Systematic comparison of racemic and enantiopure multicomponent crystals of phenylsuccinic acid—the role of chirality
Odounga Odounga, Jean-Eudes; Báthori, Nikoletta B.; CrystEngComm  (2020) –; doi:10.1039/D0CE00072H

data_7240060
_publ_section_title
;
 Systematic comparison of racemic and enantiopure multicomponent crystals
 of phenylsuccinic acid---the role of chirality
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00072H
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_sum            'C44 H48 N2 O12'
_chemical_formula_weight         796.84
_chemical_melting_point          370.27
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2020-01-09 deposited with the CCDC.	2020-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                84.66(3)
_cell_angle_beta                 86.58(3)
_cell_angle_gamma                76.63(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3469(17)
_cell_length_b                   12.268(3)
_cell_length_c                   20.595(4)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.51
_cell_volume                     2041.3(8)
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  BRUKER
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46913
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.361
_diffrn_reflns_theta_min         1.712
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       chunk
_exptl_crystal_F_000             844
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 3,5-lutidine'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 5564 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1062
_refine_ls_number_reflns         19773
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1122P)^2^+1.3745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1977
_refine_ls_wR_factor_ref         0.2177
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                14901
_reflns_number_total             19773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00072h2.cif
_cod_data_source_block           spsa-35lut
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C88 H96 N4 O24'
_cod_original_formula_weight         1593.68
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2041.2(8)
_cod_database_code               7240060
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              524