# Electronic Supplementary Material (ESI) for ChemComm.
# 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_E465
_database_code_depnum_ccdc_archive 'CCDC 1042529'
_audit_update_record             
;
2015-01-08 deposited with the CCDC.
2015-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        Na-Cr-OA
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H6 Fe Na3 O17'
_chemical_formula_weight         474.93

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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.4212(9)
_cell_length_b                   12.5545(7)
_cell_length_c                   14.9217(8)
_cell_angle_alpha                90
_cell_angle_beta                 101.047(2)
_cell_angle_gamma                90
_cell_volume                     3203.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9844
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      43.10

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_F_000             1896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.115
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6062
_exptl_absorpt_correction_T_max  0.7485
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21361
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.313
_diffrn_reflns_theta_max         28.276
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3978
_reflns_number_gt                3862
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0695P)²+4.9988P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3978
_refine_ls_number_parameters     277
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1144
_refine_ls_wR_factor_gt          0.1137
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.216
_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
O15 O 0.82317(12) 0.45329(17) 0.49624(13) 0.0239(4) Uani 0.801(4) 1 d D . P A 1
O15A O 0.7889(5) 0.5015(7) 0.4732(5) 0.0239(4) Uani 0.199(4) 1 d D . P A 2
Fe1 Fe 0.80589(2) 0.86501(2) 0.26289(2) 0.01162(11) Uani 1 1 d . . . . .
Na1 Na 0.86757(6) 0.63102(7) 0.47805(7) 0.0279(2) Uani 1 1 d D . . . .
Na2 Na 0.95603(5) 0.88858(7) 0.50007(6) 0.02030(18) Uani 1 1 d . . . . .
Na3 Na 1.0000 1.22653(8) 0.2500 0.0139(2) Uani 1 2 d S T P . .
Na4 Na 1.0000 1.49404(9) 0.2500 0.0163(2) Uani 1 2 d S T P . .
O1 O 0.89714(8) 0.93746(11) 0.34259(9) 0.0158(3) Uani 1 1 d . . . . .
O2 O 0.80412(8) 1.00202(11) 0.19471(9) 0.0151(3) Uani 1 1 d . . . . .
O3 O 0.96877(8) 1.08691(11) 0.34936(9) 0.0165(3) Uani 1 1 d . . . . .
O4 O 0.86936(8) 1.15510(11) 0.19380(9) 0.0155(3) Uani 1 1 d . . . . .
O5 O 0.73171(8) 0.89159(12) 0.34763(9) 0.0162(3) Uani 1 1 d . . . . .
O6 O 0.70339(8) 0.83204(11) 0.17671(9) 0.0153(3) Uani 1 1 d . . . . .
O7 O 0.60381(8) 0.89035(12) 0.35337(10) 0.0166(3) Uani 1 1 d . . . . .
O8 O 0.57393(8) 0.84022(11) 0.17018(9) 0.0148(3) Uani 1 1 d . . . . .
O9 O 0.86631(8) 0.79674(11) 0.17415(9) 0.0168(3) Uani 1 1 d . . . . .
O10 O 0.83191(8) 0.72478(11) 0.32476(9) 0.0154(3) Uani 1 1 d . . . . .
O11 O 0.93125(9) 0.64732(12) 0.15253(11) 0.0206(3) Uani 1 1 d . . . . .
O12 O 0.89616(8) 0.57293(11) 0.31582(10) 0.0178(3) Uani 1 1 d . . . . .
O13 O 0.83343(10) 0.80762(14) 0.51168(10) 0.0241(3) Uani 1 1 d D . . . .
H13X H 0.7934(17) 0.836(3) 0.476(2) 0.056(11) Uiso 1 1 d D . . . .
H13Y H 0.830(2) 0.826(3) 0.5669(15) 0.039(9) Uiso 1 1 d D . . . .
O14 O 0.99394(10) 0.70374(14) 0.49325(11) 0.0261(3) Uani 1 1 d D . . . .
H14X H 1.0265(18) 0.693(3) 0.456(2) 0.047(10) Uiso 1 1 d D . . . .
H14Y H 1.0311(18) 0.695(3) 0.540(2) 0.055(11) Uiso 1 1 d D . . . .
O16 O 1.08127(9) 0.93371(13) 0.46709(11) 0.0237(3) Uani 1 1 d D . . . .
H16X H 1.1219(15) 0.915(3) 0.5072(19) 0.040(9) Uiso 1 1 d D . . . .
H16Y H 1.091(2) 0.906(3) 0.4174(17) 0.044(9) Uiso 1 1 d D . . . .
C1 C 0.91405(10) 1.02997(15) 0.31440(12) 0.0128(3) Uani 1 1 d . . . . .
C2 C 0.85803(10) 1.06805(15) 0.22648(12) 0.0128(3) Uani 1 1 d . . . . .
C3 C 0.65868(11) 0.87988(14) 0.31323(13) 0.0128(3) Uani 1 1 d . . . . .
C4 C 0.64193(10) 0.84810(14) 0.21064(12) 0.0121(3) Uani 1 1 d . . . . .
C5 C 0.89280(10) 0.70300(15) 0.19574(13) 0.0145(3) Uani 1 1 d . . . . .
C6 C 0.87273(10) 0.65991(15) 0.28630(13) 0.0141(3) Uani 1 1 d . . . . .
O1W O 0.70810(12) 0.62184(16) 0.10017(15) 0.0273(4) Uani 0.832(4) 1 d . . P B 1
O2W O 0.7184(6) 0.6749(8) 0.0552(7) 0.0273(4) Uani 0.168(4) 1 d . . P B 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
O15 Na1 2.394(2) . ?
O15A Na1 2.118(7) . ?
Fe1 O2 1.9956(14) . ?
Fe1 O10 1.9992(14) . ?
Fe1 O5 2.0017(14) . ?
Fe1 O1 2.0111(13) . ?
Fe1 O9 2.0321(14) . ?
Fe1 O6 2.0331(13) . ?
Na1 O14 2.354(2) . ?
Na1 O13 2.374(2) . ?
Na1 O7 2.4835(17) 7_666 ?
Na1 O10 2.5414(17) . ?
Na1 O12 2.6650(17) . ?
Na1 C6 2.903(2) . ?
Na1 Na2 3.5700(13) . ?
Na2 O3 2.3940(16) 5_776 ?
Na2 O16 2.3947(18) . ?
Na2 O16 2.4004(19) 5_776 ?
Na2 O13 2.4014(19) . ?
Na2 O14 2.4201(19) . ?
Na2 O1 2.4550(16) . ?
Na2 Na2 3.1898(18) 5_776 ?
Na2 Na3 3.9356(9) 5_776 ?
Na3 O8 2.3879(15) 4_655 ?
Na3 O8 2.3879(15) 3 ?
Na3 O3 2.4240(16) . ?
Na3 O3 2.4241(16) 2_755 ?
Na3 O4 2.4404(14) 2_755 ?
Na3 O4 2.4405(14) . ?
Na3 O7 2.9682(16) 3 ?
Na3 O7 2.9682(16) 4_655 ?
Na3 C4 3.0569(19) 3 ?
Na3 C4 3.0569(19) 4_655 ?
