# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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
_audit_block_doi                 10.5517/cc6pg0b
_database_code_depnum_ccdc_archive 'CCDC 199361'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/aoc.455 2003
_audit_update_record             
;
2002-12-07 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H7.50 Ag2 B11 Br6 I5 N2.50'
_chemical_formula_weight         1563.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
I I -0.4742 1.8119 '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'

_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                   10.689(3)
_cell_length_b                   11.002(3)
_cell_length_c                   13.971(2)
_cell_angle_alpha                87.527(17)
_cell_angle_beta                 79.020(14)
_cell_angle_gamma                74.460(9)
_cell_volume                     1553.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1370
_exptl_absorpt_coefficient_mu    13.948
_exptl_absorpt_correction_type   ABSCOR
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_T_max  1.227
_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3769
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3769
_reflns_number_gt                2995
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0783P)²+10.5146P] 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       0.00184(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3769
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.1883
_refine_ls_wR_factor_gt          0.1717
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.084
_refine_ls_shift/su_mean         0.005

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag -0.5000 0.0000 0.5000 0.0555(3) Uani 1 2 d S . .
Ag2 Ag -0.01438(15) -0.29864(15) 0.24507(16) 0.2174(9) Uani 1 1 d . . .
Ag3 Ag -0.5000 0.5000 0.5000 0.1134(6) Uani 1 2 d S . .
Br11 Br -0.34996(10) 0.47410(8) 0.29792(6) 0.0633(3) Uani 1 1 d . . .
Br7 Br -0.02429(9) 0.22043(10) 0.29709(7) 0.0706(3) Uani 1 1 d . . .
Br8 Br -0.01983(9) -0.05510(9) 0.13407(6) 0.0632(3) Uani 1 1 d . . .
Br9 Br -0.34972(10) 0.02280(9) 0.04276(6) 0.0669(3) Uani 1 1 d . . .
Br10 Br -0.55428(10) 0.35432(10) 0.14493(7) 0.0713(3) Uani 1 1 d . . .
Br12 Br -0.18323(10) 0.28796(9) 0.06426(6) 0.0664(3) Uani 1 1 d . . .
C1 C -0.3972(8) 0.0754(7) 0.3748(4) 0.047(2) Uani 1 1 d . . .
C3 C 0.0922(11) -0.5576(10) 0.0970(9) 0.098(5) Uani 1 1 d . . .
C2 C 0.1598(11) -0.6816(11) 0.0419(9) 0.105(4) Uani 1 1 d . . .
H2A H 0.2391 -0.6739 -0.0007 0.157 Uiso 1 1 calc R . .
H2B H 0.1012 -0.7008 0.0041 0.157 Uiso 1 1 calc R . .
H2C H 0.1816 -0.7480 0.0876 0.157 Uiso 1 1 calc R . .
C5 C 0.2966(11) -0.3150(11) 0.1972(6) 0.095(4) Uani 1 1 d . . .
C4 C 0.4190(12) -0.2969(9) 0.1389(8) 0.105(5) Uani 1 1 d . . .
H4A H 0.4932 -0.3570 0.1581 0.158 Uiso 1 1 calc R . .
H4B H 0.4247 -0.2130 0.1493 0.158 Uiso 1 1 calc R . .
H4C H 0.4197 -0.3088 0.0712 0.158 Uiso 1 1 calc R . .
C7 C -1.0128(13) 0.5461(13) 0.4198(9) 0.137(5) Uiso 0.50 1 d P A 1
N3 N -1.0128(13) 0.5461(13) 0.4198(9) 0.137(5) Uiso 0.50 1 d P A 2
C6 C -1.0000 0.5000 0.5000 0.156(9) Uiso 1 2 d S . .
I2 I -0.30751(7) 0.25268(6) 0.53013(4) 0.0678(2) Uani 1 1 d . . .
I3 I -0.09990(6) -0.08797(6) 0.42662(4) 0.0675(2) Uani 1 1 d . . .
I4 I -0.30465(6) -0.21312(5) 0.26476(4) 0.0658(2) Uani 1 1 d . . .
I5 I -0.64959(6) 0.05134(6) 0.26784(5) 0.0721(2) Uani 1 1 d . . .
