Synthesis of Swinhoeisterol A, Dankasterone A and B, and Periconiastone A by Radical Framework Reconstruction.
Duecker, Fenja L.; Heinze, Robert C.; Heretsch, Philipp; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b12899

data_4133872
_publ_section_title
;
 Synthesis of Swinhoeisterol A, Dankasterone A and B, and Periconiastone A
 by Radical Framework Reconstruction.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12899
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H41 I O2'
_chemical_formula_sum            'C28 H41 I O2'
_chemical_formula_weight         536.54
_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_Int_Tables_number      4
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.747(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8801(14)
_cell_length_b                   11.6963(17)
_cell_length_c                   11.5219(17)
_cell_volume                     1287.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.96
_diffrn_measured_fraction_theta_full 0.9924
_diffrn_measured_fraction_theta_max 0.9919
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33879
_diffrn_reflns_theta_full        27.5808
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    1.265
_exptl_crystal_density_diffrn    1.3838
_exptl_crystal_F_000             555.3797
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.7104
_refine_diff_density_min         -0.4519
_refine_diff_density_rms         0.0754
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.026(15)
_refine_ls_d_res_high            0.7675
_refine_ls_d_res_low             8.3840
_refine_ls_goodness_of_fit_ref   1.0496
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    63
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5901
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0496
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.0200
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+0.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.988
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                5454
_reflns_number_total             5901
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja9b12899_si_002.cif
_cod_data_source_block           FD402_1_c
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               4133872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C7(H7), C9(H9), C17(H17), C20(H20), C24(H24), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C4(H4a,H4b), C11(H11a,H11b), C12(H12a,H12b),
 C15(H15a,H15b), C16(H16a,H16b)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23)
2.d Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C26(H26a,H26b,
 H26c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c)
;
_olex2_submission_special_instructions 'No special instructions were received'