First structural evidence of a Se–Br–Br halogen-bonded molecular complex
Torubaev, Yury V.; Skabitskiy, Ivan V.; Pavlova, Alina V.; Pasynskii, Alexander A.; New Journal of Chemistry 41 (2017) 3606–; doi:10.1039/C6NJ04096A

data_7059095
_publ_section_title
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 First structural evidence of a Se--Br--Br halogen-bonded molecular
 complex
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3606
_journal_paper_doi               10.1039/C6NJ04096A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C8 H12 Br3 Se, 3.5(Br)'
_chemical_formula_sum            'C8 H12 Br6.5 Se'
_chemical_formula_weight         706.52
_chemical_name_systematic
'?2,6-dibromo-9-selenabicyclo[3.3.1]nonanebromide pentabromide'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_Int_Tables_number      12
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-12-27 deposited with the CCDC.
2017-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.048(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.440(2)
_cell_length_b                   14.832(2)
_cell_length_c                   13.0060(19)
_cell_measurement_reflns_used    3069
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.40
_cell_volume                     3169.3(7)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19170
_diffrn_reflns_theta_full        28.9997
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.730
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.2719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1540 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.3644.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.9612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2560.8281
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.9025
_refine_diff_density_min         -1.8642
_refine_diff_density_rms         0.4346
_refine_ls_d_res_high            0.7330
_refine_ls_d_res_low             8.5018
_refine_ls_goodness_of_fit_ref   0.9910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     150
_refine_ls_number_reflns         4359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9910
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+3.7111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2968
_reflns_number_total             4359
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6nj04096a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        3169.3(8)
_cod_database_code               7059095
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C1(H1), C4(H4), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C2(H2a,H2b), C6(H6a,H6b), C3(H3a,H3b)
;
_olex2_submission_special_instructions 'No special instructions were received'