One-pot green synthesis of biologically relevant novel spiro[indolin-2-one-3,4'-pyrano[2,3-<i>c</i>]pyrazoles] and studies on their spectral and X-ray crystallographic behaviors
Sharma, Sakshi; Brahmachari, Goutam; Kant, Rajni; Gupta, Vivek K.; Acta Crystallographica Section B 72 (2016) 335–343; doi:10.1107/S2052520616005060

data_2107505
_publ_section_title
;
 One-pot green synthesis of biologically relevant novel
 spiro[indolin-2-one-3,4'-pyrano[2,3-<i>c</i>]pyrazoles] and studies on
 their spectral and X-ray crystallographic behaviors
;
_journal_coeditor_code           BP5086
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              335
_journal_page_last               343
_journal_paper_doi               10.1107/S2052520616005060
_journal_volume                  72
_journal_year                    2016
_chemical_formula_moiety         'C19 H21 N5 O3 S'
_chemical_formula_sum            'C19 H21 N5 O3 S'
_chemical_formula_weight         399.47
_chemical_name_systematic
;
6'-amino-2-oxo-3'-propyl-2'H-spiro
[indoline-3,4'-pyrano[2,3-c]pyrazole]-5'-carboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 103.358(7)
_cell_angle_gamma                95.444(7)
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_cell_length_b                   9.7844(8)
_cell_length_c                   11.7345(10)
_cell_measurement_reflns_used    2060
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8470
_cell_measurement_theta_min      4.1900
_cell_volume                     1019.85(15)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction,2010)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 2012)'
_computing_publication_material  'PLATON (Spek,2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1049
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'Omega Scan'
_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  0.0237
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_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7141
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Crys Alis Red'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.404
_refine_ls_extinction_coef       0.032(3)
_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   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0600P)^2^+0.1872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                2912
_reflns_number_total             4006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5086sup1.cif
_cod_data_source_block           gbbb72
_cod_depositor_comments
'Adding full bibliography for 2107505--2107507.cif.'
_cod_original_cell_volume        1019.85(14)
_cod_database_code               2107505
_cod_database_fobs_code          2107505