# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 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_I
_database_code_depnum_ccdc_archive 'CCDC 1840536'
_audit_update_record             
;
2018-04-28 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;

_audit_creation_method           'Jana2006 Version : 29/01/2018'

_chemical_formula_sum            'C3 Ca1 Na4 O9'
_chemical_formula_weight         312.1
_chemical_absolute_configuration .

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I a -3 d'
_symmetry_space_group_name_Hall  '-I 4bd;2ab;3'
_symmetry_Int_Tables_number      230

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y+1/2,z
3 -x,y+1/2,-z+1/2
4 x,-y,-z+1/2
5 z,x,y
6 z,-x,-y+1/2
7 -z,-x+1/2,y
8 -z,x+1/2,-y+1/2
9 y,z,x
10 -y,z+1/2,-x+1/2
11 y,-z,-x+1/2
12 -y,-z+1/2,x
13 y+1/4,x+3/4,-z+3/4
14 -y+1/4,-x+1/4,-z+1/4
15 y+1/4,-x+1/4,z+3/4
16 -y+1/4,x+3/4,z+1/4
17 x+1/4,z+3/4,-y+3/4
18 -x+1/4,z+3/4,y+1/4
19 -x+1/4,-z+1/4,-y+1/4
20 x+1/4,-z+1/4,y+3/4
21 z+1/4,y+3/4,-x+3/4
22 z+1/4,-y+1/4,x+3/4
23 -z+1/4,y+3/4,x+1/4
24 -z+1/4,-y+1/4,-x+1/4
25 -x,-y,-z
26 x,y+1/2,-z
27 x,-y+1/2,z+1/2
28 -x,y,z+1/2
29 -z,-x,-y
30 -z,x,y+1/2
31 z,x+1/2,-y
32 z,-x+1/2,y+1/2
33 -y,-z,-x
34 y,-z+1/2,x+1/2
35 -y,z,x+1/2
36 y,z+1/2,-x
37 -y+1/4,-x+3/4,z+3/4
38 y+1/4,x+1/4,z+1/4
39 -y+1/4,x+1/4,-z+3/4
40 y+1/4,-x+3/4,-z+1/4
41 -x+1/4,-z+3/4,y+3/4
42 x+1/4,-z+3/4,-y+1/4
43 x+1/4,z+1/4,y+1/4
44 -x+1/4,z+1/4,-y+3/4
45 -z+1/4,-y+3/4,x+3/4
46 -z+1/4,y+1/4,-x+3/4
47 z+1/4,-y+3/4,-x+1/4
48 z+1/4,y+1/4,x+1/4
49 x+1/2,y+1/2,z+1/2
50 -x+1/2,-y,z+1/2
51 -x+1/2,y,-z
52 x+1/2,-y+1/2,-z
53 z+1/2,x+1/2,y+1/2
54 z+1/2,-x+1/2,-y
55 -z+1/2,-x,y+1/2
56 -z+1/2,x,-y
57 y+1/2,z+1/2,x+1/2
58 -y+1/2,z,-x
59 y+1/2,-z+1/2,-x
60 -y+1/2,-z,x+1/2
61 y+3/4,x+1/4,-z+1/4
62 -y+3/4,-x+3/4,-z+3/4
63 y+3/4,-x+3/4,z+1/4
64 -y+3/4,x+1/4,z+3/4
65 x+3/4,z+1/4,-y+1/4
66 -x+3/4,z+1/4,y+3/4
67 -x+3/4,-z+3/4,-y+3/4
68 x+3/4,-z+3/4,y+1/4
69 z+3/4,y+1/4,-x+1/4
70 z+3/4,-y+3/4,x+1/4
71 -z+3/4,y+1/4,x+3/4
72 -z+3/4,-y+3/4,-x+3/4
73 -x+1/2,-y+1/2,-z+1/2
74 x+1/2,y,-z+1/2
75 x+1/2,-y,z
76 -x+1/2,y+1/2,z
77 -z+1/2,-x+1/2,-y+1/2
78 -z+1/2,x+1/2,y
79 z+1/2,x,-y+1/2
80 z+1/2,-x,y
81 -y+1/2,-z+1/2,-x+1/2
82 y+1/2,-z,x
83 -y+1/2,z+1/2,x
84 y+1/2,z,-x+1/2
85 -y+3/4,-x+1/4,z+1/4
86 y+3/4,x+3/4,z+3/4
87 -y+3/4,x+3/4,-z+1/4
88 y+3/4,-x+1/4,-z+3/4
89 -x+3/4,-z+1/4,y+1/4
90 x+3/4,-z+1/4,-y+3/4
91 x+3/4,z+3/4,y+3/4
92 -x+3/4,z+3/4,-y+1/4
93 -z+3/4,-y+1/4,x+1/4
94 -z+3/4,y+3/4,-x+1/4
95 z+3/4,-y+1/4,-x+3/4
96 z+3/4,y+3/4,x+3/4

