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

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

data_compound-1
_database_code_depnum_ccdc_archive 'CCDC 1812090'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-03-26 downloaded from the CCDC.
;
_audit_creation_date             2017-09-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C240 H80 Cd4 N16 O96)'
_chemical_formula_sum            'C60 H20 Cd N4 O24'
_chemical_formula_weight         1293.20
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_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           15
_space_group_name_H-M_alt        'I 1 2/c 1'
_space_group_name_Hall           '-I 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z'


_cell_length_a                   18.5534(2)
_cell_length_b                   22.8539(3)
_cell_length_c                   20.0964(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.3541(15)
_cell_angle_gamma                90
_cell_volume                     8133.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16781
_cell_measurement_temperature    291.11(10)
_cell_measurement_theta_max      71.5260
_cell_measurement_theta_min      4.8180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.700
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37591
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.754
_diffrn_reflns_theta_min         4.610
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -31.00   53.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703  -57.0000  120.0000 84


#__ type_ start__ end____ width___ exp.time_
  2 omega   10.00  104.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703   77.0000  -60.0000 94


#__ type_ start__ end____ width___ exp.time_
  3 omega    1.00   75.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703  -99.0000  -90.0000 74


#__ type_ start__ end____ width___ exp.time_
  4 omega    1.00   28.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703   92.0000 -113.1244 27


#__ type_ start__ end____ width___ exp.time_
  5 omega   20.00  104.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703   57.0000  120.0000 84


#__ type_ start__ end____ width___ exp.time_
  6 omega  -31.00   53.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703  -57.0000    0.0000 84


#__ type_ start__ end____ width___ exp.time_
  7 omega   55.00  109.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703 -178.0000  -90.0000 54


#__ type_ start__ end____ width___ exp.time_
  8 omega   40.00   98.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58


#__ type_ start__ end____ width___ exp.time_
  9 omega   38.00   91.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53


#__ type_ start__ end____ width___ exp.time_
 10 omega   40.00   98.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58


#__ type_ start__ end____ width___ exp.time_
 11 omega   87.00  178.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -90.0000 91


#__ type_ start__ end____ width___ exp.time_
 12 omega   39.00  110.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -120.0000 71


#__ type_ start__ end____ width___ exp.time_
 13 omega   38.00   91.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53


#__ type_ start__ end____ width___ exp.time_
 14 omega   41.00  126.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -150.0000 85


#__ type_ start__ end____ width___ exp.time_
 15 omega  101.00  178.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  112.0000  -90.0000 77


#__ type_ start__ end____ width___ exp.time_
 16 omega   39.00  110.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 71


#__ type_ start__ end____ width___ exp.time_
 17 omega   81.00  176.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95


#__ type_ start__ end____ width___ exp.time_
 18 omega   20.00  104.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703   57.0000 -150.0000 84


#__ type_ start__ end____ width___ exp.time_
 19 omega    2.00   29.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703   91.0000  118.5628 27


#__ type_ start__ end____ width___ exp.time_
 20 omega   18.00  106.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703   38.0000   60.0000 88


#__ type_ start__ end____ width___ exp.time_
 21 omega  -33.00   55.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703  -38.0000 -120.0000 88


#__ type_ start__ end____ width___ exp.time_
 22 omega  -31.00   53.00   1.0000    3.6400
omega____ theta____ kappa____ phi______ frames
    -       36.4703  -57.0000   60.0000 84


#__ type_ start__ end____ width___ exp.time_
 23 omega   87.00  178.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 91


#__ type_ start__ end____ width___ exp.time_
 24 omega   91.00  176.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85


#__ type_ start__ end____ width___ exp.time_
 25 omega   87.00  178.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -150.0000 91


#__ type_ start__ end____ width___ exp.time_
 26 omega   91.00  176.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 85


#__ type_ start__ end____ width___ exp.time_
 27 omega   90.00  159.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   30.0000 69


#__ type_ start__ end____ width___ exp.time_
 28 omega   39.00  110.00   1.0000   14.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000    0.0000 71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6972
_reflns_number_total             7885
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.669
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7885
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0550
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1029P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1555
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.025
3.a Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C5(H5), C7(H7), C13(H13), C14(H14), C18(H18), C20(H20), C22(H22),
 C28(H28), C29(H29)
;
_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
Cd1 Cd 0.5000 0.70678(2) 0.2500 0.02483(12) Uani 1 2 d S T P . .
O1 O 0.28484(14) 0.88138(14) 0.46094(14) 0.0501(7) Uani 1 1 d . . . . .
O2 O 0.34486(17) 0.88380(14) 0.57514(14) 0.0537(7) Uani 1 1 d . . . . .
O3 O 0.63321(18) 0.88639(13) 0.62307(17) 0.0610(8) Uani 1 1 d . . . . .
O4 O 0.55903(19) 0.69657(14) 0.59026(18) 0.0646(9) Uani 1 1 d . . . . .
O5 O 0.53155(13) 0.76326(11) 0.34488(12) 0.0370(5) Uani 1 1 d . . . . .
O6 O 0.40821(14) 0.77961(12) 0.30552(12) 0.0399(5) Uani 1 1 d . . . . .
O7 O 0.55095(13) 0.63723(12) 0.18786(14) 0.0451(6) Uani 1 1 d . . . . .
O8 O 0.62278(12) 0.66546(11) 0.29126(12) 0.0360(5) Uani 1 1 d . . . . .
O9 O 0.6657(4) 0.4995(3) 0.0499(2) 0.142(3) Uani 1 1 d . U . . .
O10 O 0.7469(2) 0.43636(18) 0.11188(19) 0.0756(11) Uani 1 1 d . . . . .
O11 O 0.76562(13) 0.49191(13) 0.40683(15) 0.0493(7) Uani 1 1 d . . . . .
O12 O 0.92773(15) 0.55731(15) 0.29204(15) 0.0559(8) Uani 1 1 d . . . . .
N1 N 0.59828(18) 0.79106(13) 0.60514(16) 0.0395(7) Uani 1 1 d . . . . .
N2 N 0.84695(15) 0.52698(12) 0.35087(16) 0.0357(6) Uani 1 1 d . . . . .
C0AA C 0.3397(2) 0.87244(16) 0.50979(18) 0.0376(7) Uani 1 1 d . . . . .
C1AA C 0.40926(18) 0.84500(15) 0.50034(17) 0.0344(7) Uani 1 1 d . . . . .
C2AA C 0.4726(2) 0.83368(16) 0.55743(17) 0.0385(7) Uani 1 1 d . . . . .
H2AA H 0.4728 0.8437 0.6023 0.046 Uiso 1 1 calc R . . . .
C4 C 0.5349(2) 0.80730(17) 0.54597(18) 0.0379(7) Uani 1 1 d . . . . .
C5 C 0.5362(2) 0.79247(15) 0.48009(19) 0.0363(7) Uani 1 1 d . . . . .
H5 H 0.5793 0.7759 0.4734 0.044 Uiso 1 1 calc R . . . .
C6 C 0.47223(19) 0.80248(15) 0.42319(18) 0.0341(7) Uani 1 1 d . . . . .
C7 C 0.40896(17) 0.82920(15) 0.43383(16) 0.0323(6) Uani 1 1 d . . . . .
H7 H 0.3665 0.8364 0.3961 0.039 Uiso 1 1 calc R . . . .
C8 C 0.6460(2) 0.83581(16) 0.6406(2) 0.0421(8) Uani 1 1 d . . . . .
C9 C 0.7108(2) 0.81780(17) 0.7010(2) 0.0448(8) Uani 1 1 d . . . . .
C10 C 0.71943(19) 0.75818(16) 0.72101(18) 0.0388(8) Uani 1 1 d . . . . .
C11 C 0.6696(2) 0.71505(16) 0.6839(2) 0.0466(9) Uani 1 1 d . . . . .
C12 C 0.6043(2) 0.73189(17) 0.6234(2) 0.0442(8) Uani 1 1 d . . . . .
C13 C 0.7604(3) 0.85894(18) 0.7366(3) 0.0628(13) Uani 1 1 d . . . . .
H13 H 0.7546 0.8978 0.7222 0.075 Uiso 1 1 calc R . . . .
C14 C 0.6793(3) 0.65713(19) 0.7047(3) 0.0646(13) Uani 1 1 d . . . . .
H14 H 0.6461 0.6288 0.6800 0.078 Uiso 1 1 calc R . . . .
C15 C 0.47015(19) 0.78103(15) 0.35158(18) 0.0337(7) Uani 1 1 d . . . . .
C16 C 0.61002(17) 0.63456(13) 0.23750(17) 0.0309(6) Uani 1 1 d . . . . .
C17 C 0.66961(17) 0.59038(14) 0.23381(17) 0.0323(6) Uani 1 1 d . . . . .
C18 C 0.73160(17) 0.58131(14) 0.29158(17) 0.0303(6) Uani 1 1 d . . . . .
H18 H 0.7382 0.6038 0.3316 0.036 Uiso 1 1 calc R . . . .
C19 C 0.78358(17) 0.53873(14) 0.28942(18) 0.0334(7) Uani 1 1 d . . . . .
C20 C 0.7759(2) 0.50628(16) 0.2296(2) 0.0415(8) Uani 1 1 d . . . . .
H20 H 0.8114 0.4778 0.2288 0.050 Uiso 1 1 calc R . . . .
C21 C 0.7153(2) 0.51621(18) 0.1709(2) 0.0445(8) Uani 1 1 d . . . . .
C22 C 0.6612(2) 0.55863(17) 0.1734(2) 0.0427(8) Uani 1 1 d . . . . .
H22 H 0.6198 0.5653 0.1345 0.051 Uiso 1 1 calc R . . . .
C23 C 0.83017(18) 0.50337(15) 0.4088(2) 0.0389(7) Uani 1 1 d . . . . .
C24 C 0.89489(18) 0.49411(15) 0.4722(2) 0.0387(7) Uani 1 1 d . . . . .
C25 C 0.96924(17) 0.50509(14) 0.46982(18) 0.0340(7) Uani 1 1 d . . . . .
C26 C 0.98290(19) 0.52570(16) 0.4086(2) 0.0414(8) Uani 1 1 d . . . . .
C27 C 0.91884(19) 0.53825(17) 0.3456(2) 0.0424(8) Uani 1 1 d . . . . .
C28 C 0.8829(2) 0.47597(18) 0.5332(2) 0.0476(9) Uani 1 1 d . . . . .
H28 H 0.8338 0.4701 0.5347 0.057 Uiso 1 1 calc R . . . .
C29 C 1.0561(2) 0.53381(18) 0.4067(2) 0.0477(9) Uani 1 1 d . . . . .
H29 H 1.0649 0.5458 0.3656 0.057 Uiso 1 1 calc R . . . .
C30 C 0.7083(3) 0.4820(2) 0.1052(3) 0.0637(12) 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
Cd1 O5 2.231(2) 2_655 ?
Cd1 O5 2.231(2) . ?
Cd1 O7 2.384(2) 2_655 ?
Cd1 O7 2.384(2) . ?
Cd1 O8 2.375(2) . ?
Cd1 O8 2.375(2) 2_655 ?
Cd1 C16 2.694(3) . ?
Cd1 C16 2.694(3) 2_655 ?
O1 C0AA 1.202(4) . ?
O2 C0AA 1.314(4) . ?
O3 C8 1.211(5) . ?
O4 C12 1.211(5) . ?
O5 C15 1.254(4) . ?
O6 C15 1.242(4) . ?
O7 C16 1.244(4) . ?
O8 C16 1.253(4) . ?
O9 C30 1.222(7) . ?
O10 C30 1.250(6) . ?
O11 C23 1.215(4) . ?
O12 C27 1.217(5) . ?
N1 C4 1.449(4) . ?
N1 C8 1.401(5) . ?
N1 C12 1.397(5) . ?
N2 C19 1.454(4) . ?
N2 C23 1.399(5) . ?
N2 C27 1.393(4) . ?
C0AA C1AA 1.497(4) . ?
C1AA C2AA 1.400(4) . ?
C1AA C7 1.383(4) . ?
C2AA C4 1.382(5) . ?
C4 C5 1.374(5) . ?
C5 C6 1.399(5) . ?
C6 C7 1.395(5) . ?
C6 C15 1.510(5) . ?
C8 C9 1.488(5) . ?
C9 C10 1.416(5) . ?
C9 C13 1.361(6) . ?
C10 C10 1.413(6) 7_666 ?
C10 C11 1.404(5) . ?
C11 C12 1.489(5) . ?
C11 C14 1.384(6) . ?
C13 C14 1.410(6) 7_666 ?
C14 C13 1.410(6) 7_666 ?
C16 C17 1.515(4) . ?
C17 C18 1.385(4) . ?
C17 C22 1.383(5) . ?
C18 C19 1.380(4) . ?
C19 C20 1.383(5) . ?
C20 C21 1.384(5) . ?
C21 C22 1.408(5) . ?
C21 C30 1.505(6) . ?
C23 C24 1.483(5) . ?
C24 C25 1.417(4) . ?
C24 C28 1.373(5) . ?
C25 C25 1.415(6) 5_766 ?
C25 C26 1.409(5) . ?
C26 C27 1.483(5) . ?
C26 C29 1.381(5) . ?
C28 C29 1.406(5) 5_766 ?
C29 C28 1.406(5) 5_766 ?


