Synthesis of the Death-Cap Mushroom Toxin α-Amanitin
Matinkhoo, Kaveh; Pryyma, Alla; Todorovic, Mihajlo; Patrick, Brian O.; Perrin, David M.; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b12698

data_4127218
_publ_section_title
;
 Synthesis of the Death-Cap Mushroom Toxin \a-Amanitin
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12698
_journal_year                    2018
_chemical_formula_moiety         'Cl, C6 H12 N O3'
_chemical_formula_sum            'C6 H12 Cl N O3'
_chemical_formula_weight         181.62
_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   geom
_audit_creation_date             2015-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.60(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9511(16)
_cell_length_b                   6.7919(14)
_cell_length_c                   8.8449(18)
_cell_measurement_temperature    293(2)
_cell_volume                     444.11(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_number            2129
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.851
_diffrn_reflns_theta_min         2.477
_exptl_absorpt_coefficient_mu    0.393
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_F_000             192
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 972 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0006(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.507
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2129
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.507
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0157
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2115
_reflns_number_total             2129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12698_si_001.cif
_cod_data_source_block           dp041
_cod_database_code               4127218
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C007(H007), C009(H009), C00A(H00F)
2.b Secondary CH2 refined with riding coordinates:
 C008(H00D,H00E)
2.c Idealised Me refined as rotating group:
 N005(H00A,H00B,H00C), C00B(H00G,H00H,H00I)
2.d Idealised tetrahedral OH refined as rotating group:
 O004(H004)
;
_shelx_res_checksum              87764
_shelx_hkl_checksum              41184
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'