Transition-metal-free C(sp3)–H/C(sp3)–H dehydrogenative coupling of saturated heterocycles with N-benzyl imines
Liu, Zhengfen; Li, Minyan; Deng, Guogang; Wei, Wanshi; Feng, Ping; Zi, Quanxing; Li, Tiantian; Zhang, Hongbin; Yang, Xiaodong; Walsh, Patrick J.; Chemical Science 11 (2020) 7619–7625; doi:10.1039/D0SC00031K

data_1557696
_publ_section_title
;
 Transition-metal-free C(sp3)--H/C(sp3)--H dehydrogenative coupling of
 saturated heterocycles with N-benzyl imines
;
_journal_issue                   29
_journal_name_full               'Chemical Science'
_journal_page_first              7619
_journal_page_last               7625
_journal_paper_doi               10.1039/D0SC00031K
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C25 H26 N2 O'
_chemical_formula_sum            'C25 H26 N2 O'
_chemical_formula_weight         370.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2019-07-30 deposited with the CCDC.	2020-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9067(3)
_cell_length_b                   9.9880(3)
_cell_length_c                   18.4338(5)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    120.(2)
_cell_measurement_theta_max      72.3577
_cell_measurement_theta_min      4.0661
_cell_volume                     2001.78(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.9'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_radiation_monochromator  'Helixos MX multilayer Optic'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16000
_diffrn_reflns_theta_full        72.35
_diffrn_reflns_theta_max         72.35
_diffrn_reflns_theta_min         4.07
_diffrn_source                   'Ius Diamond'
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'translucent light colourless'
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.540
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.397
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.397
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                3756
_reflns_number_total             3934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc00031k2.cif
_cod_data_source_block           zhb_lzf
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1557695--1557696.cif.

 Adding full bibliography for 1557695--1557696.cif.
;
_cod_database_code               1557696
_shelx_res_checksum              24652