# Electronic Supplementary Material for CrystEngComm
# This journal is (C) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Andrzej Katrusiak'
_publ_contact_author_email       KATRAN@AMU.EDU.PL

_publ_section_title              
;
Isostructural relations and disproportionation of
bromoiodomethane
;
_publ_contact_author_fax         +48(61)8291505
_publ_contact_author_phone       +48(61)8291443
loop_
_publ_author_name
Andrzej
Katrusiak
Marcin
Podsiadlo

# Attachment 'bjm_all.cif'

data_bjm_220K
_database_code_depnum_ccdc_archive 'CCDC 681738'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bromoiodomethane
;

_chemical_name_common            bromoiodomethane
_chemical_melting_point          274
_chemical_formula_moiety         'C1 H2 Br1 I1'
_chemical_formula_sum            'C H2 Br I'
_chemical_formula_weight         220.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2 / c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.905(3)
_cell_length_b                   4.5730(9)
_cell_length_c                   16.072(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.79(3)
_cell_angle_gamma                90.00
_cell_volume                     861.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    220.0(1)
_cell_measurement_reflns_used    1280
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      29.06

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    16.483
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_T_max  0.05
_exptl_absorpt_process_details   
;
Correction for absorption was made using XEMP (SHELXTL,
Sheldrick (1990)).
;

_exptl_special_details           
;
Data were collected at ambient pressure (100 kPa) and 220 K with
the crystal obtained by the in-situ low-temperature crystallization
technique.
;

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            2792
_diffrn_reflns_av_R_equivalents  0.1755
_diffrn_reflns_av_sigmaI/netI    0.1153
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         29.06
_reflns_number_total             1088
_reflns_number_gt                818
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The restrains applied were that the disordered Br and I atoms
had the same xyz and Uanis parameters for Br1 and I1,
and separately for Br2 and I2. the SOF
were bound by the SOF(Be)+SOF(I)=1 relation.
The H-atom was calculated from
molecular geometry (fixed by ideallized disatances).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0611P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0045(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1088
_refine_ls_number_parameters     36
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.1660
_refine_ls_wR_factor_gt          0.1507
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.09449(3) 0.66904(18) 0.13187(5) 0.0524(4) Uani 0.648(5) 1 d PD . .
Br1 Br 0.09449(3) 0.66904(18) 0.13187(5) 0.0524(4) Uani 0.352(5) 1 d P . .
I2 I 0.35471(3) 0.6451(2) 0.12898(6) 0.0518(5) Uani 0.352(5) 1 d PD . .
Br2 Br 0.35471(3) 0.6451(2) 0.12898(6) 0.0518(5) Uani 0.648(5) 1 d P . .
C1 C 0.2110(8) 0.42786(19) 0.10694(19) 0.052(3) Uani 1 1 d D . .
H1 H 0.17525(16) 0.3501(9) 0.0407(3) 0.062 Uiso 1 1 d D . .
H2 H 0.23045(17) 0.2403(2) 0.1460(3) 0.062 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0415(5) 0.0542(6) 0.0649(7) -0.0088(4) 0.0255(4) -0.0060(3)
Br1 0.0415(5) 0.0542(6) 0.0649(7) -0.0088(4) 0.0255(4) -0.0060(3)
I2 0.0314(5) 0.0562(7) 0.0619(7) -0.0002(4) 0.0138(4) 0.0013(3)
Br2 0.0314(5) 0.0562(7) 0.0619(7) -0.0002(4) 0.0138(4) 0.0013(3)
C1 0.051(6) 0.042(5) 0.060(6) -0.005(5) 0.021(5) 0.001(5)

