# 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_r-3p
_database_code_depnum_ccdc_archive 'CCDC 1042423'
_audit_update_record             
;
2015-01-07 deposited with the CCDC.
2015-03-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H11 Cr0.50 N Na0.50 O6'
_chemical_formula_weight         218.64

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'
Cr Cr 0.3209 0.6236 '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'

_symmetry_cell_setting           HEXAGONAL
_symmetry_space_group_name_H-M   '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                   8.3280(12)
_cell_length_b                   8.3280(12)
_cell_length_c                   23.012(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1382.2(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    302(2)
_cell_measurement_reflns_used    5573
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      58.86

_exptl_crystal_description       CUBIC
_exptl_crystal_colour            DARK
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             681
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_type   ANALYTICAL
_exptl_absorpt_correction_T_min  0.9441
_exptl_absorpt_correction_T_max  1.0697
_exptl_absorpt_process_details   'CRYSALIS V.171.33.42'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      302(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  Xcalibur
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5573
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         29.43
_reflns_number_total             834
_reflns_number_gt                667
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CRYSALIS V.171.33.42'
_computing_cell_refinement       'CRYSALIS V.171.33.42'
_computing_data_reduction        'CRYSALIS V.171.33.42'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAAMOND 3.2'
_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)+(0.0500P)²+1.2500P] 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         834
_refine_ls_number_parameters     47
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.1005
_refine_ls_wR_factor_gt          0.0974
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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
Cr1 Cr 0.3333 0.6667 0.6667 0.02332(11) Uani 1 6 d S . .
Na1 Na 0.6667 0.3333 0.8333 0.0279(3) Uani 1 6 d S . .
O1 O 0.89891(14) 0.57206(16) 0.77175(5) 0.0564(3) Uani 1 1 d . . .
C1 C 0.3333 0.6667 0.47626(16) 0.0948(15) Uani 1 3 d S . .
C2 C 0.3333 0.6667 0.37136(13) 0.0545(8) Uani 1 3 d S . .
N1 N 0.2526(5) 0.5925(5) 0.42687(17) 0.0443(10) Uani 0.33 1 d P . .
O2 O 0.14740(12) 0.68461(12) 0.71566(4) 0.0335(2) Uani 1 1 d . . .
C0 C 1.01046(17) 0.55406(19) 0.74122(6) 0.0348(3) Uani 1 1 d . . .
H0 H 1.0115 0.4423 0.7628 0.050 Uiso 1 1 d . . .
H1A H 0.2524 0.5921 0.5090 0.050 Uiso 0.33 1 d P . .
H1B H 0.3614 0.7865 0.4805 0.050 Uiso 0.33 1 d P . .
H1C H 0.4472 0.6587 0.4827 0.050 Uiso 0.33 1 d P . .
H2A H 0.2509 0.5906 0.3405 0.050 Uiso 0.33 1 d P . .
H2B H 0.4503 0.6795 0.3655 0.050 Uiso 0.33 1 d P . .
H2C H 0.3434 0.7875 0.3676 0.050 Uiso 0.33 1 d P . .
H1D H 0.1418 0.5723 0.4279 0.050 Uiso 0.33 1 d P . .
H1E H 0.2421 0.4730 0.4261 0.050 Uiso 0.33 1 d 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
Cr1 O2 1.9805(10) 13_566 ?
Cr1 O2 1.9806(10) 14_456 ?
Cr1 O2 1.9806(10) . ?
Cr1 O2 1.9806(10) 3_565 ?
Cr1 O2 1.9806(10) 2_665 ?
Cr1 O2 1.9806(10) 15_556 ?
Cr1 C0 2.9208(14) 13_666 ?
Cr1 C0 2.9209(14) 15_446 ?
Cr1 C0 2.9209(14) 3_675 ?
Cr1 C0 2.9209(14) 1_455 ?
Cr1 C0 2.9209(14) 14_466 ?
Cr1 C0 2.9209(14) 2_655 ?
Na1 O1 2.4200(11) 18_546 ?
Na1 O1 2.4200(11) 16_656 ?
Na1 O1 2.4201(11) 17_556 ?
Na1 O1 2.4201(11) 3_665 ?
Na1 O1 2.4201(11) . ?
Na1 O1 2.4201(11) 2_655 ?
