# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 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_EtNaAl375K
_database_code_depnum_ccdc_archive 'CCDC 1495522'
_audit_update_record             
;
2016-07-22 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H22 Al N2 Na O12'
_chemical_formula_weight         412.26

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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

_cell_length_a                   8.0388(6)
_cell_length_b                   9.3156(11)
_cell_length_c                   12.0288(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.792(8)
_cell_angle_gamma                90
_cell_volume                     900.71(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    375(2)
_cell_measurement_reflns_used    1559
_cell_measurement_theta_min      2.7470
_cell_measurement_theta_max      23.5340

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_min  0.92630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.928
_oxdiff_exptl_absorpt_empirical_full_max 1.079
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      375(2)
_diffrn_ambient_environment      air
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6502
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.766
_diffrn_reflns_theta_max         25.673
_diffrn_reflns_theta_full        25.673
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1709
_reflns_number_gt                1083
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0550P)²+0.1300P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1709
_refine_ls_number_parameters     149
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1456
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.040
_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_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
Al Al 0.0000 0.0000 0.5000 0.0365(4) Uani 1 2 d S . P . .
Na Na 0.0000 0.0000 0.0000 0.0435(5) Uani 1 2 d S . P . .
O1 O 0.1108(3) 0.0216(2) 0.36341(17) 0.0432(6) Uani 1 1 d . . . . .
O2 O 0.1899(3) -0.0961(2) 0.55998(18) 0.0464(6) Uani 1 1 d . . . . .
O3 O 0.0890(3) 0.1769(2) 0.55195(18) 0.0445(6) Uani 1 1 d . . . . .
O4 O 0.1369(3) 0.0346(3) 0.18147(19) 0.0537(7) Uani 1 1 d . . . . .
O5 O 0.3864(3) -0.2640(3) 0.5756(2) 0.0607(7) Uani 1 1 d . . . . .
O6 O 0.2607(4) 0.3609(3) 0.5593(2) 0.0776(9) Uani 1 1 d . . . . .
C1 C 0.0570(4) 0.0082(3) 0.2645(3) 0.0413(8) Uani 1 1 d . . . . .
H1 H -0.0516 -0.0243 0.2544 0.050 Uiso 1 1 calc R U . . .
C2 C 0.2186(4) 0.2445(4) 0.5229(3) 0.0563(10) Uani 1 1 d . . . . .
H2 H 0.2860 0.2020 0.4699 0.068 Uiso 1 1 calc R U . . .
C3 C 0.2661(5) -0.2076(4) 0.5290(3) 0.0534(9) Uani 1 1 d . . . . .
H3 H 0.2270 -0.2515 0.4642 0.064 Uiso 1 1 calc R U . . .
C4 C 0.5304(13) -0.0277(8) 0.2878(8) 0.064(3) Uani 0.454(9) 1 d D U P A 1
H4A H 0.4607 -0.0515 0.3504 0.076 Uiso 0.454(9) 1 calc R U P A 1
H4B H 0.6455 -0.0288 0.3133 0.076 Uiso 0.454(9) 1 calc R U P A 1
C5 C 0.5061(17) -0.1368(10) 0.1974(11) 0.108(5) Uani 0.454(9) 1 d D U P A 1
H5A H 0.4780 -0.2277 0.2298 0.162 Uiso 0.454(9) 1 calc R U P A 1
H5B H 0.6069 -0.1462 0.1563 0.162 Uiso 0.454(9) 1 calc R U P A 1
H5C H 0.4177 -0.1063 0.1484 0.162 Uiso 0.454(9) 1 calc R U P A 1
N2 N 0.488(3) 0.1152(8) 0.2465(13) 0.067(6) Uani 0.454(9) 1 d D U P A 1
H2A H 0.3775 0.1230 0.2402 0.101 Uiso 0.454(9) 1 calc R U P A 1
H2B H 0.5332 0.1285 0.1803 0.101 Uiso 0.454(9) 1 calc R U P A 1
H2C H 0.5259 0.1811 0.2939 0.101 Uiso 0.454(9) 1 calc R U P A 1
C6 C 0.5506(10) -0.0215(7) 0.2059(7) 0.073(3) Uani 0.546(9) 1 d D U P A 2
H6A H 0.6708 -0.0123 0.2082 0.088 Uiso 0.546(9) 1 calc R U P A 2
H6B H 0.5181 -0.0573 0.1331 0.088 Uiso 0.546(9) 1 calc R U P A 2
C7 C 0.4963(13) -0.1251(8) 0.2936(9) 0.097(4) Uani 0.546(9) 1 d D U P A 2
H7A H 0.4056 -0.0845 0.3341 0.146 Uiso 0.546(9) 1 calc R U P A 2
H7B H 0.5876 -0.1441 0.3438 0.146 Uiso 0.546(9) 1 calc R U P A 2
H7C H 0.4609 -0.2131 0.2591 0.146 Uiso 0.546(9) 1 calc R U P A 2
N1 N 0.474(2) 0.1186(8) 0.2243(11) 0.050(3) Uani 0.546(9) 1 d D U P A 2
H1A H 0.3642 0.1094 0.2244 0.075 Uiso 0.546(9) 1 calc R U P A 2
H1B H 0.5035 0.1784 0.1702 0.075 Uiso 0.546(9) 1 calc R U P A 2
H1C H 0.5091 0.1535 0.2895 0.075 Uiso 0.546(9) 1 calc R U P A 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
Al O1 1.890(2) 3_556 ?
Al O1 1.890(2) . ?
Al O3 1.899(2) 3_556 ?
Al O3 1.899(2) . ?
Al O2 1.903(2) . ?
Al O2 1.904(2) 3_556 ?
Na O6 2.434(3) 4_565 ?
Na O6 2.434(3) 2_545 ?
Na O4 2.452(2) . ?
Na O4 2.452(2) 3 ?
Na O5 2.553(2) 2 ?
Na O5 2.553(2) 4 ?
O1 C1 1.267(4) . ?
O2 C3 1.264(4) . ?
O3 C2 1.271(4) . ?
O4 C1 1.219(4) . ?
O5 C3 1.230(4) . ?
O5 Na 2.553(2) 2_545 ?
O6 C2 1.215(4) . ?
O6 Na 2.434(3) 2 ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 N2 1.4600(11) . ?
C4 C5 1.4995(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C6 N1 1.4601(11) . ?
C6 C7 1.4995(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?