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
O5 Cd1 O5 109.30(13) 2_655 . ?
O5 Cd1 O7 88.97(10) 2_655 . ?
O5 Cd1 O7 142.13(8) . . ?
O5 Cd1 O7 88.97(10) . 2_655 ?
O5 Cd1 O7 142.13(8) 2_655 2_655 ?
O5 Cd1 O8 120.54(8) 2_655 . ?
O5 Cd1 O8 87.24(8) 2_655 2_655 ?
O5 Cd1 O8 87.24(8) . . ?
O5 Cd1 O8 120.54(8) . 2_655 ?
O5 Cd1 C16 114.90(9) . . ?
O5 Cd1 C16 114.90(9) 2_655 2_655 ?
O5 Cd1 C16 106.72(9) . 2_655 ?
O5 Cd1 C16 106.72(9) 2_655 . ?
O7 Cd1 O7 96.37(15) . 2_655 ?
O7 Cd1 C16 94.03(9) . 2_655 ?
O7 Cd1 C16 94.03(9) 2_655 . ?
O7 Cd1 C16 27.50(9) 2_655 2_655 ?
O7 Cd1 C16 27.50(9) . . ?
O8 Cd1 O7 92.34(8) . 2_655 ?
O8 Cd1 O7 55.18(8) 2_655 2_655 ?
O8 Cd1 O7 55.18(8) . . ?
O8 Cd1 O7 92.34(8) 2_655 . ?
O8 Cd1 O8 133.15(12) . 2_655 ?
O8 Cd1 C16 113.47(9) . 2_655 ?
O8 Cd1 C16 113.47(9) 2_655 . ?
O8 Cd1 C16 27.71(9) . . ?
O8 Cd1 C16 27.71(9) 2_655 2_655 ?
C16 Cd1 C16 104.45(13) . 2_655 ?
C15 O5 Cd1 105.3(2) . . ?
C16 O7 Cd1 90.27(19) . . ?
C16 O8 Cd1 90.47(18) . . ?
C8 N1 C4 117.8(3) . . ?
C12 N1 C4 116.4(3) . . ?
C12 N1 C8 125.8(3) . . ?
C23 N2 C19 117.0(3) . . ?
C27 N2 C19 116.8(3) . . ?
C27 N2 C23 126.2(3) . . ?
O1 C0AA O2 125.1(3) . . ?
O1 C0AA C1AA 121.3(3) . . ?
O2 C0AA C1AA 113.6(3) . . ?
C2AA C1AA C0AA 121.2(3) . . ?
C7 C1AA C0AA 118.5(3) . . ?
C7 C1AA C2AA 120.3(3) . . ?
C4 C2AA C1AA 118.9(3) . . ?
C2AA C4 N1 119.3(3) . . ?
C5 C4 N1 119.0(3) . . ?
C5 C4 C2AA 121.6(3) . . ?
C4 C5 C6 119.5(3) . . ?
C5 C6 C15 120.0(3) . . ?
C7 C6 C5 119.6(3) . . ?
C7 C6 C15 120.3(3) . . ?
C1AA C7 C6 120.1(3) . . ?
O3 C8 N1 120.6(3) . . ?
O3 C8 C9 122.8(4) . . ?
N1 C8 C9 116.6(3) . . ?
C10 C9 C8 119.6(3) . . ?
C13 C9 C8 119.5(4) . . ?
C13 C9 C10 120.9(3) . . ?
C10 C10 C9 118.9(4) 7_666 . ?
C11 C10 C9 121.6(3) . . ?
C11 C10 C10 119.5(4) . 7_666 ?
C10 C11 C12 119.9(3) . . ?
C14 C11 C10 120.3(3) . . ?
C14 C11 C12 119.7(4) . . ?
O4 C12 N1 120.9(3) . . ?
O4 C12 C11 122.6(4) . . ?
N1 C12 C11 116.5(3) . . ?
C9 C13 C14 120.2(4) . 7_666 ?
C11 C14 C13 120.1(4) . 7_666 ?
O5 C15 C6 116.2(3) . . ?
O6 C15 O5 125.4(3) . . ?
O6 C15 C6 118.3(3) . . ?
O7 C16 Cd1 62.23(16) . . ?
O7 C16 O8 124.0(3) . . ?
O7 C16 C17 118.3(3) . . ?
O8 C16 Cd1 61.82(15) . . ?
O8 C16 C17 117.7(3) . . ?
C17 C16 Cd1 175.4(2) . . ?
C18 C17 C16 119.6(3) . . ?
C22 C17 C16 120.0(3) . . ?
C22 C17 C18 120.4(3) . . ?
C19 C18 C17 119.5(3) . . ?
C18 C19 N2 119.9(3) . . ?
C18 C19 C20 120.9(3) . . ?
C20 C19 N2 119.1(3) . . ?
C19 C20 C21 120.0(3) . . ?
C20 C21 C22 119.3(3) . . ?
C20 C21 C30 119.9(3) . . ?
C22 C21 C30 120.8(4) . . ?
C17 C22 C21 119.9(3) . . ?
O11 C23 N2 121.2(3) . . ?
O11 C23 C24 122.3(3) . . ?
N2 C23 C24 116.5(3) . . ?
C25 C24 C23 119.5(3) . . ?
C28 C24 C23 120.3(3) . . ?
C28 C24 C25 120.2(3) . . ?
C25 C25 C24 119.1(4) 5_766 . ?
C26 C25 C24 121.3(3) . . ?
C26 C25 C25 119.6(4) . 5_766 ?
C25 C26 C27 120.2(3) . . ?
C29 C26 C25 120.2(3) . . ?
C29 C26 C27 119.6(3) . . ?
O12 C27 N2 121.3(3) . . ?
O12 C27 C26 122.6(3) . . ?
N2 C27 C26 116.2(3) . . ?
C24 C28 C29 120.7(3) . 5_766 ?
C26 C29 C28 120.1(4) . 5_766 ?
O9 C30 O10 124.3(5) . . ?
O9 C30 C21 119.4(4) . . ?
O10 C30 C21 116.2(4) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.007 -0.001 -0.009 3735 992 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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-2
_database_code_depnum_ccdc_archive 'CCDC 1812091'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-03-26 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C136 H52 N16 O56 Zn8)'
_chemical_formula_sum            'C34 H13 N4 O14 Zn2'
_chemical_formula_weight         832.22
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P b n m'
_space_group_name_Hall           '-P 2c 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x-1/2, -y-1/2, z-1/2'


_cell_length_a                   10.2186(2)
_cell_length_b                   36.8564(9)
_cell_length_c                   15.2343(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5737.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6986
_cell_measurement_temperature    99.98(2)
_cell_measurement_theta_max      72.5860
_cell_measurement_theta_min      4.4880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.963
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.633
_diffrn_reflns_theta_min         3.765
_diffrn_ambient_temperature      99.98(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4212
_reflns_number_total             5894
_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 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.180
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5894
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0702
_refine_ls_restrained_S_all      1.189
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1240P)²+2.2506P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2314
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Fixed Sof: H19b(0.5) H19a(0.5) H19c(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C9(H9), C12(H12), C14(H14)
4.b Idealised Me refined as rotating group:
 C19(H19b,H19a,H19c)
;
_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
Zn1 Zn 0.34807(5) 0.77734(2) 0.2500 0.0287(2) Uani 1 2 d S T P . .
Zn2 Zn 0.13301(5) 0.72212(2) 0.2500 0.0288(2) Uani 1 2 d S T P . .
O1 O 0.3317(4) 0.59490(8) 0.6003(3) 0.0937(15) Uani 1 1 d . . . . .
O2 O 0.6565(4) 0.59642(9) 0.4009(3) 0.0979(15) Uani 1 1 d . U . . .
O3 O 0.7398(3) 0.69641(7) 0.6580(2) 0.0604(9) Uani 1 1 d . . . . .
O4 O 0.5887(3) 0.74057(7) 0.65481(16) 0.0454(6) Uani 1 1 d . . . . .
O5 O 0.2396(3) 0.69570(7) 0.3409(2) 0.0638(9) Uani 1 1 d . . . . .
O6 O 0.3920(3) 0.74013(7) 0.3441(2) 0.0534(7) Uani 1 1 d . . . . .
O7 O 0.5082(4) 0.80611(11) 0.2500 0.0724(15) Uani 1 2 d S T P . .
O8 O -0.0271(4) 0.69352(11) 0.2500 0.0654(13) Uani 1 2 d S T P . .
N1 N 0.4937(3) 0.59528(8) 0.4992(2) 0.0476(8) Uani 1 1 d . . . . .
N2 N 0.7185(6) 0.8176(2) 0.2500 0.120(3) Uani 1 2 d S T P . .
N3 N -0.2397(6) 0.6830(2) 0.2500 0.115(3) Uani 1 2 d S T P . .
C1 C 0.3267(6) 0.51843(12) 0.6098(5) 0.087(2) Uani 1 1 d . . . . .
H1 H 0.2686 0.5310 0.6479 0.105 Uiso 1 1 calc R . . . .
C2 C 0.4097(5) 0.53733(10) 0.5553(4) 0.0617(12) Uani 1 1 d . . . . .
C3 C 0.4986(4) 0.51925(9) 0.5000(3) 0.0505(10) Uani 1 1 d . . . . .
C4 C 0.5845(5) 0.53825(10) 0.4449(3) 0.0611(12) Uani 1 1 d . . . . .
C5 C 0.6708(6) 0.51996(12) 0.3916(5) 0.087(2) Uani 1 1 d . . . . .
H5 H 0.7294 0.5332 0.3553 0.104 Uiso 1 1 calc R . . . .
C6 C 0.5834(5) 0.57876(11) 0.4440(4) 0.0637(13) Uani 1 1 d . . . . .
C7 C 0.4057(5) 0.57787(10) 0.5559(3) 0.0590(12) Uani 1 1 d . . . . .
C8 C 0.4913(3) 0.63433(9) 0.4996(3) 0.0438(8) Uani 1 1 d . . . . .
C9 C 0.5676(4) 0.65292(9) 0.5600(2) 0.0422(8) Uani 1 1 d . . . . .
H9 H 0.6216 0.6401 0.6001 0.051 Uiso 1 1 calc R . . . .
C10 C 0.5640(3) 0.69074(9) 0.5611(2) 0.0371(7) Uani 1 1 d . . . . .
C11 C 0.6369(4) 0.71086(10) 0.6304(3) 0.0440(9) Uani 1 1 d . . . . .
C12 C 0.4896(3) 0.70939(8) 0.4998(2) 0.0337(7) Uani 1 1 d . . . . .
H12 H 0.4891 0.7352 0.4993 0.040 Uiso 1 1 calc R . . . .
C13 C 0.4164(4) 0.69026(9) 0.4394(2) 0.0394(8) Uani 1 1 d . . . . .
C14 C 0.4148(4) 0.65249(9) 0.4403(3) 0.0426(8) Uani 1 1 d . . . . .
H14 H 0.3613 0.6395 0.4002 0.051 Uiso 1 1 calc R . . . .
C15 C 0.3423(4) 0.71041(9) 0.3682(3) 0.0436(9) Uani 1 1 d . . . . .
C16 C -0.3686(8) 0.6706(3) 0.2500 0.131(5) Uani 1 2 d S TU P . .
C17 C -0.1341(7) 0.6890(2) 0.2500 0.091(3) Uani 1 2 d S TU P . .
C18 C 0.6163(7) 0.8105(2) 0.2500 0.091(3) Uani 1 2 d S TU P . .
C19 C 0.8457(8) 0.8307(3) 0.2500 0.130(5) Uani 1 2 d S TU P . .
H19A H 0.8814 0.8294 0.3096 0.195 Uiso 0.5 1 calc GR . . A -1
H19B H 0.8461 0.8559 0.2298 0.195 Uiso 0.5 1 calc GR . . A -1
H19C H 0.8995 0.8159 0.2106 0.195 Uiso 0.5 1 calc GR . . A -1




_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
Zn1 Zn2 2.9951(8) . ?
Zn1 O3 2.030(3) 3_466 ?
Zn1 O3 2.030(3) 8_575 ?
Zn1 O6 2.034(3) 6_556 ?
Zn1 O6 2.034(3) . ?
Zn1 O7 1.950(4) . ?
Zn2 O4 2.049(2) 3_466 ?
Zn2 O4 2.049(2) 8_575 ?
Zn2 O5 2.014(3) . ?
Zn2 O5 2.013(3) 6_556 ?
Zn2 O8 1.946(4) . ?
O1 C7 1.193(6) . ?
O2 C6 1.188(6) . ?
O3 Zn1 2.030(3) 3_566 ?
O3 C11 1.252(5) . ?
O4 Zn2 2.049(2) 3_566 ?
O4 C11 1.257(5) . ?
O5 C15 1.252(5) . ?
O6 C15 1.262(5) . ?
O7 C18 1.116(8) . ?
O8 C17 1.106(8) . ?
N1 C6 1.386(6) . ?
N1 C7 1.403(6) . ?
N1 C8 1.439(4) . ?
N2 C18 1.077(9) . ?
N2 C19 1.386(9) . ?
N3 C16 1.394(9) . ?
N3 C17 1.102(9) . ?
C1 C2 1.376(7) . ?
C1 C5 1.415(6) 5_666 ?
C2 C3 1.407(6) . ?
C2 C7 1.495(5) . ?
C3 C3 1.419(7) 5_666 ?
C3 C4 1.402(6) . ?
C4 C5 1.375(7) . ?
C4 C6 1.493(5) . ?
C5 C1 1.415(6) 5_666 ?
C8 C9 1.386(5) . ?
C8 C14 1.370(5) . ?
C9 C10 1.395(4) . ?
C10 C11 1.491(5) . ?
C10 C12 1.386(4) . ?
C12 C13 1.379(4) . ?
C13 C14 1.392(4) . ?
C13 C15 1.517(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
O3 Zn1 Zn2 85.65(9) 3_466 . ?
O3 Zn1 Zn2 85.65(9) 8_575 . ?
O3 Zn1 O3 87.3(2) 8_575 3_466 ?
O3 Zn1 O6 158.11(13) 3_466 6_556 ?
O3 Zn1 O6 87.44(13) 8_575 6_556 ?
O3 Zn1 O6 87.44(13) 3_466 . ?
O3 Zn1 O6 158.11(13) 8_575 . ?
O6 Zn1 Zn2 72.78(8) 6_556 . ?
O6 Zn1 Zn2 72.78(8) . . ?
O6 Zn1 O6 89.60(17) . 6_556 ?
O7 Zn1 Zn2 170.14(13) . . ?
O7 Zn1 O3 101.42(13) . 8_575 ?
O7 Zn1 O3 101.42(13) . 3_466 ?
O7 Zn1 O6 100.45(12) . . ?
O7 Zn1 O6 100.45(12) . 6_556 ?
O4 Zn2 Zn1 72.92(8) 8_575 . ?
O4 Zn2 Zn1 72.92(8) 3_466 . ?
O4 Zn2 O4 90.11(15) 3_466 8_575 ?
O5 Zn2 Zn1 86.08(9) . . ?
O5 Zn2 Zn1 86.08(9) 6_556 . ?
O5 Zn2 O4 158.59(13) . 8_575 ?
O5 Zn2 O4 87.55(12) . 3_466 ?
O5 Zn2 O4 87.55(12) 6_556 8_575 ?
O5 Zn2 O4 158.59(13) 6_556 3_466 ?
O5 Zn2 O5 86.9(2) 6_556 . ?
O8 Zn2 Zn1 169.99(13) . . ?
O8 Zn2 O4 100.23(12) . 3_466 ?
O8 Zn2 O4 100.23(12) . 8_575 ?
O8 Zn2 O5 101.12(13) . 6_556 ?
O8 Zn2 O5 101.12(13) . . ?
C11 O3 Zn1 119.1(3) . 3_566 ?
C11 O4 Zn2 135.0(3) . 3_566 ?
C15 O5 Zn2 118.2(3) . . ?
C15 O6 Zn1 134.6(2) . . ?
C18 O7 Zn1 155.4(5) . . ?
C17 O8 Zn2 155.8(5) . . ?
C6 N1 C7 126.7(3) . . ?
C6 N1 C8 116.9(3) . . ?
C7 N1 C8 116.4(3) . . ?
C18 N2 C19 173.8(11) . . ?
C17 N3 C16 172.5(11) . . ?
C2 C1 C5 119.1(4) . 5_666 ?
C1 C2 C3 121.3(4) . . ?
C1 C2 C7 119.1(4) . . ?
C3 C2 C7 119.7(4) . . ?
C2 C3 C3 119.1(5) . 5_666 ?
C4 C3 C2 121.8(4) . . ?
C4 C3 C3 119.1(5) . 5_666 ?
C3 C4 C6 120.0(4) . . ?
C5 C4 C3 120.7(4) . . ?
C5 C4 C6 119.3(4) . . ?
C4 C5 C1 120.7(4) . 5_666 ?
O2 C6 N1 120.7(4) . . ?
O2 C6 C4 123.2(5) . . ?
N1 C6 C4 116.0(4) . . ?
O1 C7 N1 121.0(4) . . ?
O1 C7 C2 123.1(5) . . ?
N1 C7 C2 115.9(4) . . ?
C9 C8 N1 119.2(3) . . ?
C14 C8 N1 119.7(3) . . ?
C14 C8 C9 121.1(3) . . ?
C8 C9 C10 119.2(3) . . ?
C9 C10 C11 119.5(3) . . ?
C12 C10 C9 120.1(3) . . ?
C12 C10 C11 120.3(3) . . ?
O3 C11 O4 126.9(4) . . ?
O3 C11 C10 116.5(3) . . ?
O4 C11 C10 116.5(3) . . ?
C13 C12 C10 119.5(3) . . ?
C12 C13 C14 120.8(3) . . ?
C12 C13 C15 119.8(3) . . ?
C14 C13 C15 119.4(3) . . ?
C8 C14 C13 119.2(3) . . ?
O5 C15 O6 128.0(3) . . ?
O5 C15 C13 116.3(3) . . ?
O6 C15 C13 115.6(3) . . ?
N3 C17 O8 177.0(10) . . ?
N2 C18 O7 174.3(10) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.380 0.032 0.237 3086 669 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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-3
_database_code_depnum_ccdc_archive 'CCDC 1812092'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-03-26 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C71 H40 Ba4 N9 O31'
_chemical_formula_sum            'C71 H40 Ba4 N9 O31'
_chemical_formula_weight         2064.48
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -1.0456 8.4617 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'


