# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_mo_d8v3467_0m-a
_database_code_depnum_ccdc_archive 'CCDC 1899691'
loop_
_audit_author_name
_audit_author_address
'Dmitri Mitcov'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2019-02-26 deposited with the CCDC.	2020-07-27 downloaded from the CCDC.
;
_audit_creation_date             2019-01-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            'Delta enantiomer'
_chemical_name_systematic        
'Sodium delta-trisoxydiacetatoholmiate(III) with sodium tetrafluoroborate'
_chemical_formula_moiety         '0.33(C36 H72 B6 F24 Ho3 Na15 O63)'
_chemical_formula_sum            'C12 H24 B2 F8 Ho Na5 O21'
_chemical_formula_weight         957.79
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   9.5798(3)
_cell_length_b                   9.5798(3)
_cell_length_c                   27.9126(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2218.42(16)
_cell_formula_units_Z            3.00006
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.502
_cell_measurement_theta_min      2.561
_shelx_estimated_absorpt_T_max   0.640
_shelx_estimated_absorpt_T_min   0.316
_exptl_absorpt_coefficient_mu    2.886
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1300 before and 0.0714 after correction. The Ratio of minimum to maximum transmission is 0.6295. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.518
_exptl_crystal_size_mid          0.464
_exptl_crystal_size_min          0.17
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            17645
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.502
_diffrn_reflns_theta_min         2.561
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                1516
_reflns_number_total             1517
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 
;
 Flack x determined using 635 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.015(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1517
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0116
_refine_ls_R_factor_gt           0.0116
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0128P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0292
_refine_ls_wR_factor_ref         0.0292
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Ho1 Ho 0.0000 0.0000 0.5000 0.00846(5) Uani 1 6 d S T P . .
O7 O -0.02481(18) -0.18879(17) 0.55801(5) 0.0142(3) Uani 1 1 d . . . . .
C4 C -0.1451(3) -0.3270(2) 0.56595(6) 0.0115(6) Uani 1 1 d . . . . .
O5 O -0.1576(2) -0.4158(2) 0.60004(5) 0.0200(3) Uani 1 1 d . . . . .
O0AA O -0.2557(2) -0.2557(2) 0.5000 0.0136(4) Uani 1 2 d S T P . .
C5 C -0.2879(3) -0.3833(2) 0.53213(7) 0.0146(4) Uani 1 1 d . . . . .
H5A H -0.3041 -0.4792 0.5140 0.018 Uiso 1 1 calc R . . . .
H5B H -0.3871 -0.4132 0.5506 0.018 Uiso 1 1 calc R . . . .
Na1 Na -0.3333 -0.6667 0.63512(4) 0.0172(2) Uani 1 3 d S T P . .
Na3 Na 0.04477(14) -0.3333 0.6667 0.0237(3) Uani 1 2 d S T P . .
F1 F 0.2630(4) -0.2460(4) 0.71873(4) 0.0265(3) Uani 1 1 d . . . . .
B3 B 0.3333 -0.3333 0.73583(11) 0.0170(6) Uani 1 3 d S T P . .
O4 O -0.1121(2) -0.5949(2) 0.69133(6) 0.0237(4) Uani 1 1 d . . . . .
F0AA F 0.3333 -0.3333 0.78531(7) 0.0302(4) Uani 1 3 d S T P . .
H4A H -0.134(4) -0.566(10) 0.7154(11) 0.057(9) Uiso 1 1 d . . . . .
H4B H -0.053(7) -0.654(7) 0.704(2) 0.108(18) Uiso 1 1 d . . . . .


_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
Ho1 O7 2.3493(14) . ?
Ho1 O7 2.3493(14) 4_556 ?
Ho1 O7 2.3493(14) 3 ?
Ho1 O7 2.3493(14) 2 ?
Ho1 O7 2.3493(14) 6_556 ?
Ho1 O7 2.3493(14) 5_556 ?
Ho1 O0AA 2.450(2) 3 ?
Ho1 O0AA 2.450(2) 2 ?
Ho1 O0AA 2.450(2) . ?
O7 C4 1.267(3) . ?
C4 O5 1.242(2) . ?
C4 C5 1.521(3) . ?
O5 Na1 2.3501(17) . ?
O5 Na3 2.5117(18) . ?
O0AA C5 1.420(2) . ?
