Green Chemistry Oriented Multi-Component Strategy to Hybrid Heterocycle
B, Rajarathinam; Kandhasamy, kumaravel; Gnanasambandam, Vasuki; RSC Adv.  (2016) –; doi:10.1039/C6RA11543H

data_7226061
_publ_section_title
;
 Green Chemistry Oriented Multi-Component Strategy to Hybrid Heterocycle
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA11543H
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C18 H12 N4 O4'
_chemical_formula_sum            'C18 H12 N4 O4'
_chemical_formula_weight         348.32
_chemical_melting_point          273
_chemical_name_systematic
(4S)-2-amino-4-[(3R)-2-oxo-3,3a,4,5,6,7-hexahydro-2H-indol-3-yl]-6-[(oxoimino)-$l^{1}-oxidanyl]-4a,5,6,7,8,8a-hexahydro-4H-chromene-3-carbonitrile
_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           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-06-27 deposited with the CCDC.
2016-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                68.00(2)
_cell_angle_beta                 70.789(19)
_cell_angle_gamma                71.259(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7120(17)
_cell_length_b                   9.422(2)
_cell_length_c                   12.348(3)
_cell_measurement_reflns_used    2681
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      3.7950
_cell_volume                     864.4(4)
_computing_cell_refinement
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        CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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_computing_data_collection
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       CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16
;
_computing_data_reduction
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      CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
        J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0013964000
_diffrn_orient_matrix_UB_12      -0.0029925000
_diffrn_orient_matrix_UB_13      -0.0587746000
_diffrn_orient_matrix_UB_21      -0.0129059000
_diffrn_orient_matrix_UB_22      0.0824142000
_diffrn_orient_matrix_UB_23      -0.0149210000
_diffrn_orient_matrix_UB_31      0.0887562000
_diffrn_orient_matrix_UB_32      -0.0016712000
_diffrn_orient_matrix_UB_33      -0.0209034000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6710
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         4.33
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.972
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_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.99
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0715
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.2290
_reflns_number_gt                1492
_reflns_number_total             3028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra11543h2.cif
_cod_data_source_block           FINAL
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' 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_cell_volume        864.5(3)
_cod_original_sg_symbol_Hall     'P 1'
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7226061