# MOLECULAR GEOMETRY

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.036(8) . ?
Br1 C1 2.036(8) . ?
I2 C1 2.000(8) . ?
Br2 C1 2.000(8) . ?
C1 H1 1.0300(3) . ?
C1 H2 1.03000(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 C1 I2 0.00(7) . . ?
Br2 C1 I1 113.74(7) . . ?
I2 C1 I1 113.74(7) . . ?
Br2 C1 Br1 113.74(7) . . ?
I2 C1 Br1 113.74(7) . . ?
I1 C1 Br1 0.00(4) . . ?
Br2 C1 H1 109.6(6) . . ?
I2 C1 H1 109.6(6) . . ?
I1 C1 H1 110.0(6) . . ?
Br1 C1 H1 110.0(6) . . ?
Br2 C1 H2 109.6(6) . . ?
I2 C1 H2 109.6(6) . . ?
I1 C1 H2 110.0(6) . . ?
Br1 C1 H2 110.0(6) . . ?
H1 C1 H2 103.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.942
_diffrn_reflns_theta_full        29.06
_diffrn_measured_fraction_theta_full 0.942
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.294

#############################################################################

data_bjm_100K
_database_code_depnum_ccdc_archive 'CCDC 681739'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bromoiodomethane
;

_chemical_name_common            bromoiodomethane
_chemical_melting_point          274
_chemical_formula_moiety         'C1 H2 Br1 I1'
_chemical_formula_sum            'C H2 Br I'
_chemical_formula_weight         220.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2 / c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.817(3)
_cell_length_b                   4.5223(9)
_cell_length_c                   15.757(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.45(3)
_cell_angle_gamma                90.00
_cell_volume                     831.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    2420
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      29.68

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    17.072
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_T_max  0.05

_exptl_absorpt_process_details   
;
Correction for absorption was made using XEMP (SHELXTL,
Sheldrick (1990)).
;

_exptl_special_details           
;
Data were collected at ambient pressure (100 kPa) and 100 K with
the crystal obtained by the in-situ low-temperature crystallization
technique.
;

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_pressure         100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3568
_diffrn_reflns_av_R_equivalents  0.2106
_diffrn_reflns_av_sigmaI/netI    0.1026
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         29.68
_reflns_number_total             1069
_reflns_number_gt                975
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The restrains applied were that the disordered Br and I atoms
had the same xyz and Uanis parameters for Br1 and I1,
and separately for Br2 and I2. the SOF
were bound by the SOF(Be)+SOF(I)=1 relation.
The H-atom was calculated from
molecular geometry (fixed by ideallized disatances).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0282P)²+20.0717P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1069
_refine_ls_number_parameters     36
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1255
_refine_ls_wR_factor_gt          0.1200
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.09248(3) 0.68029(14) 0.13107(4) 0.0233(3) Uani 0.662(5) 1 d PD . .
Br1 Br 0.09248(3) 0.68029(14) 0.13107(4) 0.0233(3) Uani 0.338(5) 1 d P . .
I2 I 0.35594(3) 0.65873(17) 0.12886(5) 0.0244(3) Uani 0.338(5) 1 d PD . .
Br2 Br 0.35594(3) 0.65873(17) 0.12886(5) 0.0244(3) Uani 0.662(5) 1 d P . .
C1 C 0.2132(5) 0.4241(2) 0.1072(2) 0.0299(19) Uani 1 1 d D . .
H1 H 0.17570(16) 0.3625(10) 0.0381(3) 0.036 Uiso 1 1 d D . .
H2 H 0.23518(18) 0.2537(3) 0.1548(3) 0.036 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0181(4) 0.0265(4) 0.0256(4) -0.0040(2) 0.0093(2) -0.0029(2)
Br1 0.0181(4) 0.0265(4) 0.0256(4) -0.0040(2) 0.0093(2) -0.0029(2)
I2 0.0131(4) 0.0287(5) 0.0260(4) 0.0002(3) 0.0025(3) 0.0011(3)
Br2 0.0131(4) 0.0287(5) 0.0260(4) 0.0002(3) 0.0025(3) 0.0011(3)
C1 0.021(4) 0.024(4) 0.033(4) -0.011(4) 0.000(3) -0.002(3)

