# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AC-BR2_14K_phase_1
_database_code_depnum_ccdc_archive 'CCDC 1562036'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT091_AC-BR2_14K_phase_1  
;
PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check
RESPONSE: TOF experiment analagous to Laue
;
_vrf_PLAT431_AC-BR2_14K_phase_1  
;
PROBLEM: Short Inter HL..A  Contact Br1    ..  O1      ..       2.74 Ang.
RESPONSE: Short contact is indicative of halogen Bond
;
_vrf_CHEMS01_AC-BR2_14K_phase_1  
;
PROBLEM: The sum formula contains elements in the wrong order.
RESPONSE: CIF check does not recognise D as being equivalent to 2H
;
_vrf_REFI015_AC-BR2_14K_phase_1  
;
PROBLEM: _refine_ls_shift/su_max is missing
RESPONSE:  ratio is 0.08 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 requirment shift/error  < 0.05 but for Reitveld 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 18 July 2017 01:35 PM
# end Validation Reply Form


_pd_block_id                     2017-05-14T17:57|AC-BR2_14K_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2017-05-14T17:57|AC-BR2_14K_H_01|WGM|HRPD
2017-05-14T17:57|AC-BR2_14K_H_02|WGM|HRPD
2017-05-14T17:57|AC-BR2_14K_H_03|WGM|HRPD

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

_pd_char_particle_morphology     ?

_chemical_name_systematic        'Propan-2-one bromine complex'
_chemical_name_common            'acetone bromine complex'
_chemical_formula_moiety         'C3D6O  Br2'
_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    ?
_exptl_crystal_colour            orange
_cell_measurement_temperature    14

_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                   (CD3)2CO:Br2
_cell_length_a                   7.56309(12)
_cell_length_b                   7.35611(14)
_cell_length_c                   11.87474(20)
_cell_angle_alpha                90.0
_cell_angle_beta                 102.1687(6)
_cell_angle_gamma                90.0
_cell_volume                     645.806(28)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_diffrn_measurement_device_type  HRPD
_diffrn_ambient_temperature      14
_diffrn_radiation_type           neutron
_refine_ls_number_parameters     113
_refine_ls_goodness_of_fit_all   9.09
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z+1/2
-1 -x,-y,-z
-2 +x,-y,+z+1/2
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z+1/2
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z+1/2

# 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
Br BR1 0.32728(16) 0.65655(28) 0.57269(12) 1.0 Uiso 0.0051(5) 8
O O1 0.5 0.4412(5) 0.75 1.0 Uiso 0.0046(7) 4
C C3 0.5 0.2715(4) 0.75 1.0 Uiso 0.0068(7) 4
C C4 0.37071(22) 0.17029(30) 0.66038(14) 1.0 Uiso 0.0074(5) 8
D D5 0.30625(29) 0.0664(4) 0.70028(18) 1.0 Uani 0.03748 8
D D6 0.26817(30) 0.2601(4) 0.61284(18) 1.0 Uani 0.04202 8
D D7 0.44519(29) 0.1024(4) 0.60407(17) 1.0 Uani 0.04434 8

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
D5 0.0358(12) -0.0245(12) 0.0006(10) 0.0453(22) -0.0007(13) 0.0287(13)
D6 0.0424(13) 0.0025(13) -0.0292(12) 0.0214(21) 0.0010(12) 0.0453(15)
D7 0.0305(12) -0.0094(13) 0.0115(10) 0.0792(32) -0.0280(13) 0.0258(12)

