A lactone-fused cyclohexadiene as a versatile platform for diversified synthesis of 5,6,5-tricyclic scaffolds.
Shibuya, M.; Sudoh, T.; Kawamura, T.; Yamamoto, Y.; Organic & biomolecular chemistry 13 (2015) 5862–5866; doi:10.1039/c5ob00729a

data_7154474
_publ_section_title
;
 A lactone-fused cyclohexadiene as a versatile platform for diversified
 synthesis of 5,6,5-tricyclic scaffolds.
;
_journal_issue                   21
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5862
_journal_page_last               5866
_journal_paper_doi               10.1039/c5ob00729a
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C16 H21 N O6'
_chemical_formula_weight         323.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2015-01-15 deposited with the CCDC.
2015-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.2010(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6489(7)
_cell_length_b                   9.9633(5)
_cell_length_c                   20.3053(9)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    93.0(2)
_cell_measurement_theta_max      25.0426
_cell_measurement_theta_min      2.3036
_cell_volume                     3180.8(3)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v3.0.29'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruke AXS)'
_computing_publication_material  'Generate Report (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93.0(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21783
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_density_diffrn    0.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+(0.0392P)^2^+1.5229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                4730
_reflns_number_total             5561
_reflns_threshold_expression     'I > 2s(I)'
_cod_data_source_file            c5ob00729a2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
Adding full bibliography for 7154473--7154475.cif.

2017-03-03
Z value changed to be consisted with the indicated formula (and the molecular
structure of the compound)                 miguel
;
_cod_original_formula_units_Z    4
_cod_database_code               7154474
_shelx_res_checksum              34391