# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_1
_database_code_depnum_ccdc_archive 'CCDC 1436291'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 [Zn2(oPDA)2] 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H6 N2 O8 Zn2'
_chemical_formula_sum            'C14 H6 N2 O8 Zn2'
_chemical_formula_weight         460.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.057(7)
_cell_length_b                   14.017(7)
_cell_length_c                   16.702(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.938(9)
_cell_angle_gamma                90.00
_cell_volume                     3231(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1467
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      23.9

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    3.017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6280
_exptl_absorpt_correction_T_max  0.7730
_exptl_absorpt_process_details   sadabs(1997)

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart ApecII CCD diffractometer'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10867
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.49
_reflns_number_total             3711
_reflns_number_gt                2277
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0449P)²+0.5757P] 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         3711
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.1083
_refine_ls_wR_factor_gt          0.0924
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.23993(3) 0.94455(3) 0.19081(3) 0.03679(15) Uani 1 1 d . . .
Zn2 Zn 0.5000 1.19284(5) 0.2500 0.03441(18) Uani 1 2 d S . .
Zn3 Zn 0.0000 1.19252(5) 0.2500 0.0439(2) Uani 1 2 d S . .
O1 O -0.1137(2) 1.2996(2) 0.21843(16) 0.0466(8) Uani 1 1 d . . .
O2 O -0.20284(19) 1.37108(19) 0.11128(16) 0.0439(7) Uani 1 1 d . . .
O3 O 0.1004(2) 1.0858(2) 0.21946(16) 0.0466(8) Uani 1 1 d . . .
O4 O 0.14818(19) 1.0205(2) 0.11244(16) 0.0439(7) Uani 1 1 d . . .
O5 O 0.35243(19) 1.0496(2) 0.22364(17) 0.0462(7) Uani 1 1 d . . .
O6 O 0.44624(19) 1.1170(2) 0.33098(17) 0.0455(7) Uani 1 1 d . . .
O7 O 0.14025(19) 0.8375(2) 0.22327(16) 0.0453(7) Uani 1 1 d . . .
O8 O 0.09494(18) 0.76667(19) 0.32879(15) 0.0392(7) Uani 1 1 d . . .
N1 N -0.0246(2) 1.1950(2) 0.12725(17) 0.0284(7) Uani 1 1 d . . .
N2 N 0.26996(19) 0.9396(2) 0.31450(16) 0.0264(7) Uani 1 1 d . . .
C1 C -0.1397(3) 1.3126(3) 0.1437(2) 0.0355(9) Uani 1 1 d . . .
C2 C -0.0906(3) 1.2541(3) 0.0875(2) 0.0324(9) Uani 1 1 d . . .
C3 C -0.1090(3) 1.2571(3) 0.0037(2) 0.0408(10) Uani 1 1 d . . .
H3A H -0.1558 1.2981 -0.0243 0.049 Uiso 1 1 calc R . .
C4 C -0.0569(3) 1.1983(3) -0.0378(2) 0.0431(11) Uani 1 1 d . . .
H4A H -0.0678 1.1999 -0.0945 0.052 Uiso 1 1 calc R . .
C5 C 0.0114(3) 1.1369(3) 0.0045(2) 0.0397(10) Uani 1 1 d . . .
H5A H 0.0466 1.0962 -0.0228 0.048 Uiso 1 1 calc R . .
C6 C 0.0259(3) 1.1378(3) 0.0882(2) 0.0315(8) Uani 1 1 d . . .
C7 C 0.0974(3) 1.0767(3) 0.1449(2) 0.0352(9) Uani 1 1 d . . .
C8 C 0.3831(3) 1.0585(3) 0.2982(3) 0.0387(10) Uani 1 1 d . . .
C9 C 0.3395(3) 0.9942(3) 0.3544(2) 0.0336(9) Uani 1 1 d . . .
C10 C 0.3658(3) 0.9890(3) 0.4377(3) 0.0477(11) Uani 1 1 d . . .
H10A H 0.4151 1.0278 0.4651 0.057 Uiso 1 1 calc R . .
C11 C 0.3192(3) 0.9261(3) 0.4806(3) 0.0498(12) Uani 1 1 d . . .
H11A H 0.3361 0.9218 0.5371 0.060 Uiso 1 1 calc R . .
