Crystal structure of dimethyl <i>N</i>,<i>N</i>'-[(ethyne-1,2-diyl)bis(1,4-phenylenecarbonyl)]bis(<small>L</small>-alaninate)
Eissmann, Frank; Seichter, Wilhelm; Weber, Edwin; Acta Crystallographica Section E 75 (2019) 751–754; doi:10.1107/S2056989019005826

data_2242930
_publ_section_title
;
 Crystal structure of dimethyl
 <i>N</i>,<i>N</i>'-[(ethyne-1,2-diyl)bis(1,4-phenylenecarbonyl)]bis(<small>L</small>-alaninate)
;
_journal_coeditor_code           ZP2034
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              751
_journal_page_last               754
_journal_paper_doi               10.1107/S2056989019005826
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C24 H24 N2 O6'
_chemical_formula_moiety         'C24 H24 N2 O6'
_chemical_formula_sum            'C24 H24 N2 O6'
_chemical_formula_weight         436.45
_chemical_name_systematic
<i>N</i>,<i>N</i>'-[(Ethyne-1,2-diyl)bis(1,4-phenylenecarbonyl)]bis(<i>L</i>-alaninate)
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.905(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.9409(4)
_cell_length_b                   39.015(3)
_cell_length_c                   5.8447(4)
_cell_measurement_reflns_used    2881
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.53
_cell_measurement_theta_min      3.55
_cell_volume                     1106.33(15)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle Kappa'
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10506
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.519
_diffrn_reflns_theta_min         2.088
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9882
_exptl_absorpt_correction_T_min  0.9769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       irregular
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.233
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5192
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0519P)^2^+0.3338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                3859
_reflns_number_total             5192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zp2034sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1106.34(14)
_cod_database_code               2242930
_cod_database_fobs_code          2242930
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.988
_shelx_hkl_checksum              46845
_shelx_res_checksum              41846