Synthesis and crystal structure of <i>tert</i>-butyl 1-(2-iodobenzoyl)cyclopent-3-ene-1-carboxylate
Yin, Dejing; Acta Crystallographica Section E 75 (2019) 1383–1385; doi:10.1107/S2056989019011514

data_2243074
_publ_section_title
;
 Synthesis and crystal structure of <i>tert</i>-butyl
 1-(2-iodobenzoyl)cyclopent-3-ene-1-carboxylate
;
_journal_coeditor_code           WM5513
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1383
_journal_page_last               1385
_journal_paper_doi               10.1107/S2056989019011514
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C17 H19 I O3'
_chemical_formula_moiety         'C17 H19 I O3'
_chemical_formula_sum            'C17 H19 I O3'
_chemical_formula_weight         398.22
_chemical_name_systematic
;
<i>tert</i>-Butyl 1-(2-iodobenzoyl)-cyclopent-3-ene-1-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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.7520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4977(2)
_cell_length_b                   9.3635(2)
_cell_length_c                   19.8978(4)
_cell_measurement_reflns_used    5961
_cell_measurement_temperature    299.(2)
_cell_measurement_theta_max      69.85
_cell_measurement_theta_min      4.56
_cell_volume                     1725.90(6)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX3 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b), PLATON (Spek, 2009)
and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      299.(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16056
_diffrn_reflns_theta_full        70.11
_diffrn_reflns_theta_max         70.11
_diffrn_reflns_theta_min         4.56
_exptl_absorpt_coefficient_mu    14.636
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.2624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.614
_refine_diff_density_min         -1.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0548P)^2^+2.0895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                2612
_reflns_number_total             3278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5513sup1.cif
_cod_data_source_block           I
_cod_database_code               2243074
_shelx_res_checksum              90854