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 Al O1 180.0 3_556 . ?
O1 Al O3 90.79(9) 3_556 3_556 ?
O1 Al O3 89.21(9) . 3_556 ?
O1 Al O3 89.21(9) 3_556 . ?
O1 Al O3 90.79(9) . . ?
O3 Al O3 180.0 3_556 . ?
O1 Al O2 90.31(9) 3_556 . ?
O1 Al O2 89.69(9) . . ?
O3 Al O2 90.76(9) 3_556 . ?
O3 Al O2 89.24(9) . . ?
O1 Al O2 89.69(9) 3_556 3_556 ?
O1 Al O2 90.31(9) . 3_556 ?
O3 Al O2 89.24(9) 3_556 3_556 ?
O3 Al O2 90.76(9) . 3_556 ?
O2 Al O2 180.0 . 3_556 ?
O6 Na O6 180.00(14) 4_565 2_545 ?
O6 Na O4 90.92(9) 4_565 . ?
O6 Na O4 89.08(9) 2_545 . ?
O6 Na O4 89.08(9) 4_565 3 ?
O6 Na O4 90.92(9) 2_545 3 ?
O4 Na O4 180.0 . 3 ?
O6 Na O5 86.21(9) 4_565 2 ?
O6 Na O5 93.79(9) 2_545 2 ?
O4 Na O5 92.63(8) . 2 ?
O4 Na O5 87.37(8) 3 2 ?
O6 Na O5 93.79(9) 4_565 4 ?
O6 Na O5 86.21(9) 2_545 4 ?
O4 Na O5 87.37(8) . 4 ?
O4 Na O5 92.63(8) 3 4 ?
O5 Na O5 180.00(12) 2 4 ?
C1 O1 Al 130.3(2) . . ?
C3 O2 Al 131.6(2) . . ?
C2 O3 Al 130.3(2) . . ?
C1 O4 Na 117.9(2) . . ?
C3 O5 Na 119.2(2) . 2_545 ?
C2 O6 Na 125.9(3) . 2 ?
O4 C1 O1 124.9(3) . . ?
O4 C1 H1 117.5 . . ?
O1 C1 H1 117.5 . . ?
O6 C2 O3 124.6(3) . . ?
O6 C2 H2 117.7 . . ?
O3 C2 H2 117.7 . . ?
O5 C3 O2 126.7(3) . . ?
O5 C3 H3 116.7 . . ?
O2 C3 H3 116.7 . . ?
N2 C4 C5 110.1(3) . . ?
N2 C4 H4A 109.6 . . ?
C5 C4 H4A 109.6 . . ?
N2 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
H4A C4 H4B 108.2 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N1 C6 C7 110.0(3) . . ?
N1 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
N1 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 N1 H1A 109.5 . . ?
C6 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C6 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?

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
C2 H2 O1 0.93 2.53 2.949(4) 107.7 .
C4 H4B O2 0.97 2.32 3.102(9) 137.3 3_656
N2 H2A O4 0.89 2.21 3.01(3) 149.5 .
N2 H2B O3 0.89 2.43 3.154(15) 139.0 4_665
N2 H2B O6 0.89 2.36 3.18(2) 153.1 4_665
N2 H2C O5 0.89 1.88 2.732(18) 160.3 3_656
C6 H6A O6 0.97 2.40 2.879(7) 109.9 4_665
C7 H7C O4 0.96 2.58 3.361(8) 138.4 2_545
N1 H1A O4 0.89 2.02 2.86(2) 158.7 .
N1 H1B O3 0.89 2.08 2.972(11) 175.1 4_665
N1 H1B O6 0.89 2.50 3.066(15) 121.7 4_665
N1 H1C O5 0.89 2.09 2.967(16) 169.2 3_656

_refine_diff_density_max         0.259
_refine_diff_density_min         -0.247
_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_EtNaAl270K
_database_code_depnum_ccdc_archive 'CCDC 1495523'
_audit_update_record             
;
2016-07-22 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H11 Al0.50 N Na0.50 O6'
_chemical_formula_weight         206.13

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P n'
_space_group_name_Hall           'P -2yac'

_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.
;

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

_cell_length_a                   8.0343(3)
_cell_length_b                   9.2310(4)
_cell_length_c                   11.9465(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.966(3)
_cell_angle_gamma                90
_cell_volume                     885.88(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    2167
_cell_measurement_theta_min      2.7720
_cell_measurement_theta_max      26.4980

