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_7214895
_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_formula_moiety         'C H Br3, C6 H10 O'
_chemical_formula_sum            'C7 H11 Br3 O'
_chemical_formula_weight         350.89
_chemical_melting_point          224
_chemical_name_systematic
;
molecular complex of bromoform with cyclohexanone (1:1)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-06-28
_audit_creation_method
;
Olex2 1.1-beta
(compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4762(9)
_cell_length_b                   15.787(2)
_cell_length_c                   8.3158(11)
_cell_measurement_reflns_used    1847
_cell_measurement_temperature    210
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      2.57
_cell_volume                     1104.0(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8404
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.42
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           10.0
_diffrn_source_power             0.3
_diffrn_source_target            Mo
_diffrn_source_voltage           30.0
_exptl_absorpt_coefficient_mu    10.913
_exptl_absorpt_correction_T_max  0.1001
_exptl_absorpt_correction_T_min  0.0005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.1173 before and 0.0289 after correction.
The Ratio of minimum to maximum transmission is 0.004995004995.
The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            'dull white colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   white
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0400P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                1636
_reflns_number_total             2500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26191j.txt
_cod_data_source_block           I_bh1
_cod_database_code               7214895