# 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_BF_phase_1
_database_code_depnum_ccdc_archive 'CCDC 2255386'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_BF_phase_1          
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.05
RESPONSE:  The value is 0.07 i.e. > 0.05 but see  V. K. Pecharsky and P. Y. Zayalij Fundamentals of Powder  Diffraction and Structural Characterization of materials 2nd edition  2009 Springer p 641 footnote 22 IUCR imposes the requirement shift/error  < 0.05  for single crystal data but for Rietveld fits shift/error <0.1 are satisfactory.  IUCR in fact do not require shift/su_max for  powder data
;
_vrf_PLAT080_BF_phase_1          
;
PROBLEM: Maximum Shift/Error ............................       0.07 Why ?
RESPONSE:  The value is 0.07 i.e. > 0.05 but see  V. K. Pecharsky and P. Y. Zayalij Fundamentals of Powder  Diffraction and Structural Characterization of materials 2nd edition  2009 Springer p 641 footnote 22 IUCR imposes the requirement shift/error  < 0.05  for single crystal data but for Rietveld fits shift/error <0.1 are satisfactory.  IUCR in fact do not require shift/su_max for  powder data
;
# Added during the CSD deposition process: Tuesday 11 April 2023 02:18 PM
# end Validation Reply Form


_pd_block_id                     2019-09-05T22:59|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-05T22:59|BF_H_01|WGM|PEARL



#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products


_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?


_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.5689(7)
_cell_length_b                   7.9658(5)
_cell_length_c                   4.33861(30)
_cell_angle_alpha                90.0
_cell_angle_beta                 96.222(8)
_cell_angle_gamma                90.0
_cell_volume                     500.54(4)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_exptl_crystal_density_diffrn    2.792
_diffrn_measurement_pressure     637000
_pd_char_colour                  orange
_diffrn_radiation_type           neutron
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_pd_prep_pressure                637000

_pd_proc_ls_prof_R_factor        0.0317
_pd_proc_ls_prof_wR_factor       0.0268
_pd_proc_ls_prof_wR_expected     0.0248
_refine_ls_R_Fsqd_factor         0.20507

_refine_ls_shift/su_max          0.07
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.10
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2436(8) 0.5 0.7240(27) 1.0 Uiso 0.0173(13) 4
Cl Cl 0.3938(4) 0.5 0.5637(16) 1.0 Uiso 0.0347(26) 4
O O 0.0772(7) 0.5 -0.1711(20) 1.0 Uiso 0.033(4) 4
C C 0.05163(19) 0.6481(6) -0.0130(11) 1.0 Uiso 0.0509(30) 8
D D1 0.0886(5) 0.6537(10) 0.2206(16) 1.0 Uiso 0.0639(33) 8
D D2 0.0699(5) 0.7570(8) -0.1447(18) 1.0 Uiso 0.0639(33) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.366(13) . 1_555 N
I O 2.515(14) . 1_556 N
Cl I 2.366(13) . 1_555 N
Cl Cl 3.203(12) . 2_656 N
O I 2.515(14) . 1_554 N
O C 1.434(5) . 1_555 N
O C 1.434(5) . -2_565 N
O D2 2.054(6) . 1_555 N
O D2 2.054(6) . -2_565 N
C O 1.434(5) . 1_555 N
C C 1.521(5) . 2_555 N
C D1 1.096(6) . 1_555 N
C D2 1.087(6) . 1_555 N
D1 C 1.096(6) . 1_555 N
D1 D2 1.780(8) . 1_555 N
D2 O 2.054(6) . 1_555 N
D2 C 1.087(6) . 1_555 N
D2 D1 1.780(8) . 1_555 N


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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.4(7) 1_555 . 1_556 N
I Cl Cl 172.9(5) 1_555 . 2_656 N
I O C 113.1(4) 1_554 . 1_555 N
I O C 113.1(4) 1_554 . -2_565 N
C O C 110.7(5) 1_555 . -2_565 N
O C C 110.3(4) 1_555 . 2_555 N
O C D1 110.4(5) 1_555 . 1_555 N
O C D2 108.3(4) 1_555 . 1_555 N
C C D1 108.8(5) 2_555 . 1_555 N
C C D2 109.8(4) 2_555 . 1_555 N
D1 C D2 109.3(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2255387'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_BF_phase_1          
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.05
RESPONSE:  The value is 0.06 i.e. > 0.05 but see  V. K. Pecharsky and P. Y. Zayalij Fundamentals of Powder  Diffraction and Structural Characterization of materials 2nd edition  2009 Springer p 641 footnote 22 IUCR imposes the requirement shift/error  < 0.05  for single crystal data but for Rietveld fits shift/error <0.1 are satisfactory.  IUCR in fact do not require shift/su_max for  powder data
;
_vrf_PLAT080_BF_phase_1          
;
PROBLEM: Maximum Shift/Error ............................       0.06 Why ?
RESPONSE:  The value is 0.06 i.e. > 0.05 but see  V. K. Pecharsky and P. Y. Zayalij Fundamentals of Powder  Diffraction and Structural Characterization of materials 2nd edition  2009 Springer p 641 footnote 22 IUCR imposes the requirement shift/error  < 0.05  for single crystal data but for Rietveld fits shift/error <0.1 are satisfactory.  IUCR in fact do not require shift/su_max for  powder data
;
# Added during the CSD deposition process: Tuesday 11 April 2023 02:18 PM
# end Validation Reply Form


_pd_block_id                     2019-09-05T23:08|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-05T23:08|BF_H_01|WGM|PEARL



#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products


_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?


_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.5397(8)
_cell_length_b                   7.9433(6)
_cell_length_c                   4.2871(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 96.428(10)
_cell_angle_gamma                90.0
_cell_volume                     492.02(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_diffrn_radiation_type           neutron
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    2.851
_diffrn_measurement_pressure     832000

_pd_prep_cool_rate               ?
_pd_prep_pressure                832000
_refine_ls_shift/su_max          0.06
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   0.98
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0397
_pd_proc_ls_prof_wR_factor       0.0342
_pd_proc_ls_prof_wR_expected     0.0354
_refine_ls_R_Fsqd_factor         0.23884

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2451(9) 0.5 0.7252(32) 1.0 Uiso 0.0249(18) 4
Cl Cl 0.3949(6) 0.5 0.5649(20) 1.0 Uiso 0.050(4) 4
O O 0.0763(7) 0.5 -0.1776(21) 1.0 Uiso 0.037(5) 4
C C 0.05119(19) 0.6496(6) -0.0144(12) 1.0 Uiso 0.058(4) 8
D D1 0.0888(5) 0.6526(11) 0.2200(19) 1.0 Uiso 0.067(4) 8
D D2 0.0695(6) 0.7607(8) -0.1470(20) 1.0 Uiso 0.067(4) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.356(16) . 1_555 N
I O 2.535(17) . 1_556 N
Cl I 2.356(16) . 1_555 N
Cl Cl 3.168(15) . 2_656 N
O I 2.535(17) . 1_554 N
O C 1.446(5) . 1_555 N
O C 1.446(5) . -2_565 N
C O 1.446(5) . 1_555 N
C C 1.507(5) . 2_555 N
C D1 1.089(6) . 1_555 N
C D2 1.099(5) . 1_555 N
D1 C 1.089(6) . 1_555 N
D1 D2 1.787(8) . 1_555 N
D2 C 1.099(5) . 1_555 N
D2 D1 1.787(8) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 172.6(7) 1_555 . 1_556 N
I Cl Cl 173.2(7) 1_555 . 2_656 N
I O C 112.4(5) 1_554 . 1_555 N
I O C 112.4(5) 1_554 . -2_565 N
C O C 110.5(5) 1_555 . -2_565 N
O C C 110.2(4) 1_555 . 2_555 N
O C D1 109.7(5) 1_555 . 1_555 N
O C D2 108.7(4) 1_555 . 1_555 N
C C D1 108.8(5) 2_555 . 1_555 N
C C D2 109.9(4) 2_555 . 1_555 N
D1 C D2 109.5(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_B3B_phase_1
_database_code_depnum_ccdc_archive 'CCDC 2255389'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-09T22:55|B3B_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-09T22:55|B3B_H_01|WGM|PEARL



#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?

_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.5144(6)
_cell_length_b                   7.9271(5)
_cell_length_c                   4.25044(29)
_cell_angle_alpha                90.0
_cell_angle_beta                 96.570(8)
_cell_angle_gamma                90.0
_cell_volume                     485.83(4)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_pd_prep_pressure                989000
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.10
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    2.877
_diffrn_measurement_pressure     989000

_pd_proc_ls_prof_R_factor        0.0319
_pd_proc_ls_prof_wR_factor       0.0271
_pd_proc_ls_prof_wR_expected     0.0252
_refine_ls_R_Fsqd_factor         0.18846

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2440(7) 0.5 0.7292(27) 1.0 Uiso 0.0228(14) 4
Cl Cl 0.3957(4) 0.5 0.5680(16) 1.0 Uiso 0.0456(29) 4
O O 0.0768(6) 0.5 -0.1757(19) 1.0 Uiso 0.028(4) 4
C C 0.05178(19) 0.6491(6) -0.0129(11) 1.0 Uiso 0.0448(27) 8
D D1 0.0885(5) 0.6505(10) 0.2248(17) 1.0 Uiso 0.0568(31) 8
D D2 0.0711(5) 0.7613(8) -0.1427(17) 1.0 Uiso 0.0568(31) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.380(13) . 1_555 N
I O 2.506(14) . 1_556 N
Cl I 2.380(13) . 1_555 N
Cl Cl 3.147(12) . 2_656 N
Cl D2 2.698(8) . 102_545 N
Cl D2 2.698(8) . -101_565 N
O I 2.506(14) . 1_554 N
O C 1.437(5) . 1_555 N
O C 1.437(5) . -2_565 N
O D1 2.070(8) . 1_555 N
O D1 2.070(8) . -2_565 N
O D2 2.078(6) . 1_555 N
O D2 2.078(6) . -2_565 N
C O 1.437(5) . 1_555 N
C C 1.520(5) . 2_555 N
C D1 1.087(6) . 1_555 N
C D1 2.129(7) . 2_555 N
C D2 1.100(5) . 1_555 N
C D2 2.164(7) . 2_555 N
D1 O 2.070(8) . 1_555 N
D1 C 1.087(6) . 1_555 N
D1 C 2.129(7) . 2_555 N
D1 D1 2.386(16) . -2_565 N
D1 D2 1.784(8) . 1_555 N
D2 Cl 2.698(8) . 102_555 N
D2 O 2.078(6) . 1_555 N
D2 C 1.100(5) . 1_555 N
D2 C 2.164(7) . 2_555 N
D2 D1 1.784(8) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 172.6(6) 1_555 . 1_556 N
I Cl Cl 173.9(5) 1_555 . 2_656 N
I Cl D2 115.78(28) 1_555 . 102_545 N
I Cl D2 115.78(28) 1_555 . -101_565 N
Cl Cl D2 68.15(20) 2_656 . 102_545 N
Cl Cl D2 68.15(20) 2_656 . -101_565 N
D2 Cl D2 89.08(33) 102_545 . -101_565 N
I O C 112.3(4) 1_554 . 1_555 N
I O C 112.3(4) 1_554 . -2_565 N
I O D1 98.2(5) 1_554 . 1_555 N
I O D1 98.2(5) 1_554 . -2_565 N
I O D2 93.27(32) 1_554 . 1_555 N
I O D2 93.27(32) 1_554 . -2_565 N
C O C 110.7(5) 1_555 . -2_565 N
C O D1 29.70(22) 1_555 . 1_555 N
C O D1 94.6(5) 1_555 . -2_565 N
C O D2 29.96(19) 1_555 . 1_555 N
C O D2 140.7(5) 1_555 . -2_565 N
C O D1 94.6(5) -2_565 . 1_555 N
C O D1 29.70(22) -2_565 . -2_565 N
C O D2 140.7(5) -2_565 . 1_555 N
C O D2 29.96(19) -2_565 . -2_565 N
D1 O D1 70.4(5) 1_555 . -2_565 N
D1 O D2 50.96(24) 1_555 . 1_555 N
D1 O D2 121.3(5) 1_555 . -2_565 N
D1 O D2 121.3(5) -2_565 . 1_555 N
D1 O D2 50.96(24) -2_565 . -2_565 N
D2 O D2 170.6(6) 1_555 . -2_565 N
O C C 109.9(4) 1_555 . 2_555 N
O C D1 109.4(5) 1_555 . 1_555 N
O C D1 94.7(5) 1_555 . 2_555 N
O C D2 109.3(4) 1_555 . 1_555 N
O C D2 138.4(4) 1_555 . 2_555 N
C C D1 108.4(5) 2_555 . 1_555 N
C C D1 28.96(23) 2_555 . 2_555 N
C C D2 110.4(4) 2_555 . 1_555 N
C C D2 28.46(18) 2_555 . 2_555 N
D1 C D1 137.38(33) 1_555 . 2_555 N
D1 C D2 109.4(5) 1_555 . 1_555 N
D1 C D2 92.6(4) 1_555 . 2_555 N
D1 C D2 94.0(5) 2_555 . 1_555 N
D1 C D2 49.11(23) 2_555 . 2_555 N
D2 C D2 95.1(5) 1_555 . 2_555 N
O D1 C 40.91(34) 1_555 . 1_555 N
O D1 C 70.41(34) 1_555 . 2_555 N
O D1 D1 54.79(27) 1_555 . -2_565 N
O D1 D2 64.77(30) 1_555 . 1_555 N
C D1 C 42.61(33) 1_555 . 2_555 N
C D1 D1 89.4(4) 1_555 . -2_565 N
C D1 D2 35.54(29) 1_555 . 1_555 N
C D1 D1 89.70(22) 2_555 . -2_565 N
C D1 D2 66.44(32) 2_555 . 1_555 N
D1 D1 D2 119.5(4) -2_565 . 1_555 N
Cl D2 O 130.0(4) 102_555 . 1_555 N
Cl D2 C 168.1(5) 102_555 . 1_555 N
Cl D2 C 135.2(4) 102_555 . 2_555 N
Cl D2 D1 156.0(5) 102_555 . 1_555 N
O D2 C 40.73(27) 1_555 . 1_555 N
O D2 C 69.58(28) 1_555 . 2_555 N
O D2 D1 64.27(32) 1_555 . 1_555 N
C D2 C 41.18(30) 1_555 . 2_555 N
C D2 D1 35.07(28) 1_555 . 1_555 N
C D2 D1 64.45(31) 2_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2255388'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-05T23:09|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-05T23:09|BF_H_01|WGM|PEARL



#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?

_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products


_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?