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_min  0.98297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.936
_oxdiff_exptl_absorpt_empirical_full_max 1.076
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      270(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            6476
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.789
_diffrn_reflns_theta_max         25.668
_diffrn_reflns_theta_full        25.668
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3186
_reflns_number_gt                2641
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
#_refine_ls_abs_structure_Flack    0.000(0)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3186
_refine_ls_number_parameters     240
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1047
_refine_ls_wR_factor_gt          0.0932
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.038
_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_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
Al1 Al 0.3193(3) 0.72717(17) 0.53666(18) 0.0200(3) Uani 1 1 d . . . . .
Na Na -0.1853(4) 0.2286(2) 0.5378(2) 0.0247(5) Uani 1 1 d . . . . .
O1 O 0.4318(5) 0.7092(4) 0.3995(3) 0.0247(10) Uani 1 1 d . . . . .
O2 O 0.4569(5) 0.7172(5) 0.2155(3) 0.0322(11) Uani 1 1 d . . . . .
O3 O 0.5092(5) 0.8237(4) 0.5997(3) 0.0246(9) Uani 1 1 d . . . . .
O4 O 0.1759(5) 0.7850(5) 0.8547(4) 0.0343(11) Uani 1 1 d . . . . .
O5 O 0.2297(5) 0.9070(4) 0.4845(3) 0.0236(9) Uani 1 1 d . . . . .
O6 O 0.7071(5) 0.9916(4) 0.6138(4) 0.0326(10) Uani 1 1 d . . . . .
O7 O 0.4068(5) 0.5490(4) 0.5900(3) 0.0249(9) Uani 1 1 d . . . . .
O8 O 0.5703(5) 0.3573(4) 0.6000(4) 0.0366(11) Uani 1 1 d . . . . .
O9 O 0.1301(5) 0.6299(4) 0.4749(3) 0.0254(9) Uani 1 1 d . . . . .
O10 O -0.0709(5) 0.4637(4) 0.4629(4) 0.0320(10) Uani 1 1 d . . . . .
O11 O 0.2045(5) 0.7504(4) 0.6728(3) 0.0242(10) Uani 1 1 d . . . . .
O12 O 0.0399(6) 1.0806(4) 0.4759(4) 0.0419(12) Uani 1 1 d . . . . .
C1 C 0.0532(8) 0.5193(6) 0.5090(5) 0.0293(15) Uani 1 1 d . . . . .
H1 H 0.0930 0.4757 0.5743 0.035 Uiso 1 1 calc R U . . .
C2 C 0.0903(7) 0.9636(6) 0.5108(5) 0.0276(14) Uani 1 1 d . . . . .
H2 H 0.0229 0.9126 0.5595 0.033 Uiso 1 1 calc R U . . .
C3 C 0.5897(7) 0.9313(6) 0.5656(5) 0.0285(15) Uani 1 1 d . . . . .
H3 H 0.5570 0.9694 0.4967 0.034 Uiso 1 1 calc R U . . .
C4 C 0.5303(7) 0.4730(6) 0.5589(5) 0.0297(15) Uani 1 1 d . . . . .
H4 H 0.5942 0.5085 0.5008 0.036 Uiso 1 1 calc R U . . .
C5 C 0.3777(8) 0.7332(6) 0.3008(5) 0.0255(15) Uani 1 1 d . . . . .
H5 H 0.2687 0.7659 0.2929 0.031 Uiso 1 1 calc R U . . .
C6 C 0.2576(8) 0.7486(6) 0.7730(6) 0.0263(15) Uani 1 1 d . . . . .
H6 H 0.3664 0.7176 0.7860 0.032 Uiso 1 1 calc R U . . .
N2 N 0.3379(7) 0.1292(5) 0.3163(5) 0.0333(13) Uani 1 1 d . . . . .
H2A H 0.4483 0.1371 0.3195 0.050 Uiso 1 1 calc R U . . .
H2B H 0.3066 0.0952 0.2495 0.050 Uiso 1 1 calc R U . . .
H2C H 0.3045 0.0686 0.3694 0.050 Uiso 1 1 calc R U . . .
C7 C 0.2623(9) 0.2727(7) 0.3339(7) 0.0463(18) Uani 1 1 d . . . . .
H7A H 0.2980 0.3103 0.4062 0.056 Uiso 1 1 calc R U . . .
H7B H 0.1420 0.2631 0.3342 0.056 Uiso 1 1 calc R U . . .
C8 C 0.3102(10) 0.3758(7) 0.2450(8) 0.061(2) Uani 1 1 d . . . . .
H8A H 0.4275 0.3949 0.2507 0.092 Uiso 1 1 calc R U . . .
H8B H 0.2498 0.4647 0.2536 0.092 Uiso 1 1 calc R U . . .
H8C H 0.2845 0.3347 0.1729 0.092 Uiso 1 1 calc R U . . .
N1 N 0.2976(7) 0.3641(5) 0.7842(4) 0.0364(14) Uani 1 1 d . . . . .
H1A H 0.1886 0.3618 0.7696 0.055 Uiso 1 1 calc R U . . .
H1B H 0.3511 0.3921 0.7233 0.055 Uiso 1 1 calc R U . . .
H1C H 0.3183 0.4263 0.8396 0.055 Uiso 1 1 calc R U . . .
C10 C 0.3183(11) 0.1110(8) 0.7295(9) 0.073(3) Uani 1 1 d . . . . .
H10A H 0.3501 0.1491 0.6581 0.109 Uiso 1 1 calc R U . . .
H10B H 0.2013 0.0898 0.7280 0.109 Uiso 1 1 calc R U . . .
H10C H 0.3797 0.0239 0.7449 0.109 Uiso 1 1 calc R U . . .
C9 C 0.3547(9) 0.2190(7) 0.8175(7) 0.049(2) Uani 1 1 d . . . . .
H9A H 0.3001 0.1906 0.8859 0.059 Uiso 1 1 calc R U . . .
H9B H 0.4736 0.2215 0.8326 0.059 Uiso 1 1 calc R U . . .


