1 O 0.2855(8) 0.500000 0.8215(8) 0.082(4) Uani 1 2 d S TU P . .
O2 O 0.2550(7) 0.500000 0.1969(8) 0.085(4) Uani 1 2 d S TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag3 N13 2.509(8) 2_656 ?
Ag3 N13 2.509(8) . ?
Ag3 N8 2.495(7) 2_656 ?
Ag3 N8 2.495(7) . ?
Pd1 N1 2.061(8) 6_565 ?
Pd1 N1 2.061(8) . ?
Pd1 N21 2.047(9) 6_565 ?
Pd1 N21 2.047(9) . ?
Pd2 N18 2.036(9) . ?
Pd2 N18 2.036(8) 6_565 ?
Pd2 N25 2.082(10) . ?
Pd2 N25 2.082(10) 6_565 ?
N1 C6 1.355(14) . ?
N1 C2 1.322(15) . ?
N18 C17 1.313(14) . ?
N18 C19 1.396(13) . ?
N13 C14 1.4636(18) . ?
N13 C0AA 1.464(3) . ?
N13 C2AA 1.465(3) 2_656 ?
N8 C7 1.4641(18) . ?
N8 C8 1.465(4) . ?
N8 C10 1.464(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C4 1.512(12) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.516(13) . ?
C15 C16 1.435(15) . ?
C15 C20 1.385(15) . ?
C4 C3 1.379(16) . ?
C4 C5 1.409(16) . ?
C17 H17 0.9500 . ?
C17 C16 1.378(16) . ?
C16 H16 0.9500 . ?
N21 C24 1.4839(15) . ?
N21 C23 1.4647(15) . ?
N21 C22 1.4645(15) . ?
C19 H19 0.9500 . ?
C19 C20 1.370(15) . ?
C6 H6 0.9500 . ?
C6 C5 1.352(16) . ?
C20 H20 0.9500 . ?
C3 H3 0.9500 . ?
C3 C2 1.361(15) . ?
C5 H5 0.9500 . ?
N25 C27 1.4643(18) . ?
N25 C28 1.4638(18) . ?
N25 C26 1.4636(18) . ?
N25 O1 1.708(13) 6_565 ?
C2 H2 0.9500 . ?
C2 O2 1.889(13) 6_565 ?
C24 C24 1.529(3) 6_565 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C28 1.528(4) 6_565 ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C23 H23B 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C0AA H0AA 0.9900 . ?
C0AA H0AB 0.9900 . ?
C0AA C8 1.525(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C2AA H2AA 0.9900 . ?
C2AA H2AB 0.9900 . ?
C2AA C10 1.528(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O1 O1 0.00(4) 6_565 ?
O2 O2 0.00(3) 6_565 ?

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
N13 Ag3 N13 120.6(3) 2_656 . ?
N8 Ag3 N13 75.8(3) . 2_656 ?
N8 Ag3 N13 75.3(3) 2_656 2_656 ?
N8 Ag3 N13 75.3(3) . . ?
N8 Ag3 N13 75.8(3) 2_656 . ?
N8 Ag3 N8 119.6(3) . 2_656 ?
N1 Pd1 N1 85.1(5) . 6_565 ?
N21 Pd1 N1 93.4(3) . 6_565 ?
N21 Pd1 N1 93.4(3) 6_565 . ?
N21 Pd1 N1 177.6(4) 6_565 6_565 ?
N21 Pd1 N1 177.6(4) . . ?
N21 Pd1 N21 88.1(4) . 6_565 ?
N18 Pd2 N18 85.7(5) . 6_565 ?
N18 Pd2 N25 179.4(4) . 6_565 ?
N18 Pd2 N25 179.4(4) 6_565 . ?
N18 Pd2 N25 94.4(4) 6_565 6_565 ?
N18 Pd2 N25 94.4(4) . . ?
N25 Pd2 N25 85.4(5) . 6_565 ?
C6 N1 Pd1 118.8(8) . . ?
C2 N1 Pd1 121.2(8) . . ?
C2 N1 C6 119.6(10) . . ?
C17 N18 Pd2 121.4(8) . . ?
C17 N18 C19 118.5(9) . . ?
C19 N18 Pd2 119.7(7) . . ?
C14 N13 Ag3 113.5(5) . . ?
C14 N13 C0AA 116.1(10) . . ?
C14 N13 C2AA 104.5(9) . 2_656 ?
C0AA N13 Ag3 109.6(7) . . ?
C0AA N13 C2AA 106.6(4) . 2_656 ?
C2AA N13 Ag3 105.6(8) 2_656 . ?
C7 N8 Ag3 112.2(5) . . ?
C7 N8 C8 106.2(9) . . ?
C8 N8 Ag3 106.7(7) . . ?
C10 N8 Ag3 109.3(7) . . ?
C10 N8 C7 115.4(10) . . ?
C10 N8 C8 106.5(4) . . ?
N8 C7 H7A 108.9 . . ?
N8 C7 H7B 108.9 . . ?
N8 C7 C4 113.4(7) . . ?
H7A C7 H7B 107.7 . . ?
C4 C7 H7A 108.9 . . ?
C4 C7 H7B 108.9 . . ?
N13 C14 H14A 109.0 . . ?
N13 C14 H14B 109.0 . . ?
N13 C14 C15 113.0(7) . . ?
H14A C14 H14B 107.8 . . ?
C15 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
C16 C15 C14 119.5(10) . . ?
C20 C15 C14 123.5(10) . . ?
C20 C15 C16 117.0(9) . . ?
C3 C4 C7 122.4(10) . . ?
C3 C4 C5 115.7(9) . . ?
C5 C4 C7 121.8(10) . . ?
N18 C17 H17 117.9 . . ?
N18 C17 C16 124.1(11) . . ?
C16 C17 H17 117.9 . . ?
C15 C16 H16 120.9 . . ?
C17 C16 C15 118.2(10) . . ?
C17 C16 H16 120.9 . . ?
C24 N21 Pd1 109.5(5) . . ?
C23 N21 Pd1 109.4(10) . . ?
C23 N21 C24 99.8(12) . . ?
C22 N21 Pd1 115.6(10) . . ?
C22 N21 C24 111.7(12) . . ?
C22 N21 C23 109.7(4) . . ?
N18 C19 H19 119.8 . . ?
C20 C19 N18 120.3(10) . . ?
C20 C19 H19 119.8 . . ?
N1 C6 H6 119.4 . . ?
C5 C6 N1 121.1(12) . . ?
C5 C6 H6 119.4 . . ?
C15 C20 H20 119.2 . . ?
C19 C20 C15 121.5(10) . . ?
C19 C20 H20 119.2 . . ?
C4 C3 H3 119.2 . . ?
C2 C3 C4 121.7(11) . . ?
C2 C3 H3 119.2 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(11) . . ?
C6 C5 H5 119.7 . . ?
C27 N25 Pd2 112.0(9) . . ?
C27 N25 O1 139.3(12) . 6_565 ?
C28 N25 Pd2 110.3(7) . . ?
C28 N25 C27 109.7(4) . . ?
C28 N25 O1 86.8(9) . 6_565 ?
C26 N25 Pd2 111.6(9) . . ?
C26 N25 C27 107.7(14) . . ?
C26 N25 C28 105.3(12) . . ?
C26 N25 O1 102.8(11) . 6_565 ?
O1 N25 Pd2 29.5(6) 6_565 . ?
N1 C2 C3 121.2(11) . . ?
N1 C2 H2 119.4 . . ?
N1 C2 O2 86.3(9) . 6_565 ?
C3 C2 H2 119.4 . . ?
C3 C2 O2 130.7(11) . 6_565 ?
O2 C2 H2 53.2 6_565 . ?
N21 C24 C24 116.3(4) . 6_565 ?
N21 C24 H24A 108.2 . . ?
N21 C24 H24B 108.2 . . ?
C24 C24 H24A 108.2 6_565 . ?
C24 C24 H24B 108.2 6_565 . ?
H24A C24 H24B 107.4 . . ?
N25 C27 H27A 109.5 . . ?
N25 C27 H27B 109.5 . . ?
N25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N25 C28 C28 116.3(5) . 6_565 ?
N25 C28 H28A 108.2 . . ?
N25 C28 H28B 108.2 . . ?
C28 C28 H28A 108.2 6_565 . ?
C28 C28 H28B 108.2 6_565 . ?
H28A C28 H28B 107.4 . . ?
N21 C23 H23B 109.5 . . ?
N21 C23 H23A 109.5 . . ?
N21 C23 H23C 109.5 . . ?
H23B C23 H23A 109.5 . . ?
H23B C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
N25 C26 H26A 109.5 . . ?
N25 C26 H26B 109.5 . . ?
N25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N21 C22 H22A 109.5 . . ?
N21 C22 H22B 109.5 . . ?
