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

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

data_bkt20sq
_database_code_depnum_ccdc_archive 'CCDC 1422227'
_audit_update_record             
;
2015-09-03 deposited with the CCDC.
2015-11-09 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         'C52 H30 Gd2 N4 Na2 O21 Zn'
_chemical_formula_sum            'C52 H30 Gd2 N4 Na2 O21 Zn'
_chemical_formula_weight         1472.65

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'
Na Na 0.0362 0.0249 '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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

_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'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   27.6310(19)
_cell_length_b                   29.080(3)
_cell_length_c                   13.1360(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10554.9(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3101
_cell_measurement_theta_min      1.70
_cell_measurement_theta_max      25.10

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.927
_exptl_crystal_F_000             2872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.519
_shelx_estimated_absorpt_T_min   0.712
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS micro-focus'
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg/ φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_reflns_number            15176
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.701
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_full        25.101
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             4846
_reflns_number_gt                3101
_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.

 The structure contains a considerable amount of severely disordered
 solvent (DMF+water) which couldn't be resolved reliably by discrete
 atoms. The solvent contribution to the diffraction pattern was thus
 subtracted by the Squeeze technique, using the PLATON software
 (Spek, 2015).

 The 5-coordinate Zn in the porphyrin center is partly disordered
 with respect to the porphyrin plane. Some of the carboxylate
 residues also reveal rotational disorder. The disordered O-atoms
 were assigned isotropic ADPs only.
;

