# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_h
_database_code_depnum_ccdc_archive 'CCDC 998392'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C240 H144 Cd24 K4 N192 O48, 4(Br)'
_chemical_formula_sum            'C240 H144 Br4 Cd24 K4 N192 O48'
_chemical_formula_weight         9659.11
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y+1/2, -z, x+1/2'
'z+1/2, -x+1/2, -y'
'-y, z+1/2, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y-1/2, z, -x-1/2'
'-z-1/2, x-1/2, y'
'y, -z-1/2, x-1/2'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y-1/2, z-1/2, x'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.6387(10)
_cell_length_b                   20.6387(10)
_cell_length_c                   20.6387(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8791.2(13)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.689
_shelx_estimated_absorpt_T_min   0.689
_exptl_absorpt_coefficient_mu    2.010
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            90102
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         1.709
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2281
_reflns_number_total             2598
_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    ?
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2598
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0197
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.243
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0233P)²+10.7562P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0525
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B), O12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.60079(2) 0.44019(2) 0.27526(2) 0.02222(7) Uani 1 1 d . . . . .
K1 K 1.0000 0.5000 0.5000 0.0401(4) Uani 1 6 d S T P . .
O2 O 0.64380(10) 0.33756(9) 0.29596(11) 0.0397(5) Uani 1 1 d . . . . .
H2A H 0.6775 0.3406 0.3215 0.059 Uiso 1 1 d GR . . . .
H2B H 0.6151 0.3127 0.3149 0.059 Uiso 1 1 d GR . . . .
O12 O 0.53001(11) 0.42230(11) 0.36242(10) 0.0440(5) Uani 1 1 d . . . . .
H12A H 0.5306 0.3821 0.3727 0.066 Uiso 1 1 d GR . . . .
H12B H 0.5420 0.4449 0.3950 0.066 Uiso 1 1 d GR . . . .
N1 N 0.67530(11) 0.46351(11) 0.36038(11) 0.0290(5) Uani 1 1 d . . . . .
N2 N 0.72365(11) 0.43412(11) 0.45367(11) 0.0292(5) Uani 1 1 d . . . . .
N3 N 0.77276(18) 0.57601(18) 0.28027(16) 0.0700(10) Uani 1 1 d . . . . .
N4 N 0.87285(19) 0.5039(3) 0.4701(2) 0.116(2) Uani 1 1 d . . . . .
N5 N 0.51286(11) 0.38879(11) 0.22222(11) 0.0295(5) Uani 1 1 d . . . . .
N6 N 0.39744(17) 0.49060(19) 0.29774(19) 0.0783(12) Uani 1 1 d . . . . .
N7 N 0.45595(10) 0.31402(11) 0.16573(11) 0.0283(5) Uani 1 1 d . . . . .
N8 N 0.28948(13) 0.34766(15) 0.19178(17) 0.0560(8) Uani 1 1 d . . . . .
C1 C 0.67237(14) 0.42871(14) 0.41497(13) 0.0305(6) Uani 1 1 d . . . . .
H1 H 0.6371 0.4026 0.4251 0.037 Uiso 1 1 calc R . . . .
C2 C 0.73363(14) 0.49409(13) 0.36467(13) 0.0291(6) Uani 1 1 d . . . . .
C3 C 0.75540(17) 0.53917(16) 0.31748(15) 0.0427(8) Uani 1 1 d . . . . .
C4 C 0.76302(14) 0.47603(14) 0.42161(14) 0.0320(6) Uani 1 1 d . . . . .
C5 C 0.82438(18) 0.4930(2) 0.44730(18) 0.0602(11) Uani 1 1 d . . . . .
C6 C 0.51405(13) 0.33759(13) 0.18277(13) 0.0280(6) Uani 1 1 d . . . . .
H6 H 0.5526 0.3195 0.1681 0.034 Uiso 1 1 calc R . . . .
C7 C 0.44821(14) 0.39962(14) 0.23118(14) 0.0312(6) Uani 1 1 d . . . . .
C8 C 0.42136(16) 0.45040(17) 0.26895(17) 0.0467(9) Uani 1 1 d . . . . .
C9 C 0.41345(13) 0.35400(14) 0.19695(14) 0.0286(6) Uani 1 1 d . . . . .
C10 C 0.34451(14) 0.34871(15) 0.19357(15) 0.0360(7) Uani 1 1 d . . . . .
Br1 Br 0.5000 0.5000 0.5000 0.04242(19) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O2 2.3361(19) . ?
Cd1 O12 2.347(2) . ?
Cd1 N1 2.384(2) . ?
Cd1 N2 2.306(2) 15_666 ?
Cd1 N5 2.370(2) . ?
Cd1 N7 2.302(2) 19_656 ?
K1 N4 2.697(4) 4_664 ?
K1 N4 2.697(4) 5_566 ?
K1 N4 2.697(4) . ?
K1 N4 2.697(4) 16_657 ?
K1 N4 2.697(4) 17_755 ?
K1 N4 2.697(4) 13_766 ?
O2 H2A 0.8747 . ?
O2 H2B 0.8757 . ?
O12 H12A 0.8561 . ?
O12 H12B 0.8557 . ?
N1 C1 1.337(3) . ?
N1 C2 1.362(4) . ?
N2 Cd1 2.306(2) 14_666 ?
N2 C1 1.331(3) . ?
N2 C4 1.359(4) . ?
N3 C3 1.139(4) . ?
N4 C5 1.128(5) . ?
N5 C6 1.334(3) . ?
N5 C7 1.366(4) . ?
N6 C8 1.134(4) . ?
N7 Cd1 2.301(2) 18_565 ?
N7 C6 1.341(3) . ?
N7 C9 1.366(3) . ?
N8 C10 1.136(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.420(4) . ?
C2 C4 1.374(4) . ?
C4 C5 1.417(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.419(4) . ?
C7 C9 1.379(4) . ?
C9 C10 1.429(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cd1 O12 87.35(8) . . ?
O2 Cd1 N1 78.65(8) . . ?
O2 Cd1 N5 88.25(8) . . ?
O12 Cd1 N1 82.44(8) . . ?
O12 Cd1 N5 78.87(8) . . ?
N2 Cd1 O2 168.02(8) 15_666 . ?
N2 Cd1 O12 86.99(8) 15_666 . ?
N2 Cd1 N1 90.15(8) 15_666 . ?
N2 Cd1 N5 100.98(8) 15_666 . ?
N5 Cd1 N1 157.62(8) . . ?
N7 Cd1 O2 93.05(8) 19_656 . ?
N7 Cd1 O12 176.84(8) 19_656 . ?
N7 Cd1 N1 100.71(8) 19_656 . ?
N7 Cd1 N2 93.19(8) 19_656 15_666 ?
N7 Cd1 N5 98.01(8) 19_656 . ?
N4 K1 N4 75.04(14) . 5_566 ?
N4 K1 N4 75.04(14) 4_664 5_566 ?
N4 K1 N4 75.04(14) 13_766 17_755 ?
N4 K1 N4 104.96(14) . 16_657 ?
N4 K1 N4 104.96(14) 16_657 5_566 ?
N4 K1 N4 104.96(14) 4_664 17_755 ?
N4 K1 N4 180.0 . 13_766 ?
N4 K1 N4 75.04(14) . 4_664 ?
N4 K1 N4 104.96(14) . 17_755 ?
N4 K1 N4 104.96(14) 13_766 5_566 ?
N4 K1 N4 104.96(14) 13_766 4_664 ?
N4 K1 N4 75.04(14) 13_766 16_657 ?
N4 K1 N4 75.04(14) 16_657 17_755 ?
N4 K1 N4 180.0 17_755 5_566 ?
N4 K1 N4 180.0 16_657 4_664 ?
Cd1 O2 H2A 110.3 . . ?
Cd1 O2 H2B 110.8 . . ?
H2A O2 H2B 108.1 . . ?
Cd1 O12 H12A 109.5 . . ?
Cd1 O12 H12B 109.7 . . ?
H12A O12 H12B 109.2 . . ?
C1 N1 Cd1 118.90(18) . . ?
C1 N1 C2 103.5(2) . . ?
C2 N1 Cd1 135.36(18) . . ?
C1 N2 Cd1 123.49(18) . 14_666 ?
C1 N2 C4 103.7(2) . . ?
C4 N2 Cd1 130.97(18) . 14_666 ?
C5 N4 K1 162.2(5) . . ?
C6 N5 Cd1 128.49(18) . . ?
C6 N5 C7 103.3(2) . . ?
C7 N5 Cd1 127.76(18) . . ?
C6 N7 Cd1 124.71(18) . 18_565 ?
C6 N7 C9 103.4(2) . . ?
C9 N7 Cd1 131.89(18) . 18_565 ?
N1 C1 H1 122.4 . . ?
N2 C1 N1 115.1(3) . . ?
N2 C1 H1 122.4 . . ?
N1 C2 C3 122.6(3) . . ?
N1 C2 C4 108.7(2) . . ?
C4 C2 C3 128.7(3) . . ?
N3 C3 C2 179.0(4) . . ?
N2 C4 C2 109.0(2) . . ?
N2 C4 C5 120.6(3) . . ?
C2 C4 C5 130.4(3) . . ?
N4 C5 C4 176.3(4) . . ?
N5 C6 N7 115.5(2) . . ?
N5 C6 H6 122.2 . . ?
N7 C6 H6 122.2 . . ?
N5 C7 C8 125.2(3) . . ?
N5 C7 C9 109.1(2) . . ?
C9 C7 C8 125.7(3) . . ?
N6 C8 C7 177.0(4) . . ?
N7 C9 C7 108.7(2) . . ?
N7 C9 C10 124.8(3) . . ?
C7 C9 C10 126.5(3) . . ?
N8 C10 C9 176.6(3) . . ?

