Lossen rearrangement by Rh(III)-catalyzed C-H activation/annulation of aryl hydroxamates with alkynes: access to quinolone-containing amino acid derivatives.
Petropavlovskikh, Dmitry A.; Vorobyeva, Daria V.; Godovikov, Ivan A.; Nefedov, Sergey E.; Filippov, Oleg A.; Osipov, Sergey N.; Organic & biomolecular chemistry 19 (2021) 9421–9426; doi:10.1039/d1ob01711j

data_7158342
_publ_section_title
;
 Lossen rearrangement by Rh(III)-catalyzed C-H activation/annulation of
 aryl hydroxamates with alkynes: access to quinolone-containing amino acid
 derivatives.
;
_journal_issue                   43
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9421
_journal_page_last               9426
_journal_paper_doi               10.1039/d1ob01711j
_journal_volume                  19
_journal_year                    2021
_chemical_formula_sum            'C29 H24.5 Cl2 F3 N2 O5'
_chemical_formula_weight         608.90
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-07-20 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.774(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.8152(8)
_cell_length_b                   16.2213(11)
_cell_length_c                   32.017(2)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.27
_cell_volume                     5604.8(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0648
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
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_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            52853
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.207
_exptl_absorpt_coefficient_mu    0.294
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         13521
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_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1291
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_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^)+(0.0921P)^2^+7.2422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.2095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8156
_reflns_number_total             13521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob01711j2.cif
_cod_data_source_block           snoorg3
_cod_depositor_comments
;
Adding full bibliography for 7158340--7158342.cif.

2024-10-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C58 H49 Cl4 F6 N4 O10'
_cod_original_formula_weight         1217.81
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5604.7(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7158342
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              96681