# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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. 
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data_kme_999
_database_code_depnum_ccdc_archive 'CCDC 1843058'
_audit_update_record             
;
2018-05-13 deposited with the CCDC.
2018-06-06 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         
'2(C2 H8 N1 1+),(Y6 (O H)8 (C16 H6 O8)3 (H2 O) 2-), 5.5(H2 O), (C3 H7 N O)'
_chemical_formula_sum            'C55 H60 N3 O38.50 Y6'
_chemical_formula_weight         1912.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 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'
'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'
'-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'
'-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'

_cell_length_a                   25.1402(7)
_cell_length_b                   25.1402(7)
_cell_length_c                   25.1402(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15889(1)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    5645
_cell_measurement_theta_min      3.52
_cell_measurement_theta_max      63.93

_exptl_crystal_description       cubic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_F_000             7624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    6.395
_shelx_estimated_absorpt_T_min   0.883
_shelx_estimated_absorpt_T_max   0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0513
_exptl_absorpt_correction_T_max  0.1455
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0971 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.3526.
The λ/2 correction factor is 0.00150.
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\ms'
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            28451
_diffrn_reflns_av_unetI/netI     0.1368
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.485
_diffrn_reflns_theta_max         64.195
_diffrn_reflns_theta_full        64.195
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2383
_reflns_number_gt                2157
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material  
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'

_refine_special_details          
;
 The crystal structure was refined as a 2-component merohedral twin
 with the twin law -1 0 0 0 0 1 0 1 0 and fractional contributions of ~0.5.
 As the structure was hardly twinned, a set of restraints and
 constraints was applied to make both geometry and thermal parameters of
 the organic spacer reasonable. Strongly disorderd dimethylammonium cations
 and DMF molecules were refined isotropically with no restraints applied to
 their thermal parameters (only to interatomic distances, DFIXes). 
 Hydrogen atoms were placed in geometrically calculated positions
 and included in the refinement process using riding model with 
 isotropic thermal parameters: Uiso (H) = 1.2 Ueq(-CH, >NH2) or
 1.5 Ueq(-OH, -CH3). It was not possible to set H atoms at
 the geometrically calculated positions using AFIX 43 for H3A, H3B and H1D,
 so a set of DFIXes was applied.
 PLATON's SQUEEZE procedure was used to estimate diffuse electron density
 of heavily disordered solvent molecules. There are eight cavities per
 the unit cell containing about 4 electrons each. It corresponds to a half
 of water molecule in the each cavity (SQUEEZE usually underestimates
 the electron density a bit). The reported formula includes these water
 molecules but the structure factors were not corrected for the solvent
 contribution. 
;
_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   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         28451
_refine_ls_number_parameters     211
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.1496
_refine_ls_R_factor_gt           0.1252
_refine_ls_wR_factor_ref         0.3342
_refine_ls_wR_factor_gt          0.3101
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.564
_refine_ls_shift/su_max          0.000
_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
Y1 Y 0.27032(6) 0.64484(6) 0.76836(6) 0.0362(6) Uani 1 1 d . . . . .
O1H O 0.2979(4) 0.7021(4) 0.7021(4) 0.031(4) Uani 1 3 d S T P . .
H1H H 0.3209 0.6791 0.6791 0.047 Uiso 1 3 calc R U P . .
O2H O 0.2182(4) 0.7024(4) 0.8150(4) 0.023(2) Uani 1 1 d . . . . .
H2H H 0.2038 0.6810 0.8453 0.034 Uiso 1 1 calc R U . . .
O1W O 0.2888(14) 0.5433(12) 0.7819(15) 0.063(8) Uani 0.5 1 d D . P . .
O2WB O 0.359(3) 0.486(2) 0.842(3) 0.09(3) Uani 0.25 1 d D U P . .
O1A O 0.2654(5) 0.5945(6) 0.6929(5) 0.045(3) Uani 1 1 d D . . . .
O2A O 0.2367(6) 0.6414(5) 0.6192(6) 0.055(4) Uani 1 1 d D . . . .
C1A C 0.2491(9) 0.5995(8) 0.6445(7) 0.052(5) Uani 1 1 d D U . . .
C2A C 0.2544(16) 0.5487(10) 0.6138(9) 0.042(6) Uani 0.5 1 d D U P . .
C3A C 0.2508(8) 0.5000 0.6416(9) 0.052(7) Uani 1 2 d DS TU P . .
H3A H 0.254(2) 0.5000 0.6792(9) 0.062 Uiso 1 2 d DS U P . .
C4A C 0.2430(16) 0.4534(13) 0.6132(10) 0.042(6) Uani 0.5 1 d D U P . .
C5A C 0.2398(16) 0.4515(12) 0.5578(12) 0.037(6) Uani 0.5 1 d D U P . .
H5A H 0.2338 0.4190 0.5394 0.045 Uiso 0.5 1 calc R U P . .
C6A C 0.2461(14) 0.5000 0.5302(9) 0.051(6) Uani 1 2 d DS TU P . .
C7A C 0.2559(16) 0.5484(12) 0.5579(12) 0.037(6) Uani 0.5 1 d D U P . .
H7A H 0.2634 0.5801 0.5388 0.045 Uiso 0.5 1 calc R U P . .
O1B O 0.1948(5) 0.5959(5) 0.7861(6) 0.052(3) Uani 1 1 d D . . . .
O2B O 0.1197(6) 0.6425(6) 0.7879(6) 0.051(3) Uani 1 1 d D . . . .
C1B C 0.1451(7) 0.6003(7) 0.7857(9) 0.051(5) Uani 1 1 d D U . . .
C2B C 0.1151(9) 0.5483(10) 0.7791(16) 0.053(6) Uani 0.5 1 d D U P . .
C3B C 0.1415(11) 0.5000 0.7862(8) 0.058(7) Uani 1 2 d DS TU P . .
H3B H 0.1793(12) 0.5000 0.788(2) 0.070 Uiso 1 2 d DS U P . .
C4B C 0.1148(9) 0.4512(10) 0.7905(16) 0.053(6) Uani 0.5 1 d D U P . .
C5B C 0.0590(13) 0.4544(14) 0.7924(18) 0.054(7) Uani 0.5 1 d D U P . .
H5B H 0.0402 0.4229 0.8015 0.065 Uiso 0.5 1 calc R U P . .
C6B C 0.0289(12) 0.5000 0.7820(18) 0.068(7) Uani 1 2 d DS TU P . .
C7B C 0.0593(13) 0.5476(15) 0.7765(18) 0.054(7) Uani 0.5 1 d D U P . .
H7B H 0.0411 0.5803 0.7710 0.065 Uiso 0.5 1 calc R U P . .