# MOLECULAR GEOMETRY

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.087(6) . ?
Br1 C1 2.087(6) . ?
I2 C1 2.018(6) . ?
Br2 C1 2.018(6) . ?
C1 H1 1.0300(3) . ?
C1 H2 1.03000(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 C1 I2 0.00(5) . . ?
Br2 C1 I1 111.44(7) . . ?
I2 C1 I1 111.44(7) . . ?
Br2 C1 Br1 111.44(7) . . ?
I2 C1 Br1 111.44(7) . . ?
I1 C1 Br1 0.00(3) . . ?
Br2 C1 H1 108.3(4) . . ?
I2 C1 H1 108.3(4) . . ?
I1 C1 H1 106.5(4) . . ?
Br1 C1 H1 106.5(4) . . ?
Br2 C1 H2 108.3(4) . . ?
I2 C1 H2 108.3(4) . . ?
I1 C1 H2 106.5(4) . . ?
Br1 C1 H2 106.5(4) . . ?
H1 C1 H2 115.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.911
_diffrn_reflns_theta_full        29.68
_diffrn_measured_fraction_theta_full 0.911
_refine_diff_density_max         1.469
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.371

#############################################################################

data_bjm_0.54GPa
_database_code_depnum_ccdc_archive 'CCDC 681740'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bromoiodomethane
;

_chemical_name_common            bromoiodomethane
_chemical_melting_point          274
_chemical_formula_moiety         'C1 H2 Br1 I1'
_chemical_formula_sum            'C H2 Br I'
_chemical_formula_weight         220.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2 / c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.649(3)
_cell_length_b                   4.4767(9)
_cell_length_c                   15.425(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.98(3)
_cell_angle_gamma                90.00
_cell_volume                     804.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2470
_cell_measurement_theta_min      3.50
_cell_measurement_theta_max      29.70

_exptl_crystal_description       cylinder
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    17.652
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.09
_exptl_absorpt_correction_T_max  0.29
_exptl_absorpt_process_details   
;
Correction for absorption of the diamond-anvil cell and the sample
were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
Mickiewicz University Poznań; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;

# EXPERIMENTAL DATA

_exptl_special_details           
;
Data were collected at room temperature and pressure of 0.54(5) GPa
(540000 kPa) with the crystal obtained by the in-situ high-pressure
crystallization technique.
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         540000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3147
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.50
_diffrn_reflns_theta_max         29.70
_reflns_number_total             369
_reflns_number_gt                330
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_reduction        
'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A. 2003)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio.

The restrains applied were that the disordered Br and I atoms
had the same xyz and Uanis parameters for Br1 and I1,
and separately for Br2 and I2. the SOF
were bound by the SOF(Be)+SOF(I)=1 relation.
The H-atom was calculated from
molecular geometry (fixed by ideallized disatances).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0376P)²+1.4443P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0041(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         369
_refine_ls_number_parameters     36
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0698
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.08799(3) 0.67800(10) 0.12950(8) 0.0525(12) Uani 0.587(4) 1 d PD . .
Br1 Br 0.08799(3) 0.67800(10) 0.12950(8) 0.0525(12) Uani 0.413(4) 1 d P . .
I2 I 0.35414(3) 0.65609(11) 0.13041(9) 0.0529(12) Uani 0.413(4) 1 d PD . .
Br2 Br 0.35414(3) 0.65609(11) 0.13041(9) 0.0529(12) Uani 0.587(4) 1 d P . .
C1 C 0.2082(5) 0.42797(10) 0.1069(2) 0.063(10) Uani 1 1 d D . .
H1 H 0.17715(17) 0.3478(10) 0.0389(3) 0.075 Uiso 1 1 d D . .
H2 H 0.22802(15) 0.24085(19) 0.1491(3) 0.075 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0464(5) 0.0532(4) 0.065(3) -0.0082(4) 0.0298(11) -0.0061(2)
Br1 0.0464(5) 0.0532(4) 0.065(3) -0.0082(4) 0.0298(11) -0.0061(2)
I2 0.0353(5) 0.0572(4) 0.062(4) 0.0009(4) 0.0151(11) 0.0010(2)
Br2 0.0353(5) 0.0572(4) 0.062(4) 0.0009(4) 0.0151(11) 0.0010(2)
C1 0.055(5) 0.040(3) 0.09(3) -0.010(5) 0.029(11) -0.002(3)