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
####################################################################### 
# 
# 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_test
_database_code_depnum_ccdc_archive 'CCDC 998394'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.02(C240 H144 Cd24 K4 N192 O48), 0.06(Cl)'
_chemical_formula_sum            'C H Cd Cl K N O'
_chemical_formula_weight         229.98
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y+1/2, -z, x+1/2'
'z+1/2, -x+1/2, -y'
'-y, z+1/2, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y-1/2, z, -x-1/2'
'-z-1/2, x-1/2, y'
'y, -z-1/2, x-1/2'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y-1/2, z-1/2, x'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.496(7)
_cell_length_b                   20.496(7)
_cell_length_c                   20.496(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8610(8)
_cell_formula_units_Z            62
_cell_measurement_reflns_used    3841
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.62
_cell_measurement_theta_min      2.22
_shelx_estimated_absorpt_T_max   0.433
_shelx_estimated_absorpt_T_min   0.433
_exptl_absorpt_coefficient_mu    5.021
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.750
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             6572
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1856
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44900
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.222
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1895
_reflns_number_total             2544
_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    ?
_refine_diff_density_max         0.426
_refine_diff_density_min         -1.941
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      0.960
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0503P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0948
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All Cl(H,H,H,H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.85 with sigma of 0.01
 O2-H2A = O2-H2B
 0.85 with sigma of 0.01
 H1B-H1A
 1.387 with sigma of 0.02
 H2B-H2A
 1.387 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.10330(2) 0.44118(2) 0.22425(2) 0.02453(15) Uani 1 1 d . . . . .
K K 0.0000 0.5000 0.5000 0.0806(14) Uani 1 6 d S T P . .
O1 O 0.14475(19) 0.33857(17) 0.2019(2) 0.0426(10) Uani 1 1 d D . . . .
O2 O 0.0320(2) 0.4265(2) 0.13436(19) 0.0428(10) Uani 1 1 d D . . . .
N1 N 0.0677(2) 0.5468(2) 0.2276(2) 0.0295(10) Uani 1 1 d . . . . .
N2 N 0.0335(2) 0.6392(2) 0.1784(2) 0.0310(10) Uani 1 1 d . . . . .
N3 N 0.0099(3) 0.5337(3) 0.3843(3) 0.0658(18) Uani 1 1 d . . . . .
N4 N -0.0769(3) 0.7196(3) 0.2797(3) 0.0715(19) Uani 1 1 d . . . . .
N5 N 0.1690(2) 0.4568(2) 0.3144(2) 0.0302(10) Uani 1 1 d . . . . .
N6 N 0.2242(2) 0.5142(2) 0.3902(2) 0.0295(10) Uani 1 1 d . . . . .
N7 N 0.1941(3) 0.2901(3) 0.3474(3) 0.0542(15) Uani 1 1 d . . . . .
N8 N 0.2990(3) 0.3992(3) 0.4945(3) 0.076(2) Uani 1 1 d . . . . .
C1 C 0.0696(3) 0.5848(3) 0.1744(3) 0.0302(12) Uani 1 1 d . . . . .
H1 H 0.0939 0.5742 0.1377 0.036 Uiso 1 1 calc R . . . .
C2 C 0.0276(3) 0.5794(3) 0.2689(3) 0.0320(13) Uani 1 1 d . . . . .
C3 C 0.0153(3) 0.5546(3) 0.3331(3) 0.0403(15) Uani 1 1 d . . . . .
C4 C 0.0058(3) 0.6354(2) 0.2386(3) 0.0292(12) Uani 1 1 d . . . . .
C5 C -0.0395(3) 0.6828(3) 0.2615(3) 0.0416(15) Uani 1 1 d . . . . .
C6 C 0.1859(3) 0.5156(3) 0.3381(3) 0.0305(12) Uani 1 1 d . . . . .
H6 H 0.1717 0.5544 0.3193 0.037 Uiso 1 1 calc R . . . .
C7 C 0.2330(3) 0.4486(3) 0.4015(3) 0.0314(13) Uani 1 1 d . . . . .
C8 C 0.2700(3) 0.4231(3) 0.4536(3) 0.0448(16) Uani 1 1 d . . . . .
C9 C 0.1995(3) 0.4144(2) 0.3553(2) 0.0283(12) Uani 1 1 d . . . . .
C10 C 0.1957(3) 0.3450(3) 0.3500(3) 0.0371(14) Uani 1 1 d . . . . .
Cl Cl 0.0000 0.5000 0.0000 0.0453(9) Uani 1 6 d S T P . .
H1A H 0.124(2) 0.3035(17) 0.196(3) 0.068 Uiso 1 1 d DR . . . .
H1B H 0.1827(13) 0.337(3) 0.186(3) 0.068 Uiso 1 1 d DR . . . .
H2A H 0.025(3) 0.3867(9) 0.124(3) 0.068 Uiso 1 1 d DR . . . .
H2B H 0.022(3) 0.450(2) 0.1017(19) 0.068 Uiso 1 1 d DR . . . .


_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 O1 2.314(4) . ?
Cd1 O2 2.370(4) . ?
Cd1 N1 2.286(4) . ?
Cd1 N2 2.383(4) 20_565 ?
Cd1 N5 2.308(4) . ?
Cd1 N6 2.354(4) 16_556 ?
K N3 2.479(6) 4_565 ?
K N3 2.479(6) 16_556 ?
K N3 2.479(6) . ?
K N3 2.479(6) 17_665 ?
K N3 2.479(6) 13_566 ?
K N3 2.479(6) 5_456 ?
N1 C1 1.339(6) . ?
N1 C2 1.354(6) . ?
N2 Cd1 2.383(4) 21_665 ?
N2 C1 1.341(6) . ?
N2 C4 1.361(6) . ?
N3 C3 1.138(7) . ?
N4 C5 1.139(7) . ?
N5 C6 1.343(6) . ?
N5 C9 1.360(6) . ?
N6 Cd1 2.354(4) 17_665 ?
N6 C6 1.327(6) . ?
N6 C7 1.376(7) . ?
N7 C10 1.126(7) . ?
N8 C8 1.138(7) . ?
C2 C3 1.433(8) . ?
C2 C4 1.379(7) . ?
C4 C5 1.424(7) . ?
C7 C8 1.411(8) . ?
C7 C9 1.363(7) . ?
C9 C10 1.430(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O2 87.54(15) . . ?
O1 Cd1 N2 79.39(14) . 20_565 ?
O1 Cd1 N6 88.29(14) . 16_556 ?
O2 Cd1 N2 81.79(15) . 20_565 ?
N1 Cd1 O1 169.77(15) . . ?
N1 Cd1 O2 86.96(15) . . ?
N1 Cd1 N2 91.28(15) . 20_565 ?
N1 Cd1 N5 91.76(15) . . ?
N1 Cd1 N6 99.15(15) . 16_556 ?
N5 Cd1 O1 94.02(15) . . ?
N5 Cd1 O2 177.63(15) . . ?
N5 Cd1 N2 100.24(15) . 20_565 ?
N5 Cd1 N6 98.96(15) . 16_556 ?
N6 Cd1 O2 79.28(15) 16_556 . ?
N6 Cd1 N2 157.81(15) 16_556 20_565 ?
N3 K N3 180.0 . 13_566 ?
N3 K N3 80.5(2) . 5_456 ?
N3 K N3 80.5(2) 5_456 4_565 ?
N3 K N3 180.0 17_665 5_456 ?
N3 K N3 80.5(2) . 4_565 ?
N3 K N3 99.5(2) . 16_556 ?
N3 K N3 80.5(2) 17_665 16_556 ?
N3 K N3 180.0 4_565 16_556 ?
N3 K N3 80.5(2) 16_556 13_566 ?
N3 K N3 99.5(2) . 17_665 ?
N3 K N3 99.5(2) 4_565 13_566 ?
N3 K N3 99.5(2) 5_456 16_556 ?
N3 K N3 99.5(2) 5_456 13_566 ?
N3 K N3 99.5(2) 17_665 4_565 ?
N3 K N3 80.5(2) 17_665 13_566 ?
C1 N1 Cd1 121.1(3) . . ?
C1 N1 C2 103.9(4) . . ?
C2 N1 Cd1 132.8(3) . . ?
C1 N2 Cd1 116.7(3) . 21_665 ?
C1 N2 C4 103.7(4) . . ?
C4 N2 Cd1 136.0(4) . 21_665 ?
C3 N3 K 174.0(6) . . ?
C6 N5 Cd1 124.3(3) . . ?
C6 N5 C9 103.4(4) . . ?
C9 N5 Cd1 132.2(3) . . ?
C6 N6 Cd1 127.3(4) . 17_665 ?
C6 N6 C7 103.5(4) . . ?
C7 N6 Cd1 128.7(3) . 17_665 ?
N1 C1 N2 114.7(5) . . ?
N1 C2 C3 120.4(5) . . ?
N1 C2 C4 109.0(5) . . ?
C4 C2 C3 130.6(5) . . ?
N3 C3 C2 175.3(7) . . ?
N2 C4 C2 108.7(5) . . ?
N2 C4 C5 122.1(5) . . ?
C2 C4 C5 129.1(5) . . ?
N4 C5 C4 178.3(7) . . ?
N6 C6 N5 115.1(5) . . ?
N6 C7 C8 123.9(5) . . ?
C9 C7 N6 108.7(4) . . ?
C9 C7 C8 127.4(5) . . ?
N8 C8 C7 176.2(7) . . ?
N5 C9 C7 109.3(4) . . ?
N5 C9 C10 124.4(5) . . ?
C7 C9 C10 126.3(5) . . ?
N7 C10 C9 177.8(7) . . ?

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
####################################################################### 
# 
# 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_c35-3
_database_code_depnum_ccdc_archive 'CCDC 998395'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C240 H144 Cd24 N192 Na4 O48), 1(Br)'
_chemical_formula_sum            'C60 H36 Br Cd6 N48 Na O12'
_chemical_formula_weight         2398.67
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y+1/2, -z, x+1/2'
'z+1/2, -x+1/2, -y'
'-y, z+1/2, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y-1/2, z, -x-1/2'
'-z-1/2, x-1/2, y'
'y, -z-1/2, x-1/2'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y-1/2, z-1/2, x'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.5540(9)
_cell_length_b                   20.5540(9)
_cell_length_c                   20.5540(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8683.4(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.22
_shelx_estimated_absorpt_T_max   0.754
_shelx_estimated_absorpt_T_min   0.754
_exptl_absorpt_coefficient_mu    1.992
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            114947
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         1.716
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3066
_reflns_number_total             3614
_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    ?
_refine_diff_density_max         0.321
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3614
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0196
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²+9.3825P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0536
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H,H,H) groups
2. Restrained distances
 O2-H2A = O2-H2B
 0.85 with sigma of 0.01
 O1-H1A = O1-H1B
 0.85 with sigma of 0.01
 H2B-H2A
 1.387 with sigma of 0.02
 H1B-H1A
 1.387 with sigma of 0.02
 Cd1-H2A \\sim Cd1-H2B
 with sigma of 0.02
 Cd1-H1A \\sim Cd1-H1B
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.22496(2) 0.60382(2) 0.55856(2) 0.02056(5) Uani 1 1 d . . . . .
O2 O 0.20325(10) 0.64566(8) 0.66166(8) 0.0395(4) Uani 1 1 d D . . . .
N1 N 0.22752(9) 0.56808(9) 0.45264(9) 0.0260(4) Uani 1 1 d . . . . .
C7 C 0.26823(11) 0.44998(11) 0.59715(11) 0.0290(5) Uani 1 1 d . . . . .
N2 N 0.17822(9) 0.53390(9) 0.36071(9) 0.0271(4) Uani 1 1 d . . . . .
C1 C 0.17474(11) 0.56980(11) 0.41492(10) 0.0280(4) Uani 1 1 d . . . . .
H1 H 0.1381 0.5942 0.4255 0.034 Uiso 1 1 calc R . . . .
N6 N 0.33108(9) 0.45699(8) 0.68556(9) 0.0263(4) Uani 1 1 d . . . . .
N5 N 0.27734(9) 0.51477(9) 0.60878(9) 0.0274(4) Uani 1 1 d . . . . .
N7 N 0.30559(14) 0.29023(11) 0.65152(13) 0.0530(6) Uani 1 1 d . . . . .
C5 C 0.33307(12) 0.51605(13) 0.44402(12) 0.0368(5) Uani 1 1 d . . . . .
C2 C 0.26881(10) 0.52753(11) 0.42033(11) 0.0263(4) Uani 1 1 d . . . . .
O1 O 0.13727(8) 0.53243(9) 0.57659(9) 0.0408(4) Uani 1 1 d D . . . .
C6 C 0.31520(11) 0.51564(10) 0.66171(11) 0.0272(4) Uani 1 1 d . . . . .
H6 H 0.3295 0.5542 0.6806 0.033 Uiso 1 1 calc R . . . .
C9 C 0.30383(12) 0.34544(11) 0.64951(12) 0.0343(5) Uani 1 1 d . . . . .
C8 C 0.30094(11) 0.41471(10) 0.64408(11) 0.0265(4) Uani 1 1 d . . . . .
C10 C 0.23134(13) 0.42398(13) 0.54502(13) 0.0418(6) Uani 1 1 d . . . . .
C3 C 0.23861(10) 0.50642(11) 0.36429(10) 0.0265(4) Uani 1 1 d . . . . .
N8 N 0.20261(15) 0.40059(14) 0.50406(16) 0.0698(9) Uani 1 1 d . . . . .
N4 N 0.38416(12) 0.51085(15) 0.46417(14) 0.0601(7) Uani 1 1 d . . . . .
Br1 Br 0.0000 0.5000 0.5000 0.04328(15) Uani 1 6 d S T P . .
Na1 Na 0.5000 0.5000 0.5000 0.0266(4) Uani 1 6 d S T P . .
C4 C 0.26148(13) 0.46097(13) 0.31738(12) 0.0389(6) Uani 1 1 d . . . . .
N3 N 0.27858(15) 0.42394(15) 0.28018(13) 0.0679(8) Uani 1 1 d . . . . .
H2A H 0.195(2) 0.6853(6) 0.6687(11) 0.102 Uiso 1 1 d DR . . . .
H2B H 0.205(2) 0.6247(11) 0.6965(7) 0.102 Uiso 1 1 d DR . . . .
H1A H 0.1255(15) 0.5217(19) 0.6147(7) 0.102 Uiso 1 1 d DR . . . .
H1B H 0.1060(12) 0.527(2) 0.5509(11) 0.102 Uiso 1 1 d DR . . . .