O1 C0 1.2321(19) . ?
C1 N1 1.308(5) . ?
C1 N1 1.308(5) 3_565 ?
C1 N1 1.308(5) 2_665 ?
C1 H1A 0.9943 . ?
C1 H1B 0.9092 . ?
C1 H1C 0.9944 . ?
C2 N1 1.432(5) 3_565 ?
C2 N1 1.432(5) . ?
C2 N1 1.432(5) 2_665 ?
C2 H2A 0.9701 . ?
C2 H2B 0.9356 . ?
C2 H2C 0.9708 . ?
N1 N1 1.120(5) 3_565 ?
N1 N1 1.120(5) 2_665 ?
N1 H1D 0.8517 . ?
N1 H1E 0.9541 . ?
O2 C0 1.2605(15) 1_455 ?
C0 O2 1.2605(15) 1_655 ?
C0 Cr1 2.9209(14) 1_655 ?
C0 H0 1.0588 . ?

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
O2 Cr1 O2 90.80(4) 13_566 14_456 ?
O2 Cr1 O2 180.0 13_566 . ?
O2 Cr1 O2 89.20(4) 14_456 . ?
O2 Cr1 O2 89.20(4) 13_566 3_565 ?
O2 Cr1 O2 89.20(4) 14_456 3_565 ?
O2 Cr1 O2 90.80(4) . 3_565 ?
O2 Cr1 O2 89.20(4) 13_566 2_665 ?
O2 Cr1 O2 180.00(5) 14_456 2_665 ?
O2 Cr1 O2 90.80(4) . 2_665 ?
O2 Cr1 O2 90.80(4) 3_565 2_665 ?
O2 Cr1 O2 90.80(4) 13_566 15_556 ?
O2 Cr1 O2 90.80(4) 14_456 15_556 ?
O2 Cr1 O2 89.20(4) . 15_556 ?
O2 Cr1 O2 180.0 3_565 15_556 ?
O2 Cr1 O2 89.20(4) 2_665 15_556 ?
O2 Cr1 C0 20.10(4) 13_566 13_666 ?
O2 Cr1 C0 74.20(4) 14_456 13_666 ?
O2 Cr1 C0 159.90(4) . 13_666 ?
O2 Cr1 C0 77.97(4) 3_565 13_666 ?
O2 Cr1 C0 105.81(4) 2_665 13_666 ?
O2 Cr1 C0 102.03(4) 15_556 13_666 ?
O2 Cr1 C0 74.20(4) 13_566 15_446 ?
O2 Cr1 C0 102.03(4) 14_456 15_446 ?
O2 Cr1 C0 105.80(4) . 15_446 ?
O2 Cr1 C0 159.90(4) 3_565 15_446 ?
O2 Cr1 C0 77.97(4) 2_665 15_446 ?
O2 Cr1 C0 20.10(4) 15_556 15_446 ?
C0 Cr1 C0 89.00(4) 13_666 15_446 ?
O2 Cr1 C0 105.80(4) 13_566 3_675 ?
O2 Cr1 C0 77.97(4) 14_456 3_675 ?
O2 Cr1 C0 74.19(4) . 3_675 ?
O2 Cr1 C0 20.10(4) 3_565 3_675 ?
O2 Cr1 C0 102.03(4) 2_665 3_675 ?
O2 Cr1 C0 159.90(4) 15_556 3_675 ?
C0 Cr1 C0 91.00(4) 13_666 3_675 ?
C0 Cr1 C0 180.00(4) 15_446 3_675 ?
O2 Cr1 C0 159.90(4) 13_566 1_455 ?
O2 Cr1 C0 105.80(4) 14_456 1_455 ?
O2 Cr1 C0 20.10(4) . 1_455 ?
O2 Cr1 C0 102.03(4) 3_565 1_455 ?
O2 Cr1 C0 74.19(4) 2_665 1_455 ?
O2 Cr1 C0 77.98(4) 15_556 1_455 ?
C0 Cr1 C0 180.0 13_666 1_455 ?
C0 Cr1 C0 91.00(4) 15_446 1_455 ?
C0 Cr1 C0 89.00(4) 3_675 1_455 ?
O2 Cr1 C0 102.03(4) 13_566 14_466 ?
O2 Cr1 C0 20.10(4) 14_456 14_466 ?