_cell_length_a                   23.4194(4)
_cell_length_b                   13.9077(2)
_cell_length_c                   33.6040(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.9341(16)
_cell_angle_gamma                90
_cell_volume                     10943.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26951
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.6840
_cell_measurement_theta_min      4.4880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.601
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4004
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            102162
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.964
_diffrn_reflns_theta_min         3.696
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):


  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -21.00   1.00    6.11    --  -37.46 -57.00-180.00   84
  2  ω   -105.00 -11.00   1.00    6.11    --  -37.46 -77.00 -30.00   94
  3  ω     19.00 107.00   1.00    6.11    --   37.46  38.00 -30.00   88
  4  ω      1.00  76.00   1.00    6.11    --   37.46 -99.00  60.00   75
  5  ω     21.00 105.00   1.00    6.11    --   37.46  57.00  90.00   84
  6  ω      1.00  76.00   1.00    6.11    --   37.46 -99.00 -90.00   75
  7  ω    -30.00  54.00   1.00    6.11    --   37.46 -57.00  90.00   84
  8  ω     24.00  91.00   1.00    6.11    --   37.46-126.00-120.00   67
  9  ω    -32.00  56.00   1.00    6.11    --   37.46 -38.00 150.00   88
 10  ω    -32.00  56.00   1.00    6.11    --   37.46 -38.00   0.00   88
 11  ω     41.00 109.00   1.00   24.45    --  110.47 -95.00-120.00   68
 12  ω     44.00 129.00   1.00   24.45    --  110.47 -61.00 -60.00   85
 13  ω     41.00 132.00   1.00   24.45    --  110.47 -30.00 120.00   91
 14  ω     40.00 149.00   1.00   24.45    --  110.47 -15.00 -90.00  109
 15  ω     41.00 116.00   1.00   24.45    --  110.47-112.00-180.00   75
 16  ω     89.00 178.00   1.00   24.45    --  110.47  30.00 120.00   89
 17  ω     41.00 132.00   1.00   24.45    --  110.47 -30.00  30.00   91
 18  ω     44.00 129.00   1.00   24.45    --  110.47 -61.00-150.00   85
 19  ω   -105.00 -11.00   1.00    6.11    --  -37.46 -77.00-120.00   94
 20  ω   -105.00 -11.00   1.00    6.11    --  -37.46 -77.00  60.00   94
 21  ω   -105.00 -11.00   1.00    6.11    --  -37.46 -77.00-180.00   94
 22  ω   -105.00 -11.00   1.00    6.11    --  -37.46 -77.00 120.00   94
 23  ω    -32.00  56.00   1.00    6.11    --   37.46 -38.00-150.00   88
 24  ω    -30.00  54.00   1.00    6.11    --   37.46 -57.00 -60.00   84
 25  ω     21.00 105.00   1.00    6.11    --   37.46  57.00  60.00   84
 26  ω     19.00 107.00   1.00    6.11    --   37.46  38.00-150.00   88
 27  ω     72.00 130.00   1.00   24.45    --  110.47  15.00  60.00   58
 28  ω     72.00 178.00   1.00   24.45    --  110.47  15.00 -30.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11986
_reflns_number_total             21513
_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       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         3.271
_refine_diff_density_min         -2.306
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         21513
_refine_ls_number_restraints     126
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0981
_refine_ls_restrained_S_all      1.176
_refine_ls_shift/su_max          2.127
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1562P)²+40.6871P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2966
_refine_ls_wR_factor_ref         0.3198
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C41) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C62) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O31) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C14(H14), C15(H15), C19(H19), C20(H20), C24(H24),
 C26(H26), C28(H28), C33(H33), C36(H36), C38(H38), C44(H44), C45(H45), C49(H49),
  C50(H50), C54(H54), C56(H56), C58(H58), C61(H61), C63(H63), C64(H64),
 C67(H67), C69(H69)
3.b Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C70(H70A,H70B,
 H70C), C71(H71A,H71B,H71C)
;
_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
Ba1 Ba 0.56422(2) -0.09905(4) 0.73959(2) 0.02182(17) Uani 1 1 d . . . . .
Ba2 Ba 0.48541(3) 0.15303(4) 0.69850(2) 0.02274(18) Uani 1 1 d . . . . .
Ba3 Ba -0.06427(3) -0.09953(7) 0.26038(2) 0.0481(2) Uani 1 1 d . . . . .
Ba4 Ba 0.01449(3) 0.15252(7) 0.30146(2) 0.0468(2) Uani 1 1 d . . . . .
O1 O 0.4061(3) -0.4913(5) 0.6955(2) 0.0239(15) Uani 1 1 d . . . . .
O2 O 0.4367(3) -0.4001(4) 0.74630(19) 0.0230(14) Uani 1 1 d . . . . .
O3 O 0.4596(3) -0.0406(5) 0.71338(19) 0.0274(16) Uani 1 1 d . . . . .
O4 O 0.4109(5) 0.0189(6) 0.6614(3) 0.061(3) Uani 1 1 d . . . . .
O5 O 0.2405(4) -0.2563(8) 0.6252(3) 0.068(3) Uani 1 1 d . . . . .
O6 O 0.4091(4) -0.2846(7) 0.5586(3) 0.049(2) Uani 1 1 d . . . . .
O7 O 0.0921(6) -0.2874(12) 0.4417(4) 0.107(5) Uani 1 1 d . U . . .
O8 O 0.2597(5) -0.2562(7) 0.3759(2) 0.057(3) Uani 1 1 d . . . . .
O9 O 0.0945(5) -0.4922(8) 0.3047(3) 0.069(3) Uani 1 1 d . . . . .
O10 O 0.0630(3) -0.3948(7) 0.2541(3) 0.050(2) Uani 1 1 d . . . . .
O11 O 0.0407(3) -0.0423(8) 0.2866(2) 0.051(2) Uani 1 1 d . . . . .
O12 O 0.0879(5) 0.0153(8) 0.3391(3) 0.069(3) Uani 1 1 d . U . . .
O13 O 0.0764(5) -0.2364(8) 0.1715(4) 0.079(4) Uani 1 1 d . . . . .
O14 O 0.0170(3) -0.1549(7) 0.2098(2) 0.046(2) Uani 1 1 d . . . . .
O15 O 0.0522(3) 0.1952(8) 0.2275(3) 0.055(3) Uani 1 1 d . . . . .
O16 O 0.0932(6) 0.2755(9) 0.1797(3) 0.083(4) Uani 1 1 d . . . . .
O17 O 0.0890(5) 0.0280(11) 0.0522(3) 0.087(4) Uani 1 1 d . U . . .
O18 O 0.2563(5) 0.0221(7) 0.1255(3) 0.057(3) Uani 1 1 d . . . . .
O19 O 0.2451(4) 0.0215(7) -0.1256(3) 0.052(2) Uani 1 1 d . . . . .
O20 O 0.4098(3) 0.0275(7) -0.0524(3) 0.049(2) Uani 1 1 d . . . . .
O21 O 0.4230(4) -0.2386(5) -0.1707(3) 0.055(3) Uani 1 1 d . . . . .
O22 O 0.4852(3) -0.1576(4) -0.2093(2) 0.0274(16) Uani 1 1 d . . . . .
O23 O 0.4002(3) 0.2779(5) -0.1803(2) 0.0355(18) Uani 1 1 d . U . . .
O24 O 0.4511(3) 0.1998(5) -0.22787(18) 0.0239(15) Uani 1 1 d . . . . .
O25 O 0.6759(7) -0.0426(13) 0.7351(6) 0.159(7) Uani 1 1 d . U . . .
O26 O 0.5645(3) 0.0143(6) 0.6673(2) 0.041(2) Uani 1 1 d . . . . .
O27 O 0.3865(3) 0.2747(6) 0.7027(3) 0.039(2) Uani 1 1 d . . . . .
O28 O 0.4524(5) 0.2431(6) 0.6246(3) 0.061(3) Uani 1 1 d . . . . .
O29 O -0.0680(5) 0.0114(9) 0.3335(3) 0.077(3) Uani 1 1 d . . . . .
O30 O 0.0514(6) 0.2407(9) 0.3743(4) 0.087(4) Uani 1 1 d . . . . .
O31 O 0.1141(6) 0.2744(9) 0.2978(4) 0.089(4) Uani 1 1 d . U . . .
N1 N 0.3246(4) -0.2696(6) 0.5913(3) 0.030(2) Uani 1 1 d . . . . .
N2 N 0.1763(6) -0.2670(9) 0.4085(3) 0.060(4) Uani 1 1 d . . . . .
N3 N 0.1722(6) 0.0188(9) 0.0893(3) 0.066(4) Uani 1 1 d . . . . .
N4 N 0.3285(4) 0.0180(6) -0.0880(3) 0.028(2) Uani 1 1 d . . . . .
N5 N 0.1991(10) 0.2220(18) 0.3075(7) 0.143(8) Uani 1 1 d . U . . .
N6 N 0.0311(6) 0.3945(12) 0.4002(5) 0.074(4) Uani 1 1 d . U . . .
N7 N 0.2966(6) 0.2260(11) 0.6922(5) 0.079(4) Uani 1 1 d . U . . .
N8 N 0.6090(8) 0.0307(14) 0.6089(4) 0.120(6) Uani 1 1 d . U . . .
N9 N 0.4696(5) 0.3910(6) 0.5985(3) 0.037(2) Uani 1 1 d . . . . .
C1 C 0.4164(4) -0.4109(6) 0.7114(3) 0.022(2) Uani 1 1 d . . . . .
C2 C 0.4009(5) -0.3209(7) 0.6869(2) 0.026(2) Uani 1 1 d . . . . .
C3 C 0.4185(4) -0.2287(7) 0.6983(3) 0.021(2) Uani 1 1 d . . . . .
H3 H 0.4388 -0.2187 0.7226 0.026 Uiso 1 1 calc R . . . .
C4 C 0.4057(4) -0.1526(7) 0.6734(3) 0.025(2) Uani 1 1 d . U . . .
C5 C 0.4281(4) -0.0497(6) 0.6845(3) 0.027(2) Uani 1 1 d . . . . .
C6 C 0.3751(5) -0.1643(7) 0.6392(3) 0.030(2) Uani 1 1 d . U . . .
H6 H 0.3671 -0.1109 0.6224 0.036 Uiso 1 1 calc R . . . .
C7 C 0.3556(6) -0.2560(7) 0.6290(3) 0.038(3) Uani 1 1 d . . . . .
C8 C 0.3693(5) -0.3336(7) 0.6519(3) 0.031(2) Uani 1 1 d . . . . .
H8 H 0.3574 -0.3961 0.6440 0.037 Uiso 1 1 calc R . . . .
C9 C 0.2645(5) -0.2633(9) 0.5930(4) 0.038(3) Uani 1 1 d . . . . .
C10 C 0.3572(5) -0.2760(8) 0.5569(3) 0.036(3) Uani 1 1 d . . . . .
C11 C 0.3256(6) -0.2773(7) 0.5194(3) 0.037(3) Uani 1 1 d . . . . .
C12 C 0.2655(4) -0.2738(7) 0.5186(4) 0.031(2) Uani 1 1 d . . . . .
C13 C 0.2333(5) -0.2715(10) 0.5541(4) 0.041(3) Uani 1 1 d . . . . .
C14 C 0.1751(7) -0.2689(13) 0.5524(5) 0.070(5) Uani 1 1 d . U . . .
H14 H 0.1550 -0.2610 0.5764 0.085 Uiso 1 1 calc R . . . .
C15 C 0.1445(10) -0.2771(17) 0.5175(7) 0.111(8) Uani 1 1 d . U . . .
H15 H 0.1042 -0.2836 0.5178 0.133 Uiso 1 1 calc R . . . .
C16 C 0.1737(5) -0.2759(14) 0.4814(4) 0.068(5) Uani 1 1 d . . . . .
C17 C 0.2380(7) -0.2757(8) 0.4806(4) 0.048(4) Uani 1 1 d . . . . .
C18 C 0.2658(6) -0.2709(8) 0.4459(3) 0.040(3) Uani 1 1 d . . . . .
C19 C 0.3271(5) -0.2706(8) 0.4468(3) 0.034(3) Uani 1 1 d . . . . .
H19 H 0.3483 -0.2682 0.4230 0.040 Uiso 1 1 calc R . . . .
C20 C 0.3542(4) -0.2740(8) 0.4839(3) 0.032(2) Uani 1 1 d . . . . .
H20 H 0.3948 -0.2741 0.4849 0.038 Uiso 1 1 calc R . . . .
C21 C 0.1453(7) -0.2767(15) 0.4417(5) 0.077(6) Uani 1 1 d . . . . .
C22 C 0.2368(6) -0.2650(10) 0.4064(4) 0.049(4) Uani 1 1 d . . . . .
C23 C 0.1437(5) -0.2556(10) 0.3709(4) 0.045(3) Uani 1 1 d . . . . .
C24 C 0.1262(6) -0.1635(11) 0.3621(4) 0.054(4) Uani 1 1 d . . . . .
H24 H 0.1360 -0.1106 0.3787 0.065 Uiso 1 1 calc R . . . .
C25 C 0.0917(6) -0.1512(12) 0.3256(4) 0.055(4) Uani 1 1 d . . . . .
C26 C 0.0811(6) -0.2322(11) 0.3036(4) 0.055(4) Uani 1 1 d . . . . .
H26 H 0.0596 -0.2241 0.2796 0.066 Uiso 1 1 calc R . . . .
C27 C 0.0980(4) -0.3224(11) 0.3125(4) 0.043(3) Uani 1 1 d . . . . .
C28 C 0.1324(6) -0.3330(10) 0.3480(4) 0.049(3) Uani 1 1 d . . . . .
H28 H 0.1471 -0.3943 0.3552 0.059 Uiso 1 1 calc R . . . .
C29 C 0.0852(5) -0.4060(10) 0.2901(4) 0.043(3) Uani 1 1 d . . . . .
C30 C 0.0747(7) -0.0506(15) 0.3163(5) 0.072(5) Uani 1 1 d . . . . .
C31 C 0.0583(8) -0.1623(12) 0.1841(5) 0.065(5) Uani 1 1 d . . . . .
C32 C 0.0828(8) -0.0658(15) 0.1717(4) 0.084(6) Uani 1 1 d . . . . .
C33 C 0.0708(4) 0.0196(10) 0.1896(3) 0.039(3) Uani 1 1 d . . . . .
H33 H 0.0465 0.0200 0.2119 0.047 Uiso 1 1 calc R . . . .
C34 C 0.0923(5) 0.1030(10) 0.1767(3) 0.040(3) Uani 1 1 d . . . . .
C35 C 0.0762(8) 0.1981(11) 0.1954(4) 0.065(5) Uani 1 1 d . . . . .
C36 C 0.1267(6) 0.1042(12) 0.1424(4) 0.054(4) Uani 1 1 d . . . . .
H36 H 0.1416 0.1628 0.1323 0.065 Uiso 1 1 calc R . . . .
C37 C 0.1373(6) 0.0213(11) 0.1249(4) 0.055(4) Uani 1 1 d . . . . .
C38 C 0.1149(7) -0.0654(12) 0.1375(4) 0.063(4) Uani 1 1 d . . . . .
H38 H 0.1215 -0.1231 0.1231 0.075 Uiso 1 1 calc R . . . .
C39 C 0.1427(7) 0.0247(15) 0.0527(5) 0.079(6) Uani 1 1 d . . . . .
C40 C 0.1767(8) 0.0221(12) 0.0177(4) 0.069(5) Uani 1 1 d . . . . .
C41 C 0.2364(5) 0.0250(9) 0.0189(4) 0.039(3) Uani 1 1 d . U . . .
C42 C 0.2648(6) 0.0223(8) 0.0564(3) 0.046(4) Uani 1 1 d . . . . .
C43 C 0.2327(6) 0.0201(10) 0.0925(4) 0.047(3) Uani 1 1 d . . . . .
C44 C 0.1482(5) 0.0211(14) -0.0195(5) 0.081(6) Uani 1 1 d . . . . .
H44 H 0.1077 0.0169 -0.0205 0.098 Uiso 1 1 calc R . . . .
C45 C 0.1790(6) 0.0262(11) -0.0559(4) 0.056(4) Uani 1 1 d . . . . .
H45 H 0.1591 0.0309 -0.0807 0.068 Uiso 1 1 calc R . . . .
C46 C 0.2359(5) 0.0244(9) -0.0545(4) 0.042(3) Uani 1 1 d . . . . .
C47 C 0.2683(6) 0.0242(8) -0.0179(4) 0.042(3) Uani 1 1 d . . . . .
C48 C 0.3263(4) 0.0225(8) -0.0147(4) 0.032(2) Uani 1 1 d . U . . .
C49 C 0.3557(7) 0.0259(10) 0.0220(3) 0.051(4) Uani 1 1 d . . . . .
H49 H 0.3962 0.0295 0.0231 0.061 Uiso 1 1 calc R . . . .
C50 C 0.3240(6) 0.0240(8) 0.0570(3) 0.043(3) Uani 1 1 d . . . . .
H50 H 0.3437 0.0239 0.0819 0.052 Uiso 1 1 calc R . . . .
C51 C 0.2691(6) 0.0208(8) -0.0922(4) 0.044(3) Uani 1 1 d . . . . .
C52 C 0.3605(5) 0.0255(8) -0.0520(4) 0.039(3) Uani 1 1 d . . . . .
C53 C 0.3613(5) 0.0191(7) -0.1245(3) 0.035(3) Uani 1 1 d . . . . .
C54 C 0.3787(5) -0.0677(8) -0.1397(4) 0.036(3) Uani 1 1 d . . . . .
H54 H 0.3657 -0.1265 -0.1287 0.043 Uiso 1 1 calc R . . . .
C55 C 0.4165(3) -0.0677(6) -0.1722(3) 0.0175(19) Uani 1 1 d . . . . .
C56 C 0.4320(5) 0.0198(7) -0.1904(3) 0.030(2) Uani 1 1 d . . . . .
H56 H 0.4577 0.0201 -0.2120 0.036 Uiso 1 1 calc R . . . .
C57 C 0.4087(4) 0.1080(6) -0.1761(3) 0.027(2) Uani 1 1 d . . . . .
C58 C 0.3731(5) 0.1073(7) -0.1428(3) 0.031(3) Uani 1 1 d . . . . .
H58 H 0.3574 0.1654 -0.1330 0.037 Uiso 1 1 calc R . . . .
C59 C 0.4212(3) 0.2011(6) -0.1956(3) 0.021(2) Uani 1 1 d . . . . .
C60 C 0.4433(4) -0.1579(6) -0.1860(3) 0.024(2) Uani 1 1 d . . . . .
C61 C 0.6078(8) -0.0080(13) 0.6488(6) 0.085(6) Uani 1 1 d . U . . .
H61 H 0.6375 -0.0468 0.6598 0.102 Uiso 1 1 calc R . . . .
C62 C 0.2372(12) 0.253(2) 0.6805(9) 0.177(13) Uani 1 1 d . U . . .
H62A H 0.2343 0.2587 0.6515 0.266 Uiso 1 1 calc GR . . . .
H62B H 0.2274 0.3145 0.6928 0.266 Uiso 1 1 calc GR . . . .
H62C H 0.2108 0.2031 0.6896 0.266 Uiso 1 1 calc GR . . . .
C63 C 0.3378(5) 0.2903(11) 0.6894(4) 0.050(3) Uani 1 1 d . . . . .
H63 H 0.3299 0.3500 0.6767 0.060 Uiso 1 1 calc R . . . .
C64 C 0.4508(6) 0.3345(9) 0.6251(4) 0.045(3) Uani 1 1 d . U . . .
H64 H 0.4338 0.3637 0.6476 0.054 Uiso 1 1 calc R . . . .
C65 C 0.5031(7) 0.3523(10) 0.5656(4) 0.061(4) Uani 1 1 d . . . . .
H65A H 0.5438 0.3638 0.5709 0.092 Uiso 1 1 calc GR . . . .
H65B H 0.4916 0.3843 0.5407 0.092 Uiso 1 1 calc GR . . . .
H65C H 0.4962 0.2831 0.5632 0.092 Uiso 1 1 calc GR . . . .
C66 C 0.4692(5) 0.4933(8) 0.6039(3) 0.036(3) Uani 1 1 d . . . . .
H66A H 0.4396 0.5219 0.5867 0.055 Uiso 1 1 calc GR . . . .
H66B H 0.5065 0.5198 0.5970 0.055 Uiso 1 1 calc GR . . . .
H66C H 0.4611 0.5083 0.6317 0.055 Uiso 1 1 calc GR . . . .
C67 C 0.1653(8) 0.2907(15) 0.3117(5) 0.082(6) Uani 1 1 d . . . . .
H67 H 0.1761 0.3496 0.3239 0.099 Uiso 1 1 calc R . . . .
C68 C 0.2575(10) 0.246(2) 0.3294(10) 0.148(10) Uani 1 1 d . U . . .
C69 C 0.0517(7) 0.3350(15) 0.3761(5) 0.071(5) Uani 1 1 d . . . . .
H69 H 0.0714 0.3644 0.3548 0.085 Uiso 1 1 calc R . . . .
C70 C -0.0085(12) 0.3559(17) 0.4355(6) 0.130(10) Uani 1 1 d . . . . .
H70A H -0.0254 0.4107 0.4493 0.195 Uiso 1 1 calc GR . . . .
H70B H 0.0148 0.3184 0.4543 0.195 Uiso 1 1 calc GR . . . .
H70C H -0.0389 0.3152 0.4243 0.195 Uiso 1 1 calc GR . . . .
C71 C 0.0291(7) 0.4993(12) 0.3977(5) 0.069(5) Uani 1 1 d . U . . .
H71A H -0.0103 0.5213 0.4009 0.104 Uiso 1 1 calc GR . . . .
H71B H 0.0429 0.5200 0.3717 0.104 Uiso 1 1 calc GR . . . .
H71C H 0.0534 0.5270 0.4187 0.104 Uiso 1 1 calc GR . . . .