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          '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)+(0.0966P)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_number_reflns         4846
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0646
_refine_ls_wR_factor_ref         0.1959
_refine_ls_wR_factor_gt          0.1841
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.966
_refine_ls_shift/su_max          0.003
_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
Gd1 Gd 0.82260(2) 0.5000 0.5000 0.0361(2) Uani 1 2 d S T P . .
Zn1 Zn 0.5000 0.2500 0.4290(3) 0.0351(6) Uani 0.68 4 d S T P . .
Zn1' Zn 0.5000 0.2500 0.3659(6) 0.0454(17) Uani 0.32 4 d S T P . .
Na1 Na 0.7500 0.45819(14) 0.7500 0.0397(9) Uani 1 2 d S T P . .
O1 O 0.69711(18) 0.48711(17) 0.1832(4) 0.0371(12) Uiso 1 1 d . . . . .
O2 O 0.7678(3) 0.4449(3) 0.5252(6) 0.021(2) Uiso 0.5 1 d . . P . .
O2' O 0.7513(4) 0.5436(4) 0.4618(8) 0.037(3) Uiso 0.5 1 d . . P . .
O3 O 0.7111(2) 0.4145(2) 0.6351(5) 0.0642(17) Uiso 1 1 d . . . . .
O4 O 0.6403(3) 0.4447(3) 0.1192(7) 0.028(2) Uiso 0.5 1 d . . P . .
O4' O 0.6559(4) 0.4308(4) 0.1043(8) 0.037(3) Uiso 0.5 1 d . . P . .
O5 O 0.8784(3) 0.5478(3) 0.4049(6) 0.111(3) Uiso 1 1 d . . . . .
H5A H 0.8680 0.5767 0.3788 0.133 Uiso 1 1 calc R U . . .
H5B H 0.9107 0.5378 0.3937 0.133 Uiso 1 1 calc R U . . .
O6 O 0.5000 0.2500 0.6023(19) 0.121(9) Uiso 0.68 4 d S . P . .
H6A H 0.5000 0.2783 0.6384 0.145 Uiso 0.34 2 calc R U P . .
H6B H 0.5000 0.2217 0.6384 0.145 Uiso 0.34 2 calc R U P . .
O6' O 0.5000 0.2500 0.203(4) 0.098(15) Uiso 0.32 4 d S . P . .
H6'1 H 0.5000 0.2217 0.1673 0.118 Uiso 0.16 2 calc R U P . .
H6'2 H 0.5000 0.2783 0.1673 0.118 Uiso 0.16 2 calc R U P . .
N1 N 0.5738(2) 0.2500 0.4060(5) 0.0221(16) Uani 1 2 d S T P . .
N2 N 0.5000 0.3191(3) 0.4008(5) 0.0277(17) Uani 1 2 d S T P . .
C1 C 0.6026(2) 0.2879(2) 0.4030(5) 0.0295(15) Uani 1 1 d . . . . .
C2 C 0.6648(2) 0.4282(2) 0.2870(5) 0.0316(16) Uani 1 1 d . . . . .
C3 C 0.6560(3) 0.3803(3) 0.4708(5) 0.0376(18) Uani 1 1 d . . . . .
H3 H 0.6522 0.3648 0.5340 0.045 Uiso 1 1 calc R U . . .
C4 C 0.6263(2) 0.3699(3) 0.3865(5) 0.0320(16) Uani 1 1 d . . . . .
C5 C 0.6530(2) 0.2731(2) 0.3969(5) 0.0357(17) Uani 1 1 d . . . . .
H5 H 0.6807 0.2925 0.3935 0.043 Uiso 1 1 calc R U . . .
C6 C 0.5874(2) 0.3334(2) 0.3971(5) 0.0279(15) Uani 1 1 d . . . . .
C7 C 0.6709(2) 0.4529(3) 0.1898(6) 0.0414(18) Uani 1 1 d . . . . .
C8 C 0.6312(2) 0.3940(2) 0.2979(4) 0.0316(16) Uani 1 1 d . . . . .
H8 H 0.6107 0.3868 0.2422 0.038 Uiso 1 1 calc R U . . .
C9 C 0.7230(3) 0.4274(3) 0.5472(5) 0.0417(19) Uani 1 1 d . . . . .
C10 C 0.5404(2) 0.3471(2) 0.3953(5) 0.0290(15) Uani 1 1 d . . . . .
C11 C 0.5236(2) 0.3952(2) 0.3951(6) 0.0435(19) Uani 1 1 d . . . . .
H11 H 0.5437 0.4216 0.3949 0.052 Uiso 1 1 calc R U . . .
C12 C 0.6961(2) 0.4372(2) 0.3683(5) 0.0295(15) Uani 1 1 d . . . . .
H12 H 0.7210 0.4594 0.3606 0.035 Uiso 1 1 calc R U . . .
C13 C 0.6915(2) 0.4145(2) 0.4576(5) 0.0333(16) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O2 2.229(9) 4_566 ?
Gd1 O2 2.229(9) . ?
Gd1 O2' 2.396(11) . ?
Gd1 O2' 2.396(11) 4_566 ?
Gd1 O5 2.424(8) 4_566 ?
Gd1 O5 2.424(8) . ?
Gd1 O4 2.467(9) 6_655 ?
Gd1 O4 2.467(9) 7_645 ?
Gd1 O1 2.495(5) 7_645 ?
Gd1 O1 2.495(5) 6_655 ?
Gd1 O4' 2.506(10) 6_655 ?
Gd1 O4' 2.506(10) 7_645 ?
Zn1 Zn1' 0.829(6) . ?
Zn1 N2 2.044(8) . ?
Zn1 N2 2.044(8) 2_655 ?
Zn1 N1 2.062(6) 2_655 ?
Zn1 N1 2.062(6) . ?
Zn1 O6 2.28(3) . ?
Zn1' N2 2.061(8) 2_655 ?
Zn1' N2 2.061(8) . ?
Zn1' N1 2.106(6) 2_655 ?
Zn1' N1 2.106(6) . ?
Zn1' O6' 2.13(5) . ?
Na1 O3 2.245(6) . ?
Na1 O3 2.246(6) 7_646 ?
Na1 O1 2.332(6) 6_655 ?
Na1 O1 2.332(6) 4_566 ?
Na1 O2' 2.783(11) 4_566 ?
Na1 O2' 2.783(11) 6_655 ?
Na1 C9 2.908(7) 7_646 ?
Na1 C9 2.908(7) . ?
Na1 O2 3.019(9) . ?
Na1 O2 3.019(9) 7_646 ?
Na1 Gd1 4.0357(12) 6_655 ?
O1 C7 1.233(8) . ?
O1 Na1 2.332(6) 6_654 ?
O1 Gd1 2.495(5) 6_654 ?
O2 O2' 0.591(12) 4_566 ?
O2 C9 1.371(11) . ?
O2' O2 0.591(12) 4_566 ?
O2' C9 1.157(12) 4_566 ?
O2' Na1 2.783(11) 6_654 ?
O3 C9 1.256(9) . ?
O4 O4' 0.622(12) . ?
O4 C7 1.278(11) . ?
O4 Gd1 2.467(9) 6_654 ?
O4' C7 1.359(12) . ?
O4' Gd1 2.505(10) 6_654 ?
O5 H5A 0.9500 . ?
O5 H5B 0.9500 . ?
O6 H6A 0.9500 . ?
O6 H6B 0.9500 . ?
O6' H6'1 0.9500 . ?
O6' H6'2 0.9500 . ?
N1 C1 1.360(7) 11_565 ?
N1 C1 1.360(7) . ?
N2 C10 1.382(7) 12_655 ?
N2 C10 1.382(7) . ?
C1 C6 1.390(9) . ?
C1 C5 1.462(8) . ?
C2 C8 1.366(9) . ?
C2 C12 1.400(9) . ?
C2 C7 1.475(10) . ?
C3 C13 1.406(10) . ?
C3 C4 1.411(9) . ?
C3 H3 0.9500 . ?
C4 C8 1.365(9) . ?
C4 C6 1.517(8) . ?
C5 C5 1.341(13) 11_565 ?
C5 H5 0.9500 . ?
C6 C10 1.359(8) . ?
C7 Gd1 2.850(8) 6_654 ?
C8 H8 0.9500 . ?
C9 O2' 1.157(12) 4_566 ?
C9 C13 1.512(10) . ?
C10 C11 1.473(9) . ?
C11 C11 1.303(13) 12_655 ?
C11 H11 0.9500 . ?
C12 C13 1.352(9) . ?
C12 H12 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Gd1 O2 94.5(5) 4_566 . ?
O2 Gd1 O2' 81.6(4) . . ?
O2 Gd1 O2' 81.6(4) 4_566 4_566 ?
O2' Gd1 O2' 69.4(6) . 4_566 ?
O2 Gd1 O5 157.1(3) 4_566 4_566 ?
O2 Gd1 O5 86.7(3) . 4_566 ?
O2' Gd1 O5 159.2(3) . 4_566 ?
O2' Gd1 O5 96.4(3) 4_566 4_566 ?
O2 Gd1 O5 86.7(3) 4_566 . ?
O2 Gd1 O5 157.1(3) . . ?
O2' Gd1 O5 96.4(3) . . ?
O2' Gd1 O5 159.2(3) 4_566 . ?
O5 Gd1 O5 101.0(4) 4_566 . ?
O2 Gd1 O4 84.7(4) 4_566 6_655 ?
O2 Gd1 O4 131.0(3) . 6_655 ?
O2' Gd1 O4 97.4(4) . 6_655 ?
O2' Gd1 O4 123.6(3) 4_566 6_655 ?
O5 Gd1 O4 77.4(3) 4_566 6_655 ?
O5 Gd1 O4 71.9(3) . 6_655 ?
O2 Gd1 O4 131.0(3) 4_566 7_645 ?
O2 Gd1 O4 84.7(4) . 7_645 ?
O2' Gd1 O4 123.6(3) . 7_645 ?
O2' Gd1 O4 97.4(4) 4_566 7_645 ?
O5 Gd1 O4 71.9(3) 4_566 7_645 ?
O5 Gd1 O4 77.4(3) . 7_645 ?
O4 Gd1 O4 130.9(5) 6_655 7_645 ?
O2 Gd1 O1 79.5(3) 4_566 7_645 ?
O2 Gd1 O1 83.5(2) . 7_645 ?
O2' Gd1 O1 72.4(3) . 7_645 ?
O2' Gd1 O1 86.7(3) 4_566 7_645 ?
O5 Gd1 O1 123.3(2) 4_566 7_645 ?
O5 Gd1 O1 74.2(2) . 7_645 ?
O4 Gd1 O1 143.2(2) 6_655 7_645 ?
O4 Gd1 O1 51.7(2) 7_645 7_645 ?
O2 Gd1 O1 83.5(2) 4_566 6_655 ?
O2 Gd1 O1 79.5(3) . 6_655 ?
O2' Gd1 O1 86.7(3) . 6_655 ?
O2' Gd1 O1 72.4(3) 4_566 6_655 ?
O5 Gd1 O1 74.2(2) 4_566 6_655 ?
O5 Gd1 O1 123.3(2) . 6_655 ?
O4 Gd1 O1 51.7(2) 6_655 6_655 ?
O4 Gd1 O1 143.2(2) 7_645 6_655 ?