_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.5299(8)
_cell_length_b                   7.9373(7)
_cell_length_c                   4.27030(35)
_cell_angle_alpha                90.0
_cell_angle_beta                 96.457(9)
_cell_angle_gamma                90.0
_cell_volume                     489.36(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                902000
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   0.98
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      295
_cell_measurement_temperature    295
_pd_char_colour                  orange
_diffrn_radiation_type           neutron
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    2.856
_diffrn_measurement_pressure     902000


_pd_proc_ls_prof_R_factor        0.0412
_pd_proc_ls_prof_wR_factor       0.0341
_pd_proc_ls_prof_wR_expected     0.0355
_refine_ls_R_Fsqd_factor         0.19297

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2459(10) 0.5 0.7201(33) 1.0 Uiso 0.0175(16) 4
Cl Cl 0.3943(5) 0.5 0.5632(19) 1.0 Uiso 0.0349(33) 4
O O 0.0777(7) 0.5 -0.1757(22) 1.0 Uiso 0.028(5) 4
C C 0.05165(19) 0.6499(6) -0.0135(12) 1.0 Uiso 0.049(4) 8
D D1 0.0892(5) 0.6525(11) 0.2220(19) 1.0 Uiso 0.056(4) 8
D D2 0.0707(5) 0.7606(8) -0.1446(19) 1.0 Uiso 0.056(4) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.329(17) . 1_555 N
I O 2.533(17) . 1_556 N
Cl I 2.329(17) . 1_555 N
Cl Cl 3.178(15) . 2_656 N
O I 2.533(17) . 1_554 N
O C 1.449(5) . 1_555 N
O C 1.449(5) . -2_565 N
C O 1.449(5) . 1_555 N
C C 1.518(5) . 2_555 N
C D1 1.089(6) . 1_555 N
C D2 1.094(5) . 1_555 N
D1 C 1.089(6) . 1_555 N
D1 D2 1.779(8) . 1_555 N
D2 C 1.094(5) . 1_555 N
D2 D1 1.779(8) . 1_555 N


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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.4(8) 1_555 . 1_556 N
I Cl Cl 173.1(6) 1_555 . 2_656 N
I O C 113.2(5) 1_554 . 1_555 N
I O C 113.2(5) 1_554 . -2_565 N
C O C 110.5(5) 1_555 . -2_565 N
O C C 110.5(4) 1_555 . 2_555 N
O C D1 109.0(5) 1_555 . 1_555 N
O C D2 108.7(4) 1_555 . 1_555 N
C C D1 109.1(5) 2_555 . 1_555 N
C C D2 110.4(4) 2_555 . 1_555 N
D1 C D2 109.2(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2255390'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-06T09:23|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-06T09:23|BF_H_01|WGM|PEARL


#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products


_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?



_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.5013(8)
_cell_length_b                   7.9175(7)
_cell_length_c                   4.2297(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 96.647(10)
_cell_angle_gamma                90.0
_cell_volume                     482.36(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.01
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    2.897
_diffrn_measurement_pressure     115000

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0449
_pd_proc_ls_prof_wR_factor       0.0356
_pd_proc_ls_prof_wR_expected     0.0357
_refine_ls_R_Fsqd_factor         0.18900

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2438(9) 0.5 0.7254(34) 1.0 Uiso 0.0253(18) 4
Cl Cl 0.3963(6) 0.5 0.5639(20) 1.0 Uiso 0.051(4) 4
O O 0.0768(7) 0.5 -0.1799(22) 1.0 Uiso 0.028(5) 4
C C 0.05183(20) 0.6495(6) -0.0143(12) 1.0 Uiso 0.0430(33) 8
D D1 0.0892(5) 0.6499(12) 0.2247(19) 1.0 Uiso 0.061(4) 8
D D2 0.0711(5) 0.7624(9) -0.1424(20) 1.0 Uiso 0.061(4) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0



# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.389(17) . 1_555 N
I O 2.500(17) . 1_556 N
Cl I 2.389(17) . 1_555 N
Cl Cl 3.118(16) . 2_656 N
Cl D2 2.671(9) . 102_545 N
Cl D2 2.671(9) . -101_565 N
O I 2.500(17) . 1_554 N
O C 1.443(5) . 1_555 N
O C 1.443(5) . -2_565 N
C O 1.443(5) . 1_555 N
C C 1.522(5) . 2_555 N
C D1 1.090(6) . 1_555 N
C D2 1.098(6) . 1_555 N
D1 C 1.090(6) . 1_555 N
D1 D2 1.783(8) . 1_555 N
D2 Cl 2.671(9) . 102_555 N
D2 C 1.098(6) . 1_555 N
D2 D1 1.783(8) . 1_555 N


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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 172.7(7) 1_555 . 1_556 N
I Cl Cl 173.4(6) 1_555 . 2_656 N
I O C 112.3(5) 1_554 . 1_555 N
I O C 112.3(5) 1_554 . -2_565 N
C O C 110.3(5) 1_555 . -2_565 N
O C C 110.1(4) 1_555 . 2_555 N
O C D1 109.1(5) 1_555 . 1_555 N
O C D2 109.6(4) 1_555 . 1_555 N
C C D1 108.4(5) 2_555 . 1_555 N
C C D2 110.5(4) 2_555 . 1_555 N
D1 C D2 109.1(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_B3B_phase_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2255391'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-09T23:03|B3B_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-09T23:03|B3B_H_01|WGM|pearl


#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?


_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.4784(7)
_cell_length_b                   7.9013(5)
_cell_length_c                   4.20249(30)
_cell_angle_alpha                90.0
_cell_angle_beta                 96.782(8)
_cell_angle_gamma                90.0
_cell_volume                     477.39(4)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.12
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    2.928
_diffrn_measurement_pressure     1256000

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0333
_pd_proc_ls_prof_wR_factor       0.0278
_pd_proc_ls_prof_wR_expected     0.0254
_refine_ls_R_Fsqd_factor         0.16946


loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2423(7) 0.5 0.7166(28) 1.0 Uiso 0.0226(14) 4
Cl Cl 0.3965(4) 0.5 0.5659(17) 1.0 Uiso 0.0453(28) 4
O O 0.0770(6) 0.5 -0.1807(20) 1.0 Uiso 0.030(4) 4
C C 0.05213(20) 0.6492(6) -0.0165(11) 1.0 Uiso 0.0369(26) 8
D D1 0.0902(5) 0.6501(11) 0.2239(17) 1.0 Uiso 0.0561(30) 8
D D2 0.0698(5) 0.7612(8) -0.1494(18) 1.0 Uiso 0.0561(30) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0



# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.391(13) . 1_555 N
I O 2.482(14) . 1_556 N
Cl I 2.391(13) . 1_555 N
Cl Cl 3.112(12) . 2_656 N
Cl D1 2.902(8) . 102_546 N
Cl D1 2.902(8) . -101_566 N
Cl D2 2.658(8) . 102_545 N
Cl D2 2.658(8) . -101_565 N
O I 2.482(14) . 1_554 N
O C 1.434(5) . 1_555 N
O C 1.434(5) . -2_565 N
O D1 2.063(8) . 1_555 N
O D1 2.063(8) . -2_565 N
O D2 2.071(7) . 1_555 N
O D2 2.071(7) . -2_565 N
C O 1.434(5) . 1_555 N
C C 1.532(5) . 2_555 N
C D1 1.092(6) . 1_555 N
C D2 1.092(5) . 1_555 N
D1 Cl 2.902(8) . 102_556 N
D1 O 2.063(8) . 1_555 N
D1 C 1.092(6) . 1_555 N
D1 D2 1.792(8) . 1_555 N
D2 Cl 2.658(8) . 102_555 N
D2 O 2.071(7) . 1_555 N
D2 C 1.092(5) . 1_555 N
D2 D1 1.792(8) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 174.7(6) 1_555 . 1_556 N
I Cl Cl 174.9(5) 1_555 . 2_656 N
I Cl D1 87.13(22) 1_555 . 102_546 N
I Cl D1 87.13(22) 1_555 . -101_566 N
I Cl D2 115.09(27) 1_555 . 102_545 N
I Cl D2 115.09(27) 1_555 . -101_565 N
Cl Cl D1 91.34(20) 2_656 . 102_546 N
Cl Cl D1 91.34(20) 2_656 . -101_566 N
Cl Cl D2 68.11(21) 2_656 . 102_545 N
Cl Cl D2 68.11(21) 2_656 . -101_565 N
D1 Cl D1 144.6(4) 102_546 . -101_566 N
D1 Cl D2 60.87(19) 102_546 . 102_545 N
D1 Cl D2 150.00(33) 102_546 . -101_565 N
D1 Cl D2 150.00(33) -101_566 . 102_545 N
D1 Cl D2 60.87(19) -101_566 . -101_565 N
D2 Cl D2 90.5(4) 102_545 . -101_565 N
I O C 112.7(4) 1_554 . 1_555 N
I O C 112.7(4) 1_554 . -2_565 N
I O D1 98.4(5) 1_554 . 1_555 N
I O D1 98.4(5) 1_554 . -2_565 N
I O D2 93.89(32) 1_554 . 1_555 N
I O D2 93.89(32) 1_554 . -2_565 N
C O C 110.7(5) 1_555 . -2_565 N
C O D1 30.07(23) 1_555 . 1_555 N
C O D1 94.6(5) 1_555 . -2_565 N
C O D2 29.83(20) 1_555 . 1_555 N
C O D2 140.5(5) 1_555 . -2_565 N
C O D1 94.6(5) -2_565 . 1_555 N
C O D1 30.07(23) -2_565 . -2_565 N
C O D2 140.5(5) -2_565 . 1_555 N
C O D2 29.83(20) -2_565 . -2_565 N
D1 O D1 70.2(6) 1_555 . -2_565 N
D1 O D2 51.36(24) 1_555 . 1_555 N
D1 O D2 121.4(5) 1_555 . -2_565 N
D1 O D2 121.4(5) -2_565 . 1_555 N
D1 O D2 51.36(24) -2_565 . -2_565 N
D2 O D2 170.2(6) 1_555 . -2_565 N
O C C 110.5(4) 1_555 . 2_555 N
O C D1 108.8(5) 1_555 . 1_555 N
O C D2 109.4(4) 1_555 . 1_555 N
C C D1 108.1(5) 2_555 . 1_555 N
C C D2 109.8(4) 2_555 . 1_555 N
D1 C D2 110.2(5) 1_555 . 1_555 N
Cl D1 O 142.6(4) 102_556 . 1_555 N
Cl D1 C 107.2(5) 102_556 . 1_555 N
Cl D1 D2 78.3(5) 102_556 . 1_555 N
O D1 C 41.13(35) 1_555 . 1_555 N
O D1 D2 64.55(32) 1_555 . 1_555 N
C D1 D2 34.91(30) 1_555 . 1_555 N
Cl D2 O 130.6(4) 102_555 . 1_555 N
Cl D2 C 169.7(6) 102_555 . 1_555 N
Cl D2 D1 154.2(5) 102_555 . 1_555 NN
O D2 C 40.75(28) 1_555 . 1_555 N
O D2 D1 64.09(34) 1_555 . 1_555 N
C D2 D1 34.90(29) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2255394'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-09T18:08|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-09T18:08|BF_H_01|WGM|PEARL

#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?



_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.3773(6)
_cell_length_b                   7.8355(6)
_cell_length_c                   4.10430(31)
_cell_angle_alpha                90.0
_cell_angle_beta                 97.407(8)
_cell_angle_gamma                90.0
_cell_volume                     458.50(4)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'


_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      295
_cell_measurement_temperature    295
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    3.048
_diffrn_measurement_pressure     1948000

_pd_prep_cool_rate               ?
_pd_prep_pressure                194800
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     54
_refine_ls_goodness_of_fit_all   1.16
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_pd_proc_ls_prof_R_factor        0.0328
_pd_proc_ls_prof_wR_factor       0.0289
_pd_proc_ls_prof_wR_expected     0.0253
_refine_ls_R_Fsqd_factor         0.16793


loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2429(7) 0.5 0.7163(29) 1.0 Uiso 0.0211(12) 4
Cl Cl 0.3997(4) 0.5 0.5704(18) 1.0 Uiso 0.0423(24) 4
O O 0.0779(6) 0.5 -0.1742(20) 1.0 Uiso 0.0248(33) 4
C C 0.05216(20) 0.6493(6) -0.0087(11) 1.0 Uiso 0.0255(21) 8
D D1 0.0911(4) 0.6526(10) 0.2394(17) 1.0 Uiso 0.0498(25) 8
D D2 0.0705(5) 0.7609(8) -0.1474(17) 1.0 Uiso 0.0498(25) 8
loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0



# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.405(13) . 1_555 N
I O 2.471(15) . 1_556 N
Cl I 2.405(13) . 1_555 N
Cl Cl 3.015(12) . 2_656 N
Cl D2 2.627(8) . 102_545 N
Cl D2 2.627(8) . -101_565 N
O I 2.471(15) . 1_554 N
O C 1.426(5) . 1_555 N
O C 1.426(5) . -2_565 N
O D1 2.065(8) . 1_555 N
O D1 2.065(8) . -2_565 N
O D2 2.051(6) . 1_555 N
O D2 2.051(6) . -2_565 N
C O 1.426(5) . 1_555 N
C C 1.511(6) . 2_555 N
C D1 1.097(6) . 1_555 N
C D2 1.094(5) . 1_555 N
D1 O 2.065(8) . 1_555 N
D1 C 1.097(6) . 1_555 N
D1 D2 1.791(8) . 1_555 N
D2 Cl 2.627(8) . 102_555 N
D2 O 2.051(6) . 1_555 N
D2 C 1.094(5) . 1_555 N
D2 D1 1.791(8) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 176.1(6) 1_555 . 1_556 N
I Cl Cl 176.7(5) 1_555 . 2_656 N
I O C 113.6(4) 1_554 . 1_555 N
I O C 113.6(4) 1_554 . -2_565 N
C O C 110.3(6) 1_555 . -2_565 N
O C C 110.1(4) 1_555 . 2_555 N
O C D1 109.2(5) 1_555 . 1_555 N
O C D2 108.3(4) 1_555 . 1_555 N
C C D1 110.3(5) 2_555 . 1_555 N
C C D2 109.4(4) 2_555 . 1_555 N
D1 C D2 109.6(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2255392'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-09T18:01|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-09T18:01|BF_H_01|WGM|PEARL

#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products


_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?