N1D N 0.431(2) 0.629(3) 0.592(3) 0.12(6) Uiso 0.1667 1 d D . P . 1
O1D O 0.3581(11) 0.6419(11) 0.6419(11) 0.062(12) Uiso 0.5 3 d DS . P . 1
C1D C 0.3859(12) 0.6141(12) 0.6141(12) 0.09(3) Uiso 0.5 3 d DS . P . 1
H1D H 0.374(3) 0.5789(14) 0.608(3) 0.104 Uiso 0.1667 1 d D U P A 1
C2D C 0.473(4) 0.656(6) 0.621(6) 0.08(4) Uiso 0.1667 1 d D . P . 1
H2DA H 0.5027 0.6627 0.5972 0.119 Uiso 0.3333 2 calc R U P . 1
H2DB H 0.4587 0.6897 0.6344 0.119 Uiso 0.1667 1 calc R U P . 1
H2DC H 0.4843 0.6337 0.6508 0.119 Uiso 0.1667 1 calc R U P . 1
C3D C 0.443(6) 0.618(7) 0.537(4) 0.08(5) Uiso 0.1667 1 d D . P . 1
H3DA H 0.4787 0.6317 0.5285 0.126 Uiso 0.1667 1 calc R U P . 1
H3DB H 0.4423 0.5795 0.5308 0.126 Uiso 0.1667 1 calc R U P . 1
H3DC H 0.4167 0.6354 0.5145 0.126 Uiso 0.1667 1 calc R U P . 1
N1AA N 0.400(7) 0.614(7) 0.5000 0.11(7) Uiso 0.1667 2 d DS . P . 2
H1AG H 0.3868 0.6312 0.5293 0.130 Uiso 0.0833 1 calc R U P . 2
H1AF H 0.3868 0.6312 0.4707 0.130 Uiso 0.0833 1 calc R U P . 2
C1AA C 0.382(9) 0.558(7) 0.5000 0.07(5) Uiso 0.1667 2 d DS . P . 2
H1AJ H 0.3432 0.5568 0.5000 0.099 Uiso 0.1667 2 calc R U P . 2
H1AI H 0.3959 0.5404 0.4682 0.099 Uiso 0.0833 1 calc R U P . 2
H1AH H 0.3959 0.5404 0.5318 0.099 Uiso 0.0833 1 calc R U P . 2
C2AA C 0.458(7) 0.616(8) 0.5000 0.06(5) Uiso 0.1667 2 d DS . P . 2
H2AF H 0.4705 0.6529 0.5000 0.095 Uiso 0.1667 2 calc R U P . 2
H2AD H 0.4720 0.5978 0.5318 0.095 Uiso 0.0833 1 calc R U P . 2
H2AE H 0.4720 0.5978 0.4682 0.095 Uiso 0.0833 1 calc R U P . 2
N1AB N 0.123(4) 0.611(7) 0.918(6) 0.15(6) Uiso 0.25 1 d D . P . .
H1AB H 0.1387 0.5986 0.8877 0.181 Uiso 0.25 1 calc R U P . .
H1AA H 0.1285 0.6467 0.9191 0.181 Uiso 0.25 1 calc R U P . .
C1AB C 0.066(4) 0.601(5) 0.914(4) 0.08(3) Uiso 0.25 1 d D . P . .
H1AE H 0.0515 0.6190 0.8824 0.119 Uiso 0.25 1 calc R U P . .
H1AC H 0.0591 0.5629 0.9116 0.119 Uiso 0.25 1 calc R U P . .
H1AD H 0.0480 0.6154 0.9459 0.119 Uiso 0.25 1 calc R U P . .
C2AB C 0.150(5) 0.587(6) 0.963(5) 0.10(4) Uiso 0.25 1 d D . P . .
H2AC H 0.1876 0.5959 0.9619 0.153 Uiso 0.25 1 calc R U P . .
H2AB H 0.1341 0.6009 0.9961 0.153 Uiso 0.5 2 calc R U P . .
H2AA H 0.1452 0.5484 0.9618 0.153 Uiso 0.25 1 calc R U 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
Y1 O2H 2.277(9) . ?
Y1 O2H 2.281(11) 43_456 ?
Y1 O1A 2.284(13) . ?
Y1 O1B 2.306(12) . ?
Y1 O1H 2.309(4) . ?
Y1 O2A 2.315(13) 10_656 ?
Y1 O2H 2.351(10) 46_465 ?
Y1 O2B 2.369(15) 43_456 ?
Y1 O1W 2.62(3) . ?
Y1 Y1 3.836(3) 43_456 ?
Y1 Y1 3.836(3) 46_465 ?
Y1 Y1 3.891(3) 10_656 ?
O1H Y1 2.309(4) 10_656 ?
O1H Y1 2.309(4) 7_665 ?
O1H H1H 1.0000 . ?
O2H Y1 2.281(10) 46_465 ?
O2H Y1 2.351(10) 43_456 ?
O2H H2H 1.0000 . ?
O2WB O2WB 0.72(12) 27_565 ?
O1A C1A 1.29(2) . ?
O2A C1A 1.27(2) . ?
O2A Y1 2.315(13) 7_665 ?
C1A C2A 1.50(3) . ?
C1A C4A 1.55(4) 27_565 ?
C2A C4A 0.29(6) 27_565 ?
C2A C7A 1.41(3) . ?
C2A C3A 1.41(2) . ?
C2A C5A 1.45(4) 27_565 ?
C3A C4A 1.39(2) . ?
C3A C4A 1.39(2) 27_565 ?
C3A C2A 1.41(2) 27_565 ?
C3A H3A 0.950(4) . ?
C4A C5A 1.40(3) . ?
C4A C7A 1.43(5) 27_565 ?
C4A C1A 1.55(4) 27_565 ?
C5A C6A 1.41(3) . ?
C5A H5A 0.9500 . ?
C6A C5A 1.41(3) 27_565 ?
C6A C7A 1.42(3) . ?
C6A C7A 1.42(3) 27_565 ?
C6A C6A 1.52(5) 26_556 ?
C7A H7A 0.9500 . ?
O1B C1B 1.254(19) . ?
O2B C1B 1.24(2) . ?
O2B Y1 2.369(15) 46_465 ?
C1B C4B 1.51(3) 27_565 ?
C1B C2B 1.52(3) . ?
C2B C4B 0.29(6) 27_565 ?
C2B C3B 1.40(2) . ?
C2B C7B 1.40(3) . ?
C2B C5B 1.45(5) 27_565 ?
C3B C2B 1.40(2) 27_565 ?
C3B C4B 1.40(2) . ?
C3B C4B 1.40(2) 27_565 ?
C3B H3B 0.950(4) . ?
C4B C5B 1.41(3) . ?
C4B C7B 1.44(4) 27_565 ?
C4B C1B 1.51(3) 27_565 ?
C5B C6B 1.40(3) . ?
C5B H5B 0.9500 . ?
C6B C5B 1.40(3) 27_565 ?
C6B C7B 1.43(3) . ?
C6B C7B 1.43(3) 27_565 ?
C6B C6B 1.45(6) 2_565 ?
C7B H7B 0.9500 . ?
N1D C1D 1.32(3) . ?
N1D C2D 1.43(4) . ?
N1D C3D 1.44(3) . ?
O1D C1D 1.21(3) . ?
C1D N1D 1.32(3) 10_656 ?
C1D N1D 1.32(3) 7_665 ?
C1D H1D 0.950(4) . ?
C2D H2DA 0.9800 . ?
