Efficient and Stereo-selective Synthesis of Monomeric and Bi-metallic Pincer Complexes Containing Pd-bonded Stereogenic Carbons
Tay, Wee Shan; Yang, Xiangyuan; Li, Yongxin; Pullarkat, Sumod A.; Leung, Pak-Hing; RSC Adv.  (2016) –; doi:10.1039/C6RA16721G

data_7226115
_publ_section_title
;
 Efficient and Stereo-selective Synthesis of Monomeric and Bi-metallic
 Pincer Complexes Containing Pd-bonded Stereogenic Carbons
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA16721G
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C27 H23 Cl3 N O P Pd S'
_chemical_formula_weight         653.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-03-02 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.963(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7127(5)
_cell_length_b                   11.5076(6)
_cell_length_c                   12.7323(6)
_cell_measurement_reflns_used    3697
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      22.2288
_cell_measurement_theta_min      2.9435
_cell_volume                     1368.21(12)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37087
_diffrn_reflns_theta_full        35.13
_diffrn_reflns_theta_max         35.13
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.960
_refine_diff_density_min         -1.311
_refine_ls_abs_structure_details
;
Flack x determined using 3330 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         12103
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0362P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1103
_reflns_number_gt                9028
_reflns_number_total             12103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra16721g2.cif
_cod_data_source_block           I
_cod_database_code               7226115
_shelx_res_checksum              83856
_solvent_exptl_crystal_recrystallization_method 'DCM, n-hexane'