O2 Cr1 C0 77.97(4) . 14_466 ?
O2 Cr1 C0 105.80(4) 3_565 14_466 ?
O2 Cr1 C0 159.90(4) 2_665 14_466 ?
O2 Cr1 C0 74.20(4) 15_556 14_466 ?
C0 Cr1 C0 89.00(4) 13_666 14_466 ?
C0 Cr1 C0 89.00(4) 15_446 14_466 ?
C0 Cr1 C0 91.00(4) 3_675 14_466 ?
C0 Cr1 C0 91.00(4) 1_455 14_466 ?
O2 Cr1 C0 77.97(4) 13_566 2_655 ?
O2 Cr1 C0 159.90(4) 14_456 2_655 ?
O2 Cr1 C0 102.03(4) . 2_655 ?
O2 Cr1 C0 74.19(4) 3_565 2_655 ?
O2 Cr1 C0 20.10(4) 2_665 2_655 ?
O2 Cr1 C0 105.81(4) 15_556 2_655 ?
C0 Cr1 C0 91.00(4) 13_666 2_655 ?
C0 Cr1 C0 91.00(4) 15_446 2_655 ?
C0 Cr1 C0 89.00(4) 3_675 2_655 ?
C0 Cr1 C0 89.00(4) 1_455 2_655 ?
C0 Cr1 C0 180.00(5) 14_466 2_655 ?
O1 Na1 O1 89.18(4) 18_546 16_656 ?
O1 Na1 O1 89.17(4) 18_546 17_556 ?
O1 Na1 O1 89.17(4) 16_656 17_556 ?
O1 Na1 O1 179.999(1) 18_546 3_665 ?
O1 Na1 O1 90.83(4) 16_656 3_665 ?
O1 Na1 O1 90.83(4) 17_556 3_665 ?
O1 Na1 O1 90.83(4) 18_546 . ?
O1 Na1 O1 179.999(1) 16_656 . ?
O1 Na1 O1 90.83(4) 17_556 . ?
O1 Na1 O1 89.17(4) 3_665 . ?
O1 Na1 O1 90.83(4) 18_546 2_655 ?
O1 Na1 O1 90.83(4) 16_656 2_655 ?
O1 Na1 O1 180.00(7) 17_556 2_655 ?
O1 Na1 O1 89.17(4) 3_665 2_655 ?
O1 Na1 O1 89.17(4) . 2_655 ?
C0 O1 Na1 125.13(10) . . ?
N1 C1 N1 50.7(3) . 3_565 ?
N1 C1 N1 50.7(3) . 2_665 ?
N1 C1 N1 50.7(3) 3_565 2_665 ?
N1 C1 H1A 109.6 . . ?
N1 C1 H1A 145.1 3_565 . ?
N1 C1 H1A 145.0 2_665 . ?
N1 C1 H1B 113.6 . . ?
N1 C1 H1B 66.8 3_565 . ?
N1 C1 H1B 105.7 2_665 . ?
H1A C1 H1B 109.1 . . ?
N1 C1 H1C 112.3 . . ?
N1 C1 H1C 111.6 3_565 . ?
N1 C1 H1C 68.9 2_665 . ?
H1A C1 H1C 102.5 . . ?
H1B C1 H1C 109.1 . . ?
N1 C2 N1 46.1(2) 3_565 . ?
N1 C2 N1 46.1(2) 3_565 2_665 ?
N1 C2 N1 46.1(2) . 2_665 ?
N1 C2 H2A 143.9 3_565 . ?
N1 C2 H2A 110.2 . . ?
N1 C2 H2A 143.7 2_665 . ?
N1 C2 H2B 106.4 3_565 . ?
N1 C2 H2B 114.6 . . ?
N1 C2 H2B 71.9 2_665 . ?
H2A C2 H2B 109.0 . . ?
N1 C2 H2C 68.2 3_565 . ?
N1 C2 H2C 107.7 . . ?
N1 C2 H2C 107.7 2_665 . ?
H2A C2 H2C 106.1 . . ?
H2B C2 H2C 108.9 . . ?
N1 N1 N1 60.000(3) 3_565 2_665 ?
N1 N1 C1 64.63(14) 3_565 . ?
N1 N1 C1 64.63(14) 2_665 . ?
N1 N1 C2 66.97(12) 3_565 . ?