_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
Ba1 Ba2 4.1859(7) . ?
Ba1 O1 2.727(7) 2_656 ?
Ba1 O2 2.807(6) 2_656 ?
Ba1 O3 2.714(7) . ?
Ba1 O22 2.672(7) 1_556 ?
Ba1 O23 2.765(7) 2_645 ?
Ba1 O24 2.847(7) 2_645 ?
Ba1 O25 2.737(18) . ?
Ba1 O26 2.897(8) . ?
Ba1 O27 2.845(8) 2_646 ?
Ba1 C1 3.121(9) 2_656 ?
Ba1 C59 3.170(9) 2_645 ?
Ba2 O2 2.683(7) 2_656 ?
Ba2 O3 2.807(7) . ?
Ba2 O4 2.829(9) . ?
Ba2 O21 2.795(9) 2_655 ?
Ba2 O22 2.745(6) 2_655 ?
Ba2 O24 2.694(6) 1_556 ?
Ba2 O26 2.884(7) . ?
Ba2 O27 2.874(8) . ?
Ba2 O28 2.876(9) . ?
Ba2 C5 3.155(9) . ?
Ba2 C60 3.147(9) 2_655 ?
Ba3 Ba4 4.2011(13) 2_545 ?
Ba3 Ba4 4.1847(12) . ?
Ba3 O9 2.731(10) 2 ?
Ba3 O10 2.888(10) 2 ?
Ba3 O11 2.716(8) . ?
Ba3 O14 2.685(8) . ?
Ba3 O15 2.897(11) 2_545 ?
Ba3 O16 2.753(10) 2_545 ?
Ba3 O29 2.905(11) . ?
Ba3 O31 2.861(12) 2_545 ?
Ba3 C29 3.214(14) 2 ?
Ba3 C35 3.197(14) 2_545 ?
Ba4 O10 2.666(8) 2 ?
Ba4 O11 2.824(11) . ?
Ba4 O12 2.850(11) . ?
Ba4 O13 2.795(10) 2 ?
Ba4 O14 2.801(10) 2 ?
Ba4 O15 2.715(9) . ?
Ba4 O29 2.969(12) . ?
Ba4 O30 2.860(11) . ?
Ba4 O31 2.887(14) . ?
Ba4 C30 3.19(2) . ?
Ba4 C31 3.131(16) 2 ?
O1 Ba1 2.727(7) 2_646 ?
O1 C1 1.262(11) . ?
O2 Ba1 2.807(6) 2_646 ?
O2 Ba2 2.683(7) 2_646 ?
O2 C1 1.267(12) . ?
O3 C5 1.218(12) . ?
O4 C5 1.288(12) . ?
O5 C9 1.231(16) . ?
O6 C10 1.221(14) . ?
O7 C21 1.255(19) . ?
O8 C22 1.172(16) . ?
O9 Ba3 2.731(10) 2_545 ?
O9 C29 1.313(16) . ?
O10 Ba3 2.888(10) 2_545 ?
O10 Ba4 2.666(8) 2_545 ?
O10 C29 1.315(14) . ?
O11 C30 1.270(16) . ?
O12 C30 1.232(19) . ?
O13 Ba4 2.795(10) 2_545 ?
O13 C31 1.197(18) . ?
O14 Ba4 2.801(10) 2_545 ?
O14 C31 1.310(16) . ?
O15 Ba3 2.897(11) 2 ?
O15 C35 1.226(14) . ?
O16 Ba3 2.753(10) 2 ?
O16 C35 1.266(17) . ?
O17 C39 1.258(19) . ?
O18 C43 1.230(16) . ?
O19 C51 1.245(16) . ?
O20 C52 1.154(14) . ?
O21 Ba2 2.795(8) 2_645 ?
O21 C60 1.326(11) . ?
O22 Ba1 2.672(7) 1_554 ?
O22 Ba2 2.745(6) 2_645 ?
O22 C60 1.267(12) . ?
O23 Ba1 2.765(7) 2_655 ?
O23 C59 1.286(11) . ?
O24 Ba1 2.847(7) 2_655 ?
O24 Ba2 2.694(6) 1_554 ?
O24 C59 1.301(11) . ?
O26 C61 1.237(19) . ?
O27 Ba1 2.845(8) 2_656 ?
O27 C63 1.239(14) . ?
O28 C64 1.273(15) . ?
O30 C69 1.31(2) . ?
O31 Ba3 2.861(12) 2 ?
O31 C67 1.30(2) . ?
N1 C7 1.461(12) . ?
N1 C9 1.412(14) . ?
N1 C10 1.400(15) . ?
N2 C21 1.35(2) . ?
N2 C22 1.421(18) . ?
N2 C23 1.475(15) . ?
N3 C37 1.460(16) . ?
N3 C39 1.40(2) . ?
N3 C43 1.421(18) . ?
N4 C51 1.396(16) . ?
N4 C52 1.419(16) . ?
N4 C53 1.458(11) . ?
N5 C67 1.25(3) . ?
N5 C68 1.58(3) . ?
N6 C69 1.26(2) . ?
N6 C70 1.61(2) . ?
N6 C71 1.46(2) . ?
N7 C62 1.49(3) . ?
N7 C63 1.321(17) . ?
N8 C61 1.45(2) . ?
N9 C64 1.275(15) . ?
N9 C65 1.467(16) . ?
N9 C66 1.435(13) . ?
C1 Ba1 3.121(9) 2_646 ?
C1 C2 1.539(12) . ?
C2 C3 1.399(14) . ?
C2 C8 1.390(13) . ?
C3 C4 1.377(12) . ?
C4 C5 1.567(13) . ?
C4 C6 1.355(14) . ?
C6 C7 1.396(14) . ?
C7 C8 1.361(14) . ?
C9 C13 1.493(15) . ?
C10 C11 1.451(15) . ?
C11 C12 1.410(15) . ?
C11 C20 1.377(16) . ?
C12 C13 1.420(16) . ?
C12 C17 1.421(16) . ?
C13 C14 1.363(18) . ?
C14 C15 1.37(2) . ?
C15 C16 1.40(3) . ?
C16 C17 1.505(18) . ?
C16 C21 1.481(17) . ?
C17 C18 1.346(19) . ?
C18 C19 1.436(16) . ?
C18 C22 1.483(15) . ?
C19 C20 1.390(14) . ?
C23 C24 1.376(19) . ?
C23 C28 1.347(18) . ?
C24 C25 1.465(18) . ?
C25 C26 1.369(19) . ?
C25 C30 1.49(2) . ?
C26 C27 1.347(19) . ?
C27 C28 1.434(16) . ?
C27 C29 1.415(18) . ?
C29 Ba3 3.214(14) 2_545 ?
C31 Ba4 3.131(16) 2_545 ?
C31 C32 1.52(2) . ?
C32 C33 1.36(2) . ?
C32 C38 1.382(18) . ?
C33 C34 1.339(17) . ?
C34 C35 1.516(17) . ?
C34 C36 1.417(15) . ?
C35 Ba3 3.197(14) 2 ?
C36 C37 1.320(19) . ?
C37 C38 1.39(2) . ?
C39 C40 1.433(16) . ?
C40 C41 1.40(2) . ?
C40 C44 1.41(2) . ?
C41 C42 1.415(18) . ?
C41 C47 1.456(15) . ?
C42 C43 1.439(15) . ?
C42 C50 1.386(19) . ?
C44 C45 1.430(18) . ?
C45 C46 1.333(18) . ?
C46 C47 1.434(18) . ?
C46 C51 1.499(15) . ?
C47 C48 1.359(16) . ?
C48 C49 1.405(17) . ?
C48 C52 1.499(13) . ?
C49 C50 1.400(14) . ?
C53 C54 1.375(14) . ?
C53 C58 1.402(12) . ?
C54 C55 1.415(13) . ?
C55 C56 1.414(13) . ?
C55 C60 1.480(11) . ?
C56 C57 1.430(12) . ?
C57 C58 1.404(13) . ?
C57 C59 1.483(12) . ?
C59 Ba1 3.170(9) 2_655 ?
C60 Ba2 3.147(9) 2_645 ?