_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 O2 2.3302(16) . ?
Cd1 N1 2.2983(17) . ?
Cd1 N2 2.3868(18) 17_665 ?
Cd1 N6 2.2967(17) 14_666 ?
Cd1 N5 2.3611(18) . ?
Cd1 O1 2.3536(17) . ?
N1 C1 1.334(3) . ?
N1 C2 1.362(3) . ?
C7 N5 1.366(3) . ?
C7 C8 1.381(3) . ?
C7 C10 1.417(3) . ?
N2 Cd1 2.3868(18) 16_556 ?
N2 C1 1.338(3) . ?
N2 C3 1.366(3) . ?
N6 Cd1 2.2967(17) 15_666 ?
N6 C6 1.342(3) . ?
N6 C8 1.366(3) . ?
N5 C6 1.338(3) . ?
N7 C9 1.136(3) . ?
C5 C2 1.427(3) . ?
C5 N4 1.134(3) . ?
C2 C3 1.379(3) . ?
C9 C8 1.429(3) . ?
C10 N8 1.135(3) . ?
C3 C4 1.422(3) . ?
N4 Na1 2.502(2) . ?
Na1 N4 2.502(2) 14_666 ?
Na1 N4 2.502(2) 3 ?
Na1 N4 2.502(2) 2 ?
Na1 N4 2.502(2) 15_666 ?
Na1 N4 2.502(2) 13_666 ?
C4 N3 1.135(3) . ?

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
O2 Cd1 N2 79.36(6) . 17_665 ?
O2 Cd1 N5 88.61(6) . . ?
O2 Cd1 O1 86.57(7) . . ?
N1 Cd1 O2 169.69(7) . . ?
N1 Cd1 N2 91.18(6) . 17_665 ?
N1 Cd1 N5 98.97(6) . . ?
N1 Cd1 O1 88.13(7) . . ?
N6 Cd1 O2 93.72(7) 14_666 . ?
N6 Cd1 N1 92.07(6) 14_666 . ?
N6 Cd1 N2 100.83(7) 14_666 17_665 ?
N6 Cd1 N5 98.48(6) 14_666 . ?
N6 Cd1 O1 176.75(7) 14_666 . ?
N5 Cd1 N2 157.81(6) . 17_665 ?
O1 Cd1 N2 82.41(7) . 17_665 ?
O1 Cd1 N5 78.29(6) . . ?
C1 N1 Cd1 121.56(14) . . ?
C1 N1 C2 103.87(17) . . ?
C2 N1 Cd1 132.19(14) . . ?
N5 C7 C8 108.83(19) . . ?
N5 C7 C10 125.0(2) . . ?
C8 C7 C10 126.2(2) . . ?
C1 N2 Cd1 117.57(14) . 16_556 ?
C1 N2 C3 103.41(17) . . ?
C3 N2 Cd1 135.22(14) . 16_556 ?
N1 C1 N2 115.19(19) . . ?
C6 N6 Cd1 124.01(14) . 15_666 ?
C6 N6 C8 103.49(17) . . ?
C8 N6 Cd1 132.49(14) . 15_666 ?
C7 N5 Cd1 128.08(14) . . ?
C6 N5 Cd1 127.62(14) . . ?
C6 N5 C7 103.61(18) . . ?
N4 C5 C2 175.7(3) . . ?
N1 C2 C5 120.8(2) . . ?
N1 C2 C3 108.63(18) . . ?
C3 C2 C5 130.5(2) . . ?
N5 C6 N6 115.25(19) . . ?
N7 C9 C8 177.5(3) . . ?
C7 C8 C9 126.7(2) . . ?
N6 C8 C7 108.82(18) . . ?
N6 C8 C9 124.5(2) . . ?
N8 C10 C7 177.1(3) . . ?
N2 C3 C2 108.90(18) . . ?
N2 C3 C4 122.4(2) . . ?
C2 C3 C4 128.6(2) . . ?
C5 N4 Na1 175.7(3) . . ?
N4 Na1 N4 80.27(10) 15_666 13_666 ?
N4 Na1 N4 80.27(10) 2 . ?
N4 Na1 N4 99.73(10) 3 14_666 ?
N4 Na1 N4 99.73(10) 13_666 2 ?
N4 Na1 N4 180.0 13_666 . ?
N4 Na1 N4 80.27(10) 13_666 14_666 ?
N4 Na1 N4 180.0 15_666 3 ?
N4 Na1 N4 99.73(10) 15_666 2 ?
N4 Na1 N4 80.27(10) 15_666 14_666 ?
N4 Na1 N4 80.27(10) 3 . ?
N4 Na1 N4 80.27(10) 3 2 ?
N4 Na1 N4 99.73(10) 3 13_666 ?
N4 Na1 N4 99.73(10) 15_666 . ?
N4 Na1 N4 99.73(10) 14_666 . ?
N4 Na1 N4 180.0 2 14_666 ?
N3 C4 C3 178.5(3) . . ?

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
####################################################################### 
# 
# 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_p
_database_code_depnum_ccdc_archive 'CCDC 998396'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.13(C240 H144 Cd24 N192 Na4 O48), 0.5(Cl)'
_chemical_formula_sum            'C30 H18 Cd3 Cl0.50 N24 Na0.50 O6'
_chemical_formula_weight         1177.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   20.5415(7)
_cell_length_b                   20.5415(7)
_cell_length_c                   20.5415(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8667.6(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.799
_shelx_estimated_absorpt_T_min   0.745
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.2
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88908
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.983
_diffrn_reflns_theta_min         1.717
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2379
_reflns_number_total             2560
_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    ?
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2560
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0278
_refine_ls_restrained_S_all      1.185
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0206P)²+21.5411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0651
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B), O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.27612(2) 0.39816(2) 1.05954(2) 0.02185(9) Uani 1 1 d . . . . .
N1 N 0.27412(14) 0.43440(15) 0.95395(14) 0.0293(7) Uani 1 1 d . . . . .
N5 N 0.22462(14) 0.48662(14) 1.11173(15) 0.0284(7) Uani 1 1 d . . . . .
N6 N 0.16748(15) 0.54375(14) 1.18648(14) 0.0283(7) Uani 1 1 d . . . . .
N2 N 0.32221(15) 0.46490(15) 0.86038(14) 0.0278(7) Uani 1 1 d . . . . .
C6 C 0.18497(17) 0.48544(17) 1.16281(17) 0.0281(8) Uani 1 1 d . . . . .
H6 H 0.1703 0.4467 1.1810 0.034 Uiso 1 1 calc R . . . .
C7 C 0.19898(18) 0.58638(17) 1.14628(18) 0.0282(8) Uani 1 1 d . . . . .
C9 C 0.23337(18) 0.55185(18) 1.10111(19) 0.0317(8) Uani 1 1 d . . . . .
N8 N 0.1925(2) 0.71091(17) 1.1533(2) 0.0541(10) Uani 1 1 d . . . . .
C1 C 0.32528(18) 0.42942(18) 0.91484(17) 0.0285(8) Uani 1 1 d . . . . .
H1 H 0.3608 0.4031 0.9246 0.034 Uiso 1 1 calc R . . . .
C8 C 0.1949(2) 0.65552(18) 1.1513(2) 0.0350(9) Uani 1 1 d . . . . .
C4 C 0.26365(18) 0.49539(18) 0.86505(17) 0.0295(8) Uani 1 1 d . . . . .
C2 C 0.23406(19) 0.4759(2) 0.92185(19) 0.0353(9) Uani 1 1 d . . . . .
N4 N 0.2234(2) 0.5782(2) 0.7811(2) 0.0711(14) Uani 1 1 d . . . . .
C5 C 0.2410(2) 0.5412(2) 0.81804(19) 0.0415(10) Uani 1 1 d . . . . .
C3 C 0.1715(3) 0.4912(3) 0.9476(2) 0.078(2) Uani 1 1 d . . . . .
C10 C 0.2716(2) 0.5784(2) 1.0497(2) 0.0502(12) Uani 1 1 d . . . . .
N7 N 0.3000(2) 0.6027(2) 1.0090(3) 0.0825(17) Uani 1 1 d . . . . .
N3 N 0.1223(3) 0.4998(4) 0.9697(3) 0.152(4) Uani 1 1 d . . . . .
O2 O 0.29894(14) 0.35589(13) 1.16211(12) 0.0383(7) Uani 1 1 d . . . . .
H2A H 0.2785 0.3777 1.1911 0.057 Uiso 1 1 d GR . . . .
H2B H 0.2870 0.3160 1.1639 0.057 Uiso 1 1 d GR . . . .
O1 O 0.36654(13) 0.46755(14) 1.07482(14) 0.0421(7) Uani 1 1 d . . . . .
H1A H 0.3914 0.4660 1.0414 0.063 Uiso 1 1 d GR . . . .
H1B H 0.3531 0.5066 1.0801 0.063 Uiso 1 1 d GR . . . .
Cl2 Cl 0.5000 0.5000 1.0000 0.0376(5) Uani 1 6 d S T P . .
Na Na 0.0000 0.5000 1.0000 0.0483(10) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.294(3) . ?
Cd1 N5 2.360(3) . ?
Cd1 N6 2.305(3) 20_466 ?
Cd1 N2 2.384(3) 19_557 ?
Cd1 O2 2.327(2) . ?
Cd1 O1 2.362(3) . ?
N1 C1 1.327(4) . ?
N1 C2 1.356(5) . ?
N5 C6 1.328(4) . ?
N5 C9 1.370(5) . ?
N6 Cd1 2.305(3) 23_656 ?
N6 C6 1.342(4) . ?
N6 C7 1.367(5) . ?
N2 Cd1 2.384(3) 22_576 ?
N2 C1 1.337(5) . ?
N2 C4 1.360(5) . ?
C6 H6 0.9300 . ?
C7 C9 1.365(5) . ?
C7 C8 1.426(5) . ?
C9 C10 1.425(5) . ?
N8 C8 1.140(5) . ?
C1 H1 0.9300 . ?
C4 C2 1.375(5) . ?
C4 C5 1.427(5) . ?
C2 C3 1.425(6) . ?
N4 C5 1.133(5) . ?
C3 N3 1.122(7) . ?
C10 N7 1.134(6) . ?
N3 Na 2.588(6) . ?
O2 H2A 0.8552 . ?
O2 H2B 0.8549 . ?
O1 H1A 0.8559 . ?
O1 H1B 0.8554 . ?
Na N3 2.588(6) 20_466 ?
Na N3 2.588(6) 11_466 ?
Na N3 2.588(6) 23_656 ?
Na N3 2.588(6) 8_656 ?
Na N3 2.588(6) 13_567 ?

