Solid-state conformations of linear depsipeptide amides with an alternating sequence of α,α-disubstituted α-amino acid and α-hydroxy acid
Linden, Anthony; Magirius, J. E. Florian; Heimgartner, Heinz; Acta Crystallographica Section C Structural Chemistry 76 (2019) 1–; doi:10.1107/S2053229619016073

data_2021944
_publ_section_title
;
 Solid-state conformations of linear depsipeptide amides with an
 alternating sequence of \a,\a-disubstituted \a-amino acid and \a-hydroxy
 acid
;
_journal_coeditor_code           KY3193
_journal_issue                   1
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_page_first              1
_journal_paper_doi               10.1107/S2053229619016073
_journal_volume                  76
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_iupac          'C47 H58 N4 O9, C2 H3 N'
_chemical_formula_moiety         'C47 H58 N4 O9, C2 H3 N'
_chemical_formula_sum            'C49 H61 N5 O9'
_chemical_formula_weight         864.02
_chemical_name_systematic
(<i>S</i>)-Pms-Acp-(<i>S</i>)-Pms-Acp-(<i>S</i>)-Pms-Acp-NMe~2~
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.75(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.645(3)
_cell_length_b                   19.161(9)
_cell_length_c                   11.503(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10.0
_cell_volume                     2341.2(14)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1991)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1991)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation, 1989)
;
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1990)
;
_diffrn_ambient_temperature      173.0(10)
_diffrn_detector                 'scintillation counter'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-5R'
_diffrn_measurement_method       '\w--2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku RU200 rotating anode generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0864
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_min         2.526
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.357
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_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         5527
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0754
_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^)+(0.0906P)^2^+3.1019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.2175
_reflns_number_gt                3617
_reflns_number_total             5527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3193sup1.cif
_cod_data_source_block           3b
_cod_original_cell_volume        2341.5(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2021944
_cod_database_fobs_code          2021944
_shelx_hkl_checksum              86633
_shelx_res_checksum              85474