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_4087446
_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            'C43 H41 Cl3 O8 P2 Pt'
_chemical_formula_weight         1049.14
_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                   10.4318(10)
_cell_length_b                   17.092(2)
_cell_length_c                   24.423(3)
_cell_measurement_reflns_used    4513
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      23.3292
_cell_measurement_theta_min      2.4346
_cell_volume                     4354.6(8)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1304
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            80607
_diffrn_reflns_theta_full        31.13
_diffrn_reflns_theta_max         31.13
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    3.530
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.992
_refine_diff_density_min         -1.597
_refine_ls_abs_structure_details
;
Flack x determined using 4495 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         13941
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0437
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                11589
_reflns_number_total             13941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00132_si_008.cif
_cod_data_source_block           I
_cod_database_code               4087446
_shelx_res_checksum              7904
_shelx_hkl_checksum              58983