A concise total synthesis of salinosporamide A.
Mulholland, Nicholas P.; Pattenden, Gerald; Walters, Iain A. S.; Organic & biomolecular chemistry 4 (2006) 2845–2846; doi:10.1039/b607109k

data_7151269
_publ_section_title
;
 A concise total synthesis of salinosporamide A.
;
_journal_issue                   15
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2845
_journal_page_last               2846
_journal_paper_doi               10.1039/b607109k
_journal_volume                  4
_journal_year                    2006
_chemical_formula_moiety         'C18 H23 N O7'
_chemical_formula_sum            'C18 H23 N O7'
_chemical_formula_weight         365.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens
'NH and OH from delta-F; others placed geometrically'
_atom_sites_solution_primary     direct
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.090(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.292(6)
_cell_length_b                   11.057(4)
_cell_length_c                   11.287(5)
_cell_measurement_reflns_used    6831
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     1782.5(13)
_computing_cell_refinement       'SAINT version 6.36a (Bruker, 2001)'
_computing_data_collection       'SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'enCIFer (Allen et al., 2004); PLATON'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.124
_diffrn_reflns_av_sigmaI/netI    0.027
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15038
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trigonal prism'
_exptl_crystal_F_000             776
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.98
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.36
_refine_diff_density_rms         0.07
_refine_ls_extinction_coef       0.0051(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment
'N-H restrained to 0.86(1) Angstroms; OH rigid rotor; others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4068
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.064P)^2^+0.846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.111
_refine_ls_wR_factor_ref         0.123
_reflns_number_gt                3308
_reflns_number_total             4068
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b607109k.txt
_cod_data_source_block           pyrcoh
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7151269