_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.4480(8)
_cell_length_b                   7.8814(7)
_cell_length_c                   4.1699(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 96.974(10)
_cell_angle_gamma                90.0
_cell_volume                     471.32(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   0.98
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full


_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0410
_pd_proc_ls_prof_wR_factor       0.0348
_pd_proc_ls_prof_wR_expected     0.0361
_refine_ls_R_Fsqd_factor         0.20155

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      295
_cell_measurement_temperature    295
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    2.965
_diffrn_measurement_pressure     1438000


loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2431(9) 0.5 0.722(4) 1.0 Uiso 0.0248(17) 4
Cl Cl 0.3984(5) 0.5 0.5713(22) 1.0 Uiso 0.0495(35) 4
O O 0.0775(7) 0.5 -0.1790(22) 1.0 Uiso 0.029(4) 4
C C 0.05204(19) 0.6495(6) -0.0125(12) 1.0 Uiso 0.0391(33) 8
D D1 0.0899(5) 0.6506(13) 0.2297(19) 1.0 Uiso 0.063(4) 8
D D2 0.0702(5) 0.7608(9) -0.1458(20) 1.0 Uiso 0.063(4) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0



# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.403(16) . 1_555 N
I O 2.476(16) . 1_556 N
Cl I 2.403(16) . 1_555 N
Cl Cl 3.065(15) . 2_656 N
Cl D2 2.665(10) . 102_545 N
Cl D2 2.665(10) . -101_565 N
O I 2.476(16) . 1_554 N
O C 1.438(5) . 1_555 N
O C 1.438(5) . -2_565 N
O D1 2.067(8) . 1_555 N
O D1 2.067(8) . -2_565 N
O D2 2.064(7) . 1_555 N
O D2 2.064(7) . -2_565 N
C O 1.438(5) . 1_555 N
C C 1.520(5) . 2_555 N
C D1 1.089(6) . 1_555 N
C D2 1.088(5) . 1_555 N
D1 O 2.067(8) . 1_555 N
D1 C 1.089(6) . 1_555 N
D1 D2 1.783(8) . 1_555 N
D2 Cl 2.665(10) . 102_555 N
D2 O 2.064(7) . 1_555 N
D2 C 1.088(5) . 1_555 N
D2 D1 1.783(8) . 1_555 N


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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 174.4(8) 1_555 . 1_556 N
I Cl Cl 176.0(6) 1_555 . 2_656 N
I O C 112.9(5) 1_554 . 1_555 N
I O C 112.9(5) 1_554 . -2_565 N
C O C 110.0(5) 1_555 . -2_565 N
O C C 110.3(4) 1_555 . 2_555 N
O C D1 109.0(5) 1_555 . 1_555 N
O C D2 108.8(4) 1_555 . 1_555 N
C C D1 109.1(5) 2_555 . 1_555 N
C C D2 109.7(4) 2_555 . 1_555 N
D1 C D2 110.0(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 2255404'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_BF_phase_1          
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.05
RESPONSE: The value is 0.06 i.e. > 0.05 but see  V. K. Pecharsky and P. Y. Zayalij Fundamentals of Powder  Diffraction and Structural Characterization of materials 2nd edition  2009 Springer p 641 footnote 22 IUCR imposes the requirement shift/error  < 0.05  for single crystal data but for Rietveld fits shift/error <0.1 are satisfactory.  IUCR in fact do not require shift/su_max for  powder data
;
_vrf_PLAT080_BF_phase_1          
;
PROBLEM: Maximum Shift/Error ............................       0.06 Why ?
RESPONSE: The value is 0.06 i.e. > 0.05 but see  V. K. Pecharsky and P. Y. Zayalij Fundamentals of Powder  Diffraction and Structural Characterization of materials 2nd edition  2009 Springer p 641 footnote 22 IUCR imposes the requirement shift/error  < 0.05  for single crystal data but for Rietveld fits shift/error <0.1 are satisfactory.  IUCR in fact do not require shift/su_max for  powder data
;
_vrf_PLAT155_BF_phase_1          
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: Marshall, W G,
;
# Added during the CSD deposition process: Tuesday 11 April 2023 02:38 PM
# end Validation Reply Form


_pd_block_id                     2019-09-03T21:48|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-03T21:48|BF_H_01|WGM|pearl

#==============================================================================


#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   'Dioxane-(ICl)2 form III (P-1)'
_cell_length_a                   8.4578(7)
_cell_length_b                   6.3087(6)
_cell_length_c                   3.74732(29)
_cell_angle_alpha                92.411(8)
_cell_angle_beta                 78.602(7)
_cell_angle_gamma                101.346(5)
_cell_volume                     192.175(18)
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                7212000
_pd_prep_temperature             ?
_pd_char_colour                  orange
_refine_ls_shift/su_max          0.06
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     51
_refine_ls_goodness_of_fit_all   0.99
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0330
_pd_proc_ls_prof_wR_factor       0.0281
_pd_proc_ls_prof_wR_expected     0.0288
_refine_ls_R_Fsqd_factor         0.10857

_exptl_crystal_description       needle
_chemical_formula_sum            'C2 D4 Cl I O'
_chemical_formula_weight         210.43
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -P 1'
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_diffrn_measurement_device_type  PEARL
_exptl_crystal_density_diffrn    3.636
_diffrn_measurement_pressure     7212000


loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
-1 -x,-y,-z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.7140(14) 0.5248(18) 0.5272(29) 1.0 Uiso 0.0049(9) 2
Cl Cl 0.5583(7) 0.2090(10) 0.8116(15) 1.0 Uiso 0.0099(17) 2
O O 0.09575(33) 0.1457(4) -0.2651(8) 1.0 Uiso 0.0093(28) 2
C C1 -0.04221(34) 0.20492(22) -0.0128(9) 1.0 Uiso 0.0123(16) 2
C C2 0.16930(8) -0.0039(4) -0.0980(9) 1.0 Uiso 0.0123(16) 2
D D1 0.0019(5) 0.28641(34) 0.2234(13) 1.0 Uiso 0.0280(17) 2
D D2 -0.0916(6) 0.3179(6) -0.1536(15) 1.0 Uiso 0.0280(17) 2
D D3 0.21505(27) 0.0748(7) 0.1384(13) 1.0 Uiso 0.0280(17) 2
D D4 0.27050(28) -0.0409(7) -0.3026(14) 1.0 Uiso 0.0280(17) 2

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 2.0
Cl 2.0
C 4.0
O 2.0
D 8.0


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I I 3.74732(29) . 1_554 N
I I 3.74732(29) . 1_556 N
I I 3.617(22) . -1_666 N
I Cl 3.579(13) . 1_554 N
I Cl 2.330(12) . 1_555 N
I Cl 3.549(12) . -1_666 N
I O 2.471(11) . -1_665 N
I D1 2.780(12) . -1_666 N
I D2 2.755(11) . 1_656 N
I D3 2.783(12) . -1_666 N
Cl I 2.330(12) . 1_555 N
Cl I 3.579(13) . 1_556 N
Cl I 3.549(12) . -1_666 N
Cl Cl 2.943(11) . -1_657 N
Cl D4 2.727(8) . 1_556 N
Cl D4 2.490(7) . -1_655 N
O I 2.471(11) . -1_665 N
O C1 1.44929(13) . 1_555 N
O C2 1.45080(11) . 1_555 N
O D1 2.08202(18) . 1_555 N
O D2 2.05967(16) . 1_555 N
O D3 2.08373(15) . 1_555 N
O D4 2.04394(15) . 1_555 N
C1 O 1.44929(13) . 1_555 N
C1 C2 1.50577(14) . -1_555 N
C1 D1 1.09748(9) . 1_555 N
C1 D2 1.09365(8) . 1_555 N
C1 D3 2.15854(19) . -1_555 N
C1 D4 2.14740(21) . -1_555 N
C2 O 1.45080(11) . 1_555 N
C2 C1 1.50577(14) . -1_555 N
C2 D1 2.16275(19) . -1_555 N
C2 D2 2.15485(22) . -1_555 N
C2 D3 1.09726(9) . 1_555 N
C2 D4 1.08575(10) . 1_555 N
D1 I 2.780(12) . -1_666 N
D1 O 2.08202(18) . 1_555 N
D1 C1 1.09748(9) . 1_555 N
D1 C2 2.16275(19) . -1_555 N
D1 D2 1.78556(13) . 1_555 N
D2 I 2.755(11) . 1_454 N
D2 O 2.05967(16) . 1_555 N
D2 C1 1.09365(8) . 1_555 N
D2 C2 2.15485(22) . -1_555 N
D2 D1 1.78556(13) . 1_555 N
D3 I 2.783(12) . -1_666 N
D3 O 2.08373(15) . 1_555 N
D3 C1 2.15854(19) . -1_555 N
D3 C2 1.09726(9) . 1_555 N
D3 D4 1.79176(16) . 1_555 N
D4 Cl 2.727(8) . 1_554 N
D4 Cl 2.490(7) . -1_655 N
D4 O 2.04394(15) . 1_555 N
D4 C1 2.14740(21) . -1_555 N
D4 C2 1.08575(10) . 1_555 N
D4 D3 1.79176(16) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.3(5) 1_555 . -1_665 N
Cl I D1 117.6(4) 1_555 . -1_666 N
Cl I D2 69.87(29) 1_555 . 1_656 N
Cl I D3 125.9(4) 1_555 . -1_666 N
O I D1 55.80(27) -1_665 . -1_666 N
O I D2 103.6(4) -1_665 . 1_656 N
O I D3 52.18(22) -1_665 . -1_666 N
D1 I D2 53.03(20) -1_666 . 1_656 N
D1 I D3 51.38(21) -1_666 . -1_666 N
D2 I D3 97.4(4) 1_656 . -1_666 N
I Cl Cl 165.8(4) 1_555 . -1_657 N
I Cl D4 130.9(4) 1_555 . 1_556 N
I Cl D4 81.64(31) 1_555 . -1_655 N
Cl Cl D4 61.47(26) -1_657 . 1_556 N
Cl Cl D4 91.18(30) -1_657 . -1_655 N
D4 Cl D4 93.77(23) 1_556 . -1_655 N
I O C1 109.76(32) -1_665 . 1_555 N
I O C2 115.57(32) -1_665 . 1_555 N
C1 O C2 110.886(6) 1_555 . 1_555 N
O C1 C2 108.942(8) 1_555 . -1_555 N
O C1 D1 108.890(7) 1_555 . 1_555 N
O C1 D2 107.358(6) 1_555 . 1_555 N
C2 C1 D1 111.395(7) -1_555 . 1_555 N
C2 C1 D2 110.993(7) -1_555 . 1_555 N
D1 C1 D2 109.155(7) 1_555 . 1_555 N
O C2 C1 109.016(7) 1_555 . -1_555 N
O C2 D3 108.935(7) 1_555 . 1_555 N
O C2 D4 106.486(7) 1_555 . 1_555 N
C1 C2 D3 111.070(7) -1_555 . 1_555 N
C1 C2 D4 110.875(8) -1_555 . 1_555 N
D3 C2 D4 110.324(6) 1_555 . 1_555 N
I D1 C1 142.81(28) -1_666 . 1_555 N
I D1 D2 137.27(28) -1_666 . 1_555 N
C1 D1 D2 35.351(4) 1_555 . 1_555 N
I D2 C1 165.74(29) 1_454 . 1_555 N
I D2 D1 149.77(35) 1_454 . 1_555 N
C1 D2 D1 35.493(4) 1_555 . 1_555 N
I D3 C2 142.61(29) -1_666 . 1_555 N
I D3 D4 136.97(28) -1_666 . 1_555 N
C2 D3 D4 34.628(4) 1_555 . 1_555 N
Cl D4 Cl 86.23(23) 1_554 . -1_655 N
Cl D4 C2 109.59(22) 1_554 . 1_555 N
Cl D4 D3 76.45(23) 1_554 . 1_555 N
Cl D4 C2 163.99(28) -1_655 . 1_555 N
Cl D4 D3 157.70(28) -1_655 . 1_555 N
C2 D4 D3 35.048(4) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 2255402'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT155_BF_phase_1          
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: O
;
# Added during the CSD deposition process: Tuesday 11 April 2023 02:37 PM
# end Validation Reply Form


_pd_block_id                     2019-09-06T12:05|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-06T12:05|BF_H_01|WGM|pearl

#==============================================================================


#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   'Dioxane-(ICl)2 form III (P-1)'
_cell_length_a                   8.4911(6)
_cell_length_b                   6.3445(5)
_cell_length_c                   3.77185(25)
_cell_angle_alpha                92.216(7)
_cell_angle_beta                 78.415(6)
_cell_angle_gamma                101.392(5)
_cell_volume                     195.135(16)
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                6486000
_pd_prep_temperature             ?
_pd_char_colour                  orange
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     51
_refine_ls_goodness_of_fit_all   1.04
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0309
_pd_proc_ls_prof_wR_factor       0.0256
_pd_proc_ls_prof_wR_expected     0.0250
_refine_ls_R_Fsqd_factor         0.09031

_exptl_crystal_description       needle
_chemical_formula_sum            'C2 D4 Cl I O'
_chemical_formula_weight         210.43
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  '-P 1 '
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_diffrn_measurement_device_type  PEARL
_exptl_crystal_density_diffrn    3.581
_diffrn_measurement_pressure     6486000

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
-1 -x,-y,-z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.7159(12) 0.5301(16) 0.5306(26) 1.0 Uiso 0.0061(8) 2
Cl Cl 0.5597(7) 0.2104(9) 0.8123(15) 1.0 Uiso 0.0122(16) 2
O O 0.09609(29) 0.1461(4) -0.2625(7) 1.0 Uiso 0.0121(27) 2
C C1 -0.04254(29) 0.20341(19) -0.0131(8) 1.0 Uiso 0.0113(14) 2
C C2 0.16903(7) -0.0026(4) -0.0955(9) 1.0 Uiso 0.0113(14) 2
D D1 0.0002(5) 0.28391(30) 0.2227(11) 1.0 Uiso 0.0295(16) 2
D D2 -0.0914(5) 0.3158(5) -0.1536(13) 1.0 Uiso 0.0295(16) 2
D D3 0.21336(26) 0.0751(6) 0.1404(12) 1.0 Uiso 0.0295(16) 2
D D4 0.27078(25) -0.0381(6) -0.2979(13) 1.0 Uiso 0.0295(16) 2

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 2.0
Cl 2.0
C 4.0
O 2.0
D 8.0


