Total Synthesis of Dactylicapnosines A and B.
Zhao, Yinjiao; Li, Yuda; Wang, Bei; Zhao, Jingfeng; Li, Liang; Luo, Xiao-Dong; Zhang, Hongbin; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01900

data_4038911
_publ_section_title
;
 Total Synthesis of Dactylicapnosines A and B.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01900
_journal_year                    2020
_chemical_formula_moiety         'C26 H31 N O10, C H2 Cl2'
_chemical_formula_sum            'C27 H33 Cl2 N O10'
_chemical_formula_weight         602.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                104.931(3)
_cell_angle_beta                 105.413(2)
_cell_angle_gamma                92.310(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0864(13)
_cell_length_b                   12.184(2)
_cell_length_c                   15.082(3)
_cell_measurement_reflns_used    7662
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.78
_cell_measurement_theta_min      2.56
_cell_volume                     1374.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18442
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.034
_diffrn_reflns_theta_min         1.458
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.630
_exptl_crystal_size_mid          0.510
_exptl_crystal_size_min          0.430
_exptl_transmission_factor_max   0.2134
_exptl_transmission_factor_min   0.1575
_refine_diff_density_max         2.311
_refine_diff_density_min         -2.675
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         8005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.1029
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1996P)^2^+3.3628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3081
_refine_ls_wR_factor_ref         0.3293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6307
_reflns_number_total             8005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01900_si_002.cif
_cod_data_source_block           mo_zhb_zyj4_0m
_cod_database_code               4038911
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.883
_shelx_res_checksum              85827
_shelx_hkl_checksum              30717