_cell_length_a                   14.5770(5)
_cell_length_b                   14.5770(5)
_cell_length_c                   14.5770(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3097.45(18)

_cell_formula_units_Z            16

_cell_measurement_reflns_used    9688
_cell_measurement_theta_min      3.38
_cell_measurement_theta_max      29.19
_cell_measurement_temperature    293

_exptl_crystal_density_diffrn    2.6768
_exptl_crystal_F_000             2464

_exptl_absorpt_coefficient_mu    1.075
_exptl_crystal_description       irregular
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_colour            colourless
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  1

_diffrn_ambient_temperature      293
_diffrn_source                   'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_detector                 'image plate'
_diffrn_measurement_method       'ω scans'

_diffrn_reflns_number            53530
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_full        29.26
_diffrn_measured_fraction_theta_max 1
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_av_unetI/netI     0.0045
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20

_diffrn_radiation_probe          X-ray

_reflns_number_total             354
_reflns_number_gt                265
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_gt          0.0927
_refine_ls_R_factor_all          0.0671
_refine_ls_wR_factor_ref         0.0965
_refine_ls_goodness_of_fit_ref   2.54
_refine_ls_goodness_of_fit_gt    2.87
_refine_ls_number_reflns         354
_refine_ls_number_parameters     31
_refine_ls_number_restraints     0
_refine_ls_number_constraints    9
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_extinction_coef       500(400)

