One-pot synthesis of various 2-amino-4H-chromene derivatives using a highly active supported ionic liquid catalyst
Sharma, Pankaj; Gupta, Monika; Kant, Rajni; Gupta, Vivek K.; RSC Adv. 6 (2016) 32052–; doi:10.1039/C6RA06523F

data_7224752
_publ_section_title
;
 One-pot synthesis of various 2-amino-4H-chromene derivatives using a
 highly active supported ionic liquid catalyst
;
_journal_issue                   38
_journal_name_full               'RSC Adv.'
_journal_page_first              32052
_journal_paper_doi               10.1039/C6RA06523F
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C18 H17 N3 O4'
_chemical_formula_sum            'C18 H17 N3 O4'
_chemical_formula_weight         339.35
_chemical_name_systematic
2-amino-6,6,8,8-tetrahydro-7,7-dimethyl-4-(3-nitrophenyl)-5-oxo-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           SHELXL-97
_audit_update_record
;
2015-05-11 deposited with the CCDC.
2016-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                93.670(3)
_cell_angle_beta                 93.670(3)
_cell_angle_gamma                103.706(4)
_cell_formula_units_Z            8
_cell_length_a                   12.0002(5)
_cell_length_b                   12.0002(5)
_cell_length_c                   24.7801(14)
_cell_measurement_reflns_used    3589
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7860
_cell_measurement_theta_min      3.8620
_cell_volume                     3448.2(3)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction,2010)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 2012)'
_computing_publication_material  'PLATON (Spek,2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1049
_diffrn_measured_fraction_theta_full 0.780
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w 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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13673
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0021(11)
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         10570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.2065
_refine_ls_R_factor_gt           0.1682
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+41.3017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4376
_refine_ls_wR_factor_ref         0.4619
_reflns_number_gt                6910
_reflns_number_total             10570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra06523f2.cif
_cod_data_source_block           pan1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

2018-03-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C144 H136 N24 O32'
_cod_original_formula_weight         2714.77
_cod_original_formula_moiety         'C144 H136 N24 O32'
_cod_original_formula_units_Z            1
_cod_database_code               7224752