Na3 Na4 3.3584(16) . ?
Na3 Na2 3.9356(9) 6_575 ?
Na4 O12 2.4288(15) 2_765 ?
Na4 O12 2.4288(15) 1_565 ?
Na4 O7 2.5050(15) 4_655 ?
Na4 O7 2.5050(15) 3 ?
Na4 O11 2.5663(17) 2_765 ?
Na4 O11 2.5663(17) 1_565 ?
Na4 O8 2.7193(16) 4_655 ?
Na4 O8 2.7193(16) 3 ?
Na4 C3 3.0963(19) 4_655 ?
Na4 C3 3.0963(19) 3 ?
O1 C1 1.288(2) . ?
O2 C2 1.274(2) . ?
O3 C1 1.225(2) . ?
O3 Na2 2.3940(16) 5_776 ?
O4 C2 1.228(2) . ?
O5 C3 1.286(2) . ?
O6 C4 1.285(2) . ?
O7 C3 1.229(2) . ?
O7 Na1 2.4835(17) 7_666 ?
O7 Na4 2.5051(15) 3_445 ?
O7 Na3 2.9682(16) 3_445 ?
O8 C4 1.226(2) . ?
O8 Na3 2.3880(15) 3_445 ?
O8 Na4 2.7193(16) 3_445 ?
O9 C5 1.282(2) . ?
O10 C6 1.286(2) . ?
O11 C5 1.232(2) . ?
O11 Na4 2.5662(17) 1_545 ?
O12 C6 1.218(2) . ?
O12 Na4 2.4288(15) 1_545 ?
O13 H13X 0.866(19) . ?
O13 H13Y 0.870(18) . ?
O14 H14X 0.875(18) . ?
O14 H14Y 0.867(19) . ?
O16 Na2 2.4005(19) 5_776 ?
O16 H16X 0.867(18) . ?
O16 H16Y 0.860(18) . ?
C1 C2 1.553(2) . ?
C3 C4 1.554(3) . ?
C3 Na4 3.0963(19) 3_445 ?
C4 Na3 3.0569(18) 3_445 ?
C5 C6 1.556(3) . ?

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 Fe1 O10 167.02(6) . . ?
O2 Fe1 O5 103.27(6) . . ?
O10 Fe1 O5 88.38(6) . . ?
O2 Fe1 O1 81.08(5) . . ?
O10 Fe1 O1 92.38(6) . . ?
O5 Fe1 O1 94.81(6) . . ?
O2 Fe1 O9 89.47(6) . . ?
O10 Fe1 O9 80.19(5) . . ?
O5 Fe1 O9 163.66(6) . . ?
O1 Fe1 O9 97.28(6) . . ?
O2 Fe1 O6 85.82(6) . . ?
O10 Fe1 O6 101.93(6) . . ?
O5 Fe1 O6 80.70(5) . . ?
O1 Fe1 O6 164.81(6) . . ?
O9 Fe1 O6 90.22(6) . . ?
O15A Na1 O14 152.6(3) . . ?
O15A Na1 O13 122.5(3) . . ?
O14 Na1 O13 83.39(6) . . ?
O14 Na1 O15 131.85(8) . . ?
O13 Na1 O15 138.34(8) . . ?
O15A Na1 O7 87.4(2) . 7_666 ?
O14 Na1 O7 86.66(6) . 7_666 ?
O13 Na1 O7 84.07(6) . 7_666 ?
O15 Na1 O7 77.94(6) . 7_666 ?
O15A Na1 O10 106.3(2) . . ?
O14 Na1 O10 88.27(6) . . ?
O13 Na1 O10 74.32(5) . . ?
O15 Na1 O10 120.34(7) . . ?
O7 Na1 O10 158.23(6) 7_666 . ?
O15A Na1 O12 89.5(2) . . ?
O14 Na1 O12 81.92(6) . . ?
O13 Na1 O12 123.06(6) . . ?
O15 Na1 O12 88.20(6) . . ?
O7 Na1 O12 148.68(6) 7_666 . ?
O10 Na1 O12 50.60(5) . . ?
O15A Na1 C6 101.8(2) . . ?
O14 Na1 C6 80.88(6) . . ?
O13 Na1 C6 98.51(6) . . ?
O15 Na1 C6 107.45(7) . . ?
O7 Na1 C6 166.87(7) 7_666 . ?
O10 Na1 C6 26.28(5) . . ?
O12 Na1 C6 24.81(5) . . ?
O15A Na1 Na2 164.4(2) . . ?
O14 Na1 Na2 42.31(5) . . ?
O13 Na1 Na2 41.91(5) . . ?
O15 Na1 Na2 167.67(6) . . ?
O7 Na1 Na2 90.30(5) 7_666 . ?
O10 Na1 Na2 71.95(4) . . ?
O12 Na1 Na2 100.31(4) . . ?
C6 Na1 Na2 83.29(5) . . ?
O3 Na2 O16 78.82(6) 5_776 . ?
O3 Na2 O16 79.04(6) 5_776 5_776 ?
O16 Na2 O16 96.60(6) . 5_776 ?
O3 Na2 O13 108.73(6) 5_776 . ?
O16 Na2 O13 166.63(7) . . ?
O16 Na2 O13 95.70(6) 5_776 . ?
O3 Na2 O14 93.33(6) 5_776 . ?
O16 Na2 O14 87.22(6) . . ?
O16 Na2 O14 170.58(7) 5_776 . ?
O13 Na2 O14 81.42(6) . . ?
O3 Na2 O1 156.83(6) 5_776 . ?
O16 Na2 O1 88.53(6) . . ?
O16 Na2 O1 83.29(6) 5_776 . ?
O13 Na2 O1 87.74(6) . . ?
O14 Na2 O1 105.47(6) . . ?
O3 Na2 Na2 73.22(5) 5_776 5_776 ?
O16 Na2 Na2 48.38(5) . 5_776 ?
O16 Na2 Na2 48.22(5) 5_776 5_776 ?
O13 Na2 Na2 143.63(6) . 5_776 ?
O14 Na2 Na2 134.91(6) . 5_776 ?
O1 Na2 Na2 83.85(5) . 5_776 ?
O3 Na2 Na1 110.60(5) 5_776 . ?
O16 Na2 Na1 126.13(5) . . ?
O16 Na2 Na1 137.03(5) 5_776 . ?
O13 Na2 Na1 41.32(5) . . ?
O14 Na2 Na1 40.90(5) . . ?
O1 Na2 Na1 92.55(4) . . ?
Na2 Na2 Na1 173.34(5) 5_776 . ?
O3 Na2 Na3 35.48(4) 5_776 5_776 ?
O16 Na2 Na3 105.19(5) . 5_776 ?
O16 Na2 Na3 99.15(5) 5_776 5_776 ?
O13 Na2 Na3 77.91(4) . 5_776 ?
O14 Na2 Na3 71.50(4) . 5_776 ?
O1 Na2 Na3 165.60(5) . 5_776 ?
Na2 Na2 Na3 108.44(4) 5_776 5_776 ?
Na1 Na2 Na3 75.93(3) . 5_776 ?
O8 Na3 O8 106.59(8) 4_655 3 ?