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 Ba1 Ba2 84.77(14) 2_656 . ?
O1 Ba1 O2 47.63(19) 2_656 2_656 ?
O1 Ba1 O23 147.2(2) 2_656 2_645 ?
O1 Ba1 O24 132.87(19) 2_656 2_645 ?
O1 Ba1 O25 69.8(4) 2_656 . ?
O1 Ba1 O26 111.6(2) 2_656 . ?
O1 Ba1 O27 72.5(2) 2_656 2_646 ?
O1 Ba1 C1 23.7(2) 2_656 2_656 ?
O1 Ba1 C59 145.8(2) 2_656 2_645 ?
O2 Ba1 Ba2 39.24(14) 2_656 . ?
O2 Ba1 O24 172.1(2) 2_656 2_645 ?
O2 Ba1 O26 66.8(2) 2_656 . ?
O2 Ba1 O27 119.8(2) 2_656 2_646 ?
O2 Ba1 C1 23.9(2) 2_656 2_656 ?
O2 Ba1 C59 160.8(2) 2_656 2_645 ?
O3 Ba1 Ba2 41.53(15) . . ?
O3 Ba1 O1 108.16(19) . 2_656 ?
O3 Ba1 O2 75.5(2) . 2_656 ?
O3 Ba1 O23 103.4(2) . 2_645 ?
O3 Ba1 O24 98.0(2) . 2_645 ?
O3 Ba1 O25 139.0(4) . . ?
O3 Ba1 O26 65.1(2) . . ?
O3 Ba1 O27 139.4(2) . 2_646 ?
O3 Ba1 C1 92.4(2) . 2_656 ?
O3 Ba1 C59 102.4(2) . 2_645 ?
O22 Ba1 Ba2 99.26(14) 1_556 . ?
O22 Ba1 O1 79.8(2) 1_556 2_656 ?
O22 Ba1 O2 100.60(19) 1_556 2_656 ?
O22 Ba1 O3 70.7(2) 1_556 . ?
O22 Ba1 O23 119.6(2) 1_556 2_645 ?
O22 Ba1 O24 72.72(18) 1_556 2_645 ?
O22 Ba1 O25 142.7(4) 1_556 . ?
O22 Ba1 O26 135.7(2) 1_556 . ?
O22 Ba1 O27 69.6(2) 1_556 2_646 ?
O22 Ba1 C1 90.7(2) 1_556 2_656 ?
O22 Ba1 C59 96.5(2) 1_556 2_645 ?
O23 Ba1 Ba2 114.66(17) 2_645 . ?
O23 Ba1 O2 137.3(2) 2_645 2_656 ?
O23 Ba1 O24 47.98(19) 2_645 2_645 ?
O23 Ba1 O26 74.2(2) 2_645 . ?
O23 Ba1 O27 89.2(2) 2_645 2_646 ?
O23 Ba1 C1 148.9(2) 2_645 2_656 ?
O23 Ba1 C59 23.8(2) 2_645 2_645 ?
O24 Ba1 Ba2 136.36(15) 2_645 . ?
O24 Ba1 O26 114.9(2) 2_645 . ?
O24 Ba1 C1 156.1(2) 2_645 2_656 ?
O24 Ba1 C59 24.2(2) 2_645 2_645 ?
O25 Ba1 Ba2 99.1(4) . . ?
O25 Ba1 O2 74.7(4) . 2_656 ?
O25 Ba1 O23 80.7(4) . 2_645 ?
O25 Ba1 O24 113.1(4) . 2_645 ?
O25 Ba1 O26 77.4(4) . . ?
O25 Ba1 O27 80.6(4) . 2_646 ?
O25 Ba1 C1 70.0(4) . 2_656 ?
O25 Ba1 C59 96.6(4) . 2_645 ?
O26 Ba1 Ba2 43.49(14) . . ?
O26 Ba1 C1 89.1(2) . 2_656 ?
O26 Ba1 C59 94.8(3) . 2_645 ?
O27 Ba1 Ba2 155.95(16) 2_646 . ?
O27 Ba1 O24 62.4(2) 2_646 2_645 ?
O27 Ba1 O26 154.3(2) 2_646 . ?
O27 Ba1 C1 96.0(2) 2_646 2_656 ?
O27 Ba1 C59 74.4(3) 2_646 2_645 ?
C1 Ba1 Ba2 62.03(19) 2_656 . ?
C1 Ba1 C59 164.9(2) 2_656 2_645 ?
C59 Ba1 Ba2 129.12(19) 2_645 . ?
O2 Ba2 Ba1 41.43(13) 2_656 . ?
O2 Ba2 O3 76.0(2) 2_656 . ?
O2 Ba2 O4 122.0(2) 2_656 . ?
O2 Ba2 O21 82.2(3) 2_656 2_655 ?
O2 Ba2 O22 90.4(2) 2_656 2_655 ?
O2 Ba2 O24 69.0(2) 2_656 1_556 ?
O2 Ba2 O26 68.5(2) 2_656 . ?
O2 Ba2 O27 131.8(2) 2_656 . ?
O2 Ba2 O28 152.5(3) 2_656 . ?
O2 Ba2 C5 98.0(2) 2_656 . ?
O2 Ba2 C60 88.1(2) 2_656 2_655 ?
O3 Ba2 Ba1 39.87(15) . . ?
O3 Ba2 O4 46.6(2) . . ?
O3 Ba2 O26 64.2(2) . . ?
O3 Ba2 O27 112.4(2) . . ?
O3 Ba2 O28 121.1(2) . . ?
O3 Ba2 C5 22.6(2) . . ?
O3 Ba2 C60 160.3(2) . 2_655 ?
O4 Ba2 Ba1 81.85(16) . . ?
O4 Ba2 O26 78.1(3) . . ?
O4 Ba2 O27 85.3(3) . . ?
O4 Ba2 O28 75.6(2) . . ?
O4 Ba2 C5 24.1(2) . . ?
O4 Ba2 C60 144.8(3) . 2_655 ?
O21 Ba2 Ba1 103.0(2) 2_655 . ?
O21 Ba2 O3 138.2(2) 2_655 . ?
O21 Ba2 O4 132.8(3) 2_655 . ?
O21 Ba2 O26 74.8(2) 2_655 . ?
O21 Ba2 O27 108.8(2) 2_655 . ?
O21 Ba2 O28 70.9(3) 2_655 . ?
O21 Ba2 C5 139.3(3) 2_655 . ?
O21 Ba2 C60 24.9(2) 2_655 2_655 ?
O22 Ba2 Ba1 130.68(16) 2_655 . ?
O22 Ba2 O3 162.07(19) 2_655 . ?
O22 Ba2 O4 147.4(2) 2_655 . ?
O22 Ba2 O21 48.3(2) 2_655 2_655 ?
O22 Ba2 O26 121.9(2) 2_655 . ?
O22 Ba2 O27 68.2(2) 2_655 . ?
O22 Ba2 O28 76.1(2) 2_655 . ?
O22 Ba2 C5 169.2(2) 2_655 . ?
O22 Ba2 C60 23.6(2) 2_655 2_655 ?
O24 Ba2 Ba1 92.06(14) 1_556 . ?
O24 Ba2 O3 89.98(19) 1_556 . ?
O24 Ba2 O4 111.9(3) 1_556 . ?
O24 Ba2 O21 114.8(2) 1_556 2_655 ?
O24 Ba2 O22 74.0(2) 1_556 2_655 ?
O24 Ba2 O26 134.3(2) 1_556 . ?
O24 Ba2 O27 63.8(2) 1_556 . ?
O24 Ba2 O28 127.4(3) 1_556 . ?
O24 Ba2 C5 102.7(3) 1_556 . ?
O24 Ba2 C60 95.1(2) 1_556 2_655 ?
O26 Ba2 Ba1 43.73(15) . . ?
O26 Ba2 C5 67.8(3) . . ?
O26 Ba2 C60 99.5(2) . 2_655 ?
O27 Ba2 Ba1 145.92(16) . . ?
O27 Ba2 O26 159.2(3) . . ?
O27 Ba2 O28 65.2(3) . . ?
O27 Ba2 C5 101.1(2) . . ?
O27 Ba2 C60 86.8(2) . 2_655 ?
O28 Ba2 Ba1 139.5(2) . . ?
O28 Ba2 O26 98.2(3) . . ?
O28 Ba2 C5 98.7(3) . . ?
O28 Ba2 C60 69.9(3) . 2_655 ?
C5 Ba2 Ba1 59.01(19) . . ?
C60 Ba2 Ba1 120.78(19) 2_655 . ?
C60 Ba2 C5 162.2(3) 2_655 . ?
Ba4 Ba3 Ba4 136.58(2) . 2_545 ?
O9 Ba3 Ba4 85.0(2) 2 . ?
O9 Ba3 Ba4 97.1(2) 2 2_545 ?
O9 Ba3 O10 47.9(3) 2 2 ?
O9 Ba3 O15 132.4(3) 2 2_545 ?
O9 Ba3 O16 150.1(4) 2 2_545 ?
O9 Ba3 O29 112.1(3) 2 . ?
O9 Ba3 O31 72.0(3) 2 2_545 ?
O9 Ba3 C29 23.8(3) 2 2 ?
O9 Ba3 C35 146.0(4) 2 2_545 ?
O10 Ba3 Ba4 39.16(16) 2 . ?
O10 Ba3 Ba4 136.21(19) 2 2_545 ?
O10 Ba3 O15 173.6(2) 2 2_545 ?
O10 Ba3 O29 67.7(3) 2 . ?
O10 Ba3 C29 24.1(3) 2 2 ?
O10 Ba3 C35 161.3(3) 2 2_545 ?
O11 Ba3 Ba4 41.9(2) . . ?
O11 Ba3 Ba4 98.3(2) . 2_545 ?
O11 Ba3 O9 108.8(3) . 2 ?
O11 Ba3 O10 75.8(3) . 2 ?
O11 Ba3 O15 99.0(3) . 2_545 ?
O11 Ba3 O16 100.4(3) . 2_545 ?
O11 Ba3 O29 67.0(3) . . ?
O11 Ba3 O31 139.3(4) . 2_545 ?
O11 Ba3 C29 93.2(3) . 2 ?
O11 Ba3 C35 101.1(4) . 2_545 ?
O14 Ba3 Ba4 97.8(2) . . ?
O14 Ba3 Ba4 41.1(2) . 2_545 ?
O14 Ba3 O9 80.0(3) . 2 ?
O14 Ba3 O10 99.6(3) . 2 ?
O14 Ba3 O11 69.1(3) . . ?
O14 Ba3 O15 74.8(3) . 2_545 ?
O14 Ba3 O16 117.9(3) . 2_545 ?
O14 Ba3 O29 136.1(3) . . ?
O14 Ba3 O31 71.1(4) . 2_545 ?
O14 Ba3 C29 90.6(3) . 2 ?
O14 Ba3 C35 96.3(3) . 2_545 ?
O15 Ba3 Ba4 137.53(17) 2_545 . ?
O15 Ba3 Ba4 39.92(18) 2_545 2_545 ?
O15 Ba3 O29 114.1(3) 2_545 . ?
O15 Ba3 C29 155.9(3) 2_545 2 ?
O15 Ba3 C35 22.5(3) 2_545 2_545 ?
O16 Ba3 Ba4 85.2(2) 2_545 2_545 ?
O16 Ba3 Ba4 113.6(3) 2_545 . ?
O16 Ba3 O10 138.5(3) 2_545 2 ?
O16 Ba3 O15 45.6(3) 2_545 2_545 ?
O16 Ba3 O29 72.9(4) 2_545 . ?
O16 Ba3 O31 90.6(4) 2_545 2_545 ?
O16 Ba3 C29 151.3(3) 2_545 2 ?
O16 Ba3 C35 23.0(3) 2_545 2_545 ?
O29 Ba3 Ba4 150.1(2) . 2_545 ?
O29 Ba3 Ba4 45.2(2) . . ?
O29 Ba3 C29 89.7(3) . 2 ?
O29 Ba3 C35 94.0(3) . 2_545 ?
O31 Ba3 Ba4 155.7(3) 2_545 . ?
O31 Ba3 Ba4 43.3(3) 2_545 2_545 ?
O31 Ba3 O10 119.6(3) 2_545 2 ?
O31 Ba3 O15 61.9(3) 2_545 2_545 ?
O31 Ba3 O29 152.4(4) 2_545 . ?
O31 Ba3 C29 95.5(3) 2_545 2 ?
O31 Ba3 C35 74.9(4) 2_545 2_545 ?
C29 Ba3 Ba4 62.3(2) 2 . ?
C29 Ba3 Ba4 117.9(2) 2 2_545 ?
C35 Ba3 Ba4 62.2(2) 2_545 2_545 ?
C35 Ba3 Ba4 128.7(3) 2_545 . ?
C35 Ba3 C29 165.6(4) 2_545 2 ?
O10 Ba4 Ba3 43.2(2) 2 . ?
O10 Ba4 O11 77.7(3) 2 . ?
O10 Ba4 O12 123.0(3) 2 . ?
O10 Ba4 O13 81.4(4) 2 2 ?
O10 Ba4 O14 88.1(3) 2 2 ?
O10 Ba4 O15 68.9(3) 2 . ?
O10 Ba4 O29 69.6(3) 2 . ?
O10 Ba4 O30 154.0(3) 2 . ?
O10 Ba4 O31 131.0(3) 2 . ?
O10 Ba4 C30 100.6(4) 2 . ?
O10 Ba4 C31 86.9(4) 2 2 ?
O11 Ba4 Ba3 39.99(16) . . ?
O11 Ba4 O12 46.0(3) . . ?
O11 Ba4 O29 64.8(3) . . ?
O11 Ba4 O30 119.9(3) . . ?
O11 Ba4 O31 112.2(3) . . ?
O11 Ba4 C30 23.4(3) . . ?
O11 Ba4 C31 159.6(4) . 2 ?
O12 Ba4 Ba3 81.1(2) . . ?
O12 Ba4 O29 77.7(3) . . ?
O12 Ba4 O30 74.6(3) . . ?
O12 Ba4 O31 86.0(3) . . ?
O12 Ba4 C30 22.6(3) . . ?
O12 Ba4 C31 143.9(4) . 2 ?
O13 Ba4 Ba3 103.7(3) 2 . ?
O13 Ba4 O11 139.1(3) 2 . ?
O13 Ba4 O12 133.0(4) 2 . ?
O13 Ba4 O14 46.8(3) 2 2 ?
O13 Ba4 O29 75.1(3) 2 . ?
O13 Ba4 O30 72.9(4) 2 . ?
O13 Ba4 O31 108.0(4) 2 . ?
O13 Ba4 C30 140.8(4) 2 . ?
O13 Ba4 C31 22.4(3) 2 2 ?
O14 Ba4 Ba3 130.01(18) 2 . ?
O14 Ba4 O11 162.0(2) 2 . ?
O14 Ba4 O12 148.8(3) 2 . ?
O14 Ba4 O29 120.6(3) 2 . ?
O14 Ba4 O30 77.3(3) 2 . ?
O14 Ba4 O31 69.1(3) 2 . ?
O14 Ba4 C30 168.9(4) 2 . ?
O14 Ba4 C31 24.7(3) 2 2 ?
O15 Ba4 Ba3 91.7(2) . . ?
O15 Ba4 O11 88.5(3) . . ?
O15 Ba4 O12 110.5(3) . . ?
O15 Ba4 O13 116.0(3) . 2 ?
O15 Ba4 O14 75.9(3) . 2 ?
O15 Ba4 O29 134.4(3) . . ?
O15 Ba4 O30 126.3(4) . . ?
O15 Ba4 O31 63.8(3) . . ?
O15 Ba4 C30 100.8(4) . . ?
O15 Ba4 C31 98.5(3) . 2 ?
O29 Ba4 Ba3 44.0(2) . . ?
O29 Ba4 C30 69.3(4) . . ?
O29 Ba4 C31 97.4(4) . 2 ?
O30 Ba4 Ba3 140.1(3) . . ?
O30 Ba4 O29 99.3(4) . . ?
O30 Ba4 O31 63.4(4) . . ?
O30 Ba4 C30 96.9(4) . . ?
O30 Ba4 C31 70.9(4) . 2 ?
O31 Ba4 Ba3 146.1(3) . . ?
O31 Ba4 O29 159.1(3) . . ?
O31 Ba4 C30 99.9(4) . . ?
O31 Ba4 C31 88.0(4) . 2 ?
C30 Ba4 Ba3 60.1(3) . . ?
C31 Ba4 Ba3 120.1(3) 2 . ?
C31 Ba4 C30 160.7(4) 2 . ?
C1 O1 Ba1 95.9(6) . 2_646 ?
Ba2 O2 Ba1 99.3(2) 2_646 2_646 ?
C1 O2 Ba1 92.1(5) . 2_646 ?
C1 O2 Ba2 155.9(6) . 2_646 ?
Ba1 O3 Ba2 98.6(2) . . ?
C5 O3 Ba1 139.5(6) . . ?
C5 O3 Ba2 95.0(6) . . ?
C5 O4 Ba2 92.3(6) . . ?
C29 O9 Ba3 99.2(8) . 2_545 ?
Ba4 O10 Ba3 97.7(3) 2_545 2_545 ?
C29 O10 Ba3 92.0(8) . 2_545 ?
C29 O10 Ba4 157.9(8) . 2_545 ?
Ba3 O11 Ba4 98.1(3) . . ?
C30 O11 Ba3 141.3(11) . . ?
C30 O11 Ba4 94.8(11) . . ?
C30 O12 Ba4 94.5(10) . . ?
C31 O13 Ba4 94.8(10) . 2_545 ?
Ba3 O14 Ba4 99.9(3) . 2_545 ?
C31 O14 Ba3 167.8(10) . . ?
C31 O14 Ba4 91.9(9) . 2_545 ?
Ba4 O15 Ba3 96.9(3) . 2 ?
C35 O15 Ba3 92.6(10) . 2 ?
C35 O15 Ba4 166.7(11) . . ?
C35 O16 Ba3 98.6(8) . 2 ?
C60 O21 Ba2 92.6(6) . 2_645 ?
Ba1 O22 Ba2 101.7(2) 1_554 2_645 ?
C60 O22 Ba1 162.0(6) . 1_554 ?
C60 O22 Ba2 96.3(5) . 2_645 ?
C59 O23 Ba1 96.1(6) . 2_655 ?
Ba2 O24 Ba1 98.6(2) 1_554 2_655 ?
C59 O24 Ba1 91.9(5) . 2_655 ?
C59 O24 Ba2 160.4(6) . 1_554 ?
Ba2 O26 Ba1 92.8(2) . . ?
C61 O26 Ba1 107.3(10) . . ?
C61 O26 Ba2 152.5(10) . . ?
Ba1 O27 Ba2 94.5(2) 2_656 . ?
C63 O27 Ba1 120.0(9) . 2_656 ?
C63 O27 Ba2 145.4(9) . . ?
C64 O28 Ba2 115.5(8) . . ?
Ba3 O29 Ba4 90.9(3) . . ?
C69 O30 Ba4 117.9(10) . . ?
Ba3 O31 Ba4 93.9(3) 2 . ?
C67 O31 Ba3 120.1(13) . 2 ?
C67 O31 Ba4 145.9(13) . . ?
C9 N1 C7 116.0(10) . . ?
C10 N1 C7 117.1(10) . . ?
C10 N1 C9 126.5(9) . . ?
C21 N2 C22 126.4(12) . . ?
C21 N2 C23 116.3(13) . . ?
C22 N2 C23 117.3(11) . . ?
C39 N3 C37 116.4(14) . . ?
C39 N3 C43 122.9(12) . . ?
C43 N3 C37 120.4(13) . . ?
C51 N4 C52 126.6(9) . . ?
C51 N4 C53 117.0(10) . . ?
C52 N4 C53 116.0(9) . . ?
C67 N5 C68 109(2) . . ?
C69 N6 C70 119.2(17) . . ?
C69 N6 C71 129.0(17) . . ?
C71 N6 C70 110.9(15) . . ?
C63 N7 C62 119.5(18) . . ?
C64 N9 C65 119.9(11) . . ?
C64 N9 C66 121.2(10) . . ?
C66 N9 C65 117.7(10) . . ?
O1 C1 Ba1 60.4(5) . 2_646 ?
O1 C1 O2 124.3(9) . . ?
O1 C1 C2 116.9(9) . . ?
O2 C1 Ba1 64.0(5) . 2_646 ?
O2 C1 C2 118.8(8) . . ?
C2 C1 Ba1 174.6(7) . 2_646 ?
C3 C2 C1 122.2(8) . . ?
C8 C2 C1 117.9(9) . . ?
C8 C2 C3 119.9(9) . . ?
C4 C3 C2 118.5(9) . . ?
C3 C4 C5 119.3(9) . . ?
C6 C4 C3 122.0(10) . . ?
C6 C4 C5 118.7(9) . . ?
O3 C5 Ba2 62.4(5) . . ?
O3 C5 O4 125.6(9) . . ?
O3 C5 C4 118.7(9) . . ?
O4 C5 Ba2 63.6(5) . . ?
O4 C5 C4 115.8(9) . . ?
C4 C5 Ba2 172.6(7) . . ?
C4 C6 C7 119.0(10) . . ?
C6 C7 N1 119.2(9) . . ?
C8 C7 N1 119.8(9) . . ?
C8 C7 C6 120.8(10) . . ?
C7 C8 C2 119.7(9) . . ?
O5 C9 N1 120.7(11) . . ?
O5 C9 C13 123.4(12) . . ?
N1 C9 C13 115.8(10) . . ?
O6 C10 N1 121.5(11) . . ?
O6 C10 C11 122.2(11) . . ?
N1 C10 C11 116.2(11) . . ?
C12 C11 C10 120.7(11) . . ?
C20 C11 C10 120.2(12) . . ?
C20 C11 C12 118.8(11) . . ?
C11 C12 C13 121.9(11) . . ?
C11 C12 C17 117.0(12) . . ?
C13 C12 C17 121.1(10) . . ?
C12 C13 C9 118.6(10) . . ?
C14 C13 C9 120.7(13) . . ?
C14 C13 C12 120.5(12) . . ?
C13 C14 C15 122.9(18) . . ?
C14 C15 C16 119(2) . . ?
C15 C16 C17 121.0(14) . . ?
C15 C16 C21 124.2(15) . . ?
C21 C16 C17 114.7(13) . . ?
C12 C17 C16 115.0(12) . . ?
C18 C17 C12 124.0(14) . . ?
C18 C17 C16 120.8(12) . . ?
C17 C18 C19 118.7(11) . . ?
C17 C18 C22 123.9(13) . . ?
C19 C18 C22 117.4(12) . . ?
C20 C19 C18 117.4(10) . . ?
C11 C20 C19 123.8(10) . . ?
O7 C21 N2 124.1(15) . . ?
O7 C21 C16 115.5(15) . . ?
N2 C21 C16 120.4(14) . . ?
O8 C22 N2 121.0(12) . . ?
O8 C22 C18 125.6(14) . . ?
N2 C22 C18 113.4(12) . . ?
C24 C23 N2 115.7(12) . . ?
C28 C23 N2 119.9(13) . . ?
C28 C23 C24 124.5(13) . . ?
C23 C24 C25 116.5(14) . . ?
C24 C25 C30 115.4(14) . . ?
C26 C25 C24 116.7(14) . . ?
C26 C25 C30 127.9(14) . . ?
C27 C26 C25 126.6(12) . . ?
C26 C27 C28 116.0(13) . . ?
C26 C27 C29 126.0(12) . . ?
C29 C27 C28 118.0(12) . . ?
C23 C28 C27 119.7(13) . . ?
O9 C29 Ba3 57.0(7) . 2_545 ?
O9 C29 O10 120.8(12) . . ?
O9 C29 C27 121.2(12) . . ?
O10 C29 Ba3 63.9(7) . 2_545 ?
O10 C29 C27 118.0(13) . . ?
C27 C29 Ba3 176.5(8) . 2_545 ?
O11 C30 Ba4 61.8(10) . . ?
O11 C30 C25 114.5(16) . . ?
O12 C30 Ba4 62.9(10) . . ?
O12 C30 O11 124.7(18) . . ?
O12 C30 C25 120.3(15) . . ?
C25 C30 Ba4 169.1(12) . . ?
O13 C31 Ba4 62.8(9) . 2_545 ?
O13 C31 O14 124.8(15) . . ?
O13 C31 C32 121.7(15) . . ?
O14 C31 Ba4 63.4(8) . 2_545 ?
O14 C31 C32 113.5(14) . . ?
C32 C31 Ba4 167.8(13) . 2_545 ?
C33 C32 C31 124.5(13) . . ?
C33 C32 C38 118.8(17) . . ?
C38 C32 C31 116.4(16) . . ?
C34 C33 C32 122.1(12) . . ?
C33 C34 C35 121.6(10) . . ?
C33 C34 C36 119.7(12) . . ?
C36 C34 C35 118.4(13) . . ?
O15 C35 Ba3 64.8(8) . 2 ?
O15 C35 O16 123.2(14) . . ?
O15 C35 C34 117.2(13) . . ?
O16 C35 Ba3 58.4(7) . 2 ?
O16 C35 C34 119.1(11) . . ?
C34 C35 Ba3 170.3(12) . 2 ?
C37 C36 C34 117.7(14) . . ?
C36 C37 N3 119.9(14) . . ?
C36 C37 C38 123.3(13) . . ?
C38 C37 N3 116.7(13) . . ?
C32 C38 C37 118.2(16) . . ?
O17 C39 N3 119.4(13) . . ?
O17 C39 C40 124.1(18) . . ?
N3 C39 C40 116.5(16) . . ?
C41 C40 C39 123.0(15) . . ?
C41 C40 C44 119.1(11) . . ?
C44 C40 C39 117.9(17) . . ?
C40 C41 C42 118.7(11) . . ?
C40 C41 C47 120.1(12) . . ?
C42 C41 C47 121.1(12) . . ?
C41 C42 C43 120.5(13) . . ?
C50 C42 C41 117.8(10) . . ?
C50 C42 C43 121.7(13) . . ?
O18 C43 N3 120.2(12) . . ?
O18 C43 C42 121.8(13) . . ?
N3 C43 C42 118.0(13) . . ?
C40 C44 C45 121.4(12) . . ?
C46 C45 C44 119.1(14) . . ?
C45 C46 C47 123.1(12) . . ?
C45 C46 C51 120.1(13) . . ?
C47 C46 C51 116.8(11) . . ?
C46 C47 C41 117.1(12) . . ?
C48 C47 C41 117.3(13) . . ?
C48 C47 C46 125.6(11) . . ?
C47 C48 C49 122.9(11) . . ?
C47 C48 C52 118.8(12) . . ?
C49 C48 C52 118.1(10) . . ?
C50 C49 C48 118.5(14) . . ?
C42 C50 C49 122.2(13) . . ?
O19 C51 N4 121.6(11) . . ?
O19 C51 C46 122.0(13) . . ?
N4 C51 C46 116.4(12) . . ?
O20 C52 N4 120.4(10) . . ?
O20 C52 C48 124.0(13) . . ?
N4 C52 C48 115.3(10) . . ?
C54 C53 N4 117.8(9) . . ?
C54 C53 C58 122.9(9) . . ?
C58 C53 N4 119.3(9) . . ?
C53 C54 C55 118.6(10) . . ?
C54 C55 C60 121.0(9) . . ?
C56 C55 C54 120.2(9) . . ?
C56 C55 C60 118.7(8) . . ?
C55 C56 C57 119.3(9) . . ?
C56 C57 C59 121.3(8) . . ?
C58 C57 C56 119.9(9) . . ?
C58 C57 C59 118.8(8) . . ?
C53 C58 C57 118.6(9) . . ?
O23 C59 Ba1 60.2(5) . 2_655 ?
O23 C59 O24 123.9(8) . . ?
O23 C59 C57 118.0(8) . . ?
O24 C59 Ba1 63.8(5) . 2_655 ?
O24 C59 C57 118.0(8) . . ?
C57 C59 Ba1 174.7(7) . 2_655 ?
O21 C60 Ba2 62.5(5) . 2_645 ?
O21 C60 C55 116.1(8) . . ?
O22 C60 Ba2 60.1(5) . 2_645 ?
O22 C60 O21 121.9(8) . . ?
O22 C60 C55 121.8(8) . . ?
C55 C60 Ba2 168.1(7) . 2_645 ?
O26 C61 N8 113.5(18) . . ?
O27 C63 N7 121.7(15) . . ?
O28 C64 N9 126.6(13) . . ?
N5 C67 O31 114(2) . . ?
N6 C69 O30 133.0(19) . . ?


