Symmetrical Noncovalent Interactions Br···Br Observed in Crystal Structure of Exotic Primary Peroxide
Bolotin, Dmitrii S.; Il’in, Mikhail V.; Suslonov, Vitalii V.; Novikov, Alexander S.; Symmetry 12 (2020) 637–; doi:10.3390/sym12040637

data_1558009
_publ_section_title
;
 Symmetrical Noncovalent Interactions Br&#x00B7;&#x00B7;&#x00B7;Br
 Observed in Crystal Structure of Exotic Primary Peroxide
;
_journal_issue                   4
_journal_name_full               Symmetry
_journal_page_first              637
_journal_paper_doi               10.3390/sym12040637
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C12 H14 Br N3 O2'
_chemical_formula_sum            'C12 H14 Br N3 O2'
_chemical_formula_weight         312.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.179(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4894(5)
_cell_length_b                   7.24200(17)
_cell_length_c                   20.4992(5)
_cell_measurement_reflns_used    5032
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4910
_cell_measurement_theta_min      3.1190
_cell_volume                     2493.56(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -25.00    6.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.2678  -99.0000  120.0000 31

  2 omega  -42.00   42.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  -57.0000    0.0000 84

  3 omega  -38.00   66.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  -19.0000   60.0000 104

  4 omega  -19.00    7.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   19.0000    0.0000 26

  5 omega  -22.00    4.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.2678  -99.0000   60.0000 26

  6 omega    5.00   31.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   57.0000 -120.0000 26

  7 omega   62.00   88.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   57.0000 -120.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0349753000
_diffrn_orient_matrix_UB_12      -0.0088040000
_diffrn_orient_matrix_UB_13      0.0108210000
_diffrn_orient_matrix_UB_21      -0.0123967000
_diffrn_orient_matrix_UB_22      0.0892504000
_diffrn_orient_matrix_UB_23      -0.0130083000
_diffrn_orient_matrix_UB_31      -0.0201736000
_diffrn_orient_matrix_UB_32      -0.0394037000
_diffrn_orient_matrix_UB_33      -0.0317959000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15490
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.997
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+2.3392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4644
_reflns_number_total             5728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Structure.cif
_cod_data_source_block           imv319
_cod_original_cell_volume        2493.58(11)
_cod_database_code               1558009
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Br C16 N4'
_shelx_estimated_absorpt_t_max   0.559
_shelx_estimated_absorpt_t_min   0.559
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10A(H10C,H10D), C12(H12A,H12B), C10(H10A,H10B), C9(H9A,H9B), C9A(H9AA,H9AB),
 C12A(H12C,H12D), C11(H11A,H11B), C11A(H11C,H11D)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N1A(H1A), C7(H7), C8(H8), C4A(H4A), C5A(H5A), C8A(H8A), C7A(H7A),
 C5(H5), C4(H4)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O2A(H2A)
;
_shelx_res_checksum              30350
_shelx_hkl_checksum              54617
_olex2_date_sample_data_collection 1505311520.06
_olex2_submission_special_instructions 'No special instructions were received'