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_4038979
_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         'C13 H21 Cl2 N Pd S, 0.5(H2 O)'
_chemical_formula_sum            'C13 H22 Cl2 N O0.5 Pd S'
_chemical_formula_weight         409.67
_chemical_name_common            S_R_C4
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.5589(6)
_cell_length_b                   19.2664(14)
_cell_length_c                   20.8738(13)
_cell_measurement_reflns_used    1384
_cell_measurement_temperature    298.(2)
_cell_measurement_theta_max      21.5866
_cell_measurement_theta_min      2.0893
_cell_volume                     3442.1(4)
_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      298.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38298
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.793
_refine_ls_abs_structure_details
;

Flack x determined using 2385 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(18)
_refine_ls_extinction_coef       0.0043(3)
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7001
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                6154
_reflns_number_total             7001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JOC-2020-921-121332.cif
_cod_data_source_block           S_R_C4
_cod_depositor_comments
;

2025-07-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C26 H44 Cl4 N2 O Pd2 S2'
_cod_original_formula_weight         819.35
_cod_original_formula_moiety         '2(C13 H21 Cl2 N Pd S), H2 O'
_cod_original_formula_units_Z            4
_cod_database_code               4038979