(Aminoalkyl)diphenylphosphine sulfides: synthesis and application as building blocks in the design of multidentate ligands for cytotoxic Pd(II) complexes.
Konovalov, Aleksandr V.; Churusova, Svetlana G.; Aleksanyan, Diana V.; Rybalkina, Ekaterina Yu; Aksenova, Svetlana A.; Peregudov, Alexander S.; Klemenkova, Zinaida S.; Kozlov, Vladimir A.; Organic & biomolecular chemistry 21 (2023) 8379–8392; doi:10.1039/d3ob01309j

data_7159632
_publ_section_title
;
 (Aminoalkyl)diphenylphosphine sulfides: synthesis and application as
 building blocks in the design of multidentate ligands for cytotoxic
 Pd(II) complexes.
;
_journal_issue                   41
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8379
_journal_page_last               8392
_journal_paper_doi               10.1039/d3ob01309j
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C26 H19 Cl N3 O P Pd S, C H Cl3'
_chemical_formula_sum            'C27 H20 Cl4 N3 O P Pd S'
_chemical_formula_weight         713.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                103.396(4)
_cell_angle_beta                 105.449(4)
_cell_angle_gamma                112.525(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9279(7)
_cell_length_b                   12.9563(9)
_cell_length_c                   13.4185(10)
_cell_measurement_reflns_used    4536
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.24
_cell_volume                     1424.7(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15977
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.835
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.0303
_exptl_absorpt_correction_T_min  0.0080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1202 before and 0.0698 after correction.
The Ratio of minimum to maximum transmission is 0.2640.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.374
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1072P)^2^+3.9439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.1976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4926
_reflns_number_total             6197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob01309j2.cif
_cod_data_source_block           8c
_cod_original_cell_volume        1424.69(18)
_cod_database_code               7159632
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C13(H13), C1S(H1S)
1.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C26(H26), C25(H25), C24(H24), C23(H23),
  C22(H22)
;
_shelx_res_checksum              50048
_olex2_submission_special_instructions 'No special instructions were received'