N1 N1 C2 66.97(12) 2_665 . ?
C1 N1 C2 123.5(3) . . ?
N1 N1 H1D 104.0 3_565 . ?
N1 N1 H1D 163.9 2_665 . ?
C1 N1 H1D 108.6 . . ?
C2 N1 H1D 109.8 . . ?
N1 N1 H1E 150.4 3_565 . ?
N1 N1 H1E 90.4 2_665 . ?
C1 N1 H1E 105.4 . . ?
C2 N1 H1E 102.2 . . ?
H1D N1 H1E 105.6 . . ?
C0 O2 Cr1 127.22(10) 1_455 . ?
O1 C0 O2 124.97(15) . 1_655 ?
O1 C0 Cr1 157.65(11) . 1_655 ?
O2 C0 Cr1 32.68(7) 1_655 1_655 ?
O1 C0 H0 100.2 . . ?
O2 C0 H0 125.2 1_655 . ?
Cr1 C0 H0 98.5 1_655 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C0 H0 O1 1.06 2.84 3.4667(18) 118.3 3_665
C0 H0 N1 1.06 2.99 3.950(4) 150.8 6
C1 H1A O1 0.99 2.94 3.836(2) 150.7 15_446
C1 H1A O2 0.99 2.69 3.639(3) 160.6 15_556
C1 H1B O1 0.91 3.12 3.836(2) 136.7 14_466
C1 H1C O1 0.99 2.98 3.836(2) 145.0 13_666
C2 H2A O1 0.97 2.89 3.833(3) 163.2 10_666
C2 H2B O1 0.94 3.10 3.5764(19) 113.7 8_654
C2 H2B O2 0.94 2.89 3.4196(12) 116.8 7_544
C2 H2C O2 0.97 2.73 3.4196(12) 128.5 8_664
N1 H1D O1 0.85 2.41 3.065(4) 134.1 9_564
N1 H1D O2 0.85 2.32 3.099(4) 151.5 9_454
N1 H1E O1 0.95 1.93 2.877(4) 170.2 7_444
N1 H1E O2 0.95 2.83 3.537(4) 131.7 7_544

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        29.43
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.065
####################################################################### 
# 
# 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_r-3p115
_database_code_depnum_ccdc_archive 'CCDC 1042424'
_audit_update_record             
;
2015-01-07 deposited with the CCDC.
2015-03-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H11 Cr0.50 N Na0.50 O6'
_chemical_formula_weight         218.64

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'
Cr Cr 0.3209 0.6236 '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'

_symmetry_cell_setting           HEXAGONAL
_symmetry_space_group_name_H-M   '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                   8.3121(12)
_cell_length_b                   8.3121(12)
_cell_length_c                   22.778(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1362.9(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    115(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       CUBIC
_exptl_crystal_colour            DARK
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             681
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_type   ANALYTICAL
_exptl_absorpt_correction_T_min  0.8921
_exptl_absorpt_correction_T_max  1.1226
_exptl_absorpt_process_details   'CRYSALIS V.171.33.42'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      115(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  Xcalibur
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4546
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         29.58
_reflns_number_total             830
_reflns_number_gt                547
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CRYSALIS V.171.33.42'
_computing_cell_refinement       'CRYSALIS V.171.33.42'
_computing_data_reduction        'CRYSALIS V.171.33.42'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND 3.2'
_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)+(0.0250P)²+10.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         830
_refine_ls_number_parameters     47
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.1299
_refine_ls_wR_factor_gt          0.1131
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.008

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
Cr1 Cr 0.3333 0.6667 0.6667 0.02285(11) Uani 1 6 d S . .
Na1 Na 0.6667 0.3333 0.8333 0.0254(3) Uani 1 6 d S . .
O1 O 0.89650(13) 0.57304(13) 0.77190(4) 0.0432(3) Uani 1 1 d . . .
C1 C 0.3333 0.6667 0.47934(12) 0.0815(12) Uani 1 3 d S . .
C2 C 0.3333 0.6667 0.37144(9) 0.0363(6) Uani 1 3 d S . .
N1 N 0.2561(4) 0.5980(4) 0.42857(12) 0.0310(10) Uani 0.33 1 d P . .
