A K±promoted Diels‒Alder reaction by using a self-assembled macrocyclic boronic ester containing two crown ether moieties
Ono, Kosuke; Niibe, Morikazu; Iwasawa, Nobuharu; Chemical Science  (2019) –; doi:10.1039/C9SC01597C

data_1551953
_publ_section_title
;
 A K+-promoted Diels--Alder reaction by using a self-assembled macrocyclic
 boronic ester containing two crown ether moieties
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01597C
_journal_year                    2019
_chemical_formula_moiety         'C72H80B4O20, 3.75(CH2Cl2)'
_chemical_formula_sum            'C75.75 H87.5 B4 Cl7.5 O20'
_chemical_formula_weight         1627.07
_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-2013
_audit_update_record
;
2017-04-02 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6688(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3378(10)
_cell_length_b                   20.9587(10)
_cell_length_c                   22.0613(12)
_cell_measurement_reflns_used    16657
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      67.89
_cell_measurement_theta_min      3.18
_cell_volume                     8475.4(8)
_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-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.1521
_diffrn_reflns_av_unetI/netI     0.1504
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78205
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         3.203
_diffrn_source                   'rotating anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3398
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.713
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         15473
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.2748
_refine_ls_R_factor_gt           0.1203
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3170
_refine_ls_wR_factor_ref         0.4130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3923
_reflns_number_total             15473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01597c2.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C75.75 H87.50 B4 Cl7.50 O20'
_cod_database_code               1551953
_shelx_estimated_absorpt_t_min   0.676
_shelx_estimated_absorpt_t_max   0.785
_shelxl_version_number           2013-4
_shelx_res_checksum              64951