I6 I -0.64853(7) 0.33686(6) 0.43135(5) 0.0761(2) Uani 1 1 d . . .
B2 B -0.3173(10) 0.1934(10) 0.3831(6) 0.058(3) Uani 1 1 d . . .
B3 B -0.2257(10) 0.0393(9) 0.3430(6) 0.053(3) Uani 1 1 d . . .
B4 B -0.3213(9) -0.0171(9) 0.2709(6) 0.047(3) Uani 1 1 d . . .
B5 B -0.4669(8) 0.0982(9) 0.2726(6) 0.049(3) Uani 1 1 d . . .
B6 B -0.4696(9) 0.2302(9) 0.3434(6) 0.049(3) Uani 1 1 d . . .
B11 B -0.3410(10) 0.2961(8) 0.2879(6) 0.049(3) Uani 1 1 d . . .
B7 B -0.1862(9) 0.1758(9) 0.2848(6) 0.051(3) Uani 1 1 d . . .
B8 B -0.1879(10) 0.0484(8) 0.2145(6) 0.048(3) Uani 1 1 d . . .
B9 B -0.3418(9) 0.0850(9) 0.1704(6) 0.046(3) Uani 1 1 d . . .
B10 B -0.4341(10) 0.2393(9) 0.2135(6) 0.052(3) Uani 1 1 d . . .
B12 B -0.2545(10) 0.2018(9) 0.1799(6) 0.055(3) Uani 1 1 d . . .
N1 N 0.2134(17) -0.3076(11) 0.2392(7) 0.181(7) Uani 1 1 d . . .
N2 N 0.0384(12) -0.4696(10) 0.1439(8) 0.135(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 C1 2.142(7) . ?
Ag1 C1 2.142(7) 2_456 ?
Ag2 N2 2.283(12) . ?
Ag2 N1 2.396(18) . ?
Ag2 I4 2.9531(19) . ?
Ag2 Br8 3.030(2) . ?
Ag3 Br11 2.9536(10) 2_466 ?
Ag3 Br11 2.9536(10) . ?
Ag3 I6 2.9862(10) 2_466 ?
Ag3 I6 2.9862(10) . ?
Ag3 I2 3.0076(9) 2_466 ?
Ag3 I2 3.0076(9) . ?
Br11 B11 1.944(9) . ?
Br7 B7 1.960(11) . ?
Br8 B8 2.008(8) . ?
Br9 B9 1.962(9) . ?
Br10 B10 1.914(9) . ?
Br12 B12 1.969(9) . ?
C1 B5 1.713(12) . ?
C1 B3 1.741(12) . ?
C1 B4 1.743(10) . ?
C1 B6 1.747(12) . ?
C1 B2 1.753(15) . ?
C3 N2 1.144(15) . ?
C3 C2 1.525(15) . ?
C5 N1 0.953(18) . ?
C5 C4 1.462(16) . ?
C7 C6 1.226(13) . ?
C6 N3 1.226(13) 2_366 ?
C6 C7 1.226(13) 2_366 ?
I2 B2 2.211(9) . ?
I3 B3 2.141(10) . ?
I4 B4 2.120(9) . ?
I5 B5 2.161(10) . ?
I6 B6 2.138(8) . ?
B2 B11 1.719(12) . ?
B2 B7 1.741(12) . ?
B2 B6 1.759(15) . ?
B2 B3 1.770(13) . ?
B3 B8 1.768(12) . ?
B3 B7 1.788(14) . ?
B3 B4 1.797(15) . ?
B4 B5 1.722(12) . ?
B4 B9 1.769(12) . ?
B4 B8 1.801(14) . ?
B5 B9 1.742(12) . ?
B5 B6 1.784(14) . ?
B5 B10 1.812(14) . ?
B6 B11 1.760(14) . ?
B6 B10 1.785(12) . ?
B11 B10 1.802(15) . ?
B11 B7 1.815(12) . ?
B11 B12 1.816(11) . ?
B7 B12 1.738(13) . ?
B7 B8 1.753(14) . ?
B8 B12 1.733(13) . ?
B8 B9 1.804(14) . ?
B9 B10 1.784(12) . ?