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I I 3.77185(25) . 1_554 N
I I 3.77185(25) . 1_556 N
I I 3.664(20) . -1_666 N
I Cl 2.354(11) . 1_555 N
I Cl 3.573(11) . -1_666 N
I O 2.451(10) . -1_665 N
I D1 2.786(11) . -1_666 N
I D2 2.780(10) . 1_656 N
I D3 2.764(11) . -1_666 N
Cl I 2.354(11) . 1_555 N
Cl I 3.573(11) . -1_666 N
Cl Cl 2.967(10) . -1_657 N
Cl D4 2.740(8) . 1_556 N
Cl D4 2.523(7) . -1_655 N
O I 2.451(10) . -1_665 N
O C1 1.44929(11) . 1_555 N
O C2 1.45079(10) . 1_555 N
O D1 2.08202(16) . 1_555 N
O D2 2.05968(14) . 1_555 N
O D3 2.08373(13) . 1_555 N
O D4 2.04394(13) . 1_555 N
C1 O 1.44929(11) . 1_555 N
C1 C2 1.50576(13) . -1_555 N
C1 D1 1.09748(8) . 1_555 N
C1 D2 1.09366(7) . 1_555 N
C1 D3 2.15854(16) . -1_555 N
C1 D4 2.14740(18) . -1_555 N
C2 O 1.45079(10) . 1_555 N
C2 C1 1.50576(13) . -1_555 N
C2 D1 2.16274(16) . -1_555 N
C2 D2 2.15484(19) . -1_555 N
C2 D3 1.09726(8) . 1_555 N
C2 D4 1.08576(9) . 1_555 N
D1 I 2.786(11) . -1_666 N
D1 O 2.08202(16) . 1_555 N
D1 C1 1.09748(8) . 1_555 N
D1 C2 2.16274(16) . -1_555 N
D1 D2 1.78556(11) . 1_555 N
D2 I 2.780(10) . 1_454 N
D2 O 2.05968(14) . 1_555 N
D2 C1 1.09366(7) . 1_555 N
D2 C2 2.15484(19) . -1_555 N
D2 D1 1.78556(11) . 1_555 N
D3 I 2.764(11) . -1_666 N
D3 O 2.08373(13) . 1_555 N
D3 C1 2.15854(16) . -1_555 N
D3 C2 1.09726(8) . 1_555 N
D3 D4 1.79177(13) . 1_555 N
D4 Cl 2.740(8) . 1_554 N
D4 Cl 2.523(7) . -1_655 N
D4 O 2.04394(13) . 1_555 N
D4 C1 2.14740(18) . -1_555 N
D4 C2 1.08576(9) . 1_555 N
D4 D3 1.79177(13) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.7(5) 1_555 . -1_665 N
Cl I D1 117.6(4) 1_555 . -1_666 N
Cl I D2 69.10(25) 1_555 . 1_656 N
Cl I D3 126.5(4) 1_555 . -1_666 N
O I D1 56.57(25) -1_665 . -1_666 N
O I D2 104.6(4) -1_665 . 1_656 N
O I D3 52.86(20) -1_665 . -1_666 N
D1 I D2 53.66(18) -1_666 . 1_656 N
D1 I D3 51.52(19) -1_666 . -1_666 N
D2 I D3 98.17(33) 1_656 . -1_666 N
I Cl Cl 166.3(4) 1_555 . -1_657 N
I Cl D4 131.02(35) 1_555 . 1_556 N
I Cl D4 82.78(27) 1_555 . -1_655 N
Cl Cl D4 61.11(24) -1_657 . 1_556 N
Cl Cl D4 90.65(27) -1_657 . -1_655 N
D4 Cl D4 93.17(21) 1_556 . -1_655 N
I O C1 110.45(29) -1_665 . 1_555 N
I O C2 115.87(29) -1_665 . 1_555 N
C1 O C2 110.886(5) 1_555 . 1_555 N
O C1 C2 108.942(7) 1_555 . -1_555 N
O C1 D1 108.890(6) 1_555 . 1_555 N
O C1 D2 107.358(5) 1_555 . 1_555 N
C2 C1 D1 111.395(6) -1_555 . 1_555 N
C2 C1 D2 110.993(6) -1_555 . 1_555 N
D1 C1 D2 109.155(6) 1_555 . 1_555 N
O C2 C1 109.016(6) 1_555 . -1_555 N
O C2 D3 108.936(6) 1_555 . 1_555 N
O C2 D4 106.486(6) 1_555 . 1_555 N
C1 C2 D3 111.070(6) -1_555 . 1_555 N
C1 C2 D4 110.875(7) -1_555 . 1_555 N
D3 C2 D4 110.324(5) 1_555 . 1_555 N
I D1 C1 142.22(27) -1_666 . 1_555 N
I D1 D2 137.15(25) -1_666 . 1_555 N
C1 D1 D2 35.3514(35) 1_555 . 1_555 N
I D2 C1 166.43(24) 1_454 . 1_555 N
I D2 D1 148.85(31) 1_454 . 1_555 N
C1 D2 D1 35.4935(35) 1_555 . 1_555 N
I D3 C2 142.70(25) -1_666 . 1_555 N
I D3 D4 136.59(26) -1_666 . 1_555 N
C2 D3 D4 34.6281(34) 1_555 . 1_555 N
Cl D4 Cl 86.83(21) 1_554 . -1_655 N
Cl D4 C2 110.33(21) 1_554 . 1_555 N
Cl D4 D3 77.18(22) 1_554 . 1_555 N
Cl D4 C2 162.67(26) -1_655 . 1_555 N
Cl D4 D3 158.73(27) -1_655 . 1_555 N
C2 D4 D3 35.0482(34) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC8
_database_code_depnum_ccdc_archive 'CCDC 2255396'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-06T10:51|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-06T10:51|BF_H_01|WGM|PEARL

#==============================================================================

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.3151(6)
_cell_length_b                   7.7964(6)
_cell_length_c                   4.05749(32)
_cell_angle_alpha                90.0
_cell_angle_beta                 97.819(9)
_cell_angle_gamma                90.0
_cell_volume                     448.63(4)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0375
_pd_proc_ls_prof_wR_factor       0.0302
_pd_proc_ls_prof_wR_expected     0.0262
_refine_ls_R_Fsqd_factor         0.16031

#Load in tons 36 tons  
_pd_prep_cool_rate               ?
_pd_prep_pressure                2429000
_pd_prep_temperature             ?
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     54
_refine_ls_goodness_of_fit_all   1.18
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    3.115
_diffrn_measurement_pressure     2429000

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2442(8) 0.5 0.7257(29) 1.0 Uiso 0.0168(11) 4
Cl Cl 0.3997(4) 0.5 0.5753(18) 1.0 Uiso 0.0335(23) 4
O O 0.0786(6) 0.5 -0.1749(19) 1.0 Uiso 0.0144(31) 4
C C 0.05256(20) 0.6503(6) -0.0068(11) 1.0 Uiso 0.0183(19) 8
D D1 0.0919(4) 0.6544(10) 0.2418(15) 1.0 Uiso 0.0405(22) 8
D D2 0.0719(5) 0.7619(7) -0.1432(17) 1.0 Uiso 0.0405(22) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.386(13) . 1_555 N
I O 2.458(15) . 1_556 N
I C 3.299(11) . 1_556 N
I C 3.299(11) . -2_566 N
I D1 2.982(12) . 1_555 N
I D1 2.982(12) . -2_565 N
Cl I 2.386(13) . 1_555 N
Cl Cl 3.017(12) . 2_656 N
Cl C 3.262(6) . 102_546 N
Cl C 3.262(6) . -101_566 N
Cl D1 2.793(7) . 102_546 N
Cl D1 2.793(7) . -101_566 N
Cl D2 2.623(8) . 102_545 N
Cl D2 2.944(9) . 102_546 N
Cl D2 2.623(8) . -101_565 N
Cl D2 2.944(9) . -101_566 N
O I 2.458(15) . 1_554 N
O O 2.819(15) . 2_555 N
O C 1.430(5) . 1_555 N
O C 2.412(8) . 2_555 N
O C 2.412(8) . -1_565 N
O C 1.430(5) . -2_565 N
O D1 2.685(10) . 1_554 N
O D1 2.063(8) . 1_555 N
O D1 2.685(10) . -2_564 N
O D1 2.063(8) . -2_565 N
O D2 2.049(6) . 1_555 N
O D2 2.049(6) . -2_565 N
C I 3.299(11) . 1_554 N
C Cl 3.262(6) . 102_556 N
C O 1.430(5) . 1_555 N
C O 2.412(8) . 2_555 N
C C 1.513(6) . 2_555 N
C C 2.789(8) . -1_565 N
C C 2.343(9) . -2_565 N
C D1 1.087(5) . 1_555 N
C D1 2.157(7) . 2_555 N
C D1 2.612(9) . -2_565 N
C D2 1.087(5) . 1_555 N
C D2 2.145(7) . 2_555 N
D1 I 2.982(12) . 1_555 N
D1 Cl 2.793(7) . 102_556 N
D1 O 2.063(8) . 1_555 N
D1 O 2.685(10) . 1_556 N
D1 C 1.087(5) . 1_555 N
D1 C 2.157(7) . 2_555 N
D1 C 2.612(9) . -2_565 N
D1 D2 1.761(8) . 1_555 N
D2 Cl 2.623(8) . 102_555 N
D2 Cl 2.944(9) . 102_556 N
D2 O 2.049(6) . 1_555 N
D2 C 1.087(5) . 1_555 N
D2 C 2.145(7) . 2_555 N
D2 D1 1.761(8) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 174.7(6) 1_555 . 1_556 N
Cl I C 158.46(16) 1_555 . 1_556 N
Cl I C 158.46(16) 1_555 . -2_566 N
Cl I D1 117.1(4) 1_555 . 1_555 N
Cl I D1 117.1(4) 1_555 . -2_565 N
O I C 23.43(14) 1_556 . 1_556 N
O I C 23.43(14) 1_556 . -2_566 N
O I D1 58.21(31) 1_556 . 1_555 N
O I D1 58.21(31) 1_556 . -2_565 N
C I C 41.60(21) 1_556 . -2_566 N
C I D1 60.47(21) 1_556 . 1_555 N
C I D1 78.11(28) 1_556 . -2_565 N
C I D1 78.11(28) -2_566 . 1_555 N
C I D1 60.47(21) -2_566 . -2_565 N
D1 I D1 47.63(34) 1_555 . -2_565 N
I Cl Cl 176.9(5) 1_555 . 2_656 N
I Cl C 89.86(22) 1_555 . 102_546 N
I Cl C 89.86(22) 1_555 . -101_566 N
I Cl D1 86.57(21) 1_555 . 102_546 N
I Cl D1 86.57(21) 1_555 . -101_566 N
I Cl D2 113.94(28) 1_555 . 102_545 N
I Cl D2 80.45(30) 1_555 . 102_546 N
I Cl D2 113.94(28) 1_555 . -101_565 N
I Cl D2 80.45(30) 1_555 . -101_566 N
Cl Cl C 88.44(18) 2_656 . 102_546 N
Cl Cl C 88.44(18) 2_656 . -101_566 N
Cl Cl D1 92.63(18) 2_656 . 102_546 N
Cl Cl D1 92.63(18) 2_656 . -101_566 N
Cl Cl D2 68.04(23) 2_656 . 102_545 N
Cl Cl D2 97.15(26) 2_656 . 102_546 N
Cl Cl D2 68.04(23) 2_656 . -101_565 N
Cl Cl D2 97.15(26) 2_656 . -101_566 N
C Cl C 113.40(26) 102_546 . -101_566 N
C Cl D1 18.69(12) 102_546 . 102_546 N
C Cl D1 131.71(30) 102_546 . -101_566 N
C Cl D2 74.16(16) 102_546 . 102_545 N
C Cl D2 19.31(11) 102_546 . 102_546 N
C Cl D2 155.51(25) 102_546 . -101_565 N
C Cl D2 96.34(27) 102_546 . -101_566 N
C Cl D1 131.71(30) -101_566 . 102_546 N
C Cl D1 18.69(12) -101_566 . -101_566 N
C Cl D2 155.51(25) -101_566 . 102_545 N
C Cl D2 96.34(27) -101_566 . 102_546 N
C Cl D2 74.16(16) -101_566 . -101_565 N
C Cl D2 19.31(11) -101_566 . -101_566 N
D1 Cl D1 149.5(4) 102_546 . -101_566 N
D1 Cl D2 59.33(19) 102_546 . 102_545 N
D1 Cl D2 35.64(16) 102_546 . 102_546 N
D1 Cl D2 148.80(33) 102_546 . -101_565 N
D1 Cl D2 113.82(31) 102_546 . -101_566 N
D1 Cl D2 148.80(33) -101_566 . 102_545 N
D1 Cl D2 113.82(31) -101_566 . 102_546 N
D1 Cl D2 59.33(19) -101_566 . -101_565 N
D1 Cl D2 35.64(16) -101_566 . -101_566 N
D2 Cl D2 93.41(18) 102_545 . 102_546 N
D2 Cl D2 90.1(4) 102_545 . -101_565 N
D2 Cl D2 162.19(35) 102_545 . -101_566 N
D2 Cl D2 162.19(35) 102_546 . -101_565 N
D2 Cl D2 78.18(31) 102_546 . -101_566 N
D2 Cl D2 93.41(18) -101_565 . -101_566 N
I O O 159.4(6) 1_554 . 2_555 N
I O C 113.4(4) 1_554 . 1_555 N
I O C 149.13(23) 1_554 . 2_555 N
I O C 149.13(23) 1_554 . -1_565 N
I O C 113.4(4) 1_554 . -2_565 N
I O D1 70.71(33) 1_554 . 1_554 N
I O D1 98.7(4) 1_554 . 1_555 N
I O D1 70.71(33) 1_554 . -2_564 N
I O D1 98.7(4) 1_554 . -2_565 N
I O D2 93.69(34) 1_554 . 1_555 N
I O D2 93.69(34) 1_554 . -2_565 N
O O C 58.83(28) 2_555 . 1_555 N
O O C 30.49(17) 2_555 . 2_555 N
O O C 30.49(17) 2_555 . -1_565 N
O O C 58.83(28) 2_555 . -2_565 N
O O D1 126.9(5) 2_555 . 1_554 N
O O D1 65.08(31) 2_555 . 1_555 N
O O D1 126.9(5) 2_555 . -2_564 N
O O D1 65.08(31) 2_555 . -2_565 N
O O D2 85.49(31) 2_555 . 1_555 N
O O D2 85.49(31) 2_555 . -2_565 N
C O C 36.13(24) 1_555 . 2_555 N
C O C 89.3(4) 1_555 . -1_565 N
C O C 110.0(5) 1_555 . -2_565 N
C O D1 96.16(31) 1_555 . 1_554 N
C O D1 29.80(23) 1_555 . 1_555 N
C O D1 147.3(4) 1_555 . -2_564 N
C O D1 95.1(5) 1_555 . -2_565 N
C O D2 30.27(19) 1_555 . 1_555 N
C O D2 140.3(5) 1_555 . -2_565 N
C O C 58.12(31) 2_555 . -1_565 N
C O C 89.3(4) 2_555 . -2_565 N
C O D1 101.72(30) 2_555 . 1_554 N
C O D1 56.98(24) 2_555 . 1_555 N
C O D1 129.7(4) 2_555 . -2_564 N
C O D1 91.3(4) 2_555 . -2_565 N
C O D2 56.77(23) 2_555 . 1_555 N
C O D2 114.8(4) 2_555 . -2_565 N
C O C 36.13(24) -1_565 . -2_565 N
C O D1 129.7(4) -1_565 . 1_554 N
C O D1 91.3(4) -1_565 . 1_555 N
C O D1 101.72(30) -1_565 . -2_564 N
C O D1 56.98(24) -1_565 . -2_565 N
C O D2 114.8(4) -1_565 . 1_555 N
C O D2 56.77(23) -1_565 . -2_565 N
C O D1 147.3(4) -2_565 . 1_554 N
C O D1 95.1(5) -2_565 . 1_555 N
C O D1 96.16(31) -2_565 . -2_564 N
C O D1 29.80(23) -2_565 . -2_565 N
C O D2 140.3(5) -2_565 . 1_555 N
C O D2 30.27(19) -2_565 . -2_565 N
D1 O D1 116.80(34) 1_554 . 1_555 N
D1 O D1 53.28(30) 1_554 . -2_564 N
D1 O D1 167.0(4) 1_554 . -2_565 N
D1 O D2 67.54(32) 1_554 . 1_555 N
D1 O D2 120.77(33) 1_554 . -2_565 N
D1 O D1 167.0(4) 1_555 . -2_564 N
D1 O D1 71.4(5) 1_555 . -2_565 N
D1 O D2 50.72(25) 1_555 . 1_555 N
D1 O D2 122.0(5) 1_555 . -2_565 N
D1 O D1 116.80(34) -2_564 . -2_565 N
D1 O D2 120.77(33) -2_564 . 1_555 N
D1 O D2 67.54(32) -2_564 . -2_565 N
D1 O D2 122.0(5) -2_565 . 1_555 N
D1 O D2 50.72(25) -2_565 . -2_565 N
D2 O D2 170.5(6) 1_555 . -2_565 N
I C Cl 110.51(18) 1_554 . 102_556 N
I C O 43.1(4) 1_554 . 1_555 N
I C O 130.14(22) 1_554 . 2_555 N
I C C 152.55(29) 1_554 . 2_555 N
I C C 100.56(21) 1_554 . -1_565 N
I C C 69.20(10) 1_554 . -2_565 N
I C D1 88.1(4) 1_554 . 1_555 N
I C D1 130.56(34) 1_554 . 2_555 N
I C D1 70.05(20) 1_554 . -2_565 N
I C D2 80.6(4) 1_554 . 1_555 N
I C D2 176.10(26) 1_554 . 2_555 N
Cl C O 153.0(4) 102_556 . 1_555 N
Cl C O 110.92(23) 102_556 . 2_555 N
Cl C C 96.74(21) 102_556 . 2_555 N
Cl C C 139.97(24) 102_556 . -1_565 N
Cl C C 146.70(13) 102_556 . -2_565 N
Cl C D1 55.4(4) 102_556 . 1_555 N
Cl C D1 110.06(25) 102_556 . 2_555 N
Cl C D1 122.31(18) 102_556 . -2_565 N
Cl C D2 63.6(4) 102_556 . 1_555 N
Cl C D2 68.29(24) 102_556 . 2_555 N
O C O 90.7(4) 1_555 . 2_555 N
O C C 110.0(4) 1_555 . 2_555 N
O C C 59.8(4) 1_555 . -1_565 N
O C C 35.00(27) 1_555 . -2_565 N
O C D1 109.3(5) 1_555 . 1_555 N
O C D1 95.6(5) 1_555 . 2_555 N
O C D1 51.9(4) 1_555 . -2_565 N
O C D2 108.2(4) 1_555 . 1_555 N
O C D2 138.4(5) 1_555 . 2_555 N
O C C 33.86(22) 2_555 . 2_555 N
O C C 30.84(10) 2_555 . -1_565 N
O C C 60.94(16) 2_555 . -2_565 N
O C D1 93.3(5) 2_555 . 1_555 N
O C D1 53.34(25) 2_555 . 2_555 N
O C D1 64.92(22) 2_555 . -2_565 N
O C D2 143.8(5) 2_555 . 1_555 N
O C D2 53.06(18) 2_555 . 2_555 N
C C C 57.14(14) 2_555 . -1_565 N
C C C 90.0 2_555 . -2_565 N
C C D1 111.0(5) 2_555 . 1_555 N
C C D1 28.06(21) 2_555 . 2_555 N
C C D1 98.58(19) 2_555 . -2_565 N
C C D2 110.0(4) 2_555 . 1_555 N
C C D2 28.45(18) 2_555 . 2_555 N
C C C 32.86(14) -1_565 . -2_565 N
C C D1 102.7(5) -1_565 . 1_555 N
C C D1 62.22(22) -1_565 . 2_555 N
C C D1 46.92(20) -1_565 . -2_565 N
C C D2 149.1(5) -1_565 . 1_555 N
C C D2 82.18(18) -1_565 . 2_555 N
C C D1 91.7(4) -2_565 . 1_555 N
C C D1 90.87(22) -2_565 . 2_555 N
C C D1 24.57(14) -2_565 . -2_565 N
C C D2 143.2(4) -2_565 . 1_555 N
C C D2 113.95(18) -2_565 . 2_555 N
D1 C D1 138.99(33) 1_555 . 2_555 N
D1 C D1 67.1(5) 1_555 . -2_565 N
D1 C D2 108.2(5) 1_555 . 1_555 N
D1 C D2 94.0(4) 1_555 . 2_555 N
D1 C D1 109.14(23) 2_555 . -2_565 N
D1 C D2 93.4(5) 2_555 . 1_555 N
D1 C D2 48.34(23) 2_555 . 2_555 N
D1 C D2 150.2(4) -2_565 . 1_555 N
D1 C D2 113.79(22) -2_565 . 2_555 N
D2 C D2 95.7(5) 1_555 . 2_555 N
I D1 Cl 102.31(24) 1_555 . 102_556 N
I D1 O 106.4(4) 1_555 . 1_555 N
I D1 O 51.08(32) 1_555 . 1_556 N
I D1 C 147.1(5) 1_555 . 1_555 N
I D1 C 148.9(4) 1_555 . 2_555 N
I D1 C 89.25(24) 1_555 . -2_565 N
I D1 D2 142.4(4) 1_555 . 1_555 N
Cl D1 O 141.0(4) 102_556 . 1_555 N
Cl D1 O 101.77(24) 102_556 . 1_556 N
Cl D1 C 105.9(5) 102_556 . 1_555 N
Cl D1 C 97.83(29) 102_556 . 2_555 N
Cl D1 C 168.29(27) 102_556 . -2_565 N
Cl D1 D2 76.9(4) 102_556 . 1_555 N
O D1 O 116.80(34) 1_555 . 1_556 N
O D1 C 40.85(33) 1_555 . 1_555 N
O D1 C 69.68(33) 1_555 . 2_555 N
O D1 C 33.05(18) 1_555 . -2_565 N
O D1 D2 64.23(30) 1_555 . 1_555 N
O D1 C 135.6(5) 1_556 . 1_555 N
O D1 C 101.77(32) 1_556 . 2_555 N
O D1 C 83.98(23) 1_556 . -2_565 N
O D1 D2 166.5(4) 1_556 . 1_555 N
C D1 C 40.93(33) 1_555 . 2_555 N
C D1 C 63.7(4) 1_555 . -2_565 N
C D1 D2 35.91(31) 1_555 . 1_555 N
C D1 C 70.86(23) 2_555 . -2_565 N
C D1 D2 65.48(33) 2_555 . 1_555 N
C D1 D2 95.15(34) -2_565 . 1_555 N
Cl D2 Cl 93.41(18) 102_555 . 102_556 N
Cl D2 O 130.6(4) 102_555 . 1_555 N
Cl D2 C 168.6(5) 102_555 . 1_555 N
Cl D2 C 133.4(4) 102_555 . 2_555 N
Cl D2 D1 155.3(5) 102_555 . 1_555 N
Cl D2 O 132.4(4) 102_556 . 1_555 N
Cl D2 C 97.1(4) 102_556 . 1_555 N
Cl D2 C 93.75(29) 102_556 . 2_555 N
Cl D2 D1 67.5(4) 102_556 . 1_555 N
O D2 C 41.53(29) 1_555 . 1_555 N
O D2 C 70.17(29) 1_555 . 2_555 N
O D2 D1 65.05(33) 1_555 . 1_555 N
C D2 C 41.53(30) 1_555 . 2_555 N
C D2 D1 35.89(28) 1_555 . 1_555 N
C D2 D1 66.18(31) 2_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC9
_database_code_depnum_ccdc_archive 'CCDC 2255400'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT155_BF_phase_1          
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: Original Cell produced from Indexing Retained
;
# Added during the CSD deposition process: Tuesday 11 April 2023 02:37 PM
# end Validation Reply Form