C2D H2DB 0.9800 . ?
C2D H2DC 0.9800 . ?
C3D H3DA 0.9800 . ?
C3D H3DB 0.9800 . ?
C3D H3DC 0.9800 . ?
N1AA C1AA 1.48(4) . ?
N1AA C2AA 1.48(4) . ?
N1AA H1AG 0.9100 . ?
N1AA H1AF 0.9100 . ?
C1AA C2AA 1.80(17) 35_655 ?
C1AA C2AA 1.80(17) 33_666 ?
C1AA H1AJ 0.9800 . ?
C1AA H1AI 0.9800 . ?
C1AA H1AH 0.9800 . ?
C2AA H2AF 0.9800 . ?
C2AA H2AD 0.9800 . ?
C2AA H2AE 0.9800 . ?
N1AB C2AB 1.45(7) . ?
N1AB C1AB 1.47(7) . ?
N1AB H1AB 0.9100 . ?
N1AB H1AA 0.9100 . ?
C1AB H1AE 0.9800 . ?
C1AB H1AC 0.9800 . ?
C1AB H1AD 0.9800 . ?
C2AB H2AC 0.9800 . ?
C2AB H2AB 0.9800 . ?
C2AB H2AA 0.9800 . ?

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
O2H Y1 O2H 66.7(3) . 43_456 ?
O2H Y1 O1A 138.4(4) . . ?
O2H Y1 O1A 138.0(4) 43_456 . ?
O2H Y1 O1B 76.5(4) . . ?
O2H Y1 O1B 140.8(5) 43_456 . ?
O1A Y1 O1B 79.6(5) . . ?
O2H Y1 O1H 98.6(5) . . ?
O2H Y1 O1H 65.2(3) 43_456 . ?
O1A Y1 O1H 76.2(4) . . ?
O1B Y1 O1H 136.0(4) . . ?
O2H Y1 O2A 139.2(5) . 10_656 ?
O2H Y1 O2A 76.7(5) 43_456 10_656 ?
O1A Y1 O2A 81.5(5) . 10_656 ?
O1B Y1 O2A 130.6(5) . 10_656 ?
O1H Y1 O2A 81.1(5) . 10_656 ?
O2H Y1 O2H 65.5(3) . 46_465 ?
O2H Y1 O2H 100.6(4) 43_456 46_465 ?
O1A Y1 O2H 75.7(4) . 46_465 ?
O1B Y1 O2H 74.6(4) . 46_465 ?
O1H Y1 O2H 64.1(3) . 46_465 ?
O2A Y1 O2H 141.9(5) 10_656 46_465 ?
O2H Y1 O2B 77.9(4) . 43_456 ?
O2H Y1 O2B 79.6(4) 43_456 43_456 ?
O1A Y1 O2B 130.4(5) . 43_456 ?
O1B Y1 O2B 80.1(6) . 43_456 ?
O1H Y1 O2B 142.5(4) . 43_456 ?
O2A Y1 O2B 78.4(5) 10_656 43_456 ?
O2H Y1 O2B 139.2(4) 46_465 43_456 ?
O2H Y1 O1W 130.9(9) . . ?
O2H Y1 O1W 131.2(7) 43_456 . ?
O1A Y1 O1W 65.0(9) . . ?
O1B Y1 O1W 66.4(8) . . ?
O1H Y1 O1W 130.4(10) . . ?
O2A Y1 O1W 64.2(8) 10_656 . ?
O2H Y1 O1W 128.2(7) 46_465 . ?
O2B Y1 O1W 65.4(9) 43_456 . ?
O2H Y1 Y1 34.6(2) . 43_456 ?
O2H Y1 Y1 32.7(2) 43_456 43_456 ?
O1A Y1 Y1 158.0(3) . 43_456 ?
O1B Y1 Y1 108.6(4) . 43_456 ?
O1H Y1 Y1 84.4(3) . 43_456 ?
O2A Y1 Y1 105.8(4) 10_656 43_456 ?
O2H Y1 Y1 86.7(2) 46_465 43_456 ?
O2B Y1 Y1 71.6(4) 43_456 43_456 ?
O1W Y1 Y1 136.9(8) . 43_456 ?
O2H Y1 Y1 32.7(3) . 46_465 ?
O2H Y1 Y1 86.6(2) 43_456 46_465 ?
O1A Y1 Y1 106.3(4) . 46_465 ?
O1B Y1 Y1 67.9(3) . 46_465 ?
O1H Y1 Y1 84.4(3) . 46_465 ?
O2A Y1 Y1 161.4(4) 10_656 46_465 ?
O2H Y1 Y1 33.4(2) 46_465 46_465 ?
O2B Y1 Y1 107.0(4) 43_456 46_465 ?
O1W Y1 Y1 134.4(8) . 46_465 ?
Y1 Y1 Y1 60.94(6) 43_456 46_465 ?
O2H Y1 Y1 86.4(2) . 10_656 ?
O2H Y1 Y1 33.4(2) 43_456 10_656 ?
O1A Y1 Y1 105.3(3) . 10_656 ?
O1B Y1 Y1 157.8(3) . 10_656 ?
O1H Y1 Y1 32.58(15) . 10_656 ?
O2A Y1 Y1 71.5(4) 10_656 10_656 ?
O2H Y1 Y1 85.5(3) 46_465 10_656 ?
O2B Y1 Y1 110.3(4) 43_456 10_656 ?
O1W Y1 Y1 135.6(8) . 10_656 ?
Y1 Y1 Y1 59.53(3) 43_456 10_656 ?
Y1 Y1 Y1 90.001(1) 46_465 10_656 ?
Y1 O1H Y1 114.8(3) . 10_656 ?
Y1 O1H Y1 114.9(3) . 7_665 ?
Y1 O1H Y1 114.8(3) 10_656 7_665 ?
Y1 O1H H1H 103.3 . . ?
Y1 O1H H1H 103.3 10_656 . ?
Y1 O1H H1H 103.3 7_665 . ?
Y1 O2H Y1 114.6(4) . 46_465 ?
Y1 O2H Y1 111.9(4) . 43_456 ?
Y1 O2H Y1 114.3(4) 46_465 43_456 ?
Y1 O2H H2H 104.9 . . ?
Y1 O2H H2H 104.9 46_465 . ?
Y1 O2H H2H 104.9 43_456 . ?
C1A O1A Y1 138.4(12) . . ?
C1A O2A Y1 132.0(13) . 7_665 ?
O2A C1A O1A 129.1(17) . . ?
O2A C1A C2A 118.1(16) . . ?
O1A C1A C2A 112.1(17) . . ?
O2A C1A C4A 115.6(16) . 27_565 ?
O1A C1A C4A 115.3(16) . 27_565 ?
C2A C1A C4A 11(2) . 27_565 ?
C4A C2A C7A 89(8) 27_565 . ?
C4A C2A C3A 79(5) 27_565 . ?
C7A C2A C3A 119(3) . . ?
C4A C2A C5A 73(7) 27_565 27_565 ?
C7A C2A C5A 16(2) . 27_565 ?
C3A C2A C5A 117(2) . 27_565 ?
