Versatile Syntheses of Optically Pure PCE Pincer Ligands: Facile Modifications of the Pendant Arms and Ligand Backbones
Yang, Xiang-Yuan; Tay, Wee Shan; Li, Yongxin; Pullarkat, Sumod A.; Leung, Pak-Hing; Organometallics 34 (2015) 1582–; doi:10.1021/acs.organomet.5b00132

data_4087442
_publ_section_title
;
 Versatile Syntheses of Optically Pure PCE Pincer Ligands: Facile
 Modifications of the Pendant Arms and Ligand Backbones
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1582
_journal_paper_doi               10.1021/acs.organomet.5b00132
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C55 H55 Cl O2 P2 Pd'
_chemical_formula_weight         951.78
_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'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4806(5)
_cell_length_b                   14.6862(8)
_cell_length_c                   34.3657(15)
_cell_measurement_temperature    103.(2)
_cell_volume                     4784.9(4)
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2014)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2014)'
_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  0.1294
_diffrn_reflns_av_unetI/netI     0.1280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            40241
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.82
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.98
_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    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.543
_refine_ls_abs_structure_details
;
Flack x determined using 1919 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       0.0179(16)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         9058
_refine_ls_number_restraints     1568
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1017P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1911
_reflns_number_gt                5963
_reflns_number_total             9058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00132_si_002.cif
_cod_data_source_block           I
_cod_database_code               4087442
_shelx_res_checksum              22929
_shelx_hkl_checksum              56745