# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_r-3
_database_code_depnum_ccdc_archive 'CCDC 1845080'
_audit_update_record             
;
2018-05-24 deposited with the CCDC.
2018-08-13 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            'C3 H7 Cr0.50 N Na0.50 O6'
_chemical_formula_weight         190.59

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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   7.9386(5)
_cell_length_b                   7.9386(5)
_cell_length_c                   21.494(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1173.1(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1287
_cell_measurement_theta_min      2.8373
_cell_measurement_theta_max      27.6903

_exptl_crystal_description       prism
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_F_000             585
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_min  0.85463
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3383
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.843
_diffrn_reflns_theta_max         27.751
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             586
_reflns_number_gt                444
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0410P)²+0.8557P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         586
_refine_ls_number_parameters     39
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0827
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.015
_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
Cr Cr 0.0000 0.0000 1.0000 0.0278(3) Uani 1 6 d S T P . .
Na Na 0.6667 0.3333 0.8333 0.0338(6) Uani 1 6 d S T P . .
O1 O 0.1735(2) 0.2190(2) 0.94598(8) 0.0361(5) Uani 1 1 d . . . . .
C1 C 0.3428(4) 0.2640(4) 0.92965(13) 0.0437(7) Uani 1 1 d . . . . .
H1 H 0.3931 0.1904 0.9464 0.052 Uiso 1 1 calc R U . . .
O3 O 0.4477(3) 0.3939(3) 0.89418(9) 0.0483(6) Uani 1 1 d . . . . .
N2 N 0.3333 0.6667 0.8565(2) 0.0523(12) Uani 1 3 d DS T P . .
H11 H 0.365(4) 0.583(3) 0.8711(7) 0.063 Uiso 1 1 d D U . . .
H21 H 0.3333 0.6667 0.8160(3) 0.063 Uiso 1 3 d DS U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr 0.0247(4) 0.0247(4) 0.0341(6) 0.000 0.000 0.01235(19)
Na 0.0310(8) 0.0310(8) 0.0394(15) 0.000 0.000 0.0155(4)
O1 0.0283(10) 0.0344(10) 0.0451(11) 0.0077(8) 0.0069(8) 0.0153(8)
C1 0.0385(16) 0.0440(17) 0.0540(18) 0.0089(14) 0.0057(14) 0.0247(14)
O3 0.0411(12) 0.0396(11) 0.0619(13) 0.0145(10) 0.0206(10) 0.0185(9)
N2 0.0499(17) 0.0499(17) 0.057(3) 0.000 0.000 0.0250(8)

_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
Cr O1 1.9683(17) . ?
Cr O1 1.9683(16) 11_557 ?
Cr O1 1.9683(16) 2 ?
Cr O1 1.9683(16) 12_557 ?
Cr O1 1.9683(16) 3 ?
Cr O1 1.9683(17) 10_557 ?
Na O3 2.4082(19) 2_655 ?
Na O3 2.4082(19) 17_556 ?
Na O3 2.4082(19) 3_665 ?
Na O3 2.4082(19) . ?
Na O3 2.4082(19) 18_546 ?
Na O3 2.4083(19) 16_656 ?
O1 C1 1.255(3) . ?
C1 O3 1.216(3) . ?
C1 H1 0.9300 . ?
N2 H11 0.873(5) . ?
N2 H21 0.871(5) . ?

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 Cr O1 91.26(7) . 11_557 ?
O1 Cr O1 88.74(7) . 2 ?
O1 Cr O1 180.0 11_557 2 ?
O1 Cr O1 91.26(7) . 12_557 ?
O1 Cr O1 88.74(7) 11_557 12_557 ?
O1 Cr O1 91.26(7) 2 12_557 ?
O1 Cr O1 88.74(7) . 3 ?
O1 Cr O1 91.26(7) 11_557 3 ?
O1 Cr O1 88.74(7) 2 3 ?
O1 Cr O1 180.0 12_557 3 ?
O1 Cr O1 180.0 . 10_557 ?
O1 Cr O1 88.74(7) 11_557 10_557 ?
O1 Cr O1 91.26(7) 2 10_557 ?
O1 Cr O1 88.74(7) 12_557 10_557 ?
O1 Cr O1 91.26(7) 3 10_557 ?
O3 Na O3 180.0 2_655 17_556 ?
O3 Na O3 93.30(7) 2_655 3_665 ?
O3 Na O3 86.70(7) 17_556 3_665 ?
O3 Na O3 93.30(7) 2_655 . ?
O3 Na O3 86.70(7) 17_556 . ?
O3 Na O3 93.30(7) 3_665 . ?
O3 Na O3 86.70(7) 2_655 18_546 ?
O3 Na O3 93.30(7) 17_556 18_546 ?
O3 Na O3 180.0 3_665 18_546 ?
O3 Na O3 86.70(7) . 18_546 ?
O3 Na O3 86.70(7) 2_655 16_656 ?
O3 Na O3 93.30(7) 17_556 16_656 ?
O3 Na O3 86.70(7) 3_665 16_656 ?
O3 Na O3 180.00(6) . 16_656 ?
O3 Na O3 93.30(7) 18_546 16_656 ?
C1 O1 Cr 126.38(18) . . ?
O3 C1 O1 126.8(3) . . ?
O1 C1 Na 154.7(2) . . ?
O3 C1 H1 116.6 . . ?
O1 C1 H1 116.6 . . ?
H11 N2 H21 111.0(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
N2 H11 O3 0.873(5) 1.983(6) 2.852(2) 173.3(17) .
N2 H21 O1 0.871(5) 2.592(5) 3.324(4) 142.19(9) 16_556
N2 H21 O1 0.871(5) 2.592(5) 3.324(4) 142.19(9) 17_556
N2 H21 O1 0.871(5) 2.592(5) 3.324(4) 142.19(9) 18_556