C4A C2A C1A 95(10) 27_565 . ?
C7A C2A C1A 121(2) . . ?
C3A C2A C1A 118.5(18) . . ?
C5A C2A C1A 119(2) 27_565 . ?
C4A C3A C4A 115(3) . 27_565 ?
C4A C3A C2A 12(3) . 27_565 ?
C4A C3A C2A 119(2) 27_565 27_565 ?
C4A C3A C2A 119(2) . . ?
C4A C3A C2A 12(3) 27_565 . ?
C2A C3A C2A 120(3) 27_565 . ?
C4A C3A H3A 121.6(17) . . ?
C4A C3A H3A 121.6(17) 27_565 . ?
C2A C3A H3A 119.2(14) 27_565 . ?
C2A C3A H3A 119.2(14) . . ?
C3A C4A C5A 123(3) . . ?
C3A C4A C7A 120(3) . 27_565 ?
C5A C4A C7A 16(2) . 27_565 ?
C3A C4A C1A 116.6(19) . 27_565 ?
C5A C4A C1A 119(2) . 27_565 ?
C7A C4A C1A 116(2) 27_565 27_565 ?
C4A C5A C6A 117(3) . . ?
C4A C5A H5A 121.5 . . ?
C6A C5A H5A 121.5 . . ?
C5A C6A C5A 120(3) 27_565 . ?
C5A C6A C7A 16(2) 27_565 . ?
C5A C6A C7A 121(2) . . ?
C5A C6A C7A 121(2) 27_565 27_565 ?
C5A C6A C7A 16(2) . 27_565 ?
C7A C6A C7A 117(3) . 27_565 ?
C5A C6A C6A 119.4(16) 27_565 26_556 ?
C5A C6A C6A 119.4(16) . 26_556 ?
C7A C6A C6A 119.3(16) . 26_556 ?
C7A C6A C6A 119.3(16) 27_565 26_556 ?
C2A C7A C6A 119(3) . . ?
C2A C7A H7A 120.4 . . ?
C6A C7A H7A 120.4 . . ?
C1B O1B Y1 140.4(12) . . ?
C1B O2B Y1 131.5(13) . 46_465 ?
O2B C1B O1B 126.2(17) . . ?
O2B C1B C4B 118.1(16) . 27_565 ?
O1B C1B C4B 115.2(15) . 27_565 ?
O2B C1B C2B 119.0(16) . . ?
O1B C1B C2B 114.7(15) . . ?
C4B C1B C2B 11(2) 27_565 . ?
C4B C2B C3B 85(4) 27_565 . ?
C4B C2B C7B 91(7) 27_565 . ?
C3B C2B C7B 118(3) . . ?
C4B C2B C5B 75(7) 27_565 27_565 ?
C3B C2B C5B 113(3) . 27_565 ?
C7B C2B C5B 16(3) . 27_565 ?
C4B C2B C1B 82(9) 27_565 . ?
C3B C2B C1B 119.9(19) . . ?
C7B C2B C1B 121(2) . . ?
C5B C2B C1B 120(2) 27_565 . ?
C2B C3B C2B 121(3) 27_565 . ?
C2B C3B C4B 12(3) 27_565 . ?
C2B C3B C4B 123(3) . . ?
C2B C3B C4B 123(3) 27_565 27_565 ?
C2B C3B C4B 12(3) . 27_565 ?
C4B C3B C4B 122(3) . 27_565 ?
C2B C3B H3B 118.8(16) 27_565 . ?
C2B C3B H3B 118.8(16) . . ?
C4B C3B H3B 118.3(15) . . ?
C4B C3B H3B 118.3(15) 27_565 . ?
C3B C4B C5B 116(3) . . ?
C3B C4B C7B 115(3) . 27_565 ?
C5B C4B C7B 16(3) . 27_565 ?
C3B C4B C1B 120.3(19) . 27_565 ?
C5B C4B C1B 124(2) . 27_565 ?
C7B C4B C1B 119(2) 27_565 27_565 ?
C6B C5B C4B 125(4) . . ?
C6B C5B H5B 117.3 . . ?
C4B C5B H5B 117.3 . . ?
C5B C6B C5B 110(4) 27_565 . ?
C5B C6B C7B 16(3) 27_565 . ?
C5B C6B C7B 114(3) . . ?
C5B C6B C7B 114(3) 27_565 27_565 ?
C5B C6B C7B 16(3) . 27_565 ?
C7B C6B C7B 114(4) . 27_565 ?
C5B C6B C6B 123(2) 27_565 2_565 ?
C5B C6B C6B 123(2) . 2_565 ?
C7B C6B C6B 122.4(19) . 2_565 ?
C7B C6B C6B 122.4(19) 27_565 2_565 ?
C2B C7B C6B 123(3) . . ?
C2B C7B H7B 118.6 . . ?
C6B C7B H7B 118.6 . . ?
C1D N1D C2D 123(6) . . ?
C1D N1D C3D 122(6) . . ?
C2D N1D C3D 115(8) . . ?
O1D C1D N1D 126(3) . 10_656 ?
O1D C1D N1D 126(3) . . ?
N1D C1D N1D 89(4) 10_656 . ?
O1D C1D N1D 126(3) . 7_665 ?
N1D C1D N1D 89(4) 10_656 7_665 ?
N1D C1D N1D 89(4) . 7_665 ?
O1D C1D H1D 117(5) . . ?
N1D C1D H1D 51(2) 10_656 . ?
N1D C1D H1D 117(6) . . ?
N1D C1D H1D 51(2) 7_665 . ?
N1D C2D H2DA 109.5 . . ?
N1D C2D H2DB 109.5 . . ?
H2DA C2D H2DB 109.5 . . ?
N1D C2D H2DC 109.5 . . ?
H2DA C2D H2DC 109.5 . . ?
H2DB C2D H2DC 109.5 . . ?
N1D C3D H3DA 109.5 . . ?
N1D C3D H3DB 109.5 . . ?
H3DA C3D H3DB 109.5 . . ?
N1D C3D H3DC 109.5 . . ?
H3DA C3D H3DC 109.5 . . ?
H3DB C3D H3DC 109.5 . . ?
C1AA N1AA C2AA 109(10) . . ?
C1AA N1AA H1AG 109.9 . . ?
C2AA N1AA H1AG 109.9 . . ?
C1AA N1AA H1AF 109.9 . . ?
C2AA N1AA H1AF 109.9 . . ?
H1AG N1AA H1AF 108.3 . . ?
N1AA C1AA C2AA 140(9) . 35_655 ?
N1AA C1AA C2AA 140(9) . 33_666 ?
C2AA C1AA C2AA 71(10) 35_655 33_666 ?
N1AA C1AA H1AJ 109.5 . . ?
C2AA C1AA H1AJ 89.8 35_655 . ?
C2AA C1AA H1AJ 89.8 33_666 . ?
N1AA C1AA H1AI 109.5 . . ?
C2AA C1AA H1AI 31.1 35_655 . ?
C2AA C1AA H1AI 95.2 33_666 . ?
H1AJ C1AA H1AI 109.5 . . ?