_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
Al1 O1 1.892(4) . ?
Al1 O7 1.894(4) . ?
Al1 O11 1.895(5) . ?
Al1 O9 1.904(4) . ?
Al1 O5 1.910(4) . ?
Al1 O3 1.911(4) . ?
Na O12 2.394(5) 1_545 ?
Na O8 2.422(5) 1_455 ?
Na O4 2.442(6) 2_464 ?
Na O2 2.445(5) 2_465 ?
Na O6 2.526(4) 1_445 ?
Na O10 2.527(4) . ?
O1 C5 1.269(8) . ?
O2 C5 1.219(8) . ?
O2 Na 2.446(5) 2_564 ?
O3 C3 1.257(7) . ?
O4 C6 1.233(8) . ?
O4 Na 2.442(6) 2_565 ?
O5 C2 1.280(7) . ?
O6 C3 1.230(7) . ?
O6 Na 2.526(4) 1_665 ?
O7 C4 1.276(7) . ?
O8 C4 1.217(7) . ?
O8 Na 2.422(5) 1_655 ?
O9 C1 1.264(7) . ?
O10 C1 1.242(7) . ?
O11 C6 1.264(8) . ?
O12 C2 1.224(7) . ?
O12 Na 2.394(5) 1_565 ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
N2 C7 1.474(8) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C7 C8 1.483(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 C9 1.469(9) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C10 C9 1.475(11) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?

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 Al1 O7 92.00(18) . . ?
O1 Al1 O11 178.4(2) . . ?
O7 Al1 O11 89.59(18) . . ?
O1 Al1 O9 90.75(19) . . ?
O7 Al1 O9 90.59(18) . . ?
O11 Al1 O9 89.36(19) . . ?
O1 Al1 O5 88.66(18) . . ?
O7 Al1 O5 179.3(2) . . ?
O11 Al1 O5 89.75(18) . . ?
O9 Al1 O5 89.39(19) . . ?
O1 Al1 O3 89.56(19) . . ?
O7 Al1 O3 89.02(19) . . ?
O11 Al1 O3 90.34(19) . . ?
O9 Al1 O3 179.5(2) . . ?
O5 Al1 O3 90.99(18) . . ?
O12 Na O8 174.44(19) 1_545 1_455 ?
O12 Na O4 91.73(18) 1_545 2_464 ?
O8 Na O4 86.54(18) 1_455 2_464 ?
O12 Na O2 92.32(19) 1_545 2_465 ?
O8 Na O2 90.15(17) 1_455 2_465 ?
O4 Na O2 171.03(19) 2_464 2_465 ?
O12 Na O6 83.22(15) 1_545 1_445 ?
O8 Na O6 91.75(17) 1_455 1_445 ?
O4 Na O6 97.11(17) 2_464 1_445 ?
O2 Na O6 91.32(17) 2_465 1_445 ?
O12 Na O10 95.69(18) 1_545 . ?
O8 Na O10 89.37(15) 1_455 . ?
O4 Na O10 83.68(16) 2_464 . ?
O2 Na O10 87.95(16) 2_465 . ?
O6 Na O10 178.7(2) 1_445 . ?
C5 O1 Al1 128.9(4) . . ?
C5 O2 Na 117.2(4) . 2_564 ?
C3 O3 Al1 130.7(4) . . ?
C6 O4 Na 117.0(4) . 2_565 ?
C2 O5 Al1 127.0(4) . . ?
C3 O6 Na 119.2(4) . 1_665 ?
C4 O7 Al1 131.8(4) . . ?
C4 O8 Na 121.1(4) . 1_655 ?
C1 O9 Al1 130.4(4) . . ?
C1 O10 Na 119.5(4) . . ?
C6 O11 Al1 130.5(4) . . ?
C2 O12 Na 130.2(4) . 1_565 ?
O10 C1 O9 125.7(6) . . ?
O10 C1 H1 117.1 . . ?
O9 C1 H1 117.1 . . ?
O12 C2 O5 124.2(5) . . ?
O12 C2 H2 117.9 . . ?
O5 C2 H2 117.9 . . ?
O6 C3 O3 126.9(6) . . ?
O6 C3 H3 116.5 . . ?
O3 C3 H3 116.5 . . ?
O8 C4 O7 124.6(6) . . ?
O8 C4 H4 117.7 . . ?
O7 C4 H4 117.7 . . ?
O2 C5 O1 125.4(6) . . ?
O2 C5 H5 117.3 . . ?
O1 C5 H5 117.3 . . ?
O4 C6 O11 124.8(6) . . ?
O4 C6 H6 117.6 . . ?
O11 C6 H6 117.6 . . ?
C7 N2 H2A 109.5 . . ?
C7 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C7 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N2 C7 C8 111.3(6) . . ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 N1 H1A 109.5 . . ?
C9 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C9 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C9 C10 111.5(7) . . ?
N1 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
N1 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?

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
C2 H2 O11 0.93 2.48 2.899(7) 107.7 .
C4 H4 O1 0.93 2.56 2.993(7) 108.9 .
N2 H2A O4 0.89 2.00 2.858(7) 160.7 2_564
N2 H2B O6 0.89 1.97 2.848(7) 171.1 2_464
N2 H2C O5 0.89 2.12 3.009(7) 174.2 1_545
N2 H2C O12 0.89 2.50 3.118(7) 127.2 1_545
C7 H7B O12 0.97 2.53 3.052(8) 113.4 1_545
N1 H1A O2 0.89 2.09 2.941(7) 159.5 2_465
N1 H1B O7 0.89 2.20 3.023(6) 152.7 .
N1 H1B O8 0.89 2.34 3.132(7) 148.8 .
N1 H1C O10 0.89 1.99 2.850(7) 163.2 2_565
C9 H9B O9 0.97 2.51 3.199(8) 128.3 2_565

