# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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. 
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data_201972_cdt_d1_0m
_database_code_depnum_ccdc_archive 'CCDC 2020727'
loop_
_audit_author_name
_audit_author_address
'Qi Wu'
;Hubei Normal University
China
;
_audit_update_record             
;
2020-08-01 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_audit_creation_date             2019-07-19
_audit_creation_method           
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Bi2 F6), 0.08(H24 O12)'
_chemical_formula_sum            'Bi F3 H2 O'
_chemical_formula_weight         284.00
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
H H 0.0000 0.0000 '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      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'

_cell_length_a                   6.1202(5)
_cell_length_b                   6.1202(5)
_cell_length_c                   3.6957(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     119.88(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1060
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      40.30
_cell_measurement_theta_min      3.84
_shelx_estimated_absorpt_T_max   0.051
_shelx_estimated_absorpt_T_min   0.041
_exptl_absorpt_coefficient_mu    73.385
_exptl_absorpt_correction_T_max  0.001
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    7.867
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            801
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.677
_diffrn_reflns_theta_min         3.844
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                103
_reflns_number_total             115
_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 V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.898
_refine_diff_density_min         -1.999
_refine_diff_density_rms         0.565
_refine_ls_extinction_coef       0.061(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     12
_refine_ls_number_reflns         115
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0371
_refine_ls_restrained_S_all      1.234
_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)+(0.0391P)²+2.1235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0921
_refine_special_details          ?
_olex2_refinement_description    
; 
1. Fixed Uiso 
 At 1.5 times of: 
  All O(H,H) groups 
2. Uiso/Uaniso restraints and constraints 
Uanis(F1) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for 
terminal atoms of 0.01 
3. Others 
 Fixed Sof: H1A(0.16667) H1B(0.16667) 
 Fixed X: O1(1) 
 Fixed Y: O1(1) 
 Fixed Z: O1(0.5) 
4.a Riding coordinates: 
 O1(H1A,H1B) 
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_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
Bi1 Bi 0.3333 0.6667 0.2500 0.0241(8) Uani 1 6 d S T P . .
F1 F 0.3886(17) 0.3035(17) 0.2500 0.0076(18) Uani 1 2 d S TU P . .
O1 O 1.0000 1.0000 0.5000 0.020(4) Uani 1 6 d S TU P . .
H1A H 0.9896 0.8749 0.5981 0.030 Uiso 0.1667 1 d R . . . .
H1B H 0.8547 0.9505 0.4341 0.030 Uiso 0.1667 1 d R . . . .

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
Bi1 0.0145(8) 0.0145(8) 0.0435(13) 0.000 0.000 0.0072(4)
F1 0.006(3) 0.006(3) 0.011(4) 0.000 0.000 0.003(3)
O1 0.017(5) 0.017(5) 0.026(9) 0.000 0.000 0.009(2)

_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
Bi1 Bi1 3.6957(3) 1_554 ?
Bi1 Bi1 3.6957(3) 1_556 ?
Bi1 F1 2.456(6) 9_565 ?
Bi1 F1 2.409(9) 3_665 ?
Bi1 F1 2.456(6) 9_566 ?
Bi1 F1 2.409(9) 8_566 ?
Bi1 F1 2.409(9) . ?
Bi1 F1 2.456(6) 2 ?
Bi1 F1 2.456(6) 7_666 ?
Bi1 F1 2.456(6) 2_554 ?
Bi1 F1 2.456(6) 7_665 ?
F1 Bi1 2.456(6) 7_666 ?
F1 Bi1 2.456(6) 7_665 ?
O1 H1A 0.8201 . ?
O1 H1B 0.8202 . ?

