Umpolung synthesis of branched α-functionalized amines from imines via photocatalytic three-component reductive coupling reactions.
Fuentes de Arriba, Angel L.; Urbitsch, Felix; Dixon, Darren J.; Chemical communications (Cambridge, England) 52 (2016) 14434–14437; doi:10.1039/c6cc09172e

data_7125308
_publ_section_title
;
 Umpolung synthesis of branched \a-functionalized amines from imines via
 photocatalytic three-component reductive coupling reactions.
;
_journal_issue                   100
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14434
_journal_page_last               14437
_journal_paper_doi               10.1039/c6cc09172e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C22 H25 N1 O5'
_chemical_formula_sum            'C22 H25 N O5'
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_chemical_melting_point          ?
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2016-10-03
_audit_creation_method           CRYSTALS_ver_14.61_build_6019
_audit_update_record
;
2016-10-03 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.598(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   36.3214(19)
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_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      5
_cell_volume                     1957.10(16)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.049
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_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            24541
_diffrn_reflns_theta_full        75.089
_diffrn_reflns_theta_max         76.622
_diffrn_reflns_theta_min         4.870
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            clear_pale_colourless
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_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
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_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     0
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_refine_ls_shift/su_max          0.0005968
_refine_ls_shift/su_mean         0.0000558
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 4.77P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
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_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              45
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                3425
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_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.40
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0626
_oxford_refine_ls_scale          5.21(9)
_oxford_reflns_number_all        4061
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 030djd16
_cod_data_source_file            c6cc09172e2.cif
_cod_data_source_block           16
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C22 H25 N1 O5'
_cod_database_code               7125308