# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_xb2668_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2038779'
loop_
_audit_author_name
_audit_author_address
'Bin Liu'
;Northwest University
China
;
_audit_update_record             
;
2021-01-15 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H17 Cr2 Na3 O20, 2(H2 O)'
_chemical_formula_sum            'C4 H21 Cr2 Na3 O22'
_chemical_formula_weight         594.18

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'
Cr Cr 0.3209 0.6236 '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'

_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                   21.463(16)
_cell_length_b                   8.882(7)
_cell_length_c                   9.942(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.899(12)
_cell_angle_gamma                90
_cell_volume                     1882(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1515
_cell_measurement_theta_min      2.487
_cell_measurement_theta_max      25.580

_exptl_crystal_description       block
_exptl_crystal_colour            tan
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.335
_shelx_estimated_absorpt_T_min   0.706
_shelx_estimated_absorpt_T_max   0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            4499
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_av_R_equivalents  0.1077
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.156
_diffrn_reflns_theta_max         25.898
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             1793
_reflns_number_gt                1423
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 The relatively high R values may be caused by the short expose time in
 the collection of diffraction data in measurement. However, the present
 structure is correct and the atomic displacement parameters are also good.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1460P)²+36.9545P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1793
_refine_ls_number_parameters     141
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.1056
_refine_ls_wR_factor_ref         0.2840
_refine_ls_wR_factor_gt          0.2729
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_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
O11 O 0.4318(5) 0.4793(11) 0.5017(9) 0.062(3) Uani 1 1 d . . . . .
H11D H 0.403892 0.394480 0.491124 0.074 Uiso 1 1 d R U . . .
H11B H 0.422833 0.533550 0.567114 0.093 Uiso 1 1 d R U . . .
Cr1 Cr 0.23398(7) 0.19675(14) 0.59364(12) 0.0186(5) Uani 1 1 d . . . . .
Na1 Na 0.31519(19) 0.1272(4) 0.1351(4) 0.0312(9) Uani 1 1 d . . . . .
Na2 Na 0.500000 0.2815(8) 0.250000 0.0453(16) Uani 1 2 d S T P . .
C1 C 0.3705(5) 0.1929(10) 0.5934(9) 0.0261(19) Uani 1 1 d . . . . .
C2 C 0.2273(4) -0.0106(9) 0.3695(9) 0.0206(17) Uani 1 1 d . . . . .
O1 O 0.3256(3) 0.1450(8) 0.6586(7) 0.0280(15) Uani 1 1 d . . . . .
O2 O 0.3572(3) 0.2563(8) 0.4747(7) 0.0311(15) Uani 1 1 d . . . . .
O3 O 0.4260(4) 0.1766(13) 0.6456(10) 0.067(3) Uani 1 1 d . . . . .
H3B H 0.450798 0.192107 0.720270 0.100 Uiso 0.5 1 d R U P . .
O4 O 0.2222(3) -0.0058(7) 0.4980(6) 0.0259(14) Uani 1 1 d . . . . .
O5 O 0.2525(3) 0.1010(7) 0.3128(6) 0.0245(14) Uani 1 1 d . . . . .
O6 O 0.2049(3) -0.1228(7) 0.2982(6) 0.0258(14) Uani 1 1 d . . . . .
O7 O 0.4183(4) 0.1096(10) 0.2643(8) 0.0446(19) Uani 1 1 d . . . . .
H7A H 0.432688 0.023708 0.246253 0.054 Uiso 1 1 d R U . . .
H7B H 0.412278 0.107108 0.347233 0.054 Uiso 1 1 d R U . . .
O8 O 0.3488(3) 0.2378(10) -0.0663(7) 0.0380(17) Uani 1 1 d . . . . .
H8A H 0.317075 0.252549 -0.124599 0.057 Uiso 1 1 d R U . . .
H8B H 0.366835 0.321269 -0.045769 0.057 Uiso 1 1 d R U . . .
O9 O 0.5762(4) 0.4820(10) 0.2494(8) 0.047(2) Uani 1 1 d . . . . .
H9B H 0.605912 0.453894 0.205939 0.070 Uiso 1 1 d R U . . .
H9C H 0.558432 0.559044 0.211349 0.070 Uiso 1 1 d R U . . .
O10 O 0.4821(4) 0.2888(11) -0.0050(10) 0.058(3) Uani 1 1 d . . . . .
H10A H 0.454944 0.222786 -0.033443 0.087 Uiso 1 1 d R U . . .
H10C H 0.516353 0.270296 -0.036583 0.087 Uiso 1 1 d 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
O11 H11D 0.9601 . ?
O11 H11B 0.8501 . ?
Cr1 O5 2.028(6) 7_556 ?
Cr1 O4 2.036(6) . ?
Cr1 O2 2.037(7) 7_556 ?
Cr1 O1 2.047(7) . ?
Cr1 Cr1 2.268(3) 7_556 ?
Cr1 O6 2.294(6) 6_556 ?
Cr1 Na1 3.364(5) 6_556 ?
Cr1 Na1 3.393(4) 7_556 ?
Na1 O5 2.357(7) . ?
Na1 O6 2.371(7) 4 ?
Na1 O8 2.417(8) . ?
Na1 O7 2.427(9) . ?
Na1 O1 2.437(8) 6 ?
Na1 O4 2.521(8) 6 ?
Na1 C1 3.128(10) 6 ?
Na2 O7 2.342(9) . ?
Na2 O7 2.342(9) 2_655 ?
Na2 O9 2.418(10) . ?
Na2 O9 2.418(10) 2_655 ?
Na2 O10 2.520(10) . ?
Na2 O10 2.520(10) 2_655 ?
C1 O3 1.250(13) . ?
C1 O1 1.297(11) . ?
C1 O2 1.308(11) . ?
C2 O6 1.282(10) . ?
C2 O5 1.291(10) . ?
C2 O4 1.297(11) . ?
O3 H3B 0.8709 . ?
O7 H7A 0.8500 . ?
O7 H7B 0.8501 . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8499 . ?
O9 H9B 0.8500 . ?
O9 H9C 0.8500 . ?
O10 H10A 0.8500 . ?
O10 H10C 0.8499 . ?