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
Bi1 Bi1 Bi1 180.0 1_554 1_556 ?
F1 Bi1 Bi1 41.21(16) 2 1_556 ?
F1 Bi1 Bi1 90.0 . 1_556 ?
F1 Bi1 Bi1 90.000(1) 3_665 1_556 ?
F1 Bi1 Bi1 90.000(1) 8_566 1_556 ?
F1 Bi1 Bi1 138.79(16) 7_665 1_556 ?
F1 Bi1 Bi1 138.79(16) 9_565 1_556 ?
F1 Bi1 Bi1 138.79(16) 2_554 1_556 ?
F1 Bi1 Bi1 41.21(16) 7_666 1_556 ?
F1 Bi1 Bi1 41.21(16) 7_665 1_554 ?
F1 Bi1 Bi1 138.79(16) 9_566 1_554 ?
F1 Bi1 Bi1 90.000(1) 8_566 1_554 ?
F1 Bi1 Bi1 41.21(16) 9_565 1_554 ?
F1 Bi1 Bi1 41.21(16) 9_566 1_556 ?
F1 Bi1 Bi1 41.21(16) 2_554 1_554 ?
F1 Bi1 Bi1 90.000(1) 3_665 1_554 ?
F1 Bi1 Bi1 138.79(16) 2 1_554 ?
F1 Bi1 Bi1 138.79(16) 7_666 1_554 ?
F1 Bi1 Bi1 90.0 . 1_554 ?
F1 Bi1 F1 69.9(3) 3_665 9_565 ?
F1 Bi1 F1 69.6(3) 2 7_666 ?
F1 Bi1 F1 141.53(13) 9_565 7_666 ?
F1 Bi1 F1 97.6(3) 9_566 9_565 ?
F1 Bi1 F1 69.6(3) 9_566 7_666 ?
F1 Bi1 F1 131.19(17) 3_665 2_554 ?
F1 Bi1 F1 120.001(2) 8_566 . ?
F1 Bi1 F1 119.999(1) 8_566 3_665 ?
F1 Bi1 F1 131.19(16) 8_566 7_665 ?
F1 Bi1 F1 69.9(3) 8_566 2 ?
F1 Bi1 F1 71.6(3) . 2_554 ?
F1 Bi1 F1 71.6(3) . 2 ?
F1 Bi1 F1 131.19(17) 3_665 2 ?
F1 Bi1 F1 120.000(2) 3_665 . ?
F1 Bi1 F1 71.6(3) 8_566 9_566 ?
F1 Bi1 F1 141.53(13) 2_554 7_666 ?
F1 Bi1 F1 131.19(16) . 9_566 ?
F1 Bi1 F1 69.9(3) 3_665 9_566 ?
F1 Bi1 F1 69.9(3) . 7_666 ?
F1 Bi1 F1 69.9(3) . 7_665 ?
F1 Bi1 F1 141.54(13) 9_565 2 ?
F1 Bi1 F1 141.53(13) 9_566 7_665 ?
F1 Bi1 F1 69.6(3) 9_566 2 ?
F1 Bi1 F1 69.6(3) 9_565 7_665 ?
F1 Bi1 F1 69.9(3) 8_566 2_554 ?
F1 Bi1 F1 69.6(3) 2_554 7_665 ?
F1 Bi1 F1 97.6(3) 2_554 2 ?
F1 Bi1 F1 141.53(13) 2 7_665 ?
F1 Bi1 F1 71.6(3) 8_566 9_565 ?
F1 Bi1 F1 97.6(3) 7_666 7_665 ?
F1 Bi1 F1 131.19(16) 8_566 7_666 ?
F1 Bi1 F1 141.54(13) 9_566 2_554 ?
F1 Bi1 F1 69.6(3) 9_565 2_554 ?
F1 Bi1 F1 71.6(3) 3_665 7_665 ?
F1 Bi1 F1 71.6(3) 3_665 7_666 ?
F1 Bi1 F1 131.19(16) . 9_565 ?
Bi1 F1 Bi1 110.1(3) . 7_666 ?
Bi1 F1 Bi1 110.1(3) . 7_665 ?
Bi1 F1 Bi1 97.6(3) 7_666 7_665 ?
H1A O1 H1B 102.9 . . ?

_iucr_refine_instructions_details 
; 
  
    201972_cdt_d1_0m.res created by SHELXL-2014/7 
  
TITL 201972_cdtP 3_0m in P63/m 
CELL 0.71073 6.1202 6.1202 3.6957 90 90 120 
ZERR 2 0.0005 0.0005 0.0003 0 0 0 
LATT 1 
SYMM -Y+X,+X,0.5+Z 
SYMM -Y,+X-Y,+Z 
SYMM -X,-Y,0.5+Z 
SYMM +Y-X,-X,+Z 
SYMM +Y,-X+Y,0.5+Z 
SFAC Bi F H O 
UNIT 2 6 4 2 
ISOR 0.005 0.01 F1 O1 
  