O8 Na3 O3 85.49(5) 4_655 . ?
O8 Na3 O3 160.56(5) 3 . ?
O8 Na3 O3 160.56(5) 4_655 2_755 ?
O8 Na3 O3 85.49(5) 3 2_755 ?
O3 Na3 O3 87.37(8) . 2_755 ?
O8 Na3 O4 127.22(5) 4_655 2_755 ?
O8 Na3 O4 80.47(5) 3 2_755 ?
O3 Na3 O4 80.09(5) . 2_755 ?
O3 Na3 O4 68.93(5) 2_755 2_755 ?
O8 Na3 O4 80.47(5) 4_655 . ?
O8 Na3 O4 127.22(5) 3 . ?
O3 Na3 O4 68.93(5) . . ?
O3 Na3 O4 80.09(5) 2_755 . ?
O4 Na3 O4 136.88(8) 2_755 . ?
O8 Na3 O7 70.11(5) 4_655 3 ?
O8 Na3 O7 60.79(5) 3 3 ?
O3 Na3 O7 111.66(4) . 3 ?
O3 Na3 O7 129.28(4) 2_755 3 ?
O4 Na3 O7 68.95(4) 2_755 3 ?
O4 Na3 O7 150.27(5) . 3 ?
O8 Na3 O7 60.79(5) 4_655 4_655 ?
O8 Na3 O7 70.11(5) 3 4_655 ?
O3 Na3 O7 129.28(4) . 4_655 ?
O3 Na3 O7 111.66(4) 2_755 4_655 ?
O4 Na3 O7 150.27(5) 2_755 4_655 ?
O4 Na3 O7 68.95(4) . 4_655 ?
O7 Na3 O7 92.28(6) 3 4_655 ?
O8 Na3 C4 109.32(6) 4_655 3 ?
O8 Na3 C4 21.93(5) 3 3 ?
O3 Na3 C4 139.75(5) . 3 ?
O3 Na3 C4 87.65(5) 2_755 3 ?
O4 Na3 C4 60.93(5) 2_755 3 ?
O4 Na3 C4 148.52(5) . 3 ?
O7 Na3 C4 47.09(4) 3 3 ?
O7 Na3 C4 89.36(5) 4_655 3 ?
O8 Na3 C4 21.93(5) 4_655 4_655 ?
O8 Na3 C4 109.32(6) 3 4_655 ?
O3 Na3 C4 87.65(5) . 4_655 ?
O3 Na3 C4 139.75(5) 2_755 4_655 ?
O4 Na3 C4 148.52(5) 2_755 4_655 ?
O4 Na3 C4 60.93(5) . 4_655 ?
O7 Na3 C4 89.36(5) 3 4_655 ?
O7 Na3 C4 47.09(4) 4_655 4_655 ?
C4 Na3 C4 120.09(8) 3 4_655 ?
O8 Na3 Na4 53.29(4) 4_655 . ?
O8 Na3 Na4 53.29(4) 3 . ?
O3 Na3 Na4 136.31(4) . . ?
O3 Na3 Na4 136.31(4) 2_755 . ?
O4 Na3 Na4 111.56(4) 2_755 . ?
O4 Na3 Na4 111.56(4) . . ?
O7 Na3 Na4 46.14(3) 3 . ?
O7 Na3 Na4 46.14(3) 4_655 . ?
C4 Na3 Na4 60.05(4) 3 . ?
C4 Na3 Na4 60.05(4) 4_655 . ?
O8 Na3 Na2 131.80(4) 4_655 6_575 ?
O8 Na3 Na2 76.85(4) 3 6_575 ?
O3 Na3 Na2 106.76(5) . 6_575 ?
O3 Na3 Na2 34.98(3) 2_755 6_575 ?
O4 Na3 Na2 100.95(4) 2_755 6_575 ?
O4 Na3 Na2 62.62(4) . 6_575 ?
O7 Na3 Na2 137.34(3) 3 6_575 ?
O7 Na3 Na2 76.90(3) 4_655 6_575 ?
C4 Na3 Na2 91.09(4) 3 6_575 ?
C4 Na3 Na2 110.35(4) 4_655 6_575 ?
Na4 Na3 Na2 111.543(19) . 6_575 ?
O12 Na4 O12 131.87(8) 2_765 1_565 ?
O12 Na4 O7 117.95(5) 2_765 4_655 ?
O12 Na4 O7 87.43(5) 1_565 4_655 ?
O12 Na4 O7 87.43(5) 2_765 3 ?
O12 Na4 O7 117.95(5) 1_565 3 ?
O7 Na4 O7 117.38(8) 4_655 3 ?
O12 Na4 O11 67.70(5) 2_765 2_765 ?
O12 Na4 O11 76.58(5) 1_565 2_765 ?
O7 Na4 O11 160.41(6) 4_655 2_765 ?
O7 Na4 O11 80.63(5) 3 2_765 ?
O12 Na4 O11 76.58(5) 2_765 1_565 ?
O12 Na4 O11 67.70(5) 1_565 1_565 ?
O7 Na4 O11 80.63(5) 4_655 1_565 ?
O7 Na4 O11 160.41(6) 3 1_565 ?
O11 Na4 O11 82.84(8) 2_765 1_565 ?
O12 Na4 O8 156.73(6) 2_765 4_655 ?
O12 Na4 O8 70.15(4) 1_565 4_655 ?
O7 Na4 O8 63.51(5) 4_655 4_655 ?
O7 Na4 O8 73.02(5) 3 4_655 ?
O11 Na4 O8 119.54(4) 2_765 4_655 ?
O11 Na4 O8 124.89(5) 1_565 4_655 ?
O12 Na4 O8 70.15(4) 2_765 3 ?
O12 Na4 O8 156.73(6) 1_565 3 ?
O7 Na4 O8 73.02(5) 4_655 3 ?
O7 Na4 O8 63.51(5) 3 3 ?
O11 Na4 O8 124.89(5) 2_765 3 ?
O11 Na4 O8 119.54(4) 1_565 3 ?
O8 Na4 O8 89.50(7) 4_655 3 ?
O12 Na4 C3 139.13(5) 2_765 4_655 ?
O12 Na4 C3 67.74(5) 1_565 4_655 ?
O7 Na4 C3 22.30(5) 4_655 4_655 ?
O7 Na4 C3 116.37(6) 3 4_655 ?
O11 Na4 C3 144.32(5) 2_765 4_655 ?
O11 Na4 C3 83.22(5) 1_565 4_655 ?
O8 Na4 C3 48.29(5) 4_655 4_655 ?
O8 Na4 C3 90.46(5) 3 4_655 ?
O12 Na4 C3 67.74(5) 2_765 3 ?
O12 Na4 C3 139.13(5) 1_565 3 ?
O7 Na4 C3 116.37(6) 4_655 3 ?
O7 Na4 C3 22.30(5) 3 3 ?
O11 Na4 C3 83.22(5) 2_765 3 ?
O11 Na4 C3 144.32(5) 1_565 3 ?
O8 Na4 C3 90.46(5) 4_655 3 ?
O8 Na4 C3 48.29(5) 3 3 ?
C3 Na4 C3 124.86(8) 4_655 3 ?
