Pd(0)-Catalyzed Sequential C-N Bond Formation via Allylic and Aromatic C-H Amination of α-Methylstyrenes with Diaziridinone.
Ramirez, Thomas A.; Wang, Qian; Zhu, Yingguang; Zheng, Huaiji; Peng, Xingao; Cornwall, Richard G.; Shi, Yian; Organic letters 15 (2013) 4210–4213; doi:10.1021/ol401935c

data_1512235
_publ_section_title
;
 Pd(0)-Catalyzed Sequential C-N Bond Formation via Allylic and Aromatic
 C-H Amination of \a-Methylstyrenes with Diaziridinone.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4210
_journal_page_last               4213
_journal_paper_doi               10.1021/ol401935c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C26 H37 N3 O'
_chemical_formula_sum            'C26 H37 N3 O'
_chemical_formula_weight         407.59
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 92.418(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_b                   10.4162(3)
_cell_length_c                   20.8009(7)
_cell_measurement_reflns_used    9233
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.17
_cell_measurement_theta_min      2.19
_cell_volume                     2389.52(14)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2009)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0425
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_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            63042
_diffrn_reflns_theta_full        33.39
_diffrn_reflns_theta_max         33.39
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.9709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.43
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_exptl_crystal_size_min          0.25
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         9203
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_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.4325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                6610
_reflns_number_total             9203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol401935c_si_003.cif
_cod_data_source_block           shi02
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512235