# Electronic Supplementary Material (ESI) for ChemComm.
# 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_yen002
_database_code_depnum_ccdc_archive 'CCDC 2018189'
loop_
_audit_author_name
_audit_author_address
'Liling Cao'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2020-07-27 deposited with the CCDC.	2020-07-30 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         'F I O3 Zn'
_chemical_formula_sum            'F I O3 Zn'
_chemical_formula_weight         259.27

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   5.0197(4)
_cell_length_b                   5.2136(4)
_cell_length_c                   12.4572(10)
_cell_angle_alpha                90
_cell_angle_beta                 95.943(3)
_cell_angle_gamma                90
_cell_volume                     324.26(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    7255
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.311
_exptl_crystal_F_000             464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.108
_exptl_absorpt_coefficient_mu    16.948
_shelx_estimated_absorpt_T_min   0.195
_shelx_estimated_absorpt_T_max   0.262
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2022
_exptl_absorpt_correction_T_max  0.3222
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_absorpt_special_details   
; 
 The numerical absorption corrections were used for sets with
 transmission factors of 0.195 - 0.262 by SADABS (version
 2016/2). The Rint value has dropped from 0.1563 before absorption
 correction to 0.0517 after absorption correction.
;
_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8172
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.288
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             748
_reflns_number_gt                736
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0191P)²+2.4413P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         748
_refine_ls_number_parameters     43
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0565
_refine_ls_wR_factor_gt          0.0562
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_restrained_S_all      1.290
_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
I I 0.01570(6) 0.68334(6) 0.33095(2) 0.00441(13) Uani 1 1 d . . . . .
Zn Zn 0.52963(11) 0.24363(12) 0.43413(5) 0.00555(16) Uani 1 1 d . . . . .
F F 0.7341(6) -0.0777(6) 0.4748(2) 0.0085(6) Uani 1 1 d . . . . .
O1 O 0.1504(7) 0.5871(7) 0.2073(3) 0.0079(4) Uani 1 1 d . . . . .
O2 O 0.2830(7) 0.5667(7) 0.4295(3) 0.0079(4) Uani 1 1 d . . . . .
O3 O -0.2125(7) 0.4169(7) 0.3335(3) 0.0079(4) Uani 1 1 d . . . . .

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
I 0.00392(18) 0.00597(19) 0.00313(19) 0.00025(10) -0.00065(12) -0.00014(10)
Zn 0.0063(3) 0.0058(3) 0.0043(3) 0.0002(2) -0.0006(2) -0.0004(2)
F 0.0073(13) 0.0094(15) 0.0089(14) 0.0011(12) 0.0006(11) 0.0012(11)
O1 0.0084(9) 0.0098(10) 0.0052(10) -0.0005(8) -0.0014(8) -0.0002(8)
O2 0.0084(9) 0.0098(10) 0.0052(10) -0.0005(8) -0.0014(8) -0.0002(8)
O3 0.0084(9) 0.0098(10) 0.0052(10) -0.0005(8) -0.0014(8) -0.0002(8)

_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
I O3 1.803(4) . ?
I O1 1.815(4) . ?
I O2 1.827(4) . ?
Zn F 2.002(3) . ?
Zn F 2.025(3) 3_656 ?
Zn O1 2.064(4) 2_545 ?
Zn O2 2.088(4) . ?
Zn O3 2.097(4) 1_655 ?
Zn O2 2.102(4) 3_666 ?
Zn Zn 3.0556(12) 3_656 ?

