# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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. 
# 
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data_mo_2017229-63_0m_sq_s
_database_code_depnum_ccdc_archive 'CCDC 1544793'
_audit_update_record             
;
2017-12-21 deposited with the CCDC.
2017-12-29 downloaded from the CCDC.
;
_audit_creation_date             2017-12-21
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.17(N240 Na46 O18), 0.33(Na)'
_chemical_formula_sum            'N40 Na8 O3'
_chemical_formula_weight         792.32
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_H-M_alt        'P m -3 n'
_space_group_name_Hall           '-P 4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'-x-1/2, -z-1/2, y-1/2'
'x-1/2, -z-1/2, -y-1/2'
'x-1/2, z-1/2, y-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'-z-1/2, y-1/2, -x-1/2'
'z-1/2, -y-1/2, -x-1/2'
'z-1/2, y-1/2, x-1/2'

_cell_length_a                   18.238(10)
_cell_length_b                   18.238(10)
_cell_length_c                   18.238(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6067(10)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    611
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.50
_shelx_estimated_absorpt_T_max   0.979
_shelx_estimated_absorpt_T_min   0.952
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1491 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.8830. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14408
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.233
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                941
_reflns_number_total             1279
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0606
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1319P)²+1.7179P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.2027
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: O2(0.25) O1(0.125)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
N6 N 0.2500 0.59311(11) 0.09311(11) 0.0465(10) Uani 1 2 d S T P . .
Na1 Na 0.31514(4) 0.68486(4) 0.31514(4) 0.0165(4) Uani 1 3 d S T P . .
N5 N 0.29308(15) 0.59468(11) 0.15185(11) 0.0394(7) Uani 1 1 d . . . . .
Na4 Na 0.5000 0.5000 0.5000 0.229(10) Uani 1 24 d S T P . .
N1 N 0.31506(17) 0.6900(2) 0.5000 0.0359(8) Uani 1 2 d S T P . .
Na2 Na 0.5000 0.80469(7) 0.38001(8) 0.0276(4) Uani 1 2 d S T P . .
N4 N 0.27639(13) 0.65428(11) 0.18904(11) 0.0311(6) Uani 1 1 d . . . . .
N2 N 0.34965(12) 0.71580(15) 0.44153(11) 0.0390(6) Uani 1 1 d . . . . .
N3 N 0.40526(12) 0.75665(15) 0.46361(11) 0.0429(7) Uani 1 1 d . . . . .
O2 O 0.5000 0.9450(4) 0.3970(5) 0.067(2) Uani 0.5 2 d S T P . .
O1 O 0.5000 0.8887(5) 0.5000 0.061(3) Uani 0.5 4 d S T P . .
Na3 Na 0.2500 0.5000 0.0000 0.0828(18) Uani 1 8 d S T P . .


_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
N6 N5 1.329(3) . ?
N6 N5 1.329(3) 18_554 ?
N6 Na3 2.402(3) . ?
Na1 Na1 4.116(4) 13_455 ?
Na1 Na2 4.188(2) . ?
Na1 Na2 4.188(2) 6_566 ?
Na1 Na2 4.188(2) 33_666 ?
Na1 N4 2.470(3) 6_566 ?
Na1 N4 2.470(3) . ?
Na1 N4 2.470(3) 12_665 ?
Na1 N2 2.455(3) 6_566 ?
Na1 N2 2.455(3) . ?
Na1 N2 2.455(3) 12_665 ?
N5 Na2 2.475(3) 6_566 ?
N5 N4 1.317(3) . ?
N1 Na2 2.530(4) 33_666 ?
N1 N2 1.325(3) . ?
N1 N2 1.325(3) 26_556 ?
Na2 Na1 4.188(2) 28_655 ?
Na2 N5 2.475(3) 12_665 ?
Na2 N5 2.475(3) 34_565 ?
Na2 N1 2.530(4) 29_666 ?
Na2 N3 2.465(3) . ?
Na2 N3 2.465(3) 28_655 ?
Na2 O2 2.578(7) . ?
Na2 O1 2.671(6) . ?
N4 N4 1.315(4) 18_554 ?
N2 N3 1.321(3) . ?
N3 N3 1.327(4) 26_556 ?
O2 Na3 2.863(9) 9_565 ?
O1 Na2 2.671(6) 26_556 ?
Na3 N6 2.402(3) 4_565 ?
Na3 N6 2.402(3) 27_565 ?
Na3 N6 2.402(3) 26 ?
Na3 O2 2.863(9) 45_675 ?
