Total Synthesis and Structural Reassignment of Aranorosinol A, Aranorosinol B, and EI-2128-1.
Yu, Haiyong; Tian, Yingyuan; Zong, Yan; Zhang, Jianyu; Xu, Tao; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c00028

data_4038043
_publ_section_title
;
 Total Synthesis and Structural Reassignment of Aranorosinol A,
 Aranorosinol B, and EI-2128-1.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00028
_journal_year                    2020
_chemical_formula_sum            'C25 H33 Br N O7 Si'
_chemical_formula_weight         567.52
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.729(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.1583(16)
_cell_length_b                   25.873(3)
_cell_length_c                   20.170(2)
_cell_measurement_reflns_used    4948
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.1430
_cell_measurement_theta_min      4.1300
_cell_volume                     5605.0(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43770
_diffrn_reflns_theta_full        67.25
_diffrn_reflns_theta_max         67.25
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    2.761
_exptl_absorpt_correction_T_max  0.7511
_exptl_absorpt_correction_T_min  0.7329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blank
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10041
_refine_ls_number_restraints     1980
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.2187
_refine_ls_R_factor_gt           0.1066
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3096
_refine_ls_wR_factor_ref         0.4058
_reflns_number_gt                3604
_reflns_number_total             10041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0c00028_si_002.cif
_cod_data_source_block           exp_8462
_cod_depositor_comments
;

2020-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C50 H66 Br2 N2 O14 Si2'
_cod_original_formula_weight         1135.05
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5604.8(13)
_cod_database_code               4038043