O2 O 0.14890(11) 0.68823(11) 0.71597(3) 0.0275(3) Uani 1 1 d . . .
C0 C 1.00821(16) 0.55434(17) 0.74127(5) 0.0298(4) Uani 1 1 d . . .
H0 H 1.0115 0.4423 0.7628 0.050 Uiso 1 1 d . . .
H1A H 0.2524 0.5921 0.5090 0.050 Uiso 0.33 1 d P . .
H1B H 0.3614 0.7865 0.4805 0.050 Uiso 0.33 1 d P . .
H1C H 0.4472 0.6587 0.4827 0.050 Uiso 0.33 1 d P . .
H2A H 0.2509 0.5906 0.3405 0.050 Uiso 0.33 1 d P . .
H2B H 0.4503 0.6795 0.3655 0.050 Uiso 0.33 1 d P . .
H2C H 0.3434 0.7875 0.3676 0.050 Uiso 0.33 1 d P . .
H1D H 0.1418 0.5723 0.4279 0.050 Uiso 0.33 1 d P . .
H1E H 0.2421 0.4730 0.4261 0.050 Uiso 0.33 1 d 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
Cr1 O2 1.9794(10) 13_566 ?
Cr1 O2 1.9794(10) . ?
Cr1 O2 1.9794(10) 3_565 ?
Cr1 O2 1.9794(10) 14_456 ?
Cr1 O2 1.9794(9) 2_665 ?
Cr1 O2 1.9794(10) 15_556 ?
Cr1 C0 2.9222(13) 13_666 ?
Cr1 C0 2.9222(13) 15_446 ?
Cr1 C0 2.9222(13) 3_675 ?
Cr1 C0 2.9222(13) 1_455 ?
Cr1 C0 2.9222(13) 14_466 ?
Cr1 C0 2.9222(13) 2_655 ?
Na1 O1 2.4022(9) 18_546 ?
Na1 O1 2.4023(9) 16_656 ?
Na1 O1 2.4023(9) 17_556 ?
Na1 O1 2.4023(9) 3_665 ?
Na1 O1 2.4023(9) . ?
Na1 O1 2.4023(9) 2_655 ?
O1 C0 1.2318(18) . ?
C1 N1 1.307(4) . ?
C1 N1 1.307(4) 3_565 ?
C1 N1 1.307(4) 2_665 ?
C1 H1A 0.9360 . ?
C1 H1B 0.9027 . ?
C1 H1C 0.9844 . ?
C2 N1 1.437(3) 3_565 ?
C2 N1 1.437(3) 2_665 ?
C2 N1 1.437(3) . ?
C2 H2A 0.9653 . ?
C2 H2B 0.9339 . ?
C2 H2C 0.9691 . ?
N1 N1 1.056(4) 2_665 ?
N1 N1 1.056(4) 3_565 ?
N1 H1D 0.8638 . ?
N1 H1E 0.9870 . ?
O2 C0 1.2794(13) 1_455 ?
C0 O2 1.2794(12) 1_655 ?
C0 Cr1 2.9222(13) 1_655 ?
C0 H0 1.0648 . ?

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
O2 Cr1 O2 180.0 13_566 . ?
O2 Cr1 O2 89.01(4) 13_566 3_565 ?
O2 Cr1 O2 90.99(4) . 3_565 ?
O2 Cr1 O2 90.99(4) 13_566 14_456 ?
O2 Cr1 O2 89.01(4) . 14_456 ?
O2 Cr1 O2 89.01(4) 3_565 14_456 ?
O2 Cr1 O2 89.01(4) 13_566 2_665 ?
O2 Cr1 O2 90.99(4) . 2_665 ?
O2 Cr1 O2 90.99(4) 3_565 2_665 ?
O2 Cr1 O2 180.00(5) 14_456 2_665 ?
O2 Cr1 O2 90.99(4) 13_566 15_556 ?
O2 Cr1 O2 89.01(4) . 15_556 ?
O2 Cr1 O2 180.0 3_565 15_556 ?
O2 Cr1 O2 90.99(4) 14_456 15_556 ?
O2 Cr1 O2 89.01(4) 2_665 15_556 ?
O2 Cr1 C0 20.72(4) 13_566 13_666 ?
O2 Cr1 C0 159.28(4) . 13_666 ?
O2 Cr1 C0 77.22(4) 3_565 13_666 ?