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
H11D O11 H11B 109.5 . . ?
O5 Cr1 O4 178.8(3) 7_556 . ?
O5 Cr1 O2 92.9(3) 7_556 7_556 ?
O4 Cr1 O2 88.0(3) . 7_556 ?
O5 Cr1 O1 88.6(3) 7_556 . ?
O4 Cr1 O1 90.6(3) . . ?
O2 Cr1 O1 178.5(3) 7_556 . ?
O5 Cr1 Cr1 88.07(18) 7_556 7_556 ?
O4 Cr1 Cr1 91.04(18) . 7_556 ?
O2 Cr1 Cr1 90.9(2) 7_556 7_556 ?
O1 Cr1 Cr1 88.8(2) . 7_556 ?
O5 Cr1 O6 83.4(2) 7_556 6_556 ?
O4 Cr1 O6 97.4(2) . 6_556 ?
O2 Cr1 O6 90.1(3) 7_556 6_556 ?
O1 Cr1 O6 90.5(3) . 6_556 ?
Cr1 Cr1 O6 171.51(18) 7_556 6_556 ?
O5 Cr1 Na1 131.1(2) 7_556 6_556 ?
O4 Cr1 Na1 48.3(2) . 6_556 ?
O2 Cr1 Na1 132.8(2) 7_556 6_556 ?
O1 Cr1 Na1 46.0(2) . 6_556 ?
Cr1 Cr1 Na1 104.70(10) 7_556 6_556 ?
O6 Cr1 Na1 80.71(17) 6_556 6_556 ?
O5 Cr1 Na1 42.97(17) 7_556 7_556 ?
O4 Cr1 Na1 138.16(18) . 7_556 ?
O2 Cr1 Na1 78.0(2) 7_556 7_556 ?
O1 Cr1 Na1 103.4(2) . 7_556 ?
Cr1 Cr1 Na1 127.90(11) 7_556 7_556 ?
O6 Cr1 Na1 44.23(17) 6_556 7_556 ?
Na1 Cr1 Na1 120.18(8) 6_556 7_556 ?
O5 Na1 O6 75.1(2) . 4 ?
O5 Na1 O8 156.2(3) . . ?
O6 Na1 O8 86.2(3) 4 . ?
O5 Na1 O7 99.4(3) . . ?
O6 Na1 O7 95.6(3) 4 . ?
O8 Na1 O7 96.9(3) . . ?
O5 Na1 O1 83.3(2) . 6 ?
O6 Na1 O1 156.9(3) 4 6 ?
O8 Na1 O1 116.7(3) . 6 ?
O7 Na1 O1 79.5(3) . 6 ?
O5 Na1 O4 82.9(2) . 6 ?
O6 Na1 O4 113.1(3) 4 6 ?
O8 Na1 O4 91.2(3) . 6 ?
O7 Na1 O4 150.6(3) . 6 ?
O1 Na1 O4 71.6(2) 6 6 ?
O5 Na1 C1 105.6(3) . 6 ?
O6 Na1 C1 166.6(3) 4 6 ?
O8 Na1 C1 95.9(3) . 6 ?
O7 Na1 C1 71.0(3) . 6 ?
O1 Na1 C1 22.9(2) 6 6 ?
O4 Na1 C1 80.1(2) 6 6 ?
O5 Na1 Cr1 70.93(18) . 6 ?
O6 Na1 Cr1 136.6(2) 4 6 ?
O8 Na1 Cr1 116.6(2) . 6 ?
O7 Na1 Cr1 115.8(3) . 6 ?
O1 Na1 Cr1 37.17(16) 6 6 ?
O4 Na1 Cr1 37.11(15) 6 6 ?
C1 Na1 Cr1 53.52(19) 6 6 ?
O5 Na1 Cr1 35.90(16) . 7_556 ?