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
N1 Cd1 N5 99.89(11) . . ?
N1 Cd1 N6 92.44(11) . 20_466 ?
N1 Cd1 N2 91.50(10) . 19_557 ?
N1 Cd1 O2 168.86(10) . . ?
N1 Cd1 O1 86.78(11) . . ?
N5 Cd1 N2 157.67(10) . 19_557 ?
N5 Cd1 O1 80.07(10) . . ?
N6 Cd1 N5 98.99(11) 20_466 . ?
N6 Cd1 N2 99.65(11) 20_466 19_557 ?
N6 Cd1 O2 94.02(10) 20_466 . ?
N6 Cd1 O1 178.64(11) 20_466 . ?
O2 Cd1 N5 88.07(10) . . ?
O2 Cd1 N2 78.47(10) . 19_557 ?
O2 Cd1 O1 86.93(10) . . ?
O1 Cd1 N2 81.48(10) . 19_557 ?
C1 N1 Cd1 122.2(2) . . ?
C1 N1 C2 103.6(3) . . ?
C2 N1 Cd1 132.4(2) . . ?
C6 N5 Cd1 128.3(2) . . ?
C6 N5 C9 102.9(3) . . ?
C9 N5 Cd1 128.5(2) . . ?
C6 N6 Cd1 124.9(2) . 23_656 ?
C6 N6 C7 103.1(3) . . ?
C7 N6 Cd1 132.0(2) . 23_656 ?
C1 N2 Cd1 117.5(2) . 22_576 ?
C1 N2 C4 103.5(3) . . ?
C4 N2 Cd1 136.7(2) . 22_576 ?
N5 C6 N6 115.7(3) . . ?
N5 C6 H6 122.1 . . ?
N6 C6 H6 122.1 . . ?
N6 C7 C8 124.5(3) . . ?
C9 C7 N6 108.8(3) . . ?
C9 C7 C8 126.7(3) . . ?
N5 C9 C10 124.4(3) . . ?
C7 C9 N5 109.4(3) . . ?
C7 C9 C10 126.2(4) . . ?
N1 C1 N2 115.3(3) . . ?
N1 C1 H1 122.3 . . ?
N2 C1 H1 122.3 . . ?
N8 C8 C7 177.7(5) . . ?
N2 C4 C2 108.5(3) . . ?
N2 C4 C5 123.0(3) . . ?
C2 C4 C5 128.4(3) . . ?
N1 C2 C4 109.1(3) . . ?
N1 C2 C3 120.3(4) . . ?
C4 C2 C3 130.5(4) . . ?
N4 C5 C4 179.1(6) . . ?
N3 C3 C2 175.9(7) . . ?
N7 C10 C9 176.2(5) . . ?
C3 N3 Na 166.4(8) . . ?
Cd1 O2 H2A 109.6 . . ?
Cd1 O2 H2B 109.8 . . ?
H2A O2 H2B 109.3 . . ?
Cd1 O1 H1A 109.9 . . ?
Cd1 O1 H1B 109.2 . . ?
H1A O1 H1B 109.2 . . ?
N3 Na N3 76.6(2) 8_656 11_466 ?
N3 Na N3 76.6(2) 11_466 . ?
N3 Na N3 76.6(2) 8_656 . ?
N3 Na N3 103.4(2) 23_656 . ?
N3 Na N3 180.0 13_567 . ?
N3 Na N3 76.6(2) 20_466 13_567 ?
N3 Na N3 103.4(2) 8_656 23_656 ?
N3 Na N3 76.6(2) 20_466 23_656 ?
N3 Na N3 103.4(2) 20_466 . ?
N3 Na N3 103.4(2) 8_656 13_567 ?
N3 Na N3 103.4(2) 20_466 11_466 ?
N3 Na N3 76.6(2) 23_656 13_567 ?
N3 Na N3 103.4(2) 13_567 11_466 ?
N3 Na N3 180.0(4) 20_466 8_656 ?
N3 Na N3 180.0 23_656 11_466 ?

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
####################################################################### 
# 
# 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_test
_database_code_depnum_ccdc_archive 'CCDC 998397'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.08(C240 H144 Cd24 N192 Na4 O48), 0.33(I)'
_chemical_formula_sum            'C20 H12 Cd2 I0.33 N16 Na0.33 O4'
_chemical_formula_weight         815.22
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-x, y+1/2, -z+1/2'
4 'x+1/2, -y+1/2, -z'
5 'z, x, y'
6 'z+1/2, -x+1/2, -y'
7 '-z+1/2, -x, y+1/2'
8 '-z, x+1/2, -y+1/2'
9 'y, z, x'
10 '-y, z+1/2, -x+1/2'
11 'y+1/2, -z+1/2, -x'
12 '-y+1/2, -z, x+1/2'
13 '-x, -y, -z'
14 'x-1/2, y, -z-1/2'
15 'x, -y-1/2, z-1/2'
16 '-x-1/2, y-1/2, z'
17 '-z, -x, -y'
18 '-z-1/2, x-1/2, y'
19 'z-1/2, x, -y-1/2'
20 'z, -x-1/2, y-1/2'
21 '-y, -z, -x'
22 'y, -z-1/2, x-1/2'
23 '-y-1/2, z-1/2, x'
24 'y-1/2, z, -x-1/2'

_cell_length_a                   20.6279(5)
_cell_length_b                   20.6279(5)
_cell_length_c                   20.6279(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8777.4(4)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.42
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  0.7065
_exptl_absorpt_correction_T_min  0.7065
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47092
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.71
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2279
_reflns_number_total             2586
_reflns_threshold_expression     >2sigma(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2586
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0206
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.246
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0241P)²+7.9694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0525
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cd1 Cd 0.226159(9) 0.395412(9) 0.941812(9) 0.02031(8) Uani 1 d . . 1 . . .
I1 I 0.0000 0.5000 1.0000 0.04008(14) Uani 1 d . . 6 S T P
N1 N 0.31548(11) 0.33166(11) 0.95767(11) 0.0260(5) Uani 1 d . . 1 . . .
N5 N 0.22718(11) 0.43132(11) 1.04783(11) 0.0256(5) Uani 1 d . . 1 . . .
C2 C 0.40447(14) 0.27054(14) 0.95096(14) 0.0291(6) Uani 1 d . . 1 . . .
C6 C 0.17444(13) 0.42960(14) 1.08553(13) 0.0266(6) Uani 1 d . . 1 . . .
H6 H 0.1380 0.4053 1.0749 0.032 Uiso 1 calc . . 1 R . .
O1 O 0.20630(11) 0.35311(10) 0.83826(9) 0.0391(5) Uani 1 d . . 1 . . .
H1A H 0.1740 0.3263 0.8394 0.059 Uiso 1 d . . 1 GR . .
H1B H 0.1968 0.3843 0.8120 0.059 Uiso 1 d . . 1 GR . .
N6 N 0.17778(11) 0.46530(11) 1.13947(11) 0.0265(5) Uani 1 d . . 1 . . .
C9 C 0.26871(13) 0.47185(13) 1.08042(13) 0.0256(6) Uani 1 d . . 1 . . .
N3 N 0.34940(15) 0.30431(17) 0.79145(13) 0.0537(8) Uani 1 d . . 1 . . .
N2 N 0.39287(11) 0.28005(11) 1.01556(11) 0.0278(5) Uani 1 d . . 1 . . .
O2 O 0.14184(10) 0.46749(10) 0.91851(12) 0.0425(6) Uani 1 d . . 1 . . .
H2A H 0.1302 0.4632 0.8786 0.064 Uiso 1 d . . 1 GR . .
H2B H 0.1090 0.4595 0.9431 0.064 Uiso 1 d . . 1 GR . .
C10 C 0.33278(15) 0.48311(15) 1.05733(15) 0.0348(7) Uani 1 d . . 1 . . .
C1 C 0.33957(13) 0.31663(13) 1.01618(13) 0.0263(6) Uani 1 d . . 1 . . .
H1 H 0.3204 0.3307 1.0545 0.032 Uiso 1 calc . . 1 R . .
C7 C 0.23808(14) 0.49283(13) 1.13624(13) 0.0258(6) Uani 1 d . . 1 . . .
C4 C 0.35720(13) 0.30177(14) 0.91543(13) 0.0260(6) Uani 1 d . . 1 . . .
C3 C 0.45667(17) 0.23367(17) 0.92556(15) 0.0407(8) Uani 1 d . . 1 . . .
C8 C 0.26059(16) 0.53810(16) 1.18309(15) 0.0381(8) Uani 1 d . . 1 . . .
C5 C 0.35150(15) 0.30382(15) 0.84659(14) 0.0340(7) Uani 1 d . . 1 . . .
Na1 Na 0.5000 0.5000 1.0000 0.0266(6) Uani 1 d . . 6 S T P
N8 N 0.38395(14) 0.48857(16) 1.03761(16) 0.0552(9) Uani 1 d . . 1 . . .
N7 N 0.27715(18) 0.57515(17) 1.22045(16) 0.0663(10) Uani 1 d . . 1 . . .
N4 N 0.49805(17) 0.20549(18) 0.90257(16) 0.0674(10) Uani 1 d . . 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
Cd1 N1 2.287(2) . ?
Cd1 N5 2.309(2) . ?
Cd1 O1 2.3434(19) . ?
Cd1 N6 2.390(2) 20_466 ?
Cd1 N2 2.372(2) 22_576 ?
Cd1 O2 2.338(2) . ?
N1 C1 1.342(3) . ?
N1 C4 1.371(3) . ?
N5 C6 1.338(3) . ?
N5 C9 1.373(3) . ?
C2 N2 1.368(4) . ?
C2 C4 1.380(4) . ?
C2 C3 1.418(4) . ?
C6 H6 0.9300 . ?
C6 N6 1.336(3) . ?
O1 H1A 0.8653 . ?
O1 H1B 0.8643 . ?
N6 Cd1 2.390(2) 23_656 ?
N6 C7 1.369(4) . ?
C9 C10 1.424(4) . ?
C9 C7 1.383(4) . ?
N3 C5 1.138(4) . ?
N2 Cd1 2.372(2) 19_557 ?
N2 C1 1.333(3) . ?
O2 H2A 0.8618 . ?
O2 H2B 0.8621 . ?
C10 N8 1.137(4) . ?
C1 H1 0.9300 . ?
C7 C8 1.422(4) . ?
C4 C5 1.426(4) . ?
C3 N4 1.137(4) . ?
C8 N7 1.138(4) . ?
Na1 N8 2.527(3) 7_665 ?
Na1 N8 2.527(3) 19_557 ?
Na1 N8 2.527(3) 10_646 ?
Na1 N8 2.527(3) 13_667 ?
Na1 N8 2.527(3) 22_576 ?
Na1 N8 2.527(3) . ?

