Streamlined Synthesis of C(sp<sup>3</sup>)-Rich N-Heterospirocycles Enabled by Visible-Light-Mediated Photocatalysis.
Flodén, Nils J; Trowbridge, Aaron; Willcox, Darren; Walton, Scarlett M.; Kim, Yongjoon; Gaunt, Matthew J.; Journal of the American Chemical Society 141 (2019) 8426–8430; doi:10.1021/jacs.9b03372

data_4127278
_publ_section_title
;
 Streamlined Synthesis of C(sp<sup>3</sup>)-Rich N-Heterospirocycles
 Enabled by Visible-Light-Mediated Photocatalysis.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8426
_journal_page_last               8430
_journal_paper_doi               10.1021/jacs.9b03372
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C19 H26 N2 O2'
_chemical_formula_sum            'C19 H26 N2 O2'
_chemical_formula_weight         314.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
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_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.61
_cell_measurement_theta_min      2.67
_cell_volume                     1767.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
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_diffrn_ambient_temperature      180(2)
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_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_unetI/netI     0.0876
_diffrn_reflns_Laue_measured_fraction_full 0.992
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_diffrn_reflns_limit_h_max       19
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_diffrn_reflns_limit_k_min       -7
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_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11040
_diffrn_reflns_point_group_measured_fraction_full 0.992
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_diffrn_reflns_theta_min         2.670
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
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_exptl_crystal_size_min          0.040
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_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0750
_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^)+(0.0812P)^2^+0.6561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.2021
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_reflns_number_gt                1836
_reflns_number_total             3116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03372_si_003.cif
_cod_data_source_block           MG_B1_0046
_cod_depositor_comments
'Adding full bibliography for 4127277--4127278.cif.'
_cod_database_code               4127278
_cambridge_user_name             'Nils Floden'
_cambridge_user_crsid            njf41
_cambridge_supervisor_name       'Matthew Gaunt'
_cambridge_supervisor_crsid      mjg32
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             NJF-9-048
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_ccdc_publ_extra_info
;
_cambridge_sample_id NJF-9-048
_cambridge_data_id MG_B1_0046
;
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.976