O0AA C5 1.420(2) 6_556 ?
Na1 O5 2.3501(17) 2_445 ?
Na1 O5 2.3501(17) 3_545 ?
Na1 Na3 3.5392(8) 3_545 ?
Na1 Na3 3.5392(8) . ?
Na1 Na3 3.5392(8) 2_445 ?
Na1 O4 2.443(2) . ?
Na1 O4 2.443(2) 3_545 ?
Na1 O4 2.443(2) 2_445 ?
Na3 O5 2.5119(18) 10_446 ?
Na3 Na1 3.5393(8) 10_446 ?
Na3 F1 2.331(2) 10_446 ?
Na3 F1 2.331(2) . ?
Na3 O4 2.2902(17) 10_446 ?
Na3 O4 2.2902(17) . ?
F1 B3 1.3951(16) . ?
B3 F1 1.3951(16) 2_545 ?
B3 F1 1.3951(16) 3_655 ?
B3 F0AA 1.381(4) . ?

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
O7 Ho1 O7 77.73(5) . 2 ?
O7 Ho1 O7 88.02(7) 6_556 3 ?
O7 Ho1 O7 77.73(5) 6_556 4_556 ?
O7 Ho1 O7 128.37(7) . 6_556 ?
O7 Ho1 O7 147.03(7) . 4_556 ?
O7 Ho1 O7 147.03(7) 2 6_556 ?
O7 Ho1 O7 77.73(5) 2 3 ?
O7 Ho1 O7 88.01(7) . 5_556 ?
O7 Ho1 O7 147.03(7) 5_556 3 ?
O7 Ho1 O7 128.37(7) 2 5_556 ?
O7 Ho1 O7 88.02(7) 2 4_556 ?
O7 Ho1 O7 77.73(5) 6_556 5_556 ?
O7 Ho1 O7 77.73(5) 5_556 4_556 ?
O7 Ho1 O7 77.73(5) . 3 ?
O7 Ho1 O7 128.37(7) 3 4_556 ?
O7 Ho1 O0AA 73.52(4) 5_556 . ?
O7 Ho1 O0AA 135.99(4) 6_556 2 ?
O7 Ho1 O0AA 64.18(4) . . ?
O7 Ho1 O0AA 73.52(4) 2 3 ?
O7 Ho1 O0AA 135.99(4) 3 2 ?
O7 Ho1 O0AA 73.52(4) 6_556 3 ?
O7 Ho1 O0AA 64.18(4) 6_556 . ?
O7 Ho1 O0AA 135.99(4) 5_556 3 ?
O7 Ho1 O0AA 64.18(4) 5_556 2 ?
O7 Ho1 O0AA 64.18(4) 3 3 ?
O7 Ho1 O0AA 73.52(4) 4_556 2 ?
O7 Ho1 O0AA 64.18(4) 4_556 3 ?
O7 Ho1 O0AA 135.99(4) 2 . ?
O7 Ho1 O0AA 73.51(4) . 2 ?
O7 Ho1 O0AA 64.18(4) 2 2 ?
O7 Ho1 O0AA 73.52(4) 3 . ?
O7 Ho1 O0AA 135.99(4) . 3 ?
O7 Ho1 O0AA 135.99(4) 4_556 . ?
O0AA Ho1 O0AA 120.0 3 . ?
O0AA Ho1 O0AA 120.000(1) 3 2 ?
O0AA Ho1 O0AA 120.0 2 . ?
C4 O7 Ho1 127.89(14) . . ?
O7 C4 C5 116.68(17) . . ?
O5 C4 O7 125.1(2) . . ?
O5 C4 C5 118.1(2) . . ?
C4 O5 Na1 142.58(17) . . ?
C4 O5 Na3 123.86(16) . . ?
Na1 O5 Na3 93.37(5) . . ?
C5 O0AA Ho1 122.59(11) . . ?
C5 O0AA Ho1 122.59(11) 6_556 . ?
C5 O0AA C5 114.8(2) 6_556 . ?
O0AA C5 C4 108.49(16) . . ?
O5 Na1 O5 103.87(5) . 2_445 ?
O5 Na1 O5 103.86(5) . 3_545 ?
O5 Na1 O5 103.86(5) 3_545 2_445 ?
O5 Na1 Na3 45.11(4) 2_445 2_445 ?
O5 Na1 Na3 102.02(4) 3_545 . ?