C12 C 0.2464(3) 0.8695(3) 0.4372(2) 0.0426(10) Uani 1 1 d . . .
H12A H 0.2132 0.8262 0.4640 0.051 Uiso 1 1 calc R . .
C13 C 0.2243(3) 0.8785(3) 0.3538(2) 0.0312(8) Uani 1 1 d . . .
C14 C 0.1471(3) 0.8226(3) 0.2976(2) 0.0347(9) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0406(3) 0.0400(3) 0.0304(3) 0.0022(2) 0.0083(2) 0.0025(2)
Zn2 0.0344(4) 0.0371(4) 0.0311(3) 0.000 0.0046(3) 0.000
Zn3 0.0535(5) 0.0540(5) 0.0235(3) 0.000 0.0060(3) 0.000
O1 0.0568(19) 0.054(2) 0.0307(16) -0.0034(14) 0.0119(13) 0.0193(14)
O2 0.0435(17) 0.0445(18) 0.0431(16) 0.0038(14) 0.0070(13) 0.0192(13)
O3 0.0515(19) 0.055(2) 0.0306(16) 0.0071(14) 0.0024(13) 0.0186(14)
O4 0.0457(18) 0.0460(18) 0.0411(16) 0.0001(14) 0.0110(13) 0.0174(13)
O5 0.0483(18) 0.0490(19) 0.0421(17) 0.0071(14) 0.0108(14) -0.0156(13)
O6 0.0438(17) 0.0398(18) 0.0541(18) -0.0027(14) 0.0118(14) -0.0161(13)
O7 0.0521(19) 0.0505(19) 0.0315(15) -0.0024(14) 0.0031(13) -0.0195(14)
O8 0.0387(16) 0.0413(17) 0.0375(15) 0.0013(13) 0.0068(12) -0.0166(13)
N1 0.0290(18) 0.0315(19) 0.0252(16) -0.0024(13) 0.0060(13) 0.0044(13)
N2 0.0263(17) 0.0260(17) 0.0275(16) -0.0015(13) 0.0067(13) -0.0030(13)
C1 0.035(2) 0.033(2) 0.039(2) 0.0001(18) 0.0085(18) 0.0016(17)
C2 0.033(2) 0.036(2) 0.0276(19) -0.0026(17) 0.0047(16) 0.0024(16)
C3 0.042(2) 0.047(3) 0.030(2) 0.0040(19) 0.0004(18) 0.0058(19)
C4 0.053(3) 0.053(3) 0.0205(19) 0.0022(18) 0.0020(18) 0.002(2)
C5 0.045(2) 0.047(3) 0.029(2) -0.0067(19) 0.0125(18) 0.0062(19)
C6 0.030(2) 0.035(2) 0.029(2) -0.0011(17) 0.0051(16) 0.0022(16)
C7 0.033(2) 0.034(2) 0.038(2) -0.0010(18) 0.0027(18) 0.0037(16)
C8 0.034(2) 0.033(2) 0.051(3) 0.004(2) 0.0136(19) -0.0019(18)
C9 0.034(2) 0.029(2) 0.037(2) -0.0016(18) 0.0067(17) 0.0025(16)
C10 0.042(3) 0.052(3) 0.046(3) -0.004(2) -0.001(2) -0.014(2)
C11 0.057(3) 0.059(3) 0.029(2) 0.003(2) -0.003(2) -0.011(2)
C12 0.044(3) 0.047(3) 0.036(2) 0.009(2) 0.0059(18) -0.0122(19)
C13 0.032(2) 0.031(2) 0.030(2) 0.0001(17) 0.0056(16) -0.0001(16)
C14 0.034(2) 0.036(2) 0.034(2) -0.0035(18) 0.0074(17) -0.0011(17)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.967(3) . ?
Zn1 O2 1.969(3) 3_545 ?
Zn1 N2 2.030(3) . ?
Zn1 O5 2.155(3) . ?
Zn1 O7 2.190(3) . ?
Zn2 O8 1.979(2) 4 ?
Zn2 O8 1.979(2) 3 ?
Zn2 O6 1.979(3) 2_655 ?
Zn2 O6 1.979(3) . ?
Zn3 N1 2.014(3) . ?
Zn3 N1 2.014(3) 2 ?