N21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N13 C0AA H0AA 108.8 . . ?
N13 C0AA H0AB 108.8 . . ?
N13 C0AA C8 113.6(11) . . ?
H0AA C0AA H0AB 107.7 . . ?
C8 C0AA H0AA 108.8 . . ?
C8 C0AA H0AB 108.8 . . ?
N8 C8 C0AA 123.6(12) . . ?
N8 C8 H8A 106.4 . . ?
N8 C8 H8B 106.4 . . ?
C0AA C8 H8A 106.4 . . ?
C0AA C8 H8B 106.4 . . ?
H8A C8 H8B 106.5 . . ?
N13 C2AA H2AA 106.5 2_656 . ?
N13 C2AA H2AB 106.5 2_656 . ?
N13 C2AA C10 123.2(13) 2_656 . ?
H2AA C2AA H2AB 106.5 . . ?
C10 C2AA H2AA 106.5 . . ?
C10 C2AA H2AB 106.5 . . ?
N8 C10 C2AA 113.8(11) . . ?
N8 C10 H10A 108.8 . . ?
N8 C10 H10B 108.8 . . ?
C2AA C10 H10A 108.8 . . ?
C2AA C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.499 -0.463 -0.607 3187.0 1505.1 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-BF4
_database_code_depnum_ccdc_archive 'CCDC 2131470'
loop_
_audit_author_name
_audit_author_address
'Shaochuan Li'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2022-05-25 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_audit_creation_date             2022-03-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C88 H148 Ag2 N24 O2 Pd4, 2(F6 Si), 2(B F4)'
_chemical_formula_sum            'C88 H148 Ag2 B2 F20 N24 O2 Pd4 Si2'
_chemical_formula_weight         2673.44
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'C H O N Pd'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0147 0.0070 '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'
Ag Ag 0.0782 3.3823 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0070 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0583 0.0400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.0375 3.1039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2153 0.2529 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.5019(3)
_cell_length_b                   14.0260(3)
_cell_length_c                   20.0093(5)
_cell_angle_alpha                72.754(2)
_cell_angle_beta                 73.765(2)
_cell_angle_gamma                80.009(2)
_cell_volume                     3457.63(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    33626
_cell_measurement_temperature    105.1(2)
_cell_measurement_theta_max      60.6430
_cell_measurement_theta_min      2.0720
_shelx_estimated_absorpt_T_max   0.379
_shelx_estimated_absorpt_T_min   0.197
_exptl_absorpt_coefficient_mu    4.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46670
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         3.189
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105.1(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  70.00   0.50    0.05    --   -1.72  57.00 -60.00  172
  2  ω     33.00  58.00   0.50    0.05    --   -1.72  38.00 -30.00   50
  3  ω     33.00  61.00   0.50    0.05    --   -1.72  77.00  90.00   56
  4  ω     75.00 111.00   0.50    0.05    --   72.03 152.00 -16.00   72
  5  ω     82.00 122.00   0.50    0.05    --   72.03 121.00-176.00   80
  6  ω     57.00 143.00   0.50    0.05    --   72.03  57.00-180.00  172
  7  ω     58.00 101.00   0.50    0.05    --   72.03-125.00 -60.00   86
  8  ω     58.00  83.00   0.50    0.05    --   72.03-152.00 -59.00   50
  9  ω      5.00  63.00   0.50    0.05    --   72.03 -57.00 -60.00  116
 10  ω      0.00  95.00   0.50    0.05    --   72.03 -77.00 -60.00  190
 11  ω     19.00 100.00   0.50    0.05    --   72.03-121.00 100.00  162
 12  ω     41.00  66.00   0.50    0.05    --   72.03 -57.00 120.00   50
 13  ω     13.00  66.00   0.50    0.05    --   72.03 -57.00  90.00  106
 14  ω      1.00  27.00   0.50    0.05    --   72.03 -57.00 120.00   52
 15  ω     -1.00  85.00   0.50    0.05    --   72.03 -77.00  90.00  172
 16  ω      0.00  26.00   0.50    0.05    --   72.03 -19.00   0.00   52
 17  ω     -1.00  26.00   0.50    0.05    --   72.03 -19.00 -60.00   54
 18  ω     -1.00  61.00   0.50    0.05    --   72.03 -57.00-120.00  124
 19  ω      0.00  25.00   0.50    0.05    --   72.03 -19.00-120.00   50
 20  ω    -16.00  10.00   0.50    0.05    --   -1.72  77.00  90.00   52
 21  ω    -72.00   8.00   0.50    0.05    --   -1.72 -38.00 150.00  160
 22  ω    -43.00 -10.00   0.50    0.05    --  -75.46  38.00  30.00   66
 23  ω    -43.00  -6.00   0.50    0.05    --  -75.46  38.00 -60.00   74
 24  ω    -37.00 -12.00   0.50    0.05    --  -75.46  38.00-150.00   50
 25  ω    -26.00   0.00   0.50    0.05    --  -75.46  19.00-180.00   52
 26  ω    -63.00  -2.00   0.50    0.05    --  -75.46  57.00-150.00  122
 27  ω    -62.00 -21.00   0.50    0.05    --  -75.46  77.00   0.00   82
 28  ω    -26.00   0.00   0.50    0.05    --  -75.46  19.00 150.00   52
 29  ω   -115.00 -84.00   0.50    0.05    --  -75.46-121.00 100.00   62
 30  ω   -129.00 -53.00   0.50    0.05    --  -75.46 -77.00  30.00  152
 31  ω   -109.00 -84.00   0.50    0.05    --  -75.46-152.00 -59.00   50
 32  ω   -109.00 -33.00   0.50    0.05    --  -75.46 121.00-176.00  152
 33  ω   -130.00 -69.00   0.50    0.05    --  -75.46 152.00 -16.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0377489000
_diffrn_orient_matrix_UB_12      -0.0078401000
_diffrn_orient_matrix_UB_13      0.0567909000
_diffrn_orient_matrix_UB_21      0.0808683000
_diffrn_orient_matrix_UB_22      0.0484174000
_diffrn_orient_matrix_UB_23      -0.0439811000
_diffrn_orient_matrix_UB_31      -0.0530344000
_diffrn_orient_matrix_UB_32      0.0876797000
_diffrn_orient_matrix_UB_33      0.0076583000
_diffrn_oxdiff_digest_frames     
;
014a15a68038f3467a877aba0c691e0ac003114f387
;
_diffrn_oxdiff_digest_hkl        
;
01f7274b60d799f71e25286ae97fe4d9bf6365
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_source                   'micro-focus metaljet'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11075
_reflns_number_total             12164
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         3.395
_refine_diff_density_min         -2.193
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         12164
_refine_ls_number_restraints     196
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0800
_refine_ls_restrained_S_all      1.626
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1198P)²+32.2581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2111
_refine_ls_wR_factor_ref         0.2144
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C2BA-C1BA = C4-C3BA = C7-C3 = C9AA-C0BA
 1.53 with sigma of 0.005
 N11-C2BA = N11-C4 = N8-C3BA = N8-C3 = N17-C7 = N17-C9AA = N14-C0BA = N14-C1BA
 1.47 with sigma of 0.005
 N7_$1-C4AA_$1 = N4_$1-C7AA_$1 = N4_$1-C9_$1 = N4_$1-C5AA_$1 = N7_$1-C11_$1 =
 N7_$1-C10_$1 = N12_$1-C13_$1 = N15_$1-C14_$1 = N15_$1-C19_$1 = N15_$1-C18_$1 =
 N12_$1-C16_$1 = N12_$1-C17_$1 = N12-C13 = N12-C16 = N12-C17 = N15-C14 = N15-
 C18 = N15-C19 = N4-C7AA = N7-C4AA = N7-C10 = N7-C11 = N4-C9 = N4-C5AA = N11-
 C2BA = N11-C20 = N11-C4 = N8-C8AA = N8-C3BA = N8-C3 = N14-C27 = N14-C0BA = N14-
 C1BA = N17-C9AA = N17-C34 = N17-C7 = N8_$1-C3_$1 = N8_$1-C8AA_$1 = N8_$1-
 C3BA_$1 = N17_$1-C34_$1 = N17_$1-C9AA_$1 = N17_$1-C7_$1 = N14_$1-C1BA_$1 =
 N14_$1-C27_$1 = N14_$1-C0BA_$1 = N11_$1-C20_$1 = N11_$1-C4_$1 = N11_$1-C2BA_$1
 1.47 with sigma of 0.005
 C7AA-C4AA = C14-C13 = C7AA_$1-C4AA_$1 = C14_$1-C13_$1 = C7_$1-C3_$1 = C9AA_$1-
 C0BA_$1 = C4_$1-C3BA_$1 = C2BA_$1-C1BA_$1 = C7-C3 = C4-C3BA = C2BA-C1BA = C9AA-
 C0BA
 1.53 with sigma of 0.005
 N14-C27 = N8-C8AA = N8-C3BA = N8-C3 = N14-C1BA = N14-C0BA = N11-C20 = N11-C4 =
  N11-C2BA = N17-C34 = N17-C9AA = N17-C7 = N15-C19 = N15-C18 = N15-C14 = N12-
 C13 = N12-C16 = N12-C17 = N7-C4AA = N4-C7AA = N7-C11 = N7-C10 = N4-C5AA = N4-C9
 1.475 with sigma of 0.005
 H3A-H1BA
 2.45 with sigma of 0.005
 H4A-H9AA
 2.45 with sigma of 0.005
 H3A-H4A
 2.45 with sigma of 0.01
 H3A-H9AA
 2.45 with sigma of 0.01
 H1BA-H9AA
 2.45 with sigma of 0.01
 H1BA-H4A
 2.45 with sigma of 0.01
3. Rigid bond restraints
 C3BA, C4, C2BA, C1BA, C3, C7, C9AA, C0BA
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C2BA, C1BA, C0BA, C9AA, C7, C3, C3BA, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N14, N14, C1BA, C1BA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N17, N17, C9AA, C9AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N11, N11, C4, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N8, N8, C3, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C2BA, C1BA, C3, C7, N8, N14
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N11, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N17, C9AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C4 \\sim C3BA \\sim C7 \\sim C3 \\sim C2BA \\sim C1BA \\sim C0BA \\sim C9AA:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C3BA) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C9AA) \\sim Ueq, Uanis(C0BA) \\sim Ueq, Uanis(C1BA) \\sim Ueq,
Uanis(C2BA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Rotating group:
 O1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 C8AA(H8AA,H8AB), C27(H27A,H27B), C20(H20A,H20B), C34(H34A,H34B), C4AA(H4AA,
 H4AB), C13(H13A,H13B), C7AA(H7AA,H7AB), C14(H14A,H14B), C1BA(H1BA,H1BB),
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C9AA(H9AA,H9AB), C3BA(H3BA,H3BB),
 C2BA(H2BA,H2BB), C0BA(H0BA,H0BB)
5.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C32(H32), C33(H33), C1AA(H1AA), C30(H30), C26(H26), C29(H29),
 C23(H23), C22(H22), C6AA(H6AA), C2AA(H2AA), C38(H38), C35(H35), C25(H25),
 C36(H36), C39(H39)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C5AA(H5AA,H5AB,H5AC), C9(H9A,H9B,
 H9C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Ag3 Ag 0.35170(4) 0.74894(3) 0.57199(3) 0.01923(15) Uani 1 1 d . . . . .
