Rhodium catalyzed sequential dual C-H annulation of 3-arylisoxazoles with 1,6-diynes to access fused naphthalenes.
Kotipalli, Ramesh; Mahipal Reddy, T.; Nanubolu, Jagadeesh Babu; Reddy, Maddi Sridhar; Organic & biomolecular chemistry 23 (2025) 5753–5757; doi:10.1039/d5ob00466g

data_7160553
_publ_section_title
;
 Rhodium catalyzed sequential dual C-H annulation of 3-arylisoxazoles with
 1,6-diynes to access fused naphthalenes.
;
_journal_issue                   24
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5753
_journal_page_last               5757
_journal_paper_doi               10.1039/d5ob00466g
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C38 H29 N O3'
_chemical_formula_sum            'C38 H29 N O3'
_chemical_formula_weight         547.62
_chemical_name_systematic
1,1'-(4,9-diphenyl-5-(5-phenylisoxazol-3-yl)-2,3-dihydro-1H-cyclopenta[b]naphthalene-2,2-diyl)bis(ethan-1-one)
_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   geom
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_audit_update_record
;
2025-03-05 deposited with the CCDC.	2025-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                96.394(3)
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_computing_data_reduction        'Bruker SAINT'
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_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0912
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_diffrn_reflns_limit_k_max       20
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_diffrn_reflns_number            40871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.404
_diffrn_reflns_theta_min         2.542
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       plate
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_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Tetrahydrofuran'
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0753P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4478
_reflns_number_total             7969
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           kb1649_0m_a_sq
_cod_depositor_comments          'Adding full bibliography for 7160553.cif.'
_cod_database_code               7160553
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              5518
_shelx_fab_checksum              9615