loop_
_atom_type_symbol
_atom_type_number_in_cell
Br 8.0
O 4.0
C 12.0
D 24.0

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C3 D6 Br2 O'
_chemical_formula_weight         223.92
_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
BR1 BR1 2.3208(33) . -101_566 N
BR1 O1 2.7368(22) . 1_555 N
O1 BR1 2.7368(22) . 1_555 N
O1 BR1 2.7368(22) . 2_656 N
O1 C3 1.248(4) . 1_555 N
C3 O1 1.248(4) . 1_555 N
C3 C4 1.4848(25) . 1_555 N
C3 C4 1.4848(25) . 2_656 N
C3 D5 2.0998(32) . 1_555 N
C3 D5 2.0998(32) . 2_656 N
C4 C3 1.4848(25) . 1_555 N
C4 D5 1.0697(28) . 1_555 N
C4 D6 1.0827(26) . 1_555 N
C4 D7 1.0830(25) . 1_555 N
D5 C3 2.0998(32) . 1_555 N
D5 C4 1.0697(28) . 1_555 N
D5 D6 1.751(4) . 1_555 N
D5 D7 1.7280(29) . 1_555 N
D6 C4 1.0827(26) . 1_555 N
D6 D5 1.751(4) . 1_555 N
D6 D7 1.791(4) . 1_555 N
D7 C4 1.0830(25) . 1_555 N
D7 D5 1.7280(29) . 1_555 N
D7 D6 1.791(4) . 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
O1 C3 C4 120.11(14) 1_555 . 1_555 N
O1 C3 C4 120.11(14) 1_555 . 2_656 N
C4 C3 C4 119.79(28) 1_555 . 2_656 N
C3 C4 D5 109.50(18) 1_555 . 1_555 N
C3 C4 D6 111.02(25) 1_555 . 1_555 N
C3 C4 D7 108.93(18) 1_555 . 1_555 N
D5 C4 D6 108.90(25) 1_555 . 1_555 N
D5 C4 D7 106.78(28) 1_555 . 1_555 N
D6 C4 D7 111.62(24) 1_555 . 1_555 N
_exptl_crystal_description       powder
_exptl_crystal_recrystallization_method 'From the Melt'
####################################################################### 
# 
# 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_AC-BR2_35K_phase_1
_database_code_depnum_ccdc_archive 'CCDC 1562265'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT091_AC-BR2_35K_phase_1  
;
PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check
RESPONSE: TOF experiment analogous to Laue  so no unique wavelength
;
_vrf_PLAT431_AC-BR2_35K_phase_1  
;
PROBLEM: Short Inter HL..A  Contact Br1    ..  O1      ..       2.73 Ang.
RESPONSE: Short Contact is indicative of halogen bond discussed in paper
;
_vrf_CHEMS01_AC-BR2_35K_phase_1  
;
PROBLEM: The sum formula contains elements in the wrong order.
RESPONSE: CIF check does not recognise D as being equivalent to 2H
;
# Added during the CSD deposition process: Tuesday 18 July 2017 01:41 PM
# end Validation Reply Form


_pd_block_id                     2017-05-31T11:09|AC-BR2_35K_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2017-05-31T11:09|AC-BR2_35K_H_01|WGM|HRPD
2017-05-31T11:09|AC-BR2_35K_H_02|WGM|HRPD
2017-05-31T11:09|AC-BR2_35K_H_03|WGM|HRPD

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

_pd_char_particle_morphology     ?

_chemical_name_systematic        'Propan-2-one bromine complex'
_chemical_name_common            'acetone bromine complex'
_chemical_formula_moiety         'C3D6O  Br2'
_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    35

_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                   (CD3)2CO:Br2
_cell_length_a                   7.55600(11)
_cell_length_b                   7.35286(14)
_cell_length_c                   11.91193(19)
_cell_angle_alpha                90.0
_cell_angle_beta                 102.1076(6)
_cell_angle_gamma                90.0
_cell_volume                     647.084(27)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_diffrn_measurement_device_type  HRPD
_diffrn_ambient_temperature      35
_diffrn_radiation_type           neutron
_exptl_crystal_colour            orange
_refine_ls_number_parameters     87
_refine_ls_goodness_of_fit_all   5.90
_refine_ls_shift/su_max          0.03