Zn3 O3 2.183(3) . ?
Zn3 O3 2.183(3) 2 ?
Zn3 O1 2.183(3) . ?
Zn3 O1 2.183(3) 2 ?
O1 C1 1.245(5) . ?
O2 C1 1.254(4) . ?
O2 Zn1 1.969(3) 3_455 ?
O3 C7 1.244(5) . ?
O4 C7 1.253(4) . ?
O5 C8 1.244(5) . ?
O6 C8 1.255(5) . ?
O7 C14 1.244(5) . ?
O8 C14 1.253(4) . ?
O8 Zn2 1.979(2) 3_445 ?
N1 C6 1.322(4) . ?
N1 C2 1.324(4) . ?
N2 C13 1.318(4) . ?
N2 C9 1.318(4) . ?
C1 C2 1.508(5) . ?
C2 C3 1.374(5) . ?
C3 C4 1.375(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.381(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.373(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.511(5) . ?
C8 C9 1.513(5) . ?
C9 C10 1.372(5) . ?
C10 C11 1.378(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.385(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.375(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.512(5) . ?

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
O4 Zn1 O2 97.73(11) . 3_545 ?
O4 Zn1 N2 132.77(11) . . ?
O2 Zn1 N2 129.50(11) 3_545 . ?
O4 Zn1 O5 98.99(12) . . ?
O2 Zn1 O5 98.93(12) 3_545 . ?
N2 Zn1 O5 76.31(11) . . ?
O4 Zn1 O7 99.56(12) . . ?
O2 Zn1 O7 99.85(12) 3_545 . ?
N2 Zn1 O7 75.17(10) . . ?
O5 Zn1 O7 151.46(10) . . ?
O8 Zn2 O8 116.95(16) 4 3 ?
O8 Zn2 O6 97.06(11) 4 2_655 ?
O8 Zn2 O6 116.00(12) 3 2_655 ?
O8 Zn2 O6 116.00(12) 4 . ?
O8 Zn2 O6 97.06(11) 3 . ?
O6 Zn2 O6 115.07(17) 2_655 . ?
N1 Zn3 N1 178.02(17) . 2 ?
N1 Zn3 O3 76.57(11) . . ?
N1 Zn3 O3 104.83(11) 2 . ?
N1 Zn3 O3 104.83(11) . 2 ?
N1 Zn3 O3 76.57(11) 2 2 ?
O3 Zn3 O3 93.47(16) . 2 ?
N1 Zn3 O1 76.45(11) . . ?
N1 Zn3 O1 102.15(11) 2 . ?
O3 Zn3 O1 153.02(9) . . ?
O3 Zn3 O1 92.93(12) 2 . ?
N1 Zn3 O1 102.15(11) . 2 ?
N1 Zn3 O1 76.46(11) 2 2 ?
O3 Zn3 O1 92.93(12) . 2 ?
O3 Zn3 O1 153.02(9) 2 2 ?
O1 Zn3 O1 93.15(16) . 2 ?
C1 O1 Zn3 113.8(2) . . ?
C1 O2 Zn1 113.4(3) . 3_455 ?
C7 O3 Zn3 113.8(2) . . ?
C7 O4 Zn1 114.0(2) . . ?
C8 O5 Zn1 114.9(3) . . ?
C8 O6 Zn2 112.5(3) . . ?
C14 O7 Zn1 115.4(2) . . ?
C14 O8 Zn2 115.1(2) . 3_445 ?
C6 N1 C2 121.5(3) . . ?
C6 N1 Zn3 119.2(2) . . ?
C2 N1 Zn3 119.3(2) . . ?
C13 N2 C9 120.7(3) . . ?
C13 N2 Zn1 120.1(2) . . ?
C9 N2 Zn1 119.0(2) . . ?
O1 C1 O2 125.3(4) . . ?
O1 C1 C2 117.6(3) . . ?
O2 C1 C2 117.2(3) . . ?
N1 C2 C3 120.6(4) . . ?
N1 C2 C1 112.8(3) . . ?
C3 C2 C1 126.6(3) . . ?
C2 C3 C4 118.7(4) . . ?
C2 C3 H3A 120.7 . . ?
C4 C3 H3A 120.7 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C6 C5 C4 118.0(4) . . ?