Na3 O2 2.863(9) 46_656 ?
Na3 O2 2.863(9) 5_554 ?
Na3 O2 2.863(9) 6_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
N5 N6 N5 108.4(3) . 18_554 ?
N5 N6 Na3 125.83(14) . . ?
N5 N6 Na3 125.82(14) 18_554 . ?
Na1 Na1 Na2 109.06(3) 13_455 33_666 ?
Na1 Na1 Na2 109.06(3) 13_455 . ?
Na1 Na1 Na2 109.06(3) 13_455 6_566 ?
Na2 Na1 Na2 109.88(3) 33_666 . ?
Na2 Na1 Na2 109.88(3) 6_566 33_666 ?
Na2 Na1 Na2 109.88(3) 6_566 . ?
N4 Na1 Na1 55.08(6) . 13_455 ?
N4 Na1 Na1 55.08(6) 12_665 13_455 ?
N4 Na1 Na1 55.08(6) 6_566 13_455 ?
N4 Na1 Na2 122.44(6) 12_665 6_566 ?
N4 Na1 Na2 54.07(5) 12_665 . ?
N4 Na1 Na2 127.68(6) 6_566 6_566 ?
N4 Na1 Na2 127.68(6) . . ?
N4 Na1 Na2 54.07(5) . 6_566 ?
N4 Na1 Na2 122.44(6) . 33_666 ?
N4 Na1 Na2 127.68(6) 12_665 33_666 ?
N4 Na1 Na2 122.44(6) 6_566 . ?
N4 Na1 Na2 54.07(5) 6_566 33_666 ?
N4 Na1 N4 90.48(8) 12_665 . ?
N4 Na1 N4 90.48(8) 12_665 6_566 ?
N4 Na1 N4 90.48(8) 6_566 . ?
N2 Na1 Na1 123.87(7) 12_665 13_455 ?
N2 Na1 Na1 123.87(7) . 13_455 ?
N2 Na1 Na1 123.87(7) 6_566 13_455 ?
N2 Na1 Na2 53.74(6) 12_665 33_666 ?
N2 Na1 Na2 127.05(8) 6_566 33_666 ?
N2 Na1 Na2 56.15(6) . 33_666 ?
N2 Na1 Na2 56.15(6) 12_665 6_566 ?
N2 Na1 Na2 56.15(6) 6_566 . ?
N2 Na1 Na2 53.74(6) 6_566 6_566 ?
N2 Na1 Na2 127.05(8) . 6_566 ?
N2 Na1 Na2 127.05(8) 12_665 . ?
N2 Na1 Na2 53.74(6) . . ?
N2 Na1 N4 87.76(7) 12_665 . ?
N2 Na1 N4 178.22(8) . . ?
N2 Na1 N4 89.82(8) 6_566 . ?
N2 Na1 N4 89.81(8) . 12_665 ?
N2 Na1 N4 178.22(8) 6_566 6_566 ?
N2 Na1 N4 178.22(8) 12_665 12_665 ?
N2 Na1 N4 87.76(7) . 6_566 ?
N2 Na1 N4 87.76(7) 6_566 12_665 ?
N2 Na1 N4 89.81(8) 12_665 6_566 ?
N2 Na1 N2 91.95(10) 12_665 . ?
N2 Na1 N2 91.95(10) 12_665 6_566 ?
N2 Na1 N2 91.95(10) 6_566 . ?
N6 N5 Na2 128.46(16) . 6_566 ?
N4 N5 N6 107.2(2) . . ?
N4 N5 Na2 123.99(16) . 6_566 ?
N2 N1 Na2 126.16(15) 26_556 33_666 ?
N2 N1 Na2 126.17(15) . 33_666 ?
N2 N1 N2 107.1(3) 26_556 . ?
Na1 Na2 Na1 107.21(4) . 28_655 ?
N5 Na2 Na1 54.86(5) 34_565 28_655 ?
N5 Na2 Na1 123.22(8) 34_565 . ?
N5 Na2 Na1 54.86(5) 12_665 . ?
N5 Na2 Na1 123.22(8) 12_665 28_655 ?
N5 Na2 N5 88.51(13) 12_665 34_565 ?
N5 Na2 N1 87.32(9) 12_665 29_666 ?
N5 Na2 N1 87.32(9) 34_565 29_666 ?
N5 Na2 O2 76.06(15) 34_565 . ?
N5 Na2 O2 76.06(15) 12_665 . ?
N5 Na2 O1 109.96(13) 12_665 . ?
N5 Na2 O1 109.96(13) 34_565 . ?
