Expeditious synthesis of functionalized tricyclic 4-spiro pyrano[2,3-c]pyrazoles in aqueous medium using dodecylbenzenesulphonic acid as a Brønsted acid–surfactant-combined catalyst
Mukherjee, Prasun; Paul, Sanjay; Das, Asish R.; New J. Chem. 39 (2015) 9480–; doi:10.1039/C5NJ01728A

data_7055127
_publ_section_title
;
 Expeditious synthesis of functionalized tricyclic 4-spiro
 pyrano[2,3-c]pyrazoles in aqueous medium using dodecylbenzenesulphonic
 acid as a Br\/onsted acid--surfactant-combined catalyst
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              9480
_journal_paper_doi               10.1039/C5NJ01728A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C26 H24 N2 O4'
_chemical_formula_sum            'C26 H24 N2 O4'
_chemical_formula_weight         428.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-02 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                73.821(3)
_cell_angle_beta                 81.557(3)
_cell_angle_gamma                69.541(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8170(8)
_cell_length_b                   9.4031(10)
_cell_length_c                   16.4402(17)
_cell_measurement_temperature    296(2)
_cell_volume                     1085.7(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX V1.80.03'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12030
_diffrn_reflns_theta_full        24.55
_diffrn_reflns_theta_max         24.55
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.9824
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.136
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0099(15)
_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   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0400P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                2664
_reflns_number_total             3599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj01728a2.cif
_cod_data_source_block           ard_pm_phdim_0m
_cod_depositor_comments
'Adding full bibliography for 7055124--7055127.cif.'
_cod_database_code               7055127