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

# 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
Br BR1 0.32697(16) 0.65733(26) 0.57337(11) 1.0 Uiso 0.0077(4) 8
O O1 0.5 0.4427(4) 0.75 1.0 Uiso 0.0069(6) 4
C C3 0.5 0.27369(34) 0.75 1.0 Uiso 0.0062(5) 4
C C4 0.37159(21) 0.17024(27) 0.66003(14) 1.0 Uiso 0.01145(34) 8
D D5 0.30253(26) 0.07405(35) 0.69908(15) 1.0 Uani 0.05001 8
D D6 0.27285(29) 0.26085(33) 0.61239(17) 1.0 Uani 0.06298 8
D D7 0.44508(25) 0.0998(4) 0.60684(16) 1.0 Uani 0.06281 8

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
D5 0.0515(11) -0.0401(13) 0.0051(9) 0.0691(22) -0.0076(12) 0.0280(11)
D6 0.0670(13) 0.0023(13) -0.0474(11) 0.0276(17) 0.0023(12) 0.0673(15)
D7 0.0355(11) -0.0182(13) 0.0166(9) 0.1153(30) -0.0522(13) 0.0414(12)

loop_
_atom_type_symbol
_atom_type_number_in_cell
Br 8.0
O 4.0
C 12.0
D 24.0

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C3 D6 Br2 O'
_chemical_formula_weight         223.92
_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
BR1 BR1 2.3265(30) . -101_566 N
BR1 O1 2.7338(21) . 1_555 N
O1 BR1 2.7338(21) . 1_555 N
O1 BR1 2.7338(21) . 2_656 N
O1 C3 1.2425(33) . 1_555 N
C3 O1 1.2425(33) . 1_555 N
C3 C4 1.4941(20) . 1_555 N
C3 C4 1.4941(20) . 2_656 N
C3 D5 2.0903(27) . 1_555 N
C3 D5 2.0903(27) . 2_656 N
C4 C3 1.4941(20) . 1_555 N
C4 D5 1.0444(23) . 1_555 N
C4 D6 1.0700(24) . 1_555 N
C4 D7 1.0610(22) . 1_555 N
D5 C3 2.0903(27) . 1_555 N
D5 C4 1.0444(23) . 1_555 N
D5 D6 1.7047(32) . 1_555 N
D5 D7 1.7028(26) . 1_555 N
D6 C4 1.0700(24) . 1_555 N
D6 D5 1.7047(32) . 1_555 N
D6 D7 1.7710(34) . 1_555 N
D7 C4 1.0610(22) . 1_555 N
D7 D5 1.7028(26) . 1_555 N
D7 D6 1.7710(34) . 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
O1 C3 C4 120.60(11) 1_555 . 1_555 N
O1 C3 C4 120.60(11) 1_555 . 2_656 N
C4 C3 C4 118.79(22) 1_555 . 2_656 N
C3 C4 D5 109.59(17) 1_555 . 1_555 N
C3 C4 D6 109.82(20) 1_555 . 1_555 N
C3 C4 D7 109.54(16) 1_555 . 1_555 N
D5 C4 D6 107.46(23) 1_555 . 1_555 N
D5 C4 D7 107.95(25) 1_555 . 1_555 N
D6 C4 D7 112.41(23) 1_555 . 1_555 N
_exptl_crystal_description       powder
_exptl_crystal_recrystallization_method 'From the Melt'
####################################################################### 
# 
# 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_AC-BR2_75K_phase_1
_database_code_depnum_ccdc_archive 'CCDC 1562187'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT091_AC-BR2_75K_phase_1  
;
PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check
RESPONSE: TOF experiment analogous to Laue  so no unique wavelength
;
_vrf_PLAT431_AC-BR2_75K_phase_1  
;
PROBLEM: Short Inter HL..A  Contact Br1    ..  O1      ..       2.74 Ang.
RESPONSE: Short Contact is indicative of halogen bond discussed in paper
;
_vrf_CHEMS01_AC-BR2_75K_phase_1  
;
PROBLEM: The sum formula contains elements in the wrong order.
RESPONSE: CIF check does not recognise D as being equivalent to 2H
;
# Added during the CSD deposition process: Tuesday 18 July 2017 01:44 PM
# end Validation Reply Form


_pd_block_id                     2017-05-14T17:58|AC-BR2_75K_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2017-05-14T17:58|AC-BR2_75K_H_01|WGM|HRPD
2017-05-14T17:58|AC-BR2_75K_H_02|WGM|HRPD
2017-05-14T17:58|AC-BR2_75K_H_03|WGM|HRPD

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

_pd_char_particle_morphology     ?

