The relationship between the crystal habit and the energy framework pattern: a case study involving halogen bonding on the edge of a covalent bond
Torubaev, Yury V.; Howe, Devin; Leitus, Gregory; Rosokha, Sergiy V.; CrystEngComm 25 (2023) 3380–3390; doi:10.1039/D3CE00316G

data_7246715
_publ_section_title
;
 The relationship between the crystal habit and the energy framework
 pattern: a case study involving halogen bonding on the edge of a covalent
 bond
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              3380
_journal_page_last               3390
_journal_paper_doi               10.1039/D3CE00316G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C6 H12 Br0.957 I0.983 N2'
_chemical_formula_sum            'C6 H12 Br0.96 I0.98 N2'
_chemical_formula_weight         313.37
_chemical_name_systematic        '1,4-diazabicyclo[2,2,2]octane  iodine bromide'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-06-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-30 deposited with the CCDC.	2023-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6028(9)
_cell_length_b                   7.1603(3)
_cell_length_c                   5.9684(2)
_cell_measurement_reflns_used    5542
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      3.41
_cell_volume                     923.21(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8758
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.993
_diffrn_reflns_theta_min         1.885
_exptl_absorpt_coefficient_mu    7.489
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0449 after correction.
The Ratio of minimum to maximum transmission is 0.6483.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_description       plate
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00156(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0141
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0043P)^2^+0.6057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0284
_refine_ls_wR_factor_ref         0.0287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1232
_reflns_number_total             1307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00316g2.cif
_cod_data_source_block           mo_dabco_ibr_0ma
_cod_depositor_comments
'Adding full bibliography for 7246714--7246716.cif.'
_cod_database_code               7246715
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.521
_shelx_estimated_absorpt_t_min   0.118
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H2A(0.5) H2B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
;
_shelx_res_checksum              54378
_shelx_hkl_checksum              22393
_olex2_submission_special_instructions 'No special instructions were received'