Oxidative ring expansion of spirocyclic oxindole derivatives.
Bergman, Jan; Arewång, Carl-Johan; Svensson, Per H.; The Journal of organic chemistry 79 (2014) 9065–9073; doi:10.1021/jo501269f

data_4029940
_publ_section_title
;
 Oxidative ring expansion of spirocyclic oxindole derivatives.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9065
_journal_page_last               9073
_journal_paper_doi               10.1021/jo501269f
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C15 H10 N4 O2'
_chemical_formula_sum            'C15 H10 N4 O2'
_chemical_formula_weight         278.27
_chemical_name_systematic
; 
 13-Hydroxyimino-6H-quinoazolino[3,4-a]quinazoline-6 (7H)-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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.2300(10)
_cell_angle_beta                 90.1900(10)
_cell_angle_gamma                98.070(2)
_cell_formula_units_Z            8
_cell_length_a                   8.1501(4)
_cell_length_b                   17.7300(8)
_cell_length_c                   17.8702(9)
_cell_measurement_temperature    100(2)
_cell_volume                     2379.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_radiation_monochromator  'Si filter'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70611
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0165(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         11004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1264P)^2^+3.9378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2181
_reflns_number_gt                10367
_reflns_number_total             11004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo501269f_si_003.cif
_cod_data_source_block           Jasinioxim
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-06-07

 Adding full bibliography for 4029939--4029940.cif.
;
_cod_original_cell_volume        2379.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4029940