O1 Gd1 O1 154.8(2) 7_645 6_655 ?
O2 Gd1 O4' 70.4(4) 4_566 6_655 ?
O2 Gd1 O4' 131.1(3) . 6_655 ?
O2' Gd1 O4' 83.4(4) . 6_655 ?
O2' Gd1 O4' 120.4(4) 4_566 6_655 ?
O5 Gd1 O4' 91.6(3) 4_566 6_655 ?
O5 Gd1 O4' 70.7(3) . 6_655 ?
O4 Gd1 O4' 14.3(3) 6_655 6_655 ?
O4 Gd1 O4' 140.5(4) 7_645 6_655 ?
O1 Gd1 O4' 134.4(3) 7_645 6_655 ?
O1 Gd1 O4' 53.4(3) 6_655 6_655 ?
O2 Gd1 O4' 131.1(3) 4_566 7_645 ?
O2 Gd1 O4' 70.4(4) . 7_645 ?
O2' Gd1 O4' 120.4(4) . 7_645 ?
O2' Gd1 O4' 83.4(4) 4_566 7_645 ?
O5 Gd1 O4' 70.7(3) 4_566 7_645 ?
O5 Gd1 O4' 91.6(3) . 7_645 ?
O4 Gd1 O4' 140.5(4) 6_655 7_645 ?
O4 Gd1 O4' 14.3(3) 7_645 7_645 ?
O1 Gd1 O4' 53.4(3) 7_645 7_645 ?
O1 Gd1 O4' 134.4(3) 6_655 7_645 ?
O4' Gd1 O4' 152.6(5) 6_655 7_645 ?
Zn1' Zn1 N2 79.5(2) . . ?
Zn1' Zn1 N2 79.5(2) . 2_655 ?
N2 Zn1 N2 159.1(4) . 2_655 ?
Zn1' Zn1 N1 81.6(2) . 2_655 ?
N2 Zn1 N1 88.48(5) . 2_655 ?
N2 Zn1 N1 88.48(5) 2_655 2_655 ?
Zn1' Zn1 N1 81.6(2) . . ?
N2 Zn1 N1 88.48(5) . . ?
N2 Zn1 N1 88.48(5) 2_655 . ?
N1 Zn1 N1 163.1(4) 2_655 . ?
Zn1' Zn1 O6 180.0 . . ?
N2 Zn1 O6 100.5(2) . . ?
N2 Zn1 O6 100.5(2) 2_655 . ?
N1 Zn1 O6 98.4(2) 2_655 . ?
N1 Zn1 O6 98.4(2) . . ?
Zn1 Zn1' N2 77.2(3) . 2_655 ?
Zn1 Zn1' N2 77.2(3) . . ?
N2 Zn1' N2 154.3(6) 2_655 . ?
Zn1 Zn1' N1 75.5(3) . 2_655 ?
N2 Zn1' N1 86.82(11) 2_655 2_655 ?
N2 Zn1' N1 86.82(11) . 2_655 ?
Zn1 Zn1' N1 75.5(3) . . ?
N2 Zn1' N1 86.82(11) 2_655 . ?
N2 Zn1' N1 86.82(11) . . ?
N1 Zn1' N1 151.0(5) 2_655 . ?
Zn1 Zn1' O6' 180.000(15) . . ?
N2 Zn1' O6' 102.8(3) 2_655 . ?
N2 Zn1' O6' 102.8(3) . . ?
N1 Zn1' O6' 104.5(3) 2_655 . ?
N1 Zn1' O6' 104.5(3) . . ?
O3 Na1 O3 111.2(4) . 7_646 ?
O3 Na1 O1 115.6(2) . 6_655 ?
O3 Na1 O1 109.8(2) 7_646 6_655 ?
O3 Na1 O1 109.8(2) . 4_566 ?
O3 Na1 O1 115.6(2) 7_646 4_566 ?
O1 Na1 O1 94.0(3) 6_655 4_566 ?
O3 Na1 O2' 47.4(3) . 4_566 ?
O3 Na1 O2' 130.9(3) 7_646 4_566 ?
O1 Na1 O2' 68.2(3) 6_655 4_566 ?
O1 Na1 O2' 113.4(3) 4_566 4_566 ?
O3 Na1 O2' 130.9(3) . 6_655 ?
O3 Na1 O2' 47.4(3) 7_646 6_655 ?
O1 Na1 O2' 113.4(3) 6_655 6_655 ?
O1 Na1 O2' 68.2(3) 4_566 6_655 ?
O2' Na1 O2' 177.8(5) 4_566 6_655 ?
O3 Na1 C9 124.3(3) . 7_646 ?
O3 Na1 C9 24.1(2) 7_646 7_646 ?
O1 Na1 C9 113.2(2) 6_655 7_646 ?
O1 Na1 C9 91.51(18) 4_566 7_646 ?
O2' Na1 C9 155.0(3) 4_566 7_646 ?
O2' Na1 C9 23.3(2) 6_655 7_646 ?
O3 Na1 C9 24.1(2) . . ?
O3 Na1 C9 124.3(3) 7_646 . ?
O1 Na1 C9 91.51(18) 6_655 . ?
O1 Na1 C9 113.2(2) 4_566 . ?
O2' Na1 C9 23.3(2) 4_566 . ?
O2' Na1 C9 155.0(3) 6_655 . ?
C9 Na1 C9 144.1(3) 7_646 . ?
O3 Na1 O2 49.3(2) . . ?
O3 Na1 O2 120.4(3) 7_646 . ?
O1 Na1 O2 67.5(2) 6_655 . ?
O1 Na1 O2 123.9(2) 4_566 . ?
O2' Na1 O2 10.7(3) 4_566 . ?
O2' Na1 O2 167.9(3) 6_655 . ?
C9 Na1 O2 144.5(2) 7_646 . ?
C9 Na1 O2 26.7(2) . . ?
O3 Na1 O2 120.4(3) . 7_646 ?
O3 Na1 O2 49.3(2) 7_646 7_646 ?
O1 Na1 O2 123.9(2) 6_655 7_646 ?
O1 Na1 O2 67.5(2) 4_566 7_646 ?
O2' Na1 O2 167.9(3) 4_566 7_646 ?
O2' Na1 O2 10.7(3) 6_655 7_646 ?
C9 Na1 O2 26.7(2) 7_646 7_646 ?
C9 Na1 O2 144.5(2) . 7_646 ?
O2 Na1 O2 165.2(4) . 7_646 ?
O3 Na1 Gd1 118.65(15) . 6_655 ?
O3 Na1 Gd1 82.02(15) 7_646 6_655 ?
O1 Na1 Gd1 114.35(16) 6_655 6_655 ?
O1 Na1 Gd1 34.57(12) 4_566 6_655 ?
O2' Na1 Gd1 145.7(3) 4_566 6_655 ?
O2' Na1 Gd1 35.5(2) 6_655 6_655 ?
C9 Na1 Gd1 58.34(13) 7_646 6_655 ?
C9 Na1 Gd1 135.28(15) . 6_655 ?
O2 Na1 Gd1 156.33(18) . 6_655 ?
O2 Na1 Gd1 33.02(17) 7_646 6_655 ?
O3 Na1 Gd1 82.02(15) . . ?
O3 Na1 Gd1 118.65(15) 7_646 . ?
O1 Na1 Gd1 34.57(12) 6_655 . ?
O1 Na1 Gd1 114.35(16) 4_566 . ?
O2' Na1 Gd1 35.5(2) 4_566 . ?
O2' Na1 Gd1 145.7(3) 6_655 . ?
C9 Na1 Gd1 135.28(15) 7_646 . ?
C9 Na1 Gd1 58.35(13) . . ?
O2 Na1 Gd1 33.02(17) . . ?
O2 Na1 Gd1 156.33(19) 7_646 . ?
Gd1 Na1 Gd1 144.93(11) 6_655 . ?
C7 O1 Na1 153.0(5) . 6_654 ?
C7 O1 Gd1 93.5(4) . 6_654 ?
Na1 O1 Gd1 113.4(2) 6_654 6_654 ?
O2' O2 C9 56.7(15) 4_566 . ?
O2' O2 Gd1 99.2(16) 4_566 . ?
C9 O2 Gd1 155.8(8) . . ?
O2' O2 Na1 61.2(15) 4_566 . ?
C9 O2 Na1 72.1(5) . . ?
Gd1 O2 Na1 99.4(3) . . ?
O2 O2' C9 98.0(18) 4_566 4_566 ?
O2 O2' Gd1 66.7(15) 4_566 . ?
C9 O2' Gd1 164.6(10) 4_566 . ?
O2 O2' Na1 108.1(16) 4_566 6_654 ?
C9 O2' Na1 84.4(7) 4_566 6_654 ?
Gd1 O2' Na1 102.1(4) . 6_654 ?
C9 O3 Na1 109.0(5) . . ?
O4' O4 C7 83.8(15) . . ?
O4' O4 Gd1 86.4(15) . 6_654 ?
C7 O4 Gd1 93.7(6) . 6_654 ?
O4 O4' C7 69.2(15) . . ?
O4 O4' Gd1 79.3(15) . 6_654 ?
C7 O4' Gd1 90.0(6) . 6_654 ?
Gd1 O5 H5A 120.0 . . ?
Gd1 O5 H5B 120.0 . . ?
H5A O5 H5B 120.0 . . ?
Zn1 O6 H6A 120.0 . . ?
Zn1 O6 H6B 120.0 . . ?
H6A O6 H6B 120.0 . . ?
Zn1' O6' H6'1 120.0 . . ?
Zn1' O6' H6'2 120.0 . . ?
H6'1 O6' H6'2 120.0 . . ?
C1 N1 C1 108.4(7) 11_565 . ?
C1 N1 Zn1 125.6(4) 11_565 . ?
C1 N1 Zn1 125.6(4) . . ?
C1 N1 Zn1' 124.0(4) 11_565 . ?
C1 N1 Zn1' 124.0(4) . . ?
C10 N2 C10 107.6(8) 12_655 . ?
C10 N2 Zn1 126.0(4) 12_655 . ?
C10 N2 Zn1 126.0(4) . . ?
C10 N2 Zn1' 124.2(4) 12_655 . ?
C10 N2 Zn1' 124.2(4) . . ?
N1 C1 C6 126.7(6) . . ?
N1 C1 C5 108.6(6) . . ?
C6 C1 C5 124.5(6) . . ?
C8 C2 C12 118.4(6) . . ?
C8 C2 C7 121.6(6) . . ?
C12 C2 C7 119.9(6) . . ?
C13 C3 C4 117.4(6) . . ?
C13 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
C8 C4 C3 120.1(6) . . ?
C8 C4 C6 120.5(6) . . ?
C3 C4 C6 119.3(6) . . ?
C5 C5 C1 107.2(4) 11_565 . ?
C5 C5 H5 126.4 11_565 . ?
C1 C5 H5 126.4 . . ?
C10 C6 C1 124.6(6) . . ?
C10 C6 C4 118.1(6) . . ?
C1 C6 C4 117.2(6) . . ?
O1 C7 O4 119.2(8) . . ?
O1 C7 O4' 120.1(8) . . ?
O1 C7 C2 121.5(7) . . ?
O4 C7 C2 117.5(7) . . ?
O4' C7 C2 116.7(7) . . ?
O1 C7 Gd1 60.9(4) . 6_654 ?
O4 C7 Gd1 59.7(5) . 6_654 ?
O4' C7 Gd1 61.5(5) . 6_654 ?
C2 C7 Gd1 177.0(5) . 6_654 ?
C4 C8 C2 122.0(6) . . ?
C4 C8 H8 119.0 . . ?
C2 C8 H8 119.0 . . ?
O2' C9 O3 119.2(9) 4_566 . ?
O3 C9 O2 122.7(7) . . ?
O2' C9 C13 119.4(8) 4_566 . ?
O3 C9 C13 119.5(7) . . ?
O2 C9 C13 116.6(7) . . ?
O2' C9 Na1 72.3(6) 4_566 . ?
O3 C9 Na1 46.9(4) . . ?
O2 C9 Na1 81.2(5) . . ?
C13 C9 Na1 159.7(6) . . ?
C6 C10 N2 126.8(6) . . ?
C6 C10 C11 125.3(6) . . ?
N2 C10 C11 107.7(6) . . ?
C11 C11 C10 108.4(4) 12_655 . ?
C11 C11 H11 125.8 12_655 . ?
C10 C11 H11 125.8 . . ?
C13 C12 C2 120.8(6) . . ?
C13 C12 H12 119.6 . . ?
C2 C12 H12 119.6 . . ?
C12 C13 C3 121.2(6) . . ?
C12 C13 C9 120.0(6) . . ?
C3 C13 C9 118.7(6) . . ?