Pd1 Pd 0.72908(4) 0.82381(3) 0.87506(3) 0.02011(15) Uani 1 1 d . . . . .
Pd2 Pd 1.01560(4) 0.69017(4) 0.27675(3) 0.02367(16) Uani 1 1 d . . . . .
Si7 Si 0.16713(19) 0.6485(2) 0.86679(13) 0.0410(6) Uani 1 1 d . . . . .
F3 F -0.0232(5) 0.8922(4) 0.5369(3) 0.0541(14) Uani 1 1 d . . . . .
N1 N 0.2658(5) 1.0577(4) 0.2143(3) 0.0219(12) Uani 1 1 d . . . . .
N31 N 0.6420(5) 0.7658(4) 0.8312(3) 0.0244(13) Uani 1 1 d . . . . .
F6 F 0.0054(6) 0.7473(4) 0.6195(3) 0.0598(16) Uani 1 1 d . . . . .
N24 N 0.0230(5) 1.1674(4) 0.7089(3) 0.0237(13) Uani 1 1 d . . . . .
N7 N 0.7284(4) 0.7004(4) 0.9638(3) 0.0260(13) Uani 1 1 d D . . . .
F9 F 0.1757(5) 0.6416(5) 0.7830(3) 0.0625(16) Uani 1 1 d . . . . .
N37 N 0.8755(5) 0.6597(4) 0.3462(3) 0.0275(13) Uani 1 1 d . . . . .
N12 N 1.1557(4) 0.7212(4) 0.2028(3) 0.0287(14) Uani 1 1 d D . . . .
N4 N 0.8155(4) 0.8850(4) 0.9203(3) 0.0289(14) Uani 1 1 d D . . . .
F4 F -0.0171(7) 0.7403(5) 0.5150(4) 0.084(2) Uani 1 1 d . . . . .
F8 F 0.2134(6) 0.7596(4) 0.8323(3) 0.0663(18) Uani 1 1 d . . . . .
N15 N 1.0537(4) 0.5451(4) 0.2658(3) 0.0306(14) Uani 1 1 d D . . . .
C0AA C 0.3413(6) 0.9065(5) 0.2815(4) 0.0252(15) Uani 1 1 d . . . . .
H0AA H 0.391773 0.852225 0.281714 0.030 Uiso 1 1 calc R . . . .
N14 N 0.4638(6) 0.7766(5) 0.6422(3) 0.0478(19) Uani 1 1 d D U . . .
N8 N 0.3325(5) 0.8707(4) 0.4568(3) 0.0377(15) Uani 1 1 d D U . . .
C3AA C 0.2687(5) 0.9135(5) 0.3452(4) 0.0215(14) Uani 1 1 d . . . . .
C32 C 0.5394(5) 0.7888(5) 0.8465(4) 0.0240(15) Uani 1 1 d . . . . .
H32 H 0.508259 0.822536 0.881879 0.029 Uiso 1 1 calc R . . . .
N11 N 0.2630(4) 0.9025(4) 0.6088(3) 0.0347(16) Uani 1 1 d D U . . .
C33 C 0.4784(6) 0.7627(5) 0.8099(4) 0.0238(15) Uani 1 1 d . . . . .
H33 H 0.406878 0.778060 0.821967 0.029 Uiso 1 1 calc R . . . .
C8AA C 0.2736(5) 0.8396(5) 0.4165(3) 0.0230(14) Uani 1 1 d D . . . .
H8AA H 0.203536 0.830733 0.445795 0.028 Uiso 1 1 calc R . . . .
H8AB H 0.305134 0.775313 0.408084 0.028 Uiso 1 1 calc R . . . .
C1AA C 0.3388(6) 0.9790(5) 0.2185(4) 0.0228(14) Uani 1 1 d . . . . .
H1AA H 0.389513 0.973665 0.177056 0.027 Uiso 1 1 calc R . . . .
C27 C 0.4599(5) 0.6974(4) 0.7099(3) 0.0229(14) Uani 1 1 d D . . . .
H27A H 0.485279 0.633562 0.698642 0.027 Uiso 1 1 calc R . . . .
H27B H 0.388291 0.693529 0.737184 0.027 Uiso 1 1 calc R . . . .
F5 F -0.1509(6) 0.7905(5) 0.5973(6) 0.096(3) Uani 1 1 d . . . . .
C28 C 0.5226(5) 0.7142(5) 0.7561(4) 0.0209(14) Uani 1 1 d . . . . .
N17 N 0.5297(5) 0.7484(4) 0.4951(4) 0.0394(18) Uani 1 1 d D U . . .
C21 C 0.1049(5) 0.9857(5) 0.6756(4) 0.0202(14) Uani 1 1 d . . . . .
C30 C 0.6863(6) 0.7160(5) 0.7817(4) 0.0246(15) Uani 1 1 d . . . . .
H30 H 0.757644 0.699123 0.772319 0.029 Uiso 1 1 calc R . . . .
C20 C 0.1571(4) 0.8914(5) 0.6542(4) 0.0223(14) Uani 1 1 d D . . . .
H20A H 0.159463 0.837551 0.697508 0.027 Uiso 1 1 calc R . . . .
H20B H 0.115921 0.872576 0.628306 0.027 Uiso 1 1 calc R . . . .
C26 C 0.0489(6) 1.0607(5) 0.6322(4) 0.0250(15) Uani 1 1 d . . . . .
H26 H 0.039241 1.051122 0.590514 0.030 Uiso 1 1 calc R . . . .
C34 C 0.5689(5) 0.6485(4) 0.4833(4) 0.0232(14) Uani 1 1 d D . . . .
H34A H 0.522654 0.628881 0.461417 0.028 Uiso 1 1 calc R . . . .
H34B H 0.567958 0.600339 0.529634 0.028 Uiso 1 1 calc R . . . .
C29 C 0.6301(6) 0.6886(5) 0.7436(4) 0.0235(14) Uani 1 1 d . . . . .
H29 H 0.663520 0.653094 0.709676 0.028 Uiso 1 1 calc R . . . .
C23 C 0.0752(6) 1.0967(5) 0.7522(4) 0.0268(15) Uani 1 1 d . . . . .
H23 H 0.084190 1.109639 0.793006 0.032 Uiso 1 1 calc R . . . .
