Rationalizing the Lacking of Inversion Symmetry in a Noncentrosymmetric Polar Racemate: An Experimental and Theoretical Study
Lo Presti, Leonardo; Sist, Mattia; Loconte, Laura; Pinto, Andrea; Tamborini, Lucia; Gatti, Carlo; Crystal Growth & Design 14 (2014) 5822–; doi:10.1021/cg501074x

data_4512179
_publ_section_title
;
 Rationalizing the Lacking of Inversion Symmetry in a Noncentrosymmetric
 Polar Racemate: An Experimental and Theoretical Study
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5822
_journal_paper_doi               10.1021/cg501074x
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C16 H21 N3 O5'
_chemical_formula_sum            'C16 H21 N3 O5'
_chemical_formula_weight         335.36
_chemical_name_systematic
;
3-pyrazolidineacetic acid, 2-ethyl-5-oxo-\a-
[[(phenylmethoxy)carbonyl]amino]- methyl ester, 
(\aR,3S)-rel 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4188(11)
_cell_length_b                   9.2474(7)
_cell_length_c                   25.0399(18)
_cell_measurement_reflns_used    2994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.41
_cell_measurement_theta_min      2.74
_cell_volume                     3338.7(4)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.23A (Bruker, 2005)'
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker AXS APEX CCD area-detector'
_diffrn_measurement_method       /w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            292815
_diffrn_reflns_theta_full        34.95
_diffrn_reflns_theta_max         45.30
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.1
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9827
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_preparation       '1:1 ethyl acetate-hexane'
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1281
_refine_ls_number_reflns         11918
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.034
_refine_ls_R_factor_gt           0.02
_refine_ls_R_Fsqd_factor         0.022
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w2 = 1/[s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.043
_reflns_number_gt                11918
_reflns_number_total             14098
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            cg501074x_si_002.cif
_cod_data_source_block           CE30LT
_cod_depositor_comments          'Adding full bibliography for 4512179.cif.'
_cod_database_code               4512179
_atom_site_anharm_details
;
The atomic anharmonic pdf is approximated by a Gram-Charlier expansion
about the harmonic pdf, according to the expression :

      P(u) = (1 + Cijk*Hijk/3! + Dijkl*Hijkl/4!)*P(0)

The coefficients Cijk and Dijkl are refined in the least squares procedure.
The reported coefficients Cijk are multiplied by 1000 and Dijkl by 10000.
;