C6 C5 H5A 121.0 . . ?
C4 C5 H5A 121.0 . . ?
N1 C6 C5 121.2(3) . . ?
N1 C6 C7 113.0(3) . . ?
C5 C6 C7 125.8(3) . . ?
O3 C7 O4 125.7(4) . . ?
O3 C7 C6 117.5(3) . . ?
O4 C7 C6 116.8(3) . . ?
O5 C8 O6 125.8(4) . . ?
O5 C8 C9 117.2(3) . . ?
O6 C8 C9 117.0(4) . . ?
N2 C9 C10 120.9(4) . . ?
N2 C9 C8 112.4(3) . . ?
C10 C9 C8 126.7(4) . . ?
C9 C10 C11 119.9(4) . . ?
C9 C10 H10A 120.1 . . ?
C11 C10 H10A 120.1 . . ?
C10 C11 C12 118.2(4) . . ?
C10 C11 H11A 120.9 . . ?
C12 C11 H11A 120.9 . . ?
C13 C12 C11 118.6(4) . . ?
C13 C12 H12A 120.7 . . ?
C11 C12 H12A 120.7 . . ?
N2 C13 C12 121.8(3) . . ?
N2 C13 C14 112.8(3) . . ?
C12 C13 C14 125.5(4) . . ?
O7 C14 O8 125.4(4) . . ?
O7 C14 C13 116.4(3) . . ?
O8 C14 C13 118.2(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.082
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1436292'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H18 Ca Cl2 N6 O24 Pb6'
_chemical_formula_sum            'C42 H18 Ca Cl2 N6 O24 Pb6'
_chemical_formula_weight         2344.74

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   12.9099(17)
_cell_length_b                   12.9099(17)
_cell_length_c                   25.375(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3662.6(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4262
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.35

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3150
_exptl_absorpt_coefficient_mu    20.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1092
_exptl_absorpt_correction_T_max  0.1251
_exptl_absorpt_process_details   sadabs(1997)

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart ApecII CCD diffracmeter'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6616
_diffrn_reflns_av_R_equivalents  0.1581
_diffrn_reflns_av_sigmaI/netI    0.1130
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1445
_reflns_number_gt                1329
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0469P)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_extinction_coef       ?
_refine_ls_number_reflns         1445
_refine_ls_number_parameters     123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.02524(3) 0.79479(3) 0.163772(15) 0.0160(2) Uani 1 1 d . . .
Ca1 Ca -0.3333 0.3333 0.3333 0.0102(9) Uani 1 6 d S . .
Cl1 Cl 0.0000 1.0000 0.2173(2) 0.0319(11) Uani 1 3 d S . .
O1 O 0.2502(5) 0.9191(5) 0.1899(3) 0.0281(16) Uani 1 1 d . . .
O2 O 0.3949(6) 0.9322(7) 0.2401(4) 0.053(3) Uani 1 1 d . . .
O3 O -0.1472(5) 0.6434(5) 0.2196(3) 0.0223(15) Uani 1 1 d . . .
O4 O -0.2053(5) 0.4944(5) 0.2775(3) 0.0182(14) Uani 1 1 d . . .
N1 N 0.0820(6) 0.7325(5) 0.2469(3) 0.0144(16) Uani 1 1 d . . .
C1 C 0.2879(8) 0.8862(9) 0.2275(5) 0.025(3) Uani 1 1 d . . .
C2 C 0.1970(7) 0.7858(7) 0.2631(4) 0.017(2) Uani 1 1 d . . .
C3 C 0.2309(7) 0.7563(7) 0.3089(4) 0.024(2) Uani 1 1 d . . .
H3A H 0.3114 0.7914 0.3178 0.028 Uiso 1 1 calc R . .
C4 C 0.1442(8) 0.6736(8) 0.3420(5) 0.022(2) Uani 1 1 d . . .
H4A H 0.1649 0.6548 0.3742 0.026 Uiso 1 1 calc R . .
C5 C 0.0243(7) 0.6184(7) 0.3261(4) 0.0150(19) Uani 1 1 d . . .
H5A H -0.0363 0.5630 0.3477 0.018 Uiso 1 1 calc R . .
C6 C -0.0019(7) 0.6485(6) 0.2771(4) 0.013(2) Uani 1 1 d . . .