# MOLECULAR GEOMETRY

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.025(5) . ?
Br1 C1 2.025(5) . ?
I2 C1 2.015(5) . ?
Br2 C1 2.015(5) . ?
C1 H1 1.0300(3) . ?
C1 H2 1.03000(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 C1 I2 0.00(8) . . ?
Br2 C1 I1 112.68(6) . . ?
I2 C1 I1 112.68(6) . . ?
Br2 C1 Br1 112.68(6) . . ?
I2 C1 Br1 112.68(6) . . ?
I1 C1 Br1 0.00(6) . . ?
Br2 C1 H1 108.6(4) . . ?
I2 C1 H1 108.6(4) . . ?
I1 C1 H1 110.8(4) . . ?
Br1 C1 H1 110.8(4) . . ?
Br2 C1 H2 108.6(4) . . ?
I2 C1 H2 108.6(4) . . ?
I1 C1 H2 110.8(4) . . ?
Br1 C1 H2 110.8(4) . . ?
H1 C1 H2 105.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.322
_diffrn_reflns_theta_full        29.70
_diffrn_measured_fraction_theta_full 0.322
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.094

#############################################################################

data_djm_0.80GPa
_database_code_depnum_ccdc_archive 'CCDC 681741'

# CHEMICAL DATA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
diiodomethane, polymorph II
;

_chemical_name_common            'diiodomethane, polymorph II'
_chemical_melting_point          279
_chemical_formula_moiety         'C1 H2 I2'
_chemical_formula_sum            'C H2 I2'
_chemical_formula_weight         267.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F m m 2'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z'
'-x, y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'

_cell_length_a                   7.0153(14)
_cell_length_b                   12.599(3)
_cell_length_c                   4.5877(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     405.49(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    723
_cell_measurement_theta_min      5.55
_cell_measurement_theta_max      28.62

_exptl_crystal_description       cylinder
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             456
_exptl_absorpt_coefficient_mu    15.263
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_T_max  0.21

_exptl_absorpt_process_details   
;
Correction for absorption of the diamond-anvil cell and the sample
were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
Mickiewicz University Poznań; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;

# EXPERIMENTAL DATA

_exptl_special_details           
;
Data were collected at room temperature and pressure of 0.80(5) GPa
(800000 kPa) with the crystal obtained by the in-situ high-pressure
crystallization technique.
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         800000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            867
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         5.55
_diffrn_reflns_theta_max         28.62
_reflns_number_total             92
_reflns_number_gt                87
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_reduction        
'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A. 2003)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'

# REFINEMENT DATA

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
resulting in a low data:parameter ratio.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+17.9963P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0121(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(8)
_refine_ls_number_reflns         92
_refine_ls_number_parameters     14
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.0518
_refine_ls_wR_factor_gt          0.0506
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_restrained_S_all      1.207
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.0000 0.13756(5) 0.26654(9) 0.045(3) Uani 1 2 d SD . .
C1 C 0.0000 0.0000 -0.02880(16) 0.06(9) Uani 1 4 d SD . .
H1 H 0.13280(10) 0.0000 -0.1138(2) 0.084 Uiso 1 2 d SD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0467(11) 0.042(9) 0.0462(11) 0.012(7) 0.000 0.000
C1 0.04(2) 0.1(3) 0.06(3) 0.000 0.000 0.000

# MOLECULAR GEOMETRY

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.2000(9) . ?
C1 I1 2.2000(9) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 C1 I1 103.97(5) . 2 ?

_diffrn_measured_fraction_theta_max 0.305
_diffrn_reflns_theta_full        28.62
_diffrn_measured_fraction_theta_full 0.305
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.136

#############################################################################