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
N1 Cd1 N5 92.38(8) . . ?
N1 Cd1 O1 93.28(8) . . ?
N1 Cd1 N6 102.15(8) . 20_466 ?
N1 Cd1 N2 97.38(8) . 22_576 ?
N1 Cd1 O2 173.87(8) . . ?
N5 Cd1 O1 169.84(8) . . ?
N5 Cd1 N6 91.00(8) . 20_466 ?
N5 Cd1 N2 98.65(8) . 22_576 ?
N5 Cd1 O2 89.86(8) . . ?
O1 Cd1 N6 79.56(8) . 20_466 ?
O1 Cd1 N2 88.98(8) . 22_576 ?
N2 Cd1 N6 157.81(8) 22_576 20_466 ?
O2 Cd1 O1 85.37(8) . . ?
O2 Cd1 N6 83.50(8) . 20_466 ?
O2 Cd1 N2 76.63(8) . 22_576 ?
C1 N1 Cd1 124.05(17) . . ?
C1 N1 C4 103.6(2) . . ?
C4 N1 Cd1 132.32(18) . . ?
C6 N5 Cd1 122.31(18) . . ?
C6 N5 C9 103.8(2) . . ?
C9 N5 Cd1 131.67(17) . . ?
N2 C2 C4 109.1(2) . . ?
N2 C2 C3 124.7(3) . . ?
C4 C2 C3 126.2(3) . . ?
N5 C6 H6 122.3 . . ?
N6 C6 N5 115.3(2) . . ?
N6 C6 H6 122.3 . . ?
Cd1 O1 H1A 110.3 . . ?
Cd1 O1 H1B 109.5 . . ?
H1A O1 H1B 108.6 . . ?
C6 N6 Cd1 118.61(18) . 23_656 ?
C6 N6 C7 103.6(2) . . ?
C7 N6 Cd1 133.99(18) . 23_656 ?
N5 C9 C10 121.0(2) . . ?
N5 C9 C7 108.2(2) . . ?
C7 C9 C10 130.7(3) . . ?
C2 N2 Cd1 127.76(18) . 19_557 ?
C1 N2 Cd1 127.48(19) . 19_557 ?
C1 N2 C2 103.6(2) . . ?
Cd1 O2 H2A 109.8 . . ?
Cd1 O2 H2B 110.0 . . ?
H2A O2 H2B 108.8 . . ?
N8 C10 C9 176.1(4) . . ?
N1 C1 H1 122.4 . . ?
N2 C1 N1 115.3(2) . . ?
N2 C1 H1 122.3 . . ?
N6 C7 C9 109.0(2) . . ?
N6 C7 C8 122.4(3) . . ?
C9 C7 C8 128.5(3) . . ?
N1 C4 C2 108.4(2) . . ?
N1 C4 C5 124.6(3) . . ?
C2 C4 C5 127.0(3) . . ?
N4 C3 C2 176.9(4) . . ?
N7 C8 C7 178.2(4) . . ?
N3 C5 C4 177.2(4) . . ?
N8 Na1 N8 180.000(1) 19_557 7_665 ?
N8 Na1 N8 100.00(11) 13_667 7_665 ?
N8 Na1 N8 100.00(11) 19_557 . ?
N8 Na1 N8 100.00(11) 19_557 10_646 ?
N8 Na1 N8 80.00(11) 10_646 . ?
N8 Na1 N8 180.000(1) . 13_667 ?
N8 Na1 N8 100.00(11) 10_646 13_667 ?
N8 Na1 N8 80.00(11) . 7_665 ?
N8 Na1 N8 100.00(11) 22_576 . ?
N8 Na1 N8 80.00(11) 19_557 13_667 ?
N8 Na1 N8 80.00(11) 10_646 7_665 ?
N8 Na1 N8 180.000(1) 22_576 10_646 ?
N8 Na1 N8 80.00(11) 22_576 13_667 ?
N8 Na1 N8 80.00(11) 19_557 22_576 ?
N8 Na1 N8 100.00(11) 22_576 7_665 ?
C10 N8 Na1 176.9(3) . . ?

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

data_test
_database_code_depnum_ccdc_archive 'CCDC 998398'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C240 H144 Cd24 N192 O48 Rb4), 1(Cl)'
_chemical_formula_sum            'C60 H36 Cd6 Cl N48 O12 Rb'
_chemical_formula_weight         2416.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   20.6298(3)
_cell_length_b                   20.6298(3)
_cell_length_c                   20.6298(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8779.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.680
_shelx_estimated_absorpt_T_min   0.680
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47024
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.980
_diffrn_reflns_theta_min         1.710
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2301
_reflns_number_total             2586
_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    ?
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2586
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0209
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0282P)²+7.9765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0558
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.09911(2) 0.43932(2) 0.22346(2) 0.02161(8) Uani 1 1 d . . . . .
Rb1 Rb 0.0000 0.5000 0.5000 0.0559(2) Uani 1 6 d S T P . .
O1 O 0.03156(11) 0.42511(11) 0.13288(10) 0.0420(5) Uani 1 1 d . . . . .
H1A H 0.0124 0.3875 0.1344 0.063 Uiso 1 1 d GR . . . .
H1B H 0.0018 0.4552 0.1320 0.063 Uiso 1 1 d GR . . . .
O2 O 0.14252(10) 0.33721(9) 0.20119(11) 0.0385(5) Uani 1 1 d . . . . .
H2A H 0.1843 0.3357 0.2114 0.058 Uiso 1 1 d GR . . . .
H2B H 0.1227 0.3063 0.2237 0.058 Uiso 1 1 d GR . . . .
N1 N 0.06306(11) 0.54489(11) 0.22282(11) 0.0289(5) Uani 1 1 d . . . . .
N2 N 0.03751(11) 0.64022(11) 0.17597(11) 0.0284(5) Uani 1 1 d . . . . .
N3 N -0.07888(18) 0.71885(16) 0.27091(19) 0.0706(11) Uani 1 1 d . . . . .
N4 N -0.0234(3) 0.5214(2) 0.36310(18) 0.1054(17) Uani 1 1 d . . . . .
N5 N 0.01159(11) 0.38576(11) 0.27559(11) 0.0283(5) Uani 1 1 d . . . . .
N6 N -0.04454(11) 0.31303(11) 0.33545(11) 0.0281(5) Uani 1 1 d . . . . .
N7 N -0.21164(13) 0.34606(16) 0.30939(16) 0.0560(8) Uani 1 1 d . . . . .
N8 N -0.10660(18) 0.4833(2) 0.19747(19) 0.0823(13) Uani 1 1 d . . . . .
C1 C 0.07187(14) 0.58552(13) 0.17347(14) 0.0302(6) Uani 1 1 d . . . . .
H1 H 0.1001 0.5764 0.1395 0.036 Uiso 1 1 calc R . . . .
C2 C 0.00328(14) 0.63435(13) 0.23207(13) 0.0291(6) Uani 1 1 d . . . . .
C3 C -0.04221(17) 0.68165(15) 0.25380(16) 0.0415(8) Uani 1 1 d . . . . .
C4 C 0.01875(15) 0.57608(14) 0.26065(14) 0.0325(7) Uani 1 1 d . . . . .
C5 C -0.0055(2) 0.54746(17) 0.31866(17) 0.0578(11) Uani 1 1 d . . . . .
C6 C 0.01317(13) 0.33618(13) 0.31707(13) 0.0281(6) Uani 1 1 d . . . . .
H6 H 0.0519 0.3188 0.3322 0.034 Uiso 1 1 calc R . . . .
C7 C -0.05347(13) 0.39529(14) 0.26622(14) 0.0301(6) Uani 1 1 d . . . . .
C8 C -0.08096(16) 0.44457(18) 0.22663(17) 0.0471(9) Uani 1 1 d . . . . .
C9 C -0.08737(12) 0.35133(14) 0.30258(14) 0.0280(6) Uani 1 1 d . . . . .
C10 C -0.15655(14) 0.34665(15) 0.30686(15) 0.0360(7) Uani 1 1 d . . . . .
Cl1 Cl 0.0000 0.5000 0.0000 0.0411(4) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.349(2) . ?
Cd1 O2 2.3346(19) . ?
Cd1 N1 2.301(2) . ?
Cd1 N2 2.386(2) 20_565 ?
Cd1 N5 2.374(2) . ?
Cd1 N6 2.313(2) 18_665 ?
Rb1 N4 2.899(4) 6_456 ?
Rb1 N4 2.899(4) 12_565 ?
Rb1 N4 2.899(4) . ?
Rb1 N4 2.899(4) 13_566 ?
Rb1 N4 2.899(4) 24_556 ?
Rb1 N4 2.899(4) 18_665 ?
O1 H1A 0.8718 . ?
O1 H1B 0.8722 . ?
O2 H2A 0.8872 . ?
O2 H2B 0.8887 . ?
N1 C1 1.331(4) . ?
N1 C4 1.363(4) . ?
N2 Cd1 2.386(2) 23_665 ?
N2 C1 1.334(4) . ?
N2 C2 1.361(4) . ?
N3 C3 1.134(4) . ?
N4 C5 1.126(5) . ?
N5 C6 1.334(3) . ?
N5 C7 1.370(4) . ?
N6 Cd1 2.312(2) 24_556 ?
N6 C6 1.338(3) . ?
N6 C9 1.366(3) . ?
N7 C10 1.138(4) . ?
N8 C8 1.131(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.426(4) . ?
C2 C4 1.376(4) . ?
C4 C5 1.425(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.422(4) . ?
C7 C9 1.369(4) . ?
C9 C10 1.433(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 N2 81.18(8) . 20_565 ?
O1 Cd1 N5 81.44(8) . . ?
O2 Cd1 O1 87.61(8) . . ?
O2 Cd1 N2 77.54(7) . 20_565 ?
O2 Cd1 N5 87.76(7) . . ?
N1 Cd1 O1 85.52(8) . . ?
N1 Cd1 O2 167.60(8) . . ?
N1 Cd1 N2 91.20(8) . 20_565 ?
N1 Cd1 N5 101.38(8) . . ?
N1 Cd1 N6 93.27(8) . 18_665 ?
N5 Cd1 N2 157.62(8) . 20_565 ?
N6 Cd1 O1 178.76(8) 18_665 . ?
N6 Cd1 O2 93.62(8) 18_665 . ?
N6 Cd1 N2 99.11(8) 18_665 20_565 ?
N6 Cd1 N5 98.57(8) 18_665 . ?
N4 Rb1 N4 70.36(13) . 12_565 ?
N4 Rb1 N4 70.36(13) 6_456 12_565 ?
N4 Rb1 N4 70.36(13) 18_665 24_556 ?
N4 Rb1 N4 180.0 . 13_566 ?
N4 Rb1 N4 109.64(13) 13_566 12_565 ?
N4 Rb1 N4 109.64(14) 6_456 24_556 ?
N4 Rb1 N4 109.64(14) . 18_665 ?
N4 Rb1 N4 70.36(14) . 6_456 ?
N4 Rb1 N4 109.64(13) . 24_556 ?
N4 Rb1 N4 109.64(14) 18_665 12_565 ?
N4 Rb1 N4 180.0 18_665 6_456 ?
N4 Rb1 N4 70.36(13) 18_665 13_566 ?
N4 Rb1 N4 70.36(13) 13_566 24_556 ?
N4 Rb1 N4 180.0 24_556 12_565 ?
N4 Rb1 N4 109.64(14) 13_566 6_456 ?
Cd1 O1 H1A 110.6 . . ?
Cd1 O1 H1B 110.2 . . ?
H1A O1 H1B 108.3 . . ?
Cd1 O2 H2A 110.9 . . ?
Cd1 O2 H2B 111.7 . . ?
H2A O2 H2B 107.4 . . ?
C1 N1 Cd1 123.79(19) . . ?
C1 N1 C4 103.4(2) . . ?
C4 N1 Cd1 131.31(19) . . ?
C1 N2 Cd1 118.49(18) . 23_665 ?
C1 N2 C2 103.5(2) . . ?
C2 N2 Cd1 137.14(18) . 23_665 ?
C5 N4 Rb1 144.2(5) . . ?
C6 N5 Cd1 128.96(18) . . ?
C6 N5 C7 103.0(2) . . ?
C7 N5 Cd1 127.90(18) . . ?
C6 N6 Cd1 125.36(18) . 24_556 ?
C6 N6 C9 103.2(2) . . ?
C9 N6 Cd1 131.23(18) . 24_556 ?
N1 C1 N2 115.5(3) . . ?
N1 C1 H1 122.2 . . ?
N2 C1 H1 122.2 . . ?
N2 C2 C3 123.2(3) . . ?
N2 C2 C4 108.8(2) . . ?
C4 C2 C3 128.0(3) . . ?
N3 C3 C2 179.3(4) . . ?
N1 C4 C2 108.8(2) . . ?
N1 C4 C5 121.3(3) . . ?
C2 C4 C5 129.8(3) . . ?
N4 C5 C4 175.9(4) . . ?
N5 C6 N6 115.7(2) . . ?
N5 C6 H6 122.1 . . ?
N6 C6 H6 122.1 . . ?
N5 C7 C8 125.0(3) . . ?
C9 C7 N5 109.2(2) . . ?
C9 C7 C8 125.8(3) . . ?
N8 C8 C7 175.3(4) . . ?
N6 C9 C7 109.0(2) . . ?
N6 C9 C10 125.1(3) . . ?
C7 C9 C10 125.9(3) . . ?
N7 C10 C9 176.6(3) . . ?

