Rh(iii)-catalyzed spiroannulation of 3-arylquinoxalin-2(1H)-ones with alkynes: practical access to spiroquinoxalinones
Zhang, Yuanfei; Huang, Ting; Li, Xinghua; Zhang, Min; Song, Ying; Huang, Kelin; Su, Weiping; RSC Advances 10 (2020) 22216–22221; doi:10.1039/D0RA03348K

data_7240679
_publ_section_title
;
 Rh(iii)-catalyzed spiroannulation of 3-arylquinoxalin-2(1H)-ones with
 alkynes: practical access to spiroquinoxalinones
;
_journal_issue                   37
_journal_name_full               'RSC Advances'
_journal_page_first              22216
_journal_page_last               22221
_journal_paper_doi               10.1039/D0RA03348K
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C29 H21 Cl N2 O'
_chemical_formula_sum            'C29 H21 Cl N2 O'
_chemical_formula_weight         448.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-03-27 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.099(7)
_cell_length_b                   10.570(3)
_cell_length_c                   9.121(2)
_cell_measurement_reflns_used    6222
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.90
_cell_measurement_theta_min      2.61
_cell_volume                     2227.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.872
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24214
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.668
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.493
_diffrn_reflns_theta_min         2.612
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       prism
_exptl_crystal_F_000             936.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Flack x determined using 1408 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         7815
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0625P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.460
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.443
_reflns_number_gt                4260
_reflns_number_total             7815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra03348k2.cif
_cod_data_source_block           sy
_cod_depositor_comments          'Adding full bibliography for 7240679.cif.'
_cod_original_cell_volume        2226.8(11)
_cod_database_code               7240679
_shelxl_version_number           2013-2
_shelx_res_checksum              19187