Unsymmetrical CNN-palladacycles with geometry-constrained iminopyridyl ligands: an efficient precatalyst in Suzuki coupling for accessing 1,1-diarylalkanes from secondary benzylic bromides
Jin, Liqun; Wei, Wei; Sun, Nan; Hu, Baoxiang; Shen, Zhenlu; Hu, Xinquan; Organic Chemistry Frontiers 5 (2018) 2484–; doi:10.1039/C8QO00517F

data_1554361
_publ_section_title
;
 Unsymmetrical CNN-palladacycles with geometry-constrained iminopyridyl
 ligands: an efficient precatalyst in Suzuki coupling for accessing
 1,1-diarylalkanes from secondary benzylic bromides
;
_journal_issue                   16
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              2484
_journal_paper_doi               10.1039/C8QO00517F
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C28 H31 Cl3 N2 Pd'
_chemical_formula_weight         608.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.8900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3174(5)
_cell_length_b                   12.4692(6)
_cell_length_c                   20.4932(10)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.57
_cell_volume                     2617.4(2)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18137
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.331
_exptl_absorpt_coefficient_mu    1.035
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+3.9721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4251
_reflns_number_total             4595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo00517f2.cif
_cod_data_source_block           20180315_ZY1_ping_0m_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1554361
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.836
_shelx_res_checksum              75387
_shelx_hkl_checksum              65297