Structure determination of a bis[4-(di-n-butylamino)phenyl](pyridin-3-yl)borane tetramer highlighting a unique geometric conformation of the core 16-membered ring.
Lovstedt, Alex; Dempsey, Stephen H.; Kass, Steven R.; Acta crystallographica. Section C, Structural chemistry 79 (2023) 170–176; doi:10.1107/S2053229623002619

data_2312081
_publ_section_title
;
 Structure determination of a
 bis[4-(di-n-butylamino)phenyl](pyridin-3-yl)borane tetramer highlighting
 a unique geometric conformation of the core 16-membered ring.
;
_journal_coeditor_code           EP3030
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              170
_journal_page_last               176
_journal_paper_doi               10.1107/S2053229623002619
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C132 H192 B4 N12'
_chemical_formula_moiety         'C132 H192 B4 N12'
_chemical_formula_sum            'C132 H192 B4 N12'
_chemical_formula_weight         1990.22
_chemical_name_common
2\l^4^,4\l^4^,6\l^4^,8\l^4^-Tetrabora-1,3,5,7(1,3)-tetrapyridinacyclooctaphane-1^1^,3^1^,5^1^,7^1^-tetrakis(ylium)
_chemical_name_systematic
2,2,8,8,14,14,20,20-Octakis[4-(dibutylamino)phenyl]-1,7,13,19-tetraaza-2,8,14,20-tetraborapentacyclo[19.3.1.1^3,7^.1^9,13^.1^15,19^]octacosa-1(25),3,5,7(28),9(27),10,12,15(26),16,18,21,23-dodecaene-1,7,13,19-tetrakis(ylium)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                74.729(2)
_cell_angle_beta                 85.878(2)
_cell_angle_gamma                89.857(2)
_cell_formula_units_Z            2
_cell_length_a                   15.5952(11)
_cell_length_b                   15.7968(11)
_cell_length_c                   25.7779(15)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.58
_cell_volume                     6109.5(7)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
ShelXle (H\"ubschle <i>et al.</i>,  2011) and
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Photon-III CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            181628
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.409
_diffrn_reflns_theta_min         1.922
_diffrn_source                   micro
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1446
_refine_ls_number_reflns         25030
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0604P)^2^+3.2856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                19004
_reflns_number_total             25030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ep3030sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2312081.cif.'
_cod_database_code               2312081
_cod_database_fobs_code          2312081
_shelx_estimated_absorpt_t_min   0.991
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              72674
_shelx_res_checksum              71002