N1AA C1AA H1AH 109.5 . . ?
C2AA C1AA H1AH 95.2 35_655 . ?
C2AA C1AA H1AH 31.1 33_666 . ?
H1AJ C1AA H1AH 109.5 . . ?
H1AI C1AA H1AH 109.5 . . ?
N1AA C2AA H2AF 109.5 . . ?
N1AA C2AA H2AD 109.5 . . ?
H2AF C2AA H2AD 109.5 . . ?
N1AA C2AA H2AE 109.5 . . ?
H2AF C2AA H2AE 109.5 . . ?
H2AD C2AA H2AE 109.5 . . ?
C2AB N1AB C1AB 116(7) . . ?
C2AB N1AB H1AB 108.3 . . ?
C1AB N1AB H1AB 108.3 . . ?
C2AB N1AB H1AA 108.3 . . ?
C1AB N1AB H1AA 108.3 . . ?
H1AB N1AB H1AA 107.4 . . ?
N1AB C1AB H1AE 109.5 . . ?
N1AB C1AB H1AC 109.5 . . ?
H1AE C1AB H1AC 109.5 . . ?
N1AB C1AB H1AD 109.5 . . ?
H1AE C1AB H1AD 109.5 . . ?
H1AC C1AB H1AD 109.5 . . ?
N1AB C2AB H2AC 109.5 . . ?
N1AB C2AB H2AB 109.5 . . ?
H2AC C2AB H2AB 109.5 . . ?
N1AB C2AB H2AA 109.5 . . ?
H2AC C2AB H2AA 109.5 . . ?
H2AB C2AB H2AA 109.5 . . ?

_refine_diff_density_max         5.807
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.384

# start Validation Reply Form
_vrf_PLAT043_kme_999             
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      49.11 Check 
RESPONSE: It was not possible to localize H atoms of water molecules
 as well as whole water molecules in the cavities but the reported formula
 includes them.
;
_vrf_PLAT094_kme_999             
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.53 Report
RESPONSE: There is Fourier series termination error: this large peak is
 located close to Y1 - the heaviest atom in the structure.
;
_vrf_PLAT097_kme_999             
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       5.81 eA-3  
RESPONSE: This is an artefact: Fourier series termination error. This peak
 is located 1.00 A from Y1 - the heaviest atom in the structure.
;
_vrf_PLAT341_kme_999             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.035 Ang.  
RESPONSE: It is due to strongly disorderd dimethylammonium cations and
 DMF molecules.
;
_vrf_PLAT420_kme_999             
;
PROBLEM: D-H Without Acceptor       O2H    --  H2H    ...     Please Check 
RESPONSE: There is no electron density for an acceptor.
;
_vrf_CHEMW03_kme_999             
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: It was not possible to localize H atoms of water molecules
 as well as whole water molecules in the cavities but the reported formula
 includes them.
;
_vrf_DIFMX02_kme_999             
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: It was not possible to localize H atoms of water molecules
 as well as whole water molecules in the cavities but the reported formula
 includes them.
;
_vrf_THETM01_kme_999             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
RESPONSE: The data were collected up to resolution 0.84 A-1
 using Cu Ka radiation.
;
_vrf_PLAT041_kme_999             
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: It was not possible to localize H atoms of water molecules
 as well as whole water molecules in the cavities but the reported formula
 includes them.
;
_vrf_PLAT068_kme_999             
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: It was not possible to localize H atoms of water molecules
 as well as whole water molecules in the cavities but the reported formula
 includes them.
;
_vrf_PLAT082_struct1             
;
PROBLEM: High R1 Value ..................................       0.13 Report
RESPONSE: Poor crystal quality: twinning and significant disorder
 in the structure.
;
_vrf_PLAT084_kme_999             
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.33 Report
RESPONSE: Poor crystal quality: twinning and significant disorder
 in the structure.
;
_vrf_PLAT601_kme_999             
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .         47 Ang3  
RESPONSE: Each of the  voids contains about 4 electrons which corresponding to
 a half of water molecule (SQUEEZE usually underestimates the electron
 density a bit). The reported formula includes them.
;
# end Validation Reply Form







####################################################################### 
# 
# 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_kme_726b
_database_code_depnum_ccdc_archive 'CCDC 1843059'
_audit_update_record             
;
2018-05-13 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;
_audit_creation_date             2015-04-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C2 H8 N),(Tb6 (O H)8 (C16 H6 N2 O8)3 (C3 H7 N O)1.5 (H2 O)1.5), 1.75(H2 O)'
_chemical_formula_sum            'C56.50 H59 N9.50 O36.75 Tb6'
_chemical_formula_weight         2412.59
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 '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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   18.232(1)
_cell_length_b                   18.232(1)
_cell_length_c                   45.607(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13130(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      69.92
_cell_measurement_theta_min      3.40
_shelx_estimated_absorpt_T_max   0.795
_shelx_estimated_absorpt_T_min   0.326
_exptl_absorpt_coefficient_mu    24.043
_exptl_absorpt_correction_T_max  0.753288
_exptl_absorpt_correction_T_min  0.621737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0663 before and 0.0408 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0727 before and 0.0411 after correction.
 The Ratio of minimum to maximum transmission is 0.83.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 32025 reflections, Rint = 0.0490
 (18318 with I > 3sig(I), Rint = 0.0421)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             6891
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5090
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.260
_diffrn_reflns_theta_min         3.404
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2425
_reflns_number_total             2744
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2744
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0433
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0561P)²+280.1767P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1187
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-C16
 1.23 with sigma of 0.02
 N10-C16
 1.32 with sigma of 0.02
 N10-C18 = N10-C17
 1.45 with sigma of 0.02
 N11-C20 = N11-C19
 1.47 with sigma of 0.02
 N10-O9
 2.26 with sigma of 0.04
 C16-C17
 2.41 with sigma of 0.04
 C16-C18
 2.41 with sigma of 0.04
 C18-C17
 2.47 with sigma of 0.04
 C19-C20
 2.48 with sigma of 0.04
3. Restrained planarity
 O9, C16, N10, C17, C18
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O9 \\sim C16 \\sim N10 \\sim C17 \\sim C18: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C21 \\sim N12: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N12 \\sim C21: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Fixed Sof: O9(0.5) C19(0.25) H19A(0.25) H19B(0.25) H19C(0.25) N11(0.25)
 H11A(0.25) H11B(0.25) N10(0.25) C16(0.25) H16(0.25) C18(0.25) H18A(0.25)
 H18B(0.25) H18C(0.25) C17(0.25) H17A(0.25) H17B(0.25) H17C(0.25) C21(0.166)
 H21A(0.166) H21B(0.166) H21C(0.166) O12(0.25) C20(0.25) H20A(0.25) H20B(0.25)
 H20C(0.25) O14(0.04167) N12(0.083) H12A(0.083) H12B(0.083)
6.a Riding coordinates:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
6.b Ternary CH refined with riding coordinates:
 O3(H3), O4(H4)
6.c Secondary CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B)
6.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C11(H11), C10(H10), C16(H16)
6.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_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_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
Tb1 Tb 0.87831(2) 0.87361(2) 0.53552(2) 0.01509(16) Uani 1 1 d . . . . .
