The synthesis, crystal structure and spectroscopic analysis of (E)-3-(4-chlorophenyl)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)prop-2-en-1-one
Vinaya,; Richard, Austin S.; Murthy, Subbiah M.; Basavaraju, Yeriyur B.; Yathirajan, Hemmige S.; Parkin, Sean; Acta Crystallographica Section E Crystallographic Communications 79 (2023) 674–677; doi:10.1107/S2056989023005613

data_2022806
_publ_section_title
;
 The synthesis, crystal structure and spectroscopic analysis of
 (E)-3-(4-chlorophenyl)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)prop-2-en-1-one
;
_journal_coeditor_code           VM2285
_journal_issue                   7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              674
_journal_page_last               677
_journal_paper_doi               10.1107/S2056989023005613
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C17 H13 Cl O3'
_chemical_formula_moiety         'C17 H13 Cl O3'
_chemical_formula_sum            'C17 H13 Cl O3'
_chemical_formula_weight         300.72
_chemical_name_systematic
(<i>E</i>)-3-(4-Chlorophenyl)-1-(2,3-dihydrobenzo[<i>b</i>][1,4]dioxin-6-yl)prop-2-en-1-one
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.8655(5)
_cell_length_b                   14.3499(17)
_cell_length_c                   16.4803(19)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.47
_cell_volume                     1387.1(3)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2019</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17057
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         2.472
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.158
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1035 quotients [(I+)-(I-)]/[(I+)+(I-)]
[Parsons <i>et al.</i> (2013)
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2896
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0322P)^2^+0.4666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                2694
_reflns_number_total             2896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2285sup1.cif
_cod_data_source_block           I
_cod_database_code               2022806
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.940
_shelx_hkl_checksum              68324
_shelx_res_checksum              23305
_cod_database_fobs_code 2022806