Crystal structure of natural product argyrin-D determined by 3D electron diffraction
Gorelik, Tatiana E.; Tehrani, Kamal; Gruene, Tim; Monecke, Thomas; Niessing, Dierk; Kaiser, Ute; Blankenfeldt, Wulf; Müller, Rolf; CrystEngComm  (2022) –; doi:10.1039/D2CE00707J

data_7245240
_publ_section_title
;
 Crystal structure of natural product argyrin-D determined by 3D electron
 diffraction
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00707J
_journal_year                    2022
_chemical_formula_sum            'C168 H184 N40 O32 S4'
_chemical_formula_weight         3403.64
_chemical_name_systematic        Argyrin-D
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-11 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.737
_cell_length_b                   22.737
_cell_length_c                   9.143
_cell_measurement_reflns_used    3478
_cell_measurement_temperature    77
_cell_measurement_theta_max      0.736
_cell_measurement_theta_min      0.063
_cell_volume                     4726.667
_computing_cell_refinement       'XDS, Kabsch 2010. Acta Cryst. D66, 125-132'
_computing_data_collection
'PETS2, Palatinus et al., 2019. Acta Cryst. B75, 512\^a\/E?522'
_computing_data_reduction        'XDS, Kabsch 2010. Acta Cryst. D66, 125-132'
_computing_molecular_graphics
'Mercury 4.0, Macrae, et al., 2020. J. Appl. Cryst., 53, 226-235'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXD, Sheldrick 2008. Acta Cryst. A64, 112\^a\/E?122'
_diffrn_ambient_temperature      77
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device_type  'TALOS TEM'
_diffrn_measurement_method       'continuous rotation electron difraction'
_diffrn_radiation_type           electrons
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.1639
_diffrn_reflns_av_unetI/netI     0.2243
_diffrn_reflns_Laue_measured_fraction_full 0.815
_diffrn_reflns_Laue_measured_fraction_max 0.815
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7966
_diffrn_reflns_point_group_measured_fraction_full 0.769
_diffrn_reflns_point_group_measured_fraction_max 0.769
_diffrn_reflns_theta_full        0.736
_diffrn_reflns_theta_max         0.736
_diffrn_reflns_theta_min         0.063
_diffrn_source                   'Transmission Electron Microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       needle
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.0005
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Kinematical refinement of electron diffraciton data - no absolute configuration refinement,
 isotropic temperature factors
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4077
_refine_ls_number_restraints     566
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.2232
_refine_ls_R_factor_gt           0.1780
_refine_ls_shift/su_max          2.451
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4023
_refine_ls_wR_factor_ref         0.4327
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.715
_reflns_Friedel_fraction_max     0.714
_reflns_number_gt                2508
_reflns_number_total             4077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00707j2.cif
_cod_data_source_block           ARG
_cod_original_cell_volume        4726.7
_cod_database_code               7245240
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              18629
_shelx_hkl_checksum              35206