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
####################################################################### 
# 
# 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_test
_database_code_depnum_ccdc_archive 'CCDC 998399'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.02(C240 H144 Cd24 N192 O48 Rb4), 0.07(Br)'
_chemical_formula_sum            'C3.93 H0.02 Br0.07 Cd0.39 N3.15 O0.79 Rb0.07'
_chemical_formula_weight         159.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   20.6704(5)
_cell_length_b                   20.6704(5)
_cell_length_c                   20.6704(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8831.7(6)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    8356
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.788
_shelx_estimated_absorpt_T_min   0.635
_exptl_absorpt_coefficient_mu    2.500
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             4609
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47609
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.971
_diffrn_reflns_theta_min         1.706
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2228
_reflns_number_total             2603
_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    ?
_refine_diff_density_max         0.336
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2603
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0262
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.274
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²+17.0009P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0672
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.90010(2) 0.06022(2) 0.22444(2) 0.02254(10) Uani 1 1 d . . . . .
Rb3 Rb 1.0000 0.0000 0.5000 0.0611(3) Uani 1 6 d S T P . .
O1 O 0.85671(14) 0.16254(13) 0.20274(15) 0.0397(7) Uani 1 1 d . . . . .
H1A H 0.8169 0.1657 0.2173 0.060 Uiso 1 1 d GR . . . .
H1B H 0.8799 0.1927 0.2215 0.060 Uiso 1 1 d GR . . . .
O2 O 0.96958(15) 0.07779(15) 0.13708(14) 0.0452(8) Uani 1 1 d . . . . .
H2A H 0.9616 0.0504 0.1067 0.068 Uiso 1 1 d GR . . . .
H2B H 0.9641 0.1163 0.1223 0.068 Uiso 1 1 d GR . . . .
N1 N 0.93576(15) -0.04597(15) 0.22283(15) 0.0298(7) Uani 1 1 d . . . . .
N2 N 0.96262(15) -0.14020(15) 0.17537(15) 0.0292(7) Uani 1 1 d . . . . .
N3 N 1.0773(2) -0.2194(2) 0.2710(2) 0.0710(14) Uani 1 1 d . . . . .
N4 N 1.0160(4) -0.0251(3) 0.3658(3) 0.139(3) Uani 1 1 d . . . . .
N5 N 0.83553(15) 0.04418(14) 0.31378(15) 0.0285(7) Uani 1 1 d . . . . .
N6 N 0.77711(15) -0.01227(15) 0.38717(15) 0.0288(7) Uani 1 1 d . . . . .
N7 N 0.8086(2) 0.21054(18) 0.3467(2) 0.0570(11) Uani 1 1 d . . . . .
N8 N 0.7000(3) 0.1042(2) 0.4860(3) 0.0835(17) Uani 1 1 d . . . . .
C1 C 0.92828(19) -0.08528(18) 0.17285(19) 0.0311(9) Uani 1 1 d . . . . .
H1 H 0.9011 -0.0755 0.1384 0.037 Uiso 1 1 calc R . . . .
C2 C 0.9788(2) -0.07761(19) 0.26113(19) 0.0344(9) Uani 1 1 d . . . . .
C3 C 1.0005(3) -0.0496(2) 0.3201(3) 0.0699(18) Uani 1 1 d . . . . .
C4 C 0.99543(18) -0.13479(18) 0.23232(19) 0.0293(9) Uani 1 1 d . . . . .
C5 C 1.0403(2) -0.1823(2) 0.2537(2) 0.0436(11) Uani 1 1 d . . . . .
C6 C 0.81799(19) -0.01348(18) 0.33719(18) 0.0286(9) Uani 1 1 d . . . . .
H6 H 0.8333 -0.0520 0.3198 0.034 Uiso 1 1 calc R . . . .
C7 C 0.80340(19) 0.08673(17) 0.35255(19) 0.0287(8) Uani 1 1 d . . . . .
C8 C 0.8071(2) 0.1558(2) 0.3477(2) 0.0382(10) Uani 1 1 d . . . . .
C9 C 0.76794(19) 0.05234(19) 0.39729(19) 0.0318(9) Uani 1 1 d . . . . .
C10 C 0.7293(2) 0.0798(2) 0.4470(2) 0.0477(12) Uani 1 1 d . . . . .
Br1 Br 1.0000 0.0000 0.0000 0.0406(3) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.341(3) . ?
Cd1 O2 2.336(3) . ?
Cd1 N1 2.316(3) . ?
Cd1 N2 2.385(3) 17_665 ?
Cd1 N5 2.302(3) . ?
Cd1 N6 2.377(3) 22_665 ?
Rb3 N4 2.841(6) 10_646 ?
Rb3 N4 2.841(6) 19_646 ?
Rb3 N4 2.841(6) . ?
Rb3 N4 2.841(6) 22_665 ?
Rb3 N4 2.841(6) 7_665 ?
Rb3 N4 2.841(6) 13_756 ?
O1 H1A 0.8780 . ?
O1 H1B 0.8775 . ?
O2 H2A 0.8610 . ?
O2 H2B 0.8608 . ?
N1 C1 1.323(5) . ?
N1 C2 1.359(5) . ?
N2 Cd1 2.385(3) 21_656 ?
N2 C1 1.340(5) . ?
N2 C4 1.363(5) . ?
N3 C5 1.141(6) . ?
N4 C3 1.119(7) . ?
N5 C6 1.336(5) . ?
N5 C7 1.363(5) . ?
N6 Cd1 2.377(3) 19_646 ?
N6 C6 1.335(5) . ?
N6 C9 1.365(5) . ?
N7 C8 1.133(5) . ?
N8 C10 1.128(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.423(6) . ?
C2 C4 1.367(5) . ?
C4 C5 1.421(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.432(5) . ?
C7 C9 1.378(5) . ?
C9 C10 1.419(6) . ?

