The synthesis and efficient one-pot catalytic "self-breeding" of asymmetrical NC(sp(3))E-hybridised pincer complexes.
Yang, Xiang-Yuan; Tay, Wee Shan; Li, Yongxin; Pullarkat, Sumod A.; Leung, Pak-Hing; Chemical communications (Cambridge, England) 52 (2016) 4211–4214; doi:10.1039/c6cc00763e

data_7118767
_publ_section_title
;
 The synthesis and efficient one-pot catalytic &quot;self-breeding&quot;
 of asymmetrical NC(sp(3))E-hybridised pincer complexes.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4211
_journal_page_last               4214
_journal_paper_doi               10.1039/c6cc00763e
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C28 H23 Cl N O P Pd S'
_chemical_formula_weight         594.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-01-22 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3737(3)
_cell_length_b                   12.3461(4)
_cell_length_c                   23.8575(7)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      37.3082
_cell_measurement_theta_min      2.9393
_cell_volume                     2466.45(14)
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            36512
_diffrn_reflns_theta_full        37.90
_diffrn_reflns_theta_max         37.90
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/ethanol'
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.400
_refine_diff_density_max         1.144
_refine_diff_density_min         -2.716
_refine_ls_abs_structure_details
;
Flack x determined using 5201 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.048(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         13283
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0520
_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^)+4.5090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                12637
_reflns_number_total             13283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00763e2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7118767--7118768.cif.'
_cod_database_code               7118767
_shelx_res_checksum              47230