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Ca 0.2262 0.3064 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Na 0.0362 0.0249 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0 0 0 Uani 0.0459(3) 16 0.517(7) d . . .
Na1 Na 0 0 0 Uani 0.0459(3) 16 0.483(7) d . . .
Ca2 Ca 0.25 -0.00302(7) 0 Uani 0.0312(4) 48 0.1609 d . . .
Na2 Na 0.25 -0.00302(7) 0 Uani 0.0312(4) 48 0.8391 d . . .
Na3 Na 0.125 0.125 0.125 Uani 0.0228(3) 16 1 d . . .
O1 O 0.11436(11) 0.11915(9) -0.02977(10) Uani 0.0431(6) 96 1 d . . .
O2 O 0.07584(9) 0.125 -0.17416(9) Uani 0.0531(8) 48 1 d . . .
C1 C 0.13620(12) 0.125 -0.11380(12) Uani 0.0126(5) 48 1 d . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ca1 O1 . . 2.4462(15) ?
Ca1 O1 . 5_555 2.4462(15) ?
Ca1 O1 . 9_555 2.4462(15) ?
Ca1 O1 . 25_555 2.4462(15) ?
Ca1 O1 . 29_555 2.4462(15) ?
Ca1 O1 . 33_555 2.4462(15) ?
Na1 O1 . . 2.4462(15) ?
Na1 O1 . 5_555 2.4462(15) ?
Na1 O1 . 9_555 2.4462(15) ?
Na1 O1 . 25_555 2.4462(15) ?
Na1 O1 . 29_555 2.4462(15) ?
Na1 O1 . 33_555 2.4462(15) ?
Ca2 O1 . . 2.6963(16) ?
Ca2 O1 . 51_555 2.6963(16) ?
Ca2 O1 . 9_555 2.5630(15) ?
Ca2 O1 . 58_555 2.5630(15) ?
Ca2 O2 . 29_555 2.3809(10) ?
Ca2 O2 . 80_555 2.3809(10) ?
Na2 O1 . . 2.6963(16) ?
Na2 O1 . 51_555 2.6963(16) ?
Na2 O1 . 9_555 2.5630(15) ?
Na2 O1 . 58_555 2.5630(15) ?
Na2 O2 . 29_555 2.3809(10) ?
Na2 O2 . 80_555 2.3809(10) ?
Na3 O1 . . 2.2630(15) ?
Na3 O1 . 5_555 2.2630(15) ?
Na3 O1 . 9_555 2.2630(15) ?
Na3 O1 . 14_555 2.2630(15) ?
Na3 O1 . 19_555 2.2630(15) ?
Na3 O1 . 24_555 2.2630(15) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ca1 O1 . . 5_555 76.29(5) ?
O1 Ca1 O1 . . 9_555 76.29(5) ?
O1 Ca1 O1 . . 25_555 180.0(5) ?
O1 Ca1 O1 . . 29_555 103.71(5) ?
O1 Ca1 O1 . . 33_555 103.71(5) ?
O1 Ca1 O1 5_555 . 9_555 76.29(5) ?
O1 Ca1 O1 5_555 . 25_555 103.71(5) ?
O1 Ca1 O1 5_555 . 29_555 180.0(5) ?
O1 Ca1 O1 5_555 . 33_555 103.71(5) ?
O1 Ca1 O1 9_555 . 25_555 103.71(5) ?
O1 Ca1 O1 9_555 . 29_555 103.71(5) ?
O1 Ca1 O1 9_555 . 33_555 180.0(5) ?
O1 Ca1 O1 25_555 . 29_555 76.29(5) ?
O1 Ca1 O1 25_555 . 33_555 76.29(5) ?
O1 Ca1 O1 29_555 . 33_555 76.29(5) ?
O1 Na1 O1 . . 5_555 76.29(5) ?
O1 Na1 O1 . . 9_555 76.29(5) ?
O1 Na1 O1 . . 25_555 180.0(5) ?
O1 Na1 O1 . . 29_555 103.71(5) ?
O1 Na1 O1 . . 33_555 103.71(5) ?
O1 Na1 O1 5_555 . 9_555 76.29(5) ?
O1 Na1 O1 5_555 . 25_555 103.71(5) ?
O1 Na1 O1 5_555 . 29_555 180.0(5) ?
O1 Na1 O1 5_555 . 33_555 103.71(5) ?
O1 Na1 O1 9_555 . 25_555 103.71(5) ?
O1 Na1 O1 9_555 . 29_555 103.71(5) ?
O1 Na1 O1 9_555 . 33_555 180.0(5) ?
O1 Na1 O1 25_555 . 29_555 76.29(5) ?
O1 Na1 O1 25_555 . 33_555 76.29(5) ?
O1 Na1 O1 29_555 . 33_555 76.29(5) ?
O1 Ca2 O1 . . 51_555 97.32(5) ?
O1 Ca2 O1 . . 9_555 70.09(5) ?
O1 Ca2 O1 . . 58_555 122.79(5) ?
O1 Ca2 O2 . . 29_555 80.26(5) ?
O1 Ca2 O2 . . 80_555 139.30(4) ?
O1 Ca2 O1 51_555 . 9_555 122.79(5) ?
O1 Ca2 O1 51_555 . 58_555 70.09(5) ?
O1 Ca2 O2 51_555 . 29_555 139.30(4) ?
O1 Ca2 O2 51_555 . 80_555 80.26(5) ?
O1 Ca2 O1 9_555 . 58_555 162.50(6) ?
O1 Ca2 O2 9_555 . 29_555 94.84(5) ?
O1 Ca2 O2 9_555 . 80_555 77.29(4) ?
O1 Ca2 O2 58_555 . 29_555 77.29(4) ?
O1 Ca2 O2 58_555 . 80_555 94.84(5) ?
O2 Ca2 O2 29_555 . 80_555 127.05(6) ?
O1 Na2 O1 . . 51_555 97.32(5) ?
O1 Na2 O1 . . 9_555 70.09(5) ?
O1 Na2 O1 . . 58_555 122.79(5) ?
O1 Na2 O2 . . 29_555 80.26(5) ?
O1 Na2 O2 . . 80_555 139.30(4) ?
O1 Na2 O1 51_555 . 9_555 122.79(5) ?
O1 Na2 O1 51_555 . 58_555 70.09(5) ?
O1 Na2 O2 51_555 . 29_555 139.30(4) ?
O1 Na2 O2 51_555 . 80_555 80.26(5) ?
O1 Na2 O1 9_555 . 58_555 162.50(6) ?
O1 Na2 O2 9_555 . 29_555 94.84(5) ?
O1 Na2 O2 9_555 . 80_555 77.29(4) ?
O1 Na2 O2 58_555 . 29_555 77.29(4) ?
O1 Na2 O2 58_555 . 80_555 94.84(5) ?
O2 Na2 O2 29_555 . 80_555 127.05(6) ?
O1 Na3 O1 . . 5_555 83.77(5) ?
O1 Na3 O1 . . 9_555 83.77(5) ?
O1 Na3 O1 . . 14_555 177.50(5) ?
O1 Na3 O1 . . 19_555 94.58(5) ?
O1 Na3 O1 . . 24_555 97.94(6) ?
O1 Na3 O1 5_555 . 9_555 83.77(5) ?
O1 Na3 O1 5_555 . 14_555 94.58(5) ?
O1 Na3 O1 5_555 . 19_555 97.94(6) ?
O1 Na3 O1 5_555 . 24_555 177.50(5) ?
O1 Na3 O1 9_555 . 14_555 97.94(6) ?
O1 Na3 O1 9_555 . 19_555 177.50(5) ?
O1 Na3 O1 9_555 . 24_555 94.58(5) ?
O1 Na3 O1 14_555 . 19_555 83.77(5) ?
O1 Na3 O1 14_555 . 24_555 83.77(5) ?
O1 Na3 O1 19_555 . 24_555 83.77(5) ?