O12 Na4 Na3 114.07(4) 2_765 . ?
O12 Na4 Na3 114.07(4) 1_565 . ?
O7 Na4 Na3 58.69(4) 4_655 . ?
O7 Na4 Na3 58.69(4) 3 . ?
O11 Na4 Na3 138.58(4) 2_765 . ?
O11 Na4 Na3 138.58(4) 1_565 . ?
O8 Na4 Na3 44.75(3) 4_655 . ?
O8 Na4 Na3 44.75(3) 3 . ?
C3 Na4 Na3 62.43(4) 4_655 . ?
C3 Na4 Na3 62.43(4) 3 . ?
C1 O1 Fe1 114.76(11) . . ?
C1 O1 Na2 117.27(11) . . ?
Fe1 O1 Na2 126.23(7) . . ?
C2 O2 Fe1 115.64(12) . . ?
C1 O3 Na2 135.71(12) . 5_776 ?
C1 O3 Na3 114.14(12) . . ?
Na2 O3 Na3 109.54(6) 5_776 . ?
C2 O4 Na3 113.63(12) . . ?
C3 O5 Fe1 115.97(12) . . ?
C4 O6 Fe1 114.58(12) . . ?
C3 O7 Na1 117.28(12) . 7_666 ?
C3 O7 Na4 107.02(12) . 3_445 ?
Na1 O7 Na4 131.37(6) 7_666 3_445 ?
C3 O7 Na3 97.24(11) . 3_445 ?
Na1 O7 Na3 115.82(6) 7_666 3_445 ?
Na4 O7 Na3 75.17(5) 3_445 3_445 ?
C4 O8 Na3 111.42(12) . 3_445 ?
C4 O8 Na4 102.77(11) . 3_445 ?
Na3 O8 Na4 81.95(5) 3_445 3_445 ?
C5 O9 Fe1 115.45(12) . . ?
C6 O10 Fe1 116.57(12) . . ?
C6 O10 Na1 92.73(11) . . ?
Fe1 O10 Na1 144.91(7) . . ?
C5 O11 Na4 111.73(12) . 1_545 ?
C6 O12 Na4 116.31(12) . 1_545 ?
C6 O12 Na1 88.58(11) . . ?
Na4 O12 Na1 139.66(6) 1_545 . ?
Na1 O13 Na2 96.76(7) . . ?
Na1 O13 H13X 117(3) . . ?
Na2 O13 H13X 114(3) . . ?
Na1 O13 H13Y 121(3) . . ?
Na2 O13 H13Y 100(2) . . ?
H13X O13 H13Y 106(4) . . ?
Na1 O14 Na2 96.79(7) . . ?
Na1 O14 H14X 126(2) . . ?
Na2 O14 H14X 113(3) . . ?
Na1 O14 H14Y 125(3) . . ?
Na2 O14 H14Y 105(3) . . ?
H14X O14 H14Y 91(3) . . ?
Na2 O16 Na2 83.40(6) . 5_776 ?
Na2 O16 H16X 117(2) . . ?
Na2 O16 H16X 109(2) 5_776 . ?
Na2 O16 H16Y 114(2) . . ?
Na2 O16 H16Y 131(3) 5_776 . ?
H16X O16 H16Y 103(3) . . ?
O3 C1 O1 126.49(17) . . ?
O3 C1 C2 119.46(16) . . ?
O1 C1 C2 114.04(15) . . ?
O4 C2 O2 126.47(17) . . ?
O4 C2 C1 119.12(16) . . ?
O2 C2 C1 114.40(16) . . ?
O7 C3 O5 126.58(17) . . ?
O7 C3 C4 119.39(16) . . ?
O5 C3 C4 114.02(16) . . ?
O7 C3 Na4 50.68(10) . 3_445 ?
O5 C3 Na4 145.69(13) . 3_445 ?
C4 C3 Na4 80.24(10) . 3_445 ?
O8 C4 O6 126.34(17) . . ?
O8 C4 C3 119.14(16) . . ?
O6 C4 C3 114.52(15) . . ?
O8 C4 Na3 46.65(9) . 3_445 ?
O6 C4 Na3 139.73(12) . 3_445 ?
C3 C4 Na3 86.85(10) . 3_445 ?
O11 C5 O9 126.49(18) . . ?
O11 C5 C6 119.49(17) . . ?
O9 C5 C6 114.03(16) . . ?
O12 C6 O10 125.57(17) . . ?
O12 C6 C5 120.67(17) . . ?
O10 C6 C5 113.75(16) . . ?
O12 C6 Na1 66.61(10) . . ?
O10 C6 Na1 61.00(10) . . ?
C5 C6 Na1 162.53(12) . . ?

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
O13 H13X O15A 0.866(19) 2.69(4) 3.243(9) 123(3) 7_666
O13 H13X O5 0.866(19) 2.13(3) 2.929(2) 153(4) .
O14 H14X O11 0.875(18) 1.99(2) 2.832(2) 161(3) 2_755
O14 H14Y O8 0.867(19) 1.99(2) 2.794(2) 154(4) 8_566
O16 H16X O1W 0.867(18) 1.896(18) 2.762(3) 177(3) 8_566
O16 H16X O2W 0.867(18) 2.04(2) 2.844(10) 154(3) 8_566
O16 H16Y O9 0.860(18) 2.17(2) 2.995(2) 160(4) 2_755

_refine_diff_density_max         1.425
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.116

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_E501
_database_code_depnum_ccdc_archive 'CCDC 1042530'
_audit_update_record             
;
2015-01-08 deposited with the CCDC.
2015-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H10 Cr Na3 O17'
_chemical_formula_weight         475.11

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.2551(19)
_cell_length_b                   12.4639(14)
_cell_length_c                   15.1228(16)
_cell_angle_alpha                90
_cell_angle_beta                 100.454(2)
_cell_angle_gamma                90
_cell_volume                     3198.4(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5907
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      28.26

_exptl_crystal_description       Block
_exptl_crystal_colour            Dark_red
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_F_000             1912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.460
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    0.889
_shelx_estimated_absorpt_T_min   0.617
_shelx_estimated_absorpt_T_max   0.802
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6542
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11192
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.027
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3685
_reflns_number_gt                3375
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0337P)²+11.6786P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3685
_refine_ls_number_parameters     276
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0863
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.116
_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
Cr1 Cr 0.30879(2) 0.36383(3) 0.26874(2) 0.00640(9) Uani 1 1 d . . . . .
Na1 Na 0.0000 0.49714(10) 0.2500 0.0131(3) Uani 1 2 d S T P . .
Na2 Na 0.0000 0.22709(10) 0.2500 0.0105(2) Uani 1 2 d S T P . .
Na3 Na 0.37797(6) 0.13090(8) 0.48420(6) 0.0173(2) Uani 1 1 d . . . . .
Na4 Na 0.45823(5) 0.38685(7) 0.50089(6) 0.01258(19) Uani 1 1 d . . . . .
O1 O 0.21201(9) 0.31645(12) 0.18779(10) 0.0098(3) Uani 1 1 d . . . . .
O2 O 0.23332(9) 0.40327(13) 0.34678(10) 0.0107(3) Uani 1 1 d . . . . .
