Molecular diversity of TEMPO-mediated cycloaddition of ketohydrazones and 3-phenacylideneoxindoles
Ye, Rong; Sun, Jing; Han, Ying; Yan, Chao-Guo; New Journal of Chemistry 45 (2021) 5075–5080; doi:10.1039/D0NJ06036D

data_7060400
_publ_section_title
;
 Molecular diversity of TEMPO-mediated cycloaddition of ketohydrazones and
 3-phenacylideneoxindoles
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5075
_journal_page_last               5080
_journal_paper_doi               10.1039/D0NJ06036D
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C38 H30 F N3 O3'
_chemical_formula_sum            'C38 H30 F N3 O3'
_chemical_formula_weight         595.65
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-09-24 deposited with the CCDC.	2021-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.660(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6264(9)
_cell_length_b                   14.8156(15)
_cell_length_c                   19.5760(19)
_cell_measurement_reflns_used    4879
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.93
_cell_measurement_theta_min      2.38
_cell_volume                     3038.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28472
_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         25.999
_diffrn_reflns_theta_min         2.111
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0054(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5961
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0563P)^2^+2.7933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3004
_reflns_number_total             5961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj06036d2.cif
_cod_data_source_block           4e
_cod_depositor_comments
'Adding full bibliography for 7060394--7060404.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7060400
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              97129
_shelx_hkl_checksum              5727