C7 C -0.1278(7) 0.5908(8) 0.2567(5) 0.018(2) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0145(2) 0.0131(2) 0.0163(3) 0.00091(14) 0.00009(14) 0.00373(14)
Ca1 0.0070(10) 0.0070(10) 0.017(2) 0.000 0.000 0.0035(5)
Cl1 0.0345(13) 0.0345(13) 0.027(3) 0.000 0.000 0.0172(6)
O1 0.016(3) 0.028(3) 0.027(4) 0.015(4) 0.009(3) 0.001(3)
O2 0.014(3) 0.060(5) 0.067(7) 0.022(5) -0.003(4) 0.005(3)
O3 0.016(3) 0.026(3) 0.022(4) 0.010(4) -0.002(3) 0.009(3)
O4 0.012(3) 0.014(3) 0.021(4) 0.002(3) 0.006(3) 0.001(2)
N1 0.015(3) 0.014(3) 0.018(4) 0.003(4) 0.005(4) 0.010(3)
C1 0.019(5) 0.029(5) 0.026(7) -0.001(6) 0.013(5) 0.011(4)
C2 0.010(4) 0.010(4) 0.028(6) -0.006(5) 0.003(5) 0.002(3)
C3 0.016(4) 0.021(4) 0.037(7) -0.009(5) -0.011(5) 0.011(4)
C4 0.021(4) 0.019(4) 0.027(6) 0.002(5) -0.014(5) 0.011(4)
C5 0.015(4) 0.013(4) 0.015(5) 0.002(5) 0.001(4) 0.005(3)
C6 0.017(4) 0.004(3) 0.016(5) -0.002(4) -0.009(4) 0.005(3)
C7 0.011(4) 0.017(4) 0.024(6) -0.007(5) 0.002(4) 0.006(4)

_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
Pb1 N1 2.493(7) . ?
Pb1 O3 2.536(6) . ?
Pb1 O1 2.605(6) . ?
Pb1 O1 2.620(6) 15 ?
Pb1 O2 2.628(8) 15 ?
Pb1 O3 2.683(6) 13_465 ?
Ca1 O4 2.372(6) 18 ?
Ca1 O4 2.372(6) 16_455 ?
Ca1 O4 2.372(6) 3_455 ?
Ca1 O4 2.372(6) 17_445 ?
Ca1 O4 2.372(6) . ?
Ca1 O4 2.372(6) 2_565 ?
O1 C1 1.240(13) . ?
O1 Pb1 2.620(6) 14_455 ?
O2 C1 1.241(12) . ?
O2 Pb1 2.628(8) 14_455 ?
O3 C7 1.257(12) . ?
O3 Pb1 2.683(6) 13_465 ?
O4 C7 1.258(11) . ?
N1 C6 1.328(10) . ?
N1 C2 1.351(10) . ?
C1 C2 1.533(13) . ?
C2 C3 1.363(14) . ?
C3 C4 1.379(14) . ?
C3 H3A 0.9300 . ?
C4 C5 1.401(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.394(13) . ?
C5 H5A 0.9300 . ?
C6 C7 1.501(11) . ?

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
N1 Pb1 O3 64.2(2) . . ?
N1 Pb1 O1 64.3(2) . . ?
O3 Pb1 O1 127.7(2) . . ?
N1 Pb1 O1 74.9(2) . 15 ?
O3 Pb1 O1 72.4(2) . 15 ?
O1 Pb1 O1 102.7(3) . 15 ?
N1 Pb1 O2 100.9(3) . 15 ?
O3 Pb1 O2 121.6(2) . 15 ?
O1 Pb1 O2 77.3(2) . 15 ?
O1 Pb1 O2 49.5(2) 15 15 ?
N1 Pb1 O3 128.8(2) . 13_465 ?
O3 Pb1 O3 66.2(3) . 13_465 ?
O1 Pb1 O3 166.1(2) . 13_465 ?
O1 Pb1 O3 78.9(2) 15 13_465 ?
O2 Pb1 O3 94.0(2) 15 13_465 ?
O4 Ca1 O4 88.0(2) 18 16_455 ?
O4 Ca1 O4 179.999(1) 18 3_455 ?
O4 Ca1 O4 92.0(2) 16_455 3_455 ?
