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

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

data_1P
_database_code_depnum_ccdc_archive 'CCDC 1562235'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[(CH3)2NH2]10[Zn3(Zn3O)2(C27H12N6O12)4] 18(CH3)2NCHO 31H2O'
_chemical_formula_sum            'C108 H48 N24 O50 Zn9'
_chemical_formula_weight         3070.21

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           210
_space_group_name_H-M_alt        'F 41 3 2'
_space_group_name_Hall           'F 4d 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+1/2, z+1/2'
'-x+1/2, y+1/2, -z'
'x+1/2, -y, -z+1/2'
'z, x, y'
'z+1/2, -x, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y'
'y, z, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z, -x+1/2'
'-y, -z+1/2, x+1/2'
'y+3/4, x+1/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'y+1/4, -x+3/4, z+3/4'
'-y+3/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+3/4'
'-x+3/4, z+3/4, y+1/4'
'-x+1/4, -z+1/4, -y+1/4'
'x+1/4, -z+3/4, y+3/4'
'z+3/4, y+1/4, -x+3/4'
'z+1/4, -y+3/4, x+3/4'
'-z+3/4, y+3/4, x+1/4'
'-z+1/4, -y+1/4, -x+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1, z+1'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'z, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1'
'-z, -x+1, y+1'
'-z+1/2, x+1, -y+1/2'
'y, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1/2'
'y+1/2, -z+1/2, -x+1'
'-y, -z+1, x+1'
'y+3/4, x+3/4, -z+5/4'
'-y+1/4, -x+3/4, -z+3/4'
'y+1/4, -x+5/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+5/4'
'-x+3/4, z+5/4, y+3/4'
'-x+1/4, -z+3/4, -y+3/4'
'x+1/4, -z+5/4, y+5/4'
'z+3/4, y+3/4, -x+5/4'
'z+1/4, -y+5/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+1/4, -y+3/4, -x+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, z+1'
'-x+1, y+1/2, -z+1/2'
'x+1, -y, -z+1'
'z+1/2, x, y+1/2'
'z+1, -x, -y+1'
'-z+1/2, -x+1/2, y+1'
'-z+1, x+1/2, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1, z+1/2, -x+1/2'
'y+1, -z, -x+1'
'-y+1/2, -z+1/2, x+1'
'y+5/4, x+1/4, -z+5/4'
'-y+3/4, -x+1/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+5/4, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+5/4'
'-x+5/4, z+3/4, y+3/4'
'-x+3/4, -z+1/4, -y+3/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+1/4, -x+5/4'
'z+3/4, -y+3/4, x+5/4'
'-z+5/4, y+3/4, x+3/4'
'-z+3/4, -y+1/4, -x+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1, y+1, -z'
'x+1, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y'
'z+1, -x+1/2, -y+1/2'
'-z+1/2, -x+1, y+1/2'
'-z+1, x+1, -y'
'y+1/2, z+1/2, x'
'-y+1, z+1, -x'
'y+1, -z+1/2, -x+1/2'
'-y+1/2, -z+1, x+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+1/4'
'y+3/4, -x+5/4, z+3/4'
'-y+5/4, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+3/4'
'-x+5/4, z+5/4, y+1/4'
'-x+3/4, -z+3/4, -y+1/4'
'x+3/4, -z+5/4, y+3/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+5/4, x+3/4'
'-z+5/4, y+5/4, x+1/4'
'-z+3/4, -y+3/4, -x+1/4'

_cell_length_a                   45.1476(7)
_cell_length_b                   45.1476(7)
_cell_length_c                   45.1476(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     92025(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9921
_cell_measurement_theta_min      2.344
_cell_measurement_theta_max      22.3755

_exptl_crystal_description       Octahedral
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    0.886
_exptl_crystal_F_000             24544.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    0.976
_shelx_estimated_absorpt_T_min   0.761
_shelx_estimated_absorpt_T_max   0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42855
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         2.210
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_full        25.024
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6790
_reflns_number_gt                4234
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond (Brandenburg and Putz, 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6774
_refine_ls_number_parameters     265
_refine_ls_number_restraints     340
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0842
_refine_ls_wR_factor_ref         0.3152
_refine_ls_wR_factor_gt          0.2704
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_restrained_S_all      1.130
_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
Zn1 Zn 0.5000 0.5000 0.23255(3) 0.1334(8) Uani 1 2 d S TU P . .