# 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 -0.011 -0.002 0.003 6199 2614 ' '
_platon_squeeze_details          
;
 Numerous molecules of the disordered DMF (possibly + water)  solvent.
;

_refine_diff_density_max         1.496
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.150



_exptl_crystal_recrystallization_method solvothermal
####################################################################### 
# 
# 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_bkt16sq
_database_code_depnum_ccdc_archive 'CCDC 1422228'
_audit_update_record             
;
2015-09-03 deposited with the CCDC.
2015-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H30 N4 Na2 O21 Sm2 Zn'
_chemical_formula_sum            'C52 H30 N4 Na2 O21 Sm2 Zn'
_chemical_formula_weight         1458.85

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'
Na Na 0.0362 0.0249 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

_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'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   27.108(4)
_cell_length_b                   29.418(3)
_cell_length_c                   12.9723(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10345(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    4794
_cell_measurement_theta_min      1.38
_cell_measurement_theta_max      25.09

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_F_000             2856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.402
_shelx_estimated_absorpt_T_min   0.730
_shelx_estimated_absorpt_T_max   0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS micro-focus'
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_reflns_number            19423
_diffrn_reflns_av_unetI/netI     0.1556
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.384
_diffrn_reflns_theta_max         25.090
_diffrn_reflns_theta_full        25.090
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4794
_reflns_number_gt                1740
_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.

 The structure contains a considerable amount of severely disordered
 solvent (DMF+water) which couldn't be resolved reliably by discrete
 atoms. The solvent contribution to the diffraction pattern was thus
 subtracted by the Squeeze technique, using the PLATON software
 (Spek, 2015).
;

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          '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)+(0.0616P)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_number_reflns         4794
_refine_ls_number_parameters     177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.1791
_refine_ls_wR_factor_gt          0.1671
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