B9 B12 1.801(16) . ?
B10 B12 1.824(14) . ?

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 Ag1 C1 180.000(1) . 2_456 ?
N2 Ag2 N1 92.3(4) . . ?
N2 Ag2 I4 102.1(3) . . ?
N1 Ag2 I4 164.0(3) . . ?
N2 Ag2 Br8 112.4(3) . . ?
N1 Ag2 Br8 84.1(3) . . ?
I4 Ag2 Br8 84.13(5) . . ?
Br11 Ag3 Br11 180.0 2_466 . ?
Br11 Ag3 I6 84.70(3) 2_466 2_466 ?
Br11 Ag3 I6 95.30(3) . 2_466 ?
Br11 Ag3 I6 95.30(3) 2_466 . ?
Br11 Ag3 I6 84.70(3) . . ?
I6 Ag3 I6 180.0 2_466 . ?
Br11 Ag3 I2 84.13(3) 2_466 2_466 ?
Br11 Ag3 I2 95.87(3) . 2_466 ?
I6 Ag3 I2 83.88(3) 2_466 2_466 ?
I6 Ag3 I2 96.12(3) . 2_466 ?
Br11 Ag3 I2 95.87(3) 2_466 . ?
Br11 Ag3 I2 84.13(3) . . ?
I6 Ag3 I2 96.12(3) 2_466 . ?
I6 Ag3 I2 83.88(3) . . ?
I2 Ag3 I2 180.0 2_466 . ?
B11 Br11 Ag3 94.0(2) . . ?
B8 Br8 Ag2 96.4(3) . . ?
B5 C1 B3 110.5(5) . . ?
B5 C1 B4 59.7(5) . . ?
B3 C1 B4 62.1(5) . . ?
B5 C1 B6 62.1(5) . . ?
B3 C1 B6 111.1(6) . . ?
B4 C1 B6 110.8(5) . . ?
B5 C1 B2 109.6(6) . . ?
B3 C1 B2 60.9(5) . . ?
B4 C1 B2 110.1(6) . . ?
B6 C1 B2 60.4(5) . . ?
B5 C1 Ag1 117.2(6) . . ?
B3 C1 Ag1 123.6(5) . . ?
B4 C1 Ag1 120.9(5) . . ?
B6 C1 Ag1 116.7(4) . . ?
B2 C1 Ag1 122.7(4) . . ?
N2 C3 C2 175.0(13) . . ?
N1 C5 C4 167.2(15) . . ?
N3 C6 C7 0.0(14) 2_366 2_366 ?
N3 C6 C7 180.0(5) 2_366 . ?
C7 C6 C7 180.0(5) 2_366 . ?
B2 I2 Ag3 88.5(2) . . ?
B4 I4 Ag2 96.7(2) . . ?
B6 I6 Ag3 90.0(3) . . ?
B11 B2 B7 63.3(5) . . ?
B11 B2 C1 108.9(7) . . ?
B7 B2 C1 108.3(7) . . ?
B11 B2 B6 60.8(6) . . ?
B7 B2 B6 111.1(6) . . ?
C1 B2 B6 59.6(6) . . ?
B11 B2 B3 112.4(6) . . ?
B7 B2 B3 61.2(5) . . ?
C1 B2 B3 59.2(6) . . ?
B6 B2 B3 109.2(8) . . ?
B11 B2 I2 123.5(6) . . ?
B7 B2 I2 123.0(7) . . ?
C1 B2 I2 117.9(5) . . ?
B6 B2 I2 120.1(5) . . ?
B3 B2 I2 117.8(6) . . ?
C1 B3 B8 106.5(7) . . ?
C1 B3 B2 59.9(5) . . ?
B8 B3 B2 105.3(6) . . ?
C1 B3 B7 106.7(6) . . ?
B8 B3 B7 59.1(5) . . ?
B2 B3 B7 58.6(5) . . ?
C1 B3 B4 59.0(5) . . ?
B8 B3 B4 60.7(5) . . ?
B2 B3 B4 107.0(7) . . ?
B7 B3 B4 108.0(7) . . ?
C1 B3 I3 121.9(5) . . ?
B8 B3 I3 123.1(5) . . ?
