Experimental and theoretical study of intramolecular O⋯O interaction in structurally rigid β-keto carboxylic esters
Sharma, Chiranjeev; Singh, Ashawani K.; Joy, Jyothish; Jemmis, Eluvathingal D.; Awasthi, Satish K.; RSC Advances 6 (2016) 91689–; doi:10.1039/C6RA20483J

data_7236258
_publ_section_title
;
 Experimental and theoretical study of intramolecular O&#x22EF;O
 interaction in structurally rigid \b-keto carboxylic esters
;
_journal_issue                   94
_journal_name_full               'RSC Advances'
_journal_page_first              91689
_journal_paper_doi               10.1039/C6RA20483J
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C14 H15 Cl2 N1 O4'
_chemical_formula_sum            'C14 H15 Cl2 N O4'
_chemical_formula_weight         332.17
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-12-20 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.022(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5283(9)
_cell_length_b                   6.1794(4)
_cell_length_c                   17.9542(14)
_cell_measurement_reflns_used    4227
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9222
_cell_measurement_theta_min      3.2740
_cell_volume                     1582.13(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12132
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylindrical
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1573P)^2^+1.1559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.2059
_reflns_number_gt                2662
_reflns_number_total             3241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra20483j2.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C14 H15 Cl2 N1 O4'
_cod_database_code               7236258