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_4036591
_publ_section_title
;
 Self-Assembly of 4-(Diethylboryl)pyridine: Crystal Structures of the
 Cyclic Pentamer and Hexamer and Their Solvent-Dependent Selective
 Crystallization.
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_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         'C45 H70 B5 N5, 2(C6 H6)'
_chemical_formula_sum            'C57 H82 B5 N5'
_chemical_formula_weight         891.35
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.698(3)
_cell_angle_beta                 95.893(3)
_cell_angle_gamma                111.738(4)
_cell_formula_units_Z            2
_cell_length_a                   10.850(2)
_cell_length_b                   11.342(2)
_cell_length_c                   24.340(4)
_cell_measurement_reflns_used    5922
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     2750.5(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            91217
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  0.9879
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         12711
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+0.8369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1797
_reflns_number_gt                9582
_reflns_number_total             12711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b02886_si_005.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_database_code               4036591