Three component solvent-free synthesis of 1H-pyrazol-5(4H)-one-based heterocyclic ketene aminal derivatives
Yu, Fuchao; Chen, Zhiqiong; Hao, Xiaopan; Jiang, Xiuyang; Yan, Shengjiao; Lin, Jun; RSC Advances 3 (2013) 13183–; doi:10.1039/c3ra41547c

data_7239057
_publ_section_title
;
 Three component solvent-free synthesis of 1H-pyrazol-5(4H)-one-based
 heterocyclic ketene aminal derivatives
;
_journal_issue                   32
_journal_name_full               'RSC Advances'
_journal_page_first              13183
_journal_paper_doi               10.1039/c3ra41547c
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C22 H20 N4 O2'
_chemical_formula_weight         372.42
_chemical_name_systematic
;

(4Z)-4-(2-(imidazolidin-2-ylidene)-3-oxo-3-phenylpropylidene)
-3-methyl-1-phenyl-1H-pyrazol-5(4H)-one

;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.888(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.059(3)
_cell_length_b                   11.2828(16)
_cell_length_c                   15.679(2)
_cell_measurement_reflns_used    1848
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.34
_cell_measurement_theta_min      2.38
_cell_volume                     3705.7(9)
_computing_cell_refinement       'Bruker apex II'
_computing_data_collection       'Bruker apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20758
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9886
_exptl_absorpt_correction_T_min  0.9783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0023(4)
_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   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         6533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                3290
_reflns_number_total             6533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41547c.txt
_cod_data_source_block           120910b
_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/RSC/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        3705.6(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7239057