C22 C 0.1153(6) 1.0067(6) 0.7377(4) 0.0265(15) Uani 1 1 d . . . . .
H22 H 0.149693 0.958946 0.769066 0.032 Uiso 1 1 calc R . . . .
C16 C 1.1363(7) 0.7771(6) 0.1321(3) 0.041(2) Uani 1 1 d D . . . .
H16A H 1.098963 0.738294 0.116892 0.061 Uiso 1 1 calc GR . . . .
H16B H 1.201149 0.789885 0.097409 0.061 Uiso 1 1 calc GR . . . .
H16C H 1.095999 0.839682 0.135792 0.061 Uiso 1 1 calc GR . . . .
C6AA C 0.1939(6) 1.0629(5) 0.2745(4) 0.0268(15) Uani 1 1 d . . . . .
H6AA H 0.141225 1.115316 0.271802 0.032 Uiso 1 1 calc R . . . .
F11 F 0.1596(7) 0.6555(8) 0.9501(3) 0.108(4) Uani 1 1 d . . . . .
C40 C 0.6778(6) 0.6446(5) 0.4356(4) 0.0238(15) Uani 1 1 d . . . . .
C10 C 0.7982(6) 0.6167(5) 0.9409(5) 0.0369(19) Uani 1 1 d D . . . .
H10A H 0.771230 0.595259 0.908713 0.055 Uiso 1 1 calc GR . . . .
H10B H 0.803063 0.561860 0.982478 0.055 Uiso 1 1 calc GR . . . .
H10C H 0.865725 0.638420 0.916641 0.055 Uiso 1 1 calc GR . . . .
C2AA C 0.1929(6) 0.9961(5) 0.3399(4) 0.0268(15) Uani 1 1 d . . . . .
H2AA H 0.142512 1.004975 0.380681 0.032 Uiso 1 1 calc R . . . .
C38 C 0.7928(6) 0.6724(6) 0.3186(4) 0.0331(17) Uani 1 1 d . . . . .
H38 H 0.802168 0.686929 0.268938 0.040 Uiso 1 1 calc R . . . .
C35 C 0.7635(6) 0.6285(6) 0.4634(4) 0.0297(16) Uani 1 1 d . . . . .
H35 H 0.755295 0.612068 0.513044 0.036 Uiso 1 1 calc R . . . .
F10 F 0.2881(7) 0.5968(7) 0.8629(6) 0.112(3) Uani 1 1 d . . . . .
C25 C 0.0084(6) 1.1483(5) 0.6518(4) 0.0260(15) Uani 1 1 d . . . . .
H25 H -0.030752 1.195975 0.623689 0.031 Uiso 1 1 calc R . . . .
C5AA C 0.9088(5) 0.9250(6) 0.8675(4) 0.0357(18) Uani 1 1 d D . . . .
H5AA H 0.948697 0.873593 0.845592 0.054 Uiso 1 1 calc GR . . . .
H5AB H 0.949937 0.946410 0.891492 0.054 Uiso 1 1 calc GR . . . .
H5AC H 0.888745 0.980979 0.830949 0.054 Uiso 1 1 calc GR . . . .
C36 C 0.8619(6) 0.6365(6) 0.4180(4) 0.0303(16) Uani 1 1 d . . . . .
H36 H 0.919080 0.625692 0.437487 0.036 Uiso 1 1 calc R . . . .
F12 F 0.0481(5) 0.6983(8) 0.8707(5) 0.099(3) Uani 1 1 d . . . . .
C9 C 0.7508(6) 0.9660(5) 0.9498(4) 0.0356(18) Uani 1 1 d D . . . .
H9A H 0.729480 1.018040 0.911587 0.053 Uiso 1 1 calc GR . . . .
H9B H 0.790136 0.992894 0.972013 0.053 Uiso 1 1 calc GR . . . .
H9C H 0.690779 0.939746 0.985186 0.053 Uiso 1 1 calc GR . . . .
C18 C 0.9682(5) 0.5035(6) 0.2551(5) 0.0350(18) Uani 1 1 d D . . . .
H18A H 0.913955 0.493007 0.298655 0.053 Uiso 1 1 calc GR . . . .
H18B H 0.993159 0.440737 0.243238 0.053 Uiso 1 1 calc GR . . . .
H18C H 0.941669 0.549642 0.216512 0.053 Uiso 1 1 calc GR . . . .
O1 O 0.2814(8) 0.6035(6) 0.6497(5) 0.075(2) Uani 1 1 d . . . . .
H1A H 0.221150 0.573822 0.648560 0.113 Uiso 1 1 d GR . . . .
H1B H 0.304947 0.557921 0.691286 0.113 Uiso 1 1 d GR . . . .
F13 F 0.1276(10) 0.5341(7) 0.8990(5) 0.143(5) Uani 1 1 d . . . . .
C39 C 0.6942(6) 0.6644(6) 0.3626(5) 0.0343(18) Uani 1 1 d . . . . .
H39 H 0.638224 0.672599 0.342288 0.041 Uiso 1 1 calc R . . . .
C11 C 0.6252(5) 0.6651(6) 0.9989(4) 0.0349(18) Uani 1 1 d D . . . .
H11A H 0.579539 0.716635 1.017686 0.052 Uiso 1 1 calc GR . . . .
H11B H 0.630709 0.606042 1.037551 0.052 Uiso 1 1 calc GR . . . .
H11C H 0.598006 0.649557 0.964231 0.052 Uiso 1 1 calc GR . . . .
C4AA C 0.7615(6) 0.7342(6) 1.0165(3) 0.0357(19) Uani 1 1 d D . . . .
H4AA H 0.785349 0.676646 1.051181 0.043 Uiso 1 1 calc R . . . .
H4AB H 0.703357 0.771022 1.042382 0.043 Uiso 1 1 calc R . . . .
C13 C 1.2146(5) 0.6231(4) 0.1996(5) 0.038(2) Uani 1 1 d D . . . .
H13A H 1.246709 0.597435 0.239991 0.046 Uiso 1 1 calc R . . . .
H13B H 1.269022 0.630694 0.155372 0.046 Uiso 1 1 calc R . . . .
C7AA C 0.8489(6) 0.8016(5) 0.9770(4) 0.040(2) Uani 1 1 d D . . . .
H7AA H 0.867337 0.828155 1.010997 0.048 Uiso 1 1 calc R . . . .
H7AB H 0.909559 0.762734 0.955500 0.048 Uiso 1 1 calc R . . . .
C17 C 1.2155(6) 0.7805(6) 0.2244(5) 0.042(2) Uani 1 1 d D . . . .
H17A H 1.178918 0.845709 0.224078 0.063 Uiso 1 1 calc GR . . . .
H17B H 1.282233 0.787431 0.191165 0.063 Uiso 1 1 calc GR . . . .
H17C H 1.224137 0.747016 0.272074 0.063 Uiso 1 1 calc GR . . . .
C19 C 1.0846(7) 0.4822(5) 0.3314(4) 0.0385(19) Uani 1 1 d D . . . .
H19A H 1.145418 0.504849 0.335110 0.058 Uiso 1 1 calc GR . . . .
H19B H 1.099152 0.413656 0.328862 0.058 Uiso 1 1 calc GR . . . .
H19C H 1.029213 0.486891 0.372885 0.058 Uiso 1 1 calc GR . . . .
C14 C 1.1416(5) 0.5496(5) 0.2020(4) 0.038(2) Uani 1 1 d D . . . .
H14A H 1.116056 0.571121 0.158588 0.046 Uiso 1 1 calc R . . . .
H14B H 1.178735 0.483435 0.204281 0.046 Uiso 1 1 calc R . . . .
B2 B -0.0482(9) 0.7937(7) 0.5663(6) 0.042(2) Uani 1 1 d . . . . .
C1BA C 0.4437(8) 0.8851(5) 0.6343(5) 0.088(3) Uani 1 1 d D U . . .
H1BA H 0.473909 0.920569 0.584990 0.105 Uiso 1 1 calc DR . . . .
H1BB H 0.476001 0.903195 0.665828 0.105 Uiso 1 1 calc R . . . .
C3 C 0.4367(5) 0.9039(8) 0.4254(4) 0.084(3) Uani 1 1 d D U . . .
H3A H 0.449570 0.944433 0.453191 0.100 Uiso 1 1 calc DR . . . .
H3B H 0.440759 0.945213 0.376461 0.100 Uiso 1 1 calc R . . . .
C4 C 0.2974(7) 0.9833(6) 0.5439(4) 0.091(3) Uani 1 1 d D U . . .
H4A H 0.371088 0.987657 0.535294 0.109 Uiso 1 1 calc DR . . . .
H4B H 0.260560 1.047136 0.550080 0.109 Uiso 1 1 calc R . . . .