_chemical_name_systematic        'Propan-2-one bromine complex'
_chemical_name_common            'acetone bromine complex'
_chemical_formula_moiety         'C3D6O Br2'
_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    75

_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                   (CD3)2CO:Br2
_cell_length_a                   7.56429(13)
_cell_length_b                   7.36051(15)
_cell_length_c                   11.97900(21)
_cell_angle_alpha                90.0
_cell_angle_beta                 102.1146(7)
_cell_angle_gamma                90.0
_cell_volume                     652.102(30)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_diffrn_radiation_type           neutron
_exptl_crystal_colour            orange
_diffrn_measurement_device_type  HRPD
_refine_ls_number_parameters     86
_refine_ls_shift/su_max          0.05
_diffrn_ambient_temperature      75
_refine_ls_goodness_of_fit_all   6.78
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z+1/2
-1 -x,-y,-z
-2 +x,-y,+z+1/2
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z+1/2
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z+1/2

# 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
Br BR1 0.32665(19) 0.65782(29) 0.57334(13) 1.0 Uiso 0.0168(5) 8
O O1 0.5 0.4447(5) 0.75 1.0 Uiso 0.0120(7) 4
C C3 0.5 0.2749(4) 0.75 1.0 Uiso 0.0105(6) 4
C C4 0.37241(27) 0.17147(34) 0.65949(17) 1.0 Uiso 0.0199(4) 8
D D5 0.2959(4) 0.0852(5) 0.69684(18) 1.0 Uani 0.07492 8
D D6 0.2809(4) 0.2623(4) 0.61055(23) 1.0 Uani 0.09777 8
D D7 0.44496(31) 0.0970(4) 0.61133(21) 1.0 Uani 0.08875 8

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
D5 0.0775(15) -0.0676(19) 0.0163(13) 0.1134(33) -0.0190(16) 0.0358(13)
D6 0.1154(21) -0.0107(20) -0.0769(18) 0.0335(21) 0.0107(17) 0.1006(23)
D7 0.0408(14) -0.0266(16) 0.0205(13) 0.151(4) -0.0882(19) 0.0781(18)

