The vinylogous Catellani reaction: a combined computational and experimental study.
Yamamoto, Y.; Murayama, T.; Jiang, J.; Yasui, T.; Shibuya, M.; Chemical science 9 (2018) 1191–1199; doi:10.1039/c7sc04265e

data_1548345
_publ_section_title
;
 The vinylogous Catellani reaction: a combined computational and
 experimental study.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1191
_journal_page_last               1199
_journal_paper_doi               10.1039/c7sc04265e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C39 H38 N2 O3 S'
_chemical_formula_weight         614.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1p8rj7
_audit_update_record
;
2017-06-21 deposited with the CCDC.
2017-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5942(7)
_cell_length_b                   8.7199(4)
_cell_length_c                   21.4742(10)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      24.9935
_cell_measurement_theta_min      2.3260
_cell_volume                     3101.5(2)
_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      123.0(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20548
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.33
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.756
_refine_ls_extinction_coef       0.0058(5)
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+2.1814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                4679
_reflns_number_total             5453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04265e2.cif
_cod_data_source_block           murayama20170223
_cod_depositor_comments          'Adding full bibliography for 1548345.cif.'
_cod_database_code               1548345
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