O5 Na1 Na3 102.02(4) . 2_445 ?
O5 Na1 Na3 45.11(4) 3_545 3_545 ?
O5 Na1 Na3 143.95(4) 2_445 . ?
O5 Na1 Na3 102.02(4) 2_445 3_545 ?
O5 Na1 Na3 143.95(4) 3_545 2_445 ?
O5 Na1 Na3 45.11(4) . . ?
O5 Na1 Na3 143.95(4) . 3_545 ?
O5 Na1 O4 86.32(6) 3_545 . ?
O5 Na1 O4 86.32(6) 2_445 3_545 ?
O5 Na1 O4 164.61(7) 3_545 2_445 ?
O5 Na1 O4 164.61(7) 2_445 . ?
O5 Na1 O4 86.32(6) . 2_445 ?
O5 Na1 O4 164.61(7) . 3_545 ?
O5 Na1 O4 84.41(6) . . ?
O5 Na1 O4 84.41(5) 3_545 3_545 ?
O5 Na1 O4 84.41(5) 2_445 2_445 ?
Na3 Na1 Na3 114.025(15) 3_545 2_445 ?
Na3 Na1 Na3 114.025(14) . 2_445 ?
Na3 Na1 Na3 114.025(14) 3_545 . ?
O4 Na1 Na3 39.99(4) 2_445 2_445 ?
O4 Na1 Na3 39.99(4) . . ?
O4 Na1 Na3 76.84(4) 3_545 2_445 ?
O4 Na1 Na3 120.96(5) 3_545 . ?
O4 Na1 Na3 120.96(5) 2_445 3_545 ?
O4 Na1 Na3 76.84(5) 2_445 . ?
O4 Na1 Na3 76.84(4) . 3_545 ?
O4 Na1 Na3 120.96(5) . 2_445 ?
O4 Na1 Na3 39.99(4) 3_545 3_545 ?
O4 Na1 O4 83.19(7) . 3_545 ?
O4 Na1 O4 83.19(7) . 2_445 ?
O4 Na1 O4 83.19(7) 3_545 2_445 ?
O5 Na3 O5 104.17(9) . 10_446 ?
O5 Na3 Na1 92.60(5) . 10_446 ?
O5 Na3 Na1 92.60(5) 10_446 . ?
O5 Na3 Na1 41.52(4) . . ?
O5 Na3 Na1 41.52(4) 10_446 10_446 ?
Na1 Na3 Na1 110.18(4) . 10_446 ?
F1 Na3 O5 170.80(7) . . ?
F1 Na3 O5 83.95(5) 10_446 . ?
F1 Na3 O5 83.95(5) . 10_446 ?
F1 Na3 O5 170.79(7) 10_446 10_446 ?
F1 Na3 Na1 90.72(5) 10_446 . ?
F1 Na3 Na1 143.97(7) 10_446 10_446 ?
F1 Na3 Na1 143.96(7) . . ?
F1 Na3 Na1 90.71(5) . 10_446 ?
F1 Na3 F1 88.32(8) . 10_446 ?
O4 Na3 O5 84.11(6) . . ?
O4 Na3 O5 88.19(6) . 10_446 ?
O4 Na3 O5 88.20(6) 10_446 . ?
O4 Na3 O5 84.11(6) 10_446 10_446 ?
O4 Na3 Na1 43.28(5) 10_446 10_446 ?
O4 Na3 Na1 127.09(6) 10_446 . ?
O4 Na3 Na1 127.09(6) . 10_446 ?
O4 Na3 Na1 43.28(5) . . ?
O4 Na3 F1 88.34(8) . 10_446 ?
O4 Na3 F1 88.34(8) 10_446 . ?
O4 Na3 F1 100.69(9) . . ?
O4 Na3 F1 100.69(9) 10_446 10_446 ?
O4 Na3 O4 167.47(11) 10_446 . ?
B3 F1 Na3 127.84(18) . . ?
F1 B3 F1 108.92(13) 2_545 3_655 ?
F1 B3 F1 108.92(13) . 3_655 ?
F1 B3 F1 108.92(13) . 2_545 ?
F0AA B3 F1 110.02(13) . 3_655 ?
F0AA B3 F1 110.02(13) . 2_545 ?
F0AA B3 F1 110.01(13) . . ?
