# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2286960'
loop_
_audit_author_name
_audit_author_address
'Olga Yakubovich'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2023-08-05 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'sodium cobalt (II, III) posphate cloride'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl8 Co14.76 O32 P8, 2(Na)'
_chemical_formula_sum            'Cl4 Co7.38 Na O16 P4'
_chemical_formula_weight         979.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_H-M_alt        'I -4 2 m'
_space_group_name_Hall           'I -4 2'

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

_cell_length_a                   9.1150(4)
_cell_length_b                   9.1150(4)
_cell_length_c                   10.2056(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     847.91(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1696
_cell_measurement_theta_min      2.975
_cell_measurement_theta_max      32.723

_exptl_crystal_description       irregular
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.837
_exptl_crystal_F_000             933
_exptl_transmission_factor_min   0.789
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.012
_exptl_absorpt_coefficient_mu    8.157
_shelx_estimated_absorpt_T_min   0.569
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  1.272
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_reflns_number            2486
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.996
_diffrn_reflns_theta_max         29.987
_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             651
_reflns_number_gt                638
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.714
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    DIAMOND
_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)+(0.0140P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         651
_refine_ls_number_parameters     49
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0164
_refine_ls_wR_factor_ref         0.0360
_refine_ls_wR_factor_gt          0.0358
_refine_ls_goodness_of_fit_ref   1.302
_refine_ls_restrained_S_all      1.302
_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
Co1 Co 0.74583(4) 0.74583(4) 0.31152(5) 0.00510(13) Uani 1 2 d S T P . .
Co2 Co 1.0000 0.73101(7) 0.5000 0.00639(17) Uani 0.845(2) 2 d S T . . .
P1 P 1.0000 0.5000 0.2500 0.0076(3) Uani 1 4 d S T P . .
P2 P 0.5000 0.5000 0.21190(13) 0.0043(3) Uani 1 4 d S T P . .
Na1 Na 0.5000 0.5000 0.5000 0.0127(6) Uani 1 8 d S T P . .
Cl1 Cl 0.76851(8) 0.76851(8) 0.07271(8) 0.0112(2) Uani 1 2 d S T P . .
O1 O 0.5963(2) 0.4037(2) 0.1196(3) 0.0074(6) Uani 1 2 d S T P . .
O2 O 0.9227(2) 0.6110(2) 0.3396(2) 0.0116(5) Uani 1 1 d . . . . .
O3 O 0.5949(2) 0.5949(2) 0.2994(3) 0.0079(6) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O3 1.949(3) . ?
Co1 O2 2.047(2) . ?
Co1 O2 2.047(2) 8 ?
Co1 O1 2.153(3) 11_565 ?
Co1 Cl1 2.4547(10) . ?
Co1 Cl1 2.6720(10) 10_665 ?
Co2 O2 2.091(2) . ?
Co2 O2 2.091(2) 5_756 ?
Co2 O1 2.1767(17) 9 ?
Co2 O1 2.1767(17) 11_565 ?
Co2 Cl1 2.5575(7) 10_665 ?
Co2 Cl1 2.5575(7) 11_565 ?
P1 O2 1.535(2) 12_645 ?
P1 O2 1.535(2) 11_565 ?
P1 O2 1.535(2) 2_765 ?
P1 O2 1.535(2) . ?
P2 O3 1.514(3) . ?
P2 O3 1.514(3) 2_665 ?
P2 O1 1.558(3) . ?
P2 O1 1.558(3) 2_665 ?
P2 Na1 2.9403(13) . ?
Na1 O3 2.385(3) . ?
Na1 O3 2.385(3) 2_665 ?
Na1 O3 2.385(3) 4_656 ?
Na1 O3 2.385(3) 3_566 ?
Na1 P2 2.9402(13) 3_566 ?
Na1 Cl1 3.0749(10) 10_665 ?
Na1 Cl1 3.0749(10) 9_445 ?
Na1 Cl1 3.0749(10) 12_645 ?
Na1 Cl1 3.0749(10) 11_465 ?
Cl1 Co2 2.5575(7) 12_645 ?
Cl1 Co2 2.5575(7) 10_664 ?
Cl1 Co1 2.6719(10) 10_664 ?
Cl1 Na1 3.0749(10) 9_554 ?
O1 Co1 2.153(3) 12_645 ?
O1 Co2 2.1767(17) 9_444 ?
O1 Co2 2.1767(17) 12_645 ?