Zn2 Zn 0.39710(4) 0.66089(4) 0.12550(4) 0.1484(7) Uani 1 1 d . U . . .
C1 C 0.5589(3) 0.5937(2) 0.0935(2) 0.118(3) Uani 1 1 d D U . . .
C2 C 0.51454(13) 0.59776(15) 0.12700(14) 0.124(3) Uani 1 1 d DG U . . .
C3 C 0.48603(15) 0.60937(14) 0.12632(13) 0.124(3) Uani 1 1 d G U . . .
H3 H 0.4807 0.6232 0.1114 0.148 Uiso 1 1 calc R U . . .
C4 C 0.46536(12) 0.60068(16) 0.14741(15) 0.119(3) Uani 1 1 d DG U . . .
C5 C 0.47320(14) 0.58038(17) 0.16920(14) 0.133(3) Uani 1 1 d G U . . .
H5 H 0.4591 0.5744 0.1836 0.160 Uiso 1 1 calc R U . . .
C6 C 0.50170(16) 0.56877(15) 0.16988(13) 0.130(3) Uani 1 1 d DG U . . .
C7 C 0.52238(11) 0.57746(15) 0.14879(14) 0.114(3) Uani 1 1 d G U . . .
H7 H 0.5419 0.5695 0.1493 0.137 Uiso 1 1 calc R U . . .
C8 C 0.4362(3) 0.6138(3) 0.1476(3) 0.129(3) Uani 1 1 d D U . . .
C9 C 0.5117(3) 0.5464(3) 0.1912(2) 0.126(3) Uani 1 1 d D U . . .
C10 C 0.3544(2) 0.8207(3) 0.1814(2) 0.113(3) Uani 1 1 d D U . . .
C11 C 0.39660(13) 0.78652(14) 0.18994(14) 0.113(3) Uani 1 1 d DG U . . .
C12 C 0.42393(15) 0.78713(15) 0.20410(15) 0.139(4) Uani 1 1 d G U . . .
H12 H 0.4290 0.8034 0.2164 0.167 Uiso 1 1 calc R U . . .
C13 C 0.44380(11) 0.76393(18) 0.20022(16) 0.142(4) Uani 1 1 d DG U . . .
C14 C 0.43634(12) 0.74013(15) 0.18217(16) 0.117(3) Uani 1 1 d G U . . .
H14 H 0.4499 0.7243 0.1795 0.140 Uiso 1 1 calc R U . . .
C15 C 0.40901(12) 0.73953(12) 0.16800(14) 0.108(2) Uani 1 1 d DG U . . .
C16 C 0.38914(10) 0.76273(15) 0.17189(13) 0.116(3) Uani 1 1 d G U . . .
H16 H 0.3705 0.7623 0.1622 0.139 Uiso 1 1 calc R U . . .
C17 C 0.4719(4) 0.7637(4) 0.2175(5) 0.204(7) Uani 1 1 d D U . . .
C18 C 0.3998(2) 0.7146(3) 0.1495(2) 0.126(3) Uani 1 1 d D U . . .
N1 N 0.5696(2) 0.60607(17) 0.0686(2) 0.121(2) Uani 1 1 d D U . . .
N2 N 0.53312(19) 0.6065(2) 0.1038(2) 0.133(3) Uani 1 1 d D U . . .
H2 H 0.5275 0.6226 0.0944 0.160 Uiso 1 1 calc R U . . .
N3 N 0.3414(2) 0.84381(19) 0.1947(2) 0.127(3) Uani 1 1 d D U . . .
N4 N 0.37917(19) 0.8092(2) 0.1950(2) 0.139(3) Uani 1 1 d D U . . .
H4 H 0.3845 0.8195 0.2107 0.167 Uiso 1 1 calc R U . . .
O1 O 0.43050(18) 0.63156(19) 0.1259(2) 0.154(3) Uani 1 1 d D U . . .
O2 O 0.4173(2) 0.6032(2) 0.1670(2) 0.148(3) Uani 1 1 d D U . . .
O3 O 0.48858(19) 0.53290(19) 0.20697(16) 0.138(3) Uani 1 1 d D U . . .
O4 O 0.5354(2) 0.5385(2) 0.19405(16) 0.143(3) Uani 1 1 d D U . . .