Na3 O4 Na1 96.73(6) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_mo_d8v3468_0m-fin
_database_code_depnum_ccdc_archive 'CCDC 1899692'
loop_
_audit_author_name
_audit_author_address
'Dmitri Mitcov'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2019-02-26 deposited with the CCDC.	2020-07-27 downloaded from the CCDC.
;
_audit_creation_date             2019-02-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            'Lambda enantiomer'
_chemical_name_systematic        
'Sodium lambda-trisoxydiacetatoholmiate(III) with sodium tetrafluoroborate'
_chemical_formula_moiety         '0.33(C36 H72 B6 F24 Ho3 Na15 O63)'
_chemical_formula_sum            'C12 H24 B2 F8 Ho Na5 O21'
_chemical_formula_weight         957.79
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   9.5788(10)
_cell_length_b                   9.5788(10)
_cell_length_c                   27.884(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2215.7(5)
_cell_formula_units_Z            3.00006
_cell_measurement_reflns_used    9294
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.475
_cell_measurement_theta_min      2.562
_shelx_estimated_absorpt_T_max   0.663
_shelx_estimated_absorpt_T_min   0.419
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0867 before and 0.0700 after correction. The Ratio of minimum to maximum transmission is 0.8502. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.155
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            23006
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         2.191
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1522
_reflns_number_total             1522
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 
;
 Flack x determined using 637 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.008(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0125
_refine_ls_R_factor_gt           0.0125
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0136P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0280
_refine_ls_wR_factor_ref         0.0280
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Ho1 Ho 0.0000 1.0000 1.0000 0.00860(5) Uani 1 6 d S T P . .
Na2 Na 0.3333 0.6667 0.86487(4) 0.0171(2) Uani 1 3 d S T P . .
Na5 Na 0.37818(14) 1.04485(14) 0.8333 0.0238(3) Uani 1 2 d S T P . .
O7 O 0.0000 0.7443(2) 1.0000 0.0132(4) Uani 1 2 d S T P . .
O8 O 0.16411(17) 0.97534(17) 0.94195(5) 0.0138(3) Uani 1 1 d . . . . .
C3 C 0.1815(4) 0.8544(4) 0.93406(6) 0.0119(6) Uani 1 1 d . . . . .
O5 O 0.25823(18) 0.84238(19) 0.90000(5) 0.0193(3) Uani 1 1 d . . . . .
F1 F 0.50897(14) 1.2628(3) 0.78126(4) 0.0261(3) Uani 1 1 d . . . . .
B3 B 0.6667 1.3333 0.76415(11) 0.0171(6) Uani 1 3 d S T P . .
C4 C -0.0958(3) 0.6165(2) 1.03210(7) 0.0142(4) Uani 1 1 d . . . . .
H4A H -0.0267 0.5861 1.0505 0.017 Uiso 1 1 calc R . . . .
H4B H -0.1757 0.5209 1.0139 0.017 Uiso 1 1 calc R . . . .
F0AA F 0.6667 1.3333 0.71463(6) 0.0296(4) Uani 1 3 d S T P . .
O2 O 0.4828(2) 0.8878(2) 0.80874(6) 0.0238(4) Uani 1 1 d . . . . .
H2A H 0.447(7) 0.869(3) 0.7851(10) 0.041(9) Uiso 1 1 d . . . . .
H2B H 0.585(7) 0.934(7) 0.7993(19) 0.11(2) Uiso 1 1 d . . . . .


_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
Ho1 O7 2.449(2) 2_675 ?
Ho1 O7 2.449(2) 3_465 ?
Ho1 O7 2.449(2) . ?
Ho1 O8 2.3492(14) 6_467 ?
Ho1 O8 2.3492(14) 4_677 ?
Ho1 O8 2.3492(14) 3_465 ?
Ho1 O8 2.3492(14) 5_557 ?
Ho1 O8 2.3492(14) 2_675 ?
Ho1 O8 2.3491(14) . ?
Na2 Na5 3.5390(9) . ?
Na2 Na5 3.5391(9) 2_665 ?
Na2 Na5 3.5391(9) 3_565 ?
Na2 O5 2.3496(16) 2_665 ?
Na2 O5 2.3496(16) 3_565 ?
Na2 O5 2.3496(16) . ?
Na2 O2 2.440(2) 3_565 ?
Na2 O2 2.440(2) . ?