B2 B3 I3 123.3(6) . . ?
B7 B3 I3 123.1(7) . . ?
B4 B3 I3 120.9(6) . . ?
B5 B4 C1 59.2(5) . . ?
B5 B4 B9 59.9(5) . . ?
C1 B4 B9 106.1(6) . . ?
B5 B4 B3 107.5(7) . . ?
C1 B4 B3 58.9(5) . . ?
B9 B4 B3 107.8(7) . . ?
B5 B4 B8 107.7(7) . . ?
C1 B4 B8 104.9(6) . . ?
B9 B4 B8 60.7(5) . . ?
B3 B4 B8 58.9(5) . . ?
B5 B4 I4 123.9(6) . . ?
C1 B4 I4 123.2(5) . . ?
B9 B4 I4 123.7(6) . . ?
B3 B4 I4 119.6(5) . . ?
B8 B4 I4 121.6(5) . . ?
C1 B5 B4 61.0(5) . . ?
C1 B5 B9 108.7(6) . . ?
B4 B5 B9 61.4(5) . . ?
C1 B5 B6 59.9(5) . . ?
B4 B5 B6 110.1(7) . . ?
B9 B5 B6 108.3(7) . . ?
C1 B5 B10 107.5(7) . . ?
B4 B5 B10 110.2(7) . . ?
B9 B5 B10 60.2(5) . . ?
B6 B5 B10 59.5(5) . . ?
C1 B5 I5 122.0(6) . . ?
B4 B5 I5 121.5(7) . . ?
B9 B5 I5 122.2(6) . . ?
B6 B5 I5 119.6(5) . . ?
B10 B5 I5 120.3(6) . . ?
C1 B6 B2 60.0(5) . . ?
C1 B6 B11 107.3(6) . . ?
B2 B6 B11 58.5(5) . . ?
C1 B6 B5 58.0(5) . . ?
B2 B6 B5 106.1(6) . . ?
B11 B6 B5 109.0(6) . . ?
C1 B6 B10 107.3(6) . . ?
B2 B6 B10 107.0(6) . . ?
B11 B6 B10 61.1(6) . . ?
B5 B6 B10 61.0(5) . . ?
C1 B6 I6 120.0(5) . . ?
B2 B6 I6 122.1(5) . . ?
B11 B6 I6 123.3(6) . . ?
B5 B6 I6 121.3(6) . . ?
B10 B6 I6 123.5(6) . . ?
B2 B11 B6 60.8(6) . . ?
B2 B11 B10 108.0(7) . . ?
B6 B11 B10 60.1(5) . . ?
B2 B11 B7 59.0(5) . . ?
B6 B11 B7 107.7(6) . . ?
B10 B11 B7 107.0(6) . . ?
B2 B11 B12 104.4(6) . . ?
B6 B11 B12 107.1(7) . . ?
B10 B11 B12 60.5(5) . . ?
B7 B11 B12 57.2(5) . . ?
B2 B11 Br11 122.6(6) . . ?
B6 B11 Br11 123.2(5) . . ?
B10 B11 Br11 122.4(6) . . ?
B7 B11 Br11 121.1(7) . . ?
B12 B11 Br11 122.6(6) . . ?
B12 B7 B2 106.8(7) . . ?
B12 B7 B8 59.5(5) . . ?
B2 B7 B8 107.3(8) . . ?
B12 B7 B3 107.6(8) . . ?
B2 B7 B3 60.2(5) . . ?
B8 B7 B3 59.9(5) . . ?
B12 B7 B11 61.4(5) . . ?
B2 B7 B11 57.8(5) . . ?
B8 B7 B11 108.4(7) . . ?
B3 B7 B11 107.1(7) . . ?
B12 B7 Br7 123.4(6) . . ?
B2 B7 Br7 120.9(7) . . ?
B8 B7 Br7 123.5(6) . . ?
B3 B7 Br7 121.3(6) . . ?
B11 B7 Br7 121.1(7) . . ?
B12 B8 B7 59.8(5) . . ?
B12 B8 B3 108.7(6) . . ?
B7 B8 B3 61.0(5) . . ?
B12 B8 B4 108.5(7) . . ?
B7 B8 B4 109.4(6) . . ?
