# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2019

####################################################################### 
# 
# 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_lc
_database_code_depnum_ccdc_archive 'CCDC 1942083'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry
China
;
_audit_update_record             
;
2019-07-22 deposited with the CCDC.	2019-09-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H20 Ca Li2 N12 O18'
_chemical_formula_weight         674.36

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'
Li Li -0.0003 0.0001 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   16.1096(10)
_cell_length_b                   11.7548(6)
_cell_length_c                   12.7052(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2405.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13881
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         26.36
_reflns_number_total             1334
_reflns_number_gt                1116
_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)+(0.0667P)²+1.2621P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1334
_refine_ls_number_parameters     136
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.1013
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.048
_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
Ca1 Ca 0.5000 0.71839(6) 0.7500 0.0253(2) Uani 1 4 d S . .
Li1 Li 0.5000 0.1827(5) 0.7500 0.0315(13) Uani 1 4 d S . .
Li2 Li 0.5000 0.4301(5) 0.7500 0.0370(15) Uani 1 4 d S . .
O1 O 0.14538(10) -0.06612(13) 0.7500 0.0262(4) Uani 1 2 d S . .
O2 O 0.15127(10) 0.31675(14) 0.7500 0.0315(4) Uani 1 2 d S . .
O3 O 0.39261(11) 0.11658(15) 0.7500 0.0378(5) Uani 1 2 d S . .
O4 O 0.10890(11) 0.5000 0.5000 0.0399(5) Uani 1 2 d S . .
O5 O 0.35154(7) 0.30758(9) 0.51355(11) 0.0293(3) Uani 1 1 d . . .
O6 O 0.5000 0.29623(15) 0.63401(15) 0.0301(4) Uani 1 2 d SD . .
O7 O 0.5000 0.55559(14) 0.62993(14) 0.0261(4) Uani 1 2 d SD . .
O8 O 0.5000 0.84410(18) 0.89344(19) 0.0454(6) Uani 1 2 d SD . .
N1 N 0.14383(11) 0.12676(16) 0.7500 0.0228(4) Uani 1 2 d S . .
N2 N 0.26899(11) 0.02506(16) 0.7500 0.0227(4) Uani 1 2 d S . .
H2 H 0.2935 -0.0399 0.7500 0.027 Uiso 1 2 calc SR . .
N3 N 0.27370(12) 0.22029(16) 0.7500 0.0240(5) Uani 1 2 d S . .
H3 H 0.3005 0.2835 0.7500 0.029 Uiso 1 2 calc SR . .
N4 N 0.23051(8) 0.40273(11) 0.50494(11) 0.0242(4) Uani 1 1 d . . .
H4 H 0.2047 0.3387 0.5070 0.029 Uiso 1 1 calc R . .
N5 N 0.35836(11) 0.5000 0.5000 0.0229(4) Uani 1 2 d S . .
C1 C 0.18327(14) 0.02641(19) 0.7500 0.0195(5) Uani 1 2 d S . .
C2 C 0.18803(14) 0.22310(19) 0.7500 0.0215(5) Uani 1 2 d S . .
C3 C 0.31735(15) 0.1208(2) 0.7500 0.0236(5) Uani 1 2 d S . .
C4 C 0.18434(15) 0.5000 0.5000 0.0243(5) Uani 1 2 d S . .
C5 C 0.31604(10) 0.40134(13) 0.50685(13) 0.0213(4) Uani 1 1 d . . .
H6 H 0.4588(11) 0.2953(16) 0.5919(15) 0.032 Uiso 1 1 d D . .
H7 H 0.5430(10) 0.5418(16) 0.5883(15) 0.032 Uiso 1 1 d D . .
H8 H 0.5415(10) 0.8788(16) 0.9181(16) 0.032 Uiso 1 1 d 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
Ca1 O8 2.346(2) . ?
Ca1 O8 2.346(2) 10_557 ?
Ca1 O7 2.4473(17) . ?
Ca1 O7 2.4473(17) 10_557 ?