O5 O 0.4766(2) 0.7868(3) 0.2346(2) 0.179(4) Uani 1 1 d D U . . .
O6 O 0.48958(18) 0.7455(3) 0.2161(3) 0.208(6) Uani 1 1 d D U . . .
O7 O 0.41693(17) 0.69113(19) 0.15098(19) 0.139(2) Uani 1 1 d D U . . .
O8 O 0.37612(19) 0.71366(18) 0.1344(2) 0.151(3) Uani 1 1 d D U . . .
O9 O 0.36181(14) 0.63819(14) 0.13819(14) 0.159(4) Uani 1 3 d S TU P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 1.951(8) 26_654 ?
Zn1 O3 1.951(8) . ?
Zn1 O6 1.991(9) 72_565 ?
Zn1 O6 1.991(9) 93_445 ?
Zn1 C17 2.600(13) 72_565 ?
Zn1 C17 2.600(13) 93_445 ?
Zn2 O2 1.953(9) 58 ?
Zn2 O9 1.979(4) . ?
Zn2 O7 1.997(10) . ?
Zn2 O1 2.007(7) . ?
C1 N1 1.306(13) 53_554 ?
C1 N1 1.343(13) . ?
C1 N2 1.381(11) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C2 N2 1.398(10) . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C8 1.442(12) . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C9 1.466(12) . ?
C8 O1 1.294(15) . ?
C8 O2 1.313(14) . ?
C9 O4 1.137(14) . ?
C9 O3 1.402(14) . ?
C10 N3 1.331(12) 11_465 ?
C10 N3 1.340(13) . ?
C10 N4 1.378(11) . ?
C11 N4 1.313(9) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C13 C17 1.490(13) . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C15 C18 1.462(11) . ?
C17 O6 1.146(16) . ?
C17 O5 1.316(17) . ?
C17 Zn1 2.600(13) 47_544 ?
C18 O8 1.270(12) . ?
C18 O7 1.313(12) . ?
N1 C1 1.306(13) 33_554 ?
N3 C10 1.331(12) 8_556 ?
O2 Zn2 1.953(9) 79_554 ?
O6 Zn1 1.991(9) 47_544 ?
O9 Zn2 1.979(4) 58 ?
O9 Zn2 1.979(4) 79_554 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 O3 107.4(5) 26_654 . ?
O3 Zn1 O6 104.4(5) 26_654 72_565 ?
O3 Zn1 O6 120.0(4) . 72_565 ?
O3 Zn1 O6 120.0(4) 26_654 93_445 ?
O3 Zn1 O6 104.4(5) . 93_445 ?
O6 Zn1 O6 101.6(6) 72_565 93_445 ?
O3 Zn1 C17 98.0(6) 26_654 72_565 ?
O3 Zn1 C17 142.9(5) . 72_565 ?
O6 Zn1 C17 24.7(5) 72_565 72_565 ?
O6 Zn1 C17 84.8(6) 93_445 72_565 ?
O3 Zn1 C17 142.9(5) 26_654 93_445 ?
O3 Zn1 C17 98.0(6) . 93_445 ?
O6 Zn1 C17 84.8(6) 72_565 93_445 ?
O6 Zn1 C17 24.7(5) 93_445 93_445 ?
C17 Zn1 C17 75.5(11) 72_565 93_445 ?
O2 Zn2 O9 110.7(3) 58 . ?
O2 Zn2 O7 118.5(4) 58 . ?
O9 Zn2 O7 123.2(3) . . ?
O2 Zn2 O1 96.2(4) 58 . ?
O9 Zn2 O1 105.1(4) . . ?
O7 Zn2 O1 96.3(4) . . ?
N1 C1 N1 126.3(9) 53_554 . ?
N1 C1 N2 118.9(10) 53_554 . ?
N1 C1 N2 114.3(11) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 N2 115.6(5) . . ?
C7 C2 N2 124.2(5) . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 119.8(7) . . ?
C3 C4 C8 120.1(7) . . ?
C4 C5 C6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C9 116.0(7) . . ?
C5 C6 C9 124.0(7) . . ?
C6 C7 C2 120.0 . . ?
O1 C8 O2 126.9(11) . . ?
O1 C8 C4 115.6(10) . . ?