B3 B8 B4 60.5(5) . . ?
B12 B8 B9 61.2(6) . . ?
B7 B8 B9 108.7(6) . . ?
B3 B8 B9 107.6(6) . . ?
B4 B8 B9 58.7(5) . . ?
B12 B8 Br8 119.2(5) . . ?
B7 B8 Br8 120.4(7) . . ?
B3 B8 Br8 123.0(6) . . ?
B4 B8 Br8 122.9(6) . . ?
B9 B8 Br8 121.2(5) . . ?
B5 B9 B4 58.7(5) . . ?
B5 B9 B10 61.8(5) . . ?
B4 B9 B10 109.4(6) . . ?
B5 B9 B12 108.5(6) . . ?
B4 B9 B12 107.0(6) . . ?
B10 B9 B12 61.2(6) . . ?
B5 B9 B8 106.7(6) . . ?
B4 B9 B8 60.6(5) . . ?
B10 B9 B8 107.6(7) . . ?
B12 B9 B8 57.5(5) . . ?
B5 B9 Br9 124.0(7) . . ?
B4 B9 Br9 121.6(6) . . ?
B10 B9 Br9 121.6(6) . . ?
B12 B9 Br9 121.0(5) . . ?
B8 B9 Br9 120.8(5) . . ?
B9 B10 B6 106.4(6) . . ?
B9 B10 B11 108.2(6) . . ?
B6 B10 B11 58.8(5) . . ?
B9 B10 B5 57.9(5) . . ?
B6 B10 B5 59.4(5) . . ?
B11 B10 B5 105.9(6) . . ?
B9 B10 B12 59.9(5) . . ?
B6 B10 B12 105.7(6) . . ?
B11 B10 B12 60.1(5) . . ?
B5 B10 B12 104.5(6) . . ?
B9 B10 Br10 124.1(6) . . ?
B6 B10 Br10 120.7(5) . . ?
B11 B10 Br10 120.8(6) . . ?
B5 B10 Br10 123.6(7) . . ?
B12 B10 Br10 124.8(6) . . ?
B8 B12 B7 60.7(5) . . ?
B8 B12 B9 61.4(6) . . ?
B7 B12 B9 109.5(7) . . ?
B8 B12 B11 109.2(6) . . ?
B7 B12 B11 61.4(5) . . ?
B9 B12 B11 106.9(6) . . ?
B8 B12 B10 109.0(7) . . ?
B7 B12 B10 109.4(6) . . ?
B9 B12 B10 59.0(5) . . ?
B11 B12 B10 59.4(5) . . ?
B8 B12 Br12 126.1(5) . . ?
B7 B12 Br12 123.5(7) . . ?
B9 B12 Br12 121.7(5) . . ?
B11 B12 Br12 118.2(6) . . ?
B10 B12 Br12 116.2(5) . . ?
C5 N1 Ag2 144.6(13) . . ?
C3 N2 Ag2 164.9(12) . . ?

_diffrn_measured_fraction_theta_max 0.688
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.688
_refine_diff_density_max         1.546
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.227

#===END




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

data_njy1
_database_code_depnum_ccdc_archive 'CCDC 1993611'
loop_
_audit_author_name
_audit_author_address
'Rong Wan'
;Henan University
China
;
_audit_update_record             
;
2020-03-30 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;
_audit_creation_date             2017-12-06
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C48 H144 Na8 O108 Ru8 S24 W24), 3(O)'
_chemical_formula_sum            'C24 H72 Na4 O57 Ru4 S12 W12'
_chemical_formula_weight         4359.97
_chemical_absolute_configuration ?
_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'
Na Na 0.0362 0.0249 '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'
Ru Ru -1.2594 0.8363 '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'
W W -0.8490 6.8722 '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      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   17.9539(9)
_cell_length_b                   17.9539(9)
_cell_length_c                   17.9539(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5787.3(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.78
_shelx_estimated_absorpt_T_max   0.252
_shelx_estimated_absorpt_T_min   0.167
_exptl_absorpt_coefficient_mu    12.675
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0938 before and 0.0643 after correction. The Ratio of minimum to maximum transmission is 0.8077. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.604
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2029
_reflns_number_total             2398
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         2.008
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.249
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2398
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.124
_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)+(0.0433P)²+2.0371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0779
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.01(2) -0.01(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: Na2(0.25)
4.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
W1 W -0.08577(2) 0.00242(3) -0.17284(2) 0.01905(13) Uani 1 1 d . . . . .
