# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_DYMUREX
_database_code_depnum_ccdc_archive 'CCDC 1409034'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-09-18 downloaded from the CCDC.
;

_audit_creation_date             2014-09-05T14:49:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H12 Dy N15 O18'
_chemical_formula_sum            'C24 H12 Dy N15 O18'
_chemical_formula_weight         960.99
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_Int_Tables_number      56
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.4420(3)
_cell_length_b                   17.2570(3)
_cell_length_c                   19.7040(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4230.68(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2644
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      25.94
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_T_max  0.964


#----------------------------------------------------------------------------#
#                   SQUEEZE RESULTS                                          #
#----------------------------------------------------------------------------#

# 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 -0.250 0.250 0.260 343 232 ' '
2 -0.250 0.250 0.760 343 233 ' '
3 0.250 0.750 0.240 338 227 ' '
4 0.250 0.750 0.740 338 227 ' '
_platon_squeeze_details          
;
;

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_number            20045
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        27.5
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             4848
_reflns_number_gt                3140
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0810P)²+0.0000P] 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_number_reflns         4848
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.143
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.797
_refine_diff_density_min         -1.63
_refine_diff_density_rms         0.248

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.25 0.25 0.415317(17) 0.01145(13) Uani 1 2 d S . .
O2 O 0.2382(2) 0.3534(2) 0.49300(19) 0.0142(8) Uani 1 1 d . . .
N7 N 0.0751(4) 0.2564(2) 0.4848(2) 0.0128(9) Uani 1 1 d . . .
N8 N 0.25 0.25 0.2849(4) 0.0165(14) Uani 1 2 d S . .
O5 O 0.1184(3) 0.1567(2) 0.3846(2) 0.0181(8) Uani 1 1 d . . .
O6 O 0.3710(3) 0.1627(2) 0.3657(2) 0.0192(9) Uani 1 1 d . . .
N1 N -0.1143(3) 0.0971(2) 0.5159(2) 0.0189(10) Uani 1 1 d . . .
H201 H -0.1632 0.0802 0.5446 0.023 Uiso 1 1 calc R . .
O8 O 0.0483(4) 0.5327(2) 0.6079(2) 0.0316(11) Uani 1 1 d . . .
N2 N -0.0156(4) 0.0772(3) 0.4165(2) 0.0164(10) Uani 1 1 d . . .