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 I O1 95.45(17) . . ?
O3 I O2 98.95(16) . . ?
O1 I O2 99.56(16) . . ?
F Zn F 81.28(13) . 3_656 ?
F Zn O1 93.04(14) . 2_545 ?
F Zn O1 93.18(14) 3_656 2_545 ?
F Zn O2 165.69(14) . . ?
F Zn O2 86.55(13) 3_656 . ?
O1 Zn O2 95.14(14) 2_545 . ?
F Zn O3 100.35(13) . 1_655 ?
F Zn O3 177.15(13) 3_656 1_655 ?
O1 Zn O3 84.42(14) 2_545 1_655 ?
O2 Zn O3 92.12(14) . 1_655 ?
F Zn O2 90.81(14) . 3_666 ?
F Zn O2 90.70(14) 3_656 3_666 ?
O1 Zn O2 174.91(15) 2_545 3_666 ?
O2 Zn O2 81.79(15) . 3_666 ?
O3 Zn O2 91.61(14) 1_655 3_666 ?
F Zn Zn 40.91(9) . 3_656 ?
F Zn Zn 40.37(9) 3_656 3_656 ?
O1 Zn Zn 94.10(11) 2_545 3_656 ?
O2 Zn Zn 126.52(11) . 3_656 ?
O3 Zn Zn 141.22(11) 1_655 3_656 ?
O2 Zn Zn 91.00(10) 3_666 3_656 ?
Zn F Zn 98.72(13) . 3_656 ?
I O1 Zn 116.51(19) . 2 ?
I O2 Zn 132.8(2) . . ?
I O2 Zn 128.5(2) . 3_666 ?
Zn O2 Zn 98.22(15) . 3_666 ?
I O3 Zn 140.8(2) . 1_455 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 I O1 Zn 93.5(2) . . . 2 ?
O2 I O1 Zn -166.44(19) . . . 2 ?
O3 I O2 Zn 61.0(3) . . . . ?
O1 I O2 Zn -36.1(3) . . . . ?
O3 I O2 Zn -128.7(2) . . . 3_666 ?
O1 I O2 Zn 134.1(2) . . . 3_666 ?
O1 I O3 Zn 171.0(3) . . . 1_455 ?
O2 I O3 Zn 70.4(3) . . . 1_455 ?

_refine_diff_density_max         0.948
_refine_diff_density_min         -2.035
_refine_diff_density_rms         0.351

_shelx_res_file                  
; 
TITL yen002.res in P2(1)/n 
    yen002.res 
    created by SHELXL-2018/3 at 21:02:06 on 29-Jun-2020 
REM Old TITL yen002 in P2(1)/n 
  
REM SHELXT solution in P2(1)/n 
REM R1 0.043,  Rweak 0.003,  Alpha 0.021,  Orientation as input 
REM Formula found by SHELXT:  F4 Zn I 
  
CELL  0.71073   5.0197   5.2136  12.4572   90.000   95.943   90.000 
ZERR    4.000   0.0004   0.0004   0.0010    0.000    0.003    0.000 
LATT  1 
SYMM 1/2-X, 1/2+Y, 1/2-Z 
SFAC O F ZN I 
UNIT 12 4 4 4 
TEMP -133.150 
SIZE 0.108 0.14 0.143 
  
L.S. 10 
ACTA 
CONF 
  
EADP O1 O2 O3 
  
WGHT    0.019100    2.441300 
FVAR       0.14034 
I     4    0.015699    0.683342    0.330954    11.00000    0.00392    0.00597 = 
         0.00313    0.00025   -0.00065   -0.00014 
ZN    3    0.529630    0.243632    0.434128    11.00000    0.00629    0.00578 = 
         0.00434    0.00023   -0.00056   -0.00041 
F     2    0.734101   -0.077685    0.474818    11.00000    0.00727    0.00943 = 
         0.00888    0.00108    0.00058    0.00122 
O1    1    0.150401    0.587080    0.207343    11.00000    0.00836    0.00982 = 
         0.00522   -0.00048   -0.00140   -0.00015 
O2    1    0.282984    0.566724    0.429530    11.00000    0.00836    0.00982 = 
         0.00522   -0.00048   -0.00140   -0.00015 
O3    1   -0.212505    0.416881    0.333495    11.00000    0.00836    0.00982 = 
         0.00522   -0.00048   -0.00140   -0.00015 
HKLF 4 
  
