Synthesis and crystal structure of allyl 7-(diethylamino)-2-oxo-2<i>H</i>-chromene-3-carboxylate
Nowatschin, Vanessa; Näther, Christian; Lüning, Ulrich; Acta Crystallographica Section E 77 (2021) 331–334; doi:10.1107/S2056989021002218

data_2243765
_publ_section_title
;
 Synthesis and crystal structure of allyl
 7-(diethylamino)-2-oxo-2<i>H</i>-chromene-3-carboxylate
;
_journal_coeditor_code           WM5600
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              331
_journal_page_last               334
_journal_paper_doi               10.1107/S2056989021002218
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C17 H19 N O4'
_chemical_formula_moiety         'C17 H19 N O4'
_chemical_formula_sum            'C17 H19 N O4'
_chemical_formula_weight         301.33
_chemical_name_common
;
Allyl 7-(diethylamino)-2-oxo-2<i>H</i>-chromene-3-carboxylate
;
_chemical_name_systematic
;
Allyl 7-(diethylamino)-2-oxo-2<i>H</i>-chromene-3-carboxylate
;
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5220(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.72487(9)
_cell_length_b                   13.05333(9)
_cell_length_c                   8.55970(6)
_cell_measurement_reflns_used    18730
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.4630
_cell_measurement_theta_min      3.2190
_cell_volume                     1526.399(18)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009) and DIAMOND (Brandenburg,
2014)
;
_computing_publication_material
;
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26198
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.459
_diffrn_reflns_theta_min         3.235
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.176
_refine_ls_extinction_coef       0.00051(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.4857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                2975
_reflns_number_total             3125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5600sup1.cif
_cod_data_source_block           I
_cod_database_code               2243765
_cod_database_fobs_code          2243765
_shelx_hkl_checksum              71180
_shelx_res_checksum              84867