H200 H -0.0018 0.0485 0.3806 0.02 Uiso 1 1 calc R . .
O11 O -0.1346(3) 0.3257(2) 0.5250(2) 0.0261(10) Uani 1 1 d . . .
C12 C -0.0632(4) 0.1662(3) 0.5323(3) 0.0188(12) Uani 1 1 d . . .
O13 O -0.0774(3) 0.1961(2) 0.5870(2) 0.0254(10) Uani 1 1 d . . .
O14 O -0.1458(3) -0.0074(2) 0.4480(2) 0.0268(10) Uani 1 1 d . . .
N3 N -0.0416(4) 0.4258(3) 0.5706(2) 0.0218(11) Uani 1 1 d . . .
H202 H -0.1022 0.4446 0.5868 0.026 Uiso 1 1 calc R . .
C16 C 0.0126(4) 0.1931(3) 0.4804(3) 0.0139(11) Uani 1 1 d . . .
N6 N 0.4449(4) 0.0995(3) 0.2779(2) 0.0230(11) Uani 1 1 d . . .
H204 H 0.4921 0.079 0.3058 0.028 Uiso 1 1 calc R . .
C18 C 0.0581(4) 0.3213(3) 0.5185(3) 0.0162(12) Uani 1 1 d . . .
N4 N 0.1404(4) 0.4416(2) 0.5501(2) 0.0189(10) Uani 1 1 d . . .
H203 H 0.1979 0.4714 0.5515 0.023 Uiso 1 1 calc R . .
N5 N 0.3755(4) 0.1102(3) 0.1682(2) 0.0260(12) Uani 1 1 d . . .
H205 H 0.3796 0.0979 0.1249 0.031 Uiso 1 1 calc R . .
O21 O 0.2192(4) 0.1768(3) 0.1499(2) 0.0362(13) Uani 1 1 d . . .
C22 C -0.0471(4) 0.3538(3) 0.5387(3) 0.0187(12) Uani 1 1 d . . .
O23 O 0.5087(4) 0.0254(3) 0.1924(2) 0.0363(12) Uani 1 1 d . . .
C24 C 0.3078(5) 0.1961(3) 0.2562(3) 0.0217(13) Uani 1 1 d . . .
C25 C 0.3749(4) 0.1517(3) 0.3034(3) 0.0172(12) Uani 1 1 d . . .
C27 C 0.0439(4) 0.1419(3) 0.4254(3) 0.0136(11) Uani 1 1 d . . .
C29 C 0.1506(4) 0.3714(3) 0.5191(3) 0.0157(11) Uani 1 1 d . . .
C31 C 0.2964(5) 0.1627(4) 0.1871(3) 0.0242(13) Uani 1 1 d . . .
C32 C 0.4470(5) 0.0764(3) 0.2108(3) 0.0272(14) Uani 1 1 d . . .
C33 C -0.0960(4) 0.0527(3) 0.4593(3) 0.0217(13) Uani 1 1 d . . .
C35 C 0.0481(5) 0.4701(3) 0.5793(3) 0.0219(13) Uani 1 1 d . . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O6 2.344(4) . ?
Dy1 O6 2.344(4) 2 ?
Dy1 O2 2.356(4) 2 ?
Dy1 O2 2.356(4) . ?
Dy1 O5 2.375(4) 2 ?
Dy1 O5 2.375(4) . ?
Dy1 N8 2.570(7) . ?
Dy1 N7 2.573(5) 2 ?
Dy1 N7 2.573(5) . ?
O2 C29 1.244(6) . ?
N7 C18 1.319(6) . ?
N7 C16 1.342(6) . ?
N8 C24 1.304(7) 2 ?
N8 C24 1.305(7) . ?
O5 C27 1.253(6) . ?
O6 C25 1.244(7) . ?
N1 C33 1.372(7) . ?
N1 C12 1.390(6) . ?
N1 H201 0.88 . ?
O8 C35 1.219(7) . ?
N2 C27 1.352(6) . ?
N2 C33 1.375(7) . ?
N2 H200 0.88 . ?
O11 C22 1.221(6) . ?
C12 O13 1.209(7) . ?
C12 C16 1.467(7) . ?
O14 C33 1.229(6) . ?
N3 C35 1.364(7) . ?
N3 C22 1.394(7) . ?
N3 H202 0.88 . ?
C16 C27 1.452(7) . ?
N6 C25 1.348(7) . ?
N6 C32 1.381(8) . ?
N6 H204 0.88 . ?
C18 C29 1.439(7) . ?
C18 C22 1.479(7) . ?
N4 C29 1.364(6) . ?
N4 C35 1.376(7) . ?
N4 H203 0.88 . ?
N5 C32 1.356(8) . ?
N5 C31 1.389(8) . ?
N5 H205 0.88 . ?
O21 C31 1.232(8) . ?
O23 C32 1.223(7) . ?
C24 C25 1.466(8) . ?
C24 C31 1.485(8) . ?