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
O3 Co1 O2 98.10(6) . . ?
O3 Co1 O2 98.10(6) . 8 ?
O2 Co1 O2 157.80(13) . 8 ?
O3 Co1 O1 164.59(10) . 11_565 ?
O2 Co1 O1 80.17(6) . 11_565 ?
O2 Co1 O1 80.17(6) 8 11_565 ?
O3 Co1 Cl1 93.19(9) . . ?
O2 Co1 Cl1 97.07(7) . . ?
O2 Co1 Cl1 97.07(7) 8 . ?
O1 Co1 Cl1 102.21(8) 11_565 . ?
O3 Co1 Cl1 89.69(9) . 10_665 ?
O2 Co1 Cl1 82.51(7) . 10_665 ?
O2 Co1 Cl1 82.51(7) 8 10_665 ?
O1 Co1 Cl1 74.91(8) 11_565 10_665 ?
Cl1 Co1 Cl1 177.12(3) . 10_665 ?
O2 Co2 O2 116.94(12) . 5_756 ?
O2 Co2 O1 162.38(9) . 9 ?
O2 Co2 O1 78.66(9) 5_756 9 ?
O2 Co2 O1 78.66(9) . 11_565 ?
O2 Co2 O1 162.38(9) 5_756 11_565 ?
O1 Co2 O1 87.36(15) 9 11_565 ?
O2 Co2 Cl1 84.57(6) . 10_665 ?
O2 Co2 Cl1 95.53(6) 5_756 10_665 ?
O1 Co2 Cl1 102.82(7) 9 10_665 ?
O1 Co2 Cl1 77.03(6) 11_565 10_665 ?
O2 Co2 Cl1 95.53(6) . 11_565 ?
O2 Co2 Cl1 84.57(6) 5_756 11_565 ?
O1 Co2 Cl1 77.03(6) 9 11_565 ?
O1 Co2 Cl1 102.82(7) 11_565 11_565 ?
Cl1 Co2 Cl1 179.80(4) 10_665 11_565 ?
O2 P1 O2 106.91(17) 12_645 11_565 ?
O2 P1 O2 110.77(9) 12_645 2_765 ?
O2 P1 O2 110.77(9) 11_565 2_765 ?
O2 P1 O2 110.77(9) 12_645 . ?
O2 P1 O2 110.77(9) 11_565 . ?
O2 P1 O2 106.91(17) 2_765 . ?
O3 P2 O3 107.8(2) . 2_665 ?
O3 P2 O1 110.88(7) . . ?
O3 P2 O1 110.87(7) 2_665 . ?
O3 P2 O1 110.88(7) . 2_665 ?
O3 P2 O1 110.87(7) 2_665 2_665 ?
O1 P2 O1 105.6(2) . 2_665 ?
O3 P2 Na1 53.89(12) . . ?
O3 P2 Na1 53.89(12) 2_665 . ?
O1 P2 Na1 127.20(11) . . ?
O1 P2 Na1 127.20(11) 2_665 . ?
O3 Na1 O3 61.71(14) . 2_665 ?
O3 Na1 O3 137.47(9) . 4_656 ?
O3 Na1 O3 137.47(9) 2_665 4_656 ?
O3 Na1 O3 137.47(9) . 3_566 ?
O3 Na1 O3 137.47(9) 2_665 3_566 ?
O3 Na1 O3 61.71(14) 4_656 3_566 ?
O3 Na1 P2 149.14(7) . 3_566 ?
O3 Na1 P2 149.14(7) 2_665 3_566 ?
O3 Na1 P2 30.86(7) 4_656 3_566 ?
O3 Na1 P2 30.86(7) 3_566 3_566 ?
O3 Na1 P2 30.86(7) . . ?
O3 Na1 P2 30.86(7) 2_665 . ?
O3 Na1 P2 149.14(7) 4_656 . ?
O3 Na1 P2 149.14(7) 3_566 . ?
P2 Na1 P2 180.0 3_566 . ?
