Ir-Catalyzed Asymmetric Total Synthesis of (-)-Communesin F.
Liang, Xiao; Zhang, Tian-Yuan; Zeng, Xue-Yi; Zheng, Yu; Wei, Kun; Yang, Yu-Rong; Journal of the American Chemical Society 139 (2017) 3364–3367; doi:10.1021/jacs.7b00854

data_4125476
_publ_section_title
;
 Ir-Catalyzed Asymmetric Total Synthesis of (-)-Communesin F.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3364
_journal_page_last               3367
_journal_paper_doi               10.1021/jacs.7b00854
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H30 Br N3 O4, C H4 O, H2 O'
_chemical_formula_sum            'C27 H36 Br N3 O6'
_chemical_formula_weight         578.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                90
_cell_angle_beta                 101.971(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.039(6)
_cell_length_b                   8.1020(14)
_cell_length_c                   10.3858(18)
_cell_measurement_reflns_used    4040
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.15
_cell_volume                     2637.3(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13194
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.219
_diffrn_reflns_theta_min         2.004
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.5858
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 1998 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6301
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                5296
_reflns_number_total             6301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00854_si_003.cif
_cod_data_source_block           mo_af10080_0m
_cod_depositor_comments
'Adding full bibliography for 4125476--4125477.cif.'
_cod_original_cell_volume        2637.4(8)
_cod_database_code               4125476
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.297
_shelx_estimated_absorpt_t_max   0.856
_shelx_res_checksum              28176
_shelx_hkl_checksum              1552