Na2 O2 2.440(2) 2_665 ?
Na5 Na2 3.5389(9) 16_566 ?
Na5 O5 2.5118(18) . ?
Na5 O5 2.5119(18) 18_456 ?
Na5 F1 2.328(2) . ?
Na5 F1 2.328(2) 18_456 ?
Na5 O2 2.2903(17) 18_456 ?
Na5 O2 2.2903(17) . ?
O7 C4 1.421(2) . ?
O7 C4 1.421(2) 5_557 ?
O8 C3 1.269(3) . ?
C3 O5 1.241(2) . ?
C3 C4 1.517(3) 5_557 ?
F1 B3 1.3947(16) . ?
B3 F1 1.3947(16) 3_575 ?
B3 F1 1.3947(16) 2_775 ?
B3 F0AA 1.381(4) . ?
C4 C3 1.517(3) 5_557 ?

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
O7 Ho1 O7 120.000(1) 2_675 3_465 ?
O7 Ho1 O7 120.000(3) 3_465 . ?
O7 Ho1 O7 120.000(1) 2_675 . ?
O8 Ho1 O7 73.48(4) . 2_675 ?
O8 Ho1 O7 73.48(4) 4_677 . ?
O8 Ho1 O7 136.01(4) 3_465 2_675 ?
O8 Ho1 O7 136.01(4) 5_557 2_675 ?
O8 Ho1 O7 64.21(3) 5_557 . ?
O8 Ho1 O7 73.48(4) 2_675 3_465 ?
O8 Ho1 O7 64.21(4) 4_677 2_675 ?
O8 Ho1 O7 64.20(3) . . ?
O8 Ho1 O7 73.48(4) 6_467 2_675 ?
O8 Ho1 O7 73.48(4) 3_465 . ?
O8 Ho1 O7 136.01(4) . 3_465 ?
O8 Ho1 O7 136.01(4) 6_467 . ?
O8 Ho1 O7 64.21(3) 3_465 3_465 ?
O8 Ho1 O7 136.01(3) 2_675 . ?
O8 Ho1 O7 64.21(3) 6_467 3_465 ?
O8 Ho1 O7 64.21(4) 2_675 2_675 ?
O8 Ho1 O7 73.48(4) 5_557 3_465 ?
O8 Ho1 O7 136.01(4) 4_677 3_465 ?
O8 Ho1 O8 128.41(7) . 5_557 ?
O8 Ho1 O8 146.97(7) 5_557 2_675 ?
O8 Ho1 O8 146.97(7) . 6_467 ?
O8 Ho1 O8 87.98(7) 3_465 5_557 ?
O8 Ho1 O8 87.98(7) . 4_677 ?
O8 Ho1 O8 77.75(5) 4_677 5_557 ?
O8 Ho1 O8 87.98(7) 6_467 2_675 ?
O8 Ho1 O8 77.75(5) 6_467 5_557 ?
O8 Ho1 O8 77.75(5) . 3_465 ?
O8 Ho1 O8 77.75(5) . 2_675 ?
O8 Ho1 O8 77.75(5) 4_677 6_467 ?
O8 Ho1 O8 77.75(5) 3_465 2_675 ?
O8 Ho1 O8 128.41(7) 3_465 6_467 ?
O8 Ho1 O8 128.41(7) 4_677 2_675 ?
O8 Ho1 O8 146.97(7) 3_465 4_677 ?
Na5 Na2 Na5 114.038(14) 2_665 3_565 ?
Na5 Na2 Na5 114.039(14) . 3_565 ?
Na5 Na2 Na5 114.039(14) . 2_665 ?
O5 Na2 Na5 102.00(4) . 2_665 ?
O5 Na2 Na5 102.00(4) 2_665 3_565 ?
O5 Na2 Na5 143.95(4) 2_665 . ?
O5 Na2 Na5 45.12(4) 2_665 2_665 ?
O5 Na2 Na5 45.11(4) 3_565 3_565 ?
O5 Na2 Na5 45.11(4) . . ?
O5 Na2 Na5 102.01(4) 3_565 . ?
O5 Na2 Na5 143.95(4) . 3_565 ?
O5 Na2 Na5 143.95(4) 3_565 2_665 ?
O5 Na2 O5 103.85(5) . 2_665 ?
O5 Na2 O5 103.85(5) . 3_565 ?