loop_
_atom_type_symbol
_atom_type_number_in_cell
Br 8.0
O 4.0
C 12.0
D 24.0

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C3 D6 Br2 O'
_chemical_formula_weight         223.92
_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
BR1 BR1 2.3277(34) . -101_566 N
BR1 O1 2.7373(24) . 1_555 N
BR1 D6 2.976(4) . 1_555 N
BR1 D7 3.0488(31) . 101_455 N
O1 BR1 2.7373(24) . 1_555 N
O1 BR1 2.7373(24) . 2_656 N
O1 C3 1.250(4) . 1_555 N
O1 C4 2.390(4) . 1_555 N
O1 C4 2.390(4) . 2_656 N
O1 D5 2.6611(30) . 101_555 N
O1 D5 2.6611(30) . 102_556 N
O1 D6 2.4857(30) . 1_555 N
O1 D6 2.4857(30) . 2_656 N
C3 O1 1.250(4) . 1_555 N
C3 C4 1.4991(23) . 1_555 N
C3 C4 1.4991(23) . 2_656 N
C3 D5 2.0800(32) . 1_555 N
C3 D5 2.0800(32) . 2_656 N
C3 D6 2.0938(19) . 1_555 N
C3 D6 2.0938(19) . 2_656 N
C3 D7 2.0872(30) . 1_555 N
C3 D7 2.0872(30) . 2_656 N
C4 O1 2.390(4) . 1_555 N
C4 C3 1.4991(23) . 1_555 N
C4 D5 1.0234(27) . 1_555 N
C4 D6 1.0485(30) . 1_555 N
C4 D7 1.0330(26) . 1_555 N
D5 O1 2.6611(30) . 101_445 N
D5 C3 2.0800(32) . 1_555 N
D5 C4 1.0234(27) . 1_555 N
D5 D6 1.652(4) . 1_555 N
D5 D7 1.6774(33) . 1_555 N
D6 BR1 2.976(4) . 1_555 N
D6 O1 2.4857(30) . 1_555 N
D6 C3 2.0938(19) . 1_555 N
D6 C4 1.0485(30) . 1_555 N
D7 BR1 3.0488(31) . 101_545 N
D7 C4 1.0330(26) . 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
BR1 BR1 O1 178.24(12) -101_566 . 1_555 N
BR1 O1 BR1 110.08(14) 1_555 . 2_656 N
BR1 O1 C3 124.96(7) 1_555 . 1_555 N
BR1 O1 C3 124.96(7) 2_656 . 1_555 N
O1 C3 C4 120.52(13) 1_555 . 1_555 N
O1 C3 C4 120.52(13) 1_555 . 2_656 N
C4 C3 C4 118.96(27) 1_555 . 2_656 N
C3 C4 D5 109.65(22) 1_555 . 1_555 N
C3 C4 D6 109.26(26) 1_555 . 1_555 N
C3 C4 D7 109.66(21) 1_555 . 1_555 N
D5 C4 D6 105.79(30) 1_555 . 1_555 N
D5 C4 D7 109.32(33) 1_555 . 1_555 N
D6 C4 D7 113.07(31) 1_555 . 1_555 N
_exptl_crystal_description       powder
_exptl_crystal_recrystallization_method 'From the Melt'
####################################################################### 
# 
# 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_AC-BR2_200K_phase_1
_database_code_depnum_ccdc_archive 'CCDC 1562188'
_audit_update_record             
;
2017-07-18 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT091_AC-BR2_200K_phase_1 
;
PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check
RESPONSE: TOF experiment analogous to Laue  so no unique wavelength
;
_vrf_PLAT431_AC-BR2_200K_phase_1 
;
PROBLEM: Short Inter HL..A  Contact Br1    ..  O1      ..       2.80 Ang.
RESPONSE: Short Contact is indicative of halogen bond discussed in paper
;
_vrf_CHEMS01_AC-BR2_200K_phase_1 
;
PROBLEM: The sum formula contains elements in the wrong order.
RESPONSE: CIF check does not recognise D as being equivalent to 2H
;
# Added during the CSD deposition process: Tuesday 18 July 2017 01:46 PM
# end Validation Reply Form


_pd_block_id                     2017-05-14T17:49|AC-BR2_200K_phase1|WGM||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2017-05-14T17:49|AC-BR2_200K_H_01|WGM|HRPD
2017-05-14T17:49|AC-BR2_200K_H_02|WGM|HRPD
2017-05-14T17:49|AC-BR2_200K_H_03|WGM|HRPD

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

_pd_char_particle_morphology     ?

_chemical_name_systematic        'Propan-2-one Bromine complex'
_chemical_name_common            'Acetone Bromine complex'
_chemical_formula_moiety         'C3D6O  Br2'
_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    200

_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                   (CD3)2CO:Br2
_cell_length_a                   7.64626(19)
_cell_length_b                   7.43063(22)
_cell_length_c                   12.22578(31)
_cell_angle_alpha                90.0
_cell_angle_beta                 102.9966(8)
_cell_angle_gamma                90.0
_cell_volume                     676.83(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_diffrn_measurement_device_type  HRPD
_diffrn_radiation_type           neutron
_refine_ls_number_parameters     86
_refine_ls_shift/su_max          0.01
_refine_ls_goodness_of_fit_all   7.37
_exptl_crystal_colour            orange
_diffrn_ambient_temperature      200
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z+1/2
-1 -x,-y,-z
-2 +x,-y,+z+1/2
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z+1/2
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z+1/2