_refine_diff_density_max         0.224
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.056

####################################################################### 
# 
# 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_pn
_database_code_depnum_ccdc_archive 'CCDC 1495524'
_audit_update_record             
;
2016-07-22 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H22 Cr N2 Na O12'
_chemical_formula_weight         437.29

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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   Pn

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



_cell_measurement_temperature    297(2)
_cell_length_a                   8.10474(9)
_cell_length_b                   9.26392(11)
_cell_length_c                   12.04593(14)
_cell_angle_alpha                90.0
_cell_angle_beta                 91.1766(10)
_cell_angle_gamma                90.0
_cell_volume                     904.237(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16883
_cell_measurement_theta_min      3.7020
_cell_measurement_theta_max      29.1900

_exptl_crystal_description       cuboid
_exptl_crystal_colour            'dark blue'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             478
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_min  0.94852
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      297(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            31008
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         29.91
_reflns_number_total             4694
_reflns_number_gt                4362
_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)+(0.0330P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.331(9)
_refine_ls_number_reflns         4694
_refine_ls_number_parameters     240
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0600
_refine_ls_wR_factor_gt          0.0576
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_restrained_S_all      1.177
_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
Cr1 Cr 0.68078(2) 0.27150(2) 0.462766(17) 0.02135(6) Uani 1 1 d . . .
Na Na 1.18412(11) 0.77082(6) 0.46207(7) 0.02840(11) Uani 1 1 d . . .
O1 O 0.56111(14) 0.29186(12) 0.60367(10) 0.0301(2) Uani 1 1 d . . .
O2 O 0.54371(16) 0.28134(14) 0.78602(10) 0.0369(3) Uani 1 1 d . . .
O3 O 0.48464(12) 0.17428(12) 0.39617(9) 0.0303(2) Uani 1 1 d . . .
O4 O 0.82412(16) 0.21322(16) 0.14272(11) 0.0399(3) Uani 1 1 d . . .
O5 O 0.77010(12) 0.08496(11) 0.51796(9) 0.0280(2) Uani 1 1 d . . .
O6 O 0.28915(14) 0.00645(13) 0.38656(10) 0.0392(3) Uani 1 1 d . . .
O7 O 0.59503(12) 0.45767(12) 0.40646(9) 0.0301(2) Uani 1 1 d . . .
O8 O 0.42561(16) 0.64446(14) 0.39966(11) 0.0466(3) Uani 1 1 d . . .
O9 O 0.87642(13) 0.37022(11) 0.52885(9) 0.0305(2) Uani 1 1 d . . .
O10 O 1.07412(14) 0.53599(12) 0.53704(10) 0.0383(3) Uani 1 1 d . . .
O11 O 0.80206(15) 0.24715(12) 0.32371(10) 0.0290(3) Uani 1 1 d . . .
O12 O 0.96001(16) -0.08585(15) 0.52533(12) 0.0505(3) Uani 1 1 d . . .
C1 C 0.9500(2) 0.48007(18) 0.49292(14) 0.0314(3) Uani 1 1 d . . .
H1 H 0.9080 0.5225 0.4283 0.038 Uiso 1 1 calc R . .
C2 C 0.9086(2) 0.02935(18) 0.49064(14) 0.0325(4) Uani 1 1 d . . .
H2 H 0.9735 0.0802 0.4413 0.039 Uiso 1 1 calc R . .
C3 C 0.40843(19) 0.0662(2) 0.43253(14) 0.0328(4) Uani 1 1 d . . .
H3 H 0.4452 0.0281 0.5000 0.039 Uiso 1 1 calc R . .
C4 C 0.4702(2) 0.52900(19) 0.43829(14) 0.0355(4) Uani 1 1 d . . .
H4 H 0.4085 0.4900 0.4952 0.043 Uiso 1 1 calc R . .
C5 C 0.6197(2) 0.26665(18) 0.69999(16) 0.0292(4) Uani 1 1 d . . .
H5 H 0.7283 0.2347 0.7058 0.035 Uiso 1 1 calc R . .
C6 C 0.7459(2) 0.24717(19) 0.22505(17) 0.0306(4) Uani 1 1 d . . .
H6 H 0.6366 0.2751 0.2139 0.037 Uiso 1 1 calc R . .
N2 N 0.66137(19) 0.86828(17) 0.68480(13) 0.0403(4) Uani 1 1 d . . .
H2A H 0.5520 0.8603 0.6806 0.060 Uiso 1 1 calc R . .
H2B H 0.6951 0.9294 0.6330 0.060 Uiso 1 1 calc R . .
H2C H 0.6914 0.9012 0.7516 0.060 Uiso 1 1 calc R . .
C7 C 0.7367(3) 0.7259(3) 0.6669(2) 0.0570(6) Uani 1 1 d . . .
H7A H 0.8558 0.7356 0.6671 0.068 Uiso 1 1 calc R . .
H7B H 0.7015 0.6890 0.5949 0.068 Uiso 1 1 calc R . .
C8 C 0.6891(3) 0.6231(3) 0.7541(3) 0.0705(7) Uani 1 1 d . . .
H8A H 0.5745 0.5989 0.7448 0.106 Uiso 1 1 calc R . .
H8B H 0.7073 0.6663 0.8257 0.106 Uiso 1 1 calc R . .
H8C H 0.7545 0.5371 0.7486 0.106 Uiso 1 1 calc R . .
N1 N 0.7050(2) 0.63554(17) 0.21559(13) 0.0414(4) Uani 1 1 d . . .
H1A H 0.8142 0.6370 0.2248 0.062 Uiso 1 1 calc R . .
H1B H 0.6776 0.5740 0.1615 0.062 Uiso 1 1 calc R . .
H1C H 0.6587 0.6076 0.2784 0.062 Uiso 1 1 calc R . .
C10 C 0.6831(4) 0.8867(3) 0.2722(3) 0.0897(10) Uani 1 1 d . . .
H10A H 0.6613 0.8452 0.3434 0.135 Uiso 1 1 calc R . .
H10B H 0.6154 0.9707 0.2611 0.135 Uiso 1 1 calc R . .
H10C H 0.7973 0.9136 0.2692 0.135 Uiso 1 1 calc R . .
C9 C 0.6459(3) 0.7817(2) 0.1857(2) 0.0603(6) Uani 1 1 d . . .
H9A H 0.6971 0.8119 0.1174 0.072 Uiso 1 1 calc R . .
H9B H 0.5275 0.7787 0.1723 0.072 Uiso 1 1 calc R . .