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 Cd1 N2 77.78(10) . 17_665 ?
O1 Cd1 N6 88.08(10) . 22_665 ?
O2 Cd1 O1 86.96(11) . . ?
O2 Cd1 N2 82.44(11) . 17_665 ?
O2 Cd1 N6 79.31(11) . 22_665 ?
N1 Cd1 O1 167.34(11) . . ?
N1 Cd1 O2 86.59(11) . . ?
N1 Cd1 N2 90.57(11) . 17_665 ?
N1 Cd1 N6 101.40(11) . 22_665 ?
N5 Cd1 O1 93.54(11) . . ?
N5 Cd1 O2 177.31(11) . . ?
N5 Cd1 N1 93.41(11) . . ?
N5 Cd1 N2 100.25(11) . 17_665 ?
N5 Cd1 N6 98.06(11) . 22_665 ?
N6 Cd1 N2 157.45(11) 22_665 17_665 ?
N4 Rb3 N4 108.2(2) . 19_646 ?
N4 Rb3 N4 108.2(2) 10_646 19_646 ?
N4 Rb3 N4 108.2(2) 13_756 7_665 ?
N4 Rb3 N4 108.2(2) . 22_665 ?
N4 Rb3 N4 71.8(2) 22_665 19_646 ?
N4 Rb3 N4 71.8(2) 10_646 7_665 ?
N4 Rb3 N4 180.0 . 13_756 ?
N4 Rb3 N4 71.8(2) . 10_646 ?
N4 Rb3 N4 71.8(2) . 7_665 ?
N4 Rb3 N4 71.8(2) 13_756 19_646 ?
N4 Rb3 N4 108.2(2) 13_756 10_646 ?
N4 Rb3 N4 71.8(2) 13_756 22_665 ?
N4 Rb3 N4 108.2(2) 22_665 7_665 ?
N4 Rb3 N4 180.0(2) 7_665 19_646 ?
N4 Rb3 N4 180.0 22_665 10_646 ?
Cd1 O1 H1A 111.1 . . ?
Cd1 O1 H1B 110.4 . . ?
H1A O1 H1B 108.0 . . ?
Cd1 O2 H2A 110.1 . . ?
Cd1 O2 H2B 109.7 . . ?
H2A O2 H2B 108.9 . . ?
C1 N1 Cd1 123.8(3) . . ?
C1 N1 C2 103.6(3) . . ?
C2 N1 Cd1 131.0(3) . . ?
C1 N2 Cd1 119.2(2) . 21_656 ?
C1 N2 C4 103.2(3) . . ?
C4 N2 Cd1 136.3(2) . 21_656 ?
C3 N4 Rb3 150.8(8) . . ?
C6 N5 Cd1 125.2(2) . . ?
C6 N5 C7 103.3(3) . . ?
C7 N5 Cd1 131.4(2) . . ?
C6 N6 Cd1 129.0(2) . 19_646 ?
C6 N6 C9 103.0(3) . . ?
C9 N6 Cd1 127.7(2) . 19_646 ?
N1 C1 N2 115.3(3) . . ?
N1 C1 H1 122.3 . . ?
N2 C1 H1 122.3 . . ?
N1 C2 C3 120.6(4) . . ?
N1 C2 C4 109.1(3) . . ?
C4 C2 C3 130.3(4) . . ?
N4 C3 C2 176.8(6) . . ?
N2 C4 C2 108.8(3) . . ?
N2 C4 C5 122.4(4) . . ?
C2 C4 C5 128.8(4) . . ?
N3 C5 C4 178.4(5) . . ?
N5 C6 H6 122.1 . . ?
N6 C6 N5 115.8(3) . . ?
N6 C6 H6 122.1 . . ?
N5 C7 C8 125.1(4) . . ?
N5 C7 C9 108.7(3) . . ?
C9 C7 C8 126.2(4) . . ?
N7 C8 C7 176.6(5) . . ?
N6 C9 C7 109.2(3) . . ?
N6 C9 C10 125.5(4) . . ?
C7 C9 C10 125.3(4) . . ?
N8 C10 C9 176.9(5) . . ?

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
####################################################################### 
# 
# 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_test
_database_code_depnum_ccdc_archive 'CCDC 998400'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.07(I), 0.02(C240 H144 Cd24 N192 O48 Rb4)'
_chemical_formula_sum            'C H Cd I N O Rb'
_chemical_formula_weight         367.80
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   20.7438(4)
_cell_length_b                   20.7438(4)
_cell_length_c                   20.7438(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8926.2(5)
_cell_formula_units_Z            60
_cell_measurement_reflns_used    9478
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.134
_shelx_estimated_absorpt_T_min   0.134
_exptl_absorpt_coefficient_mu    16.854
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    4.105
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             9600
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47688
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         1.700
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2257
_reflns_number_total             2624
_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    ?
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2624
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0204
_refine_ls_restrained_S_all      1.047
_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)+(0.0201P)²+8.8555P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0481
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
I1 I 1.0000 0.0000 0.0000 0.03983(13) Uani 1 6 d S T P . .
Cd1 Cd 0.90037(2) 0.06002(2) 0.22561(2) 0.02261(7) Uani 1 1 d . . . . .
Rb1 Rb 0.5000 0.0000 0.0000 0.0491(2) Uani 1 6 d S T P . .
O1 O 0.85662(10) 0.16252(9) 0.20504(11) 0.0403(5) Uani 1 1 d . . . . .
H1A H 0.8162 0.1638 0.2163 0.060 Uiso 1 1 d GR . . . .
H1B H 0.8774 0.1918 0.2268 0.060 Uiso 1 1 d GR . . . .
O2 O 0.97077(11) 0.08255(12) 0.14185(10) 0.0461(6) Uani 1 1 d . . . . .
H2A H 0.9604 0.0608 0.1075 0.069 Uiso 1 1 d GR . . . .
H2B H 0.9694 0.1234 0.1325 0.069 Uiso 1 1 d GR . . . .
N1 N 0.82685(11) 0.03847(11) 0.14026(11) 0.0285(5) Uani 1 1 d . . . . .
N2 N 0.77901(11) 0.06468(12) 0.04628(11) 0.0296(5) Uani 1 1 d . . . . .
N3 N 0.63452(18) -0.0143(3) 0.0286(2) 0.121(2) Uani 1 1 d . . . . .
N4 N 0.73216(18) -0.07508(18) 0.22060(16) 0.0704(11) Uani 1 1 d . . . . .
N5 N 0.83683(11) 0.04409(11) 0.31460(11) 0.0285(5) Uani 1 1 d . . . . .
N6 N 0.78042(11) -0.01251(11) 0.38863(11) 0.0299(6) Uani 1 1 d . . . . .
N7 N 0.70345(19) 0.10314(17) 0.48800(19) 0.0819(12) Uani 1 1 d . . . . .
N8 N 0.80909(17) 0.20990(14) 0.34795(15) 0.0578(9) Uani 1 1 d . . . . .
C1 C 0.82898(14) 0.07235(14) 0.08544(13) 0.0292(7) Uani 1 1 d . . . . .
H1 H 0.8632 0.0995 0.0754 0.035 Uiso 1 1 calc R . . . .
C2 C 0.74086(14) 0.02188(15) 0.07839(14) 0.0332(7) Uani 1 1 d . . . . .
C3 C 0.77009(14) 0.00586(14) 0.13555(13) 0.0295(6) Uani 1 1 d . . . . .
C4 C 0.74870(17) -0.03863(17) 0.18309(16) 0.0437(8) Uani 1 1 d . . . . .
C5 C 0.68130(18) 0.0010(2) 0.05226(18) 0.0618(12) Uani 1 1 d . . . . .
C6 C 0.82006(13) -0.01358(13) 0.33832(13) 0.0269(6) Uani 1 1 d . . . . .
H6 H 0.8352 -0.0519 0.3207 0.032 Uiso 1 1 calc R . . . .
C7 C 0.80473(14) 0.08652(13) 0.35373(14) 0.0291(6) Uani 1 1 d . . . . .
C8 C 0.80802(16) 0.15506(15) 0.34883(15) 0.0379(7) Uani 1 1 d . . . . .
C9 C 0.77089(15) 0.05205(14) 0.39858(15) 0.0338(7) Uani 1 1 d . . . . .
C10 C 0.73250(17) 0.07895(16) 0.44881(18) 0.0487(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.351(2) . ?
Cd1 O2 2.317(2) . ?
Cd1 N1 2.379(2) . ?
Cd1 N2 2.323(2) 21_656 ?
Cd1 N5 2.292(2) . ?
Cd1 N6 2.386(2) 22_665 ?
Rb1 N3 2.868(4) 12_554 ?
Rb1 N3 2.868(4) 6 ?
Rb1 N3 2.868(4) . ?
Rb1 N3 2.868(4) 13_655 ?
Rb1 N3 2.868(4) 18_655 ?
Rb1 N3 2.868(4) 24_656 ?
N1 C1 1.337(3) . ?
N1 C3 1.362(4) . ?
N2 Cd1 2.323(2) 17_665 ?
N2 C1 1.327(3) . ?
N2 C2 1.363(4) . ?
N3 C5 1.133(5) . ?
N4 C4 1.138(4) . ?
N5 C6 1.340(3) . ?
N5 C7 1.370(3) . ?
N6 Cd1 2.386(2) 19_646 ?
N6 C6 1.329(3) . ?
N6 C9 1.369(4) . ?
N7 C10 1.130(4) . ?
N8 C8 1.138(4) . ?
C2 C3 1.373(4) . ?
C2 C5 1.417(5) . ?
C3 C4 1.422(4) . ?
C7 C8 1.427(4) . ?
C7 C9 1.367(4) . ?
C9 C10 1.425(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 N1 77.73(8) . . ?
O1 Cd1 N6 88.57(8) . 22_665 ?
O2 Cd1 O1 85.69(8) . . ?
O2 Cd1 N1 83.33(8) . . ?
O2 Cd1 N2 87.93(8) . 21_656 ?
O2 Cd1 N6 77.87(8) . 22_665 ?
N1 Cd1 N6 157.51(8) . 22_665 ?
N2 Cd1 O1 166.28(8) 21_656 . ?
N2 Cd1 N1 89.49(8) 21_656 . ?
N2 Cd1 N6 101.95(8) 21_656 22_665 ?
N5 Cd1 O1 93.13(8) . . ?
N5 Cd1 O2 174.43(8) . . ?
N5 Cd1 N1 101.75(8) . . ?
N5 Cd1 N2 94.35(8) . 21_656 ?
N5 Cd1 N6 96.67(8) . 22_665 ?
N3 Rb1 N3 108.84(14) . 18_655 ?
N3 Rb1 N3 108.84(14) . 24_656 ?
N3 Rb1 N3 180.0(3) 24_656 12_554 ?
N3 Rb1 N3 71.16(14) 13_655 24_656 ?
N3 Rb1 N3 71.16(14) . 12_554 ?
N3 Rb1 N3 71.16(14) . 6 ?
N3 Rb1 N3 108.84(14) 13_655 6 ?
N3 Rb1 N3 71.16(14) 12_554 6 ?
N3 Rb1 N3 180.0(3) 6 18_655 ?
N3 Rb1 N3 180.0 . 13_655 ?
N3 Rb1 N3 108.84(14) 12_554 18_655 ?
N3 Rb1 N3 108.84(14) 24_656 6 ?
N3 Rb1 N3 71.16(14) 24_656 18_655 ?
N3 Rb1 N3 108.84(14) 13_655 12_554 ?
N3 Rb1 N3 71.16(14) 13_655 18_655 ?
C1 N1 Cd1 120.85(18) . . ?
C1 N1 C3 103.2(2) . . ?
C3 N1 Cd1 134.52(18) . . ?
C1 N2 Cd1 125.17(19) . 17_665 ?
C1 N2 C2 103.5(2) . . ?
C2 N2 Cd1 130.02(19) . 17_665 ?
C5 N3 Rb1 153.4(5) . . ?
C6 N5 Cd1 125.03(18) . . ?
C6 N5 C7 103.3(2) . . ?
C7 N5 Cd1 131.61(18) . . ?
C6 N6 Cd1 129.25(18) . 19_646 ?
C6 N6 C9 103.0(2) . . ?
C9 N6 Cd1 127.21(18) . 19_646 ?
N2 C1 N1 115.6(3) . . ?
N2 C2 C3 108.9(2) . . ?
N2 C2 C5 121.2(3) . . ?
C3 C2 C5 129.9(3) . . ?
N1 C3 C2 108.9(2) . . ?
N1 C3 C4 122.9(3) . . ?
C2 C3 C4 128.2(3) . . ?
N4 C4 C3 178.8(5) . . ?
N3 C5 C2 176.6(4) . . ?
N6 C6 N5 115.7(2) . . ?
N5 C7 C8 125.1(3) . . ?
C9 C7 N5 108.5(2) . . ?
C9 C7 C8 126.4(3) . . ?
N8 C8 C7 176.5(4) . . ?
N6 C9 C10 125.0(3) . . ?
C7 C9 N6 109.6(2) . . ?
C7 C9 C10 125.4(3) . . ?
N7 C10 C9 176.6(4) . . ?

