# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1562487'
_audit_update_record             
;
2017-07-16 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT250_1                   
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.9 Note  
RESPONSE: The larger than normal range of thermal motion is mostly due to 
the difference between the disordered group and the other atoms 
which are not disordered.
;
_vrf_PLAT430_1                   
;
PROBLEM: Short Inter D...A Contact  O2     ..  O2      ..       2.57 Ang.
RESPONSE: This alert is generated because disorder exist in the structure.
;
_vrf_PLAT990_1                   
; 
PROBLEM: Deprecated RES file style based SQUEEZE job ....          ! Note
RESPONSE: This alert is generated because the squeeze was used.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H12 Cu3 I3 N6 O24 Ti6'
_chemical_formula_weight         1771.24

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'

_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.
;

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

_cell_length_a                   32.330(4)
_cell_length_b                   32.330(4)
_cell_length_c                   32.330(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     33794(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4817
_cell_measurement_theta_min      1.82
_cell_measurement_theta_max      26.09

_exptl_crystal_description       block
_exptl_crystal_colour            dark
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    0.696
_exptl_crystal_F_000             6720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    1.212
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 'phi and omega scans'
_diffrn_reflns_number            105274
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         0.891
_diffrn_reflns_theta_max         26.030
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3171
_reflns_number_gt                2600
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1011P)²+138.9825P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3171
_refine_ls_number_parameters     93
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.2013
_refine_ls_wR_factor_gt          0.1899
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.46073(4) 0.25260(8) 0.0669(6) Uani 0.5 2 d S T P . .
I1 I 0.0000 0.5000 0.17838(3) 0.0734(3) Uani 1 4 d S T P . .
Ti1 Ti 0.20345(3) 0.27890(4) 0.20345(3) 0.0622(5) Uani 1 2 d DS T P . .
O1 O 0.16971(16) 0.25219(19) 0.16971(16) 0.087(2) Uani 1 2 d S T P . .
O2 O 0.25334(10) 0.25334(10) 0.19073(15) 0.0666(15) Uani 1 2 d DS T P . .
O3 O 0.16069(11) 0.32472(11) 0.21725(12) 0.0694(11) Uani 1 1 d . . . . .
N1 N 0.0513(3) 0.4249(2) 0.2505(4) 0.070(3) Uani 0.5 1 d . . P . .
C1 C 0.15615(13) 0.34385(13) 0.2500 0.078(3) Uani 1 2 d S T P A .
C2 C 0.12355(15) 0.37645(15) 0.2500 0.095(3) Uani 1 2 d S T P . .
C3' C 0.1102(9) 0.3923(13) 0.2140(12) 0.087(11) Uani 0.5 1 d . . P A 1
H3' H 0.1185 0.3805 0.1892 0.105 Uiso 0.5 1 calc R U P A 1
C4 C 0.0835(7) 0.4273(6) 0.2138(8) 0.105(7) Uani 0.5 1 d . . P A 1
C3 C 0.0965(8) 0.3827(12) 0.2146(14) 0.085(9) Uani 0.5 1 d . . P A 2
H3 H 0.1023 0.3691 0.1899 0.102 Uiso 0.5 1 calc R U P A 2
C4' C 0.0645(8) 0.4067(6) 0.2167(8) 0.110(7) Uani 0.5 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu1 1.803(2) 38 ?
Cu1 Cu1 1.803(2) 37_455 ?
Cu1 N1 2.023(8) 52 ?
Cu1 N1 2.023(8) . ?
Cu1 N1 2.460(8) 88_455 ?
Cu1 N1 2.460(8) 38 ?
Cu1 Cu1 2.539(3) 2_565 ?
Cu1 I1 2.567(2) 37_455 ?
Cu1 I1 2.715(2) . ?
I1 Cu1 2.567(2) 38 ?
I1 Cu1 2.567(2) 37_455 ?
I1 Cu1 2.715(2) 2_565 ?
Ti1 O1 1.768(8) . ?
Ti1 O2 1.8583(9) . ?
Ti1 O2 1.8583(9) 5 ?
Ti1 O3 2.075(3) . ?
Ti1 O3 2.075(3) 72 ?
Ti1 O2 2.206(6) 81 ?
Ti1 Ti1 3.116(3) 81 ?
Ti1 Ti1 3.116(3) 77 ?
O2 Ti1 1.8583(9) 9 ?
O2 Ti1 2.206(6) 77 ?
O3 C1 1.235(5) . ?
N1 N1 1.088(19) 38 ?
N1 C4' 1.31(2) . ?
N1 C4 1.37(3) 38 ?
N1 C4 1.58(3) . ?
N1 C4' 1.76(2) 38 ?
N1 Cu1 2.460(8) 38 ?
C1 O3 1.235(5) 38 ?
C1 C2 1.491(9) . ?
C2 C3' 1.34(4) . ?
C2 C3' 1.34(4) 38 ?
C2 C3 1.46(4) 38 ?
C2 C3 1.46(4) . ?
C3' C4 1.42(4) . ?
C4 N1 1.37(3) 38 ?
C3 C4' 1.29(4) . ?
C4' N1 1.76(2) 38 ?