_refine_diff_density_max         0.275
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.066

_shelx_res_file                  
;

    r-3.res created by SHELXL-2014/7


TITL r-3 in R-3
CELL 0.71073   7.9386   7.9386  21.4941  90.000  90.000 120.000
ZERR    6.00   0.0005   0.0005   0.0027   0.000   0.000   0.000
LATT  3
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SFAC C H N O NA Cr
UNIT 18 42 6 36 3 3

L.S. 20
BOND
bond $h
FMAP 2
PLAN 20
acta 50
htab
HTAB N2 O3
EQIV $1 -x+1/3, -y+2/3, -z+5/3
HTAB N2 O1_$1
EQIV $2 y+1/3, -x+y+2/3, -z+5/3
HTAB N2 O1_$2
EQIV $3 x-y+1/3, x+2/3, -z+5/3
HTAB N2 O1_$3
WGHT    0.041000    0.855700
FVAR       0.21734
MOLE   1
CR    6    0.000000    0.000000    1.000000    10.16667    0.02469    0.02469 =
         0.03411    0.00000    0.00000    0.01235
NA    5    0.666667    0.333333    0.833333    10.16667    0.03105    0.03105 =
         0.03935    0.00000    0.00000    0.01552
O1    4    0.173543    0.219037    0.945979    11.00000    0.02834    0.03437 =
         0.04513    0.00770    0.00690    0.01532
C1    1    0.342759    0.264027    0.929651    11.00000    0.03848    0.04401 =
         0.05402    0.00894    0.00570    0.02467
AFIX  43
H1    2    0.393131    0.190416    0.946414    11.00000   -1.20000
AFIX   0
O3    4    0.447695    0.393919    0.894177    11.00000    0.04109    0.03959 =
         0.06188    0.01448    0.02056    0.01848
mOLE   2
MOLE   3
dfix 0.87 0.005 N2 H11 N2 H21
dfix 1.44 0.01 h11 h21
N2    3    0.333333    0.666667    0.856512    10.33333    0.04995    0.04995 =
         0.05693    0.00000    0.00000    0.02497
H11   2    0.364610    0.583260    0.871053    11.00000   -1.20000
H21   2    0.333333    0.666667    0.815974    10.33333   -1.20000
HKLF 4

REM  r-3 in R-3
REM R1 =  0.0399 for     444 Fo > 4sig(Fo)  and  0.0658 for all     586 data
REM     39 parameters refined using      3 restraints

END

WGHT      0.0395      0.9154

REM Instructions for potential hydrogen bonds
HTAB N2 O3
HTAB N2 O1_$1
HTAB N2 O1_$2
HTAB N2 O1_$3

REM Highest difference peak  0.275,  deepest hole -0.304,  1-sigma level  0.066
Q1    1   0.3333  0.6667  0.9670  10.33333  0.05    0.28
Q2    1   0.1503  0.1451  0.9948  11.00000  0.05    0.26
Q3    1   0.0988  0.1975  0.9588  11.00000  0.05    0.24
Q4    1   0.2505  0.1669  0.9760  11.00000  0.05    0.23
Q5    1   0.0544  0.0838  0.9442  11.00000  0.05    0.22
Q6    1   0.3574  0.4393  0.8881  11.00000  0.05    0.21
Q7    1   0.5612  0.4174  0.8664  11.00000  0.05    0.20
Q8    1   0.1596  0.1400  0.9206  11.00000  0.05    0.20
Q9    1   0.4173  0.2878  0.9836  11.00000  0.05    0.18
Q10   1   0.4512  0.4692  0.9270  11.00000  0.05    0.18
Q11   1   0.2398  0.2591  0.9892  11.00000  0.05    0.16
Q12   1   0.4960  0.3830  0.9463  11.00000  0.05    0.16
Q13   1   0.3417  0.0977  0.9100  11.00000  0.05    0.16
Q14   1   0.1975  0.4557  0.9056  11.00000  0.05    0.16
Q15   1   0.4181  0.3987  0.9225  11.00000  0.05    0.15
Q16   1   0.4354  0.6240  0.9331  11.00000  0.05    0.15
Q17   1   0.4993  0.2027  0.8267  11.00000  0.05    0.15
Q18   1   0.4957  0.4970  0.8171  11.00000  0.05    0.15
Q19   1   0.3970  0.3846  0.8522  11.00000  0.05    0.15
Q20   1   0.5230  0.3125  1.0212  11.00000  0.05    0.15
;
_shelx_res_checksum              88021
