Total synthesis of (±)-distomadines a and B.
Jolibois, Alexandre E. R.; Lewis, William; Moody, Christopher J.; Organic letters 16 (2014) 1064–1067; doi:10.1021/ol403598k

data_1513453
_publ_section_title
;
 Total synthesis of (+-)-distomadines a and B.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              1064
_journal_page_last               1067
_journal_paper_doi               10.1021/ol403598k
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C26 H25 N O7'
_chemical_formula_sum            'C26 H25 N O7'
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_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
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_atom_sites_solution_secondary   difmap
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Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
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_cell_formula_units_Z            2
_cell_length_a                   7.8031(4)
_cell_length_b                   9.1491(5)
_cell_length_c                   16.0757(7)
_cell_measurement_reflns_used    20421
_cell_measurement_temperature    120(2)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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_diffrn_ambient_temperature      120(2)
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_diffrn_orient_matrix_UB_23      -0.0671734000
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_diffrn_orient_matrix_UB_32      0.0917286000
_diffrn_orient_matrix_UB_33      0.0651433000
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_diffrn_reflns_number            38258
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.179
_diffrn_reflns_theta_min         2.825
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
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_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  1.310
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.2392
_exptl_crystal_size_min          0.1871
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_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.3327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                4208
_reflns_number_total             4541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol403598k_si_002.cif
_cod_data_source_block           ajcjmd
_cod_database_code               1513453
_nottingham_internal_coll_name   AJCJMD
_nottingham_internal_coll_number 12943
_nottingham_internal_coll_client AJ/CJM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '2, 3'
_nottingham_internal_coll_frame_width 2
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   24/10/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user WL
_nottingham_internal_process_date 25/10/2013
_nottingham_internal_solution_user wl
_nottingham_internal_solution_date 25/10/2012
_nottingham_internal_refinement_user wl
_nottingham_internal_refinement_date 5/12/2013
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_nottingham_internal_validation_date 5/12/2013
_nottingham_internal_archive_date 5/12/2013
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C26 H25 N O7'
_chemical_oxdiff_usercomment
'AJCJMD #12943 IN FOMBLIN FILM ON MICROMOUNT FOR AJ/CJM'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
;