  
  
  
REM  yen002.res in P2(1)/n 
REM wR2 = 0.056540, GooF = S = 1.28979, Restrained GooF = 1.28979 for all data 
REM R1 = 0.022894 for 736 Fo > 4sig(Fo) and 0.023344 for all 748 data 
REM 43 parameters refined using 0 restraints 
  
END 
  
WGHT      0.0191      2.4413 
  
REM Highest difference peak  0.948,  deepest hole -2.035,  1-sigma level  0.351 
Q1    1   0.4320  0.6871  0.2001  11.00000  0.05    0.95 
Q2    1  -0.1318  0.3310  0.3392  11.00000  0.05    0.92 
Q3    1  -0.4220  0.6245  0.2892  11.00000  0.05    0.84 
Q4    1   0.3830  0.4713  0.3847  11.00000  0.05    0.81 
Q5    1   0.1314  0.3494  0.4361  11.00000  0.05    0.73 
Q6    1   0.2130  0.4981  0.4582  11.00000  0.05    0.73 
Q7    1   0.7198 -0.3202  0.4021  11.00000  0.05    0.71 
Q8    1  -0.1241  0.3446  0.2197  11.00000  0.05    0.71 
Q9    1   0.6897 -0.2746  0.4145  11.00000  0.05    0.69 
Q10   1   0.3921  0.6264  0.4214  11.00000  0.05    0.67 
Q11   1   0.2041  0.7214  0.1867  11.00000  0.05    0.67 
Q12   1   0.6385 -0.1482  0.3803  11.00000  0.05    0.66 
Q13   1  -0.2907  0.6658  0.3020  11.00000  0.05    0.66 
Q14   1   0.7496 -0.3364  0.4991  11.00000  0.05    0.65 
Q15   1   0.0797  0.4528  0.1944  11.00000  0.05    0.65 
Q16   1   0.0401  0.3423  0.2625  11.00000  0.05    0.65 
Q17   1   0.3684  0.5346  0.4996  11.00000  0.05    0.65 
Q18   1   0.3928  0.8211  0.3815  11.00000  0.05    0.63 
Q19   1   0.8917 -0.0239  0.5550  11.00000  0.05    0.63 
Q20   1   0.1230  0.8340  0.1750  11.00000  0.05    0.63 
;
_shelx_res_checksum              38902
####################################################################### 
# 
# 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_yen003
_database_code_depnum_ccdc_archive 'CCDC 2018190'
loop_
_audit_author_name
_audit_author_address
'Liling Cao'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2020-07-27 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT434_yen003              
;
PROBLEM: Short Inter HL..HL Contact I       ..F               2.56 Ang.  
RESPONSE: This alert may result from the incorrect assignment
 of iodine by CheckCIF in this case. The valent of the iodine in this
 structure should be +5 instead of -1. The covalent radii of
 oxygen and iodine which are provided by SHELXL (version 2018/3) are
 0.660 and 1.330 A, respectively. The sum of covalent radii is 1.990 A,
 which is far smaller than the actural distances of I-F in the structure.
;
_vrf_DIFMX02_yen003              
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: Thie alert is accountable for the large positive electron
 density (4.30 eA-3) to the iodine atom with a distance of 0.685 A.This
 residual electron density is less than 10% of the atomic number of iodine
 and may be contributed from the lone-pair electrons of iodine, generated by
 the cut-off effect of the IAM refinement used in SHELXL (version 2018/3).
;
_vrf_PLAT987_yen003              
;
PROBLEM:  The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check  
RESPONSE: The two components of the twin were indexed with CELL_NOW
 (version 2008/4). The second twin component can be related to the
 first component by 86.6 degrees about the [1.000 0.267 0.277] axis
 in real space and about the [0.911 0.263 1.000] the reciprocal space.
 The reflections were integrated and written into a HKLF 5 file by
 SAINT (version 8.30A) implemented by APEX3 (Bruker AXS Inc., 2013).
 The Flack value here, which is 0.43(9), is actually the refined twin
 fraction. 
;
_vrf_STRVA01_yen003              
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: The two components of the twin were indexed with CELL_NOW
 (version 2008/4). The second twin component can be related to the
 first componenet by 86.6 degrees about the [1.000 0.267 0.277] axis
 in real space and about the [0.911 0.263 1.000] in the reciprocal space.
 The reflections were integrated and written into a HKLF 5 file by
 SAINT (version 8.30A) implemented in APEX3 (Bruker AXS Inc., 2013).
 The Flack value here, which is 0.43(9), is actually the refined twin
 fraction. 
;