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
####################################################################### 
# 
# 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_test
_database_code_depnum_ccdc_archive 'CCDC 998414'
_audit_update_record             
;
2014-04-19 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.25(C240 H144 Cd24 K4 N192 O48), 1(I)'
_chemical_formula_sum            'C60 H36 Cd6 I K N48 O12'
_chemical_formula_weight         2461.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'z, x, y'
3 'y, z, x'
4 '-y+1/2, -z, x+1/2'
5 'z+1/2, -x+1/2, -y'
6 '-y, z+1/2, -x+1/2'
7 '-z+1/2, -x, y+1/2'
8 '-z, x+1/2, -y+1/2'
9 'y+1/2, -z+1/2, -x'
10 '-x+1/2, -y, z+1/2'
11 'x+1/2, -y+1/2, -z'
12 '-x, y+1/2, -z+1/2'
13 '-x, -y, -z'
14 '-z, -x, -y'
15 '-y, -z, -x'
16 'y-1/2, z, -x-1/2'
17 '-z-1/2, x-1/2, y'
18 'y, -z-1/2, x-1/2'
19 'z-1/2, x, -y-1/2'
20 'z, -x-1/2, y-1/2'
21 '-y-1/2, z-1/2, x'
22 'x-1/2, y, -z-1/2'
23 '-x-1/2, y-1/2, z'
24 'x, -y-1/2, z-1/2'

_cell_length_a                   20.7166(4)
_cell_length_b                   20.7166(4)
_cell_length_c                   20.7166(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8891.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8690
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.20
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_T_max  0.7043
_exptl_absorpt_correction_T_min  0.7043
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47957
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.70
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2256
_reflns_number_total             2622
_reflns_threshold_expression     >2sigma(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2622
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0203
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0170P)²+10.0122P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0479
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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,H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.85 with sigma of 0.01
 O2-H2A = O2-H2B
 0.85 with sigma of 0.01
 H1B-H1A
 1.387 with sigma of 0.02
 H2B-H2A
 1.387 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cd1 Cd 0.898966(9) 0.059379(9) 0.225912(9) 0.02223(7) Uani 1 d . . 1 . . .
I1 I 1.0000 0.0000 0.0000 0.04161(14) Uani 1 d . . 6 S T P
N1 N 0.83508(11) 0.04349(11) 0.31489(11) 0.0275(5) Uani 1 d . . 1 . . .
N5 N 0.82604(11) 0.03724(11) 0.13976(11) 0.0275(5) Uani 1 d . . 1 . . .
O1 O 0.85589(11) 0.16210(10) 0.20547(13) 0.0414(6) Uani 1 d . . 1 D . .
N6 N 0.77718(11) 0.06644(11) 0.04689(11) 0.0273(5) Uani 1 d . . 1 . . .
C2 C 0.77140(14) 0.05093(14) 0.40121(15) 0.0310(7) Uani 1 d . . 1 . . .
C6 C 0.82856(14) 0.07160(14) 0.08525(13) 0.0293(7) Uani 1 d . . 1 . . .
H6 H 0.8638 0.0974 0.0748 0.035 Uiso 1 calc . . 1 R . .
C4 C 0.80417(14) 0.08584(13) 0.35522(14) 0.0281(6) Uani 1 d . . 1 . . .
N2 N 0.78078(11) -0.01343(11) 0.39059(11) 0.0293(6) Uani 1 d . . 1 . . .
C9 C 0.73797(14) 0.02493(15) 0.07966(14) 0.0309(7) Uani 1 d . . 1 . . .
C1 C 0.81907(14) -0.01420(14) 0.33897(14) 0.0282(7) Uani 1 d . . 1 . . .
H1 H 0.8338 -0.0525 0.3208 0.034 Uiso 1 calc . . 1 R . .
C7 C 0.76762(14) 0.00703(14) 0.13622(13) 0.0287(7) Uani 1 d . . 1 . . .
O2 O 0.96987(12) 0.08254(12) 0.14202(11) 0.0449(6) Uani 1 d . . 1 D . .
N3 N 0.80767(17) 0.20943(14) 0.34831(15) 0.0565(8) Uani 1 d . . 1 . . .
C10 C 0.67575(17) 0.0092(2) 0.05533(17) 0.0532(10) Uani 1 d . . 1 . . .
N4 N 0.70534(18) 0.10094(17) 0.49276(18) 0.0749(11) Uani 1 d . . 1 . . .
C5 C 0.80704(16) 0.15464(15) 0.34982(15) 0.0371(8) Uani 1 d . . 1 . . .
C3 C 0.73374(17) 0.07745(16) 0.45228(17) 0.0442(9) Uani 1 d . . 1 . . .
N7 N 0.62654(18) -0.0007(2) 0.0340(2) 0.1037(17) Uani 1 d . . 1 . . .
K1 K 0.5000 0.0000 0.0000 0.0363(4) Uani 1 d . . 6 S T P
N8 N 0.72942(18) -0.07443(18) 0.22087(16) 0.0691(10) Uani 1 d . . 1 . . .
C8 C 0.74583(17) -0.03769(17) 0.18339(16) 0.0421(8) Uani 1 d . . 1 . . .
H1A H 0.8729(14) 0.1988(9) 0.2113(18) 0.063 Uiso 1 d . . 1 DR . .
H1B H 0.8155(5) 0.1660(16) 0.2020(19) 0.063 Uiso 1 d . . 1 DR . .
H2A H 0.9817(18) 0.0581(12) 0.1116(12) 0.063 Uiso 1 d . . 1 DR . .
H2B H 0.9788(18) 0.1212(6) 0.1335(16) 0.063 Uiso 1 d . . 1 DR . .


_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 N1 2.293(2) . ?
Cd1 N5 2.383(2) . ?
Cd1 O1 2.346(2) . ?
Cd1 N6 2.316(2) 15_656 ?
Cd1 N2 2.379(2) 18_665 ?
Cd1 O2 2.326(2) . ?
N1 C4 1.370(3) . ?
N1 C1 1.337(3) . ?
N5 C6 1.336(4) . ?
N5 C7 1.364(4) . ?
N6 Cd1 2.316(2) 14_665 ?
N6 C6 1.333(3) . ?
N6 C9 1.364(4) . ?
C2 C4 1.375(4) . ?
C2 N2 1.365(4) . ?
C2 C3 1.425(4) . ?
C4 C5 1.431(4) . ?
N2 Cd1 2.379(2) 19_646 ?
N2 C1 1.332(4) . ?
C9 C7 1.374(4) . ?
C9 C10 1.422(4) . ?
C7 C8 1.420(4) . ?
N3 C5 1.135(4) . ?
C10 N7 1.130(5) . ?
N4 C3 1.134(4) . ?
N7 K1 2.714(4) . ?
K1 N7 2.714(4) 13_655 ?
K1 N7 2.714(4) 17_655 ?
K1 N7 2.714(4) 5 ?
K1 N7 2.714(4) 16_656 ?
K1 N7 2.714(4) 4_554 ?
N8 C8 1.139(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N5 102.03(8) . . ?
N1 Cd1 O1 93.20(9) . . ?
N1 Cd1 N6 93.69(8) . 15_656 ?
N1 Cd1 N2 96.82(8) . 18_665 ?
N1 Cd1 O2 174.24(8) . . ?
O1 Cd1 N5 78.36(8) . . ?
O1 Cd1 N2 88.93(8) . 18_665 ?
N6 Cd1 N5 89.57(8) 15_656 . ?
N6 Cd1 O1 167.13(8) 15_656 . ?
N6 Cd1 N2 101.03(8) 15_656 18_665 ?
N6 Cd1 O2 88.85(9) 15_656 . ?
N2 Cd1 N5 157.72(8) 18_665 . ?
O2 Cd1 N5 83.13(9) . . ?
O2 Cd1 O1 85.31(9) . . ?
O2 Cd1 N2 77.61(8) . 18_665 ?
C4 N1 Cd1 131.91(18) . . ?
C1 N1 Cd1 124.86(18) . . ?
C1 N1 C4 103.2(2) . . ?
C6 N5 Cd1 120.38(18) . . ?
C6 N5 C7 103.5(2) . . ?
C7 N5 Cd1 133.70(18) . . ?
C6 N6 Cd1 124.35(19) . 14_665 ?
C6 N6 C9 103.3(2) . . ?
C9 N6 Cd1 130.67(18) . 14_665 ?
C4 C2 C3 125.6(3) . . ?
N2 C2 C4 109.4(2) . . ?
N2 C2 C3 125.0(3) . . ?
N6 C6 N5 115.5(3) . . ?
N1 C4 C2 108.4(2) . . ?
N1 C4 C5 124.8(3) . . ?
C2 C4 C5 126.8(3) . . ?
C2 N2 Cd1 127.37(18) . 19_646 ?
C1 N2 Cd1 128.71(19) . 19_646 ?
C1 N2 C2 103.0(2) . . ?
N6 C9 C7 109.2(2) . . ?
N6 C9 C10 120.5(3) . . ?
C7 C9 C10 130.2(3) . . ?
N2 C1 N1 115.9(3) . . ?
N5 C7 C9 108.6(2) . . ?
N5 C7 C8 123.0(3) . . ?
C9 C7 C8 128.4(3) . . ?
N7 C10 C9 176.5(4) . . ?
N3 C5 C4 176.6(4) . . ?
N4 C3 C2 177.0(4) . . ?
C10 N7 K1 166.4(5) . . ?
N7 K1 N7 180.0(3) 4_554 16_656 ?
N7 K1 N7 75.10(14) 5 4_554 ?
N7 K1 N7 104.90(14) . 16_656 ?
N7 K1 N7 104.90(14) 4_554 17_655 ?
N7 K1 N7 75.10(14) 13_655 16_656 ?
N7 K1 N7 75.10(14) . 5 ?
N7 K1 N7 75.10(14) 13_655 17_655 ?
N7 K1 N7 104.90(14) . 17_655 ?
N7 K1 N7 180.00(17) 5 17_655 ?
N7 K1 N7 104.90(14) 13_655 4_554 ?
N7 K1 N7 75.10(14) 16_656 17_655 ?
N7 K1 N7 104.90(14) 5 16_656 ?
N7 K1 N7 180.0(2) 13_655 . ?
N7 K1 N7 75.10(14) . 4_554 ?
N7 K1 N7 104.90(14) 13_655 5 ?
N8 C8 C7 178.5(4) . . ?