O5 Na2 O5 103.84(5) 2_665 3_565 ?
O5 Na2 O2 164.67(7) 3_565 2_665 ?
O5 Na2 O2 84.41(5) 3_565 3_565 ?
O5 Na2 O2 164.67(7) . 3_565 ?
O5 Na2 O2 84.41(5) . . ?
O5 Na2 O2 86.30(6) 3_565 . ?
O5 Na2 O2 164.67(7) 2_665 . ?
O5 Na2 O2 86.30(6) . 2_665 ?
O5 Na2 O2 84.41(6) 2_665 2_665 ?
O5 Na2 O2 86.29(6) 2_665 3_565 ?
O2 Na2 Na5 76.85(5) 2_665 . ?
O2 Na2 Na5 121.02(5) 2_665 3_565 ?
O2 Na2 Na5 76.85(5) 3_565 2_665 ?
O2 Na2 Na5 39.99(4) . . ?
O2 Na2 Na5 76.85(5) . 3_565 ?
O2 Na2 Na5 121.02(5) 3_565 . ?
O2 Na2 Na5 121.02(5) . 2_665 ?
O2 Na2 Na5 39.98(4) 2_665 2_665 ?
O2 Na2 Na5 39.98(4) 3_565 3_565 ?
O2 Na2 O2 83.26(7) 2_665 . ?
O2 Na2 O2 83.26(7) 2_665 3_565 ?
O2 Na2 O2 83.26(7) . 3_565 ?
Na2 Na5 Na2 110.15(4) 16_566 . ?
O5 Na5 Na2 92.57(5) 18_456 . ?
O5 Na5 Na2 92.57(5) . 16_566 ?
O5 Na5 Na2 41.51(4) . . ?
O5 Na5 Na2 41.51(4) 18_456 16_566 ?
O5 Na5 O5 104.13(9) 18_456 . ?
F1 Na5 Na2 90.75(5) 18_456 . ?
F1 Na5 Na2 143.93(7) . . ?
F1 Na5 Na2 143.93(7) 18_456 16_566 ?
F1 Na5 Na2 90.75(5) . 16_566 ?
F1 Na5 O5 170.83(7) 18_456 18_456 ?
F1 Na5 O5 170.83(7) . . ?
F1 Na5 O5 83.96(5) . 18_456 ?
F1 Na5 O5 83.96(5) 18_456 . ?
F1 Na5 F1 88.33(8) . 18_456 ?
O2 Na5 Na2 127.11(6) 18_456 . ?
O2 Na5 Na2 43.20(5) . . ?
O2 Na5 Na2 127.10(6) . 16_566 ?
O2 Na5 Na2 43.20(5) 18_456 16_566 ?
O2 Na5 O5 88.24(6) 18_456 . ?
O2 Na5 O5 88.24(6) . 18_456 ?
O2 Na5 O5 84.02(6) 18_456 18_456 ?
O2 Na5 O5 84.02(6) . . ?
O2 Na5 F1 88.35(8) 18_456 . ?
O2 Na5 F1 88.35(8) . 18_456 ?
O2 Na5 F1 100.74(8) . . ?
O2 Na5 F1 100.74(8) 18_456 18_456 ?
O2 Na5 O2 167.39(12) 18_456 . ?
C4 O7 Ho1 122.60(11) . . ?
C4 O7 Ho1 122.61(11) 5_557 . ?
C4 O7 C4 114.8(2) 5_557 . ?
C3 O8 Ho1 127.65(15) . . ?
O8 C3 C4 116.91(17) . 5_557 ?
O5 C3 O8 124.8(2) . . ?
O5 C3 C4 118.2(2) . 5_557 ?
Na2 O5 Na5 93.38(5) . . ?
C3 O5 Na2 142.48(17) . . ?
C3 O5 Na5 123.93(16) . . ?
B3 F1 Na5 127.92(18) . . ?
F1 B3 F1 108.94(13) 2_775 3_575 ?
F1 B3 F1 108.94(13) 2_775 . ?
F1 B3 F1 108.94(13) 3_575 . ?
F0AA B3 F1 109.99(13) . 3_575 ?
F0AA B3 F1 110.00(13) . . ?
F0AA B3 F1 109.99(13) . 2_775 ?
O7 C4 C3 108.43(16) . 5_557 ?
Na5 O2 Na2 96.82(6) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