_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 O11 1.9724(12) . ?
Cr1 O7 1.9744(10) . ?
Cr1 O5 1.9830(10) . ?
Cr1 O9 1.9831(10) . ?
Cr1 O1 1.9811(12) . ?
Cr1 O3 1.9823(10) . ?
Na O12 2.3874(16) 1_565 ?
Na O8 2.4139(15) 1_655 ?
Na O2 2.4345(16) 2_564 ?
Na O4 2.4378(16) 2_565 ?
Na O6 2.5195(13) 1_665 ?
Na O10 2.5251(12) . ?
O1 C5 1.266(2) . ?
O2 C5 1.224(2) . ?
O2 Na 2.4345(16) 2_465 ?
O3 C3 1.259(2) . ?
O4 C6 1.229(2) . ?
O4 Na 2.4378(16) 2_464 ?
O5 C2 1.2839(19) . ?
O6 C3 1.235(2) . ?
O6 Na 2.5195(13) 1_445 ?
O7 C4 1.274(2) . ?
O8 C4 1.218(2) . ?
O8 Na 2.4139(15) 1_455 ?
O9 C1 1.2606(19) . ?
O10 C1 1.2413(19) . ?
O11 C6 1.264(2) . ?
O12 C2 1.217(2) . ?
O12 Na 2.3874(16) 1_545 ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
N2 C7 1.471(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C7 C8 1.476(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 C9 1.478(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C10 C9 1.453(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?

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
O11 Cr1 O7 89.21(5) . . ?
O11 Cr1 O5 90.01(4) . . ?
O7 Cr1 O5 179.10(5) . . ?
O11 Cr1 O9 89.16(5) . . ?
O7 Cr1 O9 90.46(4) . . ?
O5 Cr1 O9 89.08(4) . . ?
O11 Cr1 O1 178.72(5) . . ?
O7 Cr1 O1 92.07(4) . . ?
O5 Cr1 O1 88.71(5) . . ?
O9 Cr1 O1 90.78(5) . . ?
O11 Cr1 O3 90.80(5) . . ?
O7 Cr1 O3 89.09(5) . . ?
O5 Cr1 O3 91.37(4) . . ?
O9 Cr1 O3 179.55(5) . . ?
O1 Cr1 O3 89.27(5) . . ?
O12 Na O8 175.00(6) 1_565 1_655 ?
O12 Na O2 92.49(6) 1_565 2_564 ?
O8 Na O2 90.00(5) 1_655 2_564 ?
O12 Na O4 91.41(6) 1_565 2_565 ?
O8 Na O4 86.67(6) 1_655 2_565 ?
O2 Na O4 172.00(6) 2_564 2_565 ?
O12 Na O6 84.16(5) 1_565 1_665 ?
O8 Na O6 91.47(5) 1_655 1_665 ?
O2 Na O6 90.74(5) 2_564 1_665 ?
O4 Na O6 96.62(5) 2_565 1_665 ?
O12 Na O10 95.08(6) 1_565 . ?
O8 Na O10 89.32(5) 1_655 . ?
O2 Na O10 88.76(5) 2_564 . ?
O4 Na O10 83.93(5) 2_565 . ?
O6 Na O10 179.07(6) 1_665 . ?
C5 O1 Cr1 125.91(11) . . ?
C5 O2 Na 118.77(12) . 2_465 ?
C3 O3 Cr1 127.97(10) . . ?
C6 O4 Na 117.80(12) . 2_464 ?
C2 O5 Cr1 125.36(10) . . ?
C3 O6 Na 119.58(10) . 1_445 ?
C4 O7 Cr1 128.73(11) . . ?
C4 O8 Na 122.87(12) . 1_455 ?
C1 O9 Cr1 127.91(10) . . ?
C1 O10 Na 119.70(10) . . ?
C6 O11 Cr1 128.48(12) . . ?
C2 O12 Na 129.48(12) . 1_545 ?
O10 C1 O9 125.08(14) . . ?
O10 C1 H1 117.5 . . ?
O9 C1 H1 117.5 . . ?
O12 C2 O5 124.00(16) . . ?
O12 C2 H2 118.0 . . ?
O5 C2 H2 118.0 . . ?
O6 C3 O3 125.82(15) . . ?
O6 C3 H3 117.1 . . ?
O3 C3 H3 117.1 . . ?
O8 C4 O7 124.84(16) . . ?
O8 C4 H4 117.6 . . ?
O7 C4 H4 117.6 . . ?
O2 C5 O1 124.72(17) . . ?
O2 C5 H5 117.6 . . ?
O1 C5 H5 117.6 . . ?
O4 C6 O11 125.22(17) . . ?
O4 C6 H6 117.4 . . ?
O11 C6 H6 117.4 . . ?
C7 N2 H2A 109.5 . . ?
C7 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C7 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N2 C7 C8 111.0(2) . . ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 N1 H1A 109.5 . . ?
C9 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C9 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C10 C9 N1 112.1(2) . . ?
C10 C9 H9A 109.2 . . ?
N1 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
N1 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?

