Construction of Spirocyclopropane-Linked Heterocycles Containing Both Pyrazolones and Oxindoles through Michael/Alkylation Cascade Reactions.
Li, Jun-Hua; Feng, Ting-Fan; Du, Da-Ming; The Journal of organic chemistry 80 (2015) 11369–11377; doi:10.1021/acs.joc.5b01940

data_4036428
_publ_section_title
;
 Construction of Spirocyclopropane-Linked Heterocycles Containing Both
 Pyrazolones and Oxindoles through Michael/Alkylation Cascade Reactions.
;
_journal_issue                   22
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11369
_journal_page_last               11377
_journal_paper_doi               10.1021/acs.joc.5b01940
_journal_volume                  80
_journal_year                    2015
_chemical_formula_sum            'C25 H18.67 Cl N3 O2.34'
_chemical_formula_weight         433.93
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
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_symmetry_cell_setting           monoclinic
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 91.207(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.649(4)
_cell_length_b                   11.438(3)
_cell_length_c                   14.333(4)
_cell_measurement_reflns_used    6302
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.105
_cell_measurement_theta_min      2.170
_cell_volume                     2073.2(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  AFC10/Saturn724+
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_limit_k_max       15
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_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.8966
_exptl_absorpt_correction_type   Multi-scans
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             901
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_exptl_crystal_size_mid          0.08
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5240
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_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+1.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1787
_reflns_number_gt                4307
_reflns_number_total             5240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b01940_si_001.cif
_cod_data_source_block           bo4017
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2073.1(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4036428