O3 O 1.0000 1.0000 0.54818(13) 0.0094(13) Uani 1 3 d S T P . .
H3 H 1.0000 1.0000 0.5701 0.011 Uiso 1 3 calc RS T P . .
O4 O 1.0038(2) 0.8894(3) 0.51580(8) 0.0101(8) Uani 1 1 d . . . . .
H4 H 1.0058 0.8387 0.5230 0.012 Uiso 1 1 calc R . . . .
O0AA O 0.7436(3) 0.4984(3) 0.40821(8) 0.0218(10) Uani 1 1 d . . . . .
O6 O 0.6021(3) 0.4357(3) 0.40747(9) 0.0233(10) Uani 1 1 d . . . . .
O7 O 0.9027(3) 0.7378(3) 0.47734(9) 0.0215(9) Uani 1 1 d . . . . .
O8 O 0.8356(3) 0.7389(3) 0.51878(9) 0.0252(10) Uani 1 1 d . . . . .
C8 C 0.6744(4) 0.4845(4) 0.41809(13) 0.0210(14) Uani 1 1 d . . . . .
C13 C 0.8385(4) 0.7104(4) 0.49355(14) 0.0245(14) Uani 1 1 d . . . . .
C9 C 0.6774(5) 0.5311(5) 0.44618(15) 0.0318(17) Uani 1 1 d . . . . .
C14 C 0.7573(5) 0.6374(5) 0.48282(16) 0.0338(18) Uani 1 1 d . . . . .
C15 C 0.6836(6) 0.6125(7) 0.4983(2) 0.058(3) Uani 1 1 d . . . . .
H15 H 0.6853 0.6398 0.5162 0.070 Uiso 1 1 calc R . . . .
C12 C 0.6067(6) 0.5477(8) 0.4878(2) 0.069(4) Uani 1 1 d . . . . .
N9 N 0.5349(5) 0.5269(7) 0.50543(19) 0.080(4) Uani 1 1 d . . . . .
C11 C 0.7533(5) 0.5955(5) 0.45651(15) 0.0290(16) Uani 1 1 d . . . . .
H11 H 0.8037 0.6118 0.4457 0.035 Uiso 1 1 calc R . . . .
C10 C 0.6045(5) 0.5064(6) 0.46144(18) 0.048(3) Uani 1 1 d . . . . .
H10 H 0.5524 0.4614 0.4543 0.057 Uiso 1 1 calc R . . . .
O9 O 0.7622(9) 0.7534(8) 0.5685(3) 0.051(3) Uani 0.5 1 d D U . . .
C19 C 0.6667 0.3333 0.4655(5) 0.063(6) Uiso 0.75 3 d DS T P . .
H19A H 0.7229 0.3811 0.4671 0.095 Uiso 0.25 1 d R . . A -1
H19B H 0.6666 0.2934 0.4517 0.095 Uiso 0.25 1 d R . . A -1
H19C H 0.6288 0.3521 0.4588 0.095 Uiso 0.25 1 d R . . A -1
N11 N 0.639(3) 0.292(3) 0.4943(7) 0.098(15) Uiso 0.25 1 d D . . B -1
H11A H 0.6392 0.3302 0.5070 0.117 Uiso 0.25 1 calc R . . B -1
H11B H 0.5847 0.2491 0.4925 0.117 Uiso 0.25 1 calc R . . B -1
N10 N 0.665(2) 0.6225(17) 0.5808(8) 0.076(9) Uiso 0.25 1 d D U . C -1
C16 C 0.745(2) 0.6803(15) 0.5758(7) 0.066(10) Uiso 0.25 1 d D U . C -1
H16 H 0.7890 0.6665 0.5777 0.079 Uiso 0.25 1 calc R . . C -1
C18 C 0.608(3) 0.658(4) 0.5765(15) 0.12(2) Uiso 0.25 1 d D U . C -1
H18A H 0.5659 0.6244 0.5907 0.184 Uiso 0.25 1 d R . . C -1
H18B H 0.5840 0.6450 0.5572 0.184 Uiso 0.25 1 d R . . C -1
H18C H 0.6303 0.7170 0.5805 0.184 Uiso 0.25 1 d R . . C -1
C17 C 0.625(4) 0.535(2) 0.5892(14) 0.17(4) Uiso 0.25 1 d D U . C -1
H17A H 0.5705 0.4936 0.5820 0.261 Uiso 0.25 1 d R . . C -1
H17B H 0.6251 0.5329 0.6103 0.261 Uiso 0.25 1 d R . . C -1
H17C H 0.6676 0.5242 0.5816 0.261 Uiso 0.25 1 d R . . C -1
C21 C 0.913(3) 0.624(3) 0.5578(9) 0.030(9) Uiso 0.166 1 d . U . . .
H21A H 0.9681 0.6423 0.5490 0.044 Uiso 0.166 1 calc GR . . . .
H21B H 0.9108 0.6742 0.5649 0.044 Uiso 0.166 1 calc GR . . . .
H21C H 0.8683 0.5951 0.5430 0.044 Uiso 0.166 1 calc GR . . . .
O12 O 0.584(5) 0.498(5) 0.5763(16) 0.17(3) Uiso 0.25 1 d . . . D -2
C20 C 0.687(4) 0.256(4) 0.5080(11) 0.091(17) Uiso 0.25 1 d D . . B -1
H20A H 0.6750 0.2038 0.4979 0.137 Uiso 0.25 1 calc GR . . B -1
H20B H 0.6714 0.2440 0.5287 0.137 Uiso 0.25 1 calc GR . . B -1
H20C H 0.7482 0.2971 0.5066 0.137 Uiso 0.25 1 calc GR . . B -1
O14 O 0.6667 0.3333 0.5833 0.13(4) Uiso 0.25 6 d S T P . .
N12 N 0.898(7) 0.565(7) 0.5833 0.11(3) Uiso 0.166 2 d S TU P . .
H12A H 0.8875 0.5149 0.5750 0.127 Uiso 0.083 1 calc R . . . .
H12B H 0.8482 0.5542 0.5916 0.127 Uiso 0.083 1 calc R . . . .


_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
Tb1 Tb1 3.9191(7) 3_675 ?
Tb1 Tb1 3.9191(7) 2_765 ?
Tb1 Tb1 3.9516(6) 21_656 ?
Tb1 O3 2.3352(16) . ?
Tb1 O4 2.350(4) 20_566 ?
Tb1 O4 2.338(4) . ?
Tb1 O4 2.350(4) 3_675 ?
Tb1 O0AA 2.318(4) 36_665 ?
Tb1 O6 2.346(4) 35 ?
Tb1 O7 2.367(4) 20_566 ?
Tb1 O8 2.304(5) . ?
Tb1 O9 2.628(12) . ?
O3 Tb1 2.3352(16) 3_675 ?
O3 Tb1 2.3352(16) 2_765 ?
O3 H3 1.0000 . ?
O4 Tb1 2.350(4) 21_656 ?
O4 Tb1 2.350(4) 2_765 ?