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
N2 H2C O6 0.89 1.99 2.8675(19) 169.9 2_565
N2 H2B O5 0.89 2.10 2.9863(19) 176.2 1_565
N2 H2B O12 0.89 2.53 3.150(2) 126.8 1_565
N2 H2A O4 0.89 2.01 2.8708(19) 161.7 2_465
N1 H1C O7 0.89 2.15 2.9799(18) 155.6 .
N1 H1C O8 0.89 2.44 3.202(2) 144.6 .
N1 H1B O10 0.89 1.98 2.8604(19) 167.6 2_464
N1 H1A O2 0.89 2.13 2.959(2) 155.4 2_564
N1 H1A O1 0.89 2.59 3.2805(19) 135.5 2_564

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.045
####################################################################### 
# 
# 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_400K
_database_code_depnum_ccdc_archive 'CCDC 1495525'
_audit_update_record             
;
2016-07-22 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H22 Cr N2 Na O12'
_chemical_formula_weight         437.28

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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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

_cell_length_a                   8.1066(6)
_cell_length_b                   9.3455(11)
_cell_length_c                   12.1283(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.062(8)
_cell_angle_gamma                90
_cell_volume                     918.68(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    1940
_cell_measurement_theta_min      2.8180
_cell_measurement_theta_max      27.3610

_exptl_crystal_description       cuboid
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             454
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_min  0.97633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Sapphire1, long nozzle'
_diffrn_detector_area_resol_mean 8.4350
_diffrn_reflns_number            6993
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.752
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.681
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1732
_reflns_number_gt                1307
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+0.2200P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1732
_refine_ls_number_parameters     149
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1039
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001

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
Cr1 Cr 0.0000 0.0000 0.5000 0.0334(2) Uani 1 2 d S . P . .
Na1 Na 0.0000 0.0000 0.0000 0.0420(4) Uani 1 2 d S . P . .
O1 O 0.1183(2) 0.0234(2) 0.36009(15) 0.0425(5) Uani 1 1 d . . . . .
O2 O 0.1963(2) -0.0972(2) 0.56465(16) 0.0452(5) Uani 1 1 d . . . . .
O3 O 0.0876(2) 0.1848(2) 0.55538(16) 0.0433(5) Uani 1 1 d . . . . .
O4 O 0.1376(2) 0.0344(2) 0.17864(17) 0.0525(6) Uani 1 1 d . . . . .
O5 O 0.3896(2) -0.2648(2) 0.57577(18) 0.0590(6) Uani 1 1 d . . . . .
O6 O 0.2639(3) 0.3642(3) 0.5598(2) 0.0770(8) Uani 1 1 d . . . . .
C1 C 0.0615(3) 0.0098(3) 0.2625(2) 0.0411(7) Uani 1 1 d . . . . .
H1 H -0.0469 -0.0215 0.2542 0.049 Uiso 1 1 calc R U . . .
C2 C 0.2184(4) 0.2492(4) 0.5253(3) 0.0547(9) Uani 1 1 d . . . . .
H2 H 0.2831 0.2043 0.4730 0.066 Uiso 1 1 calc R U . . .
C3 C 0.2692(3) -0.2073(4) 0.5317(3) 0.0522(8) Uani 1 1 d . . . . .
H3 H 0.2278 -0.2496 0.4675 0.063 Uiso 1 1 calc R U . . .
C4 C 0.5315(12) -0.0282(8) 0.2838(8) 0.067(3) Uani 0.432(9) 1 d D U P A 1
H4A H 0.4703 -0.0553 0.3486 0.080 Uiso 0.432(9) 1 calc R U P A 1
H4B H 0.6478 -0.0250 0.3041 0.080 Uiso 0.432(9) 1 calc R U P A 1
C5 C 0.5037(16) -0.1368(10) 0.1944(10) 0.102(5) Uani 0.432(9) 1 d D U P A 1
H5A H 0.4758 -0.2272 0.2267 0.153 Uiso 0.432(9) 1 calc R U P A 1
H5B H 0.6025 -0.1470 0.1526 0.153 Uiso 0.432(9) 1 calc R U P A 1
H5C H 0.4152 -0.1057 0.1465 0.153 Uiso 0.432(9) 1 calc R U P A 1
N2 N 0.477(4) 0.1127(10) 0.2457(13) 0.056(5) Uani 0.432(9) 1 d D U P A 1
H2A H 0.3678 0.1147 0.2410 0.085 Uiso 0.432(9) 1 calc R U P A 1
H2B H 0.5191 0.1300 0.1796 0.085 Uiso 0.432(9) 1 calc R U P A 1
H2C H 0.5126 0.1791 0.2932 0.085 Uiso 0.432(9) 1 calc R U P A 1
C6 C 0.5499(10) -0.0230(7) 0.2044(7) 0.078(3) Uani 0.568(9) 1 d D U P A 2
H6A H 0.6693 -0.0166 0.2034 0.094 Uiso 0.568(9) 1 calc R U P A 2
H6B H 0.5116 -0.0570 0.1328 0.094 Uiso 0.568(9) 1 calc R U P A 2
C7 C 0.4991(10) -0.1263(8) 0.2921(8) 0.098(3) Uani 0.568(9) 1 d D U P A 2
H7A H 0.4093 -0.0866 0.3324 0.146 Uiso 0.568(9) 1 calc R U P A 2
H7B H 0.5908 -0.1438 0.3415 0.146 Uiso 0.568(9) 1 calc R U P A 2
H7C H 0.4649 -0.2147 0.2584 0.146 Uiso 0.568(9) 1 calc R U P A 2
N1 N 0.480(3) 0.1181(8) 0.2258(11) 0.058(4) Uani 0.568(9) 1 d D U P A 2
H1A H 0.3705 0.1120 0.2263 0.087 Uiso 0.568(9) 1 calc R U P A 2
H1B H 0.5102 0.1785 0.1731 0.087 Uiso 0.568(9) 1 calc R U P A 2
H1C H 0.5169 0.1498 0.2909 0.087 Uiso 0.568(9) 1 calc R U P A 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
Cr1 O1 1.9766(18) . ?
Cr1 O1 1.9767(18) 3_556 ?
Cr1 O3 1.9805(19) . ?
Cr1 O3 1.9805(19) 3_556 ?
Cr1 O2 1.9818(18) . ?
Cr1 O2 1.9818(18) 3_556 ?
Na1 O6 2.419(2) 4_565 ?
Na1 O6 2.419(2) 2_545 ?
Na1 O4 2.439(2) . ?
Na1 O4 2.439(2) 3 ?
Na1 O5 2.551(2) 2 ?
Na1 O5 2.551(2) 4 ?
O1 C1 1.268(3) . ?
O2 C3 1.256(4) . ?
O3 C2 1.278(3) . ?
O4 C1 1.221(3) . ?
O5 C3 1.228(3) . ?
O5 Na1 2.551(2) 2_545 ?
O6 C2 1.209(4) . ?
O6 Na1 2.419(2) 2 ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 N2 1.4601(11) . ?
C4 C5 1.4995(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C6 N1 1.4602(11) . ?
C6 C7 1.4993(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?

