Ultrasound-Assisted Regio- and Stereoselective Synthesis of Bis-[1`,4`-diaryl-1-oxo-spiro-benzosuberane-2,5`-pyrazoline] Derivatives via 1,3-Dipolar Cycloaddition
Behbehani, Haider; Ibrahim, Hamada Mohamed; Dawood, KM; RSC Adv.  (2015) –; doi:10.1039/C5RA02972D

data_7219732
_publ_section_title
;
 Ultrasound-Assisted Regio- and Stereoselective Synthesis of
 Bis-[1`,4`-diaryl-1-oxo-spiro-benzosuberane-2,5`-pyrazoline] Derivatives
 via 1,3-Dipolar Cycloaddition
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA02972D
_journal_year                    2015
_chemical_formula_sum            'C56 H56 N6 O4'
_chemical_formula_weight         877.07
_chemical_name_common            Hamada_24_11_14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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_update_record
;
2015-02-08 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.077(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0471(4)
_cell_length_b                   18.9631(7)
_cell_length_c                   22.9273(8)
_cell_measurement_temperature    296.(2)
_cell_volume                     4728.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53472
_diffrn_reflns_theta_full        66.71
_diffrn_reflns_theta_max         66.71
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Flake
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0804P)^2^+0.2292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1739
_reflns_number_gt                4297
_reflns_number_total             8266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra02972d1.cif
_cod_data_source_block           I
_cod_database_code               7219732