_pd_block_id                     2019-09-06T11:45|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-06T11:45|BF_H_01|WGM|pearl

#==============================================================================

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   'Form III P-1 trial'
_cell_length_a                   8.5610(6)
_cell_length_b                   6.4162(6)
_cell_length_c                   3.82603(27)
_cell_angle_alpha                91.769(7)
_cell_angle_beta                 78.002(6)
_cell_angle_gamma                101.453(5)
_cell_volume                     201.464(17)
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                5163000
_pd_prep_temperature             295
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     51
_refine_ls_goodness_of_fit_all   1.14
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0281
_pd_proc_ls_prof_wR_factor       0.0241
_pd_proc_ls_prof_wR_expected     0.0215
_refine_ls_R_Fsqd_factor         0.11126

_exptl_crystal_description       needle
_chemical_formula_sum            'C2 D4 Cl I O'
_chemical_formula_weight         210.43
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -P 1'
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    3.469
_diffrn_measurement_pressure     5163000

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
-1 -x,-y,-z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I1 0.7211(12) 0.5259(16) 0.5222(26) 1.0 Uiso 0.0083(9) 2
Cl Cl1 0.5613(6) 0.2061(8) 0.8000(16) 1.0 Uiso 0.0165(17) 2
O O 0.09576(27) 0.14638(32) -0.2595(6) 1.0 Uiso 0.0125(25) 2
C C1 -0.04307(27) 0.20057(18) -0.0131(8) 1.0 Uiso 0.0131(15) 2
C C2 0.16825(6) -0.0006(4) -0.0946(8) 1.0 Uiso 0.0131(15) 2
D D1 -0.0018(4) 0.27943(28) 0.2195(10) 1.0 Uiso 0.0355(16) 2
D D2 -0.0916(5) 0.3117(4) -0.1518(13) 1.0 Uiso 0.0355(16) 2
D D3 0.21113(26) 0.0755(6) 0.1381(12) 1.0 Uiso 0.0355(16) 2
D D4 0.27019(23) -0.0338(6) -0.2946(13) 1.0 Uiso 0.0355(16) 2

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 2.0
Cl 2.0
C 4.0
O 2.0
D 8.0


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 I1 3.773(20) . -1_666 N
I1 Cl1 2.372(10) . 1_555 N
I1 O 2.461(10) . -1_665 N
I1 D1 2.834(11) . -1_666 N
I1 D2 2.797(10) . 1_656 N
I1 D3 2.843(11) . -1_666 N
Cl1 I1 2.372(10) . 1_555 N
Cl1 Cl1 2.986(10) . -1_657 N
Cl1 D4 2.744(7) . 1_556 N
Cl1 D4 2.526(7) . -1_655 N
O I1 2.461(10) . -1_665 N
O C1 1.44929(12) . 1_555 N
O C2 1.45079(10) . 1_555 N
O D1 2.08202(17) . 1_555 N
O D2 2.05968(14) . 1_555 N
O D3 2.08372(14) . 1_555 N
O D4 2.04394(13) . 1_555 N
C1 O 1.44929(12) . 1_555 N
C1 C2 1.50577(13) . -1_555 N
C1 D1 1.09748(8) . 1_555 N
C1 D2 1.09366(8) . 1_555 N
C1 D3 2.15854(17) . -1_555 N
C1 D4 2.14740(19) . -1_555 N
C2 O 1.45079(10) . 1_555 N
C2 C1 1.50577(13) . -1_555 N
C2 D1 2.16275(17) . -1_555 N
C2 D2 2.15484(20) . -1_555 N
C2 D3 1.09726(8) . 1_555 N
C2 D4 1.08576(9) . 1_555 N
D1 I1 2.834(11) . -1_666 N
D1 O 2.08202(17) . 1_555 N
D1 C1 1.09748(8) . 1_555 N
D1 C2 2.16275(17) . -1_555 N
D1 D2 1.78556(12) . 1_555 N
D2 I1 2.797(10) . 1_454 N
D2 O 2.05968(14) . 1_555 N
D2 C1 1.09366(8) . 1_555 N
D2 C2 2.15484(20) . -1_555 N
D2 D1 1.78556(12) . 1_555 N
D3 I1 2.843(11) . -1_666 N
D3 O 2.08372(14) . 1_555 N
D3 C1 2.15854(17) . -1_555 N
D3 C2 1.09726(8) . 1_555 N
D3 D4 1.79177(14) . 1_555 N
D4 Cl1 2.744(7) . 1_554 N
D4 Cl1 2.526(7) . -1_655 N
D4 O 2.04394(13) . 1_555 N
D4 C1 2.14740(19) . -1_555 N
D4 C2 1.08576(9) . 1_555 N
D4 D3 1.79177(14) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 I1 O 175.3(5) 1_555 . -1_665 N
Cl1 I1 D2 69.22(27) 1_555 . 1_656 N
O I1 D2 106.2(4) -1_665 . 1_656 N
I1 Cl1 Cl1 165.5(4) 1_555 . -1_657 N
I1 Cl1 D4 83.38(27) 1_555 . -1_655 N
Cl1 Cl1 D4 91.89(25) -1_657 . -1_655 N
I1 O C1 109.43(29) -1_665 . 1_555 N
I1 O C2 116.70(28) -1_665 . 1_555 N
C1 O C2 110.886(6) 1_555 . 1_555 N
O C1 C2 108.942(7) 1_555 . -1_555 N
O C1 D1 108.890(6) 1_555 . 1_555 N
O C1 D2 107.358(6) 1_555 . 1_555 N
C2 C1 D1 111.395(6) -1_555 . 1_555 N
C2 C1 D2 110.993(6) -1_555 . 1_555 N
D1 C1 D2 109.155(6) 1_555 . 1_555 N
O C2 C1 109.016(6) 1_555 . -1_555 N
O C2 D3 108.935(6) 1_555 . 1_555 N
O C2 D4 106.486(6) 1_555 . 1_555 N
C1 C2 D3 111.070(6) -1_555 . 1_555 N
C1 C2 D4 110.875(7) -1_555 . 1_555 N
D3 C2 D4 110.324(6) 1_555 . 1_555 N
C1 D1 D2 35.351(4) 1_555 . 1_555 N
I1 D2 C1 167.20(22) 1_454 . 1_555 N
I1 D2 D1 149.56(30) 1_454 . 1_555 N
C1 D2 D1 35.494(4) 1_555 . 1_555 N
C2 D3 D4 34.628(4) 1_555 . 1_555 N
Cl1 D4 C2 161.93(24) -1_655 . 1_555 N
Cl1 D4 D3 158.79(27) -1_655 . 1_555 N
C2 D4 D3 35.0480(35) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC10
_database_code_depnum_ccdc_archive 'CCDC 2255395'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-06T10:56|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-06T10:56|BF_H_01|WGM|PEARL

#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products


_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?


_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.3487(7)
_cell_length_b                   7.8162(7)
_cell_length_c                   4.0826(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 97.622(10)
_cell_angle_gamma                90.0
_cell_volume                     453.83(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0433
_pd_proc_ls_prof_wR_factor       0.0363
_pd_proc_ls_prof_wR_expected     0.0367
_refine_ls_R_Fsqd_factor         0.18285

_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     54
_refine_ls_goodness_of_fit_all   1.01
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full
_pd_prep_cool_rate               ?
_pd_prep_pressure                2159000
_pd_prep_temperature             ?

