Isostructuralism in a series of methylester/methylamide derivatives of (<i>R</i>,<i>R</i>)-<i>O</i>,<i>O</i>'-dibenzoyl tartaric acid; inclusion properties and guest-dependent homeotypism of the crystals of (<i>R</i>,<i>R</i>)-<i>O</i>,<i>O</i>'-dibenzoyltartaric acid diamide
Rychlewska, Urszula; Warżajtis, Beata; Acta Crystallographica Section B 58 (2002) 265–271; doi:10.1107/S0108768101019334

data_2103263
_publ_section_title
;
 Isostructuralism in a series of methylester/methylamide derivatives of
 (<i>R</i>,<i>R</i>)-<i>O</i>,<i>O</i>'-dibenzoyl tartaric acid;
 inclusion properties and guest-dependent homeotypism of the crystals
 of (<i>R</i>,<i>R</i>)-<i>O</i>,<i>O</i>'-dibenzoyltartaric acid
 diamide
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              265
_journal_page_last               271
_journal_paper_doi               10.1107/S0108768101019334
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C20 H19 N O7'
_chemical_formula_sum            'C20 H19 N O7'
_chemical_formula_weight         385.36
_chemical_name_systematic
;
(R,R)-(-)-O,O'-Dibenzoyltartaric acid mono(N-methylamide) monomethylester
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.898(2)
_cell_length_b                   17.756(4)
_cell_length_c                   5.2640(10)
_cell_measurement_temperature    160(2)
_cell_volume                     925.1(3)
_computing_cell_refinement       'Kuma KM4CCD software'
_computing_data_collection
'Kuma KM4CCD software (Kuma Diffraction, 1999)'
_computing_data_reduction        'Kuma KM4CCD software'
_computing_molecular_graphics    'Simens Analytical X-Ray Instruments (1989)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Kuma KM4CCD \k-geometry diffractometer'
_diffrn_measurement_method       '\w scans'
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3976
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.27
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.282
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack
;
The absolute structure of the crystals was assumed from the known absolute
configuration of the reagents used in the synthesis.
;
_refine_ls_extinction_coef       0.014(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.2945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                966
_reflns_number_total             976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            na0128.cif
_cod_data_source_block           BOM2
_cod_database_code               2103263