O6 Na1 Cr1 42.44(16) 4 7_556 ?
O8 Na1 Cr1 128.6(2) . 7_556 ?
O7 Na1 Cr1 87.7(2) . 7_556 ?
O1 Na1 Cr1 114.5(2) 6 7_556 ?
O4 Na1 Cr1 108.99(19) 6 7_556 ?
C1 Na1 Cr1 133.1(2) 6 7_556 ?
Cr1 Na1 Cr1 106.59(11) 6 7_556 ?
O7 Na2 O7 98.6(5) . 2_655 ?
O7 Na2 O9 172.6(4) . . ?
O7 Na2 O9 88.2(3) 2_655 . ?
O7 Na2 O9 88.2(3) . 2_655 ?
O7 Na2 O9 172.6(4) 2_655 2_655 ?
O9 Na2 O9 85.1(5) . 2_655 ?
O7 Na2 O10 93.0(3) . . ?
O7 Na2 O10 88.9(3) 2_655 . ?
O9 Na2 O10 90.0(3) . . ?
O9 Na2 O10 87.8(3) 2_655 . ?
O7 Na2 O10 88.9(3) . 2_655 ?
O7 Na2 O10 93.0(3) 2_655 2_655 ?
O9 Na2 O10 87.8(3) . 2_655 ?
O9 Na2 O10 90.0(3) 2_655 2_655 ?
O10 Na2 O10 177.1(6) . 2_655 ?
O3 C1 O1 118.9(9) . . ?
O3 C1 O2 121.2(9) . . ?
O1 C1 O2 119.9(8) . . ?
O3 C1 Na1 101.4(7) . 6_556 ?
O1 C1 Na1 47.0(5) . 6_556 ?
O2 C1 Na1 117.8(6) . 6_556 ?
O6 C2 O5 120.3(7) . . ?
O6 C2 O4 120.0(8) . . ?
O5 C2 O4 119.6(8) . . ?
C1 O1 Cr1 120.8(6) . . ?
C1 O1 Na1 110.0(6) . 6_556 ?
Cr1 O1 Na1 96.8(3) . 6_556 ?
C1 O2 Cr1 119.0(6) . 7_556 ?
C1 O3 H3B 142.2 . . ?
C2 O4 Cr1 118.0(5) . . ?
C2 O4 Na1 111.3(5) . 6_556 ?
Cr1 O4 Na1 94.6(3) . 6_556 ?
C2 O5 Cr1 121.6(5) . 7_556 ?
C2 O5 Na1 135.2(5) . . ?
Cr1 O5 Na1 101.1(3) 7_556 . ?
C2 O6 Cr1 126.1(6) . 6 ?
C2 O6 Na1 129.9(5) . 4_545 ?
Cr1 O6 Na1 93.3(2) 6 4_545 ?
Na2 O7 Na1 124.6(4) . . ?
Na2 O7 H7A 106.2 . . ?
Na1 O7 H7A 106.1 . . ?
Na2 O7 H7B 106.2 . . ?
Na1 O7 H7B 106.2 . . ?
H7A O7 H7B 106.4 . . ?
Na1 O8 H8A 109.5 . . ?
Na1 O8 H8B 109.2 . . ?
H8A O8 H8B 109.5 . . ?
Na2 O9 H9B 109.5 . . ?
Na2 O9 H9C 109.1 . . ?
H9B O9 H9C 109.5 . . ?
Na2 O10 H10A 109.4 . . ?
Na2 O10 H10C 109.4 . . ?
H10A O10 H10C 109.5 . . ?

_refine_diff_density_max         1.550
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.225