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    3.080
_diffrn_measurement_pressure     3159000

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2443(9) 0.5 0.722(4) 1.0 Uiso 0.0208(15) 4
Cl Cl 0.3992(5) 0.5 0.5708(22) 1.0 Uiso 0.0416(30) 4
O O 0.0776(7) 0.5 -0.1771(21) 1.0 Uiso 0.015(4) 4
C C 0.05235(19) 0.6495(6) -0.0076(11) 1.0 Uiso 0.0270(27) 8
D D1 0.0911(5) 0.6511(11) 0.2413(17) 1.0 Uiso 0.0502(30) 8
D D2 0.0715(5) 0.7618(8) -0.1440(19) 1.0 Uiso 0.0502(30) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0



# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.384(16) . 1_555 N
I O 2.481(17) . 1_556 N
Cl I 2.384(16) . 1_555 N
Cl Cl 3.025(15) . 2_656 N
Cl D2 2.622(9) . 102_545 N
Cl D2 2.622(9) . -101_565 N
O I 2.481(17) . 1_554 N
O C 1.429(5) . 1_555 N
O C 1.429(5) . -2_565 N
O D1 2.064(8) . 1_555 N
O D1 2.064(8) . -2_565 N
O D2 2.053(6) . 1_555 N
O D2 2.053(6) . -2_565 N
C O 1.429(5) . 1_555 N
C C 1.512(5) . 2_555 N
C D1 1.092(5) . 1_555 N
C D2 1.094(5) . 1_555 N
D1 O 2.064(8) . 1_555 N
D1 C 1.092(5) . 1_555 N
D1 D2 1.785(8) . 1_555 N
D2 Cl 2.622(9) . 102_555 N
D2 O 2.053(6) . 1_555 N
D2 C 1.094(5) . 1_555 N
D2 D1 1.785(8) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 174.5(7) 1_555 . 1_556 N
I Cl Cl 176.0(6) 1_555 . 2_656 N
I O C 113.1(4) 1_554 . 1_555 N
I O C 113.1(4) 1_554 . -2_565 N
C O C 109.7(5) 1_555 . -2_565 N
O C C 109.7(4) 1_555 . 2_555 N
O C D1 109.2(5) 1_555 . 1_555 N
O C D2 108.2(4) 1_555 . 1_555 N
C C D1 110.4(5) 2_555 . 1_555 N
C C D2 109.8(4) 2_555 . 1_555 N
D1 C D2 109.5(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_48_TONS_A_phase_1
_database_code_depnum_ccdc_archive 'CCDC 2255398'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_48_TONS_A_phase_1   
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.05
RESPONSE: ...The value is 0.06 i.e. > 0.05 but see V. K. Pecharsky and P. Y. Zayalij Fundamentals of Powder Diffraction and Structural Characterization of materials 2nd edition 2009 Springer p 641 footnote 22 IUCR imposes the requirement shift/error
;
_vrf_PLAT080_48_TONS_A_phase_1   
;
PROBLEM: Maximum Shift/Error ............................       0.06 Why ?
RESPONSE: ...The value is 0.06 i.e. > 0.05 but see V. K. Pecharsky and P. Y. Zayalij Fundamentals of Powder Diffraction and Structural Characterization of materials 2nd edition 2009 Springer p 641 footnote 22 IUCR imposes the requirement shift/error
;
_vrf_PLAT155_48_TONS_A_phase_1   
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: Orginal cell from indexing has been retained
;
# Added during the CSD deposition process: Tuesday 11 April 2023 02:31 PM
# end Validation Reply Form


_pd_block_id                     2019-09-03T15:35|48_TONS_A_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-03T15:35|48_TONS_A_H_01|WGM|PEARL

#==============================================================================

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   'Le Bail in P-1'
_cell_length_a                   7.7483(6)
_cell_length_b                   7.5293(6)
_cell_length_c                   3.86317(28)
_cell_angle_alpha                91.598(9)
_cell_angle_beta                 91.492(7)
_cell_angle_gamma                107.613(6)
_cell_volume                     214.585(19)
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_refine_ls_shift/su_max          0.06
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     36
_refine_ls_goodness_of_fit_all   1.36
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0364
_pd_proc_ls_prof_wR_factor       0.0310
_pd_proc_ls_prof_wR_expected     0.0232
_refine_ls_R_Fsqd_factor         0.05597

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            1
_symmetry_space_group_name_Hall  ' -P 1 '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C4 D8 Cl2 I2 O2'
_exptl_crystal_density_diffrn    3.256
_diffrn_measurement_pressure     3487000
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
-1 -x,-y,-z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Cl Cl 0.4168(10) 0.7904(10) -0.4705(20) 1.0 Uiso 0.0164(23) 2
I I 0.2655(15) 0.4835(16) -0.317(4) 1.0 Uiso 0.0082(11) 2
O O 0.0975(4) 0.16578(34) -0.1493(12) 1.0 Uiso 0.0153(16) 2
C C1 -0.07410(35) 0.14986(25) 0.0079(13) 1.0 Uiso 0.0153(16) 2
C C2 0.190905(24 0.0505(4) 0.0226(10) 1.0 Uiso 0.0153(16) 2
D D1 -0.0483(6) 0.1994(6) 0.2798(15) 1.0 Uiso 0.0303(22) 2
D D2 -0.1372(6) 0.2400(5) -0.1314(21) 1.0 Uiso 0.0303(22) 2
D D3 0.2188(4) 0.0983(7) 0.2951(12) 1.0 Uiso 0.0303(22) 2
D D4 0.31682(20) 0.0693(7) -0.1095(17) 1.0 Uiso 0.0303(22) 2

loop_
_atom_type_symbol
_atom_type_number_in_cell
Cl 2.0
I 2.0
C 4.0
O 2.0
D 8.0

# If you change Z, be sure to change all 3 of the following

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl Cl 3.86317(28) . 1_554 N
Cl Cl 3.86317(28) . 1_556 N
Cl Cl 3.044(14) . -1_674 N
Cl I 3.893(16) . 1_554 N
Cl I 2.353(13) . 1_555 N
Cl I 3.751(12) . -1_664 N
Cl D2 2.573(8) . -1_564 N
Cl D3 2.752(8) . -1_665 N
Cl D4 2.798(10) . 1_565 N
Cl D4 2.638(8) . -1_664 N
Cl D4 2.950(8) . -1_665 N
I Cl 2.353(13) . 1_555 N
I Cl 3.893(16) . 1_556 N
I Cl 3.751(12) . -1_664 N
I O 2.467(11) . 1_555 N
O I 2.467(11) . 1_555 N
O C1 1.44929(11) . 1_555 N
O C2 1.45080(11) . 1_555 N
O D2 2.05968(14) . 1_555 N
O D4 2.04394(14) . 1_555 N
C1 O 1.44929(11) . 1_555 N
C1 C2 1.50577(13) . -1_555 N
C1 D1 1.09748(9) . 1_555 N
C1 D2 1.09365(8) . 1_555 N
C2 O 1.45080(11) . 1_555 N
C2 C1 1.50577(13) . -1_555 N
C2 D3 1.09726(9) . 1_555 N
C2 D4 1.08576(9) . 1_555 N
D1 C1 1.09748(9) . 1_555 N
D1 D2 1.78556(13) . 1_555 N
D2 Cl 2.573(8) . -1_564 N
D2 O 2.05968(14) . 1_555 N
D2 C1 1.09365(8) . 1_555 N
D2 D1 1.78556(13) . 1_555 N
D3 Cl 2.752(8) . -1_665 N
D3 C2 1.09726(9) . 1_555 N
D3 D4 1.79177(13) . 1_555 N
D4 Cl 2.798(10) . 1_545 N
D4 Cl 2.638(8) . -1_664 N
D4 Cl 2.950(8) . -1_665 N
D4 O 2.04394(14) . 1_555 N
D4 C2 1.08576(9) . 1_555 N
D4 D3 1.79177(13) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl Cl Cl 180.0 1_554 . 1_556 N
Cl Cl Cl 83.40(29) 1_554 . -1_674 N
Cl Cl I 35.32(20) 1_554 . 1_554 N
Cl Cl I 107.0(4) 1_554 . 1_555 N
Cl Cl I 77.27(23) 1_554 . -1_664 N
Cl Cl D2 55.01(24) 1_554 . -1_564 N
Cl Cl D3 102.18(16) 1_554 . -1_665 N
Cl Cl D4 49.72(18) 1_554 . -1_664 N
Cl Cl Cl 96.60(29) 1_556 . -1_674 N
Cl Cl I 144.68(20) 1_556 . 1_554 N
Cl Cl I 73.0(4) 1_556 . 1_555 N
Cl Cl I 102.73(23) 1_556 . -1_664 N
Cl Cl D2 124.99(24) 1_556 . -1_564 N
Cl Cl D3 77.82(16) 1_556 . -1_665 N
Cl Cl D4 130.28(18) 1_556 . -1_664 N
Cl Cl I 118.5(4) -1_674 . 1_554 N
Cl Cl I 168.2(6) -1_674 . 1_555 N
Cl Cl I 113.7(4) -1_674 . -1_664 N
Cl Cl D2 96.1(4) -1_674 . -1_564 N
Cl Cl D3 68.66(32) -1_674 . -1_665 N
Cl Cl D4 58.49(28) -1_674 . -1_664 N
I Cl I 71.6(4) 1_554 . 1_555 N
I Cl I 67.88(34) 1_554 . -1_664 N
I Cl D2 52.10(25) 1_554 . -1_564 N
I Cl D3 116.68(26) 1_554 . -1_665 N
I Cl D4 76.57(23) 1_554 . -1_664 N
I Cl I 74.9(4) 1_555 . -1_664 N
I Cl D2 85.7(4) 1_555 . -1_564 N
I Cl D3 113.3(4) 1_555 . -1_665 N
I Cl D4 132.6(5) 1_555 . -1_664 N
I Cl D2 119.98(34) -1_664 . -1_564 N
I Cl D3 55.27(23) -1_664 . -1_665 N
I Cl D4 60.88(23) -1_664 . -1_664 N
D2 Cl D3 154.99(34) -1_564 . -1_665 N
D2 Cl D4 101.54(26) -1_564 . -1_664 N
D3 Cl D4 53.78(16) -1_665 . -1_664 N
Cl I Cl 71.6(4) 1_555 . 1_556 N
Cl I Cl 105.1(4) 1_555 . -1_664 N
Cl I O 177.9(6) 1_555 . 1_555 N
Cl I Cl 112.12(34) 1_556 . -1_664 N
Cl I O 107.6(4) 1_556 . 1_555 N
Cl I O 77.01(32) -1_664 . 1_555 N
I O C1 114.6(4) 1_555 . 1_555 N
I O C2 120.5(4) 1_555 . 1_555 N
C1 O C2 110.886(6) 1_555 . 1_555 N
O C1 C2 108.942(7) 1_555 . -1_555 N
O C1 D1 108.890(7) 1_555 . 1_555 N
O C1 D2 107.358(6) 1_555 . 1_555 N
C2 C1 D1 111.395(9) -1_555 . 1_555 N
C2 C1 D2 110.993(7) -1_555 . 1_555 N
D1 C1 D2 109.156(6) 1_555 . 1_555 N
O C2 C1 109.016(7) 1_555 . -1_555 N
O C2 D3 108.935(6) 1_555 . 1_555 N
O C2 D4 106.486(6) 1_555 . 1_555 N
C1 C2 D3 111.070(9) -1_555 . 1_555 N
C1 C2 D4 110.875(7) -1_555 . 1_555 N
D3 C2 D4 110.324(7) 1_555 . 1_555 N
Cl D2 C1 138.82(26) -1_564 . 1_555 N
Cl D3 C2 112.40(25) -1_665 . 1_555 N
Cl D4 C2 159.44(31) -1_664 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC11
_database_code_depnum_ccdc_archive 'CCDC 2255397'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-06T11:09|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-06T11:09|BF_H_01|WGM|PEARL

#==============================================================================


#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.2850(7)
_cell_length_b                   7.7770(7)
_cell_length_c                   4.0372(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 98.018(10)
_cell_angle_gamma                90.0
_cell_volume                     444.13(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

# Load in tons 39 tons

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     54
_refine_ls_goodness_of_fit_all   1.01
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0465
_pd_proc_ls_prof_wR_factor       0.0370
_pd_proc_ls_prof_wR_expected     0.0373
_refine_ls_R_Fsqd_factor         0.16188

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    3.147
_diffrn_measurement_pressure     2637000

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2427(9) 0.5 0.7247(35) 1.0 Uiso 0.0159(14) 4
Cl Cl 0.3999(5) 0.5 0.5816(22) 1.0 Uiso 0.0318(27) 4
O O 0.0776(7) 0.5 -0.1798(20) 1.0 Uiso 0.016(4) 4
C C 0.05264(19) 0.6505(6) -0.0079(11) 1.0 Uiso 0.0163(23) 8
D D1 0.0923(5) 0.6526(11) 0.2432(16) 1.0 Uiso 0.0388(27) 8
D D2 0.0720(5) 0.7630(8) -0.1432(18) 1.0 Uiso 0.0388(27) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.396(15) . 1_555 N
I O 2.442(16) . 1_556 N
Cl I 2.396(15) . 1_555 N
Cl Cl 3.022(15) . 2_656 N
Cl D2 2.624(9) . 102_545 N
Cl D2 2.624(9) . -101_565 N
O I 2.442(16) . 1_554 N
O C 1.431(5) . 1_555 N
O C 1.431(5) . -2_565 N
O D1 2.066(8) . 1_555 N
O D1 2.066(8) . -2_565 N
O D2 2.053(6) . 1_555 N
O D2 2.053(6) . -2_565 N
C O 1.431(5) . 1_555 N
C C 1.514(5) . 2_555 N
C D1 1.090(5) . 1_555 N
C D2 1.087(5) . 1_555 N
D1 O 2.066(8) . 1_555 N
D1 C 1.090(5) . 1_555 N
D1 D2 1.769(8) . 1_555 N
D2 Cl 2.624(9) . 102_555 N
D2 O 2.053(6) . 1_555 N
D2 C 1.087(5) . 1_555 N
D2 D1 1.769(8) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 175.2(7) 1_555 . 1_556 N
I Cl Cl 178.7(6) 1_555 . 2_656 N
I O C 112.8(4) 1_554 . 1_555 N
I O C 112.8(4) 1_554 . -2_565 N
C O C 109.8(5) 1_555 . -2_565 N
O C C 109.7(4) 1_555 . 2_555 N
O C D1 109.3(5) 1_555 . 1_555 N
O C D2 108.5(4) 1_555 . 1_555 N
C C D1 110.6(5) 2_555 . 1_555 N
C C D2 110.2(4) 2_555 . 1_555 N
D1 C D2 108.6(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC12
_database_code_depnum_ccdc_archive 'CCDC 2255401'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT155_BF_phase_1          
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: Original Cell produced from Indexing Retained
;
# Added during the CSD deposition process: Tuesday 11 April 2023 02:37 PM
# end Validation Reply Form


_pd_block_id                     2019-09-06T12:01|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-06T12:01|BF_H_01|WGM|PEARL

#==============================================================================



#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   'Dioxane-(ICl)2 form III (P-1)'
_cell_length_a                   8.5174(6)
_cell_length_b                   6.3686(5)
_cell_length_c                   3.79126(25)
_cell_angle_alpha                92.061(7)
_cell_angle_beta                 78.263(6)
_cell_angle_gamma                101.408(5)
_cell_volume                     197.373(16)
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                6007000
_pd_prep_temperature             ?
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     51
_refine_ls_goodness_of_fit_all   1.06
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0299
_pd_proc_ls_prof_wR_factor       0.0249
_pd_proc_ls_prof_wR_expected     0.0238
_refine_ls_R_Fsqd_factor         0.08491