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
Sm1 Sm 0.82737(3) 0.5000 0.5000 0.0733(3) Uani 1 2 d S T P . .
Zn1 Zn 0.5000 0.2500 0.4404(5) 0.0465(18) Uani 0.5 4 d S T P . .
Zn1' Zn 0.5000 0.2500 0.3839(4) 0.0457(18) Uani 0.5 4 d S T P . .
Na1 Na 0.7500 0.45972(16) 0.7500 0.0870(18) Uani 1 2 d S T P . .
O1 O 0.6954(2) 0.48731(19) 0.1849(5) 0.0675(18) Uani 1 1 d . . . . .
O2 O 0.7610(3) 0.4504(2) 0.5338(5) 0.101(2) Uiso 1 1 d . . . . .
O3 O 0.6436(3) 0.4400(2) 0.1168(6) 0.104(2) Uiso 1 1 d . . . . .
O4 O 0.7153(3) 0.4138(3) 0.6408(8) 0.143(3) Uiso 1 1 d . . . . .
O5 O 0.8817(4) 0.4488(3) 0.6017(7) 0.186(4) Uiso 1 1 d . . . . .
H5A H 0.8685 0.4221 0.6322 0.223 Uiso 1 1 calc R U . . .
H5B H 0.9156 0.4560 0.6101 0.223 Uiso 1 1 calc R U . . .
O6 O 0.5000 0.2500 0.208(2) 0.110(10) Uiso 0.5 4 d S . P . .
H6A H 0.5000 0.2220 0.1718 0.132 Uiso 0.25 2 calc R U P . .
H6B H 0.5000 0.2780 0.1718 0.132 Uiso 0.25 2 calc R U P . .
O6' O 0.5000 0.2500 0.610(2) 0.096(9) Uiso 0.5 4 d S . P . .
H6'1 H 0.5000 0.2220 0.6467 0.115 Uiso 0.25 2 calc R U P . .
H6'2 H 0.5000 0.2780 0.6467 0.115 Uiso 0.25 2 calc R U P . .
N1 N 0.5000 0.3195(3) 0.4083(7) 0.046(3) Uani 1 2 d S T P . .
N2 N 0.5756(3) 0.2500 0.4121(7) 0.050(3) Uani 1 2 d S T P . .
C1 C 0.5903(3) 0.3327(3) 0.4046(7) 0.055(2) Uani 1 1 d . . . . .
C2 C 0.6602(3) 0.3795(3) 0.4737(7) 0.062(3) Uani 1 1 d . . . . .
H2 H 0.6585 0.3633 0.5369 0.074 Uiso 1 1 calc R U . . .
C3 C 0.6309(3) 0.3908(3) 0.3007(7) 0.058(3) Uani 1 1 d . . . . .
H3 H 0.6104 0.3826 0.2444 0.070 Uiso 1 1 calc R U . . .
C4 C 0.6658(3) 0.4271(3) 0.2923(7) 0.052(2) Uani 1 1 d . . . . .
C5 C 0.6282(3) 0.3686(3) 0.3925(7) 0.051(2) Uani 1 1 d . . . . .
C6 C 0.6062(3) 0.2870(3) 0.4031(6) 0.050(2) Uani 1 1 d . . . . .
C7 C 0.6981(3) 0.4362(3) 0.3700(7) 0.051(2) Uani 1 1 d . . . . .
H7 H 0.7234 0.4581 0.3609 0.062 Uiso 1 1 calc R U . . .
C8 C 0.6565(3) 0.2742(2) 0.3994(7) 0.068(3) Uani 1 1 d . . . . .
H8 H 0.6844 0.2938 0.3973 0.082 Uiso 1 1 calc R U . . .
C9 C 0.5398(3) 0.3473(2) 0.4066(7) 0.051(2) Uani 1 1 d . . . . .
C10 C 0.6935(4) 0.4133(3) 0.4615(7) 0.061(3) Uani 1 1 d . . . . .
C11 C 0.5226(3) 0.3933(3) 0.4101(7) 0.072(3) Uani 1 1 d . . . . .
H11 H 0.5429 0.4196 0.4121 0.086 Uiso 1 1 calc R U . . .
C12 C 0.6686(4) 0.4538(3) 0.1959(8) 0.074(3) Uani 1 1 d . . . . .
C13 C 0.7273(5) 0.4247(4) 0.5460(10) 0.109(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O2 2.356(8) . ?
Sm1 O2 2.356(8) 4_566 ?
Sm1 O3 2.455(7) 6_655 ?
Sm1 O3 2.455(7) 7_645 ?
Sm1 O5 2.485(9) 4_566 ?
Sm1 O5 2.485(9) . ?
Sm1 O1 2.505(6) 7_645 ?
Sm1 O1 2.505(6) 6_655 ?
Sm1 C12 2.885(10) 6_655 ?
Sm1 C12 2.885(10) 7_645 ?
Sm1 Na1 4.0398(15) . ?
Sm1 Na1 4.0398(15) 6_654 ?
Zn1 Zn1' 0.733(7) . ?
Zn1 N1 2.088(9) 2_655 ?
Zn1 N1 2.088(9) . ?
Zn1 N2 2.083(9) . ?
Zn1 N2 2.083(9) 2_655 ?
Zn1 O6' 2.20(3) . ?
Zn1' N1 2.070(8) 2_655 ?
Zn1' N1 2.070(8) . ?
Zn1' N2 2.083(9) . ?
Zn1' N2 2.083(9) 2_655 ?
Zn1' O6 2.28(3) . ?
Na1 O4 2.171(9) . ?
Na1 O4 2.171(9) 7_646 ?
Na1 O1 2.308(7) 6_655 ?
Na1 O1 2.308(7) 4_566 ?
Na1 O2 2.834(7) 7_646 ?
Na1 O2 2.834(7) . ?
Na1 C13 2.906(13) 7_646 ?
Na1 C13 2.906(13) . ?
Na1 Sm1 4.0398(15) 6_655 ?
O1 C12 1.234(9) . ?
O1 Na1 2.308(7) 6_654 ?
O1 Sm1 2.505(6) 6_654 ?
O2 C13 1.199(11) . ?
O3 C12 1.296(10) . ?
O3 Sm1 2.455(7) 6_654 ?
O4 C13 1.311(12) . ?
O5 H5A 0.9500 . ?
O5 H5B 0.9500 . ?
O6 H6A 0.9500 . ?
O6 H6B 0.9500 . ?
O6' H6'1 0.9500 . ?
O6' H6'2 0.9500 . ?
N1 C9 1.354(8) 12_655 ?
N1 C9 1.354(8) . ?
N2 C6 1.374(9) 11_565 ?
N2 C6 1.374(9) . ?
C1 C6 1.411(10) . ?
C1 C9 1.433(10) . ?
C1 C5 1.484(10) . ?
C2 C10 1.351(12) . ?
C2 C5 1.401(10) . ?
C2 H2 0.9500 . ?
C3 C5 1.360(10) . ?
C3 C4 1.430(10) . ?
C3 H3 0.9500 . ?
C4 C7 1.361(10) . ?
C4 C12 1.477(12) . ?
C6 C8 1.414(10) . ?
C7 C10 1.370(10) . ?
C7 H7 0.9500 . ?
C8 C8 1.425(14) 11_565 ?
C8 H8 0.9500 . ?
C9 C11 1.435(9) . ?
C10 C13 1.467(13) . ?
C11 C11 1.223(15) 12_655 ?
C11 H11 0.9500 . ?
C12 Sm1 2.885(10) 6_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
O2 Sm1 O2 80.5(3) . 4_566 ?
O2 Sm1 O3 125.1(3) . 6_655 ?
O2 Sm1 O3 85.1(2) 4_566 6_655 ?
O2 Sm1 O3 85.1(2) . 7_645 ?
O2 Sm1 O3 125.1(3) 4_566 7_645 ?
O3 Sm1 O3 142.6(4) 6_655 7_645 ?
O2 Sm1 O5 157.8(3) . 4_566 ?
O2 Sm1 O5 88.8(3) 4_566 4_566 ?
O3 Sm1 O5 72.7(3) 6_655 4_566 ?
O3 Sm1 O5 85.3(3) 7_645 4_566 ?
O2 Sm1 O5 88.8(3) . . ?
O2 Sm1 O5 157.8(3) 4_566 . ?
O3 Sm1 O5 85.3(3) 6_655 . ?
O3 Sm1 O5 72.7(3) 7_645 . ?
O5 Sm1 O5 107.3(5) 4_566 . ?
O2 Sm1 O1 84.1(2) . 7_645 ?
O2 Sm1 O1 74.1(2) 4_566 7_645 ?
O3 Sm1 O1 141.0(2) 6_655 7_645 ?
O3 Sm1 O1 51.8(2) 7_645 7_645 ?
O5 Sm1 O1 74.2(2) 4_566 7_645 ?
O5 Sm1 O1 124.4(2) . 7_645 ?
O2 Sm1 O1 74.1(2) . 6_655 ?
O2 Sm1 O1 84.1(2) 4_566 6_655 ?
O3 Sm1 O1 51.8(2) 6_655 6_655 ?
O3 Sm1 O1 141.0(2) 7_645 6_655 ?
O5 Sm1 O1 124.4(2) 4_566 6_655 ?
O5 Sm1 O1 74.2(2) . 6_655 ?
O1 Sm1 O1 151.4(3) 7_645 6_655 ?
O2 Sm1 C12 99.0(3) . 6_655 ?
O2 Sm1 C12 84.3(3) 4_566 6_655 ?
O3 Sm1 C12 26.5(2) 6_655 6_655 ?
O3 Sm1 C12 150.5(3) 7_645 6_655 ?
O5 Sm1 C12 99.2(3) 4_566 6_655 ?
O5 Sm1 C12 78.2(3) . 6_655 ?
O1 Sm1 C12 157.4(2) 7_645 6_655 ?
O1 Sm1 C12 25.23(19) 6_655 6_655 ?
O2 Sm1 C12 84.3(3) . 7_645 ?
O2 Sm1 C12 99.0(3) 4_566 7_645 ?
O3 Sm1 C12 150.5(3) 6_655 7_645 ?
O3 Sm1 C12 26.5(2) 7_645 7_645 ?
O5 Sm1 C12 78.2(3) 4_566 7_645 ?
O5 Sm1 C12 99.2(3) . 7_645 ?
O1 Sm1 C12 25.23(19) 7_645 7_645 ?
O1 Sm1 C12 157.4(2) 6_655 7_645 ?
C12 Sm1 C12 175.7(4) 6_655 7_645 ?
O2 Sm1 Na1 43.37(17) . . ?
O2 Sm1 Na1 86.26(18) 4_566 . ?
O3 Sm1 Na1 83.21(19) 6_655 . ?
O3 Sm1 Na1 116.80(18) 7_645 . ?
O5 Sm1 Na1 155.7(2) 4_566 . ?
O5 Sm1 Na1 72.8(2) . . ?
O1 Sm1 Na1 126.64(14) 7_645 . ?
O1 Sm1 Na1 31.44(14) 6_655 . ?
C12 Sm1 Na1 56.7(2) 6_655 . ?
C12 Sm1 Na1 126.0(2) 7_645 . ?
O2 Sm1 Na1 86.26(18) . 6_654 ?
O2 Sm1 Na1 43.37(17) 4_566 6_654 ?
O3 Sm1 Na1 116.80(18) 6_655 6_654 ?
O3 Sm1 Na1 83.21(19) 7_645 6_654 ?
O5 Sm1 Na1 72.8(2) 4_566 6_654 ?
O5 Sm1 Na1 155.7(2) . 6_654 ?
O1 Sm1 Na1 31.44(14) 7_645 6_654 ?
O1 Sm1 Na1 126.64(14) 6_655 6_654 ?
C12 Sm1 Na1 126.0(2) 6_655 6_654 ?
C12 Sm1 Na1 56.7(2) 7_645 6_654 ?
Na1 Sm1 Na1 117.45(3) . 6_654 ?
N1 Zn1 N1 157.0(6) 2_655 . ?
N1 Zn1 N2 87.99(9) 2_655 . ?
N1 Zn1 N2 87.99(9) . . ?
N1 Zn1 N2 87.99(9) 2_655 2_655 ?
N1 Zn1 N2 87.99(9) . 2_655 ?
N2 Zn1 N2 159.7(6) . 2_655 ?
N1 Zn1 O6' 101.5(3) 2_655 . ?
N1 Zn1 O6' 101.5(3) . . ?
N2 Zn1 O6' 100.1(3) . . ?
N2 Zn1 O6' 100.1(3) 2_655 . ?
N1 Zn1' N2 88.46(8) 2_655 . ?
N1 Zn1' N2 88.46(8) . . ?
N1 Zn1' N2 88.46(8) 2_655 2_655 ?
N1 Zn1' N2 88.46(8) . 2_655 ?
N2 Zn1' N2 159.7(6) . 2_655 ?
N1 Zn1' O6 98.8(3) 2_655 . ?
N1 Zn1' O6 98.8(3) . . ?
N2 Zn1' O6 100.1(3) . . ?
N2 Zn1' O6 100.1(3) 2_655 . ?
O4 Na1 O4 103.1(5) . 7_646 ?
O4 Na1 O1 117.3(3) . 6_655 ?
O4 Na1 O1 112.4(3) 7_646 6_655 ?
O4 Na1 O1 112.4(3) . 4_566 ?
O4 Na1 O1 117.3(3) 7_646 4_566 ?
O1 Na1 O1 95.1(3) 6_655 4_566 ?
O4 Na1 O2 122.7(3) . 7_646 ?
O4 Na1 O2 48.7(3) 7_646 7_646 ?
O1 Na1 O2 119.7(2) 6_655 7_646 ?
O1 Na1 O2 68.6(2) 4_566 7_646 ?
O4 Na1 O2 48.7(3) . . ?
O4 Na1 O2 122.7(3) 7_646 . ?
O1 Na1 O2 68.6(2) 6_655 . ?
O1 Na1 O2 119.7(2) 4_566 . ?
O2 Na1 O2 168.9(4) 7_646 . ?
O4 Na1 C13 117.7(4) . 7_646 ?
O1 Na1 C13 115.9(3) 6_655 7_646 ?
O1 Na1 C13 92.4(3) 4_566 7_646 ?
O2 Na1 C13 147.6(3) . 7_646 ?
O4 Na1 C13 117.7(4) 7_646 . ?
O1 Na1 C13 92.4(3) 6_655 . ?
O1 Na1 C13 115.9(3) 4_566 . ?
O2 Na1 C13 147.6(3) 7_646 . ?
C13 Na1 C13 138.4(5) 7_646 . ?
O4 Na1 Sm1 83.3(3) . . ?
O4 Na1 Sm1 118.8(3) 7_646 . ?
O1 Na1 Sm1 115.37(19) 4_566 . ?
O2 Na1 Sm1 151.37(17) 7_646 . ?
C13 Na1 Sm1 136.5(3) 7_646 . ?
C13 Na1 Sm1 58.9(2) . . ?
O4 Na1 Sm1 118.8(3) . 6_655 ?
O4 Na1 Sm1 83.3(3) 7_646 6_655 ?
O1 Na1 Sm1 115.37(19) 6_655 6_655 ?
O2 Na1 Sm1 151.37(16) . 6_655 ?
C13 Na1 Sm1 58.9(2) 7_646 6_655 ?
C13 Na1 Sm1 136.5(3) . 6_655 ?
Sm1 Na1 Sm1 145.89(13) . 6_655 ?
C12 O1 Na1 151.0(6) . 6_654 ?
C12 O1 Sm1 94.9(6) . 6_654 ?
Na1 O1 Sm1 114.1(2) 6_654 6_654 ?
C13 O2 Sm1 176.9(8) . . ?
C13 O2 Na1 81.3(7) . . ?
Sm1 O2 Na1 101.8(3) . . ?
C12 O3 Sm1 95.6(6) . 6_654 ?
C13 O4 Na1 110.7(8) . . ?
Sm1 O5 H5A 120.0 . . ?
Sm1 O5 H5B 120.0 . . ?
H5A O5 H5B 120.0 . . ?
Zn1' O6 H6A 120.0 . . ?
Zn1' O6 H6B 120.0 . . ?
H6A O6 H6B 120.0 . . ?
Zn1 O6' H6'1 120.0 . . ?
Zn1 O6' H6'2 120.0 . . ?
H6'1 O6' H6'2 120.0 . . ?
C9 N1 C9 105.8(9) 12_655 . ?
C9 N1 Zn1' 126.4(5) 12_655 . ?
C9 N1 Zn1' 126.4(5) . . ?
C9 N1 Zn1 126.4(5) 12_655 . ?
C9 N1 Zn1 126.4(5) . . ?
C6 N2 C6 104.9(9) 11_565 . ?
C6 N2 Zn1 127.5(5) 11_565 . ?
C6 N2 Zn1 127.5(5) . . ?
C6 N2 Zn1' 125.4(5) 11_565 . ?
C6 N2 Zn1' 125.4(5) . . ?
C6 C1 C9 125.3(7) . . ?
C6 C1 C5 117.6(7) . . ?
C9 C1 C5 116.7(7) . . ?
C10 C2 C5 119.6(8) . . ?
C10 C2 H2 120.2 . . ?
C5 C2 H2 120.2 . . ?
C5 C3 C4 117.5(8) . . ?
C5 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
C7 C4 C3 121.0(8) . . ?
C7 C4 C12 119.3(8) . . ?
C3 C4 C12 119.7(8) . . ?
C3 C5 C2 121.0(8) . . ?
C3 C5 C1 118.2(8) . . ?
C2 C5 C1 120.9(8) . . ?
N2 C6 C1 124.6(8) . . ?
N2 C6 C8 111.9(7) . . ?
C1 C6 C8 123.3(7) . . ?
C4 C7 C10 119.1(8) . . ?
C4 C7 H7 120.4 . . ?
C10 C7 H7 120.4 . . ?
C6 C8 C8 105.5(4) . 11_565 ?
C6 C8 H8 127.3 . . ?
C8 C8 H8 127.3 11_565 . ?
N1 C9 C11 108.0(7) . . ?
N1 C9 C1 125.5(7) . . ?
C11 C9 C1 126.5(7) . . ?
C2 C10 C7 121.5(9) . . ?
C2 C10 C13 119.8(9) . . ?
C7 C10 C13 118.6(9) . . ?
C11 C11 C9 109.1(4) 12_655 . ?
C11 C11 H11 125.5 12_655 . ?
C9 C11 H11 125.5 . . ?
O1 C12 O3 117.8(9) . . ?
O1 C12 C4 123.6(9) . . ?
O3 C12 C4 118.5(9) . . ?
O1 C12 Sm1 59.9(5) . 6_654 ?
O3 C12 Sm1 57.9(5) . 6_654 ?
C4 C12 Sm1 176.0(6) . 6_654 ?
O2 C13 O4 117.8(12) . . ?
O2 C13 C10 121.4(11) . . ?
O4 C13 C10 119.4(11) . . ?
O2 C13 Na1 74.6(7) . . ?
C10 C13 Na1 153.4(9) . . ?