Ru1 Ru -0.18015(5) -0.18015(5) -0.18015(5) 0.0239(3) Uani 1 3 d S T P . .
S1 S -0.1429(2) -0.2232(2) -0.29125(19) 0.0383(8) Uani 1 1 d . . . . .
Na1 Na 0.0000 0.0000 0.0000 0.021(2) Uani 1 12 d S T P . .
Na2 Na -0.1896(3) 0.1896(3) -0.1896(3) 0.017(2) Uani 0.75 3 d S T P . .
O1 O -0.1224(3) 0.0025(6) -0.0738(3) 0.0209(12) Uani 1 1 d . . . . .
O2 O -0.1338(5) -0.0784(5) -0.2047(5) 0.027(2) Uani 1 1 d . . . . .
O3 O -0.1354(5) 0.0726(5) -0.2129(5) 0.029(2) Uani 1 1 d . . . . .
O4 O 0.0000 0.0000 -0.2384(4) 0.0244(18) Uani 1 2 d S T P . .
O5 O -0.1798(6) -0.2890(6) -0.3228(7) 0.059(3) Uani 1 1 d . . . . .
C1 C -0.1490(12) -0.1538(10) -0.3608(8) 0.072(5) Uani 1 1 d . . . . .
H1A H -0.1256 -0.1090 -0.3434 0.107 Uiso 1 1 calc R . . . .
H1B H -0.1243 -0.1707 -0.4052 0.107 Uiso 1 1 calc R . . . .
H1C H -0.2004 -0.1440 -0.3717 0.107 Uiso 1 1 calc R . . . .
C2 C -0.0459(8) -0.2409(15) -0.2923(10) 0.085(7) Uani 1 1 d . . . . .
H2A H -0.0198 -0.1989 -0.2720 0.127 Uiso 1 1 calc R . . . .
H2B H -0.0354 -0.2843 -0.2629 0.127 Uiso 1 1 calc R . . . .
H2C H -0.0298 -0.2492 -0.3426 0.127 Uiso 1 1 calc R . . . .
O1W O 0.0000 -0.2500 -0.5000 0.111(9) Uiso 1 4 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 W1 3.0809(7) 2 ?
W1 Na1 3.4644(4) . ?
W1 O1 1.896(6) . ?
W1 O1 2.281(9) 9 ?
W1 O1 2.167(9) 12 ?
W1 O2 1.782(9) . ?
W1 O3 1.703(9) . ?
W1 O4 1.939(5) . ?
Ru1 S1 2.242(4) . ?
Ru1 S1 2.242(4) 9 ?
Ru1 S1 2.242(4) 5 ?
Ru1 O2 2.056(10) . ?
Ru1 O2 2.056(10) 5 ?
Ru1 O2 2.056(10) 9 ?
S1 O5 1.469(10) . ?
S1 C1 1.768(16) . ?
S1 C2 1.770(16) . ?
Na1 O1 2.567(6) 10 ?
Na1 O1 2.567(6) 5 ?
Na1 O1 2.567(6) 3 ?
Na1 O1 2.567(6) 6 ?
Na1 O1 2.567(6) 12 ?
Na1 O1 2.567(6) . ?
Na1 O1 2.567(6) 8 ?
Na1 O1 2.567(6) 11 ?
Na1 O1 2.567(6) 4 ?
Na1 O1 2.567(6) 9 ?
Na1 O1 2.567(6) 7 ?
Na1 O1 2.567(6) 2 ?
Na2 O3 2.354(11) . ?
Na2 O3 2.354(11) 12 ?
Na2 O3 2.354(11) 6 ?
Na2 O5 2.385(12) 16_454 ?
Na2 O5 2.385(12) 23_454 ?
Na2 O5 2.385(12) 18_454 ?
O1 W1 2.167(9) 6 ?
O1 W1 2.280(9) 5 ?
O4 W1 1.939(5) 2 ?