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
Cu1 Cu1 Cu1 89.50(3) 38 37_455 ?
Cu1 Cu1 N1 167.6(3) 38 52 ?
Cu1 Cu1 N1 79.8(3) 37_455 52 ?
Cu1 Cu1 N1 79.8(3) 38 . ?
Cu1 Cu1 N1 167.5(3) 37_455 . ?
N1 Cu1 N1 110.1(5) 52 . ?
Cu1 Cu1 N1 143.3(2) 38 88_455 ?
Cu1 Cu1 N1 54.0(2) 37_455 88_455 ?
N1 Cu1 N1 25.8(5) 52 88_455 ?
N1 Cu1 N1 135.80(17) . 88_455 ?
Cu1 Cu1 N1 54.0(2) 38 38 ?
Cu1 Cu1 N1 143.3(2) 37_455 38 ?
N1 Cu1 N1 135.79(17) 52 38 ?
N1 Cu1 N1 25.8(4) . 38 ?
N1 Cu1 N1 161.3(5) 88_455 38 ?
Cu1 Cu1 Cu1 45.251(15) 38 2_565 ?
Cu1 Cu1 Cu1 45.251(14) 37_455 2_565 ?
N1 Cu1 Cu1 124.9(3) 52 2_565 ?
N1 Cu1 Cu1 124.9(3) . 2_565 ?
N1 Cu1 Cu1 99.1(2) 88_455 2_565 ?
N1 Cu1 Cu1 99.1(2) 38 2_565 ?
Cu1 Cu1 I1 74.51(13) 38 37_455 ?
Cu1 Cu1 I1 74.51(13) 37_455 37_455 ?
N1 Cu1 I1 108.2(3) 52 37_455 ?
N1 Cu1 I1 108.2(3) . 37_455 ?
N1 Cu1 I1 96.5(3) 88_455 37_455 ?
N1 Cu1 I1 96.5(3) 38 37_455 ?
Cu1 Cu1 I1 60.36(4) 2_565 37_455 ?
Cu1 Cu1 I1 65.69(13) 38 . ?
Cu1 Cu1 I1 65.69(13) 37_455 . ?
N1 Cu1 I1 103.7(3) 52 . ?
N1 Cu1 I1 103.7(3) . . ?
N1 Cu1 I1 92.2(3) 88_455 . ?
N1 Cu1 I1 92.2(3) 38 . ?
Cu1 Cu1 I1 62.12(4) 2_565 . ?
I1 Cu1 I1 122.48(6) 37_455 . ?
Cu1 I1 Cu1 59.28(8) 38 37_455 ?
Cu1 I1 Cu1 39.80(4) 38 . ?
Cu1 I1 Cu1 39.80(4) 37_455 . ?
Cu1 I1 Cu1 39.80(4) 38 2_565 ?
Cu1 I1 Cu1 39.80(4) 37_455 2_565 ?
Cu1 I1 Cu1 55.76(7) . 2_565 ?
O1 Ti1 O2 100.5(2) . . ?
O1 Ti1 O2 100.5(2) . 5 ?
O2 Ti1 O2 100.7(2) . 5 ?
O1 Ti1 O3 94.03(19) . . ?
O2 Ti1 O3 160.6(2) . . ?
O2 Ti1 O3 89.05(12) 5 . ?
O1 Ti1 O3 94.03(19) . 72 ?
O2 Ti1 O3 89.06(12) . 72 ?
O2 Ti1 O3 160.6(2) 5 72 ?
O3 Ti1 O3 77.10(18) . 72 ?
O1 Ti1 O2 177.2(2) . 81 ?
O2 Ti1 O2 77.8(2) . 81 ?
