The Total Synthesis of Tubulysin D
Hillary M. Peltier; Jeffrey P. McMahon; Andrew W. Patterson; Jonathan A. Ellman; Journal of the American Chemical Society 128 (2006) 16018–16019; doi:10.1021/ja067177z

data_4111242
_publ_section_title
;
 The Total Synthesis of Tubulysin D
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16018
_journal_page_last               16019
_journal_paper_doi               10.1021/ja067177z
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C25 H24 Br2 N2 O5 S '
_chemical_formula_sum            'C25 H24 Br2 N2 O5 S'
_chemical_formula_weight         624.34
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             'Fri Apr 14 16:12:17 2006'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 106.824(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.472(3)
_cell_length_b                   9.565(3)
_cell_length_c                   12.691(3)
_cell_measurement_reflns_used    1396
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      18.7
_cell_measurement_theta_min      2.8
_cell_volume                     1333.0(6)
_computing_cell_refinement       'Bruker-AXS SAINT v6.40'
_computing_data_collection       'Bruker-AXS SMART v5.631'
_computing_data_reduction        'Bruker-AXS SAINT v6.40'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR97
_diffrn_measured_fraction_theta_full 1.6696
_diffrn_measured_fraction_theta_max 1.6696
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5965
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.165
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       rod
_exptl_crystal_F_000             628.00
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
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_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0505
_refine_ls_wR_factor_ref         0.0446
_reflns_number_gt                2435
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_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ja067177zsi20061006_021018.cif
_cod_data_source_block           Hmp4183_for_Hillary_Peltier
_cod_original_cell_volume        1332.9(6)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C25 H24 Br2 N2 O5 S '
_cod_database_code               4111242