O5 Na2 2.385(12) 15_444 ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

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
W1 W1 Na1 63.597(5) 2 . ?
O1 W1 W1 110.31(18) . 2 ?
O1 W1 W1 47.7(2) 12 2 ?
O1 W1 W1 44.7(2) 9 2 ?
O1 W1 Na1 47.80(15) 9 . ?
O1 W1 Na1 47.68(16) 12 . ?
O1 W1 Na1 46.71(18) . . ?
O1 W1 O1 81.2(5) . 12 ?
O1 W1 O1 73.1(3) 12 9 ?
O1 W1 O1 82.5(4) . 9 ?
O1 W1 O4 147.7(3) . . ?
O2 W1 W1 117.5(3) . 2 ?
O2 W1 Na1 119.5(3) . . ?
O2 W1 O1 88.6(3) . 9 ?
O2 W1 O1 97.7(4) . . ?
O2 W1 O1 161.7(4) . 12 ?
O2 W1 O4 99.9(3) . . ?
O3 W1 W1 123.0(3) . 2 ?
O3 W1 Na1 128.3(3) . . ?
O3 W1 O1 167.2(4) . 9 ?
O3 W1 O1 95.8(4) . 12 ?
O3 W1 O1 102.4(4) . . ?
O3 W1 O2 102.3(3) . . ?
O3 W1 O4 100.1(3) . . ?
O4 W1 W1 37.41(18) . 2 ?
O4 W1 Na1 101.00(18) . . ?
O4 W1 O1 73.7(3) . 12 ?
O4 W1 O1 71.1(2) . 9 ?
S1 Ru1 S1 93.55(14) . 5 ?
S1 Ru1 S1 93.55(14) 9 5 ?
S1 Ru1 S1 93.55(14) . 9 ?
O2 Ru1 S1 89.7(3) . . ?
O2 Ru1 S1 89.7(3) 9 9 ?
O2 Ru1 S1 91.2(3) . 5 ?
O2 Ru1 S1 91.2(3) 9 . ?
O2 Ru1 S1 91.2(3) 5 9 ?
O2 Ru1 S1 174.1(3) 5 . ?
O2 Ru1 S1 89.7(3) 5 5 ?
O2 Ru1 S1 174.1(3) . 9 ?
O2 Ru1 S1 174.1(3) 9 5 ?
O2 Ru1 O2 85.3(4) . 9 ?
O2 Ru1 O2 85.3(4) 9 5 ?
O2 Ru1 O2 85.3(4) . 5 ?
O5 S1 Ru1 119.0(5) . . ?
O5 S1 C1 105.4(8) . . ?
O5 S1 C2 107.2(9) . . ?
C1 S1 Ru1 111.5(6) . . ?
C1 S1 C2 100.4(11) . . ?
C2 S1 Ru1 111.4(6) . . ?
O1 Na1 O1 178.0(5) 2 4 ?
O1 Na1 O1 62.2(4) 2 8 ?
O1 Na1 O1 62.2(4) 5 4 ?
O1 Na1 O1 62.2(4) 10 4 ?
O1 Na1 O1 116.61(12) 2 6 ?
O1 Na1 O1 65.3(4) 6 4 ?
O1 Na1 O1 62.2(4) 9 8 ?
O1 Na1 O1 65.3(4) 9 . ?
O1 Na1 O1 115.86(12) 9 6 ?
O1 Na1 O1 178.0(5) 3 . ?
O1 Na1 O1 65.3(4) 11 4 ?
O1 Na1 O1 117.9(3) 2 . ?
O1 Na1 O1 178.0(5) 12 10 ?
O1 Na1 O1 115.86(12) 10 . ?
O1 Na1 O1 65.3(4) 3 8 ?
O1 Na1 O1 62.2(4) 6 . ?
O1 Na1 O1 65.3(4) 10 8 ?
O1 Na1 O1 178.0(5) 7 5 ?
O1 Na1 O1 115.86(12) 3 6 ?
O1 Na1 O1 116.61(12) 3 5 ?
O1 Na1 O1 116.61(12) 10 6 ?
O1 Na1 O1 115.86(12) 11 2 ?
O1 Na1 O1 116.61(12) 7 4 ?