N1 Na2 Na1 53.627(18) 29_666 . ?
N1 Na2 Na1 53.627(18) 29_666 28_655 ?
N1 Na2 O2 156.6(2) 29_666 . ?
N1 Na2 O1 155.29(19) 29_666 . ?
N3 Na2 Na1 123.60(8) . 28_655 ?
N3 Na2 Na1 54.91(5) . . ?
N3 Na2 Na1 123.60(8) 28_655 . ?
N3 Na2 Na1 54.91(5) 28_655 28_655 ?
N3 Na2 N5 91.20(8) . 12_665 ?
N3 Na2 N5 177.61(10) 28_655 12_665 ?
N3 Na2 N5 91.20(8) 28_655 34_565 ?
N3 Na2 N5 177.61(10) . 34_565 ?
N3 Na2 N1 90.30(9) . 29_666 ?
N3 Na2 N1 90.30(9) 28_655 29_666 ?
N3 Na2 N3 88.99(11) 28_655 . ?
N3 Na2 O2 106.17(15) . . ?
N3 Na2 O2 106.17(15) 28_655 . ?
N3 Na2 O1 72.36(13) . . ?
N3 Na2 O1 72.36(13) 28_655 . ?
O2 Na2 Na1 123.51(6) . 28_655 ?
O2 Na2 Na1 123.51(6) . . ?
O2 Na2 O1 48.1(3) . . ?
O1 Na2 Na1 122.05(6) . . ?
O1 Na2 Na1 122.05(6) . 28_655 ?
N5 N4 Na1 126.86(16) . . ?
N4 N4 Na1 123.32(8) 18_554 . ?
N4 N4 N5 108.59(13) 18_554 . ?
N1 N2 Na1 123.49(18) . . ?
N3 N2 Na1 127.77(16) . . ?
N3 N2 N1 108.7(2) . . ?
N2 N3 Na2 123.35(16) . . ?
N2 N3 N3 107.75(13) . 26_556 ?
N3 N3 Na2 128.20(6) 26_556 . ?
Na2 O2 Na3 103.6(2) . 9_565 ?
Na2 O1 Na2 110.0(3) 26_556 . ?
N6 Na3 N6 180.00(14) 4_565 . ?
N6 Na3 N6 90.0 4_565 27_565 ?
N6 Na3 N6 90.0 26 . ?
N6 Na3 N6 90.0 4_565 26 ?
N6 Na3 N6 180.00(14) 27_565 26 ?
N6 Na3 N6 90.0 27_565 . ?
N6 Na3 O2 75.66(8) 4_565 46_656 ?
N6 Na3 O2 75.66(8) 27_565 6_566 ?
N6 Na3 O2 75.66(8) 27_565 46_656 ?
N6 Na3 O2 75.66(8) 4_565 5_554 ?
N6 Na3 O2 75.66(8) . 6_566 ?
N6 Na3 O2 104.34(8) 27_565 45_675 ?
N6 Na3 O2 104.34(8) . 5_554 ?
N6 Na3 O2 75.66(8) 26 45_675 ?
N6 Na3 O2 104.34(8) 26 46_656 ?
N6 Na3 O2 104.34(8) 26 6_566 ?
N6 Na3 O2 104.34(8) 4_565 45_675 ?
N6 Na3 O2 104.34(8) 27_565 5_554 ?
N6 Na3 O2 104.34(8) 4_565 6_566 ?
N6 Na3 O2 75.66(8) . 45_675 ?
N6 Na3 O2 104.34(8) . 46_656 ?
N6 Na3 O2 75.66(8) 26 5_554 ?
O2 Na3 O2 151.33(17) 5_554 45_675 ?
O2 Na3 O2 41.0(2) 6_566 5_554 ?
O2 Na3 O2 151.33(17) 6_566 45_675 ?
O2 Na3 O2 151.33(17) 46_656 6_566 ?
O2 Na3 O2 41.0(2) 46_656 45_675 ?
O2 Na3 O2 151.33(17) 46_656 5_554 ?

_platon_squeeze_details          'TITL mo_2017229-63_0m_a.res in Pm-3n'
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 0.000 0.500 0.250 270 79 ' '
2 0.000 0.500 0.750 270 79 ' '
3 0.250 0.000 0.500 270 79 ' '
4 0.500 0.250 0.000 270 79 ' '
5 0.500 0.750 0.000 270 79 ' '
6 0.750 0.000 0.500 270 79 ' '

_olex2_submission_special_instructions 'No special instructions were received'