# 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 -0.016 -0.003 0.007 6010 2572 ' '
_platon_squeeze_details          
;
 Numerous molecules of severely disordered DMF (+ water) solvent.
;
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.113



_exptl_crystal_recrystallization_method solvothermal
####################################################################### 
# 
# 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_bkt17sq
_database_code_depnum_ccdc_archive 'CCDC 1422229'
_audit_update_record             
;
2015-09-03 deposited with the CCDC.
2015-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H29 Dy2 N4 Na2 O21 Zn'
_chemical_formula_sum            'C52 H29 Dy2 N4 Na2 O21 Zn'
_chemical_formula_weight         1482.16

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'
Na Na 0.0362 0.0249 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

_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'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   27.1337(11)
_cell_length_b                   29.2422(14)
_cell_length_c                   13.0757(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10374.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    2088
_cell_measurement_theta_min      2.05
_cell_measurement_theta_max      25.03

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.949
_exptl_crystal_F_000             2888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.707
_shelx_estimated_absorpt_T_min   0.628
_shelx_estimated_absorpt_T_max   0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS micro-focus'
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_reflns_number            10069
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.048
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.527
_diffrn_measured_fraction_theta_full 0.527
_diffrn_reflns_Laue_measured_fraction_max 0.527
_diffrn_reflns_Laue_measured_fraction_full 0.527
_diffrn_reflns_point_group_measured_fraction_max 0.527
_diffrn_reflns_point_group_measured_fraction_full 0.527
_reflns_number_total             2528
_reflns_number_gt                2088
_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.

 The structure contains a considerable amount of severely disordered
 solvent (DMF+water) which couldn't be resolved reliably by discrete
 atoms. The solvent contribution to the diffraction pattern was thus
 subtracted by the Squeeze technique, using the PLATON software
 (Spek, 2015).
;

