Brønsted Acid Cocatalysis in Copper(I)-Photocatalyzed α-Amino C‒H Bond Functionalization
Nicholls, Thomas P.; Constable, Grace E.; Robertson, Johnathon C.; Gardiner, Michael G.; Bissember, Alex C.; ACS Catalysis 6 (2016) 451–; doi:10.1021/acscatal.5b02014

data_4513741
_publ_section_title
;
 Br\/onsted Acid Cocatalysis in Copper(I)-Photocatalyzed \a-Amino C--H
 Bond Functionalization
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              451
_journal_paper_doi               10.1021/acscatal.5b02014
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety
'C25 H20 N2 O2', '0.386(C1 H2 Cl2)', '0.182(C1 H2 Cl2)'
_chemical_formula_sum            'C25.57 H21.14 Cl1.13 N2 O2'
_chemical_formula_weight         428.65
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 104.510(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_b                   7.2788(2)
_cell_length_c                   12.3394(3)
_cell_measurement_reflns_used    7703
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.7827
_cell_measurement_theta_min      3.7001
_cell_volume                     1066.25(5)
_computing_cell_refinement
;
'SAINT V8.34A (Bruker AXS Inc., 2013)'
;
_computing_data_collection       'Bruker Instrument Service v4.2.4'
_computing_data_reduction
;
'SAINT V8.34A (Bruker AXS Inc., 2013)'
;
_computing_molecular_graphics
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)' 
;
_computing_publication_material  'X-SEED (Barbour, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker QUEST'
_diffrn_measurement_method       omega-phi
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_laue_measured_fraction_full 0.975
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15091
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.826
_diffrn_reflns_theta_min         3.700
_diffrn_source                   'micro-focus tube'
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS V2014/5 (Bruker AXS Inc.)'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 1324 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.435(17)
_refine_ls_extinction_coef       0.0122(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3680
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0333P)^2^+0.2884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.808
_reflns_friedel_fraction_full    0.936
_reflns_friedel_fraction_max     0.955
_reflns_number_gt                3252
_reflns_number_total             3680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b02014_si_009.cif
_cod_data_source_block
C:\Users\mgg\DOCUME~1\QUESTD~1\15tn002a\15tn002a_0m
_cod_depositor_comments
'Adding full bibliography for 4513736--4513746.cif.'
_cod_database_code               4513741
_shelx_estimated_absorpt_t_min   0.697
_shelx_estimated_absorpt_t_max   0.909
_shelxl_version_number           2014-3
_shelx_res_checksum              4776
_shelx_hkl_checksum              88040