O3 O 0.08082(9) 0.33282(13) 0.17219(10) 0.0108(3) Uani 1 1 d . . . . .
O4 O 0.10434(9) 0.39381(13) 0.35059(11) 0.0126(3) Uani 1 1 d . . . . .
O5 O 0.33124(9) 0.22479(12) 0.32818(10) 0.0104(3) Uani 1 1 d . . . . .
O6 O 0.37544(9) 0.30690(12) 0.18673(10) 0.0101(3) Uani 1 1 d . . . . .
O7 O 0.39569(9) 0.07261(13) 0.31596(11) 0.0136(3) Uani 1 1 d . . . . .
O8 O 0.43667(10) 0.15507(13) 0.15999(11) 0.0152(3) Uani 1 1 d . . . . .
O9 O 0.39891(9) 0.43572(12) 0.34622(10) 0.0093(3) Uani 1 1 d . . . . .
O10 O 0.30048(9) 0.50250(12) 0.20645(10) 0.0097(3) Uani 1 1 d . . . . .
O11 O 0.47071(9) 0.58604(13) 0.35034(10) 0.0115(3) Uani 1 1 d . . . . .
O12 O 0.37135(9) 0.65040(12) 0.19504(10) 0.0103(3) Uani 1 1 d . . . . .
O13 O 0.33583(10) 0.30674(14) 0.51512(11) 0.0150(3) Uani 1 1 d D . . . .
H13X H 0.3300(16) 0.325(2) 0.5686(11) 0.018 Uiso 1 1 d D U . . .
H13Y H 0.2977(14) 0.338(2) 0.4786(15) 0.018 Uiso 1 1 d D U . . .
O14 O 0.50312(10) 0.20319(14) 0.49561(11) 0.0156(3) Uani 1 1 d D . . . .
H14X H 0.5371(15) 0.191(2) 0.5435(12) 0.019 Uiso 1 1 d D U . . .
H14Y H 0.5272(15) 0.190(2) 0.4506(13) 0.019 Uiso 1 1 d D U . . .
O15 O 0.29017(14) 0.0004(2) 0.46732(13) 0.0368(6) Uani 1 1 d D . . . .
H15X H 0.2687 0.0000 0.5045 0.044 Uiso 1 1 d D U . . .
H15Y H 0.2676(19) -0.008(3) 0.4124(10) 0.044 Uiso 1 1 d D U . . .
O16 O 0.58435(10) 0.43435(14) 0.46575(11) 0.0147(3) Uani 1 1 d D . . . .
H16X H 0.5896(16) 0.409(2) 0.4134(12) 0.018 Uiso 1 1 d D U . . .
H16Y H 0.6249(13) 0.412(2) 0.5026(14) 0.018 Uiso 1 1 d D U . . .
C1 C 0.14758(12) 0.34140(17) 0.21490(14) 0.0086(4) Uani 1 1 d . . . . .
C2 C 0.16085(13) 0.38374(17) 0.31272(14) 0.0090(4) Uani 1 1 d . . . . .
C3 C 0.37379(12) 0.16178(18) 0.28915(14) 0.0091(4) Uani 1 1 d . . . . .
C4 C 0.39828(12) 0.20934(18) 0.20351(14) 0.0093(4) Uani 1 1 d . . . . .
C5 C 0.41599(12) 0.52825(17) 0.31691(14) 0.0080(4) Uani 1 1 d . . . . .
C6 C 0.35887(12) 0.56617(17) 0.23132(14) 0.0083(4) Uani 1 1 d . . . . .
O1W O 0.27937(14) 0.62503(19) 0.40891(16) 0.0189(5) Uani 0.771(4) 1 d D . P A 1
H1W H 0.2829(18) 0.6840(15) 0.3833(19) 0.023 Uiso 1 1 d D U . B 1
H2W H 0.2590(17) 0.5777(18) 0.3707(17) 0.023 Uiso 1 1 d D U . C 1
O1X O 0.2868(4) 0.6932(6) 0.4647(5) 0.0189(5) Uani 0.229(4) 1 d . . 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 O5 1.9583(16) . ?
Cr1 O10 1.9611(16) . ?
Cr1 O6 1.9703(15) . ?
Cr1 O2 1.9717(16) . ?
Cr1 O1 1.9733(15) . ?
Cr1 O9 1.9830(15) . ?
Na1 O7 2.4022(17) 4 ?
Na1 O7 2.4022(17) 3_455 ?
Na1 O4 2.4940(17) 2 ?
Na1 O4 2.4940(17) . ?
Na1 O8 2.5262(19) 4 ?
Na1 O8 2.5262(19) 3_455 ?
Na1 O3 2.8495(18) 2 ?
Na1 C2 3.106(2) 2 ?
Na1 C3 3.126(2) 4 ?
Na1 C3 3.126(2) 3_455 ?
Na1 Na2 3.3659(18) . ?
Na2 O3 2.3794(17) 2 ?
Na2 O3 2.3794(17) . ?
Na2 O12 2.4213(16) 3_445 ?
Na2 O12 2.4213(16) 4_545 ?
Na2 O11 2.4345(18) 4_545 ?
Na2 O11 2.4345(18) 3_445 ?
Na2 O4 2.9799(18) 2 ?
Na2 C1 3.047(2) 2 ?
Na2 C6 3.128(2) 3_445 ?
Na2 C6 3.128(2) 4_545 ?
Na2 Na4 3.9678(11) 8_455 ?
Na3 O15 2.206(2) . ?
Na3 O14 2.317(2) . ?
Na3 O13 2.382(2) . ?
Na3 O4 2.4806(19) 7_556 ?
Na3 O5 2.6261(18) . ?
Na3 O7 2.7161(19) . ?
Na3 C3 2.963(2) . ?
Na3 Na4 3.4687(14) . ?
Na3 H15X 2.5535(10) . ?
Na4 O13 2.3809(19) . ?
Na4 O11 2.3829(18) 5_666 ?
Na4 O16 2.4060(19) . ?
Na4 O14 2.422(2) . ?
Na4 O16 2.4280(19) 5_666 ?
Na4 O9 2.4537(18) . ?
Na4 Na4 3.1700(18) 5_666 ?
Na4 Na2 3.9678(11) 7_556 ?
O1 C1 1.291(3) . ?
O2 C2 1.286(3) . ?
O3 C1 1.219(3) . ?
O4 C2 1.224(3) . ?
O4 Na3 2.4806(19) 7_556 ?
O5 C3 1.289(3) . ?
O6 C4 1.289(3) . ?
O7 C3 1.219(3) . ?
O7 Na1 2.4022(17) 3_545 ?
O8 C4 1.220(3) . ?
O8 Na1 2.5262(19) 3_545 ?
O9 C5 1.289(3) . ?
O10 C6 1.284(3) . ?
O11 C5 1.222(3) . ?
O11 Na4 2.3829(18) 5_666 ?
O11 Na2 2.4346(18) 3 ?
O12 C6 1.222(3) . ?
O12 Na2 2.4213(16) 3 ?
O13 H13X 0.862(16) . ?
O13 H13Y 0.870(16) . ?
O14 H14X 0.860(16) . ?
