Structural preferences in strong anion–π and halogen-bonded complexes: π- and σ-holes vs. frontier orbitals interaction
Grounds, Olivia; Zeller, Matthias; Rosokha, Sergiy V.; New Journal of Chemistry 42 (2018) 10572–; doi:10.1039/C7NJ04843B

data_7057043
_publ_section_title
;
 Structural preferences in strong anion--\p and halogen-bonded complexes:
 \p- and \s-holes vs. frontier orbitals interaction
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10572
_journal_paper_doi               10.1039/C7NJ04843B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C16 H36 N, 4(C8 N6), Br'
_chemical_formula_sum            'C48 H36 Br N25'
_chemical_formula_weight         1042.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3307(6)
_cell_length_b                   13.3307(6)
_cell_length_c                   15.2977(8)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      35.9353
_cell_measurement_theta_min      3.0583
_cell_volume                     2718.5(2)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2017/1 (Sheldrick, 2015, 2016), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29226
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.266
_diffrn_reflns_theta_min         3.430
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.7350
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       prism
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.012(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         6357
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                4805
_reflns_number_total             6357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04843b2.cif
_cod_data_source_block           RS_19_0m
_cod_depositor_comments
'Adding full bibliography for 7057037--7057043.cif.'
_cod_original_cell_volume        2718.5(3)
_cod_database_code               7057043
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.835
_shelx_res_checksum              41212