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_7115902
_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_absolute_configuration syn
_chemical_formula_moiety         'C156 H140 B12 N4 O32'
_chemical_formula_sum            'C156 H140 B12 N4 O32'
_chemical_formula_weight         2712.43
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9953(4)
_cell_length_b                   13.9953(4)
_cell_length_c                   104.431(3)
_cell_measurement_reflns_used    12918
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.04
_cell_measurement_theta_min      2.86
_cell_volume                     20454.7(10)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II IP Area Detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       125
_diffrn_reflns_limit_l_min       -125
_diffrn_reflns_number            241990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.253
_diffrn_reflns_theta_min         3.186
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5680
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.113
_exptl_transmission_factor_max   0.947
_exptl_transmission_factor_min   0.626
_platon_squeeze_details          ' '
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
; 
 Flack x determined using 4071 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         18725
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0573
_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^)+(0.1199P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                11840
_reflns_number_total             18725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05836d2.cif
_cod_data_source_block           shelxl-sr
_cod_original_cell_volume        20454.6(13)
_cod_database_code               7115902
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.947
_shelxl_version_number           2012-9
_shelx_res_checksum              23550