Ca1 N1 2.5551(19) 7_556 ?
Ca1 N1 2.5551(19) 5 ?
Ca1 O2 2.6972(17) 7_556 ?
Ca1 O2 2.6972(17) 5 ?
Ca1 C2 3.030(2) 5 ?
Ca1 C2 3.030(2) 7_556 ?
Ca1 Li2 3.389(6) . ?
Li1 O3 1.897(3) . ?
Li1 O3 1.897(3) 3_656 ?
Li1 O6 1.988(4) 10_557 ?
Li1 O6 1.988(4) . ?
Li1 Li2 2.908(9) . ?
Li2 O7 2.122(4) 10_557 ?
Li2 O7 2.122(4) . ?
Li2 O6 2.156(5) . ?
Li2 O6 2.156(5) 10_557 ?
Li2 O1 2.3424(16) 7_556 ?
Li2 O1 2.3424(16) 5 ?
O1 C1 1.247(3) . ?
O1 Li2 2.3424(16) 5_445 ?
O2 C2 1.250(3) . ?
O2 Ca1 2.6972(17) 5_445 ?
O3 C3 1.213(3) . ?
O4 C4 1.215(3) . ?
O5 C5 1.245(2) . ?
N1 C2 1.338(3) . ?
N1 C1 1.340(3) . ?
N1 Ca1 2.5551(19) 5_445 ?
N2 C3 1.369(3) . ?
N2 C1 1.381(3) . ?
N3 C3 1.364(3) . ?
N3 C2 1.380(3) . ?
N4 C4 1.3654(19) . ?
N4 C5 1.378(2) . ?
N5 C5 1.3481(19) . ?
N5 C5 1.3481(19) 4_566 ?
C2 Ca1 3.030(2) 5_445 ?
C4 N4 1.3654(19) 4_566 ?

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
O8 Ca1 O8 101.93(12) . 10_557 ?
O8 Ca1 O7 167.60(7) . . ?
O8 Ca1 O7 90.48(8) 10_557 . ?
O8 Ca1 O7 90.48(8) . 10_557 ?
O8 Ca1 O7 167.60(7) 10_557 10_557 ?
O7 Ca1 O7 77.12(8) . 10_557 ?
O8 Ca1 N1 105.40(3) . 7_556 ?
O8 Ca1 N1 105.40(3) 10_557 7_556 ?
O7 Ca1 N1 70.75(3) . 7_556 ?
O7 Ca1 N1 70.75(3) 10_557 7_556 ?
O8 Ca1 N1 105.40(3) . 5 ?
O8 Ca1 N1 105.40(3) 10_557 5 ?
O7 Ca1 N1 70.75(3) . 5 ?
O7 Ca1 N1 70.75(3) 10_557 5 ?
N1 Ca1 N1 130.14(9) 7_556 5 ?
O8 Ca1 O2 74.34(3) . 7_556 ?
O8 Ca1 O2 74.34(3) 10_557 7_556 ?
O7 Ca1 O2 109.59(3) . 7_556 ?
O7 Ca1 O2 109.59(3) 10_557 7_556 ?
N1 Ca1 O2 50.32(5) 7_556 7_556 ?
N1 Ca1 O2 179.55(6) 5 7_556 ?
O8 Ca1 O2 74.34(3) . 5 ?
O8 Ca1 O2 74.34(3) 10_557 5 ?
O7 Ca1 O2 109.59(3) . 5 ?
O7 Ca1 O2 109.59(3) 10_557 5 ?
N1 Ca1 O2 179.55(6) 7_556 5 ?
N1 Ca1 O2 50.32(5) 5 5 ?
O2 Ca1 O2 129.23(7) 7_556 5 ?
O8 Ca1 C2 89.34(3) . 5 ?
O8 Ca1 C2 89.34(3) 10_557 5 ?
O7 Ca1 C2 90.82(3) . 5 ?
O7 Ca1 C2 90.82(3) 10_557 5 ?
N1 Ca1 C2 156.12(6) 7_556 5 ?
