Self-Assembly of 4-(Diethylboryl)pyridine: Crystal Structures of the Cyclic Pentamer and Hexamer and Their Solvent-Dependent Selective Crystallization.
Wakabayashi, Shigeharu; Hori, Yuka; Komeda, Seiji; Shimizu, Yuki; Ohki, Yasuhiro; Horiuchi, Misaki; Itoh, Takahito; Sugihara, Yoshikazu; Tatsumi, Kazuyuki; The Journal of organic chemistry 81 (2016) 2399–2404; doi:10.1021/acs.joc.5b02886

data_4036589
_publ_section_title
;
 Self-Assembly of 4-(Diethylboryl)pyridine: Crystal Structures of the
 Cyclic Pentamer and Hexamer and Their Solvent-Dependent Selective
 Crystallization.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2399
_journal_page_last               2404
_journal_paper_doi               10.1021/acs.joc.5b02886
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C111 H171 B12 Cl9 N12'
_chemical_formula_sum            'C111 H171 B12 Cl9 N12'
_chemical_formula_weight         2122.45
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            3
_cell_length_a                   17.318(5)
_cell_length_b                   17.318(5)
_cell_length_c                   34.804(11)
_cell_measurement_reflns_used    2603
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      3.20
_cell_volume                     9040(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b29'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b29'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1329
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            99866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.558
_diffrn_reflns_theta_min         3.227
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3399.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     219
_refine_ls_number_reflns         4637
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1443
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2423
_reflns_number_gt                2258
_reflns_number_total             4637
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo5b02886_si_004.cif
_cod_data_source_block           wakabayashi3
_cod_original_sg_symbol_H-M      'R -3:H'
_cod_database_code               4036589