O14 H14Y 0.874(16) . ?
O15 H15X 0.727(2) . ?
O15 H15Y 0.858(16) . ?
O16 Na4 2.4280(19) 5_666 ?
O16 H16X 0.871(16) . ?
O16 H16Y 0.859(16) . ?
C1 C2 1.548(3) . ?
C3 C4 1.551(3) . ?
C3 Na1 3.126(2) 3_545 ?
C5 C6 1.551(3) . ?
C6 Na2 3.128(2) 3 ?
O1W H1W 0.838(17) . ?
O1W H2W 0.855(17) . ?

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
O5 Cr1 O10 172.53(6) . . ?
O5 Cr1 O6 83.15(6) . . ?
O10 Cr1 O6 90.87(6) . . ?
O5 Cr1 O2 92.46(7) . . ?
O10 Cr1 O2 93.96(7) . . ?
O6 Cr1 O2 172.25(7) . . ?
O5 Cr1 O1 95.42(7) . . ?
O10 Cr1 O1 89.19(6) . . ?
O6 Cr1 O1 91.53(6) . . ?
O2 Cr1 O1 82.50(6) . . ?
O5 Cr1 O9 93.44(6) . . ?
O10 Cr1 O9 82.35(6) . . ?
O6 Cr1 O9 92.86(6) . . ?
O2 Cr1 O9 93.78(6) . . ?
O1 Cr1 O9 170.52(7) . . ?
O7 Na1 O7 133.90(9) 4 3_455 ?
O7 Na1 O4 117.47(5) 4 2 ?
O7 Na1 O4 86.74(5) 3_455 2 ?
O7 Na1 O4 86.74(5) 4 . ?
O7 Na1 O4 117.47(5) 3_455 . ?
O4 Na1 O4 117.82(9) 2 . ?
O7 Na1 O8 68.61(6) 4 4 ?
O7 Na1 O8 75.79(6) 3_455 4 ?
O4 Na1 O8 157.64(7) 2 4 ?
O4 Na1 O8 83.10(6) . 4 ?
O7 Na1 O8 75.79(6) 4 3_455 ?
O7 Na1 O8 68.61(6) 3_455 3_455 ?
O4 Na1 O8 83.10(6) 2 3_455 ?
O4 Na1 O8 157.64(7) . 3_455 ?
O8 Na1 O8 77.63(9) 4 3_455 ?
O7 Na1 O3 155.87(7) 4 2 ?
O7 Na1 O3 69.53(5) 3_455 2 ?
O4 Na1 O3 61.80(5) 2 2 ?
O4 Na1 O3 74.35(5) . 2 ?
O8 Na1 O3 122.26(5) 4 2 ?
O8 Na1 O3 125.90(5) 3_455 2 ?
O7 Na1 C2 138.31(6) 4 2 ?
O7 Na1 C2 67.02(6) 3_455 2 ?
O4 Na1 C2 21.95(5) 2 2 ?
O4 Na1 C2 117.22(7) . 2 ?
O8 Na1 C2 142.60(6) 4 2 ?
O8 Na1 C2 85.12(6) 3_455 2 ?
O3 Na1 C2 47.30(5) 2 2 ?
O7 Na1 C3 20.63(6) 4 4 ?
O7 Na1 C3 114.95(7) 3_455 4 ?
O4 Na1 C3 132.38(5) 2 4 ?
O4 Na1 C3 90.22(5) . 4 ?
O8 Na1 C3 48.89(6) 4 4 ?
O8 Na1 C3 68.57(6) 3_455 4 ?
O3 Na1 C3 163.74(5) 2 4 ?
C2 Na1 C3 148.83(6) 2 4 ?
O7 Na1 C3 114.95(7) 4 3_455 ?
O7 Na1 C3 20.63(6) 3_455 3_455 ?
O4 Na1 C3 90.22(5) 2 3_455 ?
O4 Na1 C3 132.38(5) . 3_455 ?
O8 Na1 C3 68.57(6) 4 3_455 ?
O8 Na1 C3 48.89(6) 3_455 3_455 ?
O3 Na1 C3 89.06(5) 2 3_455 ?
C2 Na1 C3 75.04(6) 2 3_455 ?
C3 Na1 C3 97.95(9) 4 3_455 ?
O7 Na1 Na2 113.05(5) 4 . ?
O7 Na1 Na2 113.05(5) 3_455 . ?
O4 Na1 Na2 58.91(5) 2 . ?
O4 Na1 Na2 58.91(5) . . ?
O8 Na1 Na2 141.19(4) 4 . ?
O8 Na1 Na2 141.19(4) 3_455 . ?
O3 Na1 Na2 44.05(4) 2 . ?
C2 Na1 Na2 62.93(4) 2 . ?
C3 Na1 Na2 131.03(4) 4 . ?
C3 Na1 Na2 131.03(4) 3_455 . ?
O3 Na2 O3 112.74(9) 2 . ?
O3 Na2 O12 78.77(5) 2 3_445 ?
O3 Na2 O12 129.20(5) . 3_445 ?
O3 Na2 O12 129.20(5) 2 4_545 ?
O3 Na2 O12 78.77(5) . 4_545 ?
O12 Na2 O12 133.49(9) 3_445 4_545 ?
O3 Na2 O11 156.17(6) 2 4_545 ?
O3 Na2 O11 83.40(5) . 4_545 ?
O12 Na2 O11 77.41(6) 3_445 4_545 ?
O12 Na2 O11 69.38(6) 4_545 4_545 ?
O3 Na2 O11 83.40(5) 2 3_445 ?
O3 Na2 O11 156.17(6) . 3_445 ?
O12 Na2 O11 69.38(6) 3_445 3_445 ?
O12 Na2 O11 77.41(6) 4_545 3_445 ?
O11 Na2 O11 87.54(9) 4_545 3_445 ?
O3 Na2 O4 60.80(5) 2 2 ?
O3 Na2 O4 73.46(5) . 2 ?
O12 Na2 O4 70.65(5) 3_445 2 ?
O12 Na2 O4 151.87(6) 4_545 2 ?
O11 Na2 O4 111.09(5) 4_545 2 ?
O11 Na2 O4 130.33(5) 3_445 2 ?
O3 Na2 C1 21.82(5) 2 2 ?
O3 Na2 C1 114.24(7) . 2 ?
O12 Na2 C1 60.09(5) 3_445 2 ?
O12 Na2 C1 150.21(5) 4_545 2 ?
O11 Na2 C1 136.11(6) 4_545 2 ?
O11 Na2 C1 87.39(6) 3_445 2 ?
O4 Na2 C1 46.87(5) 2 2 ?
O3 Na2 C6 83.29(5) 2 3_445 ?
O3 Na2 C6 145.80(5) . 3_445 ?
O12 Na2 C6 20.86(5) 3_445 3_445 ?
O12 Na2 C6 115.35(7) 4_545 3_445 ?
O11 Na2 C6 74.15(6) 4_545 3_445 ?
O11 Na2 C6 49.23(6) 3_445 3_445 ?
O4 Na2 C6 90.73(5) 2 3_445 ?
C1 Na2 C6 69.76(6) 2 3_445 ?