N1 Ca1 C2 25.98(6) 5 5 ?
O2 Ca1 C2 153.57(6) 7_556 5 ?
O2 Ca1 C2 24.34(5) 5 5 ?
O8 Ca1 C2 89.34(3) . 7_556 ?
O8 Ca1 C2 89.34(3) 10_557 7_556 ?
O7 Ca1 C2 90.82(3) . 7_556 ?
O7 Ca1 C2 90.82(3) 10_557 7_556 ?
N1 Ca1 C2 25.98(6) 7_556 7_556 ?
N1 Ca1 C2 156.12(6) 5 7_556 ?
O2 Ca1 C2 24.34(5) 7_556 7_556 ?
O2 Ca1 C2 153.57(6) 5 7_556 ?
C2 Ca1 C2 177.90(9) 5 7_556 ?
O8 Ca1 Li2 129.04(6) . . ?
O8 Ca1 Li2 129.04(6) 10_557 . ?
O7 Ca1 Li2 38.56(4) . . ?
O7 Ca1 Li2 38.56(4) 10_557 . ?
N1 Ca1 Li2 65.07(4) 7_556 . ?
N1 Ca1 Li2 65.07(4) 5 . ?
O2 Ca1 Li2 115.38(4) 7_556 . ?
O2 Ca1 Li2 115.38(4) 5 . ?
C2 Ca1 Li2 91.05(4) 5 . ?
C2 Ca1 Li2 91.05(4) 7_556 . ?
O3 Li1 O3 131.6(3) . 3_656 ?
O3 Li1 O6 105.97(8) . 10_557 ?
O3 Li1 O6 105.97(8) 3_656 10_557 ?
O3 Li1 O6 105.97(8) . . ?
O3 Li1 O6 105.97(8) 3_656 . ?
O6 Li1 O6 95.7(3) 10_557 . ?
O3 Li1 Li2 114.21(17) . . ?
O3 Li1 Li2 114.21(17) 3_656 . ?
O6 Li1 Li2 47.85(14) 10_557 . ?
O6 Li1 Li2 47.85(14) . . ?
O7 Li2 O7 91.9(2) 10_557 . ?
O7 Li2 O6 177.2(2) 10_557 . ?
O7 Li2 O6 90.92(7) . . ?
O7 Li2 O6 90.92(7) 10_557 10_557 ?
O7 Li2 O6 177.2(2) . 10_557 ?
O6 Li2 O6 86.2(2) . 10_557 ?
O7 Li2 O1 89.24(11) 10_557 7_556 ?
O7 Li2 O1 89.24(11) . 7_556 ?
O6 Li2 O1 90.80(11) . 7_556 ?
O6 Li2 O1 90.80(11) 10_557 7_556 ?
O7 Li2 O1 89.24(11) 10_557 5 ?
O7 Li2 O1 89.24(11) . 5 ?
O6 Li2 O1 90.80(11) . 5 ?
O6 Li2 O1 90.80(11) 10_557 5 ?
O1 Li2 O1 177.8(3) 7_556 5 ?
O7 Li2 Li1 134.04(12) 10_557 . ?
O7 Li2 Li1 134.04(12) . . ?
O6 Li2 Li1 43.12(12) . . ?
O6 Li2 Li1 43.12(12) 10_557 . ?
O1 Li2 Li1 91.09(15) 7_556 . ?
O1 Li2 Li1 91.09(15) 5 . ?
O7 Li2 Ca1 45.96(12) 10_557 . ?
O7 Li2 Ca1 45.96(12) . . ?
O6 Li2 Ca1 136.88(12) . . ?
O6 Li2 Ca1 136.88(12) 10_557 . ?
O1 Li2 Ca1 88.91(15) 7_556 . ?
O1 Li2 Ca1 88.91(15) 5 . ?
Li1 Li2 Ca1 180.0 . . ?
C1 O1 Li2 120.4(2) . 5_445 ?
C2 O2 Ca1 92.90(14) . 5_445 ?
