Regioisomerism in coordination chemistry: oxidative addition of bifunctional ligand to palladium, stabilized with 1,2-bis(diphenylphosphino)ethane
Martyanov, Konstantin A.; Cherkasov, Vladimir Kuz'mich; Abakumov, Gleb Arsent'evich; Baranov, Evgeny V.; Shavyrin, Andrey; Kuropatov, Viacheslav; Dalton Transactions  (2017) –; doi:10.1039/C7DT03891G

data_7044727
_publ_section_title
;
 Regioisomerism in coordination chemistry: oxidative addition of
 bifunctional ligand to palladium, stabilized with
 1,2-bis(diphenylphosphino)ethane
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03891G
_journal_year                    2017
_chemical_formula_sum            'C46 H54 O3.5 P2 Pd S2'
_chemical_formula_weight         895.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-09-29 deposited with the CCDC.
2017-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                100.1770(10)
_cell_angle_beta                 106.2630(10)
_cell_angle_gamma                108.5790(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9560(3)
_cell_length_b                   12.6502(4)
_cell_length_c                   17.8929(6)
_cell_measurement_reflns_used    9137
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.80
_cell_volume                     2158.08(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25642
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.102
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.9020
_exptl_absorpt_correction_T_min  0.7955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         10402
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0350P)^2^+1.8686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9902
_reflns_number_total             10402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03891g2.cif
_cod_data_source_block           pdss4m
_cod_original_formula_sum        'C46 H54 O3.50 P2 Pd S2'
_cod_database_code               7044727
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.783
_shelx_estimated_absorpt_t_max   0.939
_shelx_res_checksum              90479