O4 Ca1 O4 88.0(2) 18 17_445 ?
O4 Ca1 O4 88.0(2) 16_455 17_445 ?
O4 Ca1 O4 92.0(2) 3_455 17_445 ?
O4 Ca1 O4 92.0(2) 18 . ?
O4 Ca1 O4 179.998(1) 16_455 . ?
O4 Ca1 O4 88.0(2) 3_455 . ?
O4 Ca1 O4 92.0(2) 17_445 . ?
O4 Ca1 O4 92.0(2) 18 2_565 ?
O4 Ca1 O4 92.0(2) 16_455 2_565 ?
O4 Ca1 O4 88.0(2) 3_455 2_565 ?
O4 Ca1 O4 179.998(1) 17_445 2_565 ?
O4 Ca1 O4 88.0(2) . 2_565 ?
C1 O1 Pb1 119.6(6) . . ?
C1 O1 Pb1 93.0(5) . 14_455 ?
Pb1 O1 Pb1 147.4(3) . 14_455 ?
C1 O2 Pb1 92.6(7) . 14_455 ?
C7 O3 Pb1 120.0(5) . . ?
C7 O3 Pb1 120.6(5) . 13_465 ?
Pb1 O3 Pb1 113.8(3) . 13_465 ?
C7 O4 Ca1 168.2(7) . . ?
C6 N1 C2 118.6(8) . . ?
C6 N1 Pb1 120.1(5) . . ?
C2 N1 Pb1 121.3(6) . . ?
O1 C1 O2 124.6(10) . . ?
O1 C1 C2 118.5(8) . . ?
O2 C1 C2 116.9(10) . . ?
N1 C2 C3 122.9(9) . . ?
N1 C2 C1 115.6(9) . . ?
C3 C2 C1 121.4(8) . . ?
C2 C3 C4 119.1(8) . . ?
C2 C3 H3A 120.5 . . ?
C4 C3 H3A 120.5 . . ?
C3 C4 C5 118.8(11) . . ?
C3 C4 H4A 120.6 . . ?
C5 C4 H4A 120.6 . . ?
C6 C5 C4 118.4(9) . . ?
C6 C5 H5A 120.8 . . ?
C4 C5 H5A 120.8 . . ?
N1 C6 C5 122.1(8) . . ?
N1 C6 C7 116.4(8) . . ?
C5 C6 C7 121.5(8) . . ?
O3 C7 O4 125.0(8) . . ?
O3 C7 C6 116.7(8) . . ?
O4 C7 C6 118.3(9) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.206
_refine_diff_density_min         -4.096
_refine_diff_density_rms         0.491
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1436293'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 [CeMg1.5(oPDA)3(H2O)3]-3.5H2O 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H22 Ce Mg1.50 N3 O18.50'
_chemical_formula_sum            'C21 H22 Ce Mg1.50 N3 O18.50'
_chemical_formula_weight         789.00

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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 6/m c c'
_symmetry_space_group_name_Hall  '-P 6 2c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   15.6115(9)
_cell_length_b                   15.6115(9)
_cell_length_c                   15.1842(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3204.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8591
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      28.4

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1572
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7393
_exptl_absorpt_correction_T_max  0.7918
_exptl_absorpt_process_details   sadabs(1997)

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart ApecII CCD diffracmeter'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21308
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         28.41
_reflns_number_total             1408
_reflns_number_gt                1249
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0559P)²+1.3368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1408
_refine_ls_number_parameters     82
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0921
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_restrained_S_all      1.250
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce -0.3333 0.3333 -0.2500 0.01796(14) Uani 1 6 d S . .
Mg1 Mg 0.0000 0.5000 0.0000 0.0199(3) Uani 1 4 d S . .
O1W O -0.12979(17) 0.51046(17) 0.0000 0.0278(5) Uani 1 2 d S . .
H1WA H -0.1664 0.4764 -0.0399 0.042 Uiso 0.50 1 calc PR . .
O2W O 0.0451(12) 0.2672(9) 0.0000 0.234(5) Uani 1 2 d SD . .
H2WA H 0.098(9) 0.264(15) 0.0000 0.351 Uiso 1 2 d SD . .