C7 C 0.5195(10) 0.8146(9) 0.4244(5) 0.091(3) Uani 1 1 d D U . . .
H7A H 0.504741 0.774487 0.397015 0.110 Uiso 1 1 calc R . . . .
H7B H 0.585916 0.840193 0.398745 0.110 Uiso 1 1 calc R . . . .
C9AA C 0.5848(6) 0.8154(7) 0.5130(5) 0.093(3) Uani 1 1 d D U . . .
H9AA H 0.554281 0.884347 0.501357 0.112 Uiso 1 1 calc DR . . . .
H9AB H 0.657799 0.812222 0.488474 0.112 Uiso 1 1 calc R . . . .
C3BA C 0.2748(11) 0.9589(9) 0.4804(7) 0.091(3) Uani 1 1 d D U . . .
H3BA H 0.201519 0.950554 0.492551 0.110 Uiso 1 1 calc R . . . .
H3BB H 0.286978 1.017118 0.439359 0.110 Uiso 1 1 calc R . . . .
C2BA C 0.3273(7) 0.9164(11) 0.6530(7) 0.087(3) Uani 1 1 d D U . . .
H2BA H 0.299482 0.879939 0.702485 0.105 Uiso 1 1 calc R . . . .
H2BB H 0.318104 0.986994 0.651787 0.105 Uiso 1 1 calc R . . . .
C0BA C 0.5686(7) 0.7713(12) 0.5945(5) 0.093(3) Uani 1 1 d D U . . .
H0BA H 0.595286 0.701053 0.602525 0.112 Uiso 1 1 calc R . . . .
H0BB H 0.611969 0.803936 0.610534 0.112 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag3 N14 2.476(6) . ?
Ag3 N8 2.478(6) . ?
Ag3 N11 2.483(5) . ?
Ag3 N17 2.466(6) . ?
Ag3 O1 2.333(7) . ?
Pd1 N1 2.044(6) 2_676 ?
Pd1 N31 2.037(6) . ?
Pd1 N7 2.079(5) . ?
Pd1 N4 2.077(6) . ?
Pd2 N24 2.060(6) 2_676 ?
Pd2 N37 2.037(6) . ?
Pd2 N12 2.073(6) . ?
Pd2 N15 2.072(5) . ?
Si7 F9 1.679(6) . ?
Si7 F8 1.659(6) . ?
Si7 F11 1.673(7) . ?
Si7 F10 1.659(8) . ?
Si7 F12 1.627(7) . ?
Si7 F13 1.663(8) . ?
F3 B2 1.392(11) . ?
N1 C1AA 1.345(9) . ?
N1 C6AA 1.331(10) . ?
N31 C32 1.335(9) . ?
N31 C30 1.327(9) . ?
F6 B2 1.392(12) . ?
N24 C23 1.350(9) . ?
N24 C25 1.318(10) . ?
N7 C10 1.473(3) . ?
N7 C11 1.471(3) . ?
N7 C4AA 1.474(3) . ?
N37 C38 1.341(11) . ?
N37 C36 1.342(10) . ?
N12 C16 1.472(3) . ?
N12 C13 1.474(3) . ?
N12 C17 1.473(3) . ?
N4 C5AA 1.473(3) . ?
N4 C9 1.472(3) . ?
N4 C7AA 1.475(3) . ?
F4 B2 1.377(13) . ?
N15 C18 1.471(3) . ?
N15 C19 1.472(3) . ?
N15 C14 1.473(3) . ?
C0AA H0AA 0.9300 . ?
C0AA C3AA 1.392(10) . ?
C0AA C1AA 1.369(10) . ?
N14 C27 1.469(3) . ?
N14 C1BA 1.467(3) . ?
N14 C0BA 1.474(3) . ?
N8 C8AA 1.469(3) . ?
N8 C3 1.466(3) . ?
N8 C3BA 1.473(3) . ?
C3AA C8AA 1.506(9) . ?
C3AA C2AA 1.405(10) . ?
C32 H32 0.9300 . ?
C32 C33 1.396(10) . ?
N11 C20 1.470(3) . ?
N11 C4 1.470(3) . ?
N11 C2BA 1.472(3) . ?
C33 H33 0.9300 . ?
C33 C28 1.383(10) . ?
C8AA H8AA 0.9700 . ?
C8AA H8AB 0.9700 . ?
C1AA H1AA 0.9300 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.504(9) . ?
F5 B2 1.355(14) . ?
C28 C29 1.403(10) . ?
N17 C34 1.471(3) . ?
N17 C7 1.472(3) . ?
N17 C9AA 1.470(3) . ?
C21 C20 1.507(9) . ?
C21 C26 1.407(10) . ?
C21 C22 1.408(10) . ?
C30 H30 0.9300 . ?
C30 C29 1.379(10) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C26 H26 0.9300 . ?
C26 C25 1.377(10) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C40 1.515(9) . ?
C29 H29 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.364(11) . ?
C22 H22 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C6AA H6AA 0.9300 . ?
C6AA C2AA 1.363(11) . ?
C40 C35 1.376(11) . ?
C40 C39 1.363(11) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C2AA H2AA 0.9300 . ?
C38 H38 0.9300 . ?
C38 C39 1.377(11) . ?
C35 H35 0.9300 . ?
C35 C36 1.385(11) . ?
C25 H25 0.9300 . ?
C5AA H5AA 0.9600 . ?
C5AA H5AB 0.9600 . ?
C5AA H5AC 0.9600 . ?
C36 H36 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O1 H1A 0.9842 . ?
O1 H1B 0.9825 . ?
C39 H39 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C4AA H4AA 0.9700 . ?
C4AA H4AB 0.9700 . ?
C4AA C7AA 1.527(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.528(3) . ?
C7AA H7AA 0.9700 . ?
C7AA H7AB 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1BA H1BA 0.9700 . ?
C1BA H1BB 0.9700 . ?
C1BA C2BA 1.526(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C7 1.528(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3BA 1.529(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C9AA H9AA 0.9700 . ?
C9AA H9AB 0.9700 . ?
C9AA C0BA 1.528(3) . ?
C3BA H3BA 0.9700 . ?
C3BA H3BB 0.9700 . ?
C2BA H2BA 0.9700 . ?
C2BA H2BB 0.9700 . ?
C0BA H0BA 0.9700 . ?
C0BA H0BB 0.9700 . ?

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
N14 Ag3 N8 121.09(16) . . ?
N14 Ag3 N11 77.2(2) . . ?
N8 Ag3 N11 76.3(2) . . ?
N17 Ag3 N14 73.4(2) . . ?
N17 Ag3 N8 76.6(2) . . ?
N17 Ag3 N11 120.47(16) . . ?
O1 Ag3 N14 100.3(2) . . ?
O1 Ag3 N8 138.5(2) . . ?
O1 Ag3 N11 112.4(3) . . ?
O1 Ag3 N17 122.9(3) . . ?
N1 Pd1 N7 177.9(2) 2_676 . ?
N1 Pd1 N4 94.6(2) 2_676 . ?
N31 Pd1 N1 85.1(2) . 2_676 ?
N31 Pd1 N7 94.6(2) . . ?
N31 Pd1 N4 178.9(2) . . ?
N4 Pd1 N7 85.72(19) . . ?
N24 Pd2 N12 95.3(2) 2_676 . ?
N24 Pd2 N15 178.2(2) 2_676 . ?
N37 Pd2 N24 85.3(2) . 2_676 ?
N37 Pd2 N12 177.7(2) . . ?
N37 Pd2 N15 93.7(2) . . ?
N15 Pd2 N12 85.72(19) . . ?
F8 Si7 F9 89.4(4) . . ?
F8 Si7 F11 90.4(4) . . ?
F8 Si7 F13 176.6(6) . . ?
F11 Si7 F9 179.5(4) . . ?
F10 Si7 F9 91.2(5) . . ?
F10 Si7 F8 88.1(4) . . ?
F10 Si7 F11 88.4(5) . . ?
F10 Si7 F13 88.8(6) . . ?
F12 Si7 F9 88.7(4) . . ?
F12 Si7 F8 92.3(5) . . ?
F12 Si7 F11 91.7(5) . . ?
F12 Si7 F10 179.5(5) . . ?
F12 Si7 F13 90.7(6) . . ?
F13 Si7 F9 89.2(5) . . ?
F13 Si7 F11 91.0(5) . . ?
C1AA N1 Pd1 123.3(5) . 2_676 ?
C6AA N1 Pd1 118.9(5) . 2_676 ?
C6AA N1 C1AA 117.3(6) . . ?
C32 N31 Pd1 118.8(5) . . ?
C30 N31 Pd1 121.0(5) . . ?
C30 N31 C32 119.8(6) . . ?
C23 N24 Pd2 120.4(5) . 2_676 ?
C25 N24 Pd2 119.9(5) . 2_676 ?