O4 H4 1.0000 . ?
O0AA Tb1 2.318(4) 30_665 ?
O0AA C8 1.242(8) . ?
O6 Tb1 2.346(4) 29_455 ?
O6 C8 1.262(9) . ?
O7 Tb1 2.367(4) 21_656 ?
O7 C13 1.257(8) . ?
O8 C13 1.274(8) . ?
C8 C9 1.523(9) . ?
C13 C14 1.495(10) . ?
C9 C11 1.374(11) . ?
C9 C10 1.362(11) . ?
C14 C15 1.379(12) . ?
C14 C11 1.405(10) . ?
C15 H15 0.9500 . ?
C15 C12 1.390(13) . ?
C12 N9 1.417(11) . ?
C12 C10 1.409(11) . ?
N9 N9 1.255(15) 19_666 ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
O9 C16 1.255(19) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9602 . ?
C19 H19C 0.9600 . ?
C19 N11 1.473(19) . ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 C20 1.47(2) . ?
N10 C16 1.334(18) . ?
N10 C18 1.471(19) . ?
N10 C17 1.432(18) . ?
C16 H16 0.9500 . ?
C18 H18A 0.9608 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9598 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9602 . ?
C17 H17C 0.9594 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 N12 1.53(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N12 C21 1.53(7) 18_545 ?
N12 H12A 0.9100 . ?
N12 H12B 0.9100 . ?

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
Tb1 Tb1 Tb1 60.273(6) 2_765 21_656 ?
Tb1 Tb1 Tb1 90.0 3_675 21_656 ?
Tb1 Tb1 Tb1 60.0 2_765 3_675 ?
O3 Tb1 Tb1 32.95(6) . 3_675 ?
O3 Tb1 Tb1 85.72(13) . 21_656 ?
O3 Tb1 Tb1 32.95(6) . 2_765 ?
O3 Tb1 O4 65.30(12) . 3_675 ?
O3 Tb1 O4 99.16(18) . 20_566 ?
O3 Tb1 O4 65.48(12) . . ?
O3 Tb1 O6 76.89(16) . 35 ?
O3 Tb1 O7 135.04(12) . 20_566 ?
O3 Tb1 O9 130.8(3) . . ?
O4 Tb1 Tb1 32.65(9) . 21_656 ?
O4 Tb1 Tb1 33.20(9) 3_675 3_675 ?
O4 Tb1 Tb1 33.38(9) . 2_765 ?
O4 Tb1 Tb1 85.46(10) 20_566 3_675 ?
O4 Tb1 Tb1 32.77(9) 20_566 21_656 ?
O4 Tb1 Tb1 84.87(10) 3_675 21_656 ?
O4 Tb1 Tb1 85.62(10) 20_566 2_765 ?
O4 Tb1 Tb1 85.60(10) . 3_675 ?
O4 Tb1 Tb1 85.46(10) 3_675 2_765 ?
O4 Tb1 O4 64.49(13) 3_675 20_566 ?
O4 Tb1 O4 98.6(2) . 3_675 ?
O4 Tb1 O4 64.66(13) . 20_566 ?
O4 Tb1 O6 76.49(15) . 35 ?
O4 Tb1 O7 142.07(14) . 20_566 ?
O4 Tb1 O7 74.08(15) 3_675 20_566 ?
O4 Tb1 O7 79.12(15) 20_566 20_566 ?
O4 Tb1 O9 130.0(3) 20_566 . ?
O4 Tb1 O9 130.8(3) . . ?
O4 Tb1 O9 130.6(3) 3_675 . ?
O0AA Tb1 Tb1 159.24(12) 36_665 21_656 ?
O0AA Tb1 Tb1 69.25(12) 36_665 3_675 ?
O0AA Tb1 Tb1 106.06(11) 36_665 2_765 ?
O0AA Tb1 O3 76.42(16) 36_665 . ?
O0AA Tb1 O4 139.96(15) 36_665 20_566 ?
O0AA Tb1 O4 138.82(15) 36_665 . ?
O0AA Tb1 O4 78.15(15) 36_665 3_675 ?
O0AA Tb1 O6 80.35(17) 36_665 35 ?
O0AA Tb1 O7 77.20(16) 36_665 20_566 ?
O0AA Tb1 O9 65.9(3) 36_665 . ?
O6 Tb1 Tb1 106.05(11) 35 21_656 ?
O6 Tb1 Tb1 107.03(12) 35 3_675 ?
O6 Tb1 Tb1 68.51(12) 35 2_765 ?
O6 Tb1 O4 138.23(15) 35 20_566 ?
O6 Tb1 O4 139.83(15) 35 3_675 ?
O6 Tb1 O7 132.64(16) 35 20_566 ?
O6 Tb1 O9 66.9(3) 35 . ?
O7 Tb1 Tb1 103.09(11) 20_566 3_675 ?
O7 Tb1 Tb1 109.65(11) 20_566 21_656 ?
O7 Tb1 Tb1 158.28(11) 20_566 2_765 ?
O7 Tb1 O9 66.0(3) 20_566 . ?
O8 Tb1 Tb1 158.29(12) . 3_675 ?
O8 Tb1 Tb1 68.54(12) . 21_656 ?
O8 Tb1 Tb1 108.78(13) . 2_765 ?
O8 Tb1 O3 141.42(13) . . ?
O8 Tb1 O4 74.73(15) . 20_566 ?
O8 Tb1 O4 78.02(16) . . ?
O8 Tb1 O4 135.66(14) . 3_675 ?
O8 Tb1 O0AA 132.22(17) . 36_665 ?
O8 Tb1 O6 83.06(17) . 35 ?
O8 Tb1 O7 82.11(17) . 20_566 ?
O8 Tb1 O9 66.3(3) . . ?
O9 Tb1 Tb1 135.4(3) . 2_765 ?
O9 Tb1 Tb1 135.2(3) . 3_675 ?
O9 Tb1 Tb1 134.8(3) . 21_656 ?
Tb1 O3 Tb1 114.10(11) 2_765 3_675 ?
Tb1 O3 Tb1 114.10(11) 2_765 . ?
Tb1 O3 Tb1 114.10(11) 3_675 . ?
Tb1 O3 H3 104.3 2_765 . ?
Tb1 O3 H3 104.3 3_675 . ?
Tb1 O3 H3 104.3 . . ?
Tb1 O4 Tb1 113.43(15) . 2_765 ?
Tb1 O4 Tb1 114.87(15) . 21_656 ?
Tb1 O4 Tb1 114.45(16) 2_765 21_656 ?
Tb1 O4 H4 104.1 . . ?
Tb1 O4 H4 104.1 2_765 . ?
Tb1 O4 H4 104.1 21_656 . ?
C8 O0AA Tb1 137.8(4) . 30_665 ?
C8 O6 Tb1 137.2(4) . 29_455 ?
C13 O7 Tb1 130.3(4) . 21_656 ?
C13 O8 Tb1 132.3(4) . . ?
O0AA C8 O6 127.0(6) . . ?
O0AA C8 C9 116.2(6) . . ?
O6 C8 C9 116.8(6) . . ?
