Microwave-Assisted <i>N</i>-Allylation/Homoallylation-RCM Approach: Access to Pyrrole-, Pyridine-, or Azepine-Appended (Het)aryl Aminoamides.
Novanna, Motakatla; Kannadasan, Sathananthan; Shanmugam, Ponnusamy; ACS omega 5 (2020) 8515–8522; doi:10.1021/acsomega.9b04038

data_4517550
_publ_section_title
;
 Microwave-Assisted <i>N</i>-Allylation/Homoallylation-RCM Approach:
 Access to Pyrrole-, Pyridine-, or Azepine-Appended (Het)aryl Aminoamides.
;
_journal_issue                   15
_journal_name_full               'ACS omega'
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_journal_page_last               8522
_journal_paper_doi               10.1021/acsomega.9b04038
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C11 H14 N2 O S'
_chemical_formula_sum            'C11 H14 N2 O S'
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_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_alpha                90
_cell_angle_beta                 114.048(2)
_cell_angle_gamma                90
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_cell_length_b                   11.9949(3)
_cell_length_c                   15.0518(5)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      3.01
_cell_volume                     2440.29(12)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3(Bruker, 2016)'
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_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
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_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker axs kappa apex3 CMOS Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.210
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_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.193
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_refine_ls_extinction_coef       0.0059(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4293
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0852P)^2^+0.7512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2462
_reflns_number_total             4293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b04038_si_002.cif
_cod_data_source_block           PSMN141
_cod_depositor_comments
'Adding full bibliography for 4517549--4517550.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4517550
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              80014
_shelx_hkl_checksum              98662