_exptl_crystal_description       needle
_chemical_formula_sum            'C2 D4 Cl I O'
_chemical_formula_weight         210.43
_cell_formula_units_Z            2.0
_symmetry_space_group_name_Hall  '-P 1 '
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_diffrn_measurement_device_type  PEARL
_exptl_crystal_density_diffrn    3.541
_diffrn_measurement_pressure     6007000

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
-1 -x,-y,-z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.7177(12) 0.5280(16) 0.5214(26) 1.0 Uiso 0.0075(9) 2
Cl Cl 0.5608(7) 0.2076(9) 0.8083(15) 1.0 Uiso 0.0149(17) 2
O O 0.09636(28) 0.14636(35) -0.2608(7) 1.0 Uiso 0.0077(24) 2
C C1 -0.04225(28) 0.20278(18) -0.0125(8) 1.0 Uiso 0.0119(14) 2
C C2 0.16864(6) -0.0025(4) -0.0948(9) 1.0 Uiso 0.0119(14) 2
D D1 -0.0001(4) 0.28217(30) 0.2225(11) 1.0 Uiso 0.0318(16) 2
D D2 -0.0906(5) 0.3153(5) -0.1521(14) 1.0 Uiso 0.0318(16) 2
D D3 0.21241(26) 0.0742(6) 0.1403(12) 1.0 Uiso 0.0318(16) 2
D D4 0.27042(24) -0.0373(6) -0.2964(13) 1.0 Uiso 0.0318(16) 2

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 2.0
Cl 2.0
C 4.0
O 2.0
D 8.0


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I I 3.79126(25) . 1_554 N
I I 3.79126(25) . 1_556 N
I I 3.691(20) . -1_666 N
I Cl 2.371(11) . 1_555 N
I O 2.449(10) . -1_665 N
I D1 2.811(10) . -1_666 N
I D2 2.802(10) . 1_656 N
I D3 2.811(11) . -1_666 N
Cl I 2.371(11) . 1_555 N
Cl Cl 2.960(10) . -1_657 N
Cl D4 2.745(7) . 1_556 N
Cl D4 2.518(7) . -1_655 N
O I 2.449(10) . -1_665 N
O C1 1.44929(11) . 1_555 N
O C2 1.45079(9) . 1_555 N
O D1 2.08202(16) . 1_555 N
O D2 2.05968(14) . 1_555 N
O D3 2.08372(13) . 1_555 N
O D4 2.04394(13) . 1_555 N
C1 O 1.44929(11) . 1_555 N
C1 C2 1.50577(12) . -1_555 N
C1 D1 1.09748(8) . 1_555 N
C1 D2 1.09365(7) . 1_555 N
C1 D3 2.15854(16) . -1_555 N
C1 D4 2.14741(18) . -1_555 N
C2 O 1.45079(9) . 1_555 N
C2 C1 1.50577(12) . -1_555 N
C2 D1 2.16275(16) . -1_555 N
C2 D2 2.15484(19) . -1_555 N
C2 D3 1.09726(8) . 1_555 N
C2 D4 1.08576(8) . 1_555 N
D1 I 2.811(10) . -1_666 N
D1 O 2.08202(16) . 1_555 N
D1 C1 1.09748(8) . 1_555 N
D1 C2 2.16275(16) . -1_555 N
D1 D2 1.78556(11) . 1_555 N
D2 I 2.802(10) . 1_454 N
D2 O 2.05968(14) . 1_555 N
D2 C1 1.09365(7) . 1_555 N
D2 C2 2.15484(19) . -1_555 N
D2 D1 1.78556(11) . 1_555 N
D3 I 2.811(11) . -1_666 N
D3 O 2.08372(13) . 1_555 N
D3 C1 2.15854(16) . -1_555 N
D3 C2 1.09726(8) . 1_555 N
D3 D4 1.79177(13) . 1_555 N
D4 Cl 2.745(7) . 1_554 N
D4 Cl 2.518(7) . -1_655 N
D4 O 2.04394(13) . 1_555 N
D4 C1 2.14741(18) . -1_555 N
D4 C2 1.08576(8) . 1_555 N
D4 D3 1.79177(13) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.6(5) 1_555 . -1_665 N
I Cl Cl 166.7(4) 1_555 . -1_657 N
I Cl D4 130.6(4) 1_555 . 1_556 N
I Cl D4 82.50(27) 1_555 . -1_655 N
Cl Cl D4 61.37(23) -1_657 . 1_556 N
Cl Cl D4 91.58(26) -1_657 . -1_655 N
D4 Cl D4 93.69(21) 1_556 . -1_655 N
I O C1 109.76(29) -1_665 . 1_555 N
I O C2 116.22(28) -1_665 . 1_555 N
C1 O C2 110.886(5) 1_555 . 1_555 N
O C1 C2 108.942(7) 1_555 . -1_555 N
O C1 D1 108.890(5) 1_555 . 1_555 N
O C1 D2 107.358(5) 1_555 . 1_555 N
C2 C1 D1 111.395(6) -1_555 . 1_555 N
C2 C1 D2 110.993(6) -1_555 . 1_555 N
D1 C1 D2 109.156(6) 1_555 . 1_555 N
O C2 C1 109.016(6) 1_555 . -1_555 N
O C2 D3 108.935(6) 1_555 . 1_555 N
O C2 D4 106.486(5) 1_555 . 1_555 N
C1 C2 D3 111.070(6) -1_555 . 1_555 N
C1 C2 D4 110.875(7) -1_555 . 1_555 N
D3 C2 D4 110.324(5) 1_555 . 1_555 N
C1 D1 D2 35.3511(34) 1_555 . 1_555 N
C1 D2 D1 35.4933(34) 1_555 . 1_555 N
C2 D3 D4 34.6279(34) 1_555 . 1_555 N
Cl D4 Cl 86.31(21) 1_554 . -1_655 N
Cl D4 C2 110.99(21) 1_554 . 1_555 N
Cl D4 D3 77.83(22) 1_554 . 1_555 N
Cl D4 C2 162.52(26) -1_655 . 1_555 N
Cl D4 D3 158.86(27) -1_655 . 1_555 N
C2 D4 D3 35.0480(34) 1_555 . 1_555 N
####################################################################### 
# 
# 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_ZERO_phase_1
_database_code_depnum_ccdc_archive 'CCDC 2255524'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2023-04-05T15:09|ZERO_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2023-04-05T15:09|ZERO_H_01|WGM|PEARL

#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products
_symmetry_space_group_name_Hall  ?

_exptl_crystal_F_000             ?
_exptl_crystal_density_diffrn    ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_cell_measurement_temperature    297
_diffrn_ambient_temperature      297
_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.6723(7)
_cell_length_b                   8.0720(4)
_cell_length_c                   4.58002(27)
_cell_angle_alpha                90.0
_cell_angle_beta                 95.535(6)
_cell_angle_gamma                90.0
_cell_volume                     539.91(4)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2408(8) 0.5 0.7218(29) 1.0 Uiso 0.023(4) 4
Cl Cl 0.3879(5) 0.5 0.5551(19) 1.0 Uiso 0.061(4) 4
O O 0.0758(8) 0.5 -0.1602(22) 1.0 Uiso 0.057(5) 4
C C 0.05025(23) 0.6462(7) -0.0164(12) 1.0 Uiso 0.072(4) 8
D D1 0.0869(5) 0.6540(13) 0.2015(19) 1.0 Uiso 0.095(4) 8
D D2 0.0665(6) 0.7504(9) -0.1389(20) 1.0 Uiso 0.095(4) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C2.00 D4 Cl I O'
_chemical_formula_weight         210.43
_cell_formula_units_Z            4

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.358(16) . 1_555 N
I O 2.531(17) . 1_556 N
Cl I 2.358(16) . 1_555 N
Cl Cl 3.375(14) . 2_656 N
O I 2.531(17) . 1_554 N
O C 1.419(6) . 1_555 N
O C 1.419(6) . -2_565 N
O D1 2.065(10) . 1_555 N
O D1 2.065(10) . -2_565 N
O D2 2.029(7) . 1_555 N
O D2 2.029(7) . -2_565 N
C O 1.419(6) . 1_555 N
C C 1.497(6) . 2_555 N
C D1 1.089(7) . 1_555 N
C D2 1.051(7) . 1_555 N
C D2 2.094(9) . 2_555 N
D1 O 2.065(10) . 1_555 N
D1 C 1.089(7) . 1_555 N
D1 D2 1.742(11) . 1_555 N
D2 O 2.029(7) . 1_555 N
D2 C 1.051(7) . 1_555 N
D2 C 2.094(9) . 2_555 N
D2 D1 1.742(11) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.5(8) 1_555 . 1_556 N
I O C 113.6(5) 1_554 . 1_555 N
I O C 113.6(5) 1_554 . -2_565 N
C O C 112.4(7) 1_555 . -2_565 N
O C C 110.7(5) 1_555 . 2_555 N
O C D1 110.1(6) 1_555 . 1_555 N
O C D2 109.5(5) 1_555 . 1_555 N
C C D1 108.2(6) 2_555 . 1_555 N
C C D2 109.3(6) 2_555 . 1_555 N
D1 C D2 108.9(7) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC13
_database_code_depnum_ccdc_archive 'CCDC 2255521'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-05T22:33|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-05T22:33|BF_H_01|WGM|PEARL


#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products


_exptl_crystal_F_000             ?
_exptl_crystal_density_diffrn    2.637
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?



_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.6472(10)
_cell_length_b                   8.0430(6)
_cell_length_c                   4.5209(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 95.742(9)
_cell_angle_gamma                90.0
_cell_volume                     529.92(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                132000
_pd_prep_temperature             297
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.05
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full


_pd_proc_ls_prof_R_factor        0.0380
_pd_proc_ls_prof_wR_factor       0.0335
_pd_proc_ls_prof_wR_expected     0.0325
_refine_ls_R_Fsqd_factor         0.25831

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      297
_diffrn_measurement_pressure     132000
_cell_measurement_temperature    297
_cell_measurement.pressure       132000
_pd_char_colour                  orange
_diffrn_radiation_type           neutron
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2411(10) 0.5 0.724(4) 1.0 Uiso 0.0280(21) 4
Cl Cl 0.3896(6) 0.5 0.5600(24) 1.0 Uiso 0.056(4) 4
O O 0.0769(8) 0.5 -0.1644(23) 1.0 Uiso 0.050(6) 4
C C 0.05099(20) 0.6477(7) -0.0136(12) 1.0 Uiso 0.073(5) 8
D D1 0.0881(5) 0.6564(14) 0.2089(20) 1.0 Uiso 0.097(5) 8
D D2 0.0677(6) 0.7531(9) -0.1417(23) 1.0 Uiso 0.097(5) 8
loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0

# If you change Z, be sure to change all 3 of the following


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.367(19) . 1_555 N
I O 2.507(20) . 1_556 N
Cl I 2.367(19) . 1_555 N
Cl Cl 3.333(16) . 2_656 N
O I 2.507(20) . 1_554 N
O C 1.439(5) . 1_555 N
O C 1.439(5) . -2_565 N
O D2 2.044(7) . 1_555 N
O D2 2.044(7) . -2_565 N
C O 1.439(5) . 1_555 N
C C 1.511(6) . 2_555 N
C D1 1.096(6) . 1_555 N
C D2 1.069(6) . 1_555 N
D1 C 1.096(6) . 1_555 N
D1 D2 1.764(9) . 1_555 N
D2 O 2.044(7) . 1_555 N
D2 C 1.069(6) . 1_555 N
D2 D1 1.764(9) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.5(9) 1_555 . 1_556 N
I Cl Cl 171.2(8) 1_555 . 2_656 N
I O C 113.5(5) 1_554 . 1_555 N
I O C 113.5(5) 1_554 . -2_565 N
C O C 111.3(6) 1_555 . -2_565 N
O C C 110.4(5) 1_555 . 2_555 N
O C D1 110.9(5) 1_555 . 1_555 N
O C D2 108.2(5) 1_555 . 1_555 N
C C D1 109.2(5) 2_555 . 1_555 N
C C D2 109.1(5) 2_555 . 1_555 N
D1 C D2 109.1(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC14
_database_code_depnum_ccdc_archive 'CCDC 2255522'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-05T22:37|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-05T22:37|BF_H_01|WGM|PEARL




#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and


_exptl_crystal_F_000             ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?



_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.6273(10)
_cell_length_b                   8.0214(6)
_cell_length_c                   4.4725(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 95.883(9)
_cell_angle_gamma                90.0
_cell_volume                     522.01(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                239000
_pd_prep_temperature             ?
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.00
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_exptl_crystal_density_diffrn    2.677
_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_measurement_pressure     239000
_diffrn_ambient_temperature      295
_cell_measurement_temperature    295
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0391
_pd_proc_ls_prof_wR_factor       0.0338
_pd_proc_ls_prof_wR_expected     0.0346
_refine_ls_R_Fsqd_factor         0.25067

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2429(11) 0.5 0.734(4) 1.0 Uiso 0.0261(20) 4
Cl Cl 0.3906(6) 0.5 0.5635(24) 1.0 Uiso 0.052(4) 4
O O 0.0765(8) 0.5 -0.1679(23) 1.0 Uiso 0.046(6) 4
C C 0.05108(20) 0.6482(6) -0.0126(12) 1.0 Uiso 0.067(5) 8
D D1 0.0869(5) 0.6542(13) 0.2144(19) 1.0 Uiso 0.083(5) 8
D D2 0.0695(6) 0.7546(8) -0.1391(22) 1.0 Uiso 0.083(5) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0

# If you change Z, be sure to change all 3 of the following


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.363(19) . 1_555 N
I O 2.518(19) . 1_556 N
Cl I 2.363(19) . 1_555 N
Cl Cl 3.308(16) . 2_656 N
O I 2.518(19) . 1_554 N
O C 1.444(5) . 1_555 N
O C 1.444(5) . -2_565 N
O D2 2.049(7) . 1_555 N
O D2 2.049(7) . -2_565 N
C O 1.444(5) . 1_555 N
C C 1.510(5) . 2_555 N
C D1 1.094(6) . 1_555 N
C D2 1.074(6) . 1_555 N
D1 C 1.094(6) . 1_555 N
D1 D2 1.769(9) . 1_555 N
D2 O 2.049(7) . 1_555 N
D2 C 1.074(6) . 1_555 N
D2 D1 1.769(9) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 171.4(9) 1_555 . 1_556 N
I Cl Cl 171.2(8) 1_555 . 2_656 N
I O C 112.7(5) 1_554 . 1_555 N
I O C 112.7(5) 1_554 . -2_565 N
C O C 110.8(5) 1_555 . -2_565 N
O C C 109.9(4) 1_555 . 2_555 N
O C D1 111.1(5) 1_555 . 1_555 N
O C D2 108.0(4) 1_555 . 1_555 N
C C D1 108.3(5) 2_555 . 1_555 N
C C D2 110.1(5) 2_555 . 1_555 N
D1 C D2 109.4(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC15
_database_code_depnum_ccdc_archive 'CCDC 2255523'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-05T22:57|BF_phase1|WGM||



#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products


_exptl_crystal_F_000             ?

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?