# 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
Br BR1 0.32354(31) 0.6575(5) 0.57160(17) 1.0 Uiso 0.0408(9) 8
O O1 0.5 0.4419(8) 0.75 1.0 Uiso 0.0300(13) 4
C C3 0.5 0.2768(7) 0.75 1.0 Uiso 0.0317(11) 4
C C4 0.3712(6) 0.1774(7) 0.6586(4) 1.0 Uiso 0.0564(11) 8
D D5 0.2956(7) 0.1019(8) 0.69325(27) 1.0 Uani 0.12275 8
D D6 0.2925(9) 0.2629(7) 0.6093(5) 1.0 Uani 0.15937 8
D D7 0.4425(5) 0.0997(9) 0.6176(4) 1.0 Uani 0.13953 8

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
D5 0.1264(32) -0.107(4) 0.0173(25) 0.166(7) -0.0220(34) 0.0736(28)
D6 0.184(5) -0.033(4) -0.127(4) 0.068(4) 0.0220(35) 0.149(5)
D7 0.0682(26) -0.0140(31) 0.0068(26) 0.210(8) -0.116(5) 0.133(4)

loop_
_atom_type_symbol
_atom_type_number_in_cell
Br 8.0
O 4.0
C 12.0
D 24.0

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C3 D6 Br2 O'
_chemical_formula_weight         223.92
_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
BR1 BR1 2.309(5) . -101_566 N
BR1 O1 2.797(4) . 1_555 N
O1 BR1 2.797(4) . 1_555 N
O1 BR1 2.797(4) . 2_656 N
O1 C3 1.227(6) . 1_555 N
C3 O1 1.227(6) . 1_555 N
C3 C4 1.506(4) . 1_555 N
C3 C4 1.506(4) . 2_656 N
C3 D5 2.031(6) . 1_555 N
C3 D5 2.031(6) . 2_656 N
C3 D6 2.0637(29) . 1_555 N
C3 D6 2.0637(29) . 2_656 N
C3 D7 2.056(6) . 1_555 N
C3 D7 2.056(6) . 2_656 N
C4 C3 1.506(4) . 1_555 N
C4 D5 0.968(5) . 1_555 N
C4 D6 0.983(5) . 1_555 N
C4 D7 1.003(5) . 1_555 N
D5 C3 2.031(6) . 1_555 N
D5 C4 0.968(5) . 1_555 N
D5 D6 1.572(7) . 1_555 N
D5 D7 1.607(5) . 1_555 N
D6 C3 2.0637(29) . 1_555 N
D6 C4 0.983(5) . 1_555 N
D6 D5 1.572(7) . 1_555 N
D6 D7 1.657(7) . 1_555 N
D7 C3 2.056(6) . 1_555 N
D7 C4 1.003(5) . 1_555 N
D7 D5 1.607(5) . 1_555 N
D7 D6 1.657(7) . 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
O1 C3 C4 119.36(28) 1_555 . 1_555 N
O1 C3 C4 119.36(28) 1_555 . 2_656 N
C4 C3 C4 121.3(6) 1_555 . 2_656 N
C3 C4 D5 108.4(5) 1_555 . 1_555 N
C3 C4 D6 110.3(5) 1_555 . 1_555 N
C3 C4 D7 108.4(5) 1_555 . 1_555 N
D5 C4 D6 107.4(7) 1_555 . 1_555 N
D5 C4 D7 109.2(7) 1_555 . 1_555 N
D6 C4 D7 113.1(7) 1_555 . 1_555 N
_exptl_crystal_description       powder
_exptl_crystal_recrystallization_method 'From the Melt'
