Second-Generation Palladium Catalyst System for Transannular C-H Functionalization of Azabicycloalkanes.
Cabrera, Pablo J.; Lee, Melissa; Sanford, Melanie S.; Journal of the American Chemical Society 140 (2018) 5599–5606; doi:10.1021/jacs.8b02142

data_4132175
_publ_section_title
;
 Second-Generation Palladium Catalyst System for Transannular C-H
 Functionalization of Azabicycloalkanes.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5599
_journal_page_last               5606
_journal_paper_doi               10.1021/jacs.8b02142
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C31 H33 F7 N2 O4'
_chemical_formula_sum            'C31 H33 F7 N2 O4'
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_space_group_name_Hall           '-P 1'
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_atom_sites_solution_hydrogens   mixed
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_cell_length_c                   15.1378(3)
_cell_measurement_reflns_used    13514
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_cell_measurement_theta_min      2.9640
_cell_volume                     1440.95(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
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_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22127
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.969
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_diffrn_source                   'micro-focus rotating anode'
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_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
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_refine_diff_density_min         -0.249
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_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0378
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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^)+(0.0570P)^2^+0.5675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4994
_reflns_number_total             5231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02142_si_001.cif
_cod_data_source_block           pc733p2
_cod_database_code               4132175
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              47306
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