A Facile and Green Approach for the Synthesis of Spiro[naphthalene-2,5'-pyrimidine]-4-carbonitrile via One-Pot Three-Component Condensation Reaction using DBU as Catalyst
M, Rajeswari; Saluja, Pooja; Khurana, Jitender; RSC Adv.  (2015) –; doi:10.1039/C5RA22817D

data_7223485
_publ_section_title
;
 A Facile and Green Approach for the Synthesis of
 Spiro[naphthalene-2,5'-pyrimidine]-4-carbonitrile via One-Pot
 Three-Component Condensation Reaction using DBU as Catalyst
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA22817D
_journal_year                    2015
_chemical_compound_source        'Layering Method at low temperature'
_chemical_formula_moiety         'C22 H21 Cl N4 O3'
_chemical_formula_sum            'C22 H21 Cl N4 O3'
_chemical_formula_weight         424.88
_chemical_name_systematic
3-amino-1-(4-chlorophenyl)-1',3'-dimethyl-2',4',6'-trioxo-2',3',4',6,6',7,8,8a-octahydro-1H,1'H-spiro[naphthalene-2,5'-pyrimidine]-4-carbonitrile
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1jpcrb
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-08-26 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.416(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.6632(11)
_cell_length_b                   10.9979(3)
_cell_length_c                   17.6446(8)
_cell_measurement_temperature    293(2)
_cell_volume                     4121.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_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  0.0936
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24129
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.217
_exptl_crystal_colour            WHITE
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1776
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.7708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.2198
_reflns_number_gt                1959
_reflns_number_total             3623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra22817d2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7223485