H2WB H 0.066(14) 0.329(3) 0.0000 0.351 Uiso 1 2 d SD . .
O3W O 0.0000 0.0000 -0.2500 0.31(2) Uani 1 12 d SU . .
O1 O -0.19558(14) 0.38449(14) -0.14142(13) 0.0334(4) Uani 1 1 d . . .
O2 O -0.05831(12) 0.38839(13) -0.09422(11) 0.0343(4) Uani 1 1 d . . .
N1 N -0.23701(11) 0.23701(11) -0.2500 0.0233(6) Uani 1 2 d S . .
C1 C -0.13465(17) 0.35303(17) -0.13922(15) 0.0259(5) Uani 1 1 d . . .
C2 C -0.15932(16) 0.26490(17) -0.19690(15) 0.0268(5) Uani 1 1 d . . .
C3 C -0.1070(2) 0.2153(2) -0.1943(2) 0.0424(7) Uani 1 1 d . . .
H3A H -0.0539 0.2352 -0.1559 0.051 Uiso 1 1 calc R . .
C4 C -0.13507(17) 0.13507(17) -0.2500 0.0548(14) Uani 1 2 d S . .
H4A H -0.1007 0.1007 -0.2500 0.066 Uiso 1 2 calc SR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ce1 0.01885(16) 0.01885(16) 0.0162(2) 0.000 0.000 0.00942(8)
Mg1 0.0164(7) 0.0227(7) 0.0175(7) 0.000 0.000 0.0075(5)
O1W 0.0249(11) 0.0326(12) 0.0257(11) 0.000 0.000 0.0143(10)
O2W 0.431(17) 0.195(10) 0.149(7) 0.000 0.000 0.212(11)
O3W 0.21(2) 0.21(2) 0.52(5) 0.000 0.000 0.104(10)
O1 0.0348(10) 0.0402(10) 0.0325(9) -0.0161(8) -0.0152(8) 0.0241(8)
O2 0.0291(9) 0.0405(9) 0.0355(9) -0.0159(8) -0.0143(7) 0.0189(8)
N1 0.0235(10) 0.0235(10) 0.0234(13) -0.0058(8) -0.0058(8) 0.0122(12)
C1 0.0246(10) 0.0289(11) 0.0235(10) -0.0051(9) -0.0054(9) 0.0128(9)
C2 0.0245(11) 0.0277(11) 0.0284(11) -0.0052(9) -0.0068(9) 0.0133(9)
C3 0.0362(14) 0.0448(15) 0.0552(17) -0.0173(13) -0.0202(13) 0.0270(13)
C4 0.048(2) 0.048(2) 0.085(4) -0.029(2) -0.029(2) 0.037(2)

_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
Ce1 O1 2.5026(18) 11_454 ?
Ce1 O1 2.5027(18) 10_554 ?
Ce1 O1 2.5027(18) 3_455 ?
Ce1 O1 2.5027(18) . ?
Ce1 O1 2.5027(18) 12_564 ?
Ce1 O1 2.5027(18) 2_565 ?
Ce1 N1 2.605(3) 3_455 ?
Ce1 N1 2.605(3) . ?
Ce1 N1 2.605(3) 2_565 ?
Mg1 O2 2.0798(16) . ?
Mg1 O2 2.0798(16) 13_565 ?
Mg1 O2 2.0798(16) 4_565 ?
Mg1 O2 2.0798(16) 16 ?
Mg1 O1W 2.113(2) . ?
Mg1 O1W 2.113(2) 13_565 ?
O1W H1WA 0.8200 . ?
O2W H2WA 0.851(10) . ?
O2W H2WB 0.850(10) . ?
O1 C1 1.270(3) . ?
O2 C1 1.239(3) . ?
N1 C2 1.335(3) 10_554 ?
N1 C2 1.335(3) . ?
C1 C2 1.510(3) . ?
C2 C3 1.378(3) . ?
C3 C4 1.389(4) . ?
C3 H3A 0.9300 . ?
C4 C3 1.388(4) 10_554 ?
C4 H4A 0.9300 . ?

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 Ce1 O1 81.31(7) 11_454 10_554 ?
O1 Ce1 O1 124.22(8) 11_454 3_455 ?
O1 Ce1 O1 83.82(10) 10_554 3_455 ?