O2 C8 C4 116.7(11) . . ?
O4 C9 O3 120.5(11) . . ?
O4 C9 C6 125.4(12) . . ?
O3 C9 C6 113.9(10) . . ?
N3 C10 N3 126.7(9) 11_465 . ?
N3 C10 N4 116.2(10) 11_465 . ?
N3 C10 N4 116.5(9) . . ?
N4 C11 C12 115.9(5) . . ?
N4 C11 C16 124.1(5) . . ?
C12 C11 C16 120.0 . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 C17 120.5(8) . . ?
C12 C13 C17 119.3(8) . . ?
C15 C14 C13 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 C18 118.0(5) . . ?
C14 C15 C18 122.0(5) . . ?
C15 C16 C11 120.0 . . ?
O6 C17 O5 119.3(13) . . ?
O6 C17 C13 124.7(15) . . ?
O5 C17 C13 115.9(12) . . ?
O6 C17 Zn1 46.4(7) . 47_544 ?
O5 C17 Zn1 74.4(7) . 47_544 ?
C13 C17 Zn1 166.2(14) . 47_544 ?
O8 C18 O7 119.8(10) . . ?
O8 C18 C15 124.9(8) . . ?
O7 C18 C15 115.2(9) . . ?
C1 N1 C1 113.5(9) 33_554 . ?
C1 N2 C2 129.9(9) . . ?
C10 N3 C10 112.5(10) 8_556 . ?
C11 N4 C10 134.5(8) . . ?
C8 O1 Zn2 124.5(7) . . ?
C8 O2 Zn2 123.5(9) . 79_554 ?
C9 O3 Zn1 115.8(7) . . ?
C17 O6 Zn1 108.9(11) . 47_544 ?
C18 O7 Zn2 105.0(7) . . ?
Zn2 O9 Zn2 109.5(3) 58 79_554 ?
Zn2 O9 Zn2 109.5(3) 58 . ?
Zn2 O9 Zn2 109.5(3) 79_554 . ?

_refine_diff_density_max         0.801
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.058



_exptl_crystal_recrystallization_method Solvothermal
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_1M
_database_code_depnum_ccdc_archive 'CCDC 1562236'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[(CH3)2NH2]10[Zn3(Zn3O)2(C27H12N6O12)4] 20(CH3)2NCHO 35H2O'
_chemical_formula_sum            'C108 H48 N24 O50 Zn9'
_chemical_formula_weight         3070.21

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           210
_space_group_name_H-M_alt        'F 41 3 2'
_space_group_name_Hall           'F 4d 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+1/2, z+1/2'
'-x+1/2, y+1/2, -z'
'x+1/2, -y, -z+1/2'
'z, x, y'
'z+1/2, -x, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y'
'y, z, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z, -x+1/2'
'-y, -z+1/2, x+1/2'
'y+3/4, x+1/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'y+1/4, -x+3/4, z+3/4'
'-y+3/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+3/4'
'-x+3/4, z+3/4, y+1/4'
'-x+1/4, -z+1/4, -y+1/4'
'x+1/4, -z+3/4, y+3/4'
'z+3/4, y+1/4, -x+3/4'
'z+1/4, -y+3/4, x+3/4'
'-z+3/4, y+3/4, x+1/4'
'-z+1/4, -y+1/4, -x+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1, z+1'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'z, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1'
'-z, -x+1, y+1'
'-z+1/2, x+1, -y+1/2'
'y, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1/2'
'y+1/2, -z+1/2, -x+1'
'-y, -z+1, x+1'
'y+3/4, x+3/4, -z+5/4'
'-y+1/4, -x+3/4, -z+3/4'
'y+1/4, -x+5/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+5/4'
'-x+3/4, z+5/4, y+3/4'
'-x+1/4, -z+3/4, -y+3/4'
'x+1/4, -z+5/4, y+5/4'
'z+3/4, y+3/4, -x+5/4'
'z+1/4, -y+5/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+1/4, -y+3/4, -x+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, z+1'
'-x+1, y+1/2, -z+1/2'
'x+1, -y, -z+1'
'z+1/2, x, y+1/2'
'z+1, -x, -y+1'
'-z+1/2, -x+1/2, y+1'
'-z+1, x+1/2, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1, z+1/2, -x+1/2'
'y+1, -z, -x+1'
'-y+1/2, -z+1/2, x+1'
'y+5/4, x+1/4, -z+5/4'
'-y+3/4, -x+1/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+5/4, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+5/4'
'-x+5/4, z+3/4, y+3/4'