_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
;
_platon_squeeze_details          
;
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.006 -0.041 0.000 1839 726 ' '
2 0.500 0.000 0.000 22 8 ' '
3 0.698 -0.005 0.500 1839 728 ' '
4 0.500 0.500 0.500 22 8 ' '
####################################################################### 
# 
# 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-4
_database_code_depnum_ccdc_archive 'CCDC 1812093'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-03-26 downloaded from the CCDC.
;
_audit_creation_date             2017-12-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H38 Ca2 Cl N5 O15, C4 H9 N O'
_chemical_formula_sum            'C46 H47 Ca2 Cl N6 O16'
_chemical_formula_weight         1055.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 O1 N1 Ca1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_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                   9.8893(9)
_cell_length_b                   16.7182(4)
_cell_length_c                   17.3044(4)
_cell_angle_alpha                63.933(2)
_cell_angle_beta                 78.652(7)
_cell_angle_gamma                86.531(5)
_cell_volume                     2518.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16875
_cell_measurement_temperature    291.87(10)
_cell_measurement_theta_max      72.8850
_cell_measurement_theta_min      4.5700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34834
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         4.562
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.87(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.982
_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   -106.00 -18.00   1.00    1.74    --  -37.03 -38.00 -90.00   88
  2  ω    -66.00  34.00   1.00    1.74    --  -37.03  19.00-180.00  100
  3  ω    -66.00  34.00   1.00    1.74    --  -37.03  19.00  90.00  100
  4  ω    -91.00  -3.00   1.00    1.74    --  -37.03 126.00  60.00   88
  5  ω     10.00 105.00   1.00    1.74    --   37.03  77.00 -90.00   95
  6  ω    -30.00  54.00   1.00    1.74    --   37.03 -57.00-120.00   84
  7  ω     20.00 104.00   1.00    1.74    --   37.03  57.00 -30.00   84
  8  ω      8.00 108.00   1.00    1.74    --   37.03  19.00-150.00  100
  9  ω      1.00  76.00   1.00    1.74    --   37.03 -99.00  90.00   75
 10  ω      1.00  76.00   1.00    1.74    --   37.03 -99.00  60.00   75
 11  ω     24.00  91.00   1.00    1.74    --   37.03-126.00  60.00   67
 12  ω     24.00  91.00   1.00    1.74    --   37.03-126.00-120.00   67
 13  ω      8.00  80.00   1.00    1.74    --   37.03-106.00-160.00   72
 14  ω     41.00 132.00   1.00    8.98    --  110.47 -30.00  30.00   91
 15  ω     41.00 109.00   1.00    8.98    --  110.47 -95.00 -60.00   68
 16  ω     44.00 129.00   1.00    8.98    --  110.47 -61.00-150.00   85
 17  ω     44.00 129.00   1.00    8.98    --  110.47 -61.00 -60.00   85
 18  ω     41.00 132.00   1.00    8.98    --  110.47 -30.00 120.00   91
 19  ω     89.00 178.00   1.00    8.98    --  110.47  30.00  90.00   89
 20  ω     41.00 116.00   1.00    8.98    --  110.47-112.00 120.00   75
 21  ω     44.00 129.00   1.00    8.98    --  110.47 -61.00 120.00   85
 22  ω     43.00 137.00   1.00    8.98    --  110.47 -77.00  30.00   94
 23  ω     93.00 178.00   1.00    8.98    --  110.47  45.00  60.00   85
 24  ω     41.00 116.00   1.00    8.98    --  110.47-112.00  60.00   75
 25  ω     40.00 149.00   1.00    8.98    --  110.47 -15.00-120.00  109
 26  ω     41.00 116.00   1.00    8.98    --  110.47-112.00-120.00   75
 27  ω     92.00 177.00   1.00    8.98    --  110.47  61.00 150.00   85
 28  ω   -104.00 -34.00   1.00    1.74    --  -37.03 -57.00 -90.00   70
 29  ω   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00 -90.00   95
 30  ω   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00-150.00   95
 31  ω   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00 120.00   95
 32  ω   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00  30.00   95
 33  ω   -107.00  -8.00   1.00    1.74    --  -37.03 -19.00 -60.00   99
 34  ω   -104.00 -20.00   1.00    1.74    --  -37.03 -57.00-120.00   84
 35  ω   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00  60.00   95
 36  ω   -106.00 -18.00   1.00    1.74    --  -37.03 -38.00  90.00   88
 37  ω    -66.00  34.00   1.00    1.74    --  -37.03  19.00-150.00  100
 38  ω   -104.00 -20.00   1.00    1.74    --  -37.03 -57.00 150.00   84
 39  ω     10.00 105.00   1.00    1.74    --   37.03  77.00   0.00   95
 40  ω    -30.00  54.00   1.00    1.74    --   37.03 -57.00 -60.00   84
 41  ω     20.00 104.00   1.00    1.74    --   37.03  57.00  60.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0607989000
_diffrn_orient_matrix_UB_12      0.0944806000
_diffrn_orient_matrix_UB_13      -0.0325675000
_diffrn_orient_matrix_UB_21      0.0561759000
_diffrn_orient_matrix_UB_22      0.0028614000
_diffrn_orient_matrix_UB_23      -0.0907998000
_diffrn_orient_matrix_UB_31      -0.1357019000
_diffrn_orient_matrix_UB_32      0.0399711000
_diffrn_orient_matrix_UB_33      -0.0297362000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7542
_reflns_number_total             8945
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.578
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         8945
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0617
_refine_ls_restrained_S_all      1.160
_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)+(0.1016P)²+2.6624P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1837
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N6-C2
 1.57 with sigma of 0.01
 N4-C11
 1.57 with sigma of 0.01
 N3-C16
 1.47 with sigma of 0.01
 N3-C14
 1.57 with sigma of 0.01
 H14A-H13B
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N5) \\sim
Ueq, Uanis(C15) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C23(H23), C30(H30), C31(H31), C35(H35), C36(H36),
 C40(H40), C42(H42), C44(H44)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_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
Ca1 Ca 0.15516(6) 1.53193(4) -0.32122(4) 0.03144(17) Uani 1 1 d . . . . .
Cl1 Cl 0.04567(11) 1.40802(6) -0.15286(6) 0.0603(3) Uani 1 1 d . . . . .
Ca2 Ca 0.86642(6) 0.23294(4) 0.35739(4) 0.03090(17) Uani 1 1 d . . . . .
O1 O 0.2015(3) 1.28364(16) -0.21335(19) 0.0612(8) Uani 1 1 d . . . . .
H1 H 0.1510 1.3184 -0.2004 0.092 Uiso 1 1 calc GR . . . .
O2 O 0.2915(3) 1.40973(14) -0.32892(16) 0.0454(6) Uani 1 1 d . . . . .
O3 O 0.6999(3) 1.38466(18) -0.54304(19) 0.0679(9) Uani 1 1 d . . . . .
O4 O 0.7864(3) 1.2524(2) -0.51807(18) 0.0578(7) Uani 1 1 d . . . . .
O5 O 0.3713(4) 1.00125(18) -0.3029(2) 0.0784(11) Uani 1 1 d . . . . .
O6 O 0.6194(4) 1.07508(17) -0.1511(2) 0.0662(9) Uani 1 1 d . . . . .
O7 O 0.3257(3) 0.55400(16) 0.01663(18) 0.0608(8) Uani 1 1 d . . . . .
O8 O 0.5092(3) 0.63860(16) 0.19009(16) 0.0533(7) Uani 1 1 d . . . . .
O9 O 0.0143(2) 0.37145(14) 0.30304(15) 0.0360(5) Uani 1 1 d . . . . .
O10 O 0.1132(2) 0.24281(14) 0.35706(16) 0.0404(5) Uani 1 1 d . . . . .
O11 O 0.6278(2) 0.24401(14) 0.33743(17) 0.0447(6) Uani 1 1 d . . . . .
O12 O 0.7368(2) 0.37508(15) 0.28203(16) 0.0411(5) Uani 1 1 d . . . . .
O13 O 0.9514(3) 0.2427(2) 0.21737(19) 0.0603(7) Uani 1 1 d . . . . .
O14 O 0.8637(4) 0.08106(19) 0.4226(3) 0.0925(12) Uani 1 1 d . . . . .
O15 O 0.0103(3) 1.4943(2) -0.3873(2) 0.0711(9) Uani 1 1 d . . . . .
N1 N 0.4938(3) 1.03744(16) -0.22602(18) 0.0369(6) Uani 1 1 d . . . . .
N2 N 0.4159(3) 0.59529(16) 0.10453(17) 0.0341(6) Uani 1 1 d . . . . .
N3 N 0.8944(11) -0.0489(5) 0.4207(6) 0.152(3) Uani 1 1 d D U . . .
N4 N 1.1435(6) 0.3020(4) 0.1202(3) 0.1054(18) Uani 1 1 d D U . . .
N6 N -0.1952(6) 1.5236(4) -0.4192(4) 0.1075(18) Uani 1 1 d D U . . .
C1 C -0.3401(5) 1.5102(4) -0.4176(4) 0.0858(16) Uani 1 1 d . . . . .
H1A H -0.3895 1.5627 -0.4214 0.129 Uiso 1 1 calc GR . . . .
H1B H -0.3783 1.4602 -0.3640 0.129 Uiso 1 1 calc GR . . . .
H1C H -0.3480 1.4990 -0.4664 0.129 Uiso 1 1 calc GR . . . .
C2 C -0.1274(8) 1.6200(4) -0.4881(4) 0.0935(18) Uani 1 1 d D . . . .
H2A H -0.1352 1.6307 -0.5462 0.140 Uiso 1 1 calc GR . . . .
H2B H -0.0318 1.6216 -0.4850 0.140 Uiso 1 1 calc GR . . . .
H2C H -0.1749 1.6651 -0.4740 0.140 Uiso 1 1 calc GR . . . .
C3 C -0.1133(7) 1.4780(6) -0.3830(5) 0.103(2) Uani 1 1 d . U . . .
C4 C -0.1802(7) 1.3804(4) -0.3199(4) 0.0944(18) Uani 1 1 d . . . . .
H4A H -0.1692 1.3449 -0.3517 0.142 Uiso 1 1 calc GR . . . .
H4B H -0.2766 1.3851 -0.2997 0.142 Uiso 1 1 calc GR . . . .
H4C H -0.1348 1.3529 -0.2706 0.142 Uiso 1 1 calc GR . . . .
C9 C 0.9774(6) 0.3970(3) 0.0959(3) 0.0730(13) Uani 1 1 d . . . . .
H9A H 0.9711 0.4029 0.0390 0.110 Uiso 1 1 calc GR . . . .
H9B H 1.0406 0.4418 0.0898 0.110 Uiso 1 1 calc GR . . . .
H9C H 0.8880 0.4043 0.1254 0.110 Uiso 1 1 calc GR . . . .
C10 C 1.0299(8) 0.3034(5) 0.1501(4) 0.103(2) Uani 1 1 d . U . . .
C11 C 1.2053(7) 0.2050(4) 0.1772(5) 0.106(2) Uani 1 1 d D . . . .
H11A H 1.2632 0.1850 0.1381 0.159 Uiso 1 1 calc GR . . . .
H11B H 1.1305 0.1627 0.2113 0.159 Uiso 1 1 calc GR . . . .
H11C H 1.2584 0.2106 0.2155 0.159 Uiso 1 1 calc GR . . . .
C12 C 1.2404(6) 0.3592(4) 0.0429(4) 0.099(2) Uani 1 1 d . . . . .
H12A H 1.3170 0.3752 0.0603 0.149 Uiso 1 1 calc GR . . . .
H12B H 1.1953 0.4121 0.0093 0.149 Uiso 1 1 calc GR . . . .
H12C H 1.2730 0.3281 0.0078 0.149 Uiso 1 1 calc GR . . . .
C13 C 0.6978(12) -0.0331(8) 0.4946(8) 0.190(5) Uani 1 1 d . U . . .
H13A H 0.7004 -0.0519 0.5553 0.285 Uiso 1 1 calc GR . . . .
H13B H 0.6777 -0.0836 0.4858 0.285 Uiso 1 1 calc DGR . . . .
H13C H 0.6275 0.0100 0.4779 0.285 Uiso 1 1 calc GR . . . .
C14 C 0.8186(15) -0.1394(7) 0.4470(8) 0.214(5) Uani 1 1 d D U . . .
H14A H 0.7699 -0.1618 0.5065 0.320 Uiso 1 1 calc DGR . . . .
H14B H 0.8851 -0.1818 0.4414 0.320 Uiso 1 1 calc GR . . . .
H14C H 0.7543 -0.1301 0.4090 0.320 Uiso 1 1 calc GR . . . .
C15 C 0.8315(9) 0.0069(4) 0.4412(5) 0.099(2) Uani 1 1 d . U . . .
C16 C 1.0329(14) -0.0209(10) 0.3714(9) 0.246(7) Uani 1 1 d D U . . .
H16A H 1.0290 0.0207 0.3122 0.369 Uiso 1 1 calc GR . . . .
H16B H 1.0833 -0.0718 0.3716 0.369 Uiso 1 1 calc GR . . . .
H16C H 1.0783 0.0071 0.3978 0.369 Uiso 1 1 calc GR . . . .
C17 C 0.2901(3) 1.3290(2) -0.2871(2) 0.0385(7) Uani 1 1 d . . . . .
C18 C 0.3909(3) 1.27218(19) -0.3151(2) 0.0344(7) Uani 1 1 d . . . . .
C19 C 0.4896(3) 1.3108(2) -0.3919(2) 0.0374(7) Uani 1 1 d . . . . .
H19 H 0.4881 1.3717 -0.4275 0.045 Uiso 1 1 calc R . . . .
C20 C 0.5905(3) 1.2600(2) -0.4164(2) 0.0374(7) Uani 1 1 d . . . . .
C21 C 0.5909(4) 1.1693(2) -0.3621(2) 0.0393(7) Uani 1 1 d . . . . .
H21 H 0.6576 1.1341 -0.3768 0.047 Uiso 1 1 calc R . . . .
C22 C 0.4917(3) 1.13105(19) -0.2860(2) 0.0359(7) Uani 1 1 d . . . . .
C23 C 0.3903(3) 1.1809(2) -0.2614(2) 0.0351(7) Uani 1 1 d . . . . .
H23 H 0.3240 1.1543 -0.2107 0.042 Uiso 1 1 calc R . . . .
C24 C 0.7012(4) 1.3027(2) -0.4994(2) 0.0456(8) Uani 1 1 d . . . . .
C25 C 0.4217(4) 0.9766(2) -0.2390(2) 0.0454(8) Uani 1 1 d . . . . .
C26 C 0.4118(4) 0.8830(2) -0.1708(2) 0.0397(7) Uani 1 1 d . . . . .
C27 C 0.4641(3) 0.8612(2) -0.0946(2) 0.0334(7) Uani 1 1 d . . . . .
C28 C 0.5358(3) 0.9247(2) -0.0842(2) 0.0364(7) Uani 1 1 d . . . . .
C29 C 0.5553(4) 1.0175(2) -0.1541(2) 0.0409(8) Uani 1 1 d . . . . .
C30 C 0.5872(4) 0.9019(2) -0.0100(2) 0.0447(8) Uani 1 1 d . . . . .
H30 H 0.6363 0.9438 -0.0038 0.054 Uiso 1 1 calc R . . . .
C31 C 0.5656(4) 0.8143(2) 0.0574(2) 0.0438(8) Uani 1 1 d . . . . .
H31 H 0.5985 0.7994 0.1087 0.053 Uiso 1 1 calc R . . . .
C32 C 0.4974(3) 0.7511(2) 0.0488(2) 0.0342(7) Uani 1 1 d . . . . .
C33 C 0.4470(3) 0.77258(19) -0.0280(2) 0.0323(6) Uani 1 1 d . . . . .
C34 C 0.3830(4) 0.7076(2) -0.0408(2) 0.0378(7) Uani 1 1 d . . . . .
C35 C 0.3357(5) 0.7303(2) -0.1164(3) 0.0538(10) Uani 1 1 d . . . . .
H35 H 0.2946 0.6870 -0.1249 0.065 Uiso 1 1 calc R . . . .
C36 C 0.3487(5) 0.8187(2) -0.1814(3) 0.0559(10) Uani 1 1 d . . . . .
H36 H 0.3141 0.8337 -0.2322 0.067 Uiso 1 1 calc R . . . .
C37 C 0.4757(3) 0.6591(2) 0.1208(2) 0.0368(7) Uani 1 1 d . . . . .
C38 C 0.3705(4) 0.6130(2) 0.0269(2) 0.0391(7) Uani 1 1 d . . . . .
C39 C 0.4027(3) 0.50356(19) 0.1724(2) 0.0326(7) Uani 1 1 d . . . . .
C40 C 0.5194(3) 0.4607(2) 0.1987(2) 0.0340(7) Uani 1 1 d . . . . .
H40 H 0.6054 0.4896 0.1739 0.041 Uiso 1 1 calc R . . . .
C41 C 0.5069(3) 0.37327(19) 0.2632(2) 0.0315(6) Uani 1 1 d . . . . .
C42 C 0.3773(3) 0.32867(19) 0.2986(2) 0.0304(6) Uani 1 1 d . . . . .
H42 H 0.3706 0.2691 0.3392 0.036 Uiso 1 1 calc R . . . .
C43 C 0.2603(3) 0.37336(19) 0.2731(2) 0.0295(6) Uani 1 1 d . . . . .
C44 C 0.2722(3) 0.46198(19) 0.2101(2) 0.0315(6) Uani 1 1 d . . . . .
H44 H 0.1937 0.4932 0.1933 0.038 Uiso 1 1 calc R . . . .
C45 C 0.6316(3) 0.3268(2) 0.2969(2) 0.0334(7) Uani 1 1 d . . . . .
C46 C 0.1206(3) 0.32594(19) 0.31460(19) 0.0297(6) Uani 1 1 d . . . . .
O16 O 0.7830(4) 0.9883(3) 0.0713(3) 0.0950(12) Uani 1 1 d . . . . .
N5 N 0.9144(7) 1.1100(4) 0.0189(5) 0.124(2) Uani 1 1 d . U . . .
C5 C 0.8547(7) 1.1425(5) -0.0674(4) 0.102(2) Uani 1 1 d . . . . .
H5A H 0.8231 1.2022 -0.0837 0.153 Uiso 1 1 calc GR . . . .
H5B H 0.7789 1.1039 -0.0577 0.153 Uiso 1 1 calc GR . . . .
H5C H 0.9255 1.1414 -0.1136 0.153 Uiso 1 1 calc GR . . . .
C6 C 1.0189(8) 1.1696(5) 0.0169(5) 0.122(3) Uani 1 1 d . . . . .
H6A H 1.1091 1.1511 -0.0002 0.183 Uiso 1 1 calc GR . . . .
H6B H 1.0104 1.1673 0.0741 0.183 Uiso 1 1 calc GR . . . .
H6C H 1.0058 1.2294 -0.0245 0.183 Uiso 1 1 calc GR . . . .
C7 C 0.8681(8) 1.0374(5) 0.0693(6) 0.113(2) Uani 1 1 d . U . . .
C8 C 0.9386(9) 1.0084(6) 0.1556(5) 0.132(3) Uani 1 1 d . . . . .
H8A H 0.9061 1.0458 0.1841 0.198 Uiso 1 1 calc GR . . . .
H8B H 1.0371 1.0150 0.1379 0.198 Uiso 1 1 calc GR . . . .
H8C H 0.9138 0.9474 0.1955 0.198 Uiso 1 1 calc GR . . . .




