Bilateral metalloheterocyclic systems based on palladacycle and piperidine-2,4-dione pharmacophores.
Bulygina, Ludmila A.; Khrushcheva, Natalya S.; Nelyubina, Yulia V.; Dorovatovskii, Pavel; Strelkova, Tatiana V.; Alexeev, Michael S.; Mandegani, Zeinab; Nabavizadeh, S. Masoud; Kuznetsov, Nikolai Yu; Organic & biomolecular chemistry 21 (2023) 2337–2354; doi:10.1039/d3ob00022b

data_7159175
_publ_section_title
;
 Bilateral metalloheterocyclic systems based on palladacycle and
 piperidine-2,4-dione pharmacophores.
;
_journal_issue                   11
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2337
_journal_page_last               2354
_journal_paper_doi               10.1039/d3ob00022b
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C38 H31 Cl N3 O P Pd, C4 H8 O2'
_chemical_formula_sum            'C42 H39 Cl N3 O3 P Pd'
_chemical_formula_weight         806.58
_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             2022-11-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-06 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                96.22(3)
_cell_angle_beta                 101.71(3)
_cell_angle_gamma                113.13(3)
_cell_formula_units_Z            2
_cell_length_a                   10.923(2)
_cell_length_b                   11.870(2)
_cell_length_c                   15.665(3)
_cell_measurement_reflns_used    2452
_cell_measurement_temperature    100
_cell_measurement_theta_max      14.85
_cell_measurement_theta_min      2.26
_cell_volume                     1788.6(8)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type
'MarExperts mardtb goniostat and Rayonix SX 165 detector'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.745
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22484
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         1.423
_exptl_absorpt_coefficient_mu    0.770
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.675
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0057(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0398P)^2^+1.7121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6670
_reflns_number_total             7957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob00022b2.cif
_cod_data_source_block           kuzn3567
_cod_depositor_comments
'Adding full bibliography for 7159174--7159176.cif.'
_cod_database_code               7159175
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3S(H3SA,H3SB)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              69184
_olex2_submission_special_instructions 'No special instructions were received'