Synthesizing the Tetracyclic Core of Nanolobatolide
Le Chang; Hao Jiang; Junkai Fu; Bin Liu; Chuang-chuang Li; Zhen Yang; Journal of Organic Chemistry 77 (2012) 3609–3614; doi:10.1021/jo300039q

data_4027110
_publ_section_title
;
 Synthesizing the Tetracyclic Core of Nanolobatolide
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3609
_journal_page_last               3614
_journal_paper_doi               10.1021/jo300039q
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C22 H23 N O6'
_chemical_formula_sum            'C22 H23 N O6'
_chemical_formula_weight         397.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                66.72(3)
_cell_angle_beta                 82.58(4)
_cell_angle_gamma                76.52(4)
_cell_formula_units_Z            2
_cell_length_a                   6.5030(13)
_cell_length_b                   12.1809(11)
_cell_length_c                   13.9183(19)
_cell_measurement_reflns_used    1221
_cell_measurement_temperature    296
_cell_measurement_theta_max      69.10
_cell_measurement_theta_min      21.60
_cell_volume                     984.0(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
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_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13212
_diffrn_reflns_theta_full        69.28
_diffrn_reflns_theta_max         69.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       prism
_exptl_crystal_F_000             420.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.530
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3542
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3585
_reflns_number_gt                2503
_reflns_number_total             3542
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo300039q_si_001.cif
_cod_data_source_block           '__20120103ChangLe'
_cod_database_code               4027110