_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
Ca1 Cl1 2.7708(11) . ?
Ca1 Ca2 3.6984(8) 2_675 ?
Ca1 O2 2.418(2) . ?
Ca1 O3 2.357(3) 2_684 ?
Ca1 O9 2.330(2) 2_575 ?
Ca1 O12 2.331(2) 2_675 ?
Ca1 O15 2.268(3) . ?
Ca1 C24 3.239(4) 2_684 ?
Ca2 Ca1 3.6984(8) 2_675 ?
Ca2 O4 2.300(3) 1_546 ?
Ca2 O9 2.518(2) 1_655 ?
Ca2 O10 2.455(2) 1_655 ?
Ca2 O11 2.436(2) . ?
Ca2 O12 2.561(2) . ?
Ca2 O13 2.339(3) . ?
Ca2 O14 2.280(3) . ?
Ca2 C45 2.832(3) . ?
Ca2 C46 2.831(3) 1_655 ?
O1 C17 1.327(4) . ?
O2 C17 1.219(4) . ?
O3 Ca1 2.357(3) 2_684 ?
O3 C24 1.241(4) . ?
O4 Ca2 2.300(3) 1_564 ?
O4 C24 1.251(5) . ?
O5 C25 1.197(4) . ?
O6 C29 1.209(4) . ?
O7 C38 1.199(4) . ?
O8 C37 1.202(4) . ?
O9 Ca1 2.330(2) 2_575 ?
O9 Ca2 2.518(2) 1_455 ?
O9 C46 1.255(4) . ?
O10 Ca2 2.455(2) 1_455 ?
O10 C46 1.253(4) . ?
O11 C45 1.246(4) . ?
O12 Ca1 2.331(2) 2_675 ?
O12 C45 1.270(4) . ?
O13 C10 1.299(7) . ?
O14 C15 1.183(6) . ?
O15 C3 1.249(8) . ?
N1 C22 1.450(4) . ?
N1 C25 1.394(4) . ?
N1 C29 1.392(4) . ?
N2 C37 1.405(4) . ?
N2 C38 1.402(4) . ?
N2 C39 1.459(4) . ?
N3 C14 1.568(8) . ?
N3 C15 1.231(11) . ?
N3 C16 1.445(9) . ?
N4 C10 1.144(8) . ?
N4 C11 1.639(7) . ?
N4 C12 1.451(7) . ?
N6 C1 1.457(7) . ?
N6 C2 1.611(7) . ?
N6 C3 1.155(8) . ?
C3 C4 1.604(10) . ?
C9 C10 1.550(9) . ?
C13 C15 1.460(12) . ?
C17 C18 1.493(4) . ?
C18 C19 1.396(5) . ?
C18 C23 1.394(4) . ?
C19 C20 1.395(5) . ?
C20 C21 1.389(4) . ?
C20 C24 1.532(5) . ?
C21 C22 1.391(5) . ?
C22 C23 1.387(5) . ?
C24 Ca1 3.239(4) 2_684 ?
C25 C26 1.484(4) . ?
C26 C27 1.401(5) . ?
C26 C36 1.371(5) . ?
C27 C28 1.405(4) . ?
C27 C33 1.415(4) . ?
C28 C29 1.484(4) . ?
C28 C30 1.363(5) . ?
C30 C31 1.410(5) . ?
C31 C32 1.364(5) . ?
C32 C33 1.401(4) . ?
C32 C37 1.488(4) . ?
C33 C34 1.407(4) . ?
C34 C35 1.362(5) . ?
C34 C38 1.492(4) . ?
C35 C36 1.404(5) . ?
C39 C40 1.368(4) . ?
C39 C44 1.397(4) . ?
C40 C41 1.390(4) . ?
C41 C42 1.407(4) . ?
C41 C45 1.494(4) . ?
C42 C43 1.378(4) . ?
C43 C44 1.396(4) . ?
C43 C46 1.515(4) . ?
C46 Ca2 2.831(3) 1_455 ?
O16 C7 1.197(9) . ?
N5 C5 1.572(9) . ?
N5 C6 1.463(9) . ?
N5 C7 1.193(9) . ?
C7 C8 1.639(11) . ?