L.S. 90 
PLAN  20 
SIZE 0.12 0.1 0.1 
TEMP -100 
BOND $H 
HTAB 
CONF 
fmap 2 
acta 
REM <olex2.extras> 
REM <HklSrc "%.\\201972_CDT_D1_0m.hkl"> 
REM </olex2.extras> 
  
WGHT    0.039100    2.123500 
EXTI    0.060940 
FVAR       0.26766 
BI1   1    0.333333    0.666667    0.250000    10.16667    0.01447    0.01447 = 
         0.04351    0.00000    0.00000    0.00723 
F1    2    0.388634    0.303550    0.250000    10.50000    0.00631    0.00560 = 
         0.01067    0.00000    0.00000    0.00289 
O1    4   11.000000   11.000000   10.500000    10.16667    0.01732    0.01732 = 
         0.02594    0.00000    0.00000    0.00866 
AFIX   3 
H1A   3    0.989550    0.874940    0.598130    10.16667   -1.50000 
H1B   3    0.854690    0.950540    0.434090    10.16667   -1.50000 
AFIX   0 
HKLF 4 
  
REM  201972_cdtP 3_0m in P63/m 
REM R1 =  0.0371 for     103 Fo > 4sig(Fo)  and  0.0419 for all     115 data 
REM     12 parameters refined using     12 restraints 
  
END 
  
WGHT      0.0391      2.1136 
  
REM Instructions for potential hydrogen bonds 
EQIV $1 -x+y+1, -x+1, -z+1/2 
HTAB O1 F1_$1 
EQIV $2 y+1, -x+y+1, -z+1 
HTAB O1 F1_$2 
EQIV $3 -x+1, -y+1, -z+1 
HTAB O1 F1_$3 
EQIV $4 -y+1, x-y+1, z 
HTAB O1 F1_$4 
  
REM Highest difference peak  1.898,  deepest hole -1.999,  1-sigma level  0.565 
Q1    1   1.0445  0.7418  0.7500  10.50000  0.05    1.90 
Q2    1   1.0000  1.0000  0.2500  10.16667  0.05    1.81 
Q3    1   0.3948  0.3741  0.3625  11.00000  0.05    1.69 
Q4    1   0.6961  0.9236  0.4897  11.00000  0.05    1.41 
Q5    1   0.1744  0.5192  0.2500  10.50000  0.05    1.29 
Q6    1   0.2628  0.4711  0.0325  11.00000  0.05    1.26 
Q7    1   0.2327  0.3331  0.2500  10.50000  0.05    1.26 
Q8    1   0.3333  0.6667 -0.1233  10.33333  0.05    1.21 
Q9    1   0.4909  0.3279  0.2500  10.50000  0.05    1.14 
Q10   1   0.5994  0.5596  0.1073  11.00000  0.05    1.13 
Q11   1   0.5369  0.5902  0.2500  10.50000  0.05    1.10 
Q12   1   0.4353  0.2248  0.2500  10.50000  0.05    1.09 
Q13   1   0.1455  0.5396  0.0638  11.00000  0.05    1.01 
Q14   1   0.3401  0.4929  0.2500  10.50000  0.05    0.77 
Q15   1   1.0832  0.9129  0.6296  11.00000  0.05    0.76 
Q16   1   0.9159  0.6856  0.5636  11.00000  0.05    0.44 
Q17   1   0.5250  0.4513  0.5076  11.00000  0.05    0.43 
  
  REM The information below was added by Olex2. 
  REM 
  REM R1 = 0.0371 for 103 Fo > 4sig(Fo) and 0.0419 for all 805 data 
  REM n/a parameters refined using n/a restraints 
  REM Highest difference peak 1.90, deepest hole -2.00 
  REM Mean Shift 0, Max Shift 0.000. 
  
  REM +++ Tabular Listing of Refinement Information +++ 
  REM R1_all = 0.0419 
  REM R1_gt = 0.0371 
  REM wR_ref = 0.0921 
  REM GOOF = 1.298 
  REM Shift_max = 0.000 
  REM Shift_mean = 0 
  REM Reflections_all = 805 
  REM Reflections_gt = 103 
  REM Parameters = n/a 
  REM Hole = -2.00 
  REM Peak = 1.90 
  REM Flack = n/a 
  
  
;
_olex2_submission_special_instructions 'No special instructions were received'