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          '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)+(0.1000P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2528
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1497
_refine_ls_wR_factor_gt          0.1465
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_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
Dy1 Dy 0.82547(2) 0.5000 0.5000 0.0499(3) Uani 1 2 d S T P . .
Zn1 Zn 0.5000 0.2500 0.3686(4) 0.0400(12) Uani 0.6 4 d S T P . .
Zn1' Zn 0.5000 0.2500 0.4225(9) 0.068(3) Uani 0.4 4 d S T P . .
Na1 Na 0.7500 0.45799(18) 0.7500 0.0592(15) Uani 1 2 d S T P . .
O1 O 0.6953(2) 0.4896(2) 0.1814(5) 0.048(2) Uani 1 1 d . . . . .
O2 O 0.7659(3) 0.4478(3) 0.5248(9) 0.096(3) Uiso 1 1 d . . . . .
O3 O 0.6486(4) 0.4363(3) 0.1088(8) 0.079(2) Uiso 1 1 d . . . . .
O4 O 0.7138(4) 0.4143(4) 0.6301(10) 0.096(3) Uiso 1 1 d . . . . .
O5 O 0.8769(4) 0.4527(4) 0.6095(8) 0.094(3) Uiso 1 1 d . . . . .
H5A H 0.8731 0.4540 0.6817 0.113 Uiso 1 1 calc R U . . .
H5B H 0.9007 0.4328 0.5801 0.113 Uiso 1 1 calc R U . . .
O6 O 0.5000 0.2500 0.212(3) 0.165(11) Uiso 1 4 d S . P . .
H6A H 0.5000 0.2775 0.1760 0.198 Uiso 0.25 2 d R U P . .
H6B H 0.5000 0.2225 0.1760 0.198 Uiso 0.25 2 d R U P . .
N1 N 0.5000 0.3197(3) 0.3988(9) 0.038(3) Uani 1 2 d S T P . .
N2 N 0.5763(3) 0.2500 0.4018(9) 0.038(2) Uani 1 2 d S T P . .
C1 C 0.5894(3) 0.3321(3) 0.3967(7) 0.041(2) Uani 1 1 d . . . . .
C2 C 0.6588(4) 0.3801(3) 0.4665(7) 0.043(3) Uani 1 1 d . . . . .
H2 H 0.6558 0.3635 0.5286 0.052 Uiso 1 1 calc R U . . .
C3 C 0.6313(3) 0.3939(3) 0.2988(7) 0.050(2) Uani 1 1 d . . . . .
H3 H 0.6089 0.3877 0.2446 0.060 Uiso 1 1 calc R U . . .
C4 C 0.6678(3) 0.4285(3) 0.2868(8) 0.048(3) Uani 1 1 d . . . . .
C5 C 0.6283(3) 0.3698(2) 0.3873(7) 0.0354(19) Uani 1 1 d . . . . .
C6 C 0.6046(3) 0.2874(3) 0.3989(7) 0.039(2) Uani 1 1 d . . . . .
C7 C 0.6971(3) 0.4362(3) 0.3658(7) 0.038(2) Uani 1 1 d . . . . .
H7 H 0.7220 0.4586 0.3563 0.045 Uiso 1 1 calc R U . . .
C8 C 0.6566(4) 0.2728(3) 0.3942(9) 0.050(2) Uani 1 1 d . . . . .
H8 H 0.6847 0.2922 0.3917 0.060 Uiso 1 1 calc R U . . .
C9 C 0.5400(3) 0.3472(3) 0.3980(8) 0.043(2) Uani 1 1 d . . . . .
C10 C 0.6957(5) 0.4157(3) 0.4586(7) 0.047(2) Uani 1 1 d . . . . .
C11 C 0.5248(4) 0.3929(3) 0.4045(10) 0.065(3) Uani 1 1 d . . . . .
H11 H 0.5456 0.4190 0.4082 0.079 Uiso 1 1 calc R U . . .
C12 C 0.6695(4) 0.4547(4) 0.1881(9) 0.059(3) Uani 1 1 d . . . . .
C13 C 0.7273(5) 0.4271(4) 0.5424(8) 0.055(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.248(8) 4_566 ?
Dy1 O2 2.248(8) . ?
Dy1 O5 2.431(10) 4_566 ?
Dy1 O5 2.431(10) . ?
Dy1 O3 2.446(9) 6_655 ?
Dy1 O3 2.446(9) 7_645 ?
Dy1 O1 2.457(7) 7_645 ?
Dy1 O1 2.457(7) 6_655 ?
Dy1 C12 2.796(10) 6_655 ?
Dy1 C12 2.796(10) 7_645 ?
Dy1 Na1 4.0483(16) . ?
Dy1 Na1 4.0483(16) 6_654 ?
Zn1 Zn1' 0.705(10) . ?
Zn1 O6 2.05(3) . ?
Zn1 N1 2.076(8) 2_655 ?
Zn1 N1 2.076(8) . ?
Zn1 N2 2.116(9) . ?
Zn1 N2 2.116(9) 2_655 ?
Zn1' N1 2.062(8) 2_655 ?
Zn1' N1 2.062(8) . ?
Zn1' N2 2.089(9) . ?
Zn1' N2 2.089(9) 2_655 ?
Na1 O4 2.250(12) 7_646 ?
Na1 O4 2.250(12) . ?
Na1 O1 2.315(7) 6_655 ?
Na1 O1 2.315(7) 4_566 ?
Na1 C13 2.926(11) 7_646 ?
Na1 C13 2.926(11) . ?
Na1 O2 2.991(11) . ?
Na1 O2 2.991(11) 7_646 ?
Na1 Dy1 4.0483(16) 6_655 ?
O1 C12 1.240(12) . ?
O1 Na1 2.315(7) 6_654 ?
O1 Dy1 2.457(7) 6_654 ?
O2 C13 1.231(13) . ?
O3 C12 1.298(14) . ?
O3 Dy1 2.446(9) 6_654 ?
O4 C13 1.261(16) . ?
O5 H5A 0.9500 . ?
O5 H5B 0.9500 . ?
O6 H6A 0.9300 . ?
O6 H6B 0.9300 . ?
N1 C9 1.351(9) 12_655 ?
N1 C9 1.351(9) . ?
N2 C6 1.336(10) 11_565 ?
N2 C6 1.336(10) . ?
C1 C6 1.371(12) . ?
C1 C9 1.409(12) . ?
C1 C5 1.532(11) . ?
C2 C5 1.359(12) . ?
C2 C10 1.448(15) . ?
C2 H2 0.9500 . ?
C3 C5 1.357(12) . ?
C3 C4 1.425(11) . ?
C3 H3 0.9500 . ?
C4 C7 1.324(14) . ?
C4 C12 1.503(14) . ?
C6 C8 1.475(13) . ?
C7 C10 1.353(14) . ?
C7 H7 0.9500 . ?
C8 C8 1.336(17) 11_565 ?
C8 H8 0.9500 . ?
C9 C11 1.403(11) . ?
C10 C13 1.431(13) . ?
C11 C11 1.346(19) 12_655 ?
C11 H11 0.9500 . ?
C12 Dy1 2.796(10) 6_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
O2 Dy1 O2 88.0(4) 4_566 . ?
O2 Dy1 O5 86.6(4) 4_566 4_566 ?
O2 Dy1 O5 152.2(4) . 4_566 ?
O2 Dy1 O5 152.2(4) 4_566 . ?
O2 Dy1 O5 86.6(4) . . ?
O5 Dy1 O5 110.0(5) 4_566 . ?
O2 Dy1 O3 76.9(3) 4_566 6_655 ?
O2 Dy1 O3 129.8(4) . 6_655 ?
O5 Dy1 O3 75.2(3) 4_566 6_655 ?
O5 Dy1 O3 85.7(4) . 6_655 ?
O2 Dy1 O3 129.8(4) 4_566 7_645 ?
O2 Dy1 O3 76.9(3) . 7_645 ?
O5 Dy1 O3 85.7(4) 4_566 7_645 ?
O5 Dy1 O3 75.2(3) . 7_645 ?
O3 Dy1 O3 146.6(5) 6_655 7_645 ?
O2 Dy1 O1 77.3(3) 4_566 7_645 ?
O2 Dy1 O1 83.7(3) . 7_645 ?
O5 Dy1 O1 68.5(3) 4_566 7_645 ?
O5 Dy1 O1 129.0(3) . 7_645 ?
O3 Dy1 O1 136.2(3) 6_655 7_645 ?
O3 Dy1 O1 53.9(3) 7_645 7_645 ?
O2 Dy1 O1 83.7(3) 4_566 6_655 ?
O2 Dy1 O1 77.3(3) . 6_655 ?
O5 Dy1 O1 129.0(3) 4_566 6_655 ?
O5 Dy1 O1 68.5(3) . 6_655 ?
O3 Dy1 O1 53.9(3) 6_655 6_655 ?
O3 Dy1 O1 136.2(3) 7_645 6_655 ?
O1 Dy1 O1 153.5(3) 7_645 6_655 ?
O2 Dy1 C12 80.8(4) 4_566 6_655 ?
O2 Dy1 C12 103.3(3) . 6_655 ?
O5 Dy1 C12 102.7(3) 4_566 6_655 ?
O5 Dy1 C12 73.9(4) . 6_655 ?
O3 Dy1 C12 27.7(3) 6_655 6_655 ?
O3 Dy1 C12 149.0(4) 7_645 6_655 ?
O1 Dy1 C12 156.8(3) 7_645 6_655 ?
O1 Dy1 C12 26.3(3) 6_655 6_655 ?
O2 Dy1 C12 103.3(3) 4_566 7_645 ?
O2 Dy1 C12 80.8(4) . 7_645 ?
O5 Dy1 C12 73.9(4) 4_566 7_645 ?
O5 Dy1 C12 102.7(3) . 7_645 ?
O3 Dy1 C12 149.0(4) 6_655 7_645 ?
O3 Dy1 C12 27.7(3) 7_645 7_645 ?
O1 Dy1 C12 26.3(3) 7_645 7_645 ?
O1 Dy1 C12 156.8(3) 6_655 7_645 ?
C12 Dy1 C12 174.4(4) 6_655 7_645 ?
O2 Dy1 Na1 87.6(3) 4_566 . ?
O2 Dy1 Na1 46.6(3) . . ?
O5 Dy1 Na1 159.8(3) 4_566 . ?
O5 Dy1 Na1 69.0(3) . . ?
O3 Dy1 Na1 84.7(2) 6_655 . ?
O3 Dy1 Na1 112.6(2) 7_645 . ?
O1 Dy1 Na1 128.78(15) 7_645 . ?
O1 Dy1 Na1 30.91(15) 6_655 . ?
C12 Dy1 Na1 57.2(2) 6_655 . ?
C12 Dy1 Na1 126.3(3) 7_645 . ?
O2 Dy1 Na1 46.6(3) 4_566 6_654 ?
O2 Dy1 Na1 87.6(3) . 6_654 ?
O5 Dy1 Na1 69.0(3) 4_566 6_654 ?
O5 Dy1 Na1 159.8(3) . 6_654 ?
O3 Dy1 Na1 112.6(2) 6_655 6_654 ?
O3 Dy1 Na1 84.7(2) 7_645 6_654 ?
O1 Dy1 Na1 30.91(15) 7_645 6_654 ?
O1 Dy1 Na1 128.78(15) 6_655 6_654 ?
C12 Dy1 Na1 126.3(3) 6_655 6_654 ?
C12 Dy1 Na1 57.2(2) 7_645 6_654 ?
Na1 Dy1 Na1 119.23(3) . 6_654 ?
O6 Zn1 N1 100.9(4) . 2_655 ?
O6 Zn1 N1 100.9(4) . . ?
N1 Zn1 N1 158.1(7) 2_655 . ?
O6 Zn1 N2 101.8(3) . . ?
N1 Zn1 N2 87.77(11) 2_655 . ?
N1 Zn1 N2 87.77(11) . . ?
O6 Zn1 N2 101.8(3) . 2_655 ?
N1 Zn1 N2 87.77(11) 2_655 2_655 ?
N1 Zn1 N2 87.77(11) . 2_655 ?
N2 Zn1 N2 156.3(7) . 2_655 ?
N1 Zn1' N1 162.7(10) 2_655 . ?
Zn1 Zn1' N2 82.6(5) . . ?
N1 Zn1' N2 88.88(12) 2_655 . ?
N1 Zn1' N2 88.88(12) . . ?
N1 Zn1' N2 88.88(12) 2_655 2_655 ?
N1 Zn1' N2 88.88(12) . 2_655 ?
N2 Zn1' N2 165.1(9) . 2_655 ?
O4 Na1 O4 110.7(7) 7_646 . ?
O4 Na1 O1 111.5(3) 7_646 6_655 ?
O4 Na1 O1 112.7(4) . 6_655 ?
O4 Na1 O1 112.7(4) 7_646 4_566 ?
O4 Na1 O1 111.5(3) . 4_566 ?
O1 Na1 O1 97.1(4) 6_655 4_566 ?
O4 Na1 C13 124.3(4) . 7_646 ?
O1 Na1 C13 115.4(4) 6_655 7_646 ?
O1 Na1 C13 88.9(3) 4_566 7_646 ?
O4 Na1 C13 124.3(4) 7_646 . ?
O1 Na1 C13 88.9(3) 6_655 . ?
O1 Na1 C13 115.4(4) 4_566 . ?
C13 Na1 C13 144.0(5) 7_646 . ?
O4 Na1 O2 124.5(4) 7_646 . ?
O1 Na1 O2 65.9(2) 6_655 . ?
O1 Na1 O2 122.7(3) 4_566 . ?
C13 Na1 O2 148.4(3) 7_646 . ?
O4 Na1 O2 124.5(4) . 7_646 ?
O1 Na1 O2 122.7(3) 6_655 7_646 ?
O1 Na1 O2 65.9(2) 4_566 7_646 ?
C13 Na1 O2 148.4(3) . 7_646 ?
O2 Na1 O2 168.6(4) . 7_646 ?
O4 Na1 Dy1 80.3(3) 7_646 6_655 ?
O4 Na1 Dy1 120.9(3) . 6_655 ?
O1 Na1 Dy1 115.9(2) 6_655 6_655 ?
O2 Na1 Dy1 153.91(17) . 6_655 ?
O4 Na1 Dy1 121.0(3) 7_646 . ?
O4 Na1 Dy1 80.3(3) . . ?
O1 Na1 Dy1 115.9(2) 4_566 . ?
C13 Na1 Dy1 137.4(3) 7_646 . ?
C13 Na1 Dy1 56.7(2) . . ?
O2 Na1 Dy1 153.91(17) 7_646 . ?
Dy1 Na1 Dy1 144.67(14) 6_655 . ?
C12 O1 Na1 151.5(7) . 6_654 ?
C12 O1 Dy1 92.3(6) . 6_654 ?
Na1 O1 Dy1 116.1(3) 6_654 6_654 ?
C13 O2 Dy1 166.6(9) . . ?
C13 O2 Na1 75.1(8) . . ?
Dy1 O2 Na1 100.2(4) . . ?
C12 O3 Dy1 91.3(6) . 6_654 ?
C13 O4 Na1 109.7(8) . . ?
Dy1 O5 H5A 120.0 . . ?
Dy1 O5 H5B 120.0 . . ?
H5A O5 H5B 120.0 . . ?
Zn1 O6 H6A 120.0 . . ?
Zn1 O6 H6B 120.0 . . ?
H6A O6 H6B 120.0 . . ?
C9 N1 C9 107.0(9) 12_655 . ?
C9 N1 Zn1' 126.1(4) 12_655 . ?
C9 N1 Zn1' 126.1(4) . . ?
C9 N1 Zn1 125.6(5) 12_655 . ?
C9 N1 Zn1 125.6(5) . . ?
C6 N2 C6 109.8(10) 11_565 . ?
C6 N2 Zn1' 125.0(5) 11_565 . ?
C6 N2 Zn1' 125.0(5) . . ?
C6 N2 Zn1 123.8(5) 11_565 . ?
C6 N2 Zn1 123.8(5) . . ?
C6 C1 C9 125.8(7) . . ?
C6 C1 C5 118.7(8) . . ?
C9 C1 C5 115.5(7) . . ?
C5 C2 C10 121.8(8) . . ?
C5 C2 H2 119.1 . . ?
C10 C2 H2 119.1 . . ?
C5 C3 C4 120.3(9) . . ?
C5 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C7 C4 C3 117.0(9) . . ?
C7 C4 C12 124.4(8) . . ?
C3 C4 C12 118.6(8) . . ?
C3 C5 C2 119.8(7) . . ?
C3 C5 C1 118.9(8) . . ?
C2 C5 C1 121.3(8) . . ?
N2 C6 C1 127.4(8) . . ?
N2 C6 C8 108.3(7) . . ?
C1 C6 C8 124.2(7) . . ?
C4 C7 C10 127.3(9) . . ?
C4 C7 H7 116.3 . . ?
C10 C7 H7 116.3 . . ?
C8 C8 C6 106.7(5) 11_565 . ?
C8 C8 H8 126.6 11_565 . ?
C6 C8 H8 126.6 . . ?
N1 C9 C1 125.3(7) . . ?
N1 C9 C11 109.3(8) . . ?
C1 C9 C11 125.4(7) . . ?
C7 C10 C13 124.5(9) . . ?
C7 C10 C2 113.7(10) . . ?
C13 C10 C2 121.8(8) . . ?
C11 C11 C9 107.1(5) 12_655 . ?
C11 C11 H11 126.4 12_655 . ?
C9 C11 H11 126.4 . . ?
O1 C12 O3 122.1(10) . . ?
O1 C12 C4 119.9(9) . . ?
O3 C12 C4 117.5(9) . . ?
O1 C12 Dy1 61.4(5) . 6_654 ?
O3 C12 Dy1 61.0(6) . 6_654 ?
C4 C12 Dy1 177.3(9) . 6_654 ?
O2 C13 O4 124.3(12) . . ?
O2 C13 C10 118.7(11) . . ?
O4 C13 C10 116.9(10) . . ?
O2 C13 Na1 81.0(7) . . ?
O4 C13 Na1 46.4(7) . . ?
C10 C13 Na1 155.3(10) . . ?

# 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 -0.013 -0.003 0.006 6102 1413 ' '
_platon_squeeze_details          
;
 Numerous molecules of severely disordered DMF (+water) solvent.
;

# start Validation Reply Form
_vrf_PLAT029_bkt17sq             
;
PROBLEM:
RESPONSE:
The structure suffers from considerable pseudosymmetry, and the very
weak reflections were omitted systematically.
;
# end Validation Reply Form

_refine_diff_density_max         1.216
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.105



_exptl_crystal_recrystallization_method solvothermal
####################################################################### 
# 
# 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_bkt26_sq
_database_code_depnum_ccdc_archive 'CCDC 1422230'
_audit_update_record             
;
2015-09-03 deposited with the CCDC.
2015-11-09 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         'C52 H34 Eu2 N4 Na2 O21 Zn'
_chemical_formula_sum            'C52 H34 Eu2 N4 Na2 O21 Zn'
_chemical_formula_weight         1466.13

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'
Na Na 0.0362 0.0249 '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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

_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'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   27.4347(11)
_cell_length_b                   28.9058(12)
_cell_length_c                   13.1157(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10401.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3745
_cell_measurement_theta_min      1.71
_cell_measurement_theta_max      25.05

_exptl_crystal_description       chunk
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.934
_exptl_crystal_F_000             2880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.472
_shelx_estimated_absorpt_T_min   0.778
_shelx_estimated_absorpt_T_max   0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS microfocus'
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_reflns_number            18462
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.705
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_full        25.047
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4800
_reflns_number_gt                3475
_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.

 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.

 The structure contains a large amount of severely disordered
 DMF solvent, which couldn't be modeled by discrete atoms.
 The solvent contribution to the diffraction pattern was thus
 subtracted by the SQUEEZE procedure, using the PLATON software
 (Spek, 2015).

