Catalyst-and solvent-free one-pot synthesis of some novel polyheterocycles from aryldiazenyl salicylaldehyde derivatives
Parmar, Narsidas J.; Patel, Rikin A.; Teraiya, Shashikant B.; Sharma, Deepak; Gupta, Vivek K.; RSC Advances 2 (2012) 3069–; doi:10.1039/c2ra00930g

data_7238567
_publ_section_title
;
 Catalyst-and solvent-free one-pot synthesis of some novel
 polyheterocycles from aryldiazenyl salicylaldehyde derivatives
;
_journal_issue                   7
_journal_name_full               'RSC Advances'
_journal_page_first              3069
_journal_paper_doi               10.1039/c2ra00930g
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C26 H22 N4 O2.C H Cl3'
_chemical_formula_sum            'C27 H23 Cl3 N4 O2'
_chemical_formula_weight         541.84
_chemical_name_systematic
;
10-(4-phenyldiazenyl)-3-(3-phenyl)-1-methyl-3,5a,6,11b-
tetrahydro-5H-benzopyrano[4',3'-4,5]pyrano[2,3-c]-
pyrazole chloroform solvate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                83.079(4)
_cell_angle_beta                 80.504(4)
_cell_angle_gamma                74.566(4)
_cell_formula_units_Z            2
_cell_length_a                   8.0866(3)
_cell_length_b                   12.1875(6)
_cell_length_c                   13.9665(7)
_cell_measurement_reflns_used    4556
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8389
_cell_measurement_theta_min      3.5004
_cell_volume                     1304.40(11)
_computing_cell_refinement       'SAINT 6.45 (Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 (Bruker, 2003)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'PLATON(Spek,1999)$ PARST(1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11791
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.004(2)
_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   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4535
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0867P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                3089
_reflns_number_total             4535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra00930g.txt
_cod_data_source_block           d3final
_cod_original_cell_volume        1304.40(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7238567