_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.6065(9)
_cell_length_b                   7.9990(6)
_cell_length_c                   4.4168(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 96.019(9)
_cell_angle_gamma                90.0
_cell_volume                     513.20(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                395000
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.01
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      295
_exptl_crystal_density_diffrn    2.723
_diffrn_measurement_pressure     395000
_cell_measurement_temperature    295
_pd_char_colour                  orange
_diffrn_radiation_type           neutron
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_pd_proc_ls_prof_R_factor        0.0396
_pd_proc_ls_prof_wR_factor       0.0348
_pd_proc_ls_prof_wR_expected     0.0348
_refine_ls_R_Fsqd_factor         0.22228
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2429(11) 0.5 0.721(4) 1.0 Uiso 0.0206(19) 4
Cl Cl 0.3914(6) 0.5 0.5626(23) 1.0 Uiso 0.041(4) 4
O O 0.0771(7) 0.5 -0.1700(23) 1.0 Uiso 0.033(6) 4
C C 0.05143(21) 0.6477(6) -0.0123(12) 1.0 Uiso 0.051(4) 8
D D1 0.0878(5) 0.6519(13) 0.2157(19) 1.0 Uiso 0.066(4) 8
D D2 0.0699(7) 0.7563(9) -0.1392(21) 1.0 Uiso 0.066(4) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0


# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.347(19) . 1_555 N
I O 2.518(18) . 1_556 N
Cl I 2.347(19) . 1_555 N
Cl Cl 3.277(16) . 2_656 N
O I 2.518(18) . 1_554 N
O C 1.441(5) . 1_555 N
O C 1.441(5) . -2_565 N
O D2 2.058(7) . 1_555 N
O D2 2.058(7) . -2_565 N
C O 1.441(5) . 1_555 N
C C 1.518(6) . 2_555 N
C D1 1.089(6) . 1_555 N
C D2 1.083(6) . 1_555 N
D1 C 1.089(6) . 1_555 N
D1 D2 1.771(9) . 1_555 N
D2 O 2.058(7) . 1_555 N
D2 C 1.083(6) . 1_555 N
D2 D1 1.771(9) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.7(9) 1_555 . 1_556 N
I Cl Cl 172.4(8) 1_555 . 2_656 N
I O C 113.4(5) 1_554 . 1_555 N
I O C 113.4(5) 1_554 . -2_565 N
C O C 110.1(5) 1_555 . -2_565 N
O C C 110.2(4) 1_555 . 2_555 N
O C D1 110.2(5) 1_555 . 1_555 N
O C D2 108.4(4) 1_555 . 1_555 N
C C D1 108.9(5) 2_555 . 1_555 N
C C D2 109.8(5) 2_555 . 1_555 N
D1 C D2 109.3(5) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC16
_database_code_depnum_ccdc_archive 'CCDC 2255403'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT155_BF_phase_1          
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: Original Cell produced from Indexing Retained
;
# Added during the CSD deposition process: Tuesday 11 April 2023 02:38 PM
# end Validation Reply Form


_pd_block_id                     2019-09-06T12:48|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-06T12:48|BF_H_01|WGM|pearl

#==============================================================================


#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   'Dioxane-(ICl)2 form III (P-1)'
_cell_length_a                   8.4752(6)
_cell_length_b                   6.3247(6)
_cell_length_c                   3.75850(27)
_cell_angle_alpha                92.336(7)
_cell_angle_beta                 78.513(7)
_cell_angle_gamma                101.367(5)
_cell_volume                     193.559(17)
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

_pd_prep_cool_rate               ?
_pd_prep_pressure                6878000
_pd_prep_temperature             ?
_pd_char_colour                  orange
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     51
_refine_ls_goodness_of_fit_all   0.99
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_diffrn_radiation_probe          neutron
_pd_proc_ls_prof_R_factor        0.0313
_pd_proc_ls_prof_wR_factor       0.0263
_pd_proc_ls_prof_wR_expected     0.0269
_refine_ls_R_Fsqd_factor         0.11766

_exptl_crystal_description       needle
_chemical_formula_sum            'C2 D4 Cl I O'
_chemical_formula_weight         210.43
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -P 1'
_diffrn_ambient_temperature      297
_cell_measurement_temperature    297
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_diffrn_measurement_device_type  PEARL
_exptl_crystal_density_diffrn    3.610
_diffrn_measurement_pressure     6878000
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
-1 -x,-y,-z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.7166(12) 0.5271(16) 0.5301(27) 1.0 Uiso 0.0052(8) 2
Cl Cl 0.5593(7) 0.2107(10) 0.8100(14) 1.0 Uiso 0.0104(16) 2
O O 0.09605(30) 0.1463(4) -0.2630(7) 1.0 Uiso 0.0104(28) 2
C C1 -0.04225(30) 0.20438(20) -0.0119(8) 1.0 Uiso 0.0135(15) 2
C C2 0.16913(7) -0.0034(4) -0.0967(9) 1.0 Uiso 0.0135(15) 2
D D1 0.0011(5) 0.28490(30) 0.2247(11) 1.0 Uiso 0.0263(16) 2
D D2 -0.0913(5) 0.3175(5) -0.1520(13) 1.0 Uiso 0.0263(16) 2
D D3 0.21410(26) 0.0744(7) 0.1400(12) 1.0 Uiso 0.0263(16) 2
D D4 0.27062(25) -0.0394(7) -0.3004(13) 1.0 Uiso 0.0263(16) 2

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 2.0
Cl 2.0
C 4.0
O 2.0
D 8.0



# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I I 3.75850(27) . 1_554 N
I I 3.75850(27) . 1_556 N
I I 3.671(20) . -1_666 N
I Cl 2.335(11) . 1_555 N
I Cl 3.570(11) . -1_666 N
I O 2.457(10) . -1_665 N
I D1 2.766(11) . -1_666 N
I D2 2.756(10) . 1_656 N
I D3 2.772(11) . -1_666 N
Cl I 2.335(11) . 1_555 N
Cl I 3.570(11) . -1_666 N
Cl Cl 2.973(10) . -1_657 N
Cl D4 2.736(8) . 1_556 N
Cl D4 2.503(7) . -1_655 N
O I 2.457(10) . -1_665 N
O C1 1.44929(12) . 1_555 N
O C2 1.45079(10) . 1_555 N
O D1 2.08202(17) . 1_555 N
O D2 2.05968(15) . 1_555 N
O D3 2.08372(14) . 1_555 N
O D4 2.04393(14) . 1_555 N
C1 O 1.44929(12) . 1_555 N
C1 C2 1.50577(13) . -1_555 N
C1 D1 1.09748(9) . 1_555 N
C1 D2 1.09366(8) . 1_555 N
C1 D3 2.15854(17) . -1_555 N
C1 D4 2.14740(19) . -1_555 N
C2 O 1.45079(10) . 1_555 N
C2 C1 1.50577(13) . -1_555 N
C2 D1 2.16275(17) . -1_555 N
C2 D2 2.15484(20) . -1_555 N
C2 D3 1.09726(8) . 1_555 N
C2 D4 1.08575(9) . 1_555 N
D1 I 2.766(11) . -1_666 N
D1 O 2.08202(17) . 1_555 N
D1 C1 1.09748(9) . 1_555 N
D1 C2 2.16275(17) . -1_555 N
D1 D2 1.78556(12) . 1_555 N
D2 I 2.756(10) . 1_454 N
D2 O 2.05968(15) . 1_555 N
D2 C1 1.09366(8) . 1_555 N
D2 C2 2.15484(20) . -1_555 N
D2 D1 1.78556(12) . 1_555 N
D3 I 2.772(11) . -1_666 N
D3 O 2.08372(14) . 1_555 N
D3 C1 2.15854(17) . -1_555 N
D3 C2 1.09726(8) . 1_555 N
D3 D4 1.79176(14) . 1_555 N
D4 Cl 2.736(8) . 1_554 N
D4 Cl 2.503(7) . -1_655 N
D4 O 2.04393(14) . 1_555 N
D4 C1 2.14740(19) . -1_555 N
D4 C2 1.08575(9) . 1_555 N
D4 D3 1.79176(14) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 174.4(5) 1_555 . -1_665 N
Cl I D1 118.3(4) 1_555 . -1_666 N
Cl I D2 69.89(26) 1_555 . 1_656 N
Cl I D3 126.4(4) 1_555 . -1_666 N
O I D1 56.34(25) -1_665 . -1_666 N
O I D2 104.6(4) -1_665 . 1_656 N
O I D3 52.58(20) -1_665 . -1_666 N
D1 I D2 53.60(19) -1_666 . 1_656 N
D1 I D3 51.62(20) -1_666 . -1_666 N
D2 I D3 98.08(34) 1_656 . -1_666 N
I Cl Cl 165.6(4) 1_555 . -1_657 N
I Cl D4 131.6(4) 1_555 . 1_556 N
I Cl D4 82.29(28) 1_555 . -1_655 N
Cl Cl D4 61.20(25) -1_657 . 1_556 N
Cl Cl D4 90.82(28) -1_657 . -1_655 N
D4 Cl D4 93.51(22) 1_556 . -1_655 N
I O C1 110.03(30) -1_665 . 1_555 N
I O C2 116.19(30) -1_665 . 1_555 N
C1 O C2 110.886(6) 1_555 . 1_555 N
O C1 C2 108.942(7) 1_555 . -1_555 N
O C1 D1 108.891(6) 1_555 . 1_555 N
O C1 D2 107.358(6) 1_555 . 1_555 N
C2 C1 D1 111.395(6) -1_555 . 1_555 N
C2 C1 D2 110.992(6) -1_555 . 1_555 N
D1 C1 D2 109.155(6) 1_555 . 1_555 N
O C2 C1 109.016(7) 1_555 . -1_555 N
O C2 D3 108.935(6) 1_555 . 1_555 N
O C2 D4 106.485(6) 1_555 . 1_555 N
C1 C2 D3 111.070(6) -1_555 . 1_555 N
C1 C2 D4 110.875(7) -1_555 . 1_555 N
D3 C2 D4 110.324(6) 1_555 . 1_555 N
I D1 C1 142.44(27) -1_666 . 1_555 N
I D1 D2 136.85(25) -1_666 . 1_555 N
C1 D1 D2 35.351(4) 1_555 . 1_555 N
I D2 C1 166.05(25) 1_454 . 1_555 N
I D2 D1 149.56(31) 1_454 . 1_555 N
C1 D2 D1 35.493(4) 1_555 . 1_555 N
I D3 C2 142.15(26) -1_666 . 1_555 N
I D3 D4 136.59(26) -1_666 . 1_555 N
C2 D3 D4 34.628(4) 1_555 . 1_555 N
Cl D4 Cl 86.49(22) 1_554 . -1_655 N
Cl D4 C2 110.07(21) 1_554 . 1_555 N
Cl D4 D3 76.99(22) 1_554 . 1_555 N
Cl D4 C2 163.22(26) -1_655 . 1_555 N
Cl D4 D3 158.05(27) -1_655 . 1_555 N
C2 D4 D3 35.048(4) 1_555 . 1_555 N
####################################################################### 
# 
# 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_BF_phase_1_CCDC17
_database_code_depnum_ccdc_archive 'CCDC 2255393'
loop_
_audit_author_name
_audit_author_address
'Richard H Jones'
;Keele University
United Kingdom
;
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;

_pd_block_id                     2019-09-09T18:05|BF_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2019-09-09T18:05|BF_H_01|WGM|PEARL

#==============================================================================

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   '1,4-dioxane.2ICl adduct (C2/m)'
_cell_length_a                   14.4152(9)
_cell_length_b                   7.8605(7)
_cell_length_c                   4.1370(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 97.206(11)
_cell_angle_gamma                90.0
_cell_volume                     465.07(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'


_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.04
_refine_ls_number_restraints     11
_refine_ls_matrix_type           full

_exptl_crystal_description       needle
_chemical_formula_sum            'C4 D8 Cl2 I2 O2'
_chemical_formula_weight         420.86
_cell_formula_units_Z            2
_symmetry_space_group_name_Hall  ' -C 2y '
_diffrn_measurement_device_type  PEARL
_diffrn_ambient_temperature      295
_cell_measurement_temperature    295
_pd_char_colour                  orange
_pd_meas_scan_method             tof
_chemical_formula_moiety         'C2 D4 Cl I O'
_exptl_crystal_density_diffrn    3.005
_diffrn_measurement_pressure     1699000



_pd_proc_ls_prof_R_factor        0.0431
_pd_proc_ls_prof_wR_factor       0.0371
_pd_proc_ls_prof_wR_expected     0.0363
_refine_ls_R_Fsqd_factor         0.18830

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
I I 0.2438(10) 0.5 0.724(4) 1.0 Uiso 0.0242(17) 4
Cl Cl 0.3980(6) 0.5 0.5668(23) 1.0 Uiso 0.0485(33) 4
O O 0.0782(7) 0.5 -0.1770(23) 1.0 Uiso 0.019(4) 4
C C 0.05229(20) 0.6496(6) -0.0114(13) 1.0 Uiso 0.0298(29) 8
D D1 0.0906(5) 0.6528(13) 0.2322(20) 1.0 Uiso 0.058(4) 8
D D2 0.0701(6) 0.7611(9) -0.1482(21) 1.0 Uiso 0.058(4) 8

loop_
_atom_type_symbol
_atom_type_number_in_cell
I 4.0
Cl 4.0
C 8.0
O 4.0
D 16.0



# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cl 2.393(17) . 1_555 N
I O 2.472(18) . 1_556 N
Cl I 2.393(17) . 1_555 N
Cl Cl 3.059(17) . 2_656 N
Cl D2 2.633(10) . 102_545 N
Cl D2 2.633(10) . -101_565 N
O I 2.472(18) . 1_554 N
O C 1.434(5) . 1_555 N
O C 1.434(5) . -2_565 N
O D1 2.065(8) . 1_555 N
O D1 2.065(8) . -2_565 N
O D2 2.060(7) . 1_555 N
O D2 2.060(7) . -2_565 N
C O 1.434(5) . 1_555 N
C C 1.522(5) . 2_555 N
C D1 1.087(6) . 1_555 N
C D2 1.091(5) . 1_555 N
D1 O 2.065(8) . 1_555 N
D1 C 1.087(6) . 1_555 N
D1 D2 1.781(8) . 1_555 N
D2 Cl 2.633(10) . 102_555 N
D2 O 2.060(7) . 1_555 N
D2 C 1.091(5) . 1_555 N
D2 D1 1.781(8) . 1_555 N


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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl I O 173.8(8) 1_555 . 1_556 N
I Cl Cl 174.7(7) 1_555 . 2_656 N
I O C 113.2(5) 1_554 . 1_555 N
I O C 113.2(5) 1_554 . -2_565 N
C O C 110.2(5) 1_555 . -2_565 N
O C C 110.4(4) 1_555 . 2_555 N
O C D1 109.2(5) 1_555 . 1_555 N
O C D2 108.6(4) 1_555 . 1_555 N
C C D1 109.5(5) 2_555 . 1_555 N
C C D2 109.4(4) 2_555 . 1_555 N
D1 C D2 109.7(5) 1_555 . 1_555 N
