Synthesis of Spiro[pyrazolin-3,3'-oxindoles] and 3-Arylcarbonylmethyl Substituted Ylideneoxindoles by 1,3-Dipolar Cycloadditions of 3-Ylideneoxindoles and In-Situ-Generated α-Diazoketones.
Jiang, Shan; Guo, Hong-Mei; Yao, Sheng; Shi, De-Qing; Xiao, Wen-Jing; The Journal of organic chemistry 82 (2017) 10433–10443; doi:10.1021/acs.joc.7b01907

data_4032909
_publ_section_title
;
 Synthesis of Spiro[pyrazolin-3,3'-oxindoles] and 3-Arylcarbonylmethyl
 Substituted Ylideneoxindoles by 1,3-Dipolar Cycloadditions of
 3-Ylideneoxindoles and In-Situ-Generated \a-Diazoketones.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10433
_journal_page_last               10443
_journal_paper_doi               10.1021/acs.joc.7b01907
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C31 H23 N3 O3'
_chemical_formula_weight         485.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.011(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.431(2)
_cell_length_b                   8.9297(15)
_cell_length_c                   21.363(4)
_cell_measurement_reflns_used    7245
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      2.49
_cell_volume                     2462.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23626
_diffrn_reflns_theta_full        29.78
_diffrn_reflns_theta_max         29.78
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+0.4274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1791
_reflns_number_gt                4594
_reflns_number_total             6994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7b01907_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4032909--4032910.cif.
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4032909