O3 Na1 Cl1 73.11(7) . 10_665 ?
O3 Na1 Cl1 134.82(7) 2_665 10_665 ?
O3 Na1 Cl1 78.044(17) 4_656 10_665 ?
O3 Na1 Cl1 78.044(17) 3_566 10_665 ?
P2 Na1 Cl1 76.036(16) 3_566 10_665 ?
P2 Na1 Cl1 103.964(17) . 10_665 ?
O3 Na1 Cl1 134.82(7) . 9_445 ?
O3 Na1 Cl1 73.11(7) 2_665 9_445 ?
O3 Na1 Cl1 78.044(17) 4_656 9_445 ?
O3 Na1 Cl1 78.044(17) 3_566 9_445 ?
P2 Na1 Cl1 76.036(16) 3_566 9_445 ?
P2 Na1 Cl1 103.964(17) . 9_445 ?
Cl1 Na1 Cl1 152.07(3) 10_665 9_445 ?
O3 Na1 Cl1 78.044(17) . 12_645 ?
O3 Na1 Cl1 78.044(17) 2_665 12_645 ?
O3 Na1 Cl1 134.82(7) 4_656 12_645 ?
O3 Na1 Cl1 73.11(7) 3_566 12_645 ?
P2 Na1 Cl1 103.964(16) 3_566 12_645 ?
P2 Na1 Cl1 76.036(16) . 12_645 ?
Cl1 Na1 Cl1 93.338(8) 10_665 12_645 ?
Cl1 Na1 Cl1 93.338(8) 9_445 12_645 ?
O3 Na1 Cl1 78.044(17) . 11_465 ?
O3 Na1 Cl1 78.044(17) 2_665 11_465 ?
O3 Na1 Cl1 73.11(7) 4_656 11_465 ?
O3 Na1 Cl1 134.82(7) 3_566 11_465 ?
P2 Na1 Cl1 103.964(16) 3_566 11_465 ?
P2 Na1 Cl1 76.036(16) . 11_465 ?
Cl1 Na1 Cl1 93.338(8) 10_665 11_465 ?
Cl1 Na1 Cl1 93.338(8) 9_445 11_465 ?
Cl1 Na1 Cl1 152.07(3) 12_645 11_465 ?
Co1 Cl1 Co2 101.98(3) . 12_645 ?
Co1 Cl1 Co2 101.98(3) . 10_664 ?
Co2 Cl1 Co2 85.36(4) 12_645 10_664 ?
Co1 Cl1 Co1 169.19(4) . 10_664 ?
Co2 Cl1 Co1 70.36(2) 12_645 10_664 ?
Co2 Cl1 Co1 70.36(2) 10_664 10_664 ?
Co1 Cl1 Na1 110.81(4) . 9_554 ?
Co2 Cl1 Na1 125.84(3) 12_645 9_554 ?
Co2 Cl1 Na1 125.84(3) 10_664 9_554 ?
Co1 Cl1 Na1 80.00(3) 10_664 9_554 ?
P2 O1 Co1 123.75(16) . 12_645 ?
P2 O1 Co2 121.28(8) . 9_444 ?
Co1 O1 Co2 88.23(9) 12_645 9_444 ?
P2 O1 Co2 121.28(8) . 12_645 ?
Co1 O1 Co2 88.23(9) 12_645 12_645 ?
Co2 O1 Co2 105.59(11) 9_444 12_645 ?
P1 O2 Co1 132.38(14) . . ?
P1 O2 Co2 131.00(12) . . ?
Co1 O2 Co2 93.50(9) . . ?
P2 O3 Co1 147.5(2) . . ?
P2 O3 Na1 95.26(15) . . ?
Co1 O3 Na1 117.21(13) . . ?

_refine_diff_density_max         0.610
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.097


_exptl_crystal_recrystallization_method hydrothermal
