Towards tetrasubstituted furans through rearrangement and cyclodimerization of acetylenic ketones
Dai, Zhenyun; Xu, Chenyong; Tian, Rongqiang; Duan, Zheng; Organic & Biomolecular Chemistry 22 (2024) 1172–1175; doi:10.1039/D3OB02036C

data_7159765
_publ_section_title
;
 Towards tetrasubstituted furans through rearrangement and
 cyclodimerization of acetylenic ketones
;
_journal_issue                   6
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              1172
_journal_page_last               1175
_journal_paper_doi               10.1039/D3OB02036C
_journal_volume                  22
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C44 H50 B O4 P'
_chemical_formula_sum            'C44 H50 B O4 P'
_chemical_formula_weight         684.683
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-17 deposited with the CCDC.	2024-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   10.982(2)
_cell_length_b                   15.999(3)
_cell_length_c                   21.423(4)
_cell_measurement_reflns_used    7237
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      20.456
_cell_measurement_theta_min      2.247
_cell_volume                     3764.0(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.00
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9981
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.9981
_diffrn_reflns_Laue_measured_fraction_max 0.9981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73466
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9988
_diffrn_reflns_theta_full        24.9951
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.115
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             1465.215
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.1807
_refine_diff_density_min         -0.2036
_refine_diff_density_rms         0.0426
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_d_res_high            0.8410
_refine_ls_d_res_low             9.7730
_refine_ls_goodness_of_fit_ref   1.0453
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0453
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.8438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         1.000
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              25
_reflns_limit_l_min              -25
_reflns_number_gt                5193
_reflns_number_total             6619
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ob02036c2.cif
_cod_data_source_block           mo_20230114c_0m_a
_cod_depositor_comments
'Adding full bibliography for 7159765--7159766.cif.'
_cod_original_cell_volume        3764.2(12)
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7159765
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 C1(H1), C31(H31), C20(H20), C24(H24), C27(H27), C28(H28), C30(H30), C21(H21),
 C39(H39), C14(H14), C18(H18), C23(H23), C33(H33), C44(H44a,H44b), C15(H15),
 C32(H32a,H32b,H32c), C9(H9), C38(H38a,H38b), C17(H17), C43(H43a,H43b),
 C16(H16), C40(H40a,H40b), C34(H34a,H34b), C11(H11), C42(H42a,H42b), C10(H10),
 C7(H7), C37(H37a,H37b), C8(H8), C25(H25a,H25b,H25c), C35(H35a,H35b), C36(H36a,
 H36b), C41(H41a,H41b), B1(H1a,H1b,H1c)
;
_olex2_submission_special_instructions 'No special instructions were received'