O2 Cr1 C0 74.00(4) 14_456 13_666 ?
O2 Cr1 C0 106.00(4) 2_665 13_666 ?
O2 Cr1 C0 102.78(4) 15_556 13_666 ?
O2 Cr1 C0 74.00(4) 13_566 15_446 ?
O2 Cr1 C0 106.00(4) . 15_446 ?
O2 Cr1 C0 159.28(4) 3_565 15_446 ?
O2 Cr1 C0 102.78(4) 14_456 15_446 ?
O2 Cr1 C0 77.22(4) 2_665 15_446 ?
O2 Cr1 C0 20.72(4) 15_556 15_446 ?
C0 Cr1 C0 89.59(3) 13_666 15_446 ?
O2 Cr1 C0 106.00(4) 13_566 3_675 ?
O2 Cr1 C0 74.00(4) . 3_675 ?
O2 Cr1 C0 20.72(4) 3_565 3_675 ?
O2 Cr1 C0 77.22(4) 14_456 3_675 ?
O2 Cr1 C0 102.78(4) 2_665 3_675 ?
O2 Cr1 C0 159.28(4) 15_556 3_675 ?
C0 Cr1 C0 90.42(3) 13_666 3_675 ?
C0 Cr1 C0 180.00(4) 15_446 3_675 ?
O2 Cr1 C0 159.28(4) 13_566 1_455 ?
O2 Cr1 C0 20.72(4) . 1_455 ?
O2 Cr1 C0 102.78(4) 3_565 1_455 ?
O2 Cr1 C0 106.00(4) 14_456 1_455 ?
O2 Cr1 C0 74.00(4) 2_665 1_455 ?
O2 Cr1 C0 77.22(4) 15_556 1_455 ?
C0 Cr1 C0 180.0 13_666 1_455 ?
C0 Cr1 C0 90.42(3) 15_446 1_455 ?
C0 Cr1 C0 89.58(3) 3_675 1_455 ?
O2 Cr1 C0 102.78(4) 13_566 14_466 ?
O2 Cr1 C0 77.22(4) . 14_466 ?
O2 Cr1 C0 106.00(4) 3_565 14_466 ?
O2 Cr1 C0 20.72(4) 14_456 14_466 ?
O2 Cr1 C0 159.28(4) 2_665 14_466 ?
O2 Cr1 C0 74.00(4) 15_556 14_466 ?
C0 Cr1 C0 89.58(3) 13_666 14_466 ?
C0 Cr1 C0 89.58(3) 15_446 14_466 ?
C0 Cr1 C0 90.42(3) 3_675 14_466 ?
C0 Cr1 C0 90.42(3) 1_455 14_466 ?
O2 Cr1 C0 77.22(4) 13_566 2_655 ?
O2 Cr1 C0 102.78(4) . 2_655 ?
O2 Cr1 C0 74.00(4) 3_565 2_655 ?
O2 Cr1 C0 159.28(4) 14_456 2_655 ?
O2 Cr1 C0 20.72(4) 2_665 2_655 ?
O2 Cr1 C0 106.00(4) 15_556 2_655 ?
C0 Cr1 C0 90.42(3) 13_666 2_655 ?
C0 Cr1 C0 90.42(3) 15_446 2_655 ?
C0 Cr1 C0 89.58(3) 3_675 2_655 ?
C0 Cr1 C0 89.58(3) 1_455 2_655 ?
C0 Cr1 C0 180.00(4) 14_466 2_655 ?
O1 Na1 O1 89.49(3) 18_546 16_656 ?
O1 Na1 O1 89.49(3) 18_546 17_556 ?
O1 Na1 O1 89.49(3) 16_656 17_556 ?
O1 Na1 O1 179.999(1) 18_546 3_665 ?
O1 Na1 O1 90.51(3) 16_656 3_665 ?
O1 Na1 O1 90.51(3) 17_556 3_665 ?
O1 Na1 O1 90.51(3) 18_546 . ?
O1 Na1 O1 179.999(1) 16_656 . ?
O1 Na1 O1 90.51(3) 17_556 . ?
O1 Na1 O1 89.49(3) 3_665 . ?
O1 Na1 O1 90.51(3) 18_546 2_655 ?
O1 Na1 O1 90.51(3) 16_656 2_655 ?