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
O6 Dy1 O6 130.71(19) . 2 ?
O6 Dy1 O2 75.15(13) . 2 ?
O6 Dy1 O2 142.95(12) 2 2 ?
O6 Dy1 O2 142.95(12) . . ?
O6 Dy1 O2 75.15(13) 2 . ?
O2 Dy1 O2 98.94(19) 2 . ?
O6 Dy1 O5 83.50(14) . 2 ?
O6 Dy1 O5 84.30(14) 2 2 ?
O2 Dy1 O5 129.50(12) 2 2 ?
O2 Dy1 O5 72.24(13) . 2 ?
O6 Dy1 O5 84.30(14) . . ?
O6 Dy1 O5 83.50(14) 2 . ?
O2 Dy1 O5 72.24(13) 2 . ?
O2 Dy1 O5 129.50(12) . . ?
O5 Dy1 O5 150.49(19) 2 . ?
O6 Dy1 N8 65.36(10) . . ?
O6 Dy1 N8 65.36(10) 2 . ?
O2 Dy1 N8 130.53(9) 2 . ?
O2 Dy1 N8 130.53(9) . . ?
O5 Dy1 N8 75.24(10) 2 . ?
O5 Dy1 N8 75.25(10) . . ?
O6 Dy1 N7 69.60(13) . 2 ?
O6 Dy1 N7 142.42(13) 2 2 ?
O2 Dy1 N7 64.48(12) 2 2 ?
O2 Dy1 N7 74.88(12) . 2 ?
O5 Dy1 N7 65.25(13) 2 2 ?
O5 Dy1 N7 133.60(12) . 2 ?
N8 Dy1 N7 122.15(10) . 2 ?
O6 Dy1 N7 142.42(13) . . ?
O6 Dy1 N7 69.60(13) 2 . ?
O2 Dy1 N7 74.88(12) 2 . ?
O2 Dy1 N7 64.48(12) . . ?
O5 Dy1 N7 133.61(12) 2 . ?
O5 Dy1 N7 65.26(13) . . ?
N8 Dy1 N7 122.16(10) . . ?
N7 Dy1 N7 115.69(19) 2 . ?
C29 O2 Dy1 120.8(3) . . ?
C18 N7 C16 129.0(5) . . ?
C18 N7 Dy1 116.1(3) . . ?
C16 N7 Dy1 114.9(3) . . ?
C24 N8 C24 128.7(8) 2 . ?
C24 N8 Dy1 115.7(4) 2 . ?
C24 N8 Dy1 115.7(4) . . ?
C27 O5 Dy1 119.0(3) . . ?
C25 O6 Dy1 122.4(3) . . ?
C33 N1 C12 126.3(5) . . ?
C33 N1 H201 116.8 . . ?
C12 N1 H201 116.8 . . ?
C27 N2 C33 125.0(5) . . ?
C27 N2 H200 117.5 . . ?
C33 N2 H200 117.5 . . ?
O13 C12 N1 120.5(5) . . ?
O13 C12 C16 125.5(5) . . ?
N1 C12 C16 113.9(5) . . ?
C35 N3 C22 126.6(5) . . ?
C35 N3 H202 116.7 . . ?
C22 N3 H202 116.7 . . ?
N7 C16 C27 112.8(5) . . ?
N7 C16 C12 125.8(5) . . ?
C27 C16 C12 120.0(5) . . ?
C25 N6 C32 124.2(5) . . ?
C25 N6 H204 117.9 . . ?
C32 N6 H204 117.9 . . ?
N7 C18 C29 112.7(5) . . ?
N7 C18 C22 126.8(5) . . ?
C29 C18 C22 118.6(5) . . ?
C29 N4 C35 125.6(5) . . ?
C29 N4 H203 117.2 . . ?
C35 N4 H203 117.2 . . ?
C32 N5 C31 125.4(5) . . ?
C32 N5 H205 117.3 . . ?
C31 N5 H205 117.3 . . ?
O11 C22 N3 119.8(5) . . ?
O11 C22 C18 125.4(5) . . ?
N3 C22 C18 114.6(5) . . ?
N8 C24 C25 114.3(5) . . ?
N8 C24 C31 128.4(6) . . ?
C25 C24 C31 115.7(5) . . ?
O6 C25 N6 119.7(5) . . ?
O6 C25 C24 121.6(5) . . ?
N6 C25 C24 118.7(5) . . ?
O5 C27 N2 119.3(5) . . ?
O5 C27 C16 123.6(5) . . ?
N2 C27 C16 117.0(5) . . ?
O2 C29 N4 119.2(5) . . ?
O2 C29 C18 123.2(5) . . ?
N4 C29 C18 117.6(5) . . ?
O21 C31 N5 121.3(6) . . ?
O21 C31 C24 123.0(6) . . ?
N5 C31 C24 115.6(5) . . ?
O23 C32 N5 122.5(6) . . ?
O23 C32 N6 120.3(6) . . ?
N5 C32 N6 117.1(5) . . ?
O14 C33 N1 122.3(5) . . ?
O14 C33 N2 121.0(5) . . ?
N1 C33 N2 116.6(5) . . ?
O8 C35 N3 123.8(5) . . ?
O8 C35 N4 120.6(5) . . ?
N3 C35 N4 115.5(5) . . ?


#----------------------------------------------------------------------------#
# END OF CIF FILE FOR DYMUREX                                                #
#----------------------------------------------------------------------------#
_exptl_crystal_preparation       'Magnetic properties'
