Backbone effects in the synthesis, coordination chemistry and catalytic properties of new chiral heterobidentate ligands with P,N and S,N donor sets
Major, Máté M.; Császár, Zsófia; Bényei, Attila C.; Balogh, Szabolcs; Bakos, József; Farkas, Gergely; Journal of Organometallic Chemistry 921 (2020) 121332–; doi:10.1016/j.jorganchem.2020.121332

data_4038980
_publ_section_title
;
 Backbone effects in the synthesis, coordination chemistry and catalytic
 properties of new chiral heterobidentate ligands with P,N and S,N donor
 sets
;
_journal_name_full               'Journal of Organometallic Chemistry'
_journal_page_first              121332
_journal_paper_doi               10.1016/j.jorganchem.2020.121332
_journal_volume                  921
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H26 Cl2 N P Pd'
_chemical_formula_sum            'C19 H26 Cl2 N P Pd'
_chemical_formula_weight         476.68
_chemical_name_common            CSZS355
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90
_cell_angle_beta                 92.288(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2972(5)
_cell_length_b                   16.7556(7)
_cell_length_c                   11.4331(5)
_cell_measurement_reflns_used    213
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      26.0328
_cell_measurement_theta_min      1.7288
_cell_volume                     2162.46(16)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    Mercury
_computing_publication_material  'WinGX, PublCIF'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \p scan'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           ' Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34994
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         2.16
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    1.18
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.608
_refine_ls_abs_structure_details
;

Flack x determined using 3024 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.039(14)
_refine_ls_extinction_coef       0.0021(4)
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8122
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0280P)^2^+0.9226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                7139
_reflns_number_total             8122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JOC-2020-921-121332.cif
_cod_data_source_block           R_R_R_N_C2
_cod_database_code               4038980