Diversity Oriented Microwave-Assisted Synthesis of (-)-Steganacin Aza-Analogues
Nuria Mont; Vaibhav Pravinchandra Mehta; Prasad Appukkuttan; Tetyana Beryozkina; Suzzane Toppet; Kristof Van Hecke; Luc Van Meervelt; Arnout Voet; Marc DeMaeyer; Erik Van der Eycken; Journal of Organic Chemistry 73 (2008) 7509–7516; doi:10.1021/jo801290j

data_4023708
_publ_contact_author_address
;Laboratory for Organic & Microwave-Assisted Chemistry (LOMAC),
Katholieke Universiteit Leuven,
Department of Chemistry,
Celestijnenlaan 200F,
B-3001 Heverlee (Leuven),
Belgium
;
_publ_contact_author_email       erik.vandereycken@chem.kuleuven.be
_publ_contact_author_fax         +32(0)16327990
_publ_contact_author_phone       +32(0)16327406
_publ_section_title
;
 Diversity Oriented Microwave-Assisted Synthesis of
 (-)-Steganacin Aza-Analogues
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7509
_journal_page_last               7516
_journal_paper_doi               10.1021/jo801290j
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C32 H27 F N4 O3, C H Cl3'
_chemical_formula_sum            'C33 H28 Cl3 F N4 O3'
_chemical_formula_weight         653.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.187(4)
_cell_angle_beta                 71.842(5)
_cell_angle_gamma                73.631(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4953(8)
_cell_length_b                   11.3283(8)
_cell_length_c                   13.9630(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1512.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  Platon
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'crossed Goebel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13603
_diffrn_reflns_theta_full        70.88
_diffrn_reflns_theta_max         70.88
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    3.149
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+0.1678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                4710
_reflns_number_total             5494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo801290j_si_002.cif
_cod_data_source_block           EV003
_cod_database_code               4023708