One-Pot Protocol to Functionalized Benzopyrrolizidine Catalyzed Successively by Rh2(OAc)4 and Cu(OTf)2: A Transition Metal-Lewis Acid Catalysis Relay.
Xu, Hua-Dong; Jia, Zhi-Hong; Xu, Ke; Zhou, Hao; Shen, Mei-Hua; Organic letters 17 (2015) 66–69; doi:10.1021/ol503247t

data_1518421
_publ_section_title
;
 One-Pot Protocol to Functionalized Benzopyrrolizidine Catalyzed
 Successively by Rh2(OAc)4 and Cu(OTf)2: A Transition Metal-Lewis Acid
 Catalysis Relay.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              66
_journal_page_last               69
_journal_paper_doi               10.1021/ol503247t
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C23 H28 N2 O4 S'
_chemical_formula_weight         428.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 92.128(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.543(2)
_cell_length_b                   9.344(2)
_cell_length_c                   22.465(5)
_cell_measurement_reflns_used    6101
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.17
_cell_volume                     2211.6(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.9519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethyl acetate'
_exptl_crystal_size_max          0.28
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_refine_diff_density_max         0.667
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_refine_ls_number_reflns         3843
_refine_ls_number_restraints     0
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2855
_refine_ls_wR_factor_ref         0.2880
_reflns_number_gt                3366
_reflns_number_total             3843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol503247t_si_003.cif
_cod_data_source_block           20140808lz_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 1518421--1518422.cif.
;
_cod_original_cell_volume        2211.4(8)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               1518421