Crystal structure of ethyl (Z)-(4-oxo-4-phenylbut-2-en-2-yl)glycinate, C14H17NO3
Safavora, A.S.; Brito, Ivan; Cisterna, Jonathan; Cárdenas, Alejandro; Huseynov, E.Z.; Khalilov, A.N.; Naghiyev, F.N.; Askerov, R.K.; Maharramov, A.M.; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1183–1185; doi:10.1515/ncrs-2019-0312

data_8105972
_publ_section_title
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 Crystal structure of ethyl (Z)-(4-oxo-4-phenylbut-2-en-2-yl)glycinate,
 C14H17NO3
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_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1183
_journal_page_last               1185
_journal_paper_doi               10.1515/ncrs-2019-0312
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C14 H17 N O3'
_chemical_formula_sum            'C14 H17 N O3'
_chemical_formula_weight         247.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.5684(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1445(7)
_cell_length_b                   8.5442(5)
_cell_length_c                   14.2503(8)
_cell_measurement_reflns_used    1899
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.49
_cell_volume                     1345.10(14)
_computing_cell_refinement       'Bruker SAINT [1]'
_computing_data_collection       'Bruker APEX3[1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [5]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [5]'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)[2]'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008) [3]'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13813
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         2.186
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7028
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.125
_refine_diff_density_min         -0.128
_refine_diff_density_rms         0.028
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0614P)^2^+0.1219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1680
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1730
_reflns_number_total             3565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0312_suppl.cif
_cod_data_source_block           a
_cod_database_code               8105972
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.08) H3(0.09) H4(0.101) H5(0.116) H6(0.099) H8(0.078)
 H10a(0.082) H10b(0.082) H12a(0.109) H12b(0.109) H13a(0.179) H13b(0.179)
 H13c(0.179) H14a(0.129) H14b(0.129) H14c(0.129)
 Fixed X: H2(0.2395) H3(0.1873) H4(0.326) H5(0.5202) H6(0.5773) H8(0.6199)
 H10a(0.5779) H10b(0.5994) H12a(0.3215) H12b(0.3088) H13a(0.3644) H13b(0.4804)
 H13c(0.4677) H14a(0.768) H14b(0.7211) H14c(0.7517)
 Fixed Y: H2(1.0025) H3(1.1538) H4(1.2045) H5(1.112) H6(0.9698) H8(0.8396)
 H10a(0.4868) H10b(0.6412) H12a(0.5038) H12b(0.3481) H13a(0.2899) H13b(0.3942)
 H13c(0.2393) H14a(0.7028) H14b(0.5516) H14c(0.7016)
 Fixed Z: H2(0.1196) H3(0.2407) H4(0.3709) H5(0.3759) H6(0.2522) H8(0.1355)
 H10a(-0.1142) H10b(-0.1693) H12a(-0.3789) H12b(-0.3218) H13a(-0.4691) H13b(-
 0.4463) H13c(-0.3894) H14a(0.0728) H14b(0.0174) H14c(-0.0381)
;
_shelx_res_checksum              98847
_shelx_hkl_checksum              47601
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
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