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 Cr1 O1 180.0 . 3_556 ?
O1 Cr1 O3 91.02(8) . . ?
O1 Cr1 O3 88.98(8) 3_556 . ?
O1 Cr1 O3 88.98(8) . 3_556 ?
O1 Cr1 O3 91.02(8) 3_556 3_556 ?
O3 Cr1 O3 180.0 . 3_556 ?
O1 Cr1 O2 89.52(8) . . ?
O1 Cr1 O2 90.48(8) 3_556 . ?
O3 Cr1 O2 89.15(8) . . ?
O3 Cr1 O2 90.85(8) 3_556 . ?
O1 Cr1 O2 90.48(8) . 3_556 ?
O1 Cr1 O2 89.52(8) 3_556 3_556 ?
O3 Cr1 O2 90.85(8) . 3_556 ?
O3 Cr1 O2 89.15(8) 3_556 3_556 ?
O2 Cr1 O2 180.00(6) . 3_556 ?
O6 Na1 O6 180.00(13) 4_565 2_545 ?
O6 Na1 O4 90.92(8) 4_565 . ?
O6 Na1 O4 89.08(8) 2_545 . ?
O6 Na1 O4 89.08(8) 4_565 3 ?
O6 Na1 O4 90.92(8) 2_545 3 ?
O4 Na1 O4 180.0 . 3 ?
O6 Na1 O5 86.61(8) 4_565 2 ?
O6 Na1 O5 93.39(8) 2_545 2 ?
O4 Na1 O5 92.80(7) . 2 ?
O4 Na1 O5 87.20(7) 3 2 ?
O6 Na1 O5 93.39(8) 4_565 4 ?
O6 Na1 O5 86.61(8) 2_545 4 ?
O4 Na1 O5 87.20(7) . 4 ?
O4 Na1 O5 92.80(7) 3 4 ?
O5 Na1 O5 180.00(10) 2 4 ?
C1 O1 Cr1 128.07(17) . . ?
C3 O2 Cr1 128.95(19) . . ?
C2 O3 Cr1 127.4(2) . . ?
C1 O4 Na1 119.06(18) . . ?
C3 O5 Na1 120.1(2) . 2_545 ?
C2 O6 Na1 126.9(2) . 2 ?
O4 C1 O1 125.3(3) . . ?
O4 C1 H1 117.3 . . ?
O1 C1 H1 117.3 . . ?
O6 C2 O3 124.7(3) . . ?
O6 C2 H2 117.7 . . ?
O3 C2 H2 117.7 . . ?
O5 C3 O2 126.5(3) . . ?
O5 C3 H3 116.8 . . ?
O2 C3 H3 116.8 . . ?
N2 C4 C5 109.9(4) . . ?
N2 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
N2 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N1 C6 C7 110.1(3) . . ?
N1 C6 H6A 109.6 . . ?
C7 C6 H6A 109.6 . . ?
N1 C6 H6B 109.6 . . ?
C7 C6 H6B 109.6 . . ?
H6A C6 H6B 108.2 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 N1 H1A 109.5 . . ?
C6 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C6 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?

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

C4 H4B O2 0.97 2.32 3.077(8) 134.8 3_656
N2 H2A O4 0.89 2.14 2.95(3) 151.6 .
N2 H2B O3 0.89 2.37 3.128(17) 143.5 4_665
N2 H2B O6 0.89 2.48 3.27(2) 148.4 4_665
N2 H2C O5 0.89 1.94 2.79(2) 160.2 3_656
N1 H1A O4 0.89 2.09 2.93(3) 156.2 .
N1 H1B O3 0.89 2.02 2.914(13) 177.9 4_665
N1 H1B O6 0.89 2.53 3.090(19) 121.8 4_665
N1 H1C O5 0.89 2.07 2.949(17) 167.5 3_656

_refine_diff_density_max         0.253
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.052