O3 Na2 C6 145.80(5) 2 4_545 ?
O3 Na2 C6 83.29(5) . 4_545 ?
O12 Na2 C6 115.35(7) 3_445 4_545 ?
O12 Na2 C6 20.86(5) 4_545 4_545 ?
O11 Na2 C6 49.23(6) 4_545 4_545 ?
O11 Na2 C6 74.15(6) 3_445 4_545 ?
O4 Na2 C6 151.84(5) 2 4_545 ?
C1 Na2 C6 161.01(6) 2 4_545 ?
C6 Na2 C6 100.23(8) 3_445 4_545 ?
O3 Na2 Na1 56.37(5) 2 . ?
O3 Na2 Na1 56.37(5) . . ?
O12 Na2 Na1 113.25(4) 3_445 . ?
O12 Na2 Na1 113.25(4) 4_545 . ?
O11 Na2 Na1 136.23(4) 4_545 . ?
O11 Na2 Na1 136.23(4) 3_445 . ?
O4 Na2 Na1 45.78(4) 2 . ?
C1 Na2 Na1 62.13(5) 2 . ?
C6 Na2 Na1 129.88(4) 3_445 . ?
C6 Na2 Na1 129.88(4) 4_545 . ?
O3 Na2 Na4 130.24(4) 2 8_455 ?
O3 Na2 Na4 75.55(4) . 8_455 ?
O12 Na2 Na4 62.32(4) 3_445 8_455 ?
O12 Na2 Na4 100.48(4) 4_545 8_455 ?
O11 Na2 Na4 34.13(4) 4_545 8_455 ?
O11 Na2 Na4 108.11(5) 3_445 8_455 ?
O4 Na2 Na4 77.06(3) 2 8_455 ?
C1 Na2 Na4 108.61(4) 2 8_455 ?
C6 Na2 Na4 71.36(4) 3_445 8_455 ?
C6 Na2 Na4 81.98(4) 4_545 8_455 ?
Na1 Na2 Na4 110.97(2) . 8_455 ?
O15 Na3 O14 155.03(10) . . ?
O15 Na3 O13 118.26(9) . . ?
O14 Na3 O13 86.63(7) . . ?
O15 Na3 O4 88.94(7) . 7_556 ?
O14 Na3 O4 91.75(7) . 7_556 ?
O13 Na3 O4 84.42(6) . 7_556 ?
O15 Na3 O5 97.60(7) . . ?
O14 Na3 O5 91.36(6) . . ?
O13 Na3 O5 73.23(6) . . ?
O4 Na3 O5 157.20(7) 7_556 . ?
O15 Na3 O7 83.46(7) . . ?
O14 Na3 O7 84.95(6) . . ?
O13 Na3 O7 121.35(6) . . ?
O4 Na3 O7 153.64(7) 7_556 . ?
O5 Na3 O7 49.15(5) . . ?
O15 Na3 C3 95.07(7) . . ?
O14 Na3 C3 82.97(6) . . ?
O13 Na3 C3 97.05(7) . . ?
O4 Na3 C3 174.41(7) 7_556 . ?
O5 Na3 C3 25.78(5) . . ?
O7 Na3 C3 24.30(6) . . ?
O15 Na3 Na4 160.63(8) . . ?
O14 Na3 Na4 44.16(5) . . ?
O13 Na3 Na4 43.25(5) . . ?
O4 Na3 Na4 93.81(5) 7_556 . ?
O5 Na3 Na4 73.08(4) . . ?
O7 Na3 Na4 101.70(5) . . ?
C3 Na3 Na4 83.70(5) . . ?
O15 Na3 H15X 15.47(5) . . ?
O14 Na3 H15X 159.70(6) . . ?
O13 Na3 H15X 107.82(5) . . ?
O4 Na3 H15X 76.01(5) 7_556 . ?
O5 Na3 H15X 106.24(5) . . ?
O7 Na3 H15X 98.79(5) . . ?
C3 Na3 H15X 108.51(5) . . ?
Na4 Na3 H15X 150.77(4) . . ?
O13 Na4 O11 106.68(6) . 5_666 ?
O13 Na4 O16 167.40(7) . . ?
O11 Na4 O16 80.94(6) 5_666 . ?
O13 Na4 O14 84.31(6) . . ?
O11 Na4 O14 92.99(6) 5_666 . ?
O16 Na4 O14 85.29(7) . . ?
O13 Na4 O16 93.40(7) . 5_666 ?
O11 Na4 O16 78.28(6) 5_666 5_666 ?
O16 Na4 O16 98.05(6) . 5_666 ?
O14 Na4 O16 169.98(7) . 5_666 ?
O13 Na4 O9 88.10(6) . . ?
O11 Na4 O9 156.78(7) 5_666 . ?
O16 Na4 O9 88.05(6) . . ?
O14 Na4 O9 106.48(6) . . ?
O16 Na4 O9 83.14(6) 5_666 . ?
O13 Na4 Na4 141.83(7) . 5_666 ?
O11 Na4 Na4 74.04(5) 5_666 5_666 ?
O16 Na4 Na4 49.32(5) . 5_666 ?
O14 Na4 Na4 133.78(6) . 5_666 ?
O16 Na4 Na4 48.72(5) 5_666 5_666 ?
O9 Na4 Na4 83.26(5) . 5_666 ?
O13 Na4 Na3 43.27(5) . . ?
O11 Na4 Na3 109.23(5) 5_666 . ?
O16 Na4 Na3 125.13(6) . . ?
O14 Na4 Na3 41.79(5) . . ?
O16 Na4 Na3 136.67(5) 5_666 . ?
O9 Na4 Na3 93.84(5) . . ?
Na4 Na4 Na3 173.67(5) 5_666 . ?
O13 Na4 Na2 77.02(5) . 7_556 ?
O11 Na4 Na2 34.98(4) 5_666 7_556 ?
O16 Na4 Na2 106.38(5) . 7_556 ?
O14 Na4 Na2 71.88(5) . 7_556 ?
O16 Na4 Na2 98.10(5) 5_666 7_556 ?
O9 Na4 Na2 165.11(5) . 7_556 ?
Na4 Na4 Na2 108.78(4) 5_666 7_556 ?
Na3 Na4 Na2 75.00(3) . 7_556 ?
C1 O1 Cr1 114.30(13) . . ?
C2 O2 Cr1 114.38(14) . . ?
C1 O3 Na2 111.65(14) . . ?
C2 O4 Na3 119.72(14) . 7_556 ?
C2 O4 Na1 108.42(14) . . ?
Na3 O4 Na1 128.44(7) 7_556 . ?
C3 O5 Cr1 114.25(14) . . ?
C3 O5 Na3 91.86(13) . . ?
Cr1 O5 Na3 144.06(8) . . ?
C4 O6 Cr1 114.09(13) . . ?
C3 O7 Na1 115.42(14) . 3_545 ?
C3 O7 Na3 89.25(13) . . ?
Na1 O7 Na3 135.55(7) 3_545 . ?
C4 O8 Na1 111.44(14) . 3_545 ?
C5 O9 Cr1 113.88(13) . . ?
C5 O9 Na4 117.91(13) . . ?
Cr1 O9 Na4 126.71(7) . . ?