O7 C13 O8 126.1(6) . . ?
O7 C13 C14 118.2(6) . . ?
O8 C13 C14 115.7(6) . . ?
C11 C9 C8 120.3(6) . . ?
C10 C9 C8 119.2(7) . . ?
C10 C9 C11 120.4(7) . . ?
C15 C14 C13 119.6(7) . . ?
C15 C14 C11 118.8(7) . . ?
C11 C14 C13 121.5(7) . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C12 120.4(7) . . ?
C12 C15 H15 119.8 . . ?
C15 C12 N9 115.9(7) . . ?
C15 C12 C10 119.6(8) . . ?
C10 C12 N9 124.5(8) . . ?
N9 N9 C12 115.1(9) 19_666 . ?
C9 C11 C14 120.9(7) . . ?
C9 C11 H11 119.6 . . ?
C14 C11 H11 119.6 . . ?
C9 C10 C12 119.8(8) . . ?
C9 C10 H10 120.1 . . ?
C12 C10 H10 120.1 . . ?
C16 O9 Tb1 134.8(18) . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N11 C19 H19A 109.4 . . ?
N11 C19 H19B 108.7 . . ?
N11 C19 H19C 110.4 . . ?
C19 N11 H11A 107.6 . . ?
C19 N11 H11B 107.6 . . ?
H11A N11 H11B 107.0 . . ?
C20 N11 C19 119(3) . . ?
C20 N11 H11A 107.6 . . ?
C20 N11 H11B 107.6 . . ?
C16 N10 C18 112(2) . . ?
C16 N10 C17 132(3) . . ?
C17 N10 C18 117(3) . . ?
O9 C16 N10 118(3) . . ?
O9 C16 H16 121.0 . . ?
N10 C16 H16 121.0 . . ?
N10 C18 H18A 98.5 . . ?
N10 C18 H18B 110.7 . . ?
N10 C18 H18C 118.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.4 . . ?
N10 C17 H17A 122.2 . . ?
N10 C17 H17B 108.0 . . ?
N10 C17 H17C 97.3 . . ?
H17A C17 H17B 109.4 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.4 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N12 C21 H21A 109.5 . . ?
N12 C21 H21B 109.5 . . ?
N12 C21 H21C 109.5 . . ?
N11 C20 H20A 109.5 . . ?
N11 C20 H20B 109.5 . . ?
N11 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 N12 C21 127(9) . 18_545 ?
C21 N12 H12A 105.5 . . ?
C21 N12 H12A 105.5 18_545 . ?
C21 N12 H12B 105.5 18_545 . ?
C21 N12 H12B 105.5 . . ?
H12A N12 H12B 106.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O0AA C8 O6 -0.1(11) 30_665 . . . ?
Tb1 O0AA C8 C9 179.4(5) 30_665 . . . ?
Tb1 O6 C8 O0AA 5.2(11) 29_455 . . . ?
Tb1 O6 C8 C9 -174.2(5) 29_455 . . . ?
Tb1 O7 C13 O8 -46.0(10) 21_656 . . . ?
Tb1 O7 C13 C14 134.4(6) 21_656 . . . ?
Tb1 O8 C13 O7 51.0(10) . . . . ?
Tb1 O8 C13 C14 -129.3(6) . . . . ?
Tb1 O9 C16 N10 -149(2) . . . . ?
O0AA C8 C9 C11 11.2(11) . . . . ?
O0AA C8 C9 C10 -166.6(8) . . . . ?
O6 C8 C9 C11 -169.2(7) . . . . ?
O6 C8 C9 C10 12.9(12) . . . . ?
O7 C13 C14 C15 -172.1(9) . . . . ?
O7 C13 C14 C11 5.1(12) . . . . ?
O8 C13 C14 C15 8.2(13) . . . . ?
O8 C13 C14 C11 -174.6(7) . . . . ?
C8 C9 C11 C14 -178.2(8) . . . . ?
C8 C9 C10 C12 178.6(11) . . . . ?
C13 C14 C15 C12 176.5(11) . . . . ?
C13 C14 C11 C9 -176.8(8) . . . . ?
C14 C15 C12 N9 179.8(12) . . . . ?
C14 C15 C12 C10 1(2) . . . . ?
C15 C14 C11 C9 0.4(14) . . . . ?
C15 C12 N9 N9 174.5(17) . . . 19_666 ?
C15 C12 C10 C9 -1(2) . . . . ?
N9 C12 C10 C9 -179.7(13) . . . . ?
C11 C9 C10 C12 0.8(17) . . . . ?
C11 C14 C15 C12 -0.7(18) . . . . ?
C10 C9 C11 C14 -0.4(14) . . . . ?
C10 C12 N9 N9 -7(3) . . . 19_666 ?
C18 N10 C16 O9 0.0(3) . . . . ?
C17 N10 C16 O9 180.0(4) . . . . ?

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

# start Validation Reply Form
_vrf_PLAT220_kme_726b            
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        8.1 Ratio 
RESPONSE: This alert is caused by significant disorder of both disordered
 dimethylammonium cations and coordinated dimethylformamide molecule.
;
_vrf_PLAT420_kme_726b            
;
PROBLEM: D-H Without Acceptor       O3     --  H3     ...     Please Check 
RESPONSE: There are no electron density be assigned to an acceptor.
;
_vrf_PLAT041_kme_726b            
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: It was not possible to localize H atoms of water molecules but
 the reported formula includes them.
;
_vrf_PLAT043_kme_726b            
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      13.04 Check 
RESPONSE: It was not possible to localize H atoms of water molecules but
 the reported formula includes them.
;
_vrf_PLAT068_kme_726b            
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: It was not possible to localize H atoms of water molecules but
 the reported formula includes them.
;
_vrf_PLAT150_kme_726b            
;
PROBLEM: Volume as Calculated Differs from that Given ...   13130.00 Ang-3 
RESPONSE: False alert. It is due to the rounding error. The calculated value
 13129.0(19) A3 was rounded to 13130(2) A3.
;
_vrf_PLAT202_kme_726b            
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check 
RESPONSE: Stronlgly disordered DMF molecules, DMA cations and water molecules
 were refined isotropically.
;
_vrf_PLAT213_kme_726b            
;
PROBLEM: Atom N9              has ADP max/min Ratio .....        3.5 prolat
RESPONSE: This alert is caused by large thermal motions of flat ligand
 molecules towards the voids in the structure.
;
_vrf_PLAT222_kme_726b            
;
PROBLEM: Non-Solvent Resd 1   H Uiso(max)/Uiso(min) Range       10.0 Ratio 
RESPONSE: This alert is caused by significant disorder of disordered
 dimethylammonium cations and coordinated dimethylformamide molecule.
;
_vrf_PLAT250_kme_726b            
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.4 Note  
RESPONSE: This alert is caused by large thermal motions of flat ligand
 molecules towards the voids in the structure.
;
_vrf_PLAT342_kme_726b            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01288 Ang.  
RESPONSE: This alert is caused by significant disorder of disordered
 dimethylammonium cations and coordinated dimethylformamide molecule.
;
# end Validation Reply Form