_vrf_PLAT094_yen003              
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.89 Report
RESPONSE: Please refer to the response to DIFMX02.
;
_vrf_PLAT097_yen003              
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       4.30 eA-3  
RESPONSE: Please refer to the response to DIFMX02.
;
_vrf_PLAT431_yen003              
;
PROBLEM: Short Inter HL..A Contact  F       ..O3       .       2.74 Ang.  
RESPONSE: In this compound, there should not be any hydrogen bonds. The
 fluorine and oxygen atoms do not contact according to their distances
 and covalent radii.
;
_vrf_PLAT911_yen003              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: The alert may be related to the overflowed images during the 
 collection, which had to be deleted.
;
_vrf_PLAT914_yen003              
;
PROBLEM: No Bijvoet Pairs in FCF for Non-centro Structure     Please Check 
RESPONSE: This data set was refined as a two component twin. Therefore the
 absolute structure of the noncentrosymmetric structure was not determined.
 The Flack parameter was refined as the twin fraction. 
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cd F I O3'
_chemical_formula_sum            'Cd F I O3'
_chemical_formula_weight         306.30

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   5.5051(4)
_cell_length_b                   5.7913(4)
_cell_length_c                   10.9326(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     348.55(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    9275
_cell_measurement_theta_min      3.70
_cell_measurement_theta_max      30.54

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.837
_exptl_crystal_F_000             536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.089
_exptl_absorpt_coefficient_mu    14.987
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.294916
_exptl_absorpt_correction_T_max  0.432999
_exptl_absorpt_process_details   'TWINABS (Bruker AXS Inc. 2012)'
_exptl_absorpt_special_details   
; 
 -The numerical absorption corrections were used for sets with
 transmission factors of 0.294916 - 0.432999 by TWINABS (version
 2012/1). The Rint value has dropped from 0.3670 before absorption
 correctionto 0.0475 after absorption correction.
;
_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            651
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.727
_diffrn_reflns_theta_max         30.537
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.608
_diffrn_reflns_point_group_measured_fraction_full 0.624
_reflns_number_total             651
_reflns_number_gt                646
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.000
_reflns_Friedel_fraction_full    0.000

_reflns_special_details          
; 
 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. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component 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)+(0.0258P)²+6.0504P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0157(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
No quotients, so Flack parameter determined by classical intensity fit 
;
_refine_ls_abs_structure_Flack   0.43(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         651
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0633
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.175
_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
I I 0.02495(10) 0.40186(9) 0.11608(4) 0.00581(16) Uani 1 1 d . . . . .
Cd Cd 0.04472(12) 0.67952(11) -0.14494(5) 0.00578(17) Uani 1 1 d . . . . .
F F -0.2433(11) 0.4352(10) -0.2117(5) 0.0090(11) Uani 1 1 d . . . . .
O1 O 0.1819(13) 0.3507(12) -0.0275(6) 0.0090(13) Uani 1 1 d . . . . .
O2 O 0.2679(13) 0.5439(11) 0.2026(6) 0.0066(13) Uani 1 1 d . . . . .
O3 O -0.1228(12) 0.6611(12) 0.0527(6) 0.0080(12) Uani 1 1 d . . . . .