C6 O10 Cr1 114.76(13) . . ?
C5 O11 Na4 134.50(14) . 5_666 ?
C5 O11 Na2 113.59(14) . 3 ?
Na4 O11 Na2 110.89(6) 5_666 3 ?
C6 O12 Na2 114.23(14) . 3 ?
Na4 O13 Na3 93.48(7) . . ?
Na4 O13 H13X 103(2) . . ?
Na3 O13 H13X 121.0(19) . . ?
Na4 O13 H13Y 110(2) . . ?
Na3 O13 H13Y 120.6(19) . . ?
H13X O13 H13Y 106(2) . . ?
Na3 O14 Na4 94.05(7) . . ?
Na3 O14 H14X 118.4(19) . . ?
Na4 O14 H14X 108(2) . . ?
Na3 O14 H14Y 116.0(19) . . ?
Na4 O14 H14Y 114(2) . . ?
H14X O14 H14Y 106(2) . . ?
Na3 O15 H15X 110.55(19) . . ?
Na3 O15 H15Y 113(2) . . ?
H15X O15 H15Y 123(2) . . ?
Na4 O16 Na4 81.96(6) . 5_666 ?
Na4 O16 H16X 111.1(19) . . ?
Na4 O16 H16X 127.1(19) 5_666 . ?
Na4 O16 H16Y 116.1(19) . . ?
Na4 O16 H16Y 113.9(19) 5_666 . ?
H16X O16 H16Y 106(2) . . ?
O3 C1 O1 126.6(2) . . ?
O3 C1 C2 119.87(19) . . ?
O1 C1 C2 113.52(18) . . ?
O4 C2 O2 126.3(2) . . ?
O4 C2 C1 119.34(19) . . ?
O2 C2 C1 114.31(18) . . ?
O7 C3 O5 124.8(2) . . ?
O7 C3 C4 120.73(19) . . ?
O5 C3 C4 114.43(18) . . ?
O7 C3 Na3 66.45(12) . . ?
O5 C3 Na3 62.37(11) . . ?
C4 C3 Na3 156.91(14) . . ?
O7 C3 Na1 43.95(11) . 3_545 ?
O5 C3 Na1 163.93(15) . 3_545 ?
C4 C3 Na1 77.77(11) . 3_545 ?
Na3 C3 Na1 102.20(7) . 3_545 ?
O8 C4 O6 126.4(2) . . ?
O8 C4 C3 119.70(19) . . ?
O6 C4 C3 113.90(18) . . ?
O11 C5 O9 126.4(2) . . ?
O11 C5 C6 119.46(19) . . ?
O9 C5 C6 114.16(18) . . ?
O12 C6 O10 126.3(2) . . ?
O12 C6 C5 119.97(19) . . ?
O10 C6 C5 113.70(18) . . ?
O12 C6 Na2 44.91(11) . 3 ?
O10 C6 Na2 168.35(15) . 3 ?
C5 C6 Na2 75.74(11) . 3 ?
H1W O1W H2W 110(2) . . ?

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
O1W H2W O2 0.855(17) 2.235(19) 2.980(3) 146(3) .
O1W H1W O1 0.838(17) 1.981(18) 2.816(3) 175(3) 4
O16 H16Y O1X 0.859(16) 2.00(2) 2.780(8) 150(2) 5_666
O16 H16Y O1W 0.859(16) 1.982(17) 2.838(3) 174(3) 5_666
O16 H16X O6 0.871(16) 2.15(2) 2.984(2) 160(3) 2_655
O15 H15Y O10 0.858(16) 1.97(2) 2.804(3) 166(4) 4_545
O14 H14Y O8 0.874(16) 1.938(17) 2.804(2) 170(3) 2_655
O14 H14X O3 0.860(16) 1.977(17) 2.798(2) 159(3) 8_556
O13 H13Y O2 0.870(16) 2.251(17) 3.070(2) 157(2) .
O13 H13X O12 0.862(16) 1.941(18) 2.731(2) 152(3) 6_566
O14 H14X O3 0.860(16) 1.977(17) 2.798(2) 159(3) 8_556
O14 H14Y O8 0.874(16) 1.938(17) 2.804(2) 170(3) 2_655
O15 H15Y O10 0.858(16) 1.97(2) 2.804(3) 166(4) 4_545
O16 H16X O6 0.871(16) 2.15(2) 2.984(2) 160(3) 2_655
O16 H16Y O1W 0.859(16) 1.982(17) 2.838(3) 174(3) 5_666
O16 H16Y O1X 0.859(16) 2.00(2) 2.780(8) 150(2) 5_666
O13 H13X O12 0.862(16) 1.941(18) 2.731(2) 152(3) 6_566
O13 H13Y O2 0.870(16) 2.251(17) 3.070(2) 157(2) .
O1W H1W O1 0.838(17) 1.981(18) 2.816(3) 175(3) 4
O1W H2W O2 0.855(17) 2.235(19) 2.980(3) 146(3) .
O13 H13X O12 0.862(16) 1.941(18) 2.731(2) 152(3) 6_566
O13 H13Y O2 0.870(16) 2.251(17) 3.070(2) 157(2) .
O14 H14X O3 0.860(16) 1.977(17) 2.798(2) 159(3) 8_556
O14 H14Y O8 0.874(16) 1.938(17) 2.804(2) 170(3) 2_655
O15 H15Y O10 0.858(16) 1.97(2) 2.804(3) 166(4) 4_545
O16 H16X O6 0.871(16) 2.15(2) 2.984(2) 160(3) 2_655
O16 H16Y O1W 0.859(16) 1.982(17) 2.838(3) 174(3) 5_666
O16 H16Y O1X 0.859(16) 2.00(2) 2.780(8) 150(2) 5_666
O1W H1W O1 0.838(17) 1.981(18) 2.816(3) 175(3) 4
O1W H2W O2 0.855(17) 2.235(19) 2.980(3) 146(3) .
O13 H13X O12 0.862(16) 1.941(18) 2.731(2) 152(3) 6_566
O13 H13Y O2 0.870(16) 2.251(17) 3.070(2) 157(2) .
O14 H14X O3 0.860(16) 1.977(17) 2.798(2) 159(3) 8_556
O14 H14Y O8 0.874(16) 1.938(17) 2.804(2) 170(3) 2_655
O15 H15Y O10 0.858(16) 1.97(2) 2.804(3) 166(4) 4_545
O16 H16X O6 0.871(16) 2.15(2) 2.984(2) 160(3) 2_655
O16 H16Y O1W 0.859(16) 1.982(17) 2.838(3) 174(3) 5_666
O16 H16Y O1X 0.859(16) 2.00(2) 2.780(8) 150(2) 5_666
O1W H1W O1 0.838(17) 1.981(18) 2.816(3) 175(3) 4
O1W H2W O2 0.855(17) 2.235(19) 2.980(3) 146(3) .
O15 H15X O1W 0.727(2) 2.286(2) 2.864(3) 137.4(2) 7_556
O15 H15X O2 0.727(2) 2.5578(15) 3.150(3) 140.06(16) 7_556

_refine_diff_density_max         0.934
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.090

_shelxl_version_number           2014/6