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
Cl1 Ca1 Ca2 115.14(3) . 2_675 ?
Cl1 Ca1 C24 169.55(7) . 2_684 ?
O2 Ca1 Cl1 84.38(6) . . ?
O2 Ca1 Ca2 149.66(6) . 2_675 ?
O2 Ca1 C24 101.09(9) . 2_684 ?
O3 Ca1 Cl1 165.06(9) 2_684 . ?
O3 Ca1 Ca2 73.67(7) 2_684 2_675 ?
O3 Ca1 O2 82.95(9) 2_684 . ?
O3 Ca1 C24 18.17(10) 2_684 2_684 ?
O9 Ca1 Cl1 87.84(6) 2_575 . ?
O9 Ca1 Ca2 42.21(5) 2_575 2_675 ?
O9 Ca1 O2 168.13(8) 2_575 . ?
O9 Ca1 O3 105.86(10) 2_575 2_684 ?
O9 Ca1 O12 74.86(8) 2_575 2_675 ?
O9 Ca1 C24 88.04(9) 2_575 2_684 ?
O12 Ca1 Cl1 97.09(7) 2_675 . ?
O12 Ca1 Ca2 43.27(5) 2_675 2_675 ?
O12 Ca1 O2 114.97(9) 2_675 . ?
O12 Ca1 O3 81.21(10) 2_675 2_684 ?
O12 Ca1 C24 72.55(9) 2_675 2_684 ?
O15 Ca1 Cl1 95.46(10) . . ?
O15 Ca1 Ca2 113.65(9) . 2_675 ?
O15 Ca1 O2 85.48(11) . . ?
O15 Ca1 O3 91.40(13) . 2_684 ?
O15 Ca1 O9 86.34(10) . 2_575 ?
O15 Ca1 O12 156.90(11) . 2_675 ?
O15 Ca1 C24 93.86(12) . 2_684 ?
C24 Ca1 Ca2 56.32(7) 2_684 2_675 ?
O4 Ca2 Ca1 65.36(7) 1_546 2_675 ?
O4 Ca2 O9 86.91(10) 1_546 1_655 ?
O4 Ca2 O10 96.70(10) 1_546 1_655 ?
O4 Ca2 O11 86.85(10) 1_546 . ?
O4 Ca2 O12 84.52(9) 1_546 . ?
O4 Ca2 O13 169.10(11) 1_546 . ?
O4 Ca2 C45 85.73(10) 1_546 . ?
O4 Ca2 C46 94.91(10) 1_546 1_655 ?
O9 Ca2 Ca1 38.43(5) 1_655 2_675 ?
O9 Ca2 O12 67.79(7) 1_655 . ?
O9 Ca2 C45 94.42(8) 1_655 . ?
O9 Ca2 C46 26.32(8) 1_655 1_655 ?
O10 Ca2 Ca1 87.76(5) 1_655 2_675 ?
O10 Ca2 O9 52.23(7) 1_655 1_655 ?
O10 Ca2 O12 119.73(7) 1_655 . ?
O10 Ca2 C45 146.14(8) 1_655 . ?
O10 Ca2 C46 26.21(8) 1_655 1_655 ?
O11 Ca2 Ca1 86.56(6) . 2_675 ?
O11 Ca2 O9 120.39(7) . 1_655 ?
O11 Ca2 O10 171.35(8) . 1_655 ?
O11 Ca2 O12 52.61(7) . . ?
O11 Ca2 C45 25.99(8) . . ?
O11 Ca2 C46 145.83(8) . 1_655 ?
O12 Ca2 Ca1 38.60(5) . 2_675 ?
O12 Ca2 C45 26.63(8) . . ?
O12 Ca2 C46 93.51(8) . 1_655 ?
O13 Ca2 Ca1 103.74(8) . 2_675 ?
O13 Ca2 O9 83.83(9) . 1_655 ?
O13 Ca2 O10 82.15(10) . 1_655 ?
O13 Ca2 O11 92.86(10) . . ?
O13 Ca2 O12 86.65(10) . . ?
O13 Ca2 C45 89.25(10) . . ?
O13 Ca2 C46 79.25(9) . 1_655 ?
O14 Ca2 Ca1 162.69(12) . 2_675 ?
O14 Ca2 O4 97.46(14) . 1_546 ?
O14 Ca2 O9 144.63(11) . 1_655 ?
O14 Ca2 O10 92.42(11) . 1_655 ?
O14 Ca2 O11 94.94(11) . . ?
O14 Ca2 O12 147.45(11) . . ?
O14 Ca2 O13 93.42(15) . . ?
O14 Ca2 C45 120.86(12) . . ?
O14 Ca2 C46 118.51(12) . 1_655 ?
C45 Ca2 Ca1 62.50(6) . 2_675 ?
C46 Ca2 Ca1 63.74(6) 1_655 2_675 ?
C46 Ca2 C45 119.98(9) 1_655 . ?
C17 O2 Ca1 137.0(2) . . ?
C24 O3 Ca1 125.5(3) . 2_684 ?
C24 O4 Ca2 134.4(3) . 1_564 ?
Ca1 O9 Ca2 99.36(7) 2_575 1_455 ?
C46 O9 Ca1 158.0(2) . 2_575 ?
C46 O9 Ca2 90.87(17) . 1_455 ?
C46 O10 Ca2 93.89(17) . 1_455 ?
C45 O11 Ca2 95.06(18) . . ?
Ca1 O12 Ca2 98.13(8) 2_675 . ?
C45 O12 Ca1 147.3(2) . 2_675 ?
C45 O12 Ca2 88.70(17) . . ?
C10 O13 Ca2 130.4(3) . . ?
C15 O14 Ca2 159.4(4) . . ?
C3 O15 Ca1 143.5(4) . . ?
C25 N1 C22 118.2(3) . . ?
C29 N1 C22 116.1(3) . . ?
C29 N1 C25 125.3(3) . . ?
C37 N2 C39 117.8(3) . . ?
C38 N2 C37 124.7(2) . . ?
C38 N2 C39 117.5(3) . . ?
C15 N3 C14 118.7(10) . . ?
C15 N3 C16 114.4(10) . . ?
C16 N3 C14 126.9(12) . . ?
C10 N4 C11 109.2(6) . . ?
C10 N4 C12 137.0(7) . . ?
C12 N4 C11 113.5(5) . . ?
C1 N6 C2 115.9(5) . . ?
C3 N6 C1 133.6(7) . . ?
C3 N6 C2 110.4(6) . . ?
O15 C3 C4 120.2(6) . . ?
N6 C3 O15 130.2(9) . . ?
N6 C3 C4 109.5(7) . . ?
O13 C10 C9 122.3(6) . . ?
N4 C10 O13 130.4(8) . . ?
N4 C10 C9 107.3(6) . . ?
O14 C15 N3 130.1(9) . . ?
O14 C15 C13 122.2(9) . . ?
N3 C15 C13 107.7(8) . . ?
O1 C17 C18 113.9(3) . . ?
O2 C17 O1 124.0(3) . . ?
O2 C17 C18 122.1(3) . . ?
C19 C18 C17 120.2(3) . . ?
C23 C18 C17 119.4(3) . . ?
C23 C18 C19 120.3(3) . . ?
C20 C19 C18 121.3(3) . . ?
C19 C20 C24 121.3(3) . . ?
C21 C20 C19 118.3(3) . . ?
C21 C20 C24 120.3(3) . . ?
C20 C21 C22 120.1(3) . . ?
C21 C22 N1 121.2(3) . . ?
C23 C22 N1 116.7(3) . . ?
C23 C22 C21 122.0(3) . . ?
C22 C23 C18 118.0(3) . . ?
O3 C24 Ca1 36.31(18) . 2_684 ?
O3 C24 O4 124.9(3) . . ?
O3 C24 C20 117.5(3) . . ?
O4 C24 Ca1 88.7(2) . 2_684 ?
O4 C24 C20 117.6(3) . . ?
C20 C24 Ca1 153.6(2) . 2_684 ?
O5 C25 N1 119.8(3) . . ?
O5 C25 C26 123.3(3) . . ?
N1 C25 C26 116.9(3) . . ?
C27 C26 C25 119.6(3) . . ?
C36 C26 C25 120.1(3) . . ?
C36 C26 C27 120.3(3) . . ?
C26 C27 C28 121.3(3) . . ?
C26 C27 C33 118.9(3) . . ?
C28 C27 C33 119.7(3) . . ?
C27 C28 C29 120.0(3) . . ?
C30 C28 C27 120.4(3) . . ?
C30 C28 C29 119.6(3) . . ?
O6 C29 N1 119.7(3) . . ?
O6 C29 C28 123.8(3) . . ?
N1 C29 C28 116.6(3) . . ?
C28 C30 C31 119.6(3) . . ?
C32 C31 C30 121.2(3) . . ?
C31 C32 C33 120.1(3) . . ?
C31 C32 C37 120.3(3) . . ?
C33 C32 C37 119.7(3) . . ?
C32 C33 C27 118.9(3) . . ?
C32 C33 C34 121.3(3) . . ?
C34 C33 C27 119.8(3) . . ?
C33 C34 C38 120.3(3) . . ?
C35 C34 C33 120.0(3) . . ?
C35 C34 C38 119.6(3) . . ?
C34 C35 C36 120.4(3) . . ?
C26 C36 C35 120.6(3) . . ?
O8 C37 N2 120.4(3) . . ?
O8 C37 C32 122.4(3) . . ?
N2 C37 C32 117.2(3) . . ?
O7 C38 N2 120.6(3) . . ?
O7 C38 C34 123.0(3) . . ?
N2 C38 C34 116.4(3) . . ?
C40 C39 N2 118.7(3) . . ?
C40 C39 C44 121.5(3) . . ?
C44 C39 N2 119.8(3) . . ?
C39 C40 C41 118.7(3) . . ?
C40 C41 C42 120.6(3) . . ?
C40 C41 C45 119.8(3) . . ?
C42 C41 C45 119.6(3) . . ?
C43 C42 C41 119.9(3) . . ?
C42 C43 C44 119.5(3) . . ?
C42 C43 C46 119.5(3) . . ?
C44 C43 C46 121.0(2) . . ?
C43 C44 C39 119.6(3) . . ?
O11 C45 Ca2 58.96(15) . . ?
O11 C45 O12 123.6(3) . . ?
O11 C45 C41 119.2(3) . . ?
O12 C45 Ca2 64.67(15) . . ?
O12 C45 C41 117.2(3) . . ?
C41 C45 Ca2 177.3(2) . . ?
O9 C46 Ca2 62.81(15) . 1_455 ?
O9 C46 C43 118.5(3) . . ?
O10 C46 Ca2 59.90(14) . 1_455 ?
O10 C46 O9 121.6(3) . . ?
O10 C46 C43 119.9(3) . . ?
C43 C46 Ca2 167.3(2) . 1_455 ?
C6 N5 C5 115.2(6) . . ?
C7 N5 C5 109.4(8) . . ?
C7 N5 C6 135.1(9) . . ?
O16 C7 C8 118.5(8) . . ?
N5 C7 O16 135.4(10) . . ?
N5 C7 C8 105.9(8) . . ?


_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 3.574
_oxdiff_exptl_absorpt_empirical_full_min 0.667







