Procedure-dependent construction of two isomers of trimeric self-assembled boronic esters
Kosuke Ono; Ryo Aizawa; Taiki Yamano; Suguru Ito; Nobuhiro Yasuda; Kohei Johmoto; Hidehiro Uekusa; Nobuharu Iwasawa; Chem.Commun. 50 (2014) 13683–; doi:10.1039/C4cc05836D

data_7115903
_publ_section_title
;
 Procedure-dependent construction of two isomers of trimeric
 self-assembled boronic esters
;
_journal_name_full               Chem.Commun.
_journal_page_first              13683
_journal_paper_doi               10.1039/C4cc05836D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety
'(C156 H140 B12 N4 O32), 2(C7 H8), 0.85(C7 H8), 0.6(C7 H8)'
_chemical_formula_sum            'C180.15 H167.6 B12 N4 O32'
_chemical_formula_weight         3030.29
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 98.2499(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7426(8)
_cell_length_b                   21.2737(6)
_cell_length_c                   42.0407(11)
_cell_measurement_temperature    90(2)
_cell_volume                     22784.9(11)
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 29
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.78215
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            301629
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        27.988
_diffrn_reflns_theta_max         28.111
_diffrn_reflns_theta_min         1.372
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6370
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.042
_exptl_transmission_factor_max   0.997
_exptl_transmission_factor_min   0.799
_platon_squeeze_details
;
;
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0133(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2027
_refine_ls_number_reflns         41282
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1756
_refine_ls_R_factor_gt           0.1104
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1825P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.2986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17919
_reflns_number_total             41282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05836d2.cif
_cod_data_source_block           shelxl-sr
_cod_original_cell_volume        22785.0(12)
_cod_original_formula_sum        'C180.15 H167.60 B12 N4 O32'
_cod_database_code               7115903
_shelx_estimated_absorpt_t_min   0.995
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2014-1
_shelx_res_checksum              58047