The synthesis of densely functionalised α-acyloxy enaminals and enaminones via a novel homogeneous silver (I) catalysed rearrangement
Keskar, Kunal; Zepeda-Velazquez, Carlos; Babu, Chanti; Jenkins, Hilary A.; McNulty, James; Chemical Communications  (2019) –; doi:10.1039/C9CC05614A

data_7124007
_publ_section_title
;
 The synthesis of densely functionalised \a-acyloxy enaminals and
 enaminones via a novel homogeneous silver (I) catalysed rearrangement
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05614A
_journal_year                    2019
_chemical_formula_moiety         'C20 H16 Br N O6, 0.841(C H Cl3), 0.318(O)'
_chemical_formula_sum            'C20.84 H16.84 Br Cl2.53 N O6.31'
_chemical_formula_weight         551.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-17 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0930(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.1961(9)
_cell_length_b                   13.3772(4)
_cell_length_c                   11.8239(4)
_cell_measurement_reflns_used    5106
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.09
_cell_measurement_theta_min      3.14
_cell_volume                     4453.3(2)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 6K CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19243
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.416
_diffrn_reflns_theta_min         3.139
_exptl_absorpt_coefficient_mu    5.673
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       needle
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0726
_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^)+(0.0998P)^2^+19.2897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2010
_refine_ls_wR_factor_ref         0.2088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3417
_reflns_number_total             4026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05614a2.cif
_cod_data_source_block           KR494_0m_a
_cod_database_code               7124007
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.210
_shelx_estimated_absorpt_t_max   0.895
_shelx_res_checksum              94454