Selective synthesis of secondary benzylic (Z)-allylboronates by Fe-catalyzed 1,4-hydroboration of 1-aryl-substituted 1,3-dienes
Cao, Yanchun; Zhang, Yanlu; Zhang, Lei; Zhang, Dan; Leng, Xuebing; Huang, Zheng; Org. Chem. Front. 1 (2014) 1101–; doi:10.1039/C4QO00206G

data_1553031
_publ_section_title
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 Selective synthesis of secondary benzylic (Z)-allylboronates by
 Fe-catalyzed 1,4-hydroboration of 1-aryl-substituted 1,3-dienes
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_journal_issue                   9
_journal_name_full               'Org. Chem. Front.'
_journal_page_first              1101
_journal_paper_doi               10.1039/C4QO00206G
_journal_volume                  1
_journal_year                    2014
_chemical_formula_sum            'C29 H29 Cl2 Fe N2 P'
_chemical_formula_weight         563.26
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.334(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.631(5)
_cell_length_b                   10.038(3)
_cell_length_c                   16.442(4)
_cell_measurement_reflns_used    1149
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      41.160
_cell_measurement_theta_min      4.756
_cell_volume                     2710.5(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1228
_diffrn_reflns_av_sigmaI/netI    0.1142
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17978
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5022
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0592P)^2^+9.0196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1931
_reflns_number_gt                3108
_reflns_number_total             5022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qo00206g2.cif
_cod_data_source_block           dm13751
_cod_depositor_comments
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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/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 '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2710.6(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1553031