C25 N24 C23 119.2(6) . . ?
C10 N7 Pd1 109.4(4) . . ?
C10 N7 C4AA 112.8(6) . . ?
C11 N7 Pd1 113.6(4) . . ?
C11 N7 C10 107.8(6) . . ?
C11 N7 C4AA 107.4(5) . . ?
C4AA N7 Pd1 105.9(4) . . ?
C38 N37 Pd2 118.3(5) . . ?
C38 N37 C36 119.2(6) . . ?
C36 N37 Pd2 122.2(5) . . ?
C16 N12 Pd2 109.3(5) . . ?
C16 N12 C13 110.9(6) . . ?
C16 N12 C17 108.8(7) . . ?
C13 N12 Pd2 106.0(4) . . ?
C17 N12 Pd2 112.5(5) . . ?
C17 N12 C13 109.4(6) . . ?
C5AA N4 Pd1 112.1(4) . . ?
C5AA N4 C7AA 108.1(5) . . ?
C9 N4 Pd1 109.5(4) . . ?
C9 N4 C5AA 109.3(6) . . ?
C9 N4 C7AA 111.9(6) . . ?
C7AA N4 Pd1 105.9(4) . . ?
C18 N15 Pd2 113.2(4) . . ?
C18 N15 C19 109.7(6) . . ?
C18 N15 C14 109.1(6) . . ?
C19 N15 Pd2 107.7(4) . . ?
C19 N15 C14 110.7(6) . . ?
C14 N15 Pd2 106.4(4) . . ?
C3AA C0AA H0AA 119.8 . . ?
C1AA C0AA H0AA 119.8 . . ?
C1AA C0AA C3AA 120.5(6) . . ?
C27 N14 Ag3 111.7(4) . . ?
C27 N14 C0BA 109.5(7) . . ?
C1BA N14 Ag3 102.4(5) . . ?
C1BA N14 C27 126.8(7) . . ?
C1BA N14 C0BA 100.3(9) . . ?
C0BA N14 Ag3 103.6(6) . . ?
C8AA N8 Ag3 115.5(4) . . ?
C8AA N8 C3BA 108.8(7) . . ?
C3 N8 Ag3 102.4(5) . . ?
C3 N8 C8AA 123.6(6) . . ?
C3 N8 C3BA 101.2(8) . . ?
C3BA N8 Ag3 102.7(6) . . ?
C0AA C3AA C8AA 122.1(6) . . ?
C0AA C3AA C2AA 116.3(7) . . ?
C2AA C3AA C8AA 121.6(7) . . ?
N31 C32 H32 119.7 . . ?
N31 C32 C33 120.6(7) . . ?
C33 C32 H32 119.7 . . ?
C20 N11 Ag3 114.2(4) . . ?
C20 N11 C2BA 107.8(7) . . ?
C4 N11 Ag3 102.9(4) . . ?
C4 N11 C20 127.4(6) . . ?
C4 N11 C2BA 98.3(8) . . ?
C2BA N11 Ag3 102.7(6) . . ?
C32 C33 H33 119.5 . . ?
C28 C33 C32 121.0(7) . . ?
C28 C33 H33 119.5 . . ?
N8 C8AA C3AA 113.5(5) . . ?
N8 C8AA H8AA 108.9 . . ?
N8 C8AA H8AB 108.9 . . ?
C3AA C8AA H8AA 108.9 . . ?
C3AA C8AA H8AB 108.9 . . ?
H8AA C8AA H8AB 107.7 . . ?
N1 C1AA C0AA 122.5(7) . . ?
N1 C1AA H1AA 118.7 . . ?
C0AA C1AA H1AA 118.7 . . ?
N14 C27 H27A 108.9 . . ?
N14 C27 H27B 108.9 . . ?
N14 C27 C28 113.4(5) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C33 C28 C27 121.5(6) . . ?
C33 C28 C29 116.2(6) . . ?
C29 C28 C27 122.1(6) . . ?
C34 N17 Ag3 111.2(4) . . ?
C34 N17 C7 106.1(7) . . ?
C7 N17 Ag3 104.6(6) . . ?
C9AA N17 Ag3 107.8(4) . . ?
C9AA N17 C34 127.4(7) . . ?
C9AA N17 C7 96.4(9) . . ?
C26 C21 C20 122.1(6) . . ?
C26 C21 C22 116.1(6) . . ?
C22 C21 C20 121.7(6) . . ?
N31 C30 H30 118.9 . . ?
N31 C30 C29 122.1(7) . . ?
C29 C30 H30 118.9 . . ?
N11 C20 C21 113.1(5) . . ?
N11 C20 H20A 109.0 . . ?
N11 C20 H20B 109.0 . . ?
C21 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C21 C26 H26 120.1 . . ?
C25 C26 C21 119.7(7) . . ?
C25 C26 H26 120.1 . . ?
N17 C34 H34A 108.9 . . ?
N17 C34 H34B 108.9 . . ?
N17 C34 C40 113.2(5) . . ?
H34A C34 H34B 107.7 . . ?
C40 C34 H34A 108.9 . . ?
C40 C34 H34B 108.9 . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.1(6) . . ?
C30 C29 H29 119.9 . . ?
N24 C23 H23 119.2 . . ?
N24 C23 C22 121.7(7) . . ?
C22 C23 H23 119.2 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.5(7) . . ?
C23 C22 H22 119.7 . . ?
N12 C16 H16A 109.5 . . ?
N12 C16 H16B 109.5 . . ?
N12 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C6AA H6AA 118.1 . . ?
N1 C6AA C2AA 123.8(7) . . ?
C2AA C6AA H6AA 118.1 . . ?
C35 C40 C34 121.5(7) . . ?
C39 C40 C34 120.8(7) . . ?
C39 C40 C35 117.4(7) . . ?
N7 C10 H10A 109.5 . . ?
N7 C10 H10B 109.5 . . ?
N7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3AA C2AA H2AA 120.3 . . ?
C6AA C2AA C3AA 119.5(7) . . ?
C6AA C2AA H2AA 120.3 . . ?
N37 C38 H38 119.4 . . ?
N37 C38 C39 121.2(7) . . ?
C39 C38 H38 119.4 . . ?
C40 C35 H35 119.7 . . ?
C40 C35 C36 120.6(7) . . ?
C36 C35 H35 119.7 . . ?
N24 C25 C26 122.7(7) . . ?
N24 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
N4 C5AA H5AA 109.5 . . ?
N4 C5AA H5AB 109.5 . . ?
N4 C5AA H5AC 109.5 . . ?
H5AA C5AA H5AB 109.5 . . ?
H5AA C5AA H5AC 109.5 . . ?
H5AB C5AA H5AC 109.5 . . ?
N37 C36 C35 120.7(7) . . ?
N37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
N4 C9 H9A 109.5 . . ?
N4 C9 H9B 109.5 . . ?
N4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N15 C18 H18A 109.5 . . ?
N15 C18 H18B 109.5 . . ?
N15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Ag3 O1 H1A 128.1 . . ?
Ag3 O1 H1B 127.9 . . ?
H1A O1 H1B 104.0 . . ?
C40 C39 C38 120.8(8) . . ?
C40 C39 H39 119.6 . . ?
C38 C39 H39 119.6 . . ?
N7 C11 H11A 109.5 . . ?
N7 C11 H11B 109.5 . . ?
N7 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N7 C4AA H4AA 109.8 . . ?
N7 C4AA H4AB 109.8 . . ?
N7 C4AA C7AA 109.4(6) . . ?
H4AA C4AA H4AB 108.2 . . ?
C7AA C4AA H4AA 109.8 . . ?
C7AA C4AA H4AB 109.8 . . ?
N12 C13 H13A 109.8 . . ?
N12 C13 H13B 109.8 . . ?
N12 C13 C14 109.5(5) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
N4 C7AA C4AA 109.9(5) . . ?
N4 C7AA H7AA 109.7 . . ?
N4 C7AA H7AB 109.7 . . ?
C4AA C7AA H7AA 109.7 . . ?
C4AA C7AA H7AB 109.7 . . ?
H7AA C7AA H7AB 108.2 . . ?
N12 C17 H17A 109.5 . . ?
N12 C17 H17B 109.5 . . ?
N12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N15 C19 H19A 109.5 . . ?
N15 C19 H19B 109.5 . . ?
N15 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N15 C14 C13 109.8(5) . . ?
N15 C14 H14A 109.7 . . ?
N15 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
F6 B2 F3 108.5(8) . . ?
F4 B2 F3 111.0(9) . . ?
F4 B2 F6 107.2(8) . . ?
F5 B2 F3 111.1(8) . . ?
F5 B2 F6 108.0(9) . . ?
F5 B2 F4 110.8(9) . . ?
N14 C1BA H1BA 109.5 . . ?
