Gold-catalyzed chemo- and diastereoselective C(sp(2))-H functionalization of enaminones for the synthesis of pyrrolo[3,4-c]-quinolin-1-one derivatives.
Zhao, Yulei; Duan, Qizhao; Zhou, Yuanyuan; Yao, Qiyi; Li, Yanzhong; Organic & biomolecular chemistry 14 (2016) 2177–2181; doi:10.1039/c5ob02556g

data_7154904
_publ_section_title
;
 Gold-catalyzed chemo- and diastereoselective C(sp(2))-H functionalization
 of enaminones for the synthesis of pyrrolo[3,4-c]-quinolin-1-one
 derivatives.
;
_journal_issue                   7
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2177
_journal_page_last               2181
_journal_paper_doi               10.1039/c5ob02556g
_journal_volume                  14
_journal_year                    2016
_chemical_formula_sum            'C25.5 H21 Cl2 N2 O3.5'
_chemical_formula_weight         482.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-11-16 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                83.296(5)
_cell_angle_beta                 80.970(5)
_cell_angle_gamma                87.489(5)
_cell_formula_units_Z            4
_cell_length_a                   11.980(3)
_cell_length_b                   13.777(3)
_cell_length_c                   14.492(3)
_cell_measurement_reflns_used    1413
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.931
_cell_measurement_theta_min      4.355
_cell_volume                     2345.3(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13088
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         1.947
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.180
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_refine_ls_number_reflns         8312
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_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1326
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_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^)+(0.1042P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.2211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4872
_reflns_number_total             8312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob02556g2.cif
_cod_data_source_block           cd15125
_cod_depositor_comments
;
Adding full bibliography for 7154904--7154905.cif.

2017-03-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2345.2(9)
_cod_original_formula_sum        'C51 H42 Cl4 N4 O7'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     964.68
_cod_database_code               7154904
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-4
_shelx_res_checksum              71209