# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_DyNaL
_database_code_depnum_ccdc_archive 'CCDC 1444210'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H20 Dy N8 Na O8'
_chemical_formula_weight         733.97

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'
Dy Dy -0.1892 4.4098 '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'
H H 0.0000 0.0000 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   18.0441(8)
_cell_length_b                   18.0441(8)
_cell_length_c                   8.3135(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2706.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10174
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      28.48

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_F_000             1444
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.840
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24638
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.257
_diffrn_reflns_theta_max         28.870
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1771
_reflns_number_gt                1406
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexII'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury Software (CCDC, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0784P)²+18.2372P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1771
_refine_ls_number_parameters     95
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1508
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_restrained_S_all      1.231
_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
Dy1 Dy 0.0000 0.2500 0.6250 0.0241(2) Uani 1 4 d S T P . .
Na1 Na 0.0000 0.2500 1.1250 0.0412(13) Uani 1 4 d S T P . .
C1 C 0.1318(4) 0.1921(3) 0.8595(9) 0.0322(15) Uani 1 1 d . . . . .
C2 C 0.1691(3) 0.1817(3) 0.7028(10) 0.0315(14) Uani 1 1 d . . . . .
C3 C 0.2398(4) 0.1497(4) 0.6870(10) 0.0374(15) Uani 1 1 d . . . . .
H3 H 0.2653 0.1337 0.7778 0.045 Uiso 1 1 calc R U . . .
C4 C 0.2712(4) 0.1420(4) 0.5382(9) 0.0363(15) Uani 1 1 d . . . . .
H4 H 0.3181 0.1211 0.5285 0.044 Uiso 1 1 calc R U . . .
C5 C 0.2336(3) 0.1650(3) 0.4019(9) 0.0298(14) Uani 1 1 d . . . . .
C6 C 0.1628(3) 0.1969(3) 0.4267(8) 0.0274(12) Uani 1 1 d . . . . .
H6 H 0.1364 0.2132 0.3373 0.033 Uiso 1 1 calc R U . . .
N1 N 0.1319(3) 0.2048(3) 0.5711(7) 0.0264(10) Uani 1 1 d . . . . .
N2 N 0.2628(3) 0.1565(3) 0.2535(7) 0.0351(12) Uani 1 1 d . . . . .
H2A H 0.3057 0.1364 0.2422 0.042 Uiso 1 1 calc R U . . .
H2B H 0.2386 0.1711 0.1704 0.042 Uiso 1 1 calc R U . . .
O1 O 0.0680(2) 0.2250(2) 0.8542(6) 0.0324(10) Uani 1 1 d . . . . .
O2 O 0.1591(3) 0.1683(3) 0.9845(7) 0.0452(13) 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 O1 2.311(5) 14_556 ?
Dy1 O1 2.311(5) 7_454 ?
Dy1 O1 2.311(5) 12_667 ?
Dy1 O1 2.311(5) . ?
Dy1 N1 2.555(5) . ?
Dy1 N1 2.555(5) 12_667 ?
Dy1 N1 2.555(5) 14_556 ?
Dy1 N1 2.555(5) 7_454 ?
Na1 O1 2.603(5) 12_668 ?
Na1 O1 2.603(5) 7_454 ?
Na1 O1 2.603(5) 14_557 ?
Na1 O1 2.603(5) . ?
C1 O2 1.228(8) . ?
C1 O1 1.296(8) . ?
C1 C2 1.479(11) . ?
C2 N1 1.351(9) . ?
C2 C3 1.406(9) . ?
C3 C4 1.367(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(10) . ?
C4 H4 0.9300 . ?
C5 N2 1.350(9) . ?
C5 C6 1.418(8) . ?
C6 N1 1.331(9) . ?
C6 H6 0.9300 . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O1 132.84(15) 14_556 7_454 ?
O1 Dy1 O1 68.9(2) 14_556 12_667 ?
O1 Dy1 O1 132.84(15) 7_454 12_667 ?
O1 Dy1 O1 132.84(15) 14_556 . ?
O1 Dy1 O1 68.9(2) 7_454 . ?
O1 Dy1 O1 132.84(15) 12_667 . ?
O1 Dy1 N1 82.42(16) 14_556 . ?
O1 Dy1 N1 134.54(18) 7_454 . ?
O1 Dy1 N1 80.95(16) 12_667 . ?
O1 Dy1 N1 65.65(18) . . ?
O1 Dy1 N1 134.54(18) 14_556 12_667 ?
O1 Dy1 N1 80.95(16) 7_454 12_667 ?
O1 Dy1 N1 65.65(18) 12_667 12_667 ?
O1 Dy1 N1 82.42(16) . 12_667 ?
N1 Dy1 N1 91.76(5) . 12_667 ?
O1 Dy1 N1 65.65(18) 14_556 14_556 ?
O1 Dy1 N1 82.42(16) 7_454 14_556 ?
O1 Dy1 N1 134.54(18) 12_667 14_556 ?
O1 Dy1 N1 80.95(16) . 14_556 ?
N1 Dy1 N1 91.76(5) . 14_556 ?
N1 Dy1 N1 159.8(3) 12_667 14_556 ?
O1 Dy1 N1 80.95(16) 14_556 7_454 ?
O1 Dy1 N1 65.65(18) 7_454 7_454 ?
O1 Dy1 N1 82.42(16) 12_667 7_454 ?
O1 Dy1 N1 134.54(18) . 7_454 ?
N1 Dy1 N1 159.8(3) . 7_454 ?
N1 Dy1 N1 91.76(5) 12_667 7_454 ?
N1 Dy1 N1 91.76(5) 14_556 7_454 ?
O1 Na1 O1 138.40(13) 12_668 7_454 ?
O1 Na1 O1 60.29(19) 12_668 14_557 ?
O1 Na1 O1 138.40(13) 7_454 14_557 ?
O1 Na1 O1 138.40(13) 12_668 . ?
O1 Na1 O1 60.29(19) 7_454 . ?
O1 Na1 O1 138.40(13) 14_557 . ?
O2 C1 O1 123.0(7) . . ?
O2 C1 C2 121.2(6) . . ?
O1 C1 C2 115.7(6) . . ?
N1 C2 C3 120.1(7) . . ?
N1 C2 C1 116.6(6) . . ?
C3 C2 C1 123.3(6) . . ?
C4 C3 C2 120.1(7) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.5(6) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N2 C5 C4 121.5(6) . . ?
N2 C5 C6 122.1(6) . . ?
C4 C5 C6 116.4(6) . . ?
N1 C6 C5 123.5(6) . . ?
N1 C6 H6 118.2 . . ?
C5 C6 H6 118.2 . . ?
C6 N1 C2 119.3(5) . . ?
C6 N1 Dy1 125.6(4) . . ?
C2 N1 Dy1 114.8(5) . . ?
C5 N2 H2A 120.0 . . ?
C5 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 O1 Dy1 126.1(4) . . ?
C1 O1 Na1 117.9(4) . . ?
Dy1 O1 Na1 115.40(18) . . ?

_refine_diff_density_max         1.203
_refine_diff_density_min         -2.381
_refine_diff_density_rms         0.327

_shelxl_version_number           2014-3