'-x+3/4, -z+1/4, -y+3/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+1/4, -x+5/4'
'z+3/4, -y+3/4, x+5/4'
'-z+5/4, y+3/4, x+3/4'
'-z+3/4, -y+1/4, -x+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1, y+1, -z'
'x+1, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y'
'z+1, -x+1/2, -y+1/2'
'-z+1/2, -x+1, y+1/2'
'-z+1, x+1, -y'
'y+1/2, z+1/2, x'
'-y+1, z+1, -x'
'y+1, -z+1/2, -x+1/2'
'-y+1/2, -z+1, x+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+1/4'
'y+3/4, -x+5/4, z+3/4'
'-y+5/4, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+3/4'
'-x+5/4, z+5/4, y+1/4'
'-x+3/4, -z+3/4, -y+1/4'
'x+3/4, -z+5/4, y+3/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+5/4, x+3/4'
'-z+5/4, y+5/4, x+1/4'
'-z+3/4, -y+3/4, -x+1/4'

_cell_length_a                   45.1207(6)
_cell_length_b                   45.1207(6)
_cell_length_c                   45.1207(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     91860(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9900
_cell_measurement_theta_min      2.6705
_cell_measurement_theta_max      23.0135

_exptl_crystal_description       Octahedral
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_F_000             24544.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_exptl_absorpt_coefficient_mu    0.977
_shelx_estimated_absorpt_T_min   0.753
_shelx_estimated_absorpt_T_max   0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40964
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         2.211
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_full        25.021
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6782
_reflns_number_gt                3302
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond (Brandenburg and Putz, 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6745
_refine_ls_number_parameters     265
_refine_ls_number_restraints     334
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.2974
_refine_ls_wR_factor_gt          0.2305
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_restrained_S_all      0.964
_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
Zn1 Zn 1.0000 0.0000 0.23274(3) 0.1425(8) Uani 1 2 d S TU P . .
Zn2 Zn 0.83898(4) 0.10282(4) 0.12620(4) 0.1551(8) Uani 1 1 d . U . . .
C1 C 0.9067(3) -0.0580(3) 0.0939(2) 0.124(3) Uani 1 1 d D U . . .
C2 C 0.90196(16) -0.01411(15) 0.12754(15) 0.133(3) Uani 1 1 d DG U . . .
C3 C 0.89001(14) 0.01428(17) 0.12733(14) 0.120(3) Uani 1 1 d G U . . .
H3 H 0.8759 0.0196 0.1127 0.144 Uiso 1 1 calc R U . . .
C4 C 0.89876(16) 0.03483(13) 0.14854(16) 0.127(3) Uani 1 1 d DG U . . .
C5 C 0.91945(17) 0.02700(16) 0.16997(14) 0.135(3) Uani 1 1 d G U . . .
H5 H 0.9254 0.0410 0.1845 0.162 Uiso 1 1 calc R U . . .
C6 C 0.93140(15) -0.00140(18) 0.17019(14) 0.137(3) Uani 1 1 d DG U . . .
C7 C 0.92266(17) -0.02195(13) 0.14897(17) 0.128(3) Uani 1 1 d G U . . .
H7 H 0.9308 -0.0414 0.1491 0.153 Uiso 1 1 calc R U . . .
C8 C 0.8861(3) 0.0643(3) 0.1477(3) 0.139(3) Uani 1 1 d D U . . .
C9 C 0.9540(3) -0.0111(3) 0.1918(2) 0.134(3) Uani 1 1 d D U . . .
C10 C 0.6787(3) 0.1452(2) 0.1812(3) 0.130(3) Uani 1 1 d D U . . .
C11 C 0.71319(15) 0.10365(15) 0.19069(18) 0.134(4) Uani 1 1 d DG U . . .
C12 C 0.71271(16) 0.07674(17) 0.20567(18) 0.160(5) Uani 1 1 d G U . . .
H12 H 0.6966 0.0720 0.2183 0.191 Uiso 1 1 calc R U . . .
C13 C 0.73586(19) 0.05672(13) 0.20211(18) 0.155(5) Uani 1 1 d DG U . . .