C3 O3 Li1 153.4(2) . . ?
Li1 O6 Li2 89.03(19) . . ?
Li2 O7 Ca1 95.48(13) . . ?
C2 N1 C1 119.5(2) . . ?
C2 N1 Ca1 97.23(14) . 5_445 ?
C1 N1 Ca1 143.24(15) . 5_445 ?
C3 N2 C1 124.0(2) . . ?
C3 N3 C2 122.39(19) . . ?
C4 N4 C5 123.74(15) . . ?
C5 N5 C5 119.2(2) . 4_566 ?
O1 C1 N1 122.4(2) . . ?
O1 C1 N2 118.6(2) . . ?
N1 C1 N2 119.0(2) . . ?
O2 C2 N1 119.6(2) . . ?
O2 C2 N3 119.7(2) . . ?
N1 C2 N3 120.8(2) . . ?
O2 C2 Ca1 62.76(12) . 5_445 ?
N1 C2 Ca1 56.79(12) . 5_445 ?
N3 C2 Ca1 177.58(15) . 5_445 ?
O3 C3 N3 123.4(2) . . ?
O3 C3 N2 122.3(2) . . ?
N3 C3 N2 114.3(2) . . ?
O4 C4 N4 123.01(10) . 4_566 ?
O4 C4 N4 123.01(10) . . ?
N4 C4 N4 114.0(2) 4_566 . ?
O5 C5 N5 122.27(16) . . ?
O5 C5 N4 118.11(15) . . ?
N5 C5 N4 119.62(15) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_exp_5606
_database_code_depnum_ccdc_archive 'CCDC 1942092'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry
China
;
_audit_update_record             
;
2019-07-22 deposited with the CCDC.	2019-09-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H20 Ba N12 Na2 O18'
_chemical_formula_weight         803.72

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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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                   17.0294(6)
_cell_length_b                   6.5546(2)
_cell_length_c                   23.1652(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.245(3)
_cell_angle_gamma                90.00
_cell_volume                     2536.08(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1592
_exptl_absorpt_coefficient_mu    1.712
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16240
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         26.37
_reflns_number_total             2599
_reflns_number_gt                2538
_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)+(0.0212P)²+3.2254P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2599
_refine_ls_number_parameters     222
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.0456
_refine_ls_wR_factor_gt          0.0453
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.092
_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
Ba1 Ba 0.5000 0.30296(2) 0.7500 0.02101(6) Uani 1 2 d S . .
Na1 Na 0.51333(5) 0.48259(14) 0.57942(4) 0.03295(19) Uani 1 1 d . . .
C1 C 0.17847(11) 0.5058(3) 0.47514(8) 0.0222(4) Uani 1 1 d . . .
C2 C 0.69355(11) 0.4306(3) 0.75666(8) 0.0224(4) Uani 1 1 d . . .
C3 C 0.81927(11) 0.4483(3) 0.72422(8) 0.0223(4) Uani 1 1 d . . .
C4 C 0.69103(11) 0.4430(3) 0.65701(8) 0.0225(4) Uani 1 1 d . . .
C5 C 0.30432(11) 0.4853(3) 0.54415(9) 0.0245(4) Uani 1 1 d . . .
C6 C 0.17650(11) 0.4770(3) 0.57470(8) 0.0227(4) Uani 1 1 d . . .
N1 N 0.26106(9) 0.5031(3) 0.48840(7) 0.0240(3) Uani 1 1 d . . .
H1 H 0.2866 0.5132 0.4599 0.029 Uiso 1 1 calc R . .
N2 N 0.13688(9) 0.4941(3) 0.51875(7) 0.0236(3) Uani 1 1 d . . .
N3 N 0.77445(9) 0.4467(3) 0.66915(7) 0.0259(4) Uani 1 1 d . . .
H3 H 0.7988 0.4479 0.6400 0.031 Uiso 1 1 calc R . .
N4 N 0.65164(9) 0.4305(3) 0.70169(7) 0.0240(3) Uani 1 1 d . . .