N14 C1BA H1BB 109.5 . . ?
N14 C1BA C2BA 110.6(9) . . ?
H1BA C1BA H1BB 108.1 . . ?
C2BA C1BA H1BA 109.5 . . ?
C2BA C1BA H1BB 109.5 . . ?
N8 C3 H3A 109.4 . . ?
N8 C3 H3B 109.4 . . ?
N8 C3 C7 111.3(9) . . ?
H3A C3 H3B 108.0 . . ?
C7 C3 H3A 109.4 . . ?
C7 C3 H3B 109.4 . . ?
N11 C4 H4A 110.2 . . ?
N11 C4 H4B 110.2 . . ?
N11 C4 C3BA 107.7(9) . . ?
H4A C4 H4B 108.5 . . ?
C3BA C4 H4A 110.2 . . ?
C3BA C4 H4B 110.2 . . ?
N17 C7 C3 116.5(8) . . ?
N17 C7 H7A 108.2 . . ?
N17 C7 H7B 108.2 . . ?
C3 C7 H7A 108.2 . . ?
C3 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
N17 C9AA H9AA 111.6 . . ?
N17 C9AA H9AB 111.6 . . ?
N17 C9AA C0BA 101.0(9) . . ?
H9AA C9AA H9AB 109.4 . . ?
C0BA C9AA H9AA 111.6 . . ?
C0BA C9AA H9AB 111.6 . . ?
N8 C3BA C4 118.7(8) . . ?
N8 C3BA H3BA 107.6 . . ?
N8 C3BA H3BB 107.6 . . ?
C4 C3BA H3BA 107.6 . . ?
C4 C3BA H3BB 107.6 . . ?
H3BA C3BA H3BB 107.1 . . ?
N11 C2BA C1BA 119.2(8) . . ?
N11 C2BA H2BA 107.5 . . ?
N11 C2BA H2BB 107.5 . . ?
C1BA C2BA H2BA 107.5 . . ?
C1BA C2BA H2BB 107.5 . . ?
H2BA C2BA H2BB 107.0 . . ?
N14 C0BA C9AA 120.0(8) . . ?
N14 C0BA H0BA 107.3 . . ?
N14 C0BA H0BB 107.3 . . ?
C9AA C0BA H0BA 107.3 . . ?
C9AA C0BA H0BB 107.3 . . ?
H0BA C0BA H0BB 106.9 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.199 -0.514 0.648 1049.1 406.3 ?
2 0.071 0.280 0.224 9.5 10.0 ?
3 -0.071 0.720 0.776 9.5 10.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.240
_oxdiff_exptl_absorpt_empirical_full_min 0.303
####################################################################### 
# 
# 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_djn184d
_audit_block_doi                 10.5517/cc754n5
_database_code_depnum_ccdc_archive 'CCDC 213486'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1142/S1088424603000744 2003
_audit_update_record             
;
2003-06-23 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2,3,8,12,17,18-hexaethyl-7,13-dimethylbiliverdin
;
_chemical_name_common            
2,3,8,12,17,18-hexaethyl-7,13-dimethylbiliverdin
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H42 N4 O2'
_chemical_formula_sum            'C33 H42 N4 O2'

_chemical_formula_weight         526.71

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'

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

_cell_length_a                   14.8284(8)
_cell_length_b                   17.9936(10)
_cell_length_c                   21.3095(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5685.7(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    949
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      30.41

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.24
_exptl_crystal_preparation       
;
Crystals were grown from methanol.
;
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2272
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9712
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         0
_diffrn_standards_interval_count 
;
50 frames measured at the beginning and end of the data collection.
;
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <0.1
_diffrn_reflns_number            71051
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         30.00
_reflns_number_total             8303
_reflns_number_gt                6742
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0715P)²+2.0292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8303
_refine_ls_number_parameters     372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1186
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.60338(5) 0.01830(4) 0.54145(4) 0.01856(16) Uani 1 1 d . . .
N1 N 0.57318(6) -0.07262(5) 0.46729(4) 0.01571(18) Uani 1 1 d . . .
C1 C 0.62900(7) -0.02981(6) 0.50427(5) 0.0155(2) Uani 1 1 d . . .
O2 O 0.62526(6) -0.14072(5) 0.61916(4) 0.02256(18) Uani 1 1 d . . .
N2 N 0.43379(6) -0.18377(5) 0.41572(4) 0.01472(17) Uani 1 1 d . . .
C2 C 0.72271(7) -0.05220(6) 0.49038(5) 0.0167(2) Uani 1 1 d . . .
C2A C 0.80223(8) -0.01944(7) 0.52370(6) 0.0222(2) Uani 1 1 d . . .
H2A1 H 0.7866 0.0314 0.5379 0.027 Uiso 1 1 calc R . .
H2A2 H 0.8531 -0.0153 0.4938 0.027 Uiso 1 1 calc R . .
C2B C 0.83235(10) -0.06465(8) 0.57982(7) 0.0326(3) Uani 1 1 d . . .
H2B1 H 0.7824 -0.0691 0.6097 0.049 Uiso 1 1 calc R . .
H2B2 H 0.8834 -0.0399 0.6002 0.049 Uiso 1 1 calc R . .
H2B3 H 0.8508 -0.1143 0.5659 0.049 Uiso 1 1 calc R . .
N3 N 0.32290(6) -0.16091(5) 0.52490(4) 0.01572(18) Uani 1 1 d . . .
C3 C 0.71971(7) -0.10486(6) 0.44481(5) 0.0159(2) Uani 1 1 d . . .
C3A C 0.79832(7) -0.14412(6) 0.41527(5) 0.0183(2) Uani 1 1 d . . .
H3A1 H 0.7795 -0.1947 0.4024 0.022 Uiso 1 1 calc R . .
H3A2 H 0.8472 -0.1492 0.4466 0.022 Uiso 1 1 calc R . .
C3B C 0.83404(9) -0.10217(7) 0.35809(6) 0.0256(2) Uani 1 1 d . . .
H3B1 H 0.7863 -0.0983 0.3264 0.038 Uiso 1 1 calc R . .
H3B2 H 0.8856 -0.1290 0.3404 0.038 Uiso 1 1 calc R . .
H3B3 H 0.8531 -0.0522 0.3708 0.038 Uiso 1 1 calc R . .
C4 C 0.62513(7) -0.11796(6) 0.42812(5) 0.01501(19) Uani 1 1 d . . .
N4 N 0.47123(6) -0.12453(5) 0.60597(5) 0.01744(18) Uani 1 1 d . . .
C5 C 0.59422(7) -0.16681(6) 0.38456(5) 0.0160(2) Uani 1 1 d . . .
H5 H 0.6386 -0.1874 0.3575 0.019 Uiso 1 1 calc R . .
C6 C 0.50342(7) -0.19157(6) 0.37389(5) 0.01524(19) Uani 1 1 d . . .
C7 C 0.47185(7) -0.23587(6) 0.32376(5) 0.0161(2) Uani 1 1 d . . .
C7A C 0.52446(8) -0.25865(7) 0.26688(5) 0.0217(2) Uani 1 1 d . . .
H7A1 H 0.5080 -0.2267 0.2314 0.032 Uiso 1 1 calc R . .
H7A2 H 0.5107 -0.3105 0.2566 0.032 Uiso 1 1 calc R . .
H7A3 H 0.5891 -0.2536 0.2754 0.032 Uiso 1 1 calc R . .
C8 C 0.38196(7) -0.25516(6) 0.33686(5) 0.0161(2) Uani 1 1 d . . .
C8A C 0.32133(8) -0.30157(7) 0.29642(5) 0.0201(2) Uani 1 1 d . . .
H8A1 H 0.2690 -0.3181 0.3216 0.024 Uiso 1 1 calc R . .
H8A2 H 0.3546 -0.3464 0.2827 0.024 Uiso 1 1 calc R . .
C8B C 0.28723(10) -0.26002(8) 0.23867(7) 0.0313(3) Uani 1 1 d . . .
H8B1 H 0.2540 -0.2156 0.2519 0.047 Uiso 1 1 calc R . .
H8B2 H 0.2472 -0.2925 0.2144 0.047 Uiso 1 1 calc R . .
H8B3 H 0.3386 -0.2453 0.2125 0.047 Uiso 1 1 calc R . .
C9 C 0.35943(7) -0.22240(6) 0.39490(5) 0.01526(19) Uani 1 1 d . . .
C10 C 0.27700(7) -0.22583(6) 0.42850(5) 0.0160(2) Uani 1 1 d . . .
H10 H 0.2291 -0.2522 0.4090 0.019 Uiso 1 1 calc R . .
C11 C 0.25872(7) -0.19514(6) 0.48626(5) 0.0153(2) Uani 1 1 d . . .
C12 C 0.16866(7) -0.18742(6) 0.51289(5) 0.0159(2) Uani 1 1 d . . .