O2 Ti1 O2 77.8(2) 5 81 ?
O3 Ti1 O2 88.17(16) . 81 ?
O3 Ti1 O2 88.17(16) 72 81 ?
O1 Ti1 Ti1 142.98(8) . 81 ?
O2 Ti1 Ti1 97.83(18) . 81 ?
O2 Ti1 Ti1 44.25(18) 5 81 ?
O3 Ti1 Ti1 77.50(12) . 81 ?
O3 Ti1 Ti1 118.26(16) 72 81 ?
O2 Ti1 Ti1 35.99(5) 81 81 ?
O1 Ti1 Ti1 142.98(8) . 77 ?
O2 Ti1 Ti1 44.25(18) . 77 ?
O2 Ti1 Ti1 97.83(18) 5 77 ?
O3 Ti1 Ti1 118.26(16) . 77 ?
O3 Ti1 Ti1 77.51(12) 72 77 ?
O2 Ti1 Ti1 35.99(5) 81 77 ?
Ti1 Ti1 Ti1 67.22(7) 81 77 ?
Ti1 O2 Ti1 136.31(18) 9 . ?
Ti1 O2 Ti1 99.8(2) 9 77 ?
Ti1 O2 Ti1 99.8(2) . 77 ?
C1 O3 Ti1 128.4(4) . . ?
N1 N1 C4' 93.7(15) 38 . ?
N1 N1 C4 78.8(14) 38 38 ?
N1 N1 C4 58.6(12) 38 . ?
C4 N1 C4 108.0(14) 38 . ?
N1 N1 C4' 48.2(11) 38 38 ?
C4' N1 C4' 109.7(18) . 38 ?
N1 N1 Cu1 100.1(3) 38 . ?
C4' N1 Cu1 123.6(12) . . ?
C4 N1 Cu1 119.8(10) 38 . ?
C4 N1 Cu1 122.6(8) . . ?
C4' N1 Cu1 120.1(9) 38 . ?
N1 N1 Cu1 54.1(2) 38 38 ?
C4' N1 Cu1 117.5(10) . 38 ?
C4 N1 Cu1 108.0(11) 38 38 ?
C4 N1 Cu1 91.5(7) . 38 ?
C4' N1 Cu1 87.4(8) 38 38 ?
Cu1 N1 Cu1 46.18(17) . 38 ?
O3 C1 O3 128.0(6) . 38 ?
O3 C1 C2 116.0(3) . . ?
O3 C1 C2 116.0(3) 38 . ?
C3' C2 C3' 120(3) . 38 ?
C3 C2 C3 117(3) 38 . ?
C3' C2 C1 119.8(15) . . ?
C3' C2 C1 119.8(15) 38 . ?
C3 C2 C1 121.5(16) 38 . ?
C3 C2 C1 121.5(16) . . ?
C2 C3' C4 120(3) . . ?
N1 C4 C3' 121(2) 38 . ?
N1 C4 N1 42.5(10) 38 . ?
C3' C4 N1 111.0(19) . . ?
C4' C3 C2 121(4) . . ?
C3 C4' N1 125(3) . . ?
C3 C4' N1 110(3) . 38 ?
N1 C4' N1 38.1(9) . 38 ?

_refine_diff_density_max         1.317
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.096

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.007 -0.014 -0.007 25321 7564 ' '
_platon_squeeze_details          ?