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
I 0.0052(2) 0.0065(2) 0.0057(2) -0.00130(17) -0.00056(19) 0.00056(19)
Cd 0.0059(3) 0.0061(3) 0.0054(3) -0.0009(2) -0.0011(2) 0.0002(2)
F 0.008(2) 0.008(2) 0.011(3) 0.000(2) -0.001(2) -0.001(2)
O1 0.011(3) 0.008(3) 0.008(3) 0.001(2) 0.007(2) 0.002(3)
O2 0.007(3) 0.005(3) 0.008(3) 0.001(2) -0.003(2) -0.002(2)
O3 0.007(3) 0.008(3) 0.009(3) 0.001(3) 0.004(2) 0.004(3)

_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
I O1 1.816(6) . ?
I O2 1.833(7) . ?
I O3 1.843(7) . ?
I Cd 3.2772(8) . ?
Cd F 2.247(6) . ?
Cd O3 2.285(7) 4_565 ?
Cd O2 2.299(7) 4_465 ?
Cd O2 2.349(7) 2_564 ?
Cd O3 2.352(6) . ?
Cd O1 2.418(7) . ?
Cd F 2.418(6) 3_554 ?

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
O1 I O2 99.9(3) . . ?
O1 I O3 91.0(3) . . ?
O2 I O3 98.6(3) . . ?
O1 I Cd 46.5(2) . . ?
O2 I Cd 101.8(2) . . ?
O3 I Cd 44.6(2) . . ?
F Cd O3 164.4(2) . 4_565 ?
F Cd O2 83.2(2) . 4_465 ?
O3 Cd O2 111.8(2) 4_565 4_465 ?
F Cd O2 74.5(2) . 2_564 ?
O3 Cd O2 100.6(3) 4_565 2_564 ?
O2 Cd O2 118.71(13) 4_465 2_564 ?
F Cd O3 89.6(2) . . ?
O3 Cd O3 85.81(13) 4_565 . ?
O2 Cd O3 91.3(2) 4_465 . ?
O2 Cd O3 143.1(2) 2_564 . ?
F Cd O1 84.1(2) . . ?
O3 Cd O1 80.4(3) 4_565 . ?
O2 Cd O1 154.3(2) 4_465 . ?
O2 Cd O1 78.8(2) 2_564 . ?
O3 Cd O1 66.3(2) . . ?
F Cd F 119.62(11) . 3_554 ?
O3 Cd F 71.1(2) 4_565 3_554 ?
O2 Cd F 72.3(2) 4_465 3_554 ?
O2 Cd F 71.3(2) 2_564 3_554 ?
O3 Cd F 143.2(2) . 3_554 ?
O1 Cd F 133.3(2) . 3_554 ?
F Cd I 87.16(15) . . ?
O3 Cd I 80.82(17) 4_565 . ?
O2 Cd I 123.95(17) 4_465 . ?
O2 Cd I 111.24(17) 2_564 . ?
O3 Cd I 33.35(16) . . ?
O1 Cd I 33.02(15) . . ?
F Cd I 151.65(14) 3_554 . ?
Cd F Cd 106.1(2) . 3_544 ?
I O1 Cd 100.5(3) . . ?
I O2 Cd 130.9(3) . 4_565 ?
I O2 Cd 116.1(3) . 2_565 ?
Cd O2 Cd 106.7(3) 4_565 2_565 ?
I O3 Cd 121.1(3) . 4_465 ?
I O3 Cd 102.1(3) . . ?
Cd O3 Cd 134.5(3) 4_465 . ?