C12A C 0.08374(7) -0.21572(6) 0.48320(5) 0.0189(2) Uani 1 1 d . . .
H12A H 0.0354 -0.2169 0.5152 0.023 Uiso 1 1 calc R . .
H12B H 0.0938 -0.2673 0.4686 0.023 Uiso 1 1 calc R . .
C12B C 0.05234(9) -0.16835(9) 0.42776(7) 0.0319(3) Uani 1 1 d . . .
H12C H 0.0393 -0.1178 0.4423 0.048 Uiso 1 1 calc R . .
H12D H -0.0023 -0.1902 0.4096 0.048 Uiso 1 1 calc R . .
H12E H 0.0999 -0.1667 0.3959 0.048 Uiso 1 1 calc R . .
C13 C 0.17856(7) -0.14556(6) 0.56585(5) 0.0163(2) Uani 1 1 d . . .
C13A C 0.10649(8) -0.11752(7) 0.60905(6) 0.0214(2) Uani 1 1 d . . .
H13A H 0.0935 -0.0654 0.5994 0.032 Uiso 1 1 calc R . .
H13B H 0.1272 -0.1216 0.6526 0.032 Uiso 1 1 calc R . .
H13C H 0.0517 -0.1472 0.6035 0.032 Uiso 1 1 calc R . .
C14 C 0.27545(7) -0.13111(6) 0.57184(5) 0.0155(2) Uani 1 1 d . . .
C15 C 0.31494(7) -0.08884(6) 0.62245(5) 0.0167(2) Uani 1 1 d . . .
H15 H 0.2749 -0.0611 0.6482 0.020 Uiso 1 1 calc R . .
C16 C 0.40395(7) -0.08521(6) 0.63649(5) 0.0155(2) Uani 1 1 d . . .
C17 C 0.44787(7) -0.04196(6) 0.68677(5) 0.0163(2) Uani 1 1 d . . .
C17A C 0.39163(8) 0.00757(7) 0.72805(6) 0.0220(2) Uani 1 1 d . . .
H17A H 0.3595 0.0432 0.7006 0.026 Uiso 1 1 calc R . .
H17B H 0.3453 -0.0237 0.7486 0.026 Uiso 1 1 calc R . .
C17B C 0.43879(10) 0.05129(10) 0.77833(8) 0.0416(4) Uani 1 1 d . . .
H17C H 0.4662 0.0171 0.8086 0.062 Uiso 1 1 calc R . .
H17D H 0.3951 0.0832 0.7999 0.062 Uiso 1 1 calc R . .
H17E H 0.4858 0.0822 0.7593 0.062 Uiso 1 1 calc R . .
C18 C 0.53767(8) -0.05632(6) 0.68482(5) 0.0166(2) Uani 1 1 d . . .
C18A C 0.61725(8) -0.02724(6) 0.72055(5) 0.0196(2) Uani 1 1 d . . .
H18A H 0.6644 -0.0661 0.7222 0.024 Uiso 1 1 calc R . .
H18B H 0.5986 -0.0161 0.7641 0.024 Uiso 1 1 calc R . .
C18B C 0.65704(8) 0.04321(7) 0.69079(6) 0.0233(2) Uani 1 1 d . . .
H18C H 0.6703 0.0338 0.6464 0.035 Uiso 1 1 calc R . .
H18D H 0.7127 0.0568 0.7127 0.035 Uiso 1 1 calc R . .
H18E H 0.6134 0.0839 0.6942 0.035 Uiso 1 1 calc R . .
C19 C 0.55388(7) -0.11137(6) 0.63341(5) 0.0170(2) Uani 1 1 d . . .
H1 H 0.5135(13) -0.0585(10) 0.4599(9) 0.039(5) Uiso 1 1 d . . .
H2 H 0.4326(10) -0.1588(9) 0.4510(7) 0.023(4) Uiso 1 1 d . . .
H4 H 0.4618(11) -0.1526(9) 0.5741(8) 0.030(4) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.2335(13) . ?
N1 C1 1.3782(14) . ?
N1 C4 1.3985(14) . ?
C1 C2 1.4768(15) . ?
O2 C19 1.2213(14) . ?
N2 C6 1.3713(13) . ?
N2 C9 1.3768(13) . ?
C2 C3 1.3574(15) . ?
C2 C2A 1.4974(15) . ?
C2A C2B 1.5138(18) . ?
N3 C14 1.3354(14) . ?
N3 C11 1.4011(13) . ?
C3 C4 1.4661(14) . ?
C3 C3A 1.5013(15) . ?
C3A C3B 1.5281(16) . ?
C4 C5 1.3581(15) . ?
N4 C19 1.3785(14) . ?
N4 C16 1.3854(14) . ?
C5 C6 1.4363(15) . ?
C6 C7 1.4126(15) . ?
C7 C8 1.4053(15) . ?
C7 C7A 1.4987(15) . ?
C8 C9 1.4103(15) . ?
C8 C8A 1.4994(15) . ?
C8A C8B 1.5261(18) . ?
C9 C10 1.4179(15) . ?
C10 C11 1.3761(15) . ?
C11 C12 1.4575(15) . ?
C12 C13 1.3647(15) . ?
C12 C12A 1.4984(15) . ?
C12A C12B 1.5294(17) . ?
C13 C14 1.4656(15) . ?
C13 C13A 1.4982(15) . ?
C14 C15 1.4437(15) . ?
C15 C16 1.3549(15) . ?
C16 C17 1.4758(15) . ?
C17 C18 1.3571(15) . ?
C17 C17A 1.5046(15) . ?
C17A C17B 1.5019(18) . ?
C18 C19 1.4963(15) . ?
C18 C18A 1.4986(15) . ?
C18A C18B 1.5353(17) . ?

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 N1 C4 109.66(9) . . ?
O1 C1 N1 125.07(10) . . ?
O1 C1 C2 127.59(10) . . ?
N1 C1 C2 107.34(9) . . ?
C6 N2 C9 109.99(9) . . ?
C3 C2 C1 107.64(9) . . ?
C3 C2 C2A 129.78(10) . . ?
C1 C2 C2A 122.58(10) . . ?
C2 C2A C2B 113.29(10) . . ?
C14 N3 C11 105.00(9) . . ?
C2 C3 C4 108.49(9) . . ?
C2 C3 C3A 127.08(10) . . ?
C4 C3 C3A 124.43(10) . . ?
C3 C3A C3B 111.78(9) . . ?
C5 C4 N1 126.84(10) . . ?
C5 C4 C3 126.36(10) . . ?
N1 C4 C3 106.76(9) . . ?
C19 N4 C16 110.69(9) . . ?
C4 C5 C6 128.71(10) . . ?
N2 C6 C7 107.44(9) . . ?
N2 C6 C5 124.83(10) . . ?
C7 C6 C5 127.26(10) . . ?
C8 C7 C6 107.67(9) . . ?
C8 C7 C7A 125.93(10) . . ?
C6 C7 C7A 126.40(10) . . ?
C7 C8 C9 107.20(9) . . ?
C7 C8 C8A 126.31(10) . . ?
C9 C8 C8A 126.50(10) . . ?
C8 C8A C8B 112.91(10) . . ?
N2 C9 C8 107.69(9) . . ?
N2 C9 C10 123.34(9) . . ?
C8 C9 C10 128.97(10) . . ?
C11 C10 C9 127.16(10) . . ?
C10 C11 N3 124.63(10) . . ?
C10 C11 C12 124.53(10) . . ?
N3 C11 C12 110.59(9) . . ?
C13 C12 C11 106.02(9) . . ?
C13 C12 C12A 128.83(10) . . ?
C11 C12 C12A 124.98(10) . . ?
C12 C12A C12B 113.12(10) . . ?
C12 C13 C14 105.99(9) . . ?
C12 C13 C13A 128.13(10) . . ?
C14 C13 C13A 125.87(10) . . ?
N3 C14 C15 123.87(10) . . ?
N3 C14 C13 112.33(9) . . ?
C15 C14 C13 123.80(10) . . ?
C16 C15 C14 125.84(10) . . ?
C15 C16 N4 124.98(10) . . ?
C15 C16 C17 128.00(10) . . ?
N4 C16 C17 107.00(9) . . ?
C18 C17 C16 108.08(9) . . ?
C18 C17 C17A 132.43(10) . . ?
C16 C17 C17A 119.48(10) . . ?
C17B C17A C17 117.98(11) . . ?
C17 C18 C19 107.82(9) . . ?
C17 C18 C18A 133.67(10) . . ?
C19 C18 C18A 118.46(10) . . ?
C18 C18A C18B 112.40(9) . . ?
O2 C19 N4 126.20(10) . . ?
O2 C19 C18 127.42(10) . . ?
N4 C19 C18 106.35(9) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.052