 The five-coordinate zinc ion exhibits twofold disorder.
 Some of the O-sites (water, carboxylate) are disordered as well.
;

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          '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)+(0.1000P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4800
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.1036
_refine_ls_wR_factor_ref         0.2903
_refine_ls_wR_factor_gt          0.2823
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002

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
Eu1 Eu 0.82764(2) 0.5000 0.5000 0.0603(4) Uani 1 2 d S T P . .
Zn1 Zn 0.5000 0.2500 0.3893(6) 0.0459(18) Uani 0.5 4 d S T P . .
Zn1' Zn 0.5000 0.2500 0.4449(5) 0.0359(16) Uani 0.5 4 d S T P . .
Na1 Na 0.7500 0.4586(2) 0.7500 0.097(2) Uani 1 2 d S T P . .
O1 O 0.6941(2) 0.4891(2) 0.1842(5) 0.0502(17) Uani 1 1 d . . . . .
O2 O 0.7646(4) 0.4495(4) 0.5253(8) 0.120(4) Uiso 1 1 d . . . . .
O3 O 0.6444(3) 0.4398(3) 0.1197(7) 0.088(2) Uiso 1 1 d . . . . .
O4 O 0.7188(3) 0.4149(3) 0.6319(7) 0.101(3) Uiso 1 1 d . . . . .
O5 O 0.8843(5) 0.4532(5) 0.5900(11) 0.068(4) Uiso 0.5 1 d . . P . .
H5A H 0.8837 0.4523 0.6624 0.082 Uiso 1 1 calc R U . . .
H5B H 0.9076 0.4354 0.5536 0.082 Uiso 1 1 calc R U . . .
O5' O 0.6884(4) 0.4309(4) 0.7847(8) 0.040(3) Uiso 0.5 1 d . . P . .
H5'1 H 0.6852 0.3982 0.7865 0.048 Uiso 0.5 1 calc R U P . .
H5'2 H 0.6612 0.4500 0.8001 0.048 Uiso 0.5 1 calc R U P . .
O6 O 0.5000 0.2500 0.211(3) 0.102(11) Uiso 0.5 4 d S . P . .
H6A H 0.5000 0.2775 0.1758 0.122 Uiso 0.25 2 d R U P . .
H6B H 0.5000 0.2225 0.1758 0.122 Uiso 0.25 2 d R U P . .
O6' O 0.5000 0.2500 0.611(2) 0.075(9) Uiso 0.5 4 d S . P . .
H6'1 H 0.5000 0.2215 0.6472 0.090 Uiso 0.25 2 calc R U P . .
H6'2 H 0.5000 0.2785 0.6472 0.090 Uiso 0.25 2 calc R U P . .
N1 N 0.5000 0.3197(3) 0.4107(9) 0.047(3) Uani 1 2 d S T P . .
N2 N 0.5746(3) 0.2500 0.4173(8) 0.037(2) Uani 1 2 d S T P . .
C1 C 0.5887(3) 0.3334(3) 0.4078(7) 0.045(2) Uani 1 1 d . . . . .
C2 C 0.6586(3) 0.3817(3) 0.4750(5) 0.041(2) Uani 1 1 d . . . . .
H2 H 0.6558 0.3662 0.5385 0.049 Uiso 1 1 calc R U . . .
C3 C 0.6299(3) 0.3931(3) 0.3063(8) 0.043(2) Uani 1 1 d . . . . .
H3 H 0.6077 0.3859 0.2531 0.051 Uiso 1 1 calc R U . . .
C4 C 0.6660(3) 0.4280(3) 0.2907(6) 0.038(2) Uani 1 1 d . . . . .
C5 C 0.6271(3) 0.3701(3) 0.3954(8) 0.044(2) Uani 1 1 d . . . . .
C6 C 0.6046(3) 0.2887(3) 0.4115(7) 0.041(2) Uani 1 1 d . . . . .
C7 C 0.6977(3) 0.4394(3) 0.3708(7) 0.045(2) Uani 1 1 d . . . . .
H7 H 0.7214 0.4630 0.3625 0.054 Uiso 1 1 calc R U . . .
C8 C 0.6555(3) 0.2741(3) 0.4069(7) 0.050(2) Uani 1 1 d . . . . .
H8 H 0.6832 0.2937 0.4043 0.060 Uiso 1 1 calc R U . . .
C9 C 0.5407(3) 0.3481(3) 0.4097(9) 0.053(3) Uani 1 1 d . . . . .
C10 C 0.6938(4) 0.4156(3) 0.4627(7) 0.045(2) Uani 1 1 d . . . . .
C11 C 0.5245(3) 0.3955(3) 0.4099(10) 0.076(4) Uani 1 1 d . . . . .
H11 H 0.5448 0.4221 0.4100 0.092 Uiso 1 1 calc R U . . .
C12 C 0.6691(3) 0.4543(3) 0.1944(7) 0.050(3) Uani 1 1 d . . . . .
C13 C 0.7287(6) 0.4282(5) 0.5436(8) 0.097(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O2 2.287(13) 4_566 ?
Eu1 O2 2.287(13) . ?
Eu1 O5 2.375(13) . ?
Eu1 O5 2.375(13) 4_566 ?
Eu1 O3 2.467(8) 6_655 ?
Eu1 O3 2.467(8) 7_645 ?
Eu1 O1 2.508(7) 7_645 ?
Eu1 O1 2.508(7) 6_655 ?
Eu1 C12 2.874(10) 7_645 ?
Eu1 C12 2.874(10) 6_655 ?
Eu1 Na1 4.089(2) 6_654 ?
Eu1 Na1 4.089(2) . ?
Zn1 Zn1' 0.730(7) . ?
Zn1 N1 2.035(9) 2_655 ?
Zn1 N1 2.035(9) . ?
Zn1 N2 2.079(9) 2_655 ?
Zn1 N2 2.079(9) . ?
Zn1 O6 2.33(4) . ?
Zn1' N1 2.065(9) 2_655 ?
Zn1' N1 2.065(9) . ?
Zn1' N2 2.078(9) 2_655 ?
Zn1' N2 2.078(9) . ?
Zn1' O6' 2.18(3) . ?
Na1 O5' 1.924(11) . ?
Na1 O5' 1.924(11) 7_646 ?
Na1 O4 2.173(10) . ?
Na1 O4 2.173(10) 7_646 ?
Na1 O1 2.320(8) 6_655 ?
Na1 O1 2.320(8) 4_566 ?
Na1 C13 2.906(11) 7_646 ?
Na1 C13 2.906(11) . ?
Na1 O2 2.986(11) 7_646 ?
Na1 O2 2.986(11) . ?
Na1 Eu1 4.089(2) 6_655 ?
O1 C12 1.226(10) . ?
O1 Na1 2.320(8) 6_654 ?
O1 Eu1 2.508(7) 6_654 ?
O2 C13 1.186(15) . ?
O3 C12 1.263(11) . ?
O3 Eu1 2.467(8) 6_654 ?
O4 C13 1.250(12) . ?
O5 H5A 0.9500 . ?
O5 H5B 0.9500 . ?
O5' H5'1 0.9500 . ?
O5' H5'2 0.9500 . ?
O6 H6A 0.9227 . ?
O6 H6B 0.9227 . ?
O6' H6'1 0.9500 . ?
O6' H6'2 0.9500 . ?
N1 C9 1.386(9) . ?
N1 C9 1.386(9) 12_655 ?
N2 C6 1.392(9) 11_565 ?
N2 C6 1.392(9) . ?
C1 C6 1.365(11) . ?
C1 C9 1.383(11) . ?
C1 C5 1.506(11) . ?
C2 C10 1.384(13) . ?
C2 C5 1.395(12) . ?
C2 H2 0.9500 . ?
C3 C5 1.346(12) . ?
C3 C4 1.429(11) . ?
C3 H3 0.9500 . ?
C4 C7 1.402(11) . ?
C4 C12 1.476(12) . ?
C6 C8 1.459(11) . ?
C7 C10 1.392(12) . ?
C7 H7 0.9500 . ?
C8 C8 1.393(17) 11_565 ?
C8 H8 0.9500 . ?
C9 C11 1.440(12) . ?
C10 C13 1.476(15) . ?
C11 C11 1.342(16) 12_655 ?
C11 H11 0.9500 . ?
C12 Eu1 2.874(10) 6_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
O2 Eu1 O2 81.8(6) 4_566 . ?
O2 Eu1 O5 158.5(4) 4_566 . ?
O2 Eu1 O5 93.4(4) . . ?
O2 Eu1 O5 93.4(4) 4_566 4_566 ?
O2 Eu1 O5 158.5(4) . 4_566 ?
O5 Eu1 O5 98.2(7) . 4_566 ?
O2 Eu1 O3 82.9(4) 4_566 6_655 ?
O2 Eu1 O3 126.4(3) . 6_655 ?
O5 Eu1 O3 83.2(4) . 6_655 ?
O5 Eu1 O3 73.2(4) 4_566 6_655 ?
O2 Eu1 O3 126.4(3) 4_566 7_645 ?
O2 Eu1 O3 82.9(4) . 7_645 ?
O5 Eu1 O3 73.2(4) . 7_645 ?
O5 Eu1 O3 83.2(4) 4_566 7_645 ?
O3 Eu1 O3 143.7(4) 6_655 7_645 ?
O2 Eu1 O1 76.2(3) 4_566 7_645 ?
O2 Eu1 O1 83.1(3) . 7_645 ?
O5 Eu1 O1 124.3(4) . 7_645 ?
O5 Eu1 O1 75.5(4) 4_566 7_645 ?
O3 Eu1 O1 140.9(2) 6_655 7_645 ?
O3 Eu1 O1 51.1(2) 7_645 7_645 ?
O2 Eu1 O1 83.1(3) 4_566 6_655 ?
O2 Eu1 O1 76.2(3) . 6_655 ?
O5 Eu1 O1 75.5(4) . 6_655 ?
O5 Eu1 O1 124.3(4) 4_566 6_655 ?
O3 Eu1 O1 51.1(2) 6_655 6_655 ?
O3 Eu1 O1 140.9(2) 7_645 6_655 ?
O1 Eu1 O1 152.4(3) 7_645 6_655 ?
O2 Eu1 C12 100.9(3) 4_566 7_645 ?
O2 Eu1 C12 81.9(3) . 7_645 ?
O5 Eu1 C12 99.1(4) . 7_645 ?
O5 Eu1 C12 78.5(4) 4_566 7_645 ?
O3 Eu1 C12 151.6(3) 6_655 7_645 ?
O3 Eu1 C12 26.0(2) 7_645 7_645 ?
O1 Eu1 C12 25.2(2) 7_645 7_645 ?
O1 Eu1 C12 156.9(2) 6_655 7_645 ?
O2 Eu1 C12 81.9(3) 4_566 6_655 ?
O2 Eu1 C12 100.9(3) . 6_655 ?
O5 Eu1 C12 78.5(4) . 6_655 ?
O5 Eu1 C12 99.1(4) 4_566 6_655 ?
O3 Eu1 C12 26.0(2) 6_655 6_655 ?
O3 Eu1 C12 151.6(3) 7_645 6_655 ?
O1 Eu1 C12 156.9(2) 7_645 6_655 ?
O1 Eu1 C12 25.2(2) 6_655 6_655 ?
C12 Eu1 C12 176.4(4) 7_645 6_655 ?
O2 Eu1 Na1 45.8(3) 4_566 6_654 ?
O2 Eu1 Na1 84.8(3) . 6_654 ?
O5 Eu1 Na1 155.0(4) . 6_654 ?
O5 Eu1 Na1 77.1(3) 4_566 6_654 ?
O3 Eu1 Na1 117.8(2) 6_655 6_654 ?
O3 Eu1 Na1 81.9(2) 7_645 6_654 ?
O1 Eu1 Na1 30.74(15) 7_645 6_654 ?
O1 Eu1 Na1 127.68(15) 6_655 6_654 ?
C12 Eu1 Na1 55.91(19) 7_645 6_654 ?
C12 Eu1 Na1 126.4(2) 6_655 6_654 ?
O2 Eu1 Na1 84.8(3) 4_566 . ?
O2 Eu1 Na1 45.8(3) . . ?
O5 Eu1 Na1 77.1(3) . . ?
O5 Eu1 Na1 155.0(4) 4_566 . ?
O3 Eu1 Na1 81.9(2) 6_655 . ?
O3 Eu1 Na1 117.8(2) 7_645 . ?
O1 Eu1 Na1 127.68(15) 7_645 . ?
O1 Eu1 Na1 30.74(15) 6_655 . ?
C12 Eu1 Na1 126.4(2) 7_645 . ?
C12 Eu1 Na1 55.91(19) 6_655 . ?
Na1 Eu1 Na1 117.22(4) 6_654 . ?
Zn1' Zn1 N1 82.1(4) . 2_655 ?
Zn1' Zn1 N1 82.1(4) . . ?
N1 Zn1 N1 164.1(8) 2_655 . ?
Zn1' Zn1 N2 79.8(3) . 2_655 ?
N1 Zn1 N2 88.60(10) 2_655 2_655 ?
N1 Zn1 N2 88.60(10) . 2_655 ?
Zn1' Zn1 N2 79.8(3) . . ?
N1 Zn1 N2 88.60(10) 2_655 . ?
N1 Zn1 N2 88.60(10) . . ?
N2 Zn1 N2 159.6(7) 2_655 . ?
Zn1' Zn1 O6 180.000(12) . . ?
N1 Zn1 O6 97.9(4) 2_655 . ?
N1 Zn1 O6 97.9(4) . . ?
N2 Zn1 O6 100.2(3) 2_655 . ?
N2 Zn1 O6 100.2(3) . . ?
Zn1 Zn1' N1 77.4(4) . 2_655 ?
Zn1 Zn1' N1 77.4(4) . . ?
N1 Zn1' N1 154.9(8) 2_655 . ?
Zn1 Zn1' N2 80.0(3) . 2_655 ?
N1 Zn1' N2 87.83(11) 2_655 2_655 ?
N1 Zn1' N2 87.83(11) . 2_655 ?
Zn1 Zn1' N2 80.0(3) . . ?
N1 Zn1' N2 87.83(11) 2_655 . ?
N1 Zn1' N2 87.83(11) . . ?
N2 Zn1' N2 159.9(6) 2_655 . ?
Zn1 Zn1' O6' 180.000(12) . . ?
N1 Zn1' O6' 102.6(4) 2_655 . ?
N1 Zn1' O6' 102.6(4) . . ?
N2 Zn1' O6' 100.0(3) 2_655 . ?
N2 Zn1' O6' 100.0(3) . . ?
O5' Na1 O5' 130.9(8) . 7_646 ?
O5' Na1 O4 65.3(4) . . ?
O5' Na1 O4 86.3(4) 7_646 . ?
O5' Na1 O4 86.3(4) . 7_646 ?
O5' Na1 O4 65.3(4) 7_646 7_646 ?
O4 Na1 O4 109.0(6) . 7_646 ?
O5' Na1 O1 159.9(4) . 6_655 ?
O5' Na1 O1 66.6(4) 7_646 6_655 ?
O4 Na1 O1 111.9(3) . 6_655 ?
O4 Na1 O1 112.6(3) 7_646 6_655 ?
O5' Na1 O1 66.6(4) . 4_566 ?
O5' Na1 O1 159.9(4) 7_646 4_566 ?
O4 Na1 O1 112.6(3) . 4_566 ?
O4 Na1 O1 111.9(3) 7_646 4_566 ?
O1 Na1 O1 98.6(4) 6_655 4_566 ?
O5' Na1 C13 80.2(5) . 7_646 ?
O5' Na1 C13 85.3(4) 7_646 7_646 ?
O4 Na1 C13 124.6(5) . 7_646 ?
O4 Na1 C13 23.3(3) 7_646 7_646 ?
O1 Na1 C13 114.3(4) 6_655 7_646 ?
O1 Na1 C13 89.0(3) 4_566 7_646 ?
O5' Na1 C13 85.3(4) . . ?
O5' Na1 C13 80.2(5) 7_646 . ?
O4 Na1 C13 23.3(3) . . ?
O4 Na1 C13 124.6(5) 7_646 . ?
O1 Na1 C13 89.0(3) 6_655 . ?
O1 Na1 C13 114.3(4) 4_566 . ?
C13 Na1 C13 144.8(6) 7_646 . ?
O5' Na1 O2 67.1(4) . 7_646 ?
O5' Na1 O2 108.4(4) 7_646 7_646 ?
O4 Na1 O2 126.8(4) . 7_646 ?
O4 Na1 O2 45.4(3) 7_646 7_646 ?
O1 Na1 O2 120.9(3) 6_655 7_646 ?
O1 Na1 O2 66.5(3) 4_566 7_646 ?
C13 Na1 O2 23.2(3) 7_646 7_646 ?
C13 Na1 O2 150.0(4) . 7_646 ?
O5' Na1 O2 108.4(4) . . ?
O5' Na1 O2 67.1(4) 7_646 . ?
O4 Na1 O2 45.4(3) . . ?
O4 Na1 O2 126.8(4) 7_646 . ?
O1 Na1 O2 66.5(3) 6_655 . ?
O1 Na1 O2 120.9(3) 4_566 . ?
C13 Na1 O2 150.0(4) 7_646 . ?
C13 Na1 O2 23.2(3) . . ?
O2 Na1 O2 169.9(6) 7_646 . ?
O5' Na1 Eu1 140.3(3) . . ?
O5' Na1 Eu1 58.3(3) 7_646 . ?
O4 Na1 Eu1 78.7(3) . . ?
O4 Na1 Eu1 122.5(3) 7_646 . ?
O1 Na1 Eu1 33.55(17) 6_655 . ?
O1 Na1 Eu1 116.8(3) 4_566 . ?
C13 Na1 Eu1 137.0(3) 7_646 . ?
C13 Na1 Eu1 56.4(2) . . ?
O2 Na1 Eu1 152.5(2) 7_646 . ?
O2 Na1 Eu1 33.3(2) . . ?
O5' Na1 Eu1 58.3(3) . 6_655 ?
O5' Na1 Eu1 140.3(3) 7_646 6_655 ?
O4 Na1 Eu1 122.5(3) . 6_655 ?
O4 Na1 Eu1 78.7(3) 7_646 6_655 ?
O1 Na1 Eu1 116.8(3) 6_655 6_655 ?
O1 Na1 Eu1 33.55(17) 4_566 6_655 ?
C13 Na1 Eu1 56.4(2) 7_646 6_655 ?
C13 Na1 Eu1 137.0(3) . 6_655 ?
O2 Na1 Eu1 33.3(2) 7_646 6_655 ?
O2 Na1 Eu1 152.5(2) . 6_655 ?
Eu1 Na1 Eu1 145.94(18) . 6_655 ?
C12 O1 Na1 149.9(7) . 6_654 ?
C12 O1 Eu1 94.3(6) . 6_654 ?
Na1 O1 Eu1 115.7(3) 6_654 6_654 ?
C13 O2 Eu1 171.2(12) . . ?
C13 O2 Na1 74.6(8) . . ?
Eu1 O2 Na1 100.9(4) . . ?
C12 O3 Eu1 95.3(6) . 6_654 ?
C13 O4 Na1 113.4(8) . . ?
Eu1 O5 H5A 120.0 . . ?
Eu1 O5 H5B 120.0 . . ?
H5A O5 H5B 120.0 . . ?
Na1 O5' H5'1 120.0 . . ?
Na1 O5' H5'2 120.0 . . ?
H5'1 O5' H5'2 120.0 . . ?
Zn1 O6 H6A 120.4 . . ?
Zn1 O6 H6B 120.4 . . ?
H6A O6 H6B 119.3 . . ?
Zn1' O6' H6'1 120.0 . . ?
Zn1' O6' H6'2 120.0 . . ?
H6'1 O6' H6'2 120.0 . . ?
C9 N1 C9 107.3(10) . 12_655 ?
C9 N1 Zn1 125.8(5) . . ?
C9 N1 Zn1 125.8(5) 12_655 . ?
C9 N1 Zn1' 125.5(5) . . ?
C9 N1 Zn1' 125.5(5) 12_655 . ?
C6 N2 C6 107.0(9) 11_565 . ?
C6 N2 Zn1' 126.3(5) 11_565 . ?
C6 N2 Zn1' 126.3(5) . . ?
C6 N2 Zn1 125.0(5) 11_565 . ?
C6 N2 Zn1 125.0(5) . . ?
C6 C1 C9 126.6(8) . . ?
C6 C1 C5 116.5(7) . . ?
C9 C1 C5 116.9(7) . . ?
C10 C2 C5 120.9(8) . . ?
C10 C2 H2 119.6 . . ?
C5 C2 H2 119.6 . . ?
C5 C3 C4 120.8(8) . . ?
C5 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C7 C4 C3 119.2(8) . . ?
C7 C4 C12 119.0(7) . . ?
C3 C4 C12 121.7(7) . . ?
C3 C5 C2 119.8(8) . . ?
C3 C5 C1 118.7(8) . . ?
C2 C5 C1 121.5(8) . . ?
C1 C6 N2 125.0(7) . . ?
C1 C6 C8 125.4(7) . . ?
N2 C6 C8 109.6(7) . . ?
C10 C7 C4 119.0(8) . . ?
C10 C7 H7 120.5 . . ?
C4 C7 H7 120.5 . . ?
C8 C8 C6 106.8(5) 11_565 . ?
C8 C8 H8 126.6 11_565 . ?
C6 C8 H8 126.6 . . ?
C1 C9 N1 125.7(8) . . ?
C1 C9 C11 126.0(7) . . ?
N1 C9 C11 108.3(7) . . ?
C2 C10 C7 120.3(8) . . ?
C2 C10 C13 122.9(8) . . ?
C7 C10 C13 116.8(8) . . ?
C11 C11 C9 108.0(5) 12_655 . ?
C11 C11 H11 126.0 12_655 . ?
C9 C11 H11 126.0 . . ?
O1 C12 O3 119.2(9) . . ?
O1 C12 C4 123.2(8) . . ?
O3 C12 C4 117.6(8) . . ?
O1 C12 Eu1 60.5(5) . 6_654 ?
O3 C12 Eu1 58.7(5) . 6_654 ?
C4 C12 Eu1 176.1(6) . 6_654 ?
O2 C13 O4 121.8(13) . . ?
O2 C13 C10 121.5(10) . . ?
O4 C13 C10 116.7(11) . . ?
O2 C13 Na1 82.2(8) . . ?
C10 C13 Na1 151.1(10) . . ?

# SQUEEZE RESULTS (Version =  30715)
# 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 -0.016 -0.003 0.007 5822 2100 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
 Molecules of DMF solvent
;

_refine_diff_density_max         2.095
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.172




_exptl_crystal_recrystallization_method solvothermal