C14 C 0.75948(16) 0.06362(14) 0.18358(18) 0.144(4) Uani 1 1 d G U . . .
H14 H 0.7753 0.0499 0.1812 0.173 Uiso 1 1 calc R U . . .
C15 C 0.75996(14) 0.09054(15) 0.16860(16) 0.128(3) Uani 1 1 d DG U . . .
C16 C 0.73681(16) 0.11055(12) 0.17216(16) 0.128(3) Uani 1 1 d G U . . .
H16 H 0.7371 0.1289 0.1619 0.153 Uiso 1 1 calc R U . . .
C17 C 0.7367(4) 0.0287(4) 0.2194(4) 0.209(8) Uani 1 1 d D U . . .
C18 C 0.7848(3) 0.0994(3) 0.1500(3) 0.137(3) Uani 1 1 d D U . . .
N1 N 0.9311(2) -0.0685(2) 0.10645(16) 0.123(2) Uani 1 1 d D U . . .
N2 N 0.8939(2) -0.03352(18) 0.1046(2) 0.133(3) Uani 1 1 d D U . . .
H2 H 0.8772 -0.0287 0.0957 0.159 Uiso 1 1 calc R U . . .
N3 N 0.65603(19) 0.1584(2) 0.1949(2) 0.131(3) Uani 1 1 d D U . . .
N4 N 0.6909(2) 0.1212(2) 0.1952(2) 0.155(4) Uani 1 1 d D U . . .
H4 H 0.6810 0.1164 0.2113 0.186 Uiso 1 1 calc R U . . .
O1 O 0.8680(2) 0.06901(18) 0.1273(2) 0.155(3) Uani 1 1 d D U . . .
O2 O 0.89616(19) 0.08384(18) 0.16694(19) 0.145(3) Uani 1 1 d D U . . .
O3 O 0.9658(2) 0.0108(2) 0.20786(16) 0.160(3) Uani 1 1 d D U . . .
O4 O 0.9625(2) -0.0356(2) 0.19372(17) 0.159(3) Uani 1 1 d D U . . .
O5 O 0.7138(3) 0.0239(3) 0.2363(3) 0.207(5) Uani 1 1 d D U . . .
O6 O 0.7534(3) 0.01026(19) 0.2147(3) 0.230(6) Uani 1 1 d D U . . .
O7 O 0.80816(18) 0.08271(17) 0.15160(19) 0.143(3) Uani 1 1 d D U . . .
O8 O 0.78540(18) 0.1231(2) 0.1347(2) 0.159(3) Uani 1 1 d D U . . .
O9 O 0.86121(13) 0.13879(13) 0.13879(13) 0.145(4) Uani 1 3 d S TU P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 1.970(9) . ?
Zn1 O3 1.970(9) 26_744 ?
Zn1 O6 2.026(11) 44_544 ?
Zn1 O6 2.026(11) 18_645 ?
Zn1 C17 2.562(13) 44_544 ?
Zn1 C17 2.562(13) 18_645 ?
Zn2 O2 1.931(9) 31_654 ?
Zn2 O9 1.991(4) . ?
Zn2 O1 2.011(7) . ?
Zn2 O7 2.018(9) . ?
C1 N1 1.327(13) . ?
C1 N2 1.340(11) . ?
C1 N1 1.380(12) 80_535 ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C2 N2 1.403(10) . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C8 1.447(12) . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C9 1.478(12) . ?
C8 O1 1.253(15) . ?
C8 O2 1.316(14) . ?
C9 O4 1.173(14) . ?
C9 O3 1.338(15) . ?
C10 N3 1.334(13) . ?
C10 N3 1.355(12) 77_545 ?
C10 N4 1.368(12) . ?
C11 N4 1.296(10) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C13 C17 1.487(13) . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C15 C18 1.455(12) . ?
C17 O6 1.142(15) . ?
C17 O5 1.301(17) . ?
C17 Zn1 2.562(13) 41_444 ?
C18 O8 1.274(14) . ?
C18 O7 1.300(13) . ?
N1 C1 1.380(12) 59 ?
N3 C10 1.355(12) 57_554 ?
O2 Zn2 1.931(9) 82_546 ?
O6 Zn1 2.026(11) 41_444 ?
O9 Zn2 1.991(4) 82_546 ?