N5 N 0.77632(9) 0.4402(3) 0.76774(7) 0.0232(3) Uani 1 1 d . . .
H5 H 0.8016 0.4411 0.8037 0.028 Uiso 1 1 calc R . .
N6 N 0.25898(9) 0.4717(3) 0.58625(7) 0.0267(4) Uani 1 1 d . . .
H6 H 0.2833 0.4590 0.6223 0.032 Uiso 1 1 calc R . .
O1 O 0.65940(8) 0.4208(3) 0.79960(6) 0.0320(3) Uani 1 1 d . . .
O2 O 0.89301(8) 0.4568(2) 0.73433(6) 0.0285(3) Uani 1 1 d . . .
O3 O 0.49934(9) 0.1558(2) 0.63571(7) 0.0301(3) Uani 1 1 d D . .
O4 O 0.49946(9) 0.7351(2) 0.50644(8) 0.0327(3) Uani 1 1 d D . .
O5 O 0.14509(8) 0.5207(3) 0.42272(6) 0.0322(3) Uani 1 1 d . . .
O6 O 0.65657(8) 0.4525(2) 0.60495(6) 0.0305(3) Uani 1 1 d . . .
O7 O 0.49380(11) 0.6557(3) 0.67521(9) 0.0435(4) Uani 1 1 d D . .
O8 O 0.14158(8) 0.4638(2) 0.61689(6) 0.0303(3) Uani 1 1 d . . .
O9 O 0.37685(8) 0.4793(3) 0.55520(7) 0.0390(4) Uani 1 1 d . . .
H4A H 0.5402(15) 0.815(4) 0.5085(14) 0.058 Uiso 1 1 d D . .
H3A H 0.5387(15) 0.091(5) 0.6256(13) 0.058 Uiso 1 1 d D . .
H4B H 0.4579(15) 0.815(4) 0.5025(14) 0.058 Uiso 1 1 d D . .
H3B H 0.4570(14) 0.101(5) 0.6163(12) 0.058 Uiso 1 1 d D . .
H7A H 0.4524(15) 0.729(4) 0.6724(14) 0.058 Uiso 1 1 d D . .
H7B H 0.5294(17) 0.742(4) 0.6925(14) 0.058 Uiso 1 1 d 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
Ba1 O3 2.8157(15) . ?
Ba1 O3 2.8157(15) 2_656 ?
Ba1 O1 2.8406(13) 2_656 ?
Ba1 O1 2.8406(14) . ?
Ba1 O7 2.8788(18) . ?
Ba1 O7 2.8788(18) 2_656 ?
Ba1 O2 2.8881(15) 3_445 ?
Ba1 O2 2.8881(14) 4_646 ?
Ba1 N4 3.1220(15) . ?
Ba1 N4 3.1220(15) 2_656 ?
Ba1 C2 3.3748(18) . ?
Ba1 C2 3.3748(18) 2_656 ?
Na1 O9 2.2822(16) . ?
Na1 O4 2.3446(18) . ?
Na1 O6 2.4034(15) . ?
Na1 O4 2.4228(19) 5_666 ?
Na1 O3 2.5430(18) . ?
Na1 O7 2.571(2) . ?
Na1 Na1 3.6255(17) 5_666 ?
C1 O5 1.240(2) . ?
C1 N2 1.344(2) . ?
C1 N1 1.380(2) . ?
C2 O1 1.248(2) . ?
C2 N4 1.333(2) . ?
C2 N5 1.384(2) . ?
C3 O2 1.233(2) . ?
C3 N3 1.353(2) . ?
C3 N5 1.357(2) . ?
C4 O6 1.236(2) . ?
C4 N4 1.341(2) . ?
C4 N3 1.393(2) . ?
C5 O9 1.212(2) . ?
C5 N6 1.360(2) . ?
C5 N1 1.361(2) . ?
C6 O8 1.242(2) . ?
C6 N2 1.344(2) . ?
C6 N6 1.378(2) . ?
O2 Ba1 2.8881(14) 3 ?