_refine_diff_density_max         4.302
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.344

_shelx_res_file                  
; 
TITL yen003.res in P2(1)2(1)2(1) 
    yen003.res 
    created by SHELXL-2018/3 at 17:58:33 on 06-Jul-2020 
CELL 0.71073   5.5051   5.7913  10.9326  90.000  90.000  90.000 
ZERR    4.00   0.0004   0.0004   0.0007   0.000   0.000   0.000 
LATT -1 
SYMM 0.5-X, -Y, 0.5+Z 
SYMM -X, 0.5+Y, 0.5-Z 
SYMM 0.5+X, 0.5-Y, -Z 
SFAC O F CD I 
UNIT 12 4 4 4 
TEMP -133.15 
  
L.S. 10 
ACTA 
  
WGHT    0.025800    6.050400 
EXTI    0.015682 
BASF   0.02796 
FVAR       0.44438 
I     4    0.024952    0.401861    0.116077    11.00000    0.00520    0.00650 = 
         0.00574   -0.00130   -0.00056    0.00056 
CD    3    0.044721    0.679522   -0.144935    11.00000    0.00587    0.00606 = 
         0.00539   -0.00090   -0.00108    0.00023 
F     2   -0.243350    0.435220   -0.211697    11.00000    0.00773    0.00807 = 
         0.01120    0.00013   -0.00085   -0.00070 
O1    1    0.181859    0.350694   -0.027508    11.00000    0.01074    0.00803 = 
         0.00830    0.00102    0.00659    0.00213 
O2    1    0.267874    0.543930    0.202574    11.00000    0.00661    0.00484 = 
         0.00833    0.00079   -0.00341   -0.00156 
O3    1   -0.122786    0.661074    0.052696    11.00000    0.00693    0.00801 = 
         0.00912    0.00141    0.00362    0.00444 
HKLF 5 
  
  
  
  
REM  yen003.res in P2(1)2(1)2(1) 
REM wR2 = 0.063420, GooF = S = 1.17452, Restrained GooF = 1.17452 for all data 
REM R1 = 0.027165 for 646 Fo > 4sig(Fo) and 0.027443 for all 651 data 
REM 57 parameters refined using 0 restraints 
  
END 
  
WGHT      0.0258      6.0504 
  
REM Highest difference peak  4.302,  deepest hole -1.490,  1-sigma level  0.344 
Q1    1  -0.0342  0.3143  0.1459  11.00000  0.05    4.30 
Q2    1  -0.0137  0.5966 -0.1083  11.00000  0.05    4.14 
Q3    1  -0.0175  0.7664 -0.1216  11.00000  0.05    1.91 
Q4    1   0.0055  0.6411 -0.1909  11.00000  0.05    1.24 
Q5    1  -0.0570  0.4859  0.1400  11.00000  0.05    0.95 
Q6    1   0.0734  0.5990  0.1362  11.00000  0.05    0.95 
Q7    1   0.0616  0.8299 -0.0455  11.00000  0.05    0.93 
Q8    1   0.4883  0.4577  0.1195  11.00000  0.05    0.82 
Q9    1   0.0067  0.5497 -0.1909  11.00000  0.05    0.80 
Q10   1  -0.1003  0.3158 -0.1413  11.00000  0.05    0.79 
Q11   1  -0.1897  0.5774  0.0367  11.00000  0.05    0.79 
Q12   1  -0.5502  0.4770 -0.1574  11.00000  0.05    0.77 
Q13   1  -0.2456  0.2588 -0.1463  11.00000  0.05    0.75 
Q14   1  -0.4719  0.4150 -0.1041  11.00000  0.05    0.74 
Q15   1   0.1438  0.2238 -0.0250  11.00000  0.05    0.71 
Q16   1   0.2851  0.5200  0.2664  11.00000  0.05    0.71 
Q17   1  -0.0518  0.4428 -0.1581  11.00000  0.05    0.70 
Q18   1  -0.0041  0.4039  0.0766  11.00000  0.05    0.69 
Q19   1   0.0363  0.2284 -0.1597  11.00000  0.05    0.69 
Q20   1   0.2570  0.6038  0.2071  11.00000  0.05    0.67 
;
_shelx_res_checksum              61709
