Spirocyclopropanes from Intramolecular Cyclopropanation of Pyranopyrazoles and Pyranopyrimidine-diones and Lewis Acid Mediated (3 + 2) Cycloadditions of Spirocyclopropylpyrazolones.
Mukherjee, Prasun; Das, Asish R.; The Journal of organic chemistry 82 (2017) 2794–2802; doi:10.1021/acs.joc.7b00089

data_4032248
_publ_section_title
;
 Spirocyclopropanes from Intramolecular Cyclopropanation of
 Pyranopyrazoles and Pyranopyrimidine-diones and Lewis Acid Mediated (3 +
 2) Cycloadditions of Spirocyclopropylpyrazolones.
;
_journal_issue                   5
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2794
_journal_page_last               2802
_journal_paper_doi               10.1021/acs.joc.7b00089
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C27 H19 N5 O S'
_chemical_formula_sum            'C27 H19 N5 O S'
_chemical_formula_weight         461.53
_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                 93.247(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.565(11)
_cell_length_b                   11.634(9)
_cell_length_c                   14.456(11)
_cell_measurement_reflns_used    1668
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.27
_cell_measurement_theta_min      2.25
_cell_volume                     2278(3)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16269
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.173
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             960
_refine_diff_density_max         0.194
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         4282
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                2364
_reflns_number_total             4282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7b00089_si_003.cif
_cod_data_source_block           ard_pm_scnl_0m
_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/current/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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4032248