O9 Zn2 1.991(4) 31_654 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 O3 110.5(5) . 26_744 ?
O3 Zn1 O6 102.3(5) . 44_544 ?
O3 Zn1 O6 119.1(4) 26_744 44_544 ?
O3 Zn1 O6 119.1(4) . 18_645 ?
O3 Zn1 O6 102.3(5) 26_744 18_645 ?
O6 Zn1 O6 104.4(7) 44_544 18_645 ?
O3 Zn1 C17 98.2(6) . 44_544 ?
O3 Zn1 C17 141.1(5) 26_744 44_544 ?
O6 Zn1 C17 25.6(5) 44_544 44_544 ?
O6 Zn1 C17 84.9(6) 18_645 44_544 ?
O3 Zn1 C17 141.2(5) . 18_645 ?
O3 Zn1 C17 98.2(6) 26_744 18_645 ?
O6 Zn1 C17 84.9(6) 44_544 18_645 ?
O6 Zn1 C17 25.6(5) 18_645 18_645 ?
C17 Zn1 C17 72.1(11) 44_544 18_645 ?
O2 Zn2 O9 109.5(3) 31_654 . ?
O2 Zn2 O1 97.5(4) 31_654 . ?
O9 Zn2 O1 106.5(4) . . ?
O2 Zn2 O7 118.5(4) 31_654 . ?
O9 Zn2 O7 123.5(3) . . ?
O1 Zn2 O7 95.4(4) . . ?
N1 C1 N2 119.9(11) . . ?
N1 C1 N1 125.9(9) . 80_535 ?
N2 C1 N1 114.0(11) . 80_535 ?
C3 C2 C7 120.0 . . ?
C3 C2 N2 118.0(6) . . ?
C7 C2 N2 121.9(6) . . ?
C4 C3 C2 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 121.0(8) . . ?
C3 C4 C8 118.9(8) . . ?
C6 C5 C4 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C9 123.1(7) . . ?
C7 C6 C9 116.9(7) . . ?
C6 C7 C2 120.0 . . ?
O1 C8 O2 126.7(11) . . ?
O1 C8 C4 115.5(11) . . ?
O2 C8 C4 117.6(11) . . ?
O4 C9 O3 121.8(12) . . ?
O4 C9 C6 123.7(12) . . ?
O3 C9 C6 114.4(11) . . ?
N3 C10 N3 127.4(9) . 77_545 ?
N3 C10 N4 116.6(10) . . ?
N3 C10 N4 114.7(10) 77_545 . ?
N4 C11 C12 116.5(6) . . ?
N4 C11 C16 123.5(6) . . ?
C12 C11 C16 120.0 . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 C17 119.2(8) . . ?
C12 C13 C17 120.7(8) . . ?
C15 C14 C13 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 C18 122.2(6) . . ?
C16 C15 C18 117.7(6) . . ?
C15 C16 C11 120.0 . . ?
O6 C17 O5 120.8(15) . . ?
O6 C17 C13 122.5(15) . . ?
O5 C17 C13 115.5(12) . . ?
O6 C17 Zn1 50.0(8) . 41_444 ?
O5 C17 Zn1 74.6(8) . 41_444 ?
C13 C17 Zn1 167.6(13) . 41_444 ?
O8 C18 O7 119.9(11) . . ?
O8 C18 C15 124.2(9) . . ?
O7 C18 C15 115.7(10) . . ?
C1 N1 C1 114.0(10) . 59 ?
C1 N2 C2 132.0(10) . . ?
C10 N3 C10 111.4(10) . 57_554 ?
C11 N4 C10 136.4(10) . . ?
C8 O1 Zn2 124.8(8) . . ?
C8 O2 Zn2 125.5(9) . 82_546 ?
C9 O3 Zn1 115.9(9) . . ?
C17 O6 Zn1 104.5(11) . 41_444 ?
C18 O7 Zn2 105.5(8) . . ?
Zn2 O9 Zn2 108.8(3) . 82_546 ?
Zn2 O9 Zn2 108.8(3) . 31_654 ?
Zn2 O9 Zn2 108.8(3) 82_546 31_654 ?

_refine_diff_density_max         0.461
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.069



_exptl_crystal_recrystallization_method Solvothermal
_exptl_crystal_preparation       Luminescent