O1 Ce1 O1 147.91(9) 11_454 . ?
O1 Ce1 O1 124.22(8) 10_554 . ?
O1 Ce1 O1 81.31(7) 3_455 . ?
O1 Ce1 O1 81.32(7) 11_454 12_564 ?
O1 Ce1 O1 81.32(7) 10_554 12_564 ?
O1 Ce1 O1 147.91(9) 3_455 12_564 ?
O1 Ce1 O1 83.82(10) . 12_564 ?
O1 Ce1 O1 83.82(10) 11_454 2_565 ?
O1 Ce1 O1 147.91(9) 10_554 2_565 ?
O1 Ce1 O1 81.32(7) 3_455 2_565 ?
O1 Ce1 O1 81.32(7) . 2_565 ?
O1 Ce1 O1 124.22(8) 12_564 2_565 ?
O1 Ce1 N1 62.11(4) 11_454 3_455 ?
O1 Ce1 N1 73.96(4) 10_554 3_455 ?
O1 Ce1 N1 62.11(4) 3_455 3_455 ?
O1 Ce1 N1 138.09(5) . 3_455 ?
O1 Ce1 N1 138.09(5) 12_564 3_455 ?
O1 Ce1 N1 73.95(4) 2_565 3_455 ?
O1 Ce1 N1 138.09(5) 11_454 . ?
O1 Ce1 N1 62.11(4) 10_554 . ?
O1 Ce1 N1 73.96(4) 3_455 . ?
O1 Ce1 N1 62.11(4) . . ?
O1 Ce1 N1 73.96(5) 12_564 . ?
O1 Ce1 N1 138.09(5) 2_565 . ?
N1 Ce1 N1 120.0 3_455 . ?
O1 Ce1 N1 73.96(4) 11_454 2_565 ?
O1 Ce1 N1 138.09(5) 10_554 2_565 ?
O1 Ce1 N1 138.09(5) 3_455 2_565 ?
O1 Ce1 N1 73.96(4) . 2_565 ?
O1 Ce1 N1 62.11(4) 12_564 2_565 ?
O1 Ce1 N1 62.11(4) 2_565 2_565 ?
N1 Ce1 N1 120.0 3_455 2_565 ?
N1 Ce1 N1 120.0 . 2_565 ?
O2 Mg1 O2 180.0 . 13_565 ?
O2 Mg1 O2 93.07(10) . 4_565 ?
O2 Mg1 O2 86.93(10) 13_565 4_565 ?
O2 Mg1 O2 86.93(10) . 16 ?
O2 Mg1 O2 93.07(10) 13_565 16 ?
O2 Mg1 O2 180.0 4_565 16 ?
O2 Mg1 O1W 91.71(6) . . ?
O2 Mg1 O1W 88.29(6) 13_565 . ?
O2 Mg1 O1W 88.29(6) 4_565 . ?
O2 Mg1 O1W 91.71(6) 16 . ?
O2 Mg1 O1W 88.29(6) . 13_565 ?
O2 Mg1 O1W 91.71(6) 13_565 13_565 ?
O2 Mg1 O1W 91.71(6) 4_565 13_565 ?
O2 Mg1 O1W 88.29(6) 16 13_565 ?
O1W Mg1 O1W 180.0 . 13_565 ?
Mg1 O1W H1WA 109.5 . . ?
H2WA O2W H2WB 104(3) . . ?
C1 O1 Ce1 125.72(15) . . ?
C1 O2 Mg1 132.33(15) . . ?
C2 N1 C2 119.4(3) 10_554 . ?
C2 N1 Ce1 120.29(15) 10_554 . ?
C2 N1 Ce1 120.29(15) . . ?
O2 C1 O1 125.6(2) . . ?
O2 C1 C2 118.4(2) . . ?
O1 C1 C2 115.98(19) . . ?
N1 C2 C3 122.1(2) . . ?
N1 C2 C1 115.1(2) . . ?
C3 C2 C1 122.9(2) . . ?
C2 C3 C4 118.8(3) . . ?
C2 C3 H3A 120.6 . . ?
C4 C3 H3A 120.6 . . ?
C3 C4 C3 118.9(4) 10_554 . ?
C3 C4 H4A 120.5 10_554 . ?
C3 C4 H4A 120.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.41
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.111

