(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_7159634
_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         'C25 H19 Cl F N2 O P Pd S, C H Cl3'
_chemical_formula_sum            'C26 H20 Cl4 F N2 O P Pd S'
_chemical_formula_weight         706.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 95.3030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4217(3)
_cell_length_b                   15.3527(5)
_cell_length_c                   19.3509(5)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.50
_cell_volume                     2787.10(15)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33648
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.114
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1381 before and 0.0445 after correction.
The Ratio of minimum to maximum transmission is 0.6206.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0225P)^2^+2.8751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6226
_reflns_number_total             6733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob01309j2.cif
_cod_data_source_block           8d
_cod_database_code               7159634
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.712
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C13(H13), C1S(H1S)
1.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C2(H2), C7(H7), C8(H8), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25)
;
_shelx_res_checksum              36464
_olex2_submission_special_instructions 'No special instructions were received'