Low-melting molecular complexes. Halogen bonds in molecular complexes of bromoform
Yufit, Dmitry S.; Zubatyuk, Roman; Shishkin, Oleg V.; Howard, Judith A. K.; CrystEngComm 14 (2012) 8222–; doi:10.1039/c2ce26191j

data_7214896
_publ_section_title
;
 Low-melting molecular complexes. Halogen bonds in molecular complexes of
 bromoform
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              8222
_journal_paper_doi               10.1039/c2ce26191j
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C2 H6 O S, C H Br3'
_chemical_formula_sum            'C3 H7 Br3 O S'
_chemical_formula_weight         330.88
_chemical_melting_point          237.0(10)
_chemical_name_systematic
;
molecular complex of bromoform with dimethylsulfoxide (1:1)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.923(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9562(8)
_cell_length_b                   9.6768(9)
_cell_length_c                   12.0633(17)
_cell_measurement_reflns_used    2036
_cell_measurement_temperature    225
_cell_measurement_theta_max      33.0749
_cell_measurement_theta_min      3.3155
_cell_volume                     925.33(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      225
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
1 omega -63.00 32.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.1216 77.0000 120.0000 190

2 omega -101.00 35.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.1216 -19.0000 -30.0000 272

3 omega 71.00 103.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- 31.7466 179.0000 120.0000 64

4 omega -102.00 -7.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.1216 -57.0000 -90.0000 190

5 omega -105.00 0.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.1216 -38.0000 150.0000 210

6 omega -55.00 39.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.1216 57.0000 0.0000 188

7 omega 56.00 112.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- 31.7466 179.0000 -60.0000 112

8 omega -1.00 104.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- 31.7466 77.0000 90.0000 210

9 omega 56.00 112.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- 31.7466 179.0000 0.0000 112

10 omega -111.00 -81.00 0.5000 15.0000
omega____ theta____ kappa____ phi______ frames
- -31.1216 -179.0000 -30.0000 60
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0824365000
_diffrn_orient_matrix_UB_12      0.0219456000
_diffrn_orient_matrix_UB_13      0.0195218000
_diffrn_orient_matrix_UB_21      -0.0312668000
_diffrn_orient_matrix_UB_22      0.0672882000
_diffrn_orient_matrix_UB_23      0.0089208000
_diffrn_orient_matrix_UB_31      -0.0160243000
_diffrn_orient_matrix_UB_32      -0.0186913000
_diffrn_orient_matrix_UB_33      0.0549584000
_diffrn_radiation_collimation    monochromator
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_xray_symbol    Mo
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_unetI/netI     0.0979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7041
_diffrn_reflns_theta_full        29.47
_diffrn_reflns_theta_max         29.47
_diffrn_reflns_theta_min         3.32
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_type              'sealed tube'
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    13.229
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull light white'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             616
_exptl_crystal_recrystallization_method 'Grown in situ @228K'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.841
_refine_diff_density_min         -2.000
_refine_diff_density_rms         0.267
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(4)
_refine_ls_extinction_coef       0.0049(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         2557
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1357P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2358
_reflns_number_gt                1915
_reflns_number_total             2557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26191j.txt
_cod_data_source_block           II_bbs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '236-238' was changed to '237.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               7214896
_chemical_oxdiff_formula         'C3 H7 Br3 S1 O1'
_chemical_oxdiff_usercomment     'Grown in situ at 228K'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44