O1 Na1 O1 180.00(6) 17_556 2_655 ?
O1 Na1 O1 89.49(3) 3_665 2_655 ?
O1 Na1 O1 89.49(3) . 2_655 ?
C0 O1 Na1 124.21(9) . . ?
N1 C1 N1 47.6(2) . 3_565 ?
N1 C1 N1 47.6(2) . 2_665 ?
N1 C1 N1 47.6(2) 3_565 2_665 ?
N1 C1 H1A 108.4 . . ?
N1 C1 H1A 143.9 3_565 . ?
N1 C1 H1A 142.3 2_665 . ?
N1 C1 H1B 107.9 . . ?
N1 C1 H1B 64.1 3_565 . ?
N1 C1 H1B 101.9 2_665 . ?
H1A C1 H1B 114.5 . . ?
N1 C1 H1C 108.5 . . ?
N1 C1 H1C 106.5 3_565 . ?
N1 C1 H1C 66.7 2_665 . ?
H1A C1 H1C 107.2 . . ?
H1B C1 H1C 110.2 . . ?
N1 C2 N1 43.10(18) 3_565 2_665 ?
N1 C2 N1 43.10(18) 3_565 . ?
N1 C2 N1 43.10(18) 2_665 . ?
N1 C2 H2A 144.5 3_565 . ?
N1 C2 H2A 142.9 2_665 . ?
N1 C2 H2A 111.8 . . ?
N1 C2 H2B 105.3 3_565 . ?
N1 C2 H2B 73.8 2_665 . ?
N1 C2 H2B 114.2 . . ?
H2A C2 H2B 109.0 . . ?
N1 C2 H2C 70.1 3_565 . ?
N1 C2 H2C 107.6 2_665 . ?
N1 C2 H2C 106.4 . . ?
H2A C2 H2C 106.1 . . ?
H2B C2 H2C 108.9 . . ?
N1 N1 N1 60.000(2) 2_665 3_565 ?
N1 N1 C1 66.18(10) 2_665 . ?
N1 N1 C1 66.18(10) 3_565 . ?
N1 N1 C2 68.45(9) 2_665 . ?
N1 N1 C2 68.45(9) 3_565 . ?
C1 N1 C2 127.1(2) . . ?
N1 N1 H1D 168.1 2_665 . ?
N1 N1 H1D 108.1 3_565 . ?
C1 N1 H1D 111.2 . . ?
C2 N1 H1D 107.5 . . ?
N1 N1 H1E 90.1 2_665 . ?
N1 N1 H1E 149.9 3_565 . ?
C1 N1 H1E 106.5 . . ?
C2 N1 H1E 99.3 . . ?
H1D N1 H1E 101.7 . . ?
C0 O2 Cr1 126.10(9) 1_455 . ?
O1 C0 O2 124.35(13) . 1_655 ?
O1 C0 Cr1 157.53(9) . 1_655 ?
O2 C0 Cr1 33.18(6) 1_655 1_655 ?
O1 C0 H0 101.5 . . ?
O2 C0 H0 123.8 1_655 . ?
Cr1 C0 H0 97.1 1_655 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C0 H0 O1 1.06 2.81 3.4350(16) 117.7 3_665
C0 H0 N1 1.06 3.02 3.995(3) 152.1 6
C1 H1A O1 0.94 2.95 3.8027(17) 152.7 15_446
C1 H1A O2 0.94 2.66 3.541(3) 157.9 15_556
C1 H1B O1 0.90 3.12 3.8027(17) 133.7 14_466
C1 H1C O1 0.98 2.98 3.8027(17) 142.0 13_666
C2 H2A O1 0.97 2.87 3.804(2) 163.0 10_666
C2 H2B O1 0.93 3.07 3.5525(14) 113.9 8_654
C2 H2B O2 0.93 2.87 3.3941(12) 117.0 7_544
C2 H2C O2 0.97 2.70 3.3941(12) 128.7 8_664
N1 H1D O1 0.86 2.40 3.036(4) 130.7 9_564
N1 H1D O2 0.86 2.29 3.094(4) 154.2 9_454
N1 H1E O1 0.99 1.91 2.884(4) 167.8 7_444
N1 H1E O2 0.99 2.81 3.537(4) 131.1 7_544

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        29.58
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.097