O1 Na1 O1 62.2(4) 9 2 ?
O1 Na1 O1 62.2(4) 5 10 ?
O1 Na1 O1 65.3(4) 7 2 ?
O1 Na1 O1 116.61(12) 11 8 ?
O1 Na1 O1 62.2(3) 3 2 ?
O1 Na1 O1 117.9(3) 7 8 ?
O1 Na1 O1 115.86(12) 5 2 ?
O1 Na1 O1 62.2(3) 5 8 ?
O1 Na1 O1 117.9(3) 11 12 ?
O1 Na1 O1 115.86(12) 12 8 ?
O1 Na1 O1 62.2(3) 9 12 ?
O1 Na1 O1 65.3(4) 11 6 ?
O1 Na1 O1 65.3(4) 7 12 ?
O1 Na1 O1 62.2(3) 7 6 ?
O1 Na1 O1 116.61(12) 3 12 ?
O1 Na1 O1 117.9(3) 5 6 ?
O1 Na1 O1 116.61(12) 5 12 ?
O1 Na1 O1 62.2(4) 12 6 ?
O1 Na1 O1 65.3(4) 2 12 ?
O1 Na1 O1 178.0(5) 8 6 ?
O1 Na1 O1 62.2(3) 11 10 ?
O1 Na1 O1 116.61(12) 9 4 ?
O1 Na1 O1 117.9(3) 9 10 ?
O1 Na1 O1 117.9(3) 3 4 ?
O1 Na1 O1 115.86(12) 7 10 ?
O1 Na1 O1 65.3(4) 3 10 ?
O1 Na1 O1 115.86(12) 12 4 ?
O1 Na1 O1 178.0(5) 11 9 ?
O1 Na1 O1 115.86(12) 8 4 ?
O1 Na1 O1 62.2(4) 11 7 ?
O1 Na1 O1 116.61(12) 11 . ?
O1 Na1 O1 116.61(12) 9 7 ?
O1 Na1 O1 115.86(12) 7 . ?
O1 Na1 O1 62.2(4) 11 3 ?
O1 Na1 O1 65.3(4) 5 . ?
O1 Na1 O1 115.86(12) 9 3 ?
O1 Na1 O1 62.2(4) 12 . ?
O1 Na1 O1 62.2(4) 7 3 ?
O1 Na1 O1 116.61(12) 8 . ?
O1 Na1 O1 115.86(12) 11 5 ?
O1 Na1 O1 62.2(3) 4 . ?
O1 Na1 O1 65.3(4) 9 5 ?
O1 Na1 O1 116.61(12) 2 10 ?
O3 Na2 O3 82.1(4) . 12 ?
O3 Na2 O3 82.1(4) . 6 ?
O3 Na2 O3 82.1(4) 12 6 ?
O3 Na2 O5 86.0(3) 12 16_454 ?
O3 Na2 O5 163.9(4) 6 23_454 ?
O3 Na2 O5 86.0(3) . 23_454 ?
O3 Na2 O5 107.1(4) 6 16_454 ?
O3 Na2 O5 107.1(4) . 18_454 ?
O3 Na2 O5 107.1(4) 12 23_454 ?
O3 Na2 O5 163.9(4) 12 18_454 ?
O3 Na2 O5 86.0(3) 6 18_454 ?
O3 Na2 O5 163.9(4) . 16_454 ?
O5 Na2 O5 87.1(4) 18_454 23_454 ?
O5 Na2 O5 87.1(4) 16_454 23_454 ?
O5 Na2 O5 87.1(4) 18_454 16_454 ?
W1 O1 W1 134.4(6) . 6 ?
W1 O1 W1 134.4(5) . 5 ?
W1 O1 W1 87.6(2) 6 5 ?
W1 O1 Na1 93.7(3) 6 . ?
W1 O1 Na1 91.0(3) 5 . ?
W1 O1 Na1 100.8(2) . . ?
W1 O2 Ru1 148.3(5) . . ?
W1 O3 Na2 143.4(6) . . ?
W1 O4 W1 105.2(4) . 2 ?
S1 O5 Na2 122.5(6) . 15_444 ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.01(2)
2 -0.01(2)

