From propenolysis to enyne metathesis: tools for expedited assembly of 4<i>a</i>,8<i>a</i>-azaboranaphthalene and extended polycycles with embedded BN.
Rulli, Federica; Sanz-Liarte, Guillem; Roca, Pol; Martínez, Nina; Medina, Víctor; Puig de la Bellacasa, Raimon; Shafir, Alexandr; Cuenca, Ana B.; Chemical science 15 (2024) 5674–5680; doi:10.1039/d3sc06676b

data_1571177
_publ_section_title
;
 From propenolysis to enyne metathesis: tools for expedited assembly of
 4<i>a</i>,8<i>a</i>-azaboranaphthalene and extended polycycles with
 embedded BN.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              5674
_journal_page_last               5680
_journal_paper_doi               10.1039/d3sc06676b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C20 H24 B N O8), 2(C2 H5 O0.50)'
_chemical_formula_sum            'C22 H29 B N O8.5'
_chemical_formula_weight         454.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2023-09-24 deposited with the CCDC.	2024-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                79.685(2)
_cell_angle_beta                 85.884(2)
_cell_angle_gamma                82.938(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0333(3)
_cell_length_b                   11.0537(5)
_cell_length_c                   15.3641(7)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.22
_cell_measurement_theta_min      2.50
_cell_volume                     1164.73(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60033
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.639
_diffrn_reflns_theta_min         1.884
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       prism
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7146
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0726
_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^)+(0.0937P)^2^+0.8888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5087
_reflns_number_total             7146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06676b2.cif
_cod_data_source_block           mo_3ANABB45_0m_a
_cod_depositor_comments
'Adding full bibliography for 1571177--1571178.cif.'
_cod_original_formula_sum        'C22 H29 B N O8.50'
_cod_database_code               1571177
_shelx_shelxl_version_number     2019/1
_shelx_res_checksum              61296