O4 Na1 2.4228(19) 5_666 ?

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
O3 Ba1 O3 139.93(7) . 2_656 ?
O3 Ba1 O1 83.37(4) . 2_656 ?
O3 Ba1 O1 107.57(4) 2_656 2_656 ?
O3 Ba1 O1 107.57(4) . . ?
O3 Ba1 O1 83.37(4) 2_656 . ?
O1 Ba1 O1 148.43(7) 2_656 . ?
O3 Ba1 O7 73.52(5) . . ?
O3 Ba1 O7 146.51(5) 2_656 . ?
O1 Ba1 O7 67.55(5) 2_656 . ?
O1 Ba1 O7 86.85(5) . . ?
O3 Ba1 O7 146.51(5) . 2_656 ?
O3 Ba1 O7 73.52(5) 2_656 2_656 ?
O1 Ba1 O7 86.85(5) 2_656 2_656 ?
O1 Ba1 O7 67.55(5) . 2_656 ?
O7 Ba1 O7 73.13(8) . 2_656 ?
O3 Ba1 O2 74.09(4) . 3_445 ?
O3 Ba1 O2 74.68(4) 2_656 3_445 ?
O1 Ba1 O2 68.48(4) 2_656 3_445 ?
O1 Ba1 O2 142.58(4) . 3_445 ?
O7 Ba1 O2 127.38(5) . 3_445 ?
O7 Ba1 O2 130.91(5) 2_656 3_445 ?
O3 Ba1 O2 74.68(4) . 4_646 ?
O3 Ba1 O2 74.09(4) 2_656 4_646 ?
O1 Ba1 O2 142.58(5) 2_656 4_646 ?
O1 Ba1 O2 68.48(4) . 4_646 ?
O7 Ba1 O2 130.91(5) . 4_646 ?
O7 Ba1 O2 127.38(5) 2_656 4_646 ?
O2 Ba1 O2 76.45(6) 3_445 4_646 ?
O3 Ba1 N4 66.84(4) . . ?
O3 Ba1 N4 125.23(4) 2_656 . ?
O1 Ba1 N4 125.04(4) 2_656 . ?
O1 Ba1 N4 43.96(4) . . ?
O7 Ba1 N4 60.34(5) . . ?
O7 Ba1 N4 93.72(5) 2_656 . ?
O2 Ba1 N4 135.31(4) 3_445 . ?
O2 Ba1 N4 73.13(4) 4_646 . ?
O3 Ba1 N4 125.23(4) . 2_656 ?
O3 Ba1 N4 66.84(4) 2_656 2_656 ?
O1 Ba1 N4 43.96(4) 2_656 2_656 ?
O1 Ba1 N4 125.04(4) . 2_656 ?
O7 Ba1 N4 93.72(5) . 2_656 ?
O7 Ba1 N4 60.34(5) 2_656 2_656 ?
O2 Ba1 N4 73.13(4) 3_445 2_656 ?
O2 Ba1 N4 135.31(4) 4_646 2_656 ?
N4 Ba1 N4 148.94(6) . 2_656 ?
O3 Ba1 C2 87.29(4) . . ?
O3 Ba1 C2 102.54(4) 2_656 . ?
O1 Ba1 C2 143.01(5) 2_656 . ?
O1 Ba1 C2 20.99(4) . . ?
O7 Ba1 C2 75.48(5) . . ?
O7 Ba1 C2 81.52(5) 2_656 . ?
O2 Ba1 C2 141.91(4) 3_445 . ?
O2 Ba1 C2 66.58(4) 4_646 . ?
N4 Ba1 C2 23.26(4) . . ?
N4 Ba1 C2 141.81(5) 2_656 . ?
O3 Ba1 C2 102.54(4) . 2_656 ?
O3 Ba1 C2 87.29(4) 2_656 2_656 ?
O1 Ba1 C2 20.99(4) 2_656 2_656 ?
O1 Ba1 C2 143.01(5) . 2_656 ?
O7 Ba1 C2 81.52(5) . 2_656 ?
O7 Ba1 C2 75.48(5) 2_656 2_656 ?
O2 Ba1 C2 66.58(4) 3_445 2_656 ?
O2 Ba1 C2 141.91(4) 4_646 2_656 ?
N4 Ba1 C2 141.81(5) . 2_656 ?
N4 Ba1 C2 23.26(4) 2_656 2_656 ?
C2 Ba1 C2 151.29(7) . 2_656 ?
O9 Na1 O4 82.81(6) . . ?
O9 Na1 O6 174.75(8) . . ?
O4 Na1 O6 100.96(6) . . ?
O9 Na1 O4 82.44(6) . 5_666 ?
O4 Na1 O4 81.00(6) . 5_666 ?
O6 Na1 O4 94.48(6) . 5_666 ?
O9 Na1 O3 85.72(6) . . ?
O4 Na1 O3 163.34(7) . . ?
O6 Na1 O3 89.81(6) . . ?
O4 Na1 O3 85.56(6) 5_666 . ?
O9 Na1 O7 85.38(6) . . ?
O4 Na1 O7 107.40(7) . . ?
O6 Na1 O7 96.88(6) . . ?
O4 Na1 O7 164.24(7) 5_666 . ?
O3 Na1 O7 83.59(6) . . ?
O9 Na1 Na1 80.28(5) . 5_666 ?
O4 Na1 Na1 41.30(5) . 5_666 ?
O6 Na1 Na1 100.08(5) . 5_666 ?
O4 Na1 Na1 39.70(4) 5_666 5_666 ?
O3 Na1 Na1 124.59(6) . 5_666 ?
O7 Na1 Na1 146.77(6) . 5_666 ?
O9 Na1 Ba1 89.39(5) . . ?
O4 Na1 Ba1 149.97(5) . . ?
O6 Na1 Ba1 89.07(4) . . ?
O4 Na1 Ba1 126.77(5) 5_666 . ?
O3 Na1 Ba1 41.29(4) . . ?
O7 Na1 Ba1 42.85(4) . . ?
Na1 Na1 Ba1 163.72(4) 5_666 . ?
O5 C1 N2 122.16(17) . . ?
O5 C1 N1 118.14(16) . . ?
N2 C1 N1 119.70(17) . . ?
O1 C2 N4 121.04(16) . . ?
O1 C2 N5 118.07(17) . . ?
N4 C2 N5 120.89(16) . . ?
O1 C2 Ba1 54.62(9) . . ?
N4 C2 Ba1 67.66(10) . . ?
N5 C2 Ba1 165.94(13) . . ?
O2 C3 N3 123.07(17) . . ?
O2 C3 N5 122.50(17) . . ?
N3 C3 N5 114.43(16) . . ?
O6 C4 N4 122.85(17) . . ?
O6 C4 N3 117.88(16) . . ?
N4 C4 N3 119.26(16) . . ?
O9 C5 N6 122.97(18) . . ?
O9 C5 N1 122.94(18) . . ?
N6 C5 N1 114.09(16) . . ?
O8 C6 N2 122.50(17) . . ?
O8 C6 N6 118.14(17) . . ?
N2 C6 N6 119.36(16) . . ?
C5 N1 C1 123.49(16) . . ?
C6 N2 C1 119.38(16) . . ?
C3 N3 C4 123.77(16) . . ?
C2 N4 C4 118.82(16) . . ?
C2 N4 Ba1 89.08(11) . . ?
C4 N4 Ba1 150.01(12) . . ?
C3 N5 C2 122.75(16) . . ?
C5 N6 C6 123.97(16) . . ?
C2 O1 Ba1 104.39(11) . . ?
C3 O2 Ba1 130.80(13) . 3 ?
Na1 O3 Ba1 102.13(6) . . ?
Na1 O4 Na1 99.00(6) . 5_666 ?
C4 O6 Na1 120.69(12) . . ?
Na1 O7 Ba1 99.74(6) . . ?
C5 O9 Na1 176.88(16) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.068
