Boroxine template for macrocyclization and postfunctionalization
Ono, Kosuke; Onodera, Satoru; Kawai, Hidetoshi; Chemical Communications  (2022) –; doi:10.1039/D2CC04691A

data_7130836
_publ_section_title
;
 Boroxine template for macrocyclization and postfunctionalization
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04691A
_journal_year                    2022
_chemical_formula_moiety         'C54 H75 B3 O9'
_chemical_formula_sum            'C54 H75 B3 O9'
_chemical_formula_weight         900.61
_chemical_name_systematic        'Boroxine macrocycle'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-08-09 deposited with the CCDC.	2022-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.201(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.6791(3)
_cell_length_b                   19.9517(4)
_cell_length_c                   18.0668(3)
_cell_measurement_reflns_used    21648
_cell_measurement_temperature    193
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      3.73
_cell_volume                     5304.1(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30762
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.232
_diffrn_reflns_theta_min         3.733
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944.00
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     381
_refine_ls_number_reflns         4866
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0652P)^2^+5.7297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2747
_reflns_number_total             4866
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d2cc04691a2.cif
_cod_data_source